#------------------------------------------------------------------------------ #$Date: 2019-04-23 01:23:18 +0300 (Tue, 23 Apr 2019) $ #$Revision: 214716 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/09/1550915.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_1550915 loop_ _publ_author_name 'Dehnen, Stefanie Susanne' 'Peters, Bertram' 'Santner, Silke' 'Donsbach, Carsten' 'Smarsly, Bernd' 'Voepel, Pascal' _publ_section_title ; Ionic liquid cations as methylation agent for extremely weak chalcogenido metalate nucleophiles ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC01358J _journal_year 2019 _chemical_formula_moiety 'C4 H12 O4 S20 Sn10, 2(C9 H17 N2), 2(B0.5 F2), C5 H6 N2, 0.5(C6 H7 N2), 0.5(C6 H8 N2), 0.5(C5 H8 N2), 0.25(C3 N2)' _chemical_formula_sum 'C36.25 H63.5 B F4 N9.5 O4 S20 Sn10' _chemical_formula_weight 2611.37 _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' _space_group_name_H-M_alt 'P b c m' _symmetry_space_group_name_Hall '-P 2c 2b' _symmetry_space_group_name_H-M 'P b c m' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-02-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-03-13 deposited with the CCDC. 2019-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.727(4) _cell_length_b 35.611(7) _cell_length_c 31.733(6) _cell_measurement_reflns_used 679 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.76 _cell_measurement_theta_min 1.15 _cell_volume 20032(7) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDS-2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_unetI/netI 0.1135 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 152311 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 1.283 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.904 _exptl_absorpt_correction_T_max 0.8333 _exptl_absorpt_correction_T_min 0.4361 _exptl_absorpt_correction_type sphere _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.732 _exptl_crystal_description plank _exptl_crystal_F_000 9924 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_size_rad 0.0914 _refine_diff_density_max 1.749 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.159 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.645 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 640 _refine_ls_number_reflns 20058 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 0.645 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_gt 0.0500 _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^)+(0.0791P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1279 _refine_ls_wR_factor_ref 0.1463 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5781 _reflns_number_total 20058 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc01358j2.cif _cod_data_source_block bpp-1_pl_sq _cod_original_formula_sum 'C36.25 H63.50 B F4 N9.50 O4 S20 Sn10' _cod_database_code 1550915 _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 0.823 _shelx_estimated_absorpt_t_min 0.430 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances F04A-B05E 1.4 with sigma of 0.02 B05E-F04F 1.4 with sigma of 0.02 F03T-B05E 1.4 with sigma of 0.02 C9E-N2E 1.47 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(CI) = Uanis(CIII) = Uanis(CII) = Uanis(CIV) Uanis(C7) = Uanis(C6) Uanis(C5A) = Uanis(C6A) Uanis(C2) = Uanis(C3) 4. Others Fixed Sof: H9BB(0.5) H9BC(0.5) H8BB(0.5) H8BC(0.5) H9DA(0.5) H9DB(0.5) H9DC(0.5) H8DB(0.5) H8DC(0.5) H8CB(0.5) H8CC(0.5) H9CB(0.5) H9CC(0.5) C1F(0.25) N1F(0.25) C3F(0.25) C2F(0.25) N2F(0.25) 5.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C4A(H4AA,H4AB) 5.b Me refined with riding coordinates: CIV(HIVA,HIVB,HIVC), C8E(H8EA,H8EB,H8EC), C9E(H9EA,H9EB,H9EC), C9B(H9BA,H9BB, H9BC), C8B(H8BA,H8BB,H8BC), C8D(H8DA,H8DB,H8DC), C8C(H8CA,H8CB,H8CC), C9C(H9CA, H9CB,H9CC) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C2(H2), C2A(H2A), C3A(H3A), C3B(H3B), C3D(H3D), C2D(H2D), C2C(H2C), C3C(H3C) 5.d Fitted pentagon refined as free rotating group: C1F(N1F,C3F,C2F,N2F), N1E(C1E,N2E,C2E,C3E) 5.e Idealised Me refined as rotating group: CIII(HIIA,HIIB,HIIC), CII(HIID,HIIE,HIIF), CI(HIA,HIB,HIC), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC), C9D(H9DA,H9DB,H9DC) ; _shelx_res_file ; TITL bpp-1_a.res in P-1 New: Pbcm bpp-1_pl_sq.res created by SHELXL-2016/6 at 16:02:21 on 11-Feb-2019 CELL 0.71073 17.727 35.611 31.733 90 90 90 ZERR 8 0.004 0.007 0.006 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM +X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H B F N O S Sn UNIT 290 508 8 32 76 32 160 80 DFIX 1.4 F04A B05E DFIX 1.4 B05E F04F DFIX 1.4 F03T B05E DFIX 1.47 C9E N2E EADP CI CIII CII CIV EADP C7 C6 EADP C5A C6A EADP C2 C3 L.S. 50 0 141 PLAN 99 SIZE 0.07 0.14 0.35 TEMP -173.15 CONF ABIN fmap 2 acta OMIT 0 52 REM REM REM WGHT 0.079100 FVAR 0.03607 SN9 8 0.255134 0.041662 0.020475 11.00000 0.07253 0.04083 = 0.03867 -0.00225 -0.00143 -0.00153 SN5 8 0.354241 0.128665 0.021723 11.00000 0.07070 0.04460 = 0.04064 -0.00493 0.01200 -0.00294 SN6 8 0.152136 0.069577 0.112327 11.00000 0.05808 0.04766 = 0.04181 0.00126 0.00104 -0.00456 SN7 8 0.152370 0.127538 0.019743 11.00000 0.06479 0.04736 = 0.04361 0.00271 -0.00361 0.00065 SN1 8 0.449224 0.158420 0.113900 11.00000 0.06235 0.05984 = 0.05524 -0.00866 0.00600 -0.00862 SN3 8 0.052133 0.155417 0.110382 11.00000 0.06188 0.06645 = 0.05736 0.00295 0.00356 0.00891 SN8 8 0.254646 -0.015298 0.111767 11.00000 0.08828 0.04423 = 0.04366 0.00085 -0.00373 -0.00223 SN4 8 0.353823 0.070861 0.113020 11.00000 0.05585 0.04637 = 0.04184 -0.00249 0.00078 0.00277 SN2 8 0.250395 0.157230 0.112688 11.00000 0.05843 0.04239 = 0.04003 -0.00345 0.00461 0.00054 SN10 8 0.258833 0.099615 -0.070841 11.00000 0.11480 0.04522 = 0.03917 -0.00051 0.00254 -0.00241 S15 7 0.393804 0.059179 0.035348 11.00000 0.06871 0.05106 = 0.04548 -0.00384 0.01019 0.00232 S2 7 0.350505 0.196201 0.143402 11.00000 0.07192 0.04463 = 0.04466 -0.00337 0.00397 -0.00153 S11 7 0.370157 0.007403 0.142648 11.00000 0.08302 0.05414 = 0.04203 0.00164 -0.00344 0.01552 S18 7 0.255681 -0.025756 0.036815 11.00000 0.10106 0.04015 = 0.04556 -0.00050 -0.00682 -0.00227 S6 7 0.250286 0.180327 0.034384 11.00000 0.07366 0.04082 = 0.04538 0.00019 0.00675 -0.00180 S13 7 0.374684 0.131571 -0.054612 11.00000 0.09942 0.05502 = 0.04192 -0.00213 0.02242 -0.00079 S12 7 0.140032 0.006627 0.143469 11.00000 0.07416 0.05092 = 0.04956 0.00349 -0.00180 -0.00965 S9 7 0.032363 0.094231 0.141184 11.00000 0.06247 0.07618 = 0.06026 0.00569 0.00845 -0.00880 S3 7 0.146147 0.194683 0.142953 11.00000 0.07414 0.05620 = 0.05017 -0.00509 0.01256 0.01367 S8 7 0.470079 0.164479 0.039111 11.00000 0.07494 0.06523 = 0.05651 -0.00955 0.01857 -0.01482 S10 7 0.033959 0.159657 0.035611 11.00000 0.06761 0.06227 = 0.06719 0.00451 -0.00866 0.00727 S14 7 0.142269 0.132128 -0.057572 11.00000 0.10418 0.05790 = 0.04687 0.00481 -0.01151 -0.00133 S20 7 0.281091 0.104299 -0.146461 11.00000 0.10128 0.07225 = 0.04425 -0.00709 0.00113 -0.00278 S4 7 -0.057556 0.189853 0.136523 11.00000 0.09646 0.11791 = 0.09761 0.00866 0.02922 0.04564 S5 7 0.251702 0.099433 0.163343 11.00000 0.05863 0.04389 = 0.03803 -0.00251 0.00277 -0.00016 S19 7 0.255510 0.033464 -0.056767 11.00000 0.09995 0.04744 = 0.03929 -0.00475 0.00500 0.00128 S16 7 0.112904 0.058045 0.033878 11.00000 0.06902 0.05702 = 0.04737 0.00069 -0.00735 -0.01223 S7 7 0.470252 0.097051 0.143138 11.00000 0.05294 0.06331 = 0.05740 -0.00735 -0.00460 0.00135 S17 7 0.247542 -0.079982 0.137685 11.00000 0.17420 0.05180 = 0.06782 0.00941 -0.01351 -0.00451 S1 7 0.555917 0.194152 0.142822 11.00000 0.07079 0.11304 = 0.10588 -0.04383 0.01178 -0.02953 O2 6 0.165111 0.123756 0.085636 11.00000 0.04529 0.04927 = 0.04301 -0.00180 -0.00774 -0.00363 O3 6 0.254447 0.050274 0.086465 11.00000 0.06171 0.03823 = 0.04732 -0.00186 0.01026 0.00149 O1 6 0.336868 0.124262 0.087712 11.00000 0.07532 0.03300 = 0.03829 0.00067 -0.00356 -0.00840 O4 6 0.253339 0.099496 0.008902 11.00000 0.07358 0.04334 = 0.03854 -0.00115 0.00926 -0.00099 CIII 1 0.308401 -0.100545 0.105150 11.00000 0.11069 0.14949 = 0.19419 -0.01760 -0.01339 -0.01887 AFIX 137 HIIA 2 0.281160 -0.110946 0.080944 11.00000 -1.50000 HIIB 2 0.334662 -0.120810 0.120027 11.00000 -1.50000 HIIC 2 0.345241 -0.081995 0.095307 11.00000 -1.50000 AFIX 0 CII 1 -0.131984 0.169213 0.104659 11.00000 0.11069 0.14949 = 0.19419 -0.01760 -0.01339 -0.01887 AFIX 137 HIID 2 -0.113258 0.164926 0.076003 11.00000 -1.50000 HIIE 2 -0.175228 0.186336 0.103708 11.00000 -1.50000 HIIF 2 -0.147597 0.145248 0.117084 11.00000 -1.50000 AFIX 0 CIV 1 0.221503 0.070599 -0.164215 11.00000 0.11069 0.14949 = 0.19419 -0.01760 -0.01339 -0.01887 AFIX 33 HIVA 2 0.224464 0.069229 -0.195015 11.00000 -1.50000 HIVB 2 0.235810 0.046307 -0.152103 11.00000 -1.50000 HIVC 2 0.169786 0.076779 -0.155790 11.00000 -1.50000 AFIX 0 CI 1 0.632274 0.165770 0.123000 11.00000 0.11069 0.14949 = 0.19419 -0.01760 -0.01339 -0.01887 AFIX 137 HIA 2 0.624025 0.160529 0.093035 11.00000 -1.50000 HIB 2 0.634289 0.142070 0.138657 11.00000 -1.50000 HIC 2 0.680019 0.179281 0.126532 11.00000 -1.50000 AFIX 0 N1 5 0.417301 -0.011695 -0.095796 11.00000 0.08738 0.09221 = 0.04772 0.01112 0.00525 0.03524 N2 5 0.445281 0.035354 -0.130326 11.00000 0.06832 0.10264 = 0.06028 0.00476 0.00089 0.01540 C1 1 0.454796 0.020065 -0.094536 11.00000 0.09011 0.07981 = 0.03256 0.00178 -0.00183 0.01347 C3 1 0.379160 -0.016414 -0.135023 11.00000 0.07953 0.14012 = 0.06123 0.00090 -0.00058 0.01481 AFIX 43 H3 2 0.348862 -0.036840 -0.144207 11.00000 -1.20000 AFIX 0 C8 1 0.501000 0.033202 -0.058783 11.00000 0.07133 0.08165 = 0.03946 -0.00006 0.00430 0.02017 AFIX 137 H8A 2 0.473753 0.052915 -0.043530 11.00000 -1.50000 H8B 2 0.548842 0.043274 -0.069350 11.00000 -1.50000 H8C 2 0.511092 0.012141 -0.039721 11.00000 -1.50000 AFIX 0 C2 1 0.396742 0.015068 -0.155559 11.00000 0.07953 0.14012 = 0.06123 0.00090 -0.00058 0.01481 AFIX 43 H2 2 0.379050 0.022226 -0.182652 11.00000 -1.20000 AFIX 0 C4 1 0.411910 -0.037918 -0.060437 11.00000 0.04547 0.13612 = 0.12954 0.02952 0.01609 0.01733 AFIX 23 H4A 2 0.404683 -0.023334 -0.034186 11.00000 -1.20000 H4B 2 0.460345 -0.051574 -0.057912 11.00000 -1.20000 AFIX 0 C5 1 0.346118 -0.067537 -0.064208 11.00000 0.10639 0.08359 = 0.11980 -0.01082 0.04071 0.01921 AFIX 23 H5A 2 0.296826 -0.054493 -0.063322 11.00000 -1.20000 H5B 2 0.349998 -0.080915 -0.091470 11.00000 -1.20000 AFIX 0 C6 1 0.351017 -0.095928 -0.027759 11.00000 0.14442 0.08907 = 0.15368 -0.00616 0.04134 0.02881 AFIX 23 H6A 2 0.395312 -0.112520 -0.031542 11.00000 -1.20000 H6B 2 0.356279 -0.082589 -0.000545 11.00000 -1.20000 AFIX 0 C7 1 0.279140 -0.118797 -0.028195 11.00000 0.14442 0.08907 = 0.15368 -0.00616 0.04134 0.02881 AFIX 137 H7A 2 0.272040 -0.129877 -0.056184 11.00000 -1.50000 H7B 2 0.236210 -0.102496 -0.021565 11.00000 -1.50000 H7C 2 0.282591 -0.138838 -0.007118 11.00000 -1.50000 AFIX 0 C9 1 0.479665 0.073332 -0.142403 11.00000 0.12151 0.13346 = 0.04745 0.02560 0.01858 0.03630 AFIX 137 H9A 2 0.461384 0.092722 -0.123013 11.00000 -1.50000 H9B 2 0.464830 0.079764 -0.171264 11.00000 -1.50000 H9C 2 0.534774 0.071802 -0.140658 11.00000 -1.50000 AFIX 0 F03T 4 0.192614 -0.000445 -0.250000 10.50000 0.07949 F04A 4 0.323371 0.018831 -0.250000 10.50000 0.13639 F04F 4 0.273160 -0.035673 -0.215092 11.00000 0.19053 F04T 4 0.377062 0.152134 -0.250000 10.50000 0.13898 F040 4 0.421962 0.095063 -0.250000 10.50000 0.11113 F049 4 0.489847 0.138116 -0.214925 11.00000 0.11771 B05E 3 0.269320 -0.011753 -0.250000 10.50000 0.07018 B40 3 0.450726 0.130214 -0.250000 10.50000 0.06639 N2A 5 0.108452 -0.020599 -0.127851 11.00000 0.08940 0.11973 = 0.06121 0.01701 -0.01163 -0.04258 N1A 5 0.036601 0.017719 -0.097590 11.00000 0.08911 0.09658 = 0.06380 0.01316 -0.00618 -0.03319 C9A 1 0.161105 -0.053301 -0.134885 11.00000 0.13286 0.16643 = 0.07961 -0.01441 0.00791 -0.01669 AFIX 137 H9AA 2 0.195125 -0.055746 -0.110697 11.00000 -1.50000 H9AB 2 0.190759 -0.048983 -0.160494 11.00000 -1.50000 H9AC 2 0.131626 -0.076412 -0.138031 11.00000 -1.50000 AFIX 0 C8A 1 0.091053 -0.034140 -0.051502 11.00000 0.08878 0.13477 = 0.07811 0.04972 -0.00305 -0.01037 AFIX 137 H8AA 2 0.134741 -0.050825 -0.054241 11.00000 -1.50000 H8AB 2 0.046136 -0.049027 -0.044792 11.00000 -1.50000 H8AC 2 0.100272 -0.015978 -0.028879 11.00000 -1.50000 AFIX 0 C2A 1 0.087119 0.003375 -0.158052 11.00000 0.11537 0.16413 = 0.05207 0.00853 0.03393 -0.05056 AFIX 43 H2A 2 0.101336 0.002582 -0.186903 11.00000 -1.20000 AFIX 0 C3A 1 0.042901 0.028122 -0.140194 11.00000 0.10715 0.19281 = 0.03929 0.04902 -0.00944 -0.03267 AFIX 43 H3A 2 0.019591 0.049046 -0.153434 11.00000 -1.20000 AFIX 0 C5A 1 -0.036772 0.073730 -0.077395 11.00000 0.11218 0.10290 = 0.10185 -0.00176 -0.01837 -0.03697 AFIX 23 H5AA 2 -0.072260 0.070988 -0.101286 11.00000 -1.20000 H5AB 2 0.007021 0.088408 -0.087569 11.00000 -1.20000 AFIX 0 C1A 1 0.078895 -0.013732 -0.091970 11.00000 0.04906 0.14304 = 0.06336 0.01431 0.01007 -0.01848 C6A 1 -0.076109 0.096195 -0.042371 11.00000 0.11218 0.10290 = 0.10185 -0.00176 -0.01837 -0.03697 AFIX 23 H6AA 2 -0.117724 0.080487 -0.031321 11.00000 -1.20000 H6AB 2 -0.039377 0.099417 -0.019151 11.00000 -1.20000 AFIX 0 C7A 1 -0.107645 0.133472 -0.052032 11.00000 0.08475 0.11173 = 0.16452 0.03090 -0.01069 -0.00992 AFIX 137 H7AA 2 -0.151486 0.130642 -0.070575 11.00000 -1.50000 H7AB 2 -0.069280 0.148789 -0.066138 11.00000 -1.50000 H7AC 2 -0.123156 0.145793 -0.025812 11.00000 -1.50000 AFIX 0 C4A 1 -0.010263 0.036109 -0.065043 11.00000 0.12810 0.09528 = 0.04762 0.00180 -0.01528 -0.02361 AFIX 23 H4AA 2 -0.054550 0.020040 -0.059040 11.00000 -1.20000 H4AB 2 0.019467 0.038255 -0.038743 11.00000 -1.20000 AFIX 0 C8E 1 0.376407 0.237400 -0.050167 11.00000 0.08387 AFIX 33 H8EA 2 0.322963 0.242447 -0.044662 11.00000 -1.50000 H8EB 