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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 _publ_contact_author_name 'Bednarchuk, Tamara J.' _publ_contact_author_address ;Institute of Low Temperature and Structure Research, PO Box 1410, Wroclaw, 50-950, Poland ; _publ_contact_author_email t.bednarchuk@intibs.pl loop_ _publ_author_name _publ_author_address 'Bednarchuk, Tamara J.' ;Institute of Low Temperature and Structure Research, PO Box 1410, Wroclaw, 50-950, Poland ; 'Hornfeck, Wolfgang' ;Institute of Physics of the Czech Academy of Sciences, Na Slovance 2, CZ-182 21, Prague 8, Czech Republic ; 'Kinzhybalo, Vasyl' ;Institute of Low Temperature and Structure Research, PO Box 1410, Wroclaw, 50-950, Poland ; 'Zhou, Zhengyang' ;Institute of Physics of the Czech Academy of Sciences, Na Slovance 2, CZ-182 21, Prague 8, Czech Republic ; 'Dusek, Michal ' ;Institute of Low Temperature and Structure Research, PO Box 1410, Wroclaw, 50-950, Poland ; 'Pietraszko, Adam' ;Institute of Low Temperature and Structure Research, PO Box 1410, Wroclaw, 50-950, Poland ; _publ_section_title ;The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C~5~H~7~N~2~)[Fe^III^(H~2~O)~4~(SO~4~)~2~] ; _journal_date_recd_electronic 2019-03-12 _journal_date_accepted 2019-09-24 _journal_coeditor_code DQ5037SUP1 _journal_paper_category FA _journal_techeditor_code B191315 _iucr_compatibility_tag ACTA95 _journal_name_full 'Acta Crystallographica Section B' _journal_volume 75 _journal_year 2019 _journal_page_first 1144 _journal_page_last 1151 _journal_paper_doi https://doi.org/10.1107/S2052520619013155 data_PhaseII _exptl_crystal_type_of_structure mod _audit_creation_method 'Jana2006 Version : 31/08/2019' _chemical_formula_sum 'Fe S2 O12 N2 C5 H15' _chemical_formula_weight 415.1 _chemical_absolute_configuration ? _space_group_crystal_system monoclinic _space_group_ssg_name X2/c(\a0\g)0s loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,-x3+1/2,-x4+1/2 3 -x1,-x2,-x3,-x4 4 x1,-x2,x3+1/2,x4+1/2 5 x1+1/2,x2+1/2,x3,x4+1/2 6 -x1+1/2,x2+1/2,-x3+1/2,-x4 7 -x1+1/2,-x2+1/2,-x3,-x4+1/2 8 x1+1/2,-x2+1/2,x3+1/2,x4 _cell_length_a 12.1601(3) _cell_length_b 17.2511(3) _cell_length_c 6.7758(2) _cell_angle_alpha 90 _cell_angle_beta 100.715(2) _cell_angle_gamma 90 _cell_volume 1396.61(6) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.294300 0.000000 0.564000 _cell_formula_units_Z 4 _cell_measurement_reflns_used 6734 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 29.33 _cell_measurement_temperature 244.9(2) _exptl_crystal_density_diffrn 1.9744 _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.45 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.443 _exptl_crystal_size_min 0.295 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.12b (Rigaku Oxford Diffraction, 2015) 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 0.586 _exptl_absorpt_correction_T_max 0.751 _diffrn_ambient_temperature 244.9 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6249 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 23230 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 29.58 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_max 0.9 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_radiation_probe x-ray _reflns_number_total 5303 _reflns_number_gt 2856 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_gt 0.0790 _refine_ls_R_factor_all 0.0604 _refine_ls_wR_factor_ref 0.0887 _refine_ls_goodness_of_fit_ref 1.34 _refine_ls_goodness_of_fit_gt 1.68 _refine_ls_number_reflns 5303 _refine_ls_number_parameters 384 _refine_ls_number_constraints 41 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 3.8037 _refine_ls_shift/su_mean 0.1426 _refine_diff_density_max 1.24 _refine_diff_density_min -0.61 _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 5408.21 _refine_special_details ;WARNING: Unrealiable negative Uiso for atoms H1o5w1, H2o5w1, H1o5w2 and H2o5w2. ; loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' 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 Fe1 Fe 0.5 0.356897(15) 0.25 Uani 0.01310(9) 4 1 d ? ? ? S1 S 0.33286(3) 0.351013(19) -0.19593(5) Uani 0.01402(11) 8 1 d ? ? ? O2s O 0.22908(8) 0.34282(6) -0.11998(17) Uani 0.0264(4) 8 1 d ? ? ? O4s O 0.33393(13) 0.42245(6) -0.3114(2) Uani 0.0277(4) 8 1 d ? ? ? O3s O 0.35027(13) 0.28467(7) -0.3189(2) Uani 0.0258(7) 8 1 d ? ? ? O6w O 0.6044(2) 0.27668(14) 0.1791(4) Uani 0.0317(9) 8 1 d ? ? ? O5w1 O 0.5921(7) 0.4411(3) 0.1541(10) Uani 0.0516(12) 8 0.5 d ? ? ? O5w2 O 0.6067(6) 0.4360(3) 0.1756(8) Uani 0.0213(10) 8 0.5 d ? ? ? N1 N 0.5 0.08806(12) 0.25 Uani 0.0280(8) 4 1 d ? ? ? O1b1 O 0.4271(5) 0.3484(4) -0.0265(8) Uani 0.0204(8) 8 0.5 d ? ? ? O1b2 O 0.4281(5) 0.3630(5) -0.0241(8) Uani 0.045(2) 8 0.5 d ? ? ? N2 N 0.5 -0.14851(10) 0.25 Uani 0.0282(7) 4 1 d ? ? ? C1 C 0.5 0.01091(12) 0.25 Uani 0.0200(6) 4 1 d ? ? ? C2 C 0.39963(12) -0.03151(9) 0.2237(2) Uani 0.0267(5) 8 1 d ? ? ? C3 C 0.40199(13) -0.11030(9) 0.2261(2) Uani 0.0294(5) 8 1 d ? ? ? H1c2 H 0.329214 -0.00477 0.204043 Uiso 0.032 8 1 d ? ? ? H1c3 H 0.333185 -0.138886 0.21059 Uiso 0.0352 8 1 d ? ? ? H1n1 H 0.544(5) 0.108(3) 0.293(7) Uiso 0.033620(2) 8 0.5 d ? ? ? H2n1 H 0.559(5) 0.113(3) 0.242(7) Uiso 0.033620(2) 8 0.5 d ? ? ? H1n2 H 0.5 -0.198938 0.25 Uiso 0.0338 4 1 d ? ? ? H1o6w H 0.6228(18) 0.2806(12) 0.069(4) Uiso 0.016(9) 8 1 d ? ? ? H2o6w H 0.642(3) 0.2512(15) 0.243(5) Uiso 0.000(8) 8 1 d ? ? ? H1o5w1 H 0.605(3) 0.436(2) 0.094(6) Uiso -0.030(6) 8 0.5 d ? ? ? H2o5w1 H 0.629(3) 0.508(3) 0.239(6) Uiso -0.010(8) 8 0.5 d ? ? ? H1o5w2 H 0.631(2) 0.437(2) 0.123(7) Uiso -0.012(7) 8 0.5 d ? ? ? H2o5w2 H 0.630(3) 0.515(3) 0.239(5) Uiso -0.001(8) 8 0.5 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 Fe1 Fe 0.01362(15) 0.01408(15) 0.01110(16) 0 0.00098(12) 0 S1 S 0.01275(17) 0.01712(18) 0.01179(19) 0.00005(12) 0.00129(14) 0.00043(12) O2s O 0.0172(5) 0.0314(6) 0.0327(7) -0.0009(4) 0.0106(5) 0.0004(5) O4s O 0.0431(7) 0.0153(5) 0.0270(7) -0.0005(5) 0.0128(6) 0.0016(5) O3s O 0.0422(12) 0.0150(9) 0.0232(15) 0.0015(8) 0.0137(10) -0.0003(10) O6w O 0.0359(15) 0.0348(15) 0.0279(15) 0.0201(10) 0.0147(12) 0.0082(9) O5w1 O 0.094(2) 0.0295(19) 0.0460(15) -0.0328(19) 0.0502(16) -0.0181(14) O5w2 O 0.0245(19) 0.0222(14) 0.0176(18) -0.0090(12) 0.0046(13) -0.0011(11) N1 N 0.0214(12) 0.0180(10) 0.0435(15) 0 0.0032(11) 0 O1b1 O 0.0235(9) 0.019(2) 0.0152(9) 0.0029(16) -0.0046(7) -0.0039(15) O1b2 O 0.019(2) 0.101(6) 0.0140(15) 0.001(3) -0.0031(12) 0.005(2) N2 N 0.0348(11) 0.0140(9) 0.0336(12) 0 0.0009(10) 0 C1 C 0.0206(10) 0.0192(10) 0.0204(11) 0 0.0040(9) 0 C2 C 0.0171(7) 0.0241(8) 0.0379(10) 0.0008(6) 0.0026(7) -0.0008(7) C3 C 0.0232(8) 0.0260(8) 0.0378(10) -0.0061(7) 0.0027(7) -0.0011(7) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w O3s 0.2381 1 O6w 0.5946 1 O5w1 0.3268 0.5 O5w2 0.8439 0.5 O1b1 0.1754(5) 0.5 O1b2 0.6771(8) 0.5 H1o6w 0.5412 1 H2o6w 0.6447 1 H1o5w1 0.2722 0.5 H2o5w1 0.3709 0.5 H1o5w2 0.7835 0.5 H2o5w2 0.9003 0.5 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 Fe1x1 Fe1 x 1 Fe1y1 Fe1 y 1 Fe1z1 Fe1 z 1 S1x1 S1 x 1 S1y1 S1 y 1 S1z1 S1 z 1 O2sx1 O2s x 1 O2sy1 O2s y 1 O2sz1 O2s z 1 O4sx1 O4s x 1 O4sy1 O4s y 1 O4sz1 O4s z 1 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N2x1 N2 x 1 N2y1 N2 y 1 N2z1 N2 z 1 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 H1c2x1 H1c2 x 1 H1c2y1 H1c2 y 1 H1c2z1 H1c2 z 1 H1c3x1 H1c3 x 1 H1c3y1 H1c3 y 1 H1c3z1 H1c3 z 1 H1n1x1 H1n1 x 1 H1n1y1 H1n1 y 1 H1n1z1 H1n1 z 1 H2n1x1 H2n1 x 1 H2n1y1 H2n1 y 1 H2n1z1 H2n1 z 1 H1n2x1 H1n2 x 1 H1n2y1 H1n2 y 1 H1n2z1 H1n2 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Fe1x1 0.00246(3) 0 Fe1y1 0 0.001805(19) Fe1z1 0.00233(5) 0 S1x1 -0.00085(3) -0.00136(3) S1y1 -0.00173(3) -0.00459(3) S1z1 -0.00082(7) -0.00365(7) O2sx1 -0.00140(9) -0.00303(9) O2sy1 -0.00020(7) -0.00069(7) O2sz1 -0.00237(19) -0.00742(20) O4sx1 0.00566(16) 0.00926(16) O4sy1 -0.00216(8) -0.00013(9) O4sz1 0.0066(3) 0.0159(3) N1x1 -0.00344(17) 0 N1y1 0 0.00094(12) N1z1 -0.0011(3) 0 N2x1 -0.00002(18) 0 N2y1 0 0.00101(12) N2z1 -0.0042(3) 0 C1x1 -0.0023(2) 0 C1y1 0 0.00088(15) C1z1 -0.0022(4) 0 C2x1 -0.00180(15) 0.00037(15) C2y1 -0.00050(11) 0.00109(11) C2z1 -0.0030(3) -0.0010(3) C3x1 -0.00056(16) 0.00006(16) C3y1 -0.00046(11) 0.00117(11) C3z1 -0.0039(3) -0.0003(3) H1c2x1 -0.0021 0.0009 H1c2y1 -0.0007 0.0014 H1c2z1 -0.0034 -0.0018 H1c3x1 -0.0001 0 H1c3y1 -0.0007 0.0015 H1c3z1 -0.0045 -0.0001 H1n1x1 -0.00344(17) 0 H1n1y1 0 0.00094(12) H1n1z1 -0.0011(3) 0 H2n1x1 -0.00344(17) 0 H2n1y1 0 0.00094(12) H2n1z1 -0.0011(3) 0 H1n2x1 