#------------------------------------------------------------------------------ #$Date: 2020-10-08 01:21:31 +0300 (Thu, 08 Oct 2020) $ #$Revision: 258232 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003692.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4003692 loop_ _publ_author_name 'Liu, Xitao' 'Xu, Zhiyun' 'Long, Peiqing' 'Yao, Yunpeng' 'Ji, Chengmin' 'Li, Lina' 'Sun, Zhihua' 'Hong, Maochun' 'Luo, Junhua' _publ_section_title ; A Multiaxial Layered Halide Double Perovskite Ferroelectric with Multiple Ferroic Orders ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/acs.chemmater.0c02966 _journal_year 2020 _chemical_formula_moiety 'Ag Bi Br7 Cs, 2(C4 H12 N)' _chemical_formula_sum 'C8 H24 Ag Bi Br7 Cs N2' _chemical_formula_weight 1157.42 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-12-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 101.734(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.0618(5) _cell_length_b 7.8928(4) _cell_length_c 19.7697(12) _cell_measurement_reflns_used 7199 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 27.477 _cell_measurement_theta_min 2.787 _cell_volume 1231.66(12) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 199.98 _diffrn_detector 'Bruker APEX3 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX3 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18268 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.987 _diffrn_reflns_theta_max 24.987 _diffrn_reflns_theta_min 2.581 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 20.734 _exptl_absorpt_correction_T_max 0.2616 _exptl_absorpt_correction_T_min 0.1489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1245 before and 0.0641 after correction. The Ratio of minimum to maximum transmission is 0.5692. The \l/2 correction factor is Not present.' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 3.121 _exptl_crystal_description block _exptl_crystal_F_000 1032 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.864 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.172 _refine_ls_abs_structure_details ; Flack x determined using 1748 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.282(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 4363 _refine_ls_number_restraints 52 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0358 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+16.6632P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.0764 _reflns_Friedel_coverage 0.854 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 4107 _reflns_number_total 4363 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cm0c02966_si_002.cif _cod_data_source_block x1 _cod_database_code 4003692 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.575 _shelx_estimated_absorpt_t_min 0.424 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.526(2) 