#------------------------------------------------------------------------------ #$Date: 2024-07-05 17:10:15 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292873 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/16/1571699.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_1571699 loop_ _publ_author_name 'Zhou, Lei' 'Li, Kailei' 'Chang, Yuanyuan' 'Yao, Yuan' 'Peng, Yuqi' 'Li, Ming' 'He, Rongxing' _publ_section_title ; High-efficiency color-tunable ultralong room-temperature phosphorescence from organic--inorganic metal halides via synergistic inter/intramolecular interactions ; _journal_issue 26 _journal_name_full 'Chemical Science' _journal_page_first 10046 _journal_page_last 10055 _journal_paper_doi 10.1039/D4SC01630K _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'Cl6 In, H2 O, H3 O, 2(C8 H10 N O)' _chemical_formula_sum 'C16 H25 Cl6 In N2 O4' _chemical_formula_weight 636.90 _chemical_name_common A2H3OInCl6,H2O _chemical_name_systematic A2H3OInCl6,H2O _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2022-12-17 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-12-27 deposited with the CCDC. 2024-05-21 downloaded from the CCDC. ; _cell_angle_alpha 89.703(4) _cell_angle_beta 88.498(4) _cell_angle_gamma 82.907(4) _cell_formula_units_Z 2 _cell_length_a 7.3505(6) _cell_length_b 9.0364(6) _cell_length_c 18.5560(14) _cell_measurement_reflns_used 6092 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 59.73 _cell_measurement_theta_min 4.29 _cell_volume 1222.67(16) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2019)' _computing_data_collection 'APEX4 V2022.1-1 (Bruker, 2022)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE Metaljet PHOTON II' _diffrn_measurement_method '\w and \f shutterless scans' _diffrn_measurement_specimen_support 'nylon loop' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_unetI/netI 0.0633 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.944 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5088 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.458 _diffrn_reflns_theta_min 2.072 _diffrn_source MetalJet _diffrn_source_current 2.86 _diffrn_source_power 0.19937059999999998 _diffrn_source_type 'Liquid Metal source' _diffrn_source_voltage 69.71 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 9.430 _exptl_absorpt_correction_T_max 0.154453 _exptl_absorpt_correction_T_min 0.042795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.1254 before and 0.0821 after correction. For component 2: wR2(int) was 0.1079 before and 0.0635 after correction. The Ratio of minimum to maximum transmission is 0.28. Final HKLF 4 output contains 16300 reflections, Rint = 0.0954 (9755 with I > 3sig(I), Rint = 0.0875) ; _exptl_crystal_density_diffrn 1.730 _exptl_crystal_description block _exptl_crystal_F_000 636 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.512 _refine_diff_density_min -1.889 _refine_diff_density_rms 0.192 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 5088 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0694 _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^)+(0.1670P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1914 _refine_ls_wR_factor_ref 0.2136 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4237 _reflns_number_total 5088 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01630k2.cif _cod_data_source_block 221215_wqangz_300899_0m_5 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1571699--1571704.cif. ; _cod_database_code 1571699 _shelx_shelxl_version_number 2019/2 _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 0.452 _shelx_estimated_absorpt_t_min 0.374 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.494(3) 0.506(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H) groups 3.a Riding coordinates: O4(H4A,H4B), O3(H3A,H3B,H3C) 3.b Aromatic/amide H refined with riding coordinates: C7(H7), C4(H4), C15(H15), C6(H6), C5(H5), C12(H12), C13(H13), C14(H14) 3.c Idealised Me refined as rotating group: N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), C1(H1D,H1E,H1F), C9(H9A,H9B,H9C) ; _shelx_res_file ; TITL 221215_wqangz_300899_0m_4_a.res in P-1 221215_wqangz_300899_0m_5.res created by SHELXL-2019/2 at 17:09:44 on 17-Dec-2022 REM Old TITL 221215_WQANGZ_300899_0m_4 in P-1 REM SHELXT solution in P-1: R1 0.250, Rweak 0.019, Alpha 0.050 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C16 N2 O10 In CELL 1.34139 7.3505 9.0364 18.556 89.703 88.498 82.907 ZERR 2 0.0006 0.0006 0.0014 0.004 0.004 0.004 LATT 1 SFAC C H Cl In N O DISP C 0.0137 0.0067 57.1 DISP Cl 0.3281 0.5435 4162.2 DISP H 0 0 0.6 DISP In 0.1167 3.9932 30756.5 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 UNIT 32 50 12 2 4 8 L.S. 10 PLAN 10 SIZE 0.1 0.12 0.13 TEMP -80.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT -1 -1 18 OMIT 5 -5 7 OMIT -4 -1 8 OMIT -1 -1 17 OMIT -3 4 6 OMIT 4 2 9 OMIT 1 1 17 OMIT -5 5 6 OMIT -4 7 9 REM REM REM WGHT 0.167000 BASF 0.50635 FVAR 0.53083 IN1 4 0.767237 0.098359 0.250224 11.00000 0.03991 0.02760 = 0.02798 0.00014 -0.00170 -0.00335 CL2 3 0.547213 0.067951 0.150904 11.00000 0.04703 0.03696 = 0.03234 -0.00052 -0.00757 -0.00362 CL3 3 0.645676 0.375332 0.252809 11.00000 0.04870 0.02653 = 0.04101 -0.00042 -0.00271 -0.00125 CL5 3 0.536266 0.063295 0.348520 11.00000 0.04411 0.03631 = 0.03276 0.00286 0.00376 -0.00152 CL1 3 0.855201 -0.179249 0.247116 11.00000 0.05872 0.02764 = 0.04521 -0.00237 -0.00198 -0.00071 CL4 3 0.995642 0.130524 0.345662 11.00000 0.04546 0.04491 = 0.03249 -0.00706 -0.00866 -0.00452 CL6 3 1.007509 0.144449 0.158843 11.00000 