Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Hor 'Qingchun Ge' _publ_contact_author_name 'Tzi Sum Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG # Attachment '5197.cif' data_5197 _database_code_depnum_ccdc_archive 'CCDC 620352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C117 H102 Cl10 N2 P8 Pd Ru2' _chemical_formula_weight 2446.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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' P P 0.1023 0.0942 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7826(6) _cell_length_b 11.4946(6) _cell_length_c 24.0888(13) _cell_angle_alpha 94.6910(10) _cell_angle_beta 102.7270(10) _cell_angle_gamma 106.0610(10) _cell_volume 2765.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1818 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.90 _exptl_crystal_description 'Thin Plate' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.9673 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19911 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12637 _reflns_number_gt 7559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0543P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12637 _refine_ls_number_parameters 646 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 1.0000 0.0000 0.5000 0.03113(17) Uani 1 2 d S . . Ru1 Ru 0.28360(4) 0.11218(4) 0.228692(17) 0.01995(11) Uani 1 1 d . . . Cl1 Cl 1.03475(16) -0.13575(15) 0.43365(6) 0.0458(4) Uani 1 1 d . . . Cl2 Cl 0.06181(12) 0.10888(12) 0.17010(5) 0.0287(3) Uani 1 1 d . . . P1 P 0.39473(13) 0.08219(12) 0.15725(6) 0.0227(3) Uani 1 1 d . . . P2 P 0.40546(13) 0.30164(12) 0.21153(6) 0.0241(3) Uani 1 1 d . . . P3 P 0.18085(13) 0.14594(12) 0.30357(6) 0.0238(3) Uani 1 1 d . . . P4 P 0.16623(13) -0.07793(12) 0.24792(6) 0.0238(3) Uani 1 1 d . . . N1 N 0.8594(4) 0.0339(4) 0.43723(19) 0.0320(11) Uani 1 1 d . . . C1 C 0.4518(5) 0.1041(5) 0.2793(2) 0.0234(12) Uani 1 1 d . . . C2 C 0.5522(5) 0.0941(5) 0.3098(2) 0.0300(13) Uani 1 1 d . . . C3 C 0.8420(6) 0.1446(5) 0.4364(2) 0.0345(14) Uani 1 1 d . . . H3 H 0.8979 0.2092 0.4654 0.041 Uiso 1 1 calc R . . C4 C 0.7448(6) 0.1676(5) 0.3947(2) 0.0381(15) Uani 1 1 d . . . H4 H 0.7379 0.2474 0.3953 0.046 Uiso 1 1 calc R . . C5 C 0.6575(5) 0.0750(5) 0.3521(2) 0.0270(12) Uani 1 1 d . . . C6 C 0.6777(6) -0.0394(5) 0.3531(3) 0.0419(16) Uani 1 1 d . . . H6 H 0.6236 -0.1054 0.3245 0.050 Uiso 1 1 calc R . . C7 C 0.7767(6) -0.0564(5) 0.3958(3) 0.0440(17) Uani 1 1 d . . . H7 H 0.7866 -0.1352 0.3959 0.053 Uiso 1 1 calc R . . C8 C 0.5152(5) 0.2358(4) 0.1793(2) 0.0273(12) Uani 1 1 d . . . H8A H 0.5378 0.2744 0.1466 0.033 Uiso 1 1 calc R . . H8B H 0.5965 0.2369 0.2075 0.033 Uiso 1 1 calc R . . C9 C 0.0707(5) -0.0131(5) 0.2903(2) 0.0264(12) Uani 1 1 d . . . H9A H -0.0198 -0.0215 0.2678 0.032 Uiso 1 1 calc R . . H9B H 0.0673 -0.0479 0.3259 0.032 Uiso 1 1 calc R . . C1A C 0.3341(5) 0.0818(5) 0.0799(2) 0.0256(12) Uani 1 1 d . . . C2A C 0.2025(5) 0.0794(5) 0.0571(2) 0.0323(13) Uani 1 1 d . . . H2A H 0.1419 0.0690 0.0804 0.039 Uiso 1 1 calc R . . C3A C 0.1624(6) 0.0923(5) 0.0000(2) 0.0384(15) Uani 1 1 d . . . H3A H 0.0736 0.0898 -0.0158 0.046 Uiso 1 1 calc R . . C4A C 0.2507(6) 0.1087(6) -0.0338(3) 0.0416(16) Uani 1 1 d . . . H4A H 0.2227 0.1194 -0.0723 0.050 Uiso 1 1 calc R . . C5A C 0.3810(7) 0.1096(6) -0.0118(3) 0.0457(17) Uani 1 1 d . . . H5A H 0.4412 0.1196 -0.0352 0.055 Uiso 1 1 calc R . . C6A C 0.4205(6) 0.0955(5) 0.0450(2) 0.0369(14) Uani 1 1 d . . . H6A H 0.5085 0.0953 0.0602 0.044 Uiso 1 1 calc R . . C1B C 0.4903(5) -0.0264(5) 0.1586(2) 0.0242(12) Uani 1 1 d . . . C2B C 0.4216(6) -0.1493(5) 0.1420(3) 0.0359(14) Uani 1 1 d . . . H2B H 0.3280 -0.1745 0.1296 0.043 Uiso 1 1 calc R . . C3B C 0.4889(7) -0.2358(6) 0.1434(3) 0.0466(17) Uani 1 1 d . . . H3B H 0.4409 -0.3193 0.1322 0.056 Uiso 1 1 calc R . . C4B C 0.6269(7) -0.2000(6) 0.1613(3) 0.0452(17) Uani 1 1 d . . . H4B H 0.6723 -0.2591 0.1628 0.054 Uiso 1 1 calc R . . C5B C 0.6970(6) -0.0778(6) 0.1768(2) 0.0426(17) Uani 1 1 d . . . H5B H 0.7907 -0.0529 0.1881 0.051 Uiso 1 1 calc R . . C6B C 0.6289(5) 0.0095(5) 0.1759(2) 0.0345(14) Uani 1 1 d . . . H6B H 0.6770 0.0930 0.1870 0.041 Uiso 1 1 calc R . . C1C C 0.3293(5) 0.3814(5) 0.1580(2) 0.0306(13) Uani 1 1 d . . . C2C C 0.3539(8) 0.3893(6) 0.1041(3) 0.056(2) Uani 1 1 d . . . H2C H 0.4187 0.3571 0.0942 0.067 Uiso 1 1 calc R . . C3C C 0.2833(10) 0.4445(6) 0.0647(3) 0.075(3) Uani 1 1 d . . . H3C H 0.2982 0.4472 0.0278 0.090 Uiso 1 1 calc R . . C4C C 0.1923(8) 0.4946(7) 0.0796(4) 0.073(3) Uani 1 1 d . . . H4C H 0.1463 0.5333 0.0530 0.088 Uiso 1 1 calc R . . C5C C 0.1670(7) 0.4898(7) 0.1321(4) 0.079(3) Uani 1 1 d . . . H5C H 0.1040 0.5247 0.1419 0.094 Uiso 1 1 calc R . . C6C C 0.2351(7) 0.4330(6) 0.1711(3) 0.0551(19) Uani 1 1 d . . . H6C H 0.2172 0.4291 0.2075 0.066 Uiso 1 1 calc R . . C1D C 0.5206(5) 0.4252(5) 0.2672(2) 0.0290(13) Uani 1 1 d . . . C2D C 0.5992(6) 0.5307(5) 0.2541(3) 0.0361(14) Uani 1 1 d . . . H2D H 0.5881 0.5437 0.2155 0.043 Uiso 1 1 calc R . . C3D C 0.6942(6) 0.6179(5) 0.2970(3) 0.0447(17) Uani 1 1 d . . . H3D H 0.7462 0.6900 0.2876 0.054 Uiso 1 1 calc R . . C4D C 0.7120(6) 0.5988(6) 0.3530(3) 0.0502(19) Uani 1 1 d . . . H4D H 0.7796 0.6558 0.3819 0.060 Uiso 1 1 calc R . . C5D C 0.6314(7) 0.4965(6) 0.3673(3) 0.0495(18) Uani 1 1 d . . . H5D H 0.6417 0.4860 0.4062 0.059 Uiso 1 1 calc R . . C6D C 0.5347(6) 0.4083(5) 0.3248(2) 0.0372(15) Uani 1 1 d . . . H6D H 0.4797 0.3384 0.3347 0.045 Uiso 1 1 calc R . . C1E C 0.0768(5) 0.2472(5) 0.2984(2) 0.0253(12) Uani 1 1 d . . . C2E C 0.1392(6) 0.3718(5) 0.3033(3) 0.0409(15) Uani 1 1 d . . . H2E H 0.2321 0.4008 0.3083 0.049 Uiso 1 1 calc R . . C3E C 0.0659(7) 0.4543(6) 0.3009(3) 0.0524(19) Uani 1 1 d . . . H3E H 0.1091 0.5384 0.3035 0.063 Uiso 1 1 calc R . . C4E C -0.0690(6) 0.4136(6) 0.2947(3) 0.0434(16) Uani 1 1 d . . . H4E H -0.1184 0.4695 0.2936 0.052 Uiso 1 1 calc R . . C5E C -0.1314(6) 0.2908(5) 0.2900(2) 0.0355(14) Uani 1 1 d . . . H5E H -0.2242 0.2623 0.2851 0.043 Uiso 1 1 calc R . . C6E C -0.0589(5) 0.2084(5) 0.2925(2) 0.0311(13) Uani 1 1 d . . . H6E H -0.1029 0.1246 0.2902 0.037 Uiso 1 1 calc R . . C1F C 0.2580(5) 0.1740(5) 0.3813(2) 0.0297(13) Uani 1 1 d . . . C2F C 0.2028(7) 0.2219(7) 0.4201(3) 0.0533(19) Uani 1 1 d . . . H2F H 0.1261 0.2454 0.4065 0.064 Uiso 1 1 calc R . . C3F C 0.2565(8) 0.2365(7) 0.4784(3) 0.063(2) Uani 1 1 d . . . H3F H 0.2170 0.2698 0.5043 0.075 Uiso 1 1 calc R . . C4F C 0.3684(8) 0.2021(8) 0.4986(3) 0.069(2) Uani 1 1 d . . . H4F H 0.4062 0.2122 0.5385 0.083 Uiso 1 1 calc R . . C5F C 0.4242(8) 0.1537(8) 0.4612(3) 0.075(3) Uani 1 1 d . . . H5F H 0.5004 0.1298 0.4753 0.090 Uiso 1 1 calc R . . C6F C 0.3703(6) 0.1386(7) 0.4020(3) 0.0512(19) Uani 1 1 d . . . H6F H 0.4098 0.1048 0.3763 0.061 Uiso 1 1 calc R . . C1G C 0.0439(5) -0.2012(5) 0.1940(2) 0.0277(13) Uani 1 1 d . . . C2G C -0.0387(5) -0.2991(5) 0.2116(2) 0.0328(13) Uani 1 1 d . . . H2G H -0.0338 -0.3014 0.2509 0.039 Uiso 1 1 calc R . . C3G C -0.1288(6) -0.3940(5) 0.1701(3) 0.0389(15) Uani 1 1 d . . . H3G H -0.1867 -0.4593 0.1817 0.047 Uiso 1 1 calc R . . C4G C -0.1345(6) -0.3940(5) 0.1128(3) 0.0440(17) Uani 1 1 d . . . H4G H -0.1938 -0.4599 0.0853 0.053 Uiso 1 1 calc R . . C5G C -0.0536(7) -0.2975(6) 0.0960(3) 0.0441(17) Uani 1 1 d . . . H5G H -0.0587 -0.2972 0.0565 0.053 Uiso 1 1 calc R . . C6G C 0.0366(6) -0.1994(5) 0.1353(2) 0.0339(14) Uani 1 1 d . . . H6G H 0.0914 -0.1333 0.1229 0.041 Uiso 1 1 calc R . . C1H C 0.2504(5) -0.1664(5) 0.2933(2) 0.0277(13) Uani 1 1 d . . . C2H C 0.2569(7) -0.1643(6) 0.3505(3) 0.0478(17) Uani 1 1 d . . . H2H H 0.2166 -0.1144 0.3683 0.057 Uiso 1 1 calc R . . C3H C 0.3229(8) -0.2354(6) 0.3833(3) 0.058(2) Uani 1 1 d . . . H3H H 0.3270 -0.2330 0.4228 0.070 Uiso 1 1 calc R . . C4H C 0.3805(7) -0.3074(6) 0.3572(3) 0.057(2) Uani 1 1 d . . . H4H H 0.4226 -0.3569 0.3785 0.069 Uiso 1 1 calc R . . C5H C 0.3780(6) -0.3089(6) 0.3000(3) 0.0508(19) Uani 1 1 d . . . H5H H 0.4205 -0.3572 0.2825 0.061 Uiso 1 1 calc R . . C6H C 0.3132(6) -0.2394(5) 0.2684(3) 0.0382(15) Uani 1 1 d . . . H6H H 0.3111 -0.2412 0.2291 0.046 Uiso 1 1 calc R . . C2S C 0.8730(8) 0.2224(7) 0.0752(3) 0.063(2) Uani 1 1 d . . . H2S1 H 0.8458 0.1335 0.0744 0.076 Uiso 1 1 calc R . . H2S2 H 0.9705 