#------------------------------------------------------------------------------ #$Date: 2020-04-21 04:55:24 +0300 (Tue, 21 Apr 2020) $ #$Revision: 250972 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240348.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_7240348 loop_ _publ_author_name 'Rani, Jyoti' 'Grover, Vratta' 'Dhamija, Swati' 'Titi, Hatem M.' 'Patra, Ranjan' _publ_section_title ; Computational insight into the halogen bonded self-assembly of hexa-coordinated metalloporphyrins ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/D0CP00351D _journal_year 2020 _chemical_formula_sum 'C58 H32 Br2 I4 N4 O4 Sn' _chemical_formula_weight 1634.98 _chemical_name_common 4-bromobenzoate-tin-tetraiodoporphrin _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc24cj35 _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2020-01-13 deposited with the CCDC. 2020-04-17 downloaded from the CCDC. ; _cell_angle_alpha 99.763(7) _cell_angle_beta 100.739(5) _cell_angle_gamma 96.909(5) _cell_formula_units_Z 1 _cell_length_a 8.8174(5) _cell_length_b 10.8226(8) _cell_length_c 15.2360(12) _cell_measurement_reflns_used 6334 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.265 _cell_measurement_theta_min 3.657 _cell_volume 1390.35(18) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 18793 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.448 _diffrn_reflns_theta_min 3.199 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 4.166 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.59871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 772 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.141 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.136 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5938 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0575 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+5.6300P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1512 _refine_ls_wR_factor_ref 0.1669 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3838 _reflns_number_total 5938 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cp00351d2.cif _cod_data_source_block s2 _cod_original_cell_volume 1390.35(17) _cod_database_code 7240348 _shelx_shelxl_version_number 2017/1 _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_res_file ; TITL rpm-z23_a.res in P-1 s2.res created by SHELXL-2017/1 at 17:08:22 on 04-Jan-2020 CELL 0.71073 8.8174 10.8226 15.236 99.763 100.739 96.909 ZERR 1 0.0005 0.0008 0.0012 0.007 0.005 0.005 LATT 1 SFAC C H Br I N O Sn UNIT 58 32 2 4 4 4 1 SADI Br1 C26 Br1 C26a SADI Br2 C28 Br2 C28a SADI C23 C24 C23 C24a SADI C24 C25 C24a C25a SADI C24 C29 C24a C29a