0.474(2) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C4-C3 1.5 with sigma of 0.02 N1-C1 = N2-C5 1.47 with sigma of 0.02 4. Uiso/Uaniso restraints and constraints N2 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 C1 \\sim N1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 5.a Secondary CH2 refined with riding coordinates: C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C1(H1A,H1B), C2(H2D,H2E), C3(H3A,H3B) 5.b Idealised Me refined as rotating group: N2(H2A,H2B,H2C), C8(H8A,H8B,H8C), N1(H1C,H1D,H1E), C4(H4A,H4B,H4C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.1704(5) 1.0177(7) 0.16099(9) 0.0365(6) Uani 1 1 d . . . . . Bi1 Bi 0.3195(2) 0.5120(4) 0.14168(4) 0.02094(17) Uani 1 1 d . . . . . Br1 Br 0.5601(7) 0.2461(7) 0.1468(4) 0.0340(16) Uani 1 1 d . . . . . Cs1 Cs -0.2576(2) 0.5169(3) 0.00046(7) 0.0321(3) Uani 1 1 d . . . . . Br2 Br 0.0474(7) 0.2749(7) 0.1301(3) 0.0287(13) Uani 1 1 d . . . . . Br3 Br 0.5823(7) 0.7519(7) 0.1474(4) 0.0324(15) Uani 1 1 d . . . . . Br4 Br 0.3486(4) 0.4831(6) 0.29224(12) 0.0335(10) Uani 1 1 d . . . . . Br5 Br 0.2714(4) 0.5113(5) -0.00175(12) 0.0318(5) Uani 1 1 d . . . . . Br6 Br 0.0794(6) 0.7777(7) 0.1318(4) 0.0314(14) Uani 1 1 d . . . . . Br7 Br -0.0536(4) 0.9806(6) 0.29888(15) 0.0420(11) Uani 1 1 d . . . . . N2 N 0.327(3) 1.055(3) 0.2602(11) 0.036(6) Uani 1 1 d D U . . . H2A H 0.357367 1.074764 0.218984 0.044 Uiso 1 1 calc GR . . . . H2B H 0.308733 1.154825 0.280153 0.044 Uiso 1 1 calc GR . . . . H2C H 0.231041 0.991234 0.253162 0.044 Uiso 1 1 calc GR . . . . C5 C 0.465(3) 0.962(4) 0.3062(13) 0.040(6) Uani 1 1 d D U . . . H5A H 0.450374 0.838822 0.297217 0.048 Uiso 1 1 calc R . . . . H5B H 0.575125 0.995614 0.295256 0.048 Uiso 1 1 calc R . . . . C6 C 0.469(4) 0.994(6) 0.3786(10) 0.039(6) Uani 1 1 d . U . . . H6A H 0.357110 0.967862 0.388951 0.047 Uiso 1 1 calc R . . . . H6B H 0.492994 1.115596 0.388454 0.047 Uiso 1 1 calc R . . . . C7 C 0.599(5) 0.892(5) 0.4232(16) 0.053(7) Uani 1 1 d . U . . . H7A H 0.710066 0.916487 0.411387 0.063 Uiso 1 1 calc R . . . . H7B H 0.573701 0.770604 0.413027 0.063 Uiso 1 1 calc R . . . . C8 C 0.614(5) 0.920(6) 0.5009(15) 0.072(10) Uani 1 1 d . U . . . H8A H 0.571933 1.033610 0.508729 0.108 Uiso 1 1 calc GR . . . . H8B H 0.732984 0.910575 0.524363 0.108 Uiso 1 1 calc GR . . . . H8C H 0.546667 0.834927 0.519245 0.108 Uiso 1 1 calc GR . . . . C1 C -0.163(4) 0.464(4) 0.3027(14) 0.051(7) Uani 1 1 d D U . . . H1A H -0.162883 0.342453 0.290284 0.061 Uiso 1 1 calc R . . . . H1B H -0.282954 0.500972 0.296419 0.061 Uiso 1 1 calc R . . . . N1 N -0.079(3) 0.562(3) 0.2567(11) 0.045(8) Uani 1 1 d D U . . . H1C H -0.138317 0.553314 0.212547 0.055 Uiso 1 1 calc GR . . . . H1D H 0.027903 0.520878 0.259164 0.055 Uiso 1 1 calc GR . . . . H1E H -0.072722 0.672667 0.269887 0.055 Uiso 1 1 calc GR . . . . C2 