#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:08:29 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296018 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573217.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_1573217 loop_ _publ_author_name 'Chen, Jingwen' 'Zhou, Kang' 'Li, Jingbai' 'Xu, Guozhong' 'Hei, Xiuze' 'Li, Jing' _publ_section_title ; Strongly Photoluminescent and Radioluminescent Copper(I) Iodide Hybrid Materials Made of Coordinated Ionic Chains ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06242F _journal_year 2024 _chemical_formula_moiety 'C16 H23 Cu2 I3 N4 O, C2 H3 N' _chemical_formula_sum 'C18 H26 Cu2 I3 N5 O' _chemical_formula_weight 836.22 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-12-13 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2024-07-31 deposited with the CCDC. 2024-11-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.855(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.4530(13) _cell_length_b 17.025(2) _cell_length_c 12.8883(13) _cell_measurement_reflns_used 2170 _cell_measurement_temperature 200.0 _cell_measurement_theta_max 23.680 _cell_measurement_theta_min 2.759 _cell_volume 2504.0(5) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 200.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_unetI/netI 0.0700 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 26280 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.695 _diffrn_reflns_theta_min 1.986 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.416 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0946 after correction. The Ratio of minimum to maximum transmission is 0.5865. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.218 _exptl_crystal_description plate _exptl_crystal_F_000 1576 _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.984 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.182 _refine_ls_extinction_coef 0.00183(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 278 _refine_ls_number_reflns 5854 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.166 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0605 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+20.7752P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1240 _refine_ls_wR_factor_ref 0.1352 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4436 _reflns_number_total 5854 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06242f2.cif _cod_data_source_block 1686_hxz_0m _cod_original_cell_volume 2504.1(5) _cod_database_code 1573217 _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 0.813 _shelx_estimated_absorpt_t_min 0.137 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H1A of O1A, {H11A,H11B,H11} of C11, {H13A,H13B,H13} of C13, All C(H,H) groups At 1.5 times of: H1B of O1B, {H18A,H18B,H18C} of C18 2. Restrained distances O1A-H1A 0.84 with sigma of 0.02 3. Others Sof(O1B)=Sof(H1B)=Sof(H11)=Sof(H13A)=Sof(H13B)=1-FVAR(1) Sof(O1A)=Sof(H1A)=Sof(H11A)=Sof(H11B)=Sof(H13)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C11(H11), C13(H13), C16(H16) 4.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B) 4.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5) 4.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C) 4.e Idealised tetrahedral OH refined as rotating group: O1B(H1B) ; _shelx_res_file ; TITL 1686_hxz_0m_a.res in P2(1)/c 1686_hxz_0m.res created by SHELXL-2017/1 at 21:39:28 on 13-Dec-2023 REM Old TITL 1686_HXZ_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.141, Rweak 0.014, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C17 N3 O4 Cu2 I3 CELL 0.71073 11.453 17.0252 12.8883 90 94.855 90 ZERR 4 0.0013 0.002 0.0013 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cu I N O UNIT 72 104 8 12 20 4 DFIX 0.84 O1A H1A L.S. 10 PLAN 99 SIZE 0.61 0.22 0.04 TEMP -73.15 CONF BOND $H list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.000000 20.775200 EXTI 0.001833 FVAR 0.20259 0.51604 I1 4 0.687976 0.777375 0.302694 11.00000 0.03395 0.06828 = 0.04078 -0.00195 0.00310 0.00023 I2 4 0.888907 0.861078 0.583931 11.00000 0.05818 0.03387 = 0.03357 0.00161 0.00220 -0.00066 I3 4 1.075058 0.736679 0.835427 11.00000 0.03496 0.04683 = 0.03927 -0.00063 0.00196 0.00026 CU1 3 0.878509 0.756914 0.431245 11.00000 0.05356 0.03947 = 0.03861 0.00631 0.00450 -0.00267 CU2 3 0.884540 0.738097 0.708636 11.00000 0.05062 0.04386 = 0.03803 0.00176 0.00145 -0.00215 