0.2512 0.0831 0.076 Uiso 1 1 calc R . . Cl1A Cl 0.8251(2) 0.2891(2) 0.12975(11) 0.0844(7) Uani 1 1 d . . . Cl2A Cl 0.8058(3) 0.2542(3) 0.00856(10) 0.1230(11) Uani 1 1 d . . . C3S C 0.0302(14) 0.530(3) 0.4471(8) 0.170(11) Uani 0.50 1 d PDU . . H3S1 H 0.0237 0.6046 0.4314 0.204 Uiso 0.50 1 calc PR . . H3S2 H -0.0058 0.4618 0.4150 0.204 Uiso 0.50 1 calc PR . . Cl2S Cl -0.0705(11) 0.5030(8) 0.4969(5) 0.196(5) Uani 0.50 1 d PD . -1 Cl1S Cl 0.2015(15) 0.5457(10) 0.4766(4) 0.231(6) Uani 0.50 1 d PD . -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 0.0277(3) 0.0390(4) 0.0251(3) 0.0077(3) -0.0047(3) 0.0156(3) Ru1 0.0168(2) 0.0245(2) 0.0193(2) 0.00419(17) 0.00081(16) 0.01021(17) Cl1 0.0526(10) 0.0572(10) 0.0320(8) 0.0067(7) 0.0032(7) 0.0293(8) Cl2 0.0218(7) 0.0397(8) 0.0264(7) 0.0082(6) 0.0007(5) 0.0156(6) P1 0.0215(7) 0.0276(7) 0.0207(7) 0.0044(6) 0.0030(6) 0.0117(6) P2 0.0221(7) 0.0267(7) 0.0246(7) 0.0048(6) 0.0027(6) 0.0115(6) P3 0.0220(7) 0.0285(8) 0.0232(7) 0.0042(6) 0.0039(6) 0.0129(6) P4 0.0227(7) 0.0252(7) 0.0245(7) 0.0050(6) 0.0038(6) 0.0103(6) N1 0.029(3) 0.035(3) 0.029(3) 0.005(2) -0.006(2) 0.017(2) C1 0.023(3) 0.028(3) 0.026(3) 0.009(2) 0.008(2) 0.015(2) C2 0.027(3) 0.037(3) 0.031(3) 0.012(3) 0.006(2) 0.016(3) C3 0.035(3) 0.036(3) 0.031(3) 0.005(3) -0.001(3) 0.014(3) C4 0.039(4) 0.042(4) 0.031(3) -0.001(3) -0.006(3) 0.020(3) C5 0.022(3) 0.037(3) 0.028(3) 0.011(2) 0.010(2) 0.014(3) C6 0.038(4) 0.033(3) 0.042(4) 0.006(3) -0.013(3) 0.010(3) C7 0.041(4) 0.031(3) 0.054(4) 0.004(3) -0.008(3) 0.018(3) C8 0.023(3) 0.029(3) 0.029(3) 0.001(2) 0.004(2) 0.010(2) C9 0.025(3) 0.033(3) 0.027(3) 0.010(2) 0.008(2) 0.015(2) C1A 0.030(3) 0.028(3) 0.021(3) 0.005(2) 0.004(2) 0.014(2) C2A 0.029(3) 0.038(3) 0.032(3) 0.007(3) 0.009(3) 0.012(3) C3A 0.037(4) 0.049(4) 0.028(3) 0.008(3) -0.001(3) 0.017(3) C4A 0.052(4) 0.052(4) 0.028(3) 0.016(3) 0.011(3) 0.024(3) C5A 0.052(4) 0.064(5) 0.037(4) 0.019(3) 0.025(3) 0.028(4) C6A 0.039(4) 0.047(4) 0.030(3) 0.006(3) 0.007(3) 0.021(3) C1B 0.028(3) 0.028(3) 0.019(3) 0.005(2) 0.007(2) 0.011(2) C2B 0.027(3) 0.038(3) 0.046(4) 0.006(3) 0.009(3) 0.015(3) C3B 0.054(4) 0.029(3) 0.065(5) 0.009(3) 0.025(4) 0.018(3) C4B 0.054(4) 0.050(4) 0.049(4) 0.014(3) 0.020(3) 0.037(4) C5B 0.037(4) 0.057(4) 0.037(4) -0.001(3) -0.005(3) 0.032(3) C6B 0.030(3) 0.036(3) 0.037(3) 0.002(3) 0.002(3) 0.015(3) C1C 0.031(3) 0.021(3) 0.033(3) 0.006(2) 0.000(2) 0.002(2) C2C 0.080(5) 0.049(4) 0.041(4) 0.009(3) 0.008(4) 0.030(4) C3C 0.126(8) 0.054(5) 0.039(4) 0.014(4) -0.009(5) 0.041(5) C4C 0.065(6) 0.049(5) 0.082(6) 0.042(5) -0.026(5) 0.007(4) C5C 0.036(4) 0.075(6) 0.134(8) 0.066(6) 0.015(5) 0.022(4) C6C 0.043(4) 0.068(5) 0.069(5) 0.036(4) 0.019(4) 0.031(4) C1D 0.027(3) 0.026(3) 0.038(3) 0.000(3) 0.006(2) 0.018(3) C2D 0.030(3) 0.034(3) 0.046(4) 0.003(3) 0.013(3) 0.010(3) C3D 0.036(4) 0.031(3) 0.066(5) -0.006(3) 0.017(3) 0.009(3) C4D 0.036(4) 0.043(4) 0.060(5) -0.014(4) -0.008(3) 0.016(3) C5D 0.057(5) 0.052(4) 0.032(4) -0.005(3) -0.009(3) 0.024(4) C6D 0.046(4) 0.033(3) 0.028(3) -0.001(3) 0.000(3) 0.013(3) C1E 0.023(3) 0.032(3) 0.025(3) 0.003(2) 0.006(2) 0.013(2) C2E 0.032(3) 0.036(3) 0.060(4) 0.009(3) 0.017(3) 0.014(3) C3E 0.050(4) 0.029(3) 0.087(6) 0.009(3) 0.026(4) 0.018(3) C4E 0.045(4) 0.047(4) 0.054(4) 0.017(3) 0.020(3) 0.032(3) C5E 0.022(3) 0.045(4) 0.040(4) 0.009(3) 0.002(3) 0.015(3) C6E 0.031(3) 0.029(3) 0.034(3) 0.008(3) 0.007(3) 0.011(3) C1F 0.027(3) 0.035(3) 0.021(3) 0.002(2) 0.000(2) 0.006(3) C2F 0.048(4) 0.085(5) 0.030(4) -0.001(4) 0.003(3) 0.032(4) C3F 0.068(5) 0.095(6) 0.025(4) -0.006(4) 0.007(3) 0.033(5) C4F 0.058(5) 0.121(7) 0.022(4) 0.005(4) -0.001(3) 0.027(5) C5F 0.053(5) 0.144(8) 0.032(4) 0.016(5) -0.001(4) 0.048(5) C6F 0.043(4) 0.097(6) 0.027(3) 0.013(3) 0.011(3) 0.040(4) C1G 0.020(3) 0.028(3) 0.032(3) -0.001(2) 0.000(2) 0.009(2) C2G 0.029(3) 0.033(3) 0.034(3) 0.000(3) 0.009(3) 0.007(3) C3G 0.029(3) 0.033(3) 0.052(4) 0.007(3) 0.013(3) 0.003(3) C4G 0.041(4) 0.027(3) 0.051(4) -0.003(3) -0.011(3) 0.011(3) C5G 0.057(4) 0.037(4) 0.034(4) -0.002(3) -0.005(3) 0.023(3) C6G 0.038(3) 0.033(3) 0.035(3) 0.010(3) 0.007(3) 0.018(3) C1H 0.016(3) 0.025(3) 0.040(3) 0.008(2) 0.001(2) 0.008(2) C2H 0.061(5) 0.059(4) 0.035(4) 0.010(3) 0.011(3) 0.038(4) C3H 0.078(5) 0.063(5) 0.039(4) 0.011(3) 0.002(4) 0.038(4) C4H 0.054(5) 0.045(4) 0.067(5) 0.017(4) -0.010(4) 0.023(4) C5H 0.043(4) 0.038(4) 0.083(6) 0.014(4) 0.016(4) 0.030(3) C6H 0.040(4) 0.040(4) 0.047(4) 0.017(3) 0.017(3) 0.023(3) C2S 0.080(6) 0.064(5) 0.042(4) 0.003(4) -0.004(4) 0.034(4) Cl1A 0.1036(18) 0.0740(14) 0.1064(18) 0.0280(13) 0.0599(15) 0.0457(14) Cl2A 0.170(3) 0.124(2) 0.0620(15) 0.0352(15) -0.0133(17) 0.053(2) C3S 0.21(2) 0.168(18) 0.122(17) 0.031(15) 0.000(15) 0.068(16) Cl2S 0.230(14) 0.112(6) 0.193(9) 0.008(6) -0.034(11) 0.040(9) Cl1S 0.382(19) 0.177(9) 0.151(8) 0.079(7) 0.055(10) 0.104(11) _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 N1 2.037(4) 2_756 ? Pd1 N1 2.037(4) . ? Pd1 Cl1 2.3042(15) . ? Pd1 Cl1 2.3043(15) 2_756 ? Ru1 C1 1.981(5) . ? Ru1 P2 2.3331(15) . ? Ru1 P4 2.3421(15) . ? Ru1 P1 2.3572(15) . ? Ru1 P3 2.3738(15) . ? Ru1 Cl2 2.4833(12) . ? P1 C1B 1.824(5) . ? P1 C8 1.833(5) . ? P1 C1A 1.834(5) . ? P2 C1C 1.823(5) . ? P2 C1D 1.827(5) . ? P2 C8 1.838(5) . ? P3 C1E 1.820(5) . ? P3 C1F 1.835(5) . ? P3 C9 1.841(5) . ? P4 C1H 1.819(5) . ? P4 C1G 1.828(5) . ? P4 C9 1.849(5) . ? N1 C3 1.338(6) . ? N1 C7 1.339(7) . ? C1 C2 1.208(7) . ? C2 C5 1.427(7) . ? C3 C4 1.382(7) . ? C4 C5 1.383(7) . ? C5 C6 1.393(7) . ? C6 C7 1.379(7) . ? C1A C6A 1.372(8) . ? C1A C2A 1.395(7) . ? C2A C3A 1.381(7) . ? C3A C4A 1.369(8) . ? C4A C5A 1.384(8) . ? C5A C6A 1.378(8) . ? C1B C2B 1.379(7) . ? C1B C6B 1.390(7) . ? C2B C3B 1.382(7) . ? C3B C4B 1.384(9) . ? C4B C5B 1.373(8) . ? C5B C6B 1.396(7) . ? C1C C2C 1.385(9) . ? C1C C6C 1.388(8) . ? C2C C3C 1.390(9) . ? C3C C4C 1.363(11) . ? C4C C5C 1.353(12) . ? C5C C6C 1.382(9) . ? C1D C2D 1.379(8) . ? C1D C6D 1.397(8) . ? C2D C3D 1.384(8) . ? C3D C4D 1.366(9) . ? C4D C5D 1.374(10) . ? C5D C6D 1.393(8) . ? C1E C6E 1.377(7) . ? C1E C2E 1.387(8) . ? C2E C3E 1.390(8) . ? C3E C4E 1.369(9) . ? C4E C5E 1.368(8) . ? C5E C6E 1.382(7) . ? C1F C2F 1.369(8) . ? C1F C6F 1.386(7) . ? C2F C3F 1.373(8) . ? C3F C4F 1.373(9) . ? C4F C5F 1.352(10) . ? C5F C6F 1.392(8) . ? C1G C2G 1.388(8) . ? C1G C6G 1.401(8) . ? C2G C3G 1.392(7) . ? C3G C4G 1.370(9) . ? C4G C5G 1.360(9) . ? C5G C6G 1.388(8) . ? C1H C2H 1.361(8) . ? C1H C6H 1.391(7) . ? C2H C3H 1.407(8) . ? C3H C4H 1.356(9) . ? C4H C5H 1.370(10) . ? C5H C6H 1.371(8) . ? C2S Cl1A 1.714(7) . ? C2S Cl2A 1.722(7) . ? C3S Cl2S 1.44(3) 2_566 ? C3S Cl2S 1.779(3) . ? C3S Cl1S 1.779(3) . ? Cl2S C3S 1.44(3) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 179.999(1) 2_756 . ? N1 Pd1 Cl1 89.94(13) 2_756 . ? N1 Pd1 Cl1 90.06(13) . . ? N1 Pd1 Cl1 90.06(13) 2_756 2_756 ? N1 Pd1 Cl1 89.94(13) . 2_756 ? Cl1 Pd1 Cl1 180.0 . 2_756 ? C1 Ru1 P2 87.39(15) . . ? C1 Ru1 P4 91.08(15) . . ? P2 Ru1 P4 178.45(5) . . ? C1 Ru1 P1 81.39(15) . . ? P2 Ru1 P1 70.45(5) . . ? P4 Ru1 P1 109.62(5) . . ? C1 Ru1 P3 96.33(15) . . ? P2 Ru1 P3 108.54(5) . . ? P4 Ru1 P3 71.33(5) . . ? P1 Ru1 P3 177.51(5) . . ? C1 Ru1 Cl2 174.83(16) . . ? P2 Ru1 Cl2 97.40(5) . . ? P4 Ru1 Cl2 84.11(5) . . ? P1 Ru1 Cl2 102.01(5) . . ? P3 Ru1 Cl2 80.33(5) . . ? C1B P1 C8 107.1(2) . . ? C1B P1 C1A 102.4(2) . . ? C8 P1 C1A 101.1(3) . . ? C1B P1 Ru1 122.78(17) . . ? C8 P1 Ru1 92.47(18) . . ? C1A P1 Ru1 126.26(18) . . ? C1C P2 C1D 103.8(2) . . ? C1C P2 C8 106.7(3) . . ? C1D P2 C8 104.1(2) . . ? C1C P2 Ru1 120.70(18) . . ? C1D P2 Ru1 124.9(2) . . ? C8 P2 Ru1 93.12(17) . . ? C1E P3 C1F 101.2(2) . . ? C1E P3 C9 108.1(2) . . ? C1F P3 C9 103.9(2) . . ? C1E P3 Ru1 120.51(18) . . ? C1F P3 Ru1 126.80(19) . . ? C9 P3 Ru1 93.53(17) . . ? C1H P4 C1G 100.3(2) . . ? C1H P4 C9 107.1(2) . . ? C1G P4 C9 106.4(2) . . ? C1H P4 Ru1 121.39(18) . . ? C1G P4 Ru1 125.1(2) . . ? C9 P4 Ru1 94.36(17) . . ? C3 N1 C7 117.1(4) . . ? C3 N1 Pd1 122.2(3) . . ? C7 N1 Pd1 120.6(4) . . ? C2 C1 Ru1 177.4(5) . . ? C1 C2 C5 170.6(6) . . ? N1 C3 C4 122.6(5) . . ? C3 C4 C5 121.0(5) . . ? C4 C5 C6 115.7(5) . . ? C4 C5 C2 122.7(5) . . ? C6 C5 C2 121.6(5) . . ? C7 C6 C5 120.4(5) . . ? N1 C7 C6 123.1(5) . . ? P1 C8 P2 94.9(3) . . ? P3 