data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- compound3b.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ;Laboratoire de Chimie de Coordination UMR 7177 CNRS Universit\'e de Strasbourg Institut Le Bel - 4 rue Blaise Pascal, CS 90032, F-67081 STRASBOURG cedex France ; _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_author_phone '+33 (0)3 68 85 13 08' _publ_contact_author_fax '+33 (0)3 68 85 13 22' loop_ _publ_author_name _publ_author_address P.Braunstein ;Laboratoire de Chimie de Coordination UMR 7177 CNRS Universit\'e de Strasbourg Institut Le Bel - 4 rue Blaise Pascal, CS 90032, F-67081 STRASBOURG cedex France ; S.Zhang ;Laboratoire de Chimie de Coordination UMR 7177 CNRS Universit\'e de Strasbourg Institut Le Bel - 4 rue Blaise Pascal, CS 90032, F-67081 STRASBOURG cedex France ; R.Pattacini ;Laboratoire de Chimie de Coordination UMR 7177 CNRS Universit\'e de Strasbourg Institut Le Bel - 4 rue Blaise Pascal, CS 90032, F-67081 STRASBOURG cedex France ; data_compound3b _database_code_depnum_ccdc_archive 'CCDC 801707' #TrackingRef '- compound3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H22 N6 P2 Pd S2' _chemical_formula_sum 'C28 H22 N6 P2 Pd S2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 173(2) _chemical_formula_weight 674.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3926(4) _cell_length_b 14.0042(4) _cell_length_c 18.9125(8) _cell_angle_alpha 99.963(2) _cell_angle_beta 91.366(2) _cell_angle_gamma 109.306(2) _cell_volume 2794.08(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10042 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.10 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11343 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 26.34 _reflns_number_total 11343 _reflns_number_gt 7695 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11343 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.30173(3) 0.21834(2) -0.016024(17) 0.02925(10) Uani 1 1 d . . . Pd2 Pd 0.79221(2) 0.22474(2) 0.514439(17) 0.02868(10) Uani 1 1 d . . . P1 P 0.24936(9) 0.27557(7) 0.09421(6) 0.0342(3) Uani 1 1 d . . . P2 P 0.18355(9) 0.26702(7) -0.09066(6) 0.0339(3) Uani 1 1 d . . . P3 P 0.68371(9) 0.30652(7) 0.58592(6) 0.0326(3) Uani 1 1 d . . . P4 P 0.72546(9) 0.23517(7) 0.40303(6) 0.0315(3) Uani 1 1 d . . . N1 N 0.3371(3) 0.2466(3) 0.1527(2) 0.0431(9) Uani 1 1 d . . . N2 N 0.4113(3) 0.1699(2) 0.04948(19) 0.0334(8) Uani 1 1 d . . . N3 N 0.4873(3) 0.1138(2) 0.0291(2) 0.0437(9) Uani 1 1 d . . . N4 N 0.2128(3) 0.2242(2) -0.17358(19) 0.0388(8) Uani 1 1 d . . . N5 N 0.3558(3) 0.1657(2) -0.11550(19) 0.0336(8) Uani 1 1 d . . . N6 N 0.4431(3) 0.1174(3) -0.1304(2) 0.0470(9) Uani 1 1 d . . . N7 N 0.7285(3) 0.3044(2) 0.66970(19) 0.0417(9) Uani 1 1 d . . . N8 N 0.8584(3) 0.2151(2) 0.61606(18) 0.0315(8) Uani 1 1 d . . . N9 N 0.9478(3) 0.1739(2) 0.6341(2) 0.0442(9) Uani 1 1 d . . . N10 N 0.7921(3) 0.1681(2) 0.34657(19) 0.0397(8) Uani 1 1 d . . . N11 N 0.8914(3) 0.1467(2) 0.45099(19) 0.0324(8) Uani 1 1 d . . . N12 N 0.9725(3) 0.1012(3) 0.4719(2) 0.0451(9) Uani 1 1 d . . . S1 S 0.50218(10) 0.14787(8) 0.16720(7) 0.0449(3) Uani 1 1 d . . . S2 S 0.35438(11) 0.13126(9) -0.25250(7) 0.0489(3) Uani 1 1 d . . . S3 S 0.87688(11) 0.24613(8) 0.75331(7) 0.0475(3) Uani 1 1 d . . . S4 S 0.95631(10) 0.06543(8) 0.33392(7) 0.0468(3) Uani 1 1 d . . . C1 C 0.4049(3) 0.1956(3) 0.1211(2) 0.0346(10) Uani 1 1 d . . . C2 C 0.5393(4) 0.0972(3) 0.0837(3) 0.0469(12) Uani 1 1 d . . . H2 H 0.5939 0.0601 0.0792 0.056 Uiso 1 1 calc R . . C3 C 0.2831(4) 0.4132(3) 0.1209(2) 0.0392(10) Uani 1 1 d . . . C4 C 0.3982(4) 0.4751(3) 0.1556(3) 0.0609(14) Uani 1 1 d . . . H4 H 0.4566 0.4459 0.1675 0.073 Uiso 1 1 calc R . . C5 C 0.4259(6) 0.5810(4) 0.1723(4) 0.086(2) Uani 1 1 d . . . H5 H 0.5036 0.6226 0.1953 0.103 Uiso 1 1 calc R . . C6 C 0.3411(6) 0.6251(4) 0.1557(4) 0.086(2) Uani 1 1 d . . . H6 H 0.3604 0.6962 0.1678 0.104 Uiso 1 1 calc R . . C7 C 0.2271(6) 0.5638(4) 0.1211(3) 0.0757(17) Uani 1 1 d . . . H7 H 0.1697 0.5937 0.1088 0.091 Uiso 1 1 calc R . . C8 C 0.1967(5) 0.4583(3) 0.1045(3) 0.0578(14) Uani 1 1 d . . . H8 H 0.1182 0.4173 0.0822 0.069 Uiso 1 1 calc R . . C9 C 0.0899(4) 0.2175(3) 0.1142(2) 0.0388(10) Uani 1 1 d . . . C10 C 0.0121(4) 0.1263(3) 0.0714(3) 0.0474(12) Uani 1 1 d . . . H10 H 0.0389 0.0982 0.0293 0.057 Uiso 1 1 calc R . . C11 C -0.1057(4) 0.0775(4) 0.0916(3) 0.0668(16) Uani 1 1 d . . . H11 H -0.1575 0.0162 0.0630 0.080 Uiso 1 1 calc R . . C12 C -0.1462(4) 0.1184(5) 0.1530(4) 0.0710(18) Uani 1 1 d . . . H12 H -0.2254 0.0851 0.1661 0.085 Uiso 1 1 calc R . . C13 C -0.0701(5) 0.2090(5) 0.1956(3) 0.0740(17) Uani 1 1 d . . . H13 H -0.0977 0.2365 0.2376 0.089 Uiso 1 1 calc R . . C14 C 0.0472(4) 0.2589(4) 0.1761(3) 0.0613(14) Uani 1 1 d . . . H14 H 0.0979 0.3206 0.2045 0.074 Uiso 1 1 calc R . . C15 C 0.2992(3) 0.1800(3) -0.1740(2) 0.0334(10) Uani 1 1 d . . . C16 C 0.4509(4) 0.0957(3) -0.1981(3) 0.0520(12) Uani 1 1 d . . . H16 H 0.5051 0.0628 -0.2171 0.062 Uiso 1 1 calc R . . C17 C 0.0157(3) 0.2088(3) -0.0901(2) 0.0346(10) Uani 1 1 d . . . C18 C -0.0400(4) 0.1081(3) -0.1267(2) 0.0421(11) Uani 1 1 d . . . H18 H 0.0083 0.0746 -0.1525 0.050 Uiso 1 1 calc R . . C19 C -0.1668(4) 0.0564(3) -0.1253(3) 0.0538(13) Uani 1 1 d . . . H19 H -0.2027 -0.0118 -0.1490 0.065 Uiso 1 1 calc R . . C20 C -0.2381(4) 0.1059(4) -0.0892(3) 0.0627(15) Uani 1 1 d . . . H20 H -0.3234 0.0719 -0.0893 0.075 Uiso 1 1 calc R . . C21 C -0.1855(4) 0.2057(4) -0.0524(3) 0.0580(13) Uani 1 1 d . . . H21 H -0.2349 0.2387 -0.0272 0.070 Uiso 1 1 calc R . . C22 C -0.0581(4) 0.2573(3) -0.0527(2) 0.0448(11) Uani 1 1 d . . . H22 H -0.0225 0.3248 -0.0276 0.054 Uiso 1 1 calc R . . C23 C 0.2177(3) 0.4053(3) -0.0833(2) 0.0364(10) Uani 1 1 d . . . C24 C 0.1381(4) 0.4441(3) -0.1155(3) 0.0553(13) Uani 1 1 d . . . H24 H 0.0619 0.3998 -0.1389 0.066 Uiso 1 1 calc R . . C25 C 0.1721(5) 0.5498(3) -0.1130(3) 0.0691(16) Uani 1 1 d . . . H25 H 0.1179 0.5763 -0.1338 0.083 Uiso 1 1 calc R . . C26 C 0.2862(5) 0.6150(3) -0.0796(3) 0.0659(16) Uani 1 1 d . . . H26 H 0.3095 0.6855 -0.0784 0.079 Uiso 1 1 calc R . . C27 C 0.3649(5) 0.5760(3) -0.0484(3) 0.0691(16) Uani 1 1 d . . . H27 H 0.4420 0.6201 -0.0260 0.083 Uiso 1 1 calc R . . C28 C 0.3310(4) 0.4716(3) -0.0498(3) 0.0525(13) Uani 1 1 d . . . H28 H 0.3850 0.4458 -0.0281 0.063 Uiso 1 1 calc R . . C29 C 0.8124(4) 0.2594(3) 0.6728(2) 0.0338(10) Uani 1 1 d . . . C30 C 0.9664(4) 0.1859(3) 0.7031(3) 0.0458(11) Uani 1 1 d . . . H30 H 1.0244 0.1636 0.7245 0.055 Uiso 1 1 calc R . . C31 C 0.5152(3) 0.2502(3) 0.5777(2) 0.0375(10) Uani 1 1 d . . . C32 C 0.4560(4) 0.1500(3) 0.5415(3) 0.0510(12) Uani 1 1 d . . . H32 H 0.5026 0.1117 0.5193 0.061 Uiso 1 1 calc R . . C33 C 0.3267(5) 0.1067(4) 0.5383(3) 0.0693(16) Uani 1 1 d . . . H33 H 0.2871 0.0393 0.5140 0.083 Uiso 1 1 calc R . . C34 C 0.2577(5) 0.1617(5) 0.5703(3) 0.078(2) Uani 1 1 d . . . H34 H 0.1711 0.1327 0.5666 0.094 Uiso 1 1 calc R . . C35 C 0.3156(5) 0.2601(5) 0.6080(4) 0.079(2) Uani 1 1 d . . . H35 H 0.2681 0.2969 0.6310 0.094 Uiso 1 1 calc R . . C36 C 0.4441(4) 0.3051(3) 0.6124(3) 0.0544(13) Uani 1 1 d . . . H36 H 0.4828 0.3718 0.6383 0.065 Uiso 1 1 calc R . . C37 C 0.7165(4) 0.4410(3) 0.5820(2) 0.0397(10) Uani 1 1 d . . . C38 C 0.8158(4) 0.5163(3) 0.6254(3) 0.0568(13) Uani 1 1 d . . . H38 H 0.8585 0.4983 0.6606 0.068 Uiso 1 1 calc R . . C39 C 0.8515(5) 0.6179(4) 0.6166(3) 0.0778(18) Uani 1 1 d . . . H39 H 0.9191 0.6678 0.6450 0.093 Uiso 1 1 calc R . . C40 C 0.7875(5) 0.6440(4) 0.5665(4) 0.0771(19) Uani 1 1 d . . . H40 H 0.8119 0.7124 0.5611 0.093 Uiso 1 1 calc R . . C41 C 0.6876(5) 0.5726(4) 0.5235(3) 0.0665(16) Uani 1 1 d . . . H41 H 0.6441 0.5919 0.4896 0.080 Uiso 1 1 calc R . . C42 C 0.6530(4) 0.4701(3) 0.5320(3) 0.0484(12) Uani 1 1 d . . . H42 H 0.5855 0.4207 0.5032 0.058 Uiso 1 1 calc R . . C43 C 0.8684(3) 0.1347(3) 0.3789(2) 0.0337(10) Uani 1 1 d . . . C44 C 1.0121(4) 0.0575(3) 0.4176(3) 0.0488(12) Uani 1 1 d . . . H44 H 1.0681 0.0231 0.4227 0.059 Uiso 1 1 calc R . . C45 C 0.5607(3) 0.1742(3) 0.3752(2) 0.0346(10) Uani 1 1 d . . . C46 C 0.5157(4) 0.0668(3) 0.3622(3) 0.0493(12) Uani 1 1 d . . . H46 H 0.5701 0.0312 0.3681 0.059 Uiso 1 1 calc R . . C47 C 0.3908(5) 0.0125(4) 0.3406(3) 0.0739(17) Uani 1 1 d . . . H47 H 0.3610 -0.0591 0.3331 0.089 Uiso 1 1 calc R . . C48 C 0.3120(5) 0.0647(5) 0.3305(3) 0.083(2) Uani 1 1 d . . . H48 H 0.2284 0.0282 0.3152 0.100 Uiso 1 1 calc R . . C49 C 0.3539(4) 0.1700(5) 0.3423(3) 0.0775(17) Uani 1 1 d . . . H49 H 0.2995 0.2047 0.3342 0.093 Uiso 1 1 calc R . . C50 C 0.4787(4) 0.2254(4) 0.3667(3) 0.0516(12) Uani 1 1 d . . . H50 H 0.5063 0.2971 0.3771 0.062 Uiso 1 1 calc R . . C51 C 0.7722(4) 0.3617(3) 0.3797(2) 0.0352(10) Uani 1 1 d . . . C52 C 0.7280(5) 0.3770(3) 0.3162(3) 0.0612(14) Uani 1 1 d . . . H52 H 0.6679 0.3225 0.2859 0.073 Uiso 1 1 calc R . . C53 C 0.7719(5) 0.4729(4) 0.2965(3) 0.0778(18) Uani 1 1 d . . . H53 H 0.7411 0.4826 0.2533 0.093 Uiso 1 1 calc R . . C54 C 0.8603(5) 0.5526(4) 0.3408(3) 0.0656(16) Uani 1 1 d . . . H54 H 0.8897 0.6168 0.3276 0.079 Uiso 1 1 calc R . . C55 C 0.9061(4) 0.5394(4) 0.4042(3) 0.0669(16) Uani 1 1 d . . . H55 H 0.9669 0.5940 0.4340 0.080 Uiso 1 1 calc R . . C56 C 0.8613(4) 0.4441(3) 0.4238(3) 0.0502(12) Uani 1 1 d . . . H56 H 0.8916 0.4352 0.4675 0.060 Uiso 1 1 calc R . . 