Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ebbe Nordlander' 'Matti Haukka' 'Pertti Homanen' 'Viktor Moberg' 'Magda Monari' 'Tapani Pakkanen' 'Roger Persson' 'Simona Selva' _publ_contact_author_name 'Dr Ebbe Nordlander' _publ_contact_author_address ; Inorganic Chemistry Center for Chemistry and Chemical Engineering Lund University Box 124 Lund SE-221 00 SWEDEN ; _publ_contact_author_email EBBE.NORDLANDER@INORG.LU.SE _publ_section_title ;Synthesis, characterizSupplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ation and reactivity of tetranuclear ruthenium hydrido clusters containing chiral phosphine ligands ; data_H4Ru4(CO)11(NMDPP)_(1) _database_code_depnum_ccdc_archive 'CCDC 287842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H33 O11 P Ru4' _chemical_formula_weight 1040.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.30740(10) _cell_length_b 17.7513(3) _cell_length_c 22.3268(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3688.80(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41845 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8385 _reflns_number_gt 7859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+0.5566P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.033(19) _refine_ls_number_reflns 8385 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0427 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.17135(2) 0.388253(12) 0.764991(10) 0.01439(5) Uani 1 1 d . . . Ru2 Ru 0.15310(2) 0.247931(12) 0.836980(10) 0.01629(5) Uani 1 1 d . . . Ru3 Ru 0.20785(2) 0.381784(13) 0.897133(10) 0.01811(5) Uani 1 1 d . . . Ru4 Ru 0.42993(2) 0.323942(12) 0.827475(11) 0.01694(5) Uani 1 1 d . . . P1 P 0.20004(7) 0.35796(4) 0.66223(3) 0.01413(14) Uani 1 1 d . . . O1 O -0.1483(2) 0.41580(13) 0.74800(10) 0.0313(5) Uani 1 1 d . . . O2 O 0.2561(3) 0.55356(12) 0.76461(11) 0.0362(6) Uani 1 1 d . . . O3 O 0.1142(3) 0.09686(12) 0.77245(11) 0.0388(6) Uani 1 1 d . . . O4 O -0.1659(2) 0.26303(16) 0.86208(11) 0.0456(6) Uani 1 1 d . . . O5 O 0.2246(3) 0.17828(12) 0.95789(10) 0.0328(5) Uani 1 1 d . . . O6 O -0.0943(3) 0.40360(16) 0.94790(11) 0.0479(7) Uani 1 1 d . . . O7 O 0.3458(2) 0.32832(11) 1.01335(9) 0.0278(5) Uani 1 1 d . . . O8 O 0.2983(3) 0.54495(12) 0.91354(12) 0.0423(6) Uani 1 1 d . . . O9 O 0.5601(2) 0.24224(14) 0.93430(10) 0.0348(5) Uani 1 1 d . . . O11 O 0.5871(3) 0.47041(14) 0.85350(13) 0.0543(8) Uani 1 1 d . . . O10 O 0.6479(2) 0.25805(14) 0.73862(10) 0.0396(6) Uani 1 1 d . . . C1 C -0.0271(3) 0.40686(16) 0.75377(13) 0.0218(7) Uani 1 1 d . . . C2 C 0.2263(3) 0.49122(17) 0.76175(14) 0.0228(6) Uani 1 1 d . . . C3 C 0.1317(3) 0.15410(17) 0.79298(14) 0.0256(7) Uani 1 1 d . . . C4 C -0.0455(3) 0.25786(18) 0.85432(14) 0.0281(7) Uani 1 1 d . . . C5 C 0.1973(3) 0.20635(15) 0.91325(14) 0.0217(7) Uani 1 1 d . . . C6 C 0.0196(3) 0.3938(2) 0.93028(14) 0.0305(8) Uani 1 1 d . . . C7 C 0.2947(3) 0.34637(15) 0.96931(14) 0.0213(6) Uani 1 1 d . . . C8 C 0.2695(3) 0.48272(18) 0.90836(14) 0.0265(7) Uani 1 1 d . . . C9 C 0.5108(3) 0.27448(18) 0.89526(15) 0.0244(7) Uani 1 1 d . . . C11 C 0.5262(3) 0.41544(19) 0.84376(15) 0.0303(8) Uani 1 1 d . . . C10 C 0.5645(3) 0.28136(17) 0.77093(14) 0.0241(7) Uani 1 1 d . . . C12 C 0.1370(3) 0.26181(15) 0.64801(12) 0.0157(6) Uani 1 1 d . . . C13 C 0.2284(3) 0.20036(16) 0.64336(14) 0.0229(7) Uani 1 1 d . . . H13 H 0.3291 0.2082 0.6463 0.028 Uiso 1 1 calc R . . C14 C 0.1772(3) 0.12814(16) 0.63456(14) 0.0268(7) Uani 1 1 d . . . H14 H 0.2422 0.0872 0.6306 0.032 Uiso 1 1 calc R . . C15 C 0.0298(3) 0.11577(17) 0.63155(14) 0.0259(7) Uani 1 1 d . . . H15 H -0.0065 0.0664 0.6251 0.031 Uiso 1 1 calc R . . C16 C -0.0630(3) 0.17551(17) 0.63806(14) 0.0271(7) Uani 1 1 d . . . H16 H -0.1637 0.1669 0.6372 0.032 Uiso 1 1 calc R . . C17 C -0.0115(3) 0.24795(16) 0.64581(13) 0.0214(6) Uani 1 1 d . . . H17 H -0.0771 0.2887 0.6497 0.026 Uiso 1 1 calc R . . C18 C 0.0920(3) 0.41517(15) 0.61072(13) 0.0167(6) Uani 1 1 d . . . C19 C 0.0529(3) 0.48821(16) 0.62631(13) 0.0222(7) Uani 1 1 d . . . H19 H 0.0748 0.5066 0.6652 0.027 Uiso 1 1 calc R . . C20 C -0.0179(3) 0.53478(17) 0.58585(14) 0.0259(7) Uani 1 1 d . . . H20 H -0.0420 0.5849 0.5969 0.031 Uiso 1 1 calc R . . C21 C -0.0532(3) 0.50841(17) 0.52981(13) 0.0242(7) Uani 1 1 d . . . H21 H -0.1014 0.5402 0.5021 0.029 Uiso 1 1 calc R . . C22 C -0.0180(3) 0.43506(17) 0.51409(13) 0.0207(6) Uani 1 1 d . . . H22 H -0.0436 0.4164 0.4757 0.025 Uiso 1 1 calc R . . C23 C 0.0539(3) 0.38910(16) 0.55394(12) 0.0175(6) Uani 1 1 d . . . H23 H 0.0778 0.3391 0.5426 0.021 Uiso 1 1 calc R . . C24 C 0.3853(3) 0.35639(16) 0.63029(13) 0.0180(6) Uani 1 1 d . . . H24 H 0.4316 0.3124 0.6505 0.022 Uiso 1 1 calc R . . C29 C 0.4852(3) 0.42311(16) 0.64606(13) 0.0202(6) Uani 1 1 d . . . H29 H 0.4980 0.4201 0.6905 0.024 Uiso 1 1 calc R . . C28 C 0.6358(3) 0.40646(19) 0.61989(14) 0.0293(8) Uani 1 1 d . . . H28A H 0.6951 0.4525 0.6236 0.035 Uiso 1 1 calc R . . H28B H 0.6816 0.3668 0.6446 0.035 Uiso 1 1 calc R . . C27 C 0.6380(3) 0.3809(2) 0.55402(15) 0.0350(8) Uani 1 1 d . . . H27A H 0.6094 0.4237 0.5282 0.042 Uiso 1 1 calc R . . H27B H 0.7373 0.3665 0.5430 0.042 Uiso 1 1 calc R . . C26 C 0.5391(3) 0.3152(2) 0.54214(14) 0.0286(7) Uani 1 1 d . . . H26 H 0.5347 0.3079 0.4978 0.034 Uiso 1 1 calc R . . C25 C 0.3866(3) 0.33457(17) 0.56362(13) 0.0209(6) Uani 1 1 d . . . H25A H 0.3230 0.2905 0.5573 0.025 Uiso 1 1 calc R . . H25B H 0.3484 0.3769 0.5396 0.025 Uiso 1 1 calc R . . C30 C 0.4289(4) 0.50410(16) 0.63431(14) 0.0268(7) Uani 1 1 d . . . H30 H 0.3315 0.5066 0.6532 0.032 Uiso 1 1 calc R . . C31 C 0.5216(4) 0.56147(19) 0.6677(2) 0.0447(9) Uani 1 1 d . . . H31A H 0.6129 0.5681 0.6465 0.067 Uiso 1 1 calc R . . H31B H 0.5404 0.5433 0.7084 0.067 Uiso 1 1 calc R . . H31C H 0.4710 0.6098 0.6697 0.067 Uiso 1 1 calc R . . C32 C 0.4089(4) 0.5288(2) 0.56961(17) 0.0424(9) Uani 1 1 d . . . H32A H 0.3684 0.5798 0.5687 0.064 Uiso 1 1 calc R . . H32B H 0.3434 0.4940 0.5493 0.064 Uiso 1 1 calc R . . H32C H 0.5021 0.5287 0.5492 0.064 Uiso 1 1 calc R . . C33 C 0.5952(3) 0.2420(2) 0.56962(15) 0.0342(8) Uani 1 1 d . . . H33A H 0.6866 0.2284 0.5507 0.051 Uiso 1 1 calc R . . H33B H 0.5250 0.2017 0.5630 0.051 Uiso 1 1 calc R . . H33C H 0.6098 0.2490 0.6127 0.051 Uiso 1 1 calc R . . H112 H 0.134(3) 0.2983(16) 0.7750(13) 0.022(8) Uiso 1 1 d . . . H113 H 0.112(3) 0.4181(18) 0.8333(18) 0.045(10) Uiso 1 1 d . . . H114 H 0.350(3) 0.3664(17) 0.7651(14) 0.030(8) Uiso 1 1 d . . . H124 H 0.318(4) 0.250(2) 0.8145(17) 0.060(12) 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 Ru1 0.01518(11) 0.01396(10) 0.01403(11) 0.00034(9) -0.00035(8) 0.00000(10) Ru2 0.01609(10) 0.01659(10) 0.01618(11) 0.00246(10) -0.00152(9) -0.00275(10) Ru3 0.01869(11) 0.02054(11) 0.01511(12) -0.00151(10) -0.00076(9) -0.00002(10) Ru4 0.01322(11) 0.01884(11) 0.01875(12) 0.00128(10) -0.00140(9) -0.00057(9) P1 0.0139(3) 0.0131(3) 0.0153(4) 0.0002(3) -0.0005(3) 0.0005(3) O1 0.0183(11) 0.0430(13) 0.0325(13) 0.0040(10) -0.0004(10) 0.0042(11) O2 0.0564(16) 0.0177(11) 0.0344(14) -0.0033(10) 0.0004(12) -0.0060(11) O3 0.0648(17) 0.0234(12) 0.0281(14) -0.0013(10) -0.0045(12) -0.0132(11) O4 0.0177(12) 0.0762(18) 0.0429(15) 0.0132(13) 0.0015(11) -0.0016(14) O5 0.0476(14) 0.0274(11) 0.0235(12) 0.0091(10) -0.0125(10) -0.0095(11) O6 0.0291(13) 0.080(2) 0.0347(15) -0.0122(13) 0.0085(11) 0.0063(14) O7 0.0344(12) 0.0294(11) 0.0197(12) 0.0012(9) -0.0051(10) 0.0033(11) O8 0.0553(16) 0.0213(12) 0.0503(16) -0.0015(11) -0.0237(13) 0.0031(12) O9 0.0288(12) 0.0495(14) 0.0261(13) 0.0100(11) -0.0044(10) 0.0104(12) O11 0.0487(16) 0.0423(15) 0.072(2) -0.0102(14) -0.0032(14) -0.0226(14) O10 0.0328(13) 0.0549(15) 0.0312(13) -0.0023(12) 0.0068(11) 0.0129(13) C1 0.0278(17) 0.0208(15) 0.0168(16) 0.0002(12) 0.0026(12) -0.0010(13) C2 0.0263(16) 0.0238(16) 0.0184(16) -0.0009(13) -0.0004(13) 0.0055(14) C3 0.0356(18) 0.0229(16) 0.0182(16) 0.0073(13) -0.0016(13) -0.0045(15) C4 0.0282(18) 0.0351(18) 0.0211(16) 0.0064(14) -0.0031(13) -0.0036(16) C5 0.0249(16) 0.0137(13) 0.0265(18) 0.0007(12) -0.0020(13) -0.0093(12) C6 0.0307(18) 0.042(2) 0.0191(17) -0.0044(15) -0.0057(13) 0.0048(16) C7 0.0224(15) 0.0164(14) 0.0251(17) -0.0044(12) 0.0005(13) -0.0019(13) C8 0.0309(17) 0.0269(17) 0.0216(17) 0.0006(14) -0.0090(14) 0.0046(15) C9 0.0141(14) 0.0305(17) 0.0286(18) -0.0035(14) 0.0037(14) -0.0015(13) C11 0.0235(16) 0.0355(18) 0.032(2) -0.0008(15) -0.0021(14) -0.0074(15) C10 0.0187(15) 0.0278(16) 0.0258(18) 0.0019(13) -0.0029(14) 0.0031(14) C12 0.0184(14) 0.0153(13) 0.0135(14) 0.0005(11) -0.0003(10) 0.0015(12) C13 0.0186(14) 0.0210(15) 0.0291(17) 0.0010(13) 0.0004(13) 0.0006(13) C14 0.0320(17) 0.0150(14) 0.0332(18) -0.0036(12) 0.0014(14) 0.0078(14) C15 0.0341(17) 0.0153(14) 0.0283(17) 0.0007(13) -0.0076(13) -0.0073(15) C16 0.0221(15) 0.0242(16) 0.0350(19) 0.0029(14) -0.0084(14) -0.0068(15) C17 0.0194(14) 0.0165(14) 0.0284(16) 0.0009(13) -0.0007(12) -0.0004(13) C18 0.0138(13) 0.0172(13) 0.0192(15) 0.0017(11) 0.0024(11) -0.0016(11) C19 0.0262(16) 0.0208(15) 0.0196(16) 0.0022(12) -0.0017(13) 0.0038(14) C20 0.0326(17) 0.0203(15) 0.0246(18) 0.0024(13) -0.0005(13) 0.0056(14) C21 0.0256(16) 0.0260(16) 0.0211(17) 0.0104(13) 0.0004(13) 0.0053(14) C22 0.0176(14) 0.0276(16) 0.0169(16) 0.0044(13) -0.0023(12) -0.0019(13) C23 0.0178(14) 0.0182(13) 0.0166(14) -0.0002(12) 0.0021(11) -0.0013(13) C24 0.0146(14) 0.0213(14) 0.0182(15) 0.0007(12) 0.0015(11) 0.0002(12) C29 0.0190(15) 0.0233(15) 0.0183(15) 0.0062(12) -0.0006(12) -0.0078(12) C28 0.0187(15) 0.0417(19) 0.0276(18) 0.0046(14) -0.0022(13) -0.0094(15) C27 0.0169(15) 0.056(2) 0.0320(19) 0.0004(17) 0.0072(13) -0.0021(17) C26 0.0208(16) 0.048(2) 0.0168(16) -0.0024(15) 0.0045(12) 0.0048(16) C25 0.0153(14) 0.0306(16) 0.0168(15) 0.0006(12) -0.0007(11) -0.0022(13) C30 0.0311(17) 0.0197(15) 0.0295(18) 0.0048(13) -0.0020(15) -0.0086(14) C31 0.046(2) 0.0289(18) 0.060(3) 0.0002(19) -0.004(2) -0.0162(16) C32 0.056(2) 0.036(2) 0.035(2) 0.0143(16) 0.0008(18) -0.0026(19) C33 0.0261(17) 0.050(2) 0.0265(18) -0.0114(16) 0.0024(14) 0.0143(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.893(3) . ? Ru1 C2 1.899(3) . ? Ru1 P1 2.3716(8) . ? Ru1 Ru2 2.9693(3) . ? Ru1 Ru3 2.9720(3) . ? Ru1 Ru4 3.0069(3) . ? Ru1 H112 1.65(3) . ? Ru1 H113 1.71(4) . ? Ru1 H114 1.70(3) . ? Ru2 C4 1.897(3) . ? Ru2 C5 1.901(3) . ? Ru2 C3 1.944(3) . ? Ru2 Ru3 2.7765(3) . ? Ru2 Ru4 2.9162(3) . ? Ru2 H112 1.66(3) . ? Ru2 H124 1.62(4) . ? Ru3 C8 1.898(3) . ? Ru3 C7 1.909(3) . ? Ru3 C6 1.914(3) . ? Ru3 Ru4 2.7830(3) . ? Ru3 H113 1.80(4) . ? Ru4 C11 1.890(3) . ? Ru4 C9 1.904(3) . ? Ru4 C10 1.932(3) . ? Ru4 H114 1.75(3) . ? Ru4 H124 1.70(4) . ? P1 C12 1.833(3) . ? P1 C18 1.834(3) . ? P1 C24 1.866(3) . ? O1 C1 1.147(4) . ? O3 C3 1.127(4) . ? O4 C4 1.138(4) . ? O5 C5 1.143(3) . ? O6 C6 1.144(4) . ? O7 C7 1.138(3) . ? O8 C8 1.143(4) . ? O9 C9 1.139(4) . ? O11 C11 1.149(4) . ? O10 C10 1.138(4) . ? O2 C2 1.143(4) . ? C12 C13 1.387(4) . ? C12 C17 1.404(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.391(4) . ? C14 H14 0.9500 . ? C15 C16 1.375(4) . ? C15 H15 0.9500 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.391(4) . ? C18 C23 1.395(4) . ? C19 C20 1.391(4) . ? C19 H19 0.9500 . ? C20 C21 1.376(4) . ? C20 H20 0.9500 . ? C21 C22 1.388(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.538(4) . ? C24 C29 1.546(4) . ? C24 H24 1.0000 . ? C29 C28 1.547(4) . ? C29 C30 1.553(4) . ? C29 H29 1.0000 . ? C28 C27 1.539(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C27 C26 1.509(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C26 C33 1.529(5) . ? C26 C25 1.538(4) . ? C26 H26 1.0000 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C30 C32 1.521(5) . ? C30 C31 1.530(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 C1 Ru1 C2 95.14(12) . . ? C1 Ru1 P1 91.23(9) . . ? C2 Ru1 P1 98.68(9) . . ? C1 Ru1 Ru2 99.33(9) . . ? C2 Ru1 Ru2 147.50(9) . . ? P1 Ru1 Ru2 109.873(18) . . ? C1 Ru1 Ru3 104.46(9) . . ? C2 Ru1 Ru3 92.54(9) . . ? P1 Ru1 Ru3 159.841(19) . . ? Ru2 Ru1 Ru3 55.722(7) . . ? C1 Ru1 Ru4 155.31(9) . . ? C2 Ru1 Ru4 99.66(9) . . ? P1 Ru1 Ru4 105.823(18) . . ? Ru2 Ru1 Ru4 58.411(7) . . ? Ru3 Ru1 Ru4 55.478(7) . . ? C1 Ru1 H112 89.0(10) . . ? C2 Ru1 H112 173.4(10) . . ? P1 Ru1 H112 86.3(10) . . ? Ru2 Ru1 H112 26.1(10) . . ? Ru3 Ru1 H112 81.5(10) . . ? Ru4 Ru1 H112 74.7(10) . . ? C1 Ru1 H113 75.4(11) . . ? C2 Ru1 H113 79.8(11) . . ? P1 Ru1 H113 166.2(11) . . ? Ru2 Ru1 H113 76.0(11) . . ? Ru3 Ru1 H113 33.1(11) . . ? Ru4 Ru1 H113 87.9(11) . . ? H112 Ru1 H113 96.4(15) . . ? C1 Ru1 H114 171.9(10) . . ? C2 Ru1 H114 87.6(10) . . ? P1 Ru1 H114 80.8(10) . . ? Ru2 Ru1 H114 82.2(10) . . ? Ru3 Ru1 H114 83.1(10) . . ? Ru4 Ru1 H114 30.0(10) . . ? H112 Ru1 H114 89.0(14) . . ? H113 Ru1 H114 112.7(15) . . ? C4 Ru2 C5 93.67(13) . . ? C4 Ru2 C3 94.75(14) . . ? C5 Ru2 C3 98.17(12) . . ? C4 Ru2 Ru3 90.03(10) . . ? C5 Ru2 Ru3 81.91(8) . . ? C3 Ru2 Ru3 175.19(10) . . ? C4 Ru2 Ru4 146.40(10) . . ? C5 Ru2 Ru4 93.08(8) . . ? C3 Ru2 Ru4 116.76(10) . . ? Ru3 Ru2 Ru4 58.471(8) . . ? C4 Ru2 Ru1 95.07(9) . . ? C5 Ru2 Ru1 142.96(8) . . ? C3 Ru2 Ru1 116.81(9) . . ? Ru3 Ru2 Ru1 62.188(8) . . ? Ru4 Ru2 Ru1 61.439(7) . . ? C4 Ru2 H112 91.0(10) . . ? C5 Ru2 H112 168.7(10) . . ? C3 Ru2 H112 91.7(10) . . ? Ru3 Ru2 H112 87.8(10) . . ? Ru4 Ru2 H112 77.4(10) . . ? Ru1 Ru2 H112 26.0(10) . . ? C4 Ru2 H124 170.8(13) . . ? C5 Ru2 H124 94.7(14) . . ? C3 Ru2 H124 87.8(13) . . ? Ru3 Ru2 H124 87.4(13) . . ? Ru4 Ru2 H124 29.1(13) . . ? Ru1 Ru2 H124 75.9(13) . . ? H112 Ru2 H124 80.0(16) . . ? C8 Ru3 C7 94.09(12) . . ? C8 Ru3 C6 96.92(14) . . ? C7 Ru3 C6 95.63(13) . . ? C8 Ru3 Ru2 158.01(10) . . ? C7 Ru3 Ru2 101.78(8) . . ? C6 Ru3 Ru2 96.56(10) . . ? C8 Ru3 Ru4 101.39(10) . . ? C7 Ru3 Ru4 92.04(9) . . ? C6 Ru3 Ru4 159.57(10) . . ? Ru2 Ru3 Ru4 63.274(8) . . ? C8 Ru3 Ru1 97.42(9) . . ? C7 Ru3 Ru1 154.02(9) . . ? C6 Ru3 Ru1 105.95(9) . . ? Ru2 Ru3 Ru1 62.090(8) . . ? Ru4 Ru3 Ru1 62.896(8) . . ? C8 Ru3 H113 85.2(10) . . ? C7 Ru3 H113 174.6(11) . . ? C6 Ru3 H113 79.2(11) . . ? Ru2 Ru3 H113 80.3(10) . . ? Ru4 Ru3 H113 93.3(11) . . ? Ru1 Ru3 H113 31.1(11) . . ? C11 Ru4 C9 93.21(14) . . ? C11 Ru4 C10 98.90(14) . . ? C9 Ru4 C10 94.75(12) . . ? C11 Ru4 Ru3 85.84(10) . . ? C9 Ru4 Ru3 91.11(9) . . ? C10 Ru4 Ru3 172.22(9) . . ? C11 Ru4 Ru2 143.35(10) . . ? C9 Ru4 Ru2 94.47(9) . . ? C10 Ru4 Ru2 116.05(9) . . ? Ru3 Ru4 Ru2 58.254(8) . . ? C11 Ru4 Ru1 98.18(10) . . ? C9 Ru4 Ru1 149.30(9) . . ? C10 Ru4 Ru1 111.35(9) . . ? Ru3 Ru4 Ru1 61.626(7) . . ? Ru2 Ru4 Ru1 60.150(7) . . ? C11 Ru4 H114 89.2(10) . . ? C9 Ru4 H114 177.5(10) . . ? C10 Ru4 H114 85.7(10) . . ? Ru3 Ru4 H114 88.2(10) . . ? Ru2 Ru4 H114 83.1(10) . . ? Ru1 Ru4 H114 29.1(10) . . ? C11 Ru4 H124 170.5(12) . . ? C9 Ru4 H124 91.3(13) . . ? C10 Ru4 H124 89.1(13) . . ? Ru3 Ru4 H124 85.7(13) . . ? Ru2 Ru4 H124 27.6(13) . . ? Ru1 Ru4 H124 73.9(12) . . ? H114 Ru4 H124 86.2(16) . . ? C12 P1 C18 103.38(12) . . ? C12 P1 C24 102.46(12) . . ? C18 P1 C24 105.98(13) . . ? C12 P1 Ru1 110.04(9) . . ? C18 P1 Ru1 114.79(9) . . ? C24 P1 Ru1 118.50(9) . . ? O1 C1 Ru1 177.6(3) . . ? O2 C2 Ru1 174.4(3) . . ? O3 C3 Ru2 173.3(3) . . ? O4 C4 Ru2 176.9(3) . . ? O5 C5 Ru2 176.9(3) . . ? O6 C6 Ru3 176.6(3) . . ? O7 C7 Ru3 177.0(3) . . ? O8 C8 Ru3 175.6(3) . . ? O9 C9 Ru4 177.1(3) . . ? O11 C11 Ru4 178.7(3) . . ? O10 C10 Ru4 177.2(3) . . ? C13 C12 C17 117.6(3) . . ? C13 C12 P1 123.3(2) . . ? C17 C12 P1 119.0(2) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.8(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C19 C18 C23 118.0(3) . . ? C19 C18 P1 120.2(2) . . ? C23 C18 P1 121.7(2) . . ? C20 C19 C18 121.1(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.5(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 120.9(3) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C25 C24 C29 114.1(2) . . ? C25 C24 P1 112.37(19) . . ? C29 C24 P1 117.21(19) . . ? C25 C24 H24 103.7 . . ? C29 C24 H24 103.7 . . ? P1 C24 H24 103.7 . . ? C24 C29 C28 108.2(2) . . ? C24 C29 C30 117.9(2) . . ? C28 C29 C30 114.8(2) . . ? C24 C29 H29 104.9 . . ? C28 C29 H29 104.9 . . ? C30 C29 H29 104.9 . . ? C27 C28 C29 115.4(2) . . ? C27 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? C27 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C26 C27 C28 112.8(3) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C26 C33 112.2(3) . . ? C27 C26 C25 109.6(3) . . ? C33 C26 C25 112.3(3) . . ? C27 C26 H26 107.5 . . ? C33 C26 H26 107.5 . . ? C25 C26 H26 107.5 . . ? C26 C25 C24 111.4(2) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C32 C30 C31 109.9(3) . . ? C32 C30 C29 118.0(3) . . ? C31 C30 C29 110.1(3) . . ? C32 C30 H30 106.0 . . ? C31 C30 H30 106.0 . . ? C29 C30 H30 106.