0.04512 0.04187 = 0.04003 0.00499 0.00871 -0.00452 O4 6 0.054280 0.481849 0.247355 11.00000 0.04380 0.03821 = 0.07446 0.00193 -0.00776 -0.00434 AFIX 3 H4A 2 -0.064640 0.493199 0.252245 11.00000 -1.50000 H4B 2 0.081970 0.571309 0.239085 11.00000 -1.50000 AFIX 0 O3 6 0.288867 0.880910 0.249891 11.00000 0.08834 0.05603 = 0.04472 -0.00993 -0.00741 -0.01712 AFIX 3 H3A 2 0.324977 0.837360 0.289841 11.00000 -1.50000 H3B 2 0.275037 0.813700 0.217761 11.00000 -1.50000 H3C 2 0.197437 0.951470 0.254451 11.00000 -1.50000 AFIX 0 O1 6 0.289202 0.675541 0.133560 11.00000 0.10487 0.03598 = 0.03552 -0.00254 -0.00533 0.00088 O2 6 0.273001 0.665253 0.364176 11.00000 0.09630 0.04142 = 0.03918 0.00481 0.00568 -0.00906 N2 5 0.278215 0.372828 0.366332 11.00000 0.06370 0.04386 = 0.01994 0.00319 -0.00222 0.00210 AFIX 137 H2A 2 0.211907 0.451573 0.344606 11.00000 -1.20000 H2B 2 0.232168 0.287222 0.354901 11.00000 -1.20000 H2C 2 0.397388 0.366818 0.350844 11.00000 -1.20000 AFIX 0 N1 5 0.309667 0.382779 0.135613 11.00000 0.05814 0.03178 = 0.04047 0.00950 -0.00579 0.00265 AFIX 137 H1A 2 0.357985 0.286841 0.144117 11.00000 -1.20000 H1B 2 0.200349 0.402538 0.159964 11.00000 -1.20000 H1C 2 0.388230 0.445717 0.150839 11.00000 -1.20000 AFIX 0 C8 1 0.280662 0.404644 0.056210 11.00000 0.03458 0.03338 = 0.02880 -0.00073 -0.00261 0.00324 C3 1 0.258367 0.543050 0.026645 11.00000 0.04235 0.02649 = 0.03191 0.00883 -0.00671 -0.00530 C16 1 0.267515 0.393036 0.442698 11.00000 0.04111 0.03830 = 0.03603 -0.00597 -0.00628 -0.00119 C7 1 0.283909 0.274897 0.017173 11.00000 0.04149 0.03230 = 0.05823 0.00040 0.00039 0.00111 AFIX 43 H7 2 0.301091 0.180431 0.040380 11.00000 -1.20000 AFIX 0 C10 1 0.256137 0.673926 0.428832 11.00000 0.05293 0.02767 = 0.03845 -0.00107 -0.00259 -0.00694 C4 1 0.232025 0.552055 -0.047725 11.00000 0.05194 0.03281 = 0.02968 0.00756 -0.00481 -0.00521 AFIX 43 H4 2 0.211614 0.647164 -0.070181 11.00000 -1.20000 AFIX 0 C11 1 0.253936 0.536249 0.473203 11.00000 0.03554 0.04284 = 0.03940 0.01035 -0.00647 -0.00430 C15 1 0.258167 0.269358 0.485304 11.00000 0.05204 0.03255 = 0.02462 0.00118 -0.00459 -0.00352 AFIX 43 H15 2 0.258355 0.174408 0.463543 11.00000 -1.20000 AFIX 0 C6 1 0.261611 0.285345 -0.056470 11.00000 0.05390 0.04111 = 0.04669 -0.00215 -0.00125 -0.01272 AFIX 43 H6 2 0.264148 0.198116 -0.085020 11.00000 -1.20000 AFIX 0 C5 1 0.235127 0.427489 -0.088256 11.00000 0.06095 0.05234 = 0.03463 0.00431 -0.00256 -0.00652 AFIX 43 H5 2 0.219193 0.436393 -0.138801 11.00000 -1.20000 AFIX 0 C2 1 0.254919 0.682916 0.068773 11.00000 0.05849 0.04998 = 0.04411 -0.00501 0.01063 -0.01256 C12 1 0.241427 0.544547 0.548774 11.00000 0.04881 0.03554 = 0.04396 0.00422 -0.00569 -0.00586 AFIX 43 H12 2 0.233210 0.639402 0.571288 11.00000 -1.20000 AFIX 0 C13 1 0.240728 0.416559 0.591973 11.00000 