PART 2 O1B 6 0.543172 0.392024 1.121129 -21.00000 0.09013 0.08292 = 0.09981 -0.00966 0.06958 -0.00966 AFIX 147 H1B 2 0.472974 0.382212 1.101137 -21.00000 -1.50000 AFIX 0 PART 1 O1A 6 0.409899 0.412522 0.960060 21.00000 0.04947 0.04914 = 0.10959 -0.00563 0.03506 0.00494 H1A 2 0.368112 0.375833 0.980471 21.00000 -1.20000 PART 0 N1 5 0.864958 0.650330 0.504571 11.00000 0.04702 0.03281 = 0.03376 0.00325 0.00655 0.00043 N2 5 0.880925 0.642050 0.606572 11.00000 0.05004 0.02924 = 0.03313 0.00399 0.00587 -0.00933 N3 5 0.878796 0.564314 0.629025 11.00000 0.04842 0.03243 = 0.03200 0.00738 0.00754 -0.00243 N4 5 0.698824 0.414708 0.905840 11.00000 0.03276 0.03015 = 0.03638 0.00301 0.00829 -0.00300 C1 1 0.850335 0.577084 0.460050 11.00000 0.05289 0.03206 = 0.03145 0.00333 0.01481 -0.00571 C2 1 0.828755 0.554117 0.356293 11.00000 0.06361 0.05286 = 0.03861 -0.00993 0.00486 -0.00670 AFIX 43 H2 2 0.819351 0.591738 0.301789 11.00000 -1.20000 AFIX 0 C3 1 0.821741 0.476130 0.336332 11.00000 0.07756 0.06117 = 0.04062 -0.01234 0.00917 -0.01683 AFIX 43 H3 2 0.807253 0.459155 0.266207 11.00000 -1.20000 AFIX 0 C4 1 0.835208 0.418988 0.416140 11.00000 0.06160 0.03684 = 0.06529 -0.01531 0.01721 -0.00750 AFIX 43 H4 2 0.830569 0.364782 0.398794 11.00000 -1.20000 AFIX 0 C5 1 0.854799 0.441163 0.517769 11.00000 0.04880 0.02917 = 0.05410 0.00861 0.02096 -0.00381 AFIX 43 H5 2 0.863627 0.403368 0.572093 11.00000 -1.20000 AFIX 0 C6 1 0.861310 0.520577 0.538702 11.00000 0.04483 0.03035 = 0.03443 -0.00186 0.01020 0.00249 C7 1 0.891020 0.536436 0.737023 11.00000 0.04320 0.04175 = 0.03432 0.01450 0.00210 -0.00313 AFIX 23 H7A 2 0.907013 0.581471 0.784710 11.00000 -1.20000 H7B 2 0.957889 0.499565 0.746773 11.00000 -1.20000 AFIX 0 C8 1 0.778967 0.495159 0.762838 11.00000 0.05082 0.04585 = 0.03329 0.00755 0.00398 -0.01012 AFIX 23 H8A 2 0.710786 0.529923 0.745594 11.00000 -1.20000 H8B 2 0.767750 0.446640 0.720837 11.00000 -1.20000 AFIX 0 C9 1 0.787076 0.474927 0.877164 11.00000 0.03410 0.04710 = 0.03219 0.00421 -0.00037 -0.00384 AFIX 23 H9A 2 0.866783 0.454855 0.897868 11.00000 -1.20000 H9B 2 0.776010 0.523492 0.917425 11.00000 -1.20000 AFIX 0 C10 1 0.702038 0.410878 1.023207 11.00000 0.05054 0.06238 = 0.03356 0.01108 0.00884 -0.00108 AFIX 23 H10A 2 0.782382 0.397405 1.052109 11.00000 -1.20000 H10B 2 0.682273 0.463143 1.050485 11.00000 -1.20000 AFIX 0 C11 1 0.617211 0.350677 1.058835 11.00000 0.06206 0.08353 = 0.06721 0.03517 0.02145 0.00215 PART 1 AFIX 23 H11A 2 0.562123 0.375979 1.103722 21.00000 -1.20000 H11B 2 0.660518 0.309163 1.099809 21.00000 -1.20000 AFIX 13 PART 2 H11 2 0.660588 0.308853 1.100730 -21.00000 -1.20000 AFIX 0 PART 0 C12 1 0.575983 0.437582 0.863593 11.00000 0.03229 0.05795 = 0.04873 0.00688 0.00156 -0.00204 AFIX 23 H12A 2 0.571373 0.439549 0.786585 11.00000 -1.20000 H12B 2 0.556798 0.490382 0.889483 11.00000 -1.20000 AFIX 0 C13 1 0.487883 0.377257 0.898740 11.00000 0.03813 0.07531 = 0.07577 -0.00251 0.01461 -0.01049 PART 2 AFIX 23 H13A 2 0.431027 0.403936 0.940551 -21.00000 -1.20000 H13B 2 0.443909 0.353936 0.836822 -21.00000 -1.20000 AFIX 13 PART 1 H13 2 0.443798 0.353609 0.836090 21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.728527 0.334794 0.865633 11.00000 0.06785 0.03064 = 0.09164 -0.01458 0.03088 0.00062 AFIX 23 H14A 2 0.807018 0.318668 0.896364 11.00000 -1.20000 H14B 2 0.730485 0.336800 0.789032 11.00000 -1.20000 AFIX 0 C15 1 0.637366 0.275238 0.894077 11.00000 0.07174 0.03234 = 0.14558 -0.00315 0.05103 -0.00898 AFIX 23 H15A 2 0.676763 0.231054 0.932773 11.00000 -1.20000 H15B 2 0.595617 0.253943 0.829760 11.00000 -1.20000 AFIX 0 C16 1 0.548407 0.314068 0.961789 11.00000 0.05289 0.04714 = 0.09816 0.00308 0.04354 -0.01446 AFIX 13 H16 2 0.490636 0.274454 0.983236 11.00000 -1.20000 AFIX 0 N5 5 0.580758 0.381496 0.606662 11.00000 0.12464 0.20649 = 0.08002 -0.04809 -0.00347 -0.05696 C17 1 0.516226 0.387665 0.538701 11.00000 0.06317 0.10040 = 0.08898 -0.03043 -0.00075 -0.00463 C18 1 0.435971 0.394845 0.450053 11.00000 0.13424 0.14943 = 0.17586 -0.06897 -0.07644 0.05908 AFIX 137 H18A 2 0.478417 0.407402 0.389261 11.00000 -1.50000 H18B 2 0.380025 0.436923 0.461279 11.00000 -1.50000 H18C 2 0.393680 0.345199 0.437995 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1686_hxz_0m_a.res in P2(1)/c REM R1 = 0.0605 for 4436 Fo > 4sig(Fo) and 0.0861 for all 5854 data REM 278 parameters refined using 1 restraints END WGHT 0.0000 20.7789 