#------------------------------------------------------------------------------ #$Date: 2021-10-13 03:24:40 +0300 (Wed, 13 Oct 2021) $ #$Revision: 269907 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061014.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_7061014 loop_ _publ_author_name 'Liu, Yao' 'Li, Yu-Kong' 'Ying, Ting-Ting' 'Tan, Yu-Hui' 'Tang, Yun Zhi' 'Han, Ding-Chong' 'Du, Peng-Kang' 'Zhang, Hao' _publ_section_title ; Multisequential reversible phase transition materials with Semiconducting and fluorescence properties：(C8H18BrN)2SnBr6 ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ04448F _journal_year 2021 _chemical_formula_moiety 'Br6 Sn, 2(C8 H18 Br N)' _chemical_formula_sum 'C16 H36 Br8 N2 Sn' _chemical_formula_weight 1014.44 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2021-10-02 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-10-06 deposited with the CCDC. 2021-10-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.855(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.4401(14) _cell_length_b 14.7764(13) _cell_length_c 13.9147(12) _cell_measurement_reflns_used 7294 _cell_measurement_temperature 300 _cell_measurement_theta_max 27.451 _cell_measurement_theta_min 2.821 _cell_volume 2968.7(5) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_temperature 300 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16738 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.822 _exptl_absorpt_coefficient_mu 11.636 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.3055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1421 before and 0.0930 after correction. The Ratio of minimum to maximum transmission is 0.4097. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'metallic light colourless' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.270 _exptl_crystal_description block _exptl_crystal_F_000 1904 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.180 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.185 _refine_ls_extinction_coef 0.00116(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 2625 _refine_ls_number_restraints 112 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0610 _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^)+120.9526P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.1331 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1735 _reflns_number_total 2625 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04448f2.cif _cod_data_source_block 1_LTP _cod_database_code 7061014 _shelx_shelxl_version_number 2018/3 _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 0.204 _shelx_estimated_absorpt_t_min 0.128 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C7A-C8B 1.5 with sigma of 0.02 N2-C7A = N2-C6A = N2-C6B 