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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_I _publ_contact_author_name 'Bosak, Alexei' _publ_contact_author_address ;European Synchrotron Radiation Facility, 71 avenue de Martyrs, Grenoble, 38043, France ; _publ_contact_author_email bossak@esrf.fr loop_ _publ_author_name _publ_author_address 'Bosak, Alexei' ;European Synchrotron Radiation Facility 71 avenue de Martyrs Grenoble 38043 France ; 'Svitlyk, Volodymir' ;European Synchrotron Radiation Facility 71 avenue de Martyrs Grenoble 38043 France ; 'Arakcheeva, Alla' ;Phase Solution Sarl Chemin des M\'esanges 7 Lausanne CH-1012 Switzerland Laboratoire de Physique de la Mati\`ere Complexe Ecole Polytechnique Federale de Lausanne Lausanne CH-1015 Switzerland ; 'Burkovskiy, Roman' ;Peter the Great Saint-Petersburg Polytechnic University Saint-Petersburg Russian Federation ; 'Diadkin, Vadim' ;Swiss-Norwegian Beam Lines at ESRF 71 avenue de Martyrs Grenoble 38043 France ; 'Roleder, Krystian' ;Institute of Physics University of Silesia ulica Uniwersytecka 4 Katowice PL-40-007 Poland ; 'Chernyshov, Dmitry' ;Peter the Great Saint-Petersburg Polytechnic University Saint-Petersburg Russian Federation Swiss-Norwegian Beam Lines at ESRF 71 avenue de Martyrs Grenoble 38043 France ; _publ_section_title ;Incommensurate crystal structure of PbHfO~3~ ; _journal_date_recd_electronic 2019-01-18 _journal_date_accepted 2019-11-05 _journal_coeditor_code DK5080SUP1 _journal_paper_category FA _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2020 _journal_volume 76 _journal_issue 1 _journal_page_first 7 _journal_page_last 12 _journal_paper_doi https://doi.org/10.1107/S205252061901494X _journal_techeditor_code B191494 _iucr_compatibility_tag ACTA95 _chemical_formula_sum 'Pb Hf O3' _chemical_formula_weight 433.7 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Imma(00\g)s00 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2+1/2,x3,x4+1/2 3 -x1,x2+1/2,-x3,-x4 4 x1,-x2,-x3,-x4+1/2 5 -x1,-x2,-x3,-x4 6 x1,x2+1/2,-x3,-x4+1/2 7 x1,-x2+1/2,x3,x4 8 -x1,x2,x3,x4+1/2 9 x1+1/2,x2+1/2,x3+1/2,x4 10 -x1+1/2,-x2,x3+1/2,x4+1/2 11 -x1+1/2,x2,-x3+1/2,-x4 12 x1+1/2,-x2+1/2,-x3+1/2,-x4+1/2 13 -x1+1/2,-x2+1/2,-x3+1/2,-x4 14 x1+1/2,x2,-x3+1/2,-x4+1/2 15 x1+1/2,-x2,x3+1/2,x4 16 -x1+1/2,x2+1/2,x3+1/2,x4+1/2 _cell_length_a 5.8522(8) _cell_length_b 8.236(3) _cell_length_c 5.867(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 282.8(3) _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 0.000000 0.298200 _cell_formula_units_Z 