REM Highest difference peak 0.984, deepest hole -0.989, 1-sigma level 0.182 Q1 1 0.8242 0.8587 0.5945 11.00000 0.05 0.98 Q2 1 1.0761 0.6992 0.8785 11.00000 0.05 0.96 Q3 1 0.6870 0.8552 0.2863 11.00000 0.05 0.84 Q4 1 1.0642 0.7655 0.7879 11.00000 0.05 0.82 Q5 1 0.6832 0.8221 0.3487 11.00000 0.05 0.76 Q6 1 0.8961 0.8912 0.6225 11.00000 0.05 0.76 Q7 1 0.7193 0.7235 0.3497 11.00000 0.05 0.75 Q8 1 0.9677 0.8594 0.4992 11.00000 0.05 0.74 Q9 1 1.0863 0.7604 0.8807 11.00000 0.05 0.73 Q10 1 0.6831 0.6798 0.3179 11.00000 0.05 0.71 Q11 1 1.0049 0.7950 0.8601 11.00000 0.05 0.70 Q12 1 0.6404 0.7600 0.3187 11.00000 0.05 0.70 Q13 1 0.6829 0.2445 1.0621 11.00000 0.05 0.69 Q14 1 0.9191 0.3634 0.7962 11.00000 0.05 0.69 Q15 1 0.9121 0.8199 0.5027 11.00000 0.05 0.68 Q16 1 0.7120 0.5585 0.6784 11.00000 0.05 0.68 Q17 1 0.5070 0.3585 0.4656 11.00000 0.05 0.68 Q18 1 0.8860 0.8875 0.5361 11.00000 0.05 0.66 Q19 1 0.8816 0.9392 0.5718 11.00000 0.05 0.66 Q20 1 1.0660 0.7171 0.7963 11.00000 0.05 0.65 Q21 1 0.5261 0.2797 1.0301 11.00000 0.05 0.63 Q22 1 1.0722 0.8192 0.8320 11.00000 0.05 0.62 Q23 1 0.8541 0.6816 0.5828 11.00000 0.05 0.62 Q24 1 0.7695 0.6010 0.2074 11.00000 0.05 0.62 Q25 1 0.7473 0.8020 0.6759 11.00000 0.05 0.61 Q26 1 0.5129 0.4202 0.9824 11.00000 0.05 0.61 Q27 1 0.9139 0.6003 0.5794 11.00000 0.05 0.61 Q28 1 0.7403 0.4584 0.7379 11.00000 0.05 0.60 Q29 1 0.9438 0.7602 0.4887 11.00000 0.05 0.60 Q30 1 0.5242 0.4043 0.4107 11.00000 0.05 0.60 Q31 1 0.7574 0.3789 0.3948 11.00000 0.05 0.59 Q32 1 0.9058 0.6972 0.6317 11.00000 0.05 0.59 Q33 1 0.4835 0.3023 0.4399 11.00000 0.05 0.59 Q34 1 0.5058 0.4202 0.3851 11.00000 0.05 0.58 Q35 1 0.7448 0.4534 0.5432 11.00000 0.05 0.58 Q36 1 1.1638 0.7351 0.7650 11.00000 0.05 0.57 Q37 1 0.9858 0.7823 0.4155 11.00000 0.05 0.57 Q38 1 1.0400 0.4789 0.7392 11.00000 0.05 0.57 Q39 1 0.7532 0.4403 1.0913 11.00000 0.05 0.57 Q40 1 0.9662 0.7154 0.4547 11.00000 0.05 0.56 Q41 1 0.3081 0.3660 0.8250 11.00000 0.05 0.55 Q42 1 0.6864 0.7479 0.2590 11.00000 0.05 0.55 Q43 1 0.5212 0.3406 0.6262 11.00000 0.05 0.55 Q44 1 0.8591 0.8073 0.6369 11.00000 0.05 0.55 Q45 1 0.7166 0.5789 0.1794 11.00000 0.05 0.54 Q46 1 0.9835 0.4592 0.8663 11.00000 0.05 0.54 Q47 1 0.9921 0.6753 0.8636 11.00000 0.05 0.53 Q48 1 0.7364 0.5387 0.2154 11.00000 0.05 0.53 Q49 1 0.4828 0.2599 0.7645 11.00000 0.05 0.53 Q50 1 0.5911 0.7194 0.2960 11.00000 0.05 0.52 Q51 1 0.8742 0.8049 0.7269 11.00000 0.05 0.52 Q52 1 0.9810 0.8596 0.6622 11.00000 0.05 0.52 Q53 1 0.6994 0.5538 0.2714 11.00000 0.05 0.51 Q54 1 0.7213 0.2235 0.9791 11.00000 0.05 0.51 Q55 1 0.5486 0.4771 0.7960 11.00000 0.05 0.51 Q56 1 0.6800 0.7957 0.2620 11.00000 0.05 0.51 Q57 1 0.6027 0.7225 0.2657 11.00000 0.05 0.51 Q58 1 0.9150 0.6452 0.6204 11.00000 0.05 0.51 Q59 1 1.0152 0.8196 0.7068 11.00000 0.05 0.51 Q60 1 0.4778 0.4532 0.6054 11.00000 0.05 0.51 Q61 1 0.7060 0.2157 0.8999 11.00000 0.05 0.51 Q62 1 0.6949 0.2954 0.7122 11.00000 0.05 0.50 Q63 1 0.7847 0.5444 1.0334 11.00000 0.05 0.50 Q64 1 0.4557 0.3789 0.8153 11.00000 0.05 0.50 Q65 1 0.7211 0.4182 0.6020 11.00000 0.05 0.50 Q66 1 1.0221 0.6534 0.9273 11.00000 0.05 0.50 Q67 1 0.9351 0.4589 1.0854 11.00000 0.05 0.50 Q68 1 0.8215 0.3405 0.6431 11.00000 0.05 0.50 Q69 1 0.7418 0.4979 1.0640 11.00000 0.05 0.50 Q70 1 0.7454 0.6185 0.7094 11.00000 0.05 0.49 Q71 1 0.9066 0.8388 0.6279 11.00000 0.05 0.49 Q72 1 1.1222 0.7362 0.8299 11.00000 0.05 0.49 Q73 1 0.8867 0.3383 0.3181 11.00000 0.05 0.49 Q74 1 0.7412 0.5622 0.7607 11.00000 0.05 0.49 Q75 1 0.4482 0.5006 0.4945 11.00000 0.05 0.49 Q76 1 1.0105 0.6539 0.5038 11.00000 0.05 0.49 Q77 1 0.9019 0.4219 0.6405 11.00000 0.05 0.48 Q78 1 0.9344 0.6605 0.5344 11.00000 0.05 0.48 Q79 1 0.3342 0.3422 1.0606 11.00000 0.05 0.48 Q80 1 0.6967 0.3796 0.5422 11.00000 0.05 0.47 Q81 1 1.0167 0.7533 0.5433 11.00000 0.05 0.47 Q82 1 0.9521 0.5349 0.9195 11.00000 0.05 0.47 Q83 1 1.0065 0.6829 0.5964 11.00000 0.05 0.47 Q84 1 0.8796 0.7592 0.3226 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13.40 11.70 0 11 14 0.50 23.60 0 11 14 23.90 15.20 -1 -11 -14 8.30 8.50 1 -11 14 23.00 6.30 1 -11 14 16.50 13.70 1 -11 14 33.20 6.60 1 11 14 46.70 18.20 2 -11 14 35.80 7.90 2 -11 14 42.70 16.30 -3 -12 14 13.70 11.40 3 -12 -14 -2.60 8.70 3 -12 -14 40.40 13.80 -3 -12 14 4.10 5.90 2 -12 -14 0.50 8.40 -2 -12 14 -9.70 4.20 -2 -12 14 10.80 11.90 2 -12 -14 -9.40 7.70 -2 12 14 36.90 15.60 -1 -12 14 7.10 5.10 1 -12 -14 28.80 10.60 -1 -12 14 7.00 10.80 1 -12 -14 6.90 7.80 -1 12 14 29.90 16.50 0 -12 14 0.50 5.20 0 -12 -14 2.80 7.30 0 -12 14 0.40 5.00 0 -12 -14 -5.60 7.00 0 -12 14 12.10 10.40 0 12 14 5.50 13.70 -7 0 15 -17.30 10.30 -6 0 15 4.60 10.70 -5 0 15 -4.30 12.70 -5 0 15 -4.90 6.60 -4 0 15 4.80 12.10 -4 0 15 -4.10 7.70 -3 0 15 -5.80 11.60 -3 0 15 10.80 7.30 -2 0 15 -2.30 4.70 -2 0 15 -7.00 9.30 -1 0 15 -2.80 5.00 0 0 15 -0.20 6.30 0 0 15 12.00 10.20 1 0 15 24.80 13.90 1 0 15 9.80 6.30 2 0 15 2.70 6.20 2 0 15 -6.30 6.10 3 0 15 3.50 5.60 3 0 15 5.10 11.90 4 0 15 14.30 15.20 5 0 15 15.20 7.80 -7 -1 15 31.10 14.00 -7 1 15 16.40 12.70 -6 -1 15 37.90 12.50 -6 1 15 -13.50 9.60 -5 -1 15 18.40 15.50 -5 -1 15 10.30 8.10 -5 1 15 7.20 7.00 -5 1 15 15.50 14.70 -4 -1 15 4.80 13.30 -4 -1 15 21.10 8.40 -4 1 15 1.30 12.40 -4 1 15 2.50 7.80 -3 -1 15 18.10 6.50 -3 -1 15 -5.60 12.00 -3 1 15 4.10 6.30 -3 1 15 -3.10 11.80 -2 -1 15 48.90 10.50 -2 1 15 58.19 21.50 -2 1 15 30.80 10.00 -1 -1 15 15.90 7.40 -1 -1 15 12.80 19.50 -1 1 15 38.60 18.60 -1 1 15 18.40 8.40 0 -1 15 -2.70 10.70 0 -1 15 12.60 5.70 0 1 15 6.10 12.30 0 1 15 -0.30 5.50 1 -1 15 9.20 6.60 1 1 15 43.50 17.10 1 1 15 20.90 7.90 2 -1 15 37.40 9.60 2 -1 15 73.19 24.30 2 1 15 21.70 11.40 2 1 15 12.50 8.20 3 -1 15 16.90 6.90 3 -1 15 18.90 14.80 3 1 15 28.10 8.90 3 1 15 56.69 21.20 4 -1 15 9.20 7.00 4 -1 15 -21.10 11.90 4 1 15 17.00 12.20 4 1 15 1.60 5.60 5 -1 15 10.80 7.10 5 1 15 3.40 10.30 -7 -2 15 33.40 11.70 -7 2 15 17.50 13.00 -6 -2 15 22.00 9.40 -6 2 15 15.50 9.80 -5 -2 15 36.70 18.60 -5 2 15 44.80 20.70 -5 2 15 43.10 13.20 -4 -2 15 1.60 6.20 -4 -2 15 1.00 11.70 -4 2 15 11.70 7.90 -4 2 15 34.20 18.00 -3 -2 15 13.10 7.70 -3 2 15 33.00 16.10 -2 -2 15 6.00 12.40 -2 -2 15 -6.00 4.30 -2 2 15 13.20 6.40 -2 2 15 -9.80 9.60 -1 -2 15 52.69 10.50 -1 -2 15 75.09 26.80 -1 2 15 66.89 26.60 -1 2 15 76.69 14.50 0 -2 15 65.59 23.00 0 -2 15 67.19 11.80 0 2 15 79.19 16.10 0 2 15 71.19 23.60 1 -2 15 5.50 5.50 1 -2 15 38.90 24.10 1 2 15 27.60 14.50 1 2 15 20.40 9.00 2 -2 15 -2.90 12.30 2 2 15 8.90 8.20 2 2 15 18.80 8.50 3 -2 15 14.20 6.00 3 -2 15 5.90 11.00 3 2 15 12.10 14.70 3 2 15 -4.40 7.30 4 -2 15 80.29 22.80 4 -2 15 118.99 17.30 4 2 15 98.79 18.20 5 -2 15 8.00 8.10 5 2 15 25.50 10.90 -7 -3 15 12.80 10.60 -7 3 15 18.80 13.70 -6 -3 15 55.29 15.30 -6 3 15 29.80 13.70 -5 -3 15 -6.80 10.00 -5 -3 15 1.90 7.70 -5 3 15 -20.90 8.90 -5 3 15 7.50 9.00 -4 -3 15 -16.90 11.70 -4 3 15 1.70 13.70 -4 3 15 -5.90 7.60 -3 -3 15 7.60 5.30 -3 -3 15 9.70 9.70 -3 3 15 10.70 8.10 -3 3 15 -1.00 9.00 -2 -3 15 63.29 23.40 -2 -3 15 71.69 11.80 -2 3 15 60.49 13.60 -2 3 15 96.89 27.70 -1 -3 15 49.80 9.20 -1 -3 15 93.19 25.20 -1 3 15 20.00 12.40 -1 3 15 73.69 25.00 0 -3 15 -0.90 4.10 0 -3 15 29.80 14.10 0 3 15 5.10 7.60 0 3 15 -3.90 6.80 1 -3 15 8.80 3.90 1 -3 15 1.10 12.10 1 3 15 -1.50 7.70 1 3 15 -1.90 12.10 2 -3 15 4.80 4.60 2 -3 15 17.10 11.80 2 3 15 -1.10 7.10 2 3 15 3.60 6.90 3 -3 15 84.59 21.90 3 -3 15 64.79 11.70 3 3 15 64.89 15.50 3 3 15 82.69 26.30 4 -3 15 20.90 8.20 4 -3 15 -3.20 15.50 4 3 15 18.10 9.80 5 -3 15 8.90 11.20 5 -3 15 -5.10 6.30 5 3 15 -12.60 7.40 -7 -4 15 0.00 9.20 -7 4 15 6.80 13.90 -6 -4 15 21.40 10.50 -6 4 15 18.00 12.00 -5 -4 15 -5.60 7.80 -5 -4 15 -9.70 11.20 -5 4 15 -5.20 8.00 -5 4 15 13.80 8.90 -4 -4 15 13.40 18.60 -4 -4 15 3.50 6.00 -4 4 15 3.70 10.60 -4 4 15 17.40 8.20 -3 -4 15 1.50 5.10 -3 -4 15 -4.80 11.30 -3 4 15 5.10 7.10 -3 4 15 3.10 10.20 -2 -4 15 17.30 16.20 -2 4 15 22.50 14.20 -1 -4 15 22.20 16.70 -1 -4 15 28.30 6.20 -1 4 15 38.50 18.10 -1 4 15 25.70 10.30 0 -4 15 7.90 4.10 0 -4 15 5.80 8.80 0 4 15 -2.60 7.90 0 4 15 4.20 8.90 1 -4 15 8.60 4.50 1 -4 15 -4.50 10.20 1 4 15 16.10 10.10 1 4 15 28.00 15.30 2 -4 15 35.20 19.20 3 -4 15 10.00 12.60 3 -4 15 -0.60 3.90 4 -4 15 23.90 7.10 4 -4 15 40.10 17.10 4 4 15 0.20 9.10 5 -4 15 41.30 18.00 5 -4 15 -10.70 5.30 5 4 15 -0.10 7.20 -7 -5 15 18.80 11.00 -7 5 15 -21.80 11.00 -6 -5 15 22.00 13.80 -6 -5 15 27.50 11.10 -6 5 15 -6.00 10.30 -5 -5 15 35.40 10.20 -5 -5 15 3.70 10.40 -5 5 15 38.60 13.40 -4 -5 15 -5.60 5.50 -4 5 15 -1.30 13.00 -4 5 15 17.80 9.60 -3 -5 15 28.50 15.70 -3 -5 15 54.19 10.30 -3 5 15 71.99 25.20 -3 5 15 37.10 11.10 -2 -5 15 9.70 4.60 -2 -5 15 6.80 12.50 -2 5 15 -0.80 7.00 -2 5 15 35.40 17.70 -1 -5 15 -4.10 9.70 -1 -5 15 -2.90 2.80 -1 5 15 24.10 13.20 -1 5 15 -4.20 9.00 0 -5 15 15.80 11.50 0 5 15 17.60 9.40 0 5 15 18.30 13.10 1 -5 15 19.90 4.60 1 -5 15 