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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ data_global _audit_update_record '2014-09-19 # Formatted by IUCr publCIF' _audit_creation_method 'Jana2006 Version : 20/09/2013' _journal_date_recd_electronic 2014-05-22 _journal_date_from_coeditor 2014-08-06 _journal_date_accepted 2014-08-06 _journal_date_printers_first 2014-09-19 _journal_date_proofs_out 2014-09-19 _journal_date_proofs_in 2014-09-23 _journal_coeditor_code DQ5008 _journal_paper_doi https://doi.org/10.1107/S205252061401806X _journal_techeditor_code B141806 _iucr_compatibility_tag ACTA95 _journal_paper_category FA _journal_coden_ASTM ASBSDK _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2014 _journal_volume 70 _journal_issue 05 _journal_page_first 879 _journal_page_last 887 _publ_contact_author_name 'Muller, Carola J.' _publ_contact_author_address ; Centre for Analysis and Synthesis Lund University Box 124 22100 Lund Sweden ; _publ_contact_author_email carola.muller@chem.lu.se _publ_requested_journal 'Acta Crystallographica Section B' _publ_section_title 'Cu~3~Sn - understanding the systematic absences' _publ_section_title_footnote ? loop_ _publ_author_name _publ_author_address 'Muller, Carola J.' ; Centre for Analysis and Synthesis Lind University Box 124 22100 Lund Sweden ; 'Lidin, Sven' ; Centre for Analysis and Synthesis Lind University Box 124 22100 Lund Sweden ; data_473K-superstructure _chemical_name_common 'Cu3 Sn1' _chemical_formula_sum 'Cu3 Sn1' _chemical_formula_weight 309.3 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C -2x;-2yc;-2zc' _space_group_IT_number 63 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z+1/2 3 -x,y,-z+1/2 4 x,-y,-z 5 -x,-y,-z 6 x,y,-z+1/2 7 x,-y,z+1/2 8 -x,y,z 9 x+1/2,y+1/2,z 10 -x+1/2,-y+1/2,z+1/2 11 -x+1/2,y+1/2,-z+1/2 12 x+1/2,-y+1/2,-z 13 -x+1/2,-y+1/2,-z 14 x+1/2,y+1/2,-z+1/2 15 x+1/2,-y+1/2,z+1/2 16 -x+1/2,y+1/2,z _cell_length_a 5.5210(2) _cell_length_b 47.781(3) _cell_length_c 4.3340(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1143.30(10) _cell_formula_units_Z 20 _cell_measurement_reflns_used 780 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 28.39 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 8.983 _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 37.873 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.061 _exptl_crystal_size_mid 0.023 _exptl_crystal_size_min 0.017 _exptl_crystal_colour 'metallic grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.372 _exptl_absorpt_correction_T_max 0.7 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 5911 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.39 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -61 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 851 _reflns_number_gt 332 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_gt 0.1300 _refine_ls_R_factor_all 0.0966 _refine_ls_wR_factor_ref 0.1719 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_goodness_of_fit_gt 1.52 _refine_ls_number_reflns 851 _refine_ls_number_parameters 72 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0035999999I^2^) _refine_ls_shift/su_max 0.0399 _refine_ls_shift/su_mean 0.0079 _refine_diff_density_max 2.22 _refine_diff_density_min -2.36 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 43(13) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.33365(4) 0.25 Uani 0.0061(6) 4 1 d ? ? ? Sn2 Sn 0.5 0.36610(4) -0.25 Uani 0.0074(6) 4 1 d ? ? ? Sn3 Sn 0.5 0.26620(4) -0.25 Uani 0.0043(5) 4 1 d ? ? ? Cu1 Cu 0.2480(3) 0.38408(7) 0.25 Uani 0.0124(11) 8 1 d ? ? ? Cu2 Cu 0.2402(3) 0.48427(7) -0.75 Uani 0.0108(10) 8 1 d ? ? ? Cu3 Cu 0.2521(3) 0.41582(7) -0.25 Uani 0.0135(11) 8 1 d ? ? ? Cu4 Cu 0.2526(3) 0.31614(6) -0.25 Uani 0.0065(10) 8 1 d ? ? ? Cu5 Cu 0.2485(3) 0.28401(6) 0.25 Uani 0.0066(10) 8 1 d ? ? ? Sn4 Sn 0.5 0.46640(4) -0.25 Uani 0.0081(6) 4 1 d ? ? ? Sn5 Sn 0 0.43334(4) -0.75 Uani 0.0089(7) 4 1 d ? ? ? Cu6 Cu 0.5 0.43178(7) -0.75 Uani 0.0079(11) 4 1 d ? ? ? Cu7 Cu 0 0.46921(7) -1.25 Uani 0.0057(10) 4 1 d ? ? ? Cu8 Cu 0 0.36961(7) -0.25 Uani 0.0103(11) 4 1 d ? ? ? Cu9 Cu 0 0.26929(8) -0.25 Uani 0.0089(11) 4 1 d ? ? ? Cu10 Cu -0.5 0.33070(7) 0.25 Uani 0.0078(10) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0046(10) 0.0066(9) 0.0072(12) 0 0 0 Sn2 Sn 0.0076(11) 0.0069(9) 0.0077(13) 0 0 0 Sn3 Sn 0.0046(10) 0.0050(8) 0.0032(11) 0 0 0 Cu1 Cu 0.016(2) 0.0143(16) 0.007(2) 0.0005(7) 0 0 Cu2 Cu 0.0104(17) 0.0128(14) 0.009(2) -0.0015(6) 0 0 Cu3 Cu 0.0142(19) 0.0114(16) 0.015(2) -0.0011(7) 0 0 Cu4 Cu 0.0049(16) 0.0087(14) 0.006(2) -0.0016(6) 0 0 Cu5 Cu 0.0112(18) 0.0008(12) 0.008(2) 0.0002(5) 0 0 Sn4 Sn 0.0078(11) 0.0089(9) 0.0077(12) 0 0 0 Sn5 Sn 0.0092(11) 0.0082(9) 0.0092(13) 0 0 0 Cu6 Cu 0.0038(18) 0.0155(17) 0.004(2) 0 0 0 Cu7 Cu 0.0036(18) 0.0094(16) 0.004(2) 0 0 0 Cu8 Cu 0.010(2) 0.0091(16) 0.011(2) 0 0 0 Cu9 Cu 0.0075(18) 0.0124(15) 0.007(2) 0 0 0 Cu10 Cu 0.0037(17) 0.0121(16) 0.008(2) 0 0 0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 Sn1 ? 1_455 5.5210(4) ? Sn1 Sn1 ? 1_554 4.3340(4) ? Sn1 Sn1 ? 1_556 4.3340(4) ? Sn1 Sn1 ? 1_655 5.5210(4) ? Sn1 Sn2 ? 1_455 3.8367(11) ? Sn1 Sn2 ? 1_456 3.8367(11) ? Sn1 Sn2 ? ? 3.8370(11) ? Sn1 Sn2 ? 1_556 3.8369(11) ? Sn1 Sn3 ? 1_455 4.7647(18) ? Sn1 Sn3 ? 1_456 4.7648(18) ? Sn1 Sn3 ? ? 4.7643(18) ? Sn1 Sn3 ? 1_556 4.7644(18) ? Sn1 Sn3 ? 10_555 4.771(3) ? Sn1 Cu1 ? 1_455 4.800(2) ? Sn1 Cu1 ? 1_554 5.1444(19) ? Sn1 Cu1 ? ? 2.771(3) ? Sn1 Cu1 ? 1_556 5.1443(19) ? Sn1 Cu1 ? 3_554 5.1443(19) ? Sn1 Cu1 ? 3_555 2.771(3) ? Sn1 Cu1 ? 3_556 5.1442(19) ? Sn1 Cu1 ? 3_655 4.801(2) ? Sn1 Cu3 ? ? 4.696(3) ? Sn1 Cu3 ? 1_556 4.696(3) ? Sn1 Cu3 ? 3_554 4.696(3) ? Sn1 Cu3 ? 3_555 4.695(3) ? Sn1 Cu4 ? 1_455 4.7355(15) ? Sn1 Cu4 ? 1_456 4.7355(15) ? Sn1 Cu4 ? ? 2.7091(13) ? Sn1 Cu4 ? 1_556 2.7092(13) ? Sn1 Cu4 ? 3_554 2.7092(13) ? Sn1 Cu4 ? 3_555 2.7093(13) ? Sn1 Cu4 ? 3_654 4.7353(15) ? Sn1 Cu4 ? 3_655 4.7353(15) ? Sn1 Cu5 ? 1_455 4.779(2) ? Sn1 Cu5 ? 1_554 5.1274(16) ? Sn1 Cu5 ? ? 2.740(3) ? Sn1 Cu5 ? 1_556 5.1276(16) ? Sn1 Cu5 ? 3_554 5.1276(16) ? Sn1 Cu5 ? 3_555 2.740(3) ? Sn1 Cu5 ? 3_556 5.1277(16) ? Sn1 Cu5 ? 3_655 4.779(2) ? Sn1 Sn5 ? 1_556 4.763(3) ? Sn1 Cu6 ? 1_456 5.441(3) ? Sn1 Cu6 ? 1_556 5.441(3) ? Sn1 Cu8 ? ? 2.765(2) ? Sn1 Cu8 ? 1_556 2.765(2) ? Sn1 Cu9 ? ? 3.762(3) ? Sn1 Cu9 ? 1_556 3.762(3) ? Sn1 Cu9 ? 10_455 5.640(4) ? Sn1 Cu9 ? 10_555 5.640(4) ? Sn1 Cu10 ? 1_554 5.1404(4) ? Sn1 Cu10 ? ? 2.7641(3) ? Sn1 Cu10 ? 1_556 5.1404(4) ? Sn1 Cu10 ? 1_654 5.1404(4) ? Sn1 Cu10 ? 1_655 2.7641(3) ? Sn1 Cu10 ? 1_656 5.1404(4) ? Sn2 Sn2 ? 1_455 5.5210(4) ? Sn2 Sn2 ? 1_554 4.3340(4) ? Sn2 Sn2 ? 1_556 4.3340(4) ? Sn2 Sn2 ? 1_655 5.5210(4) ? Sn2 Sn3 ? ? 4.773(3) ? Sn2 Cu1 ? 1_554 2.7146(15) ? Sn2 Cu1 ? ? 2.7146(15) ? Sn2 Cu1 ? 1_654 4.7421(16) ? Sn2 Cu1 ? 1_655 4.7421(16) ? Sn2 Cu1 ? 3_554 4.7420(16) ? Sn2 Cu1 ? 3_555 4.7420(16) ? Sn2 Cu1 ? 3_654 2.7147(15) ? Sn2 Cu1 ? 3_655 2.7147(15) ? Sn2 Cu3 ? 1_554 5.1283(18) ? Sn2 Cu3 ? ? 2.741(3) ? Sn2 Cu3 ? 1_556 5.1281(18) ? Sn2 Cu3 ? 1_655 4.784(2) ? Sn2 Cu3 ? 3_554 4.784(2) ? Sn2 Cu3 ? 3_653 5.1284(18) ? Sn2 Cu3 ? 3_654 2.742(3) ? Sn2 Cu3 ? 3_655 5.1283(18) ? Sn2 Cu4 ? 1_554 5.1330(17) ? Sn2 Cu4 ? ? 2.750(3) ? Sn2 Cu4 ? 1_556 5.1332(17) ? Sn2 Cu4 ? 1_655 4.792(2) ? Sn2 Cu4 ? 3_554 4.792(2) ? Sn2 Cu4 ? 3_653 5.1329(17) ? Sn2 Cu4 ? 3_654 2.750(3) ? Sn2 Cu4 ? 3_655 5.1330(17) ? Sn2 Cu5 ? 1_554 4.691(3) ? Sn2 Cu5 ? ? 4.692(3) ? Sn2 Cu5 ? 3_654 4.691(3) ? Sn2 Cu5 ? 3_655 4.691(3) ? Sn2 Sn4 ? ? 4.792(3) ? Sn2 Sn5 ? ? 4.7576(18) ? Sn2 Sn5 ? 1_556 4.7575(18) ? Sn2 Sn5 ? 1_655 4.7580(18) ? Sn2 Sn5 ? 1_656 4.7579(18) ? Sn2 Cu6 ? ? 3.814(3) ? Sn2 Cu6 ? 1_556 3.814(3) ? Sn2 Cu7 ? 1_556 5.647(3) ? Sn2 Cu7 ? 1_656 5.647(3) ? Sn2 Cu8 ? 1_554 5.1412(4) ? Sn2 Cu8 ? ? 2.7655(3) ? Sn2 Cu8 ? 1_556 5.1412(4) ? Sn2 Cu8 ? 1_654 5.1412(4) ? Sn2 Cu8 ? 1_655 2.7656(3) ? Sn2 Cu8 ? 1_656 5.1412(4) ? Sn2 Cu9 ? ? 5.387(4) ? Sn2 Cu9 ? 1_655 5.387(4) ? Sn2 Cu10 ? 1_654 2.749(2) ? Sn2 Cu10 ? 1_655 2.749(2) ? Sn3 Sn3 ? 1_455 5.5210(4) ? Sn3 Sn3 ? 1_554 4.3340(4) ? Sn3 Sn3 ? 1_556 4.3340(4) ? Sn3 Sn3 ? 1_655 5.5210(4) ? Sn3 Sn3 ? 10_554 3.8360(11) ? Sn3 Sn3 ? 10_555 3.8360(11) ? Sn3 Sn3 ? 10_654 3.8357(11) ? Sn3 Sn3 ? 10_655 3.8358(11) ? Sn3 Cu4 ? 1_554 5.1327(17) ? Sn3 Cu4 ? ? 2.750(3) ? Sn3 Cu4 ? 1_556 5.1325(17) ? Sn3 Cu4 ? 1_655 4.792(2) ? Sn3 Cu4 ? 10_554 4.704(3) ? Sn3 Cu4 ? 10_555 4.704(3) ? Sn3 Cu4 ? 3_554 4.791(2) ? Sn3 Cu4 ? 3_653 5.1328(17) ? Sn3 Cu4 ? 3_654 2.750(3) ? Sn3 Cu4 ? 3_655 5.1326(17) ? Sn3 Cu4 ? 12_554 4.703(3) ? Sn3 Cu4 ? 12_555 4.703(3) ? Sn3 Cu5 ? 1_554 2.7105(13) ? Sn3 Cu5 ? ? 2.7105(13) ? Sn3 Cu5 ? 1_654 4.7435(15) ? Sn3 Cu5 ? 1_655 4.7434(15) ? Sn3 Cu5 ? 10_553 5.1404(17) ? Sn3 Cu5 ? 10_554 2.764(3) ? Sn3 Cu5 ? 10_555 5.1405(17) ? Sn3 Cu5 ? 10_654 4.792(2) ? Sn3 Cu5 ? 3_554 4.7433(15) ? Sn3 Cu5 ? 3_555 4.7433(15) ? Sn3 Cu5 ? 3_654 2.7106(13) ? Sn3 Cu5 ? 3_655 2.7106(13) ? Sn3 Cu5 ? 12_455 4.793(2) ? Sn3 Cu5 ? 12_554 5.1402(17) ? Sn3 Cu5 ? 12_555 2.764(3) ? Sn3 Cu5 ? 12_556 5.1404(17) ? Sn3 Cu8 ? ? 5.659(3) ? Sn3 Cu8 ? 1_655 5.660(3) ? Sn3 Cu9 ? 1_554 5.1406(4) ? Sn3 Cu9 ? ? 2.7644(3) ? Sn3 Cu9 ? 1_556 5.1406(4) ? Sn3 Cu9 ? 1_654 5.1406(4) ? Sn3 Cu9 ? 1_655 2.7644(3) ? Sn3 Cu9 ? 1_656 5.1406(4) ? Sn3 Cu9 ? 10_554 2.752(3) ? Sn3 Cu9 ? 10_555 2.752(3) ? Sn3 Cu10 ? 1_654 3.767(3) ? Sn3 Cu10 ? 1_655 3.767(3) ? Sn3 Cu10 ? 10_454 5.391(3) ? Sn3 Cu10 ? 10_554 5.390(3) ? Cu1 Cu1 ? 1_455 5.521(2) ? Cu1 Cu1 ? 1_554 4.3340(4) ? Cu1 Cu1 ? 1_556 4.3340(4) ? Cu1 Cu1 ? 1_655 5.521(2) ? Cu1 Cu1 ? 3_554 5.1265(13) ? Cu1 Cu1 ? 3_555 2.738(2) ? Cu1 Cu1 ? 3_556 5.1265(13) ? Cu1 Cu1 ? 3_654 5.1505(13) ? Cu1 Cu1 ? 3_655 2.783(2) ? Cu1 Cu1 ? 3_656 5.1505(13) ? Cu1 Cu2 ? 1_556 4.787(5) ? Cu1 Cu2 ? 3_554 5.494(4) ? Cu1 Cu2 ? 3_654 5.559(4) ? Cu1 Cu3 ? ? 2.645(3) ? Cu1 Cu3 ? 1_556 2.645(3) ? Cu1 Cu3 ? 3_554 3.823(2) ? Cu1 Cu3 ? 3_555 3.823(2) ? Cu1 Cu3 ? 3_654 3.823(2) ? Cu1 Cu3 ? 3_655 3.823(2) ? Cu1 Cu4 ? ? 3.903(4) ? Cu1 Cu4 ? 1_556 3.903(4) ? Cu1 Cu4 ? 3_554 4.782(3) ? Cu1 Cu4 ? 3_555 4.782(3) ? Cu1 Cu4 ? 3_654 4.778(3) ? Cu1 Cu4 ? 3_655 4.778(3) ? Cu1 Cu5 ? ? 4.781(4) ? Cu1 Cu5 ? 3_555 5.512(4) ? Cu1 Cu5 ? 3_655 5.530(4) ? Cu1 Sn4 ? ? 4.702(3) ? Cu1 Sn4 ? 1_556 4.701(3) ? Cu1 Sn5 ? ? 5.1184(19) ? Cu1 Sn5 ? 1_556 2.723(3) ? Cu1 Sn5 ? 1_557 5.1183(19) ? Cu1 Sn5 ? 1_656 4.773(2) ? Cu1 Cu6 ? 1_456 4.717(3) ? Cu1 Cu6 ? ? 5.091(2) ? Cu1 Cu6 ? 1_556 2.671(4) ? Cu1 Cu6 ? 1_557 5.091(2) ? Cu1 Cu7 ? 1_556 4.808(4) ? Cu1 Cu7 ? 1_557 4.808(4) ? Cu1 Cu8 ? ? 2.6549(15) ? Cu1 Cu8 ? 1_556 2.6550(15) ? Cu1 Cu8 ? 1_655 4.7341(16) ? Cu1 Cu8 ? 1_656 4.7341(16) ? Cu1 Cu10 ? ? 4.854(3) ? Cu1 Cu10 ? 1_654 5.218(2) ? Cu1 Cu10 ? 1_655 2.905(4) ? Cu1 Cu10 ? 1_656 5.218(2) ? Cu2 Cu2 ? 1_455 5.521(2) ? Cu2 Cu2 ? 1_554 4.3340(4) ? Cu2 Cu2 ? 1_556 4.3340(4) ? Cu2 Cu2 ? 1_655 5.521(2) ? Cu2 Cu2 ? 2_564 3.741(3) ? Cu2 Cu2 ? 2_565 3.740(3) ? Cu2 Cu2 ? 2_664 3.897(3) ? Cu2 Cu2 ? 2_665 3.897(3) ? Cu2 Cu2 ? 3_552 5.0813(13) ? Cu2 Cu2 ? 3_553 2.653(2) ? Cu2 Cu2 ? 3_554 5.0813(13) ? Cu2 Cu2 ? 3_652 5.1972(14) ? Cu2 Cu2 ? 3_653 2.868(2) ? Cu2 Cu2 ? 3_654 5.1972(14) ? Cu2 Cu2 ? 4_563 2.637(3) ? Cu2 Cu2 ? 4_564 2.637(3) ? Cu2 Cu3 ? 1_554 3.924(4) ? Cu2 Cu3 ? ? 3.924(4) ? Cu2 Cu3 ? 2_564 5.493(4) ? Cu2 Cu3 ? 2_664 5.536(4) ? Cu2 Cu3 ? 3_553 4.773(3) ? Cu2 Cu3 ? 3_554 4.773(3) ? Cu2 Cu3 ? 3_653 4.821(3) ? Cu2 Cu3 ? 3_654 4.821(3) ? Cu2 Cu3 ? 4_564 4.774(5) ? Cu2 Sn4 ? 1_454 4.7040(17) ? Cu2 Sn4 ? 1_455 4.7040(17) ? Cu2 Sn4 ? 1_554 2.7352(15) ? Cu2 Sn4 ? ? 