C9 P4 96.3(3) . . ? C6A C1A C2A 119.5(5) . . ? C6A C1A P1 120.3(4) . . ? C2A C1A P1 119.9(4) . . ? C3A C2A C1A 119.2(6) . . ? C4A C3A C2A 120.5(6) . . ? C3A C4A C5A 120.7(6) . . ? C6A C5A C4A 118.7(6) . . ? C1A C6A C5A 121.4(5) . . ? C2B C1B C6B 118.9(5) . . ? C2B C1B P1 118.3(4) . . ? C6B C1B P1 122.8(4) . . ? C1B C2B C3B 120.7(5) . . ? C2B C3B C4B 120.3(6) . . ? C5B C4B C3B 119.7(5) . . ? C4B C5B C6B 119.9(6) . . ? C1B C6B C5B 120.4(5) . . ? C2C C1C C6C 117.7(6) . . ? C2C C1C P2 124.7(5) . . ? C6C C1C P2 117.5(5) . . ? C1C C2C C3C 120.3(7) . . ? C4C C3C C2C 119.9(8) . . ? C5C C4C C3C 121.2(7) . . ? C4C C5C C6C 119.1(8) . . ? C5C C6C C1C 121.8(7) . . ? C2D C1D C6D 119.3(5) . . ? C2D C1D P2 122.1(4) . . ? C6D C1D P2 118.4(5) . . ? C1D C2D C3D 120.9(6) . . ? C4D C3D C2D 119.8(7) . . ? C3D C4D C5D 120.3(6) . . ? C4D C5D C6D 120.6(6) . . ? C5D C6D C1D 119.0(6) . . ? C6E C1E C2E 118.0(5) . . ? C6E C1E P3 124.2(4) . . ? C2E C1E P3 117.8(4) . . ? C1E C2E C3E 120.7(6) . . ? C4E C3E C2E 120.3(6) . . ? C5E C4E C3E 119.4(5) . . ? C4E C5E C6E 120.5(5) . . ? C1E C6E C5E 121.1(5) . . ? C2F C1F C6F 118.5(5) . . ? C2F C1F P3 121.8(4) . . ? C6F C1F P3 119.6(4) . . ? C1F C2F C3F 121.8(6) . . ? C2F C3F C4F 119.5(7) . . ? C5F C4F C3F 119.9(6) . . ? C4F C5F C6F 120.9(7) . . ? C1F C6F C5F 119.5(6) . . ? C2G C1G C6G 119.9(5) . . ? C2G C1G P4 119.7(4) . . ? C6G C1G P4 120.3(5) . . ? C1G C2G C3G 119.1(6) . . ? C4G C3G C2G 121.2(6) . . ? C5G C4G C3G 119.2(6) . . ? C4G C5G C6G 122.0(6) . . ? C5G C6G C1G 118.5(6) . . ? C2H C1H C6H 118.0(5) . . ? C2H C1H P4 123.9(4) . . ? C6H C1H P4 118.2(4) . . ? C1H C2H C3H 121.3(6) . . ? C4H C3H C2H 119.0(7) . . ? C3H C4H C5H 120.8(6) . . ? C4H C5H C6H 119.6(6) . . ? C5H C6H C1H 121.3(6) . . ? Cl1A C2S Cl2A 113.2(4) . . ? Cl2S C3S Cl2S 55.0(11) 2_566 . ? Cl2S C3S Cl1S 60.7(8) 2_566 . ? Cl2S C3S Cl1S 114.5(13) . . ? C3S Cl2S C3S 125.0(11) 2_566 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.890 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.117 # Attachment '6088.cif' data_6088 _database_code_depnum_ccdc_archive 'CCDC 620353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H48 Cl N P4 Ru' _chemical_formula_weight 1007.36 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5514(6) _cell_length_b 13.5933(6) _cell_length_c 13.8171(7) _cell_angle_alpha 108.1380(10) _cell_angle_beta 94.0600(10) _cell_angle_gamma 94.7290(10) _cell_volume 2397.98(19) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5836 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.50 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.7841 _exptl_absorpt_correction_T_max 0.8970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31494 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10991 _reflns_number_gt 9765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0404P)^2^+0.9274P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10991 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ru1 Ru 0.744318(10) 0.802584(10) 0.688230(10) 0.01898(5) Uani 1 1 d . . . P1 P 0.91811(3) 0.80775(3) 0.68924(4) 0.02307(10) Uani 1 1 d . . . P2 P 0.81598(3) 0.94833(4) 0.82517(4) 0.02442(10) Uani 1 1 d . . . P3 P 0.57355(3) 0.78803(4) 0.69885(3) 0.02202(10) Uani 1 1 d . . . P4 P 0.67003(3) 0.65899(3) 0.54981(3) 0.02343(10) Uani 1 1 d . . . Cl1 Cl 0.74825(4) 0.91890(4) 0.58411(3) 0.03049(10) Uani 1 1 d . . . N1 N 0.76785(17) 0.49547(15) 1.04859(15) 0.0478(5) Uani 1 1 d . . . C1 C 0.74703(13) 0.71183(13) 0.77583(13) 0.0232(3) Uani 1 1 d . . . C2 C 0.74831(15) 0.65901(15) 0.83212(15) 0.0307(4) Uani 1 1 d . . . C3 C 0.84775(19) 0.53244(18) 1.01523(18) 0.0455(5) Uani 1 1 d . . . H3 H 0.9103 0.5220 1.0420 0.055 Uiso 1 1 calc R . . C4 C 0.84602(17) 0.58491(17) 0.94441(17) 0.0393(5) Uani 1 1 d . . . H4 H 0.9057 0.6080 0.9236 0.047 Uiso 1 1 calc R . . C5 C 0.75449(15) 0.60335(14) 0.90397(14) 0.0289(4) Uani 1 1 d . . . C6 C 0.67029(17) 0.56472(16) 0.93862(17) 0.0389(5) Uani 1 1 d . . . H6 H 0.6064 0.5743 0.9142 0.047 Uiso 1 1 calc R . . C7 C 0.6814(2) 0.51234(18) 1.00894(19) 0.0476(6) Uani 1 1 d . . . H7 H 0.6232 0.4866 1.0304 0.057 Uiso 1 1 calc R . . C10 C 0.54883(14) 0.65703(14) 0.60289(15) 0.0291(4) Uani 1 1 d . . . H10A H 0.4927 0.6517 0.5521 0.035 Uiso 1 1 calc R . . H10B H 0.5387 0.6019 0.6342 0.035 Uiso 1 1 calc R . . C16 C 0.94600(15) 0.93019(16) 0.79770(17) 0.0366(5) Uani 1 1 d . . . H16A H 0.9866 0.9212 0.8553 0.044 Uiso 1 1 calc R . . H16B H 0.9778 0.9870 0.7773 0.044 Uiso 1 1 calc R . . C1A C 0.98632(14) 0.82661(15) 0.58579(15) 0.0298(4) Uani 1 1 d . . . C2A C 1.0543(2) 0.9113(2) 0.5978(2) 0.0586(7) Uani 1 1 d . . . H2A H 1.0701 0.9614 0.6628 0.070 Uiso 1 1 calc R . . C3A C 1.0999(2) 0.9238(3) 0.5151(2) 0.0705(9) Uani 1 1 d . . . H3A H 1.1458 0.9827 0.5250 0.085 Uiso 1 1 calc R . . C4A C 1.0802(2) 0.8537(2) 0.4212(2) 0.0550(7) Uani 1 1 d . . . H4A H 1.1115 0.8637 0.3659 0.066 Uiso 1 1 calc R . . C5A C 1.0137(2) 0.7673(2) 0.4070(2) 0.0600(7) Uani 1 1 d . . . H5A H 0.9995 0.7174 0.3417 0.072 Uiso 1 1 calc R . . C6A C 0.9673(2) 0.75384(18) 0.48952(19) 0.0507(6) Uani 1 1 d . . . H6A H 0.9223 0.6942 0.4794 0.061 Uiso 1 1 calc R . . C1B C 0.98104(13) 0.70870(15) 0.72463(14) 0.0268(4) Uani 1 1 d . . . C2B C 1.05531(15) 0.72944(19) 0.80534(16) 0.0381(5) Uani 1 1 d . . . H2B H 1.0763 0.7985 0.8461 0.046 Uiso 1 1 calc R . . C3B C 1.09856(17) 0.6475(2) 0.82568(18) 0.0487(6) Uani 1 1 d . . . H3B H 1.1477 0.6617 0.8813 0.058 Uiso 1 1 calc R . . C4B C 1.07062(19) 0.5470(2) 0.7660(2) 0.0502(6) Uani 1 1 d . . . H4B H 1.1016 0.4925 0.7795 0.060 Uiso 1 1 calc R . . C5B C 0.99698(19) 0.52532(19) 0.6861(2) 0.0496(6) Uani 1 1 d . . . H5B H 0.9774 0.4561 0.6451 0.060 Uiso 1 1 calc R . . C6B C 0.95180(16) 0.60562(16) 0.66632(18) 0.0376(5) Uani 1 1 d . . . H6B H 0.9005 0.5902 0.6126 0.045 Uiso 1 1 calc R . . C1C C 0.80290(16) 1.08169(15) 0.82823(15) 0.0315(4) Uani 1 1 d . . . C2C C 0.87879(19) 1.16124(16) 0.87508(18) 0.0445(5) Uani 1 1 d . . . H2C H 0.9370 1.1468 0.9070 0.053 Uiso 1 1 calc R . . C3C C 0.8687(2) 1.26204(18) 0.8748(2) 0.0569(7) Uani 1 1 d . . . H3C H 0.9203 1.3156 0.9062 0.068 Uiso 1 1 calc R . . C4C C 0.7837(2) 1.28397(18) 0.8289(2) 0.0561(7) Uani 1 1 d . . . H4C H 0.7774 1.3522 0.8286 0.067 Uiso 1 1 calc R . . C5C C 0.7082(2) 1.20617(18) 0.78356(18) 0.0477(6) Uani 1 1 d . . . H5C H 0.6498 1.2214 0.7528 0.057 Uiso 1 1 calc R . . C6C C 0.71728(17) 1.10472(16) 0.78269(16) 0.0373(5) Uani 1 1 d . . . H6C H 0.6652 1.0517 0.7512 0.045 Uiso 1 1 calc R . . C1D C 0.81259(15) 0.95654(15) 0.95901(14) 0.0319(4) Uani 1 1 d . . . C2D C 0.76307(17) 1.03154(18) 1.02527(16) 0.0423(5) Uani 1 1 d . . . H2D H 0.7378 1.0844 1.0036 0.051 Uiso 1 1 calc R . . C3D C 0.7511(2) 1.0282(2) 1.12325(19) 0.0584(7) Uani 1 1 d . . . H3D H 0.7181 1.0792 1.1678 0.070 Uiso 1 1 calc R . . C4D C 0.7872(2) 0.9510(3) 1.15542(19) 0.0624(8) Uani 1 1 d . . . H4D H 0.7779 0.9486 1.2215 0.075 Uiso 1 1 calc R . . C5D C 0.8368(2) 0.8772(2) 1.0914(2) 0.0564(7) Uani 1 1 d . . . H5D H 0.8622 0.8250 1.1140 0.068 Uiso 1 1 calc R . . C6D C 0.84960(17) 0.87940(18) 0.99373(17) 0.0420(5) Uani 1 1 d . . . H6D H 0.8835 0.8285 0.9503 0.050 Uiso 1 1 calc R . . C1E C 0.49419(13) 0.87287(14) 0.65891(14) 0.0258(4) Uani 1 1 d . . . C2E C 0.47577(16) 0.96358(16) 0.73233(16) 0.0365(5) Uani 1 1 d . . . H2E H 0.4984 0.9758 0.8014 0.044 Uiso 1 1 calc R . . C3E C 0.42434(18) 1.03627(18) 0.70498(17) 0.0430(5) Uani 1 1 d . . . H3E H 0.4135 1.0982 0.7552 0.052 Uiso 1 1 calc R . . C4E C 0.38903(18) 1.01828(19) 0.60476(18) 0.0454(6) Uani 1 1 d . . . H4E H 0.3535 1.0673 0.5862 0.054 Uiso 1 1 calc R . . C5E C 0.4061(2) 0.9281(2) 0.53181(18) 0.0515(6) Uani 1 1 d . . . H5E H 0.3811 0.9150 0.4632 0.062 Uiso 1 1 calc R . . C6E C 0.45983(18) 0.85619(18) 0.55809(16) 0.0411(5) Uani 1 1 d . . . H6E H 0.4729 0.7958 0.5071 0.049 Uiso 1 1 calc R . . C1F C 0.51758(13) 0.77369(14) 0.81057(14) 0.0268(4) Uani 1 1 d . . . C2F C 0.56125(18) 0.82661(19) 0.90772(17) 0.0435(5) Uani 1 1 d . . . H2F H 0.6212 0.8699 0.9169 0.052 Uiso 1 1 calc R . . C3F C 0.5175(2) 0.8167(2) 0.99235(19) 0.0592(7) Uani 1 1 d . . . H3F H 0.5471 0.8545 1.0586 0.071 Uiso 1 1 calc R . . C4F C 0.4311(2) 0.7515(2) 0.9797(2) 0.0569(7) Uani 1 1 d . . . H4F H 0.4016 0.7446 1.0372 0.068 