#------------------------------------------------------------------------------ #$Date: 2023-01-28 04:14:05 +0200 (Sat, 28 Jan 2023) $ #$Revision: 280647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/62/7246209.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_7246209 loop_ _publ_author_name 'Gusev, Alexey' 'Kiskin, Mikhail' 'Braga, Elena' 'Zamnius, Ekaterina' 'Kryukova, Mariya' 'Karaush-Karmazin, Nataliya' 'Baryshnikov, Glib' 'Minaev, Boris' 'Linert, Wolfgang' _publ_section_title ; Structure and emission properties of dinuclear copper(i) complexes with pyridyltriazole ; _journal_issue 6 _journal_name_full 'RSC Advances' _journal_page_first 3899 _journal_page_last 3909 _journal_paper_doi 10.1039/D2RA06986E _journal_volume 13 _journal_year 2023 _chemical_formula_sum 'C62 H50 Cl6 Cu2 I2 N10 P2' _chemical_formula_weight 1590.64 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-10-28 deposited with the CCDC. 2023-01-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.454(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 27.091(4) _cell_length_b 8.3928(14) _cell_length_c 28.914(5) _cell_measurement_reflns_used 3054 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.22 _cell_measurement_theta_min 2.55 _cell_volume 6366.1(18) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.1259 _diffrn_reflns_av_unetI/netI 0.1256 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 25120 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.378 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.660 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 3152 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.323 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.195 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 382 _refine_ls_number_reflns 6517 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.0878 _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^)+(0.1090P)^2^+3.5100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1960 _refine_ls_wR_factor_ref 0.2193 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4294 _reflns_number_total 6517 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2ra06986e2.cif _cod_data_source_block cup _cod_original_cell_volume 6365.9(18) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7246209 _shelx_shelxl_version_number 2018/3 _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_res_file ; TITL 1_a.res in C2/c cup.res created by SHELXL-2018/3 at 14:38:40 on 20-Oct-2020 REM Old TITL 1 in Cc REM SHELXT solution in C2/c REM R1 0.191, Rweak 0.030, Alpha 0.071, Orientation as input REM Formula found by SHELXT: C32 Cu I N4 O3 S CELL 0.71073 27.0907 8.3928 28.9136 90 104.454 90 ZERR 4 0.0042 0.0014 0.0045 0 0.005 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Cu I N P UNIT 248 200 24 8 8 40 8 L.S. 10 PLAN 20 TEMP -123 CONF BOND $H LIST 6 FMAP 2 MORE -1 acta htab OMIT 2 0 0 OMIT -2 0 2 OMIT 0 0 2 shel .8 30 REM REM REM WGHT 0.109000 3.510000 FVAR 0.09053 CU1 4 0.543827 0.957139 0.535819 11.00000 