0.06652 0.03543 = 0.02295 0.00411 0.00481 0.00260 AFIX 43 H13 2 0.234920 0.424112 0.643047 11.00000 -1.20000 AFIX 0 C14 1 0.248528 0.281689 0.559234 11.00000 0.06031 0.04741 = 0.02963 0.00861 0.00290 0.00000 AFIX 43 H14 2 0.247307 0.194367 0.587884 11.00000 -1.20000 AFIX 0 C1 1 0.214508 0.833162 0.033711 11.00000 0.06594 0.02907 = 0.06689 0.00767 -0.01269 0.00038 AFIX 137 H1D 2 0.164561 0.906672 0.069979 11.00000 -1.50000 H1E 2 0.124772 0.827933 -0.004044 11.00000 -1.50000 H1F 2 0.327826 0.862906 0.012323 11.00000 -1.50000 AFIX 0 C9 1 0.234472 0.821104 0.463579 11.00000 0.08174 0.03597 = 0.03505 0.00811 -0.00313 -0.01508 AFIX 137 H9A 2 0.247224 0.898275 0.427132 11.00000 -1.50000 H9B 2 0.328908 0.823713 0.499706 11.00000 -1.50000 H9C 2 0.112841 0.839437 0.487062 11.00000 -1.50000 AFIX 0 HKLF 5 REM 221215_wqangz_300899_0m_4_a.res in P-1 REM wR2 = 0.2136, GooF = S = 1.035, Restrained GooF = 1.035 for all data REM R1 = 0.0694 for 4237 Fo > 4sig(Fo) and 0.0844 for all 5088 data REM 267 parameters refined using 0 restraints END WGHT 0.1670 0.0000 REM Highest difference peak 1.512, deepest hole -1.889, 1-sigma level 0.192 Q1 1 0.8984 0.0947 0.2419 11.00000 0.05 1.51 Q2 1 0.7495 0.1486 0.1976 11.00000 0.05 1.37 Q3 1 0.7810 0.0661 0.3069 11.00000 0.05 1.34 Q4 1 0.7387 0.1116 0.2631 11.00000 0.05 1.24 Q5 1 0.6267 0.1075 0.2607 11.00000 0.05 1.20 Q6 1 0.8708 0.1400 0.1765 11.00000 0.05 1.08 Q7 1 0.8996 -0.0214 0.2097 11.00000 0.05 1.02 Q8 1 0.7617 0.1420 0.2879 11.00000 0.05 0.99 Q9 1 0.7757 0.0578 0.2230 11.00000 0.05 0.93 Q10 1 0.6580 0.0678 0.3288 11.00000 0.05 0.84 ; _shelx_res_checksum 89659 _olex2_submission_special_instructions 'No special instructions were received' _site XU loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.76724(10) 0.09836(5) 0.25022(5) 0.0319(2) Uani 1 1 d . . . . . Cl2 Cl 0.5472(3) 0.0680(3) 0.15090(15) 0.0388(6) Uani 1 1 d . . . . . Cl3 Cl 0.6457(3) 0.3753(2) 0.2528(2) 0.0390(5) Uani 1 1 d . . . . . Cl5 Cl 0.5363(3) 0.0633(3) 0.34852(15) 0.0381(6) Uani 1 1 d . . . . . Cl1 Cl 0.8552(4) -0.1792(2) 0.2471(2) 0.0442(6) Uani 1 1 d . . . . . Cl4 Cl 0.9956(4) 0.1305(3) 0.34566(15) 0.0409(6) Uani 1 1 d . . . . . Cl6 Cl 1.0075(4) 0.1444(3) 0.15884(16) 0.0426(6) Uani 1 1 d . . . . . O4 O 0.0543(9) 0.4818(6) 0.2474(6) 0.0521(17) Uani 1 1 d . . . . . H4A H -0.064640 0.493199 0.252245 0.078 Uiso 1 1 d R U . . . H4B H 0.081970 0.571309 0.239085 0.078 Uiso 1 1 d R U . . . O3 O 0.2889(11) 0.8809(7) 0.2499(6) 0.062(2) Uani 1 1 d . . . . . H3A H 0.324977 0.837360 0.289841 0.093 Uiso 1 1 d R U . . . H3B H 0.275037 0.813700 0.217761 0.093 Uiso 1 1 d R U . . . H3C H 0.197437 0.951470 0.254451 0.093 Uiso 1 1 d R U . . . O1 O 0.2892(15) 0.6755(11) 0.1336(5) 0.060(3) Uani 1 1 d . . . . . O2 O 0.2730(15) 0.6653(11) 0.3642(5) 0.059(3) Uani 