2.7353(15) ? Cu2 Sn4 ? 2_564 4.718(2) ? Cu2 Sn4 ? 2_663 5.1379(19) ? Cu2 Sn4 ? 2_664 2.759(3) ? Cu2 Sn4 ? 2_665 5.1378(19) ? Cu2 Sn5 ? 1_554 5.1444(19) ? Cu2 Sn5 ? ? 2.772(3) ? Cu2 Sn5 ? 1_556 5.1445(19) ? Cu2 Sn5 ? 1_655 4.849(2) ? Cu2 Sn5 ? 2_564 4.685(3) ? Cu2 Sn5 ? 2_565 4.685(3) ? Cu2 Cu6 ? 1_455 4.795(3) ? Cu2 Cu6 ? 1_554 5.209(2) ? Cu2 Cu6 ? ? 2.889(4) ? Cu2 Cu6 ? 1_556 5.209(2) ? Cu2 Cu6 ? 2_664 4.780(4) ? Cu2 Cu6 ? 2_665 4.779(4) ? Cu2 Cu7 ? ? 2.6407(15) ? Cu2 Cu7 ? 1_556 2.6407(15) ? Cu2 Cu7 ? 1_655 4.7758(17) ? Cu2 Cu7 ? 1_656 4.7759(17) ? Cu2 Cu7 ? 2_564 5.048(2) ? Cu2 Cu7 ? 2_565 2.588(4) ? Cu2 Cu7 ? 2_566 5.048(2) ? Cu2 Cu7 ? 2_665 4.748(3) ? Cu3 Cu3 ? 1_455 5.521(2) ? Cu3 Cu3 ? 1_554 4.3340(4) ? Cu3 Cu3 ? 1_556 4.3340(4) ? Cu3 Cu3 ? 1_655 5.521(2) ? Cu3 Cu3 ? 3_553 5.1511(13) ? Cu3 Cu3 ? 3_554 2.784(2) ? Cu3 Cu3 ? 3_555 5.1511(13) ? Cu3 Cu3 ? 3_653 5.1259(13) ? Cu3 Cu3 ? 3_654 2.737(2) ? Cu3 Cu3 ? 3_655 5.1259(13) ? Cu3 Cu4 ? ? 4.763(4) ? Cu3 Cu4 ? 3_554 5.518(4) ? Cu3 Cu4 ? 3_654 5.492(4) ? Cu3 Sn4 ? 1_455 4.804(2) ? Cu3 Sn4 ? 1_554 5.1476(18) ? Cu3 Sn4 ? ? 2.777(3) ? Cu3 Sn4 ? 1_556 5.1475(18) ? Cu3 Sn5 ? ? 2.7081(14) ? Cu3 Sn5 ? 1_556 2.7081(14) ? Cu3 Sn5 ? 1_655 4.7378(16) ? Cu3 Sn5 ? 1_656 4.7377(16) ? Cu3 Cu6 ? 1_455 4.7455(16) ? Cu3 Cu6 ? 1_456 4.7455(16) ? Cu3 Cu6 ? ? 2.6741(16) ? Cu3 Cu6 ? 1_556 2.6740(16) ? Cu3 Cu7 ? ? 5.218(2) ? Cu3 Cu7 ? 1_556 2.906(4) ? Cu3 Cu7 ? 1_557 5.218(2) ? Cu3 Cu7 ? 1_656 4.854(3) ? Cu3 Cu8 ? 1_554 5.059(2) ? Cu3 Cu8 ? ? 2.610(4) ? Cu3 Cu8 ? 1_556 5.059(2) ? Cu3 Cu8 ? 1_655 4.682(3) ? Cu3 Cu10 ? 1_654 4.807(4) ? Cu3 Cu10 ? 1_655 4.807(4) ? Cu4 Cu4 ? 1_455 5.521(2) ? Cu4 Cu4 ? 1_554 4.3340(4) ? Cu4 Cu4 ? 1_556 4.3340(4) ? Cu4 Cu4 ? 1_655 5.521(2) ? Cu4 Cu4 ? 3_553 5.1537(12) ? Cu4 Cu4 ? 3_554 2.789(2) ? Cu4 Cu4 ? 3_555 5.1537(12) ? Cu4 Cu4 ? 3_653 5.1233(12) ? Cu4 Cu4 ? 3_654 2.732(2) ? Cu4 Cu4 ? 3_655 5.1233(12) ? Cu4 Cu5 ? 1_554 2.656(2) ? Cu4 Cu5 ? ? 2.656(2) ? Cu4 Cu5 ? 10_554 4.786(4) ? Cu4 Cu5 ? 3_554 3.835(2) ? Cu4 Cu5 ? 3_555 3.835(2) ? Cu4 Cu5 ? 3_654 3.826(2) ? Cu4 Cu5 ? 3_655 3.826(2) ? Cu4 Cu5 ? 12_455 5.536(4) ? Cu4 Cu5 ? 12_555 5.513(4) ? Cu4 Cu8 ? 1_554 5.220(2) ? Cu4 Cu8 ? ? 2.910(4) ? Cu4 Cu8 ? 1_556 5.220(2) ? Cu4 Cu8 ? 1_655 4.853(3) ? Cu4 Cu9 ? 1_554 5.074(2) ? Cu4 Cu9 ? ? 2.638(4) ? Cu4 Cu9 ? 1_556 5.074(2) ? Cu4 Cu9 ? 1_655 4.695(3) ? Cu4 Cu9 ? 10_554 4.819(4) ? Cu4 Cu9 ? 10_555 4.819(4) ? Cu4 Cu10 ? 1_554 4.7373(15) ? Cu4 Cu10 ? ? 4.7373(15) ? Cu4 Cu10 ? 1_654 2.6544(14) ? Cu4 Cu10 ? 1_655 2.6544(14) ? Cu5 Cu5 ? 1_455 5.521(2) ? Cu5 Cu5 ? 1_554 4.3340(4) ? Cu5 Cu5 ? 1_556 4.3340(4) ? Cu5 Cu5 ? 1_655 5.521(2) ? Cu5 Cu5 ? 10_554 3.906(3) ? Cu5 Cu5 ? 10_555 3.906(3) ? Cu5 Cu5 ? 3_554 5.1299(12) ? Cu5 Cu5 ? 3_555 2.745(2) ? Cu5 Cu5 ? 3_556 5.1299(12) ? Cu5 Cu5 ? 3_654 5.1471(13) ? Cu5 Cu5 ? 3_655 2.776(2) ? Cu5 Cu5 ? 3_656 5.1471(13) ? Cu5 Cu5 ? 12_455 4.783(3) ? Cu5 Cu5 ? 12_456 4.784(3) ? Cu5 Cu5 ? 12_555 4.783(3) ? Cu5 Cu5 ? 12_556 4.783(3) ? Cu5 Cu8 ? ? 4.828(4) ? Cu5 Cu8 ? 1_556 4.827(4) ? Cu5 Cu9 ? ? 2.6597(15) ? Cu5 Cu9 ? 1_556 2.6598(15) ? Cu5 Cu9 ? 1_655 4.7331(16) ? Cu5 Cu9 ? 1_656 4.7331(16) ? Cu5 Cu9 ? 10_455 4.855(3) ? Cu5 Cu9 ? 10_554 5.215(2) ? Cu5 Cu9 ? 10_555 2.900(4) ? Cu5 Cu9 ? 10_556 5.215(2) ? Cu5 Cu10 ? ? 4.696(3) ? Cu5 Cu10 ? 1_654 5.068(2) ? Cu5 Cu10 ? 1_655 2.628(4) ? Cu5 Cu10 ? 1_656 5.068(2) ? Sn4 Sn4 ? 1_455 5.5210(4) ? Sn4 Sn4 ? 1_554 4.3340(4) ? Sn4 Sn4 ? 1_556 4.3340(4) ? Sn4 Sn4 ? 1_655 5.5210(4) ? Sn4 Sn4 ? 2_664 3.874(2) ? Sn4 Sn4 ? 2_665 3.874(2) ? Sn4 Sn5 ? ? 3.8486(11) ? Sn4 Sn5 ? 1_556 3.8487(11) ? Sn4 Sn5 ? 1_655 3.8484(11) ? Sn4 Sn5 ? 1_656 3.8485(11) ? Sn4 Sn5 ? 2_565 5.529(2) ? Sn4 Sn5 ? 2_665 5.529(2) ? Sn4 Cu6 ? ? 2.726(2) ? Sn4 Cu6 ? 1_556 2.726(2) ? Sn4 Cu6 ? 2_665 4.865(4) ? Sn4 Cu7 ? ? 5.1402(4) ? Sn4 Cu7 ? 1_556 2.7637(3) ? Sn4 Cu7 ? 1_557 5.1402(4) ? Sn4 Cu7 ? 1_655 5.1402(4) ? Sn4 Cu7 ? 1_656 2.7638(3) ? Sn4 Cu7 ? 1_657 5.1402(4) ? Sn4 Cu7 ? 2_565 4.667(2) ? Sn4 Cu7 ? 2_566 4.667(2) ? Sn4 Cu7 ? 2_665 4.668(2) ? Sn4 Cu7 ? 2_666 4.667(2) ? Sn4 Cu8 ? ? 5.386(3) ? Sn4 Cu8 ? 1_655 5.386(3) ? Sn5 Sn5 ? 1_455 5.5210(4) ? Sn5 Sn5 ? 1_554 4.3340(4) ? Sn5 Sn5 ? 1_556 4.3340(4) ? Sn5 Sn5 ? 1_655 5.5210(4) ? Sn5 Cu6 ? 1_454 5.1390(4) ? Sn5 Cu6 ? 1_455 2.7615(2) ? Sn5 Cu6 ? 1_456 5.1390(4) ? Sn5 Cu6 ? 1_554 5.1390(4) ? Sn5 Cu6 ? ? 2.7615(2) ? Sn5 Cu6 ? 1_556 5.1390(4) ? Sn5 Cu7 ? ? 2.763(2) ? Sn5 Cu7 ? 1_556 2.763(2) ? Sn5 Cu7 ? 2_565 4.656(4) ? Sn5 Cu8 ? 1_554 3.737(3) ? Sn5 Cu8 ? ? 3.738(3) ? Sn5 Cu10 ? 1_554 5.628(3) ? Sn5 Cu10 ? 1_654 5.628(3) ? Cu6 Cu6 ? 1_455 5.5210(4) ? Cu6 Cu6 ? 1_554 4.3340(4) ? Cu6 Cu6 ? 1_556 4.3340(4) ? Cu6 Cu6 ? 1_655 5.5210(4) ? Cu6 Cu7 ? ? 3.939(2) ? Cu6 Cu7 ? 1_556 3.939(2) ? Cu6 Cu7 ? 1_655 3.939(2) ? Cu6 Cu7 ? 1_656 3.939(2) ? Cu6 Cu7 ? 2_565 5.477(4) ? Cu6 Cu7 ? 2_665 5.478(4) ? Cu6 Cu8 ? 1_554 4.598(3) ? Cu6 Cu8 ? ? 4.598(3) ? Cu6 Cu8 ? 1_654 4.598(3) ? Cu6 Cu8 ? 1_655 4.598(3) ? Cu6 Cu10 ? 1_654 4.830(5) ? Cu7 Cu7 ? 1_455 5.5210(4) ? Cu7 Cu7 ? 1_554 4.3340(4) ? Cu7 Cu7 ? 1_556 4.3340(4) ? Cu7 Cu7 ? 1_655 5.5210(4) ? Cu7 Cu7 ? 2_564 3.655(4) ? Cu7 Cu7 ? 2_565 3.654(4) ? Cu7 Cu8 ? 1_554 4.759(5) ? Cu8 Cu8 ? 1_455 5.5210(4) ? Cu8 Cu8 ? 1_554 4.3340(4) ? Cu8 Cu8 ? 1_556 4.3340(4) ? Cu8 Cu8 ? 1_655 5.5210(4) ? Cu8 Cu9 ? ? 4.793(5) ? Cu8 Cu10 ? 1_554 3.972(2) ? Cu8 Cu10 ? ? 3.972(2) ? Cu8 Cu10 ? 1_654 3.971(2) ? Cu8 Cu10 ? 1_655 3.971(2) ? Cu9 Cu9 ? 1_455 5.5210(4) ? Cu9 Cu9 ? 1_554 4.3340(4) ? Cu9 Cu9 ? 1_556 4.3340(4) ? Cu9 Cu9 ? 1_655 5.5210(4) ? Cu9 Cu9 ? 10_454 3.964(2) ? Cu9 Cu9 ? 10_455 3.964(2) ? Cu9 Cu9 ? 10_554 3.964(2) ? Cu9 Cu9 ? 10_555 3.964(2) ? Cu9 Cu10 ? 1_554 4.574(3) ? Cu9 Cu10 ? ? 4.574(3) ? Cu9 Cu10 ? 1_654 4.575(3) ? Cu9 Cu10 ? 1_655 4.575(3) ? Cu9 Cu10 ? 10_454 4.777(5) ? Cu10 Cu10 ? 1_455 5.5210(4) ? Cu10 Cu10 ? 1_554 4.3340(4) ? Cu10 Cu10 ? 1_556 4.3340(4) ? Cu10 Cu10 ? 1_655 5.5210(4) ? data_573K-superstructure _chemical_formula_structural 'Cu3 Sn1' _chemical_formula_sum 'Cu3 Sn1' _chemical_formula_weight 309.3 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C -2x;-2yc;-2zc' _space_group_IT_number 63 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z+1/2 3 -x,y,-z+1/2 4 x,-y,-z 5 -x,-y,-z 6 x,y,-z+1/2 7 x,-y,z+1/2 8 -x,y,z 9 x+1/2,y+1/2,z 10 -x+1/2,-y+1/2,z+1/2 11 -x+1/2,y+1/2,-z+1/2 12 x+1/2,-y+1/2,-z 13 -x+1/2,-y+1/2,-z 14 x+1/2,y+1/2,-z+1/2 15 x+1/2,-y+1/2,z+1/2 16 -x+1/2,y+1/2,z _cell_length_a 5.5185(3) _cell_length_b 47.768(2) _cell_length_c 4.3320(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1141.95(9) _cell_formula_units_Z 20 _cell_measurement_reflns_used 1456 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 28.08 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 8.9937 _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 37.918 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.094 _exptl_crystal_size_mid 0.047 _exptl_crystal_size_min 0.028 _exptl_crystal_colour 'metallic dark grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.227 _exptl_absorpt_correction_T_max 0.551 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 8193 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.08 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0151 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -62 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 840 _reflns_number_gt 382 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_gt 0.0921 _refine_ls_R_factor_all 0.0652 _refine_ls_wR_factor_ref 0.1068 _refine_ls_goodness_of_fit_ref 1.62 _refine_ls_goodness_of_fit_gt 2.20 _refine_ls_number_reflns 840 _refine_ls_number_parameters 72 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0497 _refine_ls_shift/su_mean 0.0098 _refine_diff_density_max 1.75 _refine_diff_density_min -1.84 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 194(10) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.33372(3) 0.25 Uani 0.0076(5) 4 1 d ? ? ? Sn2 Sn 0.5 0.26613(4) 0.75 Uani 0.0065(5) 4 1 d ? ? ? Sn3 Sn 0.5 0.36618(4) 0.75 Uani 0.0062(5) 4 1 d ? ? ? Sn4 Sn 0.5 0.46628(4) 0.75 Uani 0.0081(5) 4 1 d ? ? ? Cu1 Cu 0.5 0.43182(7) 0.25 Uani 0.0073(9) 4 1 d ? ? ? Sn5 Sn 0 0.43330(4) 0.25 Uani 0.0084(5) 4 1 d ? ? ? Cu2 Cu 0 0.46890(7) 0.75 Uani 0.0062(9) 4 1 d ? ? ? Cu3 Cu 0 0.36954(6) 0.75 Uani 0.0076(9) 4 1 d ? ? ? Cu4 Cu 0.2479(2) 0.38404(6) 0.25 Uani 0.0090(9) 8 1 d ? ? ? Cu5 Cu 0.2397(3) 0.48422(7) 0.25 Uani 0.0091(8) 8 1 d ? ? ? Cu6 Cu 0.2522(2) 0.41579(6) 0.75 Uani 0.0080(9) 8 1 d ? ? ? Cu7 Cu 0.2477(2) 0.28404(7) 0.25 Uani 0.0134(10) 8 1 d ? ? ? Cu8 Cu 0.2527(2) 0.31579(6) 0.75 Uani 0.0112(10) 8 1 d ? ? ? Cu9 Cu 0 0.26942(7) 0.75 Uani 0.0125(10) 4 1 d ? ? ? Cu10 Cu 0.5 0.33085(7) 0.25 Uani 0.0119(10) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0073(9) 0.0073(8) 0.0083(11) 0 0 0 Sn2 Sn 0.0047(8) 0.0070(7) 0.0078(9) 0 0 0 Sn3 Sn 0.0053(9) 0.0054(7) 0.0077(10) 0 0 0 Sn4 Sn 0.0092(9) 0.0065(8) 0.0087(10) 0 0 0 Cu1 Cu 0.0045(16) 0.0138(16) 0.0036(17) 0 0 0 Sn5 Sn 0.0090(10) 0.0083(8) 0.0079(10) 0 0 0 Cu2 Cu 0.0065(16) 0.0075(14) 0.0046(16) 0 0 0 Cu3 Cu 0.0051(16) 0.0077(14) 0.0100(17) 0 0 0 Cu4 Cu 0.0136(18) 0.0071(13) 0.0063(17) 0.0005(5) 0 0 Cu5 Cu 0.0106(15) 0.0081(12) 0.0088(15) -0.0006(5) 0 0 Cu6 Cu 0.0092(16) 0.0054(14) 0.0092(19) 0.0003(5) 0 0 Cu7 Cu 0.0143(17) 0.0147(16) 0.0112(18) -0.0004(5) 0 0 Cu8 Cu 0.0127(17) 0.0122(16) 0.0088(18) -0.0004(5) 0 0 Cu9 Cu 0.0090(16) 0.0161(16) 0.0123(17) 0 0 0 Cu10 Cu 0.0105(18) 0.0154(16) 0.0098(19) 0 0 0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 Cu3 ? 1_554 2.760(2) ? Sn1 Cu3 ? ? 2.760(2) ? Sn1 Cu4 ? ? 2.766(3) ? Sn1 Cu4 ? 3_555 2.766(3) ? Sn1 Cu7 ? ? 2.739(3) ? Sn1 Cu7 ? 3_555 2.739(3) ? Sn1 Cu8 ? 1_554 2.7146(12) ? Sn1 Cu8 ? ? 2.7146(12) ? Sn1 Cu8 ? 3_555 2.7146(12) ? Sn1 Cu8 ? 3_556 2.7146(12) ? Sn1 Cu10 ? 1_455 2.7626(3) ? Sn1 Cu10 ? ? 2.7626(3) ? Sn2 Cu7 ? ? 2.7131(13) ? Sn2 Cu7 ? 1_556 2.7131(13) ? Sn2 Cu7 ? 10_555 2.759(3) ? Sn2 Cu7 ? 3_655 2.7131(13) ? Sn2 Cu7 ? 3_656 2.7131(13) ? Sn2 Cu7 ? 12_556 2.759(3) ? Sn2 Cu8 ? ? 2.736(3) ? Sn2 Cu8 ? 3_656 2.736(3) ? Sn2 Cu9 ? ? 2.7637(4) ? Sn2 Cu9 ? 1_655 2.7637(4) ? Sn2 Cu9 ? 10_554 2.752(2) ? Sn2 Cu9 ? 10_555 2.752(2) ? Sn3 Cu3 ? ? 2.7639(4) ? Sn3 Cu3 ? 1_655 2.7639(4) ? Sn3 Cu4 ? ? 2.7120(13) ? Sn3 Cu4 ? 1_556 2.7120(13) ? Sn3 Cu4 ? 3_655 2.7120(13) ? Sn3 Cu4 ? 3_656 2.7120(13) ? Sn3 Cu6 ? ? 2.736(3) ? Sn3 Cu6 ? 3_656 2.736(3) ? Sn3 Cu8 ? ? 2.767(3) ? Sn3 Cu8 ? 3_656 2.767(3) ? Sn3 Cu10 ? ? 2.746(2) ? Sn3 Cu10 ? 1_556 2.746(2) ? Sn4 Cu1 ? ? 2.721(2) ? Sn4 Cu1 ? 1_556 2.721(2) ? Sn4 Cu2 ? ? 2.7621(3) ? Sn4 Cu2 ? 1_655 2.7621(3) ? Sn4 Cu5 ? ? 2.7365(14) ? Sn4 Cu5 ? 1_556 2.7365(14) ? Sn4 Cu5 ? 2_665 2.767(3) ? Sn4 Cu5 ? 3_655 2.7365(14) ? Sn4 Cu5 ? 3_656 2.7365(14) ? Sn4 Cu5 ? 4_566 2.767(3) ? Sn4 Cu6 ? ? 2.773(3) ? Sn4 Cu6 ? 3_656 2.773(3) ? Cu1 Sn5 ? ? 2.7602(3) ? Cu1 Sn5 ? 1_655 2.7602(3) ? Cu1 Cu4 ? ? 2.673(4) ? Cu1 Cu4 ? 3_655 2.673(4) ? Cu1 Cu6 ? 1_554 2.6736(13) ? Cu1 Cu6 ? ? 2.6736(13) ? Cu1 Cu6 ? 3_655 2.6736(13) ? Cu1 Cu6 ? 3_656 2.6736(13) ? Sn5 Cu2 ? 1_554 2.754(2) ? Sn5 Cu2 ? ? 2.754(2) ? Sn5 Cu4 ? ? 2.722(3) ? Sn5 Cu4 ? 3_555 2.722(3) ? Sn5 Cu5 ? ? 2.769(3) ? Sn5 Cu5 ? 3_555 2.769(3) ? Sn5 Cu6 ? 1_554 2.7069(12) ? Sn5 Cu6 ? ? 2.7069(12) ? Sn5 Cu6 ? 3_555 2.7069(12) ? Sn5 Cu6 ? 3_556 2.7069(12) ? Cu2 Cu5 ? ? 2.6415(14) ? Cu2 Cu5 ? 1_556 2.6415(14) ? Cu2 Cu5 ? 2_565 2.601(4) ? Cu2 Cu5 ? 3_555 2.6415(14) ? Cu2 Cu5 ? 3_556 2.6415(14) ? Cu2 Cu5 ? 4_566 2.601(4) ? Cu3 Cu4 ? ? 2.6538(13) ? Cu3 Cu4 ? 