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 Pd1 0.03039(16) 0.02913(16) 0.0294(2) 0.00651(13) 0.00086(13) 0.01131(12) Pd2 0.02955(16) 0.02905(16) 0.0294(2) 0.00665(13) -0.00004(13) 0.01212(12) P1 0.0355(5) 0.0363(5) 0.0323(7) 0.0060(5) 0.0038(5) 0.0146(5) P2 0.0339(5) 0.0332(5) 0.0360(7) 0.0076(5) -0.0007(5) 0.0133(4) P3 0.0331(5) 0.0358(5) 0.0313(7) 0.0053(5) 0.0010(5) 0.0154(4) P4 0.0322(5) 0.0339(5) 0.0309(7) 0.0077(5) 0.0023(5) 0.0141(4) N1 0.050(2) 0.057(2) 0.030(2) 0.0078(17) 0.0062(18) 0.0285(18) N2 0.0409(18) 0.0310(17) 0.034(2) 0.0084(15) 0.0014(16) 0.0196(15) N3 0.057(2) 0.047(2) 0.038(3) 0.0077(17) -0.0007(19) 0.0320(18) N4 0.0429(19) 0.0490(19) 0.029(2) 0.0058(16) -0.0027(17) 0.0232(16) N5 0.0372(18) 0.0368(17) 0.033(2) 0.0087(15) 0.0008(16) 0.0202(15) N6 0.054(2) 0.062(2) 0.039(3) 0.014(2) 0.010(2) 0.0361(19) N7 0.0444(19) 0.057(2) 0.032(2) 0.0042(17) -0.0031(17) 0.0304(17) N8 0.0377(17) 0.0317(16) 0.029(2) 0.0072(15) -0.0026(16) 0.0162(14) N9 0.050(2) 0.0436(19) 0.046(3) 0.0089(18) -0.0044(19) 0.0255(17) N10 0.048(2) 0.051(2) 0.030(2) 0.0087(17) 0.0040(17) 0.0292(17) N11 0.0341(17) 0.0341(17) 0.034(2) 0.0079(15) -0.0031(16) 0.0184(14) N12 0.054(2) 0.052(2) 0.040(3) 0.0090(18) 0.0004(19) 0.0328(18) S1 0.0510(6) 0.0486(6) 0.0377(8) 0.0089(5) -0.0084(6) 0.0211(5) S2 0.0620(7) 0.0586(7) 0.0315(7) 0.0052(5) 0.0052(6) 0.0294(6) S3 0.0584(7) 0.0559(7) 0.0326(7) 0.0089(5) -0.0066(6) 0.0259(6) S4 0.0503(6) 0.0527(6) 0.0457(8) 0.0050(6) 0.0082(6) 0.0305(5) C1 0.036(2) 0.030(2) 0.036(3) 0.0077(19) 0.002(2) 0.0084(17) C2 0.053(3) 0.048(2) 0.051(3) 0.010(2) -0.001(2) 0.032(2) C3 0.043(2) 0.040(2) 0.037(3) 0.0061(19) 0.013(2) 0.018(2) C4 0.050(3) 0.053(3) 0.066(4) -0.005(3) 0.003(3) 0.009(2) C5 0.083(4) 0.047(3) 0.100(6) -0.015(3) 0.012(4) 0.000(3) C6 0.114(5) 0.035(3) 0.105(6) -0.002(3) 0.039(4) 0.023(3) C7 0.104(5) 0.055(3) 0.080(5) 0.008(3) 0.027(4) 0.044(3) C8 0.068(3) 0.047(3) 0.065(4) 0.002(2) 0.011(3) 0.032(2) C9 0.045(2) 0.043(2) 0.034(3) 0.015(2) 0.006(2) 0.018(2) C10 0.050(3) 0.042(2) 0.051(3) 0.015(2) 0.005(2) 0.013(2) C11 0.051(3) 0.060(3) 0.084(5) 0.035(3) -0.001(3) 0.002(3) C12 0.039(3) 0.100(4) 0.085(5) 0.057(4) 0.017(3) 0.019(3) C13 0.056(3) 0.112(5) 0.061(4) 0.034(4) 0.026(3) 0.028(3) C14 0.052(3) 0.081(3) 0.046(4) 0.009(3) 0.013(3) 0.017(3) C15 0.035(2) 0.032(2) 0.028(3) 0.0061(18) 0.0028(19) 0.0045(18) C16 0.063(3) 0.067(3) 0.039(3) 0.010(2) 0.011(3) 0.039(2) C17 0.034(2) 0.034(2) 0.036(3) 0.0090(18) -0.0060(19) 0.0117(18) C18 0.044(2) 0.032(2) 0.047(3) 0.011(2) -0.006(2) 0.0087(19) C19 0.052(3) 0.036(2) 0.065(4) 0.012(2) -0.004(3) 0.003(2) C20 0.043(3) 0.062(3) 0.074(4) 0.021(3) -0.004(3) 0.003(3) C21 0.042(3) 0.078(3) 0.060(4) 0.019(3) 0.011(3) 0.026(3) C22 0.045(2) 0.043(2) 0.045(3) 0.003(2) -0.003(2) 0.016(2) C23 0.038(2) 0.034(2) 0.036(3) 0.0056(19) 0.005(2) 0.0123(18) C24 0.059(3) 0.040(2) 0.070(4) 0.015(2) -0.010(3) 0.020(2) C25 0.082(4) 0.051(3) 0.084(5) 0.024(3) 0.002(3) 0.030(3) C26 0.090(4) 0.036(3) 0.072(4) 0.016(3) 0.027(3) 0.017(3) C27 0.062(3) 0.042(3) 0.081(5) 0.006(3) 0.009(3) -0.008(3) C28 0.044(3) 0.044(3) 0.064(4) 0.012(2) 0.002(2) 0.007(2) C29 0.040(2) 0.031(2) 0.024(3) 0.0025(17) -0.0013(19) 0.0046(18) C30 0.054(3) 0.051(3) 0.038(3) 0.011(2) -0.010(2) 0.025(2) C31 0.036(2) 0.046(2) 0.036(3) 0.018(2) 0.005(2) 0.0150(19) C32 0.047(3) 0.052(3) 0.046(3) 0.010(2) 0.005(2) 0.005(2) C33 0.051(3) 0.073(3) 0.062(4) 0.019(3) -0.007(3) -0.010(3) C34 0.039(3) 0.118(5) 0.081(5) 0.063(4) -0.001(3) 0.008(3) C35 0.051(3) 0.104(4) 0.118(6) 0.070(4) 0.034(3) 0.048(3) C36 0.042(2) 0.055(3) 0.078(4) 0.029(3) 0.017(3) 0.023(2) C37 0.036(2) 0.039(2) 0.046(3) 0.003(2) 0.004(2) 0.0183(19) C38 0.060(3) 0.047(3) 0.056(4) -0.001(2) -0.007(3) 0.015(2) C39 0.077(4) 0.036(3) 0.097(5) -0.010(3) 0.004(4) 0.001(3) C40 0.075(4) 0.045(3) 0.118(6) 0.020(3) 0.027(4) 0.025(3) C41 0.062(3) 0.065(3) 0.095(5) 0.045(3) 0.024(3) 0.034(3) C42 0.044(2) 0.046(3) 0.062(4) 0.016(2) 0.002(2) 0.020(2) C43 0.033(2) 0.029(2) 0.039(3) 0.0093(18) 0.002(2) 0.0095(17) C44 0.049(3) 0.051(3) 0.060(4) 0.009(2) 0.010(2) 0.035(2) C45 0.036(2) 0.042(2) 0.027(3) 0.0068(18) 0.0036(18) 0.0134(18) C46 0.048(3) 0.049(3) 0.044(3) 0.004(2) 0.011(2) 0.010(2) C47 0.058(3) 0.069(3) 0.062(4) -0.007(3) 0.012(3) -0.012(3) C48 0.034(3) 0.114(5) 0.067(5) -0.021(4) 0.006(3) -0.002(3) C49 0.042(3) 0.121(5) 0.066(4) -0.011(4) -0.002(3) 0.038(3) C50 0.045(3) 0.068(3) 0.044(3) -0.004(2) -0.005(2) 0.029(2) C51 0.040(2) 0.035(2) 0.034(3) 0.0108(19) 0.006(2) 0.0153(18) C52 0.083(3) 0.049(3) 0.044(3) 0.016(2) -0.006(3) 0.010(3) C53 0.110(5) 0.067(4) 0.066(5) 0.041(3) 0.014(4) 0.030(3) C54 0.072(3) 0.043(3) 0.089(5) 0.031(3) 0.027(3) 0.017(3) C55 0.054(3) 0.047(3) 0.086(5) 0.016(3) 0.010(3) -0.002(2) C56 0.040(2) 0.050(3) 0.052(3) 0.014(2) 0.002(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 N2 2.081(3) . ? Pd1 N5 2.083(3) . ? Pd1 P2 2.2626(11) . ? Pd1 P1 2.2675(12) . ? Pd2 N11 2.083(3) . ? Pd2 N8 2.090(3) . ? Pd2 P4 2.2679(11) . ? Pd2 P3 2.2688(11) . ? P1 N1 1.660(4) . ? P1 C9 1.808(4) . ? P1 C3 1.812(4) . ? P2 N4 1.662(4) . ? P2 C17 1.815(4) . ? P2 C23 1.824(4) . ? P3 N7 1.661(4) . ? P3 C31 1.810(4) . ? P3 C37 1.811(4) . ? P4 N10 1.662(3) . ? P4 C45 1.807(4) . ? P4 C51 1.809(4) . ? N1 C1 1.305(5) . ? N2 C1 1.351(5) . ? N2 N3 1.370(4) . ? N3 C2 1.271(5) . ? N4 C15 1.324(5) . ? N5 C15 1.345(5) . ? N5 N6 1.384(4) . ? N6 C16 1.277(6) . ? N7 C29 1.311(5) . ? N8 C29 1.351(5) . ? N8 N9 1.387(4) . ? N9 C30 1.289(5) . ? N10 C43 1.301(5) . ? N11 C43 1.353(5) . ? N11 N12 1.369(4) . ? N12 C44 1.274(5) . ? S1 C2 1.738(5) . ? S1 C1 1.755(4) . ? S2 C16 1.732(5) . ? S2 C15 1.745(4) . ? S3 C30 1.730(5) . ? S3 C29 1.740(4) . ? S4 C44 1.726(5) . ? S4 C43 1.750(4) . ? C3 C4 1.382(6) . ? C3 C8 1.389(6) . ? C4 C5 1.386(6) . ? C5 C6 1.365(8) . ? C6 C7 1.371(8) . ? C7 C8 1.377(6) . ? C9 C14 1.385(6) . ? C9 C10 1.389(6) . ? C10 C11 1.386(6) . ? C11 C12 1.364(8) . ? C12 C13 1.377(7) . ? C13 C14 1.381(6) . ? C17 C22 1.382(6) . ? C17 C18 1.385(5) . ? C18 C19 1.389(5) . ? C19 C20 1.357(7) . ? C20 C21 1.373(6) . ? C21 C22 1.392(5) . ? C23 C28 1.376(5) . ? C23 C24 1.379(6) . ? C24 C25 1.392(5) . ? C25 C26 1.378(7) . ? C26 C27 1.364(7) . ? C27 C28 1.378(6) . ? C31 C32 1.383(6) . ? C31 C36 1.393(6) . ? C32 C33 1.391(6) . ? C33 C34 1.356(8) . ? C34 C35 1.371(8) . ? C35 C36 1.383(6) . ? C37 C42 1.370(6) . ? C37 C38 1.391(6) . ? C38 C39 1.386(6) . ? C39 C40 1.352(8) . ? C40 C41 1.370(7) . ? C41 C42 1.396(6) . ? C45 C50 1.376(6) . ? C45 C46 1.393(5) . ? C46 C47 1.386(6) . ? C47 C48 1.361(8) . ? C48 C49 1.366(7) . ? C49 C50 1.396(6) . ? C51 C52 1.369(6) . ? C51 C56 1.382(6) . ? C52 C53 1.390(6) . ? C53 C54 1.362(7) . ? C54 C55 1.362(7) . ? C55 C56 1.382(6) . ? 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 N2 Pd1 N5 98.53(13) . . ? N2 Pd1 P2 177.94(10) . . ? N5 Pd1 P2 79.52(9) . . ? N2 Pd1 P1 79.52(10) . . ? N5 Pd1 P1 177.91(9) . . ? P2 Pd1 P1 102.44(4) . . ? N11 Pd2 N8 98.97(13) . . ? N11 Pd2 P4 79.66(9) . . ? N8 Pd2 P4 178.43(9) . . ? N11 Pd2 P3 178.29(9) . . ? N8 Pd2 P3 79.63(9) . . ? P4 Pd2 P3 101.75(4) . . ? N1 P1 C9 105.87(18) . . ? N1 P1 C3 105.03(19) . . ? C9 P1 C3 105.05(19) . . ? N1 P1 Pd1 105.38(13) . . ? C9 P1 Pd1 117.28(15) . . ? C3 P1 Pd1 117.07(14) . . ? N4 P2 C17 104.30(18) . . ? N4 P2 C23 105.97(18) . . ? C17 P2 C23 107.04(17) . . ? N4 P2 Pd1 105.63(12) . . ? C17 P2 Pd1 116.11(12) . . ? C23 P2 Pd1 116.61(14) . . ? N7 P3 C31 105.44(18) . . ? N7 P3 C37 105.97(19) . . ? C31 P3 C37 105.17(18) . . ? N7 P3 Pd2 105.29(12) . . ? C31 P3 Pd2 118.16(15) . . ? C37 P3 Pd2 115.75(14) . . ? N10 P4 C45 103.68(18) . . ? N10 P4 C51 105.27(17) . . ? C45 P4 C51 106.86(18) . . ? N10 P4 Pd2 104.84(12) . . ? C45 P4 Pd2 117.38(13) . . ? C51 P4 Pd2 117.23(15) . . ? C1 N1 P1 112.5(3) . . ? C1 N2 N3 116.0(3) . . ? C1 N2 Pd1 115.8(3) . . ? N3 N2 Pd1 128.2(3) . . ? C2 N3 N2 111.1(4) . . ? C15 N4 P2 112.5(3) . . ? C15 N5 N6 114.6(3) . . ? C15 N5 Pd1 116.5(3) . . ? N6 N5 Pd1 129.0(3) . . ? C16 N6 N5 111.3(4) . . ? C29 N7 P3 113.0(3) . . ? C29 N8 N9 114.8(3) . . ? C29 N8 Pd2 115.8(3) . . ? N9 N8 Pd2 129.3(3) . . ? C30 N9 N8 110.8(4) . . ? C43 N10 P4 113.4(3) . . ? C43 N11 N12 115.0(3) . . ? C43 N11 Pd2 115.9(2) . . ? N12 N11 Pd2 129.0(3) . . ? C44 N12 N11 111.2(4) . . ? C2 S1 C1 87.7(2) . . ? C16 S2 C15 87.6(2) . . ? C30 S3 C29 88.1(2) . . ? C44 S4 C43 87.4(2) . . ? N1 C1 N2 126.7(4) . . ? N1 C1 S1 124.1(3) . . ? N2 C1 S1 109.2(3) . . ? N3 C2 S1 116.0(3) . . ? C4 C3 C8 119.3(4) . . ? C4 C3 P1 119.8(3) . . ? C8 C3 P1 120.9(3) . . ? C3 C4 C5 119.5(5) . . ? C6 C5 C4 121.1(5) . . ? C5 C6 C7 119.4(5) . . ? C6 C7 C8 120.7(5) . . ? C7 C8 C3 120.0(5) . . ? C14 C9 C10 119.2(4) . . ? C14 C9 P1 120.0(3) . . ? C10 C9 P1 120.6(3) . . ? C11 C10 C9 119.8(5) . . ? C12 C11 C10 120.5(5) . . ? C11 C12 C13 120.1(4) . . ? C12 C13 C14 120.0(5) . . ? C13 C14 C9 120.3(5) . . ? N4 C15 N5 125.8(4) . . ? N4 C15 S2 123.6(3) . . ? N5 C15 S2 110.7(3) . . ? N6 C16 S2 115.9(3) . . ? C22 C17 C18 118.5(4) . . ? C22 C17 P2 123.8(3) . . ? C18 C17 P2 117.7(3) . . ? C17 C18 C19 121.0(4) . . ? C20 C19 C18 119.6(4) . . ? C19 C20 C21 120.7(4) . . ? C20 C21 C22 119.9(5) . . ? C17 C22 C21 120.3(4) . . ? C28 C23 C24 119.5(4) . . ? C28 C23 P2 118.5(3) . . ? C24 C23 P2 121.8(3) . . ? C23 C24 C25 119.8(4) . . ? C26 C25 C24 119.9(5) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C28 120.4(5) . . ? C23 C28 C27 120.4(4) . . ? N7 C29 N8 126.2(4) . . ? N7 C29 S3 123.3(3) . . ? N8 C29 S3 110.5(3) . . ? N9 C30 S3 115.8(3) . . ? C32 C31 C36 119.2(4) . . ? C32 C31 P3 120.6(3) . . ? C36 C31 P3 120.0(3) . . ? C31 C32 C33 119.7(5) . . ? C34 C33 C32 120.8(5) . . ? C33 C34 C35 120.0(5) . . ? C34 C35 C36 120.6(5) . . ? C35 C36 C31 119.7(5) . . ? C42 C37 C38 118.6(4) . . ? C42 C37 P3 121.3(3) . . ? C38 C37 P3 119.8(3) . . ? C39 C38 C37 120.3(5) . . ? C40 C39 C38 119.7(5) . . ? C39 C40 C41 121.9(5) . . ? C40 C41 C42 118.3(5) . . ? C37 C42 C41 121.3(4) . . ? N10 C43 N11 126.0(4) . . ? N10 C43 S4 124.0(4) . . ? N11 C43 S4 109.9(3) . . ? N12 C44 S4 116.4(3) . . ? C50 C45 C46 118.8(4) . . ? C50 C45 P4 125.1(3) . . ? C46 C45 P4 116.1(3) . . ? C47 C46 C45 120.7(5) . . ? C48 C47 C46 119.6(5) . . ? C47 C48 C49 120.9(5) . . ? C48 C49 C50 119.9(5) . . ? C45 C50 C49 120.1(4) . . ? C52 C51 C56 118.3(4) . . ? C52 C51 P4 121.5(3) . . ? C56 C51 P4 120.0(3) . . ? C51 C52 C53 120.8(5) . . ? C54 C53 C52 119.6(5) . . ? C53 C54 C55 120.8(4) . . ? C54 C55 C56 119.4(5) . . ? C55 C56 C51 121.1(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.947 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.105 # Attachment '- compound4a.cif' data_compound4a _database_code_depnum_ccdc_archive 'CCDC 801708' #TrackingRef '- compound4a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 Cl2 N6 P2 Pd Pt S2, C H2 Cl2' _chemical_formula_sum 'C29 H24 Cl4 N6 P2 Pd Pt S2' _chemical_formula_weight 1025.89 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' 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' Pd Pd -0.9988 1.0072 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2464(4) _cell_length_b 19.2382(8) _cell_length_c 19.7126(6) _cell_angle_alpha 90.00 _cell_angle_beta 120.504(2) _cell_angle_gamma 90.00 _cell_volume 3348.