#------------------------------------------------------------------------------ #$Date: 2021-03-05 20:42:05 +0200 (Fri, 05 Mar 2021) $ #$Revision: 262766 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022308.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022308 loop_ _publ_author_name 'Cao, Bing-Jun' 'Li, Ran' 'Huang, Xi-He' _publ_section_title ; Synthesis, structure and photophysical properties of two tetranuclear copper(I) iodide complexes based on acetylpyridine and diphosphine mixed ligands ; _journal_coeditor_code KY3202 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 61 _journal_page_last 67 _journal_paper_doi 10.1107/S2053229620016745 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Cu4 I4 (C6 H7 N O)2 (C27 H26 P2)2]' _chemical_formula_sum 'C68 H66 Cu4 I4 N2 O2 P4' _chemical_formula_weight 1828.86 _chemical_name_systematic '[\m~2~-1,3-Bis(diphenylphosphanyl)propane-\k^2^P:P']di-\m~3~-iodido-di-\m~2~-iodido-[1-(pyridin-4-yl)ethan-1-one-\kN]tetracopper(I)' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/1 _cell_angle_alpha 62.49(3) _cell_angle_beta 68.32(3) _cell_angle_gamma 83.71(3) _cell_formula_units_Z 1 _cell_length_a 11.981(2) _cell_length_b 12.996(3) _cell_length_c 13.230(3) _cell_measurement_reflns_used 5949 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.03 _cell_measurement_theta_min 2.99 _cell_volume 1693.1(9) _computing_cell_refinement ; RAPID AUTO (Rigaku, 1998) ; _computing_data_collection ; RAPID AUTO (Rigaku, 1998) ; _computing_data_reduction ; RAPID AUTO (Rigaku, 1998) ; _computing_molecular_graphics ; SHELXTL/PC (Sheldrick, 1993) ; _computing_publication_material ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku R-axis RAPID' _diffrn_measurement_method Oscillation _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1119 _diffrn_reflns_av_unetI/netI 0.1584 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 13417 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 2.992 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 3.202 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (RAPID AUTO; Rigaku, 1998) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.794 _exptl_crystal_description block _exptl_crystal_F_000 892 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.054 _refine_diff_density_min -1.313 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 379 _refine_ls_number_reflns 5949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0642 _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^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.1539 _reflns_number_gt 3380 _reflns_number_total 5949 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3202sup1.cif _cod_data_source_block CuL4 _cod_depositor_comments 'Adding full bibliography for 2022307--2022308.cif.' _cod_original_cell_volume 1693.2(8) _cod_database_code 2022308 _cod_database_fobs_code 2022308 _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_hkl_file ; 0 0 2 29.88 4.53 0 0 2 8.91 14.41 0 0 3 2981.79 379.24 0 0 3 3089.18 298.25 0 0 4 1923.40 303.40 0 0 4 1987.91 163.05 0 0 5 79.86 6.33 0 0 5 71.73 4.45 0 0 5 87.77 25.77 0 0 6 1319.86 78.31 0 0 6 1304.87 79.16 0 0 6 1458.98 149.96 0 0 7 141.65 39.53 0 0 8 -0.26 13.00 0 0 9 798.18 108.24 0 0 10 222.43 69.44 0 0 11 13.56 20.19 0 0 12 -0.96 34.65 0 0 13 100.04 40.72 0 -1 12 81.40 54.62 0 -1 11 21.27 21.41 0 -1 10 280.48 82.94 0 -1 9 380.82 95.92 0 -1 8 -16.89 15.07 0 -1 7 135.38 24.30 0 -1 6 505.98 73.65 0 -1 6 416.36 16.32 0 -1 6 432.20 19.67 0 -1 5 505.11 28.27 0 -1 5 584.38 79.88 0 -1 5 540.39 28.29 0 1 -4 1041.28 94.55 0 -1 4 1172.89 78.89 0 -1 4 1132.51 159.50 0 -1 4 1151.35 72.02 0 1 -3 1085.64 133.18 0 -1 3 1209.64 79.06 0 -1 3 1203.59 168.16 0 1 -2 885.15 74.02 0 1 -2 943.62 59.76 0 -1 2 950.37 60.54 0 -1 2 948.45 80.68 0 1 -1 38.64 12.68 0 1 -1 39.15 6.73 0 -1 1 47.48 7.67 0 -1 1 35.38 3.90 0 1 2 175.95 13.41 0 -1 -2 180.91 8.31 0 1 3 8552.48 1865.14 0 -1 -3 8642.57 1915.43 0 1 4 2889.12 299.11 0 -1 -4 2709.73 293.89 0 1 5 0.58 9.65 0 1 5 1.58 5.52 0 -1 -5 3.23 5.25 0 1 6 453.35 25.41 0 1 6 374.07 64.17 0 -1 -6 429.16 22.91 0 1 7 25.41 3.31 0 1 7 21.85 12.42 0 1 8 30.40 26.15 0 1 9 802.57 109.49 0 1 10 322.93 85.80 0 1 11 -23.43 21.31 0 1 12 77.77 54.03 0 1 13 38.24 28.59 0 -2 12 7.35 22.38 0 -2 11 -7.86 19.68 0 -2 10 129.97 56.71 0 -2 9 234.35 69.83 0 -2 8 -4.82 14.38 0 -2 7 81.87 7.08 0 -2 7 95.21 5.49 0 -2 7 125.18 20.73 0 -2 6 19.08 4.43 0 -2 6 14.77 5.92 0 -2 6 -4.33 11.84 0 2 -5 161.06 19.83 0 -2 5 161.63 10.60 0 -2 5 179.07 21.45 0 2 -4 257.81 23.66 0 -2 4 231.54 25.76 0 -2 4 252.30 15.86 0 2 -3 157.92 15.91 0 2 -3 147.75 18.93 0 -2 3 198.36 16.88 0 -2 3 187.56 36.51 0 2 -2 130.54 16.95 0 2 -2 139.22 15.72 0 -2 2 128.66 32.37 0 -2 2 178.15 17.49 0 2 -1 1.72 5.12 0 -2 1 -0.54 9.36 0 -2 1 14.62 13.32 0 2 0 698.92 22.37 0 2 0 11.45 16.40 