#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:22:10 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252745 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557988.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_1557988 loop_ _publ_author_name 'Deolka, Shubham' 'Rivada-Wheelaghan, Orestes' 'Aristiz\'abal, Sandra L.' 'Fayzullin, Robert R.' 'Pal, Shrinwantu' 'Nozaki, Kyoko' 'Khaskin, Eugene' 'Khusnutdinova, Julia R.' _publ_section_title ; Metal--metal cooperative bond activation by heterobimetallic alkyl, aryl, and acetylide PtII/CuI complexes ; _journal_issue 21 _journal_name_full 'Chemical Science' _journal_page_first 5494 _journal_paper_doi 10.1039/D0SC00646G _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C26 H39 Cu N4 O P Pt 1+, Cl2 Cu 1-' _chemical_formula_sum 'C26 H39 Cl2 Cu2 N4 O P Pt' _chemical_formula_weight 847.65 _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 _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-01-02 deposited with the CCDC. 2020-04-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.7026(16) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7739(2) _cell_length_b 8.98822(13) _cell_length_c 27.1150(4) _cell_measurement_reflns_used 31351 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 32.4080 _cell_measurement_theta_min 2.7410 _cell_volume 3059.04(8) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009) ; _computing_publication_material 'enCIFer (Allen, 2004)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual offset/far' _diffrn_measurement_method '\w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0310 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 61309 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.337 _diffrn_reflns_theta_min 2.734 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.193 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018). Numerical absorption correction based on gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics, frame scaling and detector area scaling, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.841 _exptl_crystal_description plate _exptl_crystal_F_000 1664 _exptl_crystal_recrystallization_method 'vapor diffusion of pentane into a benzene solution at r.t.' _exptl_crystal_size_max 0.073 _exptl_crystal_size_mid 0.046 _exptl_crystal_size_min 0.022 _refine_diff_density_max 2.417 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.132 _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 354 _refine_ls_number_reflns 10168 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0249 _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^)+(0.0259P)^2^+2.8658P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.0558 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8716 _reflns_number_total 10168 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc00646g3.cif _cod_data_source_block jk579 _cod_depositor_comments 'Adding full bibliography for 1557987--1557994.cif.' _cod_original_cell_volume 3059.03(9) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557988 _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_estimated_absorpt_t_min 0.661 _shelx_estimated_absorpt_t_max 