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.360 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.077 #===END data_H4Ru4(CO)10(NMDPP)2_(2) _database_code_depnum_ccdc_archive 'CCDC 287843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H64 Cl2 O10 P2 Ru4' _chemical_formula_weight 1422.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3092(19) _cell_length_b 19.380(4) _cell_length_c 15.867(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.51(3) _cell_angle_gamma 90.00 _cell_volume 2862.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7075 _exptl_absorpt_correction_T_max 0.8861 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12823 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12823 _reflns_number_gt 12554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(11) _refine_ls_number_reflns 12823 _refine_ls_number_parameters 680 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0399 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Ru1 Ru 0.876796(16) 0.567167(7) 0.778725(9) 0.00994(4) Uani 1 1 d . . . Ru2 Ru 0.837605(16) 0.666390(8) 0.653231(9) 0.00991(4) Uani 1 1 d . . . Ru3 Ru 1.131954(16) 0.646047(8) 0.723840(10) 0.01207(4) Uani 1 1 d . . . Ru4 Ru 0.930682(17) 0.716182(8) 0.820828(9) 0.01174(4) Uani 1 1 d . . . P1 P 0.88969(5) 0.51023(3) 0.91168(3) 0.01034(10) Uani 1 1 d . . . P2 P 0.84637(5) 0.75134(3) 0.54536(3) 0.01123(10) Uani 1 1 d . . . Cl1 Cl 1.32707(8) 0.99973(3) 0.79064(4) 0.03658(15) Uani 1 1 d . . . Cl2 Cl 1.49434(7) 0.87257(4) 0.77472(4) 0.03629(15) Uani 1 1 d . . . O1 O 0.55763(17) 0.53708(9) 0.76331(11) 0.0272(4) Uani 1 1 d . . . O2 O 0.9484(2) 0.44866(9) 0.66270(10) 0.0298(4) Uani 1 1 d . . . O3 O 0.52765(16) 0.69238(9) 0.69815(10) 0.0258(4) Uani 1 1 d . . . O4 O 0.76922(19) 0.54478(8) 0.54107(10) 0.0260(4) Uani 1 1 d . . . O5 O 1.26294(17) 0.77815(8) 0.65518(10) 0.0228(3) Uani 1 1 d . . . O6 O 1.3030(2) 0.54770(11) 0.61148(12) 0.0420(5) Uani 1 1 d . . . O7 O 1.35059(18) 0.64582(10) 0.86710(11) 0.0328(4) Uani 1 1 d . . . O8 O 1.08594(19) 0.85321(8) 0.80014(10) 0.0259(4) Uani 1 1 d . . . O9 O 1.10372(18) 0.69664(9) 0.98283(10) 0.0296(4) Uani 1 1 d . . . O10 O 0.65085(19) 0.76642(9) 0.90123(11) 0.0320(4) Uani 1 1 d . . . C1 C 0.6781(2) 0.55071(11) 0.77012(13) 0.0170(4) Uani 1 1 d . . . C2 C 0.9180(2) 0.49298(11) 0.70704(13) 0.0187(5) Uani 1 1 d . . . C3 C 0.6442(2) 0.68108(10) 0.67885(13) 0.0165(4) Uani 1 1 d . . . C4 C 0.7977(2) 0.59085(11) 0.58343(13) 0.0161(4) Uani 1 1 d . . . C5 C 1.2131(2) 0.72862(11) 0.68039(13) 0.0175(4) Uani 1 1 d . . . C6 C 1.2391(2) 0.58303(12) 0.65281(15) 0.0226(5) Uani 1 1 d . . . C7 C 1.2661(2) 0.64541(12) 0.81426(14) 0.0209(5) Uani 1 1 d . . . C8 C 1.0275(2) 0.80189(12) 0.80528(13) 0.0184(4) Uani 1 1 d . . . C9 C 1.0371(2) 0.70233(11) 0.92239(14) 0.0194(5) Uani 1 1 d . . . C10 C 0.7552(2) 0.74953(11) 0.87130(14) 0.0197(5) Uani 1 1 d . . . C11 C 0.7994(2) 0.56418(10) 0.99044(12) 0.0122(4) Uani 1 1 d . . . C12 C 0.6515(2) 0.57543(11) 0.97975(13) 0.0158(4) Uani 1 1 d . . . H12 H 0.6007 0.5519 0.9363 0.019 Uiso 1 1 calc R . . C13 C 0.5785(2) 0.62066(11) 1.03208(14) 0.0188(4) Uani 1 1 d . . . H13 H 0.4784 0.6279 1.0241 0.023 Uiso 1 1 calc R . . C14 C 0.6505(2) 0.65509(11) 1.09546(13) 0.0203(5) Uani 1 1 d . . . H14 H 0.6002 0.6862 1.1308 0.024 Uiso 1 1 calc R . . C15 C 0.7968(2) 0.64438(11) 1.10770(13) 0.0187(4) Uani 1 1 d . . . H15 H 0.8464 0.6678 1.1518 0.022 Uiso 1 1 calc R . . C16 C 0.8705(2) 0.59923(11) 1.05512(13) 0.0147(4) Uani 1 1 d . . . H16 H 0.9706 0.5923 1.0635 0.018 Uiso 1 1 calc R . . C17 C 0.7887(2) 0.42911(10) 0.92170(13) 0.0138(4) Uani 1 1 d . . . C18 C 0.7514(2) 0.38986(11) 0.85081(13) 0.0167(4) Uani 1 1 d . . . H18 H 0.7770 0.4056 0.7963 0.020 Uiso 1 1 calc R . . C19 C 0.6772(2) 0.32814(12) 0.85940(15) 0.0227(5) Uani 1 1 d . . . H19 H 0.6530 0.3020 0.8107 0.027 Uiso 1 1 calc R . . C20 C 0.6382(2) 0.30434(12) 0.93799(15) 0.0229(5) Uani 1 1 d . . . H20 H 0.5884 0.2618 0.9435 0.028 Uiso 1 1 calc R . . C21 C 0.6726(2) 0.34331(11) 1.00905(14) 0.0196(5) Uani 1 1 d . . . H21 H 0.6460 0.3274 1.0634 0.023 Uiso 1 1 calc R . . C22 C 0.7454(2) 0.40513(11) 1.00079(14) 0.0165(4) Uani 1 1 d . . . H22 H 0.7665 0.4318 1.0496 0.020 Uiso 1 1 calc R . . C23 C 1.0698(2) 0.49490(10) 0.96020(12) 0.0122(4) Uani 1 1 d . . . H23 H 1.1052 0.5423 0.9740 0.015 Uiso 1 1 calc R . . C24 C 1.0702(2) 0.45768(11) 1.04596(13) 0.0152(4) Uani 1 1 d . . . H24A H 1.0443 0.4086 1.0374 0.018 Uiso 1 1 calc R . . H24B H 0.9967 0.4787 1.0826 0.018 Uiso 1 1 calc R . . C25 C 1.2180(2) 0.46196(12) 1.09007(13) 0.0187(4) Uani 1 1 d . . . H25 H 1.2159 0.4294 1.1390 0.022 Uiso 1 1 calc R . . C26 C 1.3369(2) 0.43737(13) 1.03149(14) 0.0212(5) Uani 1 1 d . . . H26A H 1.3298 0.3867 1.0252 0.025 Uiso 1 1 calc R . . H26B H 1.4312 0.4478 1.0579 0.025 Uiso 1 1 calc R . . C27 C 1.3310(2) 0.47064(12) 0.94369(13) 0.0184(4) Uani 1 1 d . . . H27A H 1.4034 0.4479 0.9077 0.022 Uiso 1 1 calc R . . H27B H 1.3586 0.5198 0.9491 0.022 Uiso 1 1 calc R . . C28 C 1.1835(2) 0.46655(11) 0.89881(13) 0.0144(4) Uani 1 1 d . . . H28 H 1.1886 0.5019 0.8530 0.017 Uiso 1 1 calc R . . C29 C 1.1483(2) 0.39841(12) 0.85251(13) 0.0190(5) Uani 1 1 d . . . H29 H 1.0525 0.4056 0.8249 0.023 Uiso 1 1 calc R . . C30 C 1.1348(4) 0.33213(13) 0.90366(18) 0.0399(7) Uani 1 1 d . . . H30A H 1.1119 0.2936 0.8658 0.060 Uiso 1 1 calc R . . H30B H 1.0581 0.3374 0.9451 0.060 Uiso 1 1 calc R . . H30C H 1.2259 0.3228 0.9330 0.060 Uiso 1 1 calc R . . C31 C 1.2542(3) 0.38704(17) 0.78103(18) 0.0411(7) Uani 1 1 d . . . H31A H 1.3495 0.3769 0.8047 0.062 Uiso 1 1 calc R . . H31B H 1.2593 0.4288 0.7463 0.062 Uiso 1 1 calc R . . H31C H 1.2219 0.3482 0.7462 0.062 Uiso 1 1 calc R . . C32 C 1.2479(3) 0.53445(13) 1.12568(15) 0.0246(5) Uani 1 1 d . . . H32A H 1.3389 0.5341 1.1571 0.037 Uiso 1 1 calc R . . H32B H 1.1699 0.5478 1.1634 0.037 Uiso 1 1 calc R . . H32C H 1.2538 0.5676 1.0792 0.037 Uiso 1 1 calc R . . C33 C 0.9098(2) 0.83604(10) 0.58280(13) 0.0142(4) Uani 1 1 d . . . C34 C 1.0388(2) 0.86599(11) 0.55839(14) 0.0177(4) Uani 1 1 d . . . H34 H 1.1002 0.8424 0.5205 0.021 Uiso 1 1 calc R . . C35 C 1.0779(3) 0.93070(12) 0.58963(15) 0.0239(5) Uani 1 1 d . . . H35 H 1.1656 0.9510 0.5723 0.029 Uiso 1 1 calc R . . C36 C 0.9915(3) 0.96549(12) 0.64516(16) 0.0265(5) Uani 1 1 d . . . H36 H 1.0192 1.0095 0.6660 0.032 Uiso 1 1 calc R . . C37 C 0.8632(3) 0.93562(12) 0.67039(15) 0.0238(5) Uani 1 1 d . . . H37 H 0.8024 0.9595 0.7084 0.029 Uiso 1 1 calc R . . C38 C 0.8236(2) 0.87143(11) 0.64045(14) 0.0188(4) Uani 1 1 d . . . H38 H 0.7369 0.8510 0.6592 0.023 Uiso 1 1 calc R . . C39 C 0.9592(2) 0.73304(10) 0.45243(13) 0.0141(4) Uani 1 1 d . . . C40 C 1.0180(2) 0.66756(12) 0.44204(13) 0.0170(4) Uani 1 1 d . . . H40 H 1.0067 0.6338 0.4849 0.020 Uiso 1 1 calc R . . C41 C 1.0934(2) 0.65119(12) 0.36933(14) 0.0230(5) Uani 1 1 d . . . H41 H 1.1327 0.6063 0.3628 0.028 Uiso 1 1 calc R . . C42 C 1.1114(2) 0.69981(13) 0.30662(14) 0.0249(5) Uani 1 1 d . . . H42 H 1.1608 0.6880 0.2565 0.030 Uiso 1 1 calc R . . C43 C 1.0573(2) 0.76541(13) 0.31704(14) 0.0222(5) Uani 1 1 d . . . H43 H 1.0709 0.7992 0.2744 0.027 Uiso 1 1 calc R . . C44 C 0.9829(2) 0.78236(12) 0.38979(13) 0.0174(4) Uani 1 1 d . . . H44 H 0.9478 0.8280 0.3970 0.021 Uiso 1 1 calc R . . C45 C 0.6664(2) 0.77794(10) 0.50258(12) 0.0135(4) Uani 1 1 d . . . H45 H 0.6177 0.7982 0.5528 0.016 Uiso 1 1 calc R . . C46 C 0.6714(2) 0.83877(11) 0.44010(13) 0.0162(4) Uani 1 1 d . . . H46A H 0.7373 0.8746 0.4624 0.019 Uiso 1 1 calc R . . H46B H 0.7101 0.8224 0.3858 0.019 Uiso 1 1 calc R . . C47 C 0.5225(2) 0.87089(12) 0.42486(15) 0.0232(5) Uani 1 1 d . . . H47 H 0.5319 0.9055 0.3785 0.028 Uiso 1 1 calc R . . C48 C 0.4190(3) 0.81486(13) 0.39426(16) 0.0283(6) Uani 1 1 d . . . H48A H 0.4480 0.7996 0.3374 0.034 Uiso 1 1 calc R . . H48B H 0.3212 0.8346 0.3896 0.034 Uiso 1 1 calc R . . C49 C 0.4152(2) 0.75188(13) 0.45339(15) 0.0234(5) Uani 1 1 d . . . H49A H 0.3538 0.7160 0.4271 0.028 Uiso 1 1 calc R . . H49B H 0.3692 0.7659 0.5067 0.028 Uiso 1 1 calc R . . C50 C 0.5628(2) 0.71943(12) 0.47468(12) 0.0164(4) Uani 1 1 d . . . H50 H 0.5460 0.6920 0.5270 0.020 Uiso 1 1 calc R . . C51 C 0.6188(2) 0.66645(12) 0.41005(13) 0.0205(4) Uani 1 1 d . . . H51 H 0.7148 0.6509 0.4315 0.025 Uiso 1 1 calc R . . C52 C 0.6412(3) 0.68969(14) 0.31960(15) 0.0341(6) Uani 1 1 d . . . H52A H 0.6795 0.6512 0.2866 0.051 Uiso 1 1 calc R . . H52B H 0.7093 0.7282 0.3187 0.051 Uiso 1 1 calc R . . H52C H 0.5492 0.7046 0.2952 0.051 Uiso 1 1 calc R . . C53 C 0.5215(3) 0.60212(13) 0.40983(17) 0.0307(6) Uani 1 1 d . . . H53A H 0.4291 0.6135 0.3832 0.046 Uiso 1 1 calc R . . H53B H 0.5057 0.5870 0.4679 0.046 Uiso 1 1 calc R . . H53C H 0.5680 0.5650 0.3782 0.046 Uiso 1 1 calc R . . C54 C 0.4683(3) 0.90871(14) 0.50252(17) 0.0319(6) Uani 1 1 d . . . H54A H 0.3813 0.9347 0.4878 0.048 Uiso 1 1 calc R . . H54B H 0.5425 0.9406 0.5229 0.048 Uiso 1 1 calc R . . H54C H 0.4463 0.8752 0.5468 0.048 Uiso 1 1 calc R . . C55 C 1.3752(3) 0.93047(13) 0.72467(15) 0.0286(5) Uani 1 1 d . . . H55A H 1.2873 0.9053 0.7072 0.034 Uiso 1 1 calc R . . H55B H 1.4209 0.9489 0.6733 0.034 Uiso 1 1 calc R . . H131 H 1.065(3) 0.5787(14) 0.7765(16) 0.027(7) Uiso 1 1 d . . . H141 H 0.842(3) 0.6401(15) 0.8402(17) 0.037(8) Uiso 1 1 d . . . H231 H 1.020(3) 0.6535(14) 0.6398(15) 0.023(6) Uiso 1 1 d . . . H341 H 0.868(3) 0.7292(14) 0.7226(16) 0.031(7) 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 Ru1 0.01030(8) 0.00912(7) 0.01039(8) 0.00111(6) 0.00066(6) 0.00030(6) Ru2 0.00972(8) 0.00988(7) 0.01013(7) 0.00104(6) 0.00007(5) 0.00022(6) Ru3 0.00894(8) 0.01365(8) 0.01363(8) 0.00239(6) 0.00037(5) 0.00018(6) Ru4 0.01403(8) 0.01012(7) 0.01106(8) -0.00027(6) 0.00004(6) -0.00063(6) P1 0.0098(2) 0.0100(2) 0.0113(2) 0.00055(19) 0.00089(18) -0.00009(19) P2 0.0115(2) 0.0112(2) 0.0110(2) 0.00086(19) 0.00086(18) 0.00056(19) Cl1 0.0567(4) 0.0258(3) 0.0274(3) -0.0046(2) 0.0085(3) -0.0025(3) Cl2 0.0297(3) 0.0478(4) 0.0312(3) -0.0058(3) -0.0038(3) 0.0069(3) O1 0.0160(9) 0.0340(10) 0.0314(9) 0.0063(7) -0.0039(7) -0.0058(7) O2 0.0485(11) 0.0194(8) 0.0214(9) -0.0055(7) 0.0046(7) 0.0092(8) O3 0.0132(8) 0.0369(9) 0.0274(9) 0.0060(7) 0.0033(6) 0.0047(7) O4 0.0363(10) 0.0173(8) 0.0242(9) -0.0053(7) -0.0052(7) -0.0029(7) O5 0.0193(8) 0.0199(8) 0.0293(9) 0.0071(7) 0.0026(6) -0.0033(7) O6 0.0410(11) 0.0436(12) 0.0416(11) -0.0090(9) 0.0132(9) 0.0180(9) O7 0.0225(9) 0.0440(11) 0.0316(10) 0.0084(8) -0.0131(7) -0.0032(8) O8 0.0335(10) 0.0165(8) 0.0276(9) 0.0016(7) 0.0009(7) -0.0106(7) O9 0.0323(10) 0.0365(10) 0.0199(8) 0.0075(7) -0.0109(7) -0.0123(8) O10 0.0280(10) 0.0302(9) 0.0380(10) -0.0046(8) 0.0111(8) 0.0075(8) C1 0.0213(12) 0.0162(10) 0.0135(10) 0.0038(8) -0.0015(8) 0.0005(9) C2 0.0229(12) 0.0178(11) 0.0153(11) 0.0057(9) 0.0005(8) -0.0003(9) C3 0.0206(12) 0.0156(11) 0.0132(10) 0.0038(8) 0.0000(8) 0.0003(8) C4 0.0153(10) 0.0167(10) 0.0163(10) 0.0041(8) -0.0004(8) 0.0012(8) C5 0.0130(10) 0.0226(12) 0.0170(10) 0.0003(8) -0.0002(8) 0.0026(9) C6 0.0191(12) 0.0231(12) 0.0257(12) 0.0048(9) 0.0013(9) 0.0017(9) C7 0.0183(11) 0.0212(11) 0.0234(12) 0.0069(9) 0.0034(9) -0.0012(9) C8 0.0207(11) 0.0209(11) 0.0137(10) 0.0001(8) 0.0005(8) 0.0044(9) C9 0.0222(12) 0.0145(11) 0.0214(11) 0.0035(8) 0.0039(9) -0.0044(9) C10 0.0263(12) 0.0133(10) 0.0193(11) -0.0007(8) 0.0001(9) 0.0011(9) C11 0.0136(10) 0.0114(9) 0.0118(9) 0.0032(8) 0.0033(7) -0.0001(8) C12 0.0156(10) 0.0166(10) 0.0152(10) -0.0014(8) 0.0024(8) -0.0007(8) C13 0.0151(11) 0.0226(11) 0.0190(11) 0.0008(9) 0.0038(8) 0.0050(9) C14 0.0268(12) 0.0173(11) 0.0170(11) -0.0003(9) 0.0046(8) 0.0060(9) C15 0.0229(11) 0.0185(10) 0.0146(10) -0.0028(8) 0.0002(8) 0.0003(9) C16 0.0146(10) 0.0141(10) 0.0153(10) 0.0028(8) 0.0001(8) -0.0017(8) C17 0.0125(10) 0.0113(9) 0.0178(10) 0.0025(8) 0.0020(8) 0.0008(8) C18 0.0185(11) 0.0158(10) 0.0158(11) -0.0003(8) 0.0002(8) -0.0019(8) C19 0.0259(13) 0.0193(11) 0.0229(12) -0.0036(9) -0.0044(9) -0.0061(9) C20 0.0224(12) 0.0163(11) 0.0301(13) 0.0022(9) -0.0004(9) -0.0081(9) C21 0.0182(11) 0.0195(11) 0.0212(11) 0.0068(9) 0.0047(9) -0.0030(9) C22 0.0156(11) 0.0166(10) 0.0174(11) -0.0001(8) 0.0024(8) -0.0004(8) C23 0.0134(10) 0.0110(9) 0.0120(10) 0.0016(7) -0.0005(7) 0.0002(8) C24 0.0155(10) 0.0150(10) 0.0150(10) 0.0024(8) -0.0004(8) 0.0024(8) C25 0.0179(11) 0.0241(11) 0.0140(10) 0.0061(9) -0.0024(8) 0.0028(9) C26 0.0148(11) 0.0274(12) 0.0213(12) 0.0030(9) -0.0044(8) 0.0072(9) C27 0.0123(11) 0.0228(11) 0.0199(11) 0.0023(9) 0.0013(8) 0.0037(9) C28 0.0133(10) 0.0167(10) 0.0133(10) 0.0045(8) 0.0022(8) 0.0044(8) C29 0.0186(11) 0.0217(11) 0.0167(11) -0.0046(9) -0.0015(8) 0.0071(9) C30 0.068(2) 0.0186(12) 0.0326(15) -0.0072(11) -0.0102(13) 0.0065(13) C31 0.0316(15) 0.0587(19) 0.0330(15) -0.0226(14) 0.0074(11) 0.0075(14) C32 0.0223(12) 0.0303(13) 0.0212(12) -0.0014(10) -0.0047(9) 0.0001(10) C33 0.0191(11) 0.0109(9) 0.0125(10) 0.0014(8) -0.0030(8) 0.0012(8) C34 0.0186(11) 0.0147(10) 0.0197(11) 0.0040(8) -0.0020(8) -0.0009(8) C35 0.0248(13) 0.0184(11) 0.0283(13) 0.0075(9) -0.0073(9) -0.0076(9) C36 0.0344(14) 0.0119(11) 0.0330(14) -0.0015(9) -0.0105(11) 0.0001(10) C37 0.0316(13) 0.0179(11) 0.0217(12) -0.0048(9) -0.0039(9) 0.0057(10) C38 0.0168(11) 0.0205(11) 0.0192(11) -0.0015(9) -0.0018(8) 0.0020(9) C39 0.0115(10) 0.0173(11) 0.0136(10) -0.0020(8) 0.0005(7) -0.0012(8) C40 0.0154(10) 0.0159(9) 0.0198(10) -0.0005(9) 0.0022(8) -0.0032(9) C41 0.0201(11) 0.0198(12) 0.0292(13) -0.0083(9) 0.0070(9) -0.0026(9) C42 0.0208(12) 0.0355(14) 0.0186(11) -0.0099(10) 0.0073(9) -0.0077(10) C43 0.0181(11) 0.0337(13) 0.0147(11) 0.0022(9) 0.0039(8) -0.0055(10) C44 0.0153(11) 0.0212(11) 0.0158(10) 0.0015(8) 0.0021(8) -0.0010(8) C45 0.0138(10) 0.0163(10) 0.0104(10) 0.0001(8) -0.0001(7) 0.0014(8) C46 0.0166(11) 0.0179(10) 0.0142(10) 