Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email LMWHITE@CHEM.UFL.EDU _publ_contact_author_name 'Prof Lisa McElwee-White' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry and Center for Catalysis University of Florida P.O. Box 117200 Gainesville FL 32611-7200 UNITED STATES OF AMERICA ; _publ_section_title ; Heterobimetallic complexes with dppm-bridged Ru/Pd, Ru/Pt, Ru/Au and Ru/Cu centers ; loop_ _publ_author_name 'Lisa McElwee-White' 'Khalil A. Abboud' 'Ying Yang' data_yy06 _database_code_CSD 215180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 Cl14 I P3 Pd Ru' _chemical_formula_weight 1594.47 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.4480(13) _cell_length_b 12.2567(14) _cell_length_c 22.402(3) _cell_angle_alpha 98.508(2) _cell_angle_beta 96.142(2) _cell_angle_gamma 90.895(2) _cell_volume 3089.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 149 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.753 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7580 _exptl_absorpt_correction_T_max 0.8572 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 26139 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13243 _reflns_number_gt 10596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0683P)^2^+5.0185P] 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 13243 _refine_ls_number_parameters 689 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.077 _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 0.56023(3) -0.06920(3) 0.276598(15) 0.02181(9) Uani 1 1 d . . . Pd1 Pd 0.57995(3) -0.39816(3) 0.218036(15) 0.02245(9) Uani 1 1 d . . . I1 I 0.64137(3) -0.25461(2) 0.313228(13) 0.02621(9) Uani 1 1 d . . . P1 P 0.71027(10) 0.03638(10) 0.33856(5) 0.0238(2) Uani 1 1 d . . . P2 P 0.65441(10) -0.10464(9) 0.18932(5) 0.0228(2) Uani 1 1 d . . . P3 P 0.75051(10) -0.35268(10) 0.18677(5) 0.0228(2) Uani 1 1 d . . . Cl1 Cl 0.53322(10) -0.54067(9) 0.13585(5) 0.0303(2) Uani 1 1 d . . . Cl2 Cl 0.39647(10) -0.42726(11) 0.25419(6) 0.0356(3) Uani 1 1 d . . . C1 C 0.4309(4) 0.0325(5) 0.3246(2) 0.0360(12) Uani 1 1 d . . . H1 H 0.4486 0.0861 0.3629 0.043 Uiso 1 1 calc R . . C2 C 0.3956(4) -0.0798(5) 0.3206(2) 0.0363(12) Uani 1 1 d . . . H2 H 0.3852 -0.1195 0.3557 0.044 Uiso 1 1 calc R . . C3 C 0.3711(4) -0.1250(4) 0.2580(2) 0.0345(11) Uani 1 1 d . . . H3 H 0.3401 -0.2013 0.2413 0.041 Uiso 1 1 calc R . . C4 C 0.3922(4) -0.0387(4) 0.2240(2) 0.0346(11) Uani 1 1 d . . . H4 H 0.3787 -0.0448 0.1788 0.042 Uiso 1 1 calc R . . C5 C 0.4310(4) 0.0573(5) 0.2638(2) 0.0368(11) Uani 1 1 d . . . H5 H 0.4468 0.1314 0.2522 0.044 Uiso 1 1 calc R . . C6 C 0.7761(4) -0.2031(4) 0.1854(2) 0.0237(9) Uani 1 1 d . . . H6A H 0.8118 -0.1968 0.1476 0.028 Uiso 1 1 calc R . . H6B H 0.8365 -0.1761 0.2196 0.028 Uiso 1 1 calc R . . C11 C 0.7310(4) 0.0101(4) 0.4177(2) 0.0274(10) Uani 1 1 d . . . C12 C 0.6423(5) -0.0430(4) 0.4424(2) 0.0350(11) Uani 1 1 d . . . H12A H 0.5721 -0.0687 0.4174 0.042 Uiso 1 1 calc R . . C13 C 0.6552(5) -0.0583(5) 0.5024(2) 0.0437(13) Uani 1 1 d . . . H13A H 0.5934 -0.0931 0.5184 0.052 Uiso 1 1 calc R . . C14 C 0.7573(6) -0.0235(5) 0.5394(2) 0.0479(15) Uani 1 1 d . . . H14A H 0.7662 -0.0352 0.5806 0.057 Uiso 1 1 calc R . . C15 C 0.8454(5) 0.0279(5) 0.5162(2) 0.0472(14) Uani 1 1 d . . . H15A H 0.9158 0.0517 0.5415 0.057 Uiso 1 1 calc R . . C16 C 0.8331(5) 0.0457(5) 0.4558(2) 0.0357(11) Uani 1 1 d . . . H16A H 0.8946 0.0824 0.4405 0.043 Uiso 1 1 calc R . . C21 C 0.6765(4) 0.1837(4) 0.3473(2) 0.0270(9) Uani 1 1 d . . . C22 C 0.6663(5) 0.2473(5) 0.4023(2) 0.0420(13) Uani 1 1 d . . . H22A H 0.6819 0.2168 0.4388 0.050 Uiso 1 1 calc R . . C23 C 0.6329(7) 0.3576(5) 0.4046(3) 0.0598(19) Uani 1 1 d . . . H23A H 0.6246 0.4009 0.4426 0.072 Uiso 1 1 calc R . . C24 C 0.6120(6) 0.4032(5) 0.3519(3) 0.0497(15) Uani 1 1 d . . . H24A H 0.5914 0.4783 0.3538 0.060 Uiso 1 1 calc R . . C25 C 0.6211(5) 0.3394(4) 0.2966(2) 0.0413(13) Uani 1 1 d . . . H25A H 0.6050 0.3699 0.2601 0.050 Uiso 1 1 calc R . . C26 C 0.6538(5) 0.2309(4) 0.2945(2) 0.0357(11) Uani 1 1 d . . . H26A H 0.6609 0.1876 0.2563 0.043 Uiso 1 1 calc R . . C31 C 0.8636(4) 0.0371(4) 0.3218(2) 0.0307(10) Uani 1 1 d . . . C32 C 0.9255(4) -0.0595(5) 0.3217(2) 0.0362(11) Uani 1 1 d . . . H32A H 0.8882 -0.1244 0.3302 0.043 Uiso 1 1 calc R . . C33 C 1.0432(5) -0.0613(6) 0.3092(3) 0.0492(15) Uani 1 1 d . . . H33A H 1.0857 -0.1271 0.3099 0.059 Uiso 1 1 calc R . . C34 C 1.0968(5) 0.0318(6) 0.2959(3) 0.0552(17) Uani 1 1 d . . . H34A H 1.1760 0.0301 0.2868 0.066 Uiso 1 1 calc R . . C35 C 1.0372(6) 0.1256(6) 0.2959(3) 0.0606(18) Uani 1 1 d . . . H35A H 1.0754 0.1897 0.2871 0.073 Uiso 1 1 calc R . . C36 C 0.9202(5) 0.1309(5) 0.3086(3) 0.0464(14) Uani 1 1 d . . . H36A H 0.8797 0.1978 0.3081 0.056 Uiso 1 1 calc R . . C41 C 0.5596(4) -0.1607(4) 0.1202(2) 0.0275(10) Uani 1 1 d . . . C42 C 0.5774(5) -0.1359(5) 0.0630(2) 0.0397(12) Uani 1 1 d . . . H42A H 0.6365 -0.0827 0.0594 0.048 Uiso 1 1 calc R . . C43 C 0.5089(6) -0.1888(6) 0.0108(2) 0.0508(15) Uani 1 1 d . . . H43A H 0.5203 -0.1702 -0.0279 0.061 Uiso 1 1 calc R . . C44 C 0.4249(5) -0.2680(5) 0.0158(3) 0.0484(15) Uani 1 1 d . . . H44A H 0.3798 -0.3052 -0.0196 0.058 Uiso 1 1 calc R . . C45 C 0.4062(5) -0.2931(5) 0.0715(2) 0.0399(12) Uani 1 1 d . . . H45A H 0.3486 -0.3480 0.0746 0.048 Uiso 1 1 calc R . . C46 C 0.4711(4) -0.2388(4) 0.1235(2) 0.0296(10) Uani 1 1 d . . . H46A H 0.4552 -0.2549 0.1621 0.036 Uiso 1 1 calc R . . C51 C 0.7219(5) 0.0156(4) 0.1652(2) 0.0305(10) Uani 1 1 d . . . C52 C 0.6470(6) 0.0983(4) 0.1493(2) 0.0402(12) Uani 1 1 d . . . H52A H 0.5645 0.0883 0.1492 0.048 Uiso 1 1 calc R . . C53 C 0.6916(8) 0.1941(5) 0.1337(3) 0.0572(19) Uani 1 1 d . . . H53A H 0.6398 0.2496 0.1229 0.069 Uiso 1 1 calc R . . C54 C 0.8113(8) 0.2095(6) 0.1339(3) 0.067(2) Uani 1 1 d . . . H54A H 0.8416 0.2758 0.1234 0.081 Uiso 1 1 calc R . . C55 C 0.8877(7) 0.1290(6) 0.1491(3) 0.066(2) Uani 1 1 d . . . H55A H 0.9700 0.1396 0.1487 0.079 Uiso 1 1 calc R . . C56 C 0.8424(5) 0.0316(5) 0.1653(3) 0.0455(14) Uani 1 1 d . . . H56A H 0.8944 -0.0236 0.1762 0.055 Uiso 1 1 calc R . . C61 C 0.8757(4) -0.3910(4) 0.2350(2) 0.0307(10) Uani 1 1 d . . . C62 C 0.8608(5) -0.4747(5) 0.2689(3) 0.0453(14) Uani 1 1 d . . . H62A H 0.7846 -0.5064 0.2692 0.054 Uiso 1 1 calc R . . C63 C 0.9576(7) -0.5132(6) 0.3029(3) 0.067(2) Uani 1 1 d . . . H63A H 0.9474 -0.5700 0.3267 0.081 Uiso 1 1 calc R . . C64 C 1.0673(6) -0.4674(7) 0.3013(3) 0.070(2) Uani 1 1 d . . . H64A H 1.1332 -0.4938 0.3238 0.084 Uiso 1 1 calc R . . C65 C 1.0835(5) -0.3850(6) 0.2681(4) 0.0630(19) Uani 1 1 d . . . H65A H 1.1600 -0.3541 0.2678 0.076 Uiso 1 1 calc R . . C66 C 0.9885(4) -0.3464(5) 0.2347(3) 0.0452(14) Uani 1 1 d . . . H66A H 1.0001 -0.2891 0.2115 0.054 Uiso 1 1 calc R . . C71 C 0.7784(4) -0.4172(4) 0.1108(2) 0.0253(9) Uani 1 1 d . . . C72 C 0.7081(5) -0.3938(5) 0.0604(2) 0.0389(12) Uani 1 1 d . . . H72A H 0.6439 -0.3463 0.0654 0.047 Uiso 1 1 calc R . . C73 C 0.7315(5) -0.4399(5) 0.0025(2) 0.0432(13) Uani 1 1 d . . . H73A H 0.6846 -0.4220 -0.0322 0.052 Uiso 1 1 calc R . . C74 C 0.8223(5) -0.5112(5) -0.0048(2) 0.0392(12) Uani 1 1 d . . . H74A H 0.8388 -0.5420 -0.0444 0.047 Uiso 1 1 calc R . . C75 C 0.8885(5) -0.5374(5) 0.0449(3) 0.0428(13) Uani 1 1 d . . . H75A H 0.9497 -0.5882 0.0397 0.051 Uiso 1 1 calc R . . C76 C 0.8684(4) -0.4915(4) 0.1032(2) 0.0354(11) Uani 1 1 d . . . H76A H 0.9154 -0.5105 0.1375 0.042 Uiso 1 1 calc R . . C84 C 0.3912(7) 0.6254(6) 0.4099(3) 0.0636(19) Uani 1 1 d . . . H84 H 0.4093 0.6196 0.3669 0.076 Uiso 1 1 calc R . . Cl9 Cl 0.5225(2) 0.65333(19) 0.45767(9) 0.0787(6) Uani 1 1 d . . . Cl10 Cl 0.2919(2) 0.73069(19) 0.42304(10) 0.0924(8) Uani 1 1 d . . . Cl11 Cl 0.3292(2) 0.49860(17) 0.42042(9) 0.0738(5) Uani 1 1 d . . . C83 C 1.2787(5) -0.6733(5) 0.1768(3) 0.0440(13) Uani 1 1 d . . . H83 H 1.3426 -0.6165 0.1774 0.053 Uiso 1 1 calc R . . Cl12 Cl 1.27083(16) -0.69877(14) 0.25095(9) 0.0621(4) Uani 1 1 d . . . Cl13 Cl 1.3127(2) -0.79440(19) 0.13035(10) 0.0824(6) Uiso 1 1 d . . . Cl14 Cl 1.1456(2) -0.62251(19) 0.14695(10) 0.0826(6) Uiso 1 1 d . . . C82 C 1.1156(16) -0.1706(16) 0.0521(8) 0.086(5) Uiso 0.535(11) 1 d P A 1 H82 H 1.1611 -0.2397 0.0470 0.103 Uiso 0.535(11) 1 calc PR A 1 Cl6 Cl 1.1565(7) -0.0966(9) 0.0156(4) 0.134(4) Uani 0.535(11) 1 d P A 1 Cl7 Cl 1.1193(5) -0.1149(9) 0.1373(3) 0.110(3) Uani 0.535(11) 1 d P A 1 Cl8 Cl 0.9464(7) -0.2094(6) 0.0402(3) 0.099(2) Uani 0.535(11) 1 d P A 1 C82' C 1.0485(14) -0.1019(13) 0.0647(7) 0.060(4) Uiso 0.465(11) 1 d P A 2 H82' H 0.9955 -0.0493 0.0862 0.072 Uiso 0.465(11) 1 calc PR A 2 Cl6' Cl 1.1607(12) -0.0374(7) 0.0495(9) 0.200(6) Uani 0.465(11) 1 d P A 2 Cl7' Cl 1.1227(9) -0.2016(16) 0.1217(5) 0.166(6) Uani 0.465(11) 1 d P A 2 Cl8' Cl 0.9753(7) -0.1854(8) 0.0145(6) 0.114(3) Uani 0.465(11) 1 d P A 2 C81 C -0.0630(6) 0.6394(6) 0.4910(3) 0.233(10) Uiso 1 1 d D . . Cl3' Cl 0.0751(8) 0.6202(11) 0.4782(7) 0.81(4) Uani 0.567(7) 1 d PD B 3 Cl3 Cl -0.1097(13) 0.7179(8) 0.5494(4) 0.231(9) Uani 0.433(7) 1 d PD B 4 Cl4' Cl -0.1277(10) 0.7154(8) 0.4431(3) 0.301(10) Uani 0.567(7) 1 d PD B 3 Cl4 Cl -0.0023(12) 0.7159(9) 0.4466(5) 0.320(15) Uani 0.433(7) 1 d PD B 4 Cl5' Cl -0.0678(14) 0.7003(7) 0.5620(3) 0.424(18) Uani 0.567(7) 1 d PD B 3 Cl5 Cl -0.1720(8) 0.5626(7) 0.4505(3) 0.155(5) Uani 0.433(7) 1 d PD B 4 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 0.01821(17) 0.02499(19) 0.02167(18) 0.00212(13) 0.00125(13) 0.00295(13) Pd1 0.02046(16) 0.02345(18) 0.02365(17) 0.00410(13) 0.00256(12) 0.00105(13) I1 0.02781(15) 0.02799(16) 0.02275(15) 0.00425(11) 0.00169(11) 0.00253(11) P1 0.0221(5) 0.0269(6) 0.0217(5) 0.0016(4) 0.0019(4) 0.0021(4) P2 0.0233(5) 0.0244(6) 0.0202(5) 0.0028(4) 0.0006(4) 0.0028(4) P3 0.0195(5) 0.0246(6) 0.0242(6) 0.0029(4) 0.0027(4) 0.0027(4) Cl1 0.0304(6) 0.0274(6) 0.0317(6) -0.0014(4) 0.0064(4) -0.0051(4) Cl2 