1_556 2.6538(13) ? Cu3 Cu4 ? 3_555 2.6538(13) ? Cu3 Cu4 ? 3_556 2.6538(13) ? Cu3 Cu6 ? ? 2.611(4) ? Cu3 Cu6 ? 3_556 2.611(4) ? Cu4 Cu6 ? 1_554 2.644(2) ? Cu4 Cu6 ? ? 2.644(2) ? Cu5 Cu5 ? 3_555 2.646(2) ? Cu5 Cu5 ? 4_565 2.639(3) ? Cu5 Cu5 ? 4_566 2.639(3) ? Cu7 Cu8 ? 1_554 2.644(2) ? Cu7 Cu8 ? ? 2.644(2) ? Cu7 Cu9 ? 1_554 2.6549(14) ? Cu7 Cu9 ? ? 2.6549(14) ? Cu7 Cu10 ? ? 2.634(4) ? Cu8 Cu9 ? ? 2.617(4) ? Cu8 Cu10 ? ? 2.6594(13) ? Cu8 Cu10 ? 1_556 2.6594(13) ? data_673K-superstructure _chemical_formula_structural 'Cu3 Sn1' _chemical_formula_sum 'Cu3 Sn1' _chemical_formula_weight 309.3 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C -2x;-2yc;-2zc' _space_group_IT_number 63 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z+1/2 3 -x,y,-z+1/2 4 x,-y,-z 5 -x,-y,-z 6 x,y,-z+1/2 7 x,-y,z+1/2 8 -x,y,z 9 x+1/2,y+1/2,z 10 -x+1/2,-y+1/2,z+1/2 11 -x+1/2,y+1/2,-z+1/2 12 x+1/2,-y+1/2,-z 13 -x+1/2,-y+1/2,-z 14 x+1/2,y+1/2,-z+1/2 15 x+1/2,-y+1/2,z+1/2 16 -x+1/2,y+1/2,z _cell_length_a 5.51960(10) _cell_length_b 38.2386(12) _cell_length_c 4.33210(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 914.34(4) _cell_formula_units_Z 16 _cell_measurement_reflns_used 2178 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 28.38 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 8.986 _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 37.885 _exptl_crystal_description block _exptl_crystal_size_max 0.142 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.018 _exptl_crystal_colour 'metallic intense silver' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.095 _exptl_absorpt_correction_T_max 0.529 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 7324 _diffrn_reflns_theta_min 3.2 _diffrn_reflns_theta_max 28.38 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_unetI/netI 0.0124 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 689 _reflns_number_gt 389 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_gt 0.0904 _refine_ls_R_factor_all 0.0419 _refine_ls_wR_factor_ref 0.0965 _refine_ls_goodness_of_fit_ref 1.96 _refine_ls_goodness_of_fit_gt 2.54 _refine_ls_number_reflns 689 _refine_ls_number_parameters 58 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0485 _refine_ls_shift/su_mean 0.0081 _refine_diff_density_max 1.34 _refine_diff_density_min -1.25 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 225(12) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.5 0.29211(2) 0.25 Uani 0.0068(3) 4 1 d ? ? ? Sn2 Sn 0 0.33254(2) 0.75 Uani 0.0069(3) 4 1 d ? ? ? Sn3 Sn 0 0.45781(3) 0.75 Uani 0.0087(3) 4 1 d ? ? ? Sn4 Sn 0.5 0.41656(3) 0.25 Uani 0.0082(3) 4 1 d ? ? ? Cu1 Cu 0.5 0.46135(5) 0.75 Uani 0.0083(6) 4 1 d ? ? ? Cu2 Cu 0 0.28811(5) 0.25 Uani 0.0111(6) 4 1 d ? ? ? Cu3 Cu 0.26080(17) 0.48005(4) 0.25 Uani 0.0122(5) 8 1 d ? ? ? Cu4 Cu 0 0.41423(5) 0.25 Uani 0.0081(6) 4 1 d ? ? ? Cu5 Cu 0.25216(16) 0.23001(4) 0.25 Uani 0.0112(5) 8 1 d ? ? ? Cu6 Cu 0.5 0.33687(5) 0.75 Uani 0.0119(6) 4 1 d ? ? ? Cu7 Cu 0.25152(15) 0.35505(4) 0.25 Uani 0.0104(5) 8 1 d ? ? ? Cu8 Cu 0.24709(15) 0.39472(4) 0.75 Uani 0.0104(5) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0061(5) 0.0075(5) 0.0070(6) 0 0 0 Sn2 Sn 0.0071(6) 0.0062(5) 0.0074(6) 0 0 0 Sn3 Sn 0.0089(6) 0.0083(5) 0.0091(7) 0 0 0 Sn4 Sn 0.0084(6) 0.0082(5) 0.0080(6) 0 0 0 Cu1 Cu 0.0068(9) 0.0108(9) 0.0073(11) 0 0 0 Cu2 Cu 0.0101(10) 0.0127(9) 0.0105(12) 0 0 0 Cu3 Cu 0.0138(9) 0.0123(8) 0.0104(9) 0.0014(4) 0 0 Cu4 Cu 0.0065(10) 0.0125(9) 0.0052(10) 0 0 0 Cu5 Cu 0.0132(9) 0.0107(8) 0.0097(9) 0.0006(3) 0 0 Cu6 Cu 0.0110(11) 0.0135(9) 0.0113(11) 0 0 0 Cu7 Cu 0.0111(10) 0.0111(8) 0.0091(11) -0.0005(3) 0 0 Cu8 Cu 0.0145(10) 0.0093(8) 0.0074(10) 0.0003(3) 0 0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 Sn1 ? 1_455 5.5196(2) ? Sn1 Sn1 ? 1_554 4.3321(2) ? Sn1 Sn1 ? 1_556 4.3321(2) ? Sn1 Sn1 ? 1_655 5.5196(2) ? Sn1 Sn1 ? 10_554 4.7623(9) ? Sn1 Sn1 ? 10_555 4.7618(9) ? Sn1 Sn1 ? 10_654 4.7624(9) ? Sn1 Sn1 ? 10_655 4.7625(9) ? Sn1 Sn2 ? 1_554 3.8341(5) ? Sn1 Sn2 ? ? 3.8339(5) ? Sn1 Sn2 ? 1_654 3.8335(5) ? Sn1 Sn2 ? 1_655 3.8340(5) ? Sn1 Sn2 ? 10_554 4.7664(13) ? Sn1 Sn4 ? ? 4.7587(14) ? Sn1 Cu2 ? 1_554 5.1391(2) ? Sn1 Cu2 ? ? 2.76402(15) ? Sn1 Cu2 ? 1_556 5.1385(2) ? Sn1 Cu2 ? 1_654 5.1385(2) ? Sn1 Cu2 ? 1_655 2.76405(15) ? Sn1 Cu2 ? 1_656 5.1391(2) ? Sn1 Cu2 ? 10_554 3.7552(17) ? Sn1 Cu2 ? 10_555 3.7549(17) ? Sn1 Cu4 ? ? 5.4247(18) ? Sn1 Cu4 ? 1_655 5.4242(18) ? Sn1 Cu5 ? 1_554 5.1264(9) ? Sn1 Cu5 ? ? 2.7404(16) ? Sn1 Cu5 ? 1_556 5.1258(9) ? Sn1 Cu5 ? 1_655 4.7830(12) ? Sn1 Cu5 ? 10_554 2.7101(7) ? Sn1 Cu5 ? 10_555 2.7098(7) ? Sn1 Cu5 ? 10_654 4.7375(8) ? Sn1 Cu5 ? 10_655 4.7379(8) ? Sn1 Cu5 ? 3_555 4.7826(12) ? Sn1 Cu5 ? 3_654 5.1262(9) ? Sn1 Cu5 ? 3_655 2.7406(16) ? Sn1 Cu5 ? 3_656 5.1262(9) ? Sn1 Cu5 ? 12_455 4.7378(8) ? Sn1 Cu5 ? 12_456 4.7373(8) ? Sn1 Cu5 ? 12_555 2.7099(7) ? Sn1 Cu5 ? 12_556 2.7101(7) ? Sn1 Cu6 ? 1_554 2.7607(13) ? Sn1 Cu6 ? ? 2.7609(13) ? Sn1 Cu6 ? 10_554 5.6514(19) ? Sn1 Cu6 ? 10_654 5.6519(19) ? Sn1 Cu7 ? 1_554 5.1421(9) ? Sn1 Cu7 ? ? 2.7703(16) ? Sn1 Cu7 ? 1_556 5.1421(9) ? Sn1 Cu7 ? 1_655 4.7955(12) ? Sn1 Cu7 ? 3_555 4.7960(12) ? Sn1 Cu7 ? 3_654 5.1417(9) ? Sn1 Cu7 ? 3_655 2.7700(16) ? Sn1 Cu7 ? 3_656 5.1423(9) ? Sn1 Cu8 ? 1_554 4.6942(15) ? Sn1 Cu8 ? ? 4.6943(15) ? Sn1 Cu8 ? 3_655 4.6938(15) ? Sn1 Cu8 ? 3_656 4.6943(15) ? Sn2 Sn2 ? 1_455 5.5196(2) ? Sn2 Sn2 ? 1_554 4.3321(2) ? Sn2 Sn2 ? 1_556 4.3321(2) ? Sn2 Sn2 ? 1_655 5.5196(2) ? Sn2 Sn3 ? ? 4.7902(14) ? Sn2 Sn4 ? 1_455 4.7573(9) ? Sn2 Sn4 ? 1_456 4.7572(9) ? Sn2 Sn4 ? ? 4.7566(9) ? Sn2 Sn4 ? 1_556 4.7571(9) ? Sn2 Cu1 ? 1_455 5.6463(18) ? Sn2 Cu1 ? ? 5.6458(18) ? Sn2 Cu2 ? ? 2.7530(13) ? Sn2 Cu2 ? 1_556 2.7528(13) ? Sn2 Cu2 ? 10_455 5.3757(18) ? Sn2 Cu2 ? 10_555 5.3762(18) ? Sn2 Cu4 ? ? 3.8012(17) ? Sn2 Cu4 ? 1_556 3.8014(17) ? Sn2 Cu5 ? ? 4.6907(16) ? Sn2 Cu5 ? 1_556 4.6906(16) ? Sn2 Cu5 ? 10_455 4.7911(12) ? Sn2 Cu5 ? 10_554 5.1342(9) ? Sn2 Cu5 ? 10_555 2.7555(16) ? Sn2 Cu5 ? 10_556 5.1342(9) ? Sn2 Cu5 ? 3_555 4.6906(16) ? Sn2 Cu5 ? 3_556 4.6902(16) ? Sn2 Cu5 ? 12_455 5.1343(9) ? Sn2 Cu5 ? 12_456 2.7552(16) ? Sn2 Cu5 ? 12_457 5.1337(9) ? Sn2 Cu5 ? 12_556 4.7915(12) ? Sn2 Cu6 ? 1_454 5.1394(2) ? Sn2 Cu6 ? 1_455 2.76478(16) ? Sn2 Cu6 ? 1_456 5.1389(2) ? Sn2 Cu6 ? 1_554 5.1389(2) ? Sn2 Cu6 ? ? 2.76475(16) ? Sn2 Cu6 ? 1_556 5.1395(2) ? Sn2 Cu7 ? 1_455 4.7437(8) ? Sn2 Cu7 ? 1_456 4.7433(8) ? Sn2 Cu7 ? ? 2.7127(7) ? Sn2 Cu7 ? 1_556 2.7130(7) ? Sn2 Cu7 ? 3_555 2.7130(7) ? Sn2 Cu7 ? 3_556 2.7129(7) ? Sn2 Cu7 ? 3_655 4.7431(8) ? Sn2 Cu7 ? 3_656 4.7436(8) ? Sn2 Cu8 ? 1_455 4.7880(12) ? Sn2 Cu8 ? 1_554 5.1260(9) ? Sn2 Cu8 ? ? 2.7408(16) ? Sn2 Cu8 ? 1_556 5.1266(9) ? Sn2 Cu8 ? 3_555 5.1265(9) ? Sn2 Cu8 ? 3_556 2.7411(16) ? Sn2 Cu8 ? 3_557 5.1265(9) ? Sn2 Cu8 ? 3_656 4.7876(12) ? Sn3 Sn3 ? 1_455 5.5196(2) ? Sn3 Sn3 ? 1_554 4.3321(2) ? Sn3 Sn3 ? 1_556 4.3321(2) ? Sn3 Sn3 ? 1_655 5.5196(2) ? Sn3 Sn3 ? 2_564 3.8859(11) ? Sn3 Sn3 ? 2_565 3.8862(11) ? Sn3 Sn4 ? 1_455 3.8468(6) ? Sn3 Sn4 ? 1_456 3.8463(6) ? Sn3 Sn4 ? ? 3.8467(6) ? Sn3 Sn4 ? 1_556 3.8469(6) ? Sn3 Sn4 ? 2_565 5.5405(12) ? Sn3 Sn4 ? 2_665 5.5400(12) ? Sn3 Cu1 ? 1_454 5.1386(2) ? Sn3 Cu1 ? 1_455 2.76313(14) ? Sn3 Cu1 ? 1_456 5.1380(2) ? Sn3 Cu1 ? 1_554 5.1380(2) ? Sn3 Cu1 ? ? 2.76310(14) ? Sn3 Cu1 ? 1_556 5.1386(2) ? Sn3 Cu1 ? 2_564 4.6760(13) ? Sn3 Cu1 ? 2_565 4.6759(13) ? Sn3 Cu1 ? 2_664 4.6753(13) ? Sn3 Cu1 ? 2_665 4.6758(13) ? Sn3 Cu3 ? 1_455 4.6973(9) ? Sn3 Cu3 ? 1_456 4.6969(9) ? Sn3 Cu3 ? ? 2.7361(8) ? Sn3 Cu3 ? 1_556 2.7364(8) ? Sn3 Cu3 ? 2_564 5.1464(9) ? Sn3 Cu3 ? 2_565 2.7781(17) ? Sn3 Cu3 ? 2_566 5.1463(9) ? Sn3 Cu3 ? 2_665 4.7212(12) ? Sn3 Cu3 ? 3_555 2.7364(8) ? Sn3 Cu3 ? 3_556 2.7362(8) ? Sn3 Cu3 ? 3_655 4.6967(9) ? Sn3 Cu3 ? 3_656 4.6972(9) ? Sn3 Cu3 ? 4_466 4.7217(12) ? Sn3 Cu3 ? 4_565 5.1459(9) ? Sn3 Cu3 ? 4_566 2.7778(17) ? Sn3 Cu3 ? 4_567 5.1465(9) ? Sn3 Cu4 ? ? 2.7330(13) ? Sn3 Cu4 ? 1_556 2.7328(13) ? Sn3 Cu4 ? 2_565 4.893(2) ? Sn3 Cu6 ? 1_455 5.3852(19) ? Sn3 Cu6 ? ? 5.3857(19) ? Sn3 Cu7 ? ? 4.6970(15) ? Sn3 Cu7 ? 1_556 4.6969(15) ? Sn3 Cu7 ? 3_555 4.6969(15) ? Sn3 Cu7 ? 3_556 4.6965(15) ? Sn3 Cu8 ? 1_455 4.8051(12) ? Sn3 Cu8 ? 1_554 5.1428(9) ? Sn3 Cu8 ? ? 2.7716(16) ? Sn3 Cu8 ? 1_556 5.1428(9) ? Sn3 Cu8 ? 3_555 5.1430(9) ? Sn3 Cu8 ? 3_556 2.7713(16) ? Sn3 Cu8 ? 3_557 5.1424(9) ? Sn3 Cu8 ? 3_656 4.8055(12) ? Sn4 Sn4 ? 1_455 5.5196(2) ? Sn4 Sn4 ? 1_554 4.3321(2) ? Sn4 Sn4 ? 1_556 4.3321(2) ? Sn4 Sn4 ? 1_655 5.5196(2) ? Sn4 Cu1 ? 1_554 2.7614(12) ? Sn4 Cu1 ? ? 2.7616(12) ? Sn4 Cu1 ? 2_664 4.669(2) ? Sn4 Cu2 ? ? 5.6337(18) ? Sn4 Cu2 ? 1_655 5.6342(18) ? Sn4 Cu3 ? 1_554 5.1387(9) ? Sn4 Cu3 ? ? 2.7639(17) ? Sn4 Cu3 ? 1_556 5.1387(9) ? Sn4 Cu3 ? 1_655 4.8505(12) ? Sn4 Cu3 ? 2_664 4.6970(16) ? Sn4 Cu3 ? 2_665 4.6974(16) ? Sn4 Cu3 ? 3_555 4.8510(12) ? Sn4 Cu3 ? 3_654 5.1383(9) ? Sn4 Cu3 ? 3_655 2.7637(17) ? Sn4 Cu3 ? 3_656 5.1389(9) ? Sn4 Cu3 ? 4_565 4.6974(16) ? Sn4 Cu3 ? 4_566 4.6975(16) ? Sn4 Cu4 ? 1_554 5.1375(2) ? Sn4 Cu4 ? ? 2.76122(12) ? Sn4 Cu4 ? 1_556 5.1370(2) ? Sn4 Cu4 ? 1_654 5.1370(2) ? Sn4 Cu4 ? 1_655 2.76124(12) ? Sn4 Cu4 ? 1_656 5.1375(2) ? Sn4 Cu6 ? 1_554 3.7385(18) ? Sn4 Cu6 ? ? 3.7383(18) ? Sn4 Cu7 ? 1_554 5.1168(9) ? Sn4 Cu7 ? ? 2.7225(16) ? Sn4 Cu7 ? 1_556 5.1163(9) ? Sn4 Cu7 ? 1_655 4.7687(12) ? Sn4 Cu7 ? 3_555 4.7682(12) ? Sn4 Cu7 ? 3_654 5.1167(9) ? Sn4 Cu7 ? 3_655 2.7228(16) ? Sn4 Cu7 ? 3_656 5.1167(9) ? Sn4 Cu8 ? 1_554 2.7090(7) ? Sn4 Cu8 ? ? 2.7086(7) ? Sn4 Cu8 ? 1_654 4.7321(8) ? Sn4 Cu8 ? 1_655 4.7325(8) ? Sn4 Cu8 ? 3_555 4.7324(8) ? Sn4 Cu8 ? 3_556 4.7319(8) ? Sn4 Cu8 ? 3_655 2.7088(7) ? Sn4 Cu8 ? 3_656 2.7090(7) ? Cu1 Cu1 ? 1_455 5.5196(2) ? Cu1 Cu1 ? 1_554 4.3321(2) ? Cu1 Cu1 ? 1_556 4.3321(2) ? Cu1 Cu1 ? 1_655 5.5196(2) ? Cu1 Cu1 ? 2_664 3.664(2) ? Cu1 Cu1 ? 2_665 3.665(2) ? Cu1 Cu3 ? ? 2.6357(8) ? Cu1 Cu3 ? 1_556 2.6355(8) ? Cu1 Cu3 ? 1_655 4.7785(9) ? Cu1 Cu3 ? 1_656 4.7790(9) ? Cu1 Cu3 ? 2_565 4.7598(14) ? Cu1 Cu3 ? 2_664 5.0524(11) ? Cu1 Cu3 ? 2_665 2.601(2) ? Cu1 Cu3 ? 2_666 5.0530(11) ? Cu1 Cu3 ? 3_555 4.7791(9) ? Cu1 Cu3 ? 3_556 4.7787(9) ? Cu1 Cu3 ? 3_655 2.6354(8) ? Cu1 Cu3 ? 3_656 2.6357(8) ? Cu1 Cu3 ? 4_565 5.0528(11) ? Cu1 Cu3 ? 4_566 2.601(2) ? Cu1 Cu3 ? 4_567 5.0528(11) ? Cu1 Cu3 ? 4_666 4.7594(14) ? Cu1 Cu4 ? ? 3.9440(12) ? Cu1 Cu4 ? 1_556 3.9435(12) ? Cu1 Cu4 ? 1_655 3.9439(12) ? Cu1 Cu4 ? 1_656 3.9442(12) ? Cu1 Cu4 ? 2_565 5.500(2) ? Cu1 Cu4 ? 2_665 5.500(2) ? Cu1 Cu6 ? ? 4.760(3) ? Cu1 Cu7 ? ? 4.806(2) ? Cu1 Cu7 ? 1_556 4.806(2) ? Cu1 Cu7 ? 3_655 4.806(2) ? Cu1 Cu7 ? 3_656 4.806(2) ? Cu1 Cu8 ? 1_554 5.2164(12) ? Cu1 Cu8 ? ? 2.905(2) ? Cu1 Cu8 ? 1_556 5.2158(12) ? Cu1 Cu8 ? 1_655 4.8476(14) ? Cu1 Cu8 ? 3_556 4.8471(14) ? Cu1 Cu8 ? 3_655 5.2162(12) ? Cu1 Cu8 ? 3_656 2.905(2) ? Cu1 Cu8 ? 3_657 5.2162(12) ? Cu2 Cu2 ? 1_455 5.5196(2) ? Cu2 Cu2 ? 1_554 4.3321(2) ? Cu2 Cu2 ? 1_556 4.3321(2) ? Cu2 Cu2 ? 1_655 5.5196(2) ? Cu2 Cu2 ? 10_454 4.5610(16) ? Cu2 Cu2 ? 10_455 4.5605(16) ? Cu2 Cu2 ? 10_554 4.5610(16) ? Cu2 Cu2 ? 10_555 4.5612(16) ? Cu2 Cu4 ? ? 4.823(3) ? Cu2 Cu5 ? 1_455 4.6875(14) ? Cu2 Cu5 ? 1_554 5.0637(11) ? Cu2 Cu5 ? ? 2.622(2) ? Cu2 Cu5 ? 1_556 5.0637(11) ? Cu2 Cu5 ? 10_454 4.7338(9) ? Cu2 Cu5 ? 10_455 4.7333(9) ? Cu2 Cu5 ? 10_554 2.6538(8) ? Cu2 Cu5 ? 10_555 2.6540(8) ? Cu2 Cu5 ? 3_554 5.0638(11) ? Cu2 Cu5 ? 3_555 2.622(2) ? Cu2 Cu5 ? 3_556 5.0633(11) ? Cu2 Cu5 ? 3_655 4.6879(14) ? Cu2 Cu5 ? 12_455 2.6540(8) ? Cu2 Cu5 ? 12_456 2.6536(8) ? Cu2 Cu5 ? 12_555 4.7335(9) ? Cu2 Cu5 ? 12_556 4.7339(9) ? Cu2 Cu6 ? 1_454 3.9733(12) ? Cu2 Cu6 ? 1_455 3.9731(12) ? Cu2 Cu6 ? 