0.0041(8) 0.0000(8) 0.0017(8) C47 0.0203(12) 0.0264(12) 0.0229(12) 0.0074(10) -0.0005(9) 0.0069(10) C48 0.0198(12) 0.0414(15) 0.0236(12) 0.0057(11) -0.0075(9) 0.0067(11) C49 0.0163(11) 0.0324(13) 0.0216(12) 0.0009(10) -0.0026(8) -0.0017(10) C50 0.0171(10) 0.0204(10) 0.0118(9) 0.0002(9) 0.0001(7) -0.0026(9) C51 0.0236(11) 0.0208(11) 0.0171(10) -0.0022(9) -0.0019(8) -0.0020(10) C52 0.0530(17) 0.0303(13) 0.0191(12) -0.0061(10) 0.0045(11) -0.0040(12) C53 0.0317(14) 0.0249(13) 0.0353(15) -0.0052(11) -0.0018(11) -0.0073(11) C54 0.0283(15) 0.0279(13) 0.0397(15) 0.0021(11) 0.0054(11) 0.0129(11) C55 0.0423(15) 0.0236(12) 0.0198(12) -0.0012(9) 0.0016(10) -0.0031(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.875(2) . ? Ru1 C1 1.881(2) . ? Ru1 P1 2.3828(7) . ? Ru1 Ru2 2.7898(5) . ? Ru1 Ru3 2.9621(6) . ? Ru1 Ru4 3.0053(6) . ? Ru2 C3 1.871(2) . ? Ru2 C4 1.871(2) . ? Ru2 P2 2.3768(6) . ? Ru2 Ru4 2.9517(7) . ? Ru2 Ru3 2.9774(8) . ? Ru3 C7 1.894(2) . ? Ru3 C5 1.902(2) . ? Ru3 C6 1.943(2) . ? Ru3 Ru4 2.7888(7) . ? Ru4 C9 1.903(2) . ? Ru4 C8 1.907(2) . ? Ru4 C10 1.937(2) . ? P1 C11 1.839(2) . ? P1 C17 1.840(2) . ? P1 C23 1.862(2) . ? P2 C33 1.841(2) . ? P2 C39 1.852(2) . ? P2 C45 1.875(2) . ? Cl1 C55 1.763(3) . ? Cl2 C55 1.762(3) . ? O1 C1 1.156(3) . ? O2 C2 1.147(3) . ? O3 C3 1.151(3) . ? O4 C4 1.147(3) . ? O5 C5 1.140(3) . ? O6 C6 1.122(3) . ? O7 C7 1.144(3) . ? O8 C8 1.137(3) . ? O9 C9 1.143(3) . ? O10 C10 1.133(3) . ? C11 C16 1.393(3) . ? C11 C12 1.403(3) . ? C12 C13 1.389(3) . ? C13 C14 1.376(3) . ? C14 C15 1.390(3) . ? C15 C16 1.394(3) . ? C17 C18 1.399(3) . ? C17 C22 1.401(3) . ? C18 C19 1.388(3) . ? C19 C20 1.381(3) . ? C20 C21 1.392(3) . ? C21 C22 1.383(3) . ? C23 C24 1.540(3) . ? C23 C28 1.546(3) . ? C24 C25 1.540(3) . ? C25 C26 1.528(3) . ? C25 C32 1.539(3) . ? C26 C27 1.536(3) . ? C27 C28 1.544(3) . ? C28 C29 1.545(3) . ? C29 C30 1.525(4) . ? C29 C31 1.525(3) . ? C33 C34 1.392(3) . ? C33 C38 1.401(3) . ? C34 C35 1.396(3) . ? C35 C36 1.375(4) . ? C36 C37 1.389(4) . ? C37 C38 1.380(3) . ? C39 C40 1.393(3) . ? C39 C44 1.398(3) . ? C40 C41 1.392(3) . ? C41 C42 1.382(3) . ? C42 C43 1.378(3) . ? C43 C44 1.391(3) . ? C45 C46 1.541(3) . ? C45 C50 1.551(3) . ? C46 C47 1.537(3) . ? C47 C54 1.523(4) . ? C47 C48 1.528(3) . ? C48 C49 1.540(3) . ? C49 C50 1.545(3) . ? C50 C51 1.545(3) . ? C51 C52 1.520(3) . ? C51 C53 1.541(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru1 C1 91.86(10) . . ? C2 Ru1 P1 99.96(7) . . ? C1 Ru1 P1 91.58(7) . . ? C2 Ru1 Ru2 96.99(7) . . ? C1 Ru1 Ru2 86.72(7) . . ? P1 Ru1 Ru2 163.008(14) . . ? C2 Ru1 Ru3 92.77(7) . . ? C1 Ru1 Ru3 148.97(6) . . ? P1 Ru1 Ru3 117.71(3) . . ? Ru2 Ru1 Ru3 62.262(19) . . ? C2 Ru1 Ru4 146.82(7) . . ? C1 Ru1 Ru4 109.95(7) . . ? P1 Ru1 Ru4 103.957(18) . . ? Ru2 Ru1 Ru4 61.107(15) . . ? Ru3 Ru1 Ru4 55.718(11) . . ? C3 Ru2 C4 93.52(9) . . ? C3 Ru2 P2 95.19(7) . . ? C4 Ru2 P2 97.10(7) . . ? C3 Ru2 Ru1 94.00(6) . . ? C4 Ru2 Ru1 84.67(6) . . ? P2 Ru2 Ru1 170.517(14) . . ? C3 Ru2 Ru4 91.71(7) . . ? C4 Ru2 Ru4 147.59(6) . . ? P2 Ru2 Ru4 114.246(19) . . ? Ru1 Ru2 Ru4 63.052(15) . . ? C3 Ru2 Ru3 145.34(6) . . ? C4 Ru2 Ru3 107.24(7) . . ? P2 Ru2 Ru3 108.99(2) . . ? Ru1 Ru2 Ru3 61.709(18) . . ? Ru4 Ru2 Ru3 56.11(2) . . ? C7 Ru3 C5 91.07(9) . . ? C7 Ru3 C6 95.56(10) . . ? C5 Ru3 C6 96.38(9) . . ? C7 Ru3 Ru4 91.55(7) . . ? C5 Ru3 Ru4 93.49(7) . . ? C6 Ru3 Ru4 167.71(7) . . ? C7 Ru3 Ru1 107.40(7) . . ? C5 Ru3 Ru1 149.66(6) . . ? C6 Ru3 Ru1 105.25(7) . . ? Ru4 Ru3 Ru1 62.926(18) . . ? C7 Ru3 Ru2 152.19(7) . . ? C5 Ru3 Ru2 96.86(6) . . ? C6 Ru3 Ru2 109.89(7) . . ? Ru4 Ru3 Ru2 61.479(15) . . ? Ru1 Ru3 Ru2 56.029(12) . . ? C9 Ru4 C8 89.38(9) . . ? C9 Ru4 C10 97.56(10) . . ? C8 Ru4 C10 99.47(9) . . ? C9 Ru4 Ru3 92.94(7) . . ? C8 Ru4 Ru3 91.85(7) . . ? C10 Ru4 Ru3 164.60(7) . . ? C9 Ru4 Ru2 149.68(7) . . ? C8 Ru4 Ru2 107.67(6) . . ? C10 Ru4 Ru2 103.86(7) . . ? Ru3 Ru4 Ru2 62.408(18) . . ? C9 Ru4 Ru1 97.89(6) . . ? C8 Ru4 Ru1 152.42(6) . . ? C10 Ru4 Ru1 105.83(7) . . ? Ru3 Ru4 Ru1 61.356(10) . . ? Ru2 Ru4 Ru1 55.841(5) . . ? C11 P1 C17 100.95(9) . . ? C11 P1 C23 103.01(9) . . ? C17 P1 C23 106.68(9) . . ? C11 P1 Ru1 108.58(7) . . ? C17 P1 Ru1 116.78(7) . . ? C23 P1 Ru1 118.55(7) . . ? C33 P2 C39 104.18(9) . . ? C33 P2 C45 98.91(9) . . ? C39 P2 C45 106.00(9) . . ? C33 P2 Ru2 113.46(7) . . ? C39 P2 Ru2 117.65(7) . . ? C45 P2 Ru2 114.51(7) . . ? O1 C1 Ru1 176.3(2) . . ? O2 C2 Ru1 177.4(2) . . ? O3 C3 Ru2 176.29(19) . . ? O4 C4 Ru2 178.07(19) . . ? O5 C5 Ru3 179.1(2) . . ? O6 C6 Ru3 178.5(2) . . ? O7 C7 Ru3 177.7(2) . . ? O8 C8 Ru4 176.68(19) . . ? O9 C9 Ru4 177.11(19) . . ? O10 C10 Ru4 177.3(2) . . ? C16 C11 C12 118.21(18) . . ? C16 C11 P1 124.11(15) . . ? C12 C11 P1 117.42(15) . . ? C13 C12 C11 120.7(2) . . ? C14 C13 C12 120.4(2) . . ? C13 C14 C15 120.0(2) . . ? C14 C15 C16 119.8(2) . . ? C11 C16 C15 120.9(2) . . ? C18 C17 C22 117.96(19) . . ? C18 C17 P1 121.24(16) . . ? C22 C17 P1 120.80(16) . . ? C19 C18 C17 120.6(2) . . ? C20 C19 C18 120.7(2) . . ? C19 C20 C21 119.3(2) . . ? C22 C21 C20 120.2(2) . . ? C21 C22 C17 121.1(2) . . ? C24 C23 C28 113.19(16) . . ? C24 C23 P1 115.80(14) . . ? C28 C23 P1 114.53(14) . . ? C23 C24 C25 111.82(17) . . ? C26 C25 C32 112.24(19) . . ? C26 C25 C24 110.84(18) . . ? C32 C25 C24 111.95(18) . . ? C25 C26 C27 113.63(18) . . ? C26 C27 C28 114.92(18) . . ? C27 C28 C29 116.58(17) . . ? C27 C28 C23 107.61(17) . . ? C29 C28 C23 117.39(17) . . ? C30 C29 C31 109.3(2) . . ? C30 C29 C28 119.01(18) . . ? C31 C29 C28 109.9(2) . . ? C34 C33 C38 118.6(2) . . ? C34 C33 P2 123.85(16) . . ? C38 C33 P2 117.57(16) . . ? C33 C34 C35 119.9(2) . . ? C36 C35 C34 121.1(2) . . ? C35 C36 C37 119.3(2) . . ? C38 C37 C36 120.2(2) . . ? C37 C38 C33 120.9(2) . . ? C40 C39 C44 118.29(19) . . ? C40 C39 P2 119.68(15) . . ? C44 C39 P2 121.97(16) . . ? C41 C40 C39 120.5(2) . . ? C42 C41 C40 120.4(2) . . ? C43 C42 C41 119.7(2) . . ? C42 C43 C44 120.2(2) . . ? C43 C44 C39 120.8(2) . . ? C46 C45 C50 113.45(17) . . ? C46 C45 P2 114.28(14) . . ? C50 C45 P2 117.01(14) . . ? C47 C46 C45 112.25(18) . . ? C54 C47 C48 112.8(2) . . ? C54 C47 C46 111.85(19) . . ? C48 C47 C46 109.12(19) . . ? C47 C48 C49 112.79(19) . . ? C48 C49 C50 115.51(19) . . ? C49 C50 C51 115.48(18) . . ? C49 C50 C45 108.32(18) . . ? C51 C50 C45 117.54(17) . . ? C52 C51 C53 108.84(19) . . ? C52 C51 C50 118.7(2) . . ? C53 C51 C50 109.71(18) . . ? Cl2 C55 Cl1 112.31(14) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.362 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.055 #===END data_H4Ru4(CO)10(DUPHOS)_(3) _database_code_depnum_ccdc_archive 'CCDC 287844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 O10 P2 Ru4' _chemical_formula_weight 994.76 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.651(2) _cell_length_b 15.180(3) _cell_length_c 38.529(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6814(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 1.884 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13756 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.44 _reflns_number_total 13756 _reflns_number_gt 11257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.2044P] 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 0.00013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 13756 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.27997(4) 0.75625(3) 0.791281(13) 0.01398(12) Uani 1 1 d . . . Ru2 Ru 0.21895(5) 0.64902(3) 0.728739(14) 0.01660(13) Uani 1 1 d . . . Ru3 Ru 0.05341(4) 0.67665(3) 0.780644(15) 0.01677(13) Uani 1 1 d . . . Ru4 Ru 0.10681(4) 0.81885(3) 0.737733(15) 0.01695(13) Uani 1 1 d . . . P1 P 0.28739(15) 0.85333(11) 0.83726(4) 0.0168(4) Uani 1 1 d . . . P2 P 0.47020(14) 0.79604(10) 0.78402(5) 0.0161(4) Uani 1 1 d . . . C1 C 0.3228(5) 0.6630(4) 0.81904(18) 0.0197(16) Uani 1 1 d . . . C2 C 0.2300(6) 0.5419(4) 0.75321(19) 0.0250(17) Uani 1 1 d . . . C3 C 0.3470(6) 0.6387(4) 0.69704(19) 0.0242(17) Uani 1 1 d . . . C4 C 0.1133(6) 0.6045(4) 0.69561(19) 0.0240(17) Uani 1 1 d . . . C5 C 0.0707(6) 0.5768(5) 0.8114(2) 0.0280(18) Uani 1 1 d . . . C6 C -0.0570(6) 0.7326(4) 0.80899(19) 0.0225(17) Uani 1 1 d . . . C7 C -0.0541(6) 0.6190(4) 0.75193(19) 0.0244(17) Uani 1 1 d . . . C8 C 0.1568(6) 0.9152(5) 0.70854(18) 0.0241(17) Uani 1 1 d . . . C9 C -0.0198(6) 0.7853(4) 0.71000(19) 0.0250(17) Uani 1 1 d . . . C10 C 0.0088(5) 0.8827(4) 0.76774(18) 0.0210(16) Uani 1 1 d . . . Ru1B Ru 0.43167(4) 0.97827(3) 0.547811(14) 0.01479(13) Uani 1 1 d . . . Ru2B Ru 0.67281(4) 0.98065(4) 0.523718(15) 0.01816(13) Uani 1 1 d . . . Ru3B Ru 0.51156(5) 0.92310(3) 0.475395(14) 0.01662(13) Uani 1 1 d . . . Ru4B Ru 0.52180(4) 1.10841(3) 0.497608(15) 0.01754(13) Uani 1 1 d . . . P1B P 0.23516(14) 0.99278(11) 0.55365(5) 0.0170(4) Uani 1 1 d . . . P2B P 0.41064(15) 0.85399(11) 0.58158(5) 0.0176(4) Uani 1 1 d . . . O1 O 0.3448(4) 0.6017(3) 0.83632(13) 0.0331(13) Uani 1 1 d . . . O2 O 0.2430(4) 0.4749(3) 0.76711(13) 0.0350(13) Uani 1 1 d . . . O3 O 0.4202(4) 0.6313(3) 0.67806(13) 0.0399(15) Uani 1 1 d . . . O4 O 0.0549(5) 0.5810(3) 0.67310(13) 0.0382(14) Uani 1 1 d . . . O5 O 0.0812(4) 0.5193(3) 0.82963(14) 0.0362(14) Uani 1 1 d . . . O6 O -0.1235(4) 0.7658(3) 0.82668(13) 0.0287(13) Uani 1 1 d . . . O7 O -0.1229(4) 0.5823(3) 0.73603(14) 0.0333(13) Uani 1 1 d . . . O8 O 0.1816(4) 0.9708(3) 0.69043(13) 0.0319(13) Uani 1 1 d . . . O9 O -0.0967(4) 0.7679(3) 0.69276(13) 0.0352(14) Uani 1 1 d . . . O10 O -0.0511(4) 0.9228(3) 0.78479(13) 0.0321(13) Uani 1 1 d . . . C31 C 0.4379(6) 0.8710(4) 0.84831(17) 0.0194(16) Uani 1 1 d . . . C32 C 0.4744(6) 0.9104(4) 0.87905(18) 0.0252(17) Uani 1 1 d . . . H32 H 0.4207 0.9231 0.8962 0.030 Uiso 1 1 calc R . . C33 C 0.5893(6) 0.9314(5) 0.8847(2) 0.033(2) Uani 1 1 d . . . H33 H 0.6127 0.9559 0.9056 0.040 Uiso 1 1 calc R . . C34 C 0.6676(7) 0.9152(5) 0.85880(19) 0.0336(19) Uani 1 1 d . . . H34 H 0.7442 0.9303 0.8621 0.040 Uiso 1 1 calc R . . C35 C 0.6346(5) 0.8772(4) 0.82813(19) 0.0262(18) Uani 1 1 d . . . H35 H 0.6883 0.8673 0.8107 0.031 Uiso 1 1 calc R . . C36 C 0.5191(5) 0.8532(4) 0.82303(16) 0.0148(15) Uani 1 1 d . . . C11B C 0.1883(6) 1.0923(4) 0.57732(18) 0.0229(17) Uani 1 1 d . . . H11B H 0.2468 1.1373 0.5730 0.028 Uiso 1 1 calc R . . C12B C 0.0799(6) 1.1234(4) 0.5589(2) 0.033(2) Uani 1 1 d . . . H12A H 0.0136 1.0916 0.5676 0.039 Uiso 1 1 calc R . . H12B H 0.0681 1.1858 0.5630 0.039 Uiso 1 1 calc R . . C13B C 0.0956(6) 1.1061(4) 0.5206(2) 0.0305(19) Uani 1 1 d . . . H13A H 0.1549 1.1440 0.5111 0.037 Uiso 1 1 calc R . . H13B H 0.0247 1.1170 0.5081 0.037 Uiso 1 1 calc R . . C14B C 0.1311(5) 1.0079(4) 0.51720(18) 0.0204(17) Uani 1 1 d . . . H14B H 0.0632 0.9722 0.5225 0.025 Uiso 1 1 calc R . . C15B C 0.1767(6) 1.0844(5) 0.61690(18) 0.036(2) Uani 1 1 d . . . H15A H 0.1593 1.1412 0.6265 0.054 Uiso 1 1 calc R . . H15B H 0.2476 1.0632 0.6265 0.054 Uiso 1 1 calc R . . H15C H 0.1161 1.0440 0.6224 0.054 Uiso 1 1 calc R . . C16B C 0.1713(6) 0.9819(5) 0.48127(18) 0.0300(18) Uani 1 1 d . . . H16A H 0.1131 0.9967 0.4646 0.045 Uiso 1 1 calc R . . H16B H 0.1854 0.9197 0.4806 0.045 Uiso 1 1 calc R . . H16C H 0.2407 1.0130 0.4758 0.045 Uiso 1 1 calc R . . O1B O 0.4670(4) 1.1090(3) 0.60553(12) 0.0309(13) Uani 1 1 d . . . O2B O 0.7857(5) 0.8081(3) 0.54343(13) 0.0432(15) Uani 1 1 d . . . O3B O 0.7869(5) 1.0664(4) 0.58604(15) 0.068(2) Uani 1 1 d . . . O4B O 0.8632(4) 1.0295(3) 0.47283(13) 0.0321(13) Uani 1 1 d . . . O5B O 0.6103(5) 1.2287(3) 0.55450(14) 0.0422(15) Uani 1 1 d . . . O6B O 0.3397(4) 1.2438(3) 0.47678(14) 0.0397(14) Uani 1 1 d . . . O7B O 0.6995(4) 1.1714(3) 0.44491(14) 0.0405(15) Uani 1 1 d . . . O8B O 0.3268(4) 0.8621(3) 0.42453(12) 0.0311(13) Uani 1 1 d . . . O9B O 0.6010(4) 0.7366(3) 0.48534(12) 0.0292(13) Uani 1 1 d . . . O10B O 0.6791(4) 0.9553(3) 0.41673(13) 0.0321(13) Uani 1 1 d . . . C1B C 0.4532(6) 1.0560(4) 0.58399(18) 0.0214(17) Uani 1 1 d . . . C2B C 0.7427(6) 0.8710(5) 0.53503(18) 0.0288(19) Uani 1 1 d . . . C3B C 0.7421(6) 1.0385(5) 0.5617(2) 0.035(2) Uani 1 1 d . . . C4B C 0.7883(6) 1.0132(4) 0.49129(17) 0.0217(16) Uani 1 1 d . . . C5B C 0.5810(6) 1.1811(5) 0.53338(19) 0.0293(19) Uani 1 1 d . . . C6B C 0.4059(6) 1.1916(4) 0.48288(19) 0.0246(18) Uani 1 1 d . . . C7B C 0.6355(6) 1.1463(4) 0.46529(19) 0.0271(18) Uani 1 1 d . . . C8B C 0.3904(6) 0.8863(4) 0.44375(18) 0.0218(17) Uani 1 1 d . . . C9B C 0.5677(6) 0.8072(4) 0.48283(17) 0.0207(16) Uani 1 1 d . . . C10B C 0.6181(6) 0.9426(4) 0.43982(19) 0.0249(18) Uani 1 1 d . . . C31B C 0.1790(6) 0.9001(4) 0.57846(16) 0.0197(16) Uani 1 1 d . . . C32B C 0.0631(6) 0.8901(4) 0.58558(18) 0.0262(17) Uani 1 1 d . . . H32B H 0.0110 0.9310 0.5769 0.031 Uiso 1 1 calc R . . C33B C 0.0234(6) 0.8197(4) 0.60550(19) 0.0312(19) Uani 1 1 d . . . H33B H -0.0545 0.8141 0.6104 0.037 Uiso 1 1 calc R . . C34B C 0.1010(6) 0.7582(5) 0.61800(19) 0.034(2) Uani 1 1 d . . . H34B H 0.0747 0.7100 0.6306 0.041 Uiso 1 1 calc R . . C35B C 0.2176(7) 0.7677(5) 0.61186(18) 0.0310(19) Uani 1 1 d . . . H35B H 0.2691 0.7272 0.6210 0.037 Uiso 1 1 calc R . . C36B C 0.2585(5) 0.8390(4) 0.59169(17) 0.0204(16) Uani 1 1 d . . . C11 C 0.2092(6) 0.8333(5) 0.87882(17) 0.0263(17) Uani 1 1 d . . . H11 H 0.2653 0.8370 0.8977 0.032 Uiso 1 1 calc R . . C12 C 0.1313(9) 0.9147(6) 0.8812(3) 0.071(3) Uani 1 1 d . . . H12C H 0.0579 0.9009 0.8706 0.085 Uiso 1 1 calc R . . H12D H 0.1174 0.9279 0.9055 0.085 Uiso 1 1 calc R . . C13 C 0.1768(9) 0.9903(6) 0.8650(2) 0.066(3) Uani 1 1 d . . . H13C H 0.2342 1.0168 0.8799 0.079 Uiso 1 1 calc R . . H13D H 0.1162 1.0330 0.8613 0.079 Uiso 1 1 calc R . . C14 C 0.2301(6) 0.9665(4) 0.83092(18) 0.0293(18) Uani 1 1 d . . . H14 H 0.1686 0.9633 0.8136 0.035 Uiso 1 1 calc R . . C15 C 0.1484(8) 0.7489(5) 0.8823(2) 0.058(3) Uani 1 1 d . . . H15D H 0.1060 0.7484 0.9037 0.087 Uiso 1 1 calc R . . H15E H 0.2030 0.7016 0.8824 0.087 Uiso 1 1 calc R . . H15F H 0.0965 0.7417 0.8632 0.087 Uiso 1 1 calc R . . C16 C 0.3179(7) 1.0345(5) 0.8183(2) 0.062(3) Uani 1 1 d . . . H16D H 0.2801 1.0899 0.8145 0.094 Uiso 1 1 calc R . . H16E H 0.3518 1.0146 0.7970 0.094 Uiso 1 1 calc R . . H16F H 0.3766 1.0417 0.8356 0.094 Uiso 1 1 calc R . . C21B C 0.4903(6) 0.8380(4) 0.62305(16) 0.0193(15) Uani 1 1 d . . . H21B H 0.4335 0.8210 0.6406 0.023 Uiso 1 1 calc R . . C22B C 0.5667(6) 0.7586(4) 0.61720(17) 0.0270(18) Uani 1 1 d . . . H22A H 0.6397 0.7774 0.6076 0.032 Uiso 1 1 calc R . . H22B H 0.5814 0.7294 0.6392 0.032 Uiso 1 1 calc R . . C23B C 0.5095(6) 0.6955(4) 0.59264(17) 0.0213(16) Uani 1 1 d . . . H23A H 0.4477 0.6646 0.6043 0.026 Uiso 1 1 calc R . . H23B H 0.5645 0.6524 0.5843 0.026 Uiso 1 1 calc R . . C24B C 0.4627(5) 0.7489(4) 0.56254(17) 0.0219(16) Uani 1 1 d . . . H24B H 0.5294 0.7645 0.5483 0.026 Uiso 1 1 calc R . . C25B C 0.5527(6) 0.9184(5) 0.63703(18) 0.036(2) Uani 1 1 d . . . H25A H 0.5999 0.9015 0.6563 0.054 Uiso 1 1 calc R . . H25B H 0.4976 0.9615 0.6445 0.054 Uiso 1 1 calc R . . H25C H 0.6000 0.9431 0.6191 0.054 Uiso 1 1 calc R . . C26B C 0.3789(6) 0.7022(4) 0.53818(18) 0.0300(19) Uani 1 1 d . . . H26A H 0.4167 0.6533 0.5273 0.045 Uiso 1 1 calc R . . H26B H 0.3531 0.7428 0.5207 0.045 Uiso 1 1 calc R . . H26C H 0.3142 0.6813 0.5512 0.045 Uiso 1 1 calc R . . C21 C 0.5710(5) 0.7034(4) 0.77670(17) 0.0191(16) Uani 1 1 