0.0007 0 H1n2y1 0 0.001 H1n2z1 -0.005 0 loop_ _jana_atom_site_displace_Legendre_atom_site_label _jana_atom_site_displace_Legendre_axis _jana_atom_site_displace_Legendre_param_order _jana_atom_site_displace_Legendre_param_coeff O5w1 x 1 -0.0078(16) O5w1 y 1 -0.0014(9) O5w1 z 1 -0.013(2) O5w1 x 2 0.001(6) O5w1 y 2 -0.004(2) O5w1 z 2 -0.006(8) O5w2 x 1 0.0278(14) O5w2 y 1 -0.0081(9) O5w2 z 1 0.039(2) O5w2 x 2 -0.0211(12) O5w2 y 2 0.0066(10) O5w2 z 2 -0.0257(19) H1o5w1 x 1 -0.041(6) H1o5w1 y 1 0.009(4) H1o5w1 z 1 -0.063(15) H1o5w1 x 2 -0.030(7) H1o5w1 y 2 0.002(6) H1o5w1 z 2 0.149(13) H2o5w1 x 1 0.029(7) H2o5w1 y 1 0.060(6) H2o5w1 z 1 0.050(12) H2o5w1 x 2 0.047(10) H2o5w1 y 2 0.043(7) H2o5w1 z 2 0.081(17) H1o5w2 x 1 0.011(5) H1o5w2 y 1 0.006(4) H1o5w2 z 1 -0.022(16) H1o5w2 x 2 0.024(7) H1o5w2 y 2 0.018(6) H1o5w2 z 2 0.202(15) H2o5w2 x 1 0.036(7) H2o5w2 y 1 0.068(6) H2o5w2 z 1 0.080(12) H2o5w2 x 2 0.023(10) H2o5w2 y 2 0.051(8) H2o5w2 z 2 0.033(18) loop_ _jana_atom_site_displace_XHarm_site_label _jana_atom_site_displace_XHarm_axis _jana_atom_site_displace_XHarm_param_order _jana_atom_site_displace_XHarm_param_coeff O3s x 1 0.0067(8) O3s y 1 0.0003(6) O3s z 1 0.0159(12) O3s x 2 -0.01056(14) O3s y 2 -0.00082(7) O3s z 2 -0.0215(3) O3s x 3 0.0011(11) O3s y 3 0.0035(8) O3s z 3 -0.0059(16) O3s x 4 -0.0047(15) O3s y 4 -0.0001(12) O3s z 4 -0.003(3) O6w x 1 -0.0090(7) O6w y 1 -0.0037(6) O6w z 1 -0.0145(15) O6w x 2 0.0086(2) O6w y 2 0.00234(13) O6w z 2 0.0173(3) O6w x 3 0.0021(10) O6w y 3 -0.0016(7) O6w z 3 0.000(2) O6w x 4 0.0038(18) O6w y 4 0.0036(13) O6w z 4 0.008(3) O1b1 x 1 -0.0017(5) O1b1 y 1 -0.0282(5) O1b1 z 1 -0.0002(10) O1b1 x 2 0.0001(5) O1b1 y 2 -0.0077(4) O1b1 z 2 -0.0006(9) O1b2 x 1 -0.0005(6) O1b2 y 1 0.0075(6) O1b2 z 1 0.0039(11) O1b2 x 2 0.006(2) O1b2 y 2 -0.007(2) O1b2 z 2 -0.006(4) H1o6w x 1 0.000(6) H1o6w y 1 0.001(5) H1o6w z 1 -0.004(13) H1o6w x 2 0.011(2) H1o6w y 2 0.0013(15) H1o6w z 2 0.015(4) H1o6w x 3 -0.006(7) H1o6w y 3 -0.003(5) H1o6w z 3 -0.010(13) H1o6w x 4 -0.002(4) H1o6w y 4 -0.002(3) H1o6w z 4 0.067(6) H2o6w x 1 -0.008(3) H2o6w y 1 -0.003(2) H2o6w z 1 -0.019(5) H2o6w x 2 0.0045(16) H2o6w y 2 0.0018(11) H2o6w z 2 0.013(3) H2o6w x 3 0.004(4) H2o6w y 3 -0.004(3) H2o6w z 3 0.008(7) H2o6w x 4 0.030(5) H2o6w y 4 -0.016(3) H2o6w z 4 0.058(9) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Fe1U111 Fe1 U11 1 Fe1U221 Fe1 U22 1 Fe1U331 Fe1 U33 1 Fe1U121 Fe1 U12 1 Fe1U131 Fe1 U13 1 Fe1U231 Fe1 U23 1 S1U111 S1 U11 1 S1U221 S1 U22 1 S1U331 S1 U33 1 S1U121 S1 U12 1 S1U131 S1 U13 1 S1U231 S1 U23 1 O4sU111 O4s U11 1 O4sU221 O4s U22 1 O4sU331 O4s U33 1 O4sU121 O4s U12 1 O4sU131 O4s U13 1 O4sU231 O4s U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 N2U111 N2 U11 1 N2U221 N2 U22 1 N2U331 N2 U33 1 N2U121 N2 U12 1 N2U131 N2 U13 1 N2U231 N2 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Fe1U111 0 -0.00016(17) Fe1U221 0 -0.00027(19) Fe1U331 0 -0.00015(20) Fe1U121 -0.00025(15) 0 Fe1U131 0 0.00014(16) Fe1U231 -0.00047(15) 0 S1U111 0.0005(2) 0.0006(2) S1U221 0.0002(2) 0.0009(2) S1U331 0.0002(2) -0.0005(2) S1U121 0.00023(18) 0.00010(19) S1U131 0.00006(19) -0.00021(20) S1U231 0.00002(18) -0.00051(18) O4sU111 0.0141(9) 0.0063(10) O4sU221 -0.0027(7) 0.0002(7) O4sU331 0.0061(9) 0.0045(9) O4sU121 -0.0018(7) -0.0038(7) O4sU131 0.0088(7) 0.0047(8) O4sU231 -0.0005(6) -0.0020(7) N1U111 0 0.0004(12) N1U221 0 -0.0003(12) N1U331 0 -0.0021(15) N1U121 0.0008(11) 0 N1U131 0 0.0006(11) N1U231 -0.0011(11) 0 N2U111 0 0.0002(14) N2U221 0 0.0001(12) N2U331 0 -0.0014(15) N2U121 -0.0002(11) 0 N2U131 0 -0.0011(12) N2U231 -0.0004(10) 0 C1U111 0 0.0007(14) C1U221 0 -0.0016(14) C1U331 0 0.0015(15) C1U121 -0.0006(12) 0 C1U131 0 0.0011(12) C1U231 0.0003(12) 0 C2U111 0.0008(10) 0.0006(10) C2U221 0.0003(11) -0.0012(11) C2U331 0.0000(13) -0.0031(13) C2U121 -0.0003(9) 0.0004(9) C2U131 0.0013(9) -0.0014(10) C2U231 0.0003(10) -0.0004(9) C3U111 0.0009(11) 0.0008(10) C3U221 -0.0005(12) -0.0005(12) C3U331 -0.0002(13) -0.0023(14) C3U121 0.0000(9) 0.0001(9) C3U131 0.0008(10) -0.0003(10) C3U231 0.0006(10) 0.0010(10) loop_ _jana_atom_site_U_XHarm_atom_site_label _jana_atom_site_U_XHarm_tens_elem _jana_atom_site_U_XHarm_param_order _jana_atom_site_U_XHarm_param_coeff O3s U11 1 -0.0106(17) O3s U22 1 0.0005(18) O3s U33 1 -0.0068(15) O3s U12 1 -0.0003(13) O3s U13 1 -0.0070(12) O3s U23 1 0.0002(12) O3s U11 2 -0.007(3) O3s U22 2 0.0020(11) O3s U33 2 -0.001(4) O3s U12 2 -0.0058(18) O3s U13 2 -0.006(2) O3s U23 2 -0.004(2) O6w U11 1 -0.0099(14) O6w U22 1 -0.013(2) O6w U33 1 -0.0069(16) O6w U12 1 -0.0091(12) O6w U13 1 -0.0085(12) O6w U23 1 -0.0068(13) O6w U11 2 0.002(4) O6w U22 2 0.001(2) O6w U33 2 -0.005(4) O6w U12 2 0.001(3) O6w U13 2 -0.003(3) O6w U23 2 -0.003(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Fe1 O6w ? ? 2.00(2) 1.94(3) 2.04(3) ? Fe1 O6w ? 2_6555 2.00(2) 1.93(3) 2.04(3) ? Fe1 O5w1 ? ? 2.01(4) 1.98(6) 2.02(6) ? Fe1 O5w1 ? 2_6555 2.01(4) 1.98(6) 2.02(6) ? Fe1 O5w2 ? ? 2.033(17) 1.997(18) 2.074(18) ? Fe1 O5w2 ? 2_6555 2.032(17) 1.996(18) 2.070(18) ? Fe1 O1b1 ? ? 1.946(8) 1.914(8) 2.001(8) ? Fe1 O1b1 ? 2_6555 1.947(8) 1.914(8) 1.998(8) ? Fe1 O1b2 ? ? 1.917(18) 1.90(3) 1.93(3) ? Fe1 O1b2 ? 2_6555 1.917(18) 1.90(3) 1.93(3) ? Fe1 H1o5w1 ? ? 2.33(10) 1.73(10) 2.68(10) ? Fe1 H1o5w1 ? 2_6555 2.32(10) 1.76(10) 2.68(10) ? S1 O2s ? ? 1.4568(18) 1.4550(18) 1.4594(18) ? S1 O4s ? ? 1.468(2) 1.459(2) 1.481(2) ? S1 O3s ? ? 1.46(2) 1.45(3) 1.48(3) ? S1 O1b1 ? ? 1.506(8) 1.476(8) 1.582(8) ? S1 O1b2 ? ? 1.486(18) 1.48(3) 1.51(3) ? S1 H2o5w1 ? 3_6655 2.50(12) 1.36(13) 3.05(13) ? S1 H2o5w2 ? 3_6655 2.49(13) 1.07(15) 3.18(15) ? O4s H2o5w1 ? 3_6655 1.46(11) 0.11(13) 2.10(13) ? O4s H2o5w2 ? 3_6655 1.34(13) 0.11(15) 1.97(15) ? O6w H1o6w ? ? 0.84(13) 0.43(16) 1.25(16) ? O6w H2o6w ? ? 0.72(8) 0.13(10) 1.41(10) ? O5w1 H1o5w1 ? ? 0.73(11) 0.37(12) 1.07(12) ? O5w1 H2o5w1 ? ? 1.35(12) 0.59(13) 3.56(13) ? O5w2 H1o5w1 ? ? 0.59(10) 0.53(10) 0.65(10) ? O5w2 H1o5w2 ? ? 0.83(11) 0.46(12) 1.20(12) ? O5w2 H2o5w2 ? ? 1.40(13) 0.66(15) 3.36(15) ? N1 C1 ? ? 1.331(3) 1.330(4) 1.332(4) ? N1 H1n1 ? ? 0.66(6) 0.65(6) 0.66(6) ? N1 H1n1 ? 2_6555 0.66(6) 0.65(6) 0.66(6) ? N1 H2n1 ? ? 0.85(6) 0.85(6) 0.85(6) ? N1 H2n1 ? 2_6555 0.85(6) 0.85(6) 0.85(6) ? N2 C3 ? ? 1.345(3) 1.344(3) 1.346(3) ? N2 C3 ? 2_6555 1.345(3) 1.344(3) 1.346(3) ? N2 H1n2 ? ? 0.9(17) 0.9(17) 0.9(17) ? C1 C2 ? ? 1.406(3) 1.404(3) 1.408(3) ? C1 C2 ? 2_6555 1.406(3) 1.404(3) 1.408(3) ? C2 C3 ? ? 1.360(3) 1.358(3) 1.361(3) ? C2 H1c2 ? ? 1.0(13) 1.0(13) 1.0(13) ? C3 H1c3 ? ? 1.0(14) 1.0(14) 1.0(14) ? H1n1 H2n1 ? ? 0.43(8) 0.43(8) 0.44(8) ? H1o5w1 H2o5w1 ? ? 1.68(15) 0.89(16) 3.41(16) ? H1o5w2 H2o5w2 ? ? 1.52(16) 0.93(18) 2.20(18) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O6w Fe1 O6w ? ? 2_6555 91.9(10) 88.6(9) 94.4(9) ? O6w Fe1 O5w1 ? ? ? 88.9(9) 85.9(8) 91.1(9) ? O6w Fe1 O5w1 ? ? 2_6555 175.9(8) 171.5(7) 178.9(9) ? O6w Fe1 O5w2 ? ? ? 88.9(9) 87.4(8) 96.0(8) ? O6w Fe1 O5w2 ? ? 2_6555 176.2(8) 168.0(7) 178.3(8) ? O6w Fe1 O1b1 ? ? ? 86.8(7) 81.4(6) 100.2(6) ? O6w Fe1 O1b1 ? ? 2_6555 90.9(7) 83.2(6) 101.5(6) ? O6w Fe1 O1b2 ? ? ? 88.4(7) 82.3(6) 97.0(6) ? O6w Fe1 O1b2 ? ? 2_6555 92.1(7) 88.3(6) 98.1(6) ? O6w Fe1 H1o5w1 ? ? ? 83(2) 76(2) 108(3) ? O6w Fe1 H1o5w1 ? ? 2_6555 164(2) 156(2) 172(2) ? O6w Fe1 O5w1 2_6555 ? ? 175.9(8) 171.6(7) 178.9(9) ? O6w Fe1 O5w1 2_6555 ? 2_6555 88.8(9) 85.9(8) 91.1(9) ? O6w Fe1 O5w2 2_6555 ? ? 176.1(8) 167.6(7) 178.4(9) ? O6w Fe1 O5w2 2_6555 ? 2_6555 88.9(9) 87.4(9) 95.7(8) ? O6w Fe1 O1b1 2_6555 ? ? 90.9(7) 83.4(6) 101.6(6) ? O6w Fe1 O1b1 2_6555 ? 2_6555 86.8(7) 81.4(6) 100.0(6) ? O6w Fe1 O1b2 2_6555 ? ? 92.1(7) 88.3(7) 98.1(6) ? O6w Fe1 O1b2 2_6555 ? 2_6555 88.4(7) 82.3(6) 97.0(6) ? O6w Fe1 H1o5w1 2_6555 ? ? 164(2) 156(2) 172(2) ? O6w Fe1 H1o5w1 2_6555 ? 2_6555 83(2) 76(2) 105(3) ? O5w1 Fe1 O5w1 ? ? 2_6555 88.6(10) 88.1(8) 89.7(14) ? O5w1 Fe1 O5w2 ? ? 2_6555 93.5(16) 91.7(12) 94.5(15) ? O5w1 Fe1 O1b1 ? ? ? 86.1(10) 73.0(13) 91.4(13) ? O5w1 Fe1 O1b1 ? ? 2_6555 95.3(8) 85.6(9) 104.1(13) ? O5w1 Fe1 O1b2 ? ? 2_6555 92.9(13) 86.5(10) 101.0(13) ? O5w1 Fe1 H1o5w1 ? ? ? 16(2) 10(2) 21(3) ? O5w1 Fe1 O5w2 2_6555 ? ? 93.6(16) 91.8(12) 94.5(15) ? O5w1 Fe1 O1b1 2_6555 ? ? 95.3(8) 85.4(9) 104.0(13) ? O5w1 Fe1 O1b1 2_6555 ? 2_6555 86.1(10) 73.1(13) 91.4(13) ? O5w1 Fe1 O1b2 2_6555 ? ? 93.1(13) 86.6(10) 101.2(13) ? O5w1 Fe1 H1o5w1 2_6555 ? 2_6555 16(2) 10(2) 21(2) ? O5w2 Fe1 O5w2 ? ? 2_6555 88.3(7) 84.6(7) 90.4(7) ? O5w2 Fe1 O1b1 ? ? 2_6555 97.2(5) 96.4(5) 99.1(5) ? O5w2 Fe1 O1b2 ? ? ? 85.0(5) 71.7(5) 89.6(5) ? O5w2 Fe1 O1b2 ? ? 2_6555 95.4(5) 85.6(5) 107.0(5) ? O5w2 Fe1 H1o5w1 ? ? 