0.876 _shelx_res_file ; TITL jk579 in P2(1)/c shelx.res created by SHELXL-2018/3 at 20:37:28 on 24-Sep-2019 CELL 0.71073 12.773857 8.988219 27.115019 90.0000 100.7026 90.0000 ZERR 4.00 0.000220 0.000129 0.000440 0.0000 0.0016 0.0000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL CU PT UNIT 104 156 16 4 4 8 8 4 MERG 2 OMIT 1 0 2 OMIT 0 1 1 OMIT 2 1 4 OMIT -6 1 2 DFIX 0.980 C1 H1A C1 H1B C1 H1C MORE -1 FMAP 2 PLAN 10 SIZE 0.022 0.046 0.073 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -180.15 WGHT 0.025900 2.865800 FVAR 0.18182 PT1 8 0.715268 0.542965 0.290602 11.00000 0.01046 0.01068 = 0.01182 0.00054 0.00203 0.00102 CU1 7 0.710222 0.385673 0.372730 11.00000 0.01650 0.02103 = 0.01456 0.00456 0.00211 0.00535 P1 5 0.772215 0.770588 0.276512 11.00000 0.01032 0.01182 = 0.01303 0.00051 0.00176 0.00022 O1 4 0.668477 0.877251 0.285819 11.00000 0.01252 0.01302 = 0.01868 0.00159 0.00520 0.00170 N2 3 0.655002 0.250751 0.436218 11.00000 0.01737 0.01362 = 0.01752 0.00098 0.00148 0.00093 N3 3 0.847668 0.366706 0.418921 11.00000 0.01692 0.01983 = 0.01645 0.00272 0.00349 0.00473 N11 3 0.574029 0.496921 0.382261 11.00000 0.01327 0.01505 = 0.01269 0.00021 0.00128 -0.00043 N12 3 0.609486 0.678267 0.326823 11.00000 0.01225 0.01301 = 0.01383 0.00003 0.00208 0.00113 C1 1 0.632663 0.328675 0.292436 11.00000 0.00887 0.01767 = 0.00735 0.00080 0.00136 -0.00072 H1A 2 0.657264 0.257186 0.315544 11.00000 0.03516 H1B 2 0.561673 0.349360 0.292041 11.00000 0.03162 H1C 2 0.644600 0.286454 0.262969 11.00000 0.03245 C2 1 0.818025 0.424048 0.256025 11.00000 0.02049 0.01718 = 0.02175 -0.00020 0.00809 0.00383 AFIX 137 H2A 2 0.784871 0.405683 0.220973 11.00000 -1.50000 H2B 2 0.834365 0.328843 0.273363 11.00000 -1.50000 H2C 2 0.883967 0.480765 0.257207 11.00000 -1.50000 AFIX 0 C11 1 0.544646 0.293070 0.436816 11.00000 0.01549 0.01995 = 0.01676 0.00220 0.00282 -0.00002 AFIX 23 H11A 2 0.532704 0.291015 0.471855 11.00000 -1.20000 H11B 2 0.496322 0.219056 0.417398 11.00000 -1.20000 AFIX 0 C12 1 0.517128 0.446056 0.415000 11.00000 0.01464 0.01879 = 0.01289 0.00085 -0.00009 -0.00137 C13 1 0.431314 0.525417 0.428230 11.00000 0.01723 0.02275 = 0.01523 0.00009 0.00489 -0.00210 AFIX 43 H13 2 0.391350 0.484354 0.451191 11.00000 -1.20000 AFIX 0 C14 1 0.406478 0.662727 0.407439 11.00000 0.01257 0.02291 = 0.01627 -0.00241 0.00416 0.00082 AFIX 43 H14 2 0.349459 0.718576 0.416166 11.00000 -1.20000 AFIX 0 C15 1 0.466040 0.720582 0.373030 11.00000 0.01174 0.01779 = 0.01354 -0.00098 0.00098 0.00108 C16 1 0.450621 0.864699 0.351799 11.00000 0.01213 0.01881 = 0.01783 -0.00050 0.00191 0.00490 AFIX 43 H16 2 0.393598 0.925185 0.358157 11.00000 -1.20000 AFIX 0 C17 1 0.517659 0.915744 0.322380 11.00000 0.01459 0.01363 = 0.01717 0.00065 0.00039 0.00289 AFIX 43 H17 2 0.510453 1.013606 0.308941 11.00000 -1.20000 AFIX 0 C18 1 0.598704 0.819595 0.312172 11.00000 0.01052 0.01619 = 0.01285 -0.00014 0.00089 -0.00015 C19 1 0.548016 0.631120 0.360558 11.00000 0.01129 0.01681 = 0.01183 -0.00110 0.00121 0.00030 C21 1 0.667227 0.088554 0.439194 11.00000 0.03269 0.01642 = 0.02899 -0.00104 0.00046 0.00226 AFIX 137 H21A 2 0.625901 0.043056 0.408880 11.00000 -1.50000 H21B 2 0.641335 0.051585 0.468748 11.00000 -1.50000 H21C 2 0.742614 0.062657 0.441944 11.00000 -1.50000 AFIX 0 C31 1 0.729643 0.321653 0.477244 11.00000 0.01701 0.01979 = 0.01305 0.00079 0.00149 0.00223 AFIX 23 H31A 2 0.729890 0.266115 0.508795 11.00000 -1.20000 H31B 2 0.705871 0.424609 0.482035 11.00000 -1.20000 AFIX 0 C32 1 0.840706 0.324717 0.465943 11.00000 0.01908 0.01813 = 0.01631 0.00001 0.00343 0.00289 C33 1 0.930220 0.290913 0.501683 11.00000 0.02217 0.03449 = 0.01619 0.00280 0.00181 0.00545 AFIX 43 H33 2 0.923102 0.258871 0.534285 11.00000 -1.20000 AFIX 0 C34 1 1.029939 0.304556 0.489144 11.00000 0.02005 0.04353 = 0.02181 0.00468 -0.00065 0.00781 AFIX 43 H34 2 1.092271 0.282776 0.513114 11.00000 -1.20000 AFIX 0 C35 1 1.037717 0.350450 0.441118 11.00000 0.01778 0.03900 = 0.02245 0.00501 0.00524 0.00558 AFIX 43 H35 2 1.105414 0.362329 0.431875 11.00000 -1.20000 AFIX 0 C36 1 0.945350 0.378588 0.406958 11.00000 0.02001 0.02659 = 0.02176 0.00311 0.00722 0.00583 AFIX 43 H36 2 0.950741 0.407374 0.373811 11.00000 -1.20000 AFIX 0 C41 1 0.884112 0.845924 0.323625 11.00000 0.01428 0.01707 = 0.01762 -0.00040 -0.00067 -0.00212 C42 1 0.852657 0.821092 0.375123 11.00000 0.02100 0.03071 = 0.01556 -0.00227 -0.00109 -0.00236 AFIX 137 H42A 2 0.788991 0.879834 0.377205 11.00000 -1.50000 H42B 2 0.911366 0.852267 0.401729 11.00000 -1.50000 H42C 2 0.837590 0.715366 0.379222 11.00000 -1.50000 AFIX 0 C43 1 0.908919 1.010488 0.317812 11.00000 0.02530 0.02007 = 0.02936 0.00077 -0.00426 -0.00784 AFIX 137 H43A 2 0.938749 1.024637 0.287352 11.00000 -1.50000 H43B 2 0.960651 1.043717 0.347066 11.00000 -1.50000 H43C 2 0.843279 1.068724 0.315287 11.00000 -1.50000 AFIX 0 C44 1 0.983002 0.750066 0.321444 11.00000 0.01346 0.02794 = 0.02481 0.00159 -0.00105 0.00022 AFIX 137 H44A 2 0.966007 0.645059 0.325682 11.00000 -1.50000 H44B 2 1.041401 0.780192 0.348365 11.00000 -1.50000 H44C 2 1.004559 0.763917 0.288898 11.00000 -1.50000 AFIX 0 C51 1 0.773462 0.833119 0.211300 11.00000 0.01644 0.01554 = 0.01285 0.00204 0.00290 -0.00065 C52 1 0.757715 1.001330 0.203384 11.00000 0.03713 0.01657 = 0.02066 0.00459 0.00212 -0.00045 AFIX 137 H52A 2 0.691714 1.031989 0.214027 11.00000 -1.50000 H52B 2 0.753241 1.024952 0.167769 11.00000 -1.50000 H52C 2 0.818138 1.054437 0.223301 11.00000 -1.50000 AFIX 0 C53 1 0.680192 0.752890 0.178243 11.00000 0.01572 0.02561 = 0.01517 -0.00035 -0.00086 -0.00203 AFIX 137 H53A 2 0.690684 0.645092 0.181573 11.00000 -1.50000 H53B 2 0.676697 0.781900 0.143136 11.00000 -1.50000 H53C 2 0.613522 0.780347 0.188872 11.00000 -1.50000 AFIX 0 C54 1 0.877058 0.784333 0.195264 11.00000 0.01703 0.03637 = 0.02017 0.00165 0.00763 0.00097 AFIX 137 H54A 2 0.937437 0.835824 0.215836 11.00000 -1.50000 H54B 2 0.874008 0.809334 0.159846 11.00000 -1.50000 H54C 2 0.886007 0.676630 0.199851 11.00000 -1.50000 AFIX 0 CU2 7 0.738281 -0.120261 0.543511 11.00000 0.01849 0.01842 = 0.02271 0.00222 0.00273 0.00035 CL1 6 0.795735 0.043631 0.597101 11.00000 0.02281 0.02526 = 0.02246 -0.00128 0.00105 0.00276 CL2 6 0.682202 -0.278933 0.487481 11.00000 0.02243 0.01785 = 0.03029 -0.00050 0.00257 -0.00286 HKLF 4 REM jk579 in P2(1)/c REM wR2 = 