Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_tmt61 _database_code_CSD 190234 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Day, Michael W.' #<--'Last name, first name' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Hejl, Andrew D.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Grubbs, Robert H.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Tina M. Trnka' ; ? ; _publ_contact_author_name 'Prof Robert Grubbs' _publ_contact_author_address ; Chemistry & Chemical Engineering California Institute of Technology 1400 E. California Blvd. Pasadena CA 91125 UNITED STATES OF AMERICA ; _publ_contact_author_email RHG@CALTECH.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Terminal ruthenium carbido complexes as [sigma]-donor ligands ; _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition in the Cambridge Structural Database. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H72 Cl2 P2 Ru' _chemical_formula_weight 822.92 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' _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 9.9665(7) _cell_length_b 19.7371(15) _cell_length_c 21.5048(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.1280(10) _cell_angle_gamma 90.00 _cell_volume 4227.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 19682 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.29 _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7490 _exptl_absorpt_correction_T_max 0.9368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 5 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62446 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.49 _reflns_number_total 10049 _reflns_number_gt 7579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054' _computing_cell_refinement 'Bruker SAINT v6.022' _computing_data_reduction 'Bruker SAINT v6.022' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10049 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 3.120 _refine_ls_restrained_S_all 3.120 _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 Ru Ru 0.61036(5) 0.83188(2) 0.08018(2) 0.01121(12) Uani 1 1 d . . . Cl1 Cl 0.82334(14) 0.81181(7) 0.03686(7) 0.0182(3) Uani 1 1 d . . . Cl2 Cl 0.40059(14) 0.80333(8) 0.12139(7) 0.0188(3) Uani 1 1 d . . . P1 P 0.70536(15) 0.80637(7) 0.18315(7) 0.0130(3) Uani 1 1 d . . . P2 P 0.51062(15) 0.81614(7) -0.02346(7) 0.0115(3) Uani 1 1 d . . . C1 C 0.6084(6) 0.9145(3) 0.0835(3) 0.0181(12) Uani 1 1 d . . . C2 C 0.6098(6) 0.8389(3) 0.2492(3) 0.0157(13) Uani 1 1 d . . . H2 H 0.5228 0.8137 0.2472 0.019 Uiso 1 1 calc R . . C3 C 0.6752(7) 0.8208(3) 0.3123(3) 0.0244(15) Uani 1 1 d . . . H3A H 0.7611 0.8457 0.3178 0.029 Uiso 1 1 calc R . . H3B H 0.6954 0.7717 0.3134 0.029 Uiso 1 1 calc R . . C4 C 0.5852(7) 0.8383(3) 0.3656(3) 0.0271(15) Uani 1 1 d . . . H4A H 0.5036 0.8097 0.3629 0.033 Uiso 1 1 calc R . . H4B H 0.6332 0.8285 0.4057 0.033 Uiso 1 1 calc R . . C5 C 0.5453(6) 0.9118(3) 0.3635(3) 0.0222(15) Uani 1 1 d . . . H5A H 0.6258 0.9403 0.3716 0.027 Uiso 1 1 calc R . . H5B H 0.4814 0.9210 0.3967 0.027 Uiso 1 1 calc R . . C6 C 0.4807(7) 0.9308(3) 0.3009(3) 0.0269(16) Uani 1 1 d . . . H6A H 0.4612 0.9800 0.3004 0.032 Uiso 1 1 calc R . . H6B H 0.3945 0.9064 0.2951 0.032 Uiso 1 1 calc R . . C7 C 0.5714(6) 0.9136(3) 0.2464(3) 0.0210(14) Uani 1 1 d . . . H7A H 0.6534 0.9419 0.2491 0.025 Uiso 1 1 calc R . . H7B H 0.5231 0.9235 0.2064 0.025 Uiso 1 1 calc R . . C8 C 0.7108(6) 0.7134(3) 0.1979(3) 0.0159(13) Uani 1 1 d . . . H8 H 0.7715 0.7062 0.2354 0.019 Uiso 1 1 calc R . . C9 C 0.5766(6) 0.6810(3) 0.2119(3) 0.0217(15) Uani 1 1 d . . . H9A H 0.5383 0.7038 0.2482 0.026 Uiso 1 1 calc R . . H9B H 0.5132 0.6871 0.1758 0.026 Uiso 1 1 calc R . . C10 C 0.5927(7) 0.6057(3) 0.2256(3) 0.0270(16) Uani 1 1 d . . . H10A H 0.5036 0.5859 0.2332 0.032 Uiso 1 1 calc R . . H10B H 0.6498 0.5998 0.2639 0.032 Uiso 1 1 calc R . . C11 C 0.6558(7) 0.5681(3) 0.1723(3) 0.0308(17) Uani 1 1 d . . . H11A H 0.5947 0.5697 0.1349 0.037 Uiso 1 1 calc R . . H11B H 0.6702 0.5201 0.1838 0.037 Uiso 1 1 calc R . . C12 C 0.7885(8) 0.6006(3) 0.1579(4) 0.041(2) Uani 1 1 d . . . H12A H 0.8522 0.5944 0.1939 0.050 Uiso 1 1 calc R . . H12B H 0.8264 0.5775 0.1216 0.050 Uiso 1 1 calc R . . C13 C 0.7742(7) 0.6762(3) 0.1438(3) 0.0307(17) Uani 1 1 d . . . H13A H 0.8637 0.6957 0.1365 0.037 Uiso 1 1 calc R . . H13B H 0.7174 0.6825 0.1055 0.037 Uiso 1 1 calc R . . C14 C 0.8822(5) 0.8333(3) 0.1901(3) 0.0196(13) Uani 1 1 d . . . H14 H 0.9209 0.8192 0.1498 0.023 Uiso 1 1 calc R . . C15 C 0.9761(6) 0.8034(3) 0.2393(3) 0.0218(14) Uani 1 1 d . . . H15A H 0.9703 0.7533 0.2377 0.026 Uiso 1 1 calc R . . H15B H 0.9484 0.8182 0.2809 0.026 Uiso 1 1 calc R . . C16 C 1.1215(6) 0.8252(3) 0.2300(3) 0.0188(14) Uani 1 1 d . . . H16A H 1.1795 0.8072 0.2644 0.023 Uiso 1 1 calc R . . H16B H 1.1525 0.8057 0.1906 0.023 Uiso 1 1 calc R . . C17 C 1.1357(6) 0.9026(3) 0.2278(3) 0.0238(15) Uani 1 1 d . . . H17A H 1.1198 0.9216 0.2695 0.029 Uiso 1 1 calc R . . H17B H 1.2284 0.9145 0.2168 0.029 Uiso 1 1 calc R . . C18 C 1.0380(6) 0.9338(3) 0.1810(3) 0.0244(15) Uani 1 1 d . . . H18A H 1.0437 0.9838 0.1842 0.029 Uiso 1 1 calc R . . H18B H 1.0637 0.9208 0.1386 0.029 Uiso 1 1 calc R . . C19 C 0.8943(6) 0.9119(3) 0.1904(3) 0.0185(14) Uani 1 1 d . . . H19A H 0.8352 0.9310 0.1569 0.022 Uiso 1 1 calc R . . H19B H 0.8643 0.9297 0.2306 0.022 Uiso 1 1 calc R . . C20 C 0.3312(5) 0.8404(3) -0.0285(3) 0.0144(13) Uani 1 1 d . . . H20 H 0.2844 0.8084 -0.0005 0.017 Uiso 1 1 calc R . . C21 C 0.3042(6) 0.9124(3) -0.0027(3) 0.0165(13) Uani 1 1 d . . . H21A H 0.3481 0.9174 0.0392 0.020 Uiso 1 1 calc R . . H21B H 0.3420 0.9470 -0.0304 0.020 Uiso 1 1 calc R . . C22 C 0.1519(6) 0.9228(3) 0.0013(3) 0.0209(14) Uani 1 1 d . . . H22A H 0.1165 0.8906 0.0319 0.025 Uiso 1 1 calc R . . H22B H 0.1344 0.9692 0.0163 0.025 Uiso 1 1 calc R . . C23 C 0.0784(6) 0.9123(3) -0.0610(3) 0.0248(15) Uani 1 1 d . . . H23A H -0.0194 0.9165 -0.0557 0.030 Uiso 1 1 calc R . . H23B H 0.1057 0.9479 -0.0904 0.030 Uiso 1 1 calc R . . C24 C 0.1083(6) 0.8437(3) -0.0878(3) 0.0205(14) Uani 1 1 d . . . H24A H 0.0643 0.8397 -0.1297 0.025 Uiso 1 1 calc R . . H24B H 0.0712 0.8080 -0.0611 0.025 Uiso 1 1 calc R . . C25 C 0.2599(6) 0.8332(3) -0.0926(3) 0.0193(13) Uani 1 1 d . . . H25A H 0.2772 