2_6555 92(2) 75(3) 102.2(19) ? O5w2 Fe1 O1b1 2_6555 ? ? 97.2(5) 96.5(5) 98.9(5) ? O5w2 Fe1 O1b2 2_6555 ? ? 95.1(5) 85.6(5) 106.8(5) ? O5w2 Fe1 O1b2 2_6555 ? 2_6555 85.1(5) 72.0(5) 89.6(5) ? O5w2 Fe1 H1o5w1 2_6555 ? ? 92(2) 73(3) 102.4(19) ? O1b1 Fe1 O1b1 ? ? 2_6555 177.0(4) 175.2(4) 178.1(4) ? O1b1 Fe1 O1b2 ? ? 2_6555 172.0(5) 164.7(5) 175.7(4) ? O1b1 Fe1 H1o5w1 ? ? ? 78(2) 72.3(19) 95(3) ? O1b1 Fe1 O1b2 2_6555 ? ? 171.8(5) 164.3(5) 175.7(4) ? O1b1 Fe1 H1o5w1 2_6555 ? 2_6555 78(2) 72.3(19) 93(3) ? O1b2 Fe1 O1b2 ? ? 2_6555 175.9(9) 174.6(11) 177.7(11) ? O1b2 Fe1 H1o5w1 ? ? 2_6555 103(2) 99(3) 104(2) ? O1b2 Fe1 H1o5w1 2_6555 ? ? 103(3) 98(3) 104(2) ? O2s S1 O4s ? ? ? 111.36(12) 111.02(12) 111.62(12) ? O2s S1 O3s ? ? ? 110.5(9) 107.3(9) 112.6(9) ? O2s S1 O1b1 ? ? ? 109.6(4) 107.1(4) 110.6(3) ? O2s S1 O1b2 ? ? ? 108.9(4) 105.2(4) 111.6(4) ? O2s S1 H2o5w1 ? ? 3_6655 110(3) 101(4) 113(2) ? O2s S1 H2o5w2 ? ? 3_6655 108(2) 104.9(18) 114(4) ? O4s S1 O3s ? ? ? 110.1(9) 102.6(8) 117.5(8) ? O4s S1 O1b1 ? ? ? 108.0(4) 95.7(4) 117.8(4) ? O4s S1 O1b2 ? ? ? 105.7(5) 95.8(5) 111.3(5) ? O4s S1 H2o5w1 ? ? 3_6655 29(2) 3(4) 39.2(16) ? O4s S1 H2o5w2 ? ? 3_6655 22(2) 3(4) 39(6) ? O3s S1 O1b1 ? ? ? 107.5(9) 100.9(8) 124.9(11) ? O3s S1 O1b2 ? ? ? 109.1(9) 100.4(9) 123.0(11) ? O3s S1 H2o5w1 ? ? 3_6655 127(3) 86(5) 141(2) ? O3s S1 H2o5w2 ? ? 3_6655 125(3) 70(6) 135(2) ? O1b1 S1 H2o5w2 ? ? 3_6655 97(2) 92.0(16) 131(5) ? O1b2 S1 H2o5w1 ? ? 3_6655 85(2) 69.4(19) 132(4) ? H2o5w1 S1 H2o5w2 3_6655 ? 3_6655 58(6) 48(6) 67(6) ? S1 O4s H2o5w1 ? ? 3_6655 115(7) 67(7) 140(30) ? S1 O4s H2o5w2 ? ? 3_6655 118(7) 30(30) 135(3) ? H2o5w1 O4s H2o5w2 3_6655 ? 3_6655 173(7) 173(6) 174(7) ? Fe1 O6w H1o6w ? ? ? 117(13) 108(17) 130(20) ? Fe1 O6w H2o6w ? ? ? 130(12) 125(5) 140(40) ? H1o6w O6w H2o6w ? ? ? 107(17) 80(11) 120(11) ? Fe1 O5w1 H1o5w1 ? ? ? 106(8) 59(7) 118(6) ? Fe1 O5w1 H2o5w1 ? ? ? 129(7) 124(6) 133(5) ? H1o5w1 O5w1 H2o5w1 ? ? ? 105(12) 63(11) 114(12) ? Fe1 O5w2 H1o5w1 ? ? ? 69(8) 68(7) 70(9) ? Fe1 O5w2 H1o5w2 ? ? ? 118(7) 81(4) 178(13) ? Fe1 O5w2 H2o5w2 ? ? ? 129(5) 124(6) 134(8) ? H1o5w2 O5w2 H2o5w2 ? ? ? 88(9) 37(9) 113(10) ? C1 N1 H1n1 ? ? ? 122(5) 122(5) 123(5) ? C1 N1 H1n1 ? ? 2_6555 122(5) 122(5) 123(5) ? C1 N1 H2n1 ? ? ? 121(4) 120(4) 121(4) ? C1 N1 H2n1 ? ? 2_6555 121(4) 120(4) 121(4) ? H1n1 N1 H1n1 ? ? 2_6555 116(7) 115(7) 117(7) ? H1n1 N1 H2n1 ? ? ? 30(6) 30(5) 30(6) ? H1n1 N1 H2n1 ? ? 2_6555 109(6) 108(6) 110(6) ? H1n1 N1 H2n1 2_6555 ? ? 109(6) 108(6) 110(6) ? H1n1 N1 H2n1 2_6555 ? 2_6555 30(6) 30(5) 30(6) ? H2n1 N1 H2n1 ? ? 2_6555 119(5) 118(5) 119(5) ? Fe1 O1b1 S1 ? ? ? 148.2(6) 134.8(6) 155.9(6) ? Fe1 O1b2 S1 ? ? ? 153.5(15) 150(2) 158(2) ? C3 N2 C3 ? ? 2_6555 121.3(2) 121.3(2) 121.3(2) ? C3 N2 H1n2 ? ? ? 119.34 119.33 119.35 ? C3 N2 H1n2 2_6555 ? ? 119.34 119.33 119.35 ? N1 C1 C2 ? ? ? 121.37(17) 121.32(14) 121.42(14) ? N1 C1 C2 ? ? 2_6555 121.37(17) 121.32(14) 121.42(14) ? C2 C1 C2 ? ? 2_6555 117.3(2) 117.2(3) 117.3(3) ? C1 C2 C3 ? ? ? 120.2(2) 120.1(2) 120.3(2) ? C1 C2 H1c2 ? ? ? 119.9 119.85 119.94 ? C3 C2 H1c2 ? ? ? 119.9 119.85 119.94 ? N2 C3 C2 ? ? ? 120.5(2) 120.5(2) 120.5(2) ? N2 C3 H1c3 ? ? ? 119.75 119.73 119.77 ? C2 C3 H1c3 ? ? ? 119.75 119.73 119.77 ? N1 H1n1 H2n1 ? ? ? 101(10) 100(10) 101(10) ? N1 H2n1 H1n1 ? ? ? 49(9) 49(9) 50(9) ? Fe1 H1o5w1 O5w1 ? ? ? 58(8) 42(4) 101(11) ? Fe1 H1o5w1 O5w2 ? ? ? 93(10) 92(9) 94(11) ? Fe1 H1o5w1 H2o5w1 ? ? ? 96(6) 68(6) 148(9) ? O5w1 H1o5w1 H2o5w1 ? ? ? 47(9) 25(5) 84(13) ? S1 H2o5w1 O4s 3_6655 ? 3_6655 36(7) 24(2) 90(17) ? S1 H2o5w1 O5w1 3_6655 ? ? 144(8) 91(5) 159(10) ? S1 H2o5w1 H1o5w1 3_6655 ? ? 126(7) 98(5) 168(9) ? O4s H2o5w1 O5w1 3_6655 ? ? 151(14) 16(6) 179(14) ? O4s H2o5w1 H1o5w1 3_6655 ? ? 136(12) 14(8) 170(11) ? O5w1 H2o5w1 H1o5w1 ? ? ? 28(6) 8(2) 43(8) ? O5w2 H1o5w2 H2o5w2 ? ? ? 59(8) 27(5) 132(11) ? S1 H2o5w2 O4s 3_6655 ? 3_6655 41(8) 19.0(15) 150(60) ? S1 H2o5w2 O5w2 3_6655 ? ? 151(8) 101(7) 162(10) ? S1 H2o5w2 H1o5w2 3_6655 ? ? 131(8) 119(7) 156(9) ? O4s H2o5w2 O5w2 3_6655 ? ? 150(14) 10(7) 180(11) ? O4s H2o5w2 H1o5w2 3_6655 ? ? 142(13) 30(50) 159(16) ? O5w2 H2o5w2 H1o5w2 ? ? ? 33(5) 10(2) 53(8) ? data_PhaseIII _exptl_crystal_type_of_structure mod _audit_creation_method 'Jana2006 Version : 31/08/2019' _chemical_formula_sum 'C5 N2 O12 S2 Fe H15' _chemical_formula_weight 415.1 _chemical_absolute_configuration ? _space_group_crystal_system monoclinic _space_group_ssg_name X2/c(\a0\g)0s loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,-x3+1/2,-x4+1/2 3 -x1,-x2,-x3,-x4 4 x1,-x2,x3+1/2,x4+1/2 5 x1+1/2,x2+1/2,x3,x4+1/2 6 -x1+1/2,x2+1/2,-x3+1/2,-x4 7 -x1+1/2,-x2+1/2,-x3,-x4+1/2 8 x1+1/2,-x2+1/2,x3+1/2,x4 _cell_length_a 12.175(11) _cell_length_b 17.217(5) _cell_length_c 6.769(2) _cell_angle_alpha 90 _cell_angle_beta 100.87(4) _cell_angle_gamma 90 _cell_volume 1393.4(14) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.336600 0.000000 0.554400 _cell_formula_units_Z 4 _cell_measurement_reflns_used 7559 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 29.33 _cell_measurement_temperature 194.9(2) _exptl_crystal_density_diffrn 1.9789 _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.45 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.443 _exptl_crystal_size_min 0.295 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details Jana2006 _exptl_absorpt_correction_T_min 0.5826 _exptl_absorpt_correction_T_max 0.7523 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -14 12 0 0.1505 14 -12 0 0.1505 5 -3 8 0.13 -6 1 -8 0.1544 14 12 1 0.1649 -14 -14 0 0.1701 -2 -7 -9 0.1806 6 11 -8 0.2606 2 22 -4 0.3042 -14 14 2 0.1885 14 14 -3 0.2249 3 2 9 0.1495 6 3 8 0.1471 -10 7 -6 0.1757 1 12 -8 0.238 1 -14 8 0.2119 -6 -21 4 0.256 13 -16 1 0.1665 14 -14 -2 0.1803 3 -24 -1 0.2605 7 22 0 0.2603 -4 23 3 0.2737 _diffrn_ambient_temperature 194.9 _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6249 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 23241 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 29.61 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_max 0.9 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_unetI/netI 0.0166 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_radiation_probe x-ray _reflns_number_total 5282 _reflns_number_gt 3721 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_gt 0.0700 _refine_ls_R_factor_all 0.0475 _refine_ls_wR_factor_ref 0.0747 _refine_ls_goodness_of_fit_ref 2.01 _refine_ls_goodness_of_fit_gt 2.28 _refine_ls_number_reflns 5282 _refine_ls_number_parameters 343 _refine_ls_number_restraints 7 _refine_ls_number_constraints 105 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 0.0471 _refine_ls_shift/su_mean 0.0036 _refine_diff_density_max 0.76 _refine_diff_density_min -0.45 _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 5320(160) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param N1 ? H1n1 ? 0.87 0.001 N1 ? H2n1 ? 0.87 0.001 loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_id O6w ? H1o6w ? 1 O6w ? H2o6w ? 1 O5w1 ? H1o5w1 ? 1 O5w1 ? H2o5w1 ? 1 O5w2 ? H1o5w2 ? 1 O5w2 ? H2o5w2 ? 1 loop_ _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param 1 0.001 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 Fe1 Fe 1 0.643241(12) 0.25 Uani 0.01092(8) 4 1 d ? ? ? S1 S 0.83288(2) 0.649134(15) -0.19644(4) Uani 0.01169(9) 8 1 d ? ? ? O1b1 O 0.92703(17) 0.66428(13) -0.0272(3) Uani 0.0292(5) 8 0.5 d ? ? ? O1b2 O 0.92889(17) 0.62694(10) -0.0238(3) Uani 0.0236(4) 8 0.5 d ? ? ? O2s O 0.72909(7) 0.65734(5) -0.11977(13) Uani 0.0213(3) 8 1 d ? ? ? O3s O 0.85049(7) 0.71561(5) -0.31897(12) Uani 0.0227(3) 8 1 d ? ? ? O5w1 O 1.08154(17) 0.55665(9) 0.1413(2) Uani 0.0317(5) 8 0.5 d ? ? ? O5w2 O 1.11916(17) 0.56749(8) 0.1928(2) Uani 0.0214(4) 8 0.5 d ? ? ? O6w O 1.10435(9) 0.72361(6) 0.17929(15) Uani 0.0239(3) 8 1 d ? ? ? O4s O 0.83380(9) 0.57748(5) -0.31196(16) Uani 0.0209(6) 8 1 d ? ? ? N1 N 0.5 0.41157(8) 0.25 Uani 0.0222(5) 4 1 d ? ? ? N2 N 0.5 0.64870(8) 0.25 Uani 0.0229(5) 4 1 d ? ? ? C1 C 0.5 0.48873(9) 0.25 Uani 0.0170(5) 4 1 d ? ? ? C2 C 0.39927(10) 0.53146(7) 0.22442(19) Uani 0.0222(4) 8 1 d ? ? ? C3 C 0.40184(10) 0.61031(7) 0.22710(19) Uani 0.0245(4) 8 1 d ? ? ? H1c2 H 0.328874 0.504717 0.205097 Uiso 0.0266 8 1 d ? ? ? H1c3 H 0.333164 0.638985 0.212572 Uiso 0.0294 8 1 d ? ? ? H1n1 H 0.5581(16) 0.3871(16) 0.224(4) Uiso 0.0267(4) 8 0.5 d ? ? ? H2n1 H 0.4409(15) 0.3878(16) 0.186(4) Uiso 0.0267(4) 8 0.5 d ? ? ? H1n2 H 0.5 0.699228 0.25 Uiso 0.0275 4 1 d ? ? ? H1o6w H 1.1217(12) 0.7187(8) 0.0715(13) Uiso 0.0287(13) 8 1 d ? ? ? H1o5w1 H 1.1032(17) 