Uiso 1 1 calc R . . C5F C 0.38857(19) 0.6974(2) 0.8840(2) 0.0575(7) Uani 1 1 d . . . H5F H 0.3301 0.6519 0.8755 0.069 Uiso 1 1 calc R . . C6F C 0.43013(16) 0.7083(2) 0.79882(19) 0.0452(6) Uani 1 1 d . . . H6F H 0.3992 0.6714 0.7329 0.054 Uiso 1 1 calc R . . C1G C 0.64164(17) 0.66753(15) 0.42163(14) 0.0343(4) Uani 1 1 d . . . C2G C 0.5517(2) 0.6216(2) 0.36398(18) 0.0537(6) Uani 1 1 d . . . H2G H 0.5042 0.5870 0.3919 0.064 Uiso 1 1 calc R . . C3G C 0.5313(3) 0.6263(3) 0.2663(2) 0.0807(11) Uani 1 1 d . . . H3G H 0.4696 0.5966 0.2289 0.097 Uiso 1 1 calc R . . C4G C 0.6000(4) 0.6737(3) 0.2242(2) 0.0906(14) Uani 1 1 d . . . H4G H 0.5859 0.6762 0.1575 0.109 Uiso 1 1 calc R . . C5G C 0.6894(3) 0.7178(2) 0.2779(2) 0.0766(11) Uani 1 1 d . . . H5G H 0.7369 0.7493 0.2473 0.092 Uiso 1 1 calc R . . C6G C 0.7116(2) 0.71674(17) 0.37888(18) 0.0512(6) Uani 1 1 d . . . H6G H 0.7727 0.7489 0.4164 0.061 Uiso 1 1 calc R . . C1H C 0.70521(13) 0.52653(14) 0.52109(14) 0.0264(4) Uani 1 1 d . . . C2H C 0.74493(15) 0.47765(16) 0.43104(16) 0.0349(4) Uani 1 1 d . . . H2H H 0.7503 0.5113 0.3813 0.042 Uiso 1 1 calc R . . C3H C 0.77688(17) 0.37971(17) 0.41310(18) 0.0441(5) Uani 1 1 d . . . H3H H 0.8043 0.3479 0.3519 0.053 Uiso 1 1 calc R . . C4H C 0.76848(19) 0.32920(17) 0.48458(19) 0.0470(6) Uani 1 1 d . . . H4H H 0.7890 0.2623 0.4719 0.056 Uiso 1 1 calc R . . C5H C 0.73003(19) 0.37663(17) 0.57472(19) 0.0449(5) Uani 1 1 d . . . H5H H 0.7247 0.3421 0.6238 0.054 Uiso 1 1 calc R . . C6H C 0.69907(16) 0.47473(15) 0.59394(16) 0.0346(4) Uani 1 1 d . . . H6H H 0.6737 0.5068 0.6563 0.042 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 Ru1 0.02041(8) 0.01890(8) 0.01999(8) 0.00955(5) 0.00308(5) 0.00145(5) P1 0.0211(2) 0.0222(2) 0.0272(2) 0.00960(18) 0.00421(18) 0.00148(17) P2 0.0251(2) 0.0221(2) 0.0255(2) 0.00699(18) 0.00367(18) 0.00070(18) P3 0.0211(2) 0.0239(2) 0.0232(2) 0.01039(18) 0.00312(17) 0.00215(17) P4 0.0263(2) 0.0219(2) 0.0226(2) 0.00804(18) 0.00198(18) 0.00197(18) Cl1 0.0407(3) 0.0278(2) 0.0291(2) 0.01742(19) 0.00599(19) 0.00421(19) N1 0.0698(14) 0.0463(11) 0.0414(11) 0.0301(9) 0.0138(10) 0.0163(10) C1 0.0231(9) 0.0230(8) 0.0232(8) 0.0077(7) 0.0023(7) 0.0008(7) C2 0.0356(10) 0.0285(10) 0.0310(10) 0.0138(8) 0.0041(8) 0.0029(8) C3 0.0540(14) 0.0481(13) 0.0423(13) 0.0248(11) -0.0001(11) 0.0133(11) C4 0.0441(12) 0.0406(12) 0.0406(12) 0.0232(10) 0.0043(9) 0.0050(9) C5 0.0412(11) 0.0241(9) 0.0248(9) 0.0121(7) 0.0045(8) 0.0040(8) C6 0.0441(12) 0.0375(11) 0.0424(12) 0.0216(10) 0.0095(10) 0.0061(9) C7 0.0593(15) 0.0438(13) 0.0534(14) 0.0304(11) 0.0234(12) 0.0088(11) C10 0.0265(9) 0.0261(9) 0.0333(10) 0.0080(8) 0.0032(8) 0.0002(7) C16 0.0259(10) 0.0307(10) 0.0447(12) 0.0004(9) 0.0061(9) -0.0016(8) C1A 0.0249(9) 0.0348(10) 0.0385(11) 0.0219(9) 0.0091(8) 0.0073(8) C2A 0.0628(17) 0.0664(17) 0.0447(14) 0.0238(13) 0.0044(12) -0.0269(14) C3A 0.0678(19) 0.083(2) 0.0687(19) 0.0425(17) 0.0140(15) -0.0264(16) C4A 0.0573(16) 0.0694(17) 0.0621(17) 0.0461(15) 0.0308(13) 0.0206(13) C5A 0.090(2) 0.0492(15) 0.0509(15) 0.0205(12) 0.0380(15) 0.0213(14) C6A 0.0731(17) 0.0354(12) 0.0487(14) 0.0150(11) 0.0315(13) 0.0075(11) C1B 0.0213(9) 0.0336(10) 0.0306(9) 0.0164(8) 0.0053(7) 0.0048(7) C2B 0.0315(11) 0.0502(13) 0.0346(11) 0.0163(10) 0.0021(9) 0.0059(9) C3B 0.0358(12) 0.0811(19) 0.0403(13) 0.0325(13) 0.0018(10) 0.0195(12) C4B 0.0509(14) 0.0613(16) 0.0584(15) 0.0401(14) 0.0151(12) 0.0275(12) C5B 0.0533(15) 0.0362(12) 0.0670(16) 0.0253(12) 0.0064(12) 0.0129(11) C6B 0.0340(11) 0.0319(11) 0.0492(13) 0.0179(9) -0.0042(9) 0.0040(8) C1C 0.0416(11) 0.0246(9) 0.0287(10) 0.0078(8) 0.0088(8) 0.0043(8) C2C 0.0533(14) 0.0290(11) 0.0451(13) 0.0061(9) -0.0009(11) -0.0022(10) C3C 0.0790(19) 0.0256(11) 0.0582(16) 0.0053(11) 0.0061(14) -0.0068(12) C4C 0.095(2) 0.0280(11) 0.0481(14) 0.0128(10) 0.0158(14) 0.0151(13) C5C 0.0671(16) 0.0402(13) 0.0409(13) 0.0147(10) 0.0105(11) 0.0237(12) C6C 0.0450(12) 0.0319(10) 0.0358(11) 0.0096(9) 0.0102(9) 0.0089(9) C1D 0.0314(10) 0.0343(10) 0.0256(9) 0.0072(8) -0.0015(8) -0.0084(8) C2D 0.0454(13) 0.0432(12) 0.0333(11) 0.0062(10) 0.0085(9) -0.0039(10) C3D 0.0579(16) 0.0693(18) 0.0338(12) -0.0001(12) 0.0146(11) -0.0167(13) C4D 0.0590(17) 0.090(2) 0.0324(13) 0.0238(14) -0.0052(12) -0.0312(16) C5D 0.0539(15) 0.0728(18) 0.0457(14) 0.0343(14) -0.0156(12) -0.0190(13) C6D 0.0404(12) 0.0473(13) 0.0360(11) 0.0165(10) -0.0086(9) -0.0098(10) C1E 0.0213(8) 0.0305(9) 0.0300(9) 0.0153(8) 0.0033(7) 0.0044(7) C2E 0.0440(12) 0.0400(11) 0.0280(10) 0.0119(9) 0.0031(9) 0.0154(9) C3E 0.0529(14) 0.0413(12) 0.0397(12) 0.0148(10) 0.0080(10) 0.0225(10) C4E 0.0499(14) 0.0492(13) 0.0459(13) 0.0239(11) 0.0030(10) 0.0228(11) C5E 0.0644(16) 0.0594(15) 0.0348(12) 0.0191(11) -0.0062(11) 0.0233(13) C6E 0.0532(14) 0.0404(12) 0.0297(10) 0.0090(9) 0.0001(9) 0.0176(10) C1F 0.0248(9) 0.0303(9) 0.0313(10) 0.0170(8) 0.0076(7) 0.0059(7) C2F 0.0429(13) 0.0519(14) 0.0332(11) 0.0115(10) 0.0097(9) -0.0052(10) C3F 0.0699(18) 0.0778(19) 0.0307(12) 0.0165(12) 0.0157(12) 0.0071(15) C4F 0.0620(17) 0.0751(18) 0.0536(16) 0.0402(14) 0.0337(13) 0.0189(14) C5F 0.0401(13) 0.0757(19) 0.0708(18) 0.0420(16) 0.0221(13) -0.0023(12) C6F 0.0297(11) 0.0627(15) 0.0476(13) 0.0264(12) 0.0045(10) -0.0061(10) C1G 0.0536(13) 0.0268(10) 0.0235(9) 0.0077(8) 0.0013(9) 0.0138(9) C2G 0.0655(17) 0.0519(14) 0.0353(12) 0.0036(11) -0.0132(11) 0.0150(12) C3G 0.119(3) 0.073(2) 0.0372(15) 0.0000(15) -0.0285(17) 0.038(2) C4G 0.182(4) 0.064(2) 0.0276(14) 0.0092(14) -0.004(2) 0.056(2) C5G 0.154(3) 0.0471(16) 0.0431(16) 0.0242(13) 0.038(2) 0.0286(19) C6G 0.088(2) 0.0342(12) 0.0353(12) 0.0128(10) 0.0222(12) 0.0113(12) C1H 0.0251(9) 0.0231(9) 0.0294(9) 0.0076(7) -0.0009(7) 0.0002(7) C2H 0.0370(11) 0.0335(10) 0.0359(11) 0.0120(9) 0.0074(9) 0.0063(9) C3H 0.0476(13) 0.0371(12) 0.0465(13) 0.0074(10) 0.0112(10) 0.0160(10) C4H 0.0530(14) 0.0303(11) 0.0577(15) 0.0124(10) 0.0027(11) 0.0134(10) C5H 0.0568(14) 0.0333(11) 0.0496(14) 0.0222(10) -0.0014(11) 0.0047(10) C6H 0.0424(12) 0.0293(10) 0.0322(10) 0.0110(8) 0.0011(9) 0.0018(9) _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 Ru1 C1 1.9797(17) . ? Ru1 P3 2.3252(5) . ? Ru1 P1 2.3493(5) . ? Ru1 P2 2.3530(5) . ? Ru1 P4 2.3581(5) . ? Ru1 Cl1 2.4466(4) . ? P1 C1B 1.8219(18) . ? P1 C1A 1.8274(19) . ? P1 C16 1.850(2) . ? P2 C1D 1.822(2) . ? P2 C1C 1.8238(19) . ? P2 C16 1.849(2) . ? P3 C1E 1.8187(18) . ? P3 C1F 1.8233(18) . ? P3 C10 1.8466(19) . ? P4 C1G 1.8267(19) . ? P4 C1H 1.8304(19) . ? P4 C10 1.8470(19) . ? N1 C7 1.326(3) . ? N1 C3 1.327(3) . ? C1 C2 1.212(3) . ? C2 C5 1.425(3) . ? C3 C4 1.379(3) . ? C4 C5 1.398(3) . ? C5 C6 1.393(3) . ? C6 C7 1.379(3) . ? C1A C2A 1.374(3) . ? C1A C6A 1.380(3) . ? C2A C3A 1.385(3) . ? C3A C4A 1.342(4) . ? C4A C5A 1.374(4) . ? C5A C6A 1.393(3) . ? C1B C6B 1.389(3) . ? C1B C2B 1.391(3) . ? C2B C3B 1.394(3) . ? C3B C4B 1.363(4) . ? C4B C5B 1.377(4) . ? C5B C6B 1.383(3) . ? C1C C6C 1.385(3) . ? C1C C2C 1.390(3) . ? C2C C3C 1.389(3) . ? C3C C4C 1.374(4) . ? C4C C5C 1.370(4) . ? C5C C6C 1.391(3) . ? C1D C2D 1.395(3) . ? C1D C6D 1.395(3) . ? C2D C3D 1.389(3) . ? C3D C4D 1.372(4) . ? C4D C5D 1.373(4) . ? C5D C6D 1.381(3) . ? C1E C6E 1.379(3) . ? C1E C2E 1.385(3) . ? C2E C3E 1.383(3) . ? C3E C4E 1.372(3) . ? C4E C5E 1.372(3) . ? C5E C6E 1.385(3) . ? C1F C2F 1.373(3) . ? C1F C6F 1.389(3) . ? C2F C3F 1.386(3) . ? C3F C4F 1.375(4) . ? C4F C5F 1.356(4) . ? C5F C6F 1.383(3) . ? C1G C6G 1.384(3) . ? C1G C2G 1.391(3) . ? C2G C3G 1.381(4) . ? C3G C4G 1.352(5) . ? C4G C5G 1.361(5) . ? C5G C6G 1.411(4) . ? C1H C2H 1.385(3) . ? C1H C6H 1.400(3) . ? C2H C3H 1.388(3) . ? C3H C4H 1.373(3) . ? C4H C5H 1.373(3) . ? C5H C6H 1.383(3) . ? 