SADI C25 C26 C25a C26a SADI C26 C27 C26a C27a SADI C27 C28 C27a C28a SADI C28 C29 C28a C29a SADI 0.04 Br1 C25 Br1 C25a SADI 0.04 Br1 C27 Br1 C27a SADI 0.04 Br2 C27 Br2 C27a SADI 0.04 Br2 C29 Br2 C29a SADI 0.04 C23 C25 C23 C25a SADI 0.04 C23 C29 C23 C29a SADI 0.04 C24 C26 C24a C26a SADI 0.04 C24 C28 C24a C28a SADI 0.04 C25 C27 C25a C27a SADI 0.04 C25 C29 C25a C29a SADI 0.04 C26 C28 C26a C28a SADI 0.04 C27 C29 C27a C29a EADP C24 > C29 EADP C24 > C29A L.S. 20 PLAN 5 FMAP 2 ACTA BOND $H MERG 2 OMIT 2 1 2 OMIT 5 -1 1 OMIT 0 1 2 OMIT -1 -2 1 WGHT 0.068700 5.630000 FVAR 0.62536 0.69969 0.38398 SN1 7 1.000000 0.500000 0.500000 10.50000 0.02762 0.04315 = 0.04627 -0.01298 0.00213 0.00936 PART 1 BR1 3 1.222935 0.393447 0.106281 21.00000 0.08556 0.12299 = 0.08454 -0.02429 0.03017 0.02719 PART 0 PART 2 BR2 3 1.082357 0.919404 0.091352 -21.00000 0.20967 0.15119 = 0.11008 0.07882 0.04824 0.05492 PART 0 I1 4 0.406261 0.190628 -0.125573 11.00000 0.12693 0.14064 = 0.06058 -0.02512 -0.02333 0.04968 I2 4 0.233466 1.056907 0.626601 11.00000 0.05066 0.06529 = 0.06869 -0.00604 0.01513 0.02719 O1 6 1.124081 0.604697 0.426938 11.00000 0.03613 0.05387 = 0.05914 0.00552 0.00935 0.00825 O2 6 1.021473 0.780386 0.415487 11.00000 0.07773 0.06668 = 0.08733 -0.00350 0.02215 0.03672 N1 5 1.000131 0.347863 0.392913 11.00000 0.03376 0.04132 = 0.04099 -0.01432 0.00518 0.00687 N2 5 0.789596 0.537468 0.429866 11.00000 0.03364 0.03467 = 0.05247 -0.01699 -0.00104 0.00796 C1 1 1.122405 0.283310 0.386653 11.00000 0.03425 0.04730 = 0.04747 -0.01570 0.00399 0.00725 C2 1 1.092809 0.212268 0.295332 11.00000 0.05609 0.05777 = 0.05954 -0.02478 0.00142 0.02254 AFIX 43 H2 2 1.155772 0.157472 0.272243 11.00000 -1.20000 AFIX 0 C3 1 0.959313 0.237660 0.248455 11.00000 0.05212 0.05722 = 0.05515 -0.01761 0.00383 0.02386 AFIX 43 H3 2 0.912763 0.204189 0.187723 11.00000 -1.20000 AFIX 0 C4 1 0.903296 0.325825 0.310071 11.00000 0.03957 0.05143 = 0.04784 -0.01117 0.00024 0.01428 C5 1 0.770044 0.382988 0.285785 11.00000 0.03625 0.04389 = 0.05221 -0.00757 -0.00218 0.00680 C6 1 0.716928 0.478561 0.340818 11.00000 0.03374 0.04977 = 0.05263 -0.00138 0.00376 0.01125 C7 1 0.581075 0.533623 0.316273 11.00000 0.03511 0.06058 = 0.06144 -0.00865 -0.00176 0.01542 AFIX 43 H7 2 0.510252 0.511856 0.260576 11.00000 -1.20000 AFIX 0 C8 1 0.572394 0.622894 0.387594 11.00000 0.03268 0.06083 = 0.05379 -0.00814 0.00066 0.01426 AFIX 43 H8 2 0.494196 0.673188 0.389487 11.00000 -1.20000 AFIX 0 C9 1 0.705207 0.627583 0.460947 11.00000 0.02962 0.04299 = 0.05662 -0.00670 -0.00135 0.00985 C10 1 0.740752 0.708372 0.545099 11.00000 0.02814 0.04316 = 0.05435 -0.01107 0.00487 0.00564 C11 1 0.678966 