d . . . H21 H 0.5270 0.6582 0.7643 0.023 Uiso 1 1 calc R . . C22 C 0.6601(6) 0.7367(4) 0.75104(17) 0.0252(17) Uani 1 1 d . . . H22C H 0.6939 0.6877 0.7385 0.030 Uiso 1 1 calc R . . H22D H 0.7207 0.7679 0.7631 0.030 Uiso 1 1 calc R . . C23 C 0.5981(5) 0.7990(4) 0.72563(17) 0.0224(17) Uani 1 1 d . . . H23C H 0.5487 0.7658 0.7102 0.027 Uiso 1 1 calc R . . H23D H 0.6535 0.8312 0.7117 0.027 Uiso 1 1 calc R . . C24 C 0.5264(5) 0.8633(4) 0.74777(17) 0.0193(16) Uani 1 1 d . . . H24 H 0.5796 0.9064 0.7577 0.023 Uiso 1 1 calc R . . C25 C 0.6207(6) 0.6579(4) 0.80863(19) 0.0315(19) Uani 1 1 d . . . H25D H 0.6715 0.6116 0.8014 0.047 Uiso 1 1 calc R . . H25E H 0.5594 0.6335 0.8222 0.047 Uiso 1 1 calc R . . H25F H 0.6624 0.7000 0.8223 0.047 Uiso 1 1 calc R . . C26 C 0.4391(5) 0.9143(4) 0.72635(18) 0.0345(19) Uani 1 1 d . . . H26D H 0.4771 0.9611 0.7142 0.052 Uiso 1 1 calc R . . H26E H 0.3817 0.9386 0.7414 0.052 Uiso 1 1 calc R . . H26F H 0.4034 0.8753 0.7099 0.052 Uiso 1 1 calc R . . H112 H 0.3207 0.7317 0.7440 0.050 Uiso 1 1 d R . . H113 H 0.1357 0.7444 0.8092 0.050 Uiso 1 1 d R . . H114 H 0.2269 0.8483 0.7650 0.050 Uiso 1 1 d R . . H124 H 0.1974 0.7541 0.7047 0.050 Uiso 1 1 d R . . H212 H 0.5807 0.9432 0.5587 0.050 Uiso 1 1 d R . . H213 H 0.4052 0.9128 0.5094 0.050 Uiso 1 1 d R . . H214 H 0.3912 1.0677 0.5167 0.050 Uiso 1 1 d R . . H234 H 0.4620 1.0390 0.4647 0.050 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0125(3) 0.0144(3) 0.0151(3) 0.0010(2) -0.0014(2) 0.0003(2) Ru2 0.0163(3) 0.0149(3) 0.0187(3) -0.0015(2) -0.0014(3) 0.0003(2) Ru3 0.0137(3) 0.0160(3) 0.0206(3) 0.0016(3) -0.0003(2) -0.0008(2) Ru4 0.0171(3) 0.0151(3) 0.0187(3) 0.0015(3) -0.0029(3) 0.0007(2) P1 0.0147(9) 0.0215(9) 0.0141(10) -0.0003(8) -0.0003(8) 0.0020(8) P2 0.0127(9) 0.0175(9) 0.0180(10) 0.0009(8) 0.0001(8) 0.0004(7) C1 0.009(3) 0.024(4) 0.026(4) 0.001(3) 0.001(3) -0.002(3) C2 0.015(4) 0.028(4) 0.033(5) -0.010(4) 0.000(3) 0.002(3) C3 0.036(5) 0.014(4) 0.022(4) 0.003(3) -0.009(4) -0.003(4) C4 0.028(4) 0.015(4) 0.029(5) 0.013(3) 0.003(4) -0.003(3) C5 0.008(4) 0.035(5) 0.041(5) -0.010(4) 0.000(4) -0.006(4) C6 0.012(4) 0.021(4) 0.035(5) 0.008(4) -0.008(3) -0.012(3) C7 0.020(4) 0.022(4) 0.031(5) 0.005(3) 0.001(4) 0.004(3) C8 0.022(4) 0.030(4) 0.020(4) 0.000(4) -0.009(3) 0.005(4) C9 0.025(4) 0.023(4) 0.026(4) 0.000(3) 0.004(4) -0.001(3) C10 0.016(4) 0.017(4) 0.030(4) 0.005(3) -0.008(3) 0.001(3) Ru1B 0.0154(3) 0.0154(3) 0.0135(3) 0.0006(2) 0.0006(2) -0.0012(2) Ru2B 0.0144(3) 0.0216(3) 0.0185(3) 0.0014(3) 0.0007(3) -0.0009(3) Ru3B 0.0187(3) 0.0172(3) 0.0139(3) 0.0001(2) 0.0018(3) -0.0003(2) Ru4B 0.0180(3) 0.0157(3) 0.0190(3) 0.0024(2) 0.0020(3) -0.0017(2) P1B 0.0161(9) 0.0155(9) 0.0195(10) 0.0019(8) 0.0014(8) -0.0003(8) P2B 0.0203(10) 0.0164(9) 0.0160(10) 0.0037(8) 0.0004(8) -0.0009(8) O1 0.026(3) 0.034(3) 0.040(3) 0.025(3) -0.007(3) -0.002(3) O2 0.029(3) 0.028(3) 0.048(4) 0.012(3) 0.011(3) 0.013(3) O3 0.037(3) 0.045(3) 0.037(4) -0.010(3) 0.019(3) 0.002(3) O4 0.049(4) 0.033(3) 0.033(3) 0.004(3) -0.024(3) -0.013(3) O5 0.035(3) 0.029(3) 0.045(4) 0.021(3) 0.000(3) 0.005(3) O6 0.021(3) 0.024(3) 0.041(3) 0.001(2) 0.014(3) 0.007(2) O7 0.029(3) 0.024(3) 0.046(4) -0.007(3) -0.009(3) -0.002(2) O8 0.033(3) 0.026(3) 0.037(3) 0.015(3) -0.001(3) -0.006(3) O9 0.023(3) 0.045(3) 0.038(3) 0.001(3) -0.016(3) -0.004(3) O10 0.031(3) 0.021(3) 0.044(4) 0.001(3) 0.010(3) 0.005(2) C31 0.020(4) 0.018(4) 0.020(4) 0.002(3) -0.011(3) -0.003(3) C32 0.025(4) 0.031(4) 0.020(4) -0.005(3) 0.005(3) -0.002(4) C33 0.037(5) 0.034(5) 0.028(5) -0.015(4) -0.019(4) 0.000(4) C34 0.028(4) 0.039(5) 0.033(5) -0.006(4) -0.011(4) 0.001(4) C35 0.011(4) 0.028(4) 0.040(5) -0.014(4) -0.006(3) -0.002(3) C36 0.014(3) 0.015(3) 0.015(4) -0.001(3) -0.002(3) 0.003(3) C11B 0.023(4) 0.017(4) 0.028(4) 0.000(3) 0.008(3) 0.001(3) C12B 0.027(4) 0.019(4) 0.053(6) 0.001(4) -0.004(4) 0.000(4) C13B 0.020(4) 0.021(4) 0.050(5) 0.011(4) 0.005(4) -0.001(3) C14B 0.010(3) 0.024(4) 0.027(4) -0.001(3) 0.002(3) -0.006(3) C15B 0.033(5) 0.036(5) 0.040(5) -0.014(4) 0.012(4) 0.006(4) C16B 0.020(4) 0.044(5) 0.027(5) 0.008(4) -0.001(4) 0.002(4) O1B 0.037(3) 0.030(3) 0.025(3) -0.006(2) 0.000(3) -0.004(3) O2B 0.052(4) 0.042(3) 0.035(4) 0.016(3) 0.006(3) 0.029(3) O3B 0.053(4) 0.109(6) 0.043(4) -0.032(4) 0.001(3) -0.039(4) O4B 0.026(3) 0.043(3) 0.027(3) 0.009(3) 0.009(3) -0.007(3) O5B 0.048(4) 0.040(3) 0.038(4) -0.015(3) 0.000(3) -0.019(3) O6B 0.031(3) 0.031(3) 0.057(4) 0.012(3) 0.004(3) 0.013(3) O7B 0.040(3) 0.035(3) 0.047(4) 0.019(3) 0.022(3) 0.002(3) O8B 0.037(3) 0.034(3) 0.023(3) 0.002(2) -0.012(3) -0.008(3) O9B 0.036(3) 0.021(3) 0.031(3) 0.001(2) 0.010(2) 0.008(2) O10B 0.034(3) 0.032(3) 0.031(3) 0.000(3) 0.008(3) -0.004(3) C1B 0.018(4) 0.024(4) 0.021(4) 0.007(3) -0.004(3) 0.004(3) C2B 0.024(4) 0.038(5) 0.024(4) 0.008(4) 0.009(3) -0.003(4) C3B 0.033(5) 0.041(5) 0.030(5) -0.009(4) 0.019(4) -0.005(4) C4B 0.037(4) 0.014(3) 0.015(4) -0.001(3) -0.010(4) 0.003(4) C5B 0.033(5) 0.025(4) 0.030(5) 0.005(4) 0.014(4) -0.007(4) C6B 0.015(4) 0.023(4) 0.035(5) -0.004(4) 0.009(3) -0.009(3) C7B 0.033(4) 0.015(4) 0.033(5) 0.002(3) 0.001(4) 0.004(4) C8B 0.022(4) 0.017(4) 0.026(5) 0.008(3) 0.001(3) 0.001(3) C9B 0.020(4) 0.029(4) 0.013(4) -0.004(3) 0.003(3) -0.004(4) C10B 0.020(4) 0.024(4) 0.031(5) -0.003(4) -0.005(4) 0.002(3) C31B 0.025(4) 0.022(4) 0.012(4) 0.003(3) 0.000(3) 0.006(3) C32B 0.019(4) 0.030(4) 0.029(5) 0.004(4) 0.001(3) -0.003(4) C33B 0.020(4) 0.030(4) 0.044(5) 0.004(4) 0.008(4) -0.002(4) C34B 0.032(5) 0.028(4) 0.042(5) 0.013(4) 0.009(4) -0.012(4) C35B 0.032(4) 0.031(4) 0.030(5) 0.010(4) 0.004(4) 0.006(4) C36B 0.024(4) 0.020(4) 0.017(4) 0.002(3) 0.005(3) 0.000(3) C11 0.021(4) 0.039(5) 0.019(4) -0.002(4) -0.003(3) 0.008(4) C12 0.087(8) 0.055(7) 0.071(8) -0.017(6) 0.061(6) -0.001(6) C13 0.104(8) 0.059(7) 0.035(6) -0.006(5) -0.008(6) 0.054(6) C14 0.041(5) 0.024(4) 0.024(4) 0.000(3) -0.010(4) 0.006(4) C15 0.089(8) 0.055(6) 0.031(5) 0.002(5) 0.026(5) -0.031(6) C16 0.066(7) 0.025(5) 0.096(8) 0.005(5) -0.044(6) 0.008(5) C21B 0.022(4) 0.024(4) 0.012(4) -0.002(3) -0.001(3) -0.004(3) C22B 0.027(4) 0.033(4) 0.021(4) 0.010(4) -0.008(3) 0.002(4) C23B 0.025(4) 0.017(4) 0.021(4) 0.003(3) 0.002(3) 0.008(3) C24B 0.019(4) 0.024(4) 0.022(4) 0.005(3) -0.005(3) -0.001(3) C25B 0.041(5) 0.043(5) 0.023(4) 0.007(4) -0.015(4) -0.010(4) C26B 0.032(4) 0.024(4) 0.034(5) -0.007(3) -0.006(4) -0.008(3) C21 0.020(4) 0.015(3) 0.022(4) -0.003(3) -0.003(3) 0.006(3) C22 0.017(4) 0.037(4) 0.022(4) -0.002(4) 0.000(3) 0.010(3) C23 0.010(3) 0.039(4) 0.019(4) -0.002(3) -0.001(3) -0.004(3) C24 0.017(4) 0.024(4) 0.018(4) 0.001(3) -0.002(3) -0.002(3) C25 0.025(4) 0.023(4) 0.047(5) 0.002(4) 0.000(4) 0.003(4) C26 0.028(4) 0.044(5) 0.031(5) 0.016(4) 0.002(4) -0.006(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 Ru1 C1 1.843(7) . ? Ru1 P1 2.3059(18) . ? Ru1 P2 2.3142(18) . ? Ru1 Ru3 2.9319(9) . ? Ru1 Ru2 2.9936(8) . ? Ru1 Ru4 3.0380(8) . ? Ru1 H112 1.9191 . ? Ru1 H113 1.8259 . ? Ru1 H114 1.8331 . ? Ru2 C2 1.883(7) . ? Ru2 C4 1.898(8) . ? Ru2 C3 1.935(8) . ? Ru2 Ru3 2.8099(9) . ? Ru2 Ru4 2.9109(9) . ? Ru2 H112 1.8243 . ? Ru2 H124 1.8607 . ? Ru3 C7 1.886(7) . ? Ru3 C6 1.889(8) . ? Ru3 C5 1.935(8) . ? Ru3 Ru4 2.7893(8) . ? Ru3 H113 1.7855 . ? Ru4 C9 1.891(8) . ? Ru4 C10 1.892(7) . ? Ru4 C8 1.935(7) . ? Ru4 H114 1.8059 . ? Ru4 H124 1.9227 . ? P1 C31 1.824(7) . ? P1 C14 1.859(7) . ? P1 C11 1.867(7) . ? P2 C36 1.826(6) . ? P2 C24 1.850(6) . ? P2 C21 1.853(6) . ? C1 O1 1.173(7) . ? C2 O2 1.159(7) . ? C3 O3 1.129(8) . ? C4 O4 1.158(8) . ? C5 O5 1.126(8) . ? C6 O6 1.148(8) . ? C7 O7 1.152(7) . ? C8 O8 1.132(7) . ? C9 O9 1.146(8) . ? C10 O10 1.136(7) . ? Ru1B C1B 1.844(7) . ? Ru1B P2B 2.3048(18) . ? Ru1B P1B 2.3111(18) . ? Ru1B Ru4B 2.9575(8) . ? Ru1B Ru2B 2.9591(9) . ? Ru1B Ru3B 3.0582(9) . ? Ru1B H212 1.8644 . ? Ru1B H213 1.8088 . ? Ru1B H214 1.8719 . ? Ru2B C3B 1.888(8) . ? Ru2B C4B 1.901(8) . ? Ru2B C2B 1.904(8) . ? Ru2B Ru3B 2.7856(8) . ? Ru2B Ru4B 2.8051(8) . ? Ru2B H212 1.8134 . ? Ru3B C10B 1.873(8) . ? Ru3B C9B 1.899(7) . ? Ru3B C8B 1.947(7) . ? Ru3B Ru4B 2.9427(9) . ? Ru3B H213 1.8102 . ? Ru3B H234 1.8967 . ? Ru4B C5B 1.896(8) . ? Ru4B C7B 1.907(7) . ? Ru4B C6B 1.934(7) . ? Ru4B H214 1.7991 . ? Ru4B H234 1.7887 . ? P1B C31B 1.822(7) . ? P1B C11B 1.847(7) . ? P1B C14B 1.869(7) . ? P2B C36B 1.829(7) . ? P2B C24B 1.858(7) . ? P2B C21B 1.864(6) . ? C31 C36 1.385(9) . ? C31 C32 1.394(8) . ? C32 C33 1.393(9) . ? C32 H32 0.9300 . ? C33 C34 1.373(10) . ? C33 H33 0.9300 . ? C34 C35 1.370(9) . ? C34 H34 0.9300 . ? C35 C36 1.408(8) . ? C35 H35 0.9300 . ? C11B C12B 1.523(9) . ? C11B C15B 1.536(9) . ? C11B H11B 0.9800 . ? C12B C13B 1.514(10) . ? C12B H12A 0.9700 . ? C12B H12B 0.9700 . ? C13B C14B 1.552(8) . ? C13B H13A 0.9700 . ? C13B H13B 0.9700 . ? C14B C16B 1.513(8) . ? C14B H14B 0.9800 . ? C15B H15A 0.9600 . ? C15B H15B 0.9600 . ? C15B H15C 0.9600 . ? C16B H16A 0.9600 . ? C16B H16B 0.9600 . ? C16B H16C 0.9600 . ? O1B C1B 1.167(7) . ? O2B C2B 1.127(8) . ? O3B C3B 1.154(8) . ? O4B C4B 1.153(8) . ? O5B C5B 1.140(8) . ? O6B C6B 1.130(7) . ? O7B C7B 1.148(8) . ? O8B C8B 1.110(7) . ? O9B C9B 1.144(7) . ? O10B C10B 1.155(8) . ? C31B C32B 1.386(9) . ? C31B C36B 1.407(8) . ? C32B C33B 1.395(9) . ? C32B H32B 0.9300 . ? C33B C34B 1.387(9) . ? C33B H33B 0.9300 . ? C34B C35B 1.386(10) . ? C34B H34B 0.9300 . ? C35B C36B 1.414(9) . ? C35B H35B 0.9300 . ? C11 C15 1.470(10) . ? C11 C12 1.536(10) . ? C11 H11 0.9800 . ? C12 C13 1.409(11) . ? C12 H12C 0.9700 . ? C12 H12D 0.9700 . ? C13 C14 1.496(10) . ? C13 H13C 0.9700 . ? C13 H13D 0.9700 . ? C14 C16 1.532(10) . ? C14 H14 0.9800 . ? C15 H15D 0.9600 . ? C15 H15E 0.9600 . ? C15 H15F 0.9600 . ? C16 H16D 0.9600 . ? C16 H16E 0.9600 . ? C16 H16F 0.9600 . ? C21B C22B 1.516(9) . ? C21B C25B 1.520(9) . ? C21B H21B 0.9800 . ? C22B C23B 1.502(9) . ? C22B H22A 0.9700 . ? C22B H22B 0.9700 . ? C23B C24B 1.516(8) . ? C23B H23A 0.9700 . ? C23B H23B 0.9700 . ? C24B C26B 1.529(8) . ? C24B H24B 0.9800 . ? C25B H25A 0.9600 . ? C25B H25B 0.9600 . ? C25B H25C 0.9600 . ? C26B H26A 0.9600 . ? C26B H26B 0.9600 . ? C26B H26C 0.9600 . ? C21 C22 1.519(9) . ? C21 C25 1.525(9) . ? C21 H21 0.9800 . ? C22 C23 1.542(8) . ? C22 H22C 0.9700 . ? C22 H22D 0.9700 . ? C23 C24 1.542(8) . ? C23 H23C 0.9700 . ? C23 H23D 0.9700 . ? C24 C26 1.521(8) . ? C24 H24 0.9800 . ? C25 H25D 0.9600 . ? C25 H25E 0.9600 . ? C25 H25F 0.9600 . ? C26 H26D 0.9600 . ? C26 H26E 0.9600 . ? C26 H26F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P1 92.0(2) . . ? C1 Ru1 P2 90.6(2) . . ? P1 Ru1 P2 83.70(6) . . ? C1 Ru1 Ru3 90.5(2) . . ? P1 Ru1 Ru3 113.86(5) . . ? P2 Ru1 Ru3 162.35(5) . . ? C1 Ru1 Ru2 96.5(2) . . ? P1 Ru1 Ru2 167.11(5) . . ? P2 Ru1 Ru2 105.78(5) . . ? Ru3 Ru1 Ru2 56.603(18) . . ? C1 Ru1 Ru4 144.5(2) . . ? P1 Ru1 Ru4 110.29(5) . . ? P2 Ru1 Ru4 118.18(5) . . ? Ru3 Ru1 Ru4 55.675(19) . . ? Ru2 Ru1 Ru4 57.71(2) . . ? C1 Ru1 H112 109.6 . . ? P1 Ru1 H112 147.6 . . ? P2 Ru1 H112 72.5 . . ? Ru3 Ru1 H112 90.6 . . ? Ru2 Ru1 H112 35.8 . . ? Ru4 Ru1 H112 65.2 . . ? C1 Ru1 H113 87.4 . . ? P1 Ru1 H113 78.9 . . ? P2 Ru1 H113 162.4 . . ? Ru3 Ru1 H113 35.3 . . ? Ru2 Ru1 H113 91.8 . . ? Ru4 Ru1 H113 71.1 . . ? H112 Ru1 H113 124.6 . . ? C1 Ru1 H114 175.8 . . ? P1 Ru1 H114 87.1 . . ? P2 Ru1 H114 93.3 . . ? Ru3 Ru1 H114 86.2 . . ? Ru2 Ru1 H114 83.7 . . ? Ru4 Ru1 H114 33.1 . . ? H112 Ru1 H114 73.0 . . ? H113 Ru1 H114 88.5 . . ? C2 Ru2 C4 94.2(3) . . ? C2 Ru2 C3 101.1(3) . . ? C4 Ru2 C3 92.7(3) . . ? C2 Ru2 Ru3 79.6(2) . . ? C4 Ru2 Ru3 95.0(2) . . ? C3 Ru2 Ru3 172.2(2) . . ? C2 Ru2 Ru4 137.3(2) . . ? C4 Ru2 Ru4 96.0(2) . . ? C3 Ru2 Ru4 119.6(2) . . ? Ru3 Ru2 Ru4 58.331(19) . . ? C2 Ru2 Ru1 92.9(2) . . ? C4 Ru2 Ru1 152.8(2) . . ? C3 Ru2 Ru1 111.7(2) . . ? Ru3 Ru2 Ru1 60.59(2) . . ? Ru4 Ru2 Ru1 61.912(19) . . ? C2 Ru2 H112 112.8 . . ? C4 Ru2 H112 152.1 . . ? C3 Ru2 H112 76.0 . . ? Ru3 Ru2 H112 96.5 . . ? Ru4 Ru2 H112 69.1 . . ? Ru1 Ru2 H112 38.0 . . ? C2 Ru2 H124 176.2 . . ? C4 Ru2 H124 83.3 . . ? C3 Ru2 H124 81.9 . . ? Ru3 Ru2 H124 97.7 . . ? Ru4 Ru2 H124 40.5 . . ? Ru1 Ru2 H124 88.1 . . ? H112 Ru2 H124 70.0 . . ? C7 Ru3 C6 95.5(3) . . ? C7 Ru3 C5 93.7(3) . . ? C6 Ru3 C5 94.0(3) . . ? C7 Ru3 Ru4 99.2(2) . . ? C6 Ru3 Ru4 98.4(2) . . ? C5 Ru3 Ru4 161.1(2) . . ? C7 Ru3 Ru2 88.2(2) . . ? C6 Ru3 Ru2 161.1(2) . . ? C5 Ru3 Ru2 104.3(2) . . ? Ru4 Ru3 Ru2 62.65(2) . . ? C7 Ru3 Ru1 150.6(2) . . ? C6 Ru3 Ru1 110.31(19) . . ? C5 Ru3 Ru1 98.2(2) . . ? Ru4 Ru3 Ru1 64.091(19) . . ? Ru2 Ru3 Ru1 62.81(2) . . ? C7 Ru3 H113 170.1 . . ? C6 Ru3 H113 75.6 . . ? C5 Ru3 H113 91.0 . . ? Ru4 Ru3 H113 78.5 . . ? Ru2 Ru3 H113 99.0 . . ? Ru1 Ru3 H113 36.2 . . ? C9 Ru4 C10 90.7(3) . . ? C9 Ru4 C8 96.3(3) . . ? C10 Ru4 C8 98.6(3) . . ? C9 Ru4 Ru3 87.3(2) . . ? C10 Ru4 Ru3 84.25(19) . . ? C8 Ru4 Ru3 175.4(2) . . ? C9 Ru4 Ru2 92.5(2) . . ? C10 Ru4 Ru2 142.88(19) . . ? C8 Ru4 Ru2 117.7(2) . . ? Ru3 Ru4 Ru2 59.02(2) . . ? C9 Ru4 Ru1 144.8(2) . . ? C10 Ru4 Ru1 98.41(19) . . ? C8 Ru4 Ru1 115.54(19) . . ? Ru3 Ru4 Ru1 60.23(2) . . ? Ru2 Ru4 Ru1 60.381(18) . . ? C9 Ru4 H114 178.4 . . ? C10 Ru4 H114 89.1 . . ? C8 Ru4 H114 85.3 . . ? Ru3 Ru4 H114 91.1 . . ? Ru2 Ru4 H114 86.6 . . ? Ru1 Ru4 H114 33.7 . . ? C9 Ru4 H124 85.2 . . ? C10 Ru4 H124 175.7 . . ? C8 Ru4 H124 80.6 . . ? Ru3 Ru4 H124 96.8 . . ? Ru2 Ru4 H124 38.9 . . ? Ru1 Ru4 H124 85.7 . . ? H114 Ru4 H124 94.9 . . ? C31 P1 C14 103.9(3) . . ? C31 P1 C11 107.0(3) . . ? C14 P1 C11 95.0(3) . . ? C31 P1 Ru1 108.0(2) . . ? C14 P1 Ru1 118.4(2) . . ? C11 P1 Ru1 122.5(2) . . ? C36 P2 C24 104.4(3) . . ? C36 P2 C21 106.7(3) . . ? C24 P2 C21 94.6(3) . . ? C36 P2 Ru1 108.9(2) . . ? C24 P2 Ru1 125.1(2) . . ? C21 P2 Ru1 115.3(2) . . ? O1 C1 Ru1 176.6(6) . . ? O2 C2 Ru2 175.8(6) . . ? O3 C3 Ru2 178.4(7) . . ? O4 C4 Ru2 173.7(6) . . ? O5 C5 Ru3 179.2(7) . . ? O6 C6 Ru3 178.9(6) . . ? O7 C7 Ru3 176.2(6) . . ? O8 C8 Ru4 176.6(6) . . ? O9 C9 Ru4 177.6(6) . . ? O10 C10 Ru4 177.6(6) . . ? C1B Ru1B P2B 96.4(2) . . ? C1B Ru1B P1B 90.0(2) . . ? P2B Ru1B P1B 85.28(6) . . ? C1B Ru1B Ru4B 91.1(2) . . ? P2B Ru1B Ru4B 162.50(5) . . ? P1B Ru1B Ru4B 110.60(5) . . ? C1B Ru1B Ru2B 95.8(2) . . ? P2B Ru1B Ru2B 106.74(5) . . ? P1B Ru1B Ru2B 165.92(5) . . ? Ru4B Ru1B Ru2B 56.601(18) . . ? C1B Ru1B Ru3B 145.5(2) . . ? P2B Ru1B Ru3B 108.86(5) . . ? P1B Ru1B Ru3B 114.61(5) . . ? Ru4B Ru1B Ru3B 58.54(2) . . ? Ru2B Ru1B Ru3B 55.122(17) . . ? C1B Ru1B H212 83.5 . . ? P2B Ru1B H212 74.8 . . ? P1B Ru1B H212 158.2 . . ? Ru4B Ru1B H212 90.4 . . ? Ru2B Ru1B H212 35.8 . . ? Ru3B Ru1B H212 81.0 . . ? C1B Ru1B H213 173.4 . . ? P2B Ru1B H213 89.7 . . ? P1B Ru1B H213 87.9 . . ? Ru4B Ru1B H213 83.8 . . ? Ru2B Ru1B H213 84.9 . . ? Ru3B Ru1B H213 32.3 . . ? H212 Ru1B H213 100.7 . . ? C1B Ru1B H214 93.1 . . ? P2B Ru1B H214 158.2 . . ? P1B Ru1B H214 75.2 . . ? Ru4B Ru1B H214 35.5 . . ? Ru2B Ru1B H214 91.7 . . ? Ru3B Ru1B H214 72.0 . . ? H212 Ru1B H214 125.9 . . ? H213 Ru1B H214 80.3 . . ? C3B Ru2B C4B 94.9(3) . . ? C3B Ru2B C2B 92.6(3) . . ? C4B Ru2B C2B 94.3(3) . . ? C3B Ru2B Ru3B 162.3(2) . . ? C4B Ru2B Ru3B 96.86(19) . . ? C2B Ru2B Ru3B 99.6(2) . . ? C3B Ru2B Ru4B 103.0(2) . . ? C4B Ru2B Ru4B 91.62(19) . . ? C2B Ru2B Ru4B 162.7(2) . . ? Ru3B Ru2B Ru4B 63.52(2) . . ? C3B Ru2B Ru1B 99.7(2) . . ? C4B Ru2B Ru1B 