0.0558, GooF = S = 1.042, Restrained GooF = 1.043 for all data REM R1 = 0.0249 for 8716 Fo > 4sig(Fo) and 0.0336 for all 10168 data REM 354 parameters refined using 3 restraints END WGHT 0.0259 2.8656 REM Highest difference peak 2.417, deepest hole -0.726, 1-sigma level 0.132 Q1 1 0.7044 0.5415 0.3168 11.00000 0.05 2.42 Q2 1 0.7365 0.5481 0.2644 11.00000 0.05 1.82 Q3 1 0.6891 0.5470 0.2596 11.00000 0.05 1.24 Q4 1 0.7291 0.3800 0.3447 11.00000 0.05 0.78 Q5 1 0.7086 1.0105 0.2918 11.00000 0.05 0.77 Q6 1 0.6600 0.3615 0.2817 11.00000 0.05 0.76 Q7 1 0.6810 0.4090 0.3975 11.00000 0.05 0.73 Q8 1 0.7163 -0.1553 0.5731 11.00000 0.05 0.73 Q9 1 0.7223 0.4614 0.2916 11.00000 0.05 0.66 Q10 1 0.6345 0.2762 0.2918 11.00000 0.05 0.66 ; _shelx_res_checksum 37060 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 Pt1 Pt 0.71527(2) 0.54296(2) 0.29060(2) 0.01099(3) Uani 1 1 d . . . . . Cu1 Cu 0.71022(2) 0.38567(3) 0.37273(2) 0.01746(6) Uani 1 1 d . . . . . P1 P 0.77221(5) 0.77059(6) 0.27651(2) 0.01178(10) Uani 1 1 d . . . . . O1 O 0.66848(13) 0.87725(18) 0.28582(6) 0.0144(3) Uani 1 1 d . . . . . N2 N 0.65500(17) 0.2508(2) 0.43622(8) 0.0164(4) Uani 1 1 d . . . . . N3 N 0.84767(17) 0.3667(2) 0.41892(8) 0.0177(4) Uani 1 1 d . . . . . N11 N 0.57403(16) 0.4969(2) 0.38226(7) 0.0138(4) Uani 1 1 d . . . . . N12 N 0.60949(15) 0.6783(2) 0.32682(7) 0.0131(4) Uani 1 1 d . . . . . C1 C 0.63266(17) 0.3287(3) 0.29244(8) 0.0113(4) Uani 1 1 d D . . . . H1A H 0.657(3) 0.257(3) 0.3155(11) 0.035(9) Uiso 1 1 d D . . . . H1B H 0.5617(16) 0.349(4) 0.2920(13) 0.032(9) Uiso 1 1 d D . . . . H1C H 0.645(3) 0.286(4) 0.2630(9) 0.032(9) Uiso 1 1 d D . . . . C2 C 0.8180(2) 0.4240(3) 0.25602(10) 0.0193(5) Uani 1 1 d . . . . . H2A H 0.784871 0.405683 0.220973 0.029 Uiso 1 1 calc R U . . . H2B H 0.834365 0.328843 0.273363 0.029 Uiso 1 1 calc R U . . . H2C H 0.883967 0.480765 0.257207 0.029 Uiso 1 1 calc R U . . . C11 C 0.54465(19) 0.2931(3) 0.43682(9) 0.0174(4) Uani 1 1 d . . . . . H11A H 0.532704 0.291015 0.471855 0.021 Uiso 1 1 calc R U . . . H11B H 0.496322 0.219056 0.417398 0.021 Uiso 1 1 calc R U . . . C12 C 0.51713(19) 0.4461(3) 0.41500(9) 0.0158(4) Uani 1 1 d . . . . . C13 C 0.4313(2) 0.5254(3) 0.42823(9) 0.0182(5) Uani 1 1 d . . . . . H13 H 0.391350 0.484354 0.451191 0.022 Uiso 1 1 calc R U . . . C14 C 0.40648(19) 0.6627(3) 0.40744(9) 0.0171(4) Uani 1 1 d . . . . . H14 H 0.349459 0.718576 0.416166 0.020 Uiso 1 1 calc R U . . . C15 C 0.46604(18) 0.7206(3) 0.37303(8) 0.0145(4) Uani 1 1 d . . . . . C16 C 0.45062(19) 0.8647(3) 0.35180(9) 0.0164(4) Uani 1 1 d . . . . . H16 H 0.393598 0.925185 0.358157 0.020 Uiso 1 1 calc R U . . . C17 C 0.51766(19) 0.9157(3) 0.32238(9) 0.0155(4) Uani 1 1 d . . . . . H17 H 0.510453 1.013606 0.308941 0.019 Uiso 1 1 calc R U . . . C18 C 0.59870(18) 0.8196(3) 0.31217(8) 0.0134(4) Uani 1 1 d . . . . . C19 C 0.54802(18) 0.6311(3) 0.36056(8) 0.0134(4) Uani 1 1 d . . . . . C21 C 0.6672(2) 0.0886(3) 0.43919(11) 0.0267(6) Uani 1 1 d . . . . . H21A H 0.625901 0.043056 0.408880 0.040 Uiso 1 1 calc R U . . . H21B H 0.641335 0.051585 0.468748 0.040 Uiso 1 1 calc R U . . . H21C H 0.742614 0.062657 0.441944 0.040 Uiso 1 1 calc R U . . . C31 C 0.72964(19) 0.3217(3) 0.47724(9) 0.0168(4) Uani 1 1 d . . . . . H31A H 0.729890 0.266115 0.508795 0.020 Uiso 1 1 calc R U . . . H31B H 0.705871 0.424609 0.482035 0.020 Uiso 1 1 calc R U . . . C32 C 0.8407(2) 0.3247(3) 0.46594(9) 0.0178(5) Uani 1 1 d . . . . . C33 C 0.9302(2) 0.2909(3) 0.50168(10) 0.0245(5) Uani 1 1 d . . . . . H33 H 0.923102 0.258871 0.534285 0.029 Uiso 1 1 calc R U . . . C34 C 1.0299(2) 0.3046(4) 0.48914(10) 0.0290(6) Uani 1 1 d . . . . . H34 H 1.092271 0.282776 0.513114 0.035 Uiso 1 1 calc R U . . . C35 C 1.0377(2) 0.3504(3) 0.44112(10) 0.0262(6) Uani 1 1 d . . . . . H35 H 1.105414 0.362329 0.431875 0.031 Uiso 1 1 calc R U . . . C36 C 0.9454(2) 0.3786(3) 0.40696(10) 0.0224(5) Uani 1 1 d . . . . . H36 H 0.950741 0.407374 0.373811 0.027 Uiso 1 1 calc R U . . . C41 C 0.88411(19) 0.8459(3) 0.32363(9) 0.0168(4) Uani 1 1 d . . . . . C42 C 0.8527(2) 0.8211(3) 0.37512(9) 0.0230(5) Uani 1 1 d . . . . . H42A H 0.788991 0.879834 0.377205 0.034 Uiso 1 1 calc R U . . . H42B H 0.911366 0.852267 0.401729 0.034 Uiso 1 1 calc R U . . . H42C H 0.837590 0.715366 0.379222 0.034 Uiso 1 1 calc R U . . . C43 C 0.9089(2) 1.0105(3) 0.31781(11) 0.0261(6) Uani 1 1 d . . . . . H43A H 0.938749 1.024637 0.287352 0.039 Uiso 1 1 calc R U . . . H43B H 0.960651 1.043717 0.347066 0.039 Uiso 1 1 calc R U . . . H43C H 0.843279 1.068724 0.315287 0.039 Uiso 1 1 calc R U . . . C44 C 0.9830(2) 0.7501(3) 0.32144(10) 0.0227(5) Uani 1 1 d . . . . . H44A H 0.966007 0.645059 0.325682 0.034 Uiso 1 1 calc R U . . . H44B H 1.041401 0.780192 0.348365 0.034 Uiso 1 1 calc R U . . . H44C H 1.004559 0.763917 0.288898 0.034 Uiso 1 1 calc R U . . . C51 C 0.77346(18) 0.8331(3) 0.21130(8) 0.0149(4) Uani 1 1 d . . . . . C52 C 0.7577(3) 1.0013(3) 0.20338(10) 0.0252(6) Uani 1 1 d . . . . . H52A H 0.691714 1.031989 0.214027 0.038 Uiso 1 1 calc R U . . . H52B H 0.753241 1.024952 0.167769 0.038 Uiso 1 1 calc R U . . . H52C H 0.818138 1.054437 0.223301 0.038 Uiso 1 1 calc R U . . . C53 C 0.6802(2) 0.7529(3) 0.17824(9) 0.0193(5) Uani 1 1 d . . . . . H53A H 0.690684 0.645092 0.181573 0.029 Uiso 1 1 calc R U . . . H53B H 0.676697 0.781900 0.143136 0.029 Uiso 1 1 calc R U . . . H53C H 0.613522 0.780347 0.188872 0.029 Uiso 1 1 calc R U . . . C54 C 0.8771(2) 0.7843(3) 0.19526(10) 0.0240(5) Uani 1 1 d . . . . . H54A H 0.937437 0.835824 0.215836 0.036 Uiso 1 1 calc R U . . . H54B H 0.874008 0.809334 0.159846 0.036 Uiso 1 1 calc R U . . . H54C H 0.886007 0.676630 0.199851 0.036 Uiso 1 1 calc R U . . . Cu2 Cu 0.73828(2) -0.12026(3) 0.54351(2) 0.02001(7) Uani 1 1 d . . . . . Cl1 Cl 0.79574(5) 0.04363(7) 0.59710(2) 0.02391(12) Uani 1 1 d . . . . . Cl2 Cl 0.68220(5) -0.27893(7) 0.48748(2) 0.02382(12) 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 Pt1 0.01046(4) 0.01068(4) 0.01182(4) 0.00054(3) 0.00203(3) 0.00102(3) Cu1 0.01650(14) 0.02103(15) 0.01456(13) 0.00456(11) 0.00211(10) 0.00535(11) P1 0.0103(3) 0.0118(2) 0.0130(3) 0.00051(19) 0.00176(19) 0.0002(2) O1 0.0125(8) 0.0130(7) 0.0187(8) 0.0016(6) 0.0052(6) 0.0017(6) N2 0.0174(10) 0.0136(9) 0.0175(9) 0.0010(7) 0.0015(7) 0.0009(7) N3 0.0169(10) 0.0198(10) 0.0165(9) 0.0027(8) 0.0035(7) 0.0047(8) N11 