0 -2 0 710.43 63.51 0 2 1 53.34 8.28 0 -2 -1 68.14 8.13 0 2 2 206.60 15.28 0 -2 -2 235.08 16.36 0 2 3 853.91 52.11 0 -2 -3 922.89 59.06 0 2 4 737.15 58.18 0 -2 -4 812.60 69.80 0 2 5 14.21 6.87 0 -2 -5 21.72 7.68 0 2 6 452.99 26.26 0 -2 -6 420.62 24.34 0 2 7 215.19 17.08 0 -2 -7 189.94 15.15 0 2 8 145.63 9.73 0 2 8 204.67 42.26 0 -2 -8 171.00 13.44 0 2 9 143.50 7.45 0 2 9 192.98 28.18 0 2 10 36.50 33.99 0 2 11 18.41 19.76 0 2 12 68.28 49.71 0 2 13 17.60 25.01 0 -3 11 15.10 20.71 0 -3 10 19.28 34.23 0 -3 9 -1.03 27.53 0 -3 8 -2.27 3.04 0 -3 8 -17.39 14.66 0 -3 8 -0.28 3.70 0 -3 7 128.16 12.88 0 -3 7 125.91 13.64 0 -3 7 154.24 25.82 0 3 -6 146.43 21.24 0 -3 6 138.84 23.35 0 -3 6 145.05 11.94 0 3 -5 4.24 8.58 0 -3 5 5.87 5.85 0 -3 5 -4.68 17.45 0 3 -4 240.97 20.09 0 3 -4 195.83 23.11 0 -3 4 244.81 18.99 0 -3 4 241.40 40.74 0 3 -3 90.27 13.21 0 3 -3 96.44 14.16 0 -3 3 80.10 11.88 0 -3 3 78.69 22.84 0 3 -2 207.90 25.21 0 3 -2 234.46 22.35 0 -3 2 217.46 35.60 0 -3 2 201.95 23.84 0 3 -1 112.31 11.27 0 3 -1 97.89 24.64 0 -3 1 106.00 20.73 0 -3 1 136.24 25.41 0 3 0 91.36 19.32 0 3 0 67.21 11.83 0 -3 0 74.21 11.28 0 3 1 598.25 45.66 0 -3 -1 588.07 43.35 0 3 2 609.44 46.55 0 -3 -2 576.17 41.48 0 3 3 126.76 22.60 0 -3 -3 121.17 23.52 0 3 4 473.14 32.70 0 -3 -4 520.05 35.40 0 3 5 38.41 6.41 0 -3 -5 35.61 12.42 0 3 6 169.88 10.41 0 -3 -6 188.90 18.47 0 3 7 199.49 17.11 0 -3 -7 187.82 15.89 0 3 8 9.92 6.36 0 -3 -8 -0.79 5.58 0 3 9 279.23 42.85 0 3 9 299.34 19.99 0 -3 -9 276.36 18.52 0 3 10 124.32 50.49 0 3 10 162.00 14.41 0 -3 -10 168.52 12.30 0 3 11 65.03 20.84 0 3 11 30.44 4.55 0 3 12 -5.46 19.94 0 3 13 -27.79 42.99 0 3 14 -4.83 24.32 0 -4 10 40.09 39.71 0 -4 9 65.42 41.39 0 -4 8 33.51 15.47 0 -4 8 3.23 6.30 0 -4 8 2.54 4.67 0 -4 7 4.82 7.68 0 -4 7 31.67 15.96 0 -4 7 46.48 7.57 0 4 -6 44.28 24.55 0 -4 6 19.24 7.46 0 -4 6 28.48 23.50 0 4 -5 -11.03 17.35 0 4 -5 9.79 6.28 0 -4 5 0.54 7.15 0 -4 5 6.06 16.92 0 4 -4 1135.20 151.11 0 4 -4 1143.80 102.17 0 -4 4 1123.19 108.27 0 -4 4 1162.95 100.15 0 4 -3 1032.60 129.51 0 4 -3 1037.82 69.93 0 -4 3 1129.81 103.33 0 -4 3 1138.78 139.80 0 4 -2 150.01 19.23 0 4 -2 193.16 29.05 0 -4 2 155.85 12.78 0 -4 2 167.19 16.94 0 4 -1 454.94 53.97 0 4 -1 441.04 30.65 0 -4 1 4.06 21.66 0 -4 1 464.81 21.77 0 4 0 1788.42 244.49 0 4 0 1981.41 252.23 0 -4 0 1737.19 220.88 0 4 1 2529.29 362.79 0 -4 -1 2429.73 266.06 0 4 2 363.11 32.02 0 -4 -2 424.45 52.77 0 4 3 74.56 13.07 0 -4 -3 57.41 19.86 0 4 4 1563.81 143.00 0 -4 -4 1464.90 129.24 0 4 5 53.06 15.05 0 -4 -5 53.28 8.61 0 4 6 490.93 44.92 0 -4 -6 543.03 53.30 0 4 7 44.68 6.62 0 -4 -7 35.28 11.66 0 4 8 -6.41 8.36 0 -4 -8 5.35 5.03 0 4 9 560.66 45.82 0 -4 -9 495.21 37.55 0 4 10 857.40 67.99 0 -4 -10 786.98 62.53 0 4 11 3.10 5.74 0 4 11 7.97 29.00 0 -4 -11 19.03 7.43 0 4 12 9.05 22.35 0 4 12 44.10 7.88 0 -4 -12 44.13 6.64 0 4 13 106.26 61.90 0 4 14 12.77 25.13 0 -5 10 31.99 37.60 0 -5 9 134.98 56.18 0 -5 8 4.25 6.63 0 -5 8 11.70 7.09 0 -5 8 11.73 16.05 0 5 -7 36.65 16.03 0 -5 7 -6.20 7.20 0 -5 7 51.69 22.60 0 5 -6 77.89 28.03 0 -5 6 103.11 34.46 0 -5 6 97.87 14.88 0 5 -5 84.94 9.97 0 5 -5 75.84 28.54 0 -5 5 81.31 8.42 0 -5 5 83.07 29.42 0 5 -4 681.93 66.39 0 5 -4 692.40 65.53 0 -5 4 845.19 79.01 0 -5 4 772.37 75.15 0 5 -3 1695.85 181.05 0 5 -3 1663.64 145.70 0 -5 3 1742.62 159.28 0 -5 3 1804.71 190.86 0 5 -2 -15.97 13.33 0 5 -2 3.97 9.71 0 -5 2 5.51 8.09 0 -5 2 -7.55 9.96 0 5 -1 440.05 53.70 0 5 -1 448.41 31.25 0 -5 1 440.62 48.85 0 5 0 5282.99 912.91 0 5 0 5329.52 919.69 0 -5 0 5014.76 837.53 0 5 1 979.55 81.01 0 -5 -1 924.29 74.73 0 5 2 349.40 50.97 0 -5 -2 291.04 41.03 0 5 3 -0.72 8.33 0 -5 -3 4.80 13.48 0 5 4 1385.48 168.81 0 -5 -4 1330.68 118.75 0 5 5 250.76 34.15 0 -5 -5 243.40 20.84 0 5 6 2610.36 349.26 0 -5 -6 2456.40 322.28 0 5 7 8.55 10.90 0 -5 -7 9.90 12.32 0 5 8 5.30 10.19 0 -5 -8 24.40 7.51 0 5 9 448.57 44.40 0 -5 -9 483.48 49.98 0 5 10 768.44 71.16 0 -5 -10 667.94 59.32 0 5 11 4.37 8.61 0 -5 -11 8.14 8.03 0 5 12 16.49 19.26 0 5 12 7.85 11.36 0 -5 -12 -3.89 8.61 0 5 13 338.47 29.68 0 5 13 310.23 62.04 0 -5 -13 286.59 24.09 0 5 14 49.46 53.34 0 -6 9 77.80 27.43 0 -6 8 7.31 12.35 0 -6 8 -6.58 15.54 0 -6 8 2.26 8.20 0 6 -7 159.90 28.50 0 -6 7 79.53 15.28 0 -6 7 184.39 40.78 0 6 -6 213.02 29.94 0 -6 6 137.49 21.78 0 -6 6 216.75 45.78 0 6 -5 231.41 30.00 0 6 -5 189.37 28.63 0 -6 5 196.37 26.10 0 -6 5 193.10 28.85 0 6 -4 195.97 27.10 0 6 -4 197.89 25.62 0 -6 4 233.69 26.37 0 -6 4 193.88 16.44 0 6 -3 497.07 36.46 0 6 -3 531.07 73.95 0 -6 3 512.44 56.76 0 -6 3 601.71 54.33 0 6 -2 -7.21 11.30 0 6 -2 15.28 14.19 0 -6 2 7.10 12.05 0 6 -1 100.18 19.70 0 6 -1 46.90 17.77 0 -6 1 47.62 9.85 0 6 0 3644.81 606.65 0 6 0 3801.80 619.47 0 -6 0 3559.17 582.39 0 6 1 664.25 82.10 0 -6 -1 619.05 76.24 0 6 2 71.99 12.76 0 -6 -2 90.81 12.81 0 6 3 678.83 85.84 0 -6 -3 621.73 74.54 0 6 4 1213.74 109.00 0 -6 -4 1097.48 97.56 0 6 5 9.40 8.22 0 -6 -5 5.93 7.98 0 6 6 2338.06 315.01 0 -6 -6 2089.51 271.37 0 6 7 37.46 15.42 0 -6 -7 25.20 15.10 0 6 8 12.38 7.51 0 -6 -8 19.74 8.81 0 6 9 934.97 103.91 0 -6 -9 887.65 107.60 0 6 10 417.64 47.33 0 -6 -10 402.03 53.66 0 6 11 -3.97 10.95 0 -6 -11 9.44 11.14 0 6 12 -0.35 9.67 0 -6 -12 -2.76 5.32 0 6 13 280.06 36.93 0 6 13 164.27 53.24 0 -6 -13 194.79 17.18 0 6 14 19.34 23.57 0 -7 8 16.87 18.27 0 7 -7 -8.20 14.76 0 -7 7 47.59 18.87 0 -7 7 18.77 19.46 0 7 -6 -2.55 12.62 0 -7 6 11.36 11.46 0 -7 6 4.06 24.50 0 7 -5 68.82 20.38 0 7 -5 111.80 21.82 0 -7 5 99.10 12.79 0 -7 5 104.72 37.10 0 7 -4 200.70 30.63 0 7 -4 275.41 34.55 0 -7 4 226.29 31.82 0 -7 4 223.67 33.16 0 7 -3 21.22 8.71 0 7 -3 31.74 20.48 0 -7 3 8.61 7.61 0 7 -2 119.26 30.22 0 7 -2 133.38 15.46 0 -7 2 148.68 15.60 0 7 -1 38.75 19.11 0 7 -1 41.88 10.05 0 -7 1 33.89 15.97 0 7 0 464.47 61.46 0 7 0 486.31 40.16 0 -7 0 463.39 57.42 0 7 1 404.67 23.42 0 7 1 22.75 19.76 0 -7 -1 378.59 32.15 0 7 2 402.80 57.43 0 -7 -2 342.60 29.90 0 7 3 368.47 33.29 0 -7 -3 332.89 46.92 0 7 4 1095.63 141.88 0 -7 -4 1041.43 94.14 0 7 5 15.79 16.40 0 -7 -5 3.71 14.27 0 7 6 7.31 8.70 0 -7 -6 -1.61 13.73 0 7 7 67.38 12.48 0 -7 -7 47.51 10.86 0 7 8 159.61 29.45 0 -7 -8 114.21 15.99 0 7 9 864.01 104.47 0 -7 -9 860.44 113.91 0 7 10 147.91 17.17 0 -7 -10 200.18 36.40 0 7 11 5.14 12.70 0 -7 -11 -12.11 16.65 0 7 12 98.20 20.88 0 -7 -12 33.95 16.97 0 7 13 98.87 11.78 0 -7 -13 109.99 18.92 0 7 14 18.19 15.63 0 7 14 -15.71 22.30 0 -7 -14 26.53 16.63 0 8 -7 -40.45 19.53 0 -8 7 13.06 17.58 0 -8 7 -10.57 16.32 0 8 -6 -14.42 14.61 0 -8 6 -51.82 22.91 0 -8 6 -17.43 19.68 0 8 -5 41.56 20.00 0 8 -5 42.42 16.79 0 -8 5 0.32 19.34 0 -8 5 56.35 16.09 0 8 -4 -3.67 19.29 0 8 -4 86.83 16.19 0 -8 4 36.20 10.70 0 8 -3 29.88 10.19 0 8 -3 37.48 23.97 0 -8 3 13.43 16.29 0 8 -2 185.18 40.34 0 8 -2 198.89 20.94 0 -8 2 175.94 32.99 0 8 -1 17.75 9.81 0 8 -1 -4.28 8.64 0 -8 1 -5.23 8.78 0 8 0 22.06 19.86 0 8 0 45.85 11.30 0 -8 0 20.95 9.98 0 8 1 -13.68 14.88 0 8 1 19.31 15.97 0 -8 -1 14.42 9.65 0 8 2 246.09 27.67 0 -8 -2 228.38 39.73 0 8 3 52.37 22.93 0 -8 -3 73.28 24.74 0 8 4 398.73 38.71 0 -8 -4 302.84 32.23 0 8 5 -2.02 9.41 0 -8 -5 8.93 17.27 0 8 6 130.29 30.97 0 -8 -6 90.22 15.21 0 8 7 524.80 75.65 0 -8 -7 493.27 44.53 0 8 8 571.96 80.75 0 -8 -8 496.83 72.50 0 8 9 81.04 15.00 0 -8 -9 126.86 31.67 0 8 10 75.97 14.30 0 -8 -10 125.34 30.63 0 8 11 118.05 28.10 0 -8 -11 127.79 31.26 0 8 12 78.97 13.68 0 -8 -12 25.46 12.04 0 8 13 29.12 16.11 0 -8 -13 31.70 19.60 0 8 14 10.68 20.21 0 -8 -14 6.57 8.49 0 9 -6 30.85 17.73 0 -9 6 13.28 13.47 0 9 -5 62.65 20.25 0 9 -5 0.37 16.06 0 -9 5 14.80 13.50 0 9 -4 140.04 31.11 0 9 -4 126.49 25.34 0 -9 4 125.18 28.10 0 9 -3 152.59 31.11 0 9 -3 133.70 25.16 0 -9 3 207.73 24.32 0 9 -2 66.68 26.95 0 9 -2 53.62 23.10 0 -9 2 56.43 14.38 0 9 -1 -25.97 18.05 0 9 -1 7.91 19.13 0 -9 1 35.45 21.68 0 9 0 -6.21 10.08 0 9 0 1.90 17.05 0 -9 0 1.72 17.77 0 9 1 346.37 33.55 0 9 1 316.20 36.25 0 -9 -1 295.84 54.92 0 9 2 103.47 32.48 0 -9 -2 97.86 30.96 0 9 3 9.69 11.77 0 -9 -3 18.15 12.01 0 9 4 43.80 24.89 0 -9 -4 33.39 13.66 0 9 5 11.35 19.48 0 -9 -5 7.15 18.53 0 9 6 222.96 28.73 0 -9 -6 220.40 26.40 0 9 7 313.46 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19.40 -13 -3 -6 63.11 31.25 -13 -3 -7 70.11 11.69 -13 -3 -7 25.43 44.75 -13 -3 -8 -3.37 14.44 -13 -3 -9 4.02 17.90 -13 -3 -9 10.75 16.80 -13 -3 -10 -13.73 21.77 -13 -3 -10 65.00 19.57 -13 -3 -10 14.79 21.07 -13 -3 -11 21.10 16.88 -13 -3 -11 29.38 30.02 -13 -3 -11 9.29 12.19 -13 -4 -2 17.22 23.61 -13 -4 -3 92.20 54.04 -13 -4 -4 -11.35 35.17 -13 -4 -5 22.91 37.24 -13 -4 -6 65.54 11.53 -13 -4 -6 4.04 45.65 -13 -4 -7 -31.50 34.00 -13 -4 -7 110.87 16.43 -13 -4 -7 154.28 50.72 -13 -4 -8 49.62 23.97 -13 -4 -8 19.70 13.36 -13 -4 -8 8.36 35.65 -13 -4 -9 10.75 16.79 -13 -4 -9 -17.70 16.74 -13 -4 -9 -0.21 7.40 -13 -4 -10 13.72 19.09 -13 -4 -10 33.33 35.05 -13 -4 -10 55.57 20.78 -13 -4 -11 18.85 10.66 -13 -4 -11 -12.92 15.60 -13 -5 -3 -13.85 22.15 -13 -5 -3 59.19 23.98 -13 -5 -4 38.40 25.76 -13 -5 -4 47.64 27.83 -13 -5 -5 54.09 22.64 -13 -5 -5 1.16 22.14 -13 -5 -6 80.35 27.18 -13 -5 -6 26.91 45.64 -13 -5 -7 109.59 31.20 -13 -5 -7 68.99 52.03 -13 -5 -8 23.07 30.21 -13 -5 -8 -8.28 17.41 -13 -5 -9 62.50 33.49 -13 -5 -9 12.78 20.73 -13 -5 -10 160.01 36.16 -13 -5 -10 173.35 38.30 -13 -5 -11 7.94 28.75 -13 -5 -11 12.70 29.77 -13 -6 -4 12.71 22.99 -13 -6 -4 54.67 40.95 -13 -6 -5 116.07 49.49 -13 -6 -5 70.55 32.29 -13 -6 -6 23.04 21.88 -13 -6 -6 40.60 21.25 -13 -6 -7 -28.93 20.46 -13 -6 -7 -15.03 20.76 -13 -6 -8 -47.24 18.27 -13 -6 -8 33.76 18.27 -13 -6 -9 78.32 36.65 -13 -6 -9 20.53 21.82 -13 -6 -10 30.79 40.43 -13 -6 -10 80.89 42.01 -13 -6 -11 7.18 18.69 -13 -6 -11 32.96 31.16 -13 -7 -5 -4.96 36.15 -13 -7 -5 35.37 37.94 -13 -7 -6 56.37 39.56 -13 -7 -6 