0.7875 -0.1095 0.023 Uiso 1 1 calc R . . H25B H 0.2962 0.8670 -0.1215 0.023 Uiso 1 1 calc R . . C26 C 0.5087(6) 0.7253(3) -0.0472(3) 0.0121(12) Uani 1 1 d . . . H26 H 0.4662 0.7235 -0.0900 0.015 Uiso 1 1 calc R . . C27 C 0.4239(6) 0.6797(3) -0.0061(3) 0.0182(14) Uani 1 1 d . . . H27A H 0.3318 0.6982 -0.0044 0.022 Uiso 1 1 calc R . . H27B H 0.4636 0.6788 0.0367 0.022 Uiso 1 1 calc R . . C28 C 0.4185(6) 0.6071(3) -0.0328(3) 0.0229(15) Uani 1 1 d . . . H28A H 0.3679 0.5778 -0.0047 0.028 Uiso 1 1 calc R . . H28B H 0.3698 0.6078 -0.0738 0.028 Uiso 1 1 calc R . . C29 C 0.5582(6) 0.5773(3) -0.0405(3) 0.0207(14) Uani 1 1 d . . . H29A H 0.6028 0.5706 0.0009 0.025 Uiso 1 1 calc R . . H29B H 0.5502 0.5325 -0.0611 0.025 Uiso 1 1 calc R . . C30 C 0.6426(6) 0.6241(3) -0.0792(3) 0.0224(15) Uani 1 1 d . . . H30A H 0.6033 0.6263 -0.1221 0.027 Uiso 1 1 calc R . . H30B H 0.7344 0.6053 -0.0813 0.027 Uiso 1 1 calc R . . C31 C 0.6506(6) 0.6957(3) -0.0519(3) 0.0173(14) Uani 1 1 d . . . H31A H 0.7044 0.7250 -0.0788 0.021 Uiso 1 1 calc R . . H31B H 0.6956 0.6943 -0.0101 0.021 Uiso 1 1 calc R . . C32 C 0.6054(6) 0.8570(3) -0.0855(2) 0.0123(12) Uani 1 1 d . . . H32 H 0.7020 0.8481 -0.0742 0.015 Uiso 1 1 calc R . . C33 C 0.5847(6) 0.8298(3) -0.1514(3) 0.0214(14) Uani 1 1 d . . . H33A H 0.4920 0.8400 -0.1668 0.026 Uiso 1 1 calc R . . H33B H 0.5962 0.7800 -0.1511 0.026 Uiso 1 1 calc R . . C34 C 0.6841(7) 0.8614(3) -0.1950(3) 0.0233(15) Uani 1 1 d . . . H34A H 0.7766 0.8487 -0.1812 0.028 Uiso 1 1 calc R . . H34B H 0.6674 0.8435 -0.2376 0.028 Uiso 1 1 calc R . . C35 C 0.6708(6) 0.9380(3) -0.1957(3) 0.0198(14) Uani 1 1 d . . . H35A H 0.7394 0.9577 -0.2225 0.024 Uiso 1 1 calc R . . H35B H 0.5811 0.9508 -0.2133 0.024 Uiso 1 1 calc R . . C36 C 0.6889(6) 0.9663(3) -0.1300(3) 0.0190(14) Uani 1 1 d . . . H36A H 0.6747 1.0160 -0.1311 0.023 Uiso 1 1 calc R . . H36B H 0.7821 0.9578 -0.1144 0.023 Uiso 1 1 calc R . . C37 C 0.5914(6) 0.9345(3) -0.0856(3) 0.0173(13) Uani 1 1 d . . . H37A H 0.4983 0.9471 -0.0985 0.021 Uiso 1 1 calc R . . H37B H 0.6099 0.9521 -0.0430 0.021 Uiso 1 1 calc R . . C41 C 0.1122(7) 0.6928(3) 0.0838(3) 0.0274(15) Uani 1 1 d . . . H41 H 0.0994 0.7405 0.0858 0.033 Uiso 1 1 calc R . . C42 C 0.0430(7) 0.6560(3) 0.0396(3) 0.0279(16) Uani 1 1 d . . . H42 H -0.0185 0.6778 0.0114 0.033 Uiso 1 1 calc R . . C43 C 0.0624(7) 0.5871(4) 0.0360(3) 0.0325(18) Uani 1 1 d . . . H43 H 0.0148 0.5615 0.0049 0.039 Uiso 1 1 calc R . . C44 C 0.1506(7) 0.5549(4) 0.0773(4) 0.0339(18) Uani 1 1 d . . . H44 H 0.1636 0.5073 0.0748 0.041 Uiso 1 1 calc R . . C45 C 0.2212(7) 0.5932(4) 0.1231(3) 0.0345(19) Uani 1 1 d . . . H45 H 0.2823 0.5716 0.1517 0.041 Uiso 1 1 calc R . . C46 C 0.2011(7) 0.6615(4) 0.1260(3) 0.0364(18) Uani 1 1 d . . . H46 H 0.2479 0.6877 0.1569 0.044 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 0.0133(2) 0.0124(2) 0.0079(2) 0.0010(2) -0.00006(16) 0.0002(2) Cl1 0.0148(8) 0.0230(8) 0.0169(8) 0.0027(6) 0.0011(6) 0.0014(6) Cl2 0.0137(8) 0.0294(9) 0.0132(8) 0.0015(6) 0.0013(6) -0.0030(6) P1 0.0134(8) 0.0145(8) 0.0109(8) 0.0016(6) -0.0009(6) -0.0012(6) P2 0.0134(8) 0.0111(8) 0.0101(8) 0.0007(6) 0.0011(6) 0.0008(6) C1 0.021(3) 0.027(3) 0.006(3) 0.001(3) -0.001(2) 0.001(3) C2 0.016(3) 0.023(3) 0.009(3) -0.001(3) 0.004(2) -0.003(3) C3 0.038(4) 0.025(4) 0.010(3) -0.002(3) -0.004(3) 0.014(3) C4 0.042(4) 0.031(4) 0.008(3) 0.005(3) 0.002(3) 0.006(3) C5 0.023(4) 0.032(4) 0.012(3) -0.001(3) 0.001(3) 0.006(3) C6 0.027(4) 0.037(4) 0.017(4) 0.003(3) 0.005(3) 0.011(3) C7 0.027(4) 0.025(4) 0.011(3) 0.003(3) 0.000(3) 0.008(3) C8 0.021(3) 0.017(3) 0.009(3) 0.000(2) -0.002(3) -0.001(3) C9 0.023(3) 0.016(4) 0.027(4) 0.000(3) 0.005(3) -0.005(3) C10 0.032(4) 0.025(4) 0.024(4) 0.005(3) 0.007(3) -0.007(3) C11 0.048(5) 0.018(4) 0.027(4) 0.000(3) 0.003(3) -0.005(3) C12 0.056(5) 0.018(4) 0.051(5) 0.006(3) 0.030(4) 0.005(3) C13 0.040(4) 0.016(4) 0.037(4) 0.000(3) 0.022(3) 0.000(3) C14 0.013(3) 0.027(3) 0.018(3) 0.007(3) -0.002(2) 0.003(3) C15 0.024(4) 0.023(3) 0.018(3) 0.004(3) -0.001(3) -0.001(3) C16 0.013(3) 0.026(4) 0.017(3) 0.002(3) -0.001(2) 0.001(3) C17 0.020(4) 0.030(4) 0.021(4) 0.009(3) 0.000(3) -0.007(3) C18 0.021(4) 0.026(4) 0.026(4) 0.004(3) 0.000(3) -0.005(3) C19 0.015(3) 0.021(3) 0.019(4) 0.003(3) -0.003(3) -0.002(3) C20 0.012(3) 0.020(3) 0.011(3) -0.003(3) 0.001(2) -0.002(3) C21 0.021(3) 0.017(3) 0.012(3) -0.008(2) 0.001(3) 0.003(3) C22 0.020(3) 0.025(4) 0.018(4) -0.010(3) 0.001(3) 0.003(3) C23 0.020(4) 0.028(4) 0.026(4) -0.001(3) -0.003(3) 0.007(3) C24 0.020(3) 0.024(4) 0.017(3) -0.003(3) -0.003(3) 0.001(3) C25 0.021(3) 0.026(3) 0.011(3) -0.004(3) -0.005(2) 0.006(3) C26 0.014(3) 0.013(3) 0.010(3) 0.003(2) 0.003(2) 0.000(2) C27 0.025(3) 0.014(3) 0.016(3) -0.002(2) 0.006(3) 0.000(3) C28 0.020(4) 0.017(3) 0.032(4) 0.005(3) 0.008(3) -0.004(3) C29 0.026(4) 0.014(3) 0.022(4) 0.001(3) 0.003(3) 0.005(3) C30 0.032(4) 0.014(3) 0.022(4) 0.003(3) 0.007(3) 0.007(3) C31 0.017(3) 0.013(3) 0.022(4) 0.005(3) 0.007(3) 0.002(2) C32 0.016(3) 0.014(3) 0.008(3) 0.000(2) 0.000(2) -0.002(2) C33 0.032(4) 0.017(3) 0.016(3) -0.006(3) 0.007(3) -0.010(3) C34 0.037(4) 0.016(3) 0.017(3) -0.003(3) 0.010(3) -0.006(3) C35 0.027(4) 0.021(3) 0.011(3) 0.002(3) 0.004(3) -0.004(3) C36 0.024(3) 0.017(3) 0.016(3) 0.001(3) 0.003(3) -0.005(3) C37 0.026(4) 0.014(3) 0.011(3) 0.000(2) 0.002(3) -0.001(3) C41 0.033(4) 0.029(4) 0.021(4) -0.004(3) 0.011(3) -0.006(3) C42 0.029(4) 0.035(4) 0.021(4) 0.002(3) 0.007(3) 0.000(3) C43 0.045(5) 0.036(4) 0.017(4) -0.007(3) 0.001(3) -0.011(4) C44 0.037(5) 0.025(4) 0.041(5) 0.004(3) 0.018(4) 0.000(3) C45 0.023(4) 0.050(5) 0.031(4) 0.023(4) 0.006(3) 0.000(4) C46 0.035(4) 0.045(5) 0.029(4) 0.004(4) 0.003(3) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 1.632(6) . yes Ru Cl2 2.3689(16) . yes Ru Cl1 2.3827(16) . yes Ru P1 2.4285(17) . yes Ru P2 2.4264(16) . yes P1 C14 1.841(6) . ? P1 C8 1.863(6) . ? P1 C2 1.854(6) . ? P2 C20 1.851(6) . ? P2 C32 1.848(6) . ? P2 C26 1.864(6) . ? C2 C3 1.527(8) . ? C2 C7 1.524(8) . ? C2 H2 1.0000 . ? C3 C4 1.521(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.505(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.543(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.531(8) . ? C8 C9 1.523(8) . ? C8 H8 1.0000 . ? C9 C10 