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 53992 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 5.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.443 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31573 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 30.07 _reflns_number_total 9783 _reflns_number_gt 6870 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9783 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0650(4) 0.8670(3) 0.2289(2) 0.0212(9) Uani 1 1 d . . . C2 C 0.0420(5) 0.7493(3) 0.2652(2) 0.0294(11) Uani 1 1 d . . . C3 C 0.2008(5) 1.0464(2) 0.2879(2) 0.0229(10) Uani 1 1 d . . . C4 C 0.1231(6) 1.0400(3) 0.3283(3) 0.0360(12) Uani 1 1 d . . . C5 C 0.1338(7) 1.0914(3) 0.3799(3) 0.0510(16) Uani 1 1 d . . . C6 C 0.2211(6) 1.1491(3) 0.3919(3) 0.0405(13) Uani 1 1 d . . . C7 C 0.2955(5) 1.1570(3) 0.3512(3) 0.0344(12) Uani 1 1 d . . . C8 C 0.2874(5) 1.1057(3) 0.2997(3) 0.0286(11) Uani 1 1 d . . . C9 C 0.2140(4) 1.0027(2) 0.1492(2) 0.0215(10) Uani 1 1 d . . . C10 C 0.1268(4) 1.0597(3) 0.1076(2) 0.0257(10) Uani 1 1 d . . . C11 C 0.1125(5) 1.0761(3) 0.0353(2) 0.0287(11) Uani 1 1 d . . . C12 C 0.1848(5) 1.0377(3) 0.0061(2) 0.0347(13) Uani 1 1 d . . . C13 C 0.2734(5) 0.9807(3) 0.0473(2) 0.0347(12) Uani 1 1 d . . . C14 C 0.2866(5) 0.9624(3) 0.1190(2) 0.0292(11) Uani 1 1 d . . . C15 C 0.6837(4) 0.8253(3) 0.3914(2) 0.0217(10) Uani 1 1 d . . . C16 C 0.6305(5) 0.7096(3) 0.4204(3) 0.0313(11) Uani 1 1 d . . . C17 C 0.6362(4) 0.9843(3) 0.2682(2) 0.0233(10) Uani 1 1 d . . . C18 C 0.6308(5) 1.0557(3) 0.2575(3) 0.0322(11) Uani 1 1 d . . . C19 C 0.6570(6) 1.0833(3) 0.2005(3) 0.0410(13) Uani 1 1 d . . . C20 C 0.6859(6) 1.0403(3) 0.1536(3) 0.0415(14) Uani 1 1 d . . . C21 C 0.6879(5) 0.9698(3) 0.1626(3) 0.0361(13) Uani 1 1 d . . . C22 C 0.6641(5) 0.9408(3) 0.2205(3) 0.0304(11) Uani 1 1 d . . . C23 C 0.6760(4) 1.0115(2) 0.4198(2) 0.0211(9) Uani 1 1 d . . . C24 C 0.5907(5) 1.0357(3) 0.4507(2) 0.0277(11) Uani 1 1 d . . . C25 C 0.6499(5) 1.0853(3) 0.5103(3) 0.0327(12) Uani 1 1 d . . . C26 C 0.7943(5) 1.1100(3) 0.5394(3) 0.0331(12) Uani 1 1 d . . . C27 C 0.8812(5) 1.0861(3) 0.5097(3) 0.0351(12) Uani 1 1 d . . . C28 C 0.8237(5) 1.0372(3) 0.4502(2) 0.0294(11) Uani 1 1 d . . . C29 C 0.3090(6) 0.7415(4) 0.1182(3) 0.064(2) Uani 1 1 d . . . Cl1 Cl 0.14250(12) 0.69533(7) 0.43026(6) 0.0354(3) Uani 1 1 d . . . Cl2 Cl 0.50222(12) 0.67948(7) 0.53075(6) 0.0347(3) Uani 1 1 d . . . Cl3 Cl 0.47012(17) 0.74545(10) 0.21244(8) 0.0643(5) Uani 1 1 d . . . Cl4 Cl 0.14370(19) 0.73705(14) 0.12024(10) 0.0937(8) Uani 1 1 d . . . N1 N 0.0487(4) 0.9291(2) 0.19997(19) 0.0246(9) Uani 1 1 d . . . N2 N 0.1962(3) 0.8390(2) 0.28698(18) 0.0208(8) Uani 1 1 d . . . N3 N 0.1792(4) 0.7720(2) 0.30686(19) 0.0228(8) Uani 1 1 d . . . N4 N 0.7368(4) 0.8817(2) 0.3790(2) 0.0235(8) Uani 1 1 d . . . N5 N 0.5416(3) 0.81670(19) 0.38078(18) 0.0181(7) Uani 1 1 d . . . N6 N 0.5166(4) 0.7512(2) 0.39922(18) 0.0214(8) Uani 1 1 d . . . P1 P 0.21280(11) 0.97174(6) 0.23548(6) 0.0207(2) Uani 1 1 d . . . P2 P 0.60878(11) 0.94598(6) 0.34384(6) 0.0202(2) Uani 1 1 d . . . Pd1 Pd 0.33610(3) 0.727364(19) 0.411854(17) 0.02123(8) Uani 1 1 d . . . Pt1 Pt 0.389666(16) 0.894302(9) 0.314650(8) 0.01790(5) Uani 1 1 d . . . S1 S -0.08371(12) 0.80730(7) 0.19690(7) 0.0320(3) Uani 1 1 d . . . S2 S 0.78438(12) 0.74687(7) 0.42234(7) 0.0308(3) Uani 1 1 d . . . H2 H 0.0623 1.0001 0.3204 0.043 Uiso 1 1 calc R . . H3 H 0.0802 1.0866 0.4073 0.061 Uiso 1 1 calc R . . H4 H 0.2298 1.1836 0.4284 0.049 Uiso 1 1 calc R . . H5 H 0.3532 1.1979 0.3583 0.041 Uiso 1 1 calc R . . H6 H 0.341 1.1112 0.2724 0.034 Uiso 1 1 calc R . . H8 H 0.0776 1.0871 0.1281 0.031 Uiso 1 1 calc R . . H9 H 0.0516 1.1145 0.006 0.034 Uiso 1 1 calc R . . H10 H 0.1746 1.05 -0.043 0.042 Uiso 1 1 calc R . . H11 H 0.3242 0.9545 0.0268 0.042 Uiso 1 1 calc R . . H12 H 0.3445 0.923 0.1472 0.035 Uiso 1 1 calc R . . H14 H 0.0128 0.7041 0.2717 0.035 Uiso 1 1 calc R . . H16 H 0.6093 1.0855 0.289 0.039 Uiso 1 1 calc R . . H17 H 0.655 1.1323 0.1937 0.049 Uiso 1 1 calc R . . H18 H 0.7045 1.0598 0.115 0.05 Uiso 1 1 calc R . . H19 H 0.7055 0.9403 0.1293 0.043 Uiso 1 1 calc R . . H20 H 0.667 0.8918 0.2272 0.036 Uiso 1 1 calc R . . H22 H 0.4911 1.0184 0.4314 0.033 Uiso 1 1 calc R . . H23 H 0.5899 1.1022 0.5309 0.039 Uiso 1 1 calc R . . H24 H 0.834 1.1437 0.5802 0.04 Uiso 1 1 calc R . . H25 H 0.9812 1.1033 0.5301 0.042 Uiso 1 1 calc R . . H26 H 0.8844 1.0208 0.4298 0.035 Uiso 1 1 calc R . . H28 H 0.6288 0.6623 0.4338 0.038 Uiso 1 1 calc R . . H29A H 0.3062 0.7832 0.0881 0.076 Uiso 1 1 calc R . . H29B H 0.3164 0.7002 0.0904 0.076 Uiso 1 1 calc R . . 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 C3 0.026(2) 0.018(3) 0.023(2) 0.0057(18) 0.0112(18) 0.0068(19) C4 0.044(3) 0.032(3) 0.040(3) 0.006(2) 0.028(2) 0.005(2) C5 0.082(4) 0.045(4) 0.050(3) 0.002(3) 0.050(3) 0.010(3) C6 0.059(3) 0.030(3) 0.028(2) 0.002(2) 0.019(2) 0.017(3) C7 0.032(2) 0.019(3) 0.040(3) -0.003(2) 0.010(2) 0.005(2) C8 0.026(2) 0.023(3) 0.037(2) -0.002(2) 0.016(2) 0.005(2) C9 0.0177(19) 0.023(3) 0.0176(18) 0.0004(18) 0.0041(16) 0.0002(19) C10 0.025(2) 0.022(3) 0.026(2) -0.002(2) 0.0102(18) -0.004(2) C11 0.026(2) 0.025(3) 0.026(2) 0.006(2) 0.0063(19) -0.005(2) C12 0.034(2) 0.044(4) 0.020(2) 0.000(2) 0.009(2) -0.010(2) C13 0.037(3) 0.044(4) 0.024(2) -0.007(2) 0.015(2) -0.004(3) C14 0.023(2) 0.031(3) 0.028(2) -0.001(2) 0.0088(19) 0.003(2) C1 0.0159(19) 0.023(3) 0.022(2) -0.0038(19) 0.0076(17) -0.0007(19) C2 0.026(2) 0.026(3) 0.027(2) 0.000(2) 0.0061(19) -0.006(2) C17 0.0187(19) 0.027(3) 0.025(2) 0.000(2) 0.0114(17) -0.003(2) C18 0.037(3) 0.032(3) 0.033(2) 0.002(2) 0.021(2) 0.003(2) C19 0.057(3) 0.033(3) 0.038(3) 0.014(2) 0.027(3) 0.003(3) C20 0.049(3) 0.045(4) 0.041(3) 0.012(3) 0.030(3) 0.002(3) C21 0.042(3) 0.041(4) 0.036(2) 0.000(2) 0.028(2) 0.000(3) C22 0.031(2) 0.026(3) 0.039(2) 0.003(2) 0.021(2) 0.005(2) C23 0.0175(19) 0.018(3) 0.0215(19) 0.0007(18) 0.0057(16) -0.0018(18) C24 0.025(2) 0.031(3) 0.025(2) 0.001(2) 0.0105(19) -0.002(2) C25 0.036(3) 0.035(3) 0.031(2) -0.003(2) 0.020(2) 0.003(2) C26 0.039(3) 0.027(3) 0.022(2) -0.004(2) 0.008(2) -0.002(2) C27 0.029(2) 0.034(3) 0.032(2) -0.004(2) 0.008(2) -0.006(2) C28 0.024(2) 0.029(3) 0.034(2) -0.002(2) 0.013(2) -0.005(2) C15 0.0123(18) 0.026(3) 0.0215(19) 0.0023(19) 0.0044(16) 0.0025(18) C16 0.027(2) 0.026(3) 0.039(2) 0.007(2) 0.016(2) 0.007(2) C29 0.058(4) 0.093(6) 0.042(3) -0.002(3) 0.027(3) -0.008(4) Cl1 0.0318(6) 0.0424(9) 0.0366(6) 0.0015(6) 0.0207(5) -0.0088(6) Cl2 0.0340(6) 0.0373(8) 0.0268(5) 0.0095(5) 0.0110(5) 0.0018(6) Cl3 0.0665(10) 0.0802(14) 0.0379(7) -0.0119(8) 0.0204(7) 0.0024(9) Cl4 0.0617(10) 0.162(2) 0.0661(10) -0.0190(13) 0.0388(9) -0.0046(12) N1 0.0158(16) 0.025(2) 0.0273(18) 0.0004(17) 0.0067(15) 0.0000(17) N2 0.0159(16) 0.020(2) 0.0204(16) -0.0010(15) 0.0049(14) -0.0032(15) N3 0.0214(17) 0.021(2) 0.0238(17) 0.0011(16) 0.0102(15) -0.0028(16) N4 0.0182(17) 0.022(2) 0.0288(18) 0.0009(16) 0.0109(15) -0.0004(16) N5 0.0158(16) 0.014(2) 0.0215(16) 0.0030(15) 0.0076(14) 0.0020(15) N6 0.0223(17) 0.017(2) 0.0231(17) 0.0023(16) 0.0104(15) -0.0001(16) P1 0.0178(5) 0.0196(7) 0.0220(5) 0.0018(5) 0.0080(4) 0.0018(5) P2 0.0172(5) 0.0199(7) 0.0222(5) 0.0001(5) 0.0090(4) -0.0002(5) Pd1 0.02099(16) 0.0191(2) 0.02247(15) 0.00106(14) 0.01024(13) -0.00161(14) Pt1 0.01557(8) 0.01748(10) 0.01839(8) 0.00017(7) 0.00698(6) 0.00005(7) S1 0.0193(5) 0.0300(8) 0.0357(6) 0.0023(6) 0.0058(5) -0.0050(5) S2 0.0222(5) 0.0264(7) 0.0434(6) 0.0076(6) 0.0163(5) 0.0064(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cl1 Pd1 2.2754(11) . ? Cl2 Pd1 2.2779(11) . ? N1 P1 1.671(4) . ? N2 N3 1.383(5) . ? N2 Pt1 2.065(3) . ? N3 Pd1 2.056(3) . ? N4 P2 1.676(4) . ? N5 N6 1.371(5) . ? N5 Pt1 2.072(3) . ? N6 Pd1 2.040(3) . ? P1 Pt1 2.2512(11) . ? P2 Pt1 2.2469(11) . ? C1 N1 1.297(6) . ? C1 N2 1.359(5) . ? C1 S1 1.751(4) . ? C2 N3 1.292(5) . ? C2 S1 1.719(5) . ? C2 H14 0.9500 . ? C3 C4 1.387(6) . ? C3 C8 1.392(6) . ? C3 P1 1.810(5) . ? C4 C5 1.382(7) . ? C4 H2 0.9500 . ? C5 C6 1.369(8) . ? C5 H3 0.9500 . ? C6 C7 1.367(7) . ? C6 H4 0.9500 . ? C7 C8 1.389(6) . ? C7 H5 0.9500 . ? C8 H6 0.9500 . ? C9 C10 1.389(6) . ? C9 C14 1.399(6) . ? C9 P1 1.808(4) . ? C10 C11 1.391(6) . ? C10 H8 0.9500 . ? C11 C12 1.364(7) . ? C11 H9 0.9500 . ? C12 C13 1.392(7) . ? C12 H10 0.9500 . ? C13 C14 1.395(6) . ? C13 H11 0.9500 . ? C14 H12 0.9500 . ? C15 N4 1.291(5) . ? C15 N5 1.371(5) . ? C15 S2 1.754(5) . ? C16 N6 1.298(6) . ? C16 S2 1.715(5) . ? C16 H28 0.9500 . ? C17 C18 1.387(7) . ? C17 C22 1.394(6) . ? C17 P2 1.808(4) . ? C18 C19 1.387(6) . ? C18 H16 0.9500 . ? C19 C20 1.380(7) . ? C19 H17 0.9500 . ? C20 C21 1.368(7) . ? C20 H18 0.9500 . ? C21 C22 1.399(6) . ? C21 H19 0.9500 . ? C22 H20 0.9500 . ? C23 C24 1.376(6) . ? C23 C28 1.405(6) . ? C23 P2 1.804(4) . ? C24 C25 1.391(6) . ? C24 H22 0.9500 . ? C25 C26 1.372(7) . ? C25 H23 0.9500 . ? C26 C27 1.370(7) . ? C26 H24 0.9500 . ? C27 C28 1.381(6) . ? C27 H25 0.9500 . ? C28 H26 0.9500 . ? C29 Cl4 1.716(6) . ? C29 Cl3 1.751(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 N6 Pd1 N3 94.43(13) . . ? N6 Pd1 Cl1 176.67(11) . . ? N3 Pd1 Cl1 88.52(10) . . ? N6 Pd1 Cl2 88.07(10) . . ? N3 Pd1 Cl2 177.04(10) . . ? Cl1 Pd1 Cl2 89.03(4) . . ? N2 Pt1 N5 96.27(14) . . ? N2 Pt1 P2 175.14(11) . . ? N5 Pt1 P2 79.84(10) . . ? N2 Pt1 P1 80.25(10) . . ? N5 Pt1 P1 175.23(10) . . ? P2 Pt1 P1 103.46(4) . . ? C1 N1 P1 113.0(3) . . ? C1 N2 N3 113.3(3) . . ? C1 N2 Pt1 115.1(3) . . ? N3 N2 Pt1 130.3(2) . . ? C2 N3 N2 112.8(4) . . ? C2 N3 Pd1 122.8(3) . . ? N2 N3 Pd1 121.9(2) . . ? C15 N4 P2 112.4(3) . . ? N6 N5 C15 113.4(3) . . ? N6 N5 Pt1 130.3(2) . . ? C15 N5 Pt1 114.2(3) . . ? C16 N6 N5 113.2(4) . . ? C16 N6 Pd1 123.0(3) . . ? N5 N6 Pd1 122.8(3) . . ? N1 P1 C9 104.67(18) . . ? N1 P1 C3 106.4(2) . . ? C9 P1 C3 108.1(2) . . ? N1 P1 Pt1 104.50(14) . . ? C9 P1 Pt1 118.88(14) . . ? C3 P1 Pt1 113.17(13) . . ? N4 P2 C23 106.49(18) . . ? N4 P2 C17 103.0(2) . . ? C23 P2 C17 104.2(2) . . ? N4 P2 Pt1 104.47(14) . . ? C23 P2 Pt1 115.62(14) . . ? C17 P2 Pt1 121.49(13) . . ? C2 S1 C1 88.6(2) . . ? C16 S2 C15 88.9(2) . . ? C4 C3 C8 118.7(5) . . ? C4 C3 P1 118.8(4) . . ? C8 C3 P1 121.6(3) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H2 119.9 . . ? C3 C4 H2 119.9 . . ? C6 C5 C4 120.5(5) . . ? C6 C5 H3 119.7 . . ? C4 C5 H3 119.7 . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H4 120.0 . . ? C5 C6 H4 120.0 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H5 119.8 . . ? C8 C7 H5 119.8 . . ? C7 C8 C3 120.1(5) . . ? C7 C8 H6 119.9 . . ? C3 C8 H6 119.9 . . ? C10 C9 C14 120.5(4) . . ? C10 C9 P1 120.5(3) . . ? C14 C9 P1 118.4(3) . . ? C9 C10 C11 119.0(4) . . ? C9 C10 H8 120.5 . . ? C11 C10 H8 120.5 . . ? C12 C11 C10 120.8(5) . . ? C12 C11 H9 119.6 . . ? C10 C11 H9 119.6 . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H10 119.5 . . ? C13 C12 H10 119.5 . . ? C12 C13 C14 119.2(5) . . ? C12 C13 H11 120.4 . . ? C14 C13 H11 120.4 . . ? C13 C14 C9 119.5(4) . . ? C13 C14 H12 120.3 . . ? C9 C14 H12 120.3 . . ? N1 C1 N2 126.0(4) . . ? N1 C1 S1 123.5(3) . . ? N2 C1 S1 110.5(3) . . ? N3 C2 S1 114.8(4) . . ? N3 C2 H14 122.6 . . ? S1 C2 H14 122.6 . . ? C18 C17 C22 119.9(4) . . ? C18 C17 P2 121.2(4) . . ? C22 C17 P2 118.8(4) . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H16 120.2 . . ? C17 C18 H16 120.2 . . ? C20 C19 C18 120.6(5) . . ? C20 C19 H17 119.7 . . ? C18 C19 H17 119.7 . . ? C19 C20 C21 120.2(5) . . ? C19 C20 H18 119.9 . . ? C21 C20 H18 119.9 . . ? C20 C21 C22 120.3(5) . . ? C20 C21 H19 119.9 . . ? C20 C21 H19 119.9 . . ? C17 C22 C21 119.5(5) . . ? C17 C22 H20 120.3 . . ? C21 C22 H20 120.3 . . ? C24 C23 C28 118.7(4) . . ? C24 C23 P2 122.9(3) . . ? C28 C23 P2 118.4(3) . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H22 119.9 . . ? C25 C24 H22 119.9 . . ? C26 C25 C24 120.5(5) . . ? C26 C25 H23 119.8 . . ? C24 C25 H23 119.8 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H24 119.9 . . ? C25 C26 H24 119.9 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H25 120.0 . . ? C28 C27 H25 120.0 . . ? C27 C28 C23 120.4(4) . . ? C27 C28 H26 119.8 . . ? C23 C28 H26 119.8 . . ? N4 C15 N5 126.2(4) . . ? N4 C15 S2 123.9(3) . . ? N5 C15 S2 109.9(3) . . ? N6 C16 S2 114.5(4) . . ? N6 C16 H28 122.7 . . ? S2 C16 H28 122.7 . . ? Cl4 C29 Cl3 112.8(3) . . ? Cl4 C29 H29A 109.0 . . ? Cl3 C29 H29A 109.0 . . ? Cl4 C29 H29B 109.0 . . ? Cl3 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.697 _refine_diff_density_min -2.276 _refine_diff_density_rms 0.190 # Attachment '- compound4b.cif' data_compound4b _database_code_depnum_ccdc_archive 'CCDC 801709' #TrackingRef '- compound4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H22 Cl2 N6 P2 Pd Pt S2, 0.5(C7 H8) ' _chemical_formula_sum 'C31.50 H26 Cl2 N6 P2 Pd Pt S2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 987.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9144(3) _cell_length_b 13.1141(3) _cell_length_c 13.9616(3) _cell_angle_alpha 111.536(1) _cell_angle_beta 102.871(1) _cell_angle_gamma 91.897(1) _cell_volume 1632.85(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4556 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 5.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11407 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7496 _reflns_number_gt 5068 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A molecule of toluene was found disordered over two positions around the symmetry center. This was refined with restrained anisotropic parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7496 _refine_ls_number_parameters 431 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.79034(5) 0.27119(4) 0.26407(4) 0.01965(14) Uani 1 1 d . . . Pt1 Pt 0.70589(3) 0.45812(2) 0.09865(2) 0.02544(10) Uani 1 1 d . . . P1 P 0.9805(2) 0.18318(15) 0.28579(14) 0.0249(4) Uani 1 1 d . . . P2 P 0.6767(2) 0.24808(16) 0.38018(14) 0.0259(4) Uani 1 1 d . . . N1 N 1.0493(6) 0.1809(5) 0.1869(4) 0.0275(14) Uani 1 1 d . . . N2 N 0.8756(6) 0.2899(5) 0.1474(4) 0.0240(14) Uani 1 1 d . . . N3 N 0.8292(6) 0.3338(5) 0.0719(4) 0.0261(14) Uani 1 1 d . . . N4 N 0.5213(7) 0.2879(5) 0.3466(5) 0.0343(16) Uani 1 1 d . . . N5 N 0.6150(6) 0.3447(5) 0.2286(4) 0.0266(14) Uani 1 1 d . . . N6 N 0.5714(6) 0.3830(4) 0.1506(4) 0.0216(13) Uani 1 1 d . . . Cl1 Cl 0.8433(2) 0.54757(16) 0.03570(15) 0.0349(5) Uani 1 1 d . . . Cl2 Cl 0.5830(2) 0.60668(14) 0.13463(14) 0.0312(4) Uani 1 1 d . . . S1 S 1.0224(2) 0.22552(17) 0.01115(14) 0.0339(5) Uani 1 1 d . . . S2 S 0.3529(2) 0.35184(18) 0.20461(16) 0.0365(5) Uani 1 1 d . . . C1 C 0.9819(8) 0.2308(6) 0.1284(5) 0.0266(17) Uani 1 1 d . . . C2 C 0.8941(8) 0.3073(6) -0.0019(6) 0.0323(19) Uani 1 1 d . . . H2 H 0.8726 0.3312 -0.0594 0.039 Uiso 1 1 calc R . . C3 C 1.1120(8) 0.2556(6) 0.4085(5) 0.0254(16) Uani 1 1 d . . . C4 C 1.2021(8) 0.3420(6) 0.4140(6) 0.0324(18) Uani 1 1 d . . . H4 H 1.1961 0.3595 0.3530 0.039 Uiso 1 1 calc R . . C5 C 1.2992(9) 0.4020(7) 0.5065(6) 0.039(2) Uani 1 1 d . . . H5 H 1.3614 0.4604 0.5093 0.047 Uiso 1 1 calc R . . C6 C 1.3076(8) 0.3783(6) 0.5957(6) 0.037(2) Uani 1 1 d . . . H6 H 1.3757 0.4198 0.6598 0.044 Uiso 1 1 calc R . . C7 C 1.2181(9) 0.2954(6) 0.5919(6) 0.036(2) Uani 1 1 d . . . H7 H 1.2233 0.2803 0.6541 0.043 Uiso 1 1 calc R . . C8 C 1.1194(8) 0.2325(6) 0.4988(6) 0.0339(19) Uani 1 1 d . . . H8 H 1.0577 0.1743 0.4968 0.041 Uiso 1 1 calc R . . C9 C 0.9635(8) 0.0407(6) 0.2717(5) 0.0297(18) Uani 1 1 d . . . C10 C 1.0862(9) -0.0047(7) 0.2985(6) 0.041(2) Uani 1 1 d . . . H10 H 1.1741 0.0400 0.3268 0.049 Uiso 1 1 calc R . . C11 C 1.0768(11) -0.1159(7) 0.2831(6) 0.046(2) Uani 1 1 d . . . H11 H 1.1589 -0.1471 0.3015 0.055 Uiso 1 1 calc R . . C12 C 0.9514(12) -0.1803(7) 0.2419(7) 0.051(3) Uani 1 1 d . . . H12 H 0.9462 -0.2557 0.2332 0.061 Uiso 1 1 calc R . . C13 C 0.8315(11) -0.1369(7) 0.2124(6) 0.049(2) Uani 1 1 d . . . H13 H 0.7443 -0.1825 0.1818 0.058 Uiso 1 1 calc R . . C14 C 0.8399(9) -0.0254(6) 0.2279(6) 0.039(2) Uani 1 1 d . . . H14 H 0.7576 0.0047 0.2075 0.047 Uiso 1 1 calc R . . C15 C 0.5103(8) 0.3245(6) 0.2696(5) 0.0276(17) Uani 1 1 d . . . C16 C 0.4412(9) 0.3928(6) 0.1294(6) 0.036(2) Uani 1 1 d . . . H16 H 0.3978 0.4199 0.0773 0.043 Uiso 1 1 calc R . . C17 C 0.7510(8) 0.3264(6) 0.5204(5) 0.0264(17) Uani 1 1 d . . . C18 C 0.6759(9) 0.3205(6) 0.5926(6) 0.037(2) Uani 1 1 d . . . H18 H 0.5866 0.2780 0.5669 0.045 Uiso 1 1 calc R . . C19 C 0.7309(11) 0.3763(7) 0.7011(7) 0.051(3) Uani 1 1 d . . . H19 H 0.6786 0.3737 0.7497 0.061 Uiso 1 1 calc R . . C20 C 0.8627(10) 0.4357(7) 0.7384(6) 0.050(3) Uani 1 1 d . . . H20 H 0.9022 0.4717 0.8128 0.060 Uiso 1 1 calc R . . C21 C 0.9370(10) 0.4430(7) 0.6681(6) 0.047(3) Uani 1 1 d . . . H21 H 1.0265 0.4852 0.6938 0.057 Uiso 1 1 calc R . . C22 C 0.8799(9) 0.3878(6) 0.5595(6) 0.039(2) Uani 1 1 d . . . H22 H 0.9313 0.3928 0.5112 0.047 Uiso 1 1 calc R . . C23 C 0.6297(8) 0.1114(6) 0.3739(5) 0.0301(18) Uani 1 1 d . . . C24 C 0.7092(9) 0.0690(6) 0.4426(6) 0.038(2) Uani 1 1 d . . . H24 H 0.7894 0.1125 0.4955 0.045 Uiso 1 1 calc R . . C25 C 0.6702(11) -0.0370(7) 0.4329(7) 0.049(2) Uani 1 1 d . . . H25 H 0.7227 -0.0656 0.4809 0.059 Uiso 1 1 calc R . . C26 C 0.5571(11) -0.1016(8) 0.3551(7) 0.054(3) Uani 1 1 d . . . H26 H 0.5334 -0.1754 0.3478 0.065 Uiso 1 1 calc R . . C27 C 0.4785(10) -0.0601(7) 0.2883(7) 0.055(3) Uani 1 1 d . . . H27 H 0.3990 -0.1043 0.2351 0.066 Uiso 1 1 calc R . . C28 C 0.5151(9) 0.0475(7) 0.2980(6) 0.044(2) Uani 1 1 d . . . H28 H 0.4599 0.0766 0.2516 0.053 Uiso 1 1 calc R . . C29 C 0.6660(14) 0.010(2) -0.0273(14) 0.085(7) Uani 0.50 1 d PGU A -1 H29 H 0.7559 0.0136 -0.0401 0.102 Uiso 0.50 1 calc PR A -1 C30 C 0.590(2) 0.0990(19) -0.0189(13) 0.081(6) Uani 0.50 1 d PGU A -1 H30 H 0.6274 0.1626 -0.0260 0.097 Uiso 0.50 1 calc PR A -1 C31 C 0.458(2) 0.0944(14) -0.0001(13) 0.064(5) Uani 0.50 1 d PGU A -1 H31 H 0.4060 0.1549 0.0056 0.077 Uiso 0.50 1 calc PR A -1 C32 C 0.4030(13) 0.0014(16) 0.0104(13) 0.058(5) Uani 0.50 1 d PGU A -1 C33 C 0.4793(18) -0.0871(14) 0.0020(13) 0.064(5) Uani 0.50 1 d PGU A -1 H33 H 0.4416 -0.1507 0.0092 0.077 Uiso 0.50 1 calc PR A -1 C34 C 0.6109(18) -0.0826(19) -0.0168(14) 0.083(6) Uani 0.50 1 d PGU A -1 H34 H 0.6630 -0.1431 -0.0225 0.099 Uiso 0.50 1 calc PR A -1 C35 C 0.265(3) 0.005(2) 0.0389(17) 0.079(8) Uani 0.50 1 d P A -1 H35A H 0.2616 0.0783 0.0908 0.118 Uiso 0.50 1 calc PR A -1 H35B H 0.2545 -0.0505 0.0697 0.118 Uiso 0.50 1 calc PR A -1 H35C H 0.1893 -0.0121 -0.0253 0.118 Uiso 0.50 1 calc PR A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0192(3) 0.0235(3) 0.0195(3) 0.0120(2) 0.0045(2) 0.0035(2) Pt1 0.02433(17) 0.02937(17) 0.02560(16) 0.01584(13) 0.00319(12) 0.00211(12) P1 0.0240(11) 0.0302(11) 