151.77(19) . . ? C2B Ru2B Ru1B 108.9(2) . . ? Ru3B Ru2B Ru1B 64.25(2) . . ? Ru4B Ru2B Ru1B 61.67(2) . . ? C3B Ru2B H212 79.8 . . ? C4B Ru2B H212 171.2 . . ? C2B Ru2B H212 79.0 . . ? Ru3B Ru2B H212 89.9 . . ? Ru4B Ru2B H212 96.5 . . ? Ru1B Ru2B H212 37.0 . . ? C10B Ru3B C9B 91.6(3) . . ? C10B Ru3B C8B 93.9(3) . . ? C9B Ru3B C8B 94.5(3) . . ? C10B Ru3B Ru2B 89.6(2) . . ? C9B Ru3B Ru2B 87.6(2) . . ? C8B Ru3B Ru2B 175.9(2) . . ? C10B Ru3B Ru4B 92.0(2) . . ? C9B Ru3B Ru4B 145.9(2) . . ? C8B Ru3B Ru4B 119.06(19) . . ? Ru2B Ru3B Ru4B 58.563(19) . . ? C10B Ru3B Ru1B 145.7(2) . . ? C9B Ru3B Ru1B 102.8(2) . . ? C8B Ru3B Ru1B 115.4(2) . . ? Ru2B Ru3B Ru1B 60.63(2) . . ? Ru4B Ru3B Ru1B 59.018(17) . . ? C10B Ru3B H213 175.7 . . ? C9B Ru3B H213 92.7 . . ? C8B Ru3B H213 86.1 . . ? Ru2B Ru3B H213 90.3 . . ? Ru4B Ru3B H213 84.2 . . ? Ru1B Ru3B H213 32.3 . . ? C10B Ru3B H234 84.1 . . ? C9B Ru3B H234 175.6 . . ? C8B Ru3B H234 84.8 . . ? Ru2B Ru3B H234 93.4 . . ? Ru4B Ru3B H234 35.8 . . ? Ru1B Ru3B H234 81.4 . . ? H213 Ru3B H234 91.6 . . ? C5B Ru4B C7B 92.7(3) . . ? C5B Ru4B C6B 95.0(3) . . ? C7B Ru4B C6B 95.5(3) . . ? C5B Ru4B Ru2B 85.0(2) . . ? C7B Ru4B Ru2B 90.4(2) . . ? C6B Ru4B Ru2B 174.0(2) . . ? C5B Ru4B Ru3B 141.5(2) . . ? C7B Ru4B Ru3B 97.3(2) . . ? C6B Ru4B Ru3B 120.7(2) . . ? Ru2B Ru4B Ru3B 57.92(2) . . ? C5B Ru4B Ru1B 92.4(2) . . ? C7B Ru4B Ru1B 151.1(2) . . ? C6B Ru4B Ru1B 112.33(19) . . ? Ru2B Ru4B Ru1B 61.73(2) . . ? Ru3B Ru4B Ru1B 62.44(2) . . ? C5B Ru4B H214 102.2 . . ? C7B Ru4B H214 163.3 . . ? C6B Ru4B H214 75.7 . . ? Ru2B Ru4B H214 98.4 . . ? Ru3B Ru4B H214 75.9 . . ? Ru1B Ru4B H214 37.2 . . ? C5B Ru4B H234 178.1 . . ? C7B Ru4B H234 89.2 . . ? C6B Ru4B H234 84.5 . . ? Ru2B Ru4B H234 95.2 . . ? Ru3B Ru4B H234 38.3 . . ? Ru1B Ru4B H234 86.1 . . ? H214 Ru4B H234 75.9 . . ? C31B P1B C11B 105.4(3) . . ? C31B P1B C14B 104.8(3) . . ? C11B P1B C14B 94.5(3) . . ? C31B P1B Ru1B 109.5(2) . . ? C11B P1B Ru1B 114.8(2) . . ? C14B P1B Ru1B 125.5(2) . . ? C36B P2B C24B 107.1(3) . . ? C36B P2B C21B 106.5(3) . . ? C24B P2B C21B 93.7(3) . . ? C36B P2B Ru1B 109.0(2) . . ? C24B P2B Ru1B 116.4(2) . . ? C21B P2B Ru1B 122.5(2) . . ? C36 C31 C32 118.2(6) . . ? C36 C31 P1 117.6(5) . . ? C32 C31 P1 123.7(5) . . ? C33 C32 C31 121.6(7) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C34 C33 C32 119.0(7) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C33 121.0(7) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.9(7) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 120.3(6) . . ? C31 C36 P2 117.3(5) . . ? C35 C36 P2 122.4(5) . . ? C12B C11B C15B 114.4(6) . . ? C12B C11B P1B 105.6(5) . . ? C15B C11B P1B 116.9(5) . . ? C12B C11B H11B 106.4 . . ? C15B C11B H11B 106.4 . . ? P1B C11B H11B 106.4 . . ? C13B C12B C11B 107.4(6) . . ? C13B C12B H12A 110.2 . . ? C11B C12B H12A 110.2 . . ? C13B C12B H12B 110.2 . . ? C11B C12B H12B 110.2 . . ? H12A C12B H12B 108.5 . . ? C12B C13B C14B 106.3(6) . . ? C12B C13B H13A 110.5 . . ? C14B C13B H13A 110.5 . . ? C12B C13B H13B 110.5 . . ? C14B C13B H13B 110.5 . . ? H13A C13B H13B 108.7 . . ? C16B C14B C13B 114.1(6) . . ? C16B C14B P1B 117.1(4) . . ? C13B C14B P1B 103.2(5) . . ? C16B C14B H14B 107.3 . . ? C13B C14B H14B 107.3 . . ? P1B C14B H14B 107.3 . . ? C11B C15B H15A 109.5 . . ? C11B C15B H15B 109.5 . . ? H15A C15B H15B 109.5 . . ? C11B C15B H15C 109.5 . . ? H15A C15B H15C 109.5 . . ? H15B C15B H15C 109.5 . . ? C14B C16B H16A 109.5 . . ? C14B C16B H16B 109.5 . . ? H16A C16B H16B 109.5 . . ? C14B C16B H16C 109.5 . . ? H16A C16B H16C 109.5 . . ? H16B C16B H16C 109.5 . . ? O1B C1B Ru1B 176.2(6) . . ? O2B C2B Ru2B 176.2(7) . . ? O3B C3B Ru2B 173.9(8) . . ? O4B C4B Ru2B 175.5(6) . . ? O5B C5B Ru4B 175.2(7) . . ? O6B C6B Ru4B 174.3(7) . . ? O7B C7B Ru4B 176.4(6) . . ? O8B C8B Ru3B 175.2(6) . . ? O9B C9B Ru3B 176.2(6) . . ? O10B C10B Ru3B 176.5(6) . . ? C32B C31B C36B 119.8(6) . . ? C32B C31B P1B 122.6(5) . . ? C36B C31B P1B 117.5(5) . . ? C31B C32B C33B 121.1(7) . . ? C31B C32B H32B 119.5 . . ? C33B C32B H32B 119.5 . . ? C34B C33B C32B 119.4(7) . . ? C34B C33B H33B 120.3 . . ? C32B C33B H33B 120.3 . . ? C35B C34B C33B 120.6(7) . . ? C35B C34B H34B 119.7 . . ? C33B C34B H34B 119.7 . . ? C34B C35B C36B 120.3(7) . . ? C34B C35B H35B 119.9 . . ? C36B C35B H35B 119.9 . . ? C31B C36B C35B 118.8(6) . . ? C31B C36B P2B 118.6(5) . . ? C35B C36B P2B 122.6(5) . . ? C15 C11 C12 114.2(7) . . ? C15 C11 P1 117.1(5) . . ? C12 C11 P1 102.0(5) . . ? C15 C11 H11 107.7 . . ? C12 C11 H11 107.7 . . ? P1 C11 H11 107.7 . . ? C13 C12 C11 113.9(7) . . ? C13 C12 H12C 108.8 . . ? C11 C12 H12C 108.8 . . ? C13 C12 H12D 108.8 . . ? C11 C12 H12D 108.8 . . ? H12C C12 H12D 107.7 . . ? C12 C13 C14 110.4(7) . . ? C12 C13 H13C 109.6 . . ? C14 C13 H13C 109.6 . . ? C12 C13 H13D 109.6 . . ? C14 C13 H13D 109.6 . . ? H13C C13 H13D 108.1 . . ? C13 C14 C16 113.1(7) . . ? C13 C14 P1 104.9(5) . . ? C16 C14 P1 115.1(5) . . ? C13 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? P1 C14 H14 107.8 . . ? C11 C15 H15D 109.5 . . ? C11 C15 H15E 109.5 . . ? H15D C15 H15E 109.5 . . ? C11 C15 H15F 109.5 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? C14 C16 H16D 109.5 . . ? C14 C16 H16E 109.5 . . ? H16D C16 H16E 109.5 . . ? C14 C16 H16F 109.5 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C22B C21B C25B 114.2(6) . . ? C22B C21B P2B 105.6(4) . . ? C25B C21B P2B 115.9(5) . . ? C22B C21B H21B 106.8 . . ? C25B C21B H21B 106.8 . . ? P2B C21B H21B 106.8 . . ? C23B C22B C21B 109.9(5) . . ? C23B C22B H22A 109.7 . . ? C21B C22B H22A 109.7 . . ? C23B C22B H22B 109.7 . . ? C21B C22B H22B 109.7 . . ? H22A C22B H22B 108.2 . . ? C22B C23B C24B 107.5(5) . . ? C22B C23B H23A 110.2 . . ? C24B C23B H23A 110.2 . . ? C22B C23B H23B 110.2 . . ? C24B C23B H23B 110.2 . . ? H23A C23B H23B 108.5 . . ? C23B C24B C26B 116.8(6) . . ? C23B C24B P2B 105.9(4) . . ? C26B C24B P2B 115.6(5) . . ? C23B C24B H24B 105.9 . . ? C26B C24B H24B 105.9 . . ? P2B C24B H24B 105.9 . . ? C21B C25B H25A 109.5 . . ? C21B C25B H25B 109.5 . . ? H25A C25B H25B 109.5 . . ? C21B C25B H25C 109.5 . . ? H25A C25B H25C 109.5 . . ? H25B C25B H25C 109.5 . . ? C24B C26B H26A 109.5 . . ? C24B C26B H26B 109.5 . . ? H26A C26B H26B 109.5 . . ? C24B C26B H26C 109.5 . . ? H26A C26B H26C 109.5 . . ? H26B C26B H26C 109.5 . . ? C22 C21 C25 114.6(5) . . ? C22 C21 P2 106.3(4) . . ? C25 C21 P2 117.5(5) . . ? C22 C21 H21 105.9 . . ? C25 C21 H21 105.9 . . ? P2 C21 H21 105.9 . . ? C21 C22 C23 107.3(5) . . ? C21 C22 H22C 110.3 . . ? C23 C22 H22C 110.3 . . ? C21 C22 H22D 110.3 . . ? C23 C22 H22D 110.3 . . ? H22C C22 H22D 108.5 . . ? C22 C23 C24 106.9(5) . . ? C22 C23 H23C 110.3 . . ? C24 C23 H23C 110.3 . . ? C22 C23 H23D 110.3 . . ? C24 C23 H23D 110.3 . . ? H23C C23 H23D 108.6 . . ? C26 C24 C23 112.6(5) . . ? C26 C24 P2 117.0(4) . . ? C23 C24 P2 105.1(4) . . ? C26 C24 H24 107.2 . . ? C23 C24 H24 107.2 . . ? P2 C24 H24 107.2 . . ? C21 C25 H25D 109.5 . . ? C21 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? C21 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C24 C26 H26D 109.5 . . ? C24 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C24 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.697 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.139 #===END data_H4Ru4(CO)10(O-DUPHOS)_(4) _database_code_depnum_ccdc_archive 'CCDC 287845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 O11 P2 Ru4' _chemical_formula_weight 1010.76 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7272(19) _cell_length_b 16.058(3) _cell_length_c 12.132(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.35(3) _cell_angle_gamma 90.00 _cell_volume 1739.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.848 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6551 _exptl_absorpt_correction_T_max 0.7088 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7035 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.35 _reflns_number_total 7035 _reflns_number_gt 6923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0961P] 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 0.0024(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(16) _refine_ls_number_reflns 7035 _refine_ls_number_parameters 411 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0433 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.006 _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 0.417659(19) 0.641269(12) 0.126373(16) 0.01295(5) Uani 1 1 d . . . Ru2 Ru 0.55156(2) 0.644408(13) 0.386180(17) 0.01627(6) Uani 1 1 d . . . Ru3 Ru 0.40719(2) 0.496944(12) 0.283587(18) 0.01786(6) Uani 1 1 d . . . Ru4 Ru 0.69515(2) 0.545194(14) 0.276707(18) 0.01844(6) Uani 1 1 d . . . P1 P 0.18099(7) 0.69626(4) 0.03700(6) 0.01453(13) Uani 1 1 d . . . P2 P 0.32621(7) 0.59739(4) -0.15156(6) 0.01566(13) Uani 1 1 d . . . O1 O 0.3538(2) 0.56295(10) -0.02866(16) 0.0176(4) Uani 1 1 d . . . C11 C 0.4989(3) 0.73520(17) 0.0893(2) 0.0198(6) Uani 1 1 d . . . O11 O 0.5514(2) 0.79615(12) 0.07233(19) 0.0345(5) Uani 1 1 d . . . C21 C 0.6568(3) 0.7474(2) 0.4154(2) 0.0242(6) Uani 1 1 d . . . O21 O 0.7133(2) 0.81097(14) 0.4310(2) 0.0362(5) Uani 1 1 d . . . C22 C 0.4018(3) 0.67950(18) 0.4408(2) 0.0242(6) Uani 1 1 d . . . O22 O 0.3161(2) 0.70005(15) 0.47783(19) 0.0353(5) Uani 1 1 d . . . C23 C 0.6818(3) 0.59452(19) 0.5300(3) 0.0249(6) Uani 1 1 d . . . O23 O 0.7634(2) 0.56716(15) 0.61966(18) 0.0372(6) Uani 1 1 d . . . C31 C 0.3028(3) 0.41564(18) 0.1637(3) 0.0258(6) Uani 1 1 d . . . O31 O 0.2346(2) 0.37316(13) 0.0850(2) 0.0383(5) Uani 1 1 d . . . C32 C 0.5082(4) 0.4286(2) 0.4208(3) 0.0352(7) Uani 1 1 d . . . O32 O 0.5653(3) 0.38757(18) 0.5044(2) 0.0561(7) Uani 1 1 d . . . C33 C 0.2546(3) 0.52117(17) 0.3386(3) 0.0291(7) Uani 1 1 d . . . O33 O 0.1611(3) 0.53256(16) 0.3714(2) 0.0474(6) Uani 1 1 d . . . C41 C 0.8374(3) 0.6328(2) 0.3261(2) 0.0287(7) Uani 1 1 d . . . O41 O 0.9266(3) 0.68374(17) 0.3565(2) 0.0462(6) Uani 1 1 d . . . C42 C 0.7517(3) 0.4868(2) 0.1632(3) 0.0304(7) Uani 1 1 d . . . O42 O 0.7859(3) 0.45370(17) 0.0944(2) 0.0514(7) Uani 1 1 d . . . C43 C 0.8134(4) 0.4779(2) 0.4101(3) 0.0326(7) Uani 1 1 d . . . O43 O 0.8899(3) 0.43703(17) 0.4882(2) 0.0517(7) Uani 1 1 d . . . C51 C 0.0257(3) 0.63080(17) 0.0422(2) 0.0194(5) Uani 1 1 d . . . H51 H 0.0691 0.5968 0.1172 0.023 Uiso 1 1 calc R . . C52 C -0.0832(3) 0.69177(19) 0.0608(3) 0.0257(6) Uani 1 1 d . . . H52A H -0.1492 0.7170 -0.0166 0.031 Uiso 1 1 calc R . . H52B H -0.1464 0.6629 0.0958 0.031 Uiso 1 1 calc R . . C53 C 0.0116(3) 0.75845(19) 0.1463(3) 0.0299(7) Uani 1 1 d . . . H53A H 0.0643 0.7346 0.2276 0.036 Uiso 1 1 calc R . . H53B H -0.0531 0.8045 0.1517 0.036 Uiso 1 1 calc R . . C54 C 0.1258(3) 0.79140(17) 0.0988(2) 0.0201(6) Uani 1 1 d . . . H54 H 0.0708 0.8289 0.0295 0.024 Uiso 1 1 calc R . . C55 C -0.0416(3) 0.5693(2) -0.0614(3) 0.0358(8) Uani 1 1 d . . . H55A H -0.0887 0.6000 -0.1369 0.054 Uiso 1 1 calc R . . H55B H -0.1171 0.5351 -0.0481 0.054 Uiso 1 1 calc R . . H55C H 0.0376 0.5334 -0.0655 0.054 Uiso 1 1 calc R . . C56 C 0.2530(3) 0.84198(18) 0.1899(3) 0.0257(6) Uani 1 1 d . . . H56A H 0.3121 0.8062 0.2577 0.039 Uiso 1 1 calc R . . H56B H 0.2112 0.8885 0.2190 0.039 Uiso 1 1 calc R . . H56C H 0.3174 0.8637 0.1517 0.039 Uiso 1 1 calc R . . C61 C 0.5014(3) 0.62441(17) -0.1672(2) 0.0212(6) Uani 1 1 d . . . H61 H 0.5846 0.6143 -0.0873 0.025 Uiso 1 1 calc R . . C62 C 0.5148(3) 0.55720(19) -0.2531(3) 0.0266(7) Uani 1 1 d . . . H62A H 0.4767 0.5792 -0.3361 0.032 Uiso 1 1 calc R . . H62B H 0.6212 0.5416 -0.2293 0.032 Uiso 1 1 calc R . . C63 C 0.4235(3) 0.48046(18) -0.2478(3) 0.0284(7) Uani 1 1 d . . . H63A H 0.4124 0.4417 -0.3142 0.034 Uiso 1 1 calc R . . H63B H 0.4739 0.4507 -0.1706 0.034 Uiso 1 1 calc R . . C64 C 0.2699(3) 0.51251(16) -0.2594(2) 0.0208(6) Uani 1 1 d . . . H64 H 0.2160 0.5360 -0.3417 0.025 Uiso 1 1 calc R . . C65 C 0.5212(3) 0.71269(19) -0.2041(3) 0.0284(7) Uani 1 1 d . . . H65A H 0.4412 0.7253 -0.2823 0.043 Uiso 1 1 calc R . . H65B H 0.6185 0.7175 -0.2099 0.043 Uiso 1 1 calc R . . H65C H 0.5165 0.7521 -0.1440 0.043 Uiso 1 1 calc R . . C66 C 0.1695(3) 0.44754(19) -0.2353(3) 0.0267(6) Uani 1 1 d . . . H66A H 0.2163 0.4292 -0.1516 0.040 Uiso 1 1 calc R . . H66B H 0.1565 0.3997 -0.2886 0.040 Uiso 1 1 calc R . . H66C H 0.0716 0.4723 -0.2505 0.040 Uiso 1 1 calc R . . C71 C 0.1912(3) 0.68024(16) -0.1978(2) 0.0162(5) Uani 1 1 d . . . C72 C 0.1448(3) 0.70469(17) -0.3187(2) 0.0217(6) Uani 1 1 d . . . H72 H 0.1894 0.6792 -0.3671 0.026 Uiso 1 1 calc R . . C73 C 0.0362(3) 0.76461(17) -0.3686(3) 0.0262(6) Uani 1 1 d . . . H73 H 0.0090 0.7816 -0.4495 0.031 Uiso 1 1 calc R . . C74 C -0.0318(4) 0.7991(2) -0.3006(3) 0.0331(7) Uani 1 1 d . . . H74 H -0.1091 0.8390 -0.3353 0.040 Uiso 1 1 calc R . . C75 C 0.0109(3) 0.77653(18) -0.1807(3) 0.0275(7) Uani 1 1 d . . . H75 H -0.0388 0.8010 -0.1354 0.033 Uiso 1 1 calc R . . C76 C 0.1248(3) 0.71889(15) -0.1255(2) 0.0173(5) Uani 1 1 d . . . H112 H 0.4144 0.6998 0.2555 0.050 Uiso 1 1 d . . . H113 H 0.2959 0.5646 0.1567 0.050 Uiso 1 1 d . . . H114 H 0.5998 0.6022 0.1341 0.050 Uiso 1 1 d . . . H134 H 0.5550 0.4605 0.2351 0.050 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 Ru1 0.01235(10) 0.01539(10) 0.01019(10) 0.00073(8) 0.00350(7) -0.00031(8) Ru2 0.01520(10) 0.02270(11) 0.01038(10) 0.00068(9) 0.00452(8) 0.00171(9) Ru3 0.01811(11) 0.01878(11) 0.01700(11) 0.00497(8) 0.00729(9) 0.00080(8) Ru4 0.01368(10) 0.02710(12) 0.01406(11) 0.00091(9) 0.00498(8) 0.00399(9) P1 0.0144(3) 0.0160(3) 0.0115(3) 0.0001(3) 0.0034(3) 0.0013(3) P2 0.0158(3) 0.0179(3) 0.0129(3) -0.0003(3) 0.0053(3) -0.0004(3) O1 0.0189(9) 0.0188(9) 0.0138(9) -0.0016(7) 0.0051(7) -0.0002(7) C11 0.0207(14) 0.0240(14) 0.0143(13) -0.0034(11) 0.0063(11) 0.0013(11) O11 0.0508(14) 0.0223(11) 0.0383(13) -0.0051(10) 0.0260(11) -0.0143(10) C21 0.0165(14) 0.0363(17) 0.0145(14) 0.0008(12) 0.0005(11) 0.0032(13) O21 0.0304(12) 0.0322(12) 0.0345(12) 0.0036(10) 0.0005(10) -0.0047(10) C22 0.0242(14) 0.0325(15) 0.0113(13) 0.0031(12) 0.0020(11) 0.0003(12) O22 0.0307(11) 0.0538(14) 0.0279(11) 0.0004(11) 0.0184(10) 0.0094(10) C23 0.0246(15) 0.0324(16) 0.0211(15) 0.0004(13) 0.0127(13) 0.0026(13) O23 0.0352(12) 0.0580(16) 0.0162(11) 0.0125(10) 0.0078(9) 0.0181(11) C31 0.0259(15) 0.0203(14) 0.0321(17) 0.0061(13) 0.0125(13) 0.0012(12) O31 0.0356(13) 0.0284(12) 0.0473(15) -0.0097(11) 0.0127(11) -0.0106(10) C32 0.0322(18) 0.0348(17) 0.0361(19) 0.0129(15) 0.0109(15) 0.0037(14) O32 0.0579(16) 0.0579(16) 0.0420(15) 0.0339(13) 0.0086(13) 0.0030(14) C33 0.0302(17) 0.0278(16) 0.0274(16) 0.0038(13) 0.0095(14) -0.0015(13) O33 0.0404(13) 0.0573(16) 0.0627(17) -0.0023(13) 0.0398(13) -0.0031(12) C41 0.0218(15) 0.0488(18) 0.0192(14) -0.0011(14) 0.0121(12) 0.0005(15) O41 0.0346(13) 0.0711(16) 0.0393(14) -0.0229(13) 0.0213(11) -0.0246(13) C42 0.0283(16) 0.0374(17) 0.0247(16) 0.0059(14) 0.0098(13) 0.0087(14) O42 0.0755(18) 0.0529(15) 0.0410(15) -0.0018(12) 0.0391(14) 0.0191(14) C43 0.0329(17) 0.0447(19) 0.0216(16) -0.0012(14) 0.0122(14) 0.0109(15) O43 0.0569(17) 0.0660(17) 0.0254(13) 0.0115(12) 0.0090(12) 0.0376(15) C51 0.0161(12) 0.0242(14) 0.0163(12) 0.0030(11) 0.0048(10) 0.0001(11) C52 0.0173(14) 0.0313(15) 0.0301(16) 0.0006(13) 0.0109(12) 0.0016(12) C53 0.0277(16) 0.0359(17) 