22.70 14.00 1 5 15 31.40 11.60 1 5 15 16.80 17.30 2 -5 15 43.10 21.60 2 -5 15 56.79 8.70 2 5 15 48.80 19.70 2 5 15 76.29 16.60 3 -5 15 11.10 13.80 3 -5 15 8.10 5.60 3 5 15 3.50 8.50 4 -5 15 13.80 4.80 4 -5 15 -5.00 14.50 4 5 15 -3.60 8.80 -6 -6 15 4.30 8.90 -6 -6 15 27.90 17.20 -5 -6 15 4.30 8.30 -5 -6 15 18.90 16.20 -5 6 15 3.20 10.70 -4 -6 15 172.98 42.30 -4 -6 15 124.89 19.80 -4 6 15 168.18 26.90 -3 -6 15 41.30 20.10 -3 6 15 53.69 19.60 -3 6 15 54.89 15.40 -2 -6 15 9.80 4.60 -2 -6 15 -5.50 13.10 -2 6 15 6.40 9.30 -2 6 15 0.60 9.30 -1 -6 15 7.40 3.40 -1 6 15 7.10 8.50 -1 6 15 1.10 13.50 0 -6 15 40.70 5.40 0 -6 15 40.10 17.20 0 6 15 72.19 24.30 1 -6 15 164.68 31.90 1 6 15 122.09 23.70 1 6 15 104.49 29.30 2 -6 15 8.70 14.00 2 -6 15 8.50 2.90 3 -6 15 -0.70 3.20 3 -6 15 27.10 19.10 3 6 15 -8.90 6.70 4 -6 15 17.40 13.90 4 -6 15 5.60 4.40 4 6 15 -17.70 7.60 -6 -7 15 9.70 8.60 -6 -7 15 -18.40 12.10 -6 7 15 -0.60 10.90 -5 -7 15 15.80 13.20 -5 -7 15 3.20 7.80 -5 7 15 -1.30 12.50 -4 -7 15 32.00 18.60 -4 -7 15 -0.50 6.00 -4 7 15 -11.50 11.70 -3 -7 15 121.29 30.30 -3 -7 15 66.39 12.40 -3 7 15 76.19 19.20 -2 -7 15 -1.80 4.30 -2 -7 15 2.20 12.80 -2 7 15 2.90 8.80 -2 7 15 12.90 16.20 -1 -7 15 7.10 10.80 -1 -7 15 6.00 3.00 -1 7 15 -0.80 14.00 -1 7 15 16.70 9.80 0 -7 15 1.70 10.70 0 -7 15 4.00 1.80 0 7 15 12.30 14.50 0 7 15 3.00 10.00 1 -7 15 50.69 21.30 1 7 15 72.59 18.00 2 -7 15 182.98 35.40 2 -7 15 153.38 12.60 3 -7 15 -48.90 21.40 3 -7 15 22.70 4.40 3 7 15 8.10 9.40 -5 -8 15 20.60 15.90 -5 8 15 22.50 16.00 -4 -8 15 167.98 32.00 -4 -8 15 94.89 16.60 -3 -8 15 22.20 16.70 -3 -8 15 13.10 6.70 -3 8 15 -8.20 9.30 -2 -8 15 14.40 4.90 -2 -8 15 -20.30 10.90 -2 8 15 -7.50 9.90 -1 -8 15 0.30 3.30 -1 -8 15 -4.30 10.10 -1 8 15 22.50 10.30 0 -8 15 20.10 3.20 0 -8 15 57.39 19.50 0 8 15 30.50 15.40 1 -8 15 134.79 28.80 1 8 15 124.59 26.30 2 -8 15 1.40 1.00 2 -8 15 3.10 13.10 3 8 15 23.00 11.30 -4 -9 15 1.80 13.00 -4 -9 15 8.90 7.10 -4 9 15 -7.90 8.90 -3 -9 15 11.30 5.90 -3 9 15 28.70 16.20 -2 -9 15 17.20 4.70 -2 -9 15 0.00 12.50 -1 -9 15 35.80 15.80 -1 9 15 27.90 13.60 0 -9 15 6.70 11.20 0 -9 15 2.40 2.10 0 9 15 -20.10 11.70 1 -9 15 32.40 15.70 1 9 15 38.90 17.70 -2 -10 15 -3.20 4.60 -2 -10 15 -12.30 11.60 -2 10 15 -6.70 12.30 -1 -10 15 25.70 15.10 -1 -10 15 24.80 6.00 -1 10 15 13.00 13.90 -5 0 16 20.60 10.80 -4 0 16 68.29 15.10 -3 0 16 -8.20 6.90 -3 0 16 1.10 14.50 -2 0 16 159.48 35.80 -2 0 16 114.19 19.20 -1 0 16 48.00 20.90 -1 0 16 23.70 8.90 0 0 16 31.00 12.70 0 0 16 -6.60 6.60 1 0 16 134.49 17.90 1 0 16 124.39 34.20 2 0 16 5.30 6.80 3 0 16 27.40 11.20 -5 -1 16 3.10 9.40 -5 1 16 19.60 10.30 -4 1 16 -5.30 6.50 -3 -1 16 20.60 14.40 -3 -1 16 9.00 8.40 -3 1 16 20.40 9.30 -2 -1 16 41.10 18.90 -2 -1 16 26.60 10.10 -2 1 16 8.10 18.70 -1 -1 16 139.19 20.50 -1 -1 16 246.28 45.30 -1 1 16 194.68 37.50 -1 1 16 178.28 22.00 0 -1 16 33.60 14.40 0 1 16 28.20 10.00 0 1 16 65.69 23.50 1 -1 16 25.20 16.30 1 -1 16 15.40 8.90 1 1 16 12.80 10.30 2 -1 16 65.19 13.00 2 1 16 63.69 14.00 3 -1 16 44.20 10.90 3 1 16 14.90 10.50 -5 -2 16 -2.90 7.10 -5 2 16 -14.40 8.70 -4 -2 16 33.20 17.40 -4 -2 16 34.30 11.30 -4 2 16 35.40 11.70 -3 -2 16 1.70 13.20 -3 -2 16 -3.30 6.40 -3 2 16 -10.30 7.60 -2 -2 16 64.29 21.30 -2 -2 16 40.80 10.10 -2 2 16 13.00 10.90 -1 -2 16 -1.80 5.10 -1 -2 16 -1.30 10.50 0 -2 16 -3.30 6.20 0 -2 16 10.40 14.80 0 2 16 18.50 11.90 1 -2 16 78.29 13.70 1 -2 16 128.09 29.70 1 2 16 90.29 20.70 2 -2 16 5.90 6.80 2 -2 16 15.60 16.20 3 -2 16 2.10 5.40 3 2 16 3.00 8.90 -5 -3 16 -10.90 8.20 -5 3 16 14.40 11.30 -4 -3 16 15.70 15.10 -4 -3 16 42.60 10.90 -4 3 16 10.80 12.30 -3 -3 16 20.00 7.70 -3 -3 16 26.20 19.00 -3 3 16 13.70 9.20 -2 -3 16 44.90 21.00 -2 -3 16 51.89 10.30 -2 3 16 57.89 14.10 -1 -3 16 93.19 13.90 -1 -3 16 101.99 28.00 -1 3 16 65.79 16.60 0 -3 16 -4.00 10.20 0 -3 16 6.10 5.40 0 3 16 -16.00 8.20 1 -3 16 -15.30 8.70 1 -3 16 -8.50 5.40 1 3 16 16.10 10.70 2 -3 16 -4.60 5.20 2 -3 16 29.70 14.00 3 -3 16 22.50 8.10 3 3 16 48.20 14.10 -5 -4 16 28.70 9.80 -5 4 16 -12.80 10.80 -4 -4 16 52.69 20.50 -4 -4 16 49.50 11.60 -4 4 16 33.80 14.30 -3 -4 16 30.70 8.20 -3 -4 16 59.69 23.20 -3 4 16 39.10 12.30 -2 -4 16 10.10 12.30 -2 -4 16 -3.30 4.40 -2 4 16 15.60 8.20 -1 -4 16 52.59 19.40 -1 -4 16 18.90 7.40 -1 4 16 32.90 11.70 0 -4 16 3.60 5.20 0 -4 16 28.70 14.50 0 4 16 3.90 8.10 1 -4 16 75.79 22.20 1 4 16 91.29 19.30 2 -4 16 82.79 23.40 2 -4 16 85.99 11.60 -4 -5 16 90.99 23.20 -4 -5 16 76.69 15.20 -4 5 16 106.69 21.10 -3 -5 16 28.00 8.50 -3 -5 16 24.50 20.30 -3 5 16 47.40 16.10 -2 -5 16 64.89 10.40 -2 -5 16 68.59 26.20 -2 5 16 45.90 18.40 -1 -5 16 29.30 6.60 -1 -5 16 33.40 18.30 -1 5 16 42.30 13.20 0 -5 16 -20.10 12.70 0 -5 16 19.40 6.40 0 5 16 -16.30 10.20 1 -5 16 37.60 16.50 1 5 16 36.00 15.40 2 -5 16 16.50 16.70 -3 -6 16 5.00 6.60 -3 -6 16 35.10 20.00 -3 6 16 18.60 11.70 -2 -6 16 -2.00 4.40 -2 -6 16 6.40 17.10 -2 6 16 -5.40 10.10 -1 -6 16 17.40 17.00 -1 -6 16 -4.10 3.20 -1 6 16 -6.10 11.50 0 -6 16 23.80 16.90 0 6 16 39.40 14.80 1 -6 16 41.80 19.10 1 6 16 59.19 16.