0.340357 0.190374 11.00000 0.05087 0.05229 = 0.04778 -0.01465 -0.00455 0.01814 C12 1 0.586501 0.218922 0.162814 11.00000 0.07395 0.05765 = 0.05708 -0.01078 -0.01100 0.00178 AFIX 43 H12 2 0.579049 0.166831 0.204997 11.00000 -1.20000 AFIX 0 C13 1 0.507236 0.177336 0.073574 11.00000 0.09912 0.07879 = 0.07231 -0.01073 -0.01768 0.01440 AFIX 43 H13 2 0.447012 0.097126 0.055511 11.00000 -1.20000 AFIX 0 C14 1 0.517448 0.254720 0.011378 11.00000 0.09678 0.09847 = 0.04826 -0.00589 0.00153 0.04375 C15 1 0.604142 0.372966 0.037422 11.00000 0.07841 0.08142 = 0.05185 -0.00560 0.00493 0.02682 AFIX 43 H15 2 0.609321 0.425204 -0.004857 11.00000 -1.20000 AFIX 0 C16 1 0.685694 0.415931 0.128165 11.00000 0.06206 0.07164 = 0.05649 0.00221 0.00960 0.01718 AFIX 43 H16 2 0.744652 0.496667 0.145705 11.00000 -1.20000 AFIX 0 C17 1 0.628401 0.794014 0.568457 11.00000 0.03625 0.05257 = 0.04311 -0.00490 0.00537 0.01580 C18 1 0.472975 0.741115 0.561420 11.00000 0.03638 0.04784 = 0.06276 -0.00991 0.01182 0.00602 AFIX 43 H18 2 0.442440 0.653680 0.544218 11.00000 -1.20000 AFIX 0 C19 1 0.364600 0.818638 0.580005 11.00000 0.03588 0.06052 = 0.06373 -0.00281 0.01062 0.01120 AFIX 43 H19 2 0.260935 0.782681 0.573634 11.00000 -1.20000 AFIX 0 C20 1 0.406563 0.946188 0.607365 11.00000 0.03454 0.05479 = 0.05560 0.00165 0.01005 0.01777 C21 1 0.561697 0.999455 0.617862 11.00000 0.05082 0.04142 = 0.06231 -0.00896 0.00689 0.01203 AFIX 43 H21 2 0.592992 1.086259 0.639171 11.00000 -1.20000 AFIX 0 C22 1 0.670111 0.922269 0.596330 11.00000 0.03282 0.05045 = 0.05347 -0.00706 0.00850 0.00519 AFIX 43 H22 2 0.773031 0.958810 0.601027 11.00000 -1.20000 AFIX 0 C23 1 1.078960 0.692160 0.384195 11.00000 0.03865 0.06188 = 0.05378 -0.00716 0.00239 0.00965 PART 1 C24 1 1.100847 0.676290 0.286653 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 C25 1 1.161756 0.576004 0.251247 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 AFIX 43 H25 2 1.209076 0.526424 0.289163 31.00000 -1.20000 AFIX 0 C26 1 1.153979 0.546430 0.157907 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 C27 1 1.083959 0.619951 0.097994 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 AFIX 43 H27 2 1.084280 0.603031 0.036117 31.00000 -1.20000 AFIX 0 C28 1 1.014759 0.718573 0.136094 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 AFIX 43 H28 2 0.959743 0.764839 0.098580 31.00000 -1.20000 AFIX 0 C29 1 1.026968 0.748987 0.230236 31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 AFIX 43 H29 2 0.985351 0.818352 0.255257 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C28A 1 1.093382 0.759467 0.151428 -31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 C29A 1 1.080113 0.773763 