4 _cell_measurement_reflns_used 3769 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.39 _cell_measurement_temperature 443 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 10.1855 _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 121.752 _exptl_crystal_description rod _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.64256 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 443 _diffrn_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.77865 _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Inhouse made diffractometer coupled to Pilatus2M detector at SNBL BM01/ESRF' _diffrn_detector 'Pilatus2M detector at SNBL BM01/ESRF' _diffrn_reflns_number 3769 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.39 _diffrn_reflns_theta_full 18 _diffrn_measured_fraction_theta_max 0.75 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0105 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 _diffrn_radiation_probe x-ray _refine_special_details ; U33 for Hf shows negative value of -0.000811. This parameter is fixed for 0.000811. The positive U33 of 0.00145 is fixed for O1. X-harmonics in crenel interval are used for Pb1. Anharmonic ADPs are used for Hf1. ; _reflns_number_total 679 _reflns_number_gt 490 _reflns_threshold_expression I>4\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_gt 0.1305 _refine_ls_R_factor_all 0.0456 _refine_ls_wR_factor_ref 0.1326 _refine_ls_goodness_of_fit_ref 3.69 _refine_ls_goodness_of_fit_gt 4.40 _refine_ls_number_reflns 679 _refine_ls_number_parameters 86 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_shift/su_max 0.0259 _refine_ls_shift/su_mean 0.0048 _refine_diff_density_max 2.91 _refine_diff_density_min -4.74 _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick, 2015)' _refine_ls_extinction_coef 0.049(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Hf -0.8251 7.2554 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0141 0.0076 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Pb -6.9391 11.7619 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_structure_refinement 'Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352' _computing_molecular_graphics ; Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. ; 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 Hf1 Hf 0 0 0 Uani 0.012(4) 4 1 d ? ? ? Pb1 Pb 0.0292(5) 0.75 0.50222(6) Uani 0.0220(6) 8 0.5 d ? ? ? O1 O 0 0.75 0.0467(11) Uani 0.009(3) 4 1 d ? ? ? O2 O 0.25 0.0227(6) 0.25 Uani 0.0197(19) 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 Hf1 Hf 0.004(4) 0.031(11) 