#------------------------------------------------------------------------------ #$Date: 2021-09-23 01:11:52 +0300 (Thu, 23 Sep 2021) $ #$Revision: 269243 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564704.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_1564704 loop_ _publ_author_name 'Yi, Xiaofeng' 'Wang, Di' 'Li, Fan' 'Zhang, Jian' 'Zhang, Lei' _publ_section_title ; Molecular Bixbyite-Like In12-Oxo Clusters with Tunable Functionalization Sites for Lithography Patterning Applications ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04491E _journal_year 2021 _chemical_formula_moiety 'C56 H72 Br4 In12 N12 O34, Br2' _chemical_formula_sum 'C56 H68 Br6 In12 N12 O34' _chemical_formula_weight 3310.52 _chemical_name_systematic InOC-4 _space_group_crystal_system tetragonal _space_group_IT_number 82 _space_group_name_Hall 'I -4' _space_group_name_H-M_alt 'I -4' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2021-01-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-04-19 deposited with the CCDC. 2021-09-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.1018(4) _cell_length_b 16.1018(4) _cell_length_c 20.4257(8) _cell_measurement_reflns_used 4191 _cell_measurement_temperature 100.01(12) _cell_measurement_theta_max 74.2080 _cell_measurement_theta_min 3.3990 _cell_volume 5295.7(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.01(12) _diffrn_detector_area_resol_mean 10.3468 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 0.00 121.00 1.00 1.50 -- 41.41 19.00 0.00 121 2 \w 104.00 178.00 1.00 3.00 -- 108.23 111.00 120.00 74 3 \w 103.00 178.00 1.00 3.00 -- 108.23 77.00-120.00 75 4 \w 104.00 178.00 1.00 3.00 -- 108.23 111.00-120.00 74 5 \w 82.00 178.00 1.00 3.00 -- 108.23 45.00-150.00 96 6 \w 17.00 63.00 1.00 1.50 -- 41.41 38.00 120.00 46 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_unetI/netI 0.0464 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 7312 _diffrn_reflns_point_group_measured_fraction_full 0.925 _diffrn_reflns_point_group_measured_fraction_max 0.925 _diffrn_reflns_theta_full 66.582 _diffrn_reflns_theta_max 66.582 _diffrn_reflns_theta_min 3.495 _exptl_absorpt_coefficient_mu 23.728 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.11403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellowish _exptl_crystal_colour_modifier yellowish _exptl_crystal_density_diffrn 2.076 _exptl_crystal_description block _exptl_crystal_F_000 3116 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.712 _refine_diff_density_min -2.140 _refine_diff_density_rms 0.291 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 276 _refine_ls_number_reflns 4325 _refine_ls_number_restraints 156 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0759 _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^)+(0.1519P)^2^+83.3473P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1999 _refine_ls_wR_factor_ref 0.2069 _reflns_Friedel_coverage 0.789 _reflns_Friedel_fraction_full 0.844 _reflns_Friedel_fraction_max 0.844 _reflns_number_gt 4108 _reflns_number_total 4325 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04491e2.cif _cod_data_source_block InOC-4 _cod_database_code 1564704 _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_estimated_absorpt_t_max 0.330 _shelx_estimated_absorpt_t_min 0.163 _olex2_refinement_description ; 1. Others Fixed Sof: Br2(0.5) Fixed U13: O5(0) Fixed U23: O5(0) Fixed Uiso: H2(0.061) H1(0.072) H2A(0.071) H3(0.067) H5(0.094) H6(0.079) H9A(0.064) H9B(0.064) H10A(0.063) H10B(0.063) H11A(0.075) H11B(0.075) H12A(0.099) H12B(0.099) H13A(0.046) H13B(0.046) H14A(0.06) H14B(0.06) Fixed X: O5(0.5) H2(0.149709) H1(0.103788) H2A(0.368003) H3(0.323131) H5(0.10551) H6(0.154146) H9A(0.082368) H9B(0.139736) H10A(0.195157) H10B(0.206809) H11A(0.260938) H11B(0.199844) H12A(0.356978) H12B(0.295813) H13A(0.317532) H13B(0.352543) H14A(0.223309) H14B(0.184085) Fixed Y: O5(0.5) H2(0.457623) H1(0.512638) H2A(0.524177) H3(0.520814) H5(0.414917) H6(0.417364) H9A(0.616112) H9B(0.64395) H10A(0.598067) H10B(0.685853) H11A(0.414926) H11B(0.354432) H12A(0.349793) H12B(0.300012) H13A(0.634046) H13B(0.543348) H14A(0.540013) H14B(0.58655) Fixed