0.02831 0.02764 = 0.01923 0.00257 0.00589 -0.00261 N1 6 0.533260 0.817339 0.591483 11.00000 0.03331 0.03181 = 0.02083 0.00767 0.00669 0.00373 N2 6 0.555741 0.406443 0.729319 11.00000 0.04168 0.01535 = 0.02026 -0.00391 0.01627 0.00002 N3 6 0.573897 0.531970 0.801284 11.00000 0.04713 0.02127 = 0.01744 0.00468 0.00906 0.00754 N4 6 0.564283 0.637418 0.764565 11.00000 0.04923 0.01417 = 0.02240 0.00120 0.01222 -0.00636 H4 2 0.568609 0.745322 0.773628 11.00000 -1.20000 N5 6 0.573216 -0.043311 0.795568 11.00000 0.05899 0.02368 = 0.02344 0.00682 0.01329 0.00034 C1 1 0.538861 0.659500 0.593281 11.00000 0.03722 0.02098 = 0.02036 0.00122 0.00881 -0.00275 AFIX 43 H1 2 0.539703 0.605220 0.564656 11.00000 -1.20000 AFIX 0 C1S 1 0.716374 0.809626 0.779003 11.00000 0.06162 0.12860 = 0.07488 -0.03806 0.02141 -0.01118 AFIX 13 H1S 2 0.754085 0.795878 0.784721 11.00000 -1.20000 AFIX 0 C2 1 0.543507 0.570231 0.634195 11.00000 0.03491 0.01458 = 0.01820 0.00239 -0.00460 -0.00498 AFIX 43 H2 2 0.546224 0.457480 0.633307 11.00000 -1.20000 AFIX 0 C3 1 0.544148 0.648737 0.677032 11.00000 0.03048 0.03095 = 0.02026 0.00132 0.00689 0.00211 C4 1 0.534729 0.811573 0.674651 11.00000 0.04853 0.02606 = 0.02485 0.00248 0.02177 0.00430 AFIX 43 H4A 2 0.531517 0.867342 0.702343 11.00000 -1.20000 AFIX 0 C5 1 0.530013 0.892760 0.632280 11.00000 0.03305 0.02284 = 0.02582 0.01054 0.01741 0.00859 AFIX 43 H5 2 0.524336 1.004533 0.631565 11.00000 -1.20000 AFIX 0 C6 1 0.554217 0.563951 0.722634 11.00000 0.02484 0.01904 = 0.02728 -0.00116 0.00222 -0.00422 C7 1 0.568623 0.393939 0.778553 11.00000 0.02075 0.02293 = 0.03236 -0.00059 0.00679 -0.00200 C8 1 0.575466 0.238522 0.802580 11.00000 0.02570 0.01854 = 0.03153 -0.00393 0.01212 -0.00169 C9 1 0.567508 0.100064 0.775983 11.00000 0.05176 0.02129 = 0.03292 -0.00670 0.01765 -0.00606 AFIX 43 H9 2 0.557500 0.108119 0.742152 11.00000 -1.20000 AFIX 0 C10 1 0.586612 -0.053804 0.842960 11.00000 0.04817 0.02164 = 0.03496 0.01457 0.00721 0.00520 AFIX 43 H10 2 0.590218 -0.156853 0.856998 11.00000 -1.20000 AFIX 0 C11 1 0.595434 0.075109 0.872430 11.00000 0.04248 0.03565 = 0.01588 0.00330 0.00673 0.00656 AFIX 43 H11 2 0.605277 0.062318 0.906133 11.00000 -1.20000 AFIX 0 C12 1 0.589655 0.226399 0.851891 11.00000 0.04730 0.02568 = 0.01912 0.00442 0.01720 0.00244 AFIX 43 H12 2 0.595331 0.319207 0.871310 11.00000 -1.20000 AFIX 0 C13 1 0.675222 0.906120 0.556971 11.00000 0.02465 0.02446 = 0.03601 0.00689 0.00654 0.00119 C14 1 0.669148 0.772176 0.527544 11.00000 0.03143 0.03009 = 0.03935 0.00080 0.00956 -0.00457 AFIX 43 H14 2 0.638662 0.758108 0.503157 11.00000 -1.20000 AFIX 0 C15 1 0.707403 0.660526 0.533920 11.00000 0.04923 0.02892 = 0.04726 0.00132 0.01793 0.00701 AFIX 43 H15 2 0.703162 0.570399 0.513426 11.00000 -1.20000 AFIX 0 C16 1 0.751752 0.676548 0.569390 11.00000 0.03725 0.04632 = 0.04150 0.01428 0.01547 0.02134 AFIX 43 H16 2 0.778134 0.599567 0.572863 11.00000 -1.20000 AFIX 0 C17 1 0.757518 0.807883 0.600337 11.00000 0.02174 0.04358 = 0.04488 0.01100 0.00144 0.00399 