0.5621(11) 0.0374(18) Uiso 0.038033(2) 8 0.5 d ? ? ? H2o5w1 H 1.1076(15) 0.5181(7) 0.198(3) Uiso 0.038033(2) 8 0.5 d ? ? ? H2o6w H 1.1446(10) 0.7517(7) 0.2552(16) Uiso 0.0287(16) 8 1 d ? ? ? H1o5w2 H 1.1302(16) 0.5700(10) 0.0799(14) Uiso 0.0256(14) 8 0.5 d ? ? ? H2o5w2 H 1.1252(15) 0.5231(5) 0.228(3) Uiso 0.0256(3) 8 0.5 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 Fe1 Fe 0.01136(12) 0.01141(13) 0.00961(14) 0 0.00097(9) 0 S1 S 0.01085(14) 0.01380(15) 0.01008(16) -0.00005(10) 0.00111(11) -0.00030(10) O1b1 O 0.0172(7) 0.0541(9) 0.0137(7) -0.0033(8) -0.0038(5) 0.0035(8) O1b2 O 0.0168(6) 0.0384(8) 0.0130(7) 0.0050(7) -0.0036(5) -0.0052(7) O2s O 0.0145(4) 0.0261(5) 0.0250(5) 0.0003(3) 0.0079(4) -0.0006(4) O3s O 0.0343(5) 0.0140(4) 0.0222(5) -0.0001(4) 0.0118(4) 0.0018(3) O5w1 O 0.0564(11) 0.0190(7) 0.0272(8) 0.0183(7) 0.0270(8) 0.0088(6) O5w2 O 0.0288(8) 0.0179(7) 0.0201(7) 0.0101(6) 0.0113(6) 0.0058(5) O6w O 0.0289(5) 0.0275(5) 0.0174(5) -0.0162(4) 0.0099(4) -0.0063(4) O4s O 0.0318(11) 0.0132(7) 0.0190(12) 0.0003(7) 0.0080(8) -0.0010(7) N1 N 0.0172(7) 0.0149(7) 0.0334(9) 0 0.0018(7) 0 N2 N 0.0279(8) 0.0120(7) 0.0272(9) 0 0.0009(7) 0 C1 C 0.0172(8) 0.0168(8) 0.0167(8) 0 0.0028(7) 0 C2 C 0.0144(5) 0.0201(6) 0.0311(7) -0.0006(5) 0.0023(5) -0.0001(5) C3 C 0.0201(6) 0.0218(6) 0.0304(7) 0.0049(5) 0.0020(6) 0.0007(5) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w O1b1 0.32177(18) 0.5 O1b2 0.8243(3) 0.5 O5w1 0.4672(3) 0.5 O5w2 1.0084(3) 0.5 O6w 0.7459(3) 1 O4s 0.3825(4) 1 H1o6w 0.6920(9) 1 H1o5w1 0.4169(12) 0.5 H2o5w1 0.5074(16) 0.5 H2o6w 0.8015(10) 1 H1o5w2 0.9495(10) 0.5 H2o5w2 1.0302(16) 0.5 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 Fe1x1 Fe1 x 1 Fe1y1 Fe1 y 1 Fe1z1 Fe1 z 1 S1x1 S1 x 1 S1y1 S1 y 1 S1z1 S1 z 1 O2sx1 O2s x 1 O2sy1 O2s y 1 O2sz1 O2s z 1 O3sx1 O3s x 1 O3sy1 O3s y 1 O3sz1 O3s z 1 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N2x1 N2 x 1 N2y1 N2 y 1 N2z1 N2 z 1 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 H1c2x1 H1c2 x 1 H1c2y1 H1c2 y 1 H1c2z1 H1c2 z 1 H1c3x1 H1c3 x 1 H1c3y1 H1c3 y 1 H1c3z1 H1c3 z 1 H1n1x1 H1n1 x 1 H1n1y1 H1n1 y 1 H1n1z1 H1n1 z 1 H2n1x1 H2n1 x 1 H2n1y1 H2n1 y 1 H2n1z1 H2n1 z 1 H1n2x1 H1n2 x 1 H1n2y1 H1n2 y 1 H1n2z1 H1n2 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Fe1x1 0.00248(2) 0 Fe1y1 0 -0.002004(15) Fe1z1 0.00281(4) 0 S1x1 -0.00076(3) -0.00172(3) S1y1 0.00225(2) 0.00586(2) S1z1 -0.00096(5) -0.00406(5) O2sx1 -0.00146(7) -0.00343(7) O2sy1 0.00023(6) 0.00114(6) O2sz1 -0.00256(15) -0.00777(15) O3sx1 -0.00867(9) -0.01257(9) O3sy1 0.00285(6) 0.00110(6) O3sz1 -0.01343(16) -0.02490(16) N1x1 0.00255(6) 0 N1y1 0 0.00147(6) N1z1 -0.00058(19) 0 N2x1 -0.00045(14) 0 N2y1 0 0.00098(10) N2z1 0.0050(3) 0 C1x1 0.00245(16) 0 C1y1 0 0.00110(11) C1z1 0.0021(3) 0 C2x1 0.00154(12) -0.00026(12) C2y1 -0.00066(9) 0.00119(8) C2z1 0.0034(2) 0.0013(2) C3x1 0.00017(13) 0.00005(12) C3y1 -0.00065(9) 0.00117(9) C3z1 0.0044(2) 0.0005(2) H1c2x1 0.0019 -0.0008 H1c2y1 -0.001 0.0016 H1c2z1 0.0042 0.0024 H1c3x1 -0.0003 0.0003 H1c3y1 -0.001 0.0015 H1c3z1 0.005 0.0003 H1n1x1 0.00255(6) 0 H1n1y1 0 0.00147(6) H1n1z1 -0.00058(19) 0 H2n1x1 0.00255(6) 0 H2n1y1 0 0.00147(6) H2n1z1 -0.00058(19) 0 H1n2x1 -0.0014 0 H1n2y1 0 0.001 H1n2z1 0.0063 0 loop_ _jana_atom_site_displace_Legendre_atom_site_label _jana_atom_site_displace_Legendre_axis _jana_atom_site_displace_Legendre_param_order _jana_atom_site_displace_Legendre_param_coeff O5w1 x 1 0.0040(2) O5w1 y 1 0.00354(13) O5w1 z 1 0.0018(3) O5w1 x 2 0.0008(10) O5w1 y 2 -0.0029(5) O5w1 z 2 0.0077(11) O5w2 x 1 0.00108(19) O5w2 y 1 -0.00224(11) O5w2 z 1 0.0009(3) O5w2 x 2 0.0054(12) O5w2 y 2 0.0028(3) O5w2 z 2 0.0056(10) H1o5w1 x 1 0.0040(2) H1o5w1 y 1 0.00354(13) H1o5w1 z 1 0.0018(3) H1o5w1 x 2 0.0008(10) H1o5w1 y 2 -0.0029(5) H1o5w1 z 2 0.0077(11) H2o5w1 x 1 0.0040(2) H2o5w1 y 1 0.00354(13) H2o5w1 z 1 0.0018(3) H2o5w1 x 2 0.0008(10) H2o5w1 y 2 -0.0029(5) H2o5w1 z 2 0.0077(11) H1o5w2 x 1 0.00108(19) H1o5w2 y 1 -0.00224(11) H1o5w2 z 1 0.0009(3) H1o5w2 x 2 0.0054(12) H1o5w2 y 2 0.0028(3) H1o5w2 z 2 0.0056(10) H2o5w2 x 1 0.00108(19) H2o5w2 y 1 -0.00224(11) H2o5w2 z 1 0.0009(3) H2o5w2 x 2 0.0054(12) H2o5w2 y 2 0.0028(3) H2o5w2 z 2 0.0056(10) loop_ _jana_atom_site_displace_XHarm_site_label _jana_atom_site_displace_XHarm_axis _jana_atom_site_displace_XHarm_param_order _jana_atom_site_displace_XHarm_param_coeff O1b1 x 1 0.00097(19) O1b1 y 1 0.00152(14) O1b1 z 1 -0.0022(4) O1b1 x 2 -0.0024(8) O1b1 y 2 -0.0005(5) O1b1 z 2 -0.0011(14) O1b2 x 1 -0.00114(18) O1b2 y 1 -0.00498(12) O1b2 z 1 0.0001(3) O1b2 x 2 -0.0013(7) O1b2 y 2 -0.0012(4) O1b2 z 2 0.0016(13) O6w x 1 -0.01402(16) O6w y 1 0.00602(12) O6w z 1 -0.02735(14) O6w x 2 0.00064(8) O6w y 2 0.00204(6) O6w z 2 0.00154(8) O6w x 3 -0.0041(2) O6w y 3 0.0015(2) O6w z 3 -0.0060(2) O6w x 4 0.0005(4) O6w y 4 0.0000(3) O6w z 4 0.0014(4) O4s x 1 -0.0115(8) O4s y 1 -0.0005(7) O4s z 1 -0.0191(15) O4s x 2 0.00143(11) O4s y 2 -0.00195(6) O4s z 2 0.00569(18) O4s x 3 -0.0058(11) O4s y 3 -0.0025(9) O4s z 3 -0.008(2) O4s x 4 -0.0028(13) O4s y 4 0.0003(11) O4s z 4 -0.005(2) H1o6w x 1 -0.01402(16) H1o6w y 1 0.00602(12) H1o6w z 1 -0.02735(14) H1o6w x 2 0.00064(8) H1o6w y 2 0.00204(6) H1o6w z 2 0.00154(8) H1o6w x 3 -0.0041(2) H1o6w y 3 0.0015(2) H1o6w z 3 -0.0060(2) H1o6w x 4 0.0005(4) H1o6w y 4 0.0000(3) H1o6w z 4 0.0014(4) H2o6w x 1 -0.01402(16) H2o6w y 1 0.00602(12) H2o6w z 1 -0.02735(14) H2o6w x 2 0.00064(8) H2o6w y 2 0.00204(6) H2o6w z 2 0.00154(8) H2o6w x 3 -0.0041(2) H2o6w y 3 0.0015(2) H2o6w z 3 -0.0060(2) H2o6w x 4 0.0005(4) H2o6w y 4 0.0000(3) H2o6w z 4 0.0014(4) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Fe1U111 Fe1 U11 1 Fe1U221 Fe1 U22 1 Fe1U331 Fe1 U33 1 Fe1U121 Fe1 U12 1 Fe1U131 Fe1 U13 1 Fe1U231 Fe1 U23 1 S1U111 S1 U11 1 S1U221 S1 U22 1 S1U331 S1 U33 1 S1U121 S1 U12 1 S1U131 S1 U13 1 S1U231 S1 U23 1 O2sU111 O2s U11 1 O2sU221 O2s U22 1 O2sU331 O2s U33 1 O2sU121 O2s U12 1 O2sU131 O2s U13 1 O2sU231 O2s U23 1 O3sU111 O3s U11 1 O3sU221 O3s U22 1 O3sU331 O3s U33 1 O3sU121 O3s U12 1 O3sU131 O3s U13 1 O3sU231 O3s U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 N2U111 N2 U11 1 N2U221 N2 U22 1 N2U331 N2 U33 1 N2U121 N2 U12 1 N2U131 N2 U13 1 N2U231 N2 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Fe1U111 0 -0.00005(14) Fe1U221 0 -0.00021(15) Fe1U331 0 -0.00007(16) Fe1U121 0.00031(11) 0 Fe1U131 0 0.00027(13) Fe1U231 0.00046(11) 0 S1U111 0.00044(17) 0.00066(17) S1U221 0.00072(19) 0.00120(19) S1U331 0.00018(19) -0.0005(2) S1U121 -0.00052(14) 0.00004(14) S1U131 0.00050(16) 0.00004(16) S1U231 -0.00005(14) 0.00060(14) O2sU111 0.0001(5) 0.0005(5) O2sU221 0.0009(6) 0.0013(6) O2sU331 0.0013(7) 0.0014(7) O2sU121 0.0000(5) -0.0018(5) O2sU131 0.0001(5) 0.0001(5) O2sU231 0.0008(5) -0.0014(5) O3sU111 0.0024(7) -0.0036(7) O3sU221 0.0009(6) 0.0019(6) O3sU331 -0.0033(7) -0.0088(7) O3sU121 0.0002(5) 0.0038(5) O3sU131 -0.0009(6) -0.0066(6) O3sU231 -0.0005(5) 0.0017(5) N1U111 0 -0.0012(9) N1U221 0 0.0012(9) N1U331 0 0.0020(11) N1U121 -0.0001(8) 0 N1U131 0 0.0006(8) N1U231 0.0002(8) 0 N2U111 0 -0.0006(10) N2U221 0 0.0007(9) N2U331 0 0.0028(12) N2U121 0.0005(8) 0 N2U131 0 0.0020(10) N2U231 0.0002(8) 0 C1U111 0 -0.0001(10) C1U221 0 0.0005(11) C1U331 0 0.0003(12) C1U121 -0.0011(9) 0 C1U131 0 -0.0013(9) C1U231 0.0002(9) 0 C2U111 0.0003(7) -0.0012(7) C2U221 0.0002(8) 0.0006(8) C2U331 -0.0009(10) 0.0024(10) C2U121 0.0002(7) 0.0007(7) C2U131 -0.0009(7) 0.0006(7) C2U231 0.0008(7) 0.0007(7) C3U111 -0.0001(8) -0.0001(8) C3U221 0.0002(9) -0.0007(9) C3U331 -0.0003(10) 0.0042(10) C3U121 0.0003(7) -0.0006(7) C3U131 0.0002(7) 0.0013(8) C3U231 0.0007(7) 0.0006(7) loop_ _jana_atom_site_U_XHarm_atom_site_label _jana_atom_site_U_XHarm_tens_elem _jana_atom_site_U_XHarm_param_order _jana_atom_site_U_XHarm_param_coeff O6w U11 1 0.0007(8) O6w U22 1 -0.0079(8) O6w U33 1 0.0027(6) O6w U12 1 0.0044(6) O6w U13 1 0.0014(5) O6w U23 1 0.0007(6) O6w U11 2 0.0090(11) O6w U22 2 0.0044(9) O6w U33 2 0.0120(9) O6w U12 2 -0.0060(9) O6w U13 2 0.0102(9) O6w U23 2 -0.0071(9) O4s U11 1 -0.011(2) O4s U22 1 -0.0004(17) O4s U33 1 -0.0035(19) O4s U12 1 -0.0045(16) O4s U13 1 -0.0054(14) O4s U23 1 -0.0020(14) O4s U11 2 -0.001(3) O4s U22 2 0.0010(11) O4s U33 2 0.004(3) O4s U12 2 -0.0013(17) O4s U13 2 0.002(2) O4s U23 2 -0.0025(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Fe1 O1b1 ? ? 1.937(6) 1.926(9) 1.950(9) ? Fe1 O1b1 ? 2_7555 1.937(6) 1.926(9) 1.950(9) ? Fe1 O1b2 ? ? 1.929(6) 1.904(9) 1.937(9) ? Fe1 O1b2 ? 2_7555 1.929(6) 1.904(9) 1.937(9) ? Fe1 O5w1 ? ? 2.012(7) 2.002(10) 2.028(10) ? Fe1 O5w1 ? 