1.521(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.521(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.512(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.529(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.508(8) . ? C14 C19 1.556(8) . ? C14 H14 1.0000 . ? C15 C16 1.532(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.535(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.505(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.517(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.533(7) . ? C20 C21 1.552(7) . ? C20 H20 1.0000 . ? C21 C22 1.537(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.505(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.532(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.535(7) . ? C26 C31 1.537(8) . ? C26 H26 1.0000 . ? C27 C28 1.543(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.527(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.518(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.532(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.523(8) . ? C32 C37 1.536(8) . ? C32 H32 1.0000 . ? C33 C34 1.522(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.519(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.523(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.523(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C41 C42 1.363(9) . ? C41 C46 1.389(10) . ? C41 H41 0.9500 . ? C42 C43 1.377(9) . ? C42 H42 0.9500 . ? C43 C44 1.381(9) . ? C43 H43 0.9500 . ? C44 C45 1.408(10) . ? C44 H44 0.9500 . ? C45 C46 1.367(10) . ? C45 H45 0.9500 . ? C46 H46 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 C1 Ru Cl2 102.1(2) . . yes C1 Ru Cl1 101.3(2) . . yes Cl2 Ru Cl1 156.66(5) . . yes C1 Ru P1 99.9(2) . . yes Cl2 Ru P1 85.94(6) . . yes Cl1 Ru P1 89.95(6) . . yes C1 Ru P2 99.4(2) . . yes Cl2 Ru P2 88.63(5) . . yes Cl1 Ru P2 87.71(6) . . yes P1 Ru P2 160.66(5) . . yes C14 P1 C8 104.4(3) . . ? C14 P1 C2 110.8(3) . . ? C8 P1 C2 102.9(3) . . ? C14 P1 Ru 110.7(2) . . ? C8 P1 Ru 111.53(19) . . ? C2 P1 Ru 115.64(19) . . ? C20 P2 C32 111.3(3) . . ? C20 P2 C26 103.5(3) . . ? C32 P2 C26 102.9(3) . . ? C20 P2 Ru 112.51(18) . . ? C32 P2 Ru 113.84(19) . . ? C26 P2 Ru 111.95(19) . . ? C3 C2 C7 111.0(5) . . ? C3 C2 P1 112.7(4) . . ? C7 C2 P1 116.2(4) . . ? C3 C2 H2 105.3 . . ? C7 C2 H2 105.3 . . ? P1 C2 H2 105.3 . . ? C2 C3 C4 111.9(5) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 111.0(5) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.6(5) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 112.2(5) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C2 109.7(5) . . ? C6 C7 H7A 109.7 . . ? C2 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C2 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 109.8(5) . . ? C13 C8 P1 110.7(4) . . ? C9 C8 P1 115.3(4) . . ? C13 C8 H8 106.9 . . ? C9 C8 H8 106.9 . . ? P1 C8 H8 106.9 . . ? C10 C9 C8 111.2(5) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 112.0(5) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 109.6(6) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C11 112.2(6) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C8 C13 C12 110.8(5) . . ? C8 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C19 109.9(5) . . ? C15 C14 P1 120.8(4) . . ? C19 C14 P1 111.2(4) . . ? C15 C14 H14 104.4 . . ? C19 C14 H14 104.4 . . ? P1 C14 H14 104.4 . . ? C14 C15 C16 111.3(5) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 111.9(5) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 111.7(5) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C19 C18 C17 112.6(5) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C14 111.0(5) . . ? C18 C19 H19A 109.4 . . ? C14 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C14 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C25 C20 C21 109.1(5) . . ? C25 C20 P2 116.3(4) . . ? C21 C20 P2 113.3(4) . . ? C25 C20 H20 105.8 . . ? C21 C20 H20 105.8 . . ? P2 C20 H20 105.8 . . ? C22 C21 C20 109.0(5) . . ? C22 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? C22 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C23 C22 C21 112.2(5) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 111.4(5) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 110.9(5) . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.0 . . ? C20 C25 C24 110.6(5) . . ? C20 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C31 110.1(5) . . ? C27 C26 P2 114.0(4) . . ? C31 C26 P2 112.5(4) . . ? C27 C26 H26 106.6 . . ? C31 C26 H26 106.6 . . ? P2 C26 H26 106.6 . . ? C26 C27 C28 110.0(5) . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C29 C28 C27 112.3(5) . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 110.5(5) . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 112.0(5) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C26 109.9(5) . . ? C30 C31 H31A 109.7 . . ? C26 C31 H31A 109.7 . . ? C30 C31 H31B 109.7 . . ? C26 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C37 109.9(5) . . ? C33 C32 P2 117.6(4) . . ? C37 C32 P2 112.8(4) . . ? C33 C32 H32 105.1 . . ? C37 C32 H32 105.1 . . ? P2 C32 H32 105.1 . . ? C32 C33 C34 111.1(5) . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.8(5) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 110.4(5) . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C37 111.9(5) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C32 110.6(5) . . ? C36 C37 H37A 109.5 . . ? C32 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C42 C41 C46 120.8(6) . . ? C42 C41 H41 119.6 . . ? C46 C41 H41 119.6 . . ? C43 C42 C41 119.9(7) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.4(7) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C45 119.5(6) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 119.4(7) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C41 120.1(7) . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 2.507 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.176 #===END data_adh02 _database_code_CSD 189804 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Day, Michael W.' #<--'Last name, first name' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Hejl, Andrew D.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Grubbs, Robert H.