0.242618 -31.00000 0.05473 0.14265 = 0.08594 0.03301 0.01454 0.04612 AFIX 43 H29A 2 1.059527 0.849823 0.273187 -31.00000 -1.20000 AFIX 0 C24A 1 1.098159 0.672686 0.286606 -31.00000 0.03907 0.04729 = 0.05257 -0.00444 -0.00053 0.00611 C27A 1 1.136589 0.649250 0.108230 -31.00000 0.06360 0.20642 = 0.09070 0.01498 0.01209 0.04173 AFIX 43 H27A 2 1.153885 0.641144 0.049291 -31.00000 -1.20000 AFIX 0 C26A 1 1.153245 0.549971 0.157253 -31.00000 0.06618 0.11674 = 0.07953 -0.04630 0.01100 0.01404 AFIX 43 H26A 2 1.172244 0.472560 0.127867 -31.00000 -1.20000 AFIX 0 C25A 1 1.141952 0.565064 0.248332 -31.00000 0.03184 0.06609 = 0.06720 -0.01924 0.01108 0.00172 AFIX 43 H25A 2 1.164047 0.502556 0.281666 -31.00000 -1.20000 AFIX 0 HKLF 4 REM rpm-z23_a.res in P-1 REM R1 = 0.0575 for 3838 Fo > 4sig(Fo) and 0.0941 for all 5938 data REM 354 parameters refined using 15 restraints END WGHT 0.0693 5.7140 REM Highest difference peak 1.141, deepest hole -0.962, 1-sigma level 0.136 Q1 1 0.2821 1.1336 0.5935 11.00000 0.05 1.14 Q2 1 0.9929 0.5795 0.4744 11.00000 0.05 1.04 Q3 1 0.2862 1.0395 0.6876 11.00000 0.05 1.00 Q4 1 1.1237 0.9758 -0.0014 11.00000 0.05 0.98 Q5 1 0.2971 0.1166 -0.0971 11.00000 0.05 0.77 ; _shelx_res_checksum 33868 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Sn1 Sn 1.000000 0.500000 0.500000 0.0421(2) Uani 1 2 d S . P . . Br1 Br 1.2229(2) 0.39345(19) 0.10628(13) 0.1005(8) Uani 0.700(4) 1 d . . P A 1 Br2 Br 1.0824(9) 0.9194(6) 0.0914(4) 0.146(3) Uani 0.300(4) 1 d . . P A 2 I1 I 0.40626(12) 0.19063(10) -0.12557(6) 0.1181(4) Uani 1 1 d . . . . . I2 I 0.23347(6) 1.05691(6) 0.62660(4) 0.0620(2) Uani 1 1 d . . . . . O1 O 1.1241(6) 0.6047(5) 0.4269(4) 0.0504(13) Uani 1 1 d . . . . . O2 O 1.0215(8) 0.7804(6) 0.4155(5) 0.0767(19) Uani 1 1 d . . . . . N1 N 1.0001(6) 0.3479(5) 0.3929(4) 0.0417(14) Uani 1 1 d . . . . . N2 N 0.7896(6) 0.5375(5) 0.4299(4) 0.0445(15) Uani 1 1 d . . . . . C1 C 1.1224(8) 0.2833(7) 0.3867(5) 0.0466(19) Uani 1 1 d . . . . . C2 C 1.0928(10) 0.2123(8) 0.2953(6) 0.062(2) Uani 1 1 d . . . . . H2 H 1.155772 0.157472 0.272243 0.075 Uiso 1 1 calc R U . . . C3 C 0.9593(9) 0.2377(8) 0.2485(6) 0.058(2) Uani 1 1 d . . . . . H3 H 0.912763 0.204189 0.187723 0.070 Uiso 1 1 calc R U . . . C4 C 0.9033(8) 0.3258(7) 0.3101(5) 0.049(2) Uani 1 1 d . . . . . C5 C 0.7700(8) 0.3830(7) 0.2858(6) 0.0477(19) Uani 1 1 d . . . . . C6 C 0.7169(8) 0.4786(7) 0.3408(6) 0.0471(19) Uani 1 1 d . . . . . C7 C 0.5811(9) 0.5336(8) 0.3163(6) 0.056(2) Uani 1 1 d . . . . . H7 H 0.510252 0.511856 0.260576 0.067 Uiso 1 1 calc R U . . . C8 C 0.5724(8) 0.6229(8) 0.3876(6) 0.052(2) Uani 1 1 d . . . . . H8 H 0.494196 0.673188 0.389487 0.062 