2 0.396509 0.220989 -0.028066 11.00000 -1.50000 H8EC 2 0.404451 0.261115 -0.050336 11.00000 -1.50000 AFIX 0 C9E 1 0.532580 0.218477 -0.073090 11.00000 0.22560 AFIX 33 H9EA 2 0.577235 0.209802 -0.088474 11.00000 -1.50000 H9EB 2 0.537218 0.245420 -0.067357 11.00000 -1.50000 H9EC 2 0.528481 0.204774 -0.046407 11.00000 -1.50000 AFIX 0 N2B 5 0.412272 0.024881 0.250000 10.50000 0.08874 N1B 5 0.396377 -0.035062 0.250000 10.50000 0.11828 C9B 1 0.391242 0.065643 0.250000 10.50000 0.11513 PART -1 AFIX 33 H9BA 2 0.437141 0.080982 0.250000 10.50000 -1.50000 H9BB 2 0.361417 0.071300 0.224784 10.50000 -1.50000 H9BC 2 0.361417 0.071300 0.275216 10.50000 -1.50000 AFIX 0 PART 0 C1B 1 0.365554 -0.000596 0.250000 10.50000 0.07865 C2B 1 0.479667 0.011555 0.250000 10.50000 0.08180 C3B 1 0.471030 -0.027292 0.250000 10.50000 0.08851 AFIX 43 H3B 2 0.510697 -0.045230 0.250000 10.50000 -1.20000 AFIX 0 C4B 1 0.339287 -0.064168 0.250000 10.50000 0.21176 C8B 1 0.288196 0.013191 0.250000 10.50000 0.21113 PART -1 AFIX 33 H8BA 2 0.253278 -0.008144 0.250000 10.50000 -1.50000 H8BB 2 0.279631 0.028497 0.275216 10.50000 -1.50000 H8BC 2 0.279631 0.028497 0.224784 10.50000 -1.50000 AFIX 0 PART 0 N1D 5 0.409356 0.227193 0.250000 10.50000 0.12431 N2D 5 0.299198 0.204272 0.250000 10.50000 0.08539 C9D 1 0.231620 0.177154 0.250000 10.50000 0.11350 PART -1 AFIX 137 H9DA 2 0.239013 0.157972 0.228244 10.50000 -1.50000 H9DB 2 0.185236 0.191180 0.244120 10.50000 -1.50000 H9DC 2 0.227571 0.165037 0.277636 10.50000 -1.50000 AFIX 0 PART 0 C3D 1 0.362706 0.255706 0.250000 10.50000 0.09345 AFIX 43 H3D 2 0.376678 0.281461 0.250000 10.50000 -1.20000 AFIX 0 C2D 1 0.292558 0.242572 0.250000 10.50000 0.09602 AFIX 43 H2D 2 0.247224 0.256798 0.250000 10.50000 -1.20000 AFIX 0 C1D 1 0.368710 0.198271 0.250000 10.50000 0.07049 C8D 1 0.419753 0.163690 0.250000 10.50000 0.18513 PART -1 AFIX 33 H8DA 2 0.472666 0.171661 0.250000 10.50000 -1.50000 H8DB 2 0.409663 0.148616 0.275216 10.50000 -1.50000 H8DC 2 0.409663 0.148616 0.224784 10.50000 -1.50000 AFIX 0 PART 0 C4D 1 0.500347 0.229140 0.250000 10.50000 0.17171 N2C 5 0.037975 0.069737 0.250000 10.50000 0.07865 N1C 5 -0.062680 0.108153 0.250000 10.50000 0.16028 C2C 1 -0.020736 0.048607 0.250000 10.50000 0.10127 AFIX 43 H2C 2 -0.020053 0.021932 0.250000 10.50000 -1.20000 AFIX 0 C3C 1 -0.076506 0.067620 0.250000 10.50000 0.12581 AFIX 43 H3C 2 -0.125844 0.057205 0.250000 10.50000 -1.20000 AFIX 0 C8C 1 0.064299 0.145634 0.250000 10.50000 0.20844 PART -1 AFIX 33 H8CA 2 0.029214 0.166901 0.250000 10.50000 -1.50000 H8CB 2 0.096134 0.146778 0.275216 10.50000 -1.50000 H8CC 2 0.096134 0.146778 0.224784 10.50000 -1.50000 AFIX 0 PART 0 C1C 1 0.015400 0.105339 0.250000 10.50000 0.09044 C9C 1 0.125028 0.055540 0.250000 10.50000 0.16343 PART -1 AFIX 33 H9CA 2 0.158766 0.077340 0.250000 10.50000 -1.50000 H9CB 2 0.134426 0.040356 0.275216 10.50000 -1.50000 H9CC 2 0.134426 0.040356 0.224784 10.50000 -1.50000 AFIX 56 PART 0 C1F 1 0.056574 -0.071423 0.238585 10.25000 0.08298 N1F 5 -0.005856 -0.053216 0.257786 10.25000 0.06419 C3F 1 -0.072525 -0.072138 0.244962 10.25000 0.09918 C2F 1 -0.051300 -0.102039 0.217835 10.25000 0.09503 N2F 5 0.028488 -0.101597 0.213893 10.25000 0.05223 AFIX 56 N1E 5 0.337714 0.205089 -0.122816 11.00000 0.12298 C1E 1 0.384112 0.219431 -0.090082 11.00000 0.08751 N2E 5 0.460305 0.211179 -0.100328 11.00000 0.12591 C2E 1 0.460996 0.191736 -0.139395 11.00000 0.12098 C3E 1 0.385231 0.187973 -0.153293 11.00000 0.08497 AFIX 0 HKLF 4 REM bpp-1_a.res in P-1 New: Pbcm REM R1 = 0.0500 for 5781 Fo > 4sig(Fo) and 0.1453 for all 20058 data REM 640 parameters refined using 4 restraints END WGHT 0.0791 0.0000 REM Highest difference peak 1.749, deepest hole -0.881, 1-sigma level 0.159 Q1 1 0.2546 0.2069 -0.1289 11.00000 0.05 1.75 Q2 1 0.0421 0.2555 0.0192 11.00000 0.05 1.74 Q3 1 -0.0405 0.2415 -0.0309 11.00000 0.05 1.62 Q4 1 0.0794 0.2609 0.0410 11.00000 0.05 1.41 Q5 1 0.2113 0.1005 -0.0614 11.00000 0.05 1.37 Q6 1 -0.0610 0.2500 0.0000 10.50000 0.05 1.33 Q7 1 0.2032 0.1058 -0.1435 11.00000 0.05 1.05 Q8 1 0.1322 -0.0603 0.2500 10.50000 0.05 1.04 Q9 1 0.3472 0.0423 -0.2500 10.50000 0.05 0.97 Q10 1 0.2094 0.0444 0.0289 11.00000 0.05 0.96 Q11 1 0.4338 0.2381 -0.0416 11.00000 0.05 0.85 Q12 1 0.3792 0.1523 0.2500 10.50000 0.05 0.83 Q13 1 0.4643 0.2446 -0.0230 11.00000 0.05 0.80 Q14 1 0.3574 -0.0982 0.2682 11.00000 0.05 0.78 Q15 1 0.3478 0.0739 -0.2500 10.50000 0.05 0.76 Q16 1 0.3582 -0.0259 0.2500 10.50000 0.05 0.75 Q17 1 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15.4355 -0.1225 20 15 2 -7.3423 -0.0351 20 15 3 -6.6845 -0.0397 20 15 4 8.2003 -0.2852 20 15 5 -0.4096 -0.1243 20 15 6 7.7039 0.2478 20 15 7 5.4511 -0.1633 20 15 8 13.0471 0.1745 20 15 9 1.6336 -0.2196 20 15 10 -1.5776 0.2076 20 15 11 -8.2996 0.1043 20 15 12 6.8199 -0.0317 20 16 0 13.6842 0.7741 20 16 1 6.1453 -0.1568 20 16 2 -6.2944 -0.0158 20 16 3 -2.8374 -0.0552 20 16 4 1.7114 -0.1543 20 16 5 11.0130 -0.0948 20 16 6 -1.5970 -0.7991 20 16 7 0.4886 -0.1592 20 16 8 -1.3824 0.1470 20 16 9 3.6469 0.0657 20 16 10 5.6995 0.3306 20 16 11 -7.3301 -0.0233 20 17 0 8.9320 0.1612 20 17 1 -6.8611 -0.0541 20 17 2 1.1136 -0.0152 20 17 3 -4.3362 0.1672 20 17 4 1.6054 0.2832 20 17 5 4.8623 -0.0670 20 17 6 -6.2576 0.0400 20 17 7 -10.3402 -0.0080 20 17 8 -10.4139 -0.1578 20 17 9 2.5573 0.3106 20 17 10 1.9058 0.0161 20 18 0 -3.9009 -0.3484 20 18 1 -0.3805 -0.0032 20 18 2 2.3068 -0.1079 20 18 3 1.9761 -0.1074 20 18 4 3.2248 0.1794 20 18 5 -8.6935 0.6866 20 18 6 -2.9564 0.4367 20 18 7 -2.5297 -0.0474 20 18 8 3.4442 -0.0981 20 19 0 -9.6414 0.1608 20 19 1 7.5117 0.0382 20 19 2 -1.0713 -0.1493 20 19 3 4.1428 -0.2090 20 19 4 0.7217 -0.1009 20 19 5 -10.0908 -0.0980 20 19 6 0.0157 -0.0987 20 19 7 17.6749 -0.0782 20 20 0 -1.3804 0.3178 20 20 1 5.3504 0.3095 20 20 2 2.8779 -0.1118 20 20 3 -1.0018 0.4928 21 0 0 17.3355 -1.1893 21 0 2 9.1171 0.5607 21 0 4 -9.3788 0.6346 21 0 6 9.3297 0.1714 21 0 8 13.7304 0.2249 21 0 10 1.2825 -0.0861 21 0 12 -4.8588 -0.2327 21 0 14 -15.1988 0.1154 21 1 0 -0.5696 1.1563 21 1 1 7.1180 0.3986 21 1 2 2.1516 -1.3155 21 1 3 -6.6066 1.3409 21 1 4 -20.8573 0.2732 21 1 5 3.0608 -0.2856 21 1 6 2.0852 -0.1119 21 1 7 1.6184 -0.9739 21 1 8 4.8207 -0.9841 21 1 9 -6.5267 0.3178 21 1 10 -5.6610 -0.5469 21 1 11 1.6130 1.6417 21 1 12 2.7314 0.1972 21 1 13 -0.6395 0.5539 21 1 14 -10.6127 0.5129 21 2 0 -16.2270 0.2592 21 2 1 7.4711 -0.3840 21 2 2 -1.0878 -0.1525 21 2 3 -4.7423 0.1221 21 2 4 7.6195 -0.7295 21 2 5 6.7196 0.0129 21 2 6 -3.2008 -0.2207 21 2 7 1.2272 -0.2415 21 2 8 -11.2472 0.5124 21 2 9 3.3706 0.2531 21 2 10 1.0498 0.3530 21 2 11 11.4345 0.3147 21 2 12 -0.8632 -0.1267 21 2 13 1.4057 0.1215 21 2 14 13.2175 -0.4561 21 3 0 0.7856 0.8737 21 3 1 -12.5902 0.2465 21 3 2 -6.6111 -0.5509 21 3 3 12.9113 -0.9234 21 3 4 19.8607 0.4684 21 3 5 -0.7168 0.1315 21 3 6 2.1766 0.3130 21 3 7 -1.7807 0.5612 21 3 8 -8.9700 0.1321 21 3 9 7.0719 -0.3945 21 3 10 8.6188 0.2464 21 3 11 1.3185 -0.9756 21 3 12 -4.8277 0.2412 21 3 13 -1.6122 -0.4339 21 3 14 6.4357 -0.0064 21 4 0 8.4356 0.6819 21 4 1 -11.1640 0.6935 21 4 2 -2.3967 -0.0116 21 4 3 -8.1196 -0.2178 21 4 4 -22.2516 0.1350 21 4 5 17.0831 -0.2511 21 4 6 5.2996 0.1989 21 4 7 -10.8028 -0.1747 21 4 8 0.5293 -0.4433 21 4 9 -6.8825 0.0438 21 4 10 -8.9384 -0.2567 21 4 11 -5.7039 0.0937 21 4 12 7.0000 0.2427 21 4 13 -4.5706 0.2181 21 5 0 -5.5886 -1.1893 21 5 1 -2.5927 0.0508 21 5 2 2.4204 0.9488 21 5 3 -5.8554 0.1194 21 5 4 -9.1208 0.0588 21 5 5 -8.0009 -0.0990 21 5 6 -4.0924 -0.1815 21 5 7 4.4996 -0.1008 21 5 8 3.2444 0.1598 21 5 9 -5.2918 0.2698 21 5 10 0.5317 -0.0814 21 5 11 -0.2316 0.3048 21 5 12 -4.3784 -0.1929 21 5 13 2.7576 0.0067 21 6 0 6.8806 -0.4713 21 6 1 11.7740 -0.0442 21 6 2 -5.6588 -0.0582 21 6 3 10.6115 0.0980 21 6 4 32.8512 0.2865 21 6 5 -28.6213 0.0582 21 6 6 -8.8831 -0.0425 21 6 7 15.6802 0.2141 21 6 8 10.7746 -0.1022 21 6 9 0.7459 0.0364 21 6 10 9.4144 -0.1816 21 6 11 -2.8288 -0.1733 21 6 12 1.0184 -0.0337 21 7 0 1.6989 -0.0685 21 7 1 10.5424 -0.5954 21 7 2 7.7036 0.0412 21 7 3 2.4669 0.5088 21 7 4 -2.3586 -0.5497 21 7 5 1.1643 0.0701 21 7 6 4.3065 -0.1450 21 7 7 -2.3170 -0.2347 21 7 8 -4.7666 0.0208 21 7 9 7.0632 0.1836 21 7 10 3.4737 -0.0846 21 7 11 -4.1992 0.2497 21 7 12 9.5880 -0.3173 21 8 0 -20.6680 0.0453 21 8 1 -13.1901 -0.2162 21 8 2 13.4847 -0.0756 21 8 3 -1.6119 0.0975 21 8 4 -14.1016 -0.0809 21 8 5 21.9838 0.0659 21 8 6 -4.0688 -0.0146 21 8 7 -10.8192 0.1750 21 8 8 -8.7710 0.1262 21 8 9 1.6402 -0.0050 21 8 10 -0.5532 0.2290 21 8 11 9.2894 0.0321 21 8 12 -6.9686 0.2506 21 9 0 -3.7988 0.7067 21 9 1 -3.0945 -0.0260 21 9 2 3.6089 -0.4055 21 9 3 -0.1812 -0.2346 21 9 4 -4.1267 0.0895 21 9 5 3.1947 0.1412 21 9 6 2.3109 0.1465 21 9 7 -1.9672 0.1709 21 9 8 6.9068 0.0382 21 9 9 -5.8596 -0.1419 21 9 10 -9.8192 0.0766 21 9 11 1.5601 -0.5718 21 10 0 14.5468 0.2886 21 10 1 15.3703 -0.1315 21 10 2 -17.8944 0.0028 21 10 3 -5.8266 -0.0102 21 10 4 5.1255 -0.1065 21 10 5 -7.5180 0.1254 21 10 6 3.8511 -0.0066 21 10 7 -2.0648 -0.3536 21 10 8 3.8445 -0.0272 21 10 9 4.8605 -0.2241 21 10 10 -3.5914 0.1930 21 10 11 -10.7744 0.2517 21 11 0 1.4948 -0.3555 21 11 1 2.8205 0.6516 21 11 2 -9.3398 0.0890 21 11 3 -5.2172 -0.3207 21 11 4 4.0623 0.1705 21 11 5 3.4315 -0.2452 21 11 6 -0.7556 0.1991 21 11 7 -4.8063 0.3600 21 11 8 -9.4183 -0.0402 21 11 9 13.0172 -0.6181 21 11 10 5.6351 -0.0460 21 12 0 5.2283 -0.2222 21 12 1 -3.5027 0.0951 21 12 2 6.5481 0.0263 21 12 3 2.8567 -0.0228 21 12 4 -2.1061 0.1022 21 12 5 -11.6922 -0.1565 21 12 6 5.6602 0.0087 21 12 7 15.0213 -0.0843 21 12 8 -1.6520 0.3085 21 13 0 12.4337 -0.2229 21 13 1 1.7259 -0.1777 21 13 2 -3.7736 0.0804 21 13 3 -2.0707 0.2780 21 13 4 3.7413 -0.0109 21 13 5 7.3368 0.0004 21 13 6 -2.6490 -0.5656 21 13 7 2.8915 -0.4328 21 13 8 11.5866 -0.1463 21 14 0 -4.8588 -0.1133 21 14 1 -9.6964 -0.0871 21 14 2 8.2536 0.0244 21 14 3 8.7046 -0.0665 21 14 4 -8.5506 0.0453 21 14 5 8.5858 -0.0120 21 14 6 -5.5135 -0.0283 21 15 0 -13.7117 0.1627 21 15 1 -3.4011 -0.3047 21 15 2 4.9687 0.0672 21 15 3 3.5853 -0.0588 21 15 4 -1.8001 0.0493 21 16 0 -7.6434 0.1753 21 16 1 4.5854 0.0862 21 16 3 -4.1116 0.1283 22 0 0 -1.4684 -0.7013 22 0 2 4.3638 0.4873 22 0 4 3.2101 0.2971 22 0 6 -6.3750 0.1507 22 1 0 14.3182 0.2537 22 1 1 -2.5466 -0.6171 22 1 2 8.9950 0.2695 22 1 3 5.2492 0.2428 22 1 4 -2.2377 -0.3650 22 1 5 -15.0538 0.2573 22 1 6 -12.8243 -0.0215 22 1 7 9.5472 -0.1171 22 2 0 1.8002 0.4168 22 2 1 -1.2824 0.6887 22 2 2 -5.0527 -0.2518 22 2 3 4.2388 0.2093 22 2 4 -1.8098 -0.3963 22 2 5 -5.9269 -0.1151 22 2 6 -3.3858 -0.3703 22 2 7 2.8754 -0.3586 22 3 0 -8.1944 -0.0379 22 3 1 4.2167 0.4723 22 3 2 -0.6727 -0.1729 22 3 3 -0.6195 -0.0904 22 3 4 9.8689 0.0240 22 3 5 11.5238 0.0009 22 3 6 1.2200 0.1270 22 3 7 -13.6021 -0.1059 22 4 0 6.9118 0.1774 22 4 1 -0.9155 0.0890 22 4 2 1.0629 0.2606 22 4 3 0.0666 0.1280 22 4 4 3.0472 -0.0040 22 4 5 7.1373 0.2262 22 4 6 12.7576 0.1062 22 4 7 -2.0513 0.1157 22 5 0 8.8014 -0.5930 22 5 1 -2.3403 -0.1398 22 5 2 -1.5049 0.1993 22 5 3 -9.2205 -0.0356 22 5 4 -24.2596 -0.1361 22 5 5 16.6790 -0.0697 22 5 6 11.6099 -0.2318 22 6 0 -11.7914 -0.3896 22 6 1 -6.0551 -0.5805 22 6 2 -4.3485 -0.4322 22 6 3 0.4590 -0.0238 22 6 4 1.8021 0.4074 22 6 5 -11.1721 0.0333 22 7 0 1.2688 0.2521 22 7 1 9.8118 0.0738 22 7 2 -7.7217 -0.0125 22 7 3 -0.4143 -0.1100 22 7 4 21.1797 0.0716 22 7 5 -18.2485 -0.1349 22 8 0 8.1663 0.0473 22 8 1 4.3816 0.3399 22 8 2 9.1528 0.1136 22 8 3 -0.6033 0.0800 22 9 0 -10.0445 0.4501 22 9 2 11.7892 -0.1356 0 0 0 0.0 0.0 ; _shelx_fab_checksum 75732 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -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 Sn9 Sn 0.25513(7) 0.04166(2) 0.02048(2) 0.05067(19) Uani 1 1 d . . . . . Sn5 Sn 0.35424(6) 0.12866(3) 0.02172(3) 0.0520(3) Uani 1 1 d . . . . . Sn6 Sn 0.15214(6) 0.06958(3) 0.11233(3) 0.0492(3) Uani 1 1 d . . . . . Sn7 Sn 0.15237(6) 0.12754(3) 0.01974(3) 0.0519(3) Uani 1 1 d . . . . . Sn1 Sn 0.44922(6) 0.15842(3) 0.11390(3) 0.0591(3) Uani 1 1 d . . . . . Sn3 Sn 0.05213(6) 0.15542(3) 0.11038(3) 0.0619(3) Uani 1 1 d . . . . . Sn8 Sn 0.25465(8) -0.01530(2) 0.11177(2) 0.0587(2) Uani 1 1 d . . . . . Sn4 Sn 0.35382(6) 0.07086(3) 0.11302(3) 0.0480(3) Uani 1 1 d . . . . . Sn2 Sn 0.25040(7) 0.15723(2) 0.11269(2) 0.04695(17) Uani 1 1 d . . . . . Sn10 Sn 0.25883(9) 0.09962(2) -0.07084(2) 0.0664(3) Uani 1 1 d . . . . . S15 S 0.3938(2) 0.05918(11) 0.03535(11) 0.0551(10) Uani 1 1 d . . . . . S2 S 0.3505(2) 0.19620(11) 0.14340(11) 0.0537(10) Uani 1 1 d . . . . . S11 S 0.3702(2) 0.00740(12) 0.14265(11) 0.0597(11) Uani 1 1 d . . . . . S18 S 0.2557(3) -0.02576(7) 0.03681(8) 0.0623(8) Uani 1 1 d . . . . . S6 S 0.2503(3) 0.18033(7) 0.03438(7) 0.0533(6) Uani 1 1 d . . . . . S13 S 0.3747(3) 0.13157(12) -0.05461(11) 0.0655(12) Uani 1 1 d . . . . . S12 S 0.1400(2) 0.00663(11) 0.14347(11) 0.0582(10) Uani 1 1 d . . . . . S9 S 0.0324(2) 0.09423(13) 0.14118(12) 0.0663(12) Uani 1 1 d . . . . . S3 S 0.1461(2) 0.19468(12) 0.14295(11) 0.0602(11) Uani 1 1 d . . . . . S8 S 0.4701(2) 0.16448(13) 0.03911(12) 0.0656(11) Uani 1 1 d . . . . . S10 S 0.0340(2) 0.15966(13) 0.03561(12) 0.0657(11) Uani 1 1 d . . . . . S14 S 0.1423(3) 0.13213(13) -0.05757(11) 0.0696(12) Uani 1 1 d . . . . . S20 S 0.2811(2) 0.10430(11) -0.14646(10) 0.0726(11) Uani 1 1 d . . . . . S4 S -0.0576(3) 0.18985(17) 0.13652(16) 0.1040(18) Uani 1 1 d . . . . . S5 S 0.2517(2) 0.09943(7) 0.16334(6) 0.0468(6) Uani 1 1 d . . . . . S19 S 0.2555(3) 0.03346(7) -0.05677(7) 0.0622(8) Uani 1 1 d . . . . . S16 S 0.1129(2) 0.05804(12) 0.03388(11) 0.0578(10) Uani 1 1 d . . . . . S7 S 0.4703(2) 0.09705(12) 0.14314(11) 0.0579(10) Uani 1 1 d . . . . . S17 S 0.2475(4) -0.07998(9) 0.13768(10) 0.0979(13) Uani 1 1 d . . . . . S1 S 0.5559(3) 