#------------------------------------------------------------------------------ #$Date: 2019-04-27 03:49:00 +0300 (Sat, 27 Apr 2019) $ #$Revision: 214813 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/83/7058335.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_7058335 loop_ _publ_author_name 'Nahaei, Asma' 'Nabavizadeh, S. Masoud' 'Niroomand Hosseini, Fatemeh' 'Hoseini, S. Jafar' 'Abu-Omar, Mahdi M.' _publ_section_title ; Arene C-H bond activation and methane formation by a methylplatinum(II) complex: Experimental and theoretical elucidation of mechanism ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C9NJ01968E _journal_year 2019 _chemical_formula_sum 'C32 H34 N2 O2 Pt2 S2' _chemical_formula_weight 932.91 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-08-29 deposited with the CCDC. 2019-04-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.327(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.974(3) _cell_length_b 9.8965(16) _cell_length_c 17.603(3) _cell_measurement_reflns_used 591 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.6 _cell_measurement_theta_min 2.35 _cell_volume 2925.8(9) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13258 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.220 _diffrn_reflns_theta_min 1.802 _exptl_absorpt_coefficient_mu 9.728 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.118 _exptl_crystal_description block _exptl_crystal_F_000 1776 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.987 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.198 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 6352 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0306 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0455 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5175 _reflns_number_total 6352 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9nj01968e2.cif _cod_data_source_block s08222017_0m _cod_original_cell_volume 2925.9(9) _cod_database_code 7058335 _shelx_shelxl_version_number 2014/7 _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 0.323 _shelx_estimated_absorpt_t_max 0.443 _shelx_res_file ; s08222017_0m.res created by SHELXL-2014/7 TITL s08222017_01_a.res in P2(1)/n CELL 0.71073 16.9743 9.8965 17.6029 90.000 98.327 90.000 ZERR 4.000 0.0028 0.0016 0.0033 0.000 0.008 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O S Pt UNIT 128 136 8 8 8 8 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 conf eadp C15 C31 eadp C16 C32 size 0.15 0.1 0.1 TEMP -173.110 WGHT 0.000000 FVAR 0.12547 MOLE 1 C1 1 0.337422 0.110073 0.387500 11.00000 0.02546 0.01482 = 0.01194 -0.00325 -0.00241 -0.00091 AFIX 137 H1A 2 0.390074 0.069811 0.386895 11.00000 -1.50000 H1B 2 0.306119 0.102613 0.336333 11.00000 -1.50000 H1C 2 0.310022 0.062312 0.424843 