10.61 39.96 -13 -7 -7 85.10 43.38 -13 -7 -7 13.36 46.10 -13 -7 -8 9.81 20.82 -13 -7 -8 31.88 34.31 -13 -7 -9 32.34 22.00 -13 -7 -9 -7.85 35.20 -13 -7 -10 42.79 31.68 -13 -7 -10 -30.08 29.58 -14 1 -4 66.96 26.55 -14 1 -4 0.56 24.83 -14 1 -5 46.21 28.19 -14 1 -5 50.70 29.06 -14 0 -3 43.00 27.38 -14 0 -3 25.74 22.73 -14 0 -4 20.94 23.89 -14 0 -4 11.42 20.00 -14 0 -5 178.63 41.92 -14 0 -5 231.64 48.42 -14 0 -6 37.53 43.97 -14 0 -6 40.06 14.51 -14 0 -7 28.30 32.84 -14 0 -7 -9.58 20.06 -14 -1 -3 122.49 57.35 -14 -1 -3 65.36 13.08 -14 -1 -4 74.17 37.76 -14 -1 -4 108.02 15.86 -14 -1 -5 129.32 28.27 -14 -1 -5 106.05 67.51 -14 -1 -6 38.79 21.03 -14 -1 -6 45.90 46.04 -14 -1 -7 9.95 38.79 -14 -1 -7 28.17 19.86 -14 -2 -4 124.55 22.19 -14 -2 -4 46.84 67.99 -14 -2 -5 -3.82 13.05 -14 -2 -5 16.23 36.62 -14 -2 -6 -10.93 41.46 -14 -2 -6 28.55 10.41 -14 -2 -7 119.87 17.39 -14 -2 -7 68.96 60.77 -14 -2 -8 38.16 13.97 -14 -2 -8 33.99 24.91 -14 -3 -5 -2.42 21.78 -14 -3 -6 39.81 26.87 -14 -3 -7 155.23 16.73 -14 -3 -7 64.93 40.07 -14 -3 -8 15.64 9.58 -14 -3 -8 1.08 21.65 -14 -4 -6 42.89 27.45 -14 -4 -7 28.23 24.23 -14 -4 -7 0.32 22.30 -14 -4 -8 -18.19 24.13 -14 -4 -8 41.47 21.96 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 46545 _shelx_res_file ; TITL a in P-1 a.res created by SHELXL-2018/1 at 17:09:21 on 21-Dec-2020 CELL 0.71073 11.9813 12.9958 13.2303 62.491 68.318 83.714 ZERR 1.00 0.0024 0.0026 0.0026 0.030 0.030 0.030 LATT 1 SFAC C H N O P CU I UNIT 68 66 2 2 4 4 4 ACTA L.S. 10 BOND $H EQIV $1 -x+2, -y+1, -z EQIV $2 x+1, y, z EQIV $3 x-1, y, z HTAB C2 I1_$1 HTAB C14 O1_$2 HTAB C15 O1_$2 HTAB C32 I2 HTAB C34 I2_$3 CONF FMAP 2 PLAN 10 WGHT 0.027000 FVAR 0.33013 I1 7 0.845335 0.407481 0.043765 11.00000 0.03620 0.04782 = 0.05105 -0.02640 -0.01091 0.00816 I2 7 0.838880 0.578093 0.269924 11.00000 0.05002 0.05357 = 0.05413 -0.02905 -0.01552 0.00270 CU1 6 1.094344 0.392765 -0.046893 11.00000 0.06103 0.05572 = 0.05497 -0.02244 -0.02370 0.02156 CU2 6 0.746474 0.400787 0.266595 11.00000 0.03991 0.04614 = 0.05380 -0.02126 -0.01689 0.01163 P1 5 1.137117 0.225959 0.089507 11.00000 0.03618 0.04176 = 0.04131 -0.01973 -0.01119 0.01416 P2 5 0.779828 0.240937 0.416786 11.00000 0.03476 0.04480 = 0.04252 -0.02377 -0.01196 0.00883 N1 3 0.571664 0.438234 0.283725 11.00000 0.04415 0.05405 = 0.06000 -0.03011 -0.01805 0.01629 C1 1 1.289345 0.224394 0.092135 11.00000 0.03841 0.04230 = 0.03335 -0.02096 -0.01307 0.00609 C2 1 1.366804 0.321437 0.016222 11.00000 0.03747 0.05421 = 0.06551 -0.01711 -0.01002 0.00983 AFIX 43 H2A 2 1.341316 0.389392 -0.034145 11.00000 -1.20000 AFIX 0 C3 1 1.481722 0.318824 0.014168 11.00000 0.03970 0.08040 = 0.06293 -0.02180 -0.00719 -0.00632 AFIX 43 H3A 2 1.533874 0.385333 -0.039362 11.00000 -1.20000 AFIX 0 C4 1 1.522322 0.223320 0.086928 11.00000 0.03895 0.08893 = 0.10939 -0.06447 -0.03674 0.02852 AFIX 43 H4A 2 1.600688 0.223603 0.084963 11.00000 -1.20000 AFIX 0 C5 1 1.445777 0.127186 0.162786 11.00000 0.09801 0.05177 = 0.15989 -0.02969 -0.09068 0.02287 AFIX 43 H5A 2 1.472488 0.059774 0.212553 11.00000 -1.20000 AFIX 0 C6 1 1.327055 0.126994 0.167990 11.00000 0.05782 0.06713 = 0.10577 -0.00351 -0.04565 0.00579 AFIX 43 H6A 2 1.274463 0.060973 0.222734 11.00000 -1.20000 AFIX 0 C7 1 1.124013 0.093071 0.079397 11.00000 0.03564 0.04647 = 0.05630 -0.02952 -0.02001 0.01887 C8 1 1.191773 0.088283 -0.026940 11.00000 0.08155 0.06009 = 0.05041 -0.03200 -0.01999 0.01408 AFIX 43 H8A 2 1.241000 0.153271 -0.092066 11.00000 -1.20000 AFIX 0 C9 1 1.188888 -0.010216 -0.039894 11.00000 0.08059 0.10167 = 0.08387 -0.06813 -0.01342 0.02198 AFIX 43 H9A 2 1.238394 -0.011780 -0.112275 11.00000 -1.20000 AFIX 0 C10 1 1.113226 -0.107421 0.053379 11.00000 0.08948 0.07798 = 0.11779 -0.07142 -0.05951 0.02792 AFIX 43 H10A 2 1.108179 -0.172510 0.042846 11.00000 -1.20000 AFIX 0 C11 1 1.048145 -0.105089 0.158178 11.00000 0.09332 0.05786 = 0.08458 -0.03090 -0.03422 -0.00328 AFIX 43 H11A 2 0.999612 -0.170454 0.223444 11.00000 -1.20000 AFIX 0 C12 1 1.052590 -0.002937 0.170668 11.00000 0.06673 0.05999 = 0.07611 -0.03395 -0.02574 0.00970 AFIX 43 H12A 2 1.004881 -0.002103 0.243910 11.00000 -1.20000 AFIX 0 C13 1 1.036595 0.187258 0.244986 11.00000 0.04559 0.04619 = 0.05230 -0.01646 -0.01570 0.02013 AFIX 23 H13A 2 0.956337 0.169134 0.253179 11.00000 -1.20000 H13B 2 1.062212 0.117121 0.299562 11.00000 -1.20000 AFIX 0 C14 1 1.029702 0.278879 0.286145 11.00000 0.02903 0.04654 = 0.05090 -0.02399 -0.01375 0.00928 AFIX 23 H14A 2 1.012456 0.351706 0.227213 11.00000 -1.20000 H14B 2 1.107409 0.290651 0.287873 11.00000 -1.20000 AFIX 0 C15 1 0.933719 0.247043 0.412006 11.00000 0.05576 0.05019 = 0.05022 -0.02903 -0.01462 0.00050 AFIX 23 H15A 2 0.941161 0.303859 0.437886 11.00000 -1.20000 H15B 2 0.948274 0.171858 0.469806 11.00000 -1.20000 AFIX 0 C16 1 0.752406 0.098635 0.430008 11.00000 0.02732 0.04243 = 0.04733 -0.02135 -0.01114 -0.00002 C17 1 0.799427 -0.001380 0.491686 11.00000 0.08708 0.04424 = 0.08148 -0.02087 -0.04536 0.00416 AFIX 43 H17A 2 0.849100 0.001006 0.530573 11.00000 -1.20000 AFIX 0 C18 1 0.775355 -0.103640 0.497423 11.00000 0.10650 0.04901 = 0.10474 -0.02063 -0.05822 0.00551 AFIX 43 H18A 2 0.806441 -0.170907 0.541931 11.00000 -1.20000 AFIX 0 C19 1 0.705225 -0.108270 0.437743 11.00000 0.09530 0.05071 = 0.08549 -0.03479 -0.02795 -0.00191 AFIX 43 H19A 2 0.691618 -0.178094 0.439148 11.00000 -1.20000 AFIX 0 C20 1 0.655144 -0.010809 0.376144 11.00000 0.11123 0.05621 = 0.08001 -0.03464 -0.05852 0.01269 AFIX 43 H20A 2 0.604960 -0.013915 0.338065 11.00000 -1.20000 AFIX 0 C21 1 0.680858 0.091536 0.372009 11.00000 0.08188 0.04035 = 0.06562 -0.01700 -0.04150 0.00163 AFIX 43 H21A 2 0.648890 0.158660 0.328499 11.00000 -1.20000 AFIX 0 C22 1 0.683562 0.218475 0.571465 11.00000 0.03943 0.03855 = 0.04259 -0.02998 -0.00872 0.01340 C23 1 0.724806 0.187105 0.665780 11.00000 0.05680 0.07393 = 0.04526 -0.02471 -0.02437 0.01868 AFIX 43 H23A 2 0.806462 0.178594 0.651742 11.00000 -1.20000 AFIX 0 C24 1 0.645847 0.168191 0.781031 11.00000 0.06717 0.07735 = 0.05703 -0.03497 -0.02498 0.01543 AFIX 43 H24A 2 0.674328 0.148542 0.843764 11.00000 -1.20000 AFIX 0 C25 1 0.525704 0.178701 0.801584 11.00000 0.05844 0.08219 = 0.05670 -0.03933 -0.00568 0.00239 AFIX 43 H25A 2 0.472593 0.163210 0.879777 11.00000 -1.20000 AFIX 0 C26 1 0.480993 0.211681 0.709478 11.00000 0.03348 0.07535 = 0.06070 -0.04245 0.00223 -0.00525 AFIX 43 H26A 2 0.399431 0.221198 0.723675 11.00000 -1.20000 AFIX 0 C27 1 0.561092 0.229896 0.596371 11.00000 0.03104 0.06707 = 0.04728 -0.02725 -0.00430 0.00286 AFIX 43 H27A 2 0.532147 0.250777 0.533724 11.00000 -1.20000 AFIX 0 C28 1 0.506201 0.386347 0.257519 11.00000 0.04756 0.05134 = 0.05998 -0.02294 -0.00739 0.01090 AFIX 43 H28A 2 0.545805 0.341120 0.219148 11.00000 -1.20000 AFIX 0 C29 1 0.385014 0.392675 0.281468 11.00000 0.04715 0.05353 = 0.08751 -0.05108 -0.01935 0.00531 AFIX 43 H29A 2 0.344730 0.355154 0.258231 11.00000 -1.20000 AFIX 0 C30 1 0.325216 0.456710 0.341242 11.00000 0.04184 0.04247 = 0.06685 -0.03178 -0.02085 0.01495 C31 1 0.389519 0.511698 0.370423 11.00000 0.03790 0.09870 = 0.11675 -0.08364 -0.02499 0.02071 AFIX 43 H31A 2 0.352262 0.557765 0.408470 11.00000 -1.20000 AFIX 0 C32 1 0.511975 0.497547 0.342168 11.00000 0.04680 0.06224 = 0.06719 -0.04621 -0.02185 0.00863 AFIX 43 H32A 2 0.554468 0.532259 0.366131 11.00000 -1.20000 AFIX 0 C33 1 0.186971 0.460971 0.379557 11.00000 0.04424 0.06115 = 0.11709 -0.05938 -0.02937 0.02677 C34 1 0.140748 0.574898 0.348724 11.00000 0.05202 0.08040 = 0.25285 -0.05990 -0.05070 0.02458 AFIX 33 H34A 2 0.206577 0.633003 0.307392 11.00000 -1.50000 H34B 2 0.096937 0.589140 0.296225 11.00000 -1.50000 H34C 2 0.088070 0.578119 0.422102 11.00000 -1.50000 AFIX 0 O1 4 0.127443 0.373364 0.430497 11.00000 0.05325 0.06739 = 0.21289 -0.07115 -0.03887 -0.00859 HKLF 4 REM a in P-1 REM R1 = 0.0642 for 3380 Fo > 4sig(Fo) and 0.1266 for all 5949 data REM 379 parameters refined using 0 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 1.054, deepest hole -1.313, 1-sigma level 0.168 Q1 1 0.8873 0.3967 -0.0285 11.00000 0.05 1.05 Q2 1 0.7967 0.5965 0.3414 11.00000 0.05 1.04 Q3 1 1.1582 0.5024 -0.1617 11.00000 0.05 0.90 Q4 1 0.6991 0.4144 0.3439 11.00000 0.05 0.87 Q5 1 0.8564 0.4568 0.2613 11.00000 0.05 0.84 Q6 1 0.7956 0.4205 0.1175 11.00000 0.05 0.83 Q7 1 0.7413 0.4993 0.3827 11.00000 0.05 0.80 Q8 1 0.8932 0.5596 0.1823 11.00000 0.05 0.78 Q9 1 0.8051 0.3832 -0.0447 11.00000 0.05 0.74 Q10 1 0.7458 0.3182 0.1562 11.00000 0.05 0.74 ; _shelx_res_checksum 26138 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 0.84534(6) 0.40748(6) 0.04377(6) 0.0454(2) Uani d 1 . . I I2 0.83888(7) 0.57809(6) 0.26992(6) 0.0516(2) Uani d 1 . . Cu Cu1 1.09434(13) 0.39277(12) -0.04689(12) 0.0591(4) Uani d 1 . . Cu Cu2 0.74647(11) 0.40079(11) 0.26659(11) 0.0480(4) Uani d 1 . . P P1 1.1371(2) 0.2260(2) 0.0895(2) 0.0413(7) Uani d 1 . . P P2 0.7798(2) 0.2409(2) 0.4168(2) 0.0402(6) Uani d 1 . . N N1 0.5717(8) 0.4382(8) 0.2837(8) 0.052(2) Uani d 1 . . C C1 1.2893(9) 0.2244(8) 0.0921(8) 0.037(2) Uani d 1 . . C C2 1.3668(10) 0.3214(10) 0.0162(10) 0.060(3) Uani d 1 . . H H2A 1.341316 0.389392 -0.034145 0.072 Uiso calc 1 . . C C3 1.4817(11) 0.3188(11) 0.0142(10) 0.068(4) Uani d 1 . . H H3A 1.533874 0.385333 -0.039362 0.082 Uiso calc 1 . . C C4 1.5223(11) 0.2233(12) 0.0869(12) 0.070(4) Uani d 1 . . H H4A 1.600688 0.223603 0.084963 0.084 Uiso calc 1 . . C C5 1.4458(15) 0.1272(12) 0.1628(15) 0.098(5) Uani d 1 . . H H5A 1.472488 0.059774 0.212553 0.118 Uiso calc 1 . . C C6 1.3271(12) 0.1270(11) 0.1680(12) 0.087(5) Uani d 1 . . H H6A 1.274463 0.060973 0.222734 0.104 Uiso calc 1 . . C C7 1.1240(9) 0.0931(9) 0.0794(9) 0.044(3) Uani d 1 . . C C8 1.1918(12) 0.0883(10) -0.0269(10) 