0.19415(16) 0.14282(16) 0.0966(17) Uani 1 1 d . . . . . O2 O 0.1651(5) 0.1238(3) 0.0856(2) 0.046(2) Uani 1 1 d . . . . . O3 O 0.2544(6) 0.05027(17) 0.08646(18) 0.0491(17) Uani 1 1 d . . . . . O1 O 0.3369(5) 0.1243(2) 0.0877(2) 0.049(2) Uani 1 1 d . . . . . O4 O 0.2533(6) 0.09950(18) 0.00890(17) 0.0518(17) Uani 1 1 d . . . . . CIII C 0.3084(12) -0.1005(7) 0.1051(8) 0.151(5) Uani 1 1 d . . . . . HIIA H 0.281160 -0.110946 0.080944 0.227 Uiso 1 1 calc GR . . . . HIIB H 0.334662 -0.120810 0.120027 0.227 Uiso 1 1 calc GR . . . . HIIC H 0.345241 -0.081995 0.095307 0.227 Uiso 1 1 calc GR . . . . CII C -0.1320(12) 0.1692(7) 0.1047(8) 0.151(5) Uani 1 1 d . . . . . HIID H -0.113258 0.164926 0.076003 0.227 Uiso 1 1 calc GR . . . . HIIE H -0.175228 0.186336 0.103708 0.227 Uiso 1 1 calc GR . . . . HIIF H -0.147597 0.145248 0.117084 0.227 Uiso 1 1 calc GR . . . . CIV C 0.2215(12) 0.0706(7) -0.1642(7) 0.151(5) Uani 1 1 d . . . . . HIVA H 0.224464 0.069229 -0.195015 0.227 Uiso 1 1 calc R . . . . HIVB H 0.235810 0.046307 -0.152103 0.227 Uiso 1 1 calc R . . . . HIVC H 0.169786 0.076779 -0.155790 0.227 Uiso 1 1 calc R . . . . CI C 0.6323(12) 0.1658(7) 0.1230(8) 0.151(5) Uani 1 1 d . . . . . HIA H 0.624025 0.160529 0.093035 0.227 Uiso 1 1 calc GR . . . . HIB H 0.634289 0.142070 0.138657 0.227 Uiso 1 1 calc GR . . . . HIC H 0.680019 0.179281 0.126532 0.227 Uiso 1 1 calc GR . . . . N1 N 0.4173(8) -0.0117(5) -0.0958(4) 0.076(4) Uani 1 1 d . . . . . N2 N 0.4453(8) 0.0354(4) -0.1303(4) 0.077(4) Uani 1 1 d . . . . . C1 C 0.4548(10) 0.0201(5) -0.0945(4) 0.067(5) Uani 1 1 d . . . . . C3 C 0.3792(11) -0.0164(7) -0.1350(5) 0.094(5) Uani 1 1 d . . . . . H3 H 0.348862 -0.036840 -0.144207 0.112 Uiso 1 1 calc R . . . . C8 C 0.5010(9) 0.0332(5) -0.0588(4) 0.064(4) Uani 1 1 d . . . . . H8A H 0.473753 0.052915 -0.043530 0.096 Uiso 1 1 calc GR . . . . H8B H 0.548842 0.043274 -0.069350 0.096 Uiso 1 1 calc GR . . . . H8C H 0.511092 0.012141 -0.039721 0.096 Uiso 1 1 calc GR . . . . C2 C 0.3967(11) 0.0151(6) -0.1556(5) 0.094(5) Uani 1 1 d . . . . . H2 H 0.379050 0.022226 -0.182652 0.112 Uiso 1 1 calc R . . . . C4 C 0.4119(10) -0.0379(6) -0.0604(7) 0.104(7) Uani 1 1 d . . . . . H4A H 0.404683 -0.023334 -0.034186 0.124 Uiso 1 1 calc R . . . . H4B H 0.460345 -0.051574 -0.057912 0.124 Uiso 1 1 calc R . . . . C5 C 0.3461(11) -0.0675(5) -0.0642(6) 0.103(6) Uani 1 1 d . . . . . H5A H 0.296826 -0.054493 -0.063322 0.124 Uiso 1 1 calc R . . . . H5B H 0.349998 -0.080915 -0.091470 0.124 Uiso 1 1 calc R . . . . C6 C 0.3510(13) -0.0959(6) -0.0278(7) 0.129(6) Uani 1 1 d . . . . . H6A H 0.395312 -0.112520 -0.031542 0.155 Uiso 1 1 calc R . . . . H6B H 0.356279 -0.082589 -0.000545 0.155 Uiso 1 1 calc R . . . . C7 C 0.2791(12) -0.1188(5) -0.0282(7) 0.129(6) Uani 1 1 d . . . . . H7A H 0.272040 -0.129877 -0.056184 0.194 Uiso 1 1 calc GR . . . . H7B H 0.236210 -0.102496 -0.021565 0.194 Uiso 1 1 calc GR . . . . H7C H 0.282591 -0.138838 -0.007118 0.194 Uiso 1 1 calc GR . . . . C9 C 0.4797(11) 0.0733(5) -0.1424(4) 0.101(6) Uani 1 1 d . . . . . H9A H 0.461384 0.092722 -0.123013 0.151 Uiso 1 1 calc GR . . . . H9B H 0.464830 0.079764 -0.171264 0.151 Uiso 1 1 calc GR . . . . H9C H 0.534774 0.071802 -0.140658 0.151 Uiso 1 1 calc GR . . . . F03T F 0.1926(7) -0.0004(3) -0.250000 0.079(3) Uiso 1 2 d DS T P . . F04A F 0.3234(10) 0.0188(5) -0.250000 0.136(6) Uiso 1 2 d DS T P . . F04F F 0.2732(9) -0.0357(4) -0.2151(4) 0.191(6) Uiso 1 1 d D . . . . F04T F 0.3771(10) 0.1521(5) -0.250000 0.139(6) Uiso 1 2 d S T P . . F040 F 0.4220(8) 0.0951(4) -0.250000 0.111(4) Uiso 1 2 d S T P . . F049 F 0.4898(6) 0.1381(3) -0.2149(3) 0.118(3) Uiso 1 1 d . . . . . B05E B 0.2693(9) -0.0118(5) -0.250000 0.070(6) Uiso 1 2 d DS T P . . B40 B 0.4507(14) 0.1302(7) -0.250000 0.066(6) Uiso 1 2 d S T P . . N2A N 0.1085(9) -0.0206(5) -0.1279(5) 0.090(5) Uani 1 1 d . . . . . N1A N 0.0366(9) 0.0177(5) -0.0976(4) 0.083(4) Uani 1 1 d . . . . . C9A C 0.1611(13) -0.0533(7) -0.1349(6) 0.126(8) Uani 1 1 d . . . . . H9AA H 0.195125 -0.055746 -0.110697 0.189 Uiso 1 1 calc GR . . . . H9AB H 0.190759 -0.048983 -0.160494 0.189 Uiso 1 1 calc GR . . . . H9AC H 0.131626 -0.076412 -0.138031 0.189 Uiso 1 1 calc GR . . . . C8A C 0.0911(11) -0.0341(6) -0.0515(5) 0.101(7) Uani 1 1 d . . . . . H8AA H 0.134741 -0.050825 -0.054241 0.151 Uiso 1 1 calc GR . . . . H8AB H 0.046136 -0.049027 -0.044792 0.151 Uiso 1 1 calc GR . . . . H8AC H 0.100272 -0.015978 -0.028879 0.151 Uiso 1 1 calc GR . . . . C2A C 0.0871(13) 0.0034(7) -0.1581(6) 0.111(8) Uani 1 1 d . . . . . H2A H 0.101336 0.002582 -0.186903 0.133 Uiso 1 1 calc R . . . . C3A C 0.0429(12) 0.0281(7) -0.1402(5) 0.113(8) Uani 1 1 d . . . . . H3A H 0.019591 0.049046 -0.153434 0.136 Uiso 1 1 calc R . . . . C5A C -0.0368(11) 0.0737(5) -0.0774(6) 0.106(4) Uani 1 1 d . . . . . H5AA H -0.072260 0.070988 -0.101286 0.127 Uiso 1 1 calc R . . . . H5AB H 0.007021 0.088408 -0.087569 0.127 Uiso 1 1 calc R . . . . C1A C 0.0789(10) -0.0137(7) -0.0920(6) 0.085(6) Uani 1 1 d . . . . . C6A C -0.0761(11) 0.0962(5) -0.0424(6) 0.106(4) Uani 1 1 d . . . . . H6AA H -0.117724 0.080487 -0.031321 0.127 Uiso 1 1 calc R . . . . H6AB H -0.039377 0.099417 -0.019151 0.127 Uiso 1 1 calc R . . . . C7A C -0.1076(11) 0.1335(6) -0.0520(7) 0.120(7) Uani 1 1 d . . . . . H7AA H -0.151486 0.130642 -0.070575 0.181 Uiso 1 1 calc GR . . . . H7AB H -0.069280 0.148789 -0.066138 0.181 Uiso 1 1 calc GR . . . . H7AC H -0.123156 0.145793 -0.025812 0.181 Uiso 1 1 calc GR . . . . C4A C -0.0103(12) 0.0361(5) -0.0650(5) 0.090(6) Uani 1 1 d . . . . . H4AA H -0.054550 0.020040 -0.059040 0.108 Uiso 1 1 calc R . . . . H4AB H 0.019467 0.038255 -0.038743 0.108 Uiso 1 1 calc R . . . . C8E C 0.3764(9) 0.2374(4) -0.0502(5) 0.084(5) Uiso 1 1 d . . . . . H8EA H 0.322963 0.242447 -0.044662 0.126 Uiso 1 1 calc R . . . . H8EB H 0.396509 0.220989 -0.028066 0.126 Uiso 1 1 calc R . . . . H8EC H 0.404451 0.261115 -0.050336 0.126 Uiso 1 1 calc R . . . . C9E C 0.5326(13) 0.2185(10) -0.0731(9) 0.226(15) Uiso 1 1 d D . . . . H9EA H 0.577235 0.209802 -0.088474 0.338 Uiso 1 1 calc R . . . . H9EB H 0.537218 0.245420 -0.067357 0.338 Uiso 1 1 calc R . . . . H9EC H 0.528481 0.204774 -0.046407 0.338 Uiso 1 1 calc R . . . . N2B N 0.4123(12) 0.0249(6) 0.250000 0.089(5) Uiso 1 2 d S T P . . N1B N 0.3964(15) -0.0351(7) 0.250000 0.118(7) Uiso 1 2 d S T P . . C9B C 0.3912(17) 0.0656(8) 0.250000 0.115(9) Uiso 1 2 d S T P . . H9BA H 0.437141 0.080982 0.250000 0.173 Uiso 0.5 1 calc RS T P A -1 H9BB H 0.361417 0.071300 0.224784 0.173 Uiso 0.5 1 calc R . . A -1 H9BC H 0.361417 0.071300 0.275216 0.173 Uiso 0.5 1 calc R . . A -1 C1B C 0.3656(14) -0.0006(7) 0.250000 0.079(6) Uiso 1 2 d S T P . . C2B C 0.4797(14) 0.0116(7) 0.250000 0.082(6) Uiso 1 2 d S T P . . C3B C 0.4710(15) -0.0273(7) 0.250000 0.089(7) Uiso 1 2 d S T P . . H3B H 0.510697 -0.045230 0.250000 0.106 Uiso 1 2 calc RS