11.00000 -1.50000 AFIX 0 C2 1 0.324409 0.283751 0.222380 11.00000 0.02791 0.02676 = 0.01201 -0.00485 0.00466 -0.00506 AFIX 137 H2A 2 0.299890 0.322287 0.173319 11.00000 -1.50000 H2B 2 0.309412 0.188392 0.224808 11.00000 -1.50000 H2C 2 0.382460 0.291167 0.226711 11.00000 -1.50000 AFIX 0 C3 1 0.188465 0.323025 0.285773 11.00000 0.01318 0.02820 = 0.02484 -0.00363 0.00187 0.00459 AFIX 137 H3A 2 0.161365 0.366176 0.324910 11.00000 -1.50000 H3B 2 0.185038 0.224610 0.290527 11.00000 -1.50000 H3C 2 0.162941 0.350796 0.234642 11.00000 -1.50000 AFIX 0 C4 1 0.365930 0.628963 0.429448 11.00000 0.01294 0.01472 = 0.01211 0.00142 0.00244 0.00103 AFIX 43 H4 2 0.340552 0.632055 0.377704 11.00000 -1.20000 AFIX 0 C5 1 0.390150 0.749247 0.466529 11.00000 0.01723 0.00465 = 0.02048 0.00143 0.00296 0.00314 AFIX 43 H5 2 0.381235 0.832778 0.440089 11.00000 -1.20000 AFIX 0 C6 1 0.426791 0.747377 0.541028 11.00000 0.01861 0.00759 = 0.02227 -0.00351 0.00515 -0.00001 AFIX 43 H6 2 0.443063 0.829381 0.566668 11.00000 -1.20000 AFIX 0 C7 1 0.440083 0.623689 0.579109 11.00000 0.01112 0.01269 = 0.01534 -0.00148 0.00489 -0.00200 C8 1 0.479718 0.609601 0.656265 11.00000 0.01377 0.01686 = 0.02309 -0.00595 0.00232 -0.00562 AFIX 43 H8 2 0.497076 0.688053 0.685012 11.00000 -1.20000 AFIX 0 C9 1 0.492930 0.485150 0.689121 11.00000 0.01523 0.02276 = 0.00741 -0.00250 -0.00288 0.00361 AFIX 43 H9 2 0.519245 0.478381 0.740417 11.00000 -1.20000 AFIX 0 C10 1 0.467673 0.364272 0.647360 11.00000 0.00661 0.02062 = 0.01594 -0.00450 0.00139 -0.00126 C11 1 0.479695 0.233621 0.679881 11.00000 0.01629 0.02389 = 0.00982 0.00190 0.00077 0.00317 AFIX 43 H11 2 0.505694 0.222978 0.731066 11.00000 -1.20000 AFIX 0 C12 1 0.453377 0.122247 0.636670 11.00000 0.02652 0.01516 = 0.02115 0.00571 0.00284 0.00443 AFIX 43 H12 2 0.461587 0.034548 0.658316 11.00000 -1.20000 AFIX 0 C13 1 0.414628 0.136393 0.561171 11.00000 0.01890 0.00728 = 0.01447 -0.00749 0.00110 -0.00070 AFIX 43 H13 2 0.397176 0.057352 0.533032 11.00000 -1.20000 AFIX 0 C14 1 0.400777 0.261045 0.525971 11.00000 0.00715 0.01164 = 0.01543 -0.00516 -0.00137 0.00155 C15 1 0.427772 0.375068 0.572162 11.00000 0.01147 0.01207 = 0.00627 -0.00100 0.00410 -0.00140 C16 1 0.414047 0.506015 0.537737 11.00000 0.00738 0.01695 = 0.00940 -0.00372 0.00347 0.00209 C17 1 0.407286 0.977244 0.828518 11.00000 0.02156 0.00692 = 0.02300 -0.00180 -0.00175 -0.00259 AFIX 137 H17A 2 0.403625 1.025675 0.876441 11.00000 -1.50000 H17B 2 0.356570 0.984779 0.794233 11.00000 -1.50000 H17C 2 0.449895 1.016738 0.803587 11.00000 -1.50000 AFIX 0 C18 1 0.287988 0.773833 0.697696 11.00000 0.02236 0.02885 = 0.01448 0.00035 -0.00570 0.00668 AFIX 137 H18A 2 0.326705 0.733405 0.668201 11.00000 -1.50000 H18B 2 0.291954 0.872527 0.695722 11.00000 -1.50000 H18C 2 0.234136 0.745771 0.675668 