AFIX 43 H17 2 0.787058 0.818277 0.626012 11.00000 -1.20000 AFIX 0 C18 1 0.719254 0.922606 0.592790 11.00000 0.03519 0.02764 = 0.03092 -0.00243 0.01321 0.00385 AFIX 43 H18 2 0.723580 1.014122 0.612735 11.00000 -1.20000 AFIX 0 C19 1 0.641027 1.189215 0.595402 11.00000 0.01695 0.03554 = 0.02832 -0.00015 0.00459 -0.00225 C20 1 0.635366 1.139441 0.640683 11.00000 0.03355 0.03909 = 0.02348 -0.00253 0.00696 -0.00315 AFIX 43 H20 2 0.623881 1.034127 0.644036 11.00000 -1.20000 AFIX 0 C21 1 0.645709 1.236328 0.679208 11.00000 0.03968 0.06381 = 0.02150 -0.01061 0.01107 -0.01282 AFIX 43 H21 2 0.644069 1.197110 0.709610 11.00000 -1.20000 AFIX 0 C22 1 0.659026 1.397101 0.673691 11.00000 0.06114 0.04379 = 0.04286 -0.01837 0.01174 -0.00138 AFIX 43 H22 2 0.663607 1.468669 0.699877 11.00000 -1.20000 AFIX 0 C23 1 0.665317 1.449646 0.630668 11.00000 0.05372 0.03722 = 0.04509 -0.00199 0.01813 -0.00425 AFIX 43 H23 2 0.676279 1.555422 0.627074 11.00000 -1.20000 AFIX 0 C24 1 0.655307 1.344811 0.592678 11.00000 0.04610 0.02840 = 0.02726 -0.00530 0.00989 -0.00577 AFIX 43 H24 2 0.658534 1.383113 0.562653 11.00000 -1.20000 AFIX 0 C25 1 0.635094 1.170714 0.496125 11.00000 0.02283 0.02456 = 0.03629 -0.00656 0.00786 -0.00425 C26 1 0.680142 1.163661 0.481736 11.00000 0.04426 0.03149 = 0.02494 -0.00019 0.01438 0.00448 AFIX 43 H26 2 0.706134 1.091764 0.497188 11.00000 -1.20000 AFIX 0 C27 1 0.687982 1.259773 0.445143 11.00000 0.04092 0.04611 = 0.03447 -0.00754 0.01818 -0.01327 AFIX 43 H27 2 0.719198 1.253571 0.435886 11.00000 -1.20000 AFIX 0 C28 1 0.650639 1.363932 0.422276 11.00000 0.04171 0.03484 = 0.01734 -0.00237 0.01331 -0.00142 AFIX 43 H28 2 0.655963 1.430882 0.397472 11.00000 -1.20000 AFIX 0 C29 1 0.604541 1.369973 0.436088 11.00000 0.04493 0.03818 = 0.02198 0.01294 0.00302 -0.00606 AFIX 43 H29 2 0.578430 1.440893 0.420260 11.00000 -1.20000 AFIX 0 C30 1 0.596910 1.276800 0.471372 11.00000 0.04049 0.04508 = 0.03040 0.00130 0.01580 -0.00634 AFIX 43 H30 2 0.565286 1.282100 0.479912 11.00000 -1.20000 AFIX 0 I1 5 0.513563 0.780426 0.458625 11.00000 0.03301 0.02497 = 0.01855 -0.00094 0.00694 0.00194 CL1 3 0.693727 0.650986 0.803308 11.00000 0.10999 0.27089 = 0.10176 0.11427 0.03144 0.00541 CL2 3 0.691605 0.817985 0.719267 11.00000 0.33667 0.06945 = 0.05689 0.00887 0.02567 -0.00037 CL3 3 0.705262 0.998387 0.803661 11.00000 0.07416 0.22412 = 0.14680 -0.11935 0.00053 0.03417 P1 7 0.623296 1.052741 0.545520 11.00000 0.02716 0.02542 = 0.02105 0.00008 0.00671 -0.00244 HKLF 4 REM 1_a.res in C2/c REM wR2 = 0.2193, GooF = S = 1.042, Restrained GooF = 1.042 for all data REM R1 = 0.0878 for 4294 Fo > 4sig(Fo) and 0.1311 for all 6517 data REM 382 parameters refined using 0 restraints END WGHT 0.1021 18.8384 REM Instructions for potential hydrogen bonds EQIV $2 x, y+1, z HTAB N4 N5_$2 HTAB C1 I1 EQIV $1 -x+1, -y+2, -z+1 HTAB C5 I1_$1 HTAB C14 I1 HTAB C30 I1_$1 REM Highest difference peak 1.323, deepest hole -1.672, 1-sigma level 0.195 Q1 1 0.4774 0.7915 0.4387 11.00000 0.05 1.32 Q2 1 0.7286 0.7646 