T P . . C4B C 0.339(3) -0.0642(15) 0.250000 0.212(19) Uiso 1 2 d S T P . . C8B C 0.288(2) 0.0132(13) 0.250000 0.211(19) Uiso 1 2 d S T P . . H8BA H 0.253278 -0.008144 0.250000 0.317 Uiso 0.5 1 calc RS T P B -1 H8BB H 0.279631 0.028497 0.275216 0.317 Uiso 0.5 1 calc R . . B -1 H8BC H 0.279631 0.028497 0.224784 0.317 Uiso 0.5 1 calc R . . B -1 N1D N 0.4094(15) 0.2272(8) 0.250000 0.124(8) Uiso 1 2 d S T P . . N2D N 0.2992(11) 0.2043(5) 0.250000 0.085(5) Uiso 1 2 d S T P . . C9D C 0.2316(16) 0.1772(7) 0.250000 0.113(9) Uiso 1 2 d S T P . . H9DA H 0.239013 0.157972 0.228244 0.170 Uiso 0.5 1 calc GR . . C -1 H9DB H 0.185236 0.191180 0.244120 0.170 Uiso 0.5 1 calc GR . . C -1 H9DC H 0.227571 0.165037 0.277636 0.170 Uiso 0.5 1 calc GR . . C -1 C3D C 0.3627(15) 0.2557(8) 0.250000 0.093(7) Uiso 1 2 d S T P . . H3D H 0.376678 0.281461 0.250000 0.112 Uiso 1 2 calc RS T P . . C2D C 0.2926(15) 0.2426(7) 0.250000 0.096(7) Uiso 1 2 d S T P . . H2D H 0.247224 0.256798 0.250000 0.115 Uiso 1 2 calc RS T P . . C1D C 0.3687(13) 0.1983(6) 0.250000 0.070(5) Uiso 1 2 d S T P . . C8D C 0.420(2) 0.1637(12) 0.250000 0.185(17) Uiso 1 2 d S T P . . H8DA H 0.472666 0.171661 0.250000 0.278 Uiso 0.5 1 calc RS T P D -1 H8DB H 0.409663 0.148616 0.275216 0.278 Uiso 0.5 1 calc R . . D -1 H8DC H 0.409663 0.148616 0.224784 0.278 Uiso 0.5 1 calc R . . D -1 C4D C 0.500(2) 0.2291(12) 0.250000 0.172(14) Uiso 1 2 d S T P . . N2C N 0.0380(11) 0.0697(5) 0.250000 0.079(5) Uiso 1 2 d S T P . . N1C N -0.0627(19) 0.1082(9) 0.250000 0.160(10) Uiso 1 2 d S T P . . C2C C -0.0207(16) 0.0486(8) 0.250000 0.101(8) Uiso 1 2 d S T P . . H2C H -0.020053 0.021932 0.250000 0.122 Uiso 1 2 calc RS T P . . C3C C -0.077(2) 0.0676(9) 0.250000 0.126(10) Uiso 1 2 d S T P . . H3C H -0.125844 0.057205 0.250000 0.151 Uiso 1 2 calc RS T P . . C8C C 0.064(3) 0.1456(13) 0.250000 0.208(19) Uiso 1 2 d S T P . . H8CA H 0.029214 0.166901 0.250000 0.313 Uiso 0.5 1 calc RS T P E -1 H8CB H 0.096134 0.146778 0.275216 0.313 Uiso 0.5 1 calc R . . E -1 H8CC H 0.096134 0.146778 0.224784 0.313 Uiso 0.5 1 calc R . . E -1 C1C C 0.0154(15) 0.1053(7) 0.250000 0.090(7) Uiso 1 2 d S T P . . C9C C 0.125(2) 0.0555(11) 0.250000 0.163(15) Uiso 1 2 d S T P . . H9CA H 0.158766 0.077340 0.250000 0.245 Uiso 0.5 1 calc RS T P F -1 H9CB H 0.134426 0.040356 0.275216 0.245 Uiso 0.5 1 calc R . . F -1 H9CC H 0.134426 0.040356 0.224784 0.245 Uiso 0.5 1 calc R . . F -1 C1F C 0.0566(14) -0.0714(9) 0.2386(12) 0.083(19) Uiso 0.25 1 d . . . . . N1F N -0.006(2) -0.0532(7) 0.2578(12) 0.064(12) Uiso 0.25 1 d G . . . . C3F C -0.0725(14) -0.0721(11) 0.2450(16) 0.099(18) Uiso 0.25 1 d G . . . . C2F C -0.0513(18) -0.1020(10) 0.2178(14) 0.10(2) Uiso 0.25 1 d G . . . . N2F N 0.0285(19) -0.1016(8) 0.2139(9) 0.052(9) Uiso 0.25 1 d G . . . . N1E N 0.3377(5) 0.2051(4) -0.1228(4) 0.123(5) Uiso 1 1 d . . . . . C1E C 0.3841(7) 0.2194(3) -0.0901(3) 0.088(5) Uiso 1 1 d G . . . . N2E N 0.4603(6) 0.2112(4) -0.1003(4) 0.126(6) Uiso 1 1 d DG . . . . C2E C 0.4610(6) 0.1917(4) -0.1394(4) 0.121(7) Uiso 1 1 d G . . . . C3E C 0.3852(8) 0.1880(3) -0.1533(3) 0.085(5) Uiso 1 1 d G . . . . 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 Sn9 0.0725(6) 0.0408(3) 0.0387(3) -0.0023(3) -0.0014(6) -0.0015(6) Sn5 0.0707(8) 0.0446(6) 0.0406(5) -0.0049(5) 0.0120(5) -0.0029(5) Sn6 0.0581(7) 0.0477(6) 0.0418(5) 0.0013(5) 0.0010(5) -0.0046(5) Sn7 0.0648(7) 0.0474(7) 0.0436(5) 0.0027(5) -0.0036(5) 0.0006(5) Sn1 0.0623(7) 0.0598(7) 0.0552(6) -0.0087(5) 0.0060(5) -0.0086(5) Sn3 0.0619(7) 0.0665(8) 0.0574(6) 0.0030(5) 0.0036(5) 0.0089(6) Sn8 0.0883(6) 0.0442(4) 0.0437(3) 0.0009(3) -0.0037(6) -0.0022(7) Sn4 0.0559(7) 0.0464(6) 0.0418(5) -0.0025(5) 0.0008(4) 0.0028(5) Sn2 0.0584(5) 0.0424(3) 0.0400(3) -0.0034(3) 0.0046(6) 0.0005(6) Sn10 0.1148(9) 0.0452(4) 0.0392(3) -0.0005(3) 0.0025(6) -0.0024(7) S15 0.069(3) 0.051(2) 0.045(2) -0.0038(17) 0.0102(18) 0.0023(19) S2 0.072(3) 0.045(2) 0.0447(19) -0.0034(17) 0.0040(18) -0.0015(19) S11 0.083(3) 0.054(3) 0.0420(19) 0.0016(17) -0.0034(19) 0.016(2) S18 0.101(3) 0.0402(13) 0.0456(13) -0.0005(10) -0.007(2) -0.002(3) S6 0.0737(19) 0.0408(12) 0.0454(12) 0.0002(10) 0.007(2) -0.002(2) S13 0.099(3) 0.055(2) 0.0419(18) -0.0021(17) 0.0224(19) -0.001(2) S12 0.074(3) 0.051(2) 0.050(2) 0.0035(18) -0.0018(19) -0.010(2) S9 0.062(3) 0.076(3) 0.060(2) 0.006(2) 0.0084(19) -0.009(2) S3 0.074(3) 0.056(3) 0.050(2) -0.0051(19) 0.0126(19) 0.014(2) S8 0.075(3) 0.065(3) 0.057(2) -0.0095(18) 0.0186(19) -0.015(2) S10 0.068(3) 0.062(3) 0.067(2) 0.005(2) -0.009(2) 0.007(2) S14 0.104(3) 0.058(3) 0.047(2) 0.0048(18) -0.012(2) -0.001(2) S20 0.101(3) 0.072(2) 0.0442(15) -0.0071(16) 0.0011(16) -0.0028(19) S4 0.096(4) 0.118(4) 0.098(3) 0.009(3) 0.029(3) 0.046(3) S5 0.0586(17) 0.0439(12) 0.0380(10) -0.0025(10) 0.003(2) 0.000(2) S19 0.100(3) 0.0474(14) 0.0393(12) -0.0048(10) 0.005(2) 0.001(3) S16 0.069(3) 0.057(3) 0.047(2) 0.0007(18) -0.0073(18) -0.012(2) S7 0.053(2) 0.063(3) 0.057(2) -0.0073(19) -0.0046(18) 0.001(2) S17 0.174(4) 0.0518(17) 0.0678(18) 0.0094(14) -0.014(4) -0.005(4) S1 0.071(3) 0.113(4) 0.106(3) -0.044(3) 0.012(3) -0.030(3) O2 0.045(6) 0.049(6) 0.043(5) -0.002(4) -0.008(4) -0.004(4) O3 0.062(5) 0.038(3) 0.047(3) -0.002(3) 0.010(5) 0.001(6) O1 0.075(7) 0.033(5) 0.038(5) 0.001(4) -0.004(4) -0.008(5) O4 0.074(5) 0.043(3) 0.039(3) -0.001(3) 0.009(5) -0.001(6) CIII 0.111(9) 0.149(10) 0.194(12) -0.018(9) -0.013(9) -0.019(8) CII 0.111(9) 0.149(10) 0.194(12) -0.018(9) -0.013(9) -0.019(8) CIV 0.111(9) 0.149(10) 0.194(12) -0.018(9) -0.013(9) -0.019(8) CI 0.111(9) 0.149(10) 0.194(12) -0.018(9) -0.013(9) -0.019(8) N1 0.087(11) 0.092(11) 0.048(8) 0.011(7) 0.005(7) 0.035(9) N2 0.068(9) 0.103(11) 0.060(8) 0.005(8) 0.001(7) 0.015(8) C1 0.090(13) 0.080(12) 0.033(8) 0.002(7) -0.002(7) 0.013(10) C3 0.080(9) 0.140(15) 0.061(8) 0.001(7) -0.001(7) 0.015(9) C8 0.071(10) 0.082(11) 0.039(7) 0.000(7) 0.004(7) 0.020(8) C2 0.080(9) 0.140(15) 0.061(8) 0.001(7) -0.001(7) 0.015(9) C4 0.045(11) 0.136(19) 0.130(16) 0.030(14) 0.016(10) 0.017(11) C5 0.106(15) 0.084(12) 0.120(14) -0.011(11) 0.041(12) 0.019(11) C6 0.144(17) 0.089(11) 0.154(12) -0.006(10) 0.041(12) 0.029(9) C7 0.144(17) 0.089(11) 0.154(12) -0.006(10) 0.041(12) 0.029(9) C9 0.122(15) 0.133(16) 0.047(8) 0.026(9) 0.019(9) 0.036(13) N2A 0.089(12) 0.120(13) 0.061(9) 0.017(9) -0.012(8) -0.043(10) N1A 0.089(12) 0.097(12) 0.064(9) 0.013(8) -0.006(8) -0.033(9) C9A 0.13(2) 0.17(2) 0.080(12) -0.014(13) 0.008(12) -0.017(17) C8A 0.089(14) 0.135(18) 0.078(11) 0.050(11) -0.003(9) -0.010(12) C2A 0.115(18) 0.16(2) 0.052(10) 0.009(12) 0.034(11) -0.051(15) C3A 0.107(17) 0.19(2) 0.039(9) 0.049(12) -0.009(9) -0.033(16) C5A 0.112(12) 0.103(11) 0.102(9) -0.002(8) -0.018(8) -0.037(9) C1A 0.049(11) 0.14(2) 0.063(11) 0.014(12) 0.010(8) -0.018(11) C6A 0.112(12) 0.103(11) 0.102(9) -0.002(8) -0.018(8) -0.037(9) C7A 0.085(14) 0.112(16) 