11.00000 -1.50000 AFIX 0 C19 1 0.234888 0.813092 0.834637 11.00000 0.01449 0.02615 = 0.02322 0.00167 0.00632 0.00170 AFIX 137 H19A 2 0.181712 0.785061 0.810572 11.00000 -1.50000 H19B 2 0.242038 0.909699 0.825485 11.00000 -1.50000 H19C 2 0.240560 0.796194 0.890017 11.00000 -1.50000 AFIX 0 C20 1 0.442310 0.459331 0.867979 11.00000 0.01437 0.01718 = 0.01336 0.00080 0.00290 -0.00575 AFIX 43 H20 2 0.390376 0.456259 0.839413 11.00000 -1.20000 AFIX 0 C21 1 0.479846 0.338310 0.892191 11.00000 0.02138 0.01498 = 0.01111 0.00267 0.00159 -0.00718 AFIX 43 H21 2 0.453188 0.254704 0.880962 11.00000 -1.20000 AFIX 0 C22 1 0.555028 0.340374 0.932083 11.00000 0.02135 0.00732 = 0.02132 0.00333 0.00909 0.00696 AFIX 43 H22 2 0.581103 0.258064 0.948064 11.00000 -1.20000 AFIX 0 C23 1 0.594033 0.464942 0.949589 11.00000 0.01233 0.01317 = 0.01568 0.00206 0.00449 -0.00061 C24 1 0.671532 0.479326 0.992807 11.00000 0.01511 0.01679 = 0.02399 0.00624 0.00182 0.00410 AFIX 43 H24 2 0.700900 0.401044 1.010711 11.00000 -1.20000 AFIX 0 C25 1 0.703594 0.602992 1.008542 11.00000 0.00999 0.02665 = 0.01332 0.00178 0.00000 0.00473 AFIX 43 H25 2 0.755352 0.609384 1.037240 11.00000 -1.20000 AFIX 0 C26 1 0.661974 0.725277 0.983289 11.00000 0.00505 0.01772 = 0.01397 0.00048 0.00426 -0.00331 C27 1 0.693737 0.854863 0.998323 11.00000 0.01064 0.02524 = 0.01723 -0.00013 -0.00008 -0.00572 AFIX 43 H27 2 0.744944 0.865543 1.027598 11.00000 -1.20000 AFIX 0 C28 1 0.651030 0.965503 0.970870 11.00000 0.02255 0.01360 = 0.02075 -0.00366 0.00557 -0.00670 AFIX 43 H28 2 0.673173 1.052998 0.980783 11.00000 -1.20000 AFIX 0 C29 1 0.574280 0.952353 0.927857 11.00000 0.02161 0.01785 = 0.01708 0.00403 -0.00160 0.00234 AFIX 43 H29 2 0.545501 1.031617 0.910693 11.00000 -1.20000 AFIX 0 C30 1 0.540082 0.827999 0.910148 11.00000 0.01121 0.01253 = 0.00946 -0.00090 -0.00076 0.00031 C31 1 0.585494 0.715079 0.939442 11.00000 0.01147 0.01207 = 0.00627 -0.00100 0.00410 -0.00140 C32 1 0.552476 0.583990 0.923281 11.00000 0.00738 0.01695 = 0.00940 -0.00372 0.00347 0.00209 N1 3 0.377136 0.510451 0.463991 11.00000 0.01126 0.01146 = 0.00854 0.00044 0.00184 -0.00027 N2 3 0.476969 0.580105 0.883611 11.00000 0.00947 0.01465 = 0.01218 0.00002 0.00042 0.00040 O1 4 0.291897 0.517964 0.276188 11.00000 0.04079 0.01214 = 0.01911 0.00329 -0.00646 -0.00096 O2 4 0.282518 0.575166 0.794063 11.00000 0.01877 0.01032 = 0.03589 -0.00263 -0.00513 -0.00492 PT1 6 0.350234 0.312260 0.418050 11.00000 0.01268 0.00850 = 0.00966 -0.00010 0.00084 -0.00018 PT2 6 0.432015 0.776647 0.852249 11.00000 0.01126 0.00927 = 0.01145 -0.00005 0.00062 -0.00030 S1 5 0.290842 0.373237 0.298996 11.00000 0.01853 0.01494 = 0.01056 -0.00020 -0.00118 -0.00068 S2 5 0.308174 0.719245 0.794386 11.00000 0.01179 0.01374 = 0.01708 -0.00038 -0.00064 0.00037 HKLF 4 REM