0.0252(9) 0.0157(8) 0.0059(8) 0.0069(8) P2 0.0266(11) 0.0305(11) 0.0254(9) 0.0155(8) 0.0072(8) 0.0054(8) N1 0.029(4) 0.038(4) 0.027(3) 0.019(3) 0.017(3) 0.012(3) N2 0.025(4) 0.030(3) 0.023(3) 0.016(3) 0.006(3) 0.007(3) N3 0.026(4) 0.036(4) 0.023(3) 0.020(3) 0.002(3) 0.008(3) N4 0.030(4) 0.045(4) 0.040(4) 0.026(3) 0.013(3) 0.011(3) N5 0.026(4) 0.031(3) 0.026(3) 0.016(3) 0.003(3) 0.005(3) N6 0.019(3) 0.025(3) 0.025(3) 0.013(3) 0.005(2) 0.003(2) Cl1 0.0295(11) 0.0407(11) 0.0457(11) 0.0292(9) 0.0099(9) 0.0021(9) Cl2 0.0341(11) 0.0284(10) 0.0323(9) 0.0143(8) 0.0061(8) 0.0056(8) S1 0.0393(13) 0.0442(12) 0.0306(10) 0.0226(9) 0.0175(9) 0.0140(10) S2 0.0243(11) 0.0513(13) 0.0464(11) 0.0319(10) 0.0103(9) 0.0088(9) C1 0.022(4) 0.036(4) 0.023(3) 0.013(3) 0.007(3) 0.001(3) C2 0.035(5) 0.043(5) 0.030(4) 0.024(4) 0.012(4) 0.004(4) C3 0.022(4) 0.028(4) 0.031(4) 0.011(3) 0.015(3) 0.012(3) C4 0.034(5) 0.036(4) 0.033(4) 0.019(4) 0.009(4) 0.000(4) C5 0.036(5) 0.036(5) 0.044(5) 0.014(4) 0.008(4) -0.004(4) C6 0.027(5) 0.040(5) 0.035(4) 0.009(4) 0.000(4) 0.006(4) C7 0.038(5) 0.042(5) 0.028(4) 0.017(4) 0.005(4) 0.000(4) C8 0.026(4) 0.036(4) 0.038(4) 0.018(4) 0.000(4) -0.006(3) C9 0.039(5) 0.030(4) 0.027(4) 0.016(3) 0.012(3) 0.010(4) C10 0.047(6) 0.041(5) 0.032(4) 0.016(4) 0.002(4) 0.013(4) C11 0.065(7) 0.034(5) 0.044(5) 0.019(4) 0.013(5) 0.021(5) C12 0.095(9) 0.029(5) 0.042(5) 0.019(4) 0.035(5) 0.010(5) C13 0.061(7) 0.048(6) 0.032(4) 0.004(4) 0.022(4) -0.009(5) C14 0.044(6) 0.035(5) 0.038(4) 0.017(4) 0.004(4) -0.006(4) C15 0.028(4) 0.028(4) 0.026(4) 0.010(3) 0.004(3) 0.005(3) C16 0.033(5) 0.041(5) 0.055(5) 0.036(4) 0.021(4) 0.018(4) C17 0.032(5) 0.025(4) 0.029(4) 0.013(3) 0.016(3) 0.010(3) C18 0.045(5) 0.035(5) 0.036(4) 0.016(4) 0.014(4) 0.011(4) C19 0.073(8) 0.053(6) 0.039(5) 0.025(5) 0.023(5) 0.019(5) C20 0.055(7) 0.051(6) 0.029(4) 0.008(4) -0.009(4) 0.020(5) C21 0.054(6) 0.043(5) 0.027(4) -0.002(4) 0.000(4) 0.019(5) C22 0.043(5) 0.037(5) 0.037(4) 0.012(4) 0.013(4) 0.010(4) C23 0.036(5) 0.041(5) 0.022(3) 0.015(3) 0.018(3) 0.007(4) C24 0.044(5) 0.031(4) 0.039(4) 0.017(4) 0.006(4) 0.004(4) C25 0.067(7) 0.044(5) 0.043(5) 0.026(4) 0.013(5) 0.006(5) C26 0.072(8) 0.048(6) 0.058(6) 0.028(5) 0.033(5) 0.005(5) C27 0.046(6) 0.047(6) 0.064(6) 0.022(5) -0.002(5) -0.008(5) C28 0.042(6) 0.047(5) 0.046(5) 0.027(4) 0.000(4) -0.001(4) C29 0.080(15) 0.096(10) 0.045(8) -0.009(8) 0.011(10) -0.011(10) C30 0.080(14) 0.090(9) 0.048(8) 0.001(8) 0.014(9) -0.024(10) C31 0.066(14) 0.073(8) 0.038(7) 0.004(7) 0.018(8) -0.022(9) C32 0.061(13) 0.070(8) 0.032(7) 0.007(7) 0.011(8) -0.007(9) C33 0.065(14) 0.072(8) 0.036(7) -0.001(7) 0.011(8) -0.002(9) C34 0.078(14) 0.090(9) 0.045(8) -0.010(8) 0.012(9) -0.004(10) C35 0.09(2) 0.11(2) 0.040(11) 0.030(12) 0.006(12) 0.028(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pd1 N5 2.068(5) . ? Pd1 N2 2.079(6) . ? Pd1 P1 2.2639(19) . ? Pd1 P2 2.267(2) . ? Pt1 N6 2.036(6) . ? Pt1 N3 2.045(6) . ? Pt1 Cl1 2.278(2) . ? Pt1 Cl2 2.2900(18) . ? P1 N1 1.662(6) . ? P1 C9 1.804(7) . ? P1 C3 1.807(7) . ? P2 N4 1.666(6) . ? P2 C23 1.803(8) . ? P2 C17 1.805(7) . ? N1 C1 1.311(8) . ? N2 C1 1.345(9) . ? N2 N3 1.379(7) . ? N3 C2 1.281(9) . ? N4 C15 1.315(9) . ? N5 N6 1.352(7) . ? N5 C15 1.355(10) . ? N6 C16 1.280(9) . ? S1 C2 1.712(8) . ? S1 C1 1.748(7) . ? S2 C16 1.718(8) . ? S2 C15 1.741(7) . ? C2 H2 0.9500 . ? C3 C4 1.388(10) . ? C3 C8 1.389(10) . ? C4 C5 1.365(10) . ? C4 H4 0.9500 . ? C5 C6 1.377(11) . ? C5 H5 0.9500 . ? C6 C7 1.357(11) . ? C6 H6 0.9500 . ? C7 C8 1.386(10) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.354(11) . ? C9 C10 1.408(10) . ? C10 C11 1.390(11) . ? C10 H10 0.9500 . ? C11 C12 1.358(13) . ? C11 H11 0.9500 . ? C12 C13 1.380(13) . ? C12 H12 0.9500 . ? C13 C14 1.394(11) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.371(11) . ? C17 C18 1.402(11) . ? C18 C19 1.385(11) . ? C18 H18 0.9500 . ? C19 C20 1.385(13) . ? C19 H19 0.9500 . ? C20 C21 1.378(13) . ? C20 H20 0.9500 . ? C21 C22 1.389(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.365(11) . ? C23 C24 1.390(9) . ? C24 C25 1.379(11) . ? C24 H24 0.9500 . ? C25 C26 1.369(12) . ? C25 H25 0.9500 . ? C26 C27 1.361(11) . ? C26 H26 0.9500 . ? C27 C28 1.394(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 C35 1.50(3) . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 N5 Pd1 N2 94.7(2) . . ? N5 Pd1 P1 174.46(16) . . ? N2 Pd1 P1 80.91(16) . . ? N5 Pd1 P2 80.72(18) . . ? N2 Pd1 P2 174.42(16) . . ? P1 Pd1 P2 103.42(7) . . ? N6 Pt1 N3 94.7(2) . . ? N6 Pt1 Cl1 175.90(15) . . ? N3 Pt1 Cl1 88.82(18) . . ? N6 Pt1 Cl2 88.46(16) . . ? N3 Pt1 Cl2 175.63(17) . . ? Cl1 Pt1 Cl2 88.19(7) . . ? N1 P1 C9 103.9(3) . . ? N1 P1 C3 107.1(3) . . ? C9 P1 C3 105.7(3) . . ? N1 P1 Pd1 103.6(2) . . ? C9 P1 Pd1 121.1(3) . . ? C3 P1 Pd1 114.3(2) . . ? N4 P2 C23 102.1(4) . . ? N4 P2 C17 107.9(3) . . ? C23 P2 C17 103.4(3) . . ? N4 P2 Pd1 103.7(2) . . ? C23 P2 Pd1 120.3(2) . . ? C17 P2 Pd1 117.8(3) . . ? C1 N1 P1 113.8(5) . . ? C1 N2 N3 112.4(6) . . ? C1 N2 Pd1 114.0(4) . . ? N3 N2 Pd1 132.3(5) . . ? C2 N3 N2 113.4(6) . . ? C2 N3 Pt1 123.8(5) . . ? N2 N3 Pt1 121.1(4) . . ? C15 N4 P2 113.1(6) . . ? N6 N5 C15 112.5(5) . . ? N6 N5 Pd1 130.7(5) . . ? C15 N5 Pd1 114.0(4) . . ? C16 N6 N5 115.1(6) . . ? C16 N6 Pt1 120.5(5) . . ? N5 N6 Pt1 122.5(4) . . ? C2 S1 C1 87.9(4) . . ? C16 S2 C15 88.6(4) . . ? N1 C1 N2 126.6(7) . . ? N1 C1 S1 122.0(6) . . ? N2 C1 S1 111.4(5) . . ? N3 C2 S1 114.9(5) . . ? N3 C2 H2 122.5 . . ? S1 C2 H2 122.5 . . ? C4 C3 C8 119.3(7) . . ? C4 C3 P1 118.4(5) . . ? C8 C3 P1 122.2(6) . . ? C5 C4 C3 120.4(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.3(8) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 119.9(7) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 121.1(7) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C3 119.0(7) . . ? C7 C8 H8 120.5 . . ? C3 C8 H8 120.5 . . ? C14 C9 C10 119.5(7) . . ? C14 C9 P1 122.4(6) . . ? C10 C9 P1 117.8(6) . . ? C11 C10 C9 119.0(8) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 120.6(8) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.5(8) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.3(9) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C9 C14 C13 121.0(8) . . ? C9 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? N4 C15 N5 126.3(6) . . ? N4 C15 S2 123.1(6) . . ? N5 C15 S2 110.6(5) . . ? N6 C16 S2 113.2(5) . . ? N6 C16 H16 123.4 . . ? S2 C16 H16 123.4 . . ? C22 C17 C18 118.6(7) . . ? C22 C17 P2 122.9(6) . . ? C18 C17 P2 118.5(6) . . ? C19 C18 C17 120.5(9) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.6(9) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.4(8) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.4(9) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C17 C22 C21 121.5(9) . . ? C17 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C28 C23 C24 119.6(7) . . ? C28 C23 P2 118.8(6) . . ? C24 C23 P2 121.6(6) . . ? C25 C24 C23 119.2(8) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 121.0(8) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 119.9(9) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.9(9) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C23 C28 C27 120.4(7) . . ? C23 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C34 120.0 . . ? C30 C29 H29 120.0 . . ? C34 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 C35 117.6(17) . . ? C33 C32 C35 122.2(17) . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.083 _refine_diff_density_min -2.195 _refine_diff_density_rms 0.228 # Attachment '- compound5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 801710' #TrackingRef '- compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H22 Au2 Cl2 N6 P2 Pt S2,4(C H Cl3)' _chemical_formula_sum 'C32 H26 Au2 Cl14 N6 P2 Pt S2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1705.97 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' Au Au -2.0133 8.8022 '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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9741(5) _cell_length_b 13.6758(9) _cell_length_c 17.5503(9) _cell_angle_alpha 89.302(5) _cell_angle_beta 73.211(5) _cell_angle_gamma 80.247(2) _cell_volume 2483.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18289 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 9.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.486 _exptl_absorpt_process_details 'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28663 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 30.04 _reflns_number_total 14475 _reflns_number_gt 10108 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. one of the chloroform molecules was found disordered in two positions with equal occupancy factors with no atoms in common. A chloroform molecule was disordered in two positions with no atom in common and with equal occupancy factors. The disorder was modelled unrestrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14475 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.11010(2) 0.776400(16) 0.232112(12) 0.02500(6) Uani 1 1 d . . . Au1 Au 0.22797(3) 0.94795(2) -0.031277(14) 0.04454(9) Uani 1 1 d . . . Au2 Au 0.17027(2) 0.681348(18) 0.503417(13) 0.03206(7) Uani 1 1 d . . . P1 P 0.22971(16) 0.86479(12) 0.14121(8) 0.0293(3) Uani 1 1 d . . . P2 P 0.20540(15) 0.78269(11) 0.32893(8) 0.0261(3) Uani 1 1 d . . . S1 S -0.0210(2) 0.8101(2) 0.01012(11) 0.0601(6) Uani 1 1 d . . . S2 S -0.06619(19) 0.60343(15) 0.44387(11) 0.0462(4) Uani 1 1 d . . . N1 N 0.1567(6) 0.8749(4) 0.0675(3) 0.0354(13) Uani 1 1 d . . . N2 N 0.0205(5) 0.7707(4) 0.1438(3) 0.0329(12) Uani 1 1 d . . . N3 N -0.0803(6) 0.7227(5) 0.1431(3) 0.0491(16) Uani 1 1 d . . . N4 N 0.1285(5) 0.7096(4) 0.4000(3) 0.0296(11) Uani 1 1 d . . . N5 N 0.0000(5) 0.6938(4) 0.3149(3) 0.0319(11) Uani 1 1 d . . . N6 N -0.1017(5) 