1_554 3.9727(12) ? Cu2 Cu6 ? ? 3.9732(12) ? Cu2 Cu6 ? 10_554 4.779(3) ? Cu2 Cu7 ? 1_455 4.8603(14) ? Cu2 Cu7 ? 1_554 5.2195(12) ? Cu2 Cu7 ? ? 2.912(2) ? Cu2 Cu7 ? 1_556 5.2200(12) ? Cu2 Cu7 ? 3_554 5.2199(12) ? Cu2 Cu7 ? 3_555 2.912(2) ? Cu2 Cu7 ? 3_556 5.2199(12) ? Cu2 Cu7 ? 3_655 4.8598(14) ? Cu2 Cu8 ? 1_554 4.813(2) ? Cu2 Cu8 ? ? 4.814(2) ? Cu2 Cu8 ? 3_555 4.814(2) ? Cu2 Cu8 ? 3_556 4.814(2) ? Cu3 Cu3 ? 1_455 5.5196(13) ? Cu3 Cu3 ? 1_554 4.3321(2) ? Cu3 Cu3 ? 1_556 4.3321(2) ? Cu3 Cu3 ? 1_655 5.5196(13) ? Cu3 Cu3 ? 2_564 3.9127(13) ? Cu3 Cu3 ? 2_565 3.9124(13) ? Cu3 Cu3 ? 2_664 3.7401(13) ? Cu3 Cu3 ? 2_665 3.7406(13) ? Cu3 Cu3 ? 3_554 5.2018(8) ? Cu3 Cu3 ? 3_555 2.8790(13) ? Cu3 Cu3 ? 3_556 5.2012(8) ? Cu3 Cu3 ? 3_654 5.0732(7) ? Cu3 Cu3 ? 3_655 2.6406(13) ? Cu3 Cu3 ? 3_656 5.0737(7) ? Cu3 Cu3 ? 4_565 2.6492(13) ? Cu3 Cu3 ? 4_566 2.6494(13) ? Cu3 Cu4 ? 1_554 5.2131(12) ? Cu3 Cu4 ? ? 2.899(2) ? Cu3 Cu4 ? 1_556 5.2125(12) ? Cu3 Cu4 ? 1_655 4.7942(15) ? Cu3 Cu4 ? 2_564 4.807(2) ? Cu3 Cu4 ? 2_565 4.807(2) ? Cu3 Cu7 ? ? 4.780(2) ? Cu3 Cu7 ? 3_555 5.554(2) ? Cu3 Cu7 ? 3_655 5.486(2) ? Cu3 Cu8 ? 1_554 3.9175(18) ? Cu3 Cu8 ? ? 3.9172(18) ? Cu3 Cu8 ? 2_564 5.549(2) ? Cu3 Cu8 ? 2_664 5.505(2) ? Cu3 Cu8 ? 3_555 4.8166(17) ? Cu3 Cu8 ? 3_556 4.8161(17) ? Cu3 Cu8 ? 3_655 4.7665(17) ? Cu3 Cu8 ? 3_656 4.7666(17) ? Cu3 Cu8 ? 4_566 4.789(2) ? Cu4 Cu4 ? 1_455 5.5196(2) ? Cu4 Cu4 ? 1_554 4.3321(2) ? Cu4 Cu4 ? 1_556 4.3321(2) ? Cu4 Cu4 ? 1_655 5.5196(2) ? Cu4 Cu6 ? 1_454 4.5891(17) ? Cu4 Cu6 ? 1_455 4.5886(17) ? Cu4 Cu6 ? 1_554 4.5891(17) ? Cu4 Cu6 ? ? 4.5893(17) ? Cu4 Cu7 ? 1_455 4.7104(14) ? Cu4 Cu7 ? 1_554 5.0810(11) ? Cu4 Cu7 ? ? 2.655(2) ? Cu4 Cu7 ? 1_556 5.0810(11) ? Cu4 Cu7 ? 3_554 5.0812(11) ? Cu4 Cu7 ? 3_555 2.655(2) ? Cu4 Cu7 ? 3_556 5.0806(11) ? Cu4 Cu7 ? 3_655 4.7108(14) ? Cu4 Cu8 ? 1_454 4.7456(8) ? Cu4 Cu8 ? 1_455 4.7451(8) ? Cu4 Cu8 ? 1_554 2.6662(8) ? Cu4 Cu8 ? ? 2.6664(8) ? Cu4 Cu8 ? 3_555 2.6664(8) ? Cu4 Cu8 ? 3_556 2.6660(8) ? Cu4 Cu8 ? 3_655 4.7453(8) ? Cu4 Cu8 ? 3_656 4.7457(8) ? Cu5 Cu5 ? 1_455 5.5196(12) ? Cu5 Cu5 ? 1_554 4.3321(2) ? Cu5 Cu5 ? 1_556 4.3321(2) ? Cu5 Cu5 ? 1_655 5.5196(12) ? Cu5 Cu5 ? 10_554 2.6514(13) ? Cu5 Cu5 ? 10_555 2.6515(13) ? Cu5 Cu5 ? 3_554 5.1496(7) ? Cu5 Cu5 ? 3_555 2.7836(12) ? Cu5 Cu5 ? 3_556 5.1491(7) ? Cu5 Cu5 ? 3_654 5.1234(7) ? Cu5 Cu5 ? 3_655 2.7360(12) ? Cu5 Cu5 ? 3_656 5.1240(7) ? Cu5 Cu5 ? 12_455 3.8273(13) ? Cu5 Cu5 ? 12_456 3.8270(13) ? Cu5 Cu5 ? 12_555 3.8267(13) ? Cu5 Cu5 ? 12_556 3.8272(13) ? Cu5 Cu6 ? 1_554 4.823(2) ? Cu5 Cu6 ? ? 4.823(2) ? Cu5 Cu6 ? 10_553 5.2198(13) ? Cu5 Cu6 ? 10_554 2.911(2) ? Cu5 Cu6 ? 10_555 5.2193(13) ? Cu5 Cu6 ? 10_654 4.8560(15) ? Cu5 Cu7 ? ? 4.781(2) ? Cu5 Cu7 ? 10_554 3.9079(18) ? Cu5 Cu7 ? 10_555 3.9076(18) ? Cu5 Cu7 ? 3_555 5.531(2) ? Cu5 Cu7 ? 3_655 5.510(2) ? Cu5 Cu7 ? 12_455 4.7861(16) ? Cu5 Cu7 ? 12_456 4.7856(16) ? Cu5 Cu7 ? 12_555 4.7821(16) ? Cu5 Cu7 ? 12_556 4.7822(16) ? Cu5 Cu8 ? 10_554 4.769(2) ? Cu5 Cu8 ? 12_456 5.524(2) ? Cu5 Cu8 ? 12_556 5.497(2) ? Cu6 Cu6 ? 1_455 5.5196(2) ? Cu6 Cu6 ? 1_554 4.3321(2) ? Cu6 Cu6 ? 1_556 4.3321(2) ? Cu6 Cu6 ? 1_655 5.5196(2) ? Cu6 Cu7 ? ? 2.6564(8) ? Cu6 Cu7 ? 1_556 2.6562(8) ? Cu6 Cu7 ? 1_655 4.7306(8) ? Cu6 Cu7 ? 1_656 4.7311(8) ? Cu6 Cu7 ? 3_555 4.7312(8) ? Cu6 Cu7 ? 3_556 4.7307(8) ? Cu6 Cu7 ? 3_655 2.6561(8) ? Cu6 Cu7 ? 3_656 2.6564(8) ? Cu6 Cu8 ? 1_554 5.0605(11) ? Cu6 Cu8 ? ? 2.616(2) ? Cu6 Cu8 ? 1_556 5.0605(11) ? Cu6 Cu8 ? 1_655 4.6792(14) ? Cu6 Cu8 ? 3_556 4.6796(14) ? Cu6 Cu8 ? 3_655 5.0601(11) ? Cu6 Cu8 ? 3_656 2.615(2) ? Cu6 Cu8 ? 3_657 5.0607(11) ? Cu7 Cu7 ? 1_455 5.5196(12) ? Cu7 Cu7 ? 1_554 4.3321(2) ? Cu7 Cu7 ? 1_556 4.3321(2) ? Cu7 Cu7 ? 1_655 5.5196(12) ? Cu7 Cu7 ? 3_554 5.1458(7) ? Cu7 Cu7 ? 3_555 2.7765(12) ? Cu7 Cu7 ? 3_556 5.1452(7) ? Cu7 Cu7 ? 3_654 5.1272(7) ? Cu7 Cu7 ? 3_655 2.7431(12) ? Cu7 Cu7 ? 3_656 5.1278(7) ? Cu7 Cu8 ? 1_554 2.6444(12) ? Cu7 Cu8 ? ? 2.6446(12) ? Cu7 Cu8 ? 3_555 3.8169(12) ? Cu7 Cu8 ? 3_556 3.8166(12) ? Cu7 Cu8 ? 3_655 3.8274(12) ? Cu7 Cu8 ? 3_656 3.8279(12) ? Cu8 Cu8 ? 1_455 5.5196(12) ? Cu8 Cu8 ? 1_554 4.3321(2) ? Cu8 Cu8 ? 1_556 4.3321(2) ? Cu8 Cu8 ? 1_655 5.5196(12) ? Cu8 Cu8 ? 3_555 5.1196(7) ? Cu8 Cu8 ? 3_556 2.7277(12) ? Cu8 Cu8 ? 3_557 5.1190(7) ? Cu8 Cu8 ? 3_655 5.1535(7) ? Cu8 Cu8 ? 3_656 2.7919(12) ? Cu8 Cu8 ? 3_657 5.1541(7) ? data_723K-superstructure _chemical_formula_structural 'Cu3 Sn1' _chemical_formula_sum 'Cu3 Sn1' _chemical_formula_weight 309.3 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C -2x;-2yc;-2zc' _space_group_IT_number 63 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z+1/2 3 -x,y,-z+1/2 4 x,-y,-z 5 -x,-y,-z 6 x,y,-z+1/2 7 x,-y,z+1/2 8 -x,y,z 9 x+1/2,y+1/2,z 10 -x+1/2,-y+1/2,z+1/2 11 -x+1/2,y+1/2,-z+1/2 12 x+1/2,-y+1/2,-z 13 -x+1/2,-y+1/2,-z 14 x+1/2,y+1/2,-z+1/2 15 x+1/2,-y+1/2,z+1/2 16 -x+1/2,y+1/2,z _cell_length_a 5.5184(2) _cell_length_b 38.2337(15) _cell_length_c 4.3326(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 914.13(6) _cell_formula_units_Z 16 _cell_measurement_reflns_used 1730 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 28.28 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 8.9881 _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 37.894 _exptl_crystal_description 'trigonal primatic' _exptl_crystal_size_max 0.096 _exptl_crystal_size_mid 0.065 _exptl_crystal_size_min 0.04 _exptl_crystal_colour 'metallic grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.199 _exptl_absorpt_correction_T_max 0.434 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 5405 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0118 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 673 _reflns_number_gt 384 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_gt 0.0538 _refine_ls_R_factor_all 0.0394 _refine_ls_wR_factor_ref 0.0632 _refine_ls_goodness_of_fit_ref 1.26 _refine_ls_goodness_of_fit_gt 1.48 _refine_ls_number_reflns 673 _refine_ls_number_parameters 58 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0325 _refine_ls_shift/su_mean 0.0106 _refine_diff_density_max 1.55 _refine_diff_density_min -1.60 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 570(12) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.5 0.292227(17) 0.25 Uani 0.0095(2) 4 1 d ? ? ? Sn2 Sn 0 0.332569(16) 0.75 Uani 0.0089(2) 4 1 d ? ? ? Sn3 Sn 0 0.457737(17) 0.75 Uani 0.0095(2) 4 1 d ? ? ? Sn4 Sn 0.5 0.416506(17) 0.25 Uani 0.0093(2) 4 1 d ? ? ? Cu1 Cu 0.5 0.46133(3) 0.75 Uani 0.0125(4) 4 1 d ? ? ? Cu2 Cu 0 0.28840(3) 0.25 Uani 0.0134(4) 4 1 d ? ? ? Cu3 Cu 0.26168(12) 0.48009(3) 0.25 Uani 0.0132(3) 8 1 d ? ? ? Cu4 Cu 0 0.41409(3) 0.25 Uani 0.0114(4) 4 1 d ? ? ? Cu5 Cu 0.25213(11) 0.23017(3) 0.25 Uani 0.0116(3) 8 1 d ? ? ? Cu6 Cu 0.5 0.33679(4) 0.75 Uani 0.0124(4) 4 1 d ? ? ? Cu7 Cu 0.25115(10) 0.35503(3) 0.25 Uani 0.0132(4) 8 1 d ? ? ? Cu8 Cu 0.24682(10) 0.39476(3) 0.75 Uani 0.0124(4) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0082(4) 0.0093(4) 0.0109(4) 0 0 0 Sn2 Sn 0.0076(4) 0.0096(4) 0.0095(4) 0 0 0 Sn3 Sn 0.0081(4) 0.0092(4) 0.0113(4) 0 0 0 Sn4 Sn 0.0084(4) 0.0088(4) 0.0106(4) 0 0 0 Cu1 Cu 0.0096(7) 0.0154(7) 0.0124(7) 0 0 0 Cu2 Cu 0.0117(7) 0.0152(7) 0.0132(7) 0 0 0 Cu3 Cu 0.0137(6) 0.0123(5) 0.0137(6) 0.0012(3) 0 0 Cu4 Cu 0.0097(7) 0.0137(6) 0.0106(7) 0 0 0 Cu5 Cu 0.0121(6) 0.0126(5) 0.0102(6) 0.0005(2) 0 0 Cu6 Cu 0.0096(7) 0.0158(6) 0.0119(7) 0 0 0 Cu7 Cu 0.0138(8) 0.0132(6) 0.0124(7) -0.0002(2) 0 0 Cu8 Cu 0.0140(7) 0.0123(6) 0.0109(7) 0.0004(2) 0 0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 Sn1 ? 1_455 5.5184(4) ? Sn1 Sn1 ? 1_554 4.3326(4) ? Sn1 Sn1 ? 1_556 4.3326(4) ? Sn1 Sn1 ? 1_655 5.5184(4) ? Sn1 Sn1 ? 10_554 4.7679(7) ? Sn1 Sn1 ? 10_555 4.7679(7) ? Sn1 Sn1 ? 10_654 4.7679(7) ? Sn1 Sn1 ? 10_655 4.7679(7) ? Sn1 Sn2 ? 1_554 3.8321(4) ? Sn1 Sn2 ? ? 3.8321(4) ? Sn1 Sn2 ? 1_654 3.8321(4) ? Sn1 Sn2 ? 1_655 3.8321(4) ? Sn1 Sn2 ? 10_554 4.7714(10) ? Sn1 Sn4 ? ? 4.7516(10) ? Sn1 Cu2 ? 1_554 5.1387(4) ? Sn1 Cu2 ? ? 2.7631(2) ? Sn1 Cu2 ? 1_556 5.1387(4) ? Sn1 Cu2 ? 1_654 5.1387(4) ? Sn1 Cu2 ? 1_655 2.7631(2) ? Sn1 Cu2 ? 1_656 5.1387(4) ? Sn1 Cu2 ? 10_554 3.7677(12) ? Sn1 Cu2 ? 10_555 3.7677(12) ? Sn1 Cu4 ? ? 5.4150(13) ? Sn1 Cu4 ? 1_655 5.4150(13) ? Sn1 Cu5 ? 1_554 5.1257(7) ? Sn1 Cu5 ? ? 2.7389(12) ? Sn1 Cu5 ? 1_556 5.1257(7) ? Sn1 Cu5 ? 1_655 4.7809(9) ? Sn1 Cu5 ? 10_554 2.7133(5) ? Sn1 Cu5 ? 10_555 2.7133(5) ? Sn1 Cu5 ? 10_654 4.7390(6) ? Sn1 Cu5 ? 10_655 4.7390(6) ? Sn1 Cu5 ? 3_555 4.7809(9) ? Sn1 Cu5 ? 3_654 5.1257(7) ? Sn1 Cu5 ? 3_655 2.7389(12) ? Sn1 Cu5 ? 3_656 5.1257(7) ? Sn1 Cu5 ? 12_455 4.7390(6) ? Sn1 Cu5 ? 12_456 4.7390(6) ? Sn1 Cu5 ? 12_555 2.7133(5) ? Sn1 Cu5 ? 12_556 2.7133(5) ? Sn1 Cu6 ? 1_554 2.7561(9) ? Sn1 Cu6 ? ? 2.7561(9) ? Sn1 Cu6 ? 10_554 5.6521(13) ? Sn1 Cu6 ? 10_654 5.6521(13) ? Sn1 Cu7 ? 1_554 5.1403(7) ? Sn1 Cu7 ? ? 2.7662(12) ? Sn1 Cu7 ? 1_556 5.1403(7) ? Sn1 Cu7 ? 1_655 4.7904(9) ? Sn1 Cu7 ? 3_555 4.7904(9) ? Sn1 Cu7 ? 3_654 5.1403(7) ? Sn1 Cu7 ? 3_655 2.7662(12) ? Sn1 Cu7 ? 3_656 5.1403(7) ? Sn1 Cu8 ? 1_554 4.6918(11) ? Sn1 Cu8 ? ? 4.6918(11) ? Sn1 Cu8 ? 3_655 4.6918(11) ? Sn1 Cu8 ? 3_656 4.6918(11) ? Sn2 Sn2 ? 1_455 5.5184(4) ? Sn2 Sn2 ? 1_554 4.3326(4) ? Sn2 Sn2 ? 1_556 4.3326(4) ? Sn2 Sn2 ? 1_655 5.5184(4) ? Sn2 Sn3 ? ? 4.7856(10) ? Sn2 Sn4 ? 1_455 4.7545(6) ? Sn2 Sn4 ? 1_456 4.7545(6) ? Sn2 Sn4 ? ? 4.7545(6) ? Sn2 Sn4 ? 1_556 4.7545(6) ? Sn2 Cu1 ? 1_455 5.6436(13) ? Sn2 Cu1 ? ? 5.6436(13) ? Sn2 Cu2 ? ? 2.7468(9) ? Sn2 Cu2 ? 1_556 2.7468(9) ? Sn2 Cu2 ? 10_455 5.3855(12) ? Sn2 Cu2 ? 10_555 5.3855(12) ? Sn2 Cu4 ? ? 3.7958(12) ? Sn2 Cu4 ? 1_556 3.7958(12) ? Sn2 Cu5 ? ? 4.6859(12) ? Sn2 Cu5 ? 1_556 4.6859(12) ? Sn2 Cu5 ? 10_455 4.7938(9) ? Sn2 Cu5 ? 10_554 5.1377(7) ? Sn2 Cu5 ? 10_555 2.7612(12) ? Sn2 Cu5 ? 10_556 5.1377(7) ? Sn2 Cu5 ? 3_555 4.6859(12) ? Sn2 Cu5 ? 3_556 4.6859(12) ? Sn2 Cu5 ? 12_455 5.1377(7) ? Sn2 Cu5 ? 12_456 2.7612(12) ? Sn2 Cu5 ? 12_457 5.1377(7) ? Sn2 Cu5 ? 12_556 4.7938(9) ? Sn2 Cu6 ? 1_454 5.1391(4) ? Sn2 Cu6 ? 1_455 2.7639(2) ? Sn2 Cu6 ? 1_456 5.1391(4) ? Sn2 Cu6 ? 1_554 5.1391(4) ? Sn2 Cu6 ? ? 2.7639(2) ? Sn2 Cu6 ? 1_556 5.1391(4) ? Sn2 Cu7 ? 1_455 4.7442(6) ? Sn2 Cu7 ? 1_456 4.7442(6) ? Sn2 Cu7 ? ? 2.7113(5) ? Sn2 Cu7 ? 1_556 2.7113(5) ? Sn2 Cu7 ? 3_555 2.7113(5) ? Sn2 Cu7 ? 3_556 2.7113(5) ? Sn2 Cu7 ? 3_655 4.7442(6) ? Sn2 Cu7 ? 3_656 4.7442(6) ? Sn2 Cu8 ? 1_455 4.7884(8) ? Sn2 Cu8 ? 1_554 5.1265(7) ? Sn2 Cu8 ? ? 2.7403(11) ? Sn2 Cu8 ? 1_556 5.1265(7) ? Sn2 Cu8 ? 3_555 5.1265(7) ? Sn2 Cu8 ? 3_556 2.7403(11) ? Sn2 Cu8 ? 3_557 5.1265(7) ? Sn2 Cu8 ? 3_656 4.7884(8) ? Sn3 Sn3 ? 1_455 5.5184(4) ? Sn3 Sn3 ? 1_554 4.3326(4) ? Sn3 Sn3 ? 1_556 4.3326(4) ? Sn3 Sn3 ? 1_655 5.5184(4) ? Sn3 Sn3 ? 2_564 3.8906(8) ? Sn3 Sn3 ? 2_565 3.8906(8) ? Sn3 Sn4 ? 1_455 3.8459(4) ? Sn3 Sn4 ? 1_456 3.8459(4) ? Sn3 Sn4 ? ? 3.8459(4) ? Sn3 Sn4 ? 1_556 3.8459(4) ? Sn3 Sn4 ? 2_565 5.5436(9) ? Sn3 Sn4 ? 2_665 5.5436(9) ? Sn3 Cu1 ? 1_454 5.1384(4) ? Sn3 Cu1 ? 1_455 2.7626(2) ? Sn3 Cu1 ? 1_456 5.1384(4) ? Sn3 Cu1 ? 1_554 5.1384(4) ? Sn3 Cu1 ? ? 2.7626(2) ? Sn3 Cu1 ? 1_556 5.1384(4) ? Sn3 Cu1 ? 2_564 4.6777(10) ? Sn3 Cu1 ? 2_565 4.6777(10) ? Sn3 Cu1 ? 2_664 4.6777(10) ? Sn3 Cu1 ? 2_665 4.6777(10) ? Sn3 Cu3 ? 1_455 4.6929(7) ? Sn3 Cu3 ? 1_456 4.6929(7) ? Sn3 Cu3 ? ? 2.7402(6) ? Sn3 Cu3 ? 1_556 2.7402(6) ? Sn3 Cu3 ? 2_564 5.1484(7) ? Sn3 Cu3 ? 2_565 2.7812(12) ? Sn3 Cu3 ? 2_566 5.1484(7) ? Sn3 Cu3 ? 2_665 4.7170(9) ? Sn3 Cu3 ? 3_555 2.7402(6) ? Sn3 Cu3 ? 3_556 2.7402(6) ? Sn3 Cu3 ? 3_655 4.6929(7) ? Sn3 Cu3 ? 3_656 4.6929(7) ? Sn3 Cu3 ? 4_466 4.7170(9) ? Sn3 Cu3 ? 