s08222017_01_a.res in P2(1)/n REM R1 = 0.0306 for 5175 Fo > 4sig(Fo) and 0.0461 for all 6352 data REM 355 parameters refined using 0 restraints END WGHT 0.0161 2.0410 REM Highest difference peak 0.987, deepest hole -0.894, 1-sigma level 0.198 Q1 1 0.5180 0.2326 0.6582 11.00000 0.05 0.99 Q2 1 0.3875 0.7977 0.8034 11.00000 0.05 0.89 Q3 1 0.3818 0.3033 0.3821 11.00000 0.05 0.87 Q4 1 0.3014 0.2862 0.3787 11.00000 0.05 0.86 Q5 1 0.4051 0.7704 0.9017 11.00000 0.05 0.85 Q6 1 0.2827 0.3098 0.4060 11.00000 0.05 0.84 Q7 1 0.3001 0.2980 0.4404 11.00000 0.05 0.83 Q8 1 0.4991 0.8047 0.8558 11.00000 0.05 0.82 Q9 1 0.3221 0.0777 0.2080 11.00000 0.05 0.82 Q10 1 0.2160 1.0684 0.8695 11.00000 0.05 0.80 Q11 1 0.3558 0.4590 0.4433 11.00000 0.05 0.77 Q12 1 0.6792 0.7961 0.9723 11.00000 0.05 0.77 Q13 1 0.2969 0.3810 0.4169 11.00000 0.05 0.75 Q14 1 0.4769 0.7672 0.8945 11.00000 0.05 0.75 Q15 1 0.4978 0.1806 0.7692 11.00000 0.05 0.72 Q16 1 0.4078 0.9033 0.8306 11.00000 0.05 0.71 Q17 1 0.4575 0.2021 0.6483 11.00000 0.05 0.71 Q18 1 0.4735 0.5804 0.5237 11.00000 0.05 0.70 Q19 1 0.2808 0.3348 0.2098 11.00000 0.05 0.70 Q20 1 0.6587 0.6295 1.0871 11.00000 0.05 0.69 ; _shelx_res_checksum 57670 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 C1 C 0.3374(3) 0.1101(5) 0.3875(3) 0.0179(13) Uani 1 1 d . . H1A H 0.3901 0.0698 0.3869 0.027 Uiso 1 1 calc R U H1B H 0.3061 0.1026 0.3363 0.027 Uiso 1 1 calc R U H1C H 0.3100 0.0623 0.4248 0.027 Uiso 1 1 calc R U C2 C 0.3244(3) 0.2838(5) 0.2224(3) 0.0221(13) Uani 1 1 d . . H2A H 0.2999 0.3223 0.1733 0.033 Uiso 1 1 calc R U H2B H 0.3094 0.1884 0.2248 0.033 Uiso 1 1 calc R U H2C H 0.3825 0.2912 0.2267 0.033 Uiso 1 1 calc R U C3 C 0.1885(3) 0.3230(5) 0.2858(3) 0.0222(14) Uani 1 1 d . . H3A H 0.1614 0.3662 0.3249 0.033 Uiso 1 1 calc R U H3B H 0.1850 0.2246 0.2905 0.033 Uiso 1 1 calc R U H3C H 0.1629 0.3508 0.2346 0.033 Uiso 1 1 calc R U C4 C 0.3659(3) 0.6290(5) 0.4294(3) 0.0132(12) Uani 1 1 d . . H4 H 0.3406 0.6321 0.3777 0.016 Uiso 1 1 calc R U C5 C 0.3901(3) 0.7492(5) 0.4665(3) 0.0141(12) Uani 1 1 d . . H5 H 0.3812 0.8328 0.4401 0.017 Uiso 1 1 calc R U C6 C 0.4268(3) 0.7474(5) 0.5410(3) 0.0159(12) Uani 1 1 d . . H6 H 0.4431 0.8294 0.5667 0.019 Uiso 1 1 calc R U C7 C 0.4401(3) 0.6237(5) 0.5791(3) 0.0128(12) Uani 1 1 d . . C8 C 0.4797(3) 0.6096(5) 0.6563(3) 0.0179(13) Uani 1 1 d . . H8 H 0.4971 0.6881 0.6850 0.022 Uiso 1 1 calc R U C9 C 0.4929(3) 0.4852(5) 0.6891(3) 0.0156(12) Uani 1 1 d . . H9 H 0.5192 0.4784 0.7404 0.019 Uiso 1 1 calc R U C10 C 0.4677(3) 0.3643(5) 0.6474(3) 0.0144(12) Uani 1 1 d . . C11 C 0.4797(3) 0.2336(5) 0.6799(3) 0.0168(12) Uani 1 1 d . . H11 H 0.5057 0.2230 0.7311 0.020 Uiso 1 1 calc R U C12 C 0.4534(3) 0.1222(5) 0.6367(3) 0.0210(14) Uani 1 1 d . . H12 H 0.4616 0.0345 0.6583 0.025 Uiso 1 1 calc R U C13 