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 C1 Ru1 P3 84.63(5) . . ? C1 Ru1 P1 89.59(5) . . ? P3 Ru1 P1 174.200(16) . . ? C1 Ru1 P2 91.64(5) . . ? P3 Ru1 P2 107.461(17) . . ? P1 Ru1 P2 72.134(17) . . ? C1 Ru1 P4 89.37(5) . . ? P3 Ru1 P4 71.774(17) . . ? P1 Ru1 P4 108.741(17) . . ? P2 Ru1 P4 178.676(17) . . ? C1 Ru1 Cl1 177.38(5) . . ? P3 Ru1 Cl1 97.495(16) . . ? P1 Ru1 Cl1 88.268(16) . . ? P2 Ru1 Cl1 86.268(17) . . ? P4 Ru1 Cl1 92.750(17) . . ? C1B P1 C1A 103.11(8) . . ? C1B P1 C16 107.08(10) . . ? C1A P1 C16 106.14(10) . . ? C1B P1 Ru1 119.23(6) . . ? C1A P1 Ru1 123.79(6) . . ? C16 P1 Ru1 95.45(6) . . ? C1D P2 C1C 102.60(9) . . ? C1D P2 C16 105.58(10) . . ? C1C P2 C16 104.33(10) . . ? C1D P2 Ru1 123.19(6) . . ? C1C P2 Ru1 122.57(7) . . ? C16 P2 Ru1 95.35(6) . . ? C1E P3 C1F 102.29(8) . . ? C1E P3 C10 107.89(9) . . ? C1F P3 C10 104.13(9) . . ? C1E P3 Ru1 121.60(6) . . ? C1F P3 Ru1 123.43(6) . . ? C10 P3 Ru1 94.99(6) . . ? C1G P4 C1H 101.75(9) . . ? C1G P4 C10 105.16(10) . . ? C1H P4 C10 106.00(9) . . ? C1G P4 Ru1 122.43(7) . . ? C1H P4 Ru1 124.48(6) . . ? C10 P4 Ru1 93.89(6) . . ? C7 N1 C3 115.25(18) . . ? C2 C1 Ru1 177.90(17) . . ? C1 C2 C5 175.6(2) . . ? N1 C3 C4 125.0(2) . . ? C3 C4 C5 119.2(2) . . ? C6 C5 C4 116.01(18) . . ? C6 C5 C2 122.33(19) . . ? C4 C5 C2 121.66(19) . . ? C7 C6 C5 119.5(2) . . ? N1 C7 C6 125.0(2) . . ? P3 C10 P4 96.03(9) . . ? P2 C16 P1 96.93(9) . . ? C2A C1A C6A 117.7(2) . . ? C2A C1A P1 123.47(18) . . ? C6A C1A P1 118.85(16) . . ? C1A C2A C3A 120.7(3) . . ? C4A C3A C2A 121.5(3) . . ? C3A C4A C5A 119.2(2) . . ? C4A C5A C6A 119.9(3) . . ? C1A C6A C5A 121.0(2) . . ? C6B C1B C2B 118.47(18) . . ? C6B C1B P1 116.95(14) . . ? C2B C1B P1 124.58(16) . . ? C1B C2B C3B 119.8(2) . . ? C4B C3B C2B 120.9(2) . . ? C3B C4B C5B 119.9(2) . . ? C4B C5B C6B 119.9(2) . . ? C5B C6B C1B 121.0(2) . . ? C6C C1C C2C 119.13(19) . . ? C6C C1C P2 120.20(16) . . ? C2C C1C P2 120.66(17) . . ? C3C C2C C1C 120.0(2) . . ? C4C C3C C2C 120.4(2) . . ? C5C C4C C3C 119.9(2) . . ? C4C C5C C6C 120.5(2) . . ? C1C C6C C5C 120.1(2) . . ? C2D C1D C6D 118.5(2) . . ? C2D C1D P2 121.28(17) . . ? C6D C1D P2 119.75(17) . . ? C3D C2D C1D 120.1(2) . . ? C4D C3D C2D 120.4(3) . . ? C3D C4D C5D 120.1(2) . . ? C4D C5D C6D 120.3(3) . . ? C5D C6D C1D 120.6(2) . . ? C6E C1E C2E 118.73(17) . . ? C6E C1E P3 123.07(15) . . ? C2E C1E P3 117.89(14) . . ? C3E C2E C1E 120.63(19) . . ? C4E C3E C2E 120.3(2) . . ? C3E C4E C5E 119.4(2) . . ? C4E C5E C6E 120.7(2) . . ? C1E C6E C5E 120.2(2) . . ? C2F C1F C6F 118.75(19) . . ? C2F C1F P3 120.76(15) . . ? C6F C1F P3 120.48(16) . . ? C1F C2F C3F 120.5(2) . . ? C4F C3F C2F 120.2(2) . . ? C5F C4F C3F 119.7(2) . . ? C4F C5F C6F 120.8(2) . . ? C5F C6F C1F 120.1(2) . . ? C6G C1G C2G 119.0(2) . . ? C6G C1G P4 119.99(18) . . ? C2G C1G P4 121.00(18) . . ? C3G C2G C1G 120.9(3) . . ? C4G C3G C2G 120.1(3) . . ? C3G C4G C5G 120.5(3) . . ? C4G C5G C6G 120.8(3) . . ? C1G C6G C5G 118.7(3) . . ? C2H C1H C6H 118.09(18) . . ? C2H C1H P4 121.65(14) . . ? C6H C1H P4 120.10(15) . . ? C1H C2H C3H 121.0(2) . . ? C4H C3H C2H 120.1(2) . . ? C3H C4H C5H 119.8(2) . . ? C4H C5H C6H 120.6(2) . . ? C5H C6H C1H 120.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.496 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.066 # Attachment '6101.cif' data_6101 _database_code_depnum_ccdc_archive 'CCDC 620354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C118 H104 Cl4 N2 O P8 Pt Ru2' _chemical_formula_weight 2352.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1772(16) _cell_length_b 31.291(5) _cell_length_c 17.958(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.706(4) _cell_angle_gamma 90.00 _cell_volume 5667.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4281 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.28 _exptl_crystal_description Rod _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.7672 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32602 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9949 _reflns_number_gt 7790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0684P)^2^+2.5576P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9949 _refine_ls_number_parameters 638 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.107 _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 0.5000 0.5000 0.0000 0.04720(14) Uani 1 2 d S . . Ru1 Ru 0.49980(5) 0.320783(15) 0.41792(3) 0.03446(15) Uani 1 1 d . . . P1 P 0.70849(17) 0.35062(6) 0.45250(9) 0.0417(4) Uani 1 1 d . . . P2 P 0.65537(17) 0.27765(5) 0.36756(9) 0.0394(4) Uani 1 1 d . . . P3 P 0.35197(16) 0.36342(5) 0.47496(9) 0.0370(4) Uani 1 1 d . . . P4 P 0.28360(17) 0.29481(5) 0.38175(9) 0.0426(4) Uani 1 1 d . . . Cl1 Cl 0.4799(3) 0.44827(7) -0.09041(11) 0.0996(9) Uani 1 1 d . . . Cl2 Cl 0.4983(2) 0.27417(7) 0.52784(11) 0.0706(6) Uani 1 1 d . . . N1 N 0.4826(6) 0.45554(18) 0.0796(3) 0.0496(14) Uani 1 1 d . . . C1 C 0.4857(6) 0.35408(19) 0.3241(3) 0.0368(14) Uani 1 1 d . . . C2 C 0.4774(7) 0.3731(2) 0.2645(4) 0.0487(17) Uani 1 1 d . . . C3 C 0.5615(8) 0.4216(2) 0.0885(4) 0.062(2) Uani 1 1 d . . . H3 H 0.6203 0.4169 0.0539 0.074 Uiso 1 1 calc R . . C4 C 0.5599(8) 0.3932(2) 0.1468(4) 0.065(2) Uani 1 1 d . . . H4 H 0.6163 0.3697 0.1502 0.078 Uiso 1 1 calc R . . C5 C 0.4755(7) 0.3989(2) 0.2007(3) 0.0490(17) Uani 1 1 d . . . C6 C 0.3894(8) 0.4336(3) 0.1871(5) 0.075(3) Uani 1 1 d . . . H6 H 0.3253 0.4382 0.2186 0.090 Uiso 1 1 calc R . . C7 C 0.3977(8) 0.4608(3) 0.1285(4) 0.073(3) Uani 1 1 d . . . H7 H 0.3409 0.4842 0.1227 0.088 Uiso 1 1 calc R . . C8 C 0.8022(6) 0.3098(2) 0.4063(4) 0.0469(16) Uani 1 1 d . . . H8A H 0.8637 0.2939 0.4419 0.056 Uiso 1 1 calc R . . H8B H 0.8484 0.3219 0.3673 0.056 Uiso 1 1 calc R . . C9 C 0.2135(6) 0.3252(2) 0.4548(3) 0.0424(15) Uani 1 1 d . . . H9A H 0.2016 0.3078 0.4980 0.051 Uiso 1 1 calc R . . H9B H 0.1308 0.3392 0.4357 0.051 Uiso 1 1 calc R . . C1A C 0.7924(7) 0.3544(3) 0.5489(4) 0.060(2) Uani 1 1 d . . . C2A C 0.9249(9) 0.3630(4) 0.5650(5) 0.108(4) Uani 1 1 d . . . H2A H 0.9758 0.3662 0.5260 0.129 Uiso 1 1 calc R . . C3A C 0.9832(12) 0.3672(5) 0.6379(7) 0.147(6) Uani 1 1 d . . . H3A H 1.0731 0.3736 0.6478 0.177 Uiso 1 1 calc R . . C4A C 0.9121(13) 0.3621(5) 0.6952(6) 0.128(5) Uani 1 1 d . . . H4A H 0.9530 0.3648 0.7445 0.154 Uiso 1 1 calc R . . C5A C 0.7821(12) 0.3530(5) 0.6816(5) 0.131(5) Uani 1 1 d . . . H5A H 0.7333 0.3497 0.7214 0.157 Uiso 1 1 calc R . . C6A C 0.7202(8) 0.3485(3) 0.6082(4) 0.077(3) Uani 1 1 d . . . H6A H 0.6306 0.3415 0.5990 0.093 Uiso 1 1 calc R . . C1B C 0.7448(7) 0.4020(2) 0.4122(4) 0.0521(18) Uani 1 1 d . . . C2B C 0.7316(9) 0.4387(3) 0.4514(6) 0.088(3) Uani 1 1 d . . . H2B H 0.7157 0.4369 0.5011 0.105 Uiso 1 1 calc R . . C3B C 0.7412(12) 0.4781(4) 0.4196(9) 0.114(4) Uani 1 1 d . . . H3B H 0.7326 0.5028 0.4473 0.137 Uiso 1 1 calc R . . C4B C 0.7633(13) 0.4804(4) 0.3472(10) 0.127(5) Uani 1 1 d . . . H4B H 0.7675 0.5072 0.3253 0.152 Uiso 1 1 calc R . . C5B C 0.7799(10) 0.4446(4) 0.3044(7) 0.103(4) Uani 1 1 d . . . H5B H 0.7978 0.4469 0.2551 0.124 Uiso 1 1 calc R . . C6B C 0.7688(9) 0.4050(3) 0.3383(5) 0.076(2) Uani 1 1 d . . . H6B H 0.7777 0.3802 0.3109 0.091 Uiso 1 1 calc R . . C1C C 0.6971(6) 0.2233(2) 0.4003(4) 0.0406(15) Uani 1 1 d . . . C2C C 0.6756(7) 0.1889(2) 0.3536(4) 0.0564(19) Uani 1 1 d . . . H2C H 0.6422 0.1932 0.3033 0.068 Uiso 1 1 calc R . . C3C C 0.7022(8) 0.1478(3) 0.3791(5) 0.072(2) Uani 1 1 d . . . H3C H 0.6868 0.1247 0.3466 0.086 Uiso 1 1 calc R . . C4C C 0.7525(9) 0.1414(3) 0.4542(6) 0.075(2) Uani 1 1 d . . . H4C H 0.7710 0.1139 0.4722 0.091 Uiso 1 1 calc R . . C5C C 0.7746(9) 0.1754(3) 0.5014(5) 0.072(2) Uani 1 1 d . . . H5C H 0.8078 0.1712 0.5517 0.086 Uiso 1 1 calc R . . C6C C 0.7477(7) 0.2161(2) 0.4744(4) 0.059(2) Uani 1 1 d . . . H6C H 0.7639 0.2393 0.5068 0.071 Uiso 1 1 calc R . . C1D C 0.6550(7) 0.2737(2) 0.2675(4) 0.0491(17) Uani 1 1 d . . . C2D C 0.7672(9) 0.2760(3) 0.2313(5) 0.074(2) Uani 1 1 d . . . H2D H 0.8500 0.2804 0.2590 0.089 Uiso 1 1 calc R . . C3D C 0.7560(12) 0.2717(3) 0.1543(6) 0.091(3) Uani 1 1 d . . . H3D H 0.8319 0.2729 0.1308 0.109 Uiso 1 1 calc R . . C4D C 0.6367(13) 0.2658(3) 0.1124(5) 0.091(3) Uani 1 1 d . . . H4D H 0.6312 0.2632 0.0605 0.110 Uiso 1 1 calc R . . C5D C 0.5240(11) 0.2635(4) 0.1462(5) 0.101(4) Uani 1 1 d . . . H5D H 0.4420 0.2589 0.1177 0.121 Uiso 1 1 calc R . . C6D C 0.5343(9) 0.2683(3) 0.2231(4) 0.072(2) Uani 1 1 d . . . H6D H 0.4574 0.2678 0.2459 0.086 Uiso 1 1 calc R . . C1E C 0.3698(6) 0.3737(2) 0.5753(3) 0.0432(15) Uani 1 1 d . . . C2E C 0.4205(8) 0.4128(3) 0.6033(4) 0.067(2) Uani 1 1 d . . . H2E H 0.4384 0.4343 0.5703 0.080 Uiso 1 1 calc R . . C3E C 0.4443(11) 0.4198(3) 0.6798(5) 0.091(3) Uani 1 1 d . . . H3E H 0.4765 0.4461 0.6980 0.110 Uiso 1 1 calc R . . C4E C 0.4208(10) 0.3881(3) 0.7293(5) 0.081(3) Uani 1 1 d . . . H4E H 