0.000811 0 0 0.0035(9) Pb1 Pb 0.0168(8) 0.0291(14) 0.0201(7) 0 -0.00184(10) 0 O1 O 0.018(3) 0.009(9) 0.001445 0 0 0 O2 O 0.018(3) 0.031(4) 0.010(3) 0 -0.000006 0 loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 Hf1 Hf 0 0 0 0 0 0 0 0 0 0 loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 Hf1 Hf 0.07(3) 0 0 0.015(8) -0.0009(8) -0.002(9) 0 0 0 0 0.07(4) 0.027(3) 0.008(6) 0.002(2) 0.055(10) loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 Hf1 Hf 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 Hf1 Hf 0.13(5) 0 0 0.005(5) -0.0012(6) -0.007(8) 0 0 0 0 0.018(8) 0.0000(3) 0.0002(15) 0.0000(4) 0.003(8) 0 0 0 0 0 0 0.08(6) 0.045(5) 0.004(4) 0.0003(8) 0.005(5) 0.003(2) 0.09(2) 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 Pb1 0.75 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 Hf1x1 Hf1 x 1 Hf1y1 Hf1 y 1 Hf1z1 Hf1 z 1 Hf1x2 Hf1 x 2 Hf1y2 Hf1 y 2 Hf1z2 Hf1 z 2 Hf1x3 Hf1 x 3 Hf1y3 Hf1 y 3 Hf1z3 Hf1 z 3 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O1x3 O1 x 3 O1y3 O1 y 3 O1z3 O1 z 3 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O2x2 O2 x 2 O2y2 O2 y 2 O2z2 O2 z 2 O2x3 O2 x 3 O2y3 O2 y 3 O2z3 O2 z 3 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Hf1x1 0 -0.00464(13) Hf1y1 0 0 Hf1z1 0 0 Hf1x2 0 0 Hf1y2 0 0.00005(2) Hf1z2 0 -0.00022(3) Hf1x3 0 -0.00097(3) Hf1y3 0 0 Hf1z3 0 0 O1x1 -0.0197(8) 0.0200(9) O1y1 0 0 O1z1 0 0 O1x2 0 0 O1y2 0 0 O1z2 0.0005(5) -0.0019(5) O1x3 -0.0018(6) 0.0043(6) O1y3 0 0 O1z3 0 0 O2x1 0 0.0137(9) O2y1 -0.0097(4) 0 O2z1 0 -0.0078(7) O2x2 0 -0.0001(4) O2y2 -0.0001(3) 0 O2z2 0 -0.0004(4) O2x3 0 0.0066(4) O2y3 -0.0007(3) 0 O2z3 0 -0.0062(4) 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 Pb1 x 1 -0.00084(6) Pb1 y 1 0 Pb1 z 1 -0.0004(4) Pb1 x 2 0.0042(4) Pb1 y 2 0 Pb1 z 2 -0.00068(5) Pb1 x 3 0.00016(8) Pb1 y 3 0 Pb1 z 3 0.0012(5) Pb1 x 4 0.0082(6) Pb1 y 4 0 Pb1 z 4 -0.0004(6) 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 Pb1 U11 1 0.00308(15) Pb1 U22 1 -0.0008(4) Pb1 U33 1 0.0002(3) Pb1 U12 1 0 Pb1 U13 1 -0.0017(5) Pb1 U23 1 0 Pb1 U11 2 0.0000(9) Pb1 U22 2 -0.0007(2) Pb1 U33 2 -0.00087(15) Pb1 U12 2 0 Pb1 U13 2 -0.00013(19) Pb1 U23 2 0 Pb1 U11 3 0.0012(2) Pb1 U22 3 0.0000(5) Pb1 U33 3 -0.0005(3) Pb1 U12 3 0 Pb1 U13 3 -0.0003(7) Pb1 U23 3 0 Pb1 U11 4 -0.0111(18) Pb1 U22 4 0.0002(12) Pb1 U33 4 0.0014(7) Pb1 U12 4 0 Pb1 U13 4 -0.0007(6) Pb1 U23 4 0 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 Hf1 O1 ? 1_5455 2.0815(11) 2.0766(13) 2.0883(13) ? Hf1 O1 ? 3_5455 2.0815(11) 2.0766(13) 2.0883(13) ? Hf1 O2 ? ? 