1 1 d . . . . . N2 N 0.2782(14) 0.3728(12) 0.3663(4) 0.043(2) Uani 1 1 d . . . . . H2A H 0.211907 0.451573 0.344606 0.052 Uiso 1 1 calc R U . . . H2B H 0.232168 0.287222 0.354901 0.052 Uiso 1 1 calc R U . . . H2C H 0.397388 0.366818 0.350844 0.052 Uiso 1 1 calc R U . . . N1 N 0.3097(14) 0.3828(12) 0.1356(5) 0.044(2) Uani 1 1 d . . . . . H1A H 0.357985 0.286841 0.144117 0.053 Uiso 1 1 calc R U . . . H1B H 0.200349 0.402538 0.159964 0.053 Uiso 1 1 calc R U . . . H1C H 0.388230 0.445717 0.150839 0.053 Uiso 1 1 calc R U . . . C8 C 0.2807(15) 0.4046(14) 0.0562(5) 0.033(2) Uani 1 1 d . . . . . C3 C 0.2584(15) 0.5430(12) 0.0266(6) 0.033(2) Uani 1 1 d . . . . . C16 C 0.2675(16) 0.3930(14) 0.4427(6) 0.039(2) Uani 1 1 d . . . . . C7 C 0.2839(16) 0.2749(14) 0.0172(8) 0.045(3) Uani 1 1 d . . . . . H7 H 0.301091 0.180431 0.040380 0.053 Uiso 1 1 calc R U . . . C10 C 0.2561(15) 0.6739(13) 0.4288(6) 0.039(3) Uani 1 1 d . . . . . C4 C 0.2320(15) 0.5521(13) -0.0477(6) 0.038(3) Uani 1 1 d . . . . . H4 H 0.211614 0.647164 -0.070181 0.046 Uiso 1 1 calc R U . . . C11 C 0.2539(14) 0.5362(14) 0.4732(6) 0.039(3) Uani 1 1 d . . . . . C15 C 0.2582(16) 0.2694(13) 0.4853(6) 0.036(2) Uani 1 1 d . . . . . H15 H 0.258355 0.174408 0.463543 0.044 Uiso 1 1 calc R U . . . C6 C 0.2616(17) 0.2853(15) -0.0565(7) 0.047(3) Uani 1 1 d . . . . . H6 H 0.264148 0.198116 -0.085020 0.056 Uiso 1 1 calc R U . . . C5 C 0.2351(17) 0.4275(17) -0.0883(7) 0.049(3) Uani 1 1 d . . . . . H5 H 0.219193 0.436393 -0.138801 0.059 Uiso 1 1 calc R U . . . C2 C 0.2549(17) 0.6829(16) 0.0688(7) 0.051(3) Uani 1 1 d . . . . . C12 C 0.2414(16) 0.5445(14) 0.5488(7) 0.043(3) Uani 1 1 d . . . . . H12 H 0.233210 0.639402 0.571288 0.051 Uiso 1 1 calc R U . . . C13 C 0.2407(17) 0.4166(14) 0.5920(6) 0.042(3) Uani 1 1 d . . . . . H13 H 0.234920 0.424112 0.643047 0.051 Uiso 1 1 calc R U . . . C14 C 0.2485(17) 0.2817(15) 0.5592(6) 0.046(3) Uani 1 1 d . . . . . H14 H 0.247307 0.194367 0.587884 0.056 Uiso 1 1 calc R U . . . C1 C 0.2145(19) 0.8332(14) 0.0337(8) 0.054(3) Uani 1 1 d . . . . . H1D H 0.164561 0.906672 0.069979 0.081 Uiso 1 1 calc R U . . . H1E H 0.124772 0.827933 -0.004044 0.081 Uiso 1 1 calc R U . . . H1F H 0.327826 0.862906 0.012323 0.081 Uiso 1 1 calc R U . . . C9 C 0.2345(19) 0.8211(13) 0.4636(6) 0.050(3) Uani 1 1 d . . . . . H9A H 0.247224 0.898275 0.427132 0.075 Uiso 1 1 calc R U . . . H9B H 0.328908 0.823713 0.499706 0.075 Uiso 1 1 calc R U . . . H9C H 0.112841 0.839437 0.487062 0.075 Uiso 1 1 calc R 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 0.0399(3) 0.0276(3) 0.0280(3) 0.0001(4) -0.0017(3) -0.0033(2) Cl2 0.0470(13) 0.0370(14) 0.0323(14) -0.0005(11) -0.0076(10) -0.0036(10) Cl3 0.0487(13) 0.0265(8) 0.0410(11) -0.0004(13) -0.0027(11) -0.0013(8) Cl5 0.0441(13) 0.0363(14) 0.0328(14) 