1.51 with sigma of 0.02 C8B-C7B 1.5 with sigma of 0.02 N2-C6A \\sim N2-C6B \\sim N2-C6B_$1 \\sim N2-C6A_$1 \\sim N2-C7A \\sim N2-C7A_$1 with sigma of 0.01 C5B-C6B \\sim C5A-C6A with sigma of 0.01 Br5B-C5B \\sim Br5A-C5A with sigma of 0.01 Sn1-Br5 \\sim Sn1-Br4 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C5B \\sim C6A \\sim C6B \\sim C7A \\sim C8B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C8A \\sim C7B \\sim C8B \\sim C7A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Br4 \\sim Br5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Br5B \\sim Br5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: Br3(0.5) Br4(0.94) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) Br5A(0.25) C6A(0.5) H6AA(0.5) H6AB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) Br5B(0.25) C7B(0.5) H7BA(0.5) H7BB(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) Br5(0.06) 5.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B), C7A(H7AA,H7AB), C6A(H6AA,H6AB), C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB) 5.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C8B(H8BA,H8BB,H8BC), C8A(H8AA,H8AB,H8AC) ; _shelx_res_file ; TITL a in C2/c #15 1.res created by SHELXL-2018/3 at 19:37:36 on 02-Oct-2021 REM reset to C2/c #15 CELL 0.71073 14.4401 14.7764 13.9147 90 90.855 90 ZERR 4 0.0014 0.0013 0.0012 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Br N Sn UNIT 64 144 32 8 4 EQIV $1 1-X,+Y,1.5-Z EQIV $2 1-X,1-Y,1-Z EQIV $3 0.5+X,-0.5+Y,+Z EQIV $4 1.5-X,0.5-Y,1-Z SADI 0.01 N2 C6A N2 C6B N2 C6B_$1 N2 C6A_$1 N2 C7A N2 C7A_$1 SADI 0.01 C5B C6B C5A C6A ISOR 0.01 0.02 C6B C6A C5A C5B SIMU 0.01 0.02 2 C5B C6A C6B C7A C8B DFIX 1.5 C7A C8B SADI 0.01 Br5B C5B Br5A C5A DFIX 1.51 N2 C7A N2 C6A N2 C6B DFIX 1.5 C8B C7B SIMU 0.01 0.02 2 C8A C7B C8B C7A SADI 0.01 Sn1 Br5 Sn1 Br4 SIMU 0.01 0.02 2 Br4 Br5 SIMU 0.01 0.02 2 Br5B Br5A L.S. 20 0 0 PLAN 10 SIZE 0.3 0.3 0.2 CONF FREE C6A C6A_$1 BIND C6B N2 FREE C6B C6B_$1 FREE C7A C6B_$1 FREE C7A C6A_$1 FREE C7A C7A_$1 FREE Br5A Br3_$2 FREE Br5A Br3_$3 FREE Br5A Br3 FREE Br5A Br3_$4 FREE Br5B Br3_$2 FREE Br5B Br3_$3 FREE Br5B Br3 FREE Br5B Br3_$4 BOND MORE -1 BOND $H fmap 2 53 acta SHEL 999 0.84 REM REM REM WGHT 0.000000 120.952606 EXTI 0.001159 FVAR 0.05339 SN1 5 0.750000 0.250000 1.000000 10.50000 0.03064 0.03061 = 0.03294 0.00548 0.00154 -0.00199 BR2 3 0.579860 0.285218 1.043131 11.00000 0.03599 0.06219 = 0.07520 -0.00652 0.01130 0.00405 BR1 3 0.712415 0.077817 1.006420 11.00000 0.06370 0.03304 = 0.06918 0.00699 0.00180 -0.00916 BR3 3 0.826528 0.308223 0.583167 10.50000 0.06599 0.08284 = 0.06320 -0.01494 -0.00093 -0.02706 N1 4 1.000000 0.484289 0.750000 10.50000 0.03483 0.03928 = 0.03149 0.00000 0.00493 0.00000 C3 1 0.962784 0.427636 0.667506 11.00000 0.07059 0.04224 = 0.03943 0.00076 0.00802 0.00028 AFIX 23 H3A 2 0.935773 0.467883 0.619681 11.00000 -1.20000 H3B 2 1.014347 0.396790 0.637907 11.00000 -1.20000 AFIX 0 C2 1 1.077675 0.542483 0.712416 11.00000 0.04283 0.05614 = 0.04305 0.00913 0.00953 -0.01091 AFIX 23 H2A 2 1.106235 0.573796 0.766484 11.00000 -1.20000 H2B 2 1.124194 0.502896 0.685527 11.00000 -1.20000 AFIX 0 C1 1 1.051462 0.611772 0.637576 11.00000 0.09050 0.06697 = 0.07782 0.01981 0.01128 -0.03261 AFIX 137 H1A 2 1.023241 0.582051 0.583229 11.00000 -1.50000 H1B 2 1.105956 0.643355 0.617500 11.00000 -1.50000 H1C 2 1.008466 0.654115 0.664251 11.00000 -1.50000 AFIX 0 C4 1 0.892510 0.359217 0.693473 11.00000 0.11346 0.08688 = 0.05389 -0.01506 0.00741 -0.05365 AFIX 23 H4A 2 0.848014 0.386937 0.735927 11.00000 -1.20000 H4B 2 0.922838 0.310589 0.728619 11.00000 -1.20000 AFIX 0 PART 1 BR4 3 0.703021 0.251487 0.820417 10.94000 0.06373 0.05555 = 0.03589 0.00607 -0.00744 -0.00218 PART 0 N2 4 0.500000 0.479108 0.750000 10.50000 0.06110 0.05714 = 0.07395 0.00000 -0.01314 0.00000 PART 2 C8B 1 0.658696 0.559705 0.774780 10.50000 0.07876 0.12316 = 0.09597 -0.00628 -0.00930 -0.02773 AFIX 137 H8BA 2 0.628960 0.602207 0.732240 10.50000 -1.50000 H8BB 2 0.700148 0.522274 0.738954 10.50000 -1.50000 H8BC 2 0.692983 0.591864 0.823558 10.50000 -1.50000 AFIX 0 PART 1 C7A 1 0.556491 0.564744 0.759506 10.50000 0.07686 0.11829 = 0.09690 -0.00425 -0.01646 -0.02112 AFIX 23 H7AA 2 0.573237 0.583658 0.695312 10.50000 -1.20000 H7AB 2 0.516480 0.611294 0.785198 10.50000 -1.20000 AFIX 0 BR5A 3 0.663893 0.342324 0.526851 10.25000 0.08689 0.08710 = 0.10769 -0.03737 0.01953 -0.02821 C6A 1 0.524821 0.458753 0.647131 10.50000 0.09464 0.09243 = 0.09718 -0.00051 -0.00602 0.00001 AFIX 23 H6AA 2 0.468720 0.445719 0.610495 10.50000 -1.20000 H6AB 2 0.553549 0.511689 0.619099 10.50000 -1.20000 AFIX 0 C5A 1 0.588562 0.381266 0.640267 10.50000 0.11731 0.11463 = 0.11391 0.00285 -0.00287 0.00136 AFIX 23 H5AA 2 0.551939 0.328722 0.657079 10.50000 -1.20000 H5AB 2 0.633029 0.389340 0.692503 10.50000 -1.20000 AFIX 0 PART 2 C5B 1 0.591168 0.433528 0.602923 10.50000 0.08587 0.08467 = 0.09268 0.00226 -0.00293 0.00261 AFIX 23 H5BA 2 0.627839 0.487184 0.616339 10.50000 -1.20000 H5BB 2 0.543994 0.449850 0.555683 10.50000 -1.20000 AFIX 0 C6B 1 0.545224 0.405035 0.692297 10.50000 0.08723 0.08219 = 0.09145 0.00263 -0.00539 0.00289 AFIX 23 H6BA 2 0.590891 0.375241 0.733167 10.50000 -1.20000 H6BB 2 0.498318 0.360497 0.675640 10.50000 -1.20000 AFIX 0 BR5B 3 0.673864 0.338336 0.545950 10.25000 0.08524 0.09386 = 0.11894 -0.02272 0.00626 0.03224 C7B 1 0.586667 0.501410 0.821105 10.50000 0.07567 0.11538 = 0.09529 -0.00396 -0.01329 -0.02555 AFIX 23 H7BA 2 0.564063 0.531945 0.877834 10.50000 -1.20000 H7BB 2 0.615117 0.445040 0.841664 