2_7555 2.012(7) 2.002(10) 2.028(10) ? Fe1 O5w2 ? ? 2.032(7) 2.023(11) 2.058(11) ? Fe1 O5w2 ? 2_7555 2.031(7) 2.023(11) 2.058(11) ? Fe1 O6w ? ? 2.007(6) 1.979(8) 2.036(8) ? Fe1 O6w ? 2_7555 2.007(6) 1.978(8) 2.036(8) ? S1 O1b1 ? ? 1.493(6) 1.476(9) 1.514(9) ? S1 O1b2 ? ? 1.503(6) 1.483(8) 1.551(8) ? S1 O2s ? ? 1.462(3) 1.460(3) 1.465(3) ? S1 O3s ? ? 1.4612(14) 1.4518(14) 1.4746(14) ? S1 O4s ? ? 1.47(2) 1.47(3) 1.48(3) ? O5w1 H1o5w1 ? ? 0.801(18) 0.80(2) 0.80(2) ? O5w1 H2o5w1 ? ? 0.801(16) 0.801(18) 0.801(18) ? O5w2 H1o5w2 ? ? 0.801(14) 0.801(16) 0.801(16) ? O5w2 H2o5w2 ? ? 0.801(11) 0.801(12) 0.801(12) ? O6w H1o6w ? ? 0.801(12) 0.801(12) 0.801(12) ? O6w H2o6w ? ? 0.801(13) 0.801(13) 0.801(13) ? N1 C1 ? ? 1.328(3) 1.322(3) 1.335(3) ? N1 H1n1 ? ? 0.87(2) 0.87(2) 0.87(2) ? N1 H1n1 ? 2_6555 0.87(2) 0.87(2) 0.87(2) ? N1 H2n1 ? ? 0.87(2) 0.86(2) 0.88(2) ? N1 H2n1 ? 2_6555 0.87(2) 0.86(2) 0.88(2) ? N2 C3 ? ? 1.349(3) 1.348(3) 1.350(3) ? N2 C3 ? 2_6555 1.349(3) 1.348(3) 1.350(3) ? N2 H1n2 ? ? 0.9(17) 0.9(17) 0.9(17) ? C1 C2 ? ? 1.413(3) 1.410(4) 1.416(4) ? C1 C2 ? 2_6555 1.413(3) 1.410(4) 1.416(4) ? C2 C3 ? ? 1.358(3) 1.358(3) 1.358(3) ? C2 H1c2 ? ? 1.0(13) 1.0(13) 1.0(13) ? C3 H1c3 ? ? 1.0(14) 1.0(14) 1.0(14) ? H1n1 H2n1 ? 2_6555 0.61(4) 0.60(4) 0.61(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O1b1 Fe1 O1b2 ? ? 2_7555 177.5(2) 174.9(3) 178.6(3) ? O1b1 Fe1 O5w1 ? ? ? 87.5(2) 87.09(18) 88.6(3) ? O1b1 Fe1 O5w2 ? ? 2_7555 96.0(2) 93.7(3) 96.6(2) ? O1b1 Fe1 O6w ? ? ? 85.1(2) 80.2(3) 86.82(14) ? O1b1 Fe1 O6w ? ? 2_7555 89.0(2) 85.1(3) 90.35(13) ? O1b1 Fe1 O1b2 2_7555 ? ? 177.5(2) 174.9(3) 178.6(3) ? O1b1 Fe1 O5w1 2_7555 ? 2_7555 87.5(2) 87.09(18) 88.6(3) ? O1b1 Fe1 O5w2 2_7555 ? ? 96.0(2) 93.7(3) 96.6(2) ? O1b1 Fe1 O6w 2_7555 ? ? 89.0(2) 85.1(3) 90.35(13) ? O1b1 Fe1 O6w 2_7555 ? 2_7555 85.1(2) 80.2(3) 86.82(14) ? O1b2 Fe1 O5w1 ? ? 2_7555 94.01(19) 92.6(2) 95.3(2) ? O1b2 Fe1 O5w2 ? ? ? 85.87(19) 85.01(15) 88.1(2) ? O1b2 Fe1 O6w ? ? ? 89.6(2) 88.7(3) 91.4(2) ? O1b2 Fe1 O6w ? ? 2_7555 93.0(2) 91.7(2) 96.3(2) ? O1b2 Fe1 O5w1 2_7555 ? ? 94.00(19) 92.6(2) 95.3(2) ? O1b2 Fe1 O5w2 2_7555 ? 2_7555 85.85(19) 85.01(15) 88.1(2) ? O1b2 Fe1 O6w 2_7555 ? ? 92.9(2) 91.7(2) 96.3(2) ? O1b2 Fe1 O6w 2_7555 ? 2_7555 89.5(2) 88.7(3) 91.4(2) ? O5w1 Fe1 O5w2 ? ? 2_7555 90.9(2) 89.83(13) 92.49(13) ? O5w1 Fe1 O6w ? ? ? 90.4(3) 89.1(3) 93.18(18) ? O5w1 Fe1 O6w ? ? 2_7555 175.6(2) 171.29(15) 177.4(2) ? O5w1 Fe1 O5w2 2_7555 ? ? 90.9(2) 89.83(13) 92.48(13) ? O5w1 Fe1 O6w 2_7555 ? ? 175.5(2) 171.30(15) 177.4(2) ? O5w1 Fe1 O6w 2_7555 ? 2_7555 90.4(3) 89.1(3) 93.19(18) ? O5w2 Fe1 O6w ? ? ? 86.8(2) 82.13(18) 88.7(3) ? O5w2 Fe1 O6w ? ? 2_7555 177.10(19) 173.04(16) 178.60(18) ? O5w2 Fe1 O6w 2_7555 ? ? 177.09(19) 173.01(16) 178.60(18) ? O5w2 Fe1 O6w 2_7555 ? 2_7555 86.9(2) 82.11(18) 88.7(3) ? O6w Fe1 O6w ? ? 2_7555 91.8(2) 91.6(2) 92.4(3) ? O1b1 S1 O2s ? ? ? 109.0(3) 108.0(3) 109.4(4) ? O1b1 S1 O3s ? ? ? 105.0(3) 96.9(3) 109.76(19) ? O1b1 S1 O4s ? ? ? 110.2(9) 104.9(8) 119.1(9) ? O1b2 S1 O2s ? ? ? 109.4(3) 108.47(18) 110.6(3) ? O1b2 S1 O3s ? ? ? 110.1(2) 107.13(15) 117.6(3) ? O1b2 S1 O4s ? ? ? 104.8(9) 100.8(9) 106.3(9) ? O2s S1 O3s ? ? ? 110.62(8) 110.08(8) 111.03(8) ? O2s S1 O4s ? ? ? 111.3(9) 109.7(9) 112.0(9) ? O3s S1 O4s ? ? ? 110.4(10) 106.2(10) 112.2(10) ? Fe1 O1b1 S1 ? ? ? 150.3(4) 145.7(6) 152.5(3) ? Fe1 O1b2 S1 ? ? ? 148.9(4) 143.7(5) 150.8(2) ? Fe1 O5w1 H1o5w1 ? ? ? 120.0(15) 117.9(14) 120.9(16) ? Fe1 O5w1 H2o5w1 ? ? ? 128.4(15) 127.6(16) 130.1(13) ? H1o5w1 O5w1 H2o5w1 ? ? ? 111(2) 111(2) 111(2) ? Fe1 O5w2 H1o5w2 ? ? ? 113.9(14) 113.0(13) 114.2(15) ? Fe1 O5w2 H2o5w2 ? ? ? 125.6(16) 124.3(14) 126.2(18) ? H1o5w2 O5w2 H2o5w2 ? ? ? 108.4(19) 108.4(19) 108.4(19) ? Fe1 O6w H1o6w ? ? ? 115.5(12) 113.0(12) 118.3(12) ? Fe1 O6w H2o6w ? ? ? 127.1(10) 121.9(9) 131.5(10) ? H1o6w O6w H2o6w ? ? ? 114.4(15) 114.4(16) 114.4(16) ? C1 N1 H1n1 ? ? ? 119.0(17) 118.7(17) 119.3(17) ? C1 N1 H1n1 ? ? 2_6555 119.0(17) 118.7(17) 119.3(17) ? C1 N1 H2n1 ? ? ? 118.1(17) 117.3(17) 118.9(17) ? C1 N1 H2n1 ? ? 2_6555 118.1(17) 117.3(17) 118.9(17) ? H1n1 N1 H1n1 ? ? 2_6555 122(2) 122(2) 122(2) ? H1n1 N1 H2n1 ? ? ? 107(2) 107(2) 108(2) ? H1n1 N1 H2n1 ? ? 2_6555 41(2) 40(2) 41(2) ? H1n1 N1 H2n1 2_6555 ? ? 41(2) 40(2) 41(2) ? H1n1 N1 H2n1 2_6555 ? 2_6555 107(2) 107(2) 108(2) ? H2n1 N1 H2n1 ? ? 2_6555 124(2) 123(2) 125(2) ? C3 N2 C3 ? ? 2_6555 121.31(17) 121.2(2) 121.4(2) ? C3 N2 H1n2 ? ? ? 119.34 119.31 119.38 ? C3 N2 H1n2 2_6555 ? ? 119.34 119.31 119.38 ? N1 C1 C2 ? ? ? 121.39(13) 120.66(16) 122.13(16) ? N1 C1 C2 ? ? 2_6555 121.39(13) 120.66(16) 122.13(16) ? C2 C1 C2 ? ? 2_6555 117.22(18) 117.1(2) 117.3(2) ? C1 C2 C3 ? ? ? 120.12(17) 120.03(17) 120.22(17) ? C1 C2 H1c2 ? ? ? 119.94 119.89 119.98 ? C3 C2 H1c2 ? ? ? 119.94 119.89 119.99 ? N2 C3 C2 ? ? ? 120.60(18) 120.56(17) 120.65(17) ? N2 C3 H1c3 ? ? ? 119.7 119.68 119.72 ? C2 C3 H1c3 ? ? ? 119.7 119.67 119.72 ? N1 H1n1 H2n1 ? ? 2_6555 70(3) 69(3) 70(3) ? N1 H2n1 H1n1 ? ? 2_6555 70(3) 69(3) 70(3) ? data_PhaseIV _exptl_crystal_type_of_structure cryst _audit_creation_method SHELXL-2014/7 _chemical_formula_sum 'C5 H15 Fe N2 O12 S2' _chemical_formula_weight 415.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.516(4) _cell_length_b 11.873(4) _cell_length_c 13.099(4) _cell_angle_alpha 65.34(3) _cell_angle_beta 77.51(3) _cell_angle_gamma 68.73(3) _cell_volume 1381.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used 2322 _cell_measurement_theta_min 2.4010 _cell_measurement_theta_max 29.2810 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.997 _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.27 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.960 _oxdiff_exptl_absorpt_empirical_full_max 1.065 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _diffrn_ambient_temperature 80(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.6249 _diffrn_reflns_number 7895 _diffrn_reflns_av_unetI/netI 0.0188 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.983 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_full 25.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 7895 _reflns_number_gt 5963 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max ? _reflns_Friedel_fraction_full ? _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would bepossible theoretically, ignoring centric projections andsystematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_structure_solution 'ShelXS-2014/7 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_molecular_graphics 'Diamond 2.1c (Brandenburg, 1997)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _refine_special_details 'Refined as a 2-component twin.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7895 _refine_ls_number_parameters 446 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.85489(5) 0.80465(5) 0.05110(4) 0.00606(9) Uani 1 1 d ? ? ? ? O11W O 0.8995(2) 0.7303(2) -0.06833(19) 0.0149(5) Uani 1 1 d D ? ? ? H11A H 0.895(3) 0.659(2) -0.062(2) 0.022 Uiso 1 1 d D U ? ? H11B H 0.917(3) 0.785(2) -0.1299(18) 0.022 Uiso 1 1 d D U ? ? O12W O 1.0244(2) 0.8607(2) -0.00306(17) 0.0180(5) Uani 1 1 d D ? ? ? H12A H 1.090(2) 0.848(2) 0.032(2) 0.027 Uiso 1 1 d D U ? ? H12B H 1.035(3) 0.899(2) -0.0698(16) 0.027 Uiso 1 1 d D U ? ? O13W O 0.81186(18) 0.87453(18) 0.17633(15) 0.0121(4) Uani 1 1 d D ? ? ? H13A H 0.797(2) 0.821(2) 0.2440(16) 0.018 Uiso 1 1 d D U ? ? H13B H 0.855(3) 0.909(2) 0.196(2) 0.018 Uiso 1 1 d D U ? ? O14W O 0.6785(2) 0.7595(2) 0.10258(19) 0.0129(5) Uani 1 1 d D ? ? ? H14A H 0.600(2) 0.812(2) 0.078(2) 0.019 Uiso 1 1 d D U ? ? H14B H 0.659(3) 0.716(2) 0.1693(16) 0.019 Uiso 1 1 d D U ? ? S11 S 1.02552(8) 0.49807(7) 0.19250(6) 0.00594(17) Uani 1 1 d ? ? ? ? O11 O 0.94714(15) 0.63949(14) 0.16268(12) 0.0119(3) Uani 1 1 d ? ? ? ? O12 O 1.1177(2) 0.4786(2) 0.09617(18) 0.0117(5) Uani 1 1 d ? ? ? ? O13 O 1.1034(2) 0.4622(2) 0.28774(19) 0.0105(5) Uani 1 1 d ? ? ? ? O14 O 0.9275(2) 0.4234(2) 0.2238(2) 0.0120(5) Uani 1 1 d ? ? ? ? S12 S 0.67609(8) 1.10656(8) -0.09414(6) 0.00639(18) Uani 1 1 d ? ? ? ? O15 O 0.75980(15) 0.96622(14) -0.06330(12) 0.0140(3) Uani 1 1 d ? ? ? ? O16 O 0.7677(2) 1.1834(2) -0.10813(19) 0.0129(5) Uani 1 1 d ? ? ? ? O17 O 0.6192(2) 1.14596(19) -0.19994(18) 0.0115(5) Uani 1 1 d ? ? ? ? O18 O 0.5663(2) 1.1188(2) -0.00516(19) 0.0106(5) Uani 1 1 d ? ? ? ? Fe2 Fe 0.14147(5) 0.69703(5) 0.44620(4) 0.00613(9) Uani 1 1 d ? ? ? ? O21W O 0.12655(18) 0.67397(18) 0.30560(15) 0.0138(4) Uani 1 1 d ? ? ? ? H21A H 0.160(2) 0.717(2) 0.2402(16) 0.021 Uiso 1 1 d ? U ? ? H21B H 0.126(3) 0.607(2) 0.299(2) 0.021 Uiso 1 1 d ? U ? ? O22W O 0.3376(2) 0.69092(19) 0.39982(19) 0.0136(5) Uani 1 1 d ? ? ? ? H22A H 0.406(2) 0.656(2) 0.433(2) 0.020 Uiso 1 1 d ? U ? ? H22B H 0.359(3) 0.750(2) 0.3361(18) 0.020 Uiso 1 1 d ? U ? ? O23W O 0.1403(2) 0.73612(19) 0.58166(18) 0.0106(5) Uani 1 1 d ? ? ? ? H23A H 0.129(3) 0.8129(19) 0.576(2) 0.016 Uiso 1 1 d ? U ? ? H23B H 0.106(3) 0.690(2) 0.6342(18) 0.016 Uiso 1 1 d ? U ? ? O24W O -0.05504(19) 0.69447(17) 0.49652(16) 0.0105(4) Uani 1 1 d ? ? ? ? H24A H -0.062(3) 0.645(2) 0.5571(17) 0.016 Uiso 1 1 d ? U ? ? H24B H -0.108(2) 0.697(2) 0.4532(19) 0.016 Uiso 1 1 d ? U ? ? S21 S 0.30787(8) 0.39157(8) 0.58710(7) 0.00705(17) Uani 1 1 d ? ? ? ? O21 O 0.19184(14) 0.51098(14) 0.53521(12) 0.0121(3) Uani 1 1 d ? ? ? ? O22 O 0.4257(2) 0.3861(2) 0.50322(18) 0.0105(5) Uani 1 1 d ? ? ? ? O23 O 0.34297(19) 0.39600(19) 0.68592(18) 0.0114(5) Uani 1 1 d ? ? ? ? O24 O 0.2543(2) 0.2805(2) 0.61826(19) 0.0101(5) Uani 1 1 d ? ? ? ? S22 S -0.01189(8) 1.01117(7) 0.31362(6) 0.00706(19) Uani 1 1 d ? ? ? ? O25 O 0.09707(15) 0.88340(14) 0.35703(13) 0.0125(3) Uani 1 1 d ? ? ? ? O26 O 0.0580(2) 1.11249(19) 0.27131(19) 0.0102(5) Uani 1 1 d ? ? ? ? O27 O -0.0733(2) 1.0135(2) 0.22243(18) 0.0126(5) Uani 1 1 d ? ? ? ? O28 O -0.1149(2) 1.0298(2) 0.40460(19) 0.0125(6) Uani 1 1 d ? ? ? ? N11 N 0.6558(3) 0.4454(3) 0.1977(3) 0.0104(4) Uani 1 1 d ? U ? ? H11 H 0.7086 0.4706 0.2218 0.013 Uiso 1 1 calc R U ? ? C12 C 0.7124(4) 0.3670(4) 0.1404(3) 0.0134(9) Uani 1 1 d ? ? ? ? H12 H 0.8092 0.3391 0.1273 0.016 Uiso 1 1 calc R U ? ? C13 C 0.6372(4) 0.3262(4) 0.1007(3) 0.0114(8) Uani 1 1 d ? ? ? ? H13 H 0.6801 0.2693 0.0609 0.014 Uiso 1 1 calc R U ? ? C14 C 0.4888(5) 0.3704(5) 0.1195(4) 0.0103(4) Uani 1 1 d ? ? ? ? N14 N 0.4103(3) 0.3316(3) 0.0820(3) 0.0122(4) Uani 1 1 d ? ? ? ? H14C H 0.3208 0.3574 0.0954 0.015 Uiso 1 1 calc R U ? ? H14D H 0.4480 0.2800 0.0439 0.015 Uiso 1 1 calc R U ? ? C15 C 0.4343(4) 0.4506(4) 0.1793(3) 0.0124(9) Uani 1 1 d ? ? ? ? H15 H 0.3378 0.4813 0.1930 0.015 Uiso 1 1 calc R U ? ? C16 C 0.5167(4) 0.4877(4) 0.2198(3) 0.0127(8) Uani 1 1 d ? ? ? ? H16 H 0.4778 0.5418 0.2624 0.015 Uiso 1 1 calc R U ? ? N21 N 0.3527(3) 0.0502(3) 0.2988(3) 0.0124(4) Uani 1 1 d ? U ? ? H21 H 0.3015 0.0243 0.2737 0.015 Uiso 1 1 calc R U ? ? C22 C 0.4918(4) 0.0105(4) 0.2774(3) 0.0126(9) Uani 1 1 d ? ? ? ? H22 H 0.5327 -0.0428 0.2342 0.015 Uiso 1 1 calc R U ? ? C23 C 0.5721(4) 0.0488(4) 0.3193(3) 0.0119(9) Uani 1 1 d ? ? ? ? H23 H 0.6688 0.0197 0.3060 0.014 Uiso 1 1 calc R U ? ? C24 C 0.5145(4) 0.1282(5) 0.3797(4) 0.0097(4) Uani 1 1 d ? ? ? ? N24 N 0.5907(3) 0.1685(3) 0.4186(3) 0.0128(4) Uani 1 1 d ? ? ? ? H24C H 0.6803 0.1441 0.4055 0.015 Uiso 1 1 calc R U ? ? H24D H 0.5513 0.2194 0.4571 0.015 Uiso 1 1 calc R U ? ? C25 C 0.3660(4) 0.1699(4) 0.3980(3) 0.0131(9) Uani 1 1 d ? ? ? ? H25 H 0.3211 0.2261 0.4382 0.016 Uiso 1 1 calc R U ? ? C26 C 0.2936(4) 0.1276(4) 0.3572(3) 0.0142(9) Uani 1 1 d ? ? ? ? H26 H 0.1968 0.1536 0.3702 0.017 Uiso 1 1 calc R U ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0051(3) 0.0058(2) 0.0068(3) -0.00176(16) -0.00046(19) -0.00186(18) O11W 0.0279(12) 0.0102(11) 0.0083(9) -0.0045(8) 0.0026(8) -0.0088(9) O12W 0.0152(10) 0.0302(13) 0.0087(9) 0.0016(9) -0.0027(8) -0.0165(9) O13W 0.0186(10) 0.0124(10) 0.0086(9) -0.0046(8) 0.0010(8) -0.0088(8) O14W 0.0106(9) 0.0195(12) 0.0090(9) -0.0025(9) -0.0008(7) -0.0082(9) S11 0.0060(3) 0.0058(4) 0.0063(3) -0.0021(3) -0.0004(3) -0.0023(3) O11 0.0138(8) 0.0065(8) 0.0111(8) -0.0022(6) -0.0020(6) 0.0009(7) O12 0.0113(12) 0.0139(13) 0.0082(11) -0.0051(9) 0.0018(9) -0.0022(10) O13 0.0099(10) 0.0111(10) 0.0116(9) -0.0050(7) -0.0009(7) -0.0034(8) O14 0.0089(9) 0.0158(11) 0.0122(9) -0.0034(8) -0.0021(7) -0.0061(8) S12 0.0060(3) 0.0064(4) 0.0065(3) -0.0024(3) -0.0009(3) -0.0013(3) O15 0.0139(8) 0.0106(9) 0.0131(8) -0.0035(7) -0.0020(6) 0.0007(7) O16 0.0130(10) 0.0173(12) 0.0103(10) -0.0033(9) -0.0020(8) -0.0083(9) O17 0.0149(10) 0.0099(11) 0.0090(9) -0.0011(8) -0.0015(7) -0.0055(8) O18 0.0083(12) 0.0158(13) 0.0115(11) -0.0093(10) 0.0015(9) -0.0041(10) Fe2 0.0050(3) 0.0061(2) 0.0068(3) -0.00165(16) -0.00057(19) -0.00194(18) O21W 0.0234(11) 0.0149(11) 0.0083(9) -0.0043(8) -0.0003(8) -0.0122(9) O22W 0.0071(9) 0.0140(12) 0.0114(10) 0.0024(9) -0.0025(7) -0.0015(9) O23W 0.0172(11) 0.0073(11) 0.0079(9) -0.0026(8) 0.0011(8) -0.0056(8) O24W 0.0090(9) 0.0132(10) 0.0092(9) -0.0018(8) -0.0016(7) -0.0056(8) S21 0.0063(3) 0.0061(4) 0.0079(3) -0.0027(3) 0.0002(3) -0.0013(3) O21 0.0097(8) 0.0109(8) 0.0142(8) -0.0029(6) -0.0013(6) -0.0036(7) O22 0.0089(12) 0.0144(13) 0.0100(11) -0.0069(9) 0.0007(9) -0.0035(10) O23 0.0112(10) 0.0145(12) 0.0092(9) -0.0031(8) -0.0023(8) -0.0054(8) O24 0.0137(10) 0.0080(11) 0.0092(9) -0.0016(8) -0.0019(7) -0.0054(8) S22 0.0074(3) 0.0061(4) 0.0064(3) -0.0013(3) -0.0002(3) -0.0019(3) O25 0.0109(8) 0.0082(8) 0.0138(8) -0.0021(7) -0.0011(6) 0.0000(7) O26 0.0150(10) 0.0089(11) 0.0109(9) -0.0041(8) -0.0014(7) -0.0077(8) O27 0.0159(11) 0.0164(11) 0.0092(10) -0.0034(8) -0.0031(8) -0.0093(9) O28 0.0110(13) 0.0125(12) 0.0097(11) -0.0036(9) 0.0011(9) -0.0006(10) N11 0.0072(12) 0.0110(11) 0.0127(11) -0.0020(8) -0.0049(9) -0.0029(9) C12 0.0095(18) 0.014(2) 0.016(2) -0.0040(16) -0.0030(15) -0.0037(15) C13 0.0061(18) 0.0085(19) 0.0155(19) -0.0043(16) 0.0007(15) 0.0012(15) C14 0.007(2) 0.0102(15) 0.0089(16) 0.0020(10) -0.0019(12) -0.0030(11) N14 0.0075(17) 0.0146(13) 0.0202(15) -0.0120(9) 0.0026(11) -0.0051(10) C15 0.0080(18) 0.016(2) 0.0160(19) -0.0067(17) -0.0004(15) -0.0055(16) C16 0.0101(18) 0.011(2) 0.0132(19) -0.0028(16) -0.0009(14) -0.0013(14) N21 0.0093(13) 0.0135(11) 0.0148(11) -0.0029(8) -0.0046(9) -0.0047(9) C22 0.0099(18) 0.013(2) 0.0130(19) -0.0053(16) 0.0014(14) -0.0015(15) C23 0.0072(17) 0.015(2) 0.0160(19) -0.0064(17) 0.0009(15) -0.0062(15) C24 0.0048(19) 0.0103(16) 0.0084(16) 0.0019(10) -0.0017(11) -0.0019(11) N24 0.0084(17) 0.0144(13) 0.0210(15) -0.0117(9) 0.0022(11) -0.0053(10) C25 0.0065(18) 0.013(2) 0.018(2) -0.0079(17) 0.0014(16) 0.0000(15) C26 0.0088(18) 0.019(2) 0.016(2) -0.0079(17) -0.0002(15) -0.0043(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O11 1.9401(18) ? ? Fe1 O15 1.9451(18) ? ? Fe1 O11W 1.995(2) ? ? Fe1 O12W 2.011(2) ? ? Fe1 O14W 2.015(2) ? ? Fe1 O13W 2.031(2) ? ? O11W H11A 0.828(18) ? ? O11W H11B 0.832(18) ? ? O12W H12A 0.852(19) ? ? O12W H12B 0.804(18) ? ? O13W H13A 0.868(18) ? ? O13W H13B 0.836(19) ? ? O14W H14A 0.867(19) ? ? O14W H14B 0.835(18) ? ? S11 O12 1.462(2) ? ? S11 O13 1.467(3) ? ? S11 O14 1.481(2) ? ? S11 O11 1.4964(18) ? ? S12 O17 1.453(2) ? ? S12 O18 1.466(2) ? ? S12 O16 1.488(3) ? ? S12 O15 1.4975(18) ? ? Fe2 O21 1.9465(18) ? ? Fe2 O25 1.9514(18) ? ? Fe2 O22W 2.003(2) ? ? Fe2 O23W 2.009(2) ? ? Fe2 O21W 2.0171(19) ? ? Fe2 O24W 2.036(2) ? ? O21W H21A 0.867(18) ? ? O21W H21B 0.838(19) ? ? O22W H22A 0.808(18) ? ? O22W H22B 0.887(18) ? ? O23W H23A 0.846(18) ? ? O23W H23B 0.786(18) ? ? O24W H24A 0.773(18) ? ? O24W H24B 0.863(18) ? ? S21 O23 1.446(2) ? ? S21 O22 1.470(2) ? ? S21 O24 1.488(2) ? ? S21 O21 1.5034(18) ? ? S22 O28 1.460(2) ? ? S22 O27 1.462(3) ? ? S22 O26 1.484(2) ? ? S22 O25 1.4961(18) ? ? N11 C12 1.330(5) ? ? N11 C16 1.371(5) ? ? N11 H11 0.8800 ? ? C12 C13 1.341(5) ? ? C12 H12 0.9500 ? ? C13 C14 1.456(6) ? ? C13 H13 0.9500 ? ? C14 N14 1.332(2) ? ? C14 C15 1.372(6) ? ? N14 H14C 0.8800 ? ? N14 H14D 0.8800 ? ? C15 C16 1.377(5) ? ? C15 H15 0.9500 ? ? C16 H16 0.9500 ? ? N21 C26 1.335(5) ? ? N21 C22 1.368(5) ? ? N21 H21 0.8800 ? ? C22 C23 1.381(5) ? ? C22 H22 0.9500 ? ? C23 C24 1.372(6) ? ? C23 H23 0.9500 ? ? C24 N24 1.337(2) ? ? C24 C25 1.456(6) ? ? N24 H24C 0.8800 ? ? N24 H24D 0.8800 ? ? C25 C26 1.340(6) ? ? C25 H25 0.9500 ? ? C26 H26 0.9500 ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Fe1 O15 177.57(7) ? ? ? O11 Fe1 O11W 92.71(8) ? ? ? O15 Fe1 O11W 85.35(9) ? ? ? O11 Fe1 O12W 93.61(8) ? ? ? O15 Fe1 O12W 87.83(8) ? ? ? O11W Fe1 O12W 89.22(9) ? ? ? O11 Fe1 O14W 89.35(9) ? ? ? O15 Fe1 O14W 89.26(9) ? ? ? O11W Fe1 O14W 92.19(7) ? ? ? O12W Fe1 O14W 176.66(9) ? ? ? O11 Fe1 O13W 85.48(8) ? ? ? O15 Fe1 O13W 96.45(8) ? ? ? O11W Fe1 O13W 178.18(8) ? ? ? O12W Fe1 O13W 91.11(7) ? ? ? O14W Fe1 O13W 87.57(8) ? ? ? Fe1 O11W H11A 127(2) ? ? ? Fe1 O11W H11B 109(2) ? ? ? H11A O11W H11B 123(3) ? ? ? Fe1 O12W H12A 131.0(19) ? ? ? Fe1 O12W H12B 116(2) ? ? ? H12A O12W H12B 113(3) ? ? ? Fe1 O13W H13A 116.6(17) ? ? ? Fe1 O13W H13B 131(2) ? ? ? H13A O13W H13B 95(3) ? ? ? Fe1 O14W H14A 124.4(18) ? ? ? Fe1 O14W H14B 123(2) ? ? ? H14A O14W H14B 104(3) ? ? ? O12 S11 O13 110.68(16) ? ? ? O12 S11 O14 110.09(16) ? ? ? O13 