Z: H2(0.667508) H1(0.572869) H2A(0.285078) H3(0.176024) H5(0.239286) H6(0.343136) H9A(0.490236) H9B(0.548332) H10A(0.421687) H10B(0.45441) H11A(0.7522) H11B(0.716189) H12A(0.709513) H12B(0.665231) H13A(0.702716) H13B(0.705796) H14A(0.751849) H14B(0.691714) ; _shelx_res_file ; TITL e10-1_a.res in I-4 e10-1_sq.res created by SHELXL-2017/1 at 20:47:13 on 24-Jan-2021 REM Old TITL E10-1 in I-4 REM SHELXT solution in I-4 REM R1 0.173, Rweak 0.025, Alpha 0.040, Orientation as input REM Flack x = 0.014 ( 0.028 ) from Parsons' quotients REM Formula found by SHELXT: C28 N4 O17 Br2 In6 CELL 1.54184 16.1018 16.1018 20.4257 90 90 90 ZERR 2 0.0004 0.0004 0.0008 0 0 0 LATT -2 SYMM -X,-Y,+Z SYMM +Y,-X,-Z SYMM -Y,+X,-Z SFAC C H Br In N O UNIT 112 136 12 24 24 68 DFIX 1.5 C12 C11 DELU ISOR 0.01 0.02 C12 N2 C14 O6 C9 O5 ISOR 0.01 0.02 O3 ISOR 0.001 0.002 C8 ISOR 0.01 0.02 C3 C6 ISOR 0.01 0.02 O5 O6 ISOR 0.001 0.002 O5 ISOR 0.001 0.002 O6 L.S. 10 0 73 PLAN 2 SIZE 0.06 0.1 0.12 ABIN conf fmap 2 53 acta SHEL 999 0.84 REM REM REM WGHT 0.151900 83.347305 FVAR 0.10617 IN1 4 0.267869 0.476091 0.568218 11.00000 0.02192 0.06264 = 0.01753 0.00000 0.00137 -0.00193 IN2 4 0.387660 0.544980 0.433570 11.00000 0.02559 0.02764 = 0.00963 -0.00084 -0.00314 0.00219 IN3 4 0.348775 0.683785 0.557648 11.00000 0.04627 0.04134 = 0.02389 -0.00872 0.00238 0.02112 BR1 3 0.242409 0.773860 0.617875 11.00000 0.08285 0.08824 = 0.05513 -0.02154 0.00941 0.05594 O2 6 0.227662 0.492187 0.085065 11.00000 0.22369 0.08318 = 0.05606 0.00820 0.00124 0.01863 O1 6 0.100898 0.470348 0.123339 11.00000 0.16587 0.11446 = 0.06110 -0.02013 -0.06539 0.01428 O3 6 0.299768 0.462748 0.383207 11.00000 0.02917 0.04966 = 0.01830 0.00328 -0.01010 -0.00419 O4 6 0.390272 0.654140 0.375011 11.00000 0.04826 0.03160 = 0.01938 0.00437 -0.01047 0.00638 O5 6 0.500000 0.500000 0.391598 10.50000 0.01668 0.01695 = 0.01658 0.00000 0.00000 0.00075 O6 6 0.446326 0.628835 0.497896 11.00000 0.02176 0.02121 = 0.02078 -0.00077 -0.00042 0.00084 O9 6 0.225388 0.367851 0.516744 11.00000 0.05690 0.07037 = 0.03245 -0.00689 0.00419 -0.02259 O7 6 0.281754 0.598906 0.491952 11.00000 0.03360 0.05394 = 0.02036 -0.00304 -0.00320 0.01337 O8 6 0.323760 0.579624 0.617892 11.00000 0.05222 0.04324 = 0.02150 -0.01398 0.00719 -0.00067 N2 5 0.209854 0.464984 0.672013 11.00000 0.04614 0.07407 = 0.03117 -0.00203 0.01672 -0.00248 AFIX 13 H2 2 0.149709 0.457623 0.667508 11.00000 -1.20000 AFIX 0 N1 5 0.140597 0.516990 0.534814 11.00000 0.03113 0.09863 = 0.04918 0.00807 0.00199 0.00312 AFIX 13 H1 2 0.103788 0.512638 0.572869 11.00000 -1.20000 AFIX 0 N3 5 0.175566 0.478758 0.132630 11.00000 0.15462 0.06813 = 0.05686 -0.01709 -0.02962 -0.01209 C1 1 0.269247 0.464307 0.322304 11.00000 0.03910 0.10536 = 0.02117 -0.01316 -0.00507 -0.00593 C2 1 0.316950 0.500811 0.274397 11.00000 0.10838 0.04073 = 0.02895 -0.00211 0.00026 -0.02035 AFIX 43 H2A 2 0.368003 0.524177 0.285078 11.00000 -1.20000 AFIX 0 C3 1 0.288801 0.502815 0.209779 11.00000 0.08663 0.04723 = 0.03382 -0.00512 0.00661 -0.00079 AFIX 43 H3 2 0.323131 0.520814 0.176024 11.00000 -1.20000 AFIX 0 C4 1 0.210304 0.477853 0.197784 11.00000 0.08623 0.06450 = 0.04753 -0.01032 -0.00835 0.02315 C5 1 0.157047 0.437739 0.249228 11.00000 0.05636 0.12899 = 0.04975 -0.01909 -0.02461 -0.01857 AFIX 43 H5 2 0.105510 0.414917 0.239286 11.00000 -1.20000 AFIX 0 C6 1 0.187115 0.436606 0.308967 11.00000 0.05761 0.08406 = 0.05687 0.00487 -0.02663 -0.01087 AFIX 43 H6 2 0.154146 0.417364 0.343136 11.00000 -1.20000 AFIX 0 C7 1 0.134586 0.371480 0.504921 11.00000 0.05204 0.08747 = 0.06355 0.03438 -0.00872 -0.03941 C8 1 0.110402 0.455212 0.485676 11.00000 0.07031 0.07130 = 0.07075 -0.00008 -0.00050 -0.00040 C9 1 0.135703 0.606827 0.511067 11.00000 0.03526 0.07570 = 0.04884 -0.01313 -0.00764 0.01347 AFIX 23 H9A 2 0.082368 0.616112 0.490236 11.00000 -1.20000 H9B 2 0.139736 0.643950 0.548332 11.00000 -1.20000 AFIX 0 C10 1 0.204722 0.626602 0.462826 11.00000 0.03362 0.04476 = 0.08025 0.00117 -0.00837 