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Tina M. Trnka' ; ? ; _publ_contact_author_name 'Prof Robert Grubbs' _publ_contact_author_address ; Chemistry & Chemical Engineering California Institute of Technology 1400 E. California Blvd. Pasadena CA 91125 UNITED STATES OF AMERICA ; _publ_contact_author_email RHG@CALTECH.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Terminal ruthenium carbido complexes as [sigma]-donor ligands ; _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition in the Cambridge Structural Database. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cl2 Pd S2' _chemical_formula_weight 301.56 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.3567(10) _cell_length_b 5.9396(7) _cell_length_c 10.0652(16) _cell_angle_alpha 90.00 _cell_angle_beta 106.321(2) _cell_angle_gamma 90.00 _cell_volume 479.46(11) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 7117 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 26.05 _exptl_crystal_description Fragment _exptl_crystal_colour Orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 2.851 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5859 _exptl_absorpt_correction_T_max 0.7445 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(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 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 7 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8998 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.19 _reflns_number_total 1125 _reflns_number_gt 1057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054' _computing_cell_refinement 'Bruker SAINT v6.022' _computing_data_reduction 'Bruker SAINT v6.022' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Patterson method' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1125 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0390 _refine_ls_wR_factor_gt 0.0389 _refine_ls_goodness_of_fit_ref 1.938 _refine_ls_restrained_S_all 1.938 _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 Pd Pd 0.5000 0.5000 0.5000 0.00955(8) Uani 1 2 d S . . Cl Cl 0.24239(6) 0.54458(7) 0.53502(5) 0.01459(11) Uani 1 1 d . . . S S 0.40091(5) 0.69693(7) 0.29426(4) 0.01240(11) Uani 1 1 d . . . C1 C 0.4685(3) 0.5546(3) 0.1622(2) 0.0162(4) Uani 1 1 d . . . C2 C 0.5324(3) 0.9413(3) 0.3165(2) 0.0174(4) Uani 1 1 d . . . H1A H 0.414(3) 0.428(4) 0.140(2) 0.021(6) Uiso 1 1 d . . . H1B H 0.442(3) 0.643(4) 0.085(2) 0.018(5) Uiso 1 1 d . . . H1C H 0.577(3) 0.530(3) 0.190(3) 0.022(6) Uiso 1 1 d . . . H2A H 0.512(3) 1.012(3) 0.234(3) 0.022(6) Uiso 1 1 d . . . H2B H 0.508(3) 1.037(4) 0.378(3) 0.028(7) Uiso 1 1 d . . . H2C H 0.642(3) 0.900(4) 0.351(2) 0.020(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01065(11) 0.00906(11) 0.00860(11) 0.00030(6) 0.00216(8) -0.00014(7) Cl 0.0126(2) 0.0179(2) 0.0137(2) 0.00153(16) 0.00442(18) 0.00178(16) S 0.0139(2) 0.0122(2) 0.0107(2) 0.00133(15) 0.00284(17) 0.00031(16) C1 0.0215(11) 0.0143(9) 0.0121(10) -0.0021(7) 0.0037(8) -0.0001(8) C2 0.0249(11) 0.0117(9) 0.0142(10) 0.0003(7) 0.0029(9) -0.0036(8) _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 Cl 2.2924(5) . yes Pd Cl 2.2924(5) 3_666 yes Pd S 2.3191(5) 3_666 yes Pd S 2.3191(5) . yes S C1 1.7948(19) . yes S C2 1.796(2) . yes C1 H1A 0.88(2) . ? C1 H1B 0.91(2) . ? C1 H1C 0.88(3) . ? C2 H2A 0.90(3) . ? C2 H2B 0.90(2) . ? C2 H2C 0.92(2) . ? 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 Cl Pd Cl 180.0 . 3_666 yes Cl Pd S 92.066(16) . 3_666 yes Cl Pd S 87.934(16) 3_666 3_666 yes Cl Pd S 87.934(16) . . yes Cl Pd S 92.066(16) 3_666 . yes S Pd S 180.0 3_666 . yes C1 S C2 99.47(10) . . yes C1 S Pd 108.42(7) . . yes C2 S Pd 104.11(7) . . yes S C1 H1A 110.0(14) . . ? S C1 H1B 107.7(13) . . ? H1A C1 H1B 107(2) . . ? S C1 H1C 110.7(15) . . ? H1A C1 H1C 111(2) . . ? H1B C1 H1C 110.5(19) . . ? S C2 H2A 108.1(14) . . ? S C2 H2B 110.3(15) . . ? H2A C2 H2B 108(2) . . ? S C2 H2C 110.2(14) . . ? H2A C2 H2C 112(2) . . ? H2B C2 H2C 108(2) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.123 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.104 data_adh01 _database_code_CSD 186479 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Day, Michael W.' #<--'Last name, first name' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Hejl, Andrew D.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Grubbs, Robert H.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Tina M. Trnka' ; ? ; _publ_contact_author_name 'Prof Robert Grubbs' _publ_contact_author_address ; Chemistry & Chemical Engineering California Institute of Technology 1400 E. California Blvd. Pasadena CA 91125 UNITED STATES OF AMERICA ; _publ_contact_author_email RHG@CALTECH.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Terminal ruthenium carbido complexes as [sigma]-donor ligands ; _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition in the Cambridge Structural Database. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H84 Cl4 P2 Pd Ru S' _chemical_formula_weight 1140.45 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 9.9306(4) _cell_length_b 12.5669(5) _cell_length_c 22.8075(9) _cell_angle_alpha 87.8420(10) _cell_angle_beta 89.4140(10) _cell_angle_gamma 67.9780(10) _cell_volume 2636.74(18) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 33608 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.44 _exptl_crystal_description Lozenge _exptl_crystal_colour 'Pale tangerine' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7878 _exptl_absorpt_correction_T_max 0.8690 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 7 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54747 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.45 _reflns_number_total 12240 _reflns_number_gt 10533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054' _computing_cell_refinement 'Bruker SAINT v6.022' _computing_data_reduction 'Bruker SAINT v6.022' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Patterson method' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12240 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.596 _refine_ls_restrained_S_all 1.596 _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 0.327933(14) 0.438516(11) 0.379491(6) 0.01222(4) Uani 1 1 d . . . Ru Ru 0.381792(15) 0.321600(12) 0.235349(6) 0.01218(4) Uani 