S11 O14 111.55(13) ? ? ? O12 S11 O11 109.71(11) ? ? ? O13 S11 O11 105.85(12) ? ? ? O14 S11 O11 108.85(12) ? ? ? S11 O11 Fe1 148.86(10) ? ? ? O17 S12 O18 110.48(14) ? ? ? O17 S12 O16 110.52(12) ? ? ? O18 S12 O16 111.59(16) ? ? ? O17 S12 O15 106.79(12) ? ? ? O18 S12 O15 108.82(12) ? ? ? O16 S12 O15 108.50(12) ? ? ? S12 O15 Fe1 148.09(10) ? ? ? O21 Fe2 O25 178.14(7) ? ? ? O21 Fe2 O22W 92.16(8) ? ? ? O25 Fe2 O22W 86.06(8) ? ? ? O21 Fe2 O23W 91.07(8) ? ? ? O25 Fe2 O23W 88.43(8) ? ? ? O22W Fe2 O23W 92.40(7) ? ? ? O21 Fe2 O21W 93.49(8) ? ? ? O25 Fe2 O21W 87.12(8) ? ? ? O22W Fe2 O21W 90.87(8) ? ? ? O23W Fe2 O21W 174.29(8) ? ? ? O21 Fe2 O24W 85.32(8) ? ? ? O25 Fe2 O24W 96.46(8) ? ? ? O22W Fe2 O24W 177.46(8) ? ? ? O23W Fe2 O24W 87.98(8) ? ? ? O21W Fe2 O24W 88.96(7) ? ? ? Fe2 O21W H21A 121.4(17) ? ? ? Fe2 O21W H21B 129(2) ? ? ? H21A O21W H21B 104(3) ? ? ? Fe2 O22W H22A 133.4(19) ? ? ? Fe2 O22W H22B 120.1(18) ? ? ? H22A O22W H22B 104(3) ? ? ? Fe2 O23W H23A 120.9(19) ? ? ? Fe2 O23W H23B 109(2) ? ? ? H23A O23W H23B 120(3) ? ? ? Fe2 O24W H24A 113(2) ? ? ? Fe2 O24W H24B 122.9(17) ? ? ? H24A O24W H24B 112(3) ? ? ? O23 S21 O22 110.76(15) ? ? ? O23 S21 O24 110.81(13) ? ? ? O22 S21 O24 111.56(15) ? ? ? O23 S21 O21 109.73(11) ? ? ? O22 S21 O21 108.90(11) ? ? ? O24 S21 O21 104.89(12) ? ? ? S21 O21 Fe2 144.75(10) ? ? ? O28 S22 O27 110.94(16) ? ? ? O28 S22 O26 109.94(15) ? ? ? O27 S22 O26 110.83(13) ? ? ? O28 S22 O25 110.10(12) ? ? ? O27 S22 O25 108.87(12) ? ? ? O26 S22 O25 106.04(12) ? ? ? S22 O25 Fe2 147.48(10) ? ? ? C12 N11 C16 121.33(17) ? ? ? C12 N11 H11 119.3 ? ? ? C16 N11 H11 119.3 ? ? ? N11 C12 C13 122.1(4) ? ? ? N11 C12 H12 119.0 ? ? ? C13 C12 H12 119.0 ? ? ? C12 C13 C14 119.0(4) ? ? ? C12 C13 H13 120.5 ? ? ? C14 C13 H13 120.5 ? ? ? N14 C14 C15 121.9(5) ? ? ? N14 C14 C13 120.9(5) ? ? ? C15 C14 C13 117.21(18) ? ? ? C14 N14 H14C 120.0 ? ? ? C14 N14 H14D 120.0 ? ? ? H14C N14 H14D 120.0 ? ? ? C14 C15 C16 121.3(4) ? ? ? C14 C15 H15 119.3 ? ? ? C16 C15 H15 119.3 ? ? ? N11 C16 C15 119.1(4) ? ? ? N11 C16 H16 120.5 ? ? ? C15 C16 H16 120.5 ? ? ? C26 N21 C22 120.97(17) ? ? ? C26 N21 H21 119.5 ? ? ? C22 N21 H21 119.5 ? ? ? N21 C22 C23 119.4(4) ? ? ? N21 C22 H22 120.3 ? ? ? C23 C22 H22 120.3 ? ? ? C24 C23 C22 121.1(4) ? ? ? C24 C23 H23 119.5 ? ? ? C22 C23 H23 119.5 ? ? ? N24 C24 C23 121.7(5) ? ? ? N24 C24 C25 120.8(5) ? ? ? C23 C24 C25 117.40(18) ? ? ? C24 N24 H24C 120.0 ? ? ? C24 N24 H24D 120.0 ? ? ? H24C N24 H24D 120.0 ? ? ? C26 C25 C24 118.8(4) ? ? ? C26 C25 H25 120.6 ? ? ? C24 C25 H25 120.6 ? ? ? N21 C26 C25 122.4(4) ? ? ? N21 C26 H26 118.8 ? ? ? C25 C26 H26 118.8 ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 S11 O11 Fe1 36.7(3) ? ? ? ? ? O13 S11 O11 Fe1 156.16(19) ? ? ? ? ? O14 S11 O11 Fe1 -83.8(2) ? ? ? ? ? O17 S12 O15 Fe1 -165.54(18) ? ? ? ? ? O18 S12 O15 Fe1 -46.3(2) ? ? ? ? ? O16 S12 O15 Fe1 75.3(2) ? ? ? ? ? O23 S21 O21 Fe2 74.87(19) ? ? ? ? ? O22 S21 O21 Fe2 -46.5(2) ? ? ? ? ? O24 S21 O21 Fe2 -166.06(17) ? ? ? ? ? O28 S22 O25 Fe2 46.8(2) ? ? ? ? ? O27 S22 O25 Fe2 -75.0(2) ? ? ? ? ? O26 S22 O25 Fe2 165.68(18) ? ? ? ? ? C16 N11 C12 C13 0.5(8) ? ? ? ? ? N11 C12 C13 C14 0.8(7) ? ? ? ? ? C12 C13 C14 N14 -179.6(4) ? ? ? ? ? C12 C13 C14 C15 -1.1(8) ? ? ? ? ? N14 C14 C15 C16 178.5(4) ? ? ? ? ? C13 C14 C15 C16 0.0(8) ? ? ? ? ? C12 N11 C16 C15 -1.6(7) ? ? ? ? ? C14 C15 C16 N11 1.4(7) ? ? ? ? ? C26 N21 C22 C23 1.5(7) ? ? ? ? ? N21 C22 C23 C24 -1.4(7) ? ? ? ? ? C22 C23 C24 N24 -178.4(4) ? ? ? ? ? C22 C23 C24 C25 0.1(8) ? ? ? ? ? N24 C24 C25 C26 179.7(4) ? ? ? ? ? C23 C24 C25 C26 1.1(8) ? ? ? ? ? C22 N21 C26 C25 -0.3(8) ? ? ? ? ? C24 C25 C26 N21 -1.1(8) ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11W H11A O12 0.828(18) 1.93(2) 2.726(4) 162(3) 2_765 O11W H11B O26 0.832(18) 1.767(19) 2.589(3) 169(3) 2_675 O12W H12A O16 0.852(19) 1.811(19) 2.662(3) 178(3) 2_775 O12W H12B O27 0.804(18) 1.861(19) 2.662(3) 175(3) 2_675 O13W H13A O24 0.868(18) 1.800(18) 2.664(3) 173(2) 2_666 O13W H13B O27 0.836(19) 1.846(19) 2.672(3) 169(3) 1_655 O14W H14A O18 0.867(19) 1.91(2) 2.743(3) 160(3) 2_675 O14W H14B O23 0.835(18) 1.805(19) 2.627(3) 168(3) 2_666 O21W H21A O16 0.867(18) 1.830(18) 2.695(3) 175(3) 2_675 O21W H21B O13 0.838(19) 1.885(19) 2.720(3) 174(3) 1_455 O22W H22A O22 0.808(18) 1.93(2) 2.719(4) 166(3) 2_666 O22W H22B O17 0.887(18) 1.716(19) 2.589(3) 167(3) 2_675 O23W H23A O28 0.846(18) 1.941(19) 2.773(3) 167(3) 2_576 O23W H23B O14 0.786(18) 1.838(19) 2.599(3) 163(3) 2_666 O24W H24A O13 0.773(18) 1.948(19) 2.717(3) 172(3) 2_666 O24W H24B O24 0.863(18) 1.850(19) 2.698(3) 167(2) 2_566 N11 H11 O14 0.88 2.17 2.856(3) 135.0 ? N11 H11 O23 0.88 2.23 2.880(3) 130.9 2_666 N14 H14C O12 0.88 2.10 2.945(5) 161.2 1_455 N14 H14D O18 0.88 2.14 2.994(4) 163.7 1_545 C15 H15 O13 0.95 2.55 3.439(5) 155.3 1_455 C16 H16 O23 0.95 2.56 3.050(5) 112.6 2_666 N21 H21 O17 0.88 2.40 3.006(4) 126.1 2_665 N21 H21 O26 0.88 2.39 2.980(4) 124.6 1_545 C22 H22 O17 0.95 2.54 3.083(5) 116.6 2_665 N24 H24C O28 0.88 2.09 2.938(5) 162.2 1_645 N24 H24D O22 0.88 2.19 3.036(4) 162.2 ? C25 H25 O24 0.95 2.59 3.464(5) 153.6 ? C26 H26 O26 0.95 2.43 3.022(5) 120.2 1_545 _refine_diff_density_max 0.363 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.088 _shelx_res_file ; twin_80k_twin1_hklf4_p1b.res created by SHELXL-2014/7 TITL twin_80k_twin1_hklf4 in P1 #1 REM reset to P1 #1 CELL 0.71073 10.516 11.873 13.099 65.34 77.51 68.73 ZERR 4 0.004 0.004 0.004 0.03 0.03 0.03 LATT 1 SFAC C H Fe N O S UNIT 20 60 4 8 48 8 EQIV $1 1+X,+Y,+Z EQIV $2 -1+X,+Y,+Z EQIV $3 -X,2-Y,1-Z EQIV $4 -X,1-Y,1-Z EQIV $5 +X,-1+Y,+Z EQIV $6 1-X,1-Y,-Z EQIV $7 1+X,-1+Y,+Z EQIV $8 2-X,1-Y,-Z EQIV $9 1-X,2-Y,-Z EQIV $10 2-X,2-Y,-Z EQIV $11 1-X,1-Y,1-Z DFIX 0.84 O11W H11a O11W H11b O12W H12b O12W H12a O13W H13b O13W H13a O14W = H14B O14W H14A O21W_$1 H21A_$1 O21W_$1 H21B_$1 O24W_$1 H24B_$1 O24W_$1 = H24A_$1 O23W_$1 H23A_$1 O22W_$1 H22A_$1 O22W_$1 H22B_$1 O23W_$1 H23B_$1 ISOR 0.002 0.2 N11 ISOR 0.002 0.2 N21 L.S. 10 PLAN 20 TEMP -193 HTAB O11W O12_$8 HTAB O11W O26_$9 HTAB O12W O16_$10 HTAB O12W O27_$9 HTAB O13W O24_$11 HTAB O13W O27_$1 HTAB O14W O18_$9 HTAB O14W O23_$11 HTAB O21W O16_$9 HTAB O21W O13_$2 HTAB O22W O22_$11 HTAB O22W O17_$9 HTAB O23W O28_$3 HTAB O23W O14_$11 HTAB O24W O13_$11 HTAB O24W O24_$4 HTAB N11 O14 HTAB N11 O23_$11 HTAB N14 O12_$2 HTAB N14 O18_$5 HTAB C15 O13_$2 HTAB C16 O23_$11 HTAB N21 O17_$6 HTAB N21 O26_$5 HTAB C22 O17_$6 HTAB N24 O28_$7 HTAB N24 O22 HTAB C25 O24 HTAB C26 O26_$5 BOND MORE -1 HTAB 2 BOND $H CONF fmap 2 acta 52 OMIT 0 52 OMIT 0 -1 -1 OMIT 0 1 1 OMIT -1 0 0 OMIT 0 1 2 OMIT 0 1 -1 OMIT 0 -1 -2 OMIT -1 1 0 OMIT 1 -1 0 OMIT 1 -1 1 OMIT -1 -2 0 OMIT 1 1 1 OMIT -1 -1 1 OMIT -1 4 2 OMIT -1 0 -2 OMIT 3 -2 0 OMIT 1 1 0 OMIT 0 0 -2 OMIT -2 -1 0 OMIT -2 -2 4 OMIT 2 2 -3 REM <olex2.extras> REM <HklSrc "%.\\80Ka_twin1_hklf5.hkl"> REM </olex2.extras> WGHT 0.045300 BASF 0.42054 FVAR 2.88130 FE1 3 0.854888 0.804650 0.051104 11.00000 0.00510 0.00582 = 0.00679 -0.00176 -0.00046 -0.00186 O11W 5 0.899545 0.730336 -0.068328 11.00000 0.02790 0.01016 = 0.00834 -0.00453 0.00258 -0.00883 H11A 2 0.894710 0.659428 -0.061583 11.00000 -1.50000 H11B 2 0.916534 0.785450 -0.129856 11.00000 -1.50000 O12W 5 1.024410 0.860698 -0.003062 11.00000 0.01523 0.03021 = 0.00870 0.00158 -0.00268 -0.01647 H12A 2 1.090438 0.848030 0.032368 11.00000 -1.50000 H12B 2 1.034645 0.899164 -0.069783 11.00000 -1.50000 O13W 5 0.811863 0.874534 0.176329 11.00000 0.01863 0.01241 = 0.00857 -0.00455 0.00103 -0.00885 H13A 2 0.797015 0.821266 0.244013 11.00000 -1.50000 H13B 2 0.854920 0.908505 0.195698 11.00000 -1.50000 O14W 5 0.678465 0.759531 0.102584 11.00000 0.01064 0.01946 = 0.00897 -0.00246 -0.00081 -0.00821 H14A 2 0.599624 0.811690 0.077833 11.00000 -1.50000 H14B 2 0.659093 0.715592 0.169327 11.00000 -1.50000 S11 6 1.025518 0.498068 0.192505 11.00000 0.00597 0.00577 = 0.00635 -0.00210 -0.00040 -0.00233 O11 5 0.947140 0.639490 0.162679 11.00000 0.01379 0.00651 = 0.01108 -0.00224 -0.00196 0.00087 O12 5 1.117744 0.478619 0.096170 11.00000 0.01134 0.01386 = 0.00819 -0.00510 0.00184 -0.00215 O13 5 1.103376 0.462172 0.287736 11.00000 0.00991 0.01106 = 0.01155 -0.00500 -0.00094 -0.00344 O14 5 0.927462 0.423391 0.223823 11.00000 0.00888 0.01579 = 0.01222 -0.00337 -0.00207 -0.00611 S12 6 0.676086 1.106562 -0.094138 11.00000 0.00600 0.00641 = 0.00649 -0.00241 -0.00094 -0.00134 O15 5 0.759799 0.966224 -0.063302 11.00000 0.01387 0.01064 = 0.01306 -0.00347 -0.00201 0.00073 O16 5 0.767661 1.183429 -0.108134 11.00000 0.01297 0.01728 = 0.01034 -0.00333 -0.00202 -0.00825 O17 5 0.619199 1.145962 -0.199935 