0.01472 AFIX 23 H10A 2 0.195157 0.598067 0.421687 11.00000 -1.20000 H10B 2 0.206809 0.685853 0.454410 11.00000 -1.20000 AFIX 0 C11 1 0.243388 0.395192 0.709518 11.00000 0.06584 0.08063 = 0.04065 0.02560 0.02495 -0.01627 AFIX 23 H11A 2 0.260938 0.414926 0.752200 11.00000 -1.20000 H11B 2 0.199844 0.354432 0.716189 11.00000 -1.20000 AFIX 0 C12 1 0.313081 0.355651 0.677319 11.00000 0.06608 0.09247 = 0.08881 0.02892 0.01014 0.01430 AFIX 23 H12A 2 0.356978 0.349793 0.709513 11.00000 -1.20000 H12B 2 0.295813 0.300012 0.665231 11.00000 -1.20000 AFIX 0 C13 1 0.310632 0.578259 0.685639 11.00000 0.03716 0.05263 = 0.02514 -0.00211 0.00101 0.01654 AFIX 23 H13A 2 0.317532 0.634046 0.702716 11.00000 -1.20000 H13B 2 0.352543 0.543348 0.705796 11.00000 -1.20000 AFIX 0 C14 1 0.226135 0.546684 0.704704 11.00000 0.04708 0.07274 = 0.03061 -0.00800 0.00945 0.00116 AFIX 23 H14A 2 0.223309 0.540013 0.751849 11.00000 -1.20000 H14B 2 0.184085 0.586550 0.691714 11.00000 -1.20000 AFIX 0 BR2 3 0.000890 0.554886 0.649564 10.50000 0.02860 0.59584 = 0.06075 -0.13743 0.02024 -0.05094 HKLF 4 REM e10-1_a.res in I-4 REM R1 = 0.0759 for 4108 Fo > 4sig(Fo) and 0.0793 for all 4325 data REM 276 parameters refined using 156 restraints END WGHT 0.1520 83.3573 REM Highest difference peak 1.712, deepest hole -2.140, 1-sigma level 0.291 Q1 1 0.2392 0.5025 0.5408 11.00000 0.05 1.71 Q2 1 0.3966 0.5828 0.4644 11.00000 0.05 1.64 ; _shelx_res_checksum 52929 _shelx_hkl_file ; 0 0 2 7186.81 63.30 0 0 4 1079.52 22.37 0 0 6 1891.97 32.61 0 0 8 2331.81 38.16 0 0 10 934.60 24.43 0 0 12 31.31 5.07 0 0 14 1971.49 42.53 0 0 -16 4548.49 59.95 0 0 -18 1139.77 30.12 0 0 -20 199.87 13.01 0 0 -22 1520.70 34.96 0 0 -24 378.33 13.58 -1 0 -25 83.39 5.27 -1 0 -23 484.04 17.74 1 0 -23 420.77 16.10 -1 0 -21 376.04 17.98 1 0 -21 366.27 17.58 -1 0 -19 5.70 2.86 1 0 -19 12.12 3.57 1 0 -17 1151.28 29.14 -1 0 -17 1026.14 28.10 -1 0 -15 1562.59 30.91 1 0 -15 1557.73 30.52 0 -1 15 1498.67 40.53 0 -1 13 403.81 19.39 0 1 11 206.96 10.68 0 -1 11 208.51 13.04 0 -1 9 1158.08 29.27 0 1 9 1102.60 23.70 0 1 7 2375.24 34.62 0 -1 7 2520.19 42.12 0 -1 5 265.39 11.77 0 1 5 270.58 10.35 0 1 3 861.23 18.16 0 -1 3 882.02 18.44 0 -1 1 1981.08 21.22 1 0 1 8044.16 57.91 1 0 3 792.33 13.21 -1 0 3 727.03 22.44 1 0 5 172.56 7.88 -1 0 5 175.35 10.50 1 0 7 2715.00 40.28 -1 0 7 2889.05 43.60 1 0 9 1221.07 28.14 -1 0 9 1212.91 27.61 1 0 11 162.17 10.80 -1 0 11 145.39 9.84 1 0 13 430.86 19.35 0 1 -15 1402.18 29.77 0 -1 -15 1345.89 28.84 0 1 -17 1143.73 29.14 0 -1 -17 1156.16 28.71 0 1 -19 9.42 2.43 0 -1 -19 15.89 3.86 0 -1 -21 397.72 18.48 0 1 -21 416.07 18.35 0 -1 -23 442.58 16.84 0 1 -23 472.75 17.25 1 1 -24 87.92 6.33 -1 -1 -24 103.94 7.32 1 1 -22 214.74 12.70 -1 -1 -22 218.60 13.14 1 1 -20 107.19 9.70 -1 -1 -20 94.91 9.22 1 1 -18 210.56 12.79 -1 -1 -18 193.00 12.30 1 1 -16 993.45 25.82 1 -1 16 944.56 33.92 -1 -1 -16 891.34 24.83 1 -1 14 899.12 31.27 1 -1 12 12.79 3.85 1 -1 10 157.79 11.37 -1 1 8 814.90 20.44 1 -1 8 867.40 24.21 1 -1 6 1639.03 29.91 -1 1 6 1615.64 30.17 1 -1 4 308.02 10.29 1 -1 2 1544.94 20.60 -1 -1 0 994.06 12.92 1 -1 0 823.41 13.13 1 1 2 1239.88 12.26 1 1 4 320.24 8.92 1 1 6 1709.09 27.33 -1 -1 6 1989.22 38.45 1 1 8 871.15 20.59 -1 -1 8 1048.99 27.37 1 1 10 87.03 6.75 -1 -1 10 93.99 8.26 1 1 12 11.73 2.91 -1 -1 12 9.58 3.07 -1 -1 14 637.17 24.52 1 -1 -16 924.24 24.40 -1 1 -16 904.20 24.64 1 -1 -18 227.72 13.07 -1 1 -18 209.16 13.19 1 -1 -20 93.20 9.17 -1 1 -20 87.28 8.62 -1 1 -22 233.69 13.52 1 -1 -22 210.68 12.55 -1 1 -24 133.56 8.40 -2 1 -25 16.91 2.66 -2 1 -23 31.60 4.87 -2 1 -21 4.57 3.12 2 -1 -21 4.58 2.62 2 -1 -19 7.25 2.51 -2 1 -19 4.07 2.52 -2 1 -17 52.38 6.62 2 -1 -17 61.73 6.60 2 -1 -15 182.94 10.06 -2 1 -15 166.85 10.35 -1 -2 15 164.40 13.49 -1 -2 13 89.01 9.81 -1 -2 11 18.69 4.38 1 2 11 19.82 3.03 1 2 9 247.95 9.71 -1 -2 9 292.19 15.97 -1 -2 7 175.23 12.34 1 2 7 158.37 6.94 1 2 5 517.03 11.54 -1 -2 3 256.71 15.09 1 2 1 1083.25 13.43 -1 -2 1 928.89 29.05 2 -1 1 1065.02 17.62 -2 1 1 1022.41 16.27 2 -1 3 315.15 9.87 2 -1 5 401.30 12.90 2 -1 7 174.43 9.73 2 -1 