0.4380 0.3929 0.7807 0.098 Uiso 1 1 calc R . . C5E C 0.3731(9) 0.3503(3) 0.7035(4) 0.074(2) Uani 1 1 d . . . H5E H 0.3581 0.3288 0.7372 0.089 Uiso 1 1 calc R . . C6E C 0.3461(7) 0.3428(3) 0.6271(4) 0.059(2) Uani 1 1 d . . . H6E H 0.3114 0.3166 0.6101 0.070 Uiso 1 1 calc R . . C1F C 0.2924(7) 0.4149(2) 0.4361(4) 0.0464(16) Uani 1 1 d . . . C2F C 0.1692(8) 0.4298(3) 0.4448(6) 0.078(3) Uani 1 1 d . . . H2F H 0.1139 0.4137 0.4710 0.093 Uiso 1 1 calc R . . C3F C 0.1263(12) 0.4692(4) 0.4143(8) 0.117(5) Uani 1 1 d . . . H3F H 0.0407 0.4786 0.4180 0.141 Uiso 1 1 calc R . . C4F C 0.2083(18) 0.4935(4) 0.3798(7) 0.122(5) Uani 1 1 d . . . H4F H 0.1804 0.5202 0.3613 0.146 Uiso 1 1 calc R . . C5F C 0.3321(16) 0.4793(3) 0.3718(6) 0.120(4) Uani 1 1 d . . . H5F H 0.3883 0.4962 0.3474 0.144 Uiso 1 1 calc R . . C6F C 0.3739(9) 0.4399(2) 0.3997(5) 0.070(2) Uani 1 1 d . . . H6F H 0.4583 0.4302 0.3938 0.083 Uiso 1 1 calc R . . C1G C 0.2350(7) 0.2393(2) 0.3908(4) 0.0566(19) Uani 1 1 d . . . C2G C 0.1038(8) 0.2272(3) 0.3889(5) 0.066(2) Uani 1 1 d . . . H2G H 0.0377 0.2479 0.3827 0.080 Uiso 1 1 calc R . . C3G C 0.0698(10) 0.1856(3) 0.3960(5) 0.084(3) Uani 1 1 d . . . H3G H -0.0189 0.1780 0.3939 0.101 Uiso 1 1 calc R . . C4G C 0.1667(12) 0.1545(3) 0.4062(6) 0.096(3) Uani 1 1 d . . . H4G H 0.1434 0.1261 0.4123 0.115 Uiso 1 1 calc R . . C5G C 0.2951(12) 0.1653(3) 0.4072(7) 0.103(3) Uani 1 1 d . . . H5G H 0.3598 0.1441 0.4129 0.124 Uiso 1 1 calc R . . C6G C 0.3322(9) 0.2084(3) 0.3998(6) 0.083(3) Uani 1 1 d . . . H6G H 0.4209 0.2158 0.4011 0.099 Uiso 1 1 calc R . . C1H C 0.1874(7) 0.3117(2) 0.2937(4) 0.0535(18) Uani 1 1 d . . . C2H C 0.1342(9) 0.3523(3) 0.2844(5) 0.080(3) Uani 1 1 d . . . H2H H 0.1421 0.3710 0.3250 0.096 Uiso 1 1 calc R . . C3H C 0.0692(12) 0.3659(4) 0.2151(6) 0.111(4) Uani 1 1 d . . . H3H H 0.0334 0.3932 0.2098 0.134 Uiso 1 1 calc R . . C4H C 0.0583(13) 0.3392(5) 0.1559(6) 0.113(4) Uani 1 1 d . . . H4H H 0.0140 0.3482 0.1099 0.135 Uiso 1 1 calc R . . C5H C 0.1097(11) 0.3005(4) 0.1622(5) 0.096(4) Uani 1 1 d . . . H5H H 0.1036 0.2831 0.1199 0.115 Uiso 1 1 calc R . . C6H C 0.1740(9) 0.2848(3) 0.2316(5) 0.076(3) Uani 1 1 d . . . H6H H 0.2066 0.2570 0.2355 0.091 Uiso 1 1 calc R . . O1S O 1.024(4) 0.4910(10) 0.170(2) 0.263(15) Uani 0.50 1 d PDU . . C1S C 0.904(4) 0.4940(12) 0.124(2) 0.236(19) Uani 0.50 1 d PDU . . H1S1 H 0.8312 0.4959 0.1534 0.283 Uiso 0.50 1 calc PR . . H1S2 H 0.8907 0.4694 0.0911 0.283 Uiso 0.50 1 calc PR . . C2S C 0.916(4) 0.5352(12) 0.078(2) 0.27(2) Uani 0.50 1 d PDU . . H2S1 H 0.8400 0.5537 0.0812 0.329 Uiso 0.50 1 calc PR . . H2S2 H 0.9212 0.5287 0.0261 0.329 Uiso 0.50 1 calc PR . . C3S C 1.050(4) 0.5571(10) 0.118(2) 0.243(19) Uani 0.50 1 d PDU . . H3S1 H 1.1178 0.5570 0.0845 0.291 Uiso 0.50 1 calc PR . . H3S2 H 1.0347 0.5863 0.1326 0.291 Uiso 0.50 1 calc PR . . C4S C 1.091(4) 0.5290(13) 0.186(2) 0.26(2) Uani 0.50 1 d PDU . . H4S1 H 1.1857 0.5244 0.1938 0.307 Uiso 0.50 1 calc PR . . H4S2 H 1.0647 0.5420 0.2311 0.307 Uiso 0.50 1 calc PR . . 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 0.0818(3) 0.0338(2) 0.0275(2) 0.00931(15) 0.01297(18) 0.00430(18) Ru1 0.0471(3) 0.0310(3) 0.0272(3) 0.0064(2) 0.0124(2) 0.0035(2) P1 0.0495(10) 0.0427(10) 0.0339(9) -0.0009(7) 0.0089(8) 0.0049(8) P2 0.0517(10) 0.0365(9) 0.0321(8) 0.0018(7) 0.0132(8) 0.0044(7) P3 0.0457(9) 0.0351(9) 0.0322(8) 0.0003(7) 0.0124(7) 0.0004(7) P4 0.0555(10) 0.0353(10) 0.0399(9) -0.0038(7) 0.0174(8) -0.0046(8) Cl1 0.210(3) 0.0462(13) 0.0434(11) -0.0039(9) 0.0207(15) -0.0023(15) Cl2 0.1086(16) 0.0615(13) 0.0487(10) 0.0297(9) 0.0358(11) 0.0284(11) N1 0.078(4) 0.043(3) 0.029(3) 0.018(2) 0.012(3) 0.009(3) C1 0.040(3) 0.035(3) 0.036(3) 0.008(3) 0.006(3) 0.003(3) C2 0.059(4) 0.044(4) 0.045(4) 0.011(3) 0.016(3) 0.000(3) C3 0.101(6) 0.050(5) 0.039(4) 0.021(3) 0.030(4) 0.017(4) C4 0.093(6) 0.053(5) 0.055(5) 0.024(4) 0.027(4) 0.024(4) C5 0.068(4) 0.048(4) 0.032(3) 0.013(3) 0.009(3) -0.005(3) C6 0.086(6) 0.078(6) 0.067(5) 0.039(5) 0.039(5) 0.027(5) C7 0.091(6) 0.074(6) 0.062(5) 0.037(4) 0.035(5) 0.035(5) C8 0.041(4) 0.043(4) 0.059(4) -0.002(3) 0.015(3) 0.001(3) C9 0.051(4) 0.043(4) 0.035(3) -0.002(3) 0.014(3) -0.002(3) C1A 0.051(4) 0.086(6) 0.042(4) -0.005(4) 0.006(3) 0.009(4) C2A 0.059(6) 0.204(13) 0.060(6) -0.032(7) 0.009(5) -0.001(7) C3A 0.080(7) 0.276(19) 0.077(8) -0.037(10) -0.023(7) 0.033(9) C4A 0.102(9) 0.216(15) 0.058(7) -0.014(8) -0.021(6) 0.046(9) C5A 0.102(9) 0.243(16) 0.046(6) -0.004(8) 0.003(6) 0.029(9) C6A 0.065(5) 0.128(8) 0.037(4) 0.003(5) -0.002(4) 0.014(5) C1B 0.053(4) 0.036(4) 0.066(5) -0.008(3) 0.002(4) 0.002(3) C2B 0.102(7) 0.047(6) 0.111(8) -0.007(5) 0.003(6) 0.012(5) C3B 0.131(10) 0.057(7) 0.143(12) -0.010(8) -0.029(9) 0.000(6) C4B 0.140(11) 0.054(7) 0.171(14) 0.036(9) -0.036(11) -0.033(7) C5B 0.115(8) 0.089(8) 0.103(8) 0.041(7) 0.007(7) -0.030(7) C6B 0.098(6) 0.056(5) 0.074(6) 0.006(4) 0.013(5) -0.024(5) C1C 0.042(4) 0.036(4) 0.045(4) 0.000(3) 0.011(3) 0.010(3) C2C 0.066(5) 0.044(4) 0.057(5) -0.003(4) 0.002(4) 0.006(4) C3C 0.082(6) 0.045(5) 0.088(7) -0.010(4) 0.013(5) 0.000(4) C4C 0.091(6) 0.046(5) 0.095(7) 0.024(5) 0.029(5) 0.019(4) C5C 0.091(6) 0.068(6) 0.056(5) 0.016(4) 0.007(5) 0.026(5) C6C 0.073(5) 0.052(5) 0.052(5) 0.005(4) 0.010(4) 0.013(4) C1D 0.066(5) 0.048(4) 0.036(4) 0.005(3) 0.020(4) 0.023(3) C2D 0.092(6) 0.085(7) 0.052(5) -0.002(4) 0.031(5) 0.014(5) C3D 0.131(9) 0.082(7) 0.073(7) -0.010(5) 0.066(7) -0.002(6) C4D 0.148(10) 0.087(7) 0.044(5) 0.006(5) 0.030(6) 0.043(7) C5D 0.105(8) 0.128(9) 0.062(6) -0.012(6) -0.016(6) 0.051(7) C6D 0.081(6) 0.097(7) 0.041(4) -0.011(4) 0.016(4) 0.025(5) C1E 0.054(4) 0.046(4) 0.030(3) -0.002(3) 0.006(3) 0.001(3) C2E 0.094(6) 0.058(5) 0.045(4) 0.002(4) -0.001(4) -0.021(4) C3E 0.148(9) 0.064(6) 0.056(5) -0.017(5) -0.007(6) -0.028(6) C4E 0.117(7) 0.089(7) 0.036(4) -0.005(5) 0.003(5) 0.000(6) C5E 0.109(7) 0.080(7) 0.036(4) 0.008(4) 0.017(4) -0.016(5) C6E 0.067(5) 0.077(6) 0.033(4) -0.007(4) 0.014(3) -0.010(4) C1F 0.057(4) 0.040(4) 0.042(4) 0.000(3) 0.003(3) 0.013(3) C2F 0.060(5) 0.055(5) 0.118(8) -0.006(5) 0.007(5) 0.008(4) C3F 0.092(8) 0.074(8) 0.172(13) -0.019(8) -0.030(8) 0.039(6) C4F 0.196(15) 0.062(8) 0.094(9) -0.007(6) -0.028(9) 0.061(9) C5F 0.224(15) 0.052(6) 0.096(8) 0.027(6) 0.069(9) 0.023(8) C6F 0.096(6) 0.042(5) 0.079(6) 0.017(4) 0.041(5) 0.017(4) C1G 0.069(5) 0.046(4) 0.062(5) -0.012(4) 0.031(4) -0.013(4) C2G 0.062(5) 0.063(5) 0.079(6) -0.008(4) 0.030(4) -0.012(4) C3G 0.096(7) 0.069(7) 0.092(7) -0.007(5) 0.032(6) -0.044(6) C4G 0.124(9) 0.045(6) 0.124(9) 0.008(5) 0.034(7) -0.036(6) C5G 0.120(9) 0.043(6) 0.153(11) 0.000(6) 0.039(8) 0.000(5) C6G 0.081(6) 0.042(5) 0.133(9) 0.005(5) 0.044(6) -0.008(4) C1H 0.063(4) 0.054(5) 0.045(4) -0.011(3) 0.014(4) -0.020(4) C2H 0.112(7) 0.064(6) 0.058(5) -0.001(4) -0.014(5) -0.004(5) C3H 0.148(10) 0.097(8) 0.076(7) 0.020(6) -0.031(7) -0.014(7) C4H 0.144(11) 0.126(11) 0.061(7) -0.009(7) -0.013(7) -0.018(9) C5H 0.114(8) 0.135(10) 0.041(5) -0.037(6) 0.017(5) -0.050(8) C6H 0.085(6) 0.084(7) 0.062(6) -0.032(5) 0.021(5) -0.023(5) O1S 0.25(2) 0.27(3) 0.26(3) 0.08(2) -0.02(2) -0.04(2) C1S 0.20(3) 0.28(3) 0.23(3) 0.11(2) 0.02(2) -0.05(2) C2S 0.30(3) 0.23(3) 0.30(3) 0.00(3) 0.04(3) 0.03(3) C3S 0.26(3) 0.22(3) 0.23(3) 0.01(2) -0.02(2) -0.02(2) C4S 0.30(3) 0.22(3) 0.24(3) 0.00(3) 0.01(3) -0.02(3) _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 N1 2.020(5) 3_665 ? Pt1 N1 2.020(5) . ? Pt1 Cl1 2.282(2) . ? Pt1 Cl1 2.282(2) 3_665 ? Ru1 C1 1.970(6) . ? Ru1 P1 2.3269(18) . ? Ru1 P3 2.3465(17) . ? Ru1 P2 2.3516(17) . ? Ru1 P4 2.3538(18) . ? Ru1 Cl2 2.4560(17) . ? P1 C1B 1.821(7) . ? P1 C1A 1.828(7) . ? P1 C8 1.854(7) . ? P2 C1D 1.801(7) . ? P2 C1C 1.831(6) . ? P2 C8 1.859(6) . ? P3 C1E 1.816(6) . ? P3 C1F 1.827(7) . ? P3 C9 1.846(6) . ? P4 C1G 1.818(7) . ? P4 C1H 1.822(8) . ? P4 C9 1.840(6) . ? N1 C7 1.321(9) . ? N1 C3 1.328(9) . ? C1 C2 1.217(8) . ? C2 C5 1.399(9) . ? C3 C4 1.376(9) . ? C4 C5 1.389(10) . ? C5 C6 1.396(10) . ? C6 C7 1.366(10) . ? C1A C2A 1.368(11) . ? C1A C6A 1.386(10) . ? C2A C3A 1.369(13) . ? C3A C4A 1.346(16) . ? C4A C5A 1.343(15) . ? C5A C6A 1.389(12) . ? C1B C2B 1.363(11) . ? C1B C6B 1.385(11) . ? C2B C3B 1.367(14) . ? C3B C4B 1.351(18) . ? C4B C5B 1.381(17) . ? C5B C6B 1.394(12) . ? C1C C2C 1.365(9) . ? C1C C6C 1.380(9) . ? C2C C3C 1.380(10) . ? C3C C4C 1.391(12) . ? C4C C5C 1.359(12) . ? C5C C6C 1.378(10) . ? C1D C6D 1.382(10) . ? C1D C2D 1.390(10) . ? C2D C3D 1.377(12) . ? C3D C4D 1.353(13) . ? C4D C5D 1.369(14) . ? C5D C6D 1.380(11) . ? C1E C6E 1.385(10) . ? C1E C2E 1.394(9) . ? C2E C3E 1.380(11) . ? C3E C4E 1.373(12) . ? C4E C5E 1.339(12) . ? C5E C6E 1.383(10) . ? C1F C2F 1.365(10) . ? C1F C6F 1.369(10) . ? C2F C3F 1.393(14) . ? C3F C4F 1.340(18) . ? C4F C5F 1.361(18) . ? C5F C6F 1.377(12) . ? C1G C6G 1.378(11) . ? C1G C2G 1.385(10) . ? C2G C3G 1.358(11) . ? C3G C4G 1.379(13) . ? C4G C5G 1.346(14) . ? C5G C6G 1.412(11) . ? C1H C2H 1.384(11) . ? C1H C6H 1.389(10) . ? C2H C3H 1.395(12) . ? C3H C4H 1.343(15) . ? C4H C5H 1.318(15) . ? C5H C6H 1.416(13) . ? O1S C4S 1.377(18) . ? O1S C1S 1.384(18) . ? C1S C2S 1.541(17) . ? C2S C3S 1.608(18) . ? C3S C4S 1.522(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.0(3) 3_665 . ? N1 Pt1 Cl1 89.58(18) 3_665 . ? N1 Pt1 Cl1 90.42(18) . . ? N1 Pt1 Cl1 90.42(18) 3_665 3_665 ? N1 Pt1 Cl1 89.58(18) . 