0.0029(11) 0.0038(9) -0.0015(10) Cl1 0.0587(15) 0.0276(9) 0.0452(12) -0.0024(14) -0.0020(13) -0.0007(9) Cl4 0.0455(13) 0.0449(15) 0.0325(14) -0.0071(11) -0.0087(10) -0.0045(11) Cl6 0.0451(13) 0.0419(15) 0.0400(16) 0.0050(12) 0.0087(10) -0.0045(11) O4 0.044(4) 0.038(3) 0.074(5) 0.002(6) -0.008(4) -0.004(3) O3 0.088(6) 0.056(4) 0.045(4) -0.010(7) -0.007(7) -0.017(4) O1 0.105(7) 0.036(5) 0.036(5) -0.003(4) -0.005(5) 0.001(5) O2 0.096(7) 0.041(6) 0.039(6) 0.005(4) 0.006(5) -0.009(5) N2 0.064(6) 0.044(6) 0.020(5) 0.003(4) -0.002(4) 0.002(5) N1 0.058(6) 0.032(5) 0.040(6) 0.010(4) -0.006(4) 0.003(4) C8 0.035(4) 0.033(5) 0.029(6) -0.001(5) -0.003(4) 0.003(4) C3 0.042(5) 0.026(5) 0.032(6) 0.009(4) -0.007(4) -0.005(4) C16 0.041(5) 0.038(6) 0.036(6) -0.006(5) -0.006(5) -0.001(4) C7 0.041(5) 0.032(6) 0.058(9) 0.000(6) 0.000(5) 0.001(5) C10 0.053(6) 0.028(6) 0.038(7) -0.001(5) -0.003(5) -0.007(5) C4 0.052(6) 0.033(6) 0.030(6) 0.008(5) -0.005(4) -0.005(5) C11 0.036(6) 0.043(7) 0.039(7) 0.010(5) -0.006(4) -0.004(5) C15 0.052(6) 0.033(6) 0.025(6) 0.001(4) -0.005(4) -0.004(5) C6 0.054(7) 0.041(7) 0.047(8) -0.002(6) -0.001(5) -0.013(5) C5 0.061(7) 0.052(8) 0.035(7) 0.004(6) -0.003(5) -0.007(6) C2 0.058(7) 0.050(8) 0.044(8) -0.005(6) 0.011(5) -0.013(6) C12 0.049(6) 0.036(6) 0.044(7) 0.004(5) -0.006(5) -0.006(5) C13 0.067(6) 0.035(6) 0.023(6) 0.004(5) 0.005(5) 0.003(5) C14 0.060(7) 0.047(8) 0.030(7) 0.009(5) 0.003(5) 0.000(5) C1 0.066(8) 0.029(6) 0.067(10) 0.008(6) -0.013(6) 0.000(5) C9 0.082(9) 0.036(7) 0.035(7) 0.008(5) -0.003(6) -0.015(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.1167 3.9932 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 Cl2 In1 Cl3 88.07(10) . . ? Cl5 In1 Cl2 93.66(7) . . ? Cl5 In1 Cl3 87.31(10) . . ? Cl5 In1 Cl1 89.07(11) . . ? Cl5 In1 Cl4 88.52(9) . . ? Cl1 In1 Cl2 87.97(10) . . ? Cl1 In1 Cl3 174.45(8) . . ? Cl1 In1 Cl4 92.16(10) . . ? Cl4 In1 Cl2 177.82(9) . . ? Cl4 In1 Cl3 91.94(10) . . ? Cl6 In1 Cl2 90.03(9) . . ? Cl6 In1 Cl3 90.88(10) . . ? Cl6 In1 Cl5 175.83(9) . . ? Cl6 In1 Cl1 93.01(10) . . ? Cl6 In1 Cl4 87.79(8) . . ? H4A O4 H4B 104.5 . . ? H3A O3 H3B 109.5 . . ? H3A O3 H3C 115.3 . . ? H3B O3 H3C 114.9 . . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C16 N2 H2A 109.5 . . ? C16 N2 H2B 109.5 . . ? C16 N2 H2C 109.5 . . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C8 N1 H1A 109.5 . . ? C8 N1 H1B 109.5 . . ? C8 N1 H1C 109.5 . . ? C3 C8 N1 121.1(10) . . ? C3 C8 C7 123.9(10) . . ? C7 C8 N1 114.9(11) . . ? C8 C3 C4 116.9(10) . . ? C8 C3 C2 123.9(10) . . ? C4 C3 C2 119.2(10) . . ? C11 C16 N2 121.1(11) . . ? C15 C16 N2 117.9(11) . . ? C15 C16 C11 120.8(10) . . ? C8 C7 H7 120.7 . . ? C8 C7 C6 118.5(12) . . ? C6 C7 H7 120.7 . . ? O2 C10 C11 120.1(11) . . ? O2 C10 C9 119.7(11) . . ? C9 C10 C11 120.2(11) . . ? C3 C4 