9 312.27 15.63 2 -1 11 32.67 5.82 2 -1 13 104.00 10.86 2 -1 15 173.50 14.73 1 2 -15 143.65 9.29 -1 -2 -15 148.17 9.38 1 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16.77 3.55 4 -10 10 25.58 9.13 10 4 -8 57.00 6.11 -4 10 8 61.00 12.98 4 -10 8 62.24 12.34 4 -10 6 42.31 9.99 4 -10 4 8.60 3.81 4 -10 2 2.48 3.50 4 -10 0 15.71 5.51 4 -10 -2 8.10 3.82 4 -10 -6 46.16 6.14 4 -10 -6 47.83 9.06 4 -10 -6 40.68 6.06 4 -10 -8 61.30 9.28 4 -10 -8 56.03 6.32 4 -10 -8 59.67 7.12 4 -10 -10 17.58 3.24 4 -10 -10 15.97 4.72 4 -10 -12 84.02 8.82 4 -10 -14 63.55 6.88 -4 10 -16 12.64 2.68 -4 10 -18 9.77 2.59 -4 10 -20 3.84 1.83 10 5 -19 56.69 5.55 10 5 -17 52.40 5.96 -10 -5 -17 37.01 5.27 -10 -5 -15 5.56 2.28 10 5 -15 11.90 3.71 10 5 -13 73.16 7.49 -10 -5 -13 79.51 9.21 10 5 -11 52.20 6.17 -10 -5 -11 52.11 7.89 10 5 -9 62.62 6.71 -5 10 9 48.49 12.36 -10 -5 -9 78.37 9.62 5 -10 9 75.85 14.37 5 -10 7 14.96 5.32 10 5 -7 16.50 3.66 5 -10 5 176.68 19.64 5 -10 3 369.82 28.03 5 -10 1 93.69 14.13 5 -10 -1 96.15 13.69 5 -10 -3 354.65 26.35 5 -10 -5 158.12 11.66 5 -10 -5 157.99 16.73 5 -10 -5 148.61 11.00 5 -10 -7 4.50 2.17 5 -10 -7 8.96 4.19 5 -10 -7 6.38 2.68 5 -10 -9 48.91 8.65 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-2 -19 -3 88.70 4.68 -2 -19 -5 18.43 1.93 -2 -19 -7 5.27 0.94 -1 -19 2 4.80 1.21 -1 -19 0 7.34 1.61 -1 -19 -2 5.57 1.27 -1 -19 -4 1.29 0.85 -1 -19 -6 2.54 0.77 -1 -19 -8 5.73 0.88 0 -19 3 2.34 0.92 0 -19 1 0.67 0.86 0 -19 -1 -1.51 1.37 0 -19 -3 0.28 1.01 0 -19 -5 15.39 1.87 0 -19 -7 0.83 0.42 1 -19 2 19.36 2.79 1 -19 0 -1.92 1.28 1 -19 -2 18.92 2.47 1 -19 -4 10.17 1.68 1 -19 -6 7.27 1.23 1 -19 -8 1.92 0.56 2 -19 3 118.11 6.39 2 -19 1 47.75 4.35 2 -19 -1 36.29 3.55 2 -19 -3 105.66 5.40 2 -19 -5 49.84 3.24 2 -19 -7 21.76 1.79 3 -19 2 105.71 6.46 3 -19 0 6.96 1.73 3 -19 -2 88.84 5.13 3 -19 -4 126.80 5.43 3 -19 -6 53.57 3.00 4 -19 3 124.29 6.56 4 -19 1 23.87 2.98 4 -19 -1 19.62 2.49 4 -19 -1 17.43 2.58 4 -19 -3 103.70 5.01 4 -19 -3 112.14 5.61 4 -19 -5 64.75 3.43 5 -19 2 48.32 4.08 5 -19 0 19.13 2.47 5 -19 0 18.15 2.67 5 -19 -2 42.54 3.22 5 -19 -2 41.66 3.52 5 -19 -4 96.05 4.26 5 -19 -4 105.58 4.71 6 -19 1 45.66 3.62 6 -19 -1 49.49 3.42 6 -19 -1 45.03 3.58 6 -19 -3 91.97 4.10 6 -19 -3 95.54 4.54 0 -20 -2 17.29 1.71 0 0 0 0.00 0.00 TITL E10-1 in I-4 REM I-4 (#82 in standard setting) CELL 1.54184 16.101775 16.101775 20.425746 90.0000 90.0000 90.0000 ZERR 59.00 0.000363 0.000363 0.000762 0.0000 0.0000 0.0000 LATT -2 SYMM -x,-y, z SYMM y,-x,-z SYMM -y, x,-z SFAC C N O Br In UNIT 59.00 59.00 59.00 59.00 59.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 51524 _shelx_fab_file ; 1 1 0 242.11 -1.56 0 2 0 57.24 -1.69 2 2 0 -29.81 -0.67 -1 3 0 -106.70 -0.43 1 3 0 -10.58 -1.31 3 3 0 -18.13 -0.39 -2 4 0 -59.34 0.43 0 4 0 -20.68 -0.24 2 4 0 17.15 -0.52 4 4 0 -2.91 -0.15 -3 5 0 -20.76 0.67 -1 5 0 4.69 0.48 1 5 0 19.73 -0.13 3 5 0 1.23 0.04 5 5 0 2.92 0.03 -4 6 0 -9.49 0.34 -2 6 0 10.38 0.37 0 6 0 33.49 0.16 2 6 0 -5.05 -0.01 4 6 0 11.08 0.27 6 6 0 6.17 0.15 -5 7 0 -0.76 0.26 -3 7 0 1.44 0.13 -1 7 0 36.03 -0.15 1 7 0 7.38 0.02 3 7 0 1.68 0.55 5 7 0 19.52 0.33 7 7 0 -0.39 -0.08 -6 8 0 6.67 0.10 -4 8 0 2.63 0.00 -2 8 0 13.99 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-3 5 22 2.66 -1.90 -3 7 22 -4.31 1.48 4 6 22 -2.76 -2.79 4 4 22 1.84 3.00 -4 6 22 0.17 -1.67 5 5 22 4.48 0.37 0 1 23 0.98 -0.58 0 3 23 6.36 -2.60 0 5 23 5.32 -5.65 1 6 23 3.55 -6.89 1 4 23 5.40 -3.05 1 2 23 -0.33 2.15 -1 2 23 4.59 -5.25 -1 4 23 3.77 -3.22 -1 6 23 0.18 -1.08 2 5 23 5.03 -5.95 2 3 23 -0.72 0.30 -2 3 23 1.50 -5.12 -2 5 23 -3.10 2.37 3 4 23 3.56 -4.90 -3 4 23 -1.26 -0.36 0 0 24 7.88 0.16 0 2 24 1.93 1.51 1 1 24 5.14 -3.06 2 2 24 2.89 -4.60 -9 17 0 -1.84 -0.02 9 17 0 -2.91 0.07 -3 19 0 0.80 -0.04 3 19 0 3.09 -0.14 -12 15 1 3.37 -0.55 12 15 1 1.11 4.33 -9 17 2 -1.71 -1.32 9 17 2 -1.03 -0.26 -3 19 2 -1.31 0.52 3 19 2 0.30 2.03 -13 14 3 -1.77 -3.19 13 14 3 -1.98 3.67 -2 19 3 3.67 0.93 2 19 3 0.75 0.06 -6 18 4 1.29 -0.03 6 18 4 -1.68 3.45 -1 19 4 -1.67 -1.88 1 19 4 0.06 -3.12 -8 17 5 -0.55 -1.80 8 17 5 2.81 2.66 -11 