0.0283(6) 0.0402(7) 0.0384(6) 0.0019(5) 0.0109(5) -0.0061(5) C1 0.022(2) 0.044(3) 0.041(3) -0.002(2) 0.006(2) 0.015(2) C2 0.021(2) 0.053(3) 0.038(3) 0.012(2) 0.011(2) 0.008(2) C3 0.019(2) 0.037(3) 0.045(3) 0.001(2) -0.002(2) -0.001(2) C4 0.022(2) 0.041(3) 0.040(3) 0.004(2) 0.0026(19) 0.014(2) C5 0.026(2) 0.042(3) 0.043(3) 0.011(2) 0.001(2) 0.008(2) C6 0.022(2) 0.024(2) 0.025(2) 0.0019(17) 0.0034(17) 0.0000(17) C11 0.027(2) 0.030(2) 0.024(2) 0.0016(18) 0.0007(17) 0.0097(19) C12 0.036(3) 0.042(3) 0.027(2) 0.001(2) 0.005(2) 0.001(2) C13 0.047(3) 0.053(4) 0.033(3) 0.007(2) 0.012(2) 0.006(3) C14 0.057(4) 0.066(4) 0.023(3) 0.012(3) 0.006(2) 0.021(3) C15 0.043(3) 0.062(4) 0.031(3) -0.002(3) -0.010(2) 0.014(3) C16 0.033(3) 0.044(3) 0.028(2) 0.001(2) -0.001(2) 0.005(2) C21 0.027(2) 0.028(2) 0.025(2) 0.0032(18) 0.0018(18) 0.0011(18) C22 0.062(4) 0.037(3) 0.029(3) 0.007(2) 0.010(2) 0.013(3) C23 0.105(6) 0.036(3) 0.039(3) -0.001(3) 0.021(3) 0.020(3) C24 0.071(4) 0.030(3) 0.052(3) 0.009(2) 0.020(3) 0.015(3) C25 0.049(3) 0.037(3) 0.039(3) 0.015(2) -0.001(2) -0.003(2) C26 0.047(3) 0.031(3) 0.028(2) 0.003(2) 0.004(2) -0.003(2) C31 0.022(2) 0.040(3) 0.027(2) -0.003(2) 0.0011(18) -0.0021(19) C32 0.025(2) 0.042(3) 0.036(3) -0.008(2) -0.001(2) 0.005(2) C33 0.032(3) 0.065(4) 0.043(3) -0.015(3) -0.001(2) 0.008(3) C34 0.025(3) 0.085(5) 0.051(4) -0.008(3) 0.010(2) -0.006(3) C35 0.037(3) 0.069(5) 0.075(5) 0.003(4) 0.018(3) -0.018(3) C36 0.028(3) 0.044(3) 0.066(4) 0.003(3) 0.009(3) -0.007(2) C41 0.028(2) 0.030(2) 0.022(2) 0.0012(18) -0.0028(17) 0.0080(19) C42 0.041(3) 0.050(3) 0.026(2) 0.003(2) -0.003(2) -0.002(2) C43 0.058(4) 0.071(4) 0.020(2) 0.003(3) -0.004(2) 0.001(3) C44 0.047(3) 0.057(4) 0.033(3) -0.005(3) -0.013(2) 0.003(3) C45 0.035(3) 0.042(3) 0.039(3) 0.001(2) -0.009(2) 0.001(2) C46 0.027(2) 0.030(3) 0.030(2) 0.0004(19) -0.0022(18) 0.0028(19) C51 0.045(3) 0.026(2) 0.021(2) 0.0031(18) 0.0045(19) 0.001(2) C52 0.059(4) 0.034(3) 0.028(3) 0.006(2) 0.001(2) 0.007(2) C53 0.109(6) 0.030(3) 0.033(3) 0.010(2) 0.002(3) 0.009(3) C54 0.111(7) 0.038(4) 0.053(4) 0.013(3) 0.001(4) -0.024(4) C55 0.075(5) 0.054(4) 0.069(5) 0.019(4) 0.004(4) -0.027(4) C56 0.049(3) 0.038(3) 0.050(3) 0.012(3) 0.001(3) -0.013(3) C61 0.023(2) 0.035(3) 0.031(2) -0.001(2) 0.0002(18) 0.0086(19) C62 0.040(3) 0.045(3) 0.053(3) 0.020(3) 0.001(3) 0.011(3) C63 0.071(5) 0.070(5) 0.065(4) 0.026(4) -0.003(4) 0.034(4) C64 0.052(4) 0.080(5) 0.068(5) -0.002(4) -0.026(3) 0.036(4) C65 0.030(3) 0.064(5) 0.085(5) -0.008(4) -0.010(3) 0.015(3) C66 0.024(3) 0.048(3) 0.061(4) 0.002(3) 0.001(2) 0.005(2) C71 0.022(2) 0.022(2) 0.031(2) -0.0009(18) 0.0042(17) -0.0010(17) C72 0.041(3) 0.044(3) 0.031(3) 0.000(2) 0.002(2) 0.011(2) C73 0.049(3) 0.049(3) 0.029(3) -0.001(2) 0.001(2) 0.001(3) C74 0.038(3) 0.044(3) 0.033(3) -0.007(2) 0.015(2) -0.009(2) C75 0.038(3) 0.041(3) 0.048(3) -0.007(2) 0.014(2) 0.003(2) C76 0.032(3) 0.031(3) 0.043(3) 0.000(2) 0.008(2) 0.006(2) C84 0.092(5) 0.062(4) 0.041(3) 0.013(3) 0.020(3) 0.021(4) Cl9 0.0886(14) 0.0937(15) 0.0546(10) 0.0094(10) 0.0159(10) -0.0126(12) Cl10 0.138(2) 0.0842(15) 0.0681(12) 0.0286(11) 0.0411(13) 0.0525(14) Cl11 0.0880(14) 0.0699(12) 0.0631(11) 0.0170(9) -0.0032(10) 0.0039(10) C83 0.033(3) 0.042(3) 0.058(4) 0.011(3) 0.007(2) 0.003(2) Cl12 0.0653(10) 0.0565(10) 0.0751(11) 0.0302(8) 0.0258(9) 0.0110(8) Cl6 0.148(6) 0.165(8) 0.123(5) 0.074(5) 0.090(5) 0.048(6) Cl7 0.058(3) 0.208(8) 0.061(3) 0.021(4) -0.007(2) 0.004(4) Cl8 0.103(5) 0.097(4) 0.087(4) -0.020(3) 0.023(3) -0.031(3) Cl6' 0.184(10) 0.068(5) 0.331(18) 0.003(7) -0.012(10) -0.024(5) Cl7' 0.113(6) 0.295(18) 0.098(6) 0.035(8) 0.040(5) 0.031(9) Cl8' 0.068(4) 0.108(6) 0.149(9) -0.018(5) -0.015(4) 0.016(4) Cl3' 0.149(10) 0.36(2) 1.98(11) 0.65(4) -0.31(3) -0.099(12) Cl3 0.46(3) 0.088(6) 0.137(9) -0.005(6) 0.036(13) 0.072(11) Cl4' 0.45(2) 0.263(13) 0.135(7) -0.038(7) -0.152(9) 0.226(14) Cl4 0.32(2) 0.264(18) 0.35(2) -0.179(16) 0.243(18) -0.217(17) Cl5' 0.91(4) 0.143(9) 0.153(8) 0.084(7) -0.292(17) -0.227(16) Cl5 0.182(8) 0.172(8) 0.101(5) -0.028(5) 0.053(5) -0.122(7) _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 C5 2.189(5) . ? Ru1 C4 2.213(5) . ? Ru1 C1 2.215(5) . ? Ru1 C2 2.230(5) . ? Ru1 C3 2.238(5) . ? Ru1 P2 2.3212(12) . ? Ru1 P1 2.3325(12) . ? Ru1 I1 2.6749(5) . ? Pd1 P3 2.2333(12) . ? Pd1 Cl1 2.3528(12) . ? Pd1 Cl2 2.3710(12) . ? Pd1 I1 2.5822(5) . ? P1 C31 1.834(5) . ? P1 C21 1.839(5) . ? P1 C11 1.840(5) . ? P2 C41 1.831(4) . ? P2 C51 1.831(5) . ? P2 C6 1.858(4) . ? P3 C61 1.812(5) . ? P3 C71 1.831(5) . ? P3 C6 1.857(5) . ? C1 C2 1.416(8) . ? C1 C5 1.439(7) . ? C1 H1 1.0000 . ? C2 C3 1.426(7) . ? C2 H2 1.0000 . ? C3 C4 1.425(7) . ? C3 H3 1.0000 . ? C4 C5 1.402(8) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C11 C16 1.395(7) . ? C11 C12 1.403(7) . ? C12 C13 1.376(7) . ? C12 H12A 0.9500 . ? C13 C14 1.381(8) . ? C13 H13A 0.9500 . ? C14 C15 1.370(9) . ? C14 H14A 0.9500 . ? C15 C16 1.395(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 C22 1.375(7) . ? C21 C26 1.393(7) . ? C22 C23 1.405(8) . ? C22 H22A 0.9500 . ? C23 C24 1.378(9) . ? C23 H23A 0.9500 . ? C24 C25 1.379(8) . ? C24 H24A 0.9500 . ? C25 C26 1.384(7) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.389(7) . ? C31 C36 1.395(7) . ? C32 C33 1.405(7) . ? C32 H32A 0.9500 . ? C33 C34 1.373(9) . ? C33 H33A 0.9500 . ? C34 C35 1.346(10) . ? C34 H34A 0.9500 . ? C35 C36 1.398(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C42 1.394(7) . ? C41 C46 1.397(7) . ? C42 C43 1.403(7) . ? C42 H42A 0.9500 . ? C43 C44 1.381(9) . ? C43 H43A 0.9500 . ? C44 C45 1.366(8) . ? C44 H44A 0.9500 . ? C45 C46 1.386(7) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C56 1.390(8) . ? C51 C52 1.400(7) . ? C52 C53 1.379(8) . ? C52 H52A 0.9500 . ? C53 C54 1.380(11) . ? C53 H53A 0.9500 . ? C54 C55 1.384(11) . ? C54 H54A 0.9500 . ? C55 C56 1.405(8) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.382(8) . ? C61 C66 1.395(7) . ? C62 C63 1.404(8) . ? C62 H62A 0.9500 . ? C63 C64 1.374(11) . ? C63 H63A 0.9500 . ? C64 C65 1.362(11) . ? C64 H64A 0.9500 . ? C65 C66 1.383(8) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.382(7) . ? C71 C76 1.393(6) . ? C72 C73 1.393(7) . ? C72 H72A 0.9500 . ? C73 C74 1.376(8) . ? C73 H73A 0.9500 . ? C74 C75 1.361(8) . ? C74 H74A 0.9500 . ? C75 C76 1.386(7) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C84 Cl10 1.747(7) . ? C84 Cl9 1.747(8) . ? C84 Cl11 1.756(8) . ? C84 H84 1.0000 . ? C83 Cl12 1.746(6) . ? C83 Cl13 1.757(6) . ? C83 Cl14 1.758(6) . ? C83 H83 1.0000 . ? C82 Cl6 1.415(19) . ? C82 Cl7 1.925(19) . ? C82 Cl8 1.967(19) . ? C82 H82 1.0000 . ? C82' Cl8' 1.564(17) . ? C82' Cl6' 1.59(2) . ? C82' Cl7' 2.03(2) . ? C82' H82' 1.0000 . ? C81 Cl4' 1.648(5) . ? C81 Cl3 1.648(5) . ? C81 Cl3' 1.651(5) . ? C81 Cl5 1.654(5) . ? C81 Cl4 1.660(5) . ? C81 Cl5' 1.660(5) . ? 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 C5 Ru1 C4 37.13(19) . . ? C5 Ru1 C1 38.2(2) . . ? C4 Ru1 C1 62.20(19) . . ? C5 Ru1 C2 63.0(2) . . ? C4 Ru1 C2 62.08(19) . . ? C1 Ru1 C2 37.1(2) . . ? C5 Ru1 C3 62.8(2) . . ? C4 Ru1 C3 37.34(19) . . ? C1 Ru1 C3 62.32(19) . . ? C2 Ru1 C3 37.22(19) . . ? C5 Ru1 P2 108.26(14) . . ? C4 Ru1 P2 92.08(14) . . ? C1 Ru1 P2 146.29(15) . . ? C2 Ru1 P2 148.18(14) . . ? C3 Ru1 P2 110.96(14) . . ? C5 Ru1 P1 100.57(15) . . ? C4 Ru1 P1 137.01(14) . . ? C1 Ru1 P1 88.67(14) . . ? C2 Ru1 P1 113.31(14) . . ? C3 Ru1 P1 149.59(14) . . ? P2 Ru1 P1 98.19(4) . . ? C5 Ru1 I1 155.70(14) . . ? C4 Ru1 I1 130.37(14) . . ? C1 Ru1 I1 122.26(15) . . ? C2 Ru1 I1 92.85(14) . . ? C3 Ru1 I1 96.64(14) . . ? P2 Ru1 I1 90.70(3) . . ? P1 Ru1 I1 91.31(3) . . ? P3 Pd1 Cl1 93.88(4) . . ? P3 Pd1 Cl2 174.26(5) . . ? Cl1 Pd1 Cl2 90.61(4) . . ? P3 Pd1 I1 85.88(3) . . ? Cl1 Pd1 I1 174.85(3) . . ? Cl2 Pd1 I1 89.96(3) . . ? Pd1 I1 Ru1 101.408(16) . . ? C31 P1 C21 102.6(2) . . ? C31 P1 C11 100.0(2) . . ? C21 P1 C11 102.5(2) . . ? C31 P1 Ru1 123.30(15) . . ? C21 P1 Ru1 110.69(15) . . ? C11 P1 Ru1 115.12(16) . . ? C41 P2 C51 100.9(2) . . ? C41 P2 C6 100.4(2) . . ? C51 P2 C6 101.2(2) . . ? C41 P2 Ru1 115.25(16) . . ? C51 P2 Ru1 115.75(15) . . ? C6 P2 Ru1 120.29(15) . . ? C61 P3 C71 103.2(2) . . ? C61 P3 C6 104.4(2) . . ? C71 P3 C6 103.5(2) . . ? C61 P3 Pd1 112.14(17) . . ? C71 P3 Pd1 116.66(15) . . ? C6 P3 Pd1 115.38(14) . . ? C2 C1 C5 107.9(5) . . ? C2 C1 Ru1 72.0(3) . . ? C5 C1 Ru1 69.9(3) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Ru1 C1 H1 126.0 . . ? C1 C2 C3 108.3(5) . . ? C1 C2 Ru1 70.9(3) . . ? C3 C2 Ru1 71.7(3) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? Ru1 C2 H2 125.8 . . ? C4 C3 C2 107.0(5) . . ? C4 C3 Ru1 70.4(3) . . ? C2 C3 Ru1 71.1(3) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? Ru1 C3 H3 126.5 . . ? C5 C4 C3 109.5(5) . . ? C5 C4 Ru1 70.5(3) . . ? C3 C4 Ru1 72.3(3) . . ? C5 C4 H4 125.2 . . ? C3 C4 H4 125.2 . . ? Ru1 C4 H4 125.2 . . ? C4 C5 C1 107.2(5) . . ? C4 C5 Ru1 72.4(3) . . ? C1 C5 Ru1 71.9(3) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Ru1 C5 H5 126.2 . . ? P3 C6 P2 121.7(2) . . ? P3 C6 H6A 106.9 . . ? P2 C6 H6A 106.9 . . ? P3 C6 H6B 106.9 . . ? P2 C6 H6B 106.9 . . ? H6A C6 H6B 106.7 . . ? C16 C11 C12 117.7(4) . . ? C16 C11 P1 121.4(4) . . ? C12 C11 P1 120.8(4) . . ? C13 C12 C11 121.0(5) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 120.8(5) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C11 C16 C15 120.4(5) . . ? C11 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C22 C21 C26 118.7(5) . . ? C22 C21 P1 123.7(4) . . ? C26 C21 P1 117.5(4) . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 119.7(5) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C21 121.4(5) . . ? C25 C26 H26A 119.3 . . ? C21 C26 H26A 119.3 . . ? C32 C31 C36 118.7(5) . . ? C32 C31 P1 118.8(4) . . ? C36 C31 P1 122.5(4) . . ? C31 C32 C33 120.1(6) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 120.1(6) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 121.6(6) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C31 C36 C35 119.5(6) . . ? C31 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C42 C41 C46 117.8(4) . . ? C42 C41 P2 122.8(4) . . ? C46 C41 P2 119.1(3) . . ? C41 C42 C43 120.5(5) . . ? C41 C42 H42A 119.7 . . ? C43 C42 H42A 119.7 . . ? C44 C43 C42 119.8(5) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C45 C44 C43 120.3(5) . . ? C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 121.2(5) . . ? C45 C46 H46A 119.4 . . ? C41 C46 H46A 119.4 . . ? C56 C51 C52 118.9(5) . . ? C56 C51 P2 123.8(4) . . ? C52 C51 P2 117.2(4) . . ? C53 C52 C51 120.7(6) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C52 C53 C54 120.0(6) . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C53 C54 C55 120.6(6) . . ? C53 C54 H54A 119.7 . . ? C55 C54 H54A 119.7 . . ? C54 C55 C56 119.4(7) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C51 C56 C55 120.3(6) . . ? C51 C56 H56A 119.9 . . ? C55 C56 H56A 119.9 . . ? C62 C61 C66 118.9(5) . . ? C62 C61 P3 118.6(4) . . ? C66 C61 P3 122.2(4) . . ? C61 C62 C63 120.4(6) . . ? C61 C62 H62A 119.8 . . ? C63 C62 H62A 119.8 . . ? C64 C63 C62 119.0(7) . . ? C64 C63 H63A 120.5 . . ? C62 C63 H63A 120.5 . . ? C65 C64 C63 121.3(6) . . ? C65 C64 H64A 119.3 . . ? C63 C64 H64A 119.3 . . ? C64 C65 C66 119.9(6) . . ? C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C65 C66 C61 120.4(6) . . ? C65 C66 H66A 119.8 . . ? C61 C66 H66A 119.8 . . ? C72 C71 C76 119.6(5) . . ? C72 C71 P3 119.8(4) . . ? C76 C71 P3 120.6(4) . . ? C71 C72 C73 119.9(5) . . ? C71 C72 H72A 120.1 . . ? C73 C72 H72A 120.1 . . ? C74 C73 C72 120.2(5) . . ? C74 C73 H73A 119.9 . . ? C72 C73 H73A 119.9 . . ? C75 C74 C73 119.7(5) . . ? C75 C74 H74A 120.2 . . ? C73 C74 H74A 120.2 . . ? C74 C75 C76 121.4(5) . . ? C74 C75 H75A 119.3 . . ? C76 C75 H75A 119.3 . . ? C75 C76 C71 119.2(5) . . ? C75 C76 H76A 120.4 . . ? C71 C76 H76A 120.4 . . ? Cl10 C84 Cl9 111.4(4) . . ? Cl10 C84 Cl11 110.4(4) . . ? Cl9 C84 Cl11 109.6(4) . . ? Cl10 C84 H84 108.5 . . ? Cl9 C84 H84 108.5 . . ? Cl11 C84 H84 108.5 . . ? Cl12 C83 Cl13 110.3(3) . . ? Cl12 C83 Cl14 110.9(3) . . ? Cl13 C83 Cl14 109.9(3) . . ? Cl12 C83 H83 108.6 . . ? Cl13 C83 H83 108.6 . . ? Cl14 C83 H83 108.6 . . ? Cl6 C82 Cl7 116.0(12) . . ? Cl6 C82 Cl8 117.1(12) . . ? Cl7 C82 Cl8 95.2(9) . . ? Cl6 C82 H82 109.3 . . ? Cl7 C82 H82 109.3 . . ? Cl8 C82 H82 109.3 . . ? Cl8' C82' Cl6' 120.6(12) . . ? Cl8' C82' Cl7' 102.6(10) . . ? Cl6' C82' Cl7' 101.7(10) . . ? Cl8' C82' H82' 110.3 . . ? Cl6' C82' H82' 110.3 . . ? Cl7' C82' H82' 110.3 . . ? Cl4' C81 Cl3 91.7(6) . . ? Cl4' C81 Cl3' 110.4(4) . . ? Cl3 C81 Cl3' 126.6(6) . . ? Cl4' C81 Cl5 73.2(6) . . ? Cl3 C81 Cl5 111.2(4) . . ? Cl3' C81 Cl5 121.5(7) . . ? Cl4' C81 Cl4 51.2(7) . . ? Cl3 C81 Cl4 110.7(4) . . ? Cl3' C81 Cl4 60.8(6) . . ? Cl5 C81 Cl4 109.1(4) . . ? Cl4' C81 Cl5' 110.2(4) . . ? Cl3 C81 Cl5' 20.5(6) . . ? Cl3' C81 Cl5' 109.6(4) . . ? Cl5 C81 Cl5' 124.0(6) . . ? Cl4 C81 Cl5' 115.0(6) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.827 _refine_diff_density_min -2.275 _refine_diff_density_rms 0.126 #END=== #Compound #5 data_yy04 _database_code_CSD 215181 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H57 Cl8 P3 Pd Ru' _chemical_formula_weight 1301.99 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' 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' Pd Pd -0.9988 1.0072 '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 13.8306(6) _cell_length_b 22.8974(9) _cell_length_c 18.4161(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.070(2) _cell_angle_gamma 90.00 _cell_volume 5544.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 394 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6953 _exptl_absorpt_correction_T_max 0.8300 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 36509 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12593 _reflns_number_gt 9978 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0462P)^2^] 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 12593 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.003 _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 Pd Pd 1.465963(13) 0.776477(7) 0.684739(9) 0.02391(5) Uani 1 1 d . . . Ru Ru 1.515660(13) 0.611354(7) 0.666482(9) 0.02140(5) Uani 1 1 d . . . Cl1 Cl 1.52480(4) 0.68817(2) 0.76049(3) 0.02640(12) Uani 1 1 d . . . Cl2 Cl 1.63320(5) 0.79826(3) 0.68161(3) 0.03494(14) Uani 1 1 d . . . P1 P 1.49069(4) 0.54428(2) 0.75399(3) 0.02163(12) Uani 1 1 d . . . P2 P 1.34784(4) 0.63420(2) 0.60533(3) 0.02103(12) Uani 1 1 d . . . P3 P 1.30981(4) 0.75311(2) 0.68398(3) 0.02344(12) Uani 1 1 d . . . C1 C 1.54647(19) 0.60501(11) 0.55702(14) 0.0330(5) Uani 1 1 d . . . H1A H 1.4952 0.6107 0.5056 0.040 Uiso 1 1 calc R . . C2 C 1.5696(2) 0.55094(11) 0.59663(14) 0.0342(5) Uani 1 1 d . . . H2A H 1.5397 0.5120 0.5776 0.041 Uiso 1 1 calc R . . C3 C 1.65251(19) 0.56197(12) 0.66468(15) 0.0373(6) Uani 1 1 d . . . H3A H 1.6884 0.5319 0.7029 0.045 Uiso 1 1 calc R . . C4 C 1.67642(19) 0.62175(12) 0.66808(15) 0.0374(6) Uani 1 1 d . . . H4A H 1.7319 0.6414 0.7090 0.045 Uiso 1 1 calc R . . C5 C 1.61066(19) 0.64918(11) 0.60063(14) 0.0335(5) Uani 1 1 d . . . H5A H 1.6125 0.6911 0.5858 0.040 Uiso 1 1 calc R . . C6 C 1.27355(17) 0.67657(9) 0.65536(12) 0.0237(4) Uani 1 1 d . . . H6A H 1.2753 0.6547 0.7021 0.028 Uiso 1 1 calc R . . H6B H 1.2019 0.6769 0.6221 0.028 Uiso 1 1 calc R . . C11 C 1.50779(18) 0.46955(9) 0.72449(12) 0.0253(5) Uani 1 1 d . . . C12 C 1.4345(2) 0.44562(10) 0.66096(13) 0.0313(5) Uani 1 1 d . . . H12A H 1.3745 0.4671 0.6362 0.038 Uiso 1 1 calc R . . C13 C 1.4489(2) 0.39078(10) 0.63384(15) 0.0403(6) Uani 1 1 d . . . H13A H 1.3976 0.3743 0.5919 0.048 Uiso 1 1 calc R . . C14 C 1.5369(2) 0.36014(11) 0.66733(16) 0.0447(7) Uani 1 1 d . . . H14A H 1.5470 0.3230 0.6478 0.054 Uiso 1 1 calc R . . C15 C 1.6104(2) 0.38329(11) 0.72903(17) 0.0428(7) Uani 1 1 d . . . H15A H 1.6715 0.3622 0.7519 0.051 Uiso 1 1 calc R . . C16 C 1.59563(19) 0.43766(10) 0.75817(14) 0.0331(5) Uani 1 1 d . . . H16A H 1.6462 0.4530 0.8015 0.040 Uiso 1 1 calc R . . C21 C 1.37433(17) 0.54093(10) 0.78194(12) 0.0254(5) Uani 1 1 d . . . C22 C 1.35178(19) 0.59000(10) 0.81913(13) 0.0308(5) Uani 1 1 d . . . H22A H 1.3952 0.6231 0.8278 0.037 Uiso 1 1 calc R . . C23 C 1.2661(2) 0.59042(12) 0.84337(15) 0.0418(6) Uani 1 1 d . . . H23A H 1.2514 0.6238 0.8688 0.050 Uiso 1 1 calc R . . C24 C 1.2027(2) 0.54272(13) 0.83069(15) 0.0445(7) Uani 1 1 d . . . H24A H 1.1436 0.5434 0.8466 0.053 Uiso 1 1 calc R . . C25 C 1.2247(2) 0.49381(13) 0.79499(15) 0.0416(6) Uani 1 1 d . . . H25A H 1.1811 0.4608 0.7867 0.050 Uiso 1 1 calc R . . C26 C 1.31047(19) 0.49285(11) 0.77119(13) 0.0335(5) Uani 1 1 d . . . H26A H 1.3257 0.4588 0.7472 0.040 Uiso 1 1 calc R . . C31 C 1.58484(17) 0.54802(9) 0.84977(12) 0.0241(5) Uani 1 1 d . . . C32 C 1.67309(18) 0.58089(10) 0.86286(13) 0.0300(5) Uani 1 1 d . . . H32A H 1.6839 0.6029 0.8223 0.036 Uiso 1 1 calc R . . C33 C 1.7458(2) 0.58190(11) 0.93470(14) 0.0367(6) Uani 1 1 d . . . H33A H 1.8059 0.6045 0.9431 0.044 Uiso 1 1 calc R . . C34 C 1.7300(2) 0.54969(10) 0.99414(13) 0.0360(6) Uani 1 1 d . . . H34A H 1.7791 0.5505 1.0434 0.043 Uiso 1 1 calc R . . C35 C 1.6434(2) 0.51669(10) 0.98170(13) 0.0340(5) Uani 1 1 d . . . H35A H 1.6333 0.4943 1.0222 0.041 Uiso 1 1 calc R . . C36 C 1.57019(19) 0.51597(10) 0.90976(13) 0.0301(5) Uani 1 1 d . . . H36A H 1.5100 0.4935 0.9017 0.036 Uiso 1 1 calc R . . C41 C 1.18922(19) 0.55374(10) 0.60168(14) 0.0323(5) Uani 1 1 d . . . H41A H 1.1765 0.5762 0.6411 0.039 Uiso 1 1 calc R . . C42 C 1.1309(2) 0.50396(11) 0.57425(16) 0.0429(6) Uani 1 1 d . . . H42A H 1.0778 0.4931 0.5942 0.052 Uiso 1 1 calc R . . C43 C 1.1505(2) 0.47074(12) 0.51817(16) 0.0447(7) Uani 1 1 d . . . H43A H 1.1109 0.4368 0.4996 0.054 Uiso 1 1 calc R . . C44 C 1.2271(2) 0.48619(10) 0.48857(14) 0.0375(6) Uani 1 1 d . . . H44A H 1.2405 0.4628 0.4502 0.045 Uiso 1 1 calc R . . C45 C 1.28412(19) 0.53565(10) 0.51472(13) 0.0308(5) Uani 1 1 d . . . H45A H 1.3365 0.5462 0.4939 0.037 Uiso 1 1 calc R . . C46 C 1.26573(17) 0.57075(9) 0.57186(12) 0.0236(4) Uani 1 1 d . . . C51 C 1.32116(17) 0.67582(9) 0.51560(12) 0.0242(5) Uani 1 1 d . . . C52 C 1.38782(19) 0.71912(9) 0.50809(13) 0.0274(5) Uani 1 1 d . . . H52A H 1.4503 0.7247 0.5476 0.033 Uiso 1 1 calc R . . C53 C 1.3641(2) 0.75453(10) 0.44338(13) 0.0320(5) Uani 1 1 d . . . H53A H 1.4100 0.7843 0.4393 0.038 Uiso 1 1 calc R . . C54 C 1.2739(2) 0.74633(11) 0.38519(14) 0.0351(6) Uani 1 1 d . . . H54A H 1.2578 0.7703 0.3409 0.042 Uiso 1 1 calc R . . C55 C 1.2069(2) 0.70311(11) 0.39154(13) 0.0348(6) Uani 1 1 d . . . H55A H 1.1449 0.6973 0.3516 0.042 Uiso 1 1 calc R . . C56 C 1.23037(18) 0.66837(10) 0.45633(13) 0.0299(5) Uani 1 1 d . . . H56A H 1.1839 0.6390 0.4605 0.036 Uiso 1 1 calc R . . C61 C 1.19992(18) 0.79497(9) 0.62640(13) 0.0274(5) Uani 1 1 d . . . C62 C 1.1478(2) 0.83354(11) 0.65901(16) 0.0428(7) Uani 1 1 d . . . H62A H 1.1694 0.8390 0.7128 0.051 Uiso 1 1 calc R . . C63 C 1.0645(2) 0.86416(13) 0.61363(17) 0.0528(8) Uani 1 1 d . . . H63A H 1.0299 0.8908 0.6365 0.063 Uiso 1 1 calc R . . C64 C 1.0315(2) 0.85633(12) 0.53584(16) 0.0439(7) Uani 1 1 d . . . H64A H 0.9727 0.8764 0.5053 0.053 Uiso 1 1 calc R . . C65 C 1.0834(2) 0.81949(11) 0.50215(15) 0.0397(6) Uani 1 1 d . . . H65A H 1.0620 0.8149 0.4482 0.048 Uiso 1 1 calc R . . C66 C 1.1674(2) 0.78911(11) 0.54730(14) 0.0371(6) Uani 1 1 d . . . H66A H 1.2033 0.7638 0.5238 0.045 Uiso 1 1 calc R . . C71 C 1.29627(19) 0.75837(10) 0.77907(13) 0.0287(5) Uani 1 1 d . . . C72 C 1.3693(2) 0.78897(13) 0.83515(15) 0.0447(7) Uani 1 1 d . . . H72A H 1.4284 0.8035 0.8253 0.054 Uiso 1 1 calc R . . C73 C 1.3549(3) 0.79809(16) 0.90598(17) 0.0620(9) Uani 1 1 d . . . H73A H 1.4051 0.8185 0.9448 