0.6498(4) 0.3085(3) 0.0412(13) Uani 1 1 d . . . C1 C 0.0613(6) 0.8221(5) 0.0776(3) 0.0357(15) Uani 1 1 d . . . C2 C -0.1110(8) 0.7370(7) 0.0786(4) 0.063(2) Uani 1 1 d . . . H2 H -0.1789 0.7094 0.0685 0.075 Uiso 1 1 calc R . . C3 C 0.2277(7) 0.9910(5) 0.1692(3) 0.0388(16) Uani 1 1 d . . . C4 C 0.1158(8) 1.0607(5) 0.1759(4) 0.0468(18) Uani 1 1 d . . . H4 H 0.0464 1.0430 0.1600 0.056 Uiso 1 1 calc R . . C5 C 0.1067(11) 1.1562(6) 0.2060(5) 0.066(3) Uani 1 1 d . . . H5 H 0.0294 1.2029 0.2126 0.079 Uiso 1 1 calc R . . C6 C 0.2085(11) 1.1836(6) 0.2263(5) 0.065(3) Uani 1 1 d . . . H6 H 0.2027 1.2499 0.2444 0.078 Uiso 1 1 calc R . . C7 C 0.3192(10) 1.1152(6) 0.2205(4) 0.062(3) Uani 1 1 d . . . H7 H 0.3880 1.1338 0.2365 0.075 Uiso 1 1 calc R . . C8 C 0.3299(8) 1.0194(5) 0.1915(3) 0.0416(17) Uani 1 1 d . . . H8 H 0.4068 0.9728 0.1866 0.050 Uiso 1 1 calc R . . C9 C 0.3941(6) 0.8073(5) 0.0927(3) 0.0344(14) Uani 1 1 d . . . C10 C 0.4309(7) 0.7063(5) 0.0974(4) 0.0396(16) Uani 1 1 d . . . H10 H 0.3746 0.6694 0.1330 0.047 Uiso 1 1 calc R . . C11 C 0.5521(7) 0.6577(6) 0.0493(4) 0.0482(19) Uani 1 1 d . . . H11 H 0.5785 0.5884 0.0528 0.058 Uiso 1 1 calc R . . C12 C 0.6311(7) 0.7119(7) -0.0024(4) 0.052(2) Uani 1 1 d . . . H12 H 0.7109 0.6786 -0.0366 0.062 Uiso 1 1 calc R . . C13 C 0.5984(7) 0.8140(6) -0.0065(4) 0.049(2) Uani 1 1 d . . . H13 H 0.6569 0.8502 -0.0411 0.059 Uiso 1 1 calc R . . C14 C 0.4794(7) 0.8626(6) 0.0404(3) 0.0421(16) Uani 1 1 d . . . H14 H 0.4553 0.9323 0.0377 0.051 Uiso 1 1 calc R . . C15 C 0.0322(6) 0.6755(4) 0.3826(4) 0.0323(14) Uani 1 1 d . . . C16 C -0.1447(7) 0.6000(6) 0.3707(4) 0.0517(19) Uani 1 1 d . . . H16 H -0.2137 0.5642 0.3761 0.062 Uiso 1 1 calc R . . C17 C 0.1857(6) 0.9022(4) 0.3773(3) 0.0264(12) Uani 1 1 d . . . C18 C 0.2578(7) 0.9187(5) 0.4283(3) 0.0376(15) Uani 1 1 d . . . H18 H 0.3224 0.8670 0.4360 0.045 Uiso 1 1 calc R . . C19 C 0.2354(7) 1.0095(5) 0.4673(4) 0.0434(17) Uani 1 1 d . . . H19 H 0.2845 1.0208 0.5019 0.052 Uiso 1 1 calc R . . C20 C 0.1401(7) 1.0851(5) 0.4559(4) 0.0417(16) Uani 1 1 d . . . H20 H 0.1252 1.1480 0.4824 0.050 Uiso 1 1 calc R . . C21 C 0.0680(7) 1.0693(5) 0.4070(4) 0.0411(16) Uani 1 1 d . . . H21 H 0.0025 1.1208 0.4002 0.049 Uiso 1 1 calc R . . C22 C 0.0908(6) 0.9775(5) 0.3670(3) 0.0343(14) Uani 1 1 d . . . H22 H 0.0412 0.9666 0.3327 0.041 Uiso 1 1 calc R . . C23 C 0.3737(6) 0.7277(5) 0.3042(3) 0.0287(13) Uani 1 1 d . . . C24 C 0.4704(6) 0.7845(5) 0.2800(3) 0.0328(14) Uani 1 1 d . . . H24 H 0.4481 0.8548 0.2805 0.039 Uiso 1 1 calc R . . C25 C 0.5984(7) 0.7403(6) 0.2554(4) 0.0412(16) Uani 1 1 d . . . H25 H 0.6639 0.7802 0.2405 0.049 Uiso 1 1 calc R . . C26 C 0.6317(7) 0.6387(6) 0.2524(4) 0.0448(17) Uani 1 1 d . . . H26 H 0.7200 0.6082 0.2342 0.054 Uiso 1 1 calc R . . C27 C 0.5348(8) 0.5799(5) 0.2762(4) 0.0457(18) Uani 1 1 d . . . H27 H 0.5584 0.5097 0.2757 0.055 Uiso 1 1 calc R . . C28 C 0.4057(6) 0.6230(5) 0.3003(3) 0.0353(14) Uani 1 1 d . . . H28 H 0.3400 0.5832 0.3139 0.042 Uiso 1 1 calc R . . C29 C 0.6097(9) 0.2987(6) 0.1326(5) 0.068(3) Uani 1 1 d . . . H29 H 0.6020 0.2370 0.1057 0.081 Uiso 1 1 calc R . . C30 C 0.4509(9) 0.3159(6) 0.4380(5) 0.059(2) Uani 1 1 d . . . H30 H 0.5430 0.3065 0.4044 0.070 Uiso 1 1 calc R . . C31 C 0.7007(7) 0.0177(6) 0.3189(4) 0.0487(18) Uani 1 1 d . . . H31 H 0.6996 0.0292 0.2627 0.058 Uiso 1 1 calc R . . C32A C 0.0663(17) 0.4969(14) 0.1859(10) 0.053(5) Uani 0.50 1 d P A 1 H32A H 0.0038 0.5598 0.2054 0.064 Uiso 0.50 1 calc PR A 1 C32B C 0.0237(19) 0.5072(14) 0.1448(11) 0.064(5) Uani 0.50 1 d P B 2 H32B H -0.0284 0.5729 0.1680 0.076 Uiso 0.50 1 calc PR B 2 Cl1 Cl 0.3156(3) 1.03053(18) -0.13884(10) 0.0708(7) Uani 1 1 d . . . Cl2 Cl 0.2121(2) 0.64748(14) 0.61941(10) 0.0524(5) Uani 1 1 d . . . Cl3 Cl 0.4550(3) 0.3674(2) 0.17141(16) 0.0828(8) Uani 1 1 d . . . Cl4 Cl 0.7066(3) 0.3653(2) 0.06140(16) 0.0893(8) Uani 1 1 d . . . Cl5 Cl 0.6812(3) 0.2635(2) 0.20746(17) 0.0989(9) Uani 1 1 d . . . Cl6 Cl 0.3921(3) 0.44388(18) 0.45487(16) 0.0807(7) Uani 1 1 d . . . Cl7 Cl 0.3626(3) 0.2653(3) 0.38601(19) 0.1047(10) Uani 1 1 d . . . Cl8 Cl 0.4453(3) 0.2573(3) 0.52561(15) 0.1162(13) Uani 1 1 d . . . Cl9 Cl 0.7545(2) 0.11857(15) 0.35330(12) 0.0549(5) Uani 1 1 d . . . Cl10 Cl 0.8044(2) -0.09388(16) 0.32043(14) 0.0641(6) Uani 1 1 d . . . Cl11 Cl 0.5445(2) 0.00983(18) 0.37644(15) 0.0769(7) Uani 1 1 d . . . Cl12 Cl 0.1286(5) 0.4537(3) 0.2594(2) 0.0625(12) Uani 0.50 1 d P A 1 Cl13 Cl -0.0135(7) 0.4124(6) 0.1525(4) 0.0714(17) Uani 0.50 1 d P A 1 Cl14 Cl 0.1931(7) 0.5227(5) 0.0998(3) 0.075(2) Uani 0.50 1 d P A 1 Cl15 Cl 0.1739(9) 0.5054(8) 0.1497(6) 0.147(5) Uani 0.50 1 d P B 2 Cl16 Cl 0.0252(8) 0.5003(5) 0.0419(3) 0.118(3) Uani 0.50 1 d P . 2 Cl17 Cl -0.0570(10) 0.4176(6) 0.1926(5) 0.113(3) Uani 0.50 1 d P B 2 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 0.02530(12) 0.02526(12) 0.02591(11) 0.00018(8) -0.00771(9) -0.00787(9) Au1 0.0585(2) 0.05137(18) 0.02540(13) 0.00482(11) -0.01244(12) -0.01385(15) Au2 0.03674(15) 0.03374(14) 0.02846(12) 0.00498(9) -0.00966(10) -0.01362(11) P1 0.0335(9) 0.0314(9) 0.0232(7) 0.0015(6) -0.0062(6) -0.0096(7) P2 0.0249(8) 0.0280(8) 0.0266(7) 0.0025(6) -0.0064(6) -0.0097(6) S1 0.0448(12) 0.1060(19) 0.0366(9) 0.0018(10) -0.0212(8) -0.0162(12) S2 0.0418(11) 0.0540(11) 0.0524(10) 0.0251(8) -0.0180(8) -0.0282(9) N1 0.045(3) 0.040(3) 0.020(2) 0.004(2) -0.011(2) -0.005(3) N2 0.026(3) 0.044(3) 0.031(3) -0.004(2) -0.010(2) -0.009(2) N3 0.040(4) 0.068(4) 0.044(3) -0.009(3) -0.012(3) -0.022(3) N4 0.027(3) 0.033(3) 0.032(3) 0.011(2) -0.009(2) -0.015(2) N5 0.031(3) 0.028(3) 0.040(3) 0.005(2) -0.012(2) -0.011(2) N6 0.035(3) 0.041(3) 0.057(3) 0.011(3) -0.024(3) -0.018(3) C1 0.027(3) 0.053(4) 0.025(3) -0.008(3) -0.009(2) -0.001(3) C2 0.047(5) 0.105(7) 0.050(5) 0.003(4) -0.023(4) -0.036(5) C3 0.059(5) 0.031(3) 0.022(3) 0.004(2) -0.002(3) -0.013(3) C4 0.059(5) 0.033(4) 0.040(4) -0.005(3) -0.003(3) -0.006(4) C5 0.094(8) 0.036(4) 0.054(5) 0.009(3) -0.008(5) 0.001(5) C6 0.110(9) 0.030(4) 0.053(5) 0.000(3) -0.013(5) -0.027(5) C7 0.104(8) 0.044(5) 0.041(4) 0.006(3) -0.008(4) -0.044(5) C8 0.061(5) 0.041(4) 0.026(3) 0.007(3) -0.008(3) -0.029(4) C9 0.035(4) 0.046(4) 0.024(3) -0.001(3) -0.008(2) -0.013(3) C10 0.043(4) 0.041(4) 0.038(3) -0.001(3) -0.015(3) -0.011(3) C11 0.048(5) 0.049(4) 0.047(4) -0.021(3) -0.017(3) 0.001(4) C12 0.036(4) 0.079(6) 0.036(4) -0.022(4) -0.008(3) 0.000(4) C13 0.038(4) 0.080(6) 0.030(3) -0.002(3) -0.003(3) -0.024(4) C14 0.043(4) 0.053(4) 0.031(3) 0.007(3) -0.008(3) -0.015(3) C15 0.028(3) 0.024(3) 0.043(3) 0.007(2) -0.009(3) -0.003(3) C16 0.047(5) 0.057(5) 0.064(5) 0.024(4) -0.022(4) -0.034(4) C17 0.027(3) 0.025(3) 0.027(3) -0.002(2) -0.005(2) -0.008(2) C18 0.039(4) 0.045(4) 0.033(3) 0.001(3) -0.012(3) -0.015(3) C19 0.047(4) 0.055(5) 0.032(3) -0.008(3) -0.010(3) -0.019(4) C20 0.044(4) 0.040(4) 0.038(4) -0.010(3) -0.002(3) -0.016(3) C21 0.036(4) 0.037(4) 0.041(4) -0.001(3) 0.001(3) -0.002(3) C22 0.037(4) 0.033(3) 0.030(3) -0.003(2) -0.007(3) -0.005(3) C23 0.027(3) 0.035(3) 0.026(3) 0.002(2) -0.008(2) -0.011(3) C24 0.032(4) 0.034(3) 0.033(3) -0.002(2) -0.009(3) -0.009(3) C25 0.030(4) 0.058(5) 0.038(3) -0.004(3) -0.009(3) -0.015(3) C26 0.031(4) 0.053(5) 0.051(4) -0.010(3) -0.016(3) -0.003(3) C27 0.060(5) 0.028(4) 0.053(4) 0.011(3) -0.025(4) -0.007(3) C28 0.028(4) 0.040(4) 0.039(3) 0.003(3) -0.010(3) -0.008(3) C29 0.079(7) 0.048(5) 0.088(6) -0.008(4) -0.041(5) -0.011(5) C30 0.053(5) 0.062(6) 0.056(5) 0.006(4) -0.016(4) 0.003(4) C31 0.041(4) 0.065(5) 0.041(4) -0.003(3) -0.012(3) -0.014(4) C32A 0.026(9) 0.061(12) 0.062(11) -0.012(9) -0.009(8) 0.016(8) C32B 0.050(12) 0.051(11) 0.065(12) 0.007(9) 0.022(9) -0.009(9) Cl1 0.0980(18) 0.0935(17) 0.0323(9) 0.0196(9) -0.0201(10) -0.0469(14) Cl2 0.0781(15) 0.0556(11) 0.0380(9) 0.0122(8) -0.0280(9) -0.0328(10) Cl3 0.0723(17) 0.0864(19) 0.1017(18) -0.0164(14) -0.0469(14) -0.0069(14) Cl4 0.092(2) 0.089(2) 0.0863(17) 0.0081(14) -0.0347(15) 0.0016(16) Cl5 0.103(2) 0.100(2) 0.1025(19) 0.0310(16) -0.0542(18) -0.0020(18) Cl6 0.0763(17) 0.0526(14) 0.1033(18) 0.0088(12) -0.0041(14) -0.0226(12) Cl7 0.088(2) 0.118(3) 0.109(2) -0.0444(18) -0.0262(17) -0.0213(18) Cl8 0.105(2) 0.140(3) 0.0655(15) 0.0379(16) -0.0045(14) 0.047(2) Cl9 0.0603(13) 0.0484(11) 0.0677(12) 0.0013(9) -0.0318(10) -0.0180(10) Cl10 0.0500(12) 0.0543(12) 0.0901(15) -0.0298(11) -0.0327(11) 0.0088(10) Cl11 0.0416(12) 0.0700(16) 0.1093(18) -0.0268(13) -0.0030(12) -0.0144(11) Cl12 0.067(3) 0.047(2) 0.069(3) -0.0094(19) -0.027(2) 0.017(2) Cl13 0.085(5) 0.062(3) 0.076(4) 0.001(3) -0.026(3) -0.034(3) Cl14 0.065(4) 0.051(3) 0.087(4) -0.010(3) 0.010(3) -0.011(2) Cl15 0.078(7) 0.141(9) 0.217(11) -0.122(9) -0.059(8) 0.031(6) Cl16 0.177(7) 0.111(5) 0.057(3) -0.023(3) -0.022(4) -0.017(5) Cl17 0.130(8) 0.047(3) 0.144(8) 0.020(5) -0.009(6) -0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N5 2.063(5) . ? Pt1 N2 2.070(5) . ? Pt1 P1 2.2383(16) . ? Pt1 P2 2.2469(15) . ? Au1 N1 2.014(5) . ? Au1 Cl1 2.2431(19) . ? Au2 N4 2.014(5) . ? Au2 Cl2 2.2394(16) . ? P1 N1 1.700(5) . ? P1 C3 1.795(7) . ? P1 C9 1.801(7) . ? P2 N4 1.707(5) . ? P2 C23 1.800(6) . ? P2 C17 1.803(6) . ? S1 C1 1.708(6) . ? S1 C2 1.743(9) . ? S2 C15 1.720(6) . ? S2 C16 1.746(7) . ? N1 C1 1.339(9) . ? N2 C1 1.353(8) . ? N2 N3 1.382(8) . ? N3 C2 1.275(9) . ? N4 C15 1.337(8) . ? N5 C15 1.342(8) . ? N5 N6 1.387(7) . ? N6 C16 1.292(8) . ? C2 H2 0.9500 . ? C3 C4 1.398(10) . ? C3 C8 1.403(10) . ? C4 C5 1.393(11) . ? C4 H4 0.9500 . ? C5 C6 1.374(13) . ? C5 H5 0.9500 . ? C6 C7 1.381(13) . ? C6 H6 0.9500 . ? C7 C8 1.385(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.381(9) . ? C9 C14 1.420(9) . ? C10 C11 1.409(10) . ? C10 H10 0.9500 . ? C11 C12 1.368(11) . ? C11 H11 0.9500 . ? C12 C13 1.388(11) . ? C12 H12 0.9500 . ? C13 C14 1.386(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.385(8) . ? C17 C18 1.396(8) . ? C18 C19 1.376(9) . ? C18 H18 0.9500 . ? C19 C20 1.397(10) . ? C19 H19 0.9500 . ? C20 C21 1.364(10) . ? C20 H20 0.9500 . ? C21 C22 1.394(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.386(8) . ? C23 C28 1.413(9) . ? C24 C25 1.376(9) . ? C24 H24 0.9500 . ? C25 C26 1.373(10) . ? C25 H25 0.9500 . ? C26 C27 1.406(10) . ? C26 H26 0.9500 . ? C27 C28 1.383(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 Cl5 1.739(9) . ? C29 Cl3 1.743(10) . ? C29 Cl4 1.748(10) . ? C29 H29 1.0000 . ? C30 Cl8 1.715(8) . ? C30 Cl7 1.733(9) . ? C30 Cl6 1.757(8) . ? C30 H30 1.0000 . ? C31 Cl11 1.740(8) . ? C31 Cl10 1.747(8) . ? C31 Cl9 1.766(8) . ? C31 H31 1.0000 . ? C32A Cl12 1.683(18) . ? C32A Cl13 1.76(2) . ? C32A Cl14 1.811(19) . ? C32A H32A 1.0000 . ? C32B Cl15 1.67(2) . ? C32B Cl17 1.704(19) . ? C32B Cl16 1.80(2) . ? C32B H32B 1.0000 . ? Cl16 Cl16 1.717(12) 2_565 ? 