Uiso 1 1 calc R U . . . C9 C 0.7052(8) 0.6276(7) 0.4609(6) 0.0461(19) Uani 1 1 d . . . . . C10 C 0.7408(8) 0.7084(7) 0.5451(5) 0.0449(18) Uani 1 1 d . . . . . C11 C 0.6790(9) 0.3404(8) 0.1904(6) 0.054(2) Uani 1 1 d . . . . . C12 C 0.5865(11) 0.2189(9) 0.1628(7) 0.070(3) Uani 1 1 d . . . . . H12 H 0.579049 0.166831 0.204997 0.083 Uiso 1 1 calc R U . . . C13 C 0.5072(14) 0.1773(12) 0.0736(8) 0.091(4) Uani 1 1 d . . . . . H13 H 0.447012 0.097126 0.055511 0.109 Uiso 1 1 calc R U . . . C14 C 0.5174(14) 0.2547(12) 0.0114(7) 0.083(3) Uani 1 1 d . . . . . C15 C 0.6041(12) 0.3730(11) 0.0374(7) 0.073(3) Uani 1 1 d . . . . . H15 H 0.609321 0.425204 -0.004857 0.087 Uiso 1 1 calc R U . . . C16 C 0.6857(11) 0.4159(10) 0.1282(7) 0.064(2) Uani 1 1 d . . . . . H16 H 0.744652 0.496667 0.145705 0.077 Uiso 1 1 calc R U . . . C17 C 0.6284(8) 0.7940(7) 0.5685(5) 0.0454(19) Uani 1 1 d . . . . . C18 C 0.4730(8) 0.7411(8) 0.5614(6) 0.051(2) Uani 1 1 d . . . . . H18 H 0.442440 0.653680 0.544218 0.062 Uiso 1 1 calc R U . . . C19 C 0.3646(9) 0.8186(8) 0.5800(6) 0.055(2) Uani 1 1 d . . . . . H19 H 0.260935 0.782681 0.573634 0.066 Uiso 1 1 calc R U . . . C20 C 0.4066(8) 0.9462(8) 0.6074(6) 0.0484(19) Uani 1 1 d . . . . . C21 C 0.5617(9) 0.9995(8) 0.6179(6) 0.054(2) Uani 1 1 d . . . . . H21 H 0.592992 1.086259 0.639171 0.065 Uiso 1 1 calc R U . . . C22 C 0.6701(8) 0.9223(7) 0.5963(5) 0.0479(19) Uani 1 1 d . . . . . H22 H 0.773031 0.958810 0.601027 0.057 Uiso 1 1 calc R U . . . C23 C 1.0790(9) 0.6922(8) 0.3842(6) 0.054(2) Uani 1 1 d D . . . . C24 C 1.101(8) 0.676(5) 0.2867(19) 0.091(4) Uani 0.38(3) 1 d D . P A 1 C25 C 1.162(7) 0.576(4) 0.251(2) 0.091(4) Uani 0.38(3) 1 d D . P A 1 H25 H 1.209076 0.526424 0.289163 0.109 Uiso 0.38(3) 1 calc R U P A 1 C26 C 1.154(10) 0.546(6) 0.158(2) 0.091(4) Uani 0.38(3) 1 d D . P A 1 C27 C 1.084(5) 0.620(4) 0.098(2) 0.091(4) Uani 0.38(3) 1 d D . P A 1 H27 H 1.084280 0.603031 0.036117 0.109 Uiso 0.38(3) 1 calc R U P A 1 C28 C 1.015(4) 0.719(4) 0.1361(18) 0.091(4) Uani 0.38(3) 1 d D . P A 1 H28 H 0.959743 0.764839 0.098580 0.109 Uiso 0.38(3) 1 calc R U P A 1 C29 C 1.027(4) 0.749(4) 0.2302(18) 0.091(4) Uani 0.38(3) 1 d D . P A 1 H29 H 0.985351 0.818352 0.255257 0.109 Uiso 0.38(3) 1 calc R U P A 1 C28A C 1.093(3) 0.759(3) 0.1514(14) 0.091(4) Uani 0.62(3) 1 d D . P A 2 C29A C 1.080(3) 0.774(2) 0.2426(13) 0.091(4) Uani 0.62(3) 1 d D . P A 2 H29A H 1.059527 0.849823 0.273187 0.109 Uiso 0.62(3) 1 calc R U P A 2 C24A C 1.098(4) 0.6727(18) 0.2866(9) 0.049(4) Uani 0.62(3) 1 d D . P A 2 C27A C 1.137(3) 0.649(3) 0.1082(16) 0.121(11) Uani 0.62(3) 1 d D . P A 2 H27A H 1.153885 0.641144 0.049291 0.145 Uiso 0.62(3) 1 calc R U