0.0329(17) -0.0096(14) 0.0191(14) 0.0023(13) C54 0.0244(14) 0.0207(13) 0.0154(13) 0.0011(11) 0.0080(11) 0.0053(11) C55 0.0308(17) 0.0369(18) 0.046(2) -0.0167(15) 0.0214(15) -0.0150(14) C56 0.0313(16) 0.0181(13) 0.0252(15) -0.0072(12) 0.0084(13) 0.0019(12) C61 0.0175(13) 0.0295(15) 0.0151(13) 0.0054(11) 0.0050(10) 0.0016(11) C62 0.0247(15) 0.0283(17) 0.0310(18) 0.0043(12) 0.0156(14) 0.0042(12) C63 0.0312(16) 0.0255(15) 0.0326(17) 0.0004(13) 0.0170(13) 0.0054(13) C64 0.0232(14) 0.0222(14) 0.0147(13) -0.0017(11) 0.0050(11) 0.0010(11) C65 0.0279(15) 0.0341(17) 0.0261(17) -0.0014(14) 0.0139(13) -0.0089(13) C66 0.0303(16) 0.0265(15) 0.0238(16) -0.0096(12) 0.0113(13) -0.0050(12) C71 0.0159(13) 0.0152(12) 0.0152(13) 0.0017(10) 0.0037(10) -0.0021(10) C72 0.0238(14) 0.0257(14) 0.0146(13) -0.0026(11) 0.0067(11) -0.0025(12) C73 0.0342(17) 0.0270(15) 0.0116(14) 0.0021(11) 0.0029(12) 0.0007(13) C74 0.0383(18) 0.0345(17) 0.0155(15) 0.0024(13) -0.0010(13) 0.0198(15) C75 0.0305(16) 0.0294(15) 0.0190(15) 0.0000(12) 0.0061(12) 0.0111(13) C76 0.0179(13) 0.0188(13) 0.0121(13) -0.0003(10) 0.0025(10) 0.0018(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 Ru1 C11 1.840(3) . ? Ru1 O1 2.1399(18) . ? Ru1 P1 2.2971(9) . ? Ru1 Ru2 2.8948(9) . ? Ru1 Ru4 3.0149(9) . ? Ru1 Ru3 3.0288(5) . ? Ru1 H112 1.8380(3) . ? Ru1 H113 1.8438(3) . ? Ru1 H114 1.8472(4) . ? Ru2 C23 1.881(3) . ? Ru2 C21 1.903(3) . ? Ru2 C22 1.909(3) . ? Ru2 Ru4 2.7791(5) . ? Ru2 Ru3 2.7827(6) . ? Ru2 H112 1.8458(6) . ? Ru3 C33 1.893(3) . ? Ru3 C32 1.909(3) . ? Ru3 C31 1.918(3) . ? Ru3 Ru4 2.9391(6) . ? Ru3 H113 1.8439(5) . ? Ru3 H134 1.8511(4) . ? Ru4 C41 1.896(3) . ? Ru4 C43 1.907(3) . ? Ru4 C42 1.918(3) . ? Ru4 H114 1.8488(5) . ? Ru4 H134 1.8479(4) . ? P1 C76 1.861(3) . ? P1 C51 1.862(3) . ? P1 C54 1.872(3) . ? P2 O1 1.5113(19) . ? P2 C71 1.796(3) . ? P2 C64 1.817(3) . ? P2 C61 1.839(3) . ? C11 O11 1.159(3) . ? C21 O21 1.139(4) . ? C22 O22 1.141(3) . ? C23 O23 1.150(3) . ? C31 O31 1.147(4) . ? C32 O32 1.151(4) . ? C33 O33 1.143(4) . ? C41 O41 1.142(4) . ? C42 O42 1.145(4) . ? C43 O43 1.150(4) . ? C51 C52 1.524(4) . ? C51 C55 1.526(4) . ? C51 H51 1.0000 . ? C52 C53 1.521(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.535(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C56 1.526(4) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C61 C65 1.522(4) . ? C61 C62 1.542(4) . ? C61 H61 1.0000 . ? C62 C63 1.536(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.532(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C66 1.534(4) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.409(4) . ? C71 C76 1.422(4) . ? C72 C73 1.379(4) . ? C72 H72 0.9500 . ? C73 C74 1.363(4) . ? C73 H73 0.9500 . ? C74 C75 1.393(4) . ? C74 H74 0.9500 . ? C75 C76 1.394(4) . ? C75 H75 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 C11 Ru1 O1 105.68(9) . . ? C11 Ru1 P1 90.96(8) . . ? O1 Ru1 P1 85.61(6) . . ? C11 Ru1 Ru2 101.57(8) . . ? O1 Ru1 Ru2 144.68(5) . . ? P1 Ru1 Ru2 116.20(3) . . ? C11 Ru1 Ru4 101.48(8) . . ? O1 Ru1 Ru4 96.28(5) . . ? P1 Ru1 Ru4 166.340(19) . . ? Ru2 Ru1 Ru4 56.06(2) . . ? C11 Ru1 Ru3 155.01(8) . . ? O1 Ru1 Ru3 91.91(5) . . ? P1 Ru1 Ru3 108.29(2) . . ? Ru2 Ru1 Ru3 55.983(11) . . ? Ru4 Ru1 Ru3 58.195(15) . . ? C11 Ru1 H112 86.76(8) . . ? O1 Ru1 H112 162.30(5) . . ? P1 Ru1 H112 81.56(3) . . ? Ru2 Ru1 H112 38.299(10) . . ? Ru4 Ru1 H112 93.42(3) . . ? Ru3 Ru1 H112 80.688(16) . . ? C11 Ru1 H113 165.61(8) . . ? O1 Ru1 H113 78.30(5) . . ? P1 Ru1 H113 75.41(2) . . ? Ru2 Ru1 H113 80.89(2) . . ? Ru4 Ru1 H113 91.679(18) . . ? Ru3 Ru1 H113 34.783(16) . . ? H112 Ru1 H113 86.67(2) . . ? C11 Ru1 H114 78.15(8) . . ? O1 Ru1 H114 77.49(5) . . ? P1 Ru1 H114 156.42(2) . . ? Ru2 Ru1 H114 86.68(3) . . ? Ru4 Ru1 H114 35.359(12) . . ? Ru3 Ru1 H114 88.79(2) . . ? H112 Ru1 H114 118.09(3) . . ? H113 Ru1 H114 116.231(16) . . ? C23 Ru2 C21 94.74(12) . . ? C23 Ru2 C22 97.49(11) . . ? C21 Ru2 C22 96.13(12) . . ? C23 Ru2 Ru4 85.27(8) . . ? C21 Ru2 Ru4 104.62(9) . . ? C22 Ru2 Ru4 158.80(9) . . ? C23 Ru2 Ru3 95.01(10) . . ? C21 Ru2 Ru3 164.12(9) . . ? C22 Ru2 Ru3 95.00(9) . . ? Ru4 Ru2 Ru3 63.800(14) . . ? C23 Ru2 Ru1 148.14(9) . . ? C21 Ru2 Ru1 101.22(9) . . ? C22 Ru2 Ru1 107.88(8) . . ? Ru4 Ru2 Ru1 64.158(18) . . ? Ru3 Ru2 Ru1 64.446(16) . . ? C23 Ru2 H112 173.49(8) . . ? C21 Ru2 H112 83.88(8) . . ? C22 Ru2 H112 76.38(8) . . ? Ru4 Ru2 H112 101.234(17) . . ? Ru3 Ru2 H112 87.77(2) . . ? Ru1 Ru2 H112 38.108(15) . . ? C33 Ru3 C32 90.87(13) . . ? C33 Ru3 C31 98.85(12) . . ? C32 Ru3 C31 101.82(14) . . ? C33 Ru3 Ru2 89.69(9) . . ? C32 Ru3 Ru2 96.02(11) . . ? C31 Ru3 Ru2 160.04(9) . . ? C33 Ru3 Ru4 147.66(9) . . ? C32 Ru3 Ru4 90.53(10) . . ? C31 Ru3 Ru4 112.45(9) . . ? Ru2 Ru3 Ru4 58.040(13) . . ? C33 Ru3 Ru1 106.94(9) . . ? C32 Ru3 Ru1 148.74(10) . . ? C31 Ru3 Ru1 100.55(9) . . ? Ru2 Ru3 Ru1 59.572(19) . . ? Ru4 Ru3 Ru1 60.67(2) . . ? C33 Ru3 H113 83.70(9) . . ? C32 Ru3 H113 174.58(10) . . ? C31 Ru3 H113 78.99(9) . . ? Ru2 Ru3 H113 84.10(3) . . ? Ru4 Ru3 H113 94.11(2) . . ? Ru1 Ru3 H113 34.781(9) . . ? C33 Ru3 H134 173.31(8) . . ? C32 Ru3 H134 84.22(10) . . ? C31 Ru3 H134 77.79(9) . . ? Ru2 Ru3 H134 95.334(15) . . ? Ru4 Ru3 H134 37.348(11) . . ? Ru1 Ru3 H134 79.471(17) . . ? H113 Ru3 H134 101.17(2) . . ? C41 Ru4 C43 91.89(14) . . ? C41 Ru4 C42 102.05(13) . . ? C43 Ru4 C42 94.82(13) . . ? C41 Ru4 Ru2 82.28(8) . . ? C43 Ru4 Ru2 99.65(9) . . ? C42 Ru4 Ru2 164.78(9) . . ? C41 Ru4 Ru3 140.44(8) . . ? C43 Ru4 Ru3 95.02(10) . . ? C42 Ru4 Ru3 116.05(10) . . ? Ru2 Ru4 Ru3 58.159(16) . . ? C41 Ru4 Ru1 100.24(9) . . ? C43 Ru4 Ru1 153.88(9) . . ? C42 Ru4 Ru1 104.99(9) . . ? Ru2 Ru4 Ru1 59.785(17) . . ? Ru3 Ru4 Ru1 61.139(17) . . ? C41 Ru4 H114 87.77(9) . . ? C43 Ru4 H114 170.04(9) . . ? C42 Ru4 H114 75.54(9) . . ? Ru2 Ru4 H114 90.174(18) . . ? Ru3 Ru4 H114 91.55(3) . . ? Ru1 Ru4 H114 35.324(16) . . ? C41 Ru4 H134 177.31(8) . . ? C43 Ru4 H134 86.92(10) . . ? C42 Ru4 H134 80.47(10) . . ? Ru2 Ru4 H134 95.529(17) . . ? Ru3 Ru4 H134 37.424(9) . . ? Ru1 Ru4 H134 79.90(2) . . ? H114 Ru4 H134 93.81(3) . . ? C76 P1 C51 104.16(12) . . ? C76 P1 C54 104.73(12) . . ? C51 P1 C54 94.70(12) . . ? C76 P1 Ru1 113.19(9) . . ? C51 P1 Ru1 116.22(9) . . ? C54 P1 Ru1 121.18(9) . . ? O1 P2 C71 113.65(11) . . ? O1 P2 C64 108.71(11) . . ? C71 P2 C64 110.88(12) . . ? O1 P2 C61 112.25(11) . . ? C71 P2 C61 112.67(12) . . ? C64 P2 C61 97.45(13) . . ? P2 O1 Ru1 121.88(10) . . ? O11 C11 Ru1 176.1(2) . . ? O21 C21 Ru2 176.7(2) . . ? O22 C22 Ru2 177.4(2) . . ? O23 C23 Ru2 177.3(3) . . ? O31 C31 Ru3 173.6(3) . . ? O32 C32 Ru3 177.9(3) . . ? O33 C33 Ru3 177.3(3) . . ? O41 C41 Ru4 177.8(3) . . ? O42 C42 Ru4 178.4(3) . . ? O43 C43 Ru4 176.7(3) . . ? C52 C51 C55 116.2(2) . . ? C52 C51 P1 105.27(19) . . ? C55 C51 P1 115.26(18) . . ? C52 C51 H51 106.5 . . ? C55 C51 H51 106.5 . . ? P1 C51 H51 106.5 . . ? C53 C52 C51 106.5(2) . . ? C53 C52 H52A 110.4 . . ? C51 C52 H52A 110.4 . . ? C53 C52 H52B 110.4 . . ? C51 C52 H52B 110.4 . . ? H52A C52 H52B 108.6 . . ? C52 C53 C54 108.7(2) . . ? C52 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? C52 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.3 . . ? C56 C54 C53 114.3(2) . . ? C56 C54 P1 116.46(19) . . ? C53 C54 P1 103.55(18) . . ? C56 C54 H54 107.4 . . ? C53 C54 H54 107.4 . . ? P1 C54 H54 107.4 . . ? C51 C55 H55A 109.5 . . ? C51 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C51 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C65 C61 C62 113.5(2) . . ? C65 C61 P2 118.7(2) . . ? C62 C61 P2 103.59(18) . . ? C65 C61 H61 106.8 . . ? C62 C61 H61 106.8 . . ? P2 C61 H61 106.8 . . ? C63 C62 C61 109.1(2) . . ? C63 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? C63 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C64 C63 C62 106.6(2) . . ? C64 C63 H63A 110.4 . . ? C62 C63 H63A 110.4 . . ? C64 C63 H63B 110.4 . . ? C62 C63 H63B 110.4 . . ? H63A C63 H63B 108.6 . . ? C63 C64 C66 115.1(2) . . ? C63 C64 P2 100.43(18) . . ? C66 C64 P2 113.95(19) . . ? C63 C64 H64 109.0 . . ? C66 C64 H64 109.0 . . ? P2 C64 H64 109.0 . . ? C61 C65 H65A 109.5 . . ? C61 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C61 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C71 C76 119.0(2) . . ? C72 C71 P2 115.1(2) . . ? C76 C71 P2 125.82(19) . . ? C73 C72 C71 121.7(3) . . ? C73 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C74 C73 C72 119.2(3) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C75 120.7(3) . . ? C73 C74 H74 119.6 . . ? C75 C74 H74 119.6 . . ? C74 C75 C76 121.8(3) . . ? C74 C75 H75 119.1 . . ? C76 C75 H75 119.1 . . ? C75 C76 C71 117.5(2) . . ? C75 C76 P1 118.9(2) . . ? C71 C76 P1 123.65(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ru1 Ru2 C23 -113.83(18) . . . . ? O1 Ru1 Ru2 C23 26.14(19) . . . . ? P1 Ru1 Ru2 C23 149.29(17) . . . . ? Ru4 Ru1 Ru2 C23 -17.67(17) . . . . ? Ru3 Ru1 Ru2 C23 54.14(17) . . . . ? C11 Ru1 Ru2 C21 4.79(12) . . . . ? O1 Ru1 Ru2 C21 144.76(12) . . . . ? P1 Ru1 Ru2 C21 -92.09(9) . . . . ? Ru4 Ru1 Ru2 C21 100.94(9) . . . . ? Ru3 Ru1 Ru2 C21 172.75(9) . . . . ? C11 Ru1 Ru2 C22 105.06(12) . . . . ? O1 Ru1 Ru2 C22 -114.97(12) . . . . ? P1 Ru1 Ru2 C22 8.18(9) . . . . ? Ru4 Ru1 Ru2 C22 -158.78(9) . . . . ? Ru3 Ru1 Ru2 C22 -86.97(9) . . . . ? C11 Ru1 Ru2 Ru4 -96.16(8) . . . . ? O1 Ru1 Ru2 Ru4 43.82(8) . . . . ? P1 Ru1 Ru2 Ru4 166.97(2) . . . . ? Ru3 Ru1 Ru2 Ru4 71.810(15) . . . . ? C11 Ru1 Ru2 Ru3 -167.97(8) . . . . ? O1 Ru1 Ru2 Ru3 -27.99(8) . . . . ? P1 Ru1 Ru2 Ru3 95.16(2) . . . . ? Ru4 Ru1 Ru2 Ru3 -71.810(15) . . . . ? C23 Ru2 Ru3 C33 95.48(12) . . . . ? C21 Ru2 Ru3 C33 -136.8(3) . . . . ? C22 Ru2 Ru3 C33 -2.50(12) . . . . ? Ru4 Ru2 Ru3 C33 177.71(9) . . . . ? Ru1 Ru2 Ru3 C33 -109.95(9) . . . . ? C23 Ru2 Ru3 C32 4.64(13) . . . . ? C21 Ru2 Ru3 C32 132.3(3) . . . . ? C22 Ru2 Ru3 C32 -93.35(13) . . . . ? Ru4 Ru2 Ru3 C32 86.86(10) . . . . ? Ru1 Ru2 Ru3 C32 159.21(10) . . . . ? C23 Ru2 Ru3 C31 -148.7(3) . . . . ? C21 Ru2 Ru3 C31 -21.0(4) . . . . ? C22 Ru2 Ru3 C31 113.3(3) . . . . ? Ru4 Ru2 Ru3 C31 -66.5(2) . . . . ? Ru1 Ru2 Ru3 C31 5.9(2) . . . . ? C23 Ru2 Ru3 Ru4 -82.22(8) . . . . ? C21 Ru2 Ru3 Ru4 45.5(3) . . . . ? C22 Ru2 Ru3 Ru4 179.79(8) . . . . ? Ru1 Ru2 Ru3 Ru4 72.35(2) . . . . ? C23 Ru2 Ru3 Ru1 -154.57(8) . . . . ? C21 Ru2 Ru3 Ru1 -26.9(3) . . . . ? C22 Ru2 Ru3 Ru1 107.44(8) . . . . ? Ru4 Ru2 Ru3 Ru1 -72.35(2) . . . . ? C11 Ru1 Ru3 C33 108.2(2) . . . . ? O1 Ru1 Ru3 C33 -116.44(11) . . . . ? P1 Ru1 Ru3 C33 -30.44(10) . . . . ? Ru2 Ru1 Ru3 C33 79.31(10) . . . . ? Ru4 Ru1 Ru3 C33 147.34(10) . . . . ? C11 Ru1 Ru3 C32 -14.0(3) . . . . ? O1 Ru1 Ru3 C32 121.4(2) . . . . ? P1 Ru1 Ru3 C32 -152.6(2) . . . . ? Ru2 Ru1 Ru3 C32 -42.9(2) . . . . ? Ru4 Ru1 Ru3 C32 25.2(2) . . . . ? C11 Ru1 Ru3 C31 -149.0(2) . . . . ? O1 Ru1 Ru3 C31 -13.72(10) . . . . ? P1 Ru1 Ru3 C31 72.29(9) . . . . ? Ru2 Ru1 Ru3 C31 -177.96(9) . . . . ? Ru4 Ru1 Ru3 C31 -109.93(9) . . . . ? C11 Ru1 Ru3 Ru2 28.91(19) . . . . ? O1 Ru1 Ru3 Ru2 164.24(5) . . . . ? P1 Ru1 Ru3 Ru2 -109.75(3) . . . . ? Ru4 Ru1 Ru3 Ru2 68.03(3) . . . . ? C11 Ru1 Ru3 Ru4 -39.12(19) . . . . ? O1 Ru1 Ru3 Ru4 96.21(5) . . . . ? P1 Ru1 Ru3 Ru4 -177.782(19) . . . . ? Ru2 Ru1 Ru3 Ru4 -68.03(3) . . . . ? C23 Ru2 Ru4 C41 -82.60(13) . . . . ? C21 Ru2 Ru4 C41 11.08(12) . . . . ? C22 Ru2 Ru4 C41 178.9(2) . . . . ? Ru3 Ru2 Ru4 C41 179.45(9) . . . . ? Ru1 Ru2 Ru4 C41 106.65(9) . . . . ? C23 Ru2 Ru4 C43 8.02(14) . . . . ? C21 Ru2 Ru4 C43 101.69(14) . . . . ? C22 Ru2 Ru4 C43 -90.5(2) . . . . ? Ru3 Ru2 Ru4 C43 -89.94(11) . . . . ? Ru1 Ru2 Ru4 C43 -162.73(10) . . . . ? C23 Ru2 Ru4 C42 169.7(4) . . . . ? C21 Ru2 Ru4 C42 -96.6(4) . . . . ? C22 Ru2 Ru4 C42 71.2(4) . . . . ? Ru3 Ru2 Ru4 C42 71.7(4) . . . . ? Ru1 Ru2 Ru4 C42 -1.0(4) . . . . ? C23 Ru2 Ru4 Ru3 97.96(9) . . . . ? C21 Ru2 Ru4 Ru3 -168.37(9) . . . . ? C22 Ru2 Ru4 Ru3 -0.6(2) . . . . ? Ru1 Ru2 Ru4 Ru3 -72.79(2) . . . . ? C23 Ru2 Ru4 Ru1 170.75(9) . . . . ? C21 Ru2 Ru4 Ru1 -95.58(9) . . . . ? C22 Ru2 Ru4 Ru1 72.2(2) . . . . ? Ru3 Ru2 Ru4 Ru1 72.79(2) . . . . ? C33 Ru3 Ru4 C41 -5.2(2) . . . . ? C32 Ru3 Ru4 C41 -97.63(18) . . . . ? C31 Ru3 Ru4 C41 159.34(16) . . . . ? Ru2 Ru3 Ru4 C41 -0.86(14) . . . . ? Ru1 Ru3 Ru4 C41 69.62(14) . . . . ? C33 Ru3 Ru4 C43 93.96(19) . . . . ? C32 Ru3 Ru4 C43 1.48(14) . . . . ? C31 Ru3 Ru4 C43 -101.54(14) . . . . ? Ru2 Ru3 Ru4 C43 98.25(10) . . . . ? Ru1 Ru3 Ru4 C43 168.73(9) . . . . ? C33 Ru3 Ru4 C42 -168.18(19) . . . . ? C32 Ru3 Ru4 C42 99.35(15) . . . . ? C31 Ru3 Ru4 C42 -3.68(14) . . . . ? Ru2 Ru3 Ru4 C42 -163.88(10) . . . . ? Ru1 Ru3 Ru4 C42 -93.40(10) . . . . ? C33 Ru3 Ru4 Ru2 -4.29(17) . . . . ? C32 Ru3 Ru4 Ru2 -96.77(11) . . . . ? C31 Ru3 Ru4 Ru2 160.20(9) . . . . ? Ru1 Ru3 Ru4 Ru2 70.48(2) . . . . ? C33 Ru3 Ru4 Ru1 -74.77(17) . . . . ? C32 Ru3 Ru4 Ru1 -167.25(11) . . . . ? C31 Ru3 Ru4 Ru1 89.72(9) . . . . ? Ru2 Ru3 Ru4 Ru1 -70.48(2) . . . . ? C11 Ru1 Ru4 C41 21.57(12) . . . . ? O1 Ru1 Ru4 C41 129.01(9) . . . . ? P1 Ru1 Ru4 C41 -133.70(11) . . . . ? Ru2 Ru1 Ru4 C41 -74.74(8) . . . . ? Ru3 Ru1 Ru4 C41 -142.65(8) . . . . ? C11 Ru1 Ru4 C43 138.0(2) . . . . ? O1 Ru1 Ru4 C43 -114.6(2) . . . . ? P1 Ru1 Ru4 C43 -17.3(2) . . . . ? Ru2 Ru1 Ru4 C43 41.7(2) . . . . ? Ru3 Ru1 Ru4 C43 -26.2(2) . . . . ? C11 Ru1 Ru4 C42 -83.98(13) . . . . ? O1 Ru1 Ru4 C42 23.47(11) . . . . ? P1 Ru1 Ru4 C42 120.76(13) . . . . ? Ru2 Ru1 Ru4 C42 179.72(10) . . . . ? Ru3 Ru1 Ru4 C42 111.81(10) . . . . ? C11 Ru1 Ru4 Ru2 96.31(8) . . . . ? O1 Ru1 Ru4 Ru2 -156.25(5) . . . . ? P1 Ru1 Ru4 Ru2 -58.96(8) . . . . ? Ru3 Ru1 Ru4 Ru2 -67.907(19) . . . . ? C11 Ru1 Ru4 Ru3 164.21(8) . . . . ? O1 Ru1 Ru4 Ru3 -88.34(5) . . . . ? P1 Ru1 Ru4 Ru3 8.95(8) . . . . ? Ru2 Ru1 Ru4 Ru3 67.907(19) . . . . ? C11 Ru1 P1 C76 60.57(12) . . . . ? O1 Ru1 P1 C76 -45.08(10) . . . . ? Ru2 Ru1 P1 C76 163.97(9) . . . . ? Ru4 Ru1 P1 C76 -143.64(10) . . . . ? Ru3 Ru1 P1 C76 -135.64(9) . . . . ? C11 Ru1 P1 C51 -178.93(12) . . . . ? O1 Ru1 P1 C51 75.42(11) . . . . ? Ru2 Ru1 P1 C51 -75.53(10) . . . . ? Ru4 Ru1 P1 C51 -23.14(14) . . . . ? Ru3 Ru1 P1 C51 -15.14(10) . . . . ? C11 Ru1 P1 C54 -65.05(13) . . . . ? O1 Ru1 P1 C54 -170.70(11) . . . . ? Ru2 Ru1 P1 C54 38.34(11) . . . . ? Ru4 Ru1 P1 C54 90.73(13) . . . . ? Ru3 Ru1 P1 C54 98.74(10) . . . . ? C71 P2 O1 Ru1 -54.55(15) . . . . ? C64 P2 O1 Ru1 -178.55(12) . . . . ? C61 P2 O1 Ru1 74.79(15) . . . . ? C11 Ru1 O1 P2 -21.88(15) . . . . ? P1 Ru1 O1 P2 67.89(11) . . . . ? Ru2 Ru1 O1 P2 -161.00(6) . . . . ? Ru4 Ru1 O1 P2 -125.70(11) . . . . ? Ru3 Ru1 O1 P2 176.09(11) . . . . ? O1 Ru1 C11 O11 179(100) . . . . ? P1 Ru1 C11 O11 93(4) . . . . ? Ru2 Ru1 C11 O11 -24(4) . . . . ? Ru4 Ru1 C11 O11 -81(4) . . . . ? Ru3 Ru1 C11 O11 -48(4) . . . . ? C23 Ru2 C21 O21 -137(4) . . . . ? C22 Ru2 C21 O21 -39(4) . . . . ? Ru4 Ru2 C21 O21 137(4) . . . . ? Ru3 Ru2 C21 O21 95(4) . . . . ? Ru1 Ru2 C21 O21 71(4) . . . . ? C23 Ru2 C22 O22 17(6) . . . . ? C21 Ru2 C22 O22 -79(6) . . . . ? Ru4 Ru2 C22 O22 113(6) . . . . ? Ru3 Ru2 C22 O22 112(6) . . . . ? Ru1 Ru2 C22 O22 177(100) . . . . ? C21 Ru2 C23 O23 20(5) . . . . ? C22 Ru2 C23 O23 -77(5) . . . . ? Ru4 Ru2 C23 O23 124(5) . . . . ? Ru3 Ru2 C23 O23 -173(5) . . . . ? Ru1 Ru2 C23 O23 140(5) . . . . ? C33 Ru3 C31 O31 84(2) . . . . ? C32 Ru3 C31 O31 176(2) . . . . ? Ru2 Ru3 C31 O31 -31(2) . . . . ? Ru4 