0.074 Uiso 1 1 calc R . . C74 C 1.2692(3) 0.77793(14) 0.92012(17) 0.0536(8) Uani 1 1 d . . . H74A H 1.2594 0.7853 0.9681 0.064 Uiso 1 1 calc R . . C75 C 1.1979(2) 0.74726(13) 0.86538(16) 0.0457(7) Uani 1 1 d . . . H75A H 1.1390 0.7328 0.8757 0.055 Uiso 1 1 calc R . . C76 C 1.2110(2) 0.73715(11) 0.79514(14) 0.0344(6) Uani 1 1 d . . . H76A H 1.1614 0.7155 0.7575 0.041 Uiso 1 1 calc R . . C81 C 1.41133(17) 0.85409(9) 0.62800(13) 0.0278(5) Uani 1 1 d . . . H81A H 1.4252 0.8548 0.5790 0.042 Uiso 1 1 calc R . . H81B H 1.4452 0.8872 0.6593 0.042 Uiso 1 1 calc R . . H81C H 1.3378 0.8567 0.6191 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 Pd 0.02391(10) 0.02162(9) 0.02309(9) 0.00121(6) 0.00276(7) -0.00211(7) Ru 0.01939(9) 0.02366(9) 0.02003(9) 0.00245(6) 0.00452(7) 0.00018(7) Cl1 0.0280(3) 0.0229(2) 0.0238(3) 0.00099(19) 0.0013(2) -0.0009(2) Cl2 0.0284(3) 0.0372(3) 0.0371(3) 0.0026(2) 0.0071(3) -0.0081(3) P1 0.0212(3) 0.0218(3) 0.0198(3) 0.0009(2) 0.0031(2) 0.0003(2) P2 0.0207(3) 0.0218(3) 0.0186(3) 0.0006(2) 0.0032(2) -0.0004(2) P3 0.0242(3) 0.0216(3) 0.0224(3) -0.0002(2) 0.0042(2) 0.0005(2) C1 0.0282(13) 0.0478(14) 0.0258(12) 0.0044(10) 0.0126(10) 0.0053(11) C2 0.0359(14) 0.0369(13) 0.0356(13) -0.0002(10) 0.0193(11) 0.0037(11) C3 0.0276(13) 0.0489(15) 0.0394(14) 0.0105(12) 0.0161(11) 0.0124(12) C4 0.0210(12) 0.0547(16) 0.0377(14) 0.0042(11) 0.0111(11) -0.0015(11) C5 0.0291(13) 0.0405(13) 0.0359(13) 0.0077(10) 0.0173(11) 0.0001(11) C6 0.0228(11) 0.0233(10) 0.0237(11) 0.0000(8) 0.0049(9) -0.0001(9) C11 0.0294(12) 0.0227(10) 0.0245(11) 0.0002(8) 0.0094(10) -0.0003(9) C12 0.0358(14) 0.0282(12) 0.0287(12) 0.0014(9) 0.0084(10) 0.0022(10) C13 0.0606(19) 0.0303(13) 0.0296(13) -0.0059(10) 0.0134(13) -0.0058(13) C14 0.067(2) 0.0280(13) 0.0434(16) -0.0052(11) 0.0232(15) 0.0069(13) C15 0.0434(16) 0.0313(13) 0.0539(17) 0.0030(12) 0.0156(14) 0.0137(12) C16 0.0329(13) 0.0316(12) 0.0320(13) 0.0024(10) 0.0058(11) 0.0060(11) C21 0.0235(11) 0.0297(11) 0.0198(10) 0.0060(8) 0.0023(9) 0.0021(9) C22 0.0345(14) 0.0302(12) 0.0295(12) 0.0064(9) 0.0123(11) 0.0049(10) C23 0.0477(17) 0.0478(15) 0.0351(14) 0.0121(12) 0.0205(13) 0.0174(14) C24 0.0305(14) 0.0672(19) 0.0394(15) 0.0149(13) 0.0162(12) 0.0082(14) C25 0.0285(14) 0.0562(17) 0.0388(14) 0.0063(12) 0.0084(12) -0.0093(13) C26 0.0293(13) 0.0397(13) 0.0304(13) 0.0013(10) 0.0076(11) -0.0056(11) C31 0.0236(11) 0.0232(10) 0.0218(11) -0.0012(8) 0.0015(9) 0.0018(9) C32 0.0310(13) 0.0286(12) 0.0271(12) 0.0050(9) 0.0040(10) 0.0023(10) C33 0.0311(13) 0.0320(13) 0.0369(14) -0.0006(10) -0.0042(11) -0.0059(11) C34 0.0390(15) 0.0351(13) 0.0237(12) -0.0007(10) -0.0053(11) 0.0048(11) C35 0.0396(14) 0.0352(13) 0.0232(12) 0.0032(9) 0.0038(11) 0.0045(11) C36 0.0324(13) 0.0318(12) 0.0239(11) 0.0005(9) 0.0055(10) -0.0010(10) C41 0.0313(13) 0.0288(12) 0.0323(13) 0.0007(9) 0.0032(10) -0.0009(10) C42 0.0415(16) 0.0386(14) 0.0470(16) 0.0018(12) 0.0114(13) -0.0132(13) C43 0.0475(17) 0.0326(13) 0.0449(16) -0.0050(11) 0.0010(13) -0.0124(13) C44 0.0437(16) 0.0295(12) 0.0323(13) -0.0048(10) 0.0015(12) -0.0011(11) C45 0.0332(13) 0.0297(12) 0.0260(12) -0.0014(9) 0.0040(10) 0.0007(10) C46 0.0224(11) 0.0235(10) 0.0199(10) 0.0015(8) -0.0006(9) 0.0000(9) C51 0.0268(12) 0.0237(10) 0.0212(11) 0.0012(8) 0.0061(9) 0.0023(9) C52 0.0299(13) 0.0264(11) 0.0257(12) 0.0011(9) 0.0082(10) 0.0013(9) C53 0.0403(15) 0.0272(12) 0.0308(13) 0.0050(9) 0.0142(11) 0.0013(11) C54 0.0447(15) 0.0340(13) 0.0261(12) 0.0081(10) 0.0104(11) 0.0064(12) C55 0.0388(14) 0.0367(13) 0.0227(12) 0.0024(10) 0.0005(10) 0.0030(11) C56 0.0302(13) 0.0293(12) 0.0257(12) 0.0031(9) 0.0022(10) -0.0010(10) C61 0.0263(12) 0.0217(10) 0.0324(12) 0.0030(9) 0.0065(10) 0.0008(9) C62 0.0517(17) 0.0358(14) 0.0389(15) 0.0015(11) 0.0112(13) 0.0174(13) C63 0.059(2) 0.0488(17) 0.0522(18) 0.0096(14) 0.0204(16) 0.0319(16) C64 0.0342(15) 0.0427(15) 0.0505(17) 0.0169(12) 0.0069(13) 0.0131(12) C65 0.0363(15) 0.0431(14) 0.0344(14) 0.0068(11) 0.0032(12) 0.0041(12) C66 0.0360(14) 0.0397(14) 0.0324(13) 0.0011(10) 0.0058(11) 0.0087(12) C71 0.0335(13) 0.0271(11) 0.0238(11) -0.0011(9) 0.0065(10) 0.0044(10) C72 0.0409(16) 0.0565(17) 0.0343(14) -0.0114(12) 0.0081(13) -0.0081(14) C73 0.068(2) 0.078(2) 0.0358(16) -0.0249(15) 0.0095(16) -0.0106(19) C74 0.066(2) 0.067(2) 0.0317(15) -0.0074(13) 0.0211(15) 0.0087(17) C75 0.0485(17) 0.0530(17) 0.0415(16) 0.0032(13) 0.0224(14) 0.0093(14) C76 0.0332(14) 0.0375(13) 0.0318(13) -0.0002(10) 0.0090(11) 0.0032(11) C81 0.0227(11) 0.0241(11) 0.0316(12) 0.0124(9) 0.0014(10) -0.0003(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 Pd C81 2.081(2) . ? Pd P3 2.2208(6) . ? Pd Cl2 2.3843(6) . ? Pd Cl1 2.4479(5) . ? Ru C2 2.173(2) . ? Ru C1 2.191(2) . ? Ru C3 2.214(2) . ? Ru C5 2.222(2) . ? Ru C4 2.227(2) . ? Ru P2 2.3039(6) . ? Ru P1 2.3282(6) . ? Ru Cl1 2.4436(5) . ? P1 C11 1.833(2) . ? P1 C21 1.837(2) . ? P1 C31 1.841(2) . ? P2 C46 1.829(2) . ? P2 C51 1.843(2) . ? P2 C6 1.853(2) . ? P3 C71 1.822(2) . ? P3 C61 1.831(2) . ? P3 C6 1.854(2) . ? C1 C5 1.419(4) . ? C1 C2 1.422(3) . ? C1 H1A 1.0000 . ? C2 C3 1.434(4) . ? C2 H2A 1.0000 . ? C3 C4 1.405(4) . ? C3 H3A 1.0000 . ? C4 C5 1.437(3) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C11 C16 1.388(3) . ? C11 C12 1.400(3) . ? C12 C13 1.388(3) . ? C12 H12A 0.9500 . ? C13 C14 1.374(4) . ? C13 H13A 0.9500 . ? C14 C15 1.374(4) . ? C14 H14A 0.9500 . ? C15 C16 1.396(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 C26 1.387(3) . ? C21 C22 1.400(3) . ? C22 C23 1.389(4) . ? C22 H22A 0.9500 . ? C23 C24 1.375(4) . ? C23 H23A 0.9500 . ? C24 C25 1.380(4) . ? C24 H24A 0.9500 . ? C25 C26 1.387(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.390(3) . ? C31 C36 1.393(3) . ? C32 C33 1.392(3) . ? C32 H32A 0.9500 . ? C33 C34 1.392(4) . ? C33 H33A 0.9500 . ? C34 C35 1.374(4) . ? C34 H34A 0.9500 . ? C35 C36 1.396(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.391(3) . ? C41 C42 1.397(3) . ? C41 H41A 0.9500 . ? C42 C43 1.376(4) . ? C42 H42A 0.9500 . ? C43 C44 1.380(4) . ? C43 H43A 0.9500 . ? C44 C45 1.379(3) . ? C44 H44A 0.9500 . ? C45 C46 1.409(3) . ? C45 H45A 0.9500 . ? C51 C52 1.390(3) . ? C51 C56 1.395(3) . ? C52 C53 1.394(3) . ? C52 H52A 0.9500 . ? C53 C54 1.383(4) . ? C53 H53A 0.9500 . ? C54 C55 1.385(4) . ? C54 H54A 0.9500 . ? C55 C56 1.386(3) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.389(3) . ? C61 C66 1.391(3) . ? C62 C63 1.386(4) . ? C62 H62A 0.9500 . ? C63 C64 1.374(4) . ? C63 H63A 0.9500 . ? C64 C65 1.375(4) . ? C64 H64A 0.9500 . ? C65 C66 1.387(4) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C76 1.389(4) . ? C71 C72 1.390(3) . ? C72 C73 1.395(4) . ? C72 H72A 0.9500 . ? C73 C74 1.370(5) . ? C73 H73A 0.9500 . ? C74 C75 1.366(4) . ? C74 H74A 0.9500 . ? C75 C76 1.381(4) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 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 C81 Pd P3 90.09(7) . . ? C81 Pd Cl2 90.75(7) . . ? P3 Pd Cl2 177.51(2) . . ? C81 Pd Cl1 175.00(7) . . ? P3 Pd Cl1 87.44(2) . . ? Cl2 Pd Cl1 91.90(2) . . ? C2 Ru C1 38.04(9) . . ? C2 Ru C3 38.15(10) . . ? C1 Ru C3 62.68(9) . . ? C2 Ru C5 63.58(9) . . ? C1 Ru C5 37.52(9) . . ? C3 Ru C5 62.47(9) . . ? C2 Ru C4 63.32(10) . . ? C1 Ru C4 62.67(10) . . ? C3 Ru C4 36.89(10) . . ? C5 Ru C4 37.68(9) . . ? C2 Ru P2 109.53(7) . . ? C1 Ru P2 91.11(7) . . ? C3 Ru P2 147.68(7) . . ? C5 Ru P2 108.75(7) . . ? C4 Ru P2 146.35(7) . . ? C2 Ru P1 98.15(7) . . ? C1 Ru P1 134.92(7) . . ? C3 Ru P1 89.11(7) . . ? C5 Ru P1 151.03(7) . . ? C4 Ru P1 115.03(7) . . ? P2 Ru P1 98.33(2) . . ? C2 Ru Cl1 157.80(7) . . ? C1 Ru Cl1 135.86(7) . . ? C3 Ru Cl1 121.45(7) . . ? C5 Ru Cl1 101.34(7) . . ? C4 Ru Cl1 94.68(7) . . ? P2 Ru Cl1 90.33(2) . . ? P1 Ru Cl1 88.314(19) . . ? Ru Cl1 Pd 104.82(2) . . ? C11 P1 C21 104.41(10) . . ? C11 P1 C31 102.10(10) . . ? C21 P1 C31 98.88(10) . . ? C11 P1 Ru 110.50(7) . . ? C21 P1 Ru 123.53(7) . . ? C31 P1 Ru 114.82(7) . . ? C46 P2 C51 100.24(10) . . ? C46 P2 C6 101.62(10) . . ? C51 P2 C6 100.80(10) . . ? C46 P2 Ru 114.23(7) . . ? C51 P2 Ru 116.54(8) . . ? C6 P2 Ru 120.39(7) . . ? C71 P3 C61 101.99(11) . . ? C71 P3 C6 103.67(10) . . ? C61 P3 C6 103.15(10) . . ? C71 P3 Pd 111.58(8) . . ? C61 P3 Pd 120.56(8) . . ? C6 P3 Pd 113.97(7) . . ? C5 C1 C2 109.2(2) . . ? C5 C1 Ru 72.42(13) . . ? C2 C1 Ru 70.30(13) . . ? C5 C1 H1A 125.4 . . ? C2 C1 H1A 125.4 . . ? Ru C1 H1A 125.4 . . ? C1 C2 C3 106.7(2) . . ? C1 C2 Ru 71.67(13) . . ? C3 C2 Ru 72.47(14) . . ? C1 C2 H2A 126.5 . . ? C3 C2 H2A 126.5 . . ? Ru C2 H2A 126.5 . . ? C4 C3 C2 108.9(2) . . ? C4 C3 Ru 72.07(15) . . ? C2 C3 Ru 69.38(13) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Ru C3 H3A 125.5 . . ? C3 C4 C5 108.1(2) . . ? C3 C4 Ru 71.04(14) . . ? C5 C4 Ru 70.95(14) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Ru C4 H4A 125.9 . . ? C1 C5 C4 107.2(2) . . ? C1 C5 Ru 70.06(13) . . ? C4 C5 Ru 71.37(13) . . ? C1 C5 H5A 126.4 . . ? C4 C5 H5A 126.4 . . ? Ru C5 H5A 126.4 . . ? P2 C6 P3 119.58(12) . . ? P2 C6 H6A 107.4 . . ? P3 C6 H6A 107.4 . . ? P2 C6 H6B 107.4 . . ? P3 C6 H6B 107.4 . . ? H6A C6 H6B 107.0 . . ? C16 C11 C12 118.3(2) . . ? C16 C11 P1 122.29(18) . . ? C12 C11 P1 119.12(17) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C11 C16 C15 120.7(2) . . ? C11 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C26 C21 C22 118.6(2) . . ? C26 C21 P1 124.59(18) . . ? C22 C21 P1 116.80(18) . . ? C23 C22 C21 120.3(2) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.8(2) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? C32 C31 C36 118.9(2) . . ? C32 C31 P1 120.90(17) . . ? C36 C31 P1 120.12(17) . . ? C31 C32 C33 120.7(2) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C32 C33 C34 119.7(2) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 120.1(2) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C31 C36 C35 120.4(2) . . ? C31 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C46 C41 C42 120.7(2) . . ? C46 C41 H41A 119.6 . . ? C42 C41 H41A 119.6 . . ? C43 C42 C41 119.7(3) . . ? C43 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C42 C43 C44 120.6(2) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C45 C44 C43 119.9(2) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C46 120.9(2) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C41 C46 C45 118.1(2) . . ? C41 C46 P2 123.94(17) . . ? C45 C46 P2 117.90(17) . . ? C52 C51 C56 118.2(2) . . ? C52 C51 P2 120.24(17) . . ? C56 C51 P2 121.31(17) . . ? C51 C52 C53 120.9(2) . . ? C51 C52 H52A 119.6 . . ? C53 C52 H52A 119.6 . . ? C54 C53 C52 120.0(2) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C53 C54 C55 119.9(2) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.1 . . ? C54 C55 C56 119.9(2) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C55 C56 C51 121.1(2) . . ? C55 C56 H56A 119.4 . . ? C51 C56 H56A 119.4 . . ? C62 C61 C66 118.1(2) . . ? C62 C61 P3 122.10(19) . . ? C66 C61 P3 119.78(18) . . ? C63 C62 C61 120.5(3) . . ? C63 C62 H62A 119.8 . . ? C61 C62 H62A 119.8 . . ? C64 C63 C62 120.5(3) . . ? C64 C63 H63A 119.7 . . ? C62 C63 H63A 119.7 . . ? C63 C64 C65 120.0(3) . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C64 C65 C66 119.7(3) . . ? C64 C65 H65A 120.2 . . ? C66 C65 H65A 120.2 . . ? C65 C66 C61 121.2(2) . . ? C65 C66 H66A 119.4 . . ? C61 C66 H66A 119.4 . . ? C76 C71 C72 119.2(2) . . ? C76 C71 P3 121.91(18) . . ? C72 C71 P3 118.7(2) . . ? C71 C72 C73 119.3(3) . . ? C71 C72 H72A 120.4 . . ? C73 C72 H72A 120.4 . . ? C74 C73 C72 120.7(3) . . ? C74 C73 H73A 119.7 . . ? C72 C73 H73A 119.7 . . ? C75 C74 C73 120.2(3) . . ? C75 C74 H74A 119.9 . . ? C73 C74 H74A 119.9 . . ? C74 C75 C76 120.2(3) . . ? C74 C75 H75A 119.9 . . ? C76 C75 H75A 119.9 . . ? C75 C76 C71 120.5(3) . . ? C75 C76 H76A 119.7 . . ? C71 C76 H76A 119.7 . . ? Pd C81 H81A 109.5 . . ? Pd C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? Pd C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.882 _refine_diff_density_min -1.874 _refine_diff_density_rms 0.070 #END=== #Compound #10 data_yy03 _database_code_CSD 215182 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H48 Au Cl2 P3 Ru' _chemical_formula_weight 1122.74 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' 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' Au Au -2.0133 8.8022 '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 13.7910(6) _cell_length_b 18.5416(8) _cell_length_c 18.4876(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.800(2) _cell_angle_gamma 90.00 _cell_volume 4447.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 3.898 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3779 _exptl_absorpt_correction_T_max 0.7741 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 39309 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10148 _reflns_number_gt 8550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0321P)^2^+4.4962P] 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 10148 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.002 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 Au Au 1.004604(11) 0.131021(8) -0.355566(8) 0.03250(5) Uani 0.9404(9) 1 d P A 1 Cl2 Cl 0.91244(8) 0.20769(6) -0.44997(6) 0.0477(2) Uani 0.9404(9) 1 d P A 1 Au" Au 1.2077(6) -0.0355(5) -0.3023(5) 0.0681(18) Uiso 0.0298(4) 1 d P A 2 Cl2" Cl 1.289(9) -0.080(8) -0.368(7) 0.09(2) Uiso 0.0298(4) 1 d P A 2 Au' Au 1.1685(7) 0.1193(7) -0.1574(6) 0.0681(18) Uiso 0.0298(4) 1 d P A 3 Cl2' Cl 1.231(6) 0.156(5) -0.046(5) 0.09(2) Uiso 0.0298(4) 1 d P A 3 Ru Ru 0.580120(18) 0.184678(13) -0.172781(14) 0.02293(7) Uani 1 1 d . . . P1 P 1.09000(7) 0.05013(5) -0.26747(5) 0.02987(18) Uani 1 1 d . . . P2 P 0.70232(6) 0.16633(4) -0.23106(5) 0.02424(17) Uani 1 1 d . . . P3 P 0.69373(6) 0.21463(4) -0.05343(5) 0.02433(17) Uani 1 1 d . . . Cl1 Cl 0.58413(6) 0.05407(4) -0.14717(5) 0.03379(18) Uani 1 1 d . . . C1 C 0.5089(3) 0.28999(19) -0.2026(2) 0.0376(8) Uani 1 1 d . . . H1A H 0.5457 0.3373 -0.1955 0.045 Uiso 1 1 calc R . . C2 C 0.4793(3) 0.2477(2) -0.2695(2) 0.0378(8) Uani 1 1 d . . . H2A H 0.4935 0.2593 -0.3179 0.045 Uiso 1 1 calc R . . C3 C 0.4222(2) 0.1879(2) -0.2587(2) 0.0353(8) Uani 1 1 d . . . H3A H 0.3890 0.1498 -0.2975 0.042 Uiso 1 1 calc R . . C4 C 0.4154(3) 0.1947(2) -0.1834(2) 0.0374(8) Uani 1 1 d . . . H4A H 0.3771 0.1615 -0.1600 0.045 Uiso 1 1 calc R . . C5 C 0.4668(3) 0.2572(2) -0.1499(2) 0.0397(9) Uani 1 1 d . . . H5A H 0.4711 0.2769 -0.0985 0.048 Uiso 1 1 calc R . . C6 C 0.7963(3) 0.09355(18) -0.19408(19) 0.0307(7) Uani 1 1 d . . . H6A H 0.8462 0.1096 -0.1443 0.037 Uiso 1 1 calc R . . H6B H 0.7591 0.0515 -0.1833 0.037 Uiso 1 1 calc R . . C7 C 0.8575(2) 0.06781(18) -0.24409(19) 0.0299(7) Uani 1 1 d . A . H7A H 0.8101 0.0452 -0.2914 0.036 Uiso 1 1 calc R . . H7B H 0.8906 0.1097 -0.2595 0.036 Uiso 1 1 calc R . . C8 C 0.9395(3) 0.01377(19) -0.2013(2) 0.0324(7) Uani 1 1 d . . . H8A H 0.9053 -0.0270 -0.1851 0.039 Uiso 1 1 calc R A . H8B H 0.9859 0.0372 -0.1542 0.039 Uiso 1 1 calc R . . C9 C 1.0052(2) -0.01669(18) -0.2465(2) 0.0318(7) Uani 1 1 d . A . H9A H 0.9590 -0.0370 -0.2956 0.038 Uiso 1 1 calc R . . H9B H 1.0479 -0.0566 -0.2166 0.038 Uiso 1 1 calc R . . C11 C 1.1653(3) 0.0837(2) -0.1745(2) 0.0378(9) Uani 1 1 d . A 1 C12 C 1.2250(3) 0.0392(2) -0.1174(2) 0.0453(9) Uani 1 1 d . A 1 H12A H 1.2289 -0.0107 -0.1280 0.054 Uiso 1 1 calc R A 1 C13 C 1.2792(3) 0.0649(2) -0.0454(2) 0.0529(11) Uani 1 1 d . A 1 H13A H 1.3210 0.0330 -0.0074 0.063 Uiso 1 1 calc R A 1 C14 C 1.2737(4) 0.1362(3) -0.0277(3) 0.0561(13) Uani 1 1 d . A 1 H14A H 1.3102 0.1530 0.0227 0.067 Uiso 1 1 calc R A 1 C15 C 1.2140(4) 0.1846(3) -0.0841(3) 0.0556(12) Uani 1 1 d . A 1 H15A H 1.2104 0.2342 -0.0722 0.067 Uiso 1 1 calc R A 1 C16 C 1.1595(3) 0.1583(3) -0.1588(3) 0.0451(10) Uani 1 1 d . A 1 H16A H 1.1195 0.1901 -0.1978 0.054 Uiso 1 1 calc R A 1 C21 C 1.1780(3) -0.0001(2) -0.3000(2) 0.0339(8) Uani 1 1 d . A 1 C22 C 1.1433(3) -0.0581(2) -0.3517(2) 0.0411(8) Uani 1 1 d . A 1 H22A H 1.0732 -0.0728 -0.3669 0.049 Uiso 1 1 calc R A 1 C23 C 1.2104(4) -0.0938(2) -0.3805(2) 0.0482(10) Uani 1 1 d . A 1 H23A H 1.1868 -0.1333 -0.4147 0.058 Uiso 1 1 calc R A 1 C24 C 1.3140(5) -0.0712(5) -0.3590(4) 0.0466(17) Uani 1 1 d . A 1 H24A H 1.3601 -0.0953 -0.3792 0.056 Uiso 1 1 calc R A 1 C25 C 1.3477(3) -0.0161(2) -0.3101(3) 0.0481(10) Uani 1 1 d . A 1 H25A H 1.4174 -0.0008 -0.2962 0.058 Uiso 1 1 calc R A 1 C26 C 1.2809(3) 0.0192(2) -0.2794(2) 0.0435(9) Uani 1 1 d . A 1 H26A H 1.3065 0.0572 -0.2436 0.052 Uiso 1 1 calc R A 1 C31 C 0.6449(2) 0.14095(17) -0.33332(19) 0.0279(7) Uani 1 1 d . . . C32 C 0.5565(3) 0.0985(2) -0.3548(2) 0.0358(8) Uani 1 1 d . . . H32A H 0.5280 0.0832 -0.3172 0.043 Uiso 1 1 calc R . . C33 C 0.5097(3) 0.0785(2) -0.4314(2) 0.0422(9) Uani 1 1 d . . . H33A H 0.4485 0.0504 -0.4461 0.051 Uiso 1 1 calc R . . C34 C 0.5511(3) 0.0989(2) -0.4855(2) 0.0447(9) Uani 1 1 d . . . H34A H 0.5181 0.0858 -0.5378 0.054 Uiso 1 1 calc R . . C35 C 0.6414(3) 0.1386(2) -0.4641(2) 0.0417(9) Uani 1 1 d . . . H35A H 0.6714 0.1517 -0.5015 0.050 Uiso 1 1 calc R . . C36 C 0.6881(3) 0.1594(2) -0.3885(2) 0.0340(7) Uani 1 1 d . . . H36A H 0.7502 0.1865 -0.3742 0.041 Uiso 1 1 calc R . . C41 C 0.7814(2) 0.24413(18) -0.23750(18) 0.0284(7) Uani 1 1 d . . . C42 C 0.8876(3) 0.2472(2) -0.1993(2) 0.0382(8) Uani 1 1 d . . . H42A H 0.9224 0.2072 -0.1697 0.046 Uiso 1 1 calc R . . C43 C 0.9424(3) 0.3083(2) -0.2045(3) 0.0529(11) Uani 1 1 d . . . H43A H 1.0147 0.3095 -0.1781 0.063 Uiso 1 1 calc R . . C44 C 0.8951(3) 0.3670(2) -0.2465(3) 0.0549(12) Uani 1 1 d . . . H44A H 0.9341 0.4085 -0.2493 0.066 Uiso 1 1 calc R . . C45 C 0.7889(3) 0.3652(2) -0.2854(3) 0.0475(10) Uani 1 1 d . . . H45A H 0.7548 0.4053 -0.3153 0.057 Uiso 1 1 calc R . . C46 C 0.7337(3) 0.30409(19) -0.2797(2) 0.0357(8) Uani 1 1 d . . . H46A H 0.6613 0.3033 -0.3054 0.043 Uiso 1 1 calc R . . C51 C 0.6578(3) 0.18650(19) 0.02949(19) 0.0310(7) Uani 1 1 d . . . C52 C 0.7177(3) 0.2089(3) 0.1031(2) 0.0460(10) Uani 1 1 d . . . H52A H 0.7747 0.2401 0.1094 0.055 Uiso 1 1 calc R . . C53 C 0.6956(4) 0.1864(3) 0.1671(2) 0.0578(12) Uani 1 1 d . . . H53A H 0.7358 0.2027 0.2169 0.069 Uiso 1 1 calc R . . C54 C 0.6143(4) 0.1399(3) 0.1574(3) 0.0564(12) Uani 1 1 d . . . H54A H 0.5987 0.1241 0.2011 0.068 Uiso 1 1 calc R . . C55 C 0.5555(3) 0.1162(3) 0.0857(3) 0.0518(11) Uani 1 1 d . . . H55A H 0.5004 0.0835 0.0801 0.062 Uiso 1 1 calc R . . C56 C 0.5766(3) 0.1401(2) 0.0208(2) 0.0377(8) Uani 1 1 d . . . H56A H 0.5351 0.1245 -0.0290 0.045 Uiso 1 1 calc R . . C61 C 0.7047(2) 0.31315(18) -0.04314(18) 0.0282(7) Uani 1 1 d . . . C62 C 0.7541(3) 0.35286(18) -0.08521(19) 0.0312(7) Uani 1 1 d . . . H62A H 0.7877 0.3281 -0.1150 0.037 Uiso 1 1 calc R . . C63 C 0.7547(3) 0.42764(19) -0.0841(2) 0.0367(8) Uani 1 1 d . . . H63A H 0.7901 0.4535 -0.1119 0.044 Uiso 1 1 calc R . . C64 C 0.7040(3) 0.4644(2) -0.0428(2) 0.0449(9) Uani 1 1 d . . . H64A H 0.7041 0.5157 -0.0423 0.054 Uiso 1 1 calc R . . C65 C 0.6530(4) 0.4265(2) -0.0019(3) 0.0520(11) Uani 1 1 d . . . H65A H 0.6172 0.4519 0.0260 0.062 Uiso 1 1 calc R . . C66 C 0.6540(3) 0.3513(2) -0.0016(2) 0.0408(9) Uani 1 1 d . . . H66A H 0.6197 0.3258 0.0272 0.049 Uiso 1 1 calc R . . C71 C 0.8274(2) 0.18093(18) -0.01775(17) 0.0272(7) Uani 1 1 d . . . C72 C 0.8367(3) 0.10672(19) -0.0040(2) 0.0326(7) Uani 1 1 d . . . H72A H 0.7766 0.0782 -0.0127 0.039 Uiso 1 1 calc R . . C73 C 0.9323(3) 0.0747(2) 0.0221(2) 0.0386(8) Uani 1 1 d . . . H73A H 0.9377 0.0244 0.0323 0.046 Uiso 1 1 calc R . . C74 C 1.0206(3) 0.1151(2) 0.0337(2) 0.0436(9) Uani 1 1 d . . . H74A H 1.0864 0.0925 0.0504 0.052 Uiso 1 1 calc R . . C75 C 1.0124(3) 0.1881(2) 0.0208(2) 0.0441(9) Uani 1 1 d . . . H75A H 1.0726 0.2164 0.0291 0.053 Uiso 1 1 calc R . . C76 C 0.9159(2) 0.22057(17) -0.00430(19) 