0.165(18) 0.031(14) -0.011(13) -0.010(12) C4A 0.128(17) 0.095(15) 0.048(9) 0.002(9) -0.015(10) -0.024(12) 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 S15 Sn9 S16 146.37(8) . . S18 Sn9 S15 101.18(16) . . S18 Sn9 S19 95.39(9) . . S18 Sn9 S16 100.78(16) . . S19 Sn9 S15 101.99(16) . . S19 Sn9 S16 100.95(16) . . O3 Sn9 S15 77.8(3) . . O3 Sn9 S18 86.15(17) . . O3 Sn9 S19 178.45(18) . . O3 Sn9 S16 78.6(3) . . O4 Sn9 S15 79.0(3) . . O4 Sn9 S18 177.83(18) . . O4 Sn9 S19 86.68(16) . . O4 Sn9 S16 78.2(3) . . O4 Sn9 O3 91.8(2) . . S15 Sn5 S6 145.62(12) . . S13 Sn5 S15 99.45(13) . . S13 Sn5 S6 102.98(13) . . S13 Sn5 S8 94.34(15) . . S8 Sn5 S15 103.20(15) . . S8 Sn5 S6 100.73(14) . . O1 Sn5 S15 78.8(3) . . O1 Sn5 S6 78.4(3) . . O1 Sn5 S13 178.2(3) . . O1 Sn5 S8 86.5(3) . . O4 Sn5 S15 78.0(2) . . O4 Sn5 S6 77.3(2) . . O4 Sn5 S13 87.45(19) . . O4 Sn5 S8 177.6(2) . . O4 Sn5 O1 91.8(3) . . S12 Sn6 S9 95.73(15) . . S12 Sn6 S5 100.39(11) . . S12 Sn6 S16 102.47(13) . . S9 Sn6 S5 101.86(13) . . S9 Sn6 S16 100.36(14) . . S16 Sn6 S5 146.13(12) . . O2 Sn6 S12 178.8(3) . . O2 Sn6 S9 85.3(3) . . O2 Sn6 S5 78.7(2) . . O2 Sn6 S16 78.0(2) . . O3 Sn6 S12 86.23(19) . . O3 Sn6 S9 178.0(2) . . O3 Sn6 S5 78.1(2) . . O3 Sn6 S16 78.9(2) . . O3 Sn6 O2 92.7(3) . . S6 Sn7 S16 146.46(12) . . S10 Sn7 S6 101.43(14) . . S10 Sn7 S14 96.41(16) . . S10 Sn7 S16 100.26(15) . . S14 Sn7 S6 100.27(13) . . S14 Sn7 S16 102.38(14) . . O2 Sn7 S6 78.3(2) . . O2 Sn7 S10 85.3(3) . . O2 Sn7 S14 178.0(3) . . O2 Sn7 S16 78.3(3) . . O4 Sn7 S6 78.6(2) . . O4 Sn7 S10 177.57(19) . . O4 Sn7 S14 86.0(2) . . O4 Sn7 S16 78.7(2) . . O4 Sn7 O2 92.4(3) . . S2 Sn1 S8 116.48(15) . . S2 Sn1 S7 118.21(13) . . S2 Sn1 S1 97.20(16) . . S2 Sn1 O1 79.6(2) . . S8 Sn1 S1 101.73(17) . . S8 Sn1 O1 80.6(2) . . S7 Sn1 S8 115.95(15) . . S7 Sn1 S1 101.96(18) . . S7 Sn1 O1 78.9(2) . . S1 Sn1 O1 176.7(2) . . S9 Sn3 S4 101.54(18) . . S9 Sn3 O2 80.3(2) . . S3 Sn3 S9 116.79(15) . . S3 Sn3 S4 96.52(19) . . S3 Sn3 O2 80.7(2) . . S10 Sn3 S9 115.96(15) . . S10 Sn3 S3 118.74(15) . . S10 Sn3 S4 101.38(17) . . S10 Sn3 O2 79.6(2) . . O2 Sn3 S4 177.1(3) . . S11 Sn8 S17 102.87(19) . . S11 Sn8 O3 79.4(3) . . S18 Sn8 S11 116.56(17) . . S18 Sn8 S17 100.76(10) . . S18 Sn8 O3 79.92(15) . . S12 Sn8 S11 116.11(10) . . S12 Sn8 S18 118.12(17) . . S12 Sn8 S17 97.0(2) . . S12 Sn8 O3 80.1(2) . . S17 Sn8 O3 176.9(3) . . S15 Sn4 S5 145.99(12) . . S11 Sn4 S15 100.55(13) . . S11 Sn4 S5 101.82(11) . . S7 Sn4 S15 101.57(13) . . S7 Sn4 S11 95.79(15) . . S7 Sn4 S5 101.29(12) . . O3 Sn4 S15 77.9(2) . . O3 Sn4 S11 86.0(2) . . O3 Sn4 S5 78.4(2) . . O3 Sn4 S7 178.2(2) . . O3 Sn4 O1 92.5(3) . . O1 Sn4 S15 79.6(2) . . O1 Sn4 S11 178.4(3) . . O1 Sn4 S5 77.4(2) . . O1 Sn4 S7 85.7(3) . . S2 Sn2 S6 101.53(12) . . S2 Sn2 S3 94.65(10) . . S2 Sn2 S5 101.23(12) . . S3 Sn2 S6 101.46(13) . . S3 Sn2 S5 101.11(13) . . S5 Sn2 S6 146.30(7) . . O2 Sn2 S2 179.3(2) . . O2 Sn2 S6 77.9(2) . . O2 Sn2 S3 85.8(3) . . O2 Sn2 S5 79.1(2) . . O1 Sn2 S2 86.4(3) . . O1 Sn2 S6 79.4(2) . . O1 Sn2 S3 178.4(3) . . O1 Sn2 S5 77.5(2) . . O1 Sn2 O2 93.1(2) . . S13 Sn10 S14 117.94(11) . . S13 Sn10 S20 92.31(13) . . S13 Sn10 O4 79.6(3) . . S14 Sn10 S20 106.16(13) . . S14 Sn10 O4 78.0(3) . . S20 Sn10 O4 171.9(3) . . S19 Sn10 S13 116.49(18) . . S19 Sn10 S14 114.77(18) . . S19 Sn10 S20 104.74(11) . . S19 Sn10 O4 79.12(16) . . Sn9 S15 Sn5 86.72(13) . . Sn9 S15 Sn4 87.27(12) . . Sn4 S15 Sn5 86.10(12) . . Sn1 S2 Sn2 93.17(13) . . Sn8 S11 Sn4 93.02(13) . . Sn8 S18 Sn9 93.29(9) . . Sn7 S6 Sn5 86.26(8) . . Sn7 S6 Sn2 86.73(10) . . Sn2 S6 Sn5 85.69(10) . . Sn10 S13 Sn5 93.75(14) . . Sn8 S12 Sn6 93.11(14) . . Sn3 S9 Sn6 92.63(14) . . Sn3 S3 Sn2 92.14(14) . . Sn1 S8 Sn5 92.64(14) . . Sn3 S10 Sn7 93.38(15) . . Sn10 S14 Sn7 94.58(16) . . CIV S20 Sn10 100.2(8) . . CII S4 Sn3 100.7(8) . . Sn4 S5 Sn6 86.06(7) . . Sn2 S5 Sn6 86.19(9) . . Sn2 S5 Sn4 86.39(9) . . Sn10 S19 Sn9 93.95(9) . . Sn6 S16 Sn9 86.20(12) . . Sn7 S16 Sn9 85.72(12) . . Sn7 S16 Sn6 86.76(12) . . Sn1 S7 Sn4 93.71(14) . . CIII S17 Sn8 99.9(9) . . CI S1 Sn1 99.0(8) . . Sn6 O2 Sn3 101.8(3) . . Sn7 O2 Sn6 116.3(4) . . Sn7 O2 Sn3 101.7(3) . . Sn7 O2 Sn2 116.4(4) . . Sn2 O2 Sn6 115.5(4) . . Sn2 O2 Sn3 101.4(3) . . Sn9 O3 Sn8 100.6(2) . . Sn6 O3 Sn9 116.0(5) . . Sn6 O3 Sn8 100.6(3) . . Sn4 O3 Sn9 116.5(4) . . Sn4 O3 Sn6 117.1(3) . . Sn4 O3 Sn8 101.5(3) . . Sn5 O1 Sn1 100.3(3) . . Sn4 O1 Sn5 115.2(4) . . Sn4 O1 Sn1 101.7(4) . . Sn4 O1 Sn2 118.2(4) . . Sn2 O1 Sn5 116.1(4) . . Sn2 O1 Sn1 100.8(3) . . Sn9 O4 Sn5 116.0(5) . . Sn9 O4 Sn10 100.2(2) . . Sn5 O4 Sn10 99.2(3) . . Sn7 O4 Sn9 117.2(5) . . Sn7 O4 Sn5 117.5(3) . . Sn7 O4 Sn10 101.4(3) . . C1 N1 C3 111.6(15) . . C1 N1 C4 124.0(15) . . C3 N1 C4 124.3(18) . . C1 N2 C2 112.2(17) . . C1 N2 C9 123.3(15) . . C2 N2 C9 124.4(14) . . N1 C1 C8 125.3(14) . . N2 C1 N1 105.9(15) . . N2 C1 C8 128.7(18) . . C2 C3 N1 102.5(19) . . C3 C2 N2 107.6(17) . . N1 C4 C5 114.6(17) . . C6 C5 C4 109.9(17) . . C7 C6 C5 107.4(19) . . F03T B05E F04A 114.8(16) . . F04F B05E F03T 102.7(11) 6 . F04F B05E F03T 102.7(11) . . F04F B05E F04A 115.2(11) . . F04F B05E F04A 115.1(11) 6 . F04F B05E F04F 104.7(18) 6 . F040 B40 F04T 98.7(18) . . F049 B40 F04T 109.6(13) 6 . F049 B40 F04T 109.6(13) . . F049 B40 F040 112.9(13) 6 . F049 B40 F040 112.9(13) . . F049 B40 F049 112(2) . 6 C2A N2A C9A 124.1(18) . . C1A N2A C9A 122.2(18) . . C1A N2A C2A 114(2) . . C3A N1A C4A 126.8(19) . . C1A N1A C3A 107.4(19) . . C1A N1A C4A 125.7(15) . . C3A C2A N2A 106.8(17) . . C2A C3A N1A 107(2) . . C4A C5A C6A 115.2(16) . . N2A C1A N1A 105.5(18) . . N2A C1A C8A 128(2) . . N1A C1A C8A 126.5(18) . . C7A C6A C5A 119.4(17) . . C5A C4A N1A 113.3(15) . . C1B N2B C9B 123(2) . . C1B N2B C2B 111(2) . . C2B N2B C9B 126(2) . . C1B N1B C3B 102(2) . . C1B N1B C4B 112(3) . . C3B N1B C4B 146(3) . . N2B C1B N1B 114(3) . . N2B C1B C8B 113(3) . . N1B C1B C8B 134(3) . . N2B C2B C3B 105(2) . . N1B C3B C2B 108(2) . . C3D N1D C4D 127(3) . . C1D N1D C3D 106(3) . . C1D N1D C4D 127(3) . . C2D N2D C9D 124(2) . . C1D N2D C9D 131(2) . . C1D N2D C2D 105(2) . . N1D C3D C2D 109(3) . . C3D C2D N2D 106(2) . . N1D C1D C8D 109(3) . . N2D C1D N1D 115(2) . . N2D C1D C8D 136(3) . . C2C N2C C1C 108(2) . . C2C N2C C9C 126(2) . . C1C N2C C9C 126(2) . . C1C N1C C3C 95(3) . . C3C C2C N2C 110(3) . . C2C C3C N1C 115(3) . . N2C C1C N1C 112(3) . . N2C C1C C8C 131(3) . . N1C C1C C8C 117(3) . . C1F C1F N1F 85(3) 6_556 6_556 C1F C1F N1F 64.6(16) 6_556 . C1F C1F N2F 38.1(16) 6_556 6_556 C1F C1F N2F 123.5(15) 6_556 . N1F C1F N1F 20(3) 6_556 . N1F C1F N2F 97.4(18) 6_556 . N1F C1F N2F 89(3) 6_556 6_556 N1F C1F N2F 108.0 . . N1F C1F N2F 73.5(4) . 6_556 N2F C1F N2F 85.3(10) . 6_556 C1F N1F C1F 31(3) 6_556 . C1F N1F C3F 108.0 . . C1F N1F C3F 120.1(7) 6_556 . C1F N1F C3F 120.1(8) 6_556 6_556 N1F N1F C1F 95(3) 6_556 6_556 N1F N1F C1F 64.6 6_556 . N1F N1F C3F 73.3 6_556 . N1F N1F C3F 86(4) 6_556 6_556 C3F N1F C1F 115(2) 6_556 . C3F N1F C3F 13(4) 6_556 . N1F C3F N1F 20(3) 6_556 . N1F C3F C2F 95.9(19) 6_556 . N1F C3F C2F 108.0 . . N1F C3F C2F 100(2) 6_556 6_556 N1F C3F C2F 84.9(7) . 