0.7316 11.00000 0.05 1.19 Q3 1 0.4741 0.7221 0.4525 11.00000 0.05 1.12 Q4 1 0.7032 0.8653 0.8307 11.00000 0.05 1.08 Q5 1 0.5532 0.8346 0.4668 11.00000 0.05 0.99 Q6 1 0.5490 0.7952 0.4751 11.00000 0.05 0.98 Q7 1 0.5269 0.6618 0.4967 11.00000 0.05 0.95 Q8 1 0.6747 0.6590 0.7914 11.00000 0.05 0.91 Q9 1 0.6271 0.7694 0.5119 11.00000 0.05 0.84 Q10 1 0.4865 0.7284 0.4144 11.00000 0.05 0.81 Q11 1 0.7097 1.0272 0.7953 11.00000 0.05 0.78 Q12 1 0.5462 0.5024 0.5670 11.00000 0.05 0.77 Q13 1 0.7077 0.5445 0.7917 11.00000 0.05 0.76 Q14 1 0.5268 0.9196 0.4938 11.00000 0.05 0.76 Q15 1 0.5815 1.0214 0.5364 11.00000 0.05 0.75 Q16 1 0.5415 0.8600 0.4989 11.00000 0.05 0.75 Q17 1 0.4815 0.8732 0.4896 11.00000 0.05 0.73 Q18 1 0.5066 0.6461 0.4287 11.00000 0.05 0.72 Q19 1 0.5213 0.7835 0.5083 11.00000 0.05 0.72 Q20 1 0.5612 0.6173 0.5622 11.00000 0.05 0.71 ; _shelx_res_checksum 8478 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 Cu1 Cu 0.54383(4) 0.95714(14) 0.53582(4) 0.0251(3) Uani 1 1 d . . . . . N1 N 0.5333(3) 0.8173(10) 0.5915(3) 0.0287(19) Uani 1 1 d . . . . . N2 N 0.5557(3) 0.4064(9) 0.7293(3) 0.0242(18) Uani 1 1 d . . . . . N3 N 0.5739(3) 0.5320(9) 0.8013(3) 0.0284(19) Uani 1 1 d . . . . . N4 N 0.5643(3) 0.6374(9) 0.7646(3) 0.0280(19) Uani 1 1 d . . . . . H4 H 0.569(4) 0.745(12) 0.774(4) 0.034 Uiso 1 1 d . U . . . N5 N 0.5732(4) -0.0433(10) 0.7956(3) 0.035(2) Uani 1 1 d . . . . . C1 C 0.5389(4) 0.6595(11) 0.5933(3) 0.026(2) Uani 1 1 d . . . . . H1 H 0.539703 0.605220 0.564656 0.031 Uiso 1 1 calc R U . . . C1S C 0.7164(6) 0.810(2) 0.7790(6) 0.088(6) Uani 1 1 d . . . . . H1S H 0.754085 0.795878 0.784721 0.105 Uiso 1 1 calc R U . . . C2 C 0.5435(4) 0.5702(11) 0.6342(3) 0.025(2) Uani 1 1 d . . . . . H2 H 0.546224 0.457480 0.633307 0.029 Uiso 1 1 calc R U . . . C3 C 0.5441(4) 0.6487(12) 0.6770(3) 0.027(2) Uani 1 1 d . . . . . C4 C 0.5347(4) 0.8116(11) 0.6747(4) 0.031(2) Uani 1 1 d . . . . . H4A H 0.531517 0.867342 0.702343 0.037 Uiso 1 1 calc R U . . . C5 C 0.5300(4) 0.8928(11) 0.6323(3) 0.025(2) Uani 1 1 d . . . . . H5 H 0.524336 1.004533 0.631565 0.031 Uiso 1 1 calc R U . . . C6 C 0.5542(3) 0.5640(11) 0.7226(3) 0.024(2) Uani 1 1 d . . . . . C7 C 0.5686(3) 0.3939(11) 0.7786(3) 0.025(2) Uani 1 1 d . . . . . C8 C 0.5755(4) 0.2385(11) 0.8026(4) 0.024(2) Uani 1 1 d . . . . . C9 C 0.5675(4) 0.1001(11) 0.7760(4) 0.034(2) Uani 1 1 d . . . . . H9 H 0.557500 0.108119 0.742152 0.041 Uiso 1 1 calc R U . . . C10 C 0.5866(4) -0.0538(12) 0.8430(4) 0.035(3) Uani 1 1 d . . . . . H10 H 0.590218 -0.156853 0.856998 0.043 Uiso 1 1 calc R U . . . C11 C 0.5954(4) 0.0751(12) 0.8724(3) 0.031(2) Uani 1 1 d . . . . . H11 H 0.605277 0.062318 0.906133 0.038 Uiso 1 1 calc R U . . . C12 C 0.5897(4) 0.2264(12) 0.8519(3) 0.029(2) Uani 1 1 d . . . . . H12 H 0.595331 0.319207 0.871310 0.035 Uiso 1 1 calc R U . . . C13 C 0.6752(4) 0.9061(12) 0.5570(4) 0.029(2) Uani 1 1 d . . . . . C14 C 0.6691(4) 0.7722(12) 0.5275(4) 0.033(2) Uani 1 1 d . . . . . H14 H 0.638662 0.758108 0.503157 0.040 Uiso 1 1 calc R U . . . C15 C 0.7074(4) 0.6605(13) 0.5339(4) 0.041(3) Uani 1 1 d . . . . . H15 H 0.703162 0.570399 0.513426 0.049 Uiso 1 1 calc R U . . . C16 C 0.7518(4) 0.6765(14) 0.5694(4) 0.041(3) Uani 1 1 d . . . . . H16 H 0.778134 0.599567 0.572863 0.049 Uiso 1 1 calc R U . . . C17 C 0.7575(4) 0.8079(13) 0.6003(4) 0.038(3) Uani 1 1 d . . . . . H17 H 0.787058 0.818277 0.626012 0.046 Uiso 1 1 calc R U . . . C18 C 0.7193(4) 0.9226(12) 0.5928(4) 0.030(2) Uani 1 1 d . . . . . H18 H 0.723580 1.014122 0.612735 0.036 Uiso 1 1 calc R U . . . C19 C 0.6410(3) 1.1892(12) 0.5954(4) 0.027(2) Uani 1 1 d . . . . . C20 C 0.6354(4) 1.1394(13) 0.6407(3) 0.032(2) Uani 1 1 d . . . . . H20 H 0.623881 1.034127 0.644036 0.038 Uiso 1 1 calc R U . . . C21 C 0.6457(4) 1.2363(14) 0.6792(4) 0.041(3) Uani 1 1 d . . . . . H21 H 0.644069 1.197110 0.709610 0.049 Uiso 1 1 calc R U . . . C22 C 0.6590(5) 1.3971(15) 0.6737(4) 0.049(3) Uani 1 1 d . . . . . H22 H 0.663607 1.468669 0.699877 0.059 Uiso 1 1 calc R U . . . C23 C 0.6653(4) 1.4496(14) 0.6307(4) 0.044(3) Uani 1 1 d . . . . . H23 H 0.676279 1.555422 0.627074 0.053 Uiso 1 1 calc R U . . . C24 C 0.6553(4) 1.3448(12) 0.5927(4) 0.034(2) Uani 1 1 d . . . . . H24 H 0.658534 1.383113 0.562653 0.041 Uiso 1 1 calc R U . . . C25 C 0.6351(4) 1.1707(11) 0.4961(4) 0.028(2) Uani 1 1 d . . . . . C26 C 0.6801(4) 1.1637(12) 0.4817(4) 0.033(2) Uani 1 1 d . . . . . H26 H 0.706134 1.091764 0.497188 0.039 Uiso 1 1 calc R U . . . C27 C 0.6880(4) 1.2598(13) 0.4451(4) 0.039(3) Uani 1 1 d . . . . . H27 H 0.719198 1.253571 0.435886 0.047 Uiso 1 1 calc R U . . . C28 C 0.6506(4) 1.3639(12) 0.4223(3) 0.030(2) Uani 1 1 d . . . . . H28 H 0.655963 1.430882 0.397472 0.036 Uiso 1 1 calc R U . . . C29 C 0.6045(4) 1.3700(13) 0.4361(3) 0.036(3) Uani 1 1 d . . . . . H29 H 0.578430 1.440893 0.420260 0.043 Uiso 1 1 calc R U . . . C30 C 0.5969(4) 1.2768(13) 0.4714(4) 0.037(3) Uani 1 1 d . . . . . H30 H 0.565286 1.282100 0.479912 0.045 Uiso 1 1 calc R U . . . I1 I 0.51356(2) 0.78043(7) 0.45863(2) 0.0254(2) Uani 1 1 d . . . . . Cl1 Cl 0.6937(2) 0.6510(10) 0.8033(2) 0.160(3) Uani 1 1 d . . . . . Cl2 Cl 0.6916(3) 0.8180(6) 0.71927(18) 0.159(3) Uani 1 1 d . . . . . Cl3 Cl 0.70526(19) 0.9984(9) 0.8037(2) 0.153(3) Uani 1 1 d . . . . . P1 P 0.62330(10) 1.0527(3) 0.54552(9) 0.0244(6) Uani 1 1 d . . . . . 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 Cu1 0.0283(7) 0.0276(7) 0.0192(6) 0.0026(5) 0.0059(5) -0.0026(5) N1 0.033(5) 0.032(5) 0.021(4) 0.008(3) 0.007(4) 0.004(4) N2 0.042(5) 0.015(4) 0.020(4) -0.004(3) 0.016(3) 0.000(4) N3 0.047(5) 0.021(4) 0.017(4) 0.005(3) 0.009(4) 0.008(4) N4 0.049(6) 0.014(4) 0.022(4) 0.001(3) 0.012(4) -0.006(4) N5 0.059(6) 0.024(4) 0.023(5) 0.007(4) 0.013(4) 0.000(4) C1 0.037(6) 0.021(5) 0.020(5) 0.001(4) 0.009(4) -0.003(4) C1S 0.062(10) 0.129(16) 0.075(12) -0.038(11) 0.021(8) -0.011(10) C2 0.035(6) 0.015(4) 0.018(5) 0.002(4) -0.005(4) -0.005(4) C3 0.030(6) 0.031(5) 0.020(5) 0.001(4) 0.007(4) 0.002(4) C4 0.049(7) 0.026(6) 0.025(5) 0.002(4) 0.022(5) 0.004(5) C5 