C -0.076(5) 0.486(6) 0.3789(10) 0.050(7) Uani 1 1 d . U . . . H2D H 0.043760 0.449566 0.385472 0.060 Uiso 1 1 calc R . . . . H2E H -0.077239 0.607569 0.391745 0.060 Uiso 1 1 calc R . . . . C3 C -0.167(5) 0.382(5) 0.4251(14) 0.061(7) Uani 1 1 d D U . . . H3A H -0.289302 0.409432 0.413182 0.074 Uiso 1 1 calc R . . . . H3B H -0.154909 0.260379 0.414416 0.074 Uiso 1 1 calc R . . . . C4 C -0.108(5) 0.406(5) 0.5000(13) 0.070(10) Uani 1 1 d D U . . . H4A H -0.104550 0.527548 0.510727 0.105 Uiso 1 1 calc GR . . . . H4B H 0.006429 0.358448 0.514310 0.105 Uiso 1 1 calc GR . . . . H4C H -0.184932 0.348881 0.524910 0.105 Uiso 1 1 calc GR . . . . 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 Ag1 0.0187(11) 0.0210(11) 0.0707(12) 0.009(3) 0.0114(18) 0.0006(13) Bi1 0.0192(5) 0.0190(3) 0.0248(3) -0.0003(7) 0.0050(10) -0.0008(5) Br1 0.039(4) 0.030(3) 0.033(3) 0.001(2) 0.007(2) 0.015(3) Cs1 0.0361(9) 0.0329(5) 0.0269(5) 0.000(2) 0.0059(17) 0.0060(8) Br2 0.025(2) 0.028(2) 0.031(3) 0.0055(17) -0.0002(16) -0.010(2) Br3 0.029(3) 0.032(3) 0.037(3) -0.002(2) 0.0084(18) -0.015(3) Br4 0.0322(18) 0.042(3) 0.0260(12) -0.0018(13) 0.0054(13) -0.0008(14) Br5 0.0373(16) 0.0350(9) 0.0207(8) 0.001(4) 0.0004(18) 0.0016(16) Br6 0.027(2) 0.025(2) 0.045(3) 0.0032(18) 0.013(2) 0.011(2) Br7 0.035(2) 0.050(3) 0.0422(15) -0.0026(15) 0.0114(14) -0.0024(15) N2 0.029(13) 0.041(14) 0.035(11) 0.010(9) -0.004(9) 0.008(9) C5 0.027(11) 0.055(14) 0.036(11) 0.004(10) 0.001(9) 0.015(10) C6 0.031(12) 0.059(13) 0.027(9) 0.004(11) 0.004(8) 0.010(12) C7 0.045(13) 0.072(15) 0.040(12) 0.000(12) 0.005(11) 0.007(12) C8 0.06(2) 0.11(2) 0.041(18) 0.007(17) 0.004(15) 0.005(19) C1 0.046(13) 0.068(16) 0.038(11) 0.010(11) 0.005(11) -0.008(12) N1 0.057(18) 0.052(16) 0.023(10) 0.005(9) -0.001(10) 0.007(11) C2 0.048(12) 0.075(17) 0.025(9) 0.011(11) 0.003(11) -0.002(14) C3 0.055(15) 0.087(17) 0.041(12) 0.018(12) 0.006(12) 0.006(14) C4 0.07(2) 0.11(2) 0.034(17) 0.015(16) 0.020(15) 0.019(19) 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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' 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 Br1 Ag1 Br2 91.1(2) 1_465 1_565 ? Br1 Ag1 Br3 87.2(2) 1_465 1_455 ? Br1 Ag1 Br6 163.1(3) 1_465 . ? Br2 Ag1 Br3 162.5(3) 1_565 1_455 ? Br2 Ag1 Br6 86.5(2) 1_565 . ? Br3 Ag1 Br6 90.1(2) 1_455 . ? Br7 Ag1 Br1 105.9(2) . 1_465 ? Br7 Ag1 Br2 100.98(18) . 1_565 ? Br7 Ag1 Br3 96.2(2) . 1_455 ? Br7 Ag1 Br6 90.94(19) . . ? Br1 Bi1 Br2 91.51(16) . . ? Br1 Bi1 Br4 89.60(18) . . ? Br2 Bi1 Br4 86.12(15) . . ? Br3 Bi1 Br1 89.6(2) . . ? Br3 Bi1 Br2 177.5(2) . . ? Br3 Bi1 Br4 96.11(19) . . ? Br3 Bi1 Br6 90.16(16) . . ? Br5 Bi1 Br1 89.31(19) . . ? Br5 Bi1 Br2 88.37(17) . . ? Br5 Bi1 Br3 89.4(2) . . ? Br5 Bi1 Br4 174.35(16) . . ? Br5 Bi1 Br6 88.80(18) . . ? Br6 Bi1 Br1 178.1(3) . . ? Br6 Bi1 Br2 88.7(2) . . ? Br6 Bi1 Br4 92.30(17) . . ? Ag1 Br1 Bi1 172.0(3) 1_645 . ? Ag1 Br1 Cs1 97.63(19) 1_645 2_545 ? Ag1 Br1 Cs1 91.36(19) 1_645 1_655 ? Bi1 Br1 Cs1 89.85(17) . 