3_665 ? Cl1 Pt1 Cl1 180.00(10) . 3_665 ? C1 Ru1 P1 88.59(18) . . ? C1 Ru1 P3 95.46(18) . . ? P1 Ru1 P3 105.73(6) . . ? C1 Ru1 P2 87.15(18) . . ? P1 Ru1 P2 72.26(6) . . ? P3 Ru1 P2 176.70(6) . . ? C1 Ru1 P4 89.32(17) . . ? P1 Ru1 P4 176.54(6) . . ? P3 Ru1 P4 71.73(6) . . ? P2 Ru1 P4 110.39(6) . . ? C1 Ru1 Cl2 173.71(18) . . ? P1 Ru1 Cl2 97.32(7) . . ? P3 Ru1 Cl2 85.03(6) . . ? P2 Ru1 Cl2 92.59(6) . . ? P4 Ru1 Cl2 84.87(7) . . ? C1B P1 C1A 103.0(4) . . ? C1B P1 C8 106.6(3) . . ? C1A P1 C8 105.4(3) . . ? C1B P1 Ru1 118.3(2) . . ? C1A P1 Ru1 124.9(3) . . ? C8 P1 Ru1 96.4(2) . . ? C1D P2 C1C 103.0(3) . . ? C1D P2 C8 107.8(3) . . ? C1C P2 C8 104.1(3) . . ? C1D P2 Ru1 120.8(2) . . ? C1C P2 Ru1 123.3(2) . . ? C8 P2 Ru1 95.4(2) . . ? C1E P3 C1F 101.9(3) . . ? C1E P3 C9 106.4(3) . . ? C1F P3 C9 106.9(3) . . ? C1E P3 Ru1 123.3(2) . . ? C1F P3 Ru1 122.3(2) . . ? C9 P3 Ru1 93.6(2) . . ? C1G P4 C1H 103.5(3) . . ? C1G P4 C9 107.1(3) . . ? C1H P4 C9 104.7(3) . . ? C1G P4 Ru1 124.1(3) . . ? C1H P4 Ru1 120.9(2) . . ? C9 P4 Ru1 93.6(2) . . ? C7 N1 C3 117.3(6) . . ? C7 N1 Pt1 120.8(5) . . ? C3 N1 Pt1 121.8(5) . . ? C2 C1 Ru1 177.3(6) . . ? C1 C2 C5 173.3(8) . . ? N1 C3 C4 122.6(7) . . ? C3 C4 C5 121.3(7) . . ? C4 C5 C6 114.2(6) . . ? C4 C5 C2 123.6(7) . . ? C6 C5 C2 122.1(7) . . ? C7 C6 C5 121.2(7) . . ? N1 C7 C6 123.2(7) . . ? P1 C8 P2 96.0(3) . . ? P4 C9 P3 96.7(3) . . ? C2A C1A C6A 118.3(7) . . ? C2A C1A P1 122.3(6) . . ? C6A C1A P1 119.4(6) . . ? C1A C2A C3A 120.7(10) . . ? C4A C3A C2A 120.8(11) . . ? C5A C4A C3A 120.2(10) . . ? C4A C5A C6A 120.4(10) . . ? C1A C6A C5A 119.7(9) . . ? C2B C1B C6B 118.7(8) . . ? C2B C1B P1 119.9(7) . . ? C6B C1B P1 120.8(6) . . ? C1B C2B C3B 121.8(11) . . ? C4B C3B C2B 118.8(12) . . ? C3B C4B C5B 122.7(11) . . ? C4B C5B C6B 117.1(11) . . ? C1B C6B C5B 120.9(9) . . ? C2C C1C C6C 118.3(6) . . ? C2C C1C P2 121.6(5) . . ? C6C C1C P2 120.1(5) . . ? C1C C2C C3C 121.5(7) . . ? C2C C3C C4C 119.0(8) . . ? C5C C4C C3C 120.1(8) . . ? C4C C5C C6C 119.7(8) . . ? C5C C6C C1C 121.4(7) . . ? C6D C1D C2D 117.3(7) . . ? C6D C1D P2 117.8(5) . . ? C2D C1D P2 124.9(6) . . ? C3D C2D C1D 120.1(9) . . ? C4D C3D C2D 121.3(9) . . ? C3D C4D C5D 120.2(8) . . ? C4D C5D C6D 118.9(9) . . ? C5D C6D C1D 122.2(8) . . ? C6E C1E C2E 117.4(6) . . ? C6E C1E P3 122.6(5) . . ? C2E C1E P3 119.8(5) . . ? C3E C2E C1E 120.3(7) . . ? C4E C3E C2E 120.5(8) . . ? C5E C4E C3E 120.1(8) . . ? C4E C5E C6E 120.4(8) . . ? C5E C6E C1E 121.3(7) . . ? C2F C1F C6F 118.9(7) . . ? C2F C1F P3 121.4(6) . . ? C6F C1F P3 119.7(5) . . ? C1F C2F C3F 120.1(10) . . ? C4F C3F C2F 120.0(11) . . ? C3F C4F C5F 120.5(11) . . ? C4F C5F C6F 119.9(12) . . ? C1F C6F C5F 120.5(9) . . ? C6G C1G C2G 119.0(7) . . ? C6G C1G P4 118.8(6) . . ? C2G C1G P4 122.2(6) . . ? C3G C2G C1G 121.1(9) . . ? C2G C3G C4G 120.1(9) . . ? C5G C4G C3G 120.1(9) . . ? C4G C5G C6G 120.6(10) . . ? C1G C6G C5G 119.1(8) . . ? C2H C1H C6H 117.7(8) . . ? C2H C1H P4 121.8(6) . . ? C6H C1H P4 120.3(7) . . ? C1H C2H C3H 121.2(9) . . ? C4H C3H C2H 119.7(11) . . ? C5H C4H C3H 120.8(11) . . ? C4H C5H C6H 121.7(9) . . ? C1H C6H C5H 118.7(9) . . ? C4S O1S C1S 116(2) . . ? O1S C1S C2S 104.7(13) . . ? C1S C2S C3S 104.0(11) . . ? C4S C3S C2S 103.4(12) . . ? O1S C4S C3S 105.0(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.106 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.108 data_5437 _database_code_depnum_ccdc_archive 'CCDC 672307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H51 F6 N2 O2.50 P5 Ru' _chemical_formula_weight 1197.94 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 25.6097(6) _cell_length_b 25.6097(6) _cell_length_c 27.9465(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18328.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7955 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 19.45 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4896 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53176 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8072 _reflns_number_gt 6305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1924P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 8072 _refine_ls_number_parameters 316 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2629 _refine_ls_wR_factor_gt 0.2398 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.092 _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 Ru1 Ru 0.7500 0.99489(3) 0.8750 0.0524(2) Uani 1 2 d S . . P2 P 0.78077(7) 0.98923(7) 0.95457(6) 0.0592(5) Uani 1 1 d . . . P1 P 0.65838(6) 0.99344(7) 0.87581(6) 0.0562(4) Uani 1 1 d . . . N2 N 0.7500 1.0750(3) 0.8750 0.0561(17) Uani 1 2 d S . . C1 C 0.7500 0.9151(4) 0.8750 0.062(2) Uani 1 2 d S . . C2 C 0.7500 0.8695(4) 0.8750 0.071(3) Uani 1 2 d S . . C3 C 0.7500 0.8130(4) 0.8750 0.097(4) Uani 1 2 d SDU . . C4 C 0.7238(4) 0.7854(4) 0.9103(3) 0.132(5) Uani 1 1 d DU . . H4 H 0.7064 0.8039 0.9346 0.159 Uiso 1 1 calc R . . C5 C 0.7226(7) 0.7313(5) 0.9109(5) 0.177(8) Uani 1 1 d DU . . H5 H 0.7042 0.7123 0.9342 0.212 Uiso 1 1 calc R . . N1 N 0.7500 0.7076(9) 0.8750 0.236(12) Uani 1 2 d SDU . . C8 C 0.8487(3) 0.9745(3) 0.9376(3) 0.0700(19) Uani 1 1 d . . . H8A H 0.8574 0.9374 0.9416 0.084 Uiso 1 1 calc R . . H8B H 0.8741 0.9962 0.9547 0.084 Uiso 1 1 calc R . . C9 C 0.7500 1.1779(5) 0.8750 0.124(6) Uani 1 2 d S . . H9A H 0.7173 1.1906 0.8619 0.187 Uiso 0.50 1 calc PR . . H9B H 0.7788 1.1906 0.8556 0.187 Uiso 0.50 1 calc PR . . H9C H 0.7539 1.1906 0.9075 0.187 Uiso 0.50 1 calc PR . . C10 C 0.7500 1.1202(4) 0.8750 0.076(3) Uani 1 2 d S . . C1A C 0.61567(17) 0.9495(2) 0.9077(2) 0.0710(19) Uani 1 1 d G . . C2A C 0.56259(19) 0.9509(2) 0.8974(3) 0.095(3) Uani 1 1 d G . . H2A H 0.5494 0.9761 0.8761 0.114 Uiso 1 1 calc R . . C3A C 0.52903(17) 0.9150(3) 0.9185(3) 0.133(5) Uani 1 1 d G . . H3A H 0.4931 0.9159 0.9115 0.160 Uiso 1 1 calc R . . C4A C 0.5485(3) 0.8777(3) 0.9499(3) 0.142(5) Uani 1 1 d G . . H4A H 0.5258 0.8535 0.9642 0.171 Uiso 1 1 calc R . . C5A C 0.6016(3) 0.8764(3) 0.9603(3) 0.148(5) Uani 1 1 d G . . H5A H 0.6148 0.8512 0.9815 0.177 Uiso 1 1 calc R . . C6A C 0.63519(19) 0.9123(3) 0.9391(3) 0.107(4) Uani 1 1 d G . . H6A H 0.6711 0.9113 0.9461 0.128 Uiso 1 1 calc R . . C1B C 0.62667(19) 1.05732(17) 0.8835(2) 0.0683(19) Uani 1 1 d G . . C2B C 0.6154(2) 1.0899(3) 0.8450(2) 0.091(3) Uani 1 1 d G . . H2B H 0.6193 1.0775 0.8135 0.110 Uiso 1 1 calc R . . C3B C 0.5984(3) 1.1407(2) 0.8531(3) 0.116(4) Uani 1 1 d G . . H3B H 0.5908 1.1627 0.8271 0.139 Uiso 1 1 calc R . . C4B C 0.5927(3) 1.15890(17) 0.8997(4) 0.115(4) Uani 1 1 d G . . H4B H 0.5812 1.1932 0.9052 0.138 Uiso 1 1 calc R . . C5B C 0.6040(3) 1.1263(3) 0.9381(3) 0.115(4) Uani 1 1 d G . . H5B H 0.6001 1.1387 0.9696 0.138 Uiso 1 1 calc R . . C6B C 0.6210(2) 1.0756(3) 0.93001(19) 0.092(3) Uani 1 1 d G . . H6B H 0.6286 1.0535 0.9560 0.111 Uiso 1 1 calc R . . C1C C 0.7850(2) 1.04581(18) 0.99393(17) 0.0692(19) Uani 1 1 d G . . C2C C 0.7476(2) 1.0849(2) 0.9909(2) 0.0777(19) Uani 1 1 d G . . H2C H 0.7214 1.0832 0.9674 0.093 Uiso 1 1 calc R . . C3C C 0.7487(3) 1.1266(2) 1.0227(3) 0.121(4) Uani 1 1 d G . . H3C H 0.7234 1.1531 1.0207 0.145 Uiso 1 1 calc R . . C4C C 0.7874(3) 