H4 119.4 . . ? C5 C4 C3 121.1(11) . . ? C5 C4 H4 119.4 . . ? C16 C11 C10 122.6(10) . . ? C12 C11 C16 116.7(11) . . ? C12 C11 C10 120.6(12) . . ? C16 C15 H15 119.7 . . ? C16 C15 C14 120.6(11) . . ? C14 C15 H15 119.7 . . ? C7 C6 H6 120.7 . . ? C7 C6 C5 118.7(12) . . ? C5 C6 H6 120.7 . . ? C4 C5 C6 120.8(12) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? O1 C2 C3 119.4(12) . . ? O1 C2 C1 119.3(13) . . ? C3 C2 C1 121.3(11) . . ? C11 C12 H12 119.1 . . ? C13 C12 C11 121.8(12) . . ? C13 C12 H12 119.1 . . ? C12 C13 H13 120.7 . . ? C14 C13 C12 118.6(10) . . ? C14 C13 H13 120.7 . . ? C15 C14 H14 119.4 . . ? C13 C14 C15 121.2(12) . . ? C13 C14 H14 119.4 . . ? C2 C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? C2 C1 H1F 109.5 . . ? H1D C1 H1E 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Cl2 2.522(3) . ? In1 Cl3 2.5518(19) . ? In1 Cl5 2.505(3) . ? In1 Cl1 2.5126(19) . ? In1 Cl4 2.514(2) . ? In1 Cl6 2.487(3) . ? O4 H4A 0.8699 . ? O4 H4B 0.8696 . ? O3 H3A 0.8697 . ? O3 H3B 0.8700 . ? O3 H3C 0.8701 . ? O1 C2 1.235(16) . ? O2 C10 1.205(14) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N2 C16 1.429(13) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N1 C8 1.503(13) . ? C8 C3 1.356(15) . ? C8 C7 1.379(16) . ? C3 C4 1.399(14) . ? C3 C2 1.487(17) . ? C16 C11 1.406(17) . ? C16 C15 1.373(16) . ? C7 H7 0.9500 . ? C7 C6 1.382(19) . ? C10 C11 1.490(16) . ? C10 C9 1.470(16) . ? C4 H4 0.9500 . ? C4 C5 1.355(18) . ? C11 C12 1.405(16) . ? C15 H15 0.9500 . ? C15 C14 1.376(16) . ? C6 H6 0.9500 . ? C6 C5 1.404(19) . ? C5 H5 0.9500 . ? C2 C1 1.502(18) . ? C12 H12 0.9500 . ? C12 C13 1.404(17) . ? C13 H13 0.9500 . ? C13 C14 1.359(18) . ? C14 H14 0.9500 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C10 C11 C16 -1.2(17) . . . . ? O2 C10 C11 C12 177.5(11) . . . . ? N2 C16 C11 C10 -2.1(16) . . . . ? N2 C16 C11 C12 179.1(11) . . . . ? N2 C16 C15 C14 179.7(11) . . . . ? N1 C8 C3 C4 -179.9(9) . . . . ? N1 C8 C3 C2 -1.8(18) . . . . ? N1 C8 C7 C6 -178.8(11) . . . . ? C8 C3 C4 C5 -2.2(17) . . . . ? C8 C3 C2 O1 6.4(19) . . . . ? C8 C3 C2 C1 -175.0(11) . . . . ? C8 C7 C6 C5 -0.5(18) . . . . ? C3 C8 C7 C6 -0.6(18) . . . . ? C3 C4 C5 C6 1.2(18) . . . . ? C16 C11 C12 C13 -0.6(17) . . . . ? C16 C15 C14 C13 2.6(19) . . . . ? C7 C8 C3 C4 1.9(17) . . . . ? C7 C8 C3 C2 -180.0(11) . . . . ? C7 C6 C5 C4 0.2(19) . . . . ? C10 C11 C12 C13 -179.4(11) . . . . ? C4 C3 C2 O1 -175.6(12) . . . . ? C4 C3 C2 C1 3.1(17) . . . . ? C11 C16 C15 C14 -4.7(18) . . . . ? C11 C12 C13 C14 -1.4(19) . . . . ? C15 C16 C11 C10 -177.6(11) . . . . ? C15 C16 C11 C12 3.6(17) . . . . ? C2 C3 C4 C5 179.6(11) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C9 C10 C11 C16 177.7(11) . . . . ? C9 C10 C11 C12 -3.5(16) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.494(3) 2 0.506(3)