0.063(3) Uani d 1 . . H H8A 1.241000 0.153271 -0.092066 0.076 Uiso calc 1 . . C C9 1.1889(13) -0.0102(13) -0.0399(12) 0.084(4) Uani d 1 . . H H9A 1.238394 -0.011780 -0.112275 0.101 Uiso calc 1 . . C C10 1.1132(14) -0.1074(12) 0.0534(14) 0.079(4) Uani d 1 . . H H10A 1.108179 -0.172510 0.042846 0.094 Uiso calc 1 . . C C11 1.0481(13) -0.1051(11) 0.1582(12) 0.078(4) Uani d 1 . . H H11A 0.999612 -0.170454 0.223444 0.093 Uiso calc 1 . . C C12 1.0526(12) -0.0029(10) 0.1707(11) 0.067(3) Uani d 1 . . H H12A 1.004881 -0.002103 0.243910 0.080 Uiso calc 1 . . C C13 1.0366(10) 0.1873(9) 0.2450(9) 0.053(3) Uani d 1 . . H H13A 0.956337 0.169134 0.253179 0.063 Uiso calc 1 . . H H13B 1.062212 0.117121 0.299562 0.063 Uiso calc 1 . . C C14 1.0297(9) 0.2789(8) 0.2861(8) 0.042(2) Uani d 1 . . H H14A 1.012456 0.351706 0.227213 0.051 Uiso calc 1 . . H H14B 1.107409 0.290651 0.287873 0.051 Uiso calc 1 . . C C15 0.9337(10) 0.2470(9) 0.4120(9) 0.051(3) Uani d 1 . . H H15A 0.941161 0.303859 0.437886 0.061 Uiso calc 1 . . H H15B 0.948274 0.171858 0.469806 0.061 Uiso calc 1 . . C C16 0.7524(8) 0.0986(8) 0.4300(8) 0.039(2) Uani d 1 . . C C17 0.7994(12) -0.0014(9) 0.4917(11) 0.069(4) Uani d 1 . . H H17A 0.849100 0.001006 0.530573 0.083 Uiso calc 1 . . C C18 0.7754(14) -0.1036(11) 0.4974(13) 0.086(5) Uani d 1 . . H H18A 0.806441 -0.170907 0.541931 0.104 Uiso calc 1 . . C C19 0.7052(13) -0.1083(11) 0.4377(12) 0.076(4) Uani d 1 . . H H19A 0.691618 -0.178094 0.439148 0.092 Uiso calc 1 . . C C20 0.6551(13) -0.0108(10) 0.3761(11) 0.074(4) Uani d 1 . . H H20A 0.604960 -0.013915 0.338065 0.089 Uiso calc 1 . . C C21 0.6809(11) 0.0915(9) 0.3720(10) 0.061(3) Uani d 1 . . H H21A 0.648890 0.158660 0.328499 0.073 Uiso calc 1 . . C C22 0.6836(9) 0.2185(8) 0.5715(8) 0.038(2) Uani d 1 . . C C23 0.7248(11) 0.1871(9) 0.6658(9) 0.059(3) Uani d 1 . . H H23A 0.806462 0.178594 0.651742 0.071 Uiso calc 1 . . C C24 0.6458(12) 0.1682(10) 0.7810(10) 0.065(3) Uani d 1 . . H H24A 0.674328 0.148542 0.843764 0.079 Uiso calc 1 . . C C25 0.5257(12) 0.1787(11) 0.8016(11) 0.067(3) Uani d 1 . . H H25A 0.472593 0.163210 0.879777 0.081 Uiso calc 1 . . C C26 0.4810(10) 0.2117(10) 0.7095(10) 0.057(3) Uani d 1 . . H H26A 0.399431 0.221198 0.723675 0.068 Uiso calc 1 . . C C27 0.5611(9) 0.2299(9) 0.5964(9) 0.051(3) Uani d 1 . . H H27A 0.532147 0.250777 0.533724 0.061 Uiso calc 1 . . C C28 0.5062(11) 0.3863(9) 0.2575(10) 0.059(3) Uani d 1 . . H H28A 0.545805 0.341120 0.219148 0.070 Uiso calc 1 . . C C29 0.3850(10) 0.3927(9) 0.2815(10) 0.057(3) Uani d 1 . . H H29A 0.344730 0.355154 0.258231 0.068 Uiso calc 1 . . C C30 0.3252(10) 0.4567(9) 0.3412(9) 0.048(3) Uani d 1 . . C C31 0.3895(10) 0.5117(11) 0.3704(11) 0.072(4) Uani d 1 . . H H31A 0.352262 0.557765 0.408470 0.087 Uiso calc 1 . . C C32 0.5120(10) 0.4975(9) 0.3422(9) 0.052(3) Uani d 1 . . H H32A 0.554468 0.532259 0.366131 0.062 Uiso calc 1 . . C C33 0.1870(12) 0.4610(11) 0.3796(12) 0.068(3) Uani d 1 . . C C34 0.1407(13) 0.5749(12) 0.3487(17) 0.138(8) Uani d 1 . . H H34A 0.206577 0.633003 0.307392 0.208 Uiso calc 1 . . H H34B 0.096937 0.589140 0.296225 0.208 Uiso calc 1 . . H H34C 0.088070 0.578119 0.422102 0.208 Uiso calc 1 . . O O1 0.1274(9) 0.3734(8) 0.4305(11) 0.110(4) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0362(4) 0.0478(4) 0.0510(4) 0.0082(3) -0.0109(3) -0.0264(3) I2 0.0500(5) 0.0536(5) 0.0541(5) 0.0027(4) -0.0155(4) -0.0290(4) Cu1 0.0610(10) 0.0557(9) 0.0550(8) 0.0216(7) -0.0237(7) -0.0224(7) Cu2 0.0399(8) 0.0461(8) 0.0538(8) 0.0116(6) -0.0169(6) -0.0213(6) P1 0.0362(16) 0.0418(15) 0.0413(15) 0.0142(12) -0.0112(12) -0.0197(12) P2 0.0348(16) 0.0448(15) 0.0425(15) 0.0088(12) -0.0120(12) -0.0238(12) N1 0.044(6) 0.054(6) 0.060(6) 0.016(5) -0.018(5) -0.030(5) C1 0.038(6) 0.042(6) 0.033(5) 0.006(5) -0.013(4) -0.021(4) C2 0.037(7) 0.054(7) 0.066(7) 0.010(6) -0.010(6) -0.017(6) C3 0.040(8) 0.080(9) 0.063(8) -0.006(7) -0.007(6) -0.022(6) C4 0.039(8) 0.089(10) 0.109(10) 0.029(7) -0.037(7) -0.064(8) C5 0.098(13) 0.052(8) 0.160(14) 0.023(8) -0.091(12) -0.030(9) C6 0.058(9) 0.067(9) 0.106(11) 0.006(7) -0.046(8) -0.004(8) C7 0.036(6) 0.046(6) 0.056(7) 0.019(5) -0.020(5) -0.030(5) C8 0.082(10) 0.060(8) 0.050(7) 0.014(7) -0.020(6) -0.032(6) C9 0.081(11) 0.102(11) 0.084(10) 0.022(9) -0.013(8) -0.068(9) C10 0.089(12) 0.078(10) 0.118(13) 0.028(9) -0.060(10) -0.071(10) C11 0.093(12) 0.058(8) 0.085(10) -0.003(8) -0.034(9) -0.031(7) C12 0.067(9) 0.060(8) 0.076(8) 0.010(7) -0.026(7) -0.034(7) C13 0.046(7) 0.046(6) 0.052(6) 0.020(5) -0.016(5) -0.016(5) C14 0.029(6) 0.047(6) 0.051(6) 0.009(5) -0.014(5) -0.024(5) C15 0.056(8) 0.050(6) 0.050(6) 0.001(6) -0.015(5) -0.029(5) C16 0.027(6) 0.042(6) 0.047(6) 0.000(5) -0.011(5) -0.021(5) C17 0.087(10) 0.044(7) 0.081(9) 0.004(7) -0.045(8) -0.021(6) C18 0.107(13) 0.049(8) 0.105(11) 0.006(8) -0.058(10) -0.021(7) C19 0.095(12) 