1 1 d . . . Cl1 Cl 0.57407(5) 0.37446(4) 0.203220(19) 0.01591(9) Uani 1 1 d . . . Cl2 Cl 0.20732(5) 0.23678(4) 0.23284(2) 0.01873(10) Uani 1 1 d . . . Cl3 Cl 0.49320(5) 0.52408(4) 0.35899(2) 0.01948(10) Uani 1 1 d . . . Cl4 Cl 0.15896(5) 0.35916(4) 0.40103(2) 0.01952(10) Uani 1 1 d . . . P1 P 0.56247(5) 0.13444(4) 0.26436(2) 0.01409(10) Uani 1 1 d . . . P2 P 0.21459(5) 0.48353(4) 0.17776(2) 0.01413(10) Uani 1 1 d . . . S S 0.34066(5) 0.48672(4) 0.477539(19) 0.01495(10) Uani 1 1 d . . . C1 C 0.34992(18) 0.38020(14) 0.30069(7) 0.0135(4) Uani 1 1 d . . . C2 C 0.4478(2) 0.34469(17) 0.50625(9) 0.0219(4) Uani 1 1 d . . . C3 C 0.1754(2) 0.5110(2) 0.51743(9) 0.0218(4) Uani 1 1 d . . . C4 C 0.4953(3) 0.05502(19) 0.31965(9) 0.0319(5) Uani 1 1 d . . . C5 C 0.4782(4) 0.0999(2) 0.37860(11) 0.0464(8) Uani 1 1 d . . . C6 C 0.4091(3) 0.04856(18) 0.42293(9) 0.0242(5) Uani 1 1 d . . . C7 C 0.4346(4) -0.0740(2) 0.41781(11) 0.0515(8) Uani 1 1 d . . . C8 C 0.4572(3) -0.1202(2) 0.35851(9) 0.0288(5) Uani 1 1 d . . . C9 C 0.5243(4) -0.0670(2) 0.31397(12) 0.0537(9) Uani 1 1 d . . . C10 C 0.7357(2) 0.13918(15) 0.29007(8) 0.0158(4) Uani 1 1 d . . . C11 C 0.8567(2) 0.02241(17) 0.30335(11) 0.0268(5) Uani 1 1 d . . . C12 C 1.0001(2) 0.0381(2) 0.31253(11) 0.0327(5) Uani 1 1 d . . . C13 C 0.9886(2) 0.11959(19) 0.36152(11) 0.0278(5) Uani 1 1 d . . . C14 C 0.8653(2) 0.23354(19) 0.35038(12) 0.0289(5) Uani 1 1 d . . . C15 C 0.7216(2) 0.21959(19) 0.34022(10) 0.0242(5) Uani 1 1 d . . . C16 C 0.6167(2) 0.04143(16) 0.19982(8) 0.0168(4) Uani 1 1 d . . . C17 C 0.4863(2) 0.03911(18) 0.16535(9) 0.0217(4) Uani 1 1 d . . . C18 C 0.5346(3) -0.0458(2) 0.11595(10) 0.0299(5) Uani 1 1 d . . . C19 C 0.6389(3) -0.0179(2) 0.07460(9) 0.0298(5) Uani 1 1 d . . . C20 C 0.7667(3) -0.0117(2) 0.10807(10) 0.0269(5) Uani 1 1 d . . . C21 C 0.7183(2) 0.07270(18) 0.15782(9) 0.0219(4) Uani 1 1 d . . . C22 C 0.0225(2) 0.51340(16) 0.19673(8) 0.0162(4) Uani 1 1 d . . . C23 C -0.0927(2) 0.61135(18) 0.16229(9) 0.0224(4) Uani 1 1 d . . . C24 C -0.2435(2) 0.6085(2) 0.17489(10) 0.0293(5) Uani 1 1 d . . . C25 C -0.2773(2) 0.6154(2) 0.24005(10) 0.0288(5) Uani 1 1 d . . . C26 C -0.1601(2) 0.52074(19) 0.27479(9) 0.0231(4) Uani 1 1 d . . . C27 C -0.0098(2) 0.52258(19) 0.26282(9) 0.0211(4) Uani 1 1 d . . . C28 C 0.2596(2) 0.61320(15) 0.18143(8) 0.0158(4) Uani 1 1 d . . . C29 C 0.2034(3) 0.70326(17) 0.13128(9) 0.0231(4) Uani 1 1 d . . . C30 C 0.2635(3) 0.79805(19) 0.13716(10) 0.0266(5) Uani 1 1 d . . . C31 C 0.2254(2) 0.85397(18) 0.19606(9) 0.0241(5) Uani 1 1 d . . . C32 C 0.2783(2) 0.76466(17) 0.24586(9) 0.0238(4) Uani 1 1 d . . . C33 C 0.2198(2) 0.66965(17) 0.24050(8) 0.0179(4) Uani 1 1 d . . . C34 C 0.2273(2) 0.45431(16) 0.09810(8) 0.0163(4) Uani 1 1 d . . . C35 C 0.1676(3) 0.36386(19) 0.08145(9) 0.0240(5) Uani 1 1 d . . . C36 C 0.1767(3) 0.3475(2) 0.01506(9) 0.0277(5) Uani 1 1 d . . . C37 C 0.3307(3) 0.31710(19) -0.00729(9) 0.0286(5) Uani 1 1 d . . . C38 C 0.3887(3) 0.4078(2) 0.00869(9) 0.0265(5) Uani 1 1 d . . . C39 C 0.3821(2) 0.42389(19) 0.07508(8) 0.0215(4) Uani 1 1 d . . . H2A H 0.460(2) 0.3487(18) 0.5489(10) 0.036(6) Uiso 1 1 d . . . H2B H 0.544(2) 0.3231(18) 0.4886(9) 0.035(6) Uiso 1 1 d . . . H2C H 0.401(2) 0.2957(18) 0.4972(9) 0.025(6) Uiso 1 1 d . . . H3A H 0.141(2) 0.4529(17) 0.5123(8) 0.022(5) Uiso 1 1 d . . . H3B H 0.105(2) 0.584(2) 0.5036(9) 0.035(6) Uiso 1 1 d . . . H3C H 0.196(2) 0.5095(18) 0.5569(10) 0.029(6) Uiso 1 1 d . . . H4 H 0.379(3) 0.092(3) 0.3080(13) 0.089(11) Uiso 1 1 d . . . H5A H 0.452(2) 0.1723(19) 0.3811(9) 0.023(6) Uiso 1 1 d . . . H5B H 0.624(6) 0.055(4) 0.386(2) 0.21(2) Uiso 1 1 d . . . H6A H 0.310(3) 0.083(2) 0.4125(11) 0.062(9) Uiso 1 1 d . . . H6B H 0.401(2) 0.0755(18) 0.4590(10) 0.032(6) Uiso 1 1 d . . . H7A H 0.552(6) -0.114(5) 0.436(2) 0.20(2) Uiso 1 1 d . . . H7B H 0.388(2) -0.1030(17) 0.4438(9) 0.022(5) Uiso 1 1 d . . . H8A H 0.355(5) -0.091(3) 0.3459(18) 0.138(16) Uiso 1 1 d . . . H8B H 0.482(2) -0.198(2) 0.3577(9) 0.032(6) Uiso 1 1 d . . . H9A H 0.639(5) -0.095(4) 0.3270(19) 0.152(19) Uiso 1 1 d . . . H9B H 0.532(2) -0.0948(17) 0.2782(9) 0.020(5) Uiso 1 1 d . . . H10 H 0.760(2) 0.1722(16) 0.2587(8) 0.015(5) Uiso 1 1 d . . . H11A H 0.867(2) -0.0248(19) 0.2745(9) 0.031(6) Uiso 1 1 d . . . H11B H 0.829(2) -0.0113(18) 0.3427(10) 0.034(6) Uiso 1 1 d . . . H12A H 1.072(3) -0.035(2) 0.3216(10) 0.039(7) Uiso 1 1 d . . . H12B H 1.024(2) 0.0699(16) 0.2790(9) 0.017(5) Uiso 1 1 d . . . H13A H 0.973(2) 0.0846(18) 0.3971(9) 0.028(6) Uiso 1 1 d . . . H13B H 1.072(2) 0.1327(17) 0.3660(9) 0.026(6) Uiso 1 1 d . . . H14A H 0.886(2) 0.2682(19) 0.3167(10) 0.034(7) Uiso 1 1 d . . . H14B H 0.847(3) 0.280(2) 0.3831(10) 0.043(7) Uiso 1 1 d . . . H15A H 0.646(2) 0.296(2) 0.3315(9) 0.037(6) Uiso 1 1 d . . . H15B H 0.696(2) 0.1882(17) 0.3727(9) 0.020(5) Uiso 1 1 d . . . H16 H 0.673(2) -0.0343(16) 0.2166(8) 0.013(5) Uiso 1 1 d . . . H17A H 0.428(2) 0.0223(17) 0.1885(9) 0.023(6) Uiso 1 1 d . . . H17B H 0.432(2) 0.1151(17) 0.1484(8) 0.019(5) Uiso 1 1 d . . . H18A H 0.452(3) -0.0435(19) 0.0968(10) 0.037(7) Uiso 1 1 d . . . H18B H 0.587(2) -0.1277(17) 0.1340(8) 0.019(5) Uiso 1 1 d . . . H19A H 0.587(2) 0.056(2) 0.0537(9) 0.035(6) Uiso 1 1 d . . . H19B H 0.671(2) -0.0721(19) 0.0448(10) 0.035(6) Uiso 1 1 d . . . H20A H 0.822(2) -0.0880(19) 0.1235(9) 0.027(6) Uiso 1 1 d . . . H20B H 0.819(2) 0.0073(18) 0.0850(10) 0.030(6) Uiso 1 1 d . . . H21A H 0.671(2) 0.1471(17) 0.1413(8) 0.019(5) Uiso 1 1 d . . . H21B H 0.810(2) 0.0729(17) 0.1772(9) 0.026(6) Uiso 1 1 d . . . H22 H 0.017(2) 0.4428(16) 0.1861(8) 0.015(5) Uiso 1 1 d . . . H23A H -0.090(2) 0.6847(19) 0.1730(9) 0.030(6) Uiso 1 1 d . . . H23B H -0.073(2) 0.6079(17) 0.1213(9) 0.025(6) Uiso 1 1 d . . . H24A H -0.246(2) 0.5371(18) 0.1610(8) 0.021(5) Uiso 1 1 d . . . H24B H -0.313(2) 0.6729(18) 0.1529(9) 0.031(6) Uiso 1 1 d . . . H25A H -0.277(2) 0.6892(17) 0.2562(8) 0.019(5) Uiso 1 1 d . . . H25B H -0.371(2) 0.6089(17) 0.2457(9) 0.026(6) Uiso 1 1 d . . . H26A H -0.157(2) 0.4440(17) 0.2655(8) 0.019(5) Uiso 1 1 d . . . H26B H -0.181(2) 0.5265(17) 0.3153(9) 0.027(6) Uiso 1 1 d . . . H27A H 0.066(2) 0.4602(17) 0.2840(8) 0.022(5) Uiso 1 1 d . . . H27B H -0.004(2) 0.5911(18) 0.2738(8) 0.021(5) Uiso 1 1 d . . . H28 H 0.366(2) 0.5805(15) 0.1790(7) 