4_565 5.1484(7) ? Sn3 Cu3 ? 4_566 2.7812(12) ? Sn3 Cu3 ? 4_567 5.1484(7) ? Sn3 Cu4 ? ? 2.7345(9) ? Sn3 Cu4 ? 1_556 2.7345(9) ? Sn3 Cu4 ? 2_565 4.9005(15) ? Sn3 Cu6 ? 1_455 5.3848(13) ? Sn3 Cu6 ? ? 5.3848(13) ? Sn3 Cu7 ? ? 4.6940(11) ? Sn3 Cu7 ? 1_556 4.6940(11) ? Sn3 Cu7 ? 3_555 4.6940(11) ? Sn3 Cu7 ? 3_556 4.6940(11) ? Sn3 Cu8 ? 1_455 4.8034(9) ? Sn3 Cu8 ? 1_554 5.1405(7) ? Sn3 Cu8 ? ? 2.7664(12) ? Sn3 Cu8 ? 1_556 5.1405(7) ? Sn3 Cu8 ? 3_555 5.1405(7) ? Sn3 Cu8 ? 3_556 2.7664(12) ? Sn3 Cu8 ? 3_557 5.1405(7) ? Sn3 Cu8 ? 3_656 4.8034(9) ? Sn4 Sn4 ? 1_455 5.5184(4) ? Sn4 Sn4 ? 1_554 4.3326(4) ? Sn4 Sn4 ? 1_556 4.3326(4) ? Sn4 Sn4 ? 1_655 5.5184(4) ? Sn4 Cu1 ? 1_554 2.7623(9) ? Sn4 Cu1 ? ? 2.7623(9) ? Sn4 Cu1 ? 2_664 4.6707(15) ? Sn4 Cu2 ? ? 5.6217(13) ? Sn4 Cu2 ? 1_655 5.6217(13) ? Sn4 Cu3 ? 1_554 5.1393(7) ? Sn4 Cu3 ? ? 2.7641(12) ? Sn4 Cu3 ? 1_556 5.1393(7) ? Sn4 Cu3 ? 1_655 4.8558(9) ? Sn4 Cu3 ? 2_664 4.6959(12) ? Sn4 Cu3 ? 2_665 4.6959(12) ? Sn4 Cu3 ? 3_555 4.8558(9) ? Sn4 Cu3 ? 3_654 5.1393(7) ? Sn4 Cu3 ? 3_655 2.7641(12) ? Sn4 Cu3 ? 3_656 5.1393(7) ? Sn4 Cu3 ? 4_565 4.6959(12) ? Sn4 Cu3 ? 4_566 4.6959(12) ? Sn4 Cu4 ? 1_554 5.1374(4) ? Sn4 Cu4 ? ? 2.7607(2) ? Sn4 Cu4 ? 1_556 5.1374(4) ? Sn4 Cu4 ? 1_654 5.1374(4) ? Sn4 Cu4 ? 1_655 2.7607(2) ? Sn4 Cu4 ? 1_656 5.1374(4) ? Sn4 Cu6 ? 1_554 3.7392(12) ? Sn4 Cu6 ? ? 3.7392(12) ? Sn4 Cu7 ? 1_554 5.1168(7) ? Sn4 Cu7 ? ? 2.7222(12) ? Sn4 Cu7 ? 1_556 5.1168(7) ? Sn4 Cu7 ? 1_655 4.7652(9) ? Sn4 Cu7 ? 3_555 4.7652(9) ? Sn4 Cu7 ? 3_654 5.1168(7) ? Sn4 Cu7 ? 3_655 2.7222(12) ? Sn4 Cu7 ? 3_656 5.1168(7) ? Sn4 Cu8 ? 1_554 2.7085(5) ? Sn4 Cu8 ? ? 2.7085(5) ? Sn4 Cu8 ? 1_654 4.7296(6) ? Sn4 Cu8 ? 1_655 4.7296(6) ? Sn4 Cu8 ? 3_555 4.7296(6) ? Sn4 Cu8 ? 3_556 4.7296(6) ? Sn4 Cu8 ? 3_655 2.7085(5) ? Sn4 Cu8 ? 3_656 2.7085(5) ? Cu1 Cu1 ? 1_455 5.5184(4) ? Cu1 Cu1 ? 1_554 4.3326(4) ? Cu1 Cu1 ? 1_556 4.3326(4) ? Cu1 Cu1 ? 1_655 5.5184(4) ? Cu1 Cu1 ? 2_664 3.6655(15) ? Cu1 Cu1 ? 2_665 3.6655(15) ? Cu1 Cu3 ? ? 2.6338(6) ? Cu1 Cu3 ? 1_556 2.6338(6) ? Cu1 Cu3 ? 1_655 4.7828(7) ? Cu1 Cu3 ? 1_656 4.7828(7) ? Cu1 Cu3 ? 2_565 4.7626(10) ? Cu1 Cu3 ? 2_664 5.0514(9) ? Cu1 Cu3 ? 2_665 2.5971(15) ? Cu1 Cu3 ? 2_666 5.0514(9) ? Cu1 Cu3 ? 3_555 4.7828(7) ? Cu1 Cu3 ? 3_556 4.7828(7) ? Cu1 Cu3 ? 3_655 2.6338(6) ? Cu1 Cu3 ? 3_656 2.6338(6) ? Cu1 Cu3 ? 4_565 5.0514(9) ? Cu1 Cu3 ? 4_566 2.5971(15) ? Cu1 Cu3 ? 4_567 5.0514(9) ? Cu1 Cu3 ? 4_666 4.7626(10) ? Cu1 Cu4 ? ? 3.9457(8) ? Cu1 Cu4 ? 1_556 3.9457(8) ? Cu1 Cu4 ? 1_655 3.9457(8) ? Cu1 Cu4 ? 1_656 3.9457(8) ? Cu1 Cu4 ? 2_565 5.5045(16) ? Cu1 Cu4 ? 2_665 5.5045(16) ? Cu1 Cu6 ? ? 4.7616(19) ? Cu1 Cu7 ? ? 4.8060(15) ? Cu1 Cu7 ? 1_556 4.8060(15) ? Cu1 Cu7 ? 3_655 4.8060(15) ? Cu1 Cu7 ? 3_656 4.8060(15) ? Cu1 Cu8 ? 1_554 5.2155(9) ? Cu1 Cu8 ? ? 2.9035(15) ? Cu1 Cu8 ? 1_556 5.2155(9) ? Cu1 Cu8 ? 1_655 4.8439(10) ? Cu1 Cu8 ? 3_556 4.8439(10) ? Cu1 Cu8 ? 3_655 5.2155(9) ? Cu1 Cu8 ? 3_656 2.9035(15) ? Cu1 Cu8 ? 3_657 5.2155(9) ? Cu2 Cu2 ? 1_455 5.5184(4) ? Cu2 Cu2 ? 1_554 4.3326(4) ? Cu2 Cu2 ? 1_556 4.3326(4) ? Cu2 Cu2 ? 1_655 5.5184(4) ? Cu2 Cu2 ? 10_454 4.5746(11) ? Cu2 Cu2 ? 10_455 4.5746(11) ? Cu2 Cu2 ? 10_554 4.5746(11) ? Cu2 Cu2 ? 10_555 4.5746(11) ? Cu2 Cu4 ? ? 4.8057(18) ? Cu2 Cu5 ? 1_455 4.6893(10) ? Cu2 Cu5 ? 1_554 5.0660(8) ? Cu2 Cu5 ? ? 2.6254(15) ? Cu2 Cu5 ? 1_556 5.0660(8) ? Cu2 Cu5 ? 10_454 4.7354(6) ? Cu2 Cu5 ? 10_455 4.7354(6) ? Cu2 Cu5 ? 10_554 2.6585(6) ? Cu2 Cu5 ? 10_555 2.6585(6) ? Cu2 Cu5 ? 3_554 5.0660(8) ? Cu2 Cu5 ? 3_555 2.6254(15) ? Cu2 Cu5 ? 3_556 5.0660(8) ? Cu2 Cu5 ? 3_655 4.6893(10) ? Cu2 Cu5 ? 12_455 2.6585(6) ? Cu2 Cu5 ? 12_456 2.6585(6) ? Cu2 Cu5 ? 12_555 4.7354(6) ? Cu2 Cu5 ? 12_556 4.7354(6) ? Cu2 Cu6 ? 1_454 3.9661(9) ? Cu2 Cu6 ? 1_455 3.9661(9) ? Cu2 Cu6 ? 1_554 3.9661(9) ? Cu2 Cu6 ? ? 3.9661(9) ? Cu2 Cu6 ? 10_554 4.7865(19) ? Cu2 Cu7 ? 1_455 4.8546(10) ? Cu2 Cu7 ? 1_554 5.2137(9) ? Cu2 Cu7 ? ? 2.9002(15) ? Cu2 Cu7 ? 1_556 5.2137(9) ? Cu2 Cu7 ? 3_554 5.2137(9) ? Cu2 Cu7 ? 3_555 2.9002(15) ? Cu2 Cu7 ? 3_556 5.2137(9) ? Cu2 Cu7 ? 3_655 4.8546(10) ? Cu2 Cu8 ? 1_554 4.8047(14) ? Cu2 Cu8 ? ? 4.8047(14) ? Cu2 Cu8 ? 3_555 4.8047(14) ? Cu2 Cu8 ? 3_556 4.8047(14) ? Cu3 Cu3 ? 1_455 5.5184(10) ? Cu3 Cu3 ? 1_554 4.3326(4) ? Cu3 Cu3 ? 1_556 4.3326(4) ? Cu3 Cu3 ? 1_655 5.5184(10) ? Cu3 Cu3 ? 2_564 3.9180(9) ? Cu3 Cu3 ? 2_565 3.9180(9) ? Cu3 Cu3 ? 2_664 3.7320(9) ? Cu3 Cu3 ? 2_665 3.7320(9) ? Cu3 Cu3 ? 3_554 5.2070(6) ? Cu3 Cu3 ? 3_555 2.8881(9) ? Cu3 Cu3 ? 3_556 5.2070(6) ? Cu3 Cu3 ? 3_654 5.0685(6) ? Cu3 Cu3 ? 3_655 2.6303(9) ? Cu3 Cu3 ? 3_656 5.0685(6) ? Cu3 Cu3 ? 4_565 2.6476(10) ? Cu3 Cu3 ? 4_566 2.6476(10) ? Cu3 Cu4 ? 1_554 5.2178(9) ? Cu3 Cu4 ? ? 2.9075(15) ? Cu3 Cu4 ? 1_556 5.2178(9) ? Cu3 Cu4 ? 1_655 4.7926(11) ? Cu3 Cu4 ? 2_564 4.8110(15) ? Cu3 Cu4 ? 2_565 4.8110(15) ? Cu3 Cu7 ? ? 4.7821(17) ? Cu3 Cu7 ? 3_555 5.5564(15) ? Cu3 Cu7 ? 3_655 5.4856(15) ? Cu3 Cu8 ? 1_554 3.9172(14) ? Cu3 Cu8 ? ? 3.9172(14) ? Cu3 Cu8 ? 2_564 5.5469(15) ? Cu3 Cu8 ? 2_664 5.5000(15) ? Cu3 Cu8 ? 3_555 4.8179(12) ? Cu3 Cu8 ? 3_556 4.8179(12) ? Cu3 Cu8 ? 3_655 4.7638(12) ? Cu3 Cu8 ? 3_656 4.7638(12) ? Cu3 Cu8 ? 4_566 4.7855(17) ? Cu4 Cu4 ? 1_455 5.5184(4) ? Cu4 Cu4 ? 1_554 4.3326(4) ? Cu4 Cu4 ? 1_556 4.3326(4) ? Cu4 Cu4 ? 1_655 5.5184(4) ? Cu4 Cu6 ? 1_454 4.5870(12) ? Cu4 Cu6 ? 1_455 4.5870(12) ? Cu4 Cu6 ? 1_554 4.5870(12) ? Cu4 Cu6 ? ? 4.5870(12) ? Cu4 Cu7 ? 1_455 4.7092(10) ? Cu4 Cu7 ? 1_554 5.0785(9) ? Cu4 Cu7 ? ? 2.6495(15) ? Cu4 Cu7 ? 1_556 5.0785(9) ? Cu4 Cu7 ? 3_554 5.0785(9) ? Cu4 Cu7 ? 3_555 2.6495(15) ? Cu4 Cu7 ? 3_556 5.0785(9) ? Cu4 Cu7 ? 3_655 4.7092(10) ? Cu4 Cu8 ? 1_454 4.7449(6) ? Cu4 Cu8 ? 1_455 4.7449(6) ? Cu4 Cu8 ? 1_554 2.6635(6) ? Cu4 Cu8 ? ? 2.6635(6) ? Cu4 Cu8 ? 3_555 2.6635(6) ? Cu4 Cu8 ? 3_556 2.6635(6) ? Cu4 Cu8 ? 3_655 4.7449(6) ? Cu4 Cu8 ? 3_656 4.7449(6) ? Cu5 Cu5 ? 1_455 5.5184(9) ? Cu5 Cu5 ? 1_554 4.3326(4) ? Cu5 Cu5 ? 1_556 4.3326(4) ? Cu5 Cu5 ? 1_655 5.5184(9) ? Cu5 Cu5 ? 10_554 2.6446(10) ? Cu5 Cu5 ? 10_555 2.6446(10) ? Cu5 Cu5 ? 3_554 5.1493(6) ? Cu5 Cu5 ? 3_555 2.7827(8) ? Cu5 Cu5 ? 3_556 5.1493(6) ? Cu5 Cu5 ? 3_654 5.1240(6) ? Cu5 Cu5 ? 3_655 2.7357(8) ? Cu5 Cu5 ? 3_656 5.1240(6) ? Cu5 Cu5 ? 12_455 3.8218(9) ? Cu5 Cu5 ? 12_456 3.8218(9) ? Cu5 Cu5 ? 12_555 3.8218(9) ? Cu5 Cu5 ? 12_556 3.8218(9) ? Cu5 Cu6 ? 1_554 4.8149(15) ? Cu5 Cu6 ? ? 4.8149(15) ? Cu5 Cu6 ? 10_553 5.2212(10) ? Cu5 Cu6 ? 10_554 2.9137(16) ? Cu5 Cu6 ? 10_555 5.2212(10) ? Cu5 Cu6 ? 10_654 4.8566(11) ? Cu5 Cu7 ? ? 4.7740(17) ? Cu5 Cu7 ? 10_554 3.9120(14) ? Cu5 Cu7 ? 10_555 3.9120(14) ? Cu5 Cu7 ? 3_555 5.5231(15) ? Cu5 Cu7 ? 3_655 5.5050(15) ? Cu5 Cu7 ? 12_455 4.7902(12) ? Cu5 Cu7 ? 12_456 4.7902(12) ? Cu5 Cu7 ? 12_555 4.7840(12) ? Cu5 Cu7 ? 12_556 4.7840(12) ? Cu5 Cu8 ? 10_554 4.7764(17) ? Cu5 Cu8 ? 12_456 5.5308(15) ? Cu5 Cu8 ? 12_556 5.5015(15) ? Cu6 Cu6 ? 1_455 5.5184(4) ? Cu6 Cu6 ? 1_554 4.3326(4) ? Cu6 Cu6 ? 1_556 4.3326(4) ? Cu6 Cu6 ? 1_655 5.5184(4) ? Cu6 Cu7 ? ? 2.6580(6) ? Cu6 Cu7 ? 1_556 2.6580(6) ? Cu6 Cu7 ? 1_655 4.7288(6) ? Cu6 Cu7 ? 1_656 4.7288(6) ? Cu6 Cu7 ? 3_555 4.7288(6) ? Cu6 Cu7 ? 3_556 4.7288(6) ? Cu6 Cu7 ? 3_655 2.6580(6) ? Cu6 Cu7 ? 3_656 2.6580(6) ? Cu6 Cu8 ? 1_554 5.0632(9) ? Cu6 Cu8 ? ? 2.6199(15) ? Cu6 Cu8 ? 1_556 5.0632(9) ? Cu6 Cu8 ? 1_655 4.6794(10) ? Cu6 Cu8 ? 3_556 4.6794(10) ? Cu6 Cu8 ? 3_655 5.0632(9) ? Cu6 Cu8 ? 3_656 2.6199(15) ? Cu6 Cu8 ? 3_657 5.0632(9) ? Cu7 Cu7 ? 1_455 5.5184(9) ? Cu7 Cu7 ? 1_554 4.3326(4) ? Cu7 Cu7 ? 1_556 4.3326(4) ? Cu7 Cu7 ? 1_655 5.5184(9) ? Cu7 Cu7 ? 3_554 5.1434(6) ? Cu7 Cu7 ? 3_555 2.7718(8) ? Cu7 Cu7 ? 3_556 5.1434(6) ? Cu7 Cu7 ? 3_654 5.1298(6) ? Cu7 Cu7 ? 3_655 2.7466(8) ? Cu7 Cu7 ? 3_656 5.1298(6) ? Cu7 Cu8 ? 1_554 2.6459(9) ? Cu7 Cu8 ? ? 2.6459(9) ? Cu7 Cu8 ? 3_555 3.8147(9) ? Cu7 Cu8 ? 3_556 3.8147(9) ? Cu7 Cu8 ? 3_655 3.8309(9) ? Cu7 Cu8 ? 3_656 3.8309(9) ? Cu8 Cu8 ? 1_455 5.5184(9) ? Cu8 Cu8 ? 1_554 4.3326(4) ? Cu8 Cu8 ? 1_556 4.3326(4) ? Cu8 Cu8 ? 1_655 5.5184(9) ? Cu8 Cu8 ? 3_555 5.1179(6) ? Cu8 Cu8 ? 3_556 2.7241(8) ? Cu8 Cu8 ? 3_557 5.1179(6) ? Cu8 Cu8 ? 3_655 5.1555(6) ? Cu8 Cu8 ? 3_656 2.7943(8) ? Cu8 Cu8 ? 3_657 5.1555(6) ? data_823K-superstructure _chemical_formula_structural 'Cu3 Sn1' _chemical_formula_sum 'Cu3 Sn1' _chemical_formula_weight 309.3 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'C m c m' _space_group_name_Hall '-C -2x;-2yc;-2zc' _space_group_IT_number 63 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z+1/2 3 -x,y,-z+1/2 4 x,-y,-z 5 -x,-y,-z 6 x,y,-z+1/2 7 x,-y,z+1/2 8 -x,y,z 9 x+1/2,y+1/2,z 10 -x+1/2,-y+1/2,z+1/2 11 -x+1/2,y+1/2,-z+1/2 12 x+1/2,-y+1/2,-z 13 -x+1/2,-y+1/2,-z 14 x+1/2,y+1/2,-z+1/2 15 x+1/2,-y+1/2,z+1/2 16 -x+1/2,y+1/2,z _cell_length_a 5.51990(10) _cell_length_b 47.7904(9) _cell_length_c 4.33260(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1142.93(4) _cell_formula_units_Z 20 _cell_measurement_reflns_used 1970 _cell_measurement_theta_min 4.26 _cell_measurement_theta_max 28.18 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 8.986 _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 37.885 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.077 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.043 _exptl_crystal_colour 'metallic grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.281 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 8648 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.38 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_unetI/netI 0.0095 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -59 _diffrn_reflns_limit_k_max 61 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 855 _reflns_number_gt 447 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_gt 0.0797 _refine_ls_R_factor_all 0.0467 _refine_ls_wR_factor_ref 0.0884 _refine_ls_goodness_of_fit_ref 1.71 _refine_ls_goodness_of_fit_gt 2.23 _refine_ls_number_reflns 855 _refine_ls_number_parameters 72 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0339 _refine_ls_shift/su_mean 0.0083 _refine_diff_density_max 1.35 _refine_diff_density_min -1.20 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 255(11) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.23386(2) 0.25 Uani 0.0090(3) 4 1 d ? ? ? Sn2 Sn 0 0.13385(2) 0.25 Uani 0.0104(3) 4 1 d ? ? ? Sn3 Sn 0.5 0.06676(2) 0.75 Uani 0.0110(3) 4 1 d ? ? ? Sn4 Sn 0.5 0.16631(2) 0.75 Uani 0.0107(3) 4 1 d ? ? ? Sn5 Sn 0 0.03375(2) 0.25 Uani 0.0108(3) 4 1 d ? ? ? Cu1 Cu 0 0.16917(4) 0.75 Uani 0.0135(6) 4 1 d ? ? ? Cu2 Cu 0.5 0.03086(4) 0.25 Uani 0.0142(6) 4 1 d ? ? ? Cu3 Cu 0 0.06864(4) 0.75 Uani 0.0152(6) 4 1 d ? ? ? Cu4 Cu 0.25197(15) 0.21601(4) 0.75 Uani 0.0123(6) 8 1 d ? ? ? Cu5 Cu 0.24740(16) 0.18434(3) 0.25 Uani 0.0145(6) 8 1 d ? ? ? Cu6 Cu 0.25113(15) 0.11617(4) 0.75 Uani 0.0154(6) 8 1 d ? ? ? Cu7 Cu 0.24664(15) 0.08415(3) 0.25 Uani 0.0126(6) 8 1 d ? ? ? Cu8 Cu 0.26147(17) 0.01599(4) 0.75 Uani 0.0121(5) 8 1 d ? ? ? Cu9 Cu 0.5 0.13038(4) 0.25 Uani 0.0124(6) 4 1 d ? ? ? Cu10 Cu 0.5 0.23075(4) 0.25 Uani 0.0120(6) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0089(6) 0.0096(5) 0.0084(6) 0 0 0 Sn2 Sn 0.0103(6) 0.0114(5) 0.0095(6) 0 0 0 Sn3 Sn 0.0120(6) 0.0098(5) 0.0113(6) 0 0 0 Sn4 Sn 0.0110(6) 0.0102(5) 0.0109(6) 0 0 0 Sn5 Sn 0.0115(6) 0.0098(5) 0.0110(6) 0 0 0 Cu1 Cu 0.0131(11) 0.0153(10) 0.0122(11) 0 0 0 Cu2 Cu 0.0145(11) 0.0152(10) 0.0128(11) 0 0 0 Cu3 Cu 0.0154(11) 0.0166(9) 0.0136(12) 0 0 0 Cu4 Cu 0.0138(10) 0.0128(9) 0.0102(10) -0.0002(3) 0 0 Cu5 Cu 0.0184(11) 0.0143(10) 0.0109(11) -0.0001(3) 0 0 Cu6 Cu 0.0185(12) 0.0141(9) 0.0135(11) 0.0005(4) 0 0 Cu7 Cu 0.0153(12) 0.0117(9) 0.0110(11) -0.0004(3) 0 0 Cu8 Cu 0.0140(10) 0.0108(8) 0.0113(10) -0.0014(3) 0 0 Cu9 Cu 0.0114(11) 0.0148(10) 0.0111(11) 0 0 0 Cu10 Cu 0.0101(10) 0.0165(10) 0.0096(10) 0 0 0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 Sn1 ? 