P A 2 C26A C 1.153(7) 0.550(3) 0.1573(15) 0.096(7) Uani 0.62(3) 1 d D . P A 2 H26A H 1.172244 0.472560 0.127867 0.115 Uiso 0.62(3) 1 calc R U P A 2 C25A C 1.142(3) 0.5651(17) 0.2483(11) 0.059(5) Uani 0.62(3) 1 d D . P A 2 H25A H 1.164047 0.502556 0.281666 0.071 Uiso 0.62(3) 1 calc R 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 0.0276(3) 0.0431(4) 0.0463(4) -0.0130(3) 0.0021(3) 0.0094(3) Br1 0.0856(12) 0.1230(16) 0.0845(13) -0.0243(10) 0.0302(9) 0.0272(10) Br2 0.210(7) 0.151(5) 0.110(4) 0.079(4) 0.048(4) 0.055(5) I1 0.1269(7) 0.1406(8) 0.0606(5) -0.0251(5) -0.0233(5) 0.0497(6) I2 0.0507(3) 0.0653(4) 0.0687(4) -0.0060(3) 0.0151(3) 0.0272(3) O1 0.036(3) 0.054(3) 0.059(4) 0.006(3) 0.009(2) 0.008(2) O2 0.078(4) 0.067(4) 0.087(5) -0.003(4) 0.022(4) 0.037(4) N1 0.034(3) 0.041(3) 0.041(4) -0.014(3) 0.005(3) 0.007(2) N2 0.034(3) 0.035(3) 0.052(4) -0.017(3) -0.001(3) 0.008(2) C1 0.034(4) 0.047(4) 0.047(5) -0.016(4) 0.004(3) 0.007(3) C2 0.056(5) 0.058(5) 0.060(6) -0.025(4) 0.001(4) 0.023(4) C3 0.052(5) 0.057(5) 0.055(5) -0.018(4) 0.004(4) 0.024(4) C4 0.040(4) 0.051(5) 0.048(5) -0.011(4) 0.000(3) 0.014(3) C5 0.036(4) 0.044(4) 0.052(5) -0.008(4) -0.002(3) 0.007(3) C6 0.034(4) 0.050(5) 0.053(5) -0.001(4) 0.004(3) 0.011(3) C7 0.035(4) 0.061(5) 0.061(5) -0.009(4) -0.002(4) 0.015(4) C8 0.033(4) 0.061(5) 0.054(5) -0.008(4) 0.001(3) 0.014(3) C9 0.030(3) 0.043(4) 0.057(5) -0.007(4) -0.001(3) 0.010(3) C10 0.028(3) 0.043(4) 0.054(5) -0.011(4) 0.005(3) 0.006(3) C11 0.051(4) 0.052(5) 0.048(5) -0.015(4) -0.005(4) 0.018(4) C12 0.074(6) 0.058(6) 0.057(6) -0.011(5) -0.011(5) 0.002(5) C13 0.099(8) 0.079(7) 0.072(8) -0.011(6) -0.018(6) 0.014(6) C14 0.097(8) 0.098(9) 0.048(6) -0.006(6) 0.002(5) 0.044(7) C15 0.078(6) 0.081(7) 0.052(6) -0.006(5) 0.005(5) 0.027(6) C16 0.062(5) 0.072(6) 0.056(6) 0.002(5) 0.010(4) 0.017(5) C17 0.036(4) 0.053(5) 0.043(4) -0.005(4) 0.005(3) 0.016(3) C18 0.036(4) 0.048(5) 0.063(5) -0.010(4) 0.012(4) 0.006(3) C19 0.036(4) 0.061(5) 0.064(6) -0.003(4) 0.011(4) 0.011(4) C20 0.035(4) 0.055(5) 0.056(5) 0.002(4) 0.010(3) 0.018(3) C21 0.051(4) 0.041(4) 0.062(6) -0.009(4) 0.007(4) 0.012(4) C22 0.033(4) 0.050(5) 0.053(5) -0.007(4) 0.009(3) 0.005(3) C23 0.039(4) 0.062(5) 0.054(5) -0.007(4) 0.002(4) 0.010(4) C24 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C25 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C26 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C27 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C28 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C29 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C28A 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C29A 0.055(9) 