15 6 2.03 3.83 11 15 6 0.40 1.86 -9 16 7 -1.42 -1.51 9 16 7 -2.54 4.81 -2 18 8 -0.25 -0.86 2 18 8 0.03 -0.84 -9 15 10 2.08 1.24 9 15 10 -2.35 -2.41 -2 17 11 0.98 3.36 2 17 11 0.70 2.27 -11 12 13 1.54 4.08 11 12 13 1.80 3.71 -3 16 13 -1.82 -4.51 3 16 13 -4.82 -1.53 -9 13 14 -4.47 -3.26 9 13 14 -0.57 0.00 -5 15 14 -0.95 3.38 5 15 14 -0.83 -2.83 -8 13 15 1.92 2.63 8 13 15 -3.12 -0.05 -2 15 15 1.39 -3.37 2 15 15 3.62 -5.30 -4 14 16 -2.14 1.86 4 14 16 -0.49 0.69 -7 12 17 -6.65 -0.06 7 12 17 -0.77 2.86 -7 11 18 0.19 1.44 7 11 18 -2.43 -2.76 -1 13 18 -2.27 -4.52 1 13 18 -1.32 0.83 -8 9 19 -2.32 7.83 8 9 19 -3.25 -3.04 -7 10 19 4.11 2.89 7 10 19 4.39 -0.37 -1 12 19 2.44 3.95 1 12 19 -3.09 -0.71 -1 11 20 0.24 -3.08 1 11 20 2.38 -0.31 -4 9 21 -2.06 -3.09 4 9 21 -5.43 -0.30 6 6 22 3.83 0.28 -2 8 22 -2.60 2.40 2 8 22 -1.45 -2.75 -4 5 23 -1.05 -1.45 4 5 23 1.12 -2.49 -1 3 24 -1.01 6.22 1 3 24 1.26 -1.17 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 281019) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 582 261 ' ' 2 0.500 0.500 1.000 582 261 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL e10-1 I -4 R = 0.08 CELL 16.1018 16.1018 20.4257 90.00 90.00 90.00 SPGR I-4 # Solvent Accessible Volume = 1166 # Electrons Found in S.A.V. = 522 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.139 0.970 0.340 ! 4.36 eA-3 C102 0.861 0.981 0.389 ! 3.89 eA-3 C103 0.161 0.884 0.376 ! 3.70 eA-3 C104 0.859 0.023 0.465 ! 3.10 eA-3 C105 0.154 0.890 0.436 ! 2.90 eA-3 C106 0.244 0.926 0.359 ! 2.48 eA-3 C107 0.500 0.496 0.250 ! 2.47 eA-3 C108 0.392 0.301 0.101 ! 2.16 eA-3 C109 0.780 0.997 0.411 ! 2.04 eA-3 Q110 0.451 0.280 0.194 ! 1.97 eA-3 Q111 0.266 1.007 0.032 ! 1.91 eA-3 C112 0.885 0.094 0.405 ! 1.87 eA-3 C113 0.437 0.424-0.004 ! 1.74 eA-3 Q114 0.265 1.001 0.095 ! 1.72 eA-3 Q115 0.846 0.136 0.097 ! 1.71 eA-3 Q116 0.498 0.298 0.407 ! 1.68 eA-3 Q117 0.919 0.908 0.098 ! 1.67 eA-3 Q118 0.813 0.196 0.094 ! 1.55 eA-3 Q119 0.329 0.385 0.487 ! 1.51 eA-3 Q120 0.255 0.065 0.091 ! 1.49 eA-3 Q121 0.592 0.418 0.459 ! 1.49 eA-3 C122 0.379 0.421 0.104 ! 1.47 eA-3 Q123 0.501 0.306 0.013 ! 1.46 eA-3 Q124 0.998 0.873 0.109 ! 1.46 eA-3 Q125 0.498 0.373 0.609 ! 1.46 eA-3 Q126 0.308 0.467 0.607 ! 1.43 eA-3 Q127 0.808 0.967 0.107 ! 1.43 eA-3 Q128 0.379 0.654 0.532 ! 1.42 eA-3 C129 0.357 0.323 0.012 ! 1.40 eA-3 Q130 0.252 0.059 0.046 ! 1.39 eA-3 Q131 0.350 0.560 0.468 ! 1.36 eA-3 Q132 0.499 0.300 0.453 ! 1.35 eA-3 Q133 0.709 0.690 0.467 ! 1.35 eA-3 Q134 0.638 0.591 0.122 ! 1.31 eA-3 Q135 0.550 0.297 0.457 ! 1.30 eA-3 Q136 0.301 0.454 0.544 ! 1.30 eA-3 C137 0.079 0.886 0.459 ! 1.30 eA-3 Q138 0.419 0.519 0.453 ! 1.30 eA-3 C139 0.500 0.495 0.187 ! 1.29 eA-3 Q140 0.272 0.357 0.483 ! 1.28 eA-3 C141 0.547 0.390 0.047 ! 1.27 eA-3 C142 0.821 0.158 0.331 ! 1.26 eA-3 Q143 0.424 0.362 0.593 ! 1.20 eA-3 Q144 0.924 0.862 0.093 ! 1.20 eA-3 Q145 0.858 0.076 0.904 ! 1.20 eA-3 C146 0.279 0.328 0.125 ! 1.18 eA-3 C147 0.947 0.981 0.342 ! 1.18 eA-3 Q148 0.578 0.481 0.404 ! 1.17 eA-3 Q149 0.078 0.981 0.904 ! 1.17 eA-3 Q150 0.061 0.818 0.453 ! 1.16 eA-3 Q151 0.774 0.273 0.098 ! 1.16 eA-3 Q152 0.948 0.218 0.467 ! 1.16 eA-3 Q153 0.261 0.759 0.152 ! 1.16 eA-3 C154 0.449 0.440 0.080 ! 1.15 eA-3 Q155 0.484 0.099 0.134 ! 1.15 eA-3 Q156 0.350 0.602 0.031 ! 1.14 eA-3 Q157 1.004 0.121 0.035 ! 1.12 eA-3 Q158 0.559 0.294 0.408 ! 1.08 eA-3 Q159 0.266 0.980 0.329 ! 1.08 eA-3 Q160 0.763 0.674 0.110 ! 1.06 eA-3 Q161 0.266 0.234 0.402 ! 1.06 eA-3 Q162 0.732 0.941 0.344 ! 1.03 eA-3 Q163 0.237 0.829 0.423 ! 1.02 eA-3 Q164 0.539 0.933 0.189 ! 1.01 eA-3 C165 0.593 0.364-0.002 ! 1.00 eA-3 C166 0.500 0.503 0.110 ! 0.99 eA-3 Q167 0.838 0.894 0.449 ! 0.99 eA-3 Q168 0.793 0.797 0.339 ! 0.97 eA-3 Q169 0.720 0.305-0.005 ! 0.97 eA-3 Q170 0.826 0.988 0.298 ! 0.96 eA-3 Q171 0.407 0.407 0.215 ! 0.95 eA-3 Q172 0.545 1.009 0.325 ! 0.94 eA-3 Q173 0.280 0.328 0.190 ! 0.94 eA-3 Q174 0.704 0.339 0.032 ! 0.94 eA-3 Q175 0.525 0.378 0.237 ! 0.93 eA-3 Q176 0.841 0.052 0.281 ! 0.93 eA-3 C177 0.923 0.026 0.298 ! 0.92 eA-3 Q178 0.362 0.233 0.173 ! 0.92 eA-3 Q179 0.374 0.336 0.218 ! 