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 71032 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 I1 I 0.68798(6) 0.77738(4) 0.30269(5) 0.0477(2) Uani 1 1 d . . . . . I2 I 0.88891(6) 0.86108(3) 0.58393(4) 0.04197(19) Uani 1 1 d . . . . . I3 I 1.07506(5) 0.73668(4) 0.83543(5) 0.04042(18) Uani 1 1 d . . . . . Cu1 Cu 0.87851(12) 0.75691(7) 0.43124(9) 0.0438(3) Uani 1 1 d . . . . . Cu2 Cu 0.88454(12) 0.73810(7) 0.70864(9) 0.0443(3) Uani 1 1 d . . . . . O1B O 0.5432(19) 0.3920(12) 1.1211(16) 0.087(8) Uani 0.484(18) 1 d . . P A 2 H1B H 0.472974 0.382212 1.101137 0.131 Uiso 0.484(18) 1 calc R U P A 2 O1A O 0.4099(14) 0.4125(9) 0.9601(15) 0.068(6) Uani 0.516(18) 1 d D . P A 1 H1A H 0.368(18) 0.376(10) 0.980(18) 0.081 Uiso 0.516(18) 1 d D U P A 1 N1 N 0.8650(7) 0.6503(4) 0.5046(5) 0.0377(17) Uani 1 1 d . . . . . N2 N 0.8809(7) 0.6420(4) 0.6066(5) 0.0373(17) Uani 1 1 d . . . . . N3 N 0.8788(7) 0.5643(4) 0.6290(5) 0.0374(17) Uani 1 1 d . . . . . N4 N 0.6988(6) 0.4147(4) 0.9058(5) 0.0328(16) Uani 1 1 d . . . . . C1 C 0.8503(9) 0.5771(5) 0.4601(6) 0.038(2) Uani 1 1 d . . . . . C2 C 0.8288(10) 0.5541(6) 0.3563(8) 0.052(3) Uani 1 1 d . . . . . H2 H 0.819351 0.591738 0.301789 0.062 Uiso 1 1 calc R U . . . C3 C 0.8217(11) 0.4761(7) 0.3363(8) 0.060(3) Uani 1 1 d . . . . . H3 H 0.807253 0.459155 0.266207 0.071 Uiso 1 1 calc R U . . . C4 C 0.8352(10) 0.4190(6) 0.4161(9) 0.054(3) Uani 1 1 d . . . . . H4 H 0.830569 0.364782 0.398794 0.065 Uiso 1 1 calc R U . . . C5 C 0.8548(9) 0.4412(5) 0.5178(8) 0.043(2) Uani 1 1 d . . . . . H5 H 0.863627 0.403368 0.572093 0.052 Uiso 1 1 calc R U . . . C6 C 0.8613(8) 0.5206(5) 0.5387(7) 0.0361(19) Uani 1 1 d . . . . . C7 C 0.8910(8) 0.5364(5) 0.7370(7) 0.040(2) Uani 1 1 d . . . . . H7A H 0.907013 0.581471 0.784710 0.048 Uiso 1 1 calc R U . . . H7B H 0.957889 0.499565 0.746773 0.048 Uiso 1 1 calc R U . . . C8 C 0.7790(9) 0.4952(6) 0.7628(7) 0.043(2) Uani 1 1 d . . . . . H8A H 0.710786 0.529923 0.745594 0.052 Uiso 1 1 calc R U . . . H8B H 0.767750 0.446640 0.720837 0.052 Uiso 1 1 calc R U . . . C9 C 0.7871(8) 0.4749(6) 0.8772(6) 0.038(2) Uani 1 1 d . . . . . H9A H 0.866783 0.454855 0.897868 0.046 Uiso 1 1 calc R U . . . H9B H 0.776010 0.523492 0.917425 0.046 Uiso 1 1 calc R U . . . C10 C 0.7020(9) 0.4109(6) 1.0232(7) 0.049(2) Uani 1 1 d . . . . . H10A H 0.782382 0.397405 1.052109 0.058 Uiso 1 1 calc R U . . . H10B H 0.682273 0.463143 1.050485 0.058 Uiso 1 1 calc R U . . . C11 C 0.6172(11) 0.3507(8) 1.0588(10) 0.070(4) Uani 1 1 d . . . . . H11A H 0.562123 0.375979 1.103722 0.084 Uiso 0.516(18) 1 calc R U P A 1 H11B H 0.660518 0.309163 1.099809 0.084 Uiso 0.516(18) 1 calc R U P A 1 H11 H 0.660588 0.308853 1.100730 0.084 Uiso 0.484(18) 1 calc R U P A 2 C12 C 0.5760(8) 0.4376(6) 0.8636(8) 0.046(2) Uani 1 1 d . . . . . H12A H 0.571373 0.439549 0.786585 0.056 Uiso 1 1 calc R U . . . H12B H 0.556798 0.490382 0.889483 0.056 Uiso 1 1 calc R U . . . C13 C 0.4879(10) 0.3773(7) 0.8987(10) 0.063(3) Uani 1 1 d . . . . . H13A H 0.431027 0.403936 0.940551 0.075 Uiso 0.484(18) 1 calc R U P A 2 H13B H 0.443909 0.353936 0.836822 0.075 Uiso 0.484(18) 1 calc R U P A 2 H13 H 0.443798 0.353609 0.836090 0.075 Uiso 0.516(18) 1 calc R U P A 1 C14 C 0.7285(11) 0.3348(6) 0.8656(10) 0.062(3) Uani 1 1 d . . . . . H14A H 0.807018 0.318668 0.896364 0.074 Uiso 1 1 calc R U . . . H14B H 0.730485 0.336800 0.789032 0.074 Uiso 1 1 calc R U . . . C15 C 0.6374(12) 0.2752(6) 0.8941(13) 0.081(4) Uani 1 1 d . . . . . H15A H 0.676763 0.231054 0.932773 0.097 Uiso 1 1 calc R U . . . H15B H 0.595617 0.253943 0.829760 0.097 Uiso 1 1 calc R U . . . C16 C 0.5484(10) 0.3141(7) 0.9618(10) 0.064(3) Uani 1 1 d . . . . . H16 H 0.490636 0.274454 0.983236 0.077 Uiso 1 1 calc R U . . . N5 N 0.5808(15) 0.3815(11) 0.6067(11) 0.138(7) Uani 1 1 