0.033(6) 0.023(5) 0.026(5) 0.011(4) 0.017(4) 0.009(4) C6 0.025(5) 0.019(5) 0.027(5) -0.001(4) 0.002(4) -0.004(4) C7 0.021(5) 0.023(5) 0.032(6) -0.001(4) 0.007(4) -0.002(4) C8 0.026(5) 0.019(5) 0.032(6) -0.004(4) 0.012(4) -0.002(4) C9 0.052(7) 0.021(5) 0.033(6) -0.007(4) 0.018(5) -0.006(5) C10 0.048(7) 0.022(5) 0.035(6) 0.015(5) 0.007(5) 0.005(5) C11 0.042(6) 0.036(6) 0.016(5) 0.003(4) 0.007(4) 0.007(5) C12 0.047(6) 0.026(5) 0.019(5) 0.004(4) 0.017(4) 0.002(5) C13 0.025(5) 0.024(5) 0.036(6) 0.007(4) 0.007(4) 0.001(4) C14 0.031(6) 0.030(5) 0.039(6) 0.001(5) 0.010(5) -0.005(5) C15 0.049(7) 0.029(6) 0.047(7) 0.001(5) 0.018(6) 0.007(5) C16 0.037(7) 0.046(7) 0.041(7) 0.014(5) 0.015(5) 0.021(5) C17 0.022(5) 0.044(7) 0.045(7) 0.011(5) 0.001(5) 0.004(5) C18 0.035(6) 0.028(5) 0.031(6) -0.002(4) 0.013(4) 0.004(5) C19 0.017(5) 0.036(6) 0.028(5) 0.000(4) 0.005(4) -0.002(4) C20 0.034(6) 0.039(6) 0.023(5) -0.003(5) 0.007(4) -0.003(5) C21 0.040(6) 0.064(8) 0.021(6) -0.011(5) 0.011(5) -0.013(6) C22 0.061(8) 0.044(7) 0.043(7) -0.018(6) 0.012(6) -0.001(6) C23 0.054(8) 0.037(7) 0.045(7) -0.002(5) 0.018(6) -0.004(6) C24 0.046(7) 0.028(5) 0.027(6) -0.005(4) 0.010(5) -0.006(5) C25 0.023(5) 0.025(5) 0.036(6) -0.007(4) 0.008(4) -0.004(4) C26 0.044(7) 0.031(6) 0.025(5) 0.000(4) 0.014(5) 0.004(5) C27 0.041(7) 0.046(7) 0.034(6) -0.008(5) 0.018(5) -0.013(5) C28 0.042(6) 0.035(6) 0.017(5) -0.002(4) 0.013(4) -0.001(5) C29 0.045(7) 0.038(6) 0.022(5) 0.013(5) 0.003(5) -0.006(5) C30 0.040(6) 0.045(6) 0.030(6) 0.001(5) 0.016(5) -0.006(5) I1 0.0330(4) 0.0250(3) 0.0185(3) -0.0009(3) 0.0069(2) 0.0019(3) Cl1 0.110(4) 0.271(9) 0.102(4) 0.114(5) 0.031(3) 0.005(5) Cl2 0.337(10) 0.069(3) 0.057(3) 0.009(2) 0.026(4) 0.000(4) Cl3 0.074(3) 0.224(7) 0.147(5) -0.119(5) 0.001(3) 0.034(4) P1 0.0272(14) 0.0254(13) 0.0210(13) 0.0001(10) 0.0067(10) -0.0024(11) 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 '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 N1 Cu1 P1 114.8(2) . . ? N1 Cu1 I1 105.4(2) . . ? P1 Cu1 I1 113.10(8) . . ? N1 Cu1 I1 102.8(2) . 5_676 ? P1 Cu1 I1 104.30(8) . 5_676 ? I1 Cu1 I1 116.34(4) . 5_676 ? N1 Cu1 Cu1 117.4(2) . 5_676 ? P1 Cu1 Cu1 127.13(9) . 5_676 ? I1 Cu1 Cu1 59.71(4) . 5_676 ? I1 Cu1 Cu1 56.63(4) 5_676 5_676 ? C1 N1 C5 117.4(8) . . ? C1 N1 Cu1 123.9(7) . . ? C5 N1 Cu1 117.5(6) . . ? C6 N2 C7 102.4(7) . . ? C7 N3 N4 101.9(8) . . ? C6 N4 N3 111.6(8) . . ? C6 N4 H4 133(6) . . ? N3 N4 H4 115(6) . . ? C9 N5 C10 118.3(9) . . ? N1 C1 C2 123.9(9) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? Cl1 C1S Cl2 111.4(10) . . ? Cl1 C1S Cl3 114.6(10) . . ? Cl2 C1S Cl3 107.8(11) . . ? Cl1 C1S H1S 107.6 . . ? Cl2 C1S H1S 107.6 . . ? Cl3 C1S H1S 107.6 . . ? C1 C2 C3 118.8(9) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 117.3(9) . . ? C2 C3 C6 121.8(9) . . ? C4 C3 C6 120.9(9) . . ? C5 C4 C3 120.3(9) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? N1 C5 C4 121.9(9) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N4 C6 N2 109.6(8) . . ? N4 C6 C3 123.2(8) . . ? N2 C6 C3 