C 0.4146(3) 0.1364(5) 0.5612(3) 0.0137(12) Uani 1 1 d . . H13 H 0.3972 0.0574 0.5330 0.016 Uiso 1 1 calc R U C14 C 0.4008(3) 0.2610(5) 0.5260(3) 0.0117(12) Uani 1 1 d . . C15 C 0.4278(3) 0.3751(5) 0.5722(3) 0.0097(8) Uani 1 1 d . . C16 C 0.4140(3) 0.5060(5) 0.5377(3) 0.0110(8) Uani 1 1 d . . C17 C 0.4073(3) 0.9772(4) 0.8285(3) 0.0177(13) Uani 1 1 d . . H17A H 0.4036 1.0257 0.8764 0.026 Uiso 1 1 calc R U H17B H 0.3566 0.9848 0.7942 0.026 Uiso 1 1 calc R U H17C H 0.4499 1.0167 0.8036 0.026 Uiso 1 1 calc R U C18 C 0.2880(3) 0.7738(5) 0.6977(3) 0.0227(14) Uani 1 1 d . . H18A H 0.3267 0.7334 0.6682 0.034 Uiso 1 1 calc R U H18B H 0.2920 0.8725 0.6957 0.034 Uiso 1 1 calc R U H18C H 0.2341 0.7458 0.6757 0.034 Uiso 1 1 calc R U C19 C 0.2349(3) 0.8131(5) 0.8346(3) 0.0209(13) Uani 1 1 d . . H19A H 0.1817 0.7851 0.8106 0.031 Uiso 1 1 calc R U H19B H 0.2420 0.9097 0.8255 0.031 Uiso 1 1 calc R U H19C H 0.2406 0.7962 0.8900 0.031 Uiso 1 1 calc R U C20 C 0.4423(3) 0.4593(5) 0.8680(3) 0.0149(12) Uani 1 1 d . . H20 H 0.3904 0.4563 0.8394 0.018 Uiso 1 1 calc R U C21 C 0.4798(3) 0.3383(5) 0.8922(3) 0.0159(12) Uani 1 1 d . . H21 H 0.4532 0.2547 0.8810 0.019 Uiso 1 1 calc R U C22 C 0.5550(3) 0.3404(5) 0.9321(3) 0.0161(12) Uani 1 1 d . . H22 H 0.5811 0.2581 0.9481 0.019 Uiso 1 1 calc R U C23 C 0.5940(3) 0.4649(5) 0.9496(3) 0.0135(12) Uani 1 1 d . . C24 C 0.6715(3) 0.4793(5) 0.9928(3) 0.0187(13) Uani 1 1 d . . H24 H 0.7009 0.4010 1.0107 0.022 Uiso 1 1 calc R U C25 C 0.7036(3) 0.6030(5) 1.0085(3) 0.0168(13) Uani 1 1 d . . H25 H 0.7554 0.6094 1.0372 0.020 Uiso 1 1 calc R U C26 C 0.6620(3) 0.7253(5) 0.9833(3) 0.0120(11) Uani 1 1 d . . C27 C 0.6937(3) 0.8549(5) 0.9983(3) 0.0179(13) Uani 1 1 d . . H27 H 0.7449 0.8655 1.0276 0.021 Uiso 1 1 calc R U C28 C 0.6510(3) 0.9655(5) 0.9709(3) 0.0187(13) Uani 1 1 d . . H28 H 0.6732 1.0530 0.9808 0.022 Uiso 1 1 calc R U C29 C 0.5743(3) 0.9524(5) 0.9279(3) 0.0193(13) Uani 1 1 d . . H29 H 0.5455 1.0316 0.9107 0.023 Uiso 1 1 calc R U C30 C 0.5401(3) 0.8280(5) 0.9101(3) 0.0113(11) Uani 1 1 d . . C31 C 0.5855(3) 0.7151(5) 0.9394(3) 0.0097(8) Uani 1 1 d . . C32 C 0.5525(3) 0.5840(5) 0.9233(3) 0.0110(8) Uani 1 1 d . . N1 N 0.3771(2) 0.5105(4) 0.4640(2) 0.0104(9) Uani 1 1 d . . N2 N 0.4770(2) 0.5801(4) 0.8836(2) 0.0122(10) Uani 1 1 d . . O1 O 0.2919(2) 0.5180(3) 0.2762(2) 0.0251(10) Uani 1 1 d . . O2 O 0.2825(2) 0.5752(3) 0.7941(2) 0.0226(10) Uani 1 1 d . . Pt1 Pt 0.35023(2) 0.31226(2) 0.41805(2) 0.01035(5) Uani 1 1 d . . Pt2 Pt 0.43201(2) 0.77665(2) 0.85225(2) 0.01076(5) Uani 1 1 d . . S1 S 0.29084(8) 0.37324(13) 0.29900(8) 0.0150(3) Uani 1 1 d . . S2 S 0.30817(7) 0.71925(13) 0.79439(8) 0.0145(3) 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 C1 0.025(3) 0.015(3) 0.012(3) -0.003(2) -0.002(3) -0.001(2) C2 0.028(3) 0.027(3) 