0.0282(7) Uani 1 1 d . . . H76A H 0.9111 0.2712 -0.0124 0.034 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 Au 0.03092(8) 0.02872(8) 0.03948(9) 0.00587(6) 0.01403(6) 0.00267(6) Cl2 0.0468(6) 0.0446(6) 0.0497(6) 0.0169(5) 0.0139(5) 0.0059(5) Ru 0.01966(12) 0.02243(13) 0.02586(13) 0.00033(10) 0.00661(9) 0.00040(9) P1 0.0285(4) 0.0255(4) 0.0376(5) -0.0013(4) 0.0138(4) -0.0002(3) P2 0.0229(4) 0.0241(4) 0.0259(4) 0.0002(3) 0.0085(3) 0.0008(3) P3 0.0244(4) 0.0240(4) 0.0250(4) 0.0007(3) 0.0089(3) -0.0011(3) Cl1 0.0342(4) 0.0240(4) 0.0430(4) 0.0014(3) 0.0129(3) -0.0028(3) C1 0.0296(17) 0.0257(17) 0.050(2) 0.0032(16) 0.0031(15) 0.0087(14) C2 0.0260(16) 0.044(2) 0.0405(19) 0.0141(17) 0.0078(14) 0.0100(15) C3 0.0193(15) 0.042(2) 0.0376(18) 0.0006(16) 0.0005(13) 0.0037(14) C4 0.0204(15) 0.045(2) 0.045(2) 0.0027(17) 0.0094(14) 0.0042(15) C5 0.0292(17) 0.045(2) 0.042(2) -0.0050(17) 0.0081(15) 0.0158(16) C6 0.0302(16) 0.0302(17) 0.0342(17) 0.0062(14) 0.0141(14) 0.0063(14) C7 0.0264(16) 0.0298(17) 0.0326(17) -0.0016(14) 0.0089(13) 0.0033(13) C8 0.0269(16) 0.0316(18) 0.0411(19) 0.0078(15) 0.0148(14) 0.0024(14) C9 0.0264(16) 0.0252(16) 0.0444(19) 0.0008(14) 0.0129(14) -0.0001(13) C11 0.035(2) 0.0298(19) 0.052(2) -0.0137(18) 0.0196(17) -0.0081(16) C12 0.049(2) 0.037(2) 0.045(2) 0.0003(18) 0.0093(18) -0.0055(17) C13 0.052(2) 0.050(3) 0.046(2) 0.002(2) 0.0028(19) -0.021(2) C14 0.047(3) 0.068(4) 0.050(3) -0.018(3) 0.011(2) -0.020(3) C15 0.050(3) 0.045(3) 0.072(3) -0.024(3) 0.022(2) -0.010(2) C16 0.037(2) 0.033(2) 0.065(3) -0.001(2) 0.0174(19) 0.0021(18) C21 0.040(2) 0.0235(16) 0.0403(19) 0.0009(15) 0.0171(16) 0.0082(15) C22 0.039(2) 0.037(2) 0.048(2) -0.0075(17) 0.0150(17) -0.0038(16) C23 0.057(3) 0.044(2) 0.046(2) -0.0065(19) 0.021(2) 0.004(2) C24 0.043(3) 0.062(4) 0.040(3) 0.007(3) 0.021(3) 0.019(3) C25 0.037(2) 0.054(3) 0.059(3) 0.007(2) 0.0238(19) 0.0046(18) C26 0.039(2) 0.044(2) 0.053(2) -0.0057(18) 0.0224(18) -0.0039(17) C31 0.0269(15) 0.0279(16) 0.0282(16) -0.0007(13) 0.0084(13) 0.0040(13) C32 0.0351(18) 0.039(2) 0.0348(18) -0.0089(15) 0.0132(15) -0.0046(15) C33 0.039(2) 0.041(2) 0.043(2) -0.0130(17) 0.0098(17) -0.0047(17) C34 0.054(2) 0.042(2) 0.0321(19) -0.0108(17) 0.0069(17) 0.0033(19) C35 0.054(2) 0.042(2) 0.0331(19) 0.0013(16) 0.0195(17) 0.0059(18) C36 0.0336(18) 0.0339(18) 0.0346(18) -0.0016(15) 0.0118(14) 0.0027(15) C41 0.0290(16) 0.0274(16) 0.0303(16) -0.0021(13) 0.0119(13) -0.0012(13) C42 0.0283(17) 0.0337(19) 0.050(2) -0.0050(16) 0.0099(15) 0.0003(14) C43 0.0289(19) 0.043(2) 0.084(3) -0.011(2) 0.016(2) -0.0075(17) C44 0.047(2) 0.037(2) 0.088(3) -0.009(2) 0.032(2) -0.0158(18) C45 0.051(2) 0.0308(19) 0.065(3) 0.0067(18) 0.025(2) -0.0040(17) C46 0.0313(17) 0.0306(18) 0.046(2) 0.0028(16) 0.0145(15) -0.0044(14) C51 0.0316(17) 0.0337(18) 0.0295(16) 0.0043(14) 0.0128(13) 0.0018(14) C52 0.040(2) 0.065(3) 0.0317(18) -0.0008(18) 0.0102(16) -0.0094(19) C53 0.056(3) 0.087(4) 0.0291(19) 0.003(2) 0.0118(18) -0.004(2) C54 0.058(3) 0.073(3) 0.045(2) 0.023(2) 0.026(2) 0.009(2) C55 0.043(2) 0.063(3) 0.055(3) 0.015(2) 0.024(2) -0.005(2) C56 0.0357(19) 0.040(2) 0.0374(19) 0.0038(16) 0.0128(15) -0.0013(15) C61 0.0267(16) 0.0254(16) 0.0306(16) -0.0019(13) 0.0070(13) -0.0015(13) C62 0.0333(17) 0.0281(17) 0.0288(16) 0.0016(14) 0.0060(13) 0.0030(14) C63 0.0370(19) 0.0279(17) 0.0386(19) 0.0026(15) 0.0042(15) -0.0054(14) C64 0.055(2) 0.0245(18) 0.047(2) -0.0058(16) 0.0057(19) -0.0016(16) C65 0.069(3) 0.034(2) 0.058(3) -0.0164(19) 0.028(2) 0.001(2) C66 0.052(2) 0.0329(19) 0.044(2) -0.0082(17) 0.0235(18) -0.0050(17) C71 0.0278(16) 0.0286(16) 0.0236(15) 0.0002(13) 0.0066(12) 0.0024(13) C72 0.0289(16) 0.0308(17) 0.0356(18) 0.0029(15) 0.0076(14) -0.0030(14) C73 0.0391(19) 0.0346(19) 0.0370(19) 0.0084(16) 0.0063(15) 0.0040(16) C74 0.0295(18) 0.050(2) 0.046(2) 0.0048(18) 0.0054(16) 0.0092(17) C75 0.0274(18) 0.046(2) 0.054(2) 0.0038(19) 0.0074(16) -0.0034(16) C76 0.0269(15) 0.0236(16) 0.0337(16) 0.0067(13) 0.0099(13) 0.0018(12) _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 Au P1 2.2337(9) . ? Au Cl2 2.2759(10) . ? Au" Cl2" 2.08(13) . ? Au" P1 2.506(9) . ? Au' Cl2' 2.06(9) . ? Au' P1 2.338(12) . ? Ru C1 2.172(3) . ? Ru C2 2.194(3) . ? Ru C5 2.209(3) . ? Ru C3 2.220(3) . ? Ru C4 2.220(3) . ? Ru P3 2.3000(8) . ? Ru P2 2.3123(8) . ? Ru Cl1 2.4645(9) . ? P1 C21 1.789(4) . ? P1 C11 1.793(4) . ? P1 C9 1.833(3) . ? P2 C6 1.835(3) . ? P2 C41 1.836(3) . ? P2 C31 1.846(3) . ? P3 C61 1.838(3) . ? P3 C51 1.839(3) . ? P3 C71 1.844(3) . ? C1 C2 1.403(5) . ? C1 C5 1.429(6) . ? C2 C3 1.413(5) . ? C3 C4 1.432(5) . ? C4 C5 1.391(6) . ? C6 C7 1.524(4) . ? C7 C8 1.517(4) . ? C8 C9 1.533(5) . ? C11 C12 1.373(6) . ? C11 C16 1.421(6) . ? C12 C13 1.373(6) . ? C13 C14 1.369(7) . ? C14 C15 1.411(9) . ? C15 C16 1.416(7) . ? C21 C26 1.386(5) . ? C21 C22 1.409(5) . ? C22 C23 1.383(6) . ? C23 C24 1.410(9) . ? C24 C25 1.340(9) . ? C25 C26 1.398(5) . ? C31 C36 1.387(5) . ? C31 C32 1.392(5) . ? C32 C33 1.394(5) . ? C33 C34 1.362(6) . ? C34 C35 1.385(6) . ? C35 C36 1.381(5) . ? C41 C46 1.389(5) . ? C41 C42 1.395(5) . ? C42 C43 1.383(6) . ? C43 C44 1.368(6) . ? C44 C45 1.397(6) . ? C45 C46 1.389(5) . ? C51 C56 1.378(5) . ? C51 C52 1.396(5) . ? C52 C53 1.382(6) . ? C53 C54 1.376(7) . ? C54 C55 1.372(7) . ? C55 C56 1.399(6) . ? C61 C66 1.394(5) . ? C61 C62 1.403(5) . ? C62 C63 1.387(5) . ? C63 C64 1.378(6) . ? C64 C65 1.386(6) . ? C65 C66 1.395(5) . ? C71 C76 1.374(4) . ? C71 C72 1.397(5) . ? C72 C73 1.376(5) . ? C73 C74 1.384(5) . ? C74 C75 1.372(6) . ? C75 C76 1.389(5) . ? 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 P1 Au Cl2 176.47(4) . . ? Cl2" Au" P1 158(4) . . ? Cl2' Au' P1 165(3) . . ? C1 Ru C2 37.48(14) . . ? C1 Ru C5 38.05(15) . . ? C2 Ru C5 62.48(14) . . ? C1 Ru C3 62.87(14) . . ? C2 Ru C3 37.34(14) . . ? C5 Ru C3 62.27(14) . . ? C1 Ru C4 62.68(14) . . ? C2 Ru C4 62.39(14) . . ? C5 Ru C4 36.60(14) . . ? C3 Ru C4 37.64(14) . . ? C1 Ru P3 97.43(10) . . ? C2 Ru P3 133.71(11) . . ? C5 Ru P3 88.01(10) . . ? C3 Ru P3 149.84(10) . . ? C4 Ru P3 114.14(10) . . ? C1 Ru P2 110.63(11) . . ? C2 Ru P2 93.38(10) . . ? C5 Ru P2 148.60(11) . . ? C3 Ru P2 111.31(10) . . ? C4 Ru P2 148.88(10) . . ? P3 Ru P2 96.63(3) . . ? C1 Ru Cl1 155.66(10) . . ? C2 Ru Cl1 130.31(11) . . ? C5 Ru Cl1 122.19(11) . . ? C3 Ru Cl1 96.70(10) . . ? C4 Ru Cl1 93.14(10) . . ? P3 Ru Cl1 95.12(3) . . ? P2 Ru Cl1 88.42(3) . . ? C21 P1 C11 105.38(18) . . ? C21 P1 C9 105.84(16) . . ? C11 P1 C9 103.62(17) . . ? C21 P1 Au 110.78(12) . . ? C11 P1 Au 117.21(15) . . ? C9 P1 Au 113.06(11) . . ? C21 P1 Au' 114.3(3) . . ? C11 P1 Au' 13.4(3) . . ? C9 P1 Au' 109.1(3) . . ? Au P1 Au' 103.9(3) . . ? C21 P1 Au" 8.4(2) . . ? C11 P1 Au" 104.5(2) . . ? C9 P1 Au" 98.1(2) . . ? Au P1 Au" 117.74(19) . . ? Au' P1 Au" 114.9(3) . . ? C6 P2 C41 103.99(15) . . ? C6 P2 C31 101.41(15) . . ? C41 P2 C31 101.06(15) . . ? C6 P2 Ru 117.96(11) . . ? C41 P2 Ru 117.21(11) . . ? C31 P2 Ru 112.79(11) . . ? C61 P3 C51 103.41(16) . . ? C61 P3 C71 105.21(15) . . ? C51 P3 C71 97.17(15) . . ? C61 P3 Ru 110.18(11) . . ? C51 P3 Ru 116.28(11) . . ? C71 P3 Ru 122.34(10) . . ? C2 C1 C5 107.5(3) . . ? C2 C1 Ru 72.1(2) . . ? C5 C1 Ru 72.4(2) . . ? C1 C2 C3 108.9(3) . . ? C1 C2 Ru 70.40(19) . . ? C3 C2 Ru 72.31(19) . . ? C2 C3 C4 107.0(3) . . ? C2 C3 Ru 70.35(19) . . ? C4 C3 Ru 71.21(19) . . ? C5 C4 C3 108.4(3) . . ? C5 C4 Ru 71.3(2) . . ? C3 C4 Ru 71.16(19) . . ? C4 C5 C1 108.2(3) . . ? C4 C5 Ru 72.1(2) . . ? C1 C5 Ru 69.55(19) . . ? C7 C6 P2 118.1(2) . . ? C8 C7 C6 111.0(3) . . ? C7 C8 C9 115.7(3) . . ? C8 C9 P1 113.8(2) . . ? C12 C11 C16 119.3(4) . . ? C12 C11 P1 122.0(3) . . ? C16 C11 P1 118.6(3) . . ? C11 C12 C13 121.5(4) . . ? C14 C13 C12 120.8(4) . . ? C13 C14 C15 120.2(4) . . ? C14 C15 C16 119.0(4) . . ? C15 C16 C11 119.1(5) . . ? C26 C21 C22 117.7(4) . . ? C26 C21 P1 121.4(3) . . ? C22 C21 P1 120.8(3) . . ? C23 C22 C21 120.5(4) . . ? C22 C23 C24 119.7(4) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 120.4(4) . . ? C21 C26 C25 121.4(4) . . ? C36 C31 C32 118.9(3) . . ? C36 C31 P2 123.3(3) . . ? C32 C31 P2 117.8(3) . . ? C31 C32 C33 119.9(3) . . ? C34 C33 C32 120.6(4) . . ? C33 C34 C35 119.8(3) . . ? C36 C35 C34 120.3(4) . . ? C35 C36 C31 120.4(3) . . ? C46 C41 C42 117.9(3) . . ? C46 C41 P2 119.1(2) . . ? C42 C41 P2 122.9(3) . . ? C43 C42 C41 120.2(4) . . ? C44 C43 C42 121.7(4) . . ? C43 C44 C45 119.2(4) . . ? C46 C45 C44 119.1(4) . . ? C45 C46 C41 121.9(3) . . ? C56 C51 C52 119.3(3) . . ? C56 C51 P3 121.2(3) . . ? C52 C51 P3 119.4(3) . . ? C53 C52 C51 121.0(4) . . ? C54 C53 C52 119.0(4) . . ? C55 C54 C53 121.0(4) . . ? C54 C55 C56 120.1(4) . . ? C51 C56 C55 119.7(4) . . ? C66 C61 C62 117.8(3) . . ? C66 C61 P3 121.5(3) . . ? C62 C61 P3 120.2(3) . . ? C63 C62 C61 121.2(3) . . ? C64 C63 C62 120.1(4) . . ? C63 C64 C65 119.9(4) . . ? C64 C65 C66 120.2(4) . . ? C61 C66 C65 120.8(4) . . ? C76 C71 C72 118.2(3) . . ? C76 C71 P3 127.1(3) . . ? C72 C71 P3 114.7(2) . . ? C73 C72 C71 120.4(3) . . ? C72 C73 C74 120.6(4) . . ? C75 C74 C73 119.3(3) . . ? C74 C75 C76 120.0(3) . . ? C71 C76 C75 121.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.572 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.093 #END=== #Compound #12 data_yy01 _database_code_CSD 215183 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Cu I2 P3 Ru, C H2 Cl2, C H2 Cl2' _chemical_formula_sum 'C50 H46 Cl4 Cu I2 P3 Ru' _chemical_formula_weight 1299.99 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 20.2849(8) _cell_length_b 11.3392(5) _cell_length_c 20.9410(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.758(2) _cell_angle_gamma 90.00 _cell_volume 4814.