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 N5 Pt1 N2 98.4(2) . . ? N5 Pt1 P1 179.38(14) . . ? N2 Pt1 P1 81.13(15) . . ? N5 Pt1 P2 81.11(14) . . ? N2 Pt1 P2 179.42(14) . . ? P1 Pt1 P2 99.33(6) . . ? N1 Au1 Cl1 177.08(17) . . ? N4 Au2 Cl2 178.38(15) . . ? N1 P1 C3 104.2(3) . . ? N1 P1 C9 104.5(3) . . ? C3 P1 C9 108.9(3) . . ? N1 P1 Pt1 103.7(2) . . ? C3 P1 Pt1 117.0(2) . . ? C9 P1 Pt1 116.8(2) . . ? N4 P2 C23 104.9(3) . . ? N4 P2 C17 106.2(3) . . ? C23 P2 C17 107.8(3) . . ? N4 P2 Pt1 103.66(18) . . ? C23 P2 Pt1 116.14(18) . . ? C17 P2 Pt1 116.8(2) . . ? C1 S1 C2 87.1(3) . . ? C15 S2 C16 88.0(3) . . ? C1 N1 P1 114.6(4) . . ? C1 N1 Au1 124.8(4) . . ? P1 N1 Au1 120.3(3) . . ? C1 N2 N3 113.5(5) . . ? C1 N2 Pt1 117.7(4) . . ? N3 N2 Pt1 128.8(4) . . ? C2 N3 N2 111.0(6) . . ? C15 N4 P2 113.6(4) . . ? C15 N4 Au2 122.1(4) . . ? P2 N4 Au2 124.3(3) . . ? C15 N5 N6 114.4(5) . . ? C15 N5 Pt1 117.5(4) . . ? N6 N5 Pt1 128.1(4) . . ? C16 N6 N5 111.2(5) . . ? N1 C1 N2 122.5(5) . . ? N1 C1 S1 125.1(5) . . ? N2 C1 S1 112.3(5) . . ? N3 C2 S1 116.1(6) . . ? N3 C2 H2 122.0 . . ? S1 C2 H2 122.0 . . ? C4 C3 C8 119.2(6) . . ? C4 C3 P1 118.6(6) . . ? C8 C3 P1 122.0(6) . . ? C5 C4 C3 119.5(8) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 120.6(9) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.3(8) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 120.0(9) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C3 120.3(8) . . ? C7 C8 H8 119.9 . . ? C3 C8 H8 119.9 . . ? C10 C9 C14 119.9(6) . . ? C10 C9 P1 119.5(5) . . ? C14 C9 P1 119.9(5) . . ? C9 C10 C11 120.1(7) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 119.0(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 122.1(7) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C14 C13 C12 119.4(7) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 119.5(7) . . ? C13 C14 H14 120.3 . . ? C9 C14 H14 120.3 . . ? N4 C15 N5 124.0(6) . . ? N4 C15 S2 124.4(5) . . ? N5 C15 S2 111.7(5) . . ? N6 C16 S2 114.7(5) . . ? N6 C16 H16 122.6 . . ? S2 C16 H16 122.6 . . ? C22 C17 C18 119.6(6) . . ? C22 C17 P2 118.5(4) . . ? C18 C17 P2 121.8(5) . . ? C19 C18 C17 120.1(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 119.7(6) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.6(6) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.9(7) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C17 C22 C21 120.1(6) . . ? C17 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C28 120.0(6) . . ? C24 C23 P2 121.6(5) . . ? C28 C23 P2 117.9(5) . . ? C25 C24 C23 120.8(6) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 120.1(7) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 119.8(7) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.8(7) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C23 118.4(6) . . ? C27 C28 H28 120.8 . . ? C23 C28 H28 120.8 . . ? Cl5 C29 Cl3 111.4(5) . . ? Cl5 C29 Cl4 110.6(5) . . ? Cl3 C29 Cl4 110.7(5) . . ? Cl5 C29 H29 108.0 . . ? Cl3 C29 H29 108.0 . . ? Cl4 C29 H29 108.0 . . ? Cl8 C30 Cl7 111.1(5) . . ? Cl8 C30 Cl6 111.4(4) . . ? Cl7 C30 Cl6 109.2(5) . . ? Cl8 C30 H30 108.3 . . ? Cl7 C30 H30 108.3 . . ? Cl6 C30 H30 108.3 . . ? Cl11 C31 Cl10 109.9(4) . . ? Cl11 C31 Cl9 110.4(4) . . ? Cl10 C31 Cl9 111.1(4) . . ? Cl11 C31 H31 108.5 . . ? Cl10 C31 H31 108.5 . . ? Cl9 C31 H31 108.5 . . ? Cl12 C32A Cl13 113.3(11) . . ? Cl12 C32A Cl14 110.5(10) . . ? Cl13 C32A Cl14 106.4(9) . . ? Cl12 C32A H32A 108.8 . . ? Cl13 C32A H32A 108.8 . . ? Cl14 C32A H32A 108.8 . . ? Cl15 C32B Cl17 117.6(14) . . ? Cl15 C32B Cl16 109.6(10) . . ? Cl17 C32B Cl16 107.2(12) . . ? Cl15 C32B H32B 107.3 . . ? Cl17 C32B H32B 107.3 . . ? Cl16 C32B H32B 107.3 . . ? Cl16 Cl16 C32B 161.8(10) 2_565 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.530 _refine_diff_density_min -3.618 _refine_diff_density_rms 0.218 # Attachment '- compound6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 801711' #TrackingRef '- compound6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H24 Cl2 N6 P2 Pd Pt S2, 2(B F4)' _chemical_formula_sum 'C28 H24 B2 Cl2 F8 N6 P2 Pd Pt S2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1116.60 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5753(8) _cell_length_b 13.1508(8) _cell_length_c 21.3008(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.351(3) _cell_angle_gamma 90.00 _cell_volume 4079.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7012 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 4.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7937 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7937 _reflns_number_gt 5068 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystals were of poor quality and visibly twinned. In addition, solvent molecules were found badly disordered. Attempts to found the disordered atomic positions failed. A PLATON-SQUEEZE procedure was then applied. The estimation of the missing electron count was 379 in 651 A3. This is consistent with 2 Et2O molecules per asymmetric unit. The procedure resulted in improved refinement parameters. One of the BF4 anions was disordered. Attempts to model the disorder failed. The anion was then refined with restrained anisotropic parameters, B-F distances and F-B-F angles. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7937 _refine_ls_number_parameters 469 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 1.000 324 189 ' ' 2 0.500 0.500 0.500 324 190 ' ' _platon_squeeze_details ; ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C6 C 0.9747(11) 0.0588(11) 0.8662(7) 0.056(4) Uani 1 1 d . . . H6 H 1.0116 0.0755 0.9026 0.068 Uiso 1 1 calc R . . C17 C 0.7347(8) 0.2376(9) 0.7559(6) 0.032(3) Uani 1 1 d . . . C19 C 0.7128(9) 0.2188(12) 0.8661(6) 0.046(4) Uani 1 1 d . . . H19 H 0.6918 0.1801 0.9003 0.056 Uiso 1 1 calc R . . C8 C 0.9571(8) 0.0492(10) 0.7563(6) 0.037(3) Uani 1 1 d . . . H8 H 0.9797 0.0616 0.7159 0.044 Uiso 1 1 calc R . . C18 C 0.7053(9) 0.1789(11) 0.8052(6) 0.047(3) Uani 1 1 d . . . H18 H 0.6806 0.1129 0.7979 0.056 Uiso 1 1 calc R . . C3 C 0.8716(10) -0.0014(9) 0.7616(6) 0.039(3) Uani 1 1 d . . . C12 C 0.9768(12) -0.1347(14) 0.5297(9) 0.078(6) Uani 1 1 d . . . H12 H 1.0097 -0.1585 0.4951 0.093 Uiso 1 1 calc R . . N3 N 0.5511(6) -0.1625(8) 0.6344(4) 0.031(2) Uani 1 1 d . . . C10 C 0.8531(10) -0.0298(11) 0.5709(6) 0.048(3) Uani 1 1 d . . . H10 H 0.8051 0.0183 0.5641 0.057 Uiso 1 1 calc R . . C27 C 0.9393(10) 0.3026(11) 0.6027(7) 0.054(4) Uani 1 1 d . . . H27 H 1.0031 0.3028 0.6138 0.065 Uiso 1 1 calc R . . C13 C 1.0014(10) -0.1667(13) 0.5910(8) 0.058(4) Uani 1 1 d . . . H13 H 1.0515 -0.2120 0.5984 0.070 Uiso 1 1 calc R . . C23 C 0.7872(9) 0.2588(9) 0.6243(6) 0.037(3) Uani 1 1 d . . . C2 C 0.5448(9) -0.2553(10) 0.6507(6) 0.040(3) Uani 1 1 d . . . H2 H 0.4939 -0.2962 0.6374 0.048 Uiso 1 1 calc R . . C26 C 0.9107(10) 0.3447(12) 0.5487(6) 0.051(4) Uani 1 1 d . . . H26 H 0.9536 0.3755 0.5223 0.062 Uiso 1 1 calc R . . C9 C 0.8783(9) -0.0676(9) 0.6303(6) 0.036(3) Uani 1 1 d . . . C28 C 0.8792(10) 0.2584(11) 0.6436(7) 0.050(4) Uani 1 1 d . . . H28 H 0.8998 0.2295 0.6825 0.060 Uiso 1 1 calc R . . C7 C 1.0073(11) 0.0803(12) 0.8082(7) 0.060(4) Uani 1 1 d . . . H7 H 1.0634 0.1160 0.8043 0.072 Uiso 1 1 calc R . . C21 C 0.7793(12) 0.3715(11) 0.8275(6) 0.057(4) Uani 1 1 d . . . H21 H 0.8053 0.4368 0.8351 0.068 Uiso 1 1 calc R . . C22 C 0.7700(10) 0.3338(12) 0.7677(7) 0.055(4) Uani 1 1 d . . . H22 H 0.7882 0.3746 0.7335 0.066 Uiso 1 1 calc R . . C24 C 0.7549(10) 0.2992(12) 0.5663(6) 0.056(4) Uani 1 1 d . . . H24 H 0.6921 0.2959 0.5526 0.067 Uiso 1 1 calc R . . C20 C 0.7500(11) 0.3127(14) 0.8768(7) 0.064(5) Uani 1 1 d . . . H20 H 0.7559 0.3381 0.9186 0.077 Uiso 1 1 calc R . . C16 C 0.3953(8) 0.1011(10) 0.6178(6) 0.038(3) Uani 1 1 d . . . H16 H 0.3348 0.0774 0.6081 0.046 Uiso 1 1 calc R . . C5 C 0.8907(11) 0.0139(11) 0.8737(7) 0.053(4) Uani 1 1 d . . . H5 H 0.8687 0.0061 0.9148 0.063 Uiso 1 1 calc R . . C11 C 0.9059(11) -0.0698(15) 0.5205(7) 0.065(5) Uani 1 1 d . . . H11 H 0.8898 -0.0493 0.4787 0.078 Uiso 1 1 calc R . . C4 C 0.8361(11) -0.0211(11) 0.8211(7) 0.055(4) Uani 1 1 d . . . H4 H 0.7795 -0.0555 0.8257 0.066 Uiso 1 1 calc R . . C15 C 0.5324(8) 0.1911(9) 0.6435(5) 0.030(3) Uani 1 1 d . . . C14 C 0.9517(9) -0.1313(11) 0.6403(7) 0.053(4) Uani 1 1 d . . . H14 H 0.9687 -0.1516 0.6819 0.064 Uiso 1 1 calc R . . C25 C 0.8198(11) 0.3434(15) 0.5314(6) 0.075(5) Uani 1 1 d . . . H25 H 0.8008 0.3750 0.4930 0.090 Uiso 1 1 calc R . . N1 N 0.7633(7) -0.1564(8) 0.7163(4) 0.033(2) Uani 1 1 d . . . H1 H 0.7942 -0.1949 0.7435 0.040 Uiso 1 1 calc R . . C1 C 0.6838(7) -0.1852(8) 0.6908(5) 0.025(2) Uani 1 1 d . . . N2 N 0.6309(7) -0.1186(7) 0.6572(4) 0.030(2) Uani 1 1 d . . . N4 N 0.6026(7) 0.2492(8) 0.6581(4) 0.037(2) Uani 1 1 d . . . H4A H 0.5961 0.3157 0.6587 0.044 Uiso 1 1 calc R . . N6 N 0.4647(7) 0.0434(7) 0.6170(5) 0.034(2) Uani 1 1 d . . . N5 N 0.5452(6) 0.0929(7) 0.6336(4) 0.025(2) Uani 1 1 d . . . P2 P 0.7072(2) 0.1957(2) 0.67613(14) 0.0313(7) Uani 1 1 d . . . P1 P 0.8041(2) -0.0395(2) 0.69371(14) 0.0294(7) Uani 1 1 d . . . S2 S 0.4181(2) 0.2264(3) 0.63788(14) 0.0371(7) Uani 1 1 d . . . S1 S 0.6322(2) -0.3019(2) 0.69722(14) 0.0381(8) Uani 1 1 d . . . Cl1 Cl 0.4649(2) -0.2378(2) 0.51205(14) 0.0418(8) Uani 1 1 d . . . Cl2 Cl 0.3585(2) -0.0252(3) 0.49859(13) 0.0399(7) Uani 1 1 d . . . Pd1 Pd 0.46408(6) -0.09229(7) 0.56952(4) 0.0306(3) Uani 1 1 d . . . Pt1 Pt 0.67134(3) 0.03253(4) 0.660782(19) 0.02740(17) Uani 1 1 d . . . B1 B 0.8391(13) -0.3265(15) 0.8294(8) 0.057(5) Uani 1 1 d . . . B2 B 0.4884(8) 0.4682(8) 0.7030(5) 0.061(5) Uani 1 1 d DU . . F1 F 0.8906(5) -0.2630(6) 0.7926(4) 0.052(2) Uani 1 1 d . . . F2 F 0.7740(7) -0.3720(9) 0.7880(5) 0.098(4) Uani 1 1 d . . . F3 F 0.7889(8) -0.2734(9) 0.8716(5) 0.105(4) Uani 1 1 d . . . F4 F 0.8921(6) -0.4005(7) 0.8581(4) 0.067(2) Uani 1 1 d . . . F8 F 0.4927(7) 0.5634(6) 0.7278(4) 0.079(2) Uani 1 1 d DU . . F6 F 0.5123(8) 0.3921(9) 0.7456(5) 0.125(3) Uani 1 1 d DU . . F7 F 0.5467(7) 0.4586(7) 0.6554(4) 0.101(3) Uani 1 1 d DU . . F5 F 0.3998(7) 0.4466(9) 0.6862(6) 0.130(3) Uani 1 1 d DU . . 