2_545 ? Bi1 Br1 Cs1 85.97(17) . 1_655 ? Cs1 Br1 Cs1 88.50(16) 2_545 1_655 ? Br1 Cs1 Br1 121.06(11) 2 1_455 ? Br1 Cs1 Br2 63.32(10) 2 2 ? Br1 Cs1 Br3 58.91(13) 2 2_545 ? Br1 Cs1 Br3 94.92(9) 2 1_455 ? Br1 Cs1 Br5 120.21(10) 1_455 . ? Br1 Cs1 Br5 117.42(11) 2 2_545 ? Br1 Cs1 Br5 61.35(10) 2 2 ? Br1 Cs1 Br5 118.49(11) 2 . ? Br1 Cs1 Br6 119.95(17) 2 . ? Br2 Cs1 Br1 174.87(16) . 2 ? Br2 Cs1 Br1 61.69(11) . 1_455 ? Br2 Cs1 Br1 175.47(14) 2 1_455 ? Br2 Cs1 Br2 114.04(10) . 2 ? Br2 Cs1 Br3 118.07(16) . 2_545 ? Br2 Cs1 Br3 95.42(14) 2 2_545 ? Br2 Cs1 Br3 90.21(15) . 1_455 ? Br2 Cs1 Br5 121.68(10) . 1_455 ? Br2 Cs1 Br5 59.69(10) . 2_545 ? Br2 Cs1 Br5 122.56(9) 2 2_545 ? Br2 Cs1 Br5 55.56(10) 2 . ? Br2 Cs1 Br5 121.80(10) . 2 ? Br2 Cs1 Br5 58.53(10) . . ? Br2 Cs1 Br6 62.67(13) . . ? Br2 Cs1 Br6 80.22(8) 2 . ? Br2 Cs1 Br6 85.87(8) . 2_545 ? Br3 Cs1 Br1 59.99(12) 1_455 1_455 ? Br3 Cs1 Br1 88.20(9) 2_545 1_455 ? Br3 Cs1 Br2 119.80(15) 1_455 2 ? Br3 Cs1 Br3 121.22(11) 1_455 2_545 ? Br3 Cs1 Br5 117.32(10) 1_455 2_545 ? Br3 Cs1 Br5 119.79(10) 1_455 . ? Br3 Cs1 Br5 118.91(10) 2_545 . ? Br3 Cs1 Br5 60.21(9) 1_455 2 ? Br3 Cs1 Br6 63.04(10) 1_455 . ? Br5 Cs1 Br1 61.15(10) 1_455 2 ? Br5 Cs1 Br1 60.01(10) 1_455 1_455 ? Br5 Cs1 Br1 57.34(10) 2_545 1_455 ? Br5 Cs1 Br1 120.09(10) 2 1_455 ? Br5 Cs1 Br2 124.27(10) 1_455 2 ? Br5 Cs1 Br2 60.21(9) 2 2 ? Br5 Cs1 Br3 58.51(9) 2_545 2_545 ? Br5 Cs1 Br3 61.91(10) 1_455 1_455 ? Br5 Cs1 Br3 120.13(10) 2 2_545 ? Br5 Cs1 Br3 59.37(10) 1_455 2_545 ? Br5 Cs1 Br5 88.96(9) 1_455 2 ? Br5 Cs1 Br5 92.30(9) 2 . ? Br5 Cs1 Br5 87.67(9) 1_455 2_545 ? Br5 Cs1 Br5 178.26(12) 1_455 . ? Br5 Cs1 Br5 176.55(11) 2 2_545 ? Br5 Cs1 Br5 91.09(9) 2_545 . ? Br5 Cs1 Br6 124.72(10) 1_455 . ? Br5 Cs1 Br6 59.31(10) 2 . ? Br6 Cs1 Br1 89.01(15) 2_545 2 ? Br6 Cs1 Br1 118.28(18) 2_545 1_455 ? Br6 Cs1 Br1 96.07(14) . 1_455 ? Br6 Cs1 Br2 61.61(13) 2_545 2 ? Br6 Cs1 Br3 176.04(16) 2_545 1_455 ? Br6 Cs1 Br3 175.25(15) . 2_545 ? Br6 Cs1 Br3 61.47(10) 2_545 2_545 ? Br6 Cs1 Br5 61.00(10) 2_545 2_545 ? Br6 Cs1 Br5 122.35(10) . 2_545 ? Br6 Cs1 Br5 57.44(10) 2_545 . ? Br6 Cs1 Br5 57.02(9) . . ? Br6 Cs1 Br5 121.63(11) 2_545 2 ? Br6 Cs1 Br5 120.84(10) 2_545 1_455 ? Br6 Cs1 Br6 114.40(10) 2_545 . ? Ag1 Br2 Bi1 162.2(3) 1_545 . ? Ag1 Br2 Cs1 98.00(18) 1_545 2_545 ? Ag1 Br2 Cs1 99.52(17) 1_545 . ? Bi1 Br2 Cs1 96.24(16) . . ? Bi1 Br2 Cs1 88.02(16) . 2_545 ? Cs1 Br2 Cs1 97.30(16) . 2_545 ? Ag1 Br3 Cs1 95.12(19) 1_655 1_655 ? Ag1 Br3 Cs1 91.41(17) 1_655 2 ? Bi1 Br3 Ag1 174.0(3) . 1_655 ? Bi1 Br3 Cs1 90.60(18) . 1_655 ? Bi1 Br3 Cs1 87.05(18) . 2 ? Cs1 Br3 Cs1 88.36(17) 1_655 2 ? Ag1 Br5 Cs1 91.21(13) 2_545 2_545 ? Ag1 Br5 Cs1 87.33(9) 2_545 . ? Ag1 Br5 Cs1 93.87(10) 2_545 1_655 ? Ag1 Br5 Cs1 89.32(12) 2_545 2 ? Bi1 Br5 Ag1 172.80(13) . 