Ru3 C31 O31 -88(2) . . . . ? Ru1 Ru3 C31 O31 -26(2) . . . . ? C33 Ru3 C32 O32 11(9) . . . . ? C31 Ru3 C32 O32 -88(9) . . . . ? Ru2 Ru3 C32 O32 101(9) . . . . ? Ru4 Ru3 C32 O32 158(9) . . . . ? Ru1 Ru3 C32 O32 137(8) . . . . ? C32 Ru3 C33 O33 -63(6) . . . . ? C31 Ru3 C33 O33 39(6) . . . . ? Ru2 Ru3 C33 O33 -159(6) . . . . ? Ru4 Ru3 C33 O33 -155(6) . . . . ? Ru1 Ru3 C33 O33 143(6) . . . . ? C43 Ru4 C41 O41 45(7) . . . . ? C42 Ru4 C41 O41 -50(7) . . . . ? Ru2 Ru4 C41 O41 145(7) . . . . ? Ru3 Ru4 C41 O41 146(7) . . . . ? Ru1 Ru4 C41 O41 -158(7) . . . . ? C41 Ru4 C42 O42 -42(10) . . . . ? C43 Ru4 C42 O42 -135(10) . . . . ? Ru2 Ru4 C42 O42 63(11) . . . . ? Ru3 Ru4 C42 O42 127(10) . . . . ? Ru1 Ru4 C42 O42 62(10) . . . . ? C41 Ru4 C43 O43 -67(5) . . . . ? C42 Ru4 C43 O43 35(5) . . . . ? Ru2 Ru4 C43 O43 -149(5) . . . . ? Ru3 Ru4 C43 O43 152(5) . . . . ? Ru1 Ru4 C43 O43 175(5) . . . . ? C76 P1 C51 C52 -92.31(19) . . . . ? C54 P1 C51 C52 14.18(19) . . . . ? Ru1 P1 C51 C52 142.46(15) . . . . ? C76 P1 C51 C55 37.0(2) . . . . ? C54 P1 C51 C55 143.5(2) . . . . ? Ru1 P1 C51 C55 -88.2(2) . . . . ? C55 C51 C52 C53 -166.7(2) . . . . ? P1 C51 C52 C53 -37.9(3) . . . . ? C51 C52 C53 C54 50.8(3) . . . . ? C52 C53 C54 C56 -165.3(2) . . . . ? C52 C53 C54 P1 -37.6(3) . . . . ? C76 P1 C54 C56 -114.8(2) . . . . ? C51 P1 C54 C56 139.2(2) . . . . ? Ru1 P1 C54 C56 14.6(2) . . . . ? C76 P1 C54 C53 118.9(2) . . . . ? C51 P1 C54 C53 12.9(2) . . . . ? Ru1 P1 C54 C53 -111.73(18) . . . . ? O1 P2 C61 C65 -124.2(2) . . . . ? C71 P2 C61 C65 5.7(3) . . . . ? C64 P2 C61 C65 122.1(2) . . . . ? O1 P2 C61 C62 108.96(17) . . . . ? C71 P2 C61 C62 -121.19(18) . . . . ? C64 P2 C61 C62 -4.81(19) . . . . ? C65 C61 C62 C63 -153.0(3) . . . . ? P2 C61 C62 C63 -22.9(3) . . . . ? C61 C62 C63 C64 47.9(3) . . . . ? C62 C63 C64 C66 -170.3(2) . . . . ? C62 C63 C64 P2 -47.4(3) . . . . ? O1 P2 C64 C63 -86.47(18) . . . . ? C71 P2 C64 C63 147.89(17) . . . . ? C61 P2 C64 C63 30.12(19) . . . . ? O1 P2 C64 C66 37.2(2) . . . . ? C71 P2 C64 C66 -88.4(2) . . . . ? C61 P2 C64 C66 153.8(2) . . . . ? O1 P2 C71 C72 -170.19(18) . . . . ? C64 P2 C71 C72 -47.4(2) . . . . ? C61 P2 C71 C72 60.7(2) . . . . ? O1 P2 C71 C76 6.7(3) . . . . ? C64 P2 C71 C76 129.5(2) . . . . ? C61 P2 C71 C76 -122.4(2) . . . . ? C76 C71 C72 C73 -0.4(4) . . . . ? P2 C71 C72 C73 176.7(2) . . . . ? C71 C72 C73 C74 -2.3(4) . . . . ? C72 C73 C74 C75 2.2(5) . . . . ? C73 C74 C75 C76 0.6(5) . . . . ? C74 C75 C76 C71 -3.3(4) . . . . ? C74 C75 C76 P1 177.0(2) . . . . ? C72 C71 C76 C75 3.1(4) . . . . ? P2 C71 C76 C75 -173.7(2) . . . . ? C72 C71 C76 P1 -177.20(19) . . . . ? P2 C71 C76 P1 6.0(3) . . . . ? C51 P1 C76 C75 74.5(2) . . . . ? C54 P1 C76 C75 -24.4(2) . . . . ? Ru1 P1 C76 C75 -158.4(2) . . . . ? C51 P1 C76 C71 -105.2(2) . . . . ? C54 P1 C76 C71 155.9(2) . . . . ? Ru1 P1 C76 C71 21.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.489 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.138 #===END data_H4Ru4(CO)10(DIOP)_(5) _database_code_depnum_ccdc_archive 'CCDC 287846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H37 Cl3 O12 P2 Ru4' _chemical_formula_weight 1306.29 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.7512(2) _cell_length_b 18.7601(4) _cell_length_c 21.1114(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5050.14(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 1.450 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14742 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1466 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.03 _reflns_number_total 14742 _reflns_number_gt 7084 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT+ _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 14742 _refine_ls_number_parameters 535 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.777 _refine_ls_restrained_S_all 0.789 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.00538(4) 0.92344(3) 0.07356(2) 0.04007(13) Uani 1 d D . . Ru2 Ru -0.14791(4) 1.01239(3) 0.14954(2) 0.03704(13) Uani 1 d D . . Ru3 Ru -0.09238(4) 1.05936(3) 0.02912(2) 0.04285(14) Uani 1 d D . . Ru4 Ru 0.06173(4) 1.07035(3) 0.12177(2) 0.04009(13) Uani 1 d D . . H1 H -0.093(3) 0.9243(13) 0.134(2) 0.080 Uiso 1 d D . . H2 H -0.025(2) 1.040(3) 0.1831(11) 0.080 Uiso 1 d D . . H3 H -0.043(4) 0.9726(15) 0.0070(12) 0.080 Uiso 1 d D . . H4 H 0.104(2) 0.9775(12) 0.112(3) 0.080 Uiso 1 d D . . P1 P 0.08907(13) 0.84048(8) 0.14046(8) 0.0377(4) Uani 1 d . . . P2 P -0.18481(13) 0.97027(9) 0.25251(8) 0.0394(4) Uani 1 d . . . C1 C 0.1024(6) 0.9049(4) 0.0075(4) 0.058(2) Uani 1 d . . . O1 O 0.1583(5) 0.8939(3) -0.0333(3) 0.104(2) Uani 1 d . . . C2 C -0.0904(6) 0.8548(4) 0.0432(4) 0.063(2) Uani 1 d . . . O2 O -0.1479(5) 0.8129(3) 0.0251(3) 0.0928(19) Uani 1 d . . . C3 C -0.2730(5) 0.9759(4) 0.1160(3) 0.0507(18) Uani 1 d . . . O3 O -0.3489(4) 0.9540(3) 0.0974(2) 0.0818(17) Uani 1 d . . . C4 C -0.2076(5) 1.0999(4) 0.1685(3) 0.0511(19) Uani 1 d . . . O4 O -0.2438(5) 1.1553(3) 0.1832(3) 0.091(2) Uani 1 d . . . C5 C -0.1387(6) 1.1529(4) 0.0421(3) 0.0563(19) Uani 1 d . . . O5 O -0.1678(5) 1.2099(3) 0.0428(3) 0.0908(19) Uani 1 d . . . C6 C -0.0233(6) 1.0826(4) -0.0472(4) 0.065(2) Uani 1 d . . . O6 O 0.0131(5) 1.1003(3) -0.0943(3) 0.094(2) Uani 1 d . . . C7 C -0.2185(6) 1.0299(4) -0.0112(3) 0.060(2) Uani 1 d . . . O7 O -0.2934(4) 1.0122(3) -0.0363(3) 0.0905(19) Uani 1 d . . . C8 C 0.1712(5) 1.0661(4) 0.1854(4) 0.063(2) Uani 1 d . . . O8 O 0.2407(5) 1.0706(3) 0.2174(3) 0.107(2) Uani 1 d . . . C9 C 0.0279(6) 1.1667(4) 0.1394(4) 0.060(2) Uani 1 d . . . O9 O 0.0136(5) 1.2248(3) 0.1523(3) 0.103(2) Uani 1 d . . . C10 C 0.1479(7) 1.0953(4) 0.0520(4) 0.071(2) Uani 1 d . . . O10 O 0.2029(6) 1.1115(4) 0.0135(3) 0.131(3) Uani 1 d . . . C11 C 0.0625(4) 0.74938(18) 0.1150(2) 0.0463(17) Uani 1 d G . . C12 C 0.1169(3) 0.7224(2) 0.0633(2) 0.062(2) Uani 1 d G . . H12 H 0.1708 0.7487 0.0451 0.074 Uiso 1 calc R . . C13 C 0.0908(4) 0.6559(3) 0.0388(2) 0.092(3) Uani 1 d G . . H13 H 0.1272 0.6379 0.0041 0.111 Uiso 1 calc R . . C14 C 0.0103(5) 0.61652(19) 0.0660(3) 0.086(3) Uani 1 d G . . H14 H -0.0072 0.5721 0.0496 0.104 Uiso 1 calc R . . C15 C -0.0441(3) 0.6435(2) 0.1177(3) 0.079(3) Uani 1 d G . . H15 H -0.0980 0.6172 0.1360 0.094 Uiso 1 calc R . . C16 C -0.0180(4) 0.7100(3) 0.1423(2) 0.066(2) Uani 1 d G . . H16 H -0.0544 0.7280 0.1769 0.080 Uiso 1 calc R . . C17 C 0.2304(3) 0.8431(2) 0.1477(2) 0.0477(17) Uani 1 d G . . C18 C 0.2789(4) 0.7917(2) 0.1851(2) 0.069(2) Uani 1 d G . . H18 H 0.2391 0.7559 0.2038 0.083 Uiso 1 calc R . . C19 C 0.3867(4) 0.7939(3) 0.1944(2) 0.091(3) Uani 1 d G . . H19 H 0.4192 0.7595 0.2194 0.109 Uiso 1 calc R . . C20 C 0.4461(3) 0.8474(3) 0.1663(3) 0.104(4) Uani 1 d G . . H20 H 0.5183 0.8489 0.1726 0.125 Uiso 1 calc R . . C21 C 0.3976(4) 0.8988(3) 0.1290(3) 0.103(3) Uani 1 d G . . H21 H 0.4373 0.9346 0.1102 0.124 Uiso 1 calc R . . C22 C 0.2897(4) 0.8966(2) 0.1197(2) 0.066(2) Uani 1 d G . . H22 H 0.2573 0.9310 0.0947 0.080 Uiso 1 calc R . . C23 C 0.0425(5) 0.8435(3) 0.2221(3) 0.0386(15) Uani 1 d . . . H23A H -0.0325 0.8352 0.2224 0.046 Uiso 1 calc R . . H23B H 0.0754 0.8052 0.2457 0.046 Uiso 1 calc R . . C24 C 0.0650(4) 0.9138(3) 0.2555(3) 0.0337(14) Uani 1 d . . . H24 H 0.0468 0.9528 0.2267 0.040 Uiso 1 calc R . . C25 C 0.0032(5) 0.9231(3) 0.3163(3) 0.0429(15) Uani 1 d . . . H25 H -0.0252 0.8770 0.3300 0.051 Uiso 1 calc R . . C26 C -0.0832(5) 0.9780(3) 0.3143(3) 0.0475(17) Uani 1 d . . . H26A H -0.0506 1.0244 0.3099 0.057 Uiso 1 calc R . . H26B H -0.1182 0.9773 0.3551 0.057 Uiso 1 calc R . . O11 O 0.1717(3) 0.9213(2) 0.27289(19) 0.0505(12) Uani 1 d . . . O12 O 0.0779(3) 0.9478(2) 0.3608(2) 0.0582(12) Uani 1 d . . . C27 C 0.1767(5) 0.9225(4) 0.3417(3) 0.0531(18) Uani 1 d . . . C28 C 0.2601(6) 0.9760(4) 0.3610(4) 0.070(2) Uani 1 d . . . H28A H 0.2462 1.0209 0.3410 0.105 Uiso 1 calc R . . H28B H 0.3278 0.9589 0.3481 0.105 Uiso 1 calc R . . H28C H 0.2590 0.9818 0.4062 0.105 Uiso 1 calc R . . C29 C 0.2005(5) 0.8495(3) 0.3645(3) 0.061(2) Uani 1 d . . . H29A H 0.2005 0.8490 0.4100 0.091 Uiso 1 calc R . . H29B H 0.2683 0.8352 0.3493 0.091 Uiso 1 calc R . . H29C H 0.1483 0.8171 0.3490 0.091 Uiso 1 calc R . . C30 C -0.2938(3) 1.0210(2) 0.2861(2) 0.0450(17) Uani 1 d G . . C31 C -0.3939(4) 1.0062(2) 0.2635(2) 0.071(2) Uani 1 d G . . H31 H -0.4034 0.9709 0.2331 0.085 Uiso 1 calc R . . C32 C -0.4796(3) 1.0439(3) 0.2865(3) 0.091(3) Uani 1 d G . . H32 H -0.5465 1.0340 0.2713 0.109 Uiso 1 calc R . . C33 C -0.4653(4) 1.0966(3) 0.3320(3) 0.105(4) Uani 1 d G . . H33 H -0.5227 1.1219 0.3473 0.126 Uiso 1 calc R . . C34 C -0.3653(5) 1.1114(2) 0.3546(2) 0.087(3) Uani 1 d G . . H34 H -0.3558 1.1467 0.3851 0.104 Uiso 1 calc R . . C35 C -0.2796(3) 1.0736(3) 0.3317(2) 0.063(2) Uani 1 d G . . H35 H -0.2126 1.0836 0.3468 0.076 Uiso 1 calc R . . C36 C -0.2325(3) 0.8792(2) 0.2625(3) 0.0485(18) Uani 1 d G . . C37 C -0.2443(4) 0.8343(3) 0.2106(2) 0.064(2) Uani 1 d G . . H37 H -0.2254 0.8499 0.1704 0.077 Uiso 1 calc R . . C38 C -0.2844(4) 0.7660(3) 0.2189(3) 0.088(3) Uani 1 d G . . H38 H -0.2923 0.7359 0.1842 0.106 Uiso 1 calc R . . C39 C -0.3127(4) 0.7426(2) 0.2790(4) 0.116(4) Uani 1 d G . . H39 H -0.3395 0.6970 0.2845 0.139 Uiso 1 calc R . . C40 C -0.3009(5) 0.7876(3) 0.3308(3) 0.121(4) Uani 1 d G . . H40 H -0.3198 0.7720 0.3711 0.145 Uiso 1 calc R . . C41 C -0.2608(4) 0.8558(3) 0.3226(2) 0.099(3) Uani 1 d G . . H41 H -0.2529 0.8859 0.3573 0.119 Uiso 1 calc R . . C99 C 0.5214(19) 0.1407(9) 0.0541(6) 0.306(15) Uani 0.93 d PD . . H99 H 0.5921 0.1216 0.0607 0.367 Uiso 0.93 calc PR . . Cl1 Cl 0.5507(4) 0.2262(3) 0.0708(3) 0.278(3) Uani 0.93 d PD . . Cl2 Cl 0.4718(5) 0.1104(3) 0.1181(4) 0.304(4) Uani 0.93 d PD . . Cl3 Cl 0.5130(7) 0.1220(5) -0.0092(3) 0.464(8) Uani 0.93 d PD . . 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 0.0430(3) 0.0383(3) 0.0389(3) -0.0011(3) 0.0005(2) 0.0049(3) Ru2 0.0329(3) 0.0408(3) 0.0374(3) -0.0009(2) -0.0002(2) 0.0012(2) Ru3 0.0486(3) 0.0432(3) 0.0368(3) 0.0021(2) -0.0012(3) 0.0074(3) Ru4 0.0369(3) 0.0388(3) 0.0446(3) 0.0013(3) 0.0018(2) -0.0009(3) P1 0.0333(9) 0.0351(9) 0.0447(10) -0.0012(7) 0.0004(8) 0.0013(8) P2 0.0358(10) 0.0438(10) 0.0388(10) 0.0013(8) 0.0046(8) -0.0022(8) C1 0.048(4) 0.063(5) 0.063(5) 0.000(4) 0.008(4) 0.011(4) O1 0.116(5) 0.119(5) 0.076(4) 0.010(4) 0.047(4) 0.030(4) C2 0.063(5) 0.054(5) 0.072(6) 0.002(4) -0.020(5) 0.005(4) O2 0.087(4) 0.078(4) 0.113(5) -0.024(4) -0.034(4) -0.019(4) C3 0.040(4) 0.059(5) 0.054(5) 0.001(4) -0.011(4) 0.000(4) O3 0.056(3) 0.119(5) 0.070(4) -0.001(3) -0.019(3) -0.015(4) C4 0.050(4) 0.046(4) 0.058(5) 0.009(4) 0.003(4) -0.002(4) O4 0.112(5) 0.059(4) 0.102(5) 0.002(3) 0.026(4) 0.017(4) C5 0.071(5) 0.050(4) 0.048(4) 0.003(4) 0.006(4) 0.005(4) O5 0.111(5) 0.056(3) 0.105(5) -0.005(3) -0.011(4) 0.024(4) C6 0.057(5) 0.068(5) 0.072(6) 0.021(4) 0.009(4) 0.014(4) O6 0.084(4) 0.127(6) 0.070(4) 0.021(4) 0.023(3) 0.022(4) C7 0.061(5) 0.070(5) 0.049(5) 0.011(4) 0.001(4) 0.013(4) O7 0.077(4) 0.118(5) 0.077(4) 0.003(4) -0.037(3) -0.016(4) C8 0.043(4) 0.054(5) 0.092(6) 0.015(5) -0.008(4) -0.015(4) O8 0.089(4) 0.091(5) 0.140(6) 0.042(4) -0.065(4) -0.033(4) C9 0.055(5) 0.049(4) 0.077(6) -0.011(4) -0.001(4) -0.009(4) O9 0.116(5) 0.048(3) 0.145(6) -0.026(4) -0.002(5) 0.000(4) C10 0.060(5) 0.083(6) 0.069(6) 0.009(5) 0.003(5) -0.004(5) O10 0.116(6) 0.188(8) 0.090(5) 0.013(5) 0.054(5) -0.029(5) C11 0.051(4) 0.040(4) 0.047(4) 0.008(3) 0.001(4) 0.002(3) C12 0.070(5) 0.047(4) 0.069(5) -0.015(4) 0.009(4) 0.005(4) C13 0.137(9) 0.046(5) 0.095(7) -0.022(5) 0.017(7) 0.016(6) C14 0.113(8) 0.039(4) 0.107(8) -0.010(5) -0.035(7) -0.015(5) C15 0.085(6) 0.049(5) 0.101(7) -0.010(5) -0.001(6) -0.010(4) C16 0.067(5) 0.056(5) 0.076(6) -0.013(4) 0.011(5) 0.001(4) C17 0.040(4) 0.036(4) 0.067(5) 0.006(4) 0.002(4) 0.006(3) C18 0.037(4) 0.064(5) 0.106(7) 0.011(5) -0.011(4) 0.007(4) C19 0.055(6) 0.087(7) 0.131(8) 0.013(6) -0.026(6) 0.025(5) C20 0.043(5) 0.078(6) 0.190(12) -0.050(7) -0.015(6) 0.007(5) C21 0.048(5) 0.084(6) 0.178(11) 0.022(7) 0.014(6) -0.014(5) C22 0.041(4) 0.055(5) 0.104(7) 0.003(5) 0.011(4) 0.008(4) C23 0.038(4) 0.039(3) 0.039(4) 0.003(3) -0.005(3) 0.002(3) C24 0.030(3) 0.032(3) 0.039(3) 0.000(3) -0.004(3) 0.005(3) C25 0.045(4) 0.046(4) 0.038(3) -0.004(3) -0.004(3) -0.010(4) C26 0.053(4) 0.056(4) 0.033(3) -0.005(3) 0.001(3) -0.001(4) O11 0.040(3) 0.069(3) 0.042(3) -0.009(2) -0.007(2) -0.005(3) O12 0.056(3) 0.074(3) 0.044(3) -0.006(2) -0.017(2) 0.005(3) C27 0.052(4) 0.055(4) 0.052(4) -0.007(4) -0.019(3) 0.005(4) C28 0.074(5) 0.058(5) 0.079(6) 0.005(4) -0.022(5) -0.012(4) C29 0.060(5) 0.053(4) 0.069(5) 0.008(4) -0.027(4) -0.005(4) C30 0.035(4) 0.055(4) 0.045(4) 0.011(3) 0.007(3) 0.006(3) C31 0.044(4) 0.075(5) 0.095(6) 0.012(5) 0.013(4) 0.009(4) C32 0.054(6) 0.088(7) 0.130(9) 0.020(6) 0.027(6) 0.019(5) C33 0.097(8) 0.103(8) 0.115(9) 0.039(6) 0.069(7) 0.054(6) C34 0.089(7) 0.080(6) 0.090(6) -0.020(5) 0.017(6) 0.042(5) C35 0.068(5) 0.075(5) 0.048(5) -0.008(4) 0.005(4) 0.009(5) C36 0.031(4) 0.044(4) 0.070(5) 0.011(4) 0.010(4) -0.005(3) C37 0.052(5) 0.045(5) 0.094(7) -0.005(4) 0.000(4) -0.012(4) C38 0.063(6) 0.058(6) 0.144(10) -0.008(6) -0.005(6) -0.004(5) C39 0.094(8) 0.066(7) 0.187(12) 0.010(8) 0.065(8) -0.003(6) C40 0.127(9) 0.090(8) 0.146(11) 0.052(7) 0.077(8) 0.013(7) C41 0.110(8) 0.069(6) 0.117(9) 0.022(6) 0.053(7) -0.011(6) C99 0.50(4) 0.31(3) 0.099(13) 0.031(16) 0.13(2) 0.01(3) Cl1 0.179(5) 0.167(4) 0.489(11) -0.025(6) -0.044(6) 0.004(4) Cl2 0.330(9) 0.228(6) 0.354(9) 0.053(6) 0.120(7) 0.060(5) Cl3 0.480(11) 0.670(15) 0.241(7) -0.259(9) -0.200(7) 0.431(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.887(8) . ? Ru1 C1 1.896(8) . ? Ru1 P1 2.3569(17) . ? Ru1 Ru3 2.9894(7) . ? Ru1 Ru4 3.0245(7) . ? Ru1 Ru2 3.0295(7) . ? Ru1 H1 1.799(19) . ? Ru1 H3 1.788(19) . ? Ru1 H4 1.80(2) . ? Ru2 C4 1.853(7) . ? Ru2 C3 1.875(7) . ? Ru2 P2 2.3603(17) . ? Ru2 Ru3 2.7823(7) . ? Ru2 Ru4 2.9448(7) . ? Ru2 H1 1.821(19) . ? Ru2 H2 1.79(2) . ? Ru3 C5 1.872(7) . ? Ru3 C6 1.887(8) . ? Ru3 C7 1.902(8) . ? Ru3 Ru4 2.7803(7) . ? Ru3 H3 1.808(19) . ? Ru4 C9 1.895(7) . ? Ru4 C10 1.895(8) . ? Ru4 C8 1.939(8) . ? Ru4 H2 1.801(19) . ? Ru4 H4 1.837(19) . ? P1 C17 1.809(4) . ? P1 C11 1.823(3) . ? P1 C23 1.824(6) . ? P2 C36 1.826(4) . ? P2 C30 1.828(4) . ? P2 C26 1.844(6) . ? C1 O1 1.138(8) . ? C2 O2 1.141(8) . ? C3 O3 1.121(7) . ? C4 O4 1.178(7) . ? C5 O5 1.132(7) . ? C6 O6 1.147(8) . ? C7 O7 1.142(8) . ? C8 O8 1.117(8) . ? C9 O9 1.139(7) . ? C10 O10 1.116(9) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.521(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O11 1.416(6) . ? C24 C25 1.517(8) . ? C24 H24 0.9800 . ? C25 O12 1.417(7) . ? C25 C26 1.509(8) . ? C25 H25 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? O11 C27 1.454(7) . ? O12 C27 1.406(7) . ? C27 C29 1.483(9) . ? C27 C28 1.517(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C99 Cl3 1.387(12) . ? C99 Cl2 1.597(12) . ? C99 Cl1 1.683(14) . ? C99 H99 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 C2 Ru1 C1 92.7(3) . . ? C2 Ru1 P1 92.6(2) . . ? C1 Ru1 P1 91.4(2) . . ? C2 Ru1 Ru3 101.9(2) . . ? C1 Ru1 Ru3 101.4(2) . . ? P1 Ru1 Ru3 160.06(5) . . ? C2 Ru1 Ru4 152.9(2) . . ? C1 Ru1 Ru4 105.1(2) . . ? P1 