2.083(5) 2.042(8) 2.124(8) ? Hf1 O2 ? 10_5545 2.083(5) 2.042(8) 2.124(8) ? Hf1 O2 ? 5_5555 2.083(5) 2.042(8) 2.124(8) ? Hf1 O2 ? 14_4555 2.083(5) 2.042(8) 2.124(8) ? Pb1 O1 ? ? 2.680(8) 2.666(9) 2.697(9) ? Pb1 O1 ? 1_5565 3.207(8) 3.180(9) 3.241(9) ? Pb1 O1 ? 11_4555 3.194(12) 3.018(13) 3.288(13) ? Pb1 O1 ? 11_5555 2.686(11) 2.592(12) 2.860(12) ? Pb1 O2 ? 1_5655 2.967(7) 2.855(8) 3.089(8) ? Pb1 O2 ? 9_4555 2.936(7) 2.873(8) 3.013(8) ? Pb1 O2 ? 2_5555 3.169(7) 3.053(8) 3.268(8) ? Pb1 O2 ? 10_5655 2.648(7) 2.578(7) 2.716(7) ? Pb1 O2 ? 5_5665 2.936(7) 2.873(8) 3.013(8) ? Pb1 O2 ? 13_5555 2.967(7) 2.855(8) 3.089(8) ? Pb1 O2 ? 6_5565 2.648(7) 2.578(7) 2.716(7) ? Pb1 O2 ? 14_4655 3.169(7) 3.053(8) 3.268(8) ? 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 O1 Hf1 O1 1_5455 ? 3_5455 174.3(3) 172.6(3) 180 ? O1 Hf1 O2 1_5455 ? ? 89.7(2) 87.8(2) 91.7(3) ? O1 Hf1 O2 1_5455 ? 10_5545 90.1(2) 86.3(3) 93.8(2) ? O1 Hf1 O2 1_5455 ? 5_5555 90.1(2) 86.3(3) 93.8(2) ? O1 Hf1 O2 1_5455 ? 14_4555 89.7(2) 87.8(2) 91.7(3) ? O1 Hf1 O2 3_5455 ? ? 90.1(2) 86.3(3) 93.8(2) ? O1 Hf1 O2 3_5455 ? 10_5545 89.7(2) 87.8(2) 91.7(3) ? O1 Hf1 O2 3_5455 ? 5_5555 89.7(2) 87.8(2) 91.7(3) ? O1 Hf1 O2 3_5455 ? 14_4555 90.1(2) 86.3(3) 93.8(2) ? O2 Hf1 O2 ? ? 10_5545 90.6(3) 86.1(3) 95.3(3) ? O2 Hf1 O2 ? ? 5_5555 176.2(3) 175.0(3) 180 ? O2 Hf1 O2 ? ? 14_4555 89.4(3) 89.3(3) 89.5(3) ? O2 Hf1 O2 10_5545 ? 5_5555 89.4(3) 89.3(3) 89.5(3) ? O2 Hf1 O2 10_5545 ? 14_4555 176.2(3) 175.0(3) 180 ? O2 Hf1 O2 5_5555 ? 14_4555 90.6(3) 86.1(3) 95.3(3) ? O1 Pb1 O1 ? ? 1_5565 171.8(3) 166.7(3) 176.7(3) ? O1 Pb1 O1 ? ? 11_4555 81.4(2) 77.1(3) 85.5(2) ? O1 Pb1 O1 ? ? 11_5555 87.3(3) 82.7(3) 92.1(3) ? O1 Pb1 O2 ? ? 1_5655 62.4(2) 60.29(19) 64.3(2) ? O1 Pb1 O2 ? ? 9_4555 118.0(2) 114.4(3) 121.5(2) ? O1 Pb1 O2 ? ? 2_5555 59.6(2) 57.83(19) 61.6(2) ? O1 Pb1 O2 ? ? 10_5655 124.5(2) 121.1(2) 128.4(2) ? O1 Pb1 O2 ? ? 5_5665 118.0(2) 114.4(3) 121.5(2) ? O1 Pb1 O2 ? ? 13_5555 62.4(2) 60.29(19) 64.3(2) ? O1 Pb1 O2 ? ? 6_5565 124.5(2) 121.1(2) 128.4(2) ? O1 Pb1 O2 ? ? 14_4655 59.6(2) 57.83(19) 61.6(2) ? O1 Pb1 O1 1_5565 ? 11_4555 90.4(2) 87.3(2) 92.8(2) ? O1 Pb1 O1 1_5565 ? 11_5555 100.9(3) 98.0(3) 103.8(3) ? O1 Pb1 O2 1_5565 ? 1_5655 121.45(19) 120.40(19) 122.8(2) ? O1 Pb1 O2 1_5565 ? 9_4555 56.6(2) 55.1(2) 59.2(2) ? O1 Pb1 O2 1_5565 ? 2_5555 115.5(2) 113.1(2) 116.7(2) ? O1 Pb1 O2 1_5565 ? 10_5655 60.1(2) 57.4(2) 61.3(2) ? O1 Pb1 O2 1_5565 ? 5_5665 56.6(2) 55.1(2) 59.2(2) ? O1 Pb1 O2 1_5565 ? 13_5555 121.45(19) 120.40(19) 122.8(2) ? O1 Pb1 O2 1_5565 ? 6_5565 60.1(2) 57.4(2) 61.3(2) ? O1 Pb1 O2 1_5565 ? 