0.012(3) -0.005(2) 0.005(3) -0.005(3) C3 0.013(3) 0.028(3) 0.025(4) -0.004(3) 0.002(2) 0.005(2) C4 0.013(3) 0.015(3) 0.012(3) 0.001(2) 0.002(2) 0.001(2) C5 0.017(3) 0.005(3) 0.020(3) 0.001(2) 0.003(2) 0.003(2) C6 0.019(3) 0.008(3) 0.022(3) -0.004(2) 0.005(2) 0.000(2) C7 0.011(2) 0.013(3) 0.015(3) -0.001(2) 0.005(2) -0.002(2) C8 0.014(3) 0.017(3) 0.023(3) -0.006(2) 0.002(3) -0.006(2) C9 0.015(3) 0.023(3) 0.007(3) -0.003(2) -0.003(2) 0.004(2) C10 0.007(2) 0.021(3) 0.016(3) -0.004(2) 0.001(2) -0.001(2) C11 0.016(3) 0.024(3) 0.010(3) 0.002(2) 0.001(2) 0.003(2) C12 0.027(3) 0.015(3) 0.021(3) 0.006(2) 0.003(3) 0.004(3) C13 0.019(3) 0.007(3) 0.014(3) -0.007(2) 0.001(2) -0.001(2) C14 0.007(2) 0.012(3) 0.015(3) -0.005(2) -0.001(2) 0.002(2) C15 0.0115(17) 0.012(2) 0.0063(18) -0.0010(15) 0.0041(15) -0.0014(15) C16 0.0074(17) 0.017(2) 0.009(2) -0.0037(15) 0.0035(15) 0.0021(15) C17 0.022(3) 0.007(3) 0.023(3) -0.002(2) -0.002(3) -0.003(2) C18 0.022(3) 0.029(3) 0.014(3) 0.000(3) -0.006(3) 0.007(3) C19 0.014(3) 0.026(3) 0.023(3) 0.002(3) 0.006(2) 0.002(2) C20 0.014(3) 0.017(3) 0.013(3) 0.001(2) 0.003(2) -0.006(2) C21 0.021(3) 0.015(3) 0.011(3) 0.003(2) 0.002(2) -0.007(2) C22 0.021(3) 0.007(3) 0.021(3) 0.003(2) 0.009(3) 0.007(2) C23 0.012(3) 0.013(3) 0.016(3) 0.002(2) 0.004(2) -0.001(2) C24 0.015(3) 0.017(3) 0.024(3) 0.006(3) 0.002(3) 0.004(2) C25 0.010(3) 0.027(3) 0.013(3) 0.002(2) 0.000(2) 0.005(2) C26 0.005(2) 0.018(3) 0.014(3) 0.000(2) 0.004(2) -0.003(2) C27 0.011(3) 0.025(3) 0.017(3) 0.000(2) 0.000(2) -0.006(2) C28 0.023(3) 0.014(3) 0.021(3) -0.004(2) 0.006(3) -0.007(2) C29 0.022(3) 0.018(3) 0.017(3) 0.004(2) -0.002(3) 0.002(2) C30 0.011(2) 0.013(3) 0.009(3) -0.001(2) -0.001(2) 0.000(2) C31 0.0115(17) 0.012(2) 0.0063(18) -0.0010(15) 0.0041(15) -0.0014(15) C32 0.0074(17) 0.017(2) 0.009(2) -0.0037(15) 0.0035(15) 0.0021(15) N1 0.011(2) 0.011(2) 0.009(2) 0.0004(18) 0.0018(19) -0.0003(18) N2 0.009(2) 0.015(2) 0.012(2) 0.0000(19) 0.0004(19) 0.0004(18) O1 0.041(2) 0.012(2) 0.019(2) 0.0033(16) -0.006(2) -0.0010(18) O2 0.019(2) 0.010(2) 0.036(3) -0.0026(17) -0.0051(19) -0.0049(16) Pt1 0.01268(10) 0.00850(11) 0.00966(11) -0.00010(8) 0.00084(8) -0.00018(8) Pt2 0.01126(9) 0.00927(11) 0.01145(11) -0.00005(8) 0.00062(8) -0.00030(8) S1 0.0185(7) 0.0149(7) 0.0106(7) -0.0002(6) -0.0012(6) -0.0007(6) S2 0.0118(6) 0.0137(7) 0.0171(7) -0.0004(6) -0.0006(5) 0.0004(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 '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 Pt1 C1 H1A 109.5 Pt1 C1 H1B 109.5 H1A C1 H1B 109.5 Pt1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 S1 C2 H2A 109.5 S1 C2 H2B 109.5 H2A C2 H2B 109.5 S1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 S1 C3 H3A 109.5 S1 C3 H3B 109.5 H3A C3 H3B 109.5 S1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 