11.00000 0.01485 0.00993 = 0.00903 -0.00115 -0.00152 -0.00547 O18 5 0.566310 1.118800 -0.005162 11.00000 0.00827 0.01575 = 0.01147 -0.00927 0.00151 -0.00407 FE2 3 0.141473 0.697034 0.446203 11.00000 0.00500 0.00607 = 0.00680 -0.00165 -0.00057 -0.00194 O21W 5 0.126547 0.673971 0.305604 11.00000 0.02342 0.01488 = 0.00828 -0.00428 -0.00029 -0.01220 H21A 2 0.159627 0.717260 0.240201 11.00000 -1.50000 H21B 2 0.125739 0.607089 0.298825 11.00000 -1.50000 O22W 5 0.337565 0.690924 0.399817 11.00000 0.00711 0.01405 = 0.01141 0.00240 -0.00254 -0.00151 H22A 2 0.406064 0.656266 0.433476 11.00000 -1.50000 H22B 2 0.359341 0.750095 0.336098 11.00000 -1.50000 O23W 5 0.140270 0.736122 0.581660 11.00000 0.01717 0.00725 = 0.00790 -0.00263 0.00109 -0.00560 H23A 2 0.129254 0.812852 0.575541 11.00000 -1.50000 H23B 2 0.106419 0.690417 0.634217 11.00000 -1.50000 O24W 5 -0.055038 0.694474 0.496521 11.00000 0.00905 0.01317 = 0.00918 -0.00182 -0.00160 -0.00556 H24A 2 -0.062340 0.645023 0.557127 11.00000 -1.50000 H24B 2 -0.108383 0.697492 0.453173 11.00000 -1.50000 S21 6 0.307871 0.391572 0.587099 11.00000 0.00630 0.00611 = 0.00791 -0.00274 0.00022 -0.00126 O21 5 0.191839 0.510980 0.535213 11.00000 0.00971 0.01094 = 0.01424 -0.00285 -0.00133 -0.00361 O22 5 0.425735 0.386054 0.503220 11.00000 0.00894 0.01443 = 0.00996 -0.00692 0.00066 -0.00351 O23 5 0.342966 0.396003 0.685917 11.00000 0.01117 0.01446 = 0.00925 -0.00314 -0.00230 -0.00537 O24 5 0.254285 0.280521 0.618258 11.00000 0.01366 0.00795 = 0.00921 -0.00157 -0.00192 -0.00537 S22 6 -0.011889 1.011167 0.313618 11.00000 0.00738 0.00609 = 0.00635 -0.00130 -0.00023 -0.00194 O25 5 0.097065 0.883397 0.357027 11.00000 0.01091 0.00824 = 0.01377 -0.00213 -0.00115 0.00005 O26 5 0.057957 1.112488 0.271311 11.00000 0.01499 0.00891 = 0.01092 -0.00408 -0.00141 -0.00775 O27 5 -0.073328 1.013522 0.222426 11.00000 0.01591 0.01637 = 0.00917 -0.00339 -0.00313 -0.00930 O28 5 -0.114934 1.029754 0.404598 11.00000 0.01103 0.01251 = 0.00969 -0.00356 0.00112 -0.00063 N11 4 0.655768 0.445390 0.197652 11.00000 0.00719 0.01104 = 0.01270 -0.00204 -0.00485 -0.00291 AFIX 43 H11 2 0.708629 0.470578 0.221821 11.00000 -1.20000 AFIX 0 C12 1 0.712392 0.367025 0.140410 11.00000 0.00953 0.01438 = 0.01570 -0.00404 -0.00297 -0.00368 AFIX 43 H12 2 0.809177 0.339114 0.127256 11.00000 -1.20000 AFIX 0 C13 1 0.637205 0.326182 0.100689 11.00000 0.00615 0.00850 = 0.01548 -0.00434 0.00065 0.00120 AFIX 43 H13 2 0.680118 0.269295 0.060893 11.00000 -1.20000 AFIX 0 C14 1 0.488771 0.370370 0.119495 11.00000 0.00687 0.01017 = 0.00890 0.00200 -0.00187 -0.00296 N14 4 0.410319 0.331561 0.082012 11.00000 0.00751 0.01459 = 0.02018 -0.01198 0.00256 -0.00509 AFIX 93 H14C 2 0.320838 0.357445 0.095388 11.00000 -1.20000 H14D 2 0.447964 0.280035 0.043870 11.00000 -1.20000 AFIX 0 C15 1 0.434271 0.450642 0.179256 11.00000 0.00800 0.01551 = 0.01603 -0.00671 -0.00037 -0.00547 AFIX 43 H15 2 0.337758 0.481274 0.192981 11.00000 -1.20000 AFIX 0 C16 1 0.516712 0.487710 0.219757 11.00000 0.01006 0.01114 = 0.01321 -0.00279 -0.00088 -0.00134 AFIX 43 H16 2 0.477768 0.541837 0.262406 11.00000 -1.20000 AFIX 0 N21 4 0.352742 0.050174 0.298776 11.00000 0.00928 0.01351 = 0.01476 -0.00293 -0.00462 -0.00468 AFIX 43 H21 2 0.301513 0.024275 0.273653 11.00000 -1.20000 AFIX 0 C22 1 0.491780 0.010535 0.277428 11.00000 0.00991 0.01259 = 0.01304 -0.00533 0.00142 -0.00148 AFIX 43 H22 2 0.532687 -0.042812 0.234230 11.00000 -1.20000 AFIX 0 C23 1 0.572129 0.048812 0.319277 11.00000 0.00724 0.01493 = 0.01598 -0.00643 0.00089 -0.00621 AFIX 43 H23 2 0.668833 0.019723 0.305998 11.00000 -1.20000 AFIX 0 C24 1 0.514510 0.128191 0.379734 11.00000 0.00484 0.01028 = 0.00844 0.00186 -0.00170 -0.00193 N24 4 0.590735 0.168486 0.418550 11.00000 0.00841 0.01442 = 0.02102 -0.01169 0.00216 -0.00533 AFIX 93 H24C 2 0.680331 0.144124 0.405537 11.00000 -1.20000 H24D 2 0.551310 0.219370 0.457113 11.00000 -1.20000 AFIX 0 C25 1 0.365951 0.169918 0.398049 11.00000 0.00649 0.01299 = 0.01804 -0.00792 0.00139 0.00004 AFIX 43 H25 2 0.321085 0.226129 0.438241 11.00000 -1.20000 AFIX 0 C26 1 0.293636 0.127557 0.357152 11.00000 0.00884 0.01909 = 0.01570 -0.00786 -0.00025 -0.00428 AFIX 43 H26 2 0.196781 0.153561 0.370193 11.00000 -1.20000 AFIX 0 HKLF 5 REM twin_80k_twin1_hklf4 in P1 #1 REM R1 = 0.0268 for 5963 Fo > 4sig(Fo) and 0.0371 for all 7895 data REM 446 parameters refined using 28 restraints END WGHT 0.0453 0.0000 REM Instructions for potential hydrogen bonds HTAB O11W S11_$8 HTAB O11W O12_$8 HTAB O11W S22_$9 HTAB O11W O26_$9 HTAB O12W S12_$10 HTAB O12W O16_$10 HTAB O12W S22_$9 HTAB O12W O27_$9 HTAB O13W S21_$11 HTAB O13W O24_$11 HTAB O13W O27_$1 HTAB O14W S12_$9 HTAB O14W O17_$9 HTAB O14W O18_$9 HTAB O14W S21_$11 HTAB O14W O23_$11 HTAB O21W S12_$9 HTAB O21W O16_$9 HTAB O21W S11_$2 HTAB O21W O13_$2 HTAB O22W S21_$11 HTAB O22W O22_$11 HTAB O22W S12_$9 HTAB O22W O17_$9 HTAB O23W S22_$3 HTAB O23W O28_$3 HTAB O23W S11_$11 HTAB O23W O14_$11 HTAB O24W O13_$11 HTAB O24W S21_$4 HTAB O24W O24_$4 HTAB N11 O14 HTAB N11 O23_$11 HTAB C12 O14 HTAB N14 O12_$2 HTAB N14 O18_$5 HTAB C15 O13_$2 HTAB C16 O23_$11 HTAB N21 O17_$6 HTAB N21 O26_$5 HTAB C22 O17_$6 HTAB N24 O28_$7 HTAB N24 O22 HTAB C25 O24 HTAB C26 O26_$5 REM Highest difference peak 0.363, deepest hole -0.598, 1-sigma level 0.088 Q1 1 0.0451 0.8605 0.3279 11.00000 0.05 0.36 Q2 1 -0.1010 1.0319 0.2031 11.00000 0.05 0.27 Q3 1 -0.1301 1.0257 0.5016 11.00000 0.05 0.27 Q4 1 0.6381 1.1978 -0.2397 11.00000 0.05 0.27 Q5 1 0.9883 0.9801 0.0329 11.00000 0.05 0.26 Q6 1 0.6574 1.1142 -0.1597 11.00000 0.05 0.26 Q7 1 0.6008 1.1194 0.0041 11.00000 0.05 0.26 Q8 1 0.3664 0.3635 0.7025 11.00000 0.05 0.25 Q9 1 0.9179 0.7779 0.2946 11.00000 0.05 0.25 Q10 1 0.4251 0.3689 0.4728 11.00000 0.05 0.25 Q11 1 0.6810 0.1024 0.4608 11.00000 0.05 0.24 Q12 1 0.2634 0.2467 0.6610 11.00000 0.05 0.24 Q13 1 0.0226 0.7923 0.2489 11.00000 0.05 0.24 Q14 1 0.0031 0.7146 0.2631 11.00000 0.05 0.24 Q15 1 0.4766 0.4402 0.2212 11.00000 0.05 0.24 Q16 1 1.0373 0.8822 0.0119 11.00000 0.05 0.23 Q17 1 -0.1000 1.0007 0.4374 11.00000 0.05 0.23 Q18 1 0.5239 1.2471 -0.2610 11.00000 0.05 0.23 Q19 1 0.2635 0.4328 -0.0285 11.00000 0.05 0.23 Q20 1 0.4806 0.3068 0.7356 11.00000 0.05 0.23 ; _shelx_res_checksum 27158 _shelx_hkl_file ; -1 -1 1 9912.63 50.3504 -2 0 0 -2 9912.63 50.3504 1 0 0 -3 54.1567 21.4697 1 -2 -2 2 9545.62 89.0963 -2 0 0 -4 9545.62 89.0963 1 0 0 -5 29.6315 27.5980 1 -3 -3 3 30050.7 231.549 -2 0 0 -6 30050.7 231.549 1 0 0 7 393.328 36.8292 1 -4 -4 4 77163.1 326.343 -2 0 0 -8 77163.1 326.343 1 0 0 9 27.1411 41.3180 1 5 5 -5 30893.0 295.142 -2 0 0 10 30893.0 295.142 1 0 0 -11 37.6720 81.1266 1 6 6 -6 11.9516 81.4563 -2 0 0 12 11.9516 81.4563 1 0 0 13 31.4187 81.0334 1 -7 -7 7 314.376 140.781 -2 0 0 -14 314.376 140.781 1 0 0 -15 316.856 157.515 1 -8 -8 8 3904.58 378.083 -2 0 0 -16 3904.58 378.083 1 -7 -8 8 5562.06 427.532 -2 0 1 -15 5562.06 427.532 1 0 1 -14 789.363 123.827 1 -6 -7 7 6714.61 202.525 -2 0 1 -13 6714.61 202.525 1 0 -1 12 11.3808 88.2863 1 -5 -6 6 210.376 117.974 -2 0 1 -11 210.376 117.974 1 0 -1 10 264.693 79.5040 1 -4 -5 5 92.1255 98.0806 -2 0 1 -9 92.1255 98.0806 1 0 -1 8 1030.48 60.9406 1 -3 -4 4 19765.0 164.752 -2 0 1 -7 19765.0 164.752 1 0 1 -6 33.4238 28.0932 1 -2 -3 3 21699.3 107.790 -2 0 1 -5 21699.3 107.790 1 0 1 -4 75.1978 23.4801 1 1 2 -2 56488.1 127.278 -2 0 -1 3 56488.1 127.278 1 0 -1 2 1.07287 24.3903 1 0 -1 1 1047.61 29.6597 -2 0 1 -1 1047.61 29.6597 1 0 1 0 6.65023 18.0453 1 1 0 0 1727.34 28.1444 -2 0 1 1 1727.34 28.1444 1 0 -1 -2 136.488 10.3874 1 -2 -1 1 372913. 1245.13 -2 0 -1 -3 372913. 1245.13 1 0 -1 -4 2235.36 39.5311 1 -3 -2 2 1510.34 37.1316 -2 0 -1 -5 1510.34 37.1316 1 0 -1 -6 212.717 31.5752 1 -4 -3 3 20614.5 157.214 -2 0 -1 -7 20614.5 157.214 1 0 -1 -8 331.796 35.8979 1 -5 -4 4 2059.76 52.7700 -2 0 -1 -9 2059.76 52.7700 1 0 1 10 94.1565 47.4036 1 6 5 -5 912.617 65.8368 -2 0 1 11 912.617 65.8368 1 0 1 12 1367.94 80.8724 1 -7 -6 6 1652.78 96.4873 -2 0 -1 -13 1652.78 96.4873 1 0 -1 -14 145.240 107.034 1 -8 -7 7 10061.1 387.756 -2 0 -1 -15 10061.1 387.756 1 0 -1 -16 350.489 164.752 1 0 2 -15 401.765 180.386 1 0 2 -13 311.663 111.760 1 5 7 -7 1608.92 192.574 -2 0 -2 12 1608.92 192.574 1 0 -2 11 378.859 95.0227 1 -4 -6 6 43701.0 629.209 -2 0 2 -10 43701.0 629.209 1 0 -2 9 74.2695 71.3488 1 -3 -5 5 13695.9 319.408 -2 0 2 -8 13695.9 319.408 1 0 2 -7 81.1249 39.5340 1 2 4 -4 558.469 61.3163 -2 0 -2 6 558.469 61.3163 1 0 -2 5 12.3141 30.3864 1 -1 -3 3 523.748 46.4917 -2 0 2 -4 523.748 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