1.1292(3) 1.0575(2) 0.140(5) Uani 1 1 d G . . H4C H 0.7882 1.1574 1.0791 0.168 Uiso 1 1 calc R . . C5C C 0.8249(3) 1.0901(3) 1.0606(2) 0.123(4) Uani 1 1 d G . . H5C H 0.8510 1.0919 1.0841 0.148 Uiso 1 1 calc R . . C6C C 0.82370(19) 1.0484(2) 1.02876(19) 0.074(2) Uani 1 1 d G . . H6C H 0.8491 1.0219 1.0308 0.089 Uiso 1 1 calc R . . C1D C 0.7604(2) 0.93815(19) 0.99730(19) 0.073(2) Uani 1 1 d G . . C2D C 0.7758(2) 0.8866(2) 0.9909(2) 0.087(2) Uani 1 1 d G . . H2D H 0.7983 0.8778 0.9656 0.104 Uiso 1 1 calc R . . C3D C 0.7580(3) 0.84810(18) 1.0219(3) 0.104(3) Uani 1 1 d G . . H3D H 0.7685 0.8132 1.0176 0.125 Uiso 1 1 calc R . . C4D C 0.7248(3) 0.8612(3) 1.0594(3) 0.114(4) Uani 1 1 d G . . H4D H 0.7127 0.8351 1.0804 0.136 Uiso 1 1 calc R . . C5D C 0.7093(3) 0.9127(3) 1.0658(2) 0.144(5) Uani 1 1 d G . . H5D H 0.6868 0.9215 1.0911 0.173 Uiso 1 1 calc R . . C6D C 0.7271(3) 0.9512(2) 1.0347(2) 0.102(3) Uani 1 1 d G . . H6D H 0.7166 0.9861 1.0391 0.123 Uiso 1 1 calc R . . P7 P 0.6994(4) 0.6935(4) 1.0464(4) 0.104(4) Uani 0.25 1 d PD . . F3 F 0.6847(8) 0.6587(7) 1.0043(6) 0.136(9) Uiso 0.25 1 d PD . . F4 F 0.7101(10) 0.7291(7) 1.0888(6) 0.111(7) Uiso 0.25 1 d PD . . F5 F 0.7476(7) 0.7090(9) 1.0189(9) 0.179(13) Uiso 0.25 1 d PD . . F8 F 0.6707(8) 0.7369(6) 1.0235(7) 0.146(10) Uiso 0.25 1 d PD . . F7 F 0.6487(7) 0.6762(9) 1.0699(8) 0.154(11) Uiso 0.25 1 d PD . . F6 F 0.7268(8) 0.6515(7) 1.0686(7) 0.165(12) Uiso 0.25 1 d PD . . P6 P 1.0000 1.0000 1.0000 0.0569(7) Uani 1 4 d S . . F1 F 1.0000 1.0000 1.0549(3) 0.208(7) Uani 1 2 d S . . F2 F 0.9579(2) 0.9550(2) 0.9970(3) 0.130(2) Uani 1 1 d . . . O1W O 0.60036(19) 0.5107(2) 0.94766(18) 0.0804(15) Uani 1 1 d . . . O2W O 0.4982(9) 0.5308(7) 0.9891(6) 0.067(4) Uiso 0.25 1 d P . . 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 Ru1 0.0454(4) 0.0532(4) 0.0586(4) 0.000 -0.0097(3) 0.000 P2 0.0523(9) 0.0658(11) 0.0594(9) 0.0016(8) -0.0105(7) -0.0023(8) P1 0.0473(8) 0.0591(9) 0.0622(9) 0.0022(10) -0.0091(7) -0.0040(6) N2 0.035(3) 0.069(5) 0.064(5) 0.000 -0.008(4) 0.000 C1 0.047(5) 0.078(7) 0.062(6) 0.000 -0.022(5) 0.000 C2 0.095(7) 0.050(5) 0.069(6) 0.000 -0.028(6) 0.000 C3 0.129(10) 0.061(6) 0.100(9) 0.000 -0.063(9) 0.000 C4 0.178(12) 0.069(6) 0.149(9) 0.021(6) -0.079(9) -0.035(7) C5 0.25(2) 0.100(10) 0.183(16) 0.036(10) -0.048(14) -0.041(11) N1 0.32(3) 0.125(15) 0.26(3) 0.000 -0.11(2) 0.000 C8 0.057(4) 0.086(5) 0.068(4) 0.002(4) -0.008(3) 0.008(4) C9 0.109(11) 0.054(6) 0.209(19) 0.000 -0.054(13) 0.000 C10 0.063(6) 0.062(6) 0.104(8) 0.000 -0.023(6) 0.000 C1A 0.056(4) 0.066(4) 0.091(5) 0.012(4) -0.003(4) -0.011(3) C2A 0.059(5) 0.105(7) 0.120(7) 0.036(5) -0.012(5) -0.012(4) C3A 0.068(6) 0.150(10) 0.183(12) 0.055(9) -0.013(7) -0.041(6) C4A 0.082(7) 0.150(11) 0.195(14) 0.067(10) -0.016(8) -0.038(7) C5A 0.144(12) 0.129(11) 0.172(13) 0.050(10) -0.009(10) -0.042(9) C6A 0.070(5) 0.127(9) 0.123(8) 0.050(7) -0.009(5) -0.023(5) C1B 0.041(3) 0.066(4) 0.098(6) -0.001(4) -0.009(3) -0.001(3) C2B 0.065(5) 0.090(6) 0.119(7) 0.018(5) 0.010(5) 0.014(4) C3B 0.075(6) 0.085(7) 0.187(13) 0.037(8) 0.020(7) 0.009(5) C4B 0.083(7) 0.081(7) 0.181(14) -0.008(8) 0.001(8) -0.013(5) C5B 0.073(6) 0.117(9) 0.156(11) -0.038(8) -0.006(6) -0.002(6) C6B 0.065(5) 0.091(6) 0.121(7) -0.034(5) -0.016(5) 0.011(4) C1C 0.082(5) 0.069(4) 0.056(4) -0.004(3) -0.001(4) -0.020(4) C2C 0.081(5) 0.075(5) 0.077(5) -0.005(4) 0.007(4) 0.004(4) C3C 0.133(9) 0.101(7) 0.128(8) -0.045(6) -0.014(8) 0.022(7) C4C 0.208(16) 0.109(9) 0.104(8) -0.043(7) -0.001(9) -0.051(9) C5C 0.136(10) 0.149(11) 0.083(7) -0.023(7) -0.022(6) -0.072(9) C6C 0.061(4) 0.096(6) 0.065(4) -0.014(4) 0.000(3) -0.017(4) C1D 0.072(5) 0.077(5) 0.072(5) 0.009(4) -0.013(4) -0.008(4) C2D 0.105(7) 0.086(6) 0.069(5) 0.013(4) -0.020(4) -0.002(5) C3D 0.111(8) 0.088(6) 0.112(7) 0.025(6) -0.040(6) -0.020(6) C4D 0.117(9) 0.095(7) 0.129(9) 0.048(7) -0.013(7) -0.033(6) C5D 0.105(9) 0.188(14) 0.138(10) 0.070(10) 0.031(8) -0.019(9) C6D 0.095(7) 0.101(7) 0.111(7) 0.027(6) 0.033(6) 0.007(5) P7 0.103(7) 0.109(8) 0.100(7) 0.048(6) -0.038(6) -0.039(6) P6 0.0549(11) 0.0549(11) 0.0609(17) 0.000 0.000 0.000 F1 0.215(14) 0.33(2) 0.078(5) 0.000 0.000 0.056(15) F2 0.079(3) 0.069(3) 0.241(8) 0.013(4) -0.006(4) -0.017(2) O1W 0.061(3) 0.103(4) 0.078(3) 0.012(3) -0.011(2) 0.023(3) _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 Ru1 C1 2.043(10) . ? Ru1 N2 2.052(8) . ? Ru1 P1 2.3467(16) . ? Ru1 P1 2.3469(16) 5_656 ? Ru1 P2 2.3635(16) 5_656 ? Ru1 P2 2.3636(16) . ? P2 C1C 1.823(4) . ? P2 C8 1.843(7) . ? P2 C1D 1.847(4) . ? P1 C1A 1.804(4) . ? P1 C1B 1.839(4) . ? P1 C8 1.847(7) 5_656 ? N2 C10 1.157(13) . ? C1 C2 1.168(13) . ? C2 C3 1.447(15) . ? C3 C4 1.387(9) 5_656 ? C3 C4 1.387(9) . ? C4 C5 1.386(12) . ? C5 N1 1.365(12) . ? N1 C5 1.365(12) 5_656 ? C8 P1 1.847(7) 5_656 ? C9 C10 1.478(16) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C3B C4B 1.3900 . ? C4B C5B 1.3900 . ? C5B C6B 1.3900 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C3C C4C 1.3900 . ? C4C C5C 1.3900 . ? C5C C6C 1.3900 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? P7 F6 1.425(13) . ? P7 F8 1.480(13) . ? P7 F5 1.507(14) . ? P7 F4 1.520(14) . ? P7 F7 1.521(14) . ? P7 F3 1.522(13) . ? P6 F1 1.533(9) . ? P6 F1 1.533(9) 3_577 ? P6 F2 1.581(5) 3_577 ? P6 F2 1.581(5) . ? P6 F2 1.581(5) 4_757 ? P6 F2 1.581(5) 2_775 ? O2W O2W 1.27(3) 3_567 ? O2W O2W 1.27(3) 4_657 ? O2W O2W 1.58(4) 2_665 ? 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 C1 Ru1 N2 180.000(3) . . ? C1 Ru1 P1 89.09(4) . . ? N2 Ru1 P1 90.91(4) . . ? C1 Ru1 P1 89.09(4) . 5_656 ? N2 Ru1 P1 90.91(4) . 5_656 ? P1 Ru1 P1 178.18(9) . 5_656 ? C1 Ru1 P2 86.48(5) . 5_656 ? N2 Ru1 P2 93.52(5) . 5_656 ? P1 Ru1 P2 71.02(6) . 5_656 ? P1 Ru1 P2 108.86(6) 5_656 5_656 ? C1 Ru1 P2 86.48(5) . . ? N2 Ru1 P2 93.52(5) . . ? P1 Ru1 P2 108.86(6) . . ? P1 Ru1 P2 71.03(6) 5_656 . ? P2 Ru1 P2 172.96(10) 5_656 . ? C1C P2 C8 105.2(3) . . ? C1C P2 C1D 100.9(3) . . ? C8 P2 C1D 106.7(3) . . ? C1C P2 Ru1 122.62(18) . . ? C8 P2 Ru1 94.9(2) . . ? C1D P2 Ru1 123.9(2) . . ? C1A P1 C1B 103.3(3) . . ? C1A P1 C8 104.5(3) . 5_656 ? C1B P1 C8 107.6(3) . 5_656 ? C1A P1 Ru1 128.37(18) . . ? C1B P1 Ru1 115.38(18) . . ? C8 P1 Ru1 95.4(2) 5_656 . ? C10 N2 Ru1 180.000(4) . . ? C2 C1 Ru1 180.000(3) . . ? C1 C2 C3 180.000(7) . . ? C4 C3 C4 118.7(11) 5_656 . ? C4 C3 C2 120.7(5) 5_656 . ? C4 C3 C2 120.7(5) . . ? C5 C4 C3 121.9(9) . . ? N1 C5 C4 115.1(12) . . ? C5 N1 C5 127.3(19) . 5_656 ? P2 C8 P1 95.7(3) . 5_656 ? N2 C10 C9 180.000(8) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 118.3(3) . . ? C6A C1A P1 121.5(3) . . ? C1A C2A C3A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 122.4(4) . . ? C6B C1B P1 117.0(4) . . ? C3B C2B C1B 120.0 . . ? C2B C3B C4B 120.0 . . ? C5B C4B C3B 120.0 . . ? C6B C5B C4B 120.0 . . ? C5B C6B C1B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C P2 119.7(3) . . ? C6C C1C P2 120.2(3) . . ? C3C C2C C1C 120.0 . . ? C2C C3C C4C 120.0 . . ? C5C C4C C3C 120.0 . . ? C4C C5C C6C 120.0 . . ? C5C C6C C1C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D P2 120.6(3) . . ? C6D C1D P2 119.3(3) . . ? C3D C2D C1D 120.0 . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.0 . . ? C4D C5D C6D 120.0 . . ? C5D C6D C1D 120.0 . . ? F6 P7 F8 179.7(12) . . ? F6 P7 F5 91.1(8) . . ? F8 P7 F5 89.2(7) . . ? F6 P7 F4 91.4(7) . . ? F8 P7 F4 88.6(7) . . ? F5 P7 F4 95.3(15) . . ? F6 P7 F7 90.7(8) . . ? F8 P7 F7 89.0(8) . . ? F5 P7 F7 174.8(13) . . ? F4 P7 F7 89.5(16) . . ? F6 P7 F3 91.0(8) . . ? F8 P7 F3 89.0(7) . . ? F5 P7 F3 87.9(9) . . ? F4 P7 F3 176.0(13) . . ? F7 P7 F3 87.3(8) . . ? F1 P6 F1 179.997(2) . 3_577 ? F1 P6 F2 87.0(3) . 3_577 ? F1 P6 F2 93.0(3) 3_577 3_577 ? F1 P6 F2 93.0(3) . . ? F1 P6 F2 87.0(3) 3_577 . ? F2 P6 F2 90.16(4) 3_577 . ? F1 P6 F2 87.0(3) . 4_757 ? F1 P6 F2 93.0(3) 3_577 4_757 ? F2 P6 F2 174.0(7) 3_577 4_757 ? F2 P6 F2 90.15(4) . 4_757 ? F1 P6 F2 93.0(3) . 2_775 ? F1 P6 F2 87.0(3) 3_577 2_775 ? F2 P6 F2 90.15(4) 3_577 2_775 ? F2 P6 F2 174.0(7) . 2_775 ? F2 P6 F2 90.16(4) 4_757 2_775 ? O2W O2W O2W 76.8(12) 3_567 4_657 ? O2W O2W O2W 51.6(6) 3_567 2_665 ? O2W O2W O2W 51.6(6) 4_657 2_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.124 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.154