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 349 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 2.395 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6136 _exptl_absorpt_correction_T_max 0.7944 _exptl_absorpt_process_details 'based on measured indexed crystal faces, SHELXTL (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 42538 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11042 _reflns_number_gt 9283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker 1998)' _computing_cell_refinement 'Bruker SMART & SAINT (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0514P)^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 SHELXL _refine_ls_extinction_coef 0.00133(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11042 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _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 Ru Ru 0.092601(8) 0.234740(15) 0.548005(8) 0.01981(6) Uani 1 1 d . . . Cu Cu 0.209324(18) 0.00073(3) 0.454807(17) 0.03687(9) Uani 1 1 d . . . I1 I 0.141625(7) 0.010295(12) 0.559488(7) 0.02480(5) Uani 1 1 d . . . I2 I 0.1766(3) -0.1367(6) 0.3661(2) 0.0724(8) Uani 0.527(18) 1 d P . . I2' I 0.16663(18) -0.1110(5) 0.36257(18) 0.0589(6) Uani 0.473(18) 1 d P . . P1 P 0.29318(3) 0.11957(6) 0.47777(3) 0.02994(14) Uani 1 1 d . A . P2 P 0.18920(3) 0.31361(5) 0.50966(3) 0.02349(13) Uani 1 1 d . . . P3 P 0.11091(3) 0.27156(5) 0.65634(3) 0.02216(12) Uani 1 1 d . . . C1 C -0.01344(12) 0.2685(2) 0.56280(13) 0.0323(6) Uani 1 1 d . . . H1A H -0.0351 0.2717 0.6050 0.039 Uiso 1 1 calc R . . C2 C -0.00917(12) 0.1692(2) 0.52385(13) 0.0333(6) Uani 1 1 d . . . H2A H -0.0265 0.0890 0.5339 0.040 Uiso 1 1 calc R . . C3 C 0.02209(12) 0.2022(2) 0.46631(12) 0.0319(5) Uani 1 1 d . . . H3A H 0.0297 0.1499 0.4288 0.038 Uiso 1 1 calc R . . C4 C 0.03709(12) 0.3236(2) 0.47070(12) 0.0315(5) Uani 1 1 d . . . H4A H 0.0564 0.3728 0.4363 0.038 Uiso 1 1 calc R . . C5 C 0.01626(12) 0.3657(2) 0.53125(12) 0.0293(5) Uani 1 1 d . . . H5A H 0.0173 0.4494 0.5463 0.035 Uiso 1 1 calc R . . C6 C 0.27120(12) 0.2477(2) 0.52703(12) 0.0278(5) Uani 1 1 d . . . H6A H 0.3050 0.3095 0.5216 0.033 Uiso 1 1 calc R . . H6B H 0.2733 0.2233 0.5724 0.033 Uiso 1 1 calc R . . C11 C 0.35584(14) 0.0480(3) 0.52915(16) 0.0435(7) Uani 1 1 d . . . C12 C 0.3961(3) 0.1063(5) 0.5770(3) 0.0483(16) Uani 0.520(4) 1 d P A 2 H12A H 0.3932 0.1895 0.5814 0.058 Uiso 0.520(4) 1 calc PR A 2 C13 C 0.4394(3) 0.0434(7) 0.6168(3) 0.0583(19) Uani 0.520(4) 1 d P A 2 H13A H 0.4690 0.0849 0.6448 0.070 Uiso 0.520(4) 1 calc PR A 2 C14 C 0.4401(7) -0.0762(12) 0.6166(5) 0.056(3) Uani 0.520(4) 1 d P A 2 H14A H 0.4712 -0.1184 0.6426 0.067 Uiso 0.520(4) 1 calc PR A 2 C15 C 0.3960(5) -0.1341(7) 0.5790(4) 0.073(2) Uani 0.520(4) 1 d P A 2 H15A H 0.3949 -0.2178 0.5805 0.088 Uiso 0.520(4) 1 calc PR A 2 C16 C 0.3521(4) -0.0752(6) 0.5379(3) 0.0542(18) Uani 0.520(4) 1 d P A 2 H16A H 0.3189 -0.1187 0.5153 0.065 Uiso 0.520(4) 1 calc PR A 2 C12' C 0.4237(3) 0.0396(7) 0.5018(3) 0.0532(19) Uani 0.480(4) 1 d P A 1 H12B H 0.4333 0.0726 0.4614 0.064 Uiso 0.480(4) 1 calc PR A 1 C13' C 0.4712(4) -0.0189(9) 0.5388(4) 0.076(3) Uani 0.480(4) 1 d P A 1 H13B H 0.5153 -0.0239 0.5249 0.091 Uiso 0.480(4) 1 calc PR A 1 C14' C 0.4548(8) -0.0687(16) 0.5945(6) 0.067(4) Uani 0.480(4) 1 d P A 1 H14B H 0.4873 -0.1103 0.6192 0.080 Uiso 0.480(4) 1 calc PR A 1 C15' C 0.3922(5) -0.0604(8) 0.6158(4) 0.060(2) Uani 0.480(4) 1 d P A 1 H15B H 0.3817 -0.0933 0.6559 0.072 Uiso 0.480(4) 1 calc PR A 1 C16' C 0.3442(3) -0.0040(5) 0.5791(3) 0.0422(16) Uani 0.480(4) 1 d P A 1 H16B H 0.3001 -0.0053 0.5931 0.051 Uiso 0.480(4) 1 calc PR A 1 C21 C 0.33885(14) 0.1837(3) 0.41288(14) 0.0398(6) Uani 1 1 d . . . C22 C 0.32505(16) 0.1442(3) 0.35127(16) 0.0474(7) Uani 1 1 d . A . H22A H 0.2945 0.0818 0.3441 0.057 Uiso 1 1 calc R . . C23 C 0.35599(18) 0.1958(4) 0.29993(17) 0.0607(9) Uani 1 1 d . . . H23A H 0.3463 0.1689 0.2577 0.073 Uiso 1 1 calc R A . C24 C 0.4003(2) 0.2852(3) 0.3100(2) 0.0689(12) Uani 1 1 d . A . H24A H 0.4210 0.3202 0.2746 0.083 Uiso 1 1 calc R . . C25 C 0.4153(2) 0.3250(4) 0.3705(2) 0.0733(12) Uani 1 1 d . . . H25A H 0.4463 0.3869 0.3770 0.088 Uiso 1 1 calc R A . C26 C 0.38477(18) 0.2739(3) 0.42249(19) 0.0597(9) Uani 1 1 d . A . H26A H 0.3953 0.3006 0.4646 0.072 Uiso 1 1 calc R . . C31 C 0.19155(13) 0.3261(2) 0.42225(13) 0.0357(6) Uani 1 1 d . . . C32 C 0.16259(14) 0.2395(3) 0.38405(13) 0.0439(7) Uani 1 1 d . . . H32A H 0.1393 0.1769 0.4034 0.053 Uiso 1 1 calc R . . C33 C 0.16699(17) 0.2424(4) 0.31764(16) 0.0648(11) Uani 1 1 d . . . H33A H 0.1469 0.1820 0.2923 0.078 Uiso 1 1 calc R . . C34 C 0.1998(2) 0.3311(5) 0.28932(18) 0.0820(15) Uani 1 1 d . . . H34A H 0.2021 0.3337 0.2441 0.098 Uiso 1 1 calc R . . C35 C 0.2301(2) 0.4182(4) 0.3262(2) 0.0756(13) Uani 1 1 d . . . H35A H 0.2534 0.4798 0.3060 0.091 Uiso 1 1 calc R . . C36 C 0.22666(17) 0.4167(3) 0.39244(16) 0.0538(8) Uani 1 1 d . . . H36A H 0.2479 0.4764 0.4174 0.065 Uiso 1 1 calc R . . C41 C 0.20346(12) 0.4657(2) 0.53545(12) 0.0276(5) Uani 1 1 d . . . C42 C 0.16446(13) 0.5562(2) 0.50898(14) 0.0355(6) Uani 1 1 d . . . H42A H 0.1332 0.5388 0.4756 0.043 Uiso 1 1 calc R . . C43 C 0.17098(15) 0.6712(2) 0.53110(16) 0.0439(7) Uani 1 1 d . . . H43A H 0.1455 0.7324 0.5116 0.053 Uiso 1 1 calc R . . C44 C 0.21389(16) 0.6968(3) 0.58081(17) 0.0489(8) Uani 1 1 d . . . H44A H 0.2170 0.7751 0.5968 0.059 Uiso 1 1 calc R . . C45 C 0.25272(15) 0.6085(2) 0.60772(16) 0.0454(7) Uani 1 1 d . . . H45A H 0.2829 0.6264 0.6420 0.055 Uiso 1 1 calc R . . C46 C 0.24783(13) 0.4941(2) 0.58492(14) 0.0343(6) Uani 1 1 d . . . H46A H 0.2751 0.4342 0.6033 0.041 Uiso 1 1 calc R . . C51 C 0.06661(12) 0.4046(2) 0.68117(12) 0.0274(5) Uani 1 1 d . . . C52 C 0.01123(16) 0.4003(3) 0.71847(15) 0.0473(8) Uani 1 1 d . . . H52A H -0.0028 0.3270 0.7352 0.057 Uiso 1 1 calc R . . C53 C -0.02390(19) 0.5029(3) 0.7315(2) 0.0616(10) Uani 1 1 d . . . H53A H -0.0622 0.4989 0.7564 0.074 Uiso 1 1 calc R . . C54 C -0.00305(16) 0.6096(3) 0.70837(17) 0.0506(8) Uani 1 1 d . . . H54A H -0.0268 0.6794 0.7178 0.061 Uiso 1 1 calc R . . C55 C 0.05211(14) 0.6159(2) 0.67159(14) 0.0379(6) Uani 1 1 d . . . H55A H 0.0667 0.6898 0.6559 0.045 Uiso 1 1 calc R . . C56 C 0.08613(13) 0.5135(2) 0.65768(13) 0.0318(6) Uani 1 1 d . . . H56A H 0.1235 0.5178 0.6316 0.038 Uiso 1 1 calc R . . C61 C 0.07848(12) 0.1568(2) 0.70965(12) 0.0272(5) Uani 1 1 d . . . C62 C 0.03297(13) 0.0744(2) 0.68707(13) 0.0329(5) Uani 1 1 d . . . H62A H 0.0177 0.0773 0.6437 0.039 Uiso 1 1 calc R . . C63 C 0.00936(16) -0.0127(3) 0.72751(16) 0.0452(7) Uani 1 1 d . . . H63A H -0.0216 -0.0691 0.7114 0.054 Uiso 1 1 calc R . . C64 C 0.03043(16) -0.0175(3) 0.79003(16) 0.0477(8) Uani 1 1 d . . . H64A H 0.0144 -0.0774 0.8172 0.057 Uiso 1 1 calc R . . C65 C 0.07484(15) 0.0644(3) 0.81361(14) 0.0456(7) Uani 1 1 d . . . H65A H 0.0891 0.0616 0.8572 0.055 Uiso 1 1 calc R . . C66 C 0.09882(14) 0.1513(2) 0.77364(13) 0.0370(6) Uani 1 1 d . . . H66A H 0.1295 0.2076 0.7902 0.044 Uiso 1 1 calc R . . C71 C 0.19320(12) 0.2918(2) 0.69418(11) 0.0263(5) Uani 1 1 d . . . C72 C 0.23991(12) 0.2042(2) 0.68538(12) 0.0276(5) Uani 1 1 d . . . H72A H 0.2286 0.1375 0.6599 0.033 Uiso 1 1 calc R . . C73 C 0.30276(13) 0.2121(2) 0.71300(13) 0.0360(6) Uani 1 1 d . . . H73A H 0.3340 0.1511 0.7065 0.043 Uiso 1 1 calc R . . C74 C 0.31984(15) 0.3086(3) 0.74991(15) 0.0446(7) Uani 1 1 d . . . H74A H 0.3629 0.3145 0.7689 0.054 Uiso 1 1 calc R . . C75 C 0.27455(17) 0.3959(3) 0.75908(17) 0.0547(9) Uani 1 1 d . . . H75A H 0.2866 0.4629 0.7840 0.066 Uiso 1 1 calc R . . C76 C 0.21142(15) 0.3878(2) 0.73262(15) 0.0430(7) Uani 1 1 d . . . H76A H 0.1802 0.4481 0.7406 0.052 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 Ru 0.01902(10) 0.01872(9) 0.02153(10) -0.00037(6) -0.00186(7) 0.00062(6) Cu 0.03552(19) 0.0410(2) 0.03421(19) -0.00360(14) 0.00258(14) -0.00340(14) I1 0.02790(9) 0.01833(8) 0.02828(9) -0.00146(5) 0.00275(6) 0.00060(5) I2 0.0833(14) 0.0892(16) 0.0465(9) -0.0347(8) 0.0288(8) -0.0353(11) I2' 0.0470(9) 0.0940(16) 0.0360(5) -0.0223(8) 0.0054(6) -0.0240(7) P1 0.0256(3) 0.0302(3) 0.0343(3) 0.0039(3) 0.0058(3) 0.0031(3) P2 0.0224(3) 0.0223(3) 0.0258(3) 0.0045(2) 0.0008(2) 0.0014(2) P3 0.0231(3) 0.0203(3) 0.0230(3) -0.0011(2) -0.0007(2) 0.0016(2) C1 0.0180(11) 0.0425(15) 0.0360(14) 0.0003(11) -0.0039(10) 0.0039(10) C2 0.0219(12) 0.0377(14) 0.0400(15) 0.0014(11) -0.0067(10) -0.0039(10) C3 0.0291(13) 0.0367(14) 0.0292(13) -0.0033(11) -0.0104(10) 0.0013(10) C4 0.0298(13) 0.0348(14) 0.0292(13) 0.0041(10) -0.0096(10) 0.0047(10) C5 0.0238(12) 0.0289(12) 0.0347(13) -0.0007(10) -0.0068(10) 0.0084(9) C6 0.0231(12) 0.0283(12) 0.0322(13) 0.0055(10) 0.0032(10) 0.0028(9) C11 0.0346(15) 0.0331(14) 0.062(2) 0.0005(14) -0.0051(14) 0.0097(12) C12 0.043(3) 0.047(3) 0.054(4) -0.003(3) -0.007(3) 0.011(3) C13 0.047(4) 0.077(5) 0.050(4) 0.001(4) -0.011(3) 0.017(3) C14 0.065(8) 0.068(5) 0.035(6) 0.015(5) -0.004(5) 0.030(5) C15 0.108(7) 0.045(4) 0.067(5) 0.022(4) -0.010(5) 0.021(4) C16 0.065(4) 0.040(3) 0.056(4) 0.006(3) -0.009(3) 0.000(3) C12' 0.030(3) 0.075(5) 0.056(4) 0.017(4) 0.013(3) 0.019(3) C13' 0.032(4) 0.120(8) 0.075(6) 0.003(5) 0.002(4) 0.038(4) C14' 0.059(7) 0.100(9) 0.042(8) 0.009(7) 0.006(5) 0.043(6) C15' 0.064(5) 0.072(6) 0.043(4) 0.020(4) 0.004(4) 0.032(4) C16' 0.037(3) 0.047(4) 0.043(4) 0.011(3) 0.009(3) 0.016(3) C21 0.0356(15) 0.0420(15) 0.0429(16) 0.0033(12) 0.0189(12) 0.0060(12) C22 0.0419(17) 0.0514(18) 0.0498(18) 0.0071(14) 0.0155(14) 0.0094(14) C23 0.058(2) 0.078(2) 0.0482(19) 0.0122(18) 0.0245(16) 0.0114(19) C24 0.066(2) 0.067(2) 0.076(3) 0.025(2) 0.047(2) 0.0128(19) C25 0.071(3) 0.066(2) 0.085(3) 0.002(2) 0.050(2) -0.017(2) C26 0.058(2) 0.061(2) 0.062(2) -0.0064(17) 0.0317(18) -0.0138(17) C31 0.0303(13) 0.0471(16) 0.0298(13) 0.0114(12) 0.0048(11) 0.0108(11) C32 0.0345(15) 0.068(2) 0.0296(14) 0.0012(13) 0.0019(12) 0.0129(14) C33 0.0429(19) 0.120(3) 0.0310(16) -0.0075(19) -0.0012(14) 0.018(2) C34 0.070(3) 0.145(4) 0.0325(19) 0.028(2) 0.0127(18) 0.034(3) C35 0.073(3) 0.097(3) 