10.50000 -1.20000 AFIX 0 PART 1 C8A 1 0.637206 0.563269 0.815605 10.50000 0.08252 0.12916 = 0.10162 -0.00592 -0.00972 -0.02438 AFIX 137 H8AA 2 0.681521 0.523552 0.786854 10.50000 -1.50000 H8AB 2 0.623189 0.541996 0.878934 10.50000 -1.50000 H8AC 2 0.662524 0.623242 0.819683 10.50000 -1.50000 AFIX 0 PART 2 BR5 3 0.729536 0.219962 0.818386 10.06000 0.05388 0.04534 = 0.05544 0.01287 0.01681 -0.02874 HKLF 4 REM a in C2/c #15 REM wR2 = 0.1331, GooF = S = 1.031, Restrained GooF = 1.012 for all data REM R1 = 0.0610 for 1735 Fo > 4sig(Fo) and 0.1101 for all 2625 data REM 192 parameters refined using 112 restraints END WGHT 0.0000 120.9566 REM Highest difference peak 1.180, deepest hole -1.599, 1-sigma level 0.185 Q1 1 0.6989 0.2535 0.9535 11.00000 0.05 1.18 Q2 1 0.8046 0.1994 1.0028 11.00000 0.05 0.99 Q3 1 0.7571 0.2979 0.8400 11.00000 0.05 0.96 Q4 1 0.8092 0.2563 0.9529 11.00000 0.05 0.95 Q5 1 0.7750 0.2560 0.8625 11.00000 0.05 0.88 Q6 1 0.6580 0.1198 0.9870 11.00000 0.05 0.87 Q7 1 0.7503 0.0776 1.0606 11.00000 0.05 0.85 Q8 1 0.6394 0.0807 1.0551 11.00000 0.05 0.84 Q9 1 0.8059 0.2978 1.0122 11.00000 0.05 0.83 Q10 1 0.5210 0.2801 0.9932 11.00000 0.05 0.83 ; _shelx_res_checksum 58035 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Sn1 Sn 0.750000 0.250000 1.000000 0.0314(3) Uani 1 2 d DS . P . . Br2 Br 0.57986(9) 0.28522(10) 1.04313(11) 0.0577(5) Uani 1 1 d . . . . . Br1 Br 0.71242(10) 0.07782(8) 1.00642(11) 0.0553(4) Uani 1 1 d . . . . . Br3 Br 0.8265(2) 0.3082(2) 0.5832(2) 0.0707(9) Uani 0.5 1 d . . P . . N1 N 1.000000 0.4843(9) 0.750000 0.035(3) Uani 1 2 d S T P . . C3 C 0.9628(10) 0.4276(8) 0.6675(9) 0.051(3) Uani 1 1 d . . . . . H3A H 0.935773 0.467883 0.619681 0.061 Uiso 1 1 calc R U . . . H3B H 1.014347 0.396790 0.637907 0.061 Uiso 1 1 calc R U . . . C2 C 1.0777(8) 0.5425(9) 0.7124(9) 0.047(3) Uani 1 1 d . . . . . H2A H 1.106235 0.573796 0.766484 0.057 Uiso 1 1 calc R U . . . H2B H 1.124194 0.502896 0.685527 0.057 Uiso 1 1 calc R U . . . C1 C 1.0515(11) 0.6118(11) 0.6376(11) 0.078(5) Uani 1 1 d . . . . . H1A H 1.023241 0.582051 0.583229 0.117 Uiso 1 1 calc R U . . . H1B H 1.105956 0.643355 0.617500 0.117 Uiso 1 1 calc R U . . . H1C H 1.008466 0.654115 0.664251 0.117 Uiso 1 1 calc R U . . . C4 C 0.8925(13) 0.3592(12) 0.6935(11) 0.085(6) Uani 1 1 d . . . . . H4A H 0.848014 0.386937 0.735927 0.102 Uiso 1 1 calc R U . . . H4B H 0.922838 0.310589 0.728619 0.102 Uiso 1 1 calc R U . . . Br4 Br 0.70302(16) 0.25149(15) 0.82042(12) 0.0518(6) Uani 0.94 1 d D U P A 1 N2 N 0.500000 0.4791(11) 0.750000 0.064(5) Uani 1 2 d DS T P . . C8B C 0.659(3) 0.560(4) 0.775(3) 0.099(9) Uani 0.5 1 d D U P B 2 H8BA H 0.628960 0.602207 0.732240 0.149 Uiso 0.5 1 calc R U P B 2 H8BB H 0.700148 0.522274 0.738954 0.149 Uiso 0.5 1 calc