0.143(11) 0.086(7) 0.033(8) 0.015(7) 0.046(9) C24A 0.039(7) 0.047(8) 0.053(8) -0.004(7) -0.001(6) 0.006(6) C27A 0.064(17) 0.21(3) 0.091(17) 0.015(19) 0.012(12) 0.042(19) C26A 0.066(13) 0.117(17) 0.080(14) -0.046(12) 0.011(10) 0.014(12) C25A 0.032(9) 0.066(10) 0.067(10) -0.019(8) 0.011(7) 0.002(7) 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' I I -0.4742 1.8119 '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' 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 O1 Sn1 O1 180.0 . 2_766 ? O1 Sn1 N2 90.9(2) . . ? O1 Sn1 N2 89.1(2) 2_766 . ? O1 Sn1 N2 89.1(2) . 2_766 ? O1 Sn1 N2 90.9(2) 2_766 2_766 ? N2 Sn1 N2 180.0(3) . 2_766 ? O1 Sn1 N1 83.4(2) . . ? O1 Sn1 N1 96.6(2) 2_766 . ? N2 Sn1 N1 90.6(2) . . ? N2 Sn1 N1 89.4(2) 2_766 . ? O1 Sn1 N1 96.6(2) . 2_766 ? O1 Sn1 N1 83.4(2) 2_766 2_766 ? N2 Sn1 N1 89.4(2) . 2_766 ? N2 Sn1 N1 90.6(2) 2_766 2_766 ? N1 Sn1 N1 180.0 . 2_766 ? C23 O1 Sn1 127.7(5) . . ? C4 N1 C1 108.7(6) . . ? C4 N1 Sn1 124.2(5) . . ? C1 N1 Sn1 124.5(5) . . ? C9 N2 C6 109.1(6) . . ? C9 N2 Sn1 126.1(5) . . ? C6 N2 Sn1 124.6(4) . . ? N1 C1 C10 127.0(6) . 2_766 ? N1 C1 C2 106.8(6) . . ? C10 C1 C2 126.0(6) 2_766 . ? C3 C2 C1 108.9(7) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? C2 C3 C4 106.3(7) . . ? C2 C3 H3 126.8 . . ? C4 C3 H3 126.8 . . ? N1 C4 C5 126.5(7) . . ? N1 C4 C3 109.2(6) . . ? C5 C4 C3 124.2(7) . . ? C6 C5 C4 127.0(7) . . ? C6 C5 C11 116.4(6) . . ? C4 C5 C11 116.6(6) . . ? N2 C6 C5 125.8(6) . . ? N2 C6 C7 107.6(6) . . ? C5 C6 C7 126.5(7) . . ? C8 C7 C6 108.1(7) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 108.7(7) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? N2 C9 C10 126.8(6) . . ? N2 C9 C8 106.5(6) . . ? C10 C9 C8 126.7(6) . . ? C9 C10 C1 125.4(6) . 2_766 ? C9 C10 C17 118.7(6) . . ? C1 C10 C17 115.9(6) 2_766 . ? C16 C11 C12 118.9(8) . . ? C16 C11 C5 120.8(8) . . ? C12 C11 C5 120.2(9) . . ? C13 C12 C11 120.2(10) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 119.9(11) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.5(10) . . ? C15 C14 I1 119.0(9) . . ? C13 C14 I1 120.5(9) . . ? C14 C15 C16 120.0(11) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.4(10) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C22 C17 C18 118.4(6) . . ? C22 C17 C10 122.9(6) . . ? C18 C17 C10 118.7(7) . . ? C19 C18 C17 120.1(7) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 121.3(7) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.3(7) . . ? C19 C20 I2 118.7(5) . . ? C21 C20 I2 122.0(6) . . ? C20 C21 C22 119.6(7) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C17 C22 C21 121.3(7) . . ? C17 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? O2 