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 C6 0.054(10) 0.040(9) 0.073(11) -0.008(8) -0.030(8) -0.010(7) C17 0.024(6) 0.026(6) 0.045(7) -0.006(6) -0.003(5) 0.002(5) C19 0.033(8) 0.064(10) 0.042(8) -0.012(7) -0.004(6) 0.021(7) C8 0.034(7) 0.042(8) 0.033(7) 0.005(6) -0.005(5) 0.001(6) C18 0.039(8) 0.052(9) 0.049(8) -0.003(7) -0.002(6) -0.006(7) C3 0.060(9) 0.024(6) 0.032(7) 0.003(5) -0.007(6) 0.001(6) C12 0.052(11) 0.072(13) 0.111(15) -0.034(11) 0.038(11) -0.021(10) N3 0.024(5) 0.031(6) 0.037(5) -0.003(5) -0.011(4) -0.006(5) C10 0.049(9) 0.051(9) 0.044(8) -0.003(7) 0.008(6) -0.006(7) C27 0.041(9) 0.039(8) 0.081(11) 0.002(8) -0.008(8) -0.004(7) C13 0.032(8) 0.065(11) 0.077(11) 0.005(9) 0.000(7) 0.016(8) C23 0.042(8) 0.022(6) 0.049(8) -0.006(6) 0.010(6) -0.002(6) C2 0.038(8) 0.031(7) 0.050(8) -0.005(6) -0.008(6) 0.004(6) C26 0.056(10) 0.063(10) 0.035(7) -0.006(7) 0.001(7) -0.009(8) C9 0.039(8) 0.027(6) 0.042(7) -0.018(6) -0.001(6) -0.009(6) C28 0.045(9) 0.042(9) 0.064(9) 0.016(7) 0.000(7) -0.012(7) C7 0.070(11) 0.057(10) 0.052(9) 0.012(8) -0.019(8) -0.016(9) C21 0.093(13) 0.032(8) 0.045(9) -0.024(7) -0.004(8) -0.012(8) C22 0.060(10) 0.049(9) 0.055(9) 0.007(7) -0.016(7) -0.010(8) C24 0.047(9) 0.074(11) 0.046(8) 0.014(8) -0.001(7) -0.023(8) C20 0.059(10) 0.076(12) 0.057(10) -0.040(9) -0.011(8) 0.024(9) C16 0.025(7) 0.044(8) 0.046(7) -0.010(6) 0.012(5) -0.007(6) C5 0.068(11) 0.048(9) 0.040(8) -0.011(7) -0.019(7) 0.012(8) C11 0.045(10) 0.100(14) 0.050(9) 0.005(9) 0.014(7) -0.016(10) C4 0.064(10) 0.054(10) 0.045(8) -0.009(7) -0.002(7) 0.014(8) C15 0.027(7) 0.029(7) 0.034(6) 0.002(5) 0.003(5) 0.009(6) C14 0.039(8) 0.055(10) 0.066(9) -0.004(8) 0.014(7) 0.013(7) C25 0.064(11) 0.122(16) 0.037(8) 0.025(9) -0.007(7) -0.028(11) N1 0.034(6) 0.031(6) 0.035(5) 0.000(5) -0.004(4) 0.002(5) C1 0.028(7) 0.020(6) 0.025(6) 0.014(5) -0.003(5) -0.004(5) N2 0.034(6) 0.023(5) 0.035(5) 0.000(4) 0.002(4) -0.001(5) N4 0.033(6) 0.026(6) 0.051(6) 0.005(5) -0.009(5) 0.009(5) N6 0.034(6) 0.030(6) 0.038(6) 0.003(5) 0.002(5) 0.005(5) N5 0.016(5) 0.029(6) 0.031(5) -0.007(4) 0.002(4) -0.001(4) P2 0.0311(18) 0.0253(17) 0.0373(17) -0.0022(13) -0.0022(13) -0.0001(14) P1 0.0291(17) 0.0287(17) 0.0304(16) 0.0004(13) -0.0013(12) 0.0001(14) S2 0.0305(17) 0.0392(19) 0.0413(17) -0.0073(15) -0.0016(13) 0.0053(15) S1 0.043(2) 0.0300(17) 0.0402(17) 0.0071(14) -0.0077(14) -0.0041(15) Cl1 0.047(2) 0.0383(18) 0.0391(17) -0.0057(14) -0.0052(14) -0.0058(15) Cl2 0.0417(18) 0.047(2) 0.0299(15) 0.0029(14) -0.0072(13) 0.0013(16) Pd1 0.0305(5) 0.0313(6) 0.0298(5) -0.0008(4) -0.0018(4) -0.0038(4) Pt1 0.0280(3) 0.0253(3) 0.0287(3) -0.0005(2) -0.00166(18) -0.0007(2) B1 0.057(12) 0.057(12) 0.057(11) 0.014(9) -0.007(9) 0.014(10) B2 0.046(10) 0.070(11) 0.067(10) -0.017(9) 0.012(8) 0.033(9) F1 0.041(4) 0.049(5) 0.066(5) 0.033(4) 0.008(4) -0.001(4) F2 0.070(7) 0.114(9) 0.106(8) 0.041(7) -0.039(6) -0.029(6) F3 0.105(9) 0.096(9) 0.118(9) 0.019(7) 0.051(7) 0.024(7) F4 0.071(6) 0.061(6) 0.069(6) 0.023(5) -0.004(4) 0.006(5) F8 0.089(5) 0.045(4) 0.103(5) -0.010(4) 0.030(4) 0.001(4) F6 0.148(6) 0.086(5) 0.144(6) -0.005(5) 0.043(5) 0.019(5) F7 0.122(6) 0.071(5) 0.112(6) -0.008(5) 0.041(5) 0.011(5) F5 0.136(6) 0.098(6) 0.156(6) -0.039(5) 0.022(5) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C6 C7 1.37(2) . ? C6 C5 1.37(2) . ? C6 H6 0.9500 . ? C17 C22 1.385(18) . ? C17 C18 1.386(17) . ? C17 P2 1.815(12) . ? C19 C20 1.36(2) . ? C19 C18 1.398(17) . ? C19 H19 0.9500 . ? C8 C7 1.363(18) . ? C8 C3 1.422(18) . ? C8 H8 0.9500 . ? C18 H18 0.9500 . ? C3 C4 1.412(19) . ? C3 P1 1.787(13) . ? C12 C11 1.35(2) . ? C12 C13 1.40(2) . ? C12 H12 0.9500 . ? N3 C2 1.273(15) . ? N3 N2 1.370(13) . ? N3 Pd1 2.056(9) . ? C10 C9 1.395(18) . ? C10 C11 1.45(2) . ? C10 H10 0.9500 . ? C27 C26 1.328(19) . ? C27 C28 1.388(19) . ? C27 H27 0.9500 . ? C13 C14 1.381(19) . ? C13 H13 0.9500 . ? C23 C28 1.386(18) . ? C23 C24 1.407(18) . ? C23 P2 1.837(12) . ? C2 S1 1.697(13) . ? C2 H2 0.9500 . ? C26 C25 1.36(2) . ? C26 H26 0.9500 . ? C9 C14 1.369(18) . ? C9 P1 1.802(12) . ? C28 H28 0.9500 . ? C7 H7 0.9500 . ? C21 C22 1.369(18) . ? C21 C20 1.39(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C24 C25 1.36(2) . ? C24 H24 0.9500 . ? C20 H20 0.9500 . ? C16 N6 1.265(15) . ? C16 S2 1.731(13) . ? C16 H16 0.9500 . ? C5 C4 1.424(19) . ? C5 H5 0.9500 . ? C11 H11 0.9500 . ? C4 H4 0.9500 . ? C15 N4 1.305(15) . ? C15 N5 1.323(14) . ? C15 S2 1.728(12) . ? C14 H14 0.9500 . ? C25 H25 0.9500 . ? N1 C1 1.315(14) . ? N1 P1 1.724(10) . ? N1 H1 0.8800 . ? C1 N2 1.352(14) . ? C1 S1 1.716(11) . ? N2 Pt1 2.074(9) . ? N4 P2 1.708(10) . ? N4 H4A 0.8800 . ? N6 N5 1.376(13) . ? N6 Pd1 2.051(10) . ? N5 Pt1 2.063(9) . ? P2 Pt1 2.230(3) . ? P1 Pt1 2.241(3) . ? Cl1 Pd1 2.272(3) . ? Cl2 Pd1 2.288(3) . ? B1 F4 1.370(19) . ? B1 F3 1.37(2) . ? B1 F1 1.39(2) . ? B1 F2 1.40(2) . ? B2 F7 1.354(8) . ? B2 F5 1.355(9) . ? B2 F8 1.360(9) . ? B2 F6 1.386(9) . ? 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 C7 C6 C5 122.4(14) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C22 C17 C18 119.7(12) . . ? C22 C17 P2 120.9(10) . . ? C18 C17 P2 118.5(9) . . ? C20 C19 C18 120.7(14) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C7 C8 C3 121.3(12) . . ? C7 C8 H8 119.3 . . ? C3 C8 H8 119.3 . . ? C17 C18 C19 118.6(14) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C4 C3 C8 120.7(12) . . ? C4 C3 P1 117.8(11) . . ? C8 C3 P1 121.5(9) . . ? C11 C12 C13 119.4(15) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C2 N3 N2 112.1(10) . . ? C2 N3 Pd1 124.4(8) . . ? N2 N3 Pd1 122.8(7) . . ? C9 C10 C11 114.6(14) . . ? C9 C10 H10 122.7 . . ? C11 C10 H10 122.7 . . ? C26 C27 C28 122.2(14) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C14 C13 C12 118.9(14) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C28 C23 C24 123.2(12) . . ? C28 C23 P2 116.7(10) . . ? C24 C23 P2 120.0(10) . . ? N3 C2 S1 116.4(10) . . ? N3 C2 H2 121.8 . . ? S1 C2 H2 121.8 . . ? C27 C26 C25 119.8(14) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C14 C9 C10 122.2(12) . . ? C14 C9 P1 119.9(10) . . ? C10 C9 P1 117.6(10) . . ? C23 C28 C27 116.1(13) . . ? C23 C28 H28 121.9 . . ? C27 C28 H28 121.9 . . ? C8 C7 C6 118.4(14) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C22 C21 C20 118.8(14) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C17 121.5(14) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? C25 C24 C23 115.2(14) . . ? C25 C24 H24 122.4 . . ? C23 C24 H24 122.4 . . ? C19 C20 C21 120.7(13) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? N6 C16 S2 115.4(10) . . ? N6 C16 H16 122.3 . . ? S2 C16 H16 122.3 . . ? C6 C5 C4 121.2(15) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C12 C11 C10 123.4(15) . . ? C12 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C3 C4 C5 115.7(15) . . ? C3 C4 H4 122.1 . . ? C5 C4 H4 122.1 . . ? N4 C15 N5 119.6(10) . . ? N4 C15 S2 127.1(9) . . ? N5 C15 S2 113.2(9) . . ? C9 C14 C13 121.4(14) . . ? C9 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C24 C25 C26 123.4(14) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C1 N1 P1 116.8(8) . . ? C1 N1 H1 121.6 . . ? P1 N1 H1 121.6 . . ? N1 C1 N2 120.3(10) . . ? N1 C1 S1 127.3(8) . . ? N2 C1 S1 112.3(8) . . ? C1 N2 N3 111.8(9) . . ? C1 N2 Pt1 116.6(7) . . ? N3 N2 Pt1 130.7(7) . . ? C15 N4 P2 119.8(9) . . ? C15 N4 H4A 120.1 . . ? P2 N4 H4A 120.1 . . ? C16 N6 N5 112.8(10) . . ? C16 N6 Pd1 122.8(9) . . ? N5 N6 Pd1 121.6(7) . . ? C15 N5 N6 112.1(9) . . ? C15 N5 Pt1 117.5(8) . . ? N6 N5 Pt1 129.2(7) . . ? N4 P2 C17 104.3(5) . . ? N4 P2 C23 105.2(6) . . ? C17 P2 C23 107.7(6) . . ? N4 P2 Pt1 99.3(4) . . ? C17 P2 Pt1 118.1(4) . . ? C23 P2 Pt1 119.8(4) . . ? N1 P1 C3 102.1(5) . . ? N1 P1 C9 104.5(5) . . ? C3 P1 C9 109.7(6) . . ? N1 P1 Pt1 99.3(4) . . ? C3 P1 Pt1 125.1(5) . . ? C9 P1 Pt1 112.9(4) . . ? C15 S2 C16 86.3(6) . . ? C2 S1 C1 87.2(6) . . ? N6 Pd1 N3 94.0(4) . . ? N6 Pd1 Cl1 176.9(3) . . ? N3 Pd1 Cl1 88.1(3) . . ? N6 Pd1 Cl2 88.8(3) . . ? N3 Pd1 Cl2 175.1(3) . . ? Cl1 Pd1 Cl2 89.27(12) . . ? N5 Pt1 N2 96.3(4) . . ? N5 Pt1 P2 82.6(3) . . ? N2 Pt1 P2 173.0(3) . . ? N5 Pt1 P1 176.7(3) . . ? N2 Pt1 P1 81.2(3) . . ? P2 Pt1 P1 99.61(12) . . ? F4 B1 F3 111.9(14) . . ? F4 B1 F1 111.8(14) . . ? F3 B1 F1 112.3(15) . . ? F4 B1 F2 109.4(15) . . ? F3 B1 F2 105.3(15) . . ? F1 B1 F2 105.6(12) . . ? F7 B2 F5 113.8(9) . . ? F7 B2 F8 110.8(8) . . ? F5 B2 F8 108.9(10) . . ? F7 B2 F6 105.9(8) . . ? F5 B2 F6 103.5(8) . . ? F8 B2 F6 113.8(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.197 _refine_diff_density_min -1.993 _refine_diff_density_rms 0.257