0.91 eA-3 Q180 0.576 0.232 0.323 ! 0.91 eA-3 C181 0.405 0.478 0.014 ! 0.91 eA-3 Q182 0.015 0.614 0.019 ! 0.90 eA-3 C183 0.313 0.269 0.159 ! 0.89 eA-3 Q184 0.999 0.305 0.223 ! 0.88 eA-3 Q185 0.359 0.260 0.225 ! 0.88 eA-3 Q186 0.127 0.441 0.454 ! 0.82 eA-3 Q187 0.282 0.261 0.087 ! 0.80 eA-3 Q188 0.483 0.758 0.017 ! 0.80 eA-3 Q189 0.719 0.308 0.072 ! 0.79 eA-3 C190 0.596 0.453 0.043 ! 0.77 eA-3 Q191 0.688 0.094 0.407 ! 0.76 eA-3 Q192 0.751 0.962 0.501 ! 0.75 eA-3 Q193 0.390 0.477 0.079 ! 0.75 eA-3 Q194 0.418 0.659 0.487 ! 0.75 eA-3 Q195 0.375 0.212 0.072 ! 0.74 eA-3 Q196 0.408 0.501 0.190 ! 0.74 eA-3 Q197 0.029 0.026 0.220 ! 0.74 eA-3 C198 0.591 0.423 0.071 ! 0.74 eA-3 Q199 0.768 0.251 0.205 ! 0.73 eA-3 ) ; _shelx_fab_checksum 5299 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+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 In1 In 0.26787(8) 0.47609(11) 0.56822(7) 0.0340(4) Uani 1 1 d . U . . . In2 In 0.38766(8) 0.54498(8) 0.43357(6) 0.0210(4) Uani 1 1 d . U . . . In3 In 0.34877(10) 0.68379(10) 0.55765(7) 0.0372(4) Uani 1 1 d . U . . . Br1 Br 0.2424(2) 0.7739(3) 0.61787(17) 0.0754(12) Uani 1 1 d . U . . . O2 O 0.228(3) 0.492(2) 0.0851(15) 0.121(11) Uani 1 1 d . U . . . O1 O 0.101(3) 0.470(2) 0.1233(15) 0.114(10) Uani 1 1 d . U . . . O3 O 0.2998(9) 0.4627(10) 0.3832(7) 0.032(3) Uani 1 1 d . U . . . O4 O 0.3903(10) 0.6541(9) 0.3750(7) 0.033(3) Uani 1 1 d . U . . . O5 O 0.500000 0.500000 0.3916(9) 0.017(3) Uani 1 2 d S TU P . . O6 O 0.4463(8) 0.6288(8) 0.4979(6) 0.021(2) Uani 1 1 d . U . . . O9 O 0.2254(12) 0.3679(13) 0.5167(9) 0.053(4) Uani 1 1 d . U . . . O7 O 0.2818(9) 0.5989(10) 0.4920(7) 0.036(3) Uani 1 1 d . U . . . O8 O 0.3238(11) 0.5796(10) 0.6179(8) 0.039(3) Uani 1 1 d . U . . . N2 N 0.2099(15) 0.4650(16) 0.6720(10) 0.050(4) Uani 1 1 d . U . . . H2 H 0.149709 0.457623 0.667508 0.061 Uiso 1 1 calc R . . . . N1 N 0.1406(14) 0.5170(19) 0.5348(12) 0.060(4) Uani 1 1 d . U . . . H1 H 0.103788 0.512638 0.572869 0.072 Uiso 1 1 calc R . . . . N3 N 0.176(3) 0.479(2) 0.1326(16) 0.093(9) Uani 1 1 d . U . . . C1 C 0.2692(16) 0.464(2) 0.3223(12) 0.055(7) Uani 1 1 d . U . . . C2 C 0.317(2) 0.5008(17) 0.2744(13) 0.059(7) Uani 1 1 d . U . . . H2A H 0.368003 0.524177 0.285078 0.071 Uiso 1 1 calc R . . . . C3 C 0.289(2) 0.5028(18) 0.2098(14) 0.056(6) Uani 1 1 d . U . . . H3 H 0.323131 0.520814 0.176024 0.067 Uiso 1 1 calc R . . . . C4 C 0.210(2) 0.478(2) 0.1978(16) 0.066(6) Uani 1 1 d . U . . . C5 C 0.157(2) 0.438(3) 0.2492(17) 0.078(10) Uani 1 1 d . U . . . H5 H 0.105510 0.414917 0.239286 0.094 Uiso 1 1 calc R . . . . C6 C 0.187(2) 0.437(2) 0.3090(16) 0.066(7) Uani 1 1 d . U . . . H6 H 0.154146 0.417364 0.343136 0.079 Uiso 1 1 calc R . . . . C7 C 0.1346(19) 0.371(2) 0.5049(17) 0.068(7) Uani 1 1 d . U . . . C8 C 0.110(2) 0.455(2) 0.486(2) 0.071(6) Uani 1 1 d . U . . . C9 C 0.1357(16) 0.607(2) 0.5111(15) 0.053(5) Uani 1 1 d . U . . . H9A H 0.082368 0.616112 0.490236 0.064 Uiso 1 1 calc R . . . . H9B H 0.139736 0.643950 0.548332 0.064 Uiso 1 1 calc R . . . . C10 C 0.2047(15) 0.6266(17) 0.4628(17) 0.053(6) Uani 1 1 d . U . . . H10A H 0.195157 0.598067 0.421687 0.063 Uiso 1 1 calc R . . . . H10B H 0.206809 0.685853 0.454410 0.063 Uiso 1 1 calc R . . . . C11 C 0.2434(19) 0.395(2) 0.7095(14) 0.062(7) Uani 1 1 d D U . . . H11A H 0.260938 0.414926 0.752200 0.075 Uiso 1 1 calc R . . . . H11B H 0.199844 0.354432 0.716189 0.075 Uiso 1 1 calc R . . . . C12 C 0.313(2) 0.356(3) 0.677(2) 0.082(9) Uani 1 1 d D U . . . H12A H 0.356978 0.349793 0.709513 0.099 Uiso 1 1 calc R . . . . H12B H 0.295813 0.300012 0.665231 0.099 Uiso 1 1 calc R . . . . C13 C 0.3106(14) 0.5783(16) 0.6856(11) 0.038(4) Uani 1 1 d . U . . . H13A H 0.317532 0.634046 0.702716 0.046 Uiso 1 1 calc R . . . . H13B H 0.352543 0.543348 0.705796 0.046 Uiso 1 1 calc R . . . . C14 C 0.2261(16) 0.5467(19) 0.7047(13) 0.050(5) Uani 1 1 d . U . . . H14A H 0.223309 0.540013 0.751849 0.060 Uiso 1 1 calc R . . . . H14B H 0.184085 0.586550 0.691714 0.060 Uiso 1 1 calc R . . . . Br2 Br 0.0009(6) 0.5549(14) 0.6496(4) 0.228(15) Uani 0.5 1 d . U . . . 