0.058(2) 0.045(2) 0.025(2) 0.019(2) C36 0.0539(19) 0.057(2) 0.0509(19) 0.0229(16) 0.0133(15) 0.0072(15) C41 0.0249(12) 0.0221(11) 0.0356(13) 0.0058(10) -0.0005(10) -0.0020(9) C42 0.0326(14) 0.0267(13) 0.0468(16) 0.0048(11) -0.0066(12) -0.0012(10) C43 0.0458(17) 0.0220(13) 0.063(2) 0.0085(13) -0.0068(14) 0.0027(11) C44 0.0470(18) 0.0230(13) 0.076(2) -0.0015(14) -0.0117(16) -0.0047(12) C45 0.0418(16) 0.0328(15) 0.061(2) -0.0018(13) -0.0148(14) -0.0053(12) C46 0.0274(13) 0.0267(13) 0.0483(17) 0.0028(11) -0.0046(12) 0.0001(10) C51 0.0279(12) 0.0255(12) 0.0286(12) -0.0040(9) -0.0049(10) 0.0056(9) C52 0.0523(18) 0.0363(15) 0.0546(19) 0.0012(13) 0.0218(15) 0.0079(13) C53 0.058(2) 0.050(2) 0.078(3) -0.0004(17) 0.032(2) 0.0190(16) C54 0.0542(19) 0.0360(16) 0.062(2) -0.0096(14) 0.0019(16) 0.0195(14) C55 0.0432(16) 0.0249(13) 0.0447(16) -0.0067(11) -0.0118(13) 0.0075(11) C56 0.0317(14) 0.0280(13) 0.0355(14) -0.0037(10) -0.0031(11) 0.0051(10) C61 0.0266(12) 0.0253(12) 0.0300(13) 0.0016(9) 0.0058(10) 0.0045(9) C62 0.0317(13) 0.0331(13) 0.0340(14) 0.0004(11) 0.0067(11) -0.0019(10) C63 0.0442(17) 0.0371(15) 0.055(2) 0.0024(13) 0.0186(15) -0.0048(12) C64 0.0477(18) 0.0457(17) 0.0509(19) 0.0195(14) 0.0213(15) 0.0055(14) C65 0.0462(17) 0.0552(19) 0.0359(15) 0.0151(14) 0.0073(13) 0.0063(14) C66 0.0409(15) 0.0391(15) 0.0310(14) 0.0053(11) 0.0031(11) 0.0037(12) C71 0.0293(12) 0.0234(11) 0.0257(12) 0.0017(9) -0.0050(10) -0.0017(9) C72 0.0290(12) 0.0248(11) 0.0289(12) 0.0026(9) 0.0002(10) -0.0011(9) C73 0.0312(14) 0.0362(14) 0.0401(15) 0.0062(12) -0.0055(11) 0.0022(11) C74 0.0360(15) 0.0434(16) 0.0531(18) 0.0074(14) -0.0195(13) -0.0056(13) C75 0.061(2) 0.0370(16) 0.064(2) -0.0121(15) -0.0349(17) -0.0020(14) C76 0.0441(16) 0.0351(15) 0.0484(17) -0.0119(12) -0.0195(13) 0.0083(12) _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 Ru C5 2.166(2) . ? Ru C4 2.189(2) . ? Ru C1 2.216(2) . ? Ru C3 2.227(2) . ? Ru C2 2.237(2) . ? Ru P2 2.3197(6) . ? Ru P3 2.3254(6) . ? Ru I1 2.7403(2) . ? Cu P1 2.2113(8) . ? Cu I2' 2.446(4) . ? Cu I2 2.499(3) . ? Cu I1 2.6244(4) . ? P1 C21 1.820(3) . ? P1 C11 1.830(3) . ? P1 C6 1.844(2) . ? P2 C41 1.828(2) . ? P2 C31 1.838(3) . ? P2 C6 1.850(2) . ? P3 C51 1.840(2) . ? P3 C71 1.840(2) . ? P3 C61 1.848(2) . ? C1 C2 1.394(4) . ? C1 C5 1.428(4) . ? C1 H1A 1.0000 . ? C2 C3 1.428(4) . ? C2 H2A 1.0000 . ? C3 C4 1.412(4) . ? C3 H3A 1.0000 . ? C4 C5 1.431(4) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C11 C16' 1.231(7) . ? C11 C16 1.411(7) . ? C11 C12 1.434(7) . ? C11 C12' 1.511(7) . ? C12 C13 1.390(8) . ? C12 H12A 0.9500 . ? C13 C14 1.357(16) . ? C13 H13A 0.9500 . ? C14 C15 1.344(18) . ? C14 H14A 0.9500 . ? C15 C16 1.389(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C12' C13' 1.387(10) . ? C12' H12B 0.9500 . ? C13' C14' 1.346(14) . ? C13' H13B 0.9500 . ? C14' C15' 1.361(16) . ? C14' H14B 0.9500 . ? C15' C16' 1.380(10) . ? C15' H15B 0.9500 . ? C16' H16B 0.9500 . ? C21 C22 1.386(5) . ? C21 C26 1.394(5) . ? C22 C23 1.391(4) . ? C22 H22A 0.9500 . ? C23 C24 1.367(6) . ? C23 H23A 0.9500 . ? C24 C25 1.371(6) . ? C24 H24A 0.9500 . ? C25 C26 1.395(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.387(4) . ? C31 C36 1.407(4) . ? C32 C33 1.397(4) . ? C32 H32A 0.9500 . ? C33 C34 1.353(6) . ? C33 H33A 0.9500 . ? C34 C35 1.385(7) . ? C34 H34A 0.9500 . ? C35 C36 1.391(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.389(4) . ? C41 C42 1.400(3) . ? C42 C43 1.388(4) . ? C42 H42A 0.9500 . ? C43 C44 1.368(4) . ? C43 H43A 0.9500 . ? C44 C45 1.384(4) . ? C44 H44A 0.9500 . ? C45 C46 1.385(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C52 1.389(4) . ? C51 C56 1.391(3) . ? C52 C53 1.395(4) . ? C52 H52A 0.9500 . ? C53 C54 1.375(5) . ? C53 H53A 0.9500 . ? C54 C55 1.379(4) . ? C54 H54A 0.9500 . ? C55 C56 1.386(3) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.386(3) . ? C61 C66 1.391(4) . ? C62 C63 1.396(4) . ? C62 H62A 0.9500 . ? C63 C64 1.366(5) . ? C63 H63A 0.9500 . ? C64 C65 1.375(5) . ? C64 H64A 0.9500 . ? C65 C66 1.390(4) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.389(3) . ? C71 C76 1.397(3) . ? C72 C73 1.387(4) . ? C72 H72A 0.9500 . ? C73 C74 1.378(4) . ? C73 H73A 0.9500 . ? C74 C75 1.368(4) . ? C74 H74A 0.9500 . ? C75 C76 1.383(4) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? 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 C5 Ru C4 38.35(10) . . ? C5 Ru C1 38.02(10) . . ? C4 Ru C1 62.90(10) . . ? C5 Ru C3 63.25(10) . . ? C4 Ru C3 37.29(10) . . ? C1 Ru C3 62.13(10) . . ? C5 Ru C2 62.67(10) . . ? C4 Ru C2 62.32(10) . . ? C1 Ru C2 36.48(10) . . ? C3 Ru C2 37.32(10) . . ? C5 Ru P2 106.67(7) . . ? C4 Ru P2 89.27(7) . . ? C1 Ru P2 144.67(7) . . ? C3 Ru P2 109.11(7) . . ? C2 Ru P2 146.42(7) . . ? C5 Ru P3 97.29(7) . . ? C4 Ru P3 134.58(7) . . ? C1 Ru P3 87.66(7) . . ? C3 Ru P3 149.19(7) . . ? C2 Ru P3 113.51(7) . . ? P2 Ru P3 99.05(2) . . ? C5 Ru I1 155.03(7) . . ? C4 Ru I1 132.03(7) . . ? C1 Ru I1 119.95(7) . . ? C3 Ru I1 97.84(7) . . ? C2 Ru I1 92.37(7) . . ? P2 Ru I1 94.607(16) . . ? P3 Ru I1 91.974(15) . . ? P1 Cu I2' 137.62(10) . . ? P1 Cu I2 136.63(10) . . ? I2' Cu I2 8.28(19) . . ? P1 Cu I1 102.23(2) . . ? I2' Cu I1 119.95(9) . . ? I2 Cu I1 120.83(9) . . ? Cu I1 Ru 99.374(10) . . ? C21 P1 C11 104.83(14) . . ? C21 P1 C6 103.91(12) . . ? C11 P1 C6 101.30(13) . . ? C21 P1 Cu 119.14(11) . . ? C11 P1 Cu 111.93(10) . . ? C6 P1 Cu 113.84(8) . . ? C41 P2 C31 102.28(12) . . ? C41 P2 C6 100.97(11) . . ? C31 P2 C6 100.16(11) . . ? C41 P2 Ru 112.90(8) . . ? C31 P2 Ru 114.99(9) . . ? C6 P2 Ru 122.69(8) . . ? C51 P3 C71 102.75(11) . . ? C51 P3 C61 102.75(11) . . ? C71 P3 C61 99.36(11) . . ? C51 P3 Ru 110.99(8) . . ? C71 P3 Ru 123.92(8) . . ? C61 P3 Ru 114.44(8) . . ? C2 C1 C5 108.5(2) . . ? C2 C1 Ru 72.59(14) . . ? C5 C1 Ru 69.11(13) . . ? C2 C1 H1A 125.7 . . ? C5 C1 H1A 125.7 . . ? Ru C1 H1A 125.7 . . ? C1 C2 C3 108.6(2) . . ? C1 C2 Ru 70.93(14) . . ? C3 C2 Ru 70.94(14) . . ? C1 C2 H2A 125.7 . . ? C3 C2 H2A 125.7 . . ? Ru C2 H2A 125.7 . . ? C4 C3 C2 107.5(2) . . ? C4 C3 Ru 69.91(13) . . ? C2 C3 Ru 71.73(14) . . ? C4 C3 H3A 126.2 . . ? C2 C3 H3A 126.2 . . ? Ru C3 H3A 126.2 . . ? C3 C4 C5 108.3(2) . . ? C3 C4 Ru 72.80(14) . . ? C5 C4 Ru 69.96(13) . . ? C3 C4 H4A 125.8 . . ? C5 C4 H4A 125.8 . . ? Ru C4 H4A 125.8 . . ? C1 C5 C4 107.0(2) . . ? C1 C5 Ru 72.87(14) . . ? C4 C5 Ru 71.70(13) . . ? C1 C5 H5A 126.3 . . ? C4 C5 H5A 126.3 . . ? Ru C5 H5A 126.3 . . ? P1 C6 P2 116.09(14) . . ? P1 C6 H6A 108.3 . . ? P2 C6 H6A 108.3 . . ? P1 C6 H6B 108.3 . . ? P2 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C16' C11 C16 53.3(4) . . ? C16' C11 C12 75.4(5) . . ? C16 C11 C12 113.4(4) . . ? C16' C11 C12' 119.6(4) . . ? C16 C11 C12' 92.3(4) . . ? C12 C11 C12' 77.7(4) . . ? C16' C11 P1 124.4(4) . . ? C16 C11 P1 118.5(3) . . ? C12 C11 P1 125.2(3) . . ? C12' C11 P1 115.4(3) . . ? C13 C12 C11 121.2(6) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C14 C13 C12 121.2(8) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C15 C14 C13 118.9(10) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C16 122.0(8) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C15 C16 C11 121.4(6) . . ? C15 C16 H16A 119.3 . . ? C11 C16 H16A 119.3 . . ? C13' C12' C11 116.3(6) . . ? C13' C12' H12B 121.8 . . ? C11 C12' H12B 121.8 . . ? C14' C13' C12' 119.9(9) . . ? C14' C13' H13B 120.1 . . ? C12' C13' H13B 120.1 . . ? C13' C14' C15' 120.9(12) . . ? C13' C14' H14B 119.5 . . ? C15' C14' H14B 119.5 . . ? C14' C15' C16' 119.9(8) . . ? C14' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C11 C16' C15' 123.0(6) . . ? C11 C16' H16B 118.5 . . ? C15' C16' H16B 118.5 . . ? C22 C21 C26 119.1(3) . . ? C22 C21 P1 118.2(2) . . ? C26 C21 P1 122.6(2) . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C21 C26 C25 120.2(4) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C32 C31 C36 118.2(3) . . ? C32 C31 P2 119.8(2) . . ? C36 C31 P2 121.8(3) . . ? C31 C32 C33 121.3(3) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C31 119.5(4) . . ? C35 C36 H36A 120.2 . . ? C31 C36 H36A 120.2 . . ? C46 C41 C42 118.1(2) . . ? C46 C41 P2 122.11(18) . . ? C42 C41 P2 119.50(19) . . ? C43 C42 C41 120.6(3) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C43 C44 C45 119.8(3) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 120.8(2) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C52 C51 C56 118.3(2) . . ? C52 C51 P3 122.7(2) . . ? C56 C51 P3 118.78(19) . . ? C51 C52 C53 120.5(3) . . ? C51 C52 H52A 119.7 . . ? C53 C52 H52A 119.7 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C53 C54 C55 120.4(3) . . ? C53 C54 H54A 119.8 . . ? C55 C54 H54A 119.8 . . ? C54 C55 C56 119.4(3) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C55 C56 C51 121.3(3) . . ? C55 C56 H56A 119.3 . . ? C51 C56 H56A 119.3 . . ? C62 C61 C66 118.2(2) . . ? C62 C61 P3 120.93(19) . . ? C66 C61 P3 120.9(2) . . ? C61 C62 C63 120.5(3) . . ? C61 C62 H62A 119.7 . . ? C63 C62 H62A 119.7 . . ? C64 C63 C62 120.4(3) . . ? C64 C63 H63A 119.8 . . ? C62 C63 H63A 119.8 . . ? C63 C64 C65 120.0(3) . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C64 C65 C66 120.0(3) . . ? C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C65 C66 C61 120.9(3) . . ? C65 C66 H66A 119.6 . . ? C61 C66 H66A 119.6 . . ? C72 C71 C76 117.7(2) . . ? C72 C71 P3 117.87(18) . . ? C76 C71 P3 124.45(19) . . ? C73 C72 C71 121.4(2) . . ? C73 C72 H72A 119.3 . . ? C71 C72 H72A 119.3 . . ? C74 C73 C72 119.8(3) . . ? C74 C73 H73A 120.1 . . ? C72 C73 H73A 120.1 . . ? C75 C74 C73 119.7(3) . . ? C75 C74 H74A 120.2 . . ? C73 C74 H74A 120.2 . . ? C74 C75 C76 120.9(3) . . ? C74 C75 H75A 119.5 . . ? C76 C75 H75A 119.5 . . ? C75 C76 C71 120.5(3) . . ? C75 C76 H76A 119.7 . . ? C71 C76 H76A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.756 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.142 #END===