0.009(4) Uiso 1 1 d . . . H29A H 0.227(2) 0.6689(16) 0.0934(9) 0.019(5) Uiso 1 1 d . . . H29B H 0.100(2) 0.7372(16) 0.1323(8) 0.017(5) Uiso 1 1 d . . . H30A H 0.370(2) 0.7645(18) 0.1321(9) 0.032(6) Uiso 1 1 d . . . H30B H 0.233(2) 0.850(2) 0.1059(10) 0.039(7) Uiso 1 1 d . . . H31A H 0.266(2) 0.9117(17) 0.1990(8) 0.021(5) Uiso 1 1 d . . . H31B H 0.125(2) 0.8899(17) 0.1985(8) 0.022(6) Uiso 1 1 d . . . H32A H 0.248(2) 0.7990(19) 0.2855(10) 0.038(6) Uiso 1 1 d . . . H32B H 0.382(2) 0.7317(16) 0.2454(8) 0.020(5) Uiso 1 1 d . . . H33A H 0.2560(19) 0.6132(15) 0.2704(8) 0.009(5) Uiso 1 1 d . . . H33B H 0.116(2) 0.7011(15) 0.2441(8) 0.012(5) Uiso 1 1 d . . . H34 H 0.1685(19) 0.5247(16) 0.0814(8) 0.012(5) Uiso 1 1 d . . . H35A H 0.074(3) 0.3831(18) 0.0935(9) 0.032(6) Uiso 1 1 d . . . H35B H 0.222(2) 0.2935(17) 0.1025(8) 0.019(5) Uiso 1 1 d . . . H36A H 0.110(2) 0.4205(17) -0.0042(8) 0.017(5) Uiso 1 1 d . . . H36B H 0.139(2) 0.2899(19) 0.0049(9) 0.032(6) Uiso 1 1 d . . . H37A H 0.399(2) 0.2444(18) 0.0100(9) 0.028(6) Uiso 1 1 d . . . H37B H 0.335(2) 0.3088(18) -0.0515(10) 0.035(6) Uiso 1 1 d . . . H38A H 0.331(2) 0.4783(18) -0.0129(9) 0.028(6) Uiso 1 1 d . . . H38B H 0.487(3) 0.3881(19) -0.0058(10) 0.040(7) Uiso 1 1 d . . . H39A H 0.422(2) 0.4798(18) 0.0852(8) 0.024(5) Uiso 1 1 d . . . H39B H 0.444(2) 0.3533(17) 0.0957(8) 0.021(5) Uiso 1 1 d . . . C41 C 0.0739(2) 0.71794(18) 0.38823(9) 0.0271(5) Uani 1 1 d . . . C42 C -0.0650(3) 0.73106(19) 0.40425(10) 0.0305(5) Uani 1 1 d . . . C43 C -0.1283(3) 0.7964(2) 0.45161(10) 0.0335(5) Uani 1 1 d . . . C44 C -0.0530(3) 0.8482(2) 0.48245(10) 0.0340(5) Uani 1 1 d . . . C45 C 0.0862(3) 0.8350(2) 0.46629(10) 0.0329(5) Uani 1 1 d . . . C46 C 0.1507(2) 0.76897(19) 0.41901(10) 0.0285(5) Uani 1 1 d . . . H41 H 0.118(2) 0.6724(18) 0.3562(9) 0.030(6) Uiso 1 1 d . . . H42 H -0.117(2) 0.6934(18) 0.3832(9) 0.034(6) Uiso 1 1 d . . . H43 H -0.221(3) 0.8001(19) 0.4621(9) 0.036(6) Uiso 1 1 d . . . H44 H -0.094(2) 0.889(2) 0.5134(10) 0.039(7) Uiso 1 1 d . . . H45 H 0.130(2) 0.8724(19) 0.4880(9) 0.032(6) Uiso 1 1 d . . . H46 H 0.245(3) 0.7636(19) 0.4100(10) 0.041(7) Uiso 1 1 d . . . C51 C 0.9387(2) 0.22419(18) 0.12600(9) 0.0252(5) Uani 1 1 d . . . C52 C 0.8270(2) 0.27771(18) 0.08690(9) 0.0250(5) Uani 1 1 d . . . C53 C 0.8375(2) 0.24185(18) 0.02979(9) 0.0262(5) Uani 1 1 d . . . C54 C 0.9606(2) 0.15268(18) 0.01169(9) 0.0255(5) Uani 1 1 d . . . C55 C 1.0729(2) 0.09904(18) 0.05130(9) 0.0251(5) Uani 1 1 d . . . C56 C 1.0611(2) 0.13473(18) 0.10830(9) 0.0261(5) Uani 1 1 d . . . H51 H 0.933(2) 0.2489(17) 0.1625(9) 0.023(6) Uiso 1 1 d . . . H52 H 0.743(2) 0.3362(17) 0.0979(9) 0.023(6) Uiso 1 1 d . . . H53 H 0.760(2) 0.2792(17) 0.0020(9) 0.027(6) Uiso 1 1 d . . . H54 H 0.967(2) 0.1310(16) -0.0267(9) 0.018(5) Uiso 1 1 d . . . H55 H 1.155(2) 0.0370(17) 0.0405(8) 0.020(5) Uiso 1 1 d . . . H56 H 1.139(2) 0.1006(17) 0.1339(9) 0.027(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01223(7) 0.01330(7) 0.01118(7) -0.00205(5) 0.00105(5) -0.00471(6) Ru 0.01223(8) 0.01382(8) 0.01112(7) -0.00208(5) 0.00108(6) -0.00548(6) Cl1 0.0150(2) 0.0170(2) 0.0169(2) -0.00029(17) 0.00232(17) -0.00743(18) Cl2 0.0175(2) 0.0229(2) 0.0195(2) -0.00145(18) -0.00072(18) -0.01174(19) Cl3 0.0198(2) 0.0246(2) 0.0186(2) -0.00369(18) 0.00389(18) -0.0134(2) Cl4 0.0217(2) 0.0237(2) 0.0182(2) -0.00204(18) 0.00180(19) -0.0143(2) P1 0.0156(2) 0.0142(2) 0.0138(2) -0.00099(18) 0.00085(19) -0.00711(19) P2 0.0147(2) 0.0157(2) 0.0122(2) -0.00121(18) 0.00050(18) -0.00577(19) S 0.0161(2) 0.0163(2) 0.0134(2) -0.00192(17) 0.00072(18) -0.00699(19) C1 0.0109(9) 0.0135(9) 0.0163(9) 0.0010(7) 0.0005(7) -0.0047(7) C2 0.0259(12) 0.0200(11) 0.0204(11) 0.0009(8) -0.0063(9) -0.0091(9) C3 0.0212(11) 0.0284(12) 0.0179(11) -0.0061(9) 0.0076(9) -0.0115(10) C4 0.0599(17) 0.0308(12) 0.0181(11) -0.0046(9) 0.0118(11) -0.0319(12) C5 0.093(2) 0.0209(12) 0.0335(14) -0.0131(10) 0.0369(14) -0.0305(14) C6 0.0327(13) 0.0266(12) 0.0156(11) -0.0007(9) 0.0038(9) -0.0137(10) C7 0.103(3) 0.0337(14) 0.0307(14) -0.0058(11) 0.0327(16) -0.0404(16) C8 0.0465(15) 0.0240(12) 0.0248(12) 0.0002(9) 0.0051(10) -0.0236(11) C9 0.116(3) 0.0267(13) 0.0306(14) -0.0143(11) 0.0398(16) -0.0412(17) C10 0.0157(10) 0.0135(9) 0.0179(10) 0.0013(7) -0.0003(8) -0.0054(8) C11 0.0250(12) 0.0151(10) 0.0351(13) -0.0050(9) -0.0101(10) -0.0011(9) C12 0.0185(11) 0.0302(13) 0.0400(14) -0.0038(11) -0.0059(10) 0.0021(10) C13 0.0175(11) 0.0291(12) 0.0369(13) 0.0013(10) -0.0090(10) -0.0088(9) C14 0.0239(12) 0.0228(11) 0.0407(14) -0.0045(10) -0.0094(10) -0.0089(9) C15 0.0180(11) 0.0261(12) 0.0272(12) -0.0089(9) -0.0028(9) -0.0059(9) C16 0.0210(10) 0.0128(9) 0.0170(10) -0.0019(7) 0.0026(8) -0.0065(8) C17 0.0263(12) 0.0239(11) 0.0191(11) -0.0048(8) 0.0026(9) -0.0139(10) C18 0.0383(14) 0.0337(13) 0.0247(12) -0.0130(10) 0.0043(10) -0.0203(11) C19 0.0438(14) 0.0269(12) 0.0193(11) -0.0099(9) 0.0084(10) -0.0134(11) C20 0.0324(13) 0.0248(12) 0.0235(12) -0.0067(9) 0.0135(10) -0.0106(10) C21 0.0253(11) 0.0198(11) 0.0220(11) -0.0055(8) 0.0069(9) -0.0098(9) C22 0.0132(9) 0.0181(10) 0.0169(10) -0.0001(8) -0.0008(7) -0.0053(8) C23 0.0194(11) 0.0242(11) 0.0206(11) 0.0048(9) 0.0010(8) -0.0054(9) C24 0.0173(11) 0.0318(13) 0.0314(12) 0.0087(10) -0.0041(9) -0.0017(10) C25 0.0152(11) 0.0298(12) 0.0354(13) 0.0049(10) 0.0052(9) -0.0024(9) C26 0.0174(10) 0.0282(12) 0.0205(11) 0.0033(9) 0.0041(8) -0.0054(9) C27 0.0187(11) 0.0264(11) 0.0178(10) -0.0005(9) 0.0019(8) -0.0080(9) C28 0.0159(10) 0.0158(9) 0.0162(9) -0.0021(7) 0.0022(8) -0.0066(8) C29 0.0339(13) 0.0200(11) 0.0181(11) 0.0005(8) -0.0004(9) -0.0133(10) C30 0.0347(13) 0.0221(11) 0.0258(12) 0.0031(9) -0.0002(10) -0.0143(10) C31 0.0255(12) 0.0185(11) 0.0318(12) -0.0027(9) -0.0026(9) -0.0118(9) C32 0.0247(12) 0.0207(11) 0.0261(11) -0.0051(8) -0.0046(9) -0.0082(9) C33 0.0186(11) 0.0170(10) 0.0164(10) -0.0004(8) -0.0020(8) -0.0045(8) C34 0.0193(10) 0.0172(10) 0.0121(9) -0.0002(7) -0.0007(8) -0.0064(8) C35 0.0328(13) 0.0263(12) 0.0175(10) -0.0008(9) -0.0013(9) -0.0163(10) C36 0.0430(14) 0.0261(12) 0.0186(11) -0.0031(9) -0.0044(10) -0.0181(11) C37 0.0392(13) 0.0230(11) 0.0168(11) -0.0054(9) -0.0031(10) -0.0034(10) C38 0.0267(12) 0.0324(13) 0.0177(11) -0.0042(9) 0.0038(9) -0.0079(10) C39 0.0224(11) 