R U P B 2 H8BC H 0.692983 0.591864 0.823558 0.149 Uiso 0.5 1 calc R U P B 2 C7A C 0.556(2) 0.5647(18) 0.760(3) 0.098(8) Uani 0.5 1 d D U P C 1 H7AA H 0.573237 0.583658 0.695312 0.117 Uiso 0.5 1 calc R U P C 1 H7AB H 0.516480 0.611294 0.785198 0.117 Uiso 0.5 1 calc R U P C 1 Br5A Br 0.6639(18) 0.3423(17) 0.527(3) 0.094(6) Uani 0.25 1 d D U P C 1 C6A C 0.525(3) 0.459(2) 0.6471(11) 0.095(7) Uani 0.5 1 d D U P C 1 H6AA H 0.468720 0.445719 0.610495 0.114 Uiso 0.5 1 calc R U P C 1 H6AB H 0.553549 0.511689 0.619099 0.114 Uiso 0.5 1 calc R U P C 1 C5A C 0.589(3) 0.381(3) 0.640(3) 0.115(15) Uani 0.5 1 d D U P C 1 H5AA H 0.551939 0.328722 0.657079 0.138 Uiso 0.5 1 calc R U P C 1 H5AB H 0.633029 0.389340 0.692503 0.138 Uiso 0.5 1 calc R U P C 1 C5B C 0.591(2) 0.434(2) 0.603(2) 0.088(7) Uani 0.5 1 d D U P C 2 H5BA H 0.627839 0.487184 0.616339 0.105 Uiso 0.5 1 calc R U P C 2 H5BB H 0.543994 0.449850 0.555683 0.105 Uiso 0.5 1 calc R U P C 2 C6B C 0.545(2) 0.4050(17) 0.692(2) 0.087(7) Uani 0.5 1 d D U P C 2 H6BA H 0.590891 0.375241 0.733167 0.104 Uiso 0.5 1 calc R U P C 2 H6BB H 0.498318 0.360497 0.675640 0.104 Uiso 0.5 1 calc R U P C 2 Br5B Br 0.6739(19) 0.3383(18) 0.546(3) 0.099(7) Uani 0.25 1 d D U P C 2 C7B C 0.587(2) 0.501(3) 0.821(3) 0.096(8) Uani 0.5 1 d D U P B 2 H7BA H 0.564063 0.531945 0.877834 0.115 Uiso 0.5 1 calc R U P B 2 H7BB H 0.615117 0.445040 0.841664 0.115 Uiso 0.5 1 calc R U P B 2 C8A C 0.637(3) 0.563(4) 0.816(4) 0.105(9) Uani 0.5 1 d . U P C 1 H8AA H 0.681521 0.523552 0.786854 0.157 Uiso 0.5 1 calc R U P C 1 H8AB H 0.623189 0.541996 0.878934 0.157 Uiso 0.5 1 calc R U P C 1 H8AC H 0.662524 0.623242 0.819683 0.157 Uiso 0.5 1 calc R U P C 1 Br5 Br 0.730(3) 0.220(2) 0.8184(8) 0.051(8) Uani 0.06 1 d D U P A 2 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 Sn1 0.0306(6) 0.0306(6) 0.0329(6) 0.0055(5) 0.0015(5) -0.0020(5) Br2 0.0360(7) 0.0622(9) 0.0752(10) -0.0065(8) 0.0113(7) 0.0040(6) Br1 0.0637(9) 0.0330(7) 0.0692(10) 0.0070(7) 0.0018(7) -0.0092(6) Br3 0.066(2) 0.083(2) 0.063(2) -0.0149(17) -0.0009(16) -0.0271(17) N1 0.035(8) 0.039(8) 0.031(8) 0.000 0.005(6) 0.000 C3 0.071(10) 0.042(7) 0.039(7) 0.001(6) 0.008(7) 0.000(7) C2 0.043(7) 0.056(8) 0.043(8) 0.009(6) 0.010(6) -0.011(6) C1 0.091(13) 0.067(10) 0.078(12) 0.020(9) 0.011(10) -0.033(9) C4 0.113(15) 0.087(12) 0.054(10) -0.015(9) 0.007(10) -0.054(11) Br4 0.0637(14) 0.0556(14) 0.0359(9) 0.0061(8) -0.0074(7) -0.0022(9) N2 0.061(11) 0.057(11) 0.074(12) 0.000 -0.013(9) 0.000 C8B 0.079(17) 0.123(18) 0.10(2) -0.006(18) -0.009(16) -0.028(15) C7A 0.077(16) 0.118(18) 0.10(2) -0.004(16) -0.016(14) -0.021(14) Br5A 0.087(9) 0.087(9) 0.108(12) -0.037(8) 0.020(9) -0.028(9) C6A 0.095(9) 0.092(9) 0.097(9) -0.001(7) -0.006(7) 0.000(7) C5A 0.117(17) 0.115(17) 0.114(17) 