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 In1 0.0219(7) 0.0626(10) 0.0175(7) 0.0000(7) 0.0014(6) -0.0019(6) In2 0.0256(6) 0.0276(6) 0.0096(6) -0.0008(5) -0.0031(5) 0.0022(4) In3 0.0463(9) 0.0413(8) 0.0239(7) -0.0087(6) 0.0024(6) 0.0211(7) Br1 0.083(2) 0.088(2) 0.0551(19) -0.0215(18) 0.0094(17) 0.056(2) O2 0.22(3) 0.083(18) 0.056(12) 0.008(15) 0.001(18) 0.02(2) O1 0.17(2) 0.11(2) 0.061(15) -0.020(16) -0.065(16) 0.01(2) O3 0.029(6) 0.050(7) 0.018(5) 0.003(5) -0.010(5) -0.004(5) O4 0.048(9) 0.032(6) 0.019(6) 0.004(6) -0.010(6) 0.006(6) O5 0.017(3) 0.017(3) 0.017(3) 0.000 0.000 0.0008(14) O6 0.022(3) 0.021(3) 0.021(3) -0.0008(14) -0.0004(14) 0.0008(14) O9 0.057(9) 0.070(9) 0.032(8) -0.007(7) 0.004(8) -0.023(7) O7 0.034(6) 0.054(8) 0.020(6) -0.003(5) -0.003(5) 0.013(6) O8 0.052(9) 0.043(7) 0.021(6) -0.014(5) 0.007(6) -0.001(6) N2 0.046(9) 0.074(9) 0.031(7) -0.002(6) 0.017(7) -0.002(7) N1 0.031(8) 0.099(11) 0.049(11) 0.008(9) 0.002(8) 0.003(8) N3 0.15(2) 0.068(18) 0.057(11) -0.017(14) -0.030(13) -0.01(2) C1 0.039(12) 0.11(2) 0.021(8) -0.013(11) -0.005(8) -0.006(13) C2 0.108(19) 0.041(13) 0.029(9) -0.002(10) 0.000(10) -0.020(14) C3 0.087(11) 0.047(10) 0.034(8) -0.005(9) 0.007(8) -0.001(9) C4 0.086(15) 0.065(18) 0.048(10) -0.010(13) -0.008(10) 0.023(14) C5 0.056(16) 0.13(3) 0.050(12) -0.019(17) -0.025(12) -0.019(17) C6 0.058(10) 0.084(13) 0.057(10) 0.005(11) -0.027(9) -0.011(10) C7 0.052(12) 0.087(12) 0.064(18) 0.034(14) -0.009(14) -0.039(12) C8 0.070(6) 0.071(6) 0.071(6) -0.0001(14) -0.0005(14) -0.0004(14) C9 0.035(8) 0.076(9) 0.049(11) -0.013(9) -0.008(8) 0.013(8) C10 0.034(9) 0.045(13) 0.080(19) 0.001(10) -0.008(8) 0.015(8) C11 0.066(16) 0.081(14) 0.041(13) 0.026(12) 0.025(12) -0.016(12) C12 0.066(12) 0.092(14) 0.089(14) 0.029(12) 0.010(11) 0.014(10) C13 0.037(10) 0.053(12) 0.025(8) -0.002(7) 0.001(8) 0.017(8) C14 0.047(10) 0.073(10) 0.031(9) -0.008(8) 0.009(8) 0.001(9) Br2 0.029(3) 0.60(4) 0.061(4) -0.137(12) 0.020(4) -0.051(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 In2 In1 In3 61.59(4) 4_656 4_656 ? O4 In1 In2 38.8(4) 4_656 4_656 ? O4 In1 In3 83.6(4) 4_656 4_656 ? O4 In1 O7 140.0(5) 4_656 . ? O4 In1 N2 72.5(7) 4_656 . ? O4 In1 N1 149.5(8) 4_656 . ? O6 In1 In2 38.3(3) 4_656 4_656 ? O6 In1 In3 39.2(3) 4_656 4_656 ? O6 In1 O4 75.8(5) 4_656 4_656 ? O6 In1 O7 74.0(5) 4_656 . ? O6 In1 N2 148.1(7) 4_656 . ? O6 In1 N1 124.4(7) 4_656 . ? O9 In1 In2 86.3(6) . 4_656 ? O9 In1 In3 37.7(5) . 4_656 ? O9 In1 O4 86.0(7) . 4_656 ? O9 In1 O6 76.3(6) . 4_656 ? O9 In1 O7 111.2(6) . . ? O9 In1 O8 173.8(7) . . ? O9 In1 N2 104.8(8) . . ? O9 In1 N1 78.4(10) . . ? O7 In1 In2 104.3(3) . 4_656 ? O7 In1 In3 89.2(3) . 4_656 ? O8 In1 In2 87.6(5) . 4_656 ? O8 In1 In3 137.2(4) . 4_656 ? O8 In1 O4 90.0(6) . 4_656 ? O8 In1 O6 98.2(6) . 4_656 ? O8 In1 O7 69.3(6) . . ? O8 In1 N2 78.3(8) . . ? O8 In1 N1 107.2(9) . . ? N2 In1 In2 109.9(6) . 4_656 ? N2 In1 In3 137.7(6) . 4_656 ? N2 In1 O7 131.2(7) . . ? N1 In1 In2 160.4(7) . 4_656 ? N1 In1 In3 99.0(7) . 4_656 ? N1 In1 O7 70.5(8) . . ? N1 In1 N2 86.2(9) . . ? In1 In2 In3 174.19(5) 3_566 4_656 ? O3 In2 In1 144.7(4) . 3_566 ? O3 In2 In3 40.4(4) . 4_656 ? O3 In2 O7 89.6(6) . . ? O4 In2 In1 40.4(4) . 3_566 ? O4 In2 In3 144.3(4) . 4_656 ? O4 In2 O3 104.4(6) . . ? O4 In2 O5 92.2(5) . . ? O4 In2 O6 170.7(5) . 4_656 ? O4 In2 O7 89.7(6) . . ? O5 In2 In1 86.57(4) . 3_566 ? O5 In2 In3 89.57(5) . 4_656 ? O5 In2 O3 98.9(5) . . ? O5 In2 O6 96.7(4) . 4_656 ? O5 In2 O7 170.6(5) . . ? O6 In2 In1 137.2(3) 4_656 3_566 ? O6 In2 In1 40.2(3) . 3_566 ? O6 In2 In3 136.1(3) . 4_656 ? O6 In2 In3 39.1(3) 4_656 4_656 ? O6 In2 O3 77.2(5) 4_656 . ? O6 In2 O3 165.5(5) . . ? O6 In2 O4 79.2(5) . . ? O6 In2 O5 95.1(4) . . ? O6 In2 O6 97.1(4) . 4_656 ? O6 In2 O7 76.3(5) . . ? O6 In2 O7 81.1(5) 4_656 . ? O7 In2 In1 88.9(4) . 3_566 ? O7 In2 In3 94.3(4) . 4_656 ? In2 In3 In1 63.26(4) 3_566 3_566 ? Br1 In3 In1 129.88(12) . 3_566 ? Br1 In3 In2 142.74(11) . 3_566 ? O3 In3 In1 83.4(4) 3_566 3_566 ? O3 In3 In2 40.0(4) 3_566 3_566 ? O3 In3 Br1 103.0(4) 3_566 . ? O6 In3 In1 39.6(3) . 3_566 ? O6 In3 In2 38.2(3) . 