0.0133(9) 0.0151(8) 0.0127(9) 0.0002(7) 0.0013(7) -0.0004(7) N12 0.0122(9) 0.0130(9) 0.0138(9) 0.0000(7) 0.0021(7) 0.0011(7) C1 0.0089(10) 0.0177(10) 0.0073(9) 0.0008(7) 0.0014(7) -0.0007(8) C2 0.0205(12) 0.0172(11) 0.0218(12) -0.0002(9) 0.0081(9) 0.0038(9) C11 0.0155(11) 0.0199(11) 0.0168(11) 0.0022(9) 0.0028(8) 0.0000(9) C12 0.0146(11) 0.0188(11) 0.0129(10) 0.0008(8) -0.0001(8) -0.0014(9) C13 0.0172(12) 0.0227(12) 0.0152(11) 0.0001(9) 0.0049(8) -0.0021(9) C14 0.0126(11) 0.0229(12) 0.0163(11) -0.0024(9) 0.0042(8) 0.0008(9) C15 0.0117(10) 0.0178(11) 0.0135(10) -0.0010(8) 0.0010(8) 0.0011(8) C16 0.0121(11) 0.0188(11) 0.0178(11) -0.0005(9) 0.0019(8) 0.0049(9) C17 0.0146(11) 0.0136(10) 0.0172(11) 0.0007(8) 0.0004(8) 0.0029(8) C18 0.0105(10) 0.0162(10) 0.0128(10) -0.0001(8) 0.0009(8) -0.0001(8) C19 0.0113(10) 0.0168(10) 0.0118(9) -0.0011(8) 0.0012(8) 0.0003(8) C21 0.0327(15) 0.0164(11) 0.0290(14) -0.0010(10) 0.0005(11) 0.0023(11) C31 0.0170(11) 0.0198(11) 0.0130(10) 0.0008(8) 0.0015(8) 0.0022(9) C32 0.0191(12) 0.0181(11) 0.0163(11) 0.0000(9) 0.0034(9) 0.0029(9) C33 0.0222(13) 0.0345(15) 0.0162(11) 0.0028(10) 0.0018(9) 0.0055(11) C34 0.0201(13) 0.0435(17) 0.0218(13) 0.0047(12) -0.0007(10) 0.0078(12) C35 0.0178(13) 0.0390(16) 0.0225(13) 0.0050(11) 0.0052(10) 0.0056(11) C36 0.0200(12) 0.0266(13) 0.0218(12) 0.0031(10) 0.0072(10) 0.0058(10) C41 0.0143(11) 0.0171(11) 0.0176(11) -0.0004(8) -0.0007(8) -0.0021(8) C42 0.0210(13) 0.0307(14) 0.0156(11) -0.0023(10) -0.0011(9) -0.0024(10) C43 0.0253(14) 0.0201(12) 0.0294(14) 0.0008(10) -0.0043(11) -0.0078(10) C44 0.0135(12) 0.0279(13) 0.0248(13) 0.0016(10) -0.0010(9) 0.0002(10) C51 0.0164(11) 0.0155(10) 0.0129(10) 0.0020(8) 0.0029(8) -0.0006(8) C52 0.0371(16) 0.0166(11) 0.0207(13) 0.0046(9) 0.0021(11) -0.0005(11) C53 0.0157(12) 0.0256(12) 0.0152(11) -0.0003(9) -0.0009(8) -0.0020(9) C54 0.0170(12) 0.0364(15) 0.0202(12) 0.0016(11) 0.0076(9) 0.0010(11) Cu2 0.01849(15) 0.01842(14) 0.02271(15) 0.00222(11) 0.00273(12) 0.00035(11) Cl1 0.0228(3) 0.0253(3) 0.0225(3) -0.0013(2) 0.0010(2) 0.0028(2) Cl2 0.0224(3) 0.0178(3) 0.0303(3) -0.0005(2) 0.0026(2) -0.0029(2) 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' 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' Pt Pt -1.7033 8.3905 '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 C2 Pt1 N12 177.54(9) . . ? C2 Pt1 C1 84.52(9) . . ? N12 Pt1 C1 97.93(8) . . ? C2 Pt1 P1 98.23(7) . . ? N12 Pt1 P1 79.32(5) . . ? C1 Pt1 P1 168.67(6) . . ? C2 Pt1 Cu1 102.94(7) . . ? N12 Pt1 Cu1 78.77(5) . . ? C1 Pt1 Cu1 55.06(6) . . ? P1 Pt1 Cu1 133.949(17) . . ? N3 Cu1 N11 129.50(8) . . ? N3 Cu1 C1 140.21(8) . . ? N11 Cu1 C1 90.09(8) . . ? N3 Cu1 N2 80.82(8) . . ? N11 Cu1 N2 77.34(8) . . ? C1 Cu1 N2 116.98(8) . . ? N3 Cu1 Pt1 115.07(6) . . ? N11 Cu1 Pt1 89.96(6) . . ? C1 Cu1 Pt1 52.43(6) . . ? N2 Cu1 Pt1 163.96(5) . . ? N3 Cu1 H1A 126.3(8) . . ? N11 Cu1 H1A 102.1(9) . . ? C1 Cu1 H1A 23.3(5) . . ? N2 Cu1 H1A 99.9(8) . . ? Pt1 Cu1 H1A 72.9(7) . . ? O1 P1 C51 96.65(10) . . ? O1 P1 C41 102.39(10) . . ? C51 P1 C41 113.73(11) . . ? O1 P1 Pt1 101.83(6) . . ? C51 P1 Pt1 120.11(8) . . ? C41 P1 Pt1 116.78(8) . . ? C18 O1 P1 118.38(14) . . ? C11 N2 