6_556 C3F C3F N1F 73.4 6_556 . C3F C3F N1F 94(3) 6_556 6_556 C3F C3F C2F 127.3 6_556 . C3F C3F C2F 44(2) 6_556 6_556 C2F C3F C2F 84(2) . 6_556 C3F C2F C3F 9(3) . 6_556 N2F C2F C3F 106.6(5) . 6_556 N2F C2F C3F 108.0 . . C1F N2F C1F 18.4(17) . 6_556 C1F N2F C2F 108.0 . . C2F N2F C1F 101.3(11) . 6_556 C1E N1E C3E 108.0 . . N1E C1E C8E 139.1(11) . . N2E C1E C8E 112.8(11) . . N2E C1E N1E 108.0 . . C1E N2E C9E 128.1(15) . . C1E N2E C2E 108.0 . . C2E N2E C9E 123.7(15) . . N2E C2E C3E 108.0 . . C2E C3E N1E 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sn9 S15 2.580(4) . Sn9 S18 2.456(3) . Sn9 S19 2.468(2) . Sn9 S16 2.623(5) . Sn9 O3 2.116(6) . Sn9 O4 2.092(6) . Sn5 S15 2.608(4) . Sn5 S6 2.635(4) . Sn5 S13 2.451(4) . Sn5 S8 2.479(4) . Sn5 O1 2.122(8) . Sn5 O4 2.108(10) . Sn6 S12 2.459(4) . Sn6 S9 2.473(4) . Sn6 S5 2.620(4) . Sn6 S16 2.617(4) . Sn6 O2 2.120(9) . Sn6 O3 2.106(10) . Sn7 S6 2.601(4) . Sn7 S10 2.443(5) . Sn7 S14 2.465(4) . Sn7 S16 2.611(4) . Sn7 O2 2.107(8) . Sn7 O4 2.078(10) . Sn1 S2 2.398(4) . Sn1 S8 2.412(4) . Sn1 S7 2.403(4) . Sn1 S1 2.457(5) . Sn1 O1 2.477(9) . Sn3 S9 2.414(5) . Sn3 S3 2.409(5) . Sn3 S10 2.399(4) . Sn3 S4 2.444(5) . Sn3 O2 2.429(9) . Sn8 S11 2.410(5) . Sn8 S18 2.408(3) . Sn8 S12 2.398(4) . Sn8 S17 2.449(3) . Sn8 O3 2.469(6) . Sn4 S15 2.598(4) . Sn4 S11 2.465(4) . Sn4 S5 2.620(4) . Sn4 S7 2.458(4) . Sn4 O3 2.086(10) . Sn4 O1 2.086(9) . Sn2 S2 2.455(4) . Sn2 S6 2.617(2) . Sn2 S3 2.473(4) . Sn2 S5 2.612(2) . Sn2 O2 2.108(8) . Sn2 O1 2.087(9) . Sn10 S13 2.404(5) . Sn10 S14 2.406(5) . Sn10 S20 2.438(3) . Sn10 S19 2.398(3) . Sn10 O4 2.532(5) . S20 CIV 1.70(2) . S4 CII 1.82(2) . S17 CIII 1.66(2) . S1 CI 1.80(2) . N1 C1 1.31(2) . N1 C3 1.43(2) . N1 C4 1.46(2) . N2 C1 1.271(18) . N2 C2 1.38(2) . N2 C9 1.53(2) . C1 C8 1.48(2) . C3 C2 1.33(3) . C4 C5 1.58(3) . C5 C6 1.54(2) . C6 C7 1.51(3) . F03T B05E 1.418(16) . F04A B05E 1.451(16) . F04F B05E 1.399(14) . F04T B40 1.52(3) . F040 B40 1.35(3) . F049 B40 1.341(16) . N2A C9A 1.51(3) . N2A C2A 1.34(2) . N2A C1A 1.28(2) . N1A C3A 1.406(19) . N1A C1A 1.36(2) . N1A C4A 1.48(2) . C8A C1A 1.49(2) . C2A C3A 1.31(3) . C5A C6A 1.54(2) . C5A C4A 1.47(2) . C6A C7A 1.47(2) . C8E C1E 1.426(16) . C9E N2E 1.567(17) . N2B C9B 1.50(3) . N2B C1B 1.23(3) . N2B C2B 1.29(3) . N1B C1B 1.34(3) . N1B C3B 1.35(3) . N1B C4B 1.45(5) . C1B C8B 1.46(4) . C2B C3B 1.39(3) . N1D C3D 1.31(3) . N1D C1D 1.26(3) . N1D C4D 1.61(4) . N2D C9D 1.54(3) . N2D C2D 1.37(3) . N2D C1D 1.25(3) . C3D C2D 1.33(3) . C1D C8D 1.53(4) . N2C C2C 1.28(3) . N2C C1C 1.33(3) . N2C C9C 1.62(4) . N1C C3C 1.46(4) . N1C C1C 1.39(3) . C2C C3C 1.20(4) . C8C C1C 1.68(5) . C1F C1F 0.72(7) 6_556 C1F N1F 1.288(7) 6_556 C1F N1F 1.4200 . C1F N2F 1.4200 . C1F N2F 1.92(4) 6_556 N1F N1F 0.49(7) 6_556 N1F C3F 1.4200 . N1F C3F 1.363(7) 6_556 C3F C3F 0.32(10) 6_556 C3F C2F 1.4200 . C3F C2F 1.63(6) 6_556 C2F N2F 1.4200 . N1E C1E 1.4200 . N1E C3E 1.4200 . C1E N2E 1.4200 . N2E C2E 1.4200 . C2E C3E 1.4200 . 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_4 N1 C3 C2 N2 3(2) . . N1 C4 C5 C6 174.2(14) . . C1 N1 C3 C2 -1(2) . . C1 N1 C4 C5 162.9(16) . . C1 N2 C2 C3 -5(2) . . C3 N1 C1 N2 -2(2) . . C3 N1 C1 C8 -179.1(15) . . C3 N1 C4 C5 -13(2) . . C2 N2 C1 N1 4(2) . . C2 N2 C1 C8 -178.9(16) . . C4 N1 C1 N2 -178.6(14) . . C4 N1 C1 C8 4(3) . . C4 N1 C3 C2 175.9(15) . . C4 C5 C6 C7 169.5(15) . . C9 N2 C1 N1 179.9(14) . . C9 N2 C1 C8 -3(3) . . C9 N2 C2 C3 179.4(15) . . N2A C2A C3A N1A -1(2) . . C9A N2A C2A C3A -178.9(18) . . C9A N2A C1A N1A 179.0(16) . . C9A N2A C1A C8A 2(3) . . C2A N2A C1A N1A -2(2) . . C2A N2A C1A C8A -178.8(19) . . C3A N1A C1A N2A 1(2) . . C3A N1A C1A C8A 177.9(18) . . C3A N1A C4A C5A -16(3) . . C1A N2A C2A C3A 2(2) . . C1A N1A C3A C2A 0(2) . . C1A N1A C4A C5A 167.8(17) . . C6A C5A C4A N1A -171.7(14) . . C4A N1A C3A C2A -177.0(17) . . C4A N1A C1A N2A 178.3(15) . . C4A N1A C1A C8A -5(3) . . C4A C5A C6A C7A -177.3(17) . . C8E C1E N2E C9E 2(2) . . C8E C1E N2E C2E 177.0(13) . . C9E N2E C2E C3E 175.6(19) . . N2B C2B C3B N1B 0.0 . . C9B N2B C1B N1B 180.0 . . C9B N2B C1B C8B 0.0 . . C9B N2B C2B C3B 180.0 . . C1B N2B C2B C3B 0.0 . . C1B N1B C3B C2B 0.0 . . C2B N2B C1B N1B 0.0 . . C2B N2B C1B C8B 180.0 . . C3B N1B C1B N2B 0.0 . . C3B N1B C1B C8B 180.0 . . C4B N1B C1B N2B 180.0 . . C4B N1B C1B C8B 0.0 . . C4B N1B C3B C2B 180.0 . . N1D C3D C2D N2D 0.0 . . C9D N2D C2D C3D 180.0 . . C9D N2D C1D N1D 180.0 . . C9D N2D C1D C8D 0.0 . . C3D N1D C1D N2D 0.0 . . C3D N1D C1D C8D 180.0 . . C2D N2D C1D N1D 0.0 . . C2D N2D C1D C8D 180.0 . . C1D N1D C3D C2D 0.0 . . C1D N2D C2D C3D 0.0 . . C4D N1D C3D C2D 180.0 . . C4D N1D C1D N2D 180.0 . . C4D N1D C1D C8D 0.0 . . N2C C2C C3C N1C 0.0 . . C2C N2C C1C N1C 0.0 . . C2C N2C C1C C8C 180.0 . . C3C N1C C1C N2C 0.0 . . C3C N1C C1C C8C 180.0 . . C1C N2C C2C C3C 0.0 . . C1C N1C C3C C2C 0.0 . . C9C N2C C2C C3C 180.0 . . C9C N2C C1C N1C 180.0 . . C9C N2C C1C C8C 0.0 . . C1F C1F N1F N1F -180.0(17) 6_556 6_556 C1F C1F N1F C3F -119.2(17) 6_556 . C1F C1F N1F C3F -107(4) 6_556 6_556 C1F C1F N2F C2F 71(2) 6_556 . C1F N1F C3F N1F -55.4 . 6_556 C1F N1F C3F N1F -86(4) 6_556 6_556 C1F N1F C3F C3F 94(4) 6_556 6_556 C1F N1F C3F C3F 124.6 . 6_556 C1F N1F C3F C2F -31(4) 6_556 . C1F N1F C3F C2F 51(5) 6_556 6_556 C1F N1F C3F C2F 82(2) . 6_556 C1F N1F C3F C2F 0.0 . . N1F C1F N1F C1F 180.0(17) 6_556 6_556 N1F C1F N1F C3F 73(4) 6_556 6_556 N1F C1F N1F C3F 60.8 6_556 . N1F C1F N2F C1F -71(2) . 6_556 N1F C1F N2F C1F -89(3) 6_556 6_556 N1F C1F N2F C2F -18(3) 6_556 . N1F C1F N2F C2F 0.0 . . N1F N1F C3F C3F 180(100) 6_556 6_556 N1F N1F C3F C2F 55.4 6_556 . N1F N1F C3F C2F 137(2) 6_556 6_556 N1F C3F C2F C3F 99(3) 6_556 6_556 N1F C3F C2F C3F 82.5 . 6_556 N1F C3F C2F N2F 17(2) 6_556 . N1F C3F C2F N2F 0.0 . . C3F N1F C3F N1F 180(100) 6_556 6_556 C3F N1F C3F C2F -43(2) 6_556 6_556 C3F N1F C3F C2F -124.6 6_556 . C3F C3F C2F N2F -82.5 6_556 . C3F C2F N2F C1F 8(3) 6_556 6_556 C3F C2F N2F C1F 17.7(15) . 6_556 C3F C2F N2F C1F 0.0 . . C3F C2F N2F C1F -9(3) 6_556 . C2F C3F C2F C3F 0.0 6_556 6_556 C2F C3F C2F N2F -82.5 6_556 . N2F C1F N1F C1F 39.9(18) 6_556 6_556 N2F C1F N1F C1F 119.2(17) . 6_556 N2F C1F N1F N1F -60.8 . 6_556 N2F C1F N1F N1F -140.1(10) 6_556 6_556 N2F C1F N1F C3F 12(4) . 6_556 N2F C1F N1F C3F -79.3(10) 6_556 . N2F C1F N1F C3F -68(4) 6_556 6_556 N2F C1F N1F C3F 0.0 . . N2F C1F N2F C1F 0(2) 6_556 6_556 N2F C1F N2F C2F 71.0 6_556 . N1E C1E N2E C9E -175(2) . . N1E C1E N2E C2E 0.0 . . C1E N1E C3E C2E 0.0 . . C1E N2E C2E C3E 0.0 . . N2E C2E C3E N1E 0.0 . . C3E N1E C1E C8E -175.8(18) . . C3E N1E C1E N2E 0.0 . . loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 -0.188 0.250 -0.104 2178.2 206.4 2 0.188 0.750 -0.583 2178.2 210.6