0.003(10) -0.003(10) 0.001(10) C5B 0.086(9) 0.085(9) 0.093(9) 0.002(7) -0.003(7) 0.003(7) C6B 0.087(9) 0.082(9) 0.091(9) 0.003(7) -0.005(7) 0.003(7) Br5B 0.085(8) 0.094(8) 0.119(14) -0.023(8) 0.006(8) 0.032(7) C7B 0.076(16) 0.115(18) 0.10(2) -0.004(16) -0.013(14) -0.026(14) C8A 0.083(18) 0.129(18) 0.10(2) -0.006(18) -0.010(16) -0.024(15) Br5 0.054(15) 0.045(15) 0.055(13) 0.013(11) 0.017(11) -0.029(13) 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' Br Br -0.2901 2.4595 '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' Sn Sn -0.6537 1.4246 '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 Br2 Sn1 Br2 180.0 . 7_657 ? Br2 Sn1 Br1 90.61(5) 7_657 . ? Br2 Sn1 Br1 90.61(5) . 7_657 ? Br2 Sn1 Br1 89.39(5) 7_657 7_657 ? Br2 Sn1 Br1 89.40(5) . . ? Br1 Sn1 Br1 180.0 . 7_657 ? Br4 Sn1 Br2 89.20(6) . . ? Br4 Sn1 Br2 89.20(6) 7_657 7_657 ? Br4 Sn1 Br2 90.80(6) 7_657 . ? Br4 Sn1 Br2 90.80(6) . 7_657 ? Br4 Sn1 Br1 89.41(6) . . ? Br4 Sn1 Br1 89.41(6) 7_657 7_657 ? Br4 Sn1 Br1 90.60(6) 7_657 . ? Br4 Sn1 Br1 90.59(6) . 7_657 ? Br4 Sn1 Br4 180.0 . 7_657 ? Br5 Sn1 Br2 80.4(8) 7_657 . ? Br5 Sn1 Br2 99.6(8) . . ? Br5 Sn1 Br1 98.9(7) 7_657 . ? Br5 Sn1 Br1 81.1(7) . . ? Br5 Sn1 Br5 180.0 7_657 . ? C4 Br3 Br5A 137.4(10) . 7_656 ? C3 N1 C3 112.8(13) 2_756 . ? C2 N1 C3 108.0(7) . . ? C2 N1 C3 108.7(7) . 2_756 ? C2 N1 C3 108.7(7) 2_756 . ? C2 N1 C3 108.0(7) 2_756 2_756 ? C2 N1 C2 110.7(13) 2_756 . ? N1 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C4 C3 N1 115.4(10) . . ? C4 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? N1 C2 H2A 108.2 . . ? N1 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C1 C2 N1 116.5(10) . . ? C1 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Br3 C4 H4A 108.8 . . ? Br3 C4 H4B 108.8 . . ? C3 C4 Br3 113.6(10) . . ? C3 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C7A N2 C7A 66(3) . 2_656 ? C7A N2 C6A 103(2) . 2_656 ? C7A N2 C6A 97(2) 2_656 2_656 ? C7A N2 C6A 97(2) . . ? C7A N2 C6A 103(2) 2_656 . ? C7A N2 C6B 115(2) 2_656 2_656 ? C7A N2 C6B 143(2) . 2_656 ? C7A N2 C7B 107(2) . 2_656 ? C7A N2 C7B 50.5(18) 2_656 2_656 ? C6A N2 C6A 157(3) . 2_656 ? C6A N2 C6B 118(2) . 2_656 ? C6A N2 C6B 40.7(18) 2_656 2_656 ? C6A N2 C7B 115(2) 2_656 2_656 ? C6A N2 C7B 69.7(18) . 2_656 ? C6B N2 C7B 98(2) . . ? C6B N2 C7B 99.2(19) 2_656 . ? C7B N2 C7B 156(3) 2_656 . ? H8BA C8B H8BB 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? C7B C8B H8BA 109.5 . . ? C7B C8B H8BB 109.5 . . ? C7B C8B H8BC 109.5 . . ? N2 C7A H7AA 107.6 . . ? N2 C7A H7AB 107.6 . . ? H7AA C7A H7AB 107.0 . . ? C8A C7A N2 119(3) . . ? C8A C7A H7AA 107.6 . . ? C8A C7A H7AB 107.6 . . ? N2 C6A H6AA 109.2 . . ? N2 C6A H6AB 109.2 . . ? H6AA C6A H6AB 107.9 . . ? C5A C6A N2 112(2) . . ? C5A C6A H6AA 109.2 . . ? C5A C6A H6AB 