0.051(8) 0.085(9) -0.002(7) -0.028(8) -0.035(7) C20 0.111(12) 0.056(8) 0.080(9) 0.013(8) -0.059(9) -0.035(7) C21 0.082(10) 0.040(6) 0.066(8) 0.002(6) -0.041(7) -0.017(6) C22 0.039(6) 0.039(5) 0.043(6) 0.013(5) -0.009(5) -0.030(5) C23 0.057(8) 0.074(8) 0.045(7) 0.019(6) -0.024(6) -0.025(6) C24 0.067(9) 0.077(9) 0.057(8) 0.015(7) -0.025(7) -0.035(6) C25 0.058(9) 0.082(9) 0.057(8) 0.002(7) -0.006(6) -0.039(6) C26 0.033(7) 0.075(8) 0.061(7) -0.005(6) 0.002(6) -0.042(6) C27 0.031(6) 0.067(7) 0.047(6) 0.003(5) -0.004(5) -0.027(5) C28 0.048(8) 0.051(7) 0.060(7) 0.011(6) -0.007(6) -0.023(6) C29 0.047(8) 0.054(7) 0.088(8) 0.005(6) -0.019(6) -0.051(6) C30 0.042(7) 0.042(6) 0.067(7) 0.015(5) -0.021(6) -0.032(5) C31 0.038(8) 0.099(10) 0.117(10) 0.021(7) -0.025(7) -0.084(9) C32 0.047(7) 0.062(7) 0.067(7) 0.009(6) -0.022(6) -0.046(6) C33 0.044(8) 0.061(8) 0.117(10) 0.027(7) -0.029(7) -0.059(8) C34 0.052(10) 0.080(11) 0.25(2) 0.025(9) -0.051(12) -0.060(12) O1 0.053(6) 0.067(6) 0.213(12) -0.009(5) -0.039(7) -0.071(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cu2 I1 Cu1 . 2_765 66.59(6) ? Cu2 I1 Cu1 . . 117.54(5) ? Cu1 I1 Cu1 2_765 . 84.66(6) ? Cu1 I2 Cu2 2_765 . 69.51(6) ? P1 Cu1 I2 . 2_765 117.05(10) yes P1 Cu1 I1 . 2_765 114.46(10) yes I2 Cu1 I1 2_765 2_765 111.04(6) yes P1 Cu1 I1 . . 107.26(10) yes I2 Cu1 I1 2_765 . 109.28(6) yes I1 Cu1 I1 2_765 . 95.34(6) yes P1 Cu1 Cu2 . 2_765 131.81(10) ? I2 Cu1 Cu2 2_765 2_765 56.56(5) ? I1 Cu1 Cu2 2_765 2_765 55.30(5) ? I1 Cu1 Cu2 . 2_765 120.02(6) ? N1 Cu2 P2 . . 118.3(3) yes N1 Cu2 I2 . . 104.2(3) yes P2 Cu2 I2 . . 104.59(9) yes N1 Cu2 I1 . . 104.0(3) yes P2 Cu2 I1 . . 114.27(9) yes I2 Cu2 I1 . . 111.23(6) yes N1 Cu2 Cu1 . 2_765 107.2(2) ? P2 Cu2 Cu1 . 2_765 133.85(9) ? I2 Cu2 Cu1 . 2_765 53.93(5) ? I1 Cu2 Cu1 . 2_765 58.12(5) ? C13 P1 C7 . . 101.4(5) ? C13 P1 C1 . . 105.2(5) ? C7 P1 C1 . . 102.4(4) ? C13 P1 Cu1 . . 112.4(3) ? C7 P1 Cu1 . . 118.1(3) ? C1 P1 Cu1 . . 115.6(3) ? C16 P2 C15 . . 106.5(5) ? C16 P2 C22 . . 99.8(4) ? C15 P2 C22 . . 104.5(5) ? C16 P2 Cu2 . . 118.7(3) ? C15 P2 Cu2 . . 111.6(3) ? C22 P2 Cu2 . . 114.2(3) ? C32 N1 C28 . . 115.3(10) ? C32 N1 Cu2 . . 122.1(8) ? C28 N1 Cu2 . . 121.4(8) ? C6 C1 C2 . . 119.1(10) ? C6 C1 P1 . . 120.9(8) ? C2 C1 P1 . . 119.9(7) ? C3 C2 C1 . . 120.0(10) ? C3 C2 H2A . . 120.0 ? C1 C2 H2A . . 120.0 ? C4 C3 C2 . . 122.3(11) ? C4 C3 H3A . . 118.8 ? C2 C3 H3A . . 118.8 ? C3 C4 C5 . . 118.0(11) ? C3 C4 H4A . . 121.0 ? C5 C4 H4A . . 121.0 ? C4 C5 C6 . . 121.3(11) ? C4 C5 H5A . . 119.4 ? C6 C5 H5A . . 119.4 ? C1 C6 C5 . . 119.3(12) ? C1 C6 H6A . . 120.4 ? C5 C6 H6A . . 120.4 ? C12 C7 C8 . . 117.0(11) ? C12 C7 P1 . . 124.6(9) ? C8 C7 P1 . . 118.4(9) ? C7 C8 C9 . . 121.6(11) ? C7 C8 H8A . . 119.2 ? C9 C8 H8A . . 119.2 ? C8 C9 C10 . . 121.0(12) ? C8 C9 H9A . . 119.5 ? C10 C9 H9A . . 119.5 ? C11 C10 C9 . . 118.3(13) ? C11 C10 H10A . . 120.9 ? C9 C10 H10A . . 120.9 ? C10 C11 C12 . . 120.1(13) ? C10 C11 H11A . . 119.9 ? C12 C11 H11A . . 119.9 ? C7 C12 C11 . . 122.0(12) ? C7 C12 H12A . . 119.0 ? C11 C12 H12A . . 119.0 ? C14 C13 P1 . . 115.4(7) ? C14 C13 H13A . . 108.4 ? P1 C13 H13A . . 108.4 ? C14 C13 H13B . . 108.4 ? P1 C13 H13B . . 108.4 ? H13A C13 H13B . . 107.5 ? C13 C14 C15 . . 112.9(8) ? C13 C14 H14A . . 109.0 ? C15 C14 H14A . . 109.0 ? C13 C14 H14B . . 109.0 ? C15 C14 H14B . . 109.0 ? H14A C14 H14B . . 107.8 ? C14 C15 P2 . . 113.6(7) ? C14 C15 H15A . . 108.8 ? P2 C15 H15A . . 108.8 ? C14 C15 H15B . . 108.8 ? P2 C15 H15B . . 108.8 ? H15A C15 H15B . . 107.7 ? C17 C16 C21 . . 117.3(10) ? C17 C16 P2 . . 124.8(8) ? C21 C16 P2 . . 117.9(7) ? C18 C17 C16 . . 121.5(12) ? C18 C17 H17A . . 119.2 ? C16 C17 H17A . . 119.2 ? C17 C18 C19 . . 120.1(12) ? C17 C18 H18A . . 120.0 ? C19 C18 H18A . . 120.0 ? C20 C19 C18 . . 120.4(12) ? C20 C19 H19A . . 119.8 ? C18 C19 H19A . . 119.8 ? C19 C20 C21 . . 118.2(12) ? C19 C20 H20A . . 120.9 ? C21 C20 H20A . . 120.9 ? C20 C21 C16 . . 122.4(10) ? C20 C21 H21A . . 118.8 ? C16 C21 H21A . . 118.8 ? C23 C22 C27 . . 117.8(9) ? C23 C22 P2 . . 124.2(8) ? C27 C22 P2 . . 118.0(7) ? C22 C23 C24 . . 120.7(11) ? C22 C23 H23A . . 119.6 ? C24 C23 H23A . . 119.6 ? C25 C24 C23 . . 119.3(11) ? C25 C24 H24A . . 120.3 ? C23 C24 H24A . . 120.3 ? C24 C25 C26 . . 121.8(11) ? C24 C25 H25A . . 119.1 ? C26 C25 H25A . . 119.1 ? C27 C26 C25 . . 117.6(11) ? C27 C26 H26A . . 121.2 ? C25 C26 H26A . . 121.2 ? C26 C27 C22 . . 122.7(10) ? C26 C27 H27A . . 118.6 ? C22 C27 H27A . . 118.6 ? N1 C28 C29 . . 126.0(11) ? N1 C28 H28A . . 117.0 ? C29 C28 H28A . . 117.0 ? C28 C29 C30 . . 117.3(11) ? C28 C29 H29A . . 121.3 ? C30 C29 H29A . . 121.3 ? C31 C30 C29 . . 118.6(11) ? C31 C30 C33 . . 120.9(10) ? C29 C30 C33 . . 120.4(10) ? C30 C31 C32 . . 118.5(11) ? C30 C31 H31A . . 120.7 ? C32 C31 H31A . . 120.7 ? N1 C32 C31 . . 124.1(11) ? N1 C32 H32A . . 117.9 ? C31 C32 H32A . . 117.9 ? O1 C33 C34 . . 