C23 O1 125.3(9) . . ? O2 C23 C24A 120.6(10) . . ? O1 C23 C24A 114.0(8) . . ? O2 C23 C24 119.7(14) . . ? O1 C23 C24 115.0(13) . . ? C25 C24 C29 120(2) . . ? C25 C24 C23 120(2) . . ? C29 C24 C23 119(2) . . ? C24 C25 C26 120(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 122(2) . . ? C25 C26 Br1 119.7(18) . . ? C27 C26 Br1 118(2) . . ? C28 C27 C26 117(2) . . ? C28 C27 H27 121.6 . . ? C26 C27 H27 121.6 . . ? C27 C28 C29 121(2) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120(2) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C27A C28A C29A 120.3(16) . . ? C27A C28A Br2 121.7(16) . . ? C29A C28A Br2 117.3(15) . . ? C24A C29A C28A 118.9(15) . . ? C24A C29A H29A 120.5 . . ? C28A C29A H29A 120.5 . . ? C25A C24A C29A 122.9(14) . . ? C25A C24A C23 120.2(12) . . ? C29A C24A C23 116.7(12) . . ? C28A C27A C26A 117.6(17) . . ? C28A C27A H27A 121.2 . . ? C26A C27A H27A 121.2 . . ? C25A C26A C27A 121.8(15) . . ? C25A C26A H26A 119.1 . . ? C27A C26A H26A 119.1 . . ? C24A C25A C26A 118.0(14) . . ? C24A C25A H25A 121.0 . . ? C26A C25A H25A 121.0 . . ? 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 O1 2.074(6) . ? Sn1 O1 2.074(6) 2_766 ? Sn1 N2 2.083(6) . ? Sn1 N2 2.083(6) 2_766 ? Sn1 N1 2.113(5) . ? Sn1 N1 2.113(5) 2_766 ? Br1 C26 1.93(3) . ? Br2 C28A 2.09(2) . ? I1 C14 2.093(10) . ? I2 C20 2.083(7) . ? O1 C23 1.297(10) . ? O2 C23 1.203(9) . ? N1 C4 1.351(9) . ? N1 C1 1.363(9) . ? N2 C9 1.371(8) . ? N2 C6 1.394(10) . ? C1 C10 1.421(10) 2_766 ? C1 C2 1.431(11) . ? C2 C3 1.342(11) . ? C2 H2 0.9300 . ? C3 C4 1.421(10) . ? C3 H3 0.9300 . ? C4 C5 1.411(10) . ? C5 C6 1.400(10) . ? C5 C11 1.490(11) . ? C6 C7 1.418(10) . ? C7 C8 1.346(11) . ? C7 H7 0.9300 . ? C8 C9 1.450(10) . ? C8 H8 0.9300 . ? C9 C10 1.382(10) . ? C10 C17 1.486(9) . ? C11 C16 1.358(13) . ? C11 C12 1.413(12) . ? C12 C13 1.379(14) . ? C12 H12 0.9300 . ? C13 C14 1.375(16) . ? C13 H13 0.9300 . ? C14 C15 1.363(15) . ? C15 C16 1.406(13) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.364(10) . ? C17 C18 1.398(10) . ? C18 C19 1.382(10) . ? C18 H18 0.9300 . ? C19 C20 1.357(11) . ? C19 H19 0.9300 . ? C20 C21 1.388(11) . ? C21 C22 1.391(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24A 1.510(14) . ? C23 C24 1.518(18) . ? C24 C25 1.344(18) . ? C24 C29 1.39(2) . ? C25 C26 1.39(2) . ? C25 H25 0.9300 . ? C26 C27 1.41(2) . ? C27 C28 1.39(2) . ? C27 H27 0.9300 . ? C28 C29 1.40(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C28A C27A 1.39(2) . ? C28A C29A 1.400(19) . ? C29A C24A 1.386(18) . ? C29A H29A 0.9300 . ? C24A C25A 1.344(14) . ? C27A C26A 1.42(2) . ? C27A H27A 0.9300 . ? C26A C25A 1.393(19) . ? C26A H26A 0.9300 . ? C25A H25A 0.9300 . ?