N1 C4 C5 122.0(5) N1 C4 H4 119.0 C5 C4 H4 119.0 C6 C5 C4 120.1(4) C6 C5 H5 120.0 C4 C5 H5 120.0 C5 C6 C7 119.4(4) C5 C6 H6 120.3 C7 C6 H6 120.3 C6 C7 C16 117.3(5) C6 C7 C8 124.1(4) C16 C7 C8 118.6(4) C9 C8 C7 121.0(5) C9 C8 H8 119.5 C7 C8 H8 119.5 C8 C9 C10 121.1(5) C8 C9 H9 119.5 C10 C9 H9 119.5 C15 C10 C11 118.2(4) C15 C10 C9 119.2(5) C11 C10 C9 122.6(5) C12 C11 C10 119.4(5) C12 C11 H11 120.3 C10 C11 H11 120.3 C11 C12 C13 120.9(5) C11 C12 H12 119.5 C13 C12 H12 119.5 C14 C13 C12 122.6(4) C14 C13 H13 118.7 C12 C13 H13 118.7 C13 C14 C15 115.4(4) C13 C14 Pt1 131.4(3) C15 C14 Pt1 113.1(3) C10 C15 C14 123.3(4) C10 C15 C16 119.6(4) C14 C15 C16 117.0(4) N1 C16 C7 122.3(4) N1 C16 C15 117.2(4) C7 C16 C15 120.5(4) Pt2 C17 H17A 109.5 Pt2 C17 H17B 109.5 H17A C17 H17B 109.5 Pt2 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 S2 C18 H18A 109.5 S2 C18 H18B 109.5 H18A C18 H18B 109.5 S2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 S2 C19 H19A 109.5 S2 C19 H19B 109.5 H19A C19 H19B 109.5 S2 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 N2 C20 C21 122.3(4) N2 C20 H20 118.8 C21 C20 H20 118.8 C22 C21 C20 119.8(5) C22 C21 H21 120.1 C20 C21 H21 120.1 C21 C22 C23 120.0(5) C21 C22 H22 120.0 C23 C22 H22 120.0 C22 C23 C32 117.3(4) C22 C23 C24 124.7(5) C32 C23 C24 117.9(4) C25 C24 C23 120.8(5) C25 C24 H24 119.6 C23 C24 H24 119.6 C24 C25 C26 122.2(5) C24 C25 H25 118.9 C26 C25 H25 118.9 C27 C26 C31 117.8(4) C27 C26 C25 123.6(4) C31 C26 C25 118.6(4) C28 C27 C26 119.9(5) C28 C27 H27 120.1 C26 C27 H27 120.1 C27 C28 C29 121.1(5) C27 C28 H28 119.4 C29 C28 H28 119.4 C30 C29 C28 121.9(5) C30 C29 H29 119.0 C28 C29 H29 119.0 C29 C30 C31 115.8(4) C29 C30 Pt2 131.2(4) C31 C30 Pt2 113.0(3) C30 C31 C26 123.5(4) C30 C31 C32 118.0(4) C26 C31 C32 118.5(4) N2 C32 C23 121.9(4) N2 C32 C31 116.1(4) C23 C32 C31 121.9(4) C4 N1 C16 119.0(4) C4 N1 Pt1 129.0(3) C16 N1 Pt1 112.0(3) C20 N2 C32 118.7(4) C20 N2 Pt2 129.0(3) C32 N2 Pt2 112.3(3) C14 Pt1 C1 90.92(19) C14 Pt1 N1 80.66(17) C1 Pt1 N1 171.05(17) C14 Pt1 S1 178.23(15) C1 Pt1 S1 90.07(14) N1 Pt1 S1 98.43(11) C30 Pt2 C17 90.19(19) C30 Pt2 N2 80.50(17) C17 Pt2 N2 170.57(17) C30 Pt2 S2 176.52(16) C17 Pt2 S2 90.11(14) N2 Pt2 S2 99.28(11) O1 S1 C2 104.9(3) O1 S1 C3 106.3(2) C2 S1 C3 100.1(3) O1 S1 Pt1 118.91(15) C2 S1 Pt1 114.84(18) C3 S1 Pt1 109.8(2) O2 S2 C18 105.8(2) O2 S2 C19 106.3(2) C18 S2 C19 100.0(3) O2 S2 Pt2 119.46(14) C18 S2 Pt2 113.10(19) C19 S2 Pt2 110.23(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 Pt1 2.075(4) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 S1 1.775(6) C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C3 S1 1.790(5) C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C4 N1 1.322(6) C4 C5 1.391(6) C4 H4 0.9500 C5 C6 1.368(7) C5 H5 0.9500 C6 C7 1.398(7) C6 