127.2(9) . . ? N3 C7 N2 114.4(8) . . ? N3 C7 C8 123.9(9) . . ? N2 C7 C8 121.6(8) . . ? C12 C8 C9 118.4(9) . . ? C12 C8 C7 121.5(9) . . ? C9 C8 C7 120.1(9) . . ? N5 C9 C8 122.8(10) . . ? N5 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N5 C10 C11 123.5(9) . . ? N5 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 118.3(9) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C8 C12 C11 118.6(9) . . ? C8 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C18 C13 C14 119.2(9) . . ? C18 C13 P1 123.3(8) . . ? C14 C13 P1 117.5(8) . . ? C15 C14 C13 119.8(10) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.4(11) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C17 119.3(10) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 118.9(10) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C13 C18 C17 121.3(10) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C24 C19 C20 115.5(9) . . ? C24 C19 P1 125.4(8) . . ? C20 C19 P1 118.7(8) . . ? C21 C20 C19 122.4(10) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 119.1(11) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 120.1(11) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 118.2(11) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C19 C24 C23 124.3(10) . . ? C19 C24 H24 117.8 . . ? C23 C24 H24 117.8 . . ? C26 C25 C30 117.5(10) . . ? C26 C25 P1 123.3(8) . . ? C30 C25 P1 119.1(8) . . ? C27 C26 C25 121.2(10) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C28 C27 C26 120.1(10) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.1(10) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 120.8(10) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 121.3(10) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.4 . . ? Cu1 I1 Cu1 63.66(4) . 5_676 ? C19 P1 C25 102.5(5) . . ? C19 P1 C13 104.0(4) . . ? C25 P1 C13 103.2(4) . . ? C19 P1 Cu1 112.4(3) . . ? C25 P1 Cu1 116.4(3) . . ? C13 P1 Cu1 116.7(3) . . ? 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 Cu1 N1 2.069(8) . ? Cu1 P1 2.249(3) . ? Cu1 I1 2.6344(13) . ? Cu1 I1 2.7239(14) 5_676 ? Cu1 Cu1 2.827(2) 5_676 ? N1 C1 1.333(12) . ? N1 C5 1.361(12) . ? N2 C6 1.335(11) . ? N2 C7 1.382(12) . ? N3 C7 1.322(12) . ? N3 N4 1.357(10) . ? N4 C6 1.326(12) . ? N4 H4 0.94(10) . ? N5 C9 1.322(13) . ? N5 C10 1.330(12) . ? C1 C2 1.379(12) . ? C1 H1 0.9500 . ? C1S Cl1 1.691(19) . ? C1S Cl2 1.691(18) . ? C1S Cl3 1.793(18) . ? C1S H1S 1.0000 . ? C2 C3 1.399(13) . ? C2 H2 0.9500 . ? C3 C4 1.389(14) . ? C3 C6 1.463(13) . ? C4 C5 1.380(13) . ? C4 H4A 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.468(13) . ? C8 C12 1.385(13) . ? C8 C9 1.380(13) . ? C9 H9 0.9500 . ? C10 C11 1.361(14) . ? C10 H10 0.9500 . ? C11 C12 1.394(13) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.378(14) . ? C13 C14 1.395(14) . ? C13 P1 1.836(10) . ? C14 C15 1.375(15) . ? C14 H14 0.9500 . ? C15 C16 1.378(16) . ? C15 H15 0.9500 . ? C16 C17 1.404(16) . ? C16 H16 0.9500 . ? C17 C18 1.392(14) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.370(14) . ? C19 C20 