124.8(13) ? O1 C33 C30 . . 118.6(11) ? C34 C33 C30 . . 116.6(12) ? C33 C34 H34A . . 109.5 ? C33 C34 H34B . . 109.5 ? H34A C34 H34B . . 109.5 ? C33 C34 H34C . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 Cu2 . 2.7032(17) yes I1 Cu1 2_765 2.7920(18) yes I1 Cu1 . 2.7962(18) yes I2 Cu1 2_765 2.6039(17) yes I2 Cu2 . 2.6881(17) yes Cu1 P1 . 2.246(3) yes Cu1 Cu2 2_765 3.017(3) ? Cu2 N1 . 2.050(9) yes Cu2 P2 . 2.240(3) yes P1 C13 . 1.811(10) ? P1 C7 . 1.820(11) ? P1 C1 . 1.835(10) ? P2 C16 . 1.830(10) ? P2 C15 . 1.831(11) ? P2 C22 . 1.839(9) ? N1 C32 . 1.313(13) ? N1 C28 . 1.313(14) ? C1 C6 . 1.360(13) ? C1 C2 . 1.363(13) ? C2 C3 . 1.364(15) ? C2 H2A . 0.9300 ? C3 C4 . 1.347(15) ? C3 H3A . 0.9300 ? C4 C5 . 1.350(17) ? C4 H4A . 0.9300 ? C5 C6 . 1.399(18) ? C5 H5A . 0.9300 ? C6 H6A . 0.9300 ? C7 C12 . 1.351(15) ? C7 C8 . 1.367(14) ? C8 C9 . 1.373(16) ? C8 H8A . 0.9300 ? C9 C10 . 1.387(18) ? C9 H9A . 0.9300 ? C10 C11 . 1.329(18) ? C10 H10A . 0.9300 ? C11 C12 . 1.420(17) ? C11 H11A . 0.9300 ? C12 H12A . 0.9300 ? C13 C14 . 1.505(14) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C14 C15 . 1.523(13) ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C16 C17 . 1.368(13) ? C16 C21 . 1.379(13) ? C17 C18 . 1.353(17) ? C17 H17A . 0.9300 ? C18 C19 . 1.371(17) ? C18 H18A . 0.9300 ? C19 C20 . 1.367(15) ? C19 H19A . 0.9300 ? C20 C21 . 1.370(15) ? C20 H20A . 0.9300 ? C21 H21A . 0.9300 ? C22 C23 . 1.382(13) ? C22 C27 . 1.387(13) ? C23 C24 . 1.385(15) ? C23 H23A . 0.9300 ? C24 C25 . 1.366(16) ? C24 H24A . 0.9300 ? C25 C26 . 1.380(15) ? C25 H25A . 0.9300 ? C26 C27 . 1.370(14) ? C26 H26A . 0.9300 ? C27 H27A . 0.9300 ? C28 C29 . 1.369(15) ? C28 H28A . 0.9300 ? C29 C30 . 1.375(14) ? C29 H29A . 0.9300 ? C30 C31 . 1.360(15) ? C30 C33 . 1.546(16) ? C31 C32 . 1.388(15) ? C31 H31A . 0.9300 ? C32 H32A . 0.9300 ? C33 O1 . 1.172(14) ? C33 C34 . 1.447(17) ? C34 H34A . 0.9600 ? C34 H34B . 0.9600 ? C34 H34C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C2 H2A I1 2_765 0.93 3.25 4.056(11) 145.5 yes C14 H14B O1 1_655 0.97 2.65 3.265(15) 121.4 yes C15 H15A O1 1_655 0.97 2.45 3.125(14) 126.4 yes C32 H32A I2 . 0.93 3.18 3.815(11) 127.1 yes C34 H34B I2 1_455 0.96 3.26 4.109(16) 148.2 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C13 P1 C1 C6 . . . . 57.6(11) ? C7 P1 C1 C6 . . . . -48.0(11) ? Cu1 P1 C1 C6 . . . . -177.8(9) ? C13 P1 C1 C2 . . . . -123.1(9) ? C7 P1 C1 C2 . . . . 131.2(9) ? Cu1 P1 C1 C2 . . . . 1.4(10) ? C6 C1 C2 C3 . . . . 2.1(18) ? P1 C1 C2 C3 . . . . -177.1(10) ? C1 C2 C3 C4 . . . . -1(2) ? C2 C3 C4 C5 . . . . 1(2) ? C3 C4 C5 C6 . . . . -1(2) ? C2 C1 C6 C5 . . . . -3(2) ? P1 C1 C6 C5 . . . . 176.6(12) ? C4 C5 C6 C1 . . . . 2(3) ? C13 P1 C7 C12 . . . . 1.0(10) ? C1 P1 C7 C12 . . . . 109.5(10) ? Cu1 P1 C7 C12 . . . . -122.2(9) ? C13 P1 C7 C8 . . . . -178.1(9) ? C1 P1 C7 C8 . . . . -69.6(9) ? Cu1 P1 C7 C8 . . . . 58.6(9) ? C12 C7 C8 C9 . . . . -1.0(18) ? P1 C7 C8 C9 . . . . 178.2(10) ? C7 C8 C9 C10 . . . . 2(2) ? C8 C9 C10 C11 . . . . -3(2) ? C9 C10 C11 C12 . . . . 3(2) ? C8 C7 C12 C11 . . . . 0.5(17) ? P1 C7 C12 C11 . . . . -178.6(10) ? C10 C11 C12 C7 . . . . -2(2) ? C7 P1 C13 C14 . . . . 177.7(7) ? C1 P1 C13 C14 . . . . 71.3(8) ? Cu1 P1 C13 C14 . . . . -55.2(8) ? P1 C13 C14 C15 . . . . 173.5(7) ? C13 C14 C15 P2 . . . . -66.3(10) ? C16 P2 C15 C14 . . . . 81.4(8) ? C22 P2 C15 C14 . . . . -173.5(7) ? Cu2 P2 C15 C14 . . . . -49.7(8) ? C15 P2 C16 C17 . . . . 33.5(11) ? C22 P2 C16 C17 . . . . -74.9(10) ? Cu2 P2 C16 C17 . . . . 160.4(9) ? C15 P2 C16 C21 . . . . -145.3(9) ? C22 P2 C16 C21 . . . . 106.3(9) ? Cu2 P2 C16 C21 . . . . -18.4(10) ? C21 C16 C17 C18 . . . . -1.0(18) ? P2 C16 C17 C18 . . . . -179.9(11) ? C16 C17 C18 C19 . . . . 2(2) ? C17 C18 C19 C20 . . . . -3(2) ? C18 C19 C20 C21 . . . . 2(2) ? C19 C20 C21 C16 . . . . -2(2) ? C17 C16 C21 C20 . . . . 0.9(18) ? P2 C16 C21 C20 . . . . 179.9(10) ? C16 P2 C22 C23 . . . . 97.0(9) ? C15 P2 C22 C23 . . . . -13.0(10) ? Cu2 P2 C22 C23 . . . . -135.2(8) ? C16 P2 C22 C27 . . . . -80.7(9) ? C15 P2 C22 C27 . . . . 169.2(8) ? Cu2 P2 C22 C27 . . . . 47.0(9) ? C27 C22 C23 C24 . . . . -0.2(16) ? P2 C22 C23 C24 . . . . -177.9(9) ? C22 C23 C24 C25 . . . . 1.2(18) ? C23 C24 C25 C26 . . . . -2(2) ? C24 C25 C26 C27 . . . . 2.2(19) ? C25 C26 C27 C22 . . . . -1.2(18) ? C23 C22 C27 C26 . . . . 0.2(17) ? P2 C22 C27 C26 . . . . 178.0(9) ? C32 N1 C28 C29 . . . . 2.6(16) ? Cu2 N1 C28 C29 . . . . 170.4(8) ? N1 C28 C29 C30 . . . . -1.8(17) ? C28 C29 C30 C31 . . . . 1.5(16) ? C28 C29 C30 C33 . . . . -175.7(10) ? C29 C30 C31 C32 . . . . -2.1(17) ? C33 C30 C31 C32 . . . . 175.0(10) ? C28 N1 C32 C31 . . . . -3.3(16) ? Cu2 N1 C32 C31 . . . . -171.0(9) ? C30 C31 C32 N1 . . . . 3.2(18) ? C31 C30 C33 O1 . . . . -128.9(15) ? C29 C30 C33 O1 . . . . 48.2(18) ? C31 C30 C33 C34 . . . . 51.3(18) ? C29 C30 C33 C34 . . . . -131.6(14) ?