1_455 5.5199(2) ? Sn1 Sn1 ? 1_554 4.3326(2) ? Sn1 Sn1 ? 1_556 4.3326(2) ? Sn1 Sn1 ? 1_655 5.5199(2) ? Sn1 Sn1 ? 10_454 3.8329(6) ? Sn1 Sn1 ? 10_455 3.8329(6) ? Sn1 Sn1 ? 10_554 3.8329(6) ? Sn1 Sn1 ? 10_555 3.8329(6) ? Sn1 Sn2 ? ? 4.7796(15) ? Sn1 Sn4 ? 1_454 4.7678(10) ? Sn1 Sn4 ? 1_455 4.7678(10) ? Sn1 Sn4 ? 1_554 4.7678(10) ? Sn1 Sn4 ? ? 4.7678(10) ? Sn1 Sn4 ? 10_554 4.7712(14) ? Sn1 Cu1 ? 1_554 3.7749(18) ? Sn1 Cu1 ? ? 3.7749(18) ? Sn1 Cu1 ? 10_454 5.3940(18) ? Sn1 Cu1 ? 10_554 5.3940(18) ? Sn1 Cu4 ? 1_454 4.7402(8) ? Sn1 Cu4 ? 1_455 4.7402(8) ? Sn1 Cu4 ? 1_554 2.7119(8) ? Sn1 Cu4 ? ? 2.7119(8) ? Sn1 Cu4 ? 10_454 4.7925(12) ? Sn1 Cu4 ? 10_553 5.1367(10) ? Sn1 Cu4 ? 10_554 2.7594(18) ? Sn1 Cu4 ? 10_555 5.1367(10) ? Sn1 Cu4 ? 3_555 2.7119(8) ? Sn1 Cu4 ? 3_556 2.7119(8) ? Sn1 Cu4 ? 3_655 4.7402(8) ? Sn1 Cu4 ? 3_656 4.7402(8) ? Sn1 Cu4 ? 12_455 5.1367(10) ? Sn1 Cu4 ? 12_456 2.7594(18) ? Sn1 Cu4 ? 12_457 5.1367(10) ? Sn1 Cu4 ? 12_556 4.7925(12) ? Sn1 Cu5 ? 1_455 4.7809(12) ? Sn1 Cu5 ? 1_554 5.1221(9) ? Sn1 Cu5 ? ? 2.7320(17) ? Sn1 Cu5 ? 1_556 5.1221(9) ? Sn1 Cu5 ? 10_554 4.6818(16) ? Sn1 Cu5 ? 10_555 4.6818(16) ? Sn1 Cu5 ? 3_554 5.1221(9) ? Sn1 Cu5 ? 3_555 2.7320(17) ? Sn1 Cu5 ? 3_556 5.1221(9) ? Sn1 Cu5 ? 3_655 4.7809(12) ? Sn1 Cu5 ? 12_455 4.6818(16) ? Sn1 Cu5 ? 12_456 4.6818(16) ? Sn1 Cu9 ? 1_455 5.6633(18) ? Sn1 Cu9 ? ? 5.6633(18) ? Sn1 Cu10 ? 1_454 5.13914(19) ? Sn1 Cu10 ? 1_455 2.76394(15) ? Sn1 Cu10 ? 1_456 5.13914(19) ? Sn1 Cu10 ? 1_554 5.13914(19) ? Sn1 Cu10 ? ? 2.76394(15) ? Sn1 Cu10 ? 1_556 5.13914(19) ? Sn1 Cu10 ? 10_554 2.7484(13) ? Sn1 Cu10 ? 10_555 2.7484(13) ? Sn2 Sn2 ? 1_455 5.5199(2) ? Sn2 Sn2 ? 1_554 4.3326(2) ? Sn2 Sn2 ? 1_556 4.3326(2) ? Sn2 Sn2 ? 1_655 5.5199(2) ? Sn2 Sn3 ? 1_454 4.7528(10) ? Sn2 Sn3 ? 1_455 4.7528(10) ? Sn2 Sn3 ? 1_554 4.7528(10) ? Sn2 Sn3 ? ? 4.7528(10) ? Sn2 Sn4 ? 1_454 3.8362(6) ? Sn2 Sn4 ? 1_455 3.8362(6) ? Sn2 Sn4 ? 1_554 3.8362(6) ? Sn2 Sn4 ? ? 3.8362(6) ? Sn2 Sn5 ? ? 4.7838(15) ? Sn2 Cu1 ? 1_554 2.7464(13) ? Sn2 Cu1 ? ? 2.7464(13) ? Sn2 Cu2 ? 1_455 5.643(2) ? Sn2 Cu2 ? ? 5.643(2) ? Sn2 Cu3 ? 1_554 3.7954(19) ? Sn2 Cu3 ? ? 3.7954(19) ? Sn2 Cu4 ? 1_554 4.6954(17) ? Sn2 Cu4 ? ? 4.6954(17) ? Sn2 Cu4 ? 3_555 4.6954(17) ? Sn2 Cu4 ? 3_556 4.6954(17) ? Sn2 Cu5 ? 1_455 4.8044(12) ? Sn2 Cu5 ? 1_554 5.1440(9) ? Sn2 Cu5 ? ? 2.7729(17) ? Sn2 Cu5 ? 1_556 5.1440(9) ? Sn2 Cu5 ? 3_554 5.1440(9) ? Sn2 Cu5 ? 3_555 2.7729(17) ? Sn2 Cu5 ? 3_556 5.1440(9) ? Sn2 Cu5 ? 3_655 4.8044(12) ? Sn2 Cu6 ? 1_454 4.7427(8) ? Sn2 Cu6 ? 1_455 4.7427(8) ? Sn2 Cu6 ? 1_554 2.7070(8) ? Sn2 Cu6 ? ? 2.7070(8) ? Sn2 Cu6 ? 3_555 2.7070(8) ? Sn2 Cu6 ? 3_556 2.7070(8) ? Sn2 Cu6 ? 3_655 4.7427(8) ? Sn2 Cu6 ? 3_656 4.7427(8) ? Sn2 Cu7 ? 1_455 4.7890(12) ? Sn2 Cu7 ? 1_554 5.1250(9) ? Sn2 Cu7 ? ? 2.7376(17) ? Sn2 Cu7 ? 1_556 5.1250(9) ? Sn2 Cu7 ? 3_554 5.1250(9) ? Sn2 Cu7 ? 3_555 2.7376(17) ? Sn2 Cu7 ? 3_556 5.1250(9) ? Sn2 Cu7 ? 3_655 4.7890(12) ? Sn2 Cu9 ? 1_454 5.13967(19) ? Sn2 Cu9 ? 1_455 2.76492(16) ? Sn2 Cu9 ? 1_456 5.13967(19) ? Sn2 Cu9 ? 1_554 5.13967(19) ? Sn2 Cu9 ? ? 2.76492(16) ? Sn2 Cu9 ? 1_556 5.13967(19) ? Sn2 Cu10 ? 1_455 5.3911(19) ? Sn2 Cu10 ? ? 5.3911(19) ? Sn3 Sn3 ? 1_455 5.5199(2) ? Sn3 Sn3 ? 1_554 4.3326(2) ? Sn3 Sn3 ? 1_556 4.3326(2) ? Sn3 Sn3 ? 1_655 5.5199(2) ? Sn3 Sn4 ? ? 4.7573(14) ? Sn3 Sn5 ? ? 3.8470(6) ? Sn3 Sn5 ? 1_556 3.8470(6) ? Sn3 Sn5 ? 1_655 3.8470(6) ? Sn3 Sn5 ? 1_656 3.8470(6) ? Sn3 Sn5 ? 2_555 5.5397(13) ? Sn3 Sn5 ? 2_655 5.5397(13) ? Sn3 Cu1 ? ? 5.6187(19) ? Sn3 Cu1 ? 1_655 5.6187(19) ? Sn3 Cu2 ? ? 2.7636(14) ? Sn3 Cu2 ? 1_556 2.7636(14) ? Sn3 Cu2 ? 2_655 4.665(2) ? Sn3 Cu3 ? 1_554 5.13778(18) ? Sn3 Cu3 ? ? 2.76140(12) ? Sn3 Cu3 ? 1_556 5.13778(18) ? Sn3 Cu3 ? 1_654 5.13778(18) ? Sn3 Cu3 ? 1_655 2.76140(12) ? Sn3 Cu3 ? 1_656 5.13778(18) ? Sn3 Cu6 ? 1_554 5.1220(10) ? Sn3 Cu6 ? ? 2.7319(18) ? Sn3 Cu6 ? 1_556 5.1220(10) ? Sn3 Cu6 ? 1_655 4.7715(12) ? Sn3 Cu6 ? 3_556 4.7715(12) ? Sn3 Cu6 ? 3_655 5.1220(10) ? Sn3 Cu6 ? 3_656 2.7319(18) ? Sn3 Cu6 ? 3_657 5.1220(10) ? Sn3 Cu7 ? ? 2.7091(7) ? Sn3 Cu7 ? 1_556 2.7091(7) ? Sn3 Cu7 ? 1_655 4.7296(8) ? Sn3 Cu7 ? 1_656 4.7296(8) ? Sn3 Cu7 ? 3_555 4.7296(8) ? Sn3 Cu7 ? 3_556 4.7296(8) ? Sn3 Cu7 ? 3_655 2.7091(7) ? Sn3 Cu7 ? 3_656 2.7091(7) ? Sn3 Cu8 ? 1_554 5.1374(10) ? Sn3 Cu8 ? ? 2.7607(18) ? Sn3 Cu8 ? 1_556 5.1374(10) ? Sn3 Cu8 ? 1_655 4.8534(13) ? Sn3 Cu8 ? 2_654 4.6973(17) ? Sn3 Cu8 ? 2_655 4.6973(17) ? Sn3 Cu8 ? 3_556 4.8534(13) ? Sn3 Cu8 ? 3_655 5.1374(10) ? Sn3 Cu8 ? 3_656 2.7607(18) ? Sn3 Cu8 ? 3_657 5.1374(10) ? Sn3 Cu8 ? 4_556 4.6973(17) ? Sn3 Cu8 ? 4_557 4.6973(17) ? Sn3 Cu9 ? ? 3.7331(17) ? Sn3 Cu9 ? 1_556 3.7331(17) ? Sn4 Sn4 ? 1_455 5.5199(2) ? Sn4 Sn4 ? 1_554 4.3326(2) ? Sn4 Sn4 ? 1_556 4.3326(2) ? Sn4 Sn4 ? 1_655 5.5199(2) ? Sn4 Cu1 ? 1_554 5.13882(19) ? Sn4 Cu1 ? ? 2.76334(14) ? Sn4 Cu1 ? 1_556 5.13882(19) ? Sn4 Cu1 ? 1_654 5.13882(19) ? Sn4 Cu1 ? 1_655 2.76334(14) ? Sn4 Cu1 ? 1_656 5.13882(19) ? Sn4 Cu3 ? ? 5.4226(19) ? Sn4 Cu3 ? 1_655 5.4226(19) ? Sn4 Cu4 ? 1_554 5.1273(10) ? Sn4 Cu4 ? ? 2.7418(18) ? Sn4 Cu4 ? 1_556 5.1273(10) ? Sn4 Cu4 ? 1_655 4.7825(12) ? Sn4 Cu4 ? 3_556 4.7825(12) ? Sn4 Cu4 ? 3_655 5.1273(10) ? Sn4 Cu4 ? 3_656 2.7418(18) ? Sn4 Cu4 ? 3_657 5.1273(10) ? Sn4 Cu5 ? ? 2.7166(7) ? Sn4 Cu5 ? 1_556 2.7166(7) ? Sn4 Cu5 ? 1_655 4.7388(8) ? Sn4 Cu5 ? 1_656 4.7388(8) ? Sn4 Cu5 ? 3_555 4.7388(8) ? Sn4 Cu5 ? 3_556 4.7388(8) ? Sn4 Cu5 ? 3_655 2.7166(7) ? Sn4 Cu5 ? 3_656 2.7166(7) ? Sn4 Cu6 ? 1_554 5.1380(10) ? Sn4 Cu6 ? ? 2.7618(18) ? Sn4 Cu6 ? 1_556 5.1380(10) ? Sn4 Cu6 ? 1_655 4.7887(12) ? Sn4 Cu6 ? 3_556 4.7887(12) ? Sn4 Cu6 ? 3_655 5.1380(10) ? Sn4 Cu6 ? 3_656 2.7618(18) ? Sn4 Cu6 ? 3_657 5.1380(10) ? Sn4 Cu7 ? ? 4.6974(16) ? Sn4 Cu7 ? 1_556 4.6974(16) ? Sn4 Cu7 ? 3_655 4.6974(16) ? Sn4 Cu7 ? 3_656 4.6974(16) ? Sn4 Cu9 ? ? 2.7642(13) ? Sn4 Cu9 ? 1_556 2.7642(13) ? Sn4 Cu10 ? ? 3.7654(18) ? Sn4 Cu10 ? 1_556 3.7654(18) ? Sn4 Cu10 ? 10_555 5.6410(19) ? Sn4 Cu10 ? 10_655 5.6410(19) ? Sn5 Sn5 ? 1_455 5.5199(2) ? Sn5 Sn5 ? 1_554 4.3326(2) ? Sn5 Sn5 ? 1_556 4.3326(2) ? Sn5 Sn5 ? 1_655 5.5199(2) ? Sn5 Sn5 ? 2_554 3.8854(12) ? Sn5 Sn5 ? 2_555 3.8854(12) ? Sn5 Cu2 ? 1_454 5.13885(19) ? Sn5 Cu2 ? 1_455 2.76340(15) ? Sn5 Cu2 ? 1_456 5.13885(19) ? Sn5 Cu2 ? 1_554 5.13885(19) ? Sn5 Cu2 ? ? 2.76340(15) ? Sn5 Cu2 ? 1_556 5.13885(19) ? Sn5 Cu2 ? 2_554 4.6735(15) ? Sn5 Cu2 ? 2_555 4.6735(15) ? Sn5 Cu2 ? 2_654 4.6735(15) ? Sn5 Cu2 ? 2_655 4.6735(15) ? Sn5 Cu3 ? 1_554 2.7337(14) ? Sn5 Cu3 ? ? 2.7337(14) ? Sn5 Cu3 ? 2_554 4.893(2) ? Sn5 Cu6 ? 1_554 4.7044(17) ? Sn5 Cu6 ? ? 4.7044(17) ? Sn5 Cu6 ? 3_555 4.7044(17) ? Sn5 Cu6 ? 3_556 4.7044(17) ? Sn5 Cu7 ? 1_455 4.8057(12) ? Sn5 Cu7 ? 1_554 5.1407(9) ? Sn5 Cu7 ? ? 2.7668(17) ? Sn5 Cu7 ? 1_556 5.1407(9) ? Sn5 Cu7 ? 3_554 5.1407(9) ? Sn5 Cu7 ? 3_555 2.7668(17) ? Sn5 Cu7 ? 3_556 5.1407(9) ? Sn5 Cu7 ? 3_655 4.8057(12) ? Sn5 Cu8 ? 1_454 4.6938(9) ? Sn5 Cu8 ? 1_455 4.6938(9) ? Sn5 Cu8 ? 1_554 2.7379(8) ? Sn5 Cu8 ? ? 2.7379(8) ? Sn5 Cu8 ? 2_553 5.1481(10) ? Sn5 Cu8 ? 2_554 2.7807(18) ? Sn5 Cu8 ? 2_555 5.1481(10) ? Sn5 Cu8 ? 2_654 4.7189(13) ? Sn5 Cu8 ? 3_555 2.7379(8) ? Sn5 Cu8 ? 3_556 2.7379(8) ? Sn5 Cu8 ? 3_655 4.6938(9) ? Sn5 Cu8 ? 3_656 4.6938(9) ? Sn5 Cu8 ? 4_456 4.7189(13) ? Sn5 Cu8 ? 4_555 5.1481(10) ? Sn5 Cu8 ? 4_556 2.7807(18) ? Sn5 Cu8 ? 4_557 5.1481(10) ? Sn5 Cu9 ? 1_455 5.3800(18) ? Sn5 Cu9 ? ? 5.3800(18) ? Cu1 Cu1 ? 1_455 5.5199(2) ? Cu1 Cu1 ? 1_554 4.3326(2) ? Cu1 Cu1 ? 1_556 4.3326(2) ? Cu1 Cu1 ? 1_655 5.5199(2) ? Cu1 Cu3 ? ? 4.805(3) ? Cu1 Cu4 ? 1_455 4.6969(14) ? Cu1 Cu4 ? 1_554 5.0713(12) ? Cu1 Cu4 ? ? 2.636(2) ? Cu1 Cu4 ? 1_556 5.0713(12) ? Cu1 Cu4 ? 3_555 5.0713(12) ? Cu1 Cu4 ? 3_556 2.636(2) ? Cu1 Cu4 ? 3_557 5.0713(12) ? Cu1 Cu4 ? 3_656 4.6969(14) ? Cu1 Cu5 ? 1_455 4.7410(8) ? Cu1 Cu5 ? 1_456 4.7410(8) ? Cu1 Cu5 ? ? 2.6615(8) ? Cu1 Cu5 ? 1_556 2.6615(8) ? Cu1 Cu5 ? 3_555 2.6615(8) ? Cu1 Cu5 ? 3_556 2.6615(8) ? Cu1 Cu5 ? 3_655 4.7410(8) ? Cu1 Cu5 ? 3_656 4.7410(8) ? Cu1 Cu6 ? 1_455 4.8479(15) ? Cu1 Cu6 ? 1_554 5.2065(13) ? Cu1 Cu6 ? ? 2.887(2) ? Cu1 Cu6 ? 1_556 5.2065(13) ? Cu1 Cu6 ? 3_555 5.2065(13) ? Cu1 Cu6 ? 3_556 2.887(2) ? Cu1 Cu6 ? 3_557 5.2065(13) ? Cu1 Cu6 ? 3_656 4.8479(15) ? Cu1 Cu7 ? ? 4.802(2) ? Cu1 Cu7 ? 1_556 4.802(2) ? Cu1 Cu7 ? 3_555 4.802(2) ? Cu1 Cu7 ? 3_556 4.802(2) ? Cu1 Cu9 ? 1_455 3.9682(12) ? Cu1 Cu9 ? 1_456 3.9682(12) ? Cu1 Cu9 ? ? 3.9682(12) ? Cu1 Cu9 ? 1_556 3.9682(12) ? Cu1 Cu10 ? 1_455 4.5794(17) ? Cu1 Cu10 ? 1_456 4.5794(17) ? Cu1 Cu10 ? ? 4.5794(17) ? Cu1 Cu10 ? 1_556 4.5794(17) ? Cu1 Cu10 ? 10_555 4.783(3) ? Cu2 Cu2 ? 1_455 5.5199(2) ? Cu2 Cu2 ? 1_554 4.3326(2) ? Cu2 Cu2 ? 1_556 4.3326(2) ? Cu2 Cu2 ? 1_655 5.5199(2) ? Cu2 Cu2 ? 2_654 3.659(2) ? Cu2 Cu2 ? 2_655 3.659(2) ? Cu2 Cu3 ? 1_554 3.9459(13) ? Cu2 Cu3 ? ? 3.9459(13) ? Cu2 Cu3 ? 1_654 3.9459(13) ? Cu2 Cu3 ? 1_655 3.9459(13) ? Cu2 Cu3 ? 2_554 5.498(2) ? Cu2 Cu3 ? 2_654 5.498(2) ? Cu2 Cu6 ? 1_554 4.817(2) ? Cu2 Cu6 ? ? 4.817(2) ? Cu2 Cu6 ? 3_655 4.817(2) ? Cu2 Cu6 ? 3_656 4.817(2) ? Cu2 Cu7 ? 1_554 5.2167(13) ? Cu2 Cu7 ? ? 2.906(2) ? Cu2 Cu7 ? 1_556 5.2167(13) ? Cu2 Cu7 ? 1_655 4.8448(15) ? Cu2 Cu7 ? 3_555 4.8448(15) ? Cu2 Cu7 ? 3_654 5.2167(13) ? Cu2 Cu7 ? 3_655 2.906(2) ? Cu2 Cu7 ? 3_656 5.2167(13) ? Cu2 Cu8 ? 1_554 2.6328(9) ? Cu2 Cu8 ? ? 2.6328(9) ? Cu2 Cu8 ? 1_654 4.7817(9) ? Cu2 Cu8 ? 1_655 4.7817(9) ? Cu2 Cu8 ? 2_554 4.7622(15) ? Cu2 Cu8 ? 2_653 5.0514(12) ? Cu2 Cu8 ? 2_654 2.597(2) ? Cu2 Cu8 ? 2_655 5.0514(12) ? Cu2 Cu8 ? 3_555 4.7817(9) ? Cu2 Cu8 ? 3_556 4.7817(9) ? Cu2 Cu8 ? 3_655 2.6328(9) ? Cu2 Cu8 ? 3_656 2.6328(9) ? Cu2 Cu8 ? 4_555 5.0514(12) ? Cu2 Cu8 ? 4_556 2.597(2) ? Cu2 Cu8 ? 4_557 5.0514(12) ? Cu2 Cu8 ? 4_656 4.7622(15) ? Cu2 Cu9 ? ? 4.756(3) ? Cu3 Cu3 ? 1_455 5.5199(2) ? Cu3 Cu3 ? 1_554 4.3326(2) ? Cu3 Cu3 ? 1_556 4.3326(2) ? Cu3 Cu3 ? 1_655 5.5199(2) ? Cu3 Cu6 ? 1_455 4.7168(15) ? Cu3 Cu6 ? 1_554 5.0847(12) ? Cu3 Cu6 ? ? 2.661(2) ? Cu3 Cu6 ? 1_556 5.0847(12) ? Cu3 Cu6 ? 3_555 5.0847(12) ? Cu3 Cu6 ? 3_556 2.661(2) ? Cu3 Cu6 ? 3_557 5.0847(12) ? Cu3 Cu6 ? 3_656 4.7168(15) ? Cu3 Cu7 ? 1_455 4.7472(8) ? Cu3 Cu7 ? 1_456 4.7472(8) ? Cu3 Cu7 ? ? 2.6638(8) ? Cu3 Cu7 ? 1_556 2.6638(8) ? Cu3 Cu7 ? 3_555 2.6638(8) ? Cu3 Cu7 ? 3_556 2.6638(8) ? Cu3 Cu7 ? 3_655 4.7472(8) ? Cu3 Cu7 ? 3_656 4.7472(8) ? Cu3 Cu8 ? 1_455 4.7906(16) ? Cu3 Cu8 ? 1_554 5.2139(13) ? Cu3 Cu8 ? ? 2.901(2) ? Cu3 Cu8 ? 1_556 5.2139(13) ? Cu3 Cu8 ? 2_554 4.809(2) ? Cu3 Cu8 ? 2_555 4.809(2) ? Cu3 Cu8 ? 3_555 5.2139(13) ? Cu3 Cu8 ? 3_556 2.901(2) ? Cu3 Cu8 ? 3_557 5.2139(13) ? Cu3 Cu8 ? 3_656 4.7906(16) ? Cu3 Cu8 ? 4_556 4.809(2) ? Cu3 Cu8 ? 4_557 4.809(2) ? Cu3 Cu9 ? 1_455 4.5844(17) ? Cu3 Cu9 ? 1_456 4.5844(17) ? Cu3 Cu9 ? ? 4.5844(17) ? Cu3 Cu9 ? 1_556 4.5844(17) ? Cu4 Cu4 ? 1_455 5.5199(12) ? Cu4 Cu4 ? 1_554 4.3326(2) ? Cu4 Cu4 ? 1_556 4.3326(2) ? Cu4 Cu4 ? 1_655 5.5199(12) ? Cu4 Cu4 ? 10_554 3.905(2) ? Cu4 Cu4 ? 10_555 3.905(2) ? Cu4 Cu4 ? 3_555 5.1487(7) ? Cu4 Cu4 ? 3_556 2.7817(12) ? Cu4 Cu4 ? 3_557 5.1487(7) ? Cu4 Cu4 ? 3_655 5.1254(6) ? Cu4 Cu4 ? 3_656 2.7382(12) ? Cu4 Cu4 ? 3_657 5.1254(6) ? Cu4 Cu4 ? 12_456 4.7815(18) ? Cu4 Cu4 ? 12_457 4.7815(18) ? Cu4 Cu4 ? 12_556 4.7815(18) ? Cu4 Cu4 ? 12_557 4.7815(18) ? Cu4 Cu5 ? ? 2.6427(13) ? Cu4 Cu5 ? 1_556 2.6427(13) ? Cu4 Cu5 ? 10_555 4.762(2) ? Cu4 Cu5 ? 3_555 3.8186(13) ? Cu4 Cu5 ? 3_556 3.8186(13) ? Cu4 Cu5 ? 