1.419(14) . ? C19 P1 1.810(10) . ? C20 C21 1.351(14) . ? C20 H20 0.9500 . ? C21 C22 1.416(16) . ? C21 H21 0.9500 . ? C22 C23 1.370(16) . ? C22 H22 0.9500 . ? C23 C24 1.380(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.385(13) . ? C25 C30 1.416(15) . ? C25 P1 1.830(11) . ? C26 C27 1.388(14) . ? C26 H26 0.9500 . ? C27 C28 1.375(15) . ? C27 H27 0.9500 . ? C28 C29 1.404(14) . ? C28 H28 0.9500 . ? C29 C30 1.342(14) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 C7 N3 N4 C6 -0.3(10) . . . . ? C5 N1 C1 C2 -2.6(14) . . . . ? Cu1 N1 C1 C2 164.4(7) . . . . ? N1 C1 C2 C3 -2.2(15) . . . . ? C1 C2 C3 C4 6.5(14) . . . . ? C1 C2 C3 C6 -173.6(9) . . . . ? C2 C3 C4 C5 -6.1(15) . . . . ? C6 C3 C4 C5 173.9(9) . . . . ? C1 N1 C5 C4 3.1(14) . . . . ? Cu1 N1 C5 C4 -164.9(8) . . . . ? C3 C4 C5 N1 1.4(15) . . . . ? N3 N4 C6 N2 1.1(11) . . . . ? N3 N4 C6 C3 -177.9(8) . . . . ? C7 N2 C6 N4 -1.3(10) . . . . ? C7 N2 C6 C3 177.7(9) . . . . ? C2 C3 C6 N4 167.3(9) . . . . ? C4 C3 C6 N4 -12.8(15) . . . . ? C2 C3 C6 N2 -11.5(16) . . . . ? C4 C3 C6 N2 168.4(10) . . . . ? N4 N3 C7 N2 -0.5(11) . . . . ? N4 N3 C7 C8 179.7(9) . . . . ? C6 N2 C7 N3 1.1(11) . . . . ? C6 N2 C7 C8 -179.0(9) . . . . ? N3 C7 C8 C12 -1.9(15) . . . . ? N2 C7 C8 C12 178.3(9) . . . . ? N3 C7 C8 C9 177.8(10) . . . . ? N2 C7 C8 C9 -2.0(14) . . . . ? C10 N5 C9 C8 0.8(16) . . . . ? C12 C8 C9 N5 -0.5(16) . . . . ? C7 C8 C9 N5 179.8(10) . . . . ? C9 N5 C10 C11 -0.9(17) . . . . ? N5 C10 C11 C12 0.6(17) . . . . ? C9 C8 C12 C11 0.2(15) . . . . ? C7 C8 C12 C11 179.9(9) . . . . ? C10 C11 C12 C8 -0.3(15) . . . . ? C18 C13 C14 C15 -1.4(16) . . . . ? P1 C13 C14 C15 178.5(8) . . . . ? C13 C14 C15 C16 0.9(17) . . . . ? C14 C15 C16 C17 1.4(17) . . . . ? C15 C16 C17 C18 -3.2(17) . . . . ? C14 C13 C18 C17 -0.4(16) . . . . ? P1 C13 C18 C17 179.6(8) . . . . ? C16 C17 C18 C13 2.7(16) . . . . ? C24 C19 C20 C21 -3.1(15) . . . . ? P1 C19 C20 C21 -177.2(8) . . . . ? C19 C20 C21 C22 4.9(17) . . . . ? C20 C21 C22 C23 -5.2(18) . . . . ? C21 C22 C23 C24 3.9(18) . . . . ? C20 C19 C24 C23 1.7(16) . . . . ? P1 C19 C24 C23 175.4(9) . . . . ? C22 C23 C24 C19 -2.3(18) . . . . ? C30 C25 C26 C27 1.5(15) . . . . ? P1 C25 C26 C27 -177.7(8) . . . . ? C25 C26 C27 C28 -0.3(16) . . . . ? C26 C27 C28 C29 -0.8(16) . . . . ? C27 C28 C29 C30 0.6(16) . . . . ? C28 C29 C30 C25 0.6(17) . . . . ? C26 C25 C30 C29 -1.6(16) . . . . ? P1 C25 C30 C29 177.5(9) . . . . ? C24 C19 P1 C25 4.7(10) . . . . ? C20 C19 P1 C25 178.1(8) . . . . ? C24 C19 P1 C13 111.9(9) . . . . ? C20 C19 P1 C13 -74.6(8) . . . . ? C24 C19 P1 Cu1 -121.0(8) . . . . ? C20 C19 P1 Cu1 52.5(8) . . . . ? C26 C25 P1 C19 94.9(9) . . . . ? C30 C25 P1 C19 -84.3(9) . . . . ? C26 C25 P1 C13 -13.0(10) . . . . ? C30 C25 P1 C13 167.9(8) . . . . ? C26 C25 P1 Cu1 -142.1(8) . . . . ? C30 C25 P1 Cu1 38.7(9) . . . . ? C18 C13 P1 C19 -8.2(10) . . . . ? C14 C13 P1 C19 171.9(8) . . . . ? C18 C13 P1 C25 98.5(9) . . . . ? C14 C13 P1 C25 -81.4(9) . . . . ? C18 C13 P1 Cu1 -132.6(8) . . . . ? C14 C13 P1 Cu1 47.5(9) . . . . ?