Ru1 Ru4 107.01(4) . . ? Ru3 Ru1 Ru4 55.068(17) . . ? C2 Ru1 Ru2 98.0(2) . . ? C1 Ru1 Ru2 155.7(2) . . ? P1 Ru1 Ru2 109.79(4) . . ? Ru3 Ru1 Ru2 55.061(16) . . ? Ru4 Ru1 Ru2 58.210(16) . . ? C2 Ru1 H1 78.2(16) . . ? C1 Ru1 H1 169.5(10) . . ? P1 Ru1 H1 84.0(13) . . ? Ru3 Ru1 H1 85.7(10) . . ? Ru4 Ru1 H1 85.3(12) . . ? Ru2 Ru1 H1 33.4(7) . . ? C2 Ru1 H3 82.1(16) . . ? C1 Ru1 H3 75.0(13) . . ? P1 Ru1 H3 165.0(8) . . ? Ru3 Ru1 H3 34.0(7) . . ? Ru4 Ru1 H3 82.9(12) . . ? Ru2 Ru1 H3 84.9(10) . . ? H1 Ru1 H3 108(2) . . ? C2 Ru1 H4 170.4(13) . . ? C1 Ru1 H4 88.6(17) . . ? P1 Ru1 H4 77.8(11) . . ? Ru3 Ru1 H4 87.2(9) . . ? Ru4 Ru1 H4 34.2(7) . . ? Ru2 Ru1 H4 84.5(13) . . ? H1 Ru1 H4 100(2) . . ? H3 Ru1 H4 107(2) . . ? C4 Ru2 C3 93.2(3) . . ? C4 Ru2 P2 90.9(2) . . ? C3 Ru2 P2 93.2(2) . . ? C4 Ru2 Ru3 91.2(2) . . ? C3 Ru2 Ru3 89.2(2) . . ? P2 Ru2 Ru3 176.65(5) . . ? C4 Ru2 Ru4 95.1(2) . . ? C3 Ru2 Ru4 146.3(2) . . ? P2 Ru2 Ru4 119.20(5) . . ? Ru3 Ru2 Ru4 58.002(18) . . ? C4 Ru2 Ru1 150.2(2) . . ? C3 Ru2 Ru1 98.5(2) . . ? P2 Ru2 Ru1 115.59(4) . . ? Ru3 Ru2 Ru1 61.737(17) . . ? Ru4 Ru2 Ru1 60.810(17) . . ? C4 Ru2 H1 176.9(7) . . ? C3 Ru2 H1 85.8(17) . . ? P2 Ru2 H1 86.2(10) . . ? Ru3 Ru2 H1 91.7(10) . . ? Ru4 Ru2 H1 87.4(12) . . ? Ru1 Ru2 H1 33.0(7) . . ? C4 Ru2 H2 91.1(19) . . ? C3 Ru2 H2 175.2(18) . . ? P2 Ru2 H2 84.5(7) . . ? Ru3 Ru2 H2 92.8(7) . . ? Ru4 Ru2 H2 35.0(7) . . ? Ru1 Ru2 H2 78.7(16) . . ? H1 Ru2 H2 90(2) . . ? C5 Ru3 C6 93.2(3) . . ? C5 Ru3 C7 94.1(3) . . ? C6 Ru3 C7 94.5(3) . . ? C5 Ru3 Ru4 92.9(2) . . ? C6 Ru3 Ru4 104.7(2) . . ? C7 Ru3 Ru4 159.1(2) . . ? C5 Ru3 Ru2 94.8(2) . . ? C6 Ru3 Ru2 166.4(2) . . ? C7 Ru3 Ru2 95.9(2) . . ? Ru4 Ru3 Ru2 63.928(18) . . ? C5 Ru3 Ru1 152.3(2) . . ? C6 Ru3 Ru1 105.7(2) . . ? C7 Ru3 Ru1 104.2(2) . . ? Ru4 Ru3 Ru1 63.108(18) . . ? Ru2 Ru3 Ru1 63.202(18) . . ? C5 Ru3 H3 173.0(11) . . ? C6 Ru3 H3 79.9(13) . . ? C7 Ru3 H3 85.3(16) . . ? Ru4 Ru3 H3 90.0(12) . . ? Ru2 Ru3 H3 92.3(11) . . ? Ru1 Ru3 H3 33.6(7) . . ? C9 Ru4 C10 92.8(3) . . ? C9 Ru4 C8 93.8(3) . . ? C10 Ru4 C8 97.5(3) . . ? C9 Ru4 Ru3 92.8(2) . . ? C10 Ru4 Ru3 83.2(2) . . ? C8 Ru4 Ru3 173.3(2) . . ? C9 Ru4 Ru2 96.1(2) . . ? C10 Ru4 Ru2 140.5(2) . . ? C8 Ru4 Ru2 120.0(2) . . ? Ru3 Ru4 Ru2 58.070(17) . . ? C9 Ru4 Ru1 151.8(2) . . ? C10 Ru4 Ru1 95.8(2) . . ? C8 Ru4 Ru1 111.5(2) . . ? Ru3 Ru4 Ru1 61.824(17) . . ? Ru2 Ru4 Ru1 60.980(17) . . ? C9 Ru4 H2 91.3(18) . . ? C10 Ru4 H2 174.3(13) . . ? C8 Ru4 H2 86.1(8) . . ? Ru3 Ru4 H2 92.7(7) . . ? Ru2 Ru4 H2 34.8(7) . . ? Ru1 Ru4 H2 78.7(16) . . ? C9 Ru4 H4 174.1(10) . . ? C10 Ru4 H4 88.4(18) . . ? C8 Ru4 H4 80.3(9) . . ? Ru3 Ru4 H4 93.1(9) . . ? Ru2 Ru4 H4 86.5(13) . . ? Ru1 Ru4 H4 33.4(7) . . ? H2 Ru4 H4 88(2) . . ? C17 P1 C11 103.6(2) . . ? C17 P1 C23 104.0(3) . . ? C11 P1 C23 104.3(2) . . ? C17 P1 Ru1 118.96(17) . . ? C11 P1 Ru1 111.02(17) . . ? C23 P1 Ru1 113.5(2) . . ? C36 P2 C30 100.9(2) . . ? C36 P2 C26 103.0(3) . . ? C30 P2 C26 102.6(2) . . ? C36 P2 Ru2 119.07(19) . . ? C30 P2 Ru2 109.57(16) . . ? C26 P2 Ru2 119.0(2) . . ? O1 C1 Ru1 178.1(7) . . ? O2 C2 Ru1 179.5(6) . . ? O3 C3 Ru2 178.2(7) . . ? O4 C4 Ru2 177.1(7) . . ? O5 C5 Ru3 172.4(6) . . ? O6 C6 Ru3 175.0(7) . . ? O7 C7 Ru3 179.0(7) . . ? O8 C8 Ru4 170.6(7) . . ? O9 C9 Ru4 175.4(7) . . ? O10 C10 Ru4 175.7(8) . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 118.7(3) . . ? C16 C11 P1 121.0(3) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 P1 118.2(3) . . ? C22 C17 P1 121.7(3) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 120.0 . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C24 C23 P1 113.8(4) . . ? C24 C23 H23A 108.8 . . ? P1 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? P1 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? O11 C24 C25 105.5(5) . . ? O11 C24 C23 112.8(5) . . ? C25 C24 C23 113.2(5) . . ? O11 C24 H24 108.4 . . ? C25 C24 H24 108.4 . . ? C23 C24 H24 108.4 . . ? O12 C25 C26 106.6(5) . . ? O12 C25 C24 104.5(5) . . ? C26 C25 C24 115.8(5) . . ? O12 C25 H25 109.9 . . ? C26 C25 H25 109.9 . . ? C24 C25 H25 109.9 . . ? C25 C26 P2 118.6(4) . . ? C25 C26 H26A 107.7 . . ? P2 C26 H26A 107.7 . . ? C25 C26 H26B 107.7 . . ? P2 C26 H26B 107.7 . . ? H26A C26 H26B 107.1 . . ? C24 O11 C27 107.7(4) . . ? C27 O12 C25 107.5(5) . . ? O12 C27 O11 104.6(5) . . ? O12 C27 C29 113.7(6) . . ? O11 C27 C29 108.6(6) . . ? O12 C27 C28 109.1(6) . . ? O11 C27 C28 108.1(6) . . ? C29 C27 C28 112.3(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.0 . . ? C31 C30 P2 117.4(3) . . ? C35 C30 P2 122.6(3) . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C37 C36 C41 120.0 . . ? C37 C36 P2 120.8(3) . . ? C41 C36 P2 119.1(3) . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? Cl3 C99 Cl2 134.0(15) . . ? Cl3 C99 Cl1 117.4(11) . . ? Cl2 C99 Cl1 104.5(8) . . ? Cl3 C99 H99 96.6 . . ? Cl2 C99 H99 96.6 . . ? Cl1 C99 H99 96.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.774 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.102 #===END data_(H4Ru4(CO)10)(DIOP)2(H4Ru4(CO)10)_(6) _database_code_depnum_ccdc_archive 'CCDC 287847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H86 O24 P4 Ru8' _chemical_formula_weight 2460.01 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.9624(5) _cell_length_b 19.8385(6) _cell_length_c 17.5353(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.2960(10) _cell_angle_gamma 90.00 _cell_volume 5329.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57013 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.99 _reflns_number_total 23237 _reflns_number_gt 13706 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT+ _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 23237 _refine_ls_number_parameters 1037 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.819 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45820(2) 0.736921(19) 0.44855(2) 0.04114(10) Uani 1 d D . . Ru2 Ru 0.61165(2) 0.67527(2) 0.40953(2) 0.04332(10) Uani 1 d D . . Ru3 Ru 0.59072(3) 0.68198(2) 0.57251(2) 0.05043(12) Uani 1 d D . . Ru4 Ru 0.49139(3) 0.58911(2) 0.44735(2) 0.04776(11) Uani 1 d D . . H1 H 0.5267(9) 0.7358(10) 0.3837(10) 0.040 Uiso 1 d D . . H2 H 0.6624(11) 0.6973(18) 0.5121(7) 0.078 Uiso 1 d D . . H3 H 0.4104(11) 0.6547(6) 0.431(3) 0.081 Uiso 1 d D . . H4 H 0.559(2) 0.5969(8) 0.5475(11) 0.091 Uiso 1 d D . . Ru5 Ru 0.57494(3) 0.79053(2) -0.01668(2) 0.04778(11) Uani 1 d D . . Ru6 Ru 0.71095(3) 0.89795(2) 0.00349(2) 0.04828(11) Uani 1 d D . . Ru7 Ru 0.59813(3) 0.87690(2) -0.14824(2) 0.05433(13) Uani 1 d D . . Ru8 Ru 0.71644(3) 0.76554(2) -0.07679(2) 0.05797(13) Uani 1 d D . . H5 H 0.6447(11) 0.8488(9) 0.0504(10) 0.042 Uiso 1 d D . . H6 H 0.7764(12) 0.8286(8) -0.0126(16) 0.093 Uiso 1 d D . . H7 H 0.5232(11) 0.8369(12) -0.1050(11) 0.083 Uiso 1 d D . . H8 H 0.6547(15) 0.8037(10) -0.1666(10) 0.086 Uiso 1 d D . . P1 P 0.33490(8) 0.75350(6) 0.33972(7) 0.0426(3) Uani 1 d . . . P2 P 0.45504(9) 0.82900(7) 0.02457(7) 0.0467(4) Uani 1 d . . . P3 P 0.71314(8) 0.75875(7) 0.40078(7) 0.0461(3) Uani 1 d . . . P4 P 0.82664(9) 0.89578(7) 0.12154(8) 0.0522(4) Uani 1 d . . . C1 C 0.4960(3) 0.8271(3) 0.4594(3) 0.0613(16) Uani 1 d . . . O1 O 0.5210(3) 0.88151(18) 0.4654(2) 0.0832(14) Uani 1 d . . . C2 C 0.3895(3) 0.7467(3) 0.5184(3) 0.0636(17) Uani 1 d . . . O2 O 0.3477(2) 0.7529(2) 0.5599(2) 0.0921(15) Uani 1 d . . . C3 C 0.6947(4) 0.6087(3) 0.4271(4) 0.0739(19) Uani 1 d . . . O3 O 0.7478(3) 0.5664(2) 0.4405(3) 0.131(2) Uani 1 d . . . C4 C 0.5704(4) 0.6602(3) 0.3011(3) 0.0685(17) Uani 1 d . . . O4 O 0.5428(3) 0.6530(3) 0.2334(2) 0.1069(17) Uani 1 d . . . C5 C 0.6148(3) 0.7714(3) 0.6064(3) 0.0704(19) Uani 1 d . . . O5 O 0.6304(3) 0.8242(2) 0.6315(2) 0.0927(15) Uani 1 d . . . C6 C 0.5190(4) 0.6739(3) 0.6406(3) 0.0723(18) Uani 1 d . . . O6 O 0.4773(3) 0.6687(2) 0.6839(2) 0.0962(14) Uani 1 d . . . C7 C 0.6914(4) 0.6422(3) 0.6395(3) 0.080(2) Uani 1 d . . . O7 O 0.7566(3) 0.6240(3) 0.6835(3) 0.124(2) Uani 1 d . . . C8 C 0.4369(3) 0.5708(3) 0.3399(3) 0.0553(15) Uani 1 d . . . O8 O 0.4058(3) 0.5607(2) 0.2733(2) 0.0924(15) Uani 1 d . . . C9 C 0.4067(4) 0.5457(3) 0.4899(3) 0.0684(19) Uani 1 d . . . O9 O 0.3573(3) 0.5204(2) 0.5142(3) 0.1038(16) Uani 1 d . . . C10 C 0.5636(4) 0.5124(3) 0.4513(3) 0.0706(19) Uani 1 d . . . O10 O 0.6021(3) 0.4644(2) 0.4499(3) 0.1051(17) Uani 1 d . . . C11 C 0.5075(4) 0.7244(3) -0.0800(3) 0.0730(19) Uani 1 d . . . O11 O 0.4657(3) 0.6832(3) -0.1181(3) 0.1266(19) Uani 1 d . . . C12 C 0.6165(4) 0.7365(3) 0.0706(3) 0.0708(17) Uani 1 d . . . O12 O 0.6425(3) 0.7019(2) 0.1258(2) 0.1011(15) Uani 1 d . . . C13 C 0.7738(4) 0.9576(3) -0.0434(3) 0.0643(18) Uani 1 d . . . O13 O 0.8131(3) 0.9955(2) -0.0685(2) 0.0985(15) Uani 1 d . . . C14 C 0.6455(4) 0.9696(3) 0.0353(3) 0.0657(18) Uani 1 d . . . O14 O 0.6087(3) 1.0088(2) 0.0544(3) 0.0910(15) Uani 1 d . . . C15 C 0.6742(4) 0.9141(3) -0.2038(3) 0.0678(18) Uani 1 d . . . O15 O 0.7217(3) 0.9333(2) -0.2373(3) 0.0941(15) Uani 1 d . . . C16 C 0.5502(4) 0.9604(3) -0.1366(3) 0.0663(18) Uani 1 d . . . O16 O 0.5227(3) 1.0144(2) -0.1309(2) 0.0827(14) Uani 1 d . . . C17 C 0.5083(4) 0.8517(3) -0.2433(3) 0.0721(19) Uani 1 d . . . O17 O 0.4521(3) 0.8413(3) -0.2963(3) 0.123(2) Uani 1 d . . . C18 C 0.6626(4) 0.6884(3) -0.1328(3) 0.087(2) Uani 1 d . . . O18 O 0.6342(4) 0.6388(2) -0.1649(3) 0.124(2) Uani 1 d . . . C19 C 0.7676(4) 0.7118(3) 0.0096(3) 0.0720(18) Uani 1 d . . . O19 O 0.7980(3) 0.6767(2) 0.0648(2) 0.0936(15) Uani 1 d . . . C20 C 0.8111(5) 0.7671(4) -0.1239(4) 0.098(2) Uani 1 d . . . O20 O 0.8676(4) 0.7654(4) -0.1519(4) 0.181(3) Uani 1 d . . . C21 C 0.26305(16) 0.67969(13) 0.31619(17) 0.0495(14) Uani 1 d G . . C22 C 0.2326(2) 0.65354(17) 0.37699(17) 0.0624(17) Uani 1 d G . . H22 H 0.2496 0.6730 0.4272 0.075 Uiso 1 calc R . . C23 C 0.1768(2) 0.59831(18) 0.3627(3) 0.082(2) Uani 1 d G . . H23 H 0.1565 0.5808 0.4034 0.098 Uiso 1 calc R . . C24 C 0.1514(2) 0.56922(15) 0.2876(3) 0.089(2) Uani 1 d G . . H24 H 0.1141 0.5323 0.2780 0.107 Uiso 1 calc R . . C25 C 0.1818(2) 0.59537(18) 0.2268(2) 0.080(2) Uani 1 d G . . H25 H 0.1648 0.5759 0.1765 0.096 Uiso 1 calc R . . C26 C 0.2376(2) 0.65060(16) 0.24108(17) 0.0627(17) Uani 1 d G . . H26 H 0.2580 0.6681 0.2004 0.075 Uiso 1 calc R . . C27 C 0.25524(17) 0.81523(13) 0.35492(16) 0.0498(14) Uani 1 d G . . C28 C 0.2805(2) 0.86792(15) 0.40872(18) 0.0596(16) Uani 1 d G . . H28 H 0.3389 0.8730 0.4370 0.072 Uiso 1 calc R . . C29 C 0.2186(3) 0.91304(16) 0.4202(2) 0.080(2) Uani 1 d G . . H29 H 0.2355 0.9483 0.4562 0.096 Uiso 1 calc R . . C30 C 0.1313(2) 0.90546(19) 0.3779(3) 0.093(2) Uani 1 d G . . H30 H 0.0899 0.9356 0.3856 0.112 Uiso 1 calc R . . C31 C 0.10604(17) 0.8528(2) 0.3241(3) 0.095(3) Uani 1 d G . . H31 H 0.0477 0.8477 0.2959 0.115 Uiso 1 calc R . . C32 C 0.16800(18) 0.80765(16) 0.31263(19) 0.074(2) Uani 1 d G . . H32 H 0.1511 0.7724 0.2766 0.089 Uiso 1 calc R . . C33 C 0.3496(3) 0.7752(2) 0.2418(3) 0.0477(14) Uani 1 d . . . H33A H 0.3740 0.7367 0.2215 0.057 Uiso 1 calc R . . H33B H 0.2931 0.7849 0.2050 0.057 Uiso 1 calc R . . C34 C 0.4086(3) 0.8351(2) 0.2458(3) 0.0525(15) Uani 1 d . . . H34 H 0.4684 0.8219 0.2741 0.063 Uiso 1 calc R . . C35 C 0.4093(3) 0.8686(2) 0.1669(3) 0.0547(15) Uani 1 d . . . H35 H 0.3526 0.8615 0.1278 0.066 Uiso 1 calc R . . O34 O 0.3823(3) 0.88774(18) 0.2886(2) 0.0923(14) Uani 1 d . . . O35 O 0.4186(3) 0.93910(17) 0.1884(2) 0.0776(13) Uani 1 d . . . C36 C 0.4820(3) 0.8466(3) 0.1308(3) 0.0538(15) Uani 1 d . . . H36A H 0.5086 0.8063 0.1587 0.065 Uiso 1 calc R . . H36B H 0.5263 0.8815 0.1425 0.065 Uiso 1 calc R . . C37 C 0.3774(4) 0.9508(3) 0.2484(3) 0.0721(19) Uani 1 d . . . C38 C 0.4288(5) 1.0000(3) 0.3050(3) 0.105(3) Uani 1 d . . . H38A H 0.4264 1.0430 0.2794 0.157 Uiso 1 calc R . . H38B H 0.4883 0.9851 0.3231 0.157 Uiso 1 calc R . . H38C H 0.4053 1.0041 0.3495 0.157 Uiso 1 calc R . . C39 C 0.2813(5) 0.9699(4) 0.2129(4) 0.123(3) Uani 1 d . . . H39A H 0.2521 0.9350 0.1774 0.184 Uiso 1 calc R . . H39B H 0.2776 1.0116 0.1842 0.184 Uiso 1 calc R . . H39C H 0.2540 0.9752 0.2549 0.184 Uiso 1 calc R . . C40 C 0.36787(17) 0.76657(13) 0.01832(15) 0.0508(14) Uani 1 d G . . C41 C 0.27999(18) 0.78111(15) -0.01498(17) 0.0692(18) Uani 1 d G . . H41 H 0.2633 0.8231 -0.0377 0.083 Uiso 1 calc R . . C42 C 0.21707(16) 0.7328(2) -0.0144(2) 0.076(2) Uani 1 d G . . H42 H 0.1583 0.7426 -0.0367 0.092 Uiso 1 calc R . . C43 C 0.2420(2) 0.67001(18) 0.0195(2) 0.0768(19) Uani 1 d G . . H43 H 0.1999 0.6377 0.0199 0.092 Uiso 1 calc R . . C44 C 0.3299(3) 0.65546(14) 0.0528(2) 0.0687(18) Uani 1 d G . . H44 H 0.3466 0.6134 0.0754 0.082 Uiso 1 calc R . . C45 C 0.39282(19) 0.70374(14) 0.05220(17) 0.0593(16) Uani 1 d G . . H45 H 0.4516 0.6940 0.0745 0.071 Uiso 1 calc R . . C46 C 0.39964(18) 0.90267(15) -0.02838(16) 0.0599(16) Uani 1 d G . . C47 C 0.4019(2) 0.96563(17) 0.00693(19) 0.0735(19) Uani 1 d G . . H47 H 0.4291 0.9708 0.0609 0.088 Uiso 1 calc R . . C48 C 0.3636(3) 1.02079(15) -0.0385(3) 0.103(3) Uani 1 d G . . H48 H 0.3651 1.0629 -0.0148 0.124 Uiso 1 calc R . . C49 C 0.3230(3) 1.0130(2) -0.1192(3) 0.111(3) Uani 1 d G . . H49 H 0.2973 1.0499 -0.1495 0.133 Uiso 1 calc R . . C50 C 0.3207(2) 0.9500(2) -0.15448(18) 0.087(2) Uani 1 d G . . H50 H 0.2935 0.9448 -0.2085 0.104 Uiso 1 calc R . . C51 C 0.3590(2) 0.89487(19) -0.10909(17) 0.075(2) Uani 1 d G . . H51 H 0.3575 0.8528 -0.1327 0.090 Uiso 1 calc R . . C52 C 0.76471(17) 0.80233(16) 0.49429(14) 0.0553(16) Uani 1 d G . . C53 C 0.8170(2) 0.76306(17) 0.55481(17) 0.0673(18) Uani 1 d G . . H53 H 0.8279 0.7183 0.5452 0.081 Uiso 1 calc R . . C54 C 0.8530(2) 0.7908(2) 0.62968(15) 0.082(2) Uani 1 d G . . H54 H 0.8879 0.7645 0.6702 0.098 Uiso 1 calc R . . C55 C 0.8367(2) 0.8577(2) 0.64403(17) 0.083(2) Uani 1 d G . . H55 H 0.8608 0.8762 0.6941 0.099 Uiso 1 calc R . . C56 C 0.7844(3) 0.89698(17) 0.5835(2) 0.089(2) Uani 1 d G . . H56 H 0.7735 0.9418 0.5931 0.107 Uiso 1 calc R . . C57 C 0.7484(2) 0.86928(16) 0.50864(19) 0.0642(16) Uani 1 d G . . H57 H 0.7135 0.8956 0.4682 0.077 Uiso 1 calc R . . C58 C 0.80724(16) 0.72877(15) 0.36875(16) 0.0524(15) Uani 1 d G . . C59 C 0.89230(18) 0.75032(18) 0.40337(19) 0.083(2) Uani 1 d G . . H59 H 0.9037 0.7820 0.4441 0.099 Uiso 1 calc R . . C60 C 0.96030(16) 0.7245(2) 0.3771(3) 0.097(3) Uani 1 d G . . H60 H 1.0172 0.7390 0.4003 0.117 Uiso 1 calc R . . C61 C 0.9432(2) 0.6772(2) 0.3162(3) 0.102(2) Uani 1 d G . . H61 H 0.9887 0.6600 0.2987 0.122 Uiso 1 calc R . . C62 C 0.8582(3) 0.6557(2) 0.2816(2) 0.092(2) Uani 1 d G . . H62 H 0.8468 0.6240 0.2409 0.111 Uiso 1 calc R . . C63 C 0.7902(2) 0.68145(17) 0.30786(18) 0.0696(18) Uani 1 d G . . H63 H 0.7333 0.6670 0.2847 0.083 Uiso 1 calc R . . C64 C 0.6673(3) 0.8253(2) 0.3267(3) 0.0498(14) Uani 1 d . . . H64A H 0.6465 0.8038 0.2752 0.060 Uiso 1 calc R . . H64B H 0.6167 0.8441 0.3394 0.060 Uiso 1 calc R . . C65 C 0.7258(3) 0.8839(3) 0.3181(3) 0.0559(15) Uani 1 d . . . H65 H 0.7843 0.8788 0.3550 0.067 Uiso 1 calc R . . C66 C 0.7310(3) 0.8967(3) 0.2343(3) 0.0560(15) Uani 1 d . . . H66 H 0.6757 0.8846 0.1957 0.067 Uiso 1 calc R . . O65 O 0.6852(3) 0.94453(17) 0.3347(2) 0.0865(13) Uani 1 d . . . O66 O 0.7439(3) 0.96761(19) 0.2347(2) 0.1044(13) Uani 1 d . . . C67 C 0.8058(3) 0.8629(2) 0.2130(3) 0.0529(15) Uani 1 d . . . H67A H 0.7939 0.8150 0