109.2 . . ? Br5A C5A H5AA 105.3 . . ? Br5A C5A H5AB 105.3 . . ? C6A C5A Br5A 128(3) . . ? C6A C5A H5AA 105.3 . . ? C6A C5A H5AB 105.3 . . ? H5AA C5A H5AB 106.0 . . ? H5BA C5B H5BB 107.6 . . ? C6B C5B H5BA 108.7 . . ? C6B C5B H5BB 108.7 . . ? C6B C5B Br5B 114(2) . . ? Br5B C5B H5BA 108.7 . . ? Br5B C5B H5BB 108.7 . . ? N2 C6B H6BA 108.2 . . ? N2 C6B H6BB 108.2 . . ? C5B C6B N2 116(2) . . ? C5B C6B H6BA 108.2 . . ? C5B C6B H6BB 108.2 . . ? H6BA C6B H6BB 107.4 . . ? N2 C7B H7BA 109.0 . . ? N2 C7B H7BB 109.0 . . ? C8B C7B N2 113(3) . . ? C8B C7B H7BA 109.0 . . ? C8B C7B H7BB 109.0 . . ? H7BA C7B H7BB 107.8 . . ? C7A C8A H8AA 109.5 . . ? C7A C8A H8AB 109.5 . . ? C7A C8A H8AC 109.5 . . ? H8AA C8A H8AB 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 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 Sn1 Br2 2.5906(13) . ? Sn1 Br2 2.5906(13) 7_657 ? Sn1 Br1 2.6033(13) 7_657 ? Sn1 Br1 2.6033(12) . ? Sn1 Br4 2.5796(15) 7_657 ? Sn1 Br4 2.5796(15) . ? Sn1 Br5 2.578(10) . ? Sn1 Br5 2.578(10) 7_657 ? Br3 C4 1.946(15) . ? Br3 Br5A 2.71(2) 7_656 ? N1 C3 1.513(14) 2_756 ? N1 C3 1.513(14) . ? N1 C2 1.513(13) 2_756 ? N1 C2 1.513(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.481(18) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C1 1.505(18) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N2 C7A 1.510(11) 2_656 ? N2 C7A 1.510(11) . ? N2 C6A 1.511(11) . ? N2 C6A 1.511(11) 2_656 ? N2 C6B 1.512(11) . ? N2 C6B 1.512(11) 2_656 ? N2 C7B 1.62(3) 2_656 ? N2 C7B 1.62(3) . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C8B C7B 1.50(2) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C7A C8A 1.39(6) . ? Br5A C5A 2.01(3) . ? C6A H6AA 0.9700 . ? C6A H6AB 0.9700 . ? C6A C5A 1.47(3) . ? C5A H5AA 0.9700 . ? C5A H5AB 0.9700 . ? C5B H5BA 0.9700 . ? C5B H5BB 0.9700 . ? C5B C6B 1.48(3) . ? C5B Br5B 2.02(3) . ? C6B H6BA 0.9700 . ? C6B H6BB 0.9700 . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C8A H8AA 0.9600 . ? C8A H8AB 0.9600 . ? C8A H8AC 0.9600 . ? 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 N1 C3 C4 Br3 166.5(10) . . . . ? C3 N1 C3 C4 53.7(11) 2_756 . . . ? C3 N1 C2 C1 64.3(15) . . . . ? C3 N1 C2 C1 -173.0(12) 2_756 . . . ? C2 N1 C3 C4 173.8(13) . . . . ? C2 N1 C3 C4 -66.0(15) 2_756 . . . ? C2 N1 C2 C1 -54.6(11) 2_756 . . . ? N2 C6A C5A Br5A -166(3) . . . . ? C7A N2 C7A C8A 151(6) 2_656 . . . ? C7A N2 C6A C5A 174(3) 2_656 . . . ? C7A N2 C6A C5A 107(3) . . . . ? C6A N2 C7A C8A -108(4) . . . . ? C6A N2 C7A C8A 60(4) 2_656 . . . ? C6A N2 C6A C5A -39(3) 2_656 . . . ? C6B N2 C6B C5B 168(4) 2_656 . . . ? C6B N2 C7B C8B 168(4) 2_656 . . . ? C6B N2 C7B C8B 79(4) . . . . ? Br5B C5B C6B N2 167(2) . . . . ? C7B N2 C6B C5B 71(3) 2_656 . . . ? C7B N2 C6B C5B -93(3) . . . . ? C7B N2 C7B C8B -57(3) 2_656 . . . ?