H6 0.9500 C7 C16 1.410(6) C7 C8 1.432(7) C8 C9 1.365(7) C8 H8 0.9500 C9 C10 1.437(7) C9 H9 0.9500 C10 C15 1.401(7) C10 C11 1.417(7) C11 C12 1.376(7) C11 H11 0.9500 C12 C13 1.402(7) C12 H12 0.9500 C13 C14 1.385(7) C13 H13 0.9500 C14 C15 1.427(6) C14 Pt1 2.032(5) C15 C16 1.435(6) C16 N1 1.358(6) C17 Pt2 2.059(4) C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 S2 1.771(5) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 S2 1.780(5) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 N2 1.343(6) C20 C21 1.394(7) C20 H20 0.9500 C21 C22 1.365(7) C21 H21 0.9500 C22 C23 1.412(7) C22 H22 0.9500 C23 C32 1.416(6) C23 C24 1.428(6) C24 C25 1.352(7) C24 H24 0.9500 C25 C26 1.439(6) C25 H25 0.9500 C26 C27 1.401(7) C26 C31 1.415(6) C27 C28 1.363(7) C27 H27 0.9500 C28 C29 1.415(7) C28 H28 0.9500 C29 C30 1.377(7) C29 H29 0.9500 C30 C31 1.412(6) C30 Pt2 2.030(4) C31 C32 1.425(6) C32 N2 1.368(6) N1 Pt1 2.145(4) N2 Pt2 2.133(4) O1 S1 1.488(3) O2 S2 1.491(3) Pt1 S1 2.2717(13) Pt2 S2 2.2713(12) 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 N1 C4 C5 C6 0.0(8) C4 C5 C6 C7 0.5(8) C5 C6 C7 C16 -0.3(8) C5 C6 C7 C8 178.3(5) C6 C7 C8 C9 -177.9(5) C16 C7 C8 C9 0.7(8) C7 C8 C9 C10 0.1(8) C8 C9 C10 C15 -1.0(8) C8 C9 C10 C11 -179.4(5) C15 C10 C11 C12 1.1(8) C9 C10 C11 C12 179.5(5) C10 C11 C12 C13 -0.3(9) C11 C12 C13 C14 0.1(9) C12 C13 C14 C15 -0.8(8) C12 C13 C14 Pt1 177.8(4) C11 C10 C15 C14 -1.9(8) C9 C10 C15 C14 179.6(5) C11 C10 C15 C16 179.5(5) C9 C10 C15 C16 1.1(8) C13 C14 C15 C10 1.7(8) Pt1 C14 C15 C10 -177.1(4) C13 C14 C15 C16 -179.7(5) Pt1 C14 C15 C16 1.5(6) C6 C7 C16 N1 -0.3(8) C8 C7 C16 N1 -179.0(5) C6 C7 C16 C15 178.1(5) C8 C7 C16 C15 -0.6(8) C10 C15 C16 N1 178.2(5) C14 C15 C16 N1 -0.5(7) C10 C15 C16 C7 -0.3(8) C14 C15 C16 C7 -178.9(5) N2 C20 C21 C22 -1.2(9) C20 C21 C22 C23 0.9(8) C21 C22 C23 C32 -0.9(8) C21 C22 C23 C24 178.1(6) C22 C23 C24 C25 -178.3(6) C32 C23 C24 C25 0.6(8) C23 C24 C25 C26 0.2(9) C24 C25 C26 C27 -179.7(6) C24 C25 C26 C31 -1.1(8) C31 C26 C27 C28 0.0(8) C25 C26 C27 C28 178.6(6) C26 C27 C28 C29 0.7(9) C27 C28 C29 C30 -1.6(9) C28 C29 C30 C31 1.7(8) C28 C29 C30 Pt2 178.6(4) C29 C30 C31 C26 -1.0(8) Pt2 C30 C31 C26 -178.5(4) C29 C30 C31 C32 179.5(5) Pt2 C30 C31 C32 2.0(6) C27 C26 C31 C30 0.2(8) C25 C26 C31 C30 -178.5(5) C27 C26 C31 C32 179.7(5) C25 C26 C31 C32 1.0(7) C22 C23 C32 N2 1.1(8) C24 C23 C32 N2 -177.9(5) C22 C23 C32 C31 178.4(5) C24 C23 C32 C31 -0.6(8) C30 C31 C32 N2 -3.3(7) C26 C31 C32 N2 177.2(5) C30 C31 C32 C23 179.3(5) C26 C31 C32 C23 -0.2(8) C5 C4 N1 C16 -0.6(8) C5 C4 N1 Pt1 -177.0(4) C7 C16 N1 C4 0.7(8) C15 C16 N1 C4 -177.7(5) C7 C16 N1 Pt1 177.7(4) C15 C16 N1 Pt1 -0.7(6) C21 C20 N2 C32 1.4(8) C21 C20 N2 Pt2 179.5(4) C23 C32 N2 C20 -1.4(8) C31 C32 N2 C20 -178.8(5) C23 C32 N2 Pt2 -179.8(4) C31 C32 N2 Pt2 2.8(6)