0.0261(11) 0.0162(10) -0.0048(8) 0.0013(8) -0.0089(9) C41 0.0334(13) 0.0227(11) 0.0177(11) -0.0007(8) 0.0054(9) -0.0022(10) C42 0.0366(14) 0.0295(12) 0.0280(12) -0.0011(9) -0.0050(10) -0.0152(11) C43 0.0236(12) 0.0409(14) 0.0355(13) -0.0044(10) 0.0080(10) -0.0116(11) C44 0.0342(14) 0.0353(13) 0.0301(13) -0.0149(10) 0.0107(10) -0.0095(11) C45 0.0358(14) 0.0326(13) 0.0361(13) -0.0076(10) 0.0011(11) -0.0188(11) C46 0.0234(12) 0.0297(12) 0.0304(12) 0.0044(9) 0.0083(10) -0.0082(10) C51 0.0362(13) 0.0286(12) 0.0193(11) -0.0005(9) 0.0023(9) -0.0221(10) C52 0.0243(11) 0.0256(11) 0.0249(11) -0.0009(9) 0.0087(9) -0.0094(9) C53 0.0243(12) 0.0308(12) 0.0216(11) 0.0052(9) 0.0008(9) -0.0089(10) C54 0.0305(12) 0.0280(12) 0.0192(11) -0.0030(9) 0.0046(9) -0.0123(10) C55 0.0234(11) 0.0188(11) 0.0325(12) 0.0012(9) 0.0017(9) -0.0076(9) C56 0.0288(12) 0.0263(11) 0.0284(12) 0.0080(9) -0.0082(10) -0.0171(10) _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 C1 1.9457(17) . yes Pd Cl4 2.2919(5) . yes Pd Cl3 2.3104(5) . yes Pd S 2.3556(5) . yes Ru C1 1.6619(17) . yes Ru Cl1 2.3474(4) . yes Ru Cl2 2.3523(5) . yes Ru P1 2.4354(5) . yes Ru P2 2.4357(5) . yes P1 C10 1.8459(19) . ? P1 C4 1.849(2) . ? P1 C16 1.8613(19) . ? P2 C22 1.8508(19) . ? P2 C28 1.8493(19) . ? P2 C34 1.8609(18) . ? S C2 1.802(2) . ? S C3 1.797(2) . ? C2 H2A 0.99(2) . ? C2 H2B 0.98(2) . ? C2 H2C 0.93(2) . ? C3 H3A 0.93(2) . ? C3 H3B 0.96(2) . ? C3 H3C 0.92(2) . ? C4 C5 1.461(3) . ? C4 C9 1.461(3) . ? C4 H4 1.10(3) . ? C5 C6 1.476(3) . ? C5 H5A 0.85(2) . ? C5 H5B 1.35(5) . ? C6 C7 1.473(3) . ? C6 H6A 0.95(3) . ? C6 H6B 0.89(2) . ? C7 C8 1.474(3) . ? C7 H7A 1.16(5) . ? C7 H7B 0.90(2) . ? C8 C9 1.480(3) . ? C8 H8A 0.98(4) . ? C8 H8B 0.92(2) . ? C9 H9A 1.10(4) . ? C9 H9B 0.89(2) . ? C10 C15 1.525(3) . ? C10 C11 1.530(3) . ? C10 H10 0.891(19) . ? C11 C12 1.527(3) . ? C11 H11A 0.88(2) . ? C11 H11B 1.06(2) . ? C12 C13 1.519(3) . ? C12 H12A 0.95(2) . ? C12 H12B 0.919(19) . ? C13 C14 1.509(3) . ? C13 H13A 0.95(2) . ? C13 H13B 0.91(2) . ? C14 C15 1.523(3) . ? C14 H14A 0.93(2) . ? C14 H14B 0.94(2) . ? C15 H15A 0.99(2) . ? C15 H15B 0.91(2) . ? C16 C21 1.529(3) . ? C16 C17 1.532(3) . ? C16 H16 0.970(18) . ? C17 C18 1.527(3) . ? C17 H17A 0.86(2) . ? C17 H17B 0.97(2) . ? C18 C19 1.521(3) . ? C18 H18A 0.92(2) . ? C18 H18B 1.03(2) . ? C19 C20 1.516(3) . ? C19 H19A 0.98(2) . ? C19 H19B 0.95(2) . ? C20 C21 1.530(3) . ? C20 H20A 0.96(2) . ? C20 H20B 0.83(2) . ? C21 H21A 0.94(2) . ? C21 H21B 1.02(2) . ? C22 C23 1.526(3) . ? C22 C27 1.537(3) . ? C22 H22 0.948(19) . ? C23 C24 1.535(3) . ? C23 H23A 0.97(2) . ? C23 H23B 0.95(2) . ? C24 C25 1.519(3) . ? C24 H24A 0.97(2) . ? C24 H24B 0.97(2) . ? C25 C26 1.519(3) . ? C25 H25A 1.01(2) . ? C25 H25B 0.97(2) . ? C26 C27 1.523(3) . ? C26 H26A 0.98(2) . ? C26 H26B 0.94(2) . ? C27 H27A 0.97(2) . ? C27 H27B 0.93(2) . ? C28 C33 1.525(2) . ? C28 C29 1.530(3) . ? C28 H28 0.985(18) . ? C29 C30 1.530(3) . ? C29 H29A 0.968(19) . ? C29 H29B 0.95(2) . ? C30 C31 1.517(3) . ? C30 H30A 0.99(2) . ? C30 H30B 0.92(2) . ? C31 C32 1.517(3) . ? C31 H31A 0.95(2) . ? C31 H31B 0.93(2) . ? C32 C33 1.520(3) . ? C32 H32A 1.01(2) . ? C32 H32B 0.96(2) . ? C33 H33A 0.936(18) . ? C33 H33B 0.963(19) . ? C34 C35 1.526(3) . ? C34 C39 1.531(3) . ? C34 H34 0.927(18) . ? C35 C36 1.533(3) . ? C35 H35A 0.91(2) . ? C35 H35B 0.96(2) . ? C36 C37 1.519(3) . ? C36 H36A 0.998(19) . ? C36 H36B 0.97(2) . ? C37 C38 1.514(3) . ? C37 H37A 0.98(2) . ? C37 H37B 1.02(2) . ? C38 C39 1.533(3) . ? C38 H38A 0.97(2) . ? C38 H38B 0.97(2) . ? C39 H39A 0.96(2) . ? C39 H39B 0.98(2) . ? C41 C42 1.374(3) . ? C41 C46 1.377(3) . ? C41 H41 0.94(2) . ? C42 C43 1.379(3) . ? C42 H42 0.96(2) . ? C43 C44 1.374(3) . ? C43 H43 0.94(2) . ? C44 C45 1.377(3) . ? C44 H44 0.89(2) . ? C45 C46 1.384(3) . ? C45 H45 0.91(2) . ? C46 H46 0.93(2) . ? C51 C52 1.377(3) . ? C51 C56 1.379(3) . ? C51 H51 0.89(2) . ? C52 C53 1.384(3) . ? C52 H52 0.92(2) . ? C53 C54 1.385(3) . ? C53 H53 0.97(2) . ? C54 C55 1.387(3) . ? C54 H54 0.922(19) . ? C55 C56 1.381(3) . ? C55 H55 0.930(19) . ? C56 H56 0.93(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd Cl4 90.68(5) . . yes C1 Pd Cl3 90.55(5) . . yes Cl4 Pd Cl3 178.134(17) . . yes C1 Pd S 170.50(5) . . yes Cl4 Pd S 92.725(16) . . yes Cl3 Pd S 86.274(16) . . yes C1 Ru Cl1 100.49(6) . . yes C1 Ru Cl2 101.23(6) . . yes Cl1 Ru Cl2 158.274(17) . . yes C1 Ru P1 98.92(6) . . yes Cl1 Ru P1 87.769(16) . . yes Cl2 Ru P1 88.627(17) . . yes C1 Ru P2 98.19(6) . . yes Cl1 Ru P2 89.148(16) . . yes Cl2 Ru P2 88.029(17) . . yes P1 Ru P2 162.888(17) . . yes C10 P1 C4 109.28(10) . . ? C10 P1 C16 103.46(9) . . ? C4 P1 C16 105.88(9) . . ? C10 P1 Ru 114.01(6) . . ? C4 P1 Ru 113.35(9) . . ? C16 P1 Ru 110.11(6) . . ? C22 P2 C28 111.96(9) . . ? C22 P2 C34 104.81(9) . . ? C28 P2 C34 103.43(8) . . ? C22 P2 Ru 112.25(6) . . ? C28 P2 Ru 112.29(6) . . ? C34 P2 Ru 111.52(6) . . ? C2 S C3 99.43(11) . . ? C2 S Pd 97.64(7) . . ? C3 S Pd 113.15(7) . . ? Ru C1 Pd 175.11(11) . . ? S C2 H2A 108.4(12) . . ? S C2 H2B 106.9(13) . . ? H2A C2 H2B 107.3(18) . . ? S C2 H2C 108.3(12) . . ? H2A C2 H2C 112.5(18) . . ? H2B C2 H2C 113.1(18) . . ? S C3 H3A 111.8(12) . . ? S C3 H3B 107.4(13) . . ? H3A C3 H3B 110.5(18) . . ? S C3 H3C 108.0(13) . . ? H3A C3 H3C 106.4(18) . . ? H3B C3 H3C 112.7(18) . . ? C5 C4 C9 118.1(2) . . ? C5 C4 P1 114.80(15) . . ? C9 C4 P1 120.93(16) . . ? C5 C4 H4 96.2(16) . . ? C9 C4 H4 99.8(16) . . ? P1 C4 H4 98.8(16) . . ? C4 C5 C6 117.2(2) . . ? C4 C5 H5A 116.9(14) . . ? C6 C5 H5A 112.9(14) . . ? C4 C5 H5B 90(2) . . ? C6 C5 H5B 110(2) . . ? H5A C5 H5B 107(3) . . ? C5 C6 C7 116.9(2) . . ? C5 C6 H6A 102.6(16) . . ? C7 C6 H6A 100.6(16) . . ? C5 C6 H6B 116.5(14) . . ? C7 C6 H6B 117.4(14) . . ? H6A C6 H6B 97(2) . . ? C8 C7 C6 117.5(2) . . ? C8 C7 H7A 100(2) . . ? C6 C7 H7A 100(3) . . ? C8 C7 H7B 117.6(13) . . ? C6 C7 H7B 115.9(13) . . ? H7A C7 H7B 101(3) . . ? C7 C8 C9 118.0(2) . . ? C7 C8 H8A 98(2) . . ? C9 C8 H8A 102(2) . . ? C7 C8 H8B 114.4(13) . . ? C9 C8 H8B 117.2(14) . . ? H8A C8 H8B 102(3) . . ? C4 C9 C8 116.4(2) . . ? C4 C9 H9A 94(2) . . ? C8 C9 H9A 105(2) . . ? C4 C9 H9B 118.9(13) . . ? C8 C9 H9B 115.2(13) . . ? H9A C9 H9B 102(3) . . ? C15 C10 C11 110.32(17) . . ? C15 C10 P1 114.84(13) . . ? C11 C10 P1 115.55(13) . . ? C15 