C21 110.5(2) . . ? C11 N2 C31 111.71(19) . . ? C21 N2 C31 110.0(2) . . ? C11 N2 Cu1 107.38(14) . . ? C21 N2 Cu1 121.09(17) . . ? C31 N2 Cu1 95.23(14) . . ? C32 N3 C36 118.4(2) . . ? C32 N3 Cu1 114.76(17) . . ? C36 N3 Cu1 126.58(17) . . ? C12 N11 C19 118.4(2) . . ? C12 N11 Cu1 119.70(16) . . ? C19 N11 Cu1 121.39(15) . . ? C18 N12 C19 116.84(19) . . ? C18 N12 Pt1 115.86(15) . . ? C19 N12 Pt1 127.16(15) . . ? Pt1 C1 Cu1 72.51(7) . . ? Pt1 C1 H1A 122(2) . . ? Cu1 C1 H1A 58(2) . . ? Pt1 C1 H1B 107(2) . . ? Cu1 C1 H1B 103(2) . . ? H1A C1 H1B 111(3) . . ? Pt1 C1 H1C 101(2) . . ? Cu1 C1 H1C 144(2) . . ? H1A C1 H1C 102(3) . . ? H1B C1 H1C 113(3) . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C11 C12 112.7(2) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N11 C12 C13 123.0(2) . . ? N11 C12 C11 117.3(2) . . ? C13 C12 C11 119.7(2) . . ? C14 C13 C12 118.9(2) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.5(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C19 117.7(2) . . ? C14 C15 C16 123.7(2) . . ? C19 C15 C16 118.5(2) . . ? C17 C16 C15 119.6(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 118.3(2) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? N12 C18 O1 119.0(2) . . ? N12 C18 C17 124.3(2) . . ? O1 C18 C17 116.7(2) . . ? N11 C19 N12 116.0(2) . . ? N11 C19 C15 122.4(2) . . ? N12 C19 C15 121.6(2) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C31 C32 110.93(19) . . ? N2 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.0 . . ? N3 C32 C33 122.1(2) . . ? N3 C32 C31 115.3(2) . . ? C33 C32 C31 122.6(2) . . ? C34 C33 C32 119.1(2) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 119.1(2) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 118.9(3) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? N3 C36 C35 122.5(2) . . ? N3 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C43 C41 C44 110.5(2) . . ? C43 C41 C42 109.2(2) . . ? C44 C41 C42 107.9(2) . . ? C43 C41 P1 115.45(17) . . ? C44 C41 P1 107.55(17) . . ? C42 C41 P1 105.88(17) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C54 C51 C53 108.6(2) . . ? C54 C51 C52 109.9(2) . . ? C53 C51 C52 108.3(2) . . ? C54 C51 P1 110.12(17) . . ? C53 C51 P1 105.74(16) . . ? C52 C51 P1 114.01(17) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl1 Cu2 Cl2 177.68(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 Pt1 C2 2.050(2) . ? Pt1 N12 2.1823(19) . ? Pt1 C1 2.201(2) . ? Pt1 P1 2.2280(6) . ? Pt1 Cu1 2.6486(3) . ? Cu1 N3 1.966(2) . ? Cu1 N11 2.064(2) . ? Cu1 C1 2.277(2) . ? Cu1 N2 2.320(2) . ? Cu1 H1A 1.95(4) . ? P1 O1 1.6920(17) . ? P1 C51 1.858(2) . ? P1 C41 1.859(2) . ? O1 C18 1.345(3) . ? N2 C11 1.463(3) . ? N2 C21 1.467(3) . ? N2 C31 1.469(3) . ? N3 C32 1.348(3) . ? N3 C36 1.351(3) . ? N11 C12 1.329(3) . ? N11 C19 1.356(3) . ? N12 C18 1.330(3) . ? N12 C19 1.378(3) . ? C1 H1A 0.912(18) . ? C1 H1B 0.924(18) . ? C1 H1C 0.922(18) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C11 C12 1.512(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.409(3) . ? C13 C14 1.369(3) . ? C13 H13 0.9500 . ? C14 C15 1.408(3) . ? C14 H14 0.9500 . ? C15 C19 1.410(3) . ? C15 C16 1.416(3) . ? C16 C17 1.354(3) . ? C16 H16 0.9500 . ? C17 C18 1.415(3) . ? C17 H17 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C32 1.506(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.388(4) . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 C35 1.387(4) . ? C34 H34 0.9500 . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C43 1.527(4) . ? C41 C44 1.539(4) . ? C41 C42 1.539(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C51 C54 1.532(3) . ? C51 C53 1.532(3) . ? C51 C52 1.535(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Cu2 Cl1 2.1033(7) . ? Cu2 Cl2 2.1097(7) . ? 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 C51 P1 O1 C18 142.19(17) . . . . ? C41 P1 O1 C18 -101.68(17) . . . . ? Pt1 P1 O1 C18 19.47(17) . . . . ? C21 N2 C11 C12 -158.6(2) . . . . ? C31 N2 C11 C12 78.5(2) . . . . ? Cu1 N2 C11 C12 -24.6(2) . . . . ? C19 N11 C12 C13 -0.2(3) . . . . ? Cu1 N11 C12 C13 171.75(18) . . . . ? C19 N11 C12 C11 177.3(2) . . . . ? Cu1 N11 C12 C11 -10.8(3) . . . . ? N2 C11 C12 N11 25.0(3) . . . . ? N2 C11 C12 C13 -157.4(2) . . . . ? N11 C12 C13 C14 -1.5(4) . . . . ? C11 C12 C13 C14 -178.9(2) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C19 1.5(3) . . . . ? C13 C14 C15 C16 -176.2(2) . . . . ? C14 C15 C16 C17 174.3(2) . . . . ? C19 C15 C16 C17 -3.4(3) . . . . ? C15 C16 C17 C18 2.6(3) . . . . ? C19 N12 C18 O1 169.47(19) . . . . ? Pt1 N12 C18 O1 -14.5(3) . . . . ? C19 N12 C18 C17 -10.6(3) . . . . ? Pt1 N12 C18 C17 165.42(18) . . . . ? P1 O1 C18 N12 -4.7(3) . . . . ? P1 O1 C18 C17 175.42(16) . . . . ? C16 C17 C18 N12 4.6(4) . . . . ? C16 C17 C18 O1 -175.4(2) . . . . ? C12 N11 C19 N12 -179.9(2) . . . . ? Cu1 N11 C19 N12 8.4(3) . . . . ? C12 N11 C19 C15 2.7(3) . . . . ? Cu1 N11 C19 C15 -169.11(17) . . . . ? C18 N12 C19 N11 -168.0(2) . . . . ? Pt1 N12 C19 N11 16.5(3) . . . . ? C18 N12 C19 C15 9.5(3) . . . . ? Pt1 N12 C19 C15 -165.97(16) . . . . ? C14 C15 C19 N11 -3.4(3) . . . . ? C16 C15 C19 N11 174.5(2) . . . . ? C14 C15 C19 N12 179.3(2) . . . . ? C16 C15 C19 N12 -2.9(3) . . . . ? C11 N2 C31 C32 -159.20(19) . . . . ? C21 N2 C31 C32 77.7(3) . . . . ? Cu1 N2 C31 C32 -48.14(19) . . . . ? C36 N3 C32 C33 -1.3(4) . . . . ? Cu1 N3 C32 C33 173.0(2) . . . . ? C36 N3 C32 C31 177.0(2) . . . . ? Cu1 N3 C32 C31 -8.7(3) . . . . ? N2 C31 C32 N3 44.7(3) . . . . ? N2 C31 C32 C33 -137.0(2) . . . . ? N3 C32 C33 C34 1.8(4) . . . . ? C31 C32 C33 C34 -176.3(3) . . . . ? C32 C33 C34 C35 -0.5(5) . . . . ? C33 C34 C35 C36 -1.2(5) . . . . ? C32 N3 C36 C35 -0.5(4) . . . . ? Cu1 N3 C36 C35 -174.1(2) . . . . ? C34 C35 C36 N3 1.7(4) . . . . ? O1 P1 C41 C43 -59.9(2) . . . . ? C51 P1 C41 C43 43.2(2) . . . . ? Pt1 P1 C41 C43 -170.14(17) . . . . ? O1 P1 C41 C44 176.20(16) . . . . ? C51 P1 C41 C44 -80.72(19) . . . . ? Pt1 P1 C41 C44 65.96(18) . . . . ? O1 P1 C41 C42 61.00(18) . . . . ? C51 P1 C41 C42 164.07(16) . . . . ? Pt1 P1 C41 C42 -49.25(18) . . . . ? O1 P1 C51 C54 166.40(17) . . . . ? C41 P1 C51 C54 59.7(2) . . . . ? Pt1 P1 C51 C54 -85.76(18) . . . . ? O1 P1 C51 C53 -76.51(17) . . . . ? C41 P1 C51 C53 176.79(16) . . . . ? Pt1 P1 C51 C53 31.33(19) . . . . ? O1 P1 C51 C52 42.38(19) . . . . ? C41 P1 C51 C52 -64.3(2) . . . . ? Pt1 P1 C51 C52 150.21(16) . . . . ?