3_566 ? O6 In3 Br1 169.3(4) . . ? O6 In3 O3 75.9(5) . 3_566 ? O6 In3 O7 76.1(5) . . ? O9 In3 In1 38.0(5) 3_566 3_566 ? O9 In3 In2 97.9(6) 3_566 3_566 ? O9 In3 Br1 92.9(5) 3_566 . ? O9 In3 O3 100.8(7) 3_566 3_566 ? O9 In3 O6 77.0(6) 3_566 . ? O9 In3 O7 93.6(7) 3_566 . ? O7 In3 In1 88.7(4) . 3_566 ? O7 In3 In2 106.3(4) . 3_566 ? O7 In3 Br1 108.5(4) . . ? O7 In3 O3 144.6(5) . 3_566 ? O8 In3 In1 137.7(4) . 3_566 ? O8 In3 In2 82.9(5) . 3_566 ? O8 In3 Br1 92.4(4) . . ? O8 In3 O3 86.3(6) . 3_566 ? O8 In3 O6 98.1(6) . . ? O8 In3 O9 170.0(7) . 3_566 ? O8 In3 O7 76.6(6) . . ? In2 O3 In3 99.6(6) . 4_656 ? C1 O3 In2 131.4(18) . . ? C1 O3 In3 124.6(19) . 4_656 ? In2 O4 In1 100.8(6) . 3_566 ? C12 O4 In1 117.8(17) 3_566 3_566 ? C12 O4 In2 141.3(18) 3_566 . ? In2 O5 In2 132.5(9) . 2_665 ? In2 O6 In1 101.5(5) . 3_566 ? In2 O6 In1 109.6(5) 3_566 3_566 ? In2 O6 In2 131.5(7) . 3_566 ? In2 O6 In3 106.6(5) . . ? In2 O6 In3 102.7(5) 3_566 . ? In3 O6 In1 101.2(5) . 3_566 ? In3 O9 In1 104.3(8) 4_656 . ? C7 O9 In1 111(2) . . ? C7 O9 In3 124.5(18) . 4_656 ? In2 O7 In1 95.3(6) . . ? In3 O7 In1 98.8(5) . . ? In3 O7 In2 101.0(6) . . ? C10 O7 In1 114.8(15) . . ? C10 O7 In2 123.4(16) . . ? C10 O7 In3 118.7(15) . . ? In3 O8 In1 114.8(7) . . ? C13 O8 In1 113.0(15) . . ? C13 O8 In3 128.0(15) . . ? C11 N2 In1 112.9(15) . . ? C11 N2 C14 112(2) . . ? C14 N2 In1 105.6(15) . . ? C8 N1 In1 108(2) . . ? C8 N1 C9 114(2) . . ? C9 N1 In1 114.8(17) . . ? O2 N3 C4 116(4) . . ? O1 N3 O2 122(4) . . ? O1 N3 C4 121(4) . . ? O3 C1 C2 118(2) . . ? O3 C1 C6 121(3) . . ? C2 C1 C6 121(3) . . ? C1 C2 C3 120(3) . . ? C4 C3 C2 118(3) . . ? N3 C4 C5 115(3) . . ? C3 C4 N3 122(4) . . ? C3 C4 C5 122(3) . . ? C6 C5 C4 116(3) . . ? C5 C6 C1 121(3) . . ? C8 C7 O9 110(2) . . ? C7 C8 N1 110(3) . . ? C10 C9 N1 112(2) . . ? O7 C10 C9 107(2) . . ? C12 C11 N2 113(2) . . ? O4 C12 C11 120(3) 4_656 . ? O8 C13 C14 113(2) . . ? N2 C14 C13 110(2) . . ? 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 In1 In2 3.3331(18) 4_656 ? In1 In3 3.379(2) 4_656 ? In1 O4 2.198(15) 4_656 ? In1 O6 2.195(12) 4_656 ? In1 O9 2.147(19) . ? In1 O7 2.527(16) . ? In1 O8 2.149(16) . ? In1 N2 2.32(2) . ? In1 N1 2.26(2) . ? In2 In3 3.3670(19) 4_656 ? In2 O3 2.194(14) . ? In2 O4 2.126(14) . ? In2 O5 2.129(7) . ? In2 O6 2.134(12) 4_656 ? In2 O6 2.108(12) . ? In2 O7 2.255(15) . ? In3 Br1 2.559(3) . ? In3 O3 2.213(16) 3_566 ? In3 O6 2.177(13) . ? In3 O9 2.131(19) 3_566 ? In3 O7 2.198(16) . ? In3 O8 2.119(17) . ? O2 N3 1.30(5) . ? O1 N3 1.22(5) . ? O3 C1 1.34(3) . ? O4 C12 1.32(4) 3_566 ? O9 C7 1.48(4) . ? O7 C10 1.45(3) . ? O8 C13 1.40(3) . ? N2 C11 1.46(4) . ? N2 C14 1.50(4) . ? N1 C8 1.49(5) . ? N1 C9 1.53(4) . ? N3 C4 1.44(5) . ? C1 C2 1.38(4) . ? C1 C6 1.42(4) . ? C2 C3 1.40(4) . ? C3 C4 1.35(5) . ? C4 C5 1.50(5) . ? C5 C6 1.31(4) . ? C7 C8 1.46(5) . ? C9 C10 1.52(4) . ? C11 C12 1.45(3) . ? C13 C14 1.50(4) . ? Br2 Br2 1.77(5) 2_565 ? 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 In1 O9 C7 C8 41(3) . . . . ? In1 O7 C10 C9 30(3) . . . . ? In1 O8 C13 C14 -37(2) . . . . ? In1 N2 C11 C12 8(4) . . . . ? In1 N2 C14 C13 -38(2) . . . . ? In1 N1 C8 C7 38(3) . . . . ? In1 N1 C9 C10 48(3) . . . . ? In2 O3 C1 C2 27(4) . . . . ? In2 O3 C1 C6 -147(3) . . . . ? In2 O7 C10 C9 144.9(19) . . . . ? In3 O3 C1 C2 -124(3) 4_656 . . . ? In3 O3 C1 C6 62(4) 4_656 . . . ? In3 O9 C7 C8 -85(3) 4_656 . . . ? In3 O7 C10 C9 -87(2) . . . . ? In3 O8 C13 C14 119(2) . . . . ? O2 N3 C4 C3 11(5) . . . . ? O2 N3 C4 C5 -162(3) . . . . ? O1 N3 C4 C3 -167(3) . . . . ? O1 N3 C4 C5 20(5) . . . . ? O3 C1 C2 C3 179(3) . . . . ? O3 C1 C6 C5 -180(4) . . . . ? O9 C7 C8 N1 -54(4) . . . . ? O8 C13 C14 N2 52(3) . . . . ? N2 C11 C12 O4 9(5) . . . 4_656 ? N1 C9 C10 O7 -50(3) . . . . ? N3 C4 C5 C6 -180(4) . . . . ? C1 C2 C3 C4 8(5) . . . . ? C2 C1 C6 C5 7(6) . . . . ? C2 C3 C4 N3 179(3) . . . . ? C2 C3 C4 C5 -8(5) . . . . ? C3 C4 C5 C6 8(6) . . . . ? C4 C5 C6 C1 -6(6) . . . . ? C6 C1 C2 C3 -7(5) . . . . ? C8 N1 C9 C10 -76(3) . . . . ? C9 N1 C8 C7 167(3) . . . . ? C11 N2 C14 C13 86(3) . . . . ? C14 N2 C11 C12 -111(3) . . . . ?