C10 H10 105.7(12) . . ? C11 C10 H10 109.0(12) . . ? P1 C10 H10 100.4(12) . . ? C12 C11 C10 109.73(18) . . ? C12 C11 H11A 109.2(14) . . ? C10 C11 H11A 111.3(14) . . ? C12 C11 H11B 108.8(12) . . ? C10 C11 H11B 107.2(12) . . ? H11A C11 H11B 110.6(18) . . ? C13 C12 C11 111.32(19) . . ? C13 C12 H12A 110.5(14) . . ? C11 C12 H12A 107.7(14) . . ? C13 C12 H12B 106.9(12) . . ? C11 C12 H12B 109.9(12) . . ? H12A C12 H12B 110.7(18) . . ? C14 C13 C12 111.20(19) . . ? C14 C13 H13A 110.1(13) . . ? C12 C13 H13A 107.9(13) . . ? C14 C13 H13B 108.4(13) . . ? C12 C13 H13B 112.1(13) . . ? H13A C13 H13B 107.1(18) . . ? C13 C14 C15 112.09(19) . . ? C13 C14 H14A 108.2(14) . . ? C15 C14 H14A 107.8(14) . . ? C13 C14 H14B 112.0(14) . . ? C15 C14 H14B 103.4(15) . . ? H14A C14 H14B 113(2) . . ? C14 C15 C10 110.31(17) . . ? C14 C15 H15A 108.6(13) . . ? C10 C15 H15A 111.1(13) . . ? C14 C15 H15B 110.3(13) . . ? C10 C15 H15B 107.6(13) . . ? H15A C15 H15B 109.0(18) . . ? C21 C16 C17 109.26(16) . . ? C21 C16 P1 113.42(13) . . ? C17 C16 P1 112.84(13) . . ? C21 C16 H16 106.3(11) . . ? C17 C16 H16 110.6(11) . . ? P1 C16 H16 104.2(10) . . ? C18 C17 C16 111.35(18) . . ? C18 C17 H17A 110.4(14) . . ? C16 C17 H17A 110.3(14) . . ? C18 C17 H17B 108.7(11) . . ? C16 C17 H17B 109.8(12) . . ? H17A C17 H17B 106.2(17) . . ? C19 C18 C17 111.21(18) . . ? C19 C18 H18A 111.9(14) . . ? C17 C18 H18A 107.6(14) . . ? C19 C18 H18B 108.8(11) . . ? C17 C18 H18B 108.9(11) . . ? H18A C18 H18B 108.3(18) . . ? C18 C19 C20 110.89(19) . . ? C18 C19 H19A 109.4(13) . . ? C20 C19 H19A 109.7(13) . . ? C18 C19 H19B 110.7(13) . . ? C20 C19 H19B 111.0(13) . . ? H19A C19 H19B 104.9(18) . . ? C19 C20 C21 112.11(18) . . ? C19 C20 H20A 107.4(12) . . ? C21 C20 H20A 110.4(12) . . ? C19 C20 H20B 109.2(16) . . ? C21 C20 H20B 109.9(15) . . ? H20A C20 H20B 107.7(19) . . ? C20 C21 C16 110.76(17) . . ? C20 C21 H21A 108.4(12) . . ? C16 C21 H21A 110.2(12) . . ? C20 C21 H21B 106.9(11) . . ? C16 C21 H21B 114.1(11) . . ? H21A C21 H21B 106.1(16) . . ? C23 C22 C27 110.49(16) . . ? C23 C22 P2 116.98(13) . . ? C27 C22 P2 114.32(13) . . ? C23 C22 H22 108.8(11) . . ? C27 C22 H22 105.9(11) . . ? P2 C22 H22 99.0(11) . . ? C24 C23 C22 109.71(16) . . ? C24 C23 H23A 110.3(12) . . ? C22 C23 H23A 110.0(13) . . ? C24 C23 H23B 111.2(12) . . ? C22 C23 H23B 111.4(12) . . ? H23A C23 H23B 104.2(17) . . ? C25 C24 C23 111.60(19) . . ? C25 C24 H24A 108.9(12) . . ? C23 C24 H24A 108.9(12) . . ? C25 C24 H24B 111.2(12) . . ? C23 C24 H24B 106.7(13) . . ? H24A C24 H24B 109.5(17) . . ? C26 C25 C24 110.89(18) . . ? C26 C25 H25A 104.8(11) . . ? C24 C25 H25A 111.5(11) . . ? C26 C25 H25B 110.6(12) . . ? C24 C25 H25B 108.1(12) . . ? H25A C25 H25B 111.0(16) . . ? C25 C26 C27 111.79(18) . . ? C25 C26 H26A 112.0(11) . . ? C27 C26 H26A 107.5(11) . . ? C25 C26 H26B 110.5(12) . . ? C27 C26 H26B 110.4(13) . . ? H26A C26 H26B 104.4(17) . . ? C26 C27 C22 110.02(17) . . ? C26 C27 H27A 111.7(12) . . ? C22 C27 H27A 109.3(12) . . ? C26 C27 H27B 111.3(12) . . ? C22 C27 H27B 106.6(12) . . ? H27A C27 H27B 107.7(17) . . ? C33 C28 C29 110.30(16) . . ? C33 C28 P2 112.07(13) . . ? C29 C28 P2 116.77(13) . . ? C33 C28 H28 107.4(10) . . ? C29 C28 H28 107.6(10) . . ? P2 C28 H28 101.9(10) . . ? C30 C29 C28 110.28(17) . . ? C30 C29 H29A 110.9(11) . . ? C28 C29 H29A 111.5(11) . . ? C30 C29 H29B 108.5(12) . . ? C28 C29 H29B 110.0(11) . . ? H29A C29 H29B 105.4(16) . . ? C31 C30 C29 111.51(18) . . ? C31 C30 H30A 110.4(12) . . ? C29 C30 H30A 108.7(13) . . ? C31 C30 H30B 112.8(14) . . ? C29 C30 H30B 110.2(14) . . ? H30A C30 H30B 103.0(18) . . ? C32 C31 C30 110.66(17) . . ? C32 C31 H31A 111.0(12) . . ? C30 C31 H31A 110.0(12) . . ? C32 C31 H31B 108.7(12) . . ? C30 C31 H31B 108.7(12) . . ? H31A C31 H31B 107.7(17) . . ? C31 C32 C33 111.69(17) . . ? C31 C32 H32A 112.2(12) . . ? C33 C32 H32A 107.5(13) . . ? C31 C32 H32B 109.0(12) . . ? C33 C32 H32B 109.0(12) . . ? H32A C32 H32B 107.3(17) . . ? C32 C33 C28 110.99(16) . . ? C32 C33 H33A 111.3(11) . . ? C28 C33 H33A 108.8(11) . . ? C32 C33 H33B 109.7(11) . . ? C28 C33 H33B 108.8(11) . . ? H33A C33 H33B 107.2(15) . . ? C35 C34 C39 110.61(17) . . ? C35 C34 P2 113.96(13) . . ? C39 C34 P2 111.91(13) . . ? C35 C34 H34 108.7(11) . . ? C39 C34 H34 108.9(11) . . ? P2 C34 H34 102.4(11) . . ? C34 C35 C36 111.05(17) . . ? C34 C35 H35A 111.0(14) . . ? C36 C35 H35A 109.7(14) . . ? C34 C35 H35B 108.1(12) . . ? C36 C35 H35B 111.1(12) . . ? H35A C35 H35B 105.7(18) . . ? C37 C36 C35 111.61(18) . . ? C37 C36 H36A 110.7(11) . . ? C35 C36 H36A 107.5(11) . . ? C37 C36 H36B 110.8(13) . . ? C35 C36 H36B 110.6(13) . . ? H36A C36 H36B 105.4(16) . . ? C38 C37 C36 110.56(18) . . ? C38 C37 H37A 106.0(12) . . ? C36 C37 H37A 112.7(12) . . ? C38 C37 H37B 109.5(12) . . ? C36 C37 H37B 111.2(12) . . ? H37A C37 H37B 106.7(17) . . ? C37 C38 C39 111.12(18) . . ? C37 C38 H38A 106.8(12) . . ? C39 C38 H38A 111.9(12) . . ? C37 C38 H38B 110.2(13) . . ? C39 C38 H38B 111.1(13) . . ? H38A C38 H38B 105.4(18) . . ? C38 C39 C34 111.20(17) . . ? C38 C39 H39A 110.8(12) . . ? C34 C39 H39A 112.2(12) . . ? C38 C39 H39B 110.5(11) . . ? C34 C39 H39B 107.7(11) . . ? H39A C39 H39B 104.2(16) . . ? C42 C41 C46 120.8(2) . . ? C42 C41 H41 120.0(13) . . ? C46 C41 H41 119.3(13) . . ? C41 C42 C43 119.5(2) . . ? C41 C42 H42 120.2(13) . . ? C43 C42 H42 120.2(13) . . ? C44 C43 C42 120.2(2) . . ? C44 C43 H43 123.1(14) . . ? C42 C43 H43 116.7(14) . . ? C43 C44 C45 120.2(2) . . ? C43 C44 H44 119.7(15) . . ? C45 C44 H44 120.1(15) . . ? C44 C45 C46 119.9(2) . . ? C44 C45 H45 116.1(14) . . ? C46 C45 H45 123.9(14) . . ? C41 C46 C45 119.4(2) . . ? C41 C46 H46 124.5(14) . . ? C45 C46 H46 116.1(15) . . ? C52 C51 C56 120.0(2) . . ? C52 C51 H51 119.9(13) . . ? C56 C51 H51 120.1(13) . . ? C51 C52 C53 120.0(2) . . ? C51 C52 H52 121.7(13) . . ? C53 C52 H52 118.4(13) . . ? C54 C53 C52 120.3(2) . . ? C54 C53 H53 119.2(12) . . ? C52 C53 H53 120.6(12) . . ? C55 C54 C53 119.5(2) . . ? C55 C54 H54 121.2(12) . . ? C53 C54 H54 119.2(12) . . ? C54 C55 C56 119.9(2) . . ? C54 C55 H55 120.9(12) . . ? C56 C55 H55 119.2(12) . . ? C55 C56 C51 120.4(2) . . ? C55 C56 H56 119.0(13) . . ? C51 C56 H56 120.5(13) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.838 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.074 #===END