3_655 3.8236(13) ? Cu4 Cu5 ? 3_656 3.8236(13) ? Cu4 Cu5 ? 12_456 5.517(2) ? Cu4 Cu5 ? 12_556 5.491(2) ? Cu4 Cu6 ? ? 4.771(2) ? Cu4 Cu6 ? 3_556 5.521(2) ? Cu4 Cu6 ? 3_656 5.504(2) ? Cu4 Cu9 ? ? 4.829(2) ? Cu4 Cu9 ? 1_556 4.829(2) ? Cu4 Cu10 ? 1_455 4.7348(8) ? Cu4 Cu10 ? 1_456 4.7348(8) ? Cu4 Cu10 ? ? 2.6577(8) ? Cu4 Cu10 ? 1_556 2.6577(8) ? Cu4 Cu10 ? 10_554 5.2133(13) ? Cu4 Cu10 ? 10_555 2.900(2) ? Cu4 Cu10 ? 10_556 5.2133(13) ? Cu4 Cu10 ? 10_655 4.8500(15) ? Cu5 Cu5 ? 1_455 5.5199(12) ? Cu5 Cu5 ? 1_554 4.3326(2) ? Cu5 Cu5 ? 1_556 4.3326(2) ? Cu5 Cu5 ? 1_655 5.5199(12) ? Cu5 Cu5 ? 3_554 5.1216(7) ? Cu5 Cu5 ? 3_555 2.7313(12) ? Cu5 Cu5 ? 3_556 5.1216(7) ? Cu5 Cu5 ? 3_654 5.1525(7) ? Cu5 Cu5 ? 3_655 2.7886(12) ? Cu5 Cu5 ? 3_656 5.1525(7) ? Cu5 Cu6 ? 1_554 3.9125(19) ? Cu5 Cu6 ? ? 3.9125(19) ? Cu5 Cu6 ? 3_555 4.7833(17) ? Cu5 Cu6 ? 3_556 4.7833(17) ? Cu5 Cu6 ? 3_655 4.7926(17) ? Cu5 Cu6 ? 3_656 4.7926(17) ? Cu5 Cu7 ? ? 4.788(2) ? Cu5 Cu7 ? 3_555 5.510(2) ? Cu5 Cu7 ? 3_655 5.543(2) ? Cu5 Cu9 ? 1_455 4.8654(15) ? Cu5 Cu9 ? 1_554 5.2314(12) ? Cu5 Cu9 ? ? 2.932(2) ? Cu5 Cu9 ? 1_556 5.2314(12) ? Cu5 Cu10 ? 1_455 4.6839(14) ? Cu5 Cu10 ? 1_554 5.0630(11) ? Cu5 Cu10 ? ? 2.620(2) ? Cu5 Cu10 ? 1_556 5.0630(11) ? Cu5 Cu10 ? 10_554 4.798(2) ? Cu5 Cu10 ? 10_555 4.798(2) ? Cu6 Cu6 ? 1_455 5.5199(12) ? Cu6 Cu6 ? 1_554 4.3326(2) ? Cu6 Cu6 ? 1_556 4.3326(2) ? Cu6 Cu6 ? 1_655 5.5199(12) ? Cu6 Cu6 ? 3_555 5.1437(7) ? Cu6 Cu6 ? 3_556 2.7725(12) ? Cu6 Cu6 ? 3_557 5.1437(7) ? Cu6 Cu6 ? 3_655 5.1303(7) ? Cu6 Cu6 ? 3_656 2.7474(12) ? Cu6 Cu6 ? 3_657 5.1303(7) ? Cu6 Cu7 ? ? 2.6525(13) ? Cu6 Cu7 ? 1_556 2.6525(13) ? Cu6 Cu7 ? 3_555 3.8190(13) ? Cu6 Cu7 ? 3_556 3.8190(13) ? Cu6 Cu7 ? 3_655 3.8367(13) ? Cu6 Cu7 ? 3_656 3.8367(13) ? Cu6 Cu8 ? ? 4.788(2) ? Cu6 Cu8 ? 3_556 5.561(2) ? Cu6 Cu8 ? 3_656 5.492(2) ? Cu6 Cu9 ? 1_455 4.7270(8) ? Cu6 Cu9 ? 1_456 4.7270(8) ? Cu6 Cu9 ? ? 2.6535(8) ? Cu6 Cu9 ? 1_556 2.6535(8) ? Cu7 Cu7 ? 1_455 5.5199(12) ? Cu7 Cu7 ? 1_554 4.3326(2) ? Cu7 Cu7 ? 1_556 4.3326(2) ? Cu7 Cu7 ? 1_655 5.5199(12) ? Cu7 Cu7 ? 3_554 5.1171(6) ? Cu7 Cu7 ? 3_555 2.7228(12) ? Cu7 Cu7 ? 3_556 5.1171(6) ? Cu7 Cu7 ? 3_654 5.1570(6) ? Cu7 Cu7 ? 3_655 2.7971(12) ? Cu7 Cu7 ? 3_656 5.1570(6) ? Cu7 Cu8 ? 1_554 3.913(2) ? Cu7 Cu8 ? ? 3.913(2) ? Cu7 Cu8 ? 2_554 5.547(2) ? Cu7 Cu8 ? 2_654 5.502(2) ? Cu7 Cu8 ? 3_555 4.8135(18) ? Cu7 Cu8 ? 3_556 4.8135(18) ? Cu7 Cu8 ? 3_655 4.7620(18) ? Cu7 Cu8 ? 3_656 4.7620(18) ? Cu7 Cu8 ? 4_556 4.786(2) ? Cu7 Cu9 ? 1_455 4.6762(13) ? Cu7 Cu9 ? 1_554 5.0605(11) ? Cu7 Cu9 ? ? 2.615(2) ? Cu7 Cu9 ? 1_556 5.0605(11) ? Cu8 Cu8 ? 1_455 5.5199(13) ? Cu8 Cu8 ? 1_554 4.3326(2) ? Cu8 Cu8 ? 1_556 4.3326(2) ? Cu8 Cu8 ? 1_655 5.5199(13) ? Cu8 Cu8 ? 2_554 3.9192(14) ? Cu8 Cu8 ? 2_555 3.9192(14) ? Cu8 Cu8 ? 2_654 3.7366(14) ? Cu8 Cu8 ? 2_655 3.7366(14) ? Cu8 Cu8 ? 3_555 5.2061(7) ? Cu8 Cu8 ? 3_556 2.8865(13) ? Cu8 Cu8 ? 3_557 5.2061(7) ? Cu8 Cu8 ? 3_655 5.0701(7) ? Cu8 Cu8 ? 3_656 2.6334(13) ? Cu8 Cu8 ? 3_657 5.0701(7) ? Cu8 Cu8 ? 4_556 2.6510(14) ? Cu8 Cu8 ? 4_557 2.6510(14) ? Cu9 Cu9 ? 1_455 5.5199(2) ? Cu9 Cu9 ? 1_554 4.3326(2) ? Cu9 Cu9 ? 1_556 4.3326(2) ? Cu9 Cu9 ? 1_655 5.5199(2) ? Cu9 Cu10 ? ? 4.797(3) ? Cu10 Cu10 ? 1_455 5.5199(2) ? Cu10 Cu10 ? 1_554 4.3326(2) ? Cu10 Cu10 ? 1_556 4.3326(2) ? Cu10 Cu10 ? 1_655 5.5199(2) ? Cu10 Cu10 ? 10_554 3.9618(13) ? Cu10 Cu10 ? 10_555 3.9618(13) ? Cu10 Cu10 ? 10_654 3.9618(13) ? Cu10 Cu10 ? 10_655 3.9618(13) ? data_473K-modulated _chemical_formula_sum 'Cu3.048 Sn0.952' _chemical_formula_weight 306.7 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Xmcm(0\b0)000 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,x3,x4 3 x1,x2,-x3,x4 4 -x1,-x2+2/3,-x3+1/2,-x4 5 -x1,x2,-x3,x4 6 x1,-x2+2/3,-x3+1/2,-x4 7 -x1,-x2+2/3,x3+1/2,-x4 8 x1,-x2+2/3,x3+1/2,-x4 9 x1+1/2,x2,x3,x4+1/2 10 -x1+1/2,x2,x3,x4+1/2 11 x1+1/2,x2,-x3,x4+1/2 12 -x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 13 -x1+1/2,x2,-x3,x4+1/2 14 x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 15 -x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 16 x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 _cell_length_a 5.528(2) _cell_length_b 4.783(4) _cell_length_c 4.3391(18) _cell_angle_alpha 90.00(6) _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00(6) _cell_volume 114.73(11) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.094900 0.000000 _cell_formula_units_Z 2 _cell_measurement_reflns_used 776 _cell_measurement_theta_min 5.33 _cell_measurement_theta_max 27.61 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 8.8753 _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 37.664 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.026 _exptl_crystal_colour 'metallic dark grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.148 _exptl_absorpt_correction_T_max 0.474 _diffrn_ambient_temperature 293 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 4102 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 28.35 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 591 _reflns_number_gt 276 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0834 _refine_ls_R_factor_all 0.0780 _refine_ls_wR_factor_ref 0.1027 _refine_ls_goodness_of_fit_ref 1.34 _refine_ls_goodness_of_fit_gt 1.63 _refine_ls_number_reflns 591 _refine_ls_number_parameters 24 _refine_ls_number_constraints 12 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0447 _refine_ls_shift/su_mean 0.0092 _refine_diff_density_max 2.84 _refine_diff_density_min -3.75 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 111(8) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.65651(15) 0 Uani 0.0097(2) 4 0.476(3) d ? ? ? Cu1 Cu 0 0.65651(15) 0 Uani 0.0097(2) 4 0.524(3) d ? ? ? Cu2 Cu -0.25 0.49256(19) 0.5 Uani 0.0127(3) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0093(4) 0.0104(4) 0.0093(4) 0 0 0 Cu1 Cu 0.0093(4) 0.0104(4) 0.0093(4) 0 0 0 Cu2 Cu 0.0150(6) 0.0120(5) 0.0110(6) 0 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 3 3 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w Sn1 -0.2686(7) 0.476(3) Cu1 0.2314(7) 0.524(3) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Sn1x1 Sn1 x 1 Sn1y1 Sn1 y 1 Sn1z1 Sn1 z 1 Sn1x2 Sn1 x 2 Sn1y2 Sn1 y 2 Sn1z2 Sn1 z 2 Sn1x3 Sn1 x 3 Sn1y3 Sn1 y 3 Sn1z3 Sn1 z 3 Cu1x1 Cu1 x 1 Cu1y1 Cu1 y 1 Cu1z1 Cu1 z 1 Cu1x2 Cu1 x 2 Cu1y2 Cu1 y 2 Cu1z2 Cu1 z 2 Cu1x3 Cu1 x 3 Cu1y3 Cu1 y 3 Cu1z3 Cu1 z 3 Cu2x1 Cu2 x 1 Cu2y1 Cu2 y 1 Cu2z1 Cu2 z 1 Cu2x2 Cu2 x 2 Cu2y2 Cu2 y 2 Cu2z2 Cu2 z 2 Cu2x3 Cu2 x 3 Cu2y3 Cu2 y 3 Cu2z3 Cu2 z 3 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Sn1x1 0 0 Sn1y1 -0.00502(19) -0.01858(19) Sn1z1 0 0 Sn1x2 0 0 Sn1y2 0.0027(4) -0.0017(4) Sn1z2 0 0 Sn1x3 0 0 Sn1y3 -0.0015(2) -0.0037(2) Sn1z3 0 0 Cu1x1 0 0 Cu1y1 -0.00502(19) -0.01858(19) Cu1z1 0 0 Cu1x2 0 0 Cu1y2 0.0027(4) -0.0017(4) Cu1z2 0 0 Cu1x3 0 0 Cu1y3 -0.0015(2) -0.0037(2) Cu1z3 0 0 Cu2x1 0.0033(2) 0.00299(19) Cu2y1 0 0 Cu2z1 0 0 Cu2x2 0 0 Cu2y2 -0.0002(5) -0.0013(6) Cu2z2 0 0 Cu2x3 0.0032(2) 0.0013(2) Cu2y3 0 0 Cu2z3 0 0 data_573K-modulated _chemical_formula_sum 'Cu3.027 Sn0.973' _chemical_formula_weight 307.9 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Xmcm(0\b0)000 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,x3,x4 3 x1,x2,-x3,x4 4 -x1,-x2+2/3,-x3+1/2,-x4 5 -x1,x2,-x3,x4 6 x1,-x2+2/3,-x3+1/2,-x4 7 -x1,-x2+2/3,x3+1/2,-x4 8 x1,-x2+2/3,x3+1/2,-x4 9 x1+1/2,x2,x3,x4+1/2 10 -x1+1/2,x2,x3,x4+1/2 11 x1+1/2,x2,-x3,x4+1/2 12 -x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 13 -x1+1/2,x2,-x3,x4+1/2 14 x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 15 -x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 16 x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 _cell_length_a 5.525(2) _cell_length_b 4.781(3) _cell_length_c 4.3385(17) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 114.60(9) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.101400 0.000000 _cell_formula_units_Z 2 _cell_measurement_reflns_used 1434 _cell_measurement_theta_min 4.22 _cell_measurement_theta_max 27.64 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 8.9186 _exptl_crystal_F_000 273 _exptl_absorpt_coefficient_mu 37.743 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.088 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.023 _exptl_crystal_colour 'metallic dark grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.51 _diffrn_ambient_temperature 293 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 9022 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 28.09 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_unetI/netI 0.0171 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_index_m_1_min -5 _diffrn_reflns_limit_index_m_1_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 919 _reflns_number_gt 406 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_gt 0.0954 _refine_ls_R_factor_all 0.0799 _refine_ls_wR_factor_ref 0.1118 _refine_ls_goodness_of_fit_ref 1.52 _refine_ls_goodness_of_fit_gt 1.99 _refine_ls_number_reflns 919 _refine_ls_number_parameters 32 _refine_ls_number_constraints 16 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0326 _refine_ls_shift/su_mean 0.0115 _refine_diff_density_max 3.07 _refine_diff_density_min -3.48 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 272(10) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.51022(12) 0 Uani 0.00911(19) 4 0.4867(18) d ? ? ? Cu1 Cu 0 0.51022(12) 0 Uani 0.00911(19) 4 0.5133(18) d ? ? ? Cu2 Cu -0.25 0.67393(14) 0.5 Uani 0.0116(3) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0086(3) 0.0089(3) 0.0098(3) 0 0 0 Cu1 Cu 0.0086(3) 0.0089(3) 0.0098(3) 0 0 0 Cu2 Cu 0.0137(5) 0.0105(5) 0.0107(5) 0 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 3 3 4 4 5 5 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w Sn1 -0.2320(5) 0.4867(18) Cu1 0.2680(5) 0.5133(18) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Sn1x1 Sn1 x 1 Sn1y1 Sn1 y 1 Sn1z1 Sn1 z 1 Sn1x2 Sn1 x 2 Sn1y2 Sn1 y 2 Sn1z2 Sn1 z 2 Sn1x3 Sn1 x 3 Sn1y3 Sn1 y 3 Sn1z3 Sn1 z 3 Sn1x4 Sn1 x 4 Sn1y4 Sn1 y 4 Sn1z4 Sn1 z 4 Sn1x5 Sn1 x 5 Sn1y5 Sn1 y 5 Sn1z5 Sn1 z 5 Cu1x1 Cu1 x 1 Cu1y1 Cu1 y 1 Cu1z1 Cu1 z 1 Cu1x2 Cu1 x 2 Cu1y2 Cu1 y 2 Cu1z2 Cu1 z 2 Cu1x3 Cu1 x 3 Cu1y3 Cu1 y 3 Cu1z3 Cu1 z 3 Cu1x4 Cu1 x 4 Cu1y4 Cu1 y 4 Cu1z4 Cu1 z 4 Cu1x5 Cu1 x 5 Cu1y5 Cu1 y 5 Cu1z5 Cu1 z 5 Cu2x1 Cu2 x 1 Cu2y1 Cu2 y 1 Cu2z1 Cu2 z 1 Cu2x2 Cu2 x 2 Cu2y2 Cu2 y 2 Cu2z2 Cu2 z 2 Cu2x3 Cu2 x 3 Cu2y3 Cu2 y 3 Cu2z3 Cu2 z 3 Cu2x4 Cu2 x 4 Cu2y4 Cu2 y 4 Cu2z4 Cu2 z 4 Cu2x5 Cu2 x 5 Cu2y5 Cu2 y 5 Cu2z5 Cu2 z 5 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Sn1x1 0 0 Sn1y1 -0.00466(15) 0.01834(14) Sn1z1 0 0 Sn1x2 0 0 Sn1y2 -0.0020(2) -0.0002(2) Sn1z2 0 0 Sn1x3 0 0 Sn1y3 -0.00177(14) 0.00375(14) Sn1z3 0 0 Sn1x4 0 0 Sn1y4 -0.0015(2) -0.0014(3) Sn1z4 0 0 Sn1x5 0 0 Sn1y5 0.00071(17) 0.00188(15) Sn1z5 0 0 Cu1x1 0 0 Cu1y1 -0.00466(15) 0.01834(14) Cu1z1 0 0 Cu1x2 0 0 Cu1y2 -0.0020(2) -0.0002(2) Cu1z2 0 0 Cu1x3 0 0 Cu1y3 -0.00177(14) 0.00375(14) Cu1z3 0 0 Cu1x4 0 0 Cu1y4 -0.0015(2) -0.0014(3) Cu1z4 0 0 Cu1x5 0 0 Cu1y5 0.00071(17) 0.00188(15) Cu1z5 0 0 Cu2x1 -0.00367(15) 0.00310(15) Cu2y1 0 0 Cu2z1 0 0 Cu2x2 0 0 Cu2y2 -0.0001(3) 0.0019(3) Cu2z2 0 0 Cu2x3 -0.00362(15) 0.00157(13) Cu2y3 0 0 Cu2z3 0 0 Cu2x4 0 0 Cu2y4 0.0001(3) 0.0000(4) Cu2z4 0 0 Cu2x5 -0.0021(2) 0.0016(3) Cu2y5 0 0 Cu2z5 0 0 data_673K-modulated _chemical_formula_sum 'Cu3.031 Sn0.969' _chemical_formula_weight 307.6 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Xmcm(0\b0)000 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,x3,x4 