14_4655 115.5(2) 113.1(2) 116.7(2) ? O1 Pb1 O1 11_4555 ? 11_5555 168.7(3) 168.1(2) 169.2(2) ? O1 Pb1 O2 11_4555 ? 1_5655 111.9(2) 110.4(2) 112.9(2) ? O1 Pb1 O2 11_4555 ? 9_4555 58.4(2) 56.9(2) 59.9(2) ? O1 Pb1 O2 11_4555 ? 2_5555 55.17(19) 53.80(18) 56.19(18) ? O1 Pb1 O2 11_4555 ? 10_5655 121.2(2) 119.3(3) 123.1(2) ? O1 Pb1 O2 11_4555 ? 5_5665 58.4(2) 56.9(2) 59.9(2) ? O1 Pb1 O2 11_4555 ? 13_5555 111.9(2) 110.4(2) 112.9(2) ? O1 Pb1 O2 11_4555 ? 6_5565 121.2(2) 119.3(3) 123.1(2) ? O1 Pb1 O2 11_4555 ? 14_4655 55.17(19) 53.80(18) 56.19(18) ? O1 Pb1 O2 11_5555 ? 1_5655 62.0(2) 60.9(2) 63.7(2) ? O1 Pb1 O2 11_5555 ? 9_4555 128.5(2) 126.4(2) 130.7(2) ? O1 Pb1 O2 11_5555 ? 2_5555 118.5(2) 117.7(2) 119.9(2) ? O1 Pb1 O2 11_5555 ? 10_5655 65.8(2) 63.8(2) 67.5(3) ? O1 Pb1 O2 11_5555 ? 5_5665 128.5(2) 126.4(2) 130.7(2) ? O1 Pb1 O2 11_5555 ? 13_5555 62.0(2) 60.9(2) 63.7(2) ? O1 Pb1 O2 11_5555 ? 6_5565 65.8(2) 63.8(2) 67.5(3) ? O1 Pb1 O2 11_5555 ? 14_4655 118.5(2) 117.7(2) 119.9(2) ? O2 Pb1 O2 1_5655 ? 9_4555 168.9(2) 165.9(2) 171.7(2) ? O2 Pb1 O2 1_5655 ? 2_5555 121.7(2) 121.4(3) 122.1(2) ? O2 Pb1 O2 1_5655 ? 10_5655 62.1(2) 60.52(19) 64.1(2) ? O2 Pb1 O2 1_5655 ? 5_5665 89.54(18) 87.48(18) 92.86(17) ? O2 Pb1 O2 1_5655 ? 13_5555 99.8(2) 97.4(2) 102.7(2) ? O2 Pb1 O2 1_5655 ? 6_5565 126.9(3) 124.2(3) 130.2(3) ? O2 Pb1 O2 1_5655 ? 14_4655 56.9(2) 56.7(2) 57.08(18) ? O2 Pb1 O2 9_4555 ? 2_5555 58.86(19) 57.18(19) 60.3(2) ? O2 Pb1 O2 9_4555 ? 10_5655 116.6(3) 115.9(3) 117.1(3) ? O2 Pb1 O2 9_4555 ? 5_5665 80.6(2) 76.3(2) 85.3(2) ? O2 Pb1 O2 9_4555 ? 13_5555 89.54(19) 87.48(19) 92.86(18) ? O2 Pb1 O2 9_4555 ? 6_5565 63.0(2) 62.5(2) 63.3(2) ? O2 Pb1 O2 9_4555 ? 14_4655 113.0(2) 110.2(2) 115.4(2) ? O2 Pb1 O2 2_5555 ? 10_5655 174.6(3) 172.3(3) 176.3(3) ? O2 Pb1 O2 2_5555 ? 5_5665 113.0(2) 110.2(2) 115.4(2) ? O2 Pb1 O2 2_5555 ? 13_5555 56.9(2) 56.7(2) 57.1(2) ? O2 Pb1 O2 2_5555 ? 6_5565 90.97(19) 87.60(19) 93.11(18) ? O2 Pb1 O2 2_5555 ? 14_4655 89.1(2) 86.6(2) 91.0(2) ? O2 Pb1 O2 10_5655 ? 5_5665 63.0(2) 62.5(2) 63.3(2) ? O2 Pb1 O2 10_5655 ? 13_5555 126.9(3) 124.2(2) 130.2(3) ? O2 Pb1 O2 10_5655 ? 6_5565 88.5(2) 83.0(2) 93.8(3) ? O2 Pb1 O2 10_5655 ? 14_4655 90.97(19) 87.60(18) 93.11(17) ? O2 Pb1 O2 5_5665 ? 13_5555 168.9(2) 165.9(3) 171.7(2) ? O2 Pb1 O2 5_5665 ? 6_5565 116.6(3) 115.9(3) 117.1(3) ? O2 Pb1 O2 5_5665 ? 14_4655 58.86(19) 57.18(19) 60.3(2) ? O2 Pb1 O2 13_5555 ? 6_5565 62.1(2) 60.52(19) 64.1(2) ? O2 Pb1 O2 13_5555 ? 14_4655 121.7(2) 121.4(3) 122.1(2) ? O2 Pb1 O2 6_5565 ? 14_4655 174.6(3) 172.3(3) 176.3(3) ?