d . . . . . C17 C 0.5162(13) 0.3877(9) 0.5387(13) 0.085(4) Uani 1 1 d . . . . . C18 C 0.4360(18) 0.3948(13) 0.4501(17) 0.158(10) Uani 1 1 d . . . . . H18A H 0.478417 0.407402 0.389261 0.237 Uiso 1 1 calc R U . . . H18B H 0.380025 0.436923 0.461279 0.237 Uiso 1 1 calc R U . . . H18C H 0.393680 0.345199 0.437995 0.237 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 I1 0.0340(4) 0.0683(5) 0.0408(3) -0.0019(3) 0.0031(3) 0.0002(3) I2 0.0582(4) 0.0339(3) 0.0336(3) 0.0016(2) 0.0022(3) -0.0007(3) I3 0.0350(3) 0.0468(4) 0.0393(3) -0.0006(3) 0.0020(2) 0.0003(3) Cu1 0.0536(8) 0.0395(6) 0.0386(6) 0.0063(5) 0.0045(5) -0.0027(5) Cu2 0.0506(8) 0.0439(7) 0.0380(6) 0.0018(5) 0.0015(5) -0.0022(5) O1B 0.090(16) 0.083(14) 0.100(15) -0.010(11) 0.070(13) -0.010(12) O1A 0.049(10) 0.049(10) 0.110(14) -0.006(9) 0.035(9) 0.005(7) N1 0.047(5) 0.033(4) 0.034(4) 0.003(3) 0.007(3) 0.000(3) N2 0.050(5) 0.029(4) 0.033(4) 0.004(3) 0.006(3) -0.009(3) N3 0.048(5) 0.032(4) 0.032(4) 0.007(3) 0.008(3) -0.002(3) N4 0.033(4) 0.030(4) 0.036(4) 0.003(3) 0.008(3) -0.003(3) C1 0.053(6) 0.032(5) 0.031(4) 0.003(3) 0.015(4) -0.006(4) C2 0.064(7) 0.053(6) 0.039(5) -0.010(4) 0.005(5) -0.007(5) C3 0.078(9) 0.061(7) 0.041(6) -0.012(5) 0.009(5) -0.017(6) C4 0.062(7) 0.037(5) 0.065(7) -0.015(5) 0.017(5) -0.007(5) C5 0.049(6) 0.029(5) 0.054(6) 0.009(4) 0.021(5) -0.004(4) C6 0.045(5) 0.030(4) 0.034(4) -0.002(3) 0.010(4) 0.002(4) C7 0.043(6) 0.042(5) 0.034(5) 0.014(4) 0.002(4) -0.003(4) C8 0.051(6) 0.046(6) 0.033(5) 0.008(4) 0.004(4) -0.010(4) C9 0.034(5) 0.047(5) 0.032(4) 0.004(4) 0.000(4) -0.004(4) C10 0.051(6) 0.062(7) 0.034(5) 0.011(4) 0.009(4) -0.001(5) C11 0.062(8) 0.084(9) 0.067(8) 0.035(7) 0.021(6) 0.002(7) C12 0.032(5) 0.058(6) 0.049(6) 0.007(5) 0.002(4) -0.002(4) C13 0.038(6) 0.075(8) 0.076(8) -0.003(6) 0.015(5) -0.010(6) C14 0.068(8) 0.031(5) 0.092(9) -0.015(5) 0.031(7) 0.001(5) C15 0.072(9) 0.032(6) 0.146(13) -0.003(7) 0.051(9) -0.009(6) C16 0.053(7) 0.047(6) 0.098(9) 0.003(6) 0.044(7) -0.014(5) N5 0.125(14) 0.206(19) 0.080(10) -0.048(11) -0.003(9) -0.057(13) C17 0.063(9) 0.100(11) 0.089(11) -0.030(9) -0.001(8) -0.005(8) C18 0.134(18) 0.149(18) 0.18(2) -0.069(16) -0.076(16) 0.059(15) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 I1 Cu2 65.65(4) . 4_575 ? Cu2 I2 Cu1 85.37(4) . . ? Cu2 I3 Cu1 66.13(4) . 4_576 ? I1 Cu1 I3 112.89(5) . 4_575 ? I1 Cu1 Cu2 57.34(4) . 4_575 ? I2 Cu1 I1 111.11(5) . . ? I2 Cu1 I3 109.36(5) . 4_575 ? I2 Cu1 Cu2 135.97(5) . 4_575 ? I3 Cu1 Cu2 56.16(4) 4_575 4_575 ? N1 Cu1 I1 108.2(2) . . ? N1 Cu1 I2 104.5(2) . . ? N1 Cu1 I3 110.4(2) . 4_575 ? N1 Cu1 Cu2 119.5(2) . 4_575 ? I1 Cu2 Cu1 57.01(4) 4_576 4_576 ? I2 Cu2 I1 114.59(5) . 4_576 ? I2 Cu2 Cu1 125.90(5) . 4_576 ? I3 Cu2 I1 114.10(5) . 4_576 ? I3 Cu2 I2 109.26(5) . . ? I3 Cu2 Cu1 57.72(4) . 4_576 ? N2 Cu2 I1 103.7(2) . 4_576 ? N2 Cu2 I2 103.69(19) . . ? N2 Cu2 I3 110.9(2) . . ? N2 Cu2 Cu1 130.37(19) . 4_576 ? C11 O1B H1B 109.5 . . ? C13 O1A H1A 106(10) . . ? N2 N1 Cu1 122.8(5) . . ? N2 N1 C1 108.7(7) . . ? C1 N1 Cu1 128.2(6) . . ? N1 N2 Cu2 122.4(5) . . ? N1 N2 N3 108.3(7) . . ? N3 N2 Cu2 128.9(5) . . ? N2 N3 C6 110.5(7) . . ? N2 N3 C7 121.1(7) . . ? C6 N3 C7 128.4(7) . . ? C9 N4 C10 108.3(7) . . ? C9 N4 C12 111.0(7) . . ? C10 N4 C12 108.3(7) . . ? C14 N4 C9 110.8(7) . . ? C14 N4 C10 108.6(8) . . ? C14 N4 C12 109.8(8) . . ? N1 C1 C2 131.2(8) . . ? N1 C1 C6 108.7(7) . . ? C2 C1 C6 120.1(8) . . ? C1 C2 H2 121.3 . . ? C3 C2 C1 117.4(10) . . ? C3 C2 H2 121.3 . . ? C2 C3 H3 118.8 . . ? C2 C3 C4 122.4(10) . . ? C4 C3 H3 118.8 . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.5(9) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 121.3 . . ? C4 C5 C6 117.5(9) . . ? C6 C5 H5 121.3 . . ? N3 C6 C1 103.8(7) . . ? C5 C6 N3 134.0(8) . . ? C5 C6 C1 122.2(8) . . ? N3 C7 H7A 109.7 . . ? N3 C7 H7B 109.7 . . ? N3 C7 C8 110.0(7) . . ? H7A C7 H7B 108.2 . . ? C8 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C7 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C9 C8 C7 109.6(7) . . ? C9 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? N4 C9 C8 114.1(7) . . ? N4 C9 H9A 108.7 . . ? N4 C9 H9B 108.7 . . ? C8 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N4 C10 H10A 109.3 . . ? N4 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C11 C10 N4 111.8(9) . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? O1B C11 C10 105.6(13) . . ? O1B C11 H11 110.1 . . ? O1B C11 C16 111.8(14) . . ? C10 C11 H11A 109.9 . . ? C10 C11 H11B 109.9 . . ? C10 C11 H11 110.1 . . ? C10 C11 C16 108.9(9) . . ? H11A C11 H11B 108.3 . . ? C16 C11 H11A 109.9 . . ? C16 C11 H11B 109.9 . . ? C16 C11 H11 110.1 . . ? N4 C12 H12A 109.8 . . ? N4 C12 H12B 109.8 . . ? N4 C12 C13 109.6(8) . . ? H12A C12 H12B 108.2 . . ? C13 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? O1A C13 C12 110.6(12) . . ? O1A C13 H13 109.3 . . ? O1A C13 C16 107.3(12) . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C12 C13 H13 109.3 . . ? H13A C13 H13B 108.0 . . ? C16 C13 C12 111.0(9) . . ? C16 C13 H13A 109.4 . . ? C16 C13 H13B 109.4 . . ? C16 C13 H13 109.3 . . ? N4 C14 H14A 109.7 . . ? N4 C14 H14B 109.7 . . ? N4 C14 C15 109.9(9) . . ? H14A C14 H14B 108.2 . . ? C15 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C14 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C14 C15 C16 110.5(9) . . ? H15A C15 H15B 108.1 . . ? C16 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C11 C16 H16 110.5 . . ? C13 C16 C11 109.4(10) . . ? C13 C16 C15 107.5(11) . . ? C13 C16 H16 110.5 . . ? C15 C16 C11 108.2(11) . . ? C15 C16 H16 110.5 . . ? N5 C17 C18 178(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 I1 Cu1 2.6488(14) . ? I1 Cu2 2.6587(15) 4_575 ? I2 Cu1 2.6442(13) . ? I2 Cu2 2.6426(13) . ? I3 Cu1 2.6599(15) 4_576 ? I3 Cu2 2.6131(14) . ? Cu1 Cu2 2.8770(17) 4_575 ? Cu1 N1 2.058(7) . ? Cu2 N2 2.097(7) . ? O1B H1B 0.8400 . ? O1B C11 1.41(2) . ? O1A H1A 0.84(2) . ? O1A C13 1.379(19) . ? N1 N2 1.319(9) . ? N1 C1 1.377(11) . ? N2 N3 1.355(9) . ? N3 C6 1.382(11) . ? N3 C7 1.466(10) . ? N4 C9 1.507(11) . ? N4 C10 1.511(11) . ? N4 C12 1.516(11) . ? N4 C14 1.505(12) . ? C1 C2 1.395(12) . ? C1 C6 1.395(11) . ? C2 H2 0.9500 . ? C2 C3 1.354(15) . ? C3 H3 0.9500 . ? C3 C4 1.415(15) . ? C4 H4 0.9500 . ? C4 C5 1.363(14) . ? C5 H5 0.9500 . ? C5 C6 1.379(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.524(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.508(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.510(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 H11 1.0000 . ? C11 C16 1.551(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.535(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 H13 1.0000 . ? C13 C16 1.484(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.522(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.545(16) . ? C16 H16 1.0000 . ? N5 C17 1.102(19) . ? C17 C18 1.41(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 Cu1 N1 N2 Cu2 14.1(10) . . . . ? Cu1 N1 N2 N3 -173.3(6) . . . . ? Cu1 N1 C1 C2 -7.5(16) . . . . ? Cu1 N1 C1 C6 172.1(6) . . . . ? Cu2 N2 N3 C6 172.1(6) . . . . ? Cu2 N2 N3 C7 -6.4(12) . . . . ? O1B C11 C16 C13 59.1(15) . . . . ? O1B C11 C16 C15 175.9(13) . . . . ? O1A C13 C16 C11 -61.8(13) . . . . ? O1A C13 C16 C15 -179.1(12) . . . . ? N1 N2 N3 C6 0.2(10) . . . . ? N1 N2 N3 C7 -178.3(8) . . . . ? N1 C1 C2 C3 178.2(11) . . . . ? N1 C1 C6 N3 1.8(11) . . . . ? N1 C1 C6 C5 -177.8(9) . . . . ? N2 N1 C1 C2 178.6(11) . . . . ? N2 N1 C1 C6 -1.8(11) . . . . ? N2 N3 C6 C1 -1.3(10) . . . . ? N2 N3 C6 C5 178.3(11) . . . . ? N2 N3 C7 C8 115.8(9) . . . . ? N3 C7 C8 C9 -173.6(8) . . . . ? N4 C10 C11 O1B -122.9(14) . . . . ? N4 C10 C11 C16 -2.7(13) . . . . ? N4 C12 C13 O1A 118.0(13) . . . . ? N4 C12 C13 C16 -0.9(13) . . . . ? N4 C14 C15 C16 -4.1(17) . . . . ? C1 N1 N2 Cu2 -171.6(6) . . . . ? C1 N1 N2 N3 1.0(10) . . . . ? C1 C2 C3 C4 0.1(18) . . . . ? C2 C1 C6 N3 -178.5(9) . . . . ? C2 C1 C6 C5 1.8(15) . . . . ? C2 C3 C4 C5 0.7(19) . . . . ? C3 C4 C5 C6 -0.3(16) . . . . ? C4 C5 C6 N3 179.5(11) . . . . ? C4 C5 C6 C1 -1.0(15) . . . . ? C6 N3 C7 C8 -62.4(13) . . . . ? C6 C1 C2 C3 -1.4(16) . . . . ? C7 N3 C6 C1 177.1(9) . . . . ? C7 N3 C6 C5 -3.3(18) . . . . ? C7 C8 C9 N4 -163.5(8) . . . . ? C9 N4 C10 C11 -179.1(9) . . . . ? C9 N4 C12 C13 -177.2(8) . . . . ? C9 N4 C14 C15 -179.2(10) . . . . ? C10 N4 C9 C8 -170.0(8) . . . . ? C10 N4 C12 C13 -58.4(10) . . . . ? C10 N4 C14 C15 62.0(13) . . . . ? C10 C11 C16 C13 -57.2(13) . . . . ? C10 C11 C16 C15 59.6(13) . . . . ? C12 N4 C9 C8 -51.2(10) . . . . ? C12 N4 C10 C11 60.5(11) . . . . ? C12 N4 C14 C15 -56.2(13) . . . . ? C12 C13 C16 C11 59.1(12) . . . . ? C12 C13 C16 C15 -58.2(13) . . . . ? C14 N4 C9 C8 71.0(11) . . . . ? C14 N4 C10 C11 -58.7(11) . . . . ? C14 N4 C12 C13 60.0(10) . . . . ? C14 C15 C16 C11 -56.2(15) . . . . ? C14 C15 C16 C13 61.8(15) . . . . ?