3 x1,x2,-x3,x4 4 -x1,-x2+2/3,-x3+1/2,-x4 5 -x1,x2,-x3,x4 6 x1,-x2+2/3,-x3+1/2,-x4 7 -x1,-x2+2/3,x3+1/2,-x4 8 x1,-x2+2/3,x3+1/2,-x4 9 x1+1/2,x2,x3,x4+1/2 10 -x1+1/2,x2,x3,x4+1/2 11 x1+1/2,x2,-x3,x4+1/2 12 -x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 13 -x1+1/2,x2,-x3,x4+1/2 14 x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 15 -x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 16 x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 _cell_length_a 5.529(2) _cell_length_b 4.787(3) _cell_length_c 4.3381(17) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 114.82(9) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.121550 0.000000 _cell_formula_units_Z 2 _cell_measurement_reflns_used 2185 _cell_measurement_theta_min 4.26 _cell_measurement_theta_max 28.16 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 8.8955 _exptl_crystal_F_000 273 _exptl_absorpt_coefficient_mu 37.662 _exptl_crystal_description block _exptl_crystal_size_max 0.144 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_min 0.021 _exptl_crystal_colour 'metallic intense silver' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.495 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 6406 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_unetI/netI 0.0117 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 598 _reflns_number_gt 384 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_gt 0.1193 _refine_ls_R_factor_all 0.0558 _refine_ls_wR_factor_ref 0.1354 _refine_ls_goodness_of_fit_ref 2.90 _refine_ls_goodness_of_fit_gt 3.23 _refine_ls_number_reflns 598 _refine_ls_number_parameters 24 _refine_ls_number_constraints 12 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0494 _refine_ls_shift/su_mean 0.0088 _refine_diff_density_max 4.38 _refine_diff_density_min -5.80 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 330(20) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Cu2 Cu 0.25 0.17367(16) 0.5 Uani 0.0122(4) 4 1 d ? ? ? Sn1 Sn 0 0.01046(13) 0 Uani 0.0094(3) 4 0.4843(17) d ? ? ? Cu1 Cu 0 0.01046(13) 0 Uani 0.0094(3) 4 0.5157(17) d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu2 Cu 0.0142(7) 0.0119(6) 0.0104(7) 0 0 0 Sn1 Sn 0.0089(5) 0.0098(5) 0.0095(5) 0 0 0 Cu1 Cu 0.0089(5) 0.0098(5) 0.0095(5) 0 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 3 3 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w Sn1 -0.2279(6) 0.4843(17) Cu1 0.2721(6) 0.5157(17) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Cu2x1 Cu2 x 1 Cu2y1 Cu2 y 1 Cu2z1 Cu2 z 1 Cu2x2 Cu2 x 2 Cu2y2 Cu2 y 2 Cu2z2 Cu2 z 2 Cu2x3 Cu2 x 3 Cu2y3 Cu2 y 3 Cu2z3 Cu2 z 3 Sn1x1 Sn1 x 1 Sn1y1 Sn1 y 1 Sn1z1 Sn1 z 1 Sn1x2 Sn1 x 2 Sn1y2 Sn1 y 2 Sn1z2 Sn1 z 2 Sn1x3 Sn1 x 3 Sn1y3 Sn1 y 3 Sn1z3 Sn1 z 3 Cu1x1 Cu1 x 1 Cu1y1 Cu1 y 1 Cu1z1 Cu1 z 1 Cu1x2 Cu1 x 2 Cu1y2 Cu1 y 2 Cu1z2 Cu1 z 2 Cu1x3 Cu1 x 3 Cu1y3 Cu1 y 3 Cu1z3 Cu1 z 3 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Cu2x1 0.00435(17) -0.00314(19) Cu2y1 0 0 Cu2z1 0 0 Cu2x2 0 0 Cu2y2 0.0002(4) 0.0006(5) Cu2z2 0 0 Cu2x3 0.00490(17) -0.00247(18) Cu2y3 0 0 Cu2z3 0 0 Sn1x1 0 0 Sn1y1 -0.00493(18) 0.01844(18) Sn1z1 0 0 Sn1x2 0 0 Sn1y2 -0.0019(3) -0.0005(3) Sn1z2 0 0 Sn1x3 0 0 Sn1y3 -0.00181(17) 0.00369(17) Sn1z3 0 0 Cu1x1 0 0 Cu1y1 -0.00493(18) 0.01844(18) Cu1z1 0 0 Cu1x2 0 0 Cu1y2 -0.0019(3) -0.0005(3) Cu1z2 0 0 Cu1x3 0 0 Cu1y3 -0.00181(17) 0.00369(17) Cu1z3 0 0 data_723K-modulated _chemical_formula_sum 'Cu3.022 Sn0.978' _chemical_formula_weight 308.1 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Xmcm(0\b0)000 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,x3,x4 3 x1,x2,-x3,x4 4 -x1,-x2+2/3,-x3+1/2,-x4 5 -x1,x2,-x3,x4 6 x1,-x2+2/3,-x3+1/2,-x4 7 -x1,-x2+2/3,x3+1/2,-x4 8 x1,-x2+2/3,x3+1/2,-x4 9 x1+1/2,x2,x3,x4+1/2 10 -x1+1/2,x2,x3,x4+1/2 11 x1+1/2,x2,-x3,x4+1/2 12 -x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 13 -x1+1/2,x2,-x3,x4+1/2 14 x1+1/2,-x2+2/3,-x3+1/2,-x4+1/2 15 -x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 16 x1+1/2,-x2+2/3,x3+1/2,-x4+1/2 _cell_length_a 5.523(3) _cell_length_b 4.783(3) _cell_length_c 4.336(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 114.54(11) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.124340 0.000000 _cell_formula_units_Z 2 _cell_measurement_reflns_used 1695 _cell_measurement_theta_min 4.27 _cell_measurement_theta_max 28.18 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 8.9313 _exptl_crystal_F_000 273 _exptl_absorpt_coefficient_mu 37.767 _exptl_crystal_description 'trigonal primatic' _exptl_crystal_size_max 0.123 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.039 _exptl_crystal_colour 'metallic grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.107 _exptl_absorpt_correction_T_max 0.368 _diffrn_ambient_temperature 293 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 4697 _diffrn_reflns_theta_min 3.2 _diffrn_reflns_theta_max 28.26 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_unetI/netI 0.0156 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 583 _reflns_number_gt 357 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_gt 0.1232 _refine_ls_R_factor_all 0.0742 _refine_ls_wR_factor_ref 0.1290 _refine_ls_goodness_of_fit_ref 2.34 _refine_ls_goodness_of_fit_gt 2.90 _refine_ls_number_reflns 583 _refine_ls_number_parameters 24 _refine_ls_number_constraints 12 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0438 _refine_ls_shift/su_mean 0.0128 _refine_diff_density_max 6.12 _refine_diff_density_min -6.61 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 830(30) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0 0.51013(15) 0 Uani 0.0125(3) 4 0.489(3) d ? ? ? Cu1 Cu 0 0.51013(15) 0 Uani 0.0125(3) 4 0.511(3) d ? ? ? Cu2 Cu 0.25 0.99298(18) 0 Uani 0.0145(4) 4 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 Sn 0.0108(5) 0.0140(5) 0.0128(5) 0 0 0 Cu1 Cu 0.0108(5) 0.0140(5) 0.0128(5) 0 0 0 Cu2 Cu 0.0148(7) 0.0155(7) 0.0130(7) 0 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 3 3 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w Sn1 -0.2278(6) 0.489(3) Cu1 0.2722(6) 0.511(3) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Sn1x1 Sn1 x 1 Sn1y1 Sn1 y 1 Sn1z1 Sn1 z 1 Sn1x2 Sn1 x 2 Sn1y2 Sn1 y 2 Sn1z2 Sn1 z 2 Sn1x3 Sn1 x 3 Sn1y3 Sn1 y 3 Sn1z3 Sn1 z 3 Cu1x1 Cu1 x 1 Cu1y1 Cu1 y 1 Cu1z1 Cu1 z 1 Cu1x2 Cu1 x 2 Cu1y2 Cu1 y 2 Cu1z2 Cu1 z 2 Cu1x3 Cu1 x 3 Cu1y3 Cu1 y 3 Cu1z3 Cu1 z 3 Cu2x1 Cu2 x 1 Cu2y1 Cu2 y 1 Cu2z1 Cu2 z 1 Cu2x2 Cu2 x 2 Cu2y2 Cu2 y 2 Cu2z2 Cu2 z 2 Cu2x3 Cu2 x 3 Cu2y3 Cu2 y 3 Cu2z3 Cu2 z 3 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Sn1x1 0 0 Sn1y1 -0.00506(19) 0.01774(19) Sn1z1 0 0 Sn1x2 0 0 Sn1y2 0.0001(3) -0.0002(3) Sn1z2 0 0 Sn1x3 0 0 Sn1y3 -0.00220(18) 0.00444(18) Sn1z3 0 0 Cu1x1 0 0 Cu1y1 -0.00506(19) 0.01774(19) Cu1z1 0 0 Cu1x2 0 0 Cu1y2 0.0001(3) -0.0002(3) Cu1z2 0 0 Cu1x3 0 0 Cu1y3 -0.00220(18) 0.00444(18) Cu1z3 0 0 Cu2x1 0.00439(17) 0.00306(19) Cu2y1 0 0 Cu2z1 0 0 Cu2x2 0 0 Cu2y2 -0.0004(3) 0.0011(3) Cu2z2 0 0 Cu2x3 0.00538(18) 0.00253(18) Cu2y3 0 0 Cu2z3 0 0 data_823K-modulated _chemical_formula_sum 'Cu3.013 Sn0.987' _chemical_formula_weight 308.6 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Xmcm(0\b0)000 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,x3,x4 3 x1,x2,-x3+1/2,x4 4 -x1,-x2,-x3,-x4 5 -x1,x2,-x3+1/2,x4 6 x1,-x2,-x3,-x4 7 -x1,-x2,x3+1/2,-x4 8 x1,-x2,x3+1/2,-x4 9 x1+1/2,x2,x3,x4+1/2 10 -x1+1/2,x2,x3,x4+1/2 11 x1+1/2,x2,-x3+1/2,x4+1/2 12 -x1+1/2,-x2,-x3,-x4+1/2 13 -x1+1/2,x2,-x3+1/2,x4+1/2 14 x1+1/2,-x2,-x3,-x4+1/2 15 -x1+1/2,-x2,x3+1/2,-x4+1/2 16 x1+1/2,-x2,x3+1/2,-x4+1/2 _cell_length_a 5.529(2) _cell_length_b 4.788(2) _cell_length_c 4.3411(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 114.92(8) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.100150 0.000000 _cell_formula_units_Z 2 _cell_measurement_reflns_used 1973 _cell_measurement_theta_min 4.26 _cell_measurement_theta_max 28.17 _cell_measurement_temperature 293 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 8.9161 _exptl_crystal_F_000 273 _exptl_absorpt_coefficient_mu 37.66 _exptl_crystal_description 'trigonal prismatic' _exptl_crystal_size_max 0.077 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.043 _exptl_crystal_colour 'metallic grey' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.283 _diffrn_ambient_temperature 293 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1367 _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_number 9463 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 28.32 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_unetI/netI 0.0139 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_index_m_1_min -5 _diffrn_reflns_limit_index_m_1_max 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray _reflns_number_total 932 _reflns_number_gt 463 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_gt 0.1237 _refine_ls_R_factor_all 0.0778 _refine_ls_wR_factor_ref 0.1327 _refine_ls_goodness_of_fit_ref 2.08 _refine_ls_goodness_of_fit_gt 2.80 _refine_ls_number_reflns 932 _refine_ls_number_parameters 32 _refine_ls_number_constraints 16 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0453 _refine_ls_shift/su_mean 0.0054 _refine_diff_density_max 4.46 _refine_diff_density_min -5.61 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 372(16) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.3201 1.2651 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sn -0.6537 1.4246 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Cu2 Cu 0.25 0.84016(15) 0.25 Uani 0.0130(3) 4 1 d ? ? ? Cu1 Cu 0 0.67710(12) 0.75 Uani 0.0112(2) 4 0.5065(19) d ? ? ? Sn1 Sn 0 0.67710(12) 0.75 Uani 0.0112(2) 4 0.4935(19) d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu2 Cu 0.0145(6) 0.0139(5) 0.0106(5) 0 0 0 Cu1 Cu 0.0105(4) 0.0128(4) 0.0103(4) 0 0 0 Sn1 Sn 0.0105(4) 0.0128(4) 0.0103(4) 0 0 0 loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 3 3 4 4 5 5 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w Cu1 0.2676(5) 0.5065(19) Sn1 -0.2324(5) 0.4935(19) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Cu2x1 Cu2 x 1 Cu2y1 Cu2 y 1 Cu2z1 Cu2 z 1 Cu2x2 Cu2 x 2 Cu2y2 Cu2 y 2 Cu2z2 Cu2 z 2 Cu2x3 Cu2 x 3 Cu2y3 Cu2 y 3 Cu2z3 Cu2 z 3 Cu2x4 Cu2 x 4 Cu2y4 Cu2 y 4 Cu2z4 Cu2 z 4 Cu2x5 Cu2 x 5 Cu2y5 Cu2 y 5 Cu2z5 Cu2 z 5 Cu1x1 Cu1 x 1 Cu1y1 Cu1 y 1 Cu1z1 Cu1 z 1 Cu1x2 Cu1 x 2 Cu1y2 Cu1 y 2 Cu1z2 Cu1 z 2 Cu1x3 Cu1 x 3 Cu1y3 Cu1 y 3 Cu1z3 Cu1 z 3 Cu1x4 Cu1 x 4 Cu1y4 Cu1 y 4 Cu1z4 Cu1 z 4 Cu1x5 Cu1 x 5 Cu1y5 Cu1 y 5 Cu1z5 Cu1 z 5 Sn1x1 Sn1 x 1 Sn1y1 Sn1 y 1 Sn1z1 Sn1 z 1 Sn1x2 Sn1 x 2 Sn1y2 Sn1 y 2 Sn1z2 Sn1 z 2 Sn1x3 Sn1 x 3 Sn1y3 Sn1 y 3 Sn1z3 Sn1 z 3 Sn1x4 Sn1 x 4 Sn1y4 Sn1 y 4 Sn1z4 Sn1 z 4 Sn1x5 Sn1 x 5 Sn1y5 Sn1 y 5 Sn1z5 Sn1 z 5 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Cu2x1 0.00339(15) -0.00306(16) Cu2y1 0 0 Cu2z1 0 0 Cu2x2 0 0 Cu2y2 0.0003(4) 0.0006(3) Cu2z2 0 0 Cu2x3 0.00452(15) -0.00201(15) Cu2y3 0 0 Cu2z3 0 0 Cu2x4 0 0 Cu2y4 0.0002(4) -0.0004(4) Cu2z4 0 0 Cu2x5 0.00405(16) -0.00043(18) Cu2y5 0 0 Cu2z5 0 0 Cu1x1 0 0 Cu1y1 -0.00422(16) 0.01833(16) Cu1z1 0 0 Cu1x2 0 0 Cu1y2 -0.0003(2) 0.0008(2) Cu1z2 0 0 Cu1x3 0 0 Cu1y3 -0.00210(15) 0.00504(15) Cu1z3 0 0 Cu1x4 0 0 Cu1y4 -0.0020(2) -0.0008(3) Cu1z4 0 0 Cu1x5 0 0 Cu1y5 -0.00350(14) 0.00002(15) Cu1z5 0 0 Sn1x1 0 0 Sn1y1 -0.00422(16) 0.01833(16) Sn1z1 0 0 Sn1x2 0 0 Sn1y2 -0.0003(2) 0.0008(2) Sn1z2 0 0 Sn1x3 0 0 Sn1y3 -0.00210(15) 0.00504(15) Sn1z3 0 0 Sn1x4 0 0 Sn1y4 -0.0020(2) -0.0008(3) Sn1z4 0 0 Sn1x5 0 0 Sn1y5 -0.00350(14) 0.00002(15) Sn1z5 0 0