2_545 ? Bi1 Br5 Cs1 89.42(11) . 2 ? Bi1 Br5 Cs1 93.24(9) . 1_655 ? Bi1 Br5 Cs1 85.54(8) . . ? Bi1 Br5 Cs1 89.63(12) . 2_545 ? Cs1 Br5 Cs1 178.26(12) 1_655 . ? Cs1 Br5 Cs1 176.55(11) 2_545 2 ? Cs1 Br5 Cs1 92.36(10) 1_655 2_545 ? Cs1 Br5 Cs1 91.01(10) 1_655 2 ? Cs1 Br5 Cs1 87.74(8) 2 . ? Cs1 Br5 Cs1 88.87(9) 2_545 . ? Ag1 Br6 Cs1 93.37(16) . . ? Ag1 Br6 Cs1 100.96(18) . 2 ? Bi1 Br6 Ag1 163.7(3) . . ? Bi1 Br6 Cs1 91.65(17) . . ? Bi1 Br6 Cs1 93.89(16) . 2 ? Cs1 Br6 Cs1 96.60(16) 2 . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C5 N2 H2A 109.5 . . ? C5 N2 H2B 109.5 . . ? C5 N2 H2C 109.5 . . ? N2 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C6 C5 N2 113(2) . . ? C6 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? C5 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C5 C6 C7 112(3) . . ? H6A C6 H6B 107.9 . . ? C7 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C6 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? C6 C7 C8 115(3) . . ? H7A C7 H7B 107.5 . . ? C8 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H1A C1 H1B 108.0 . . ? N1 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? N1 C1 C2 112(2) . . ? C2 C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1D 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C1 C2 H2D 109.7 . . ? C1 C2 H2E 109.7 . . ? H2D C2 H2E 108.2 . . ? C3 C2 C1 110(3) . . ? C3 C2 H2D 109.7 . . ? C3 C2 H2E 109.7 . . ? C2 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C4 C3 C2 116(3) . . ? C4 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 Ag1 Br1 2.793(7) 1_465 ? Ag1 Br2 2.831(7) 1_565 ? Ag1 Br3 2.869(8) 1_455 ? Ag1 Br6 2.907(7) . ? Ag1 Br7 2.713(3) . ? Bi1 Br1 2.845(6) . ? Bi1 Br2 2.857(6) . ? Bi1 Br3 2.826(6) . ? Bi1 Br4 2.947(3) . ? Bi1 Br5 2.783(3) . ? Bi1 Br6 2.834(6) . ? Br1 Cs1 3.848(7) 2_545 ? Br1 Cs1 4.103(8) 1_655 ? Cs1 Br2 3.932(7) 2 ? Cs1 Br2 3.702(6) . ? Cs1 Br3 4.081(7) 2_545 ? Cs1 Br3 3.882(7) 1_455 ? Cs1 Br5 3.788(3) 1_455 ? Cs1 Br5 4.274(3) . ? Cs1 Br5 3.904(5) 2 ? Cs1 Br5 3.992(5) 2_545 ? Cs1 Br6 3.936(7) . ? Cs1 Br6 3.740(7) 2_545 ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N2 C5 1.48(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.45(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.47(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.53(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 N1 1.47(2) . ? C1 C2 1.54(3) . ? N1 H1C 0.9100 . ? N1 H1D 0.9100 . ? N1 H1E 0.9100 . ? C2 H2D 0.9900 . ? C2 H2E 0.9900 . ? C2 C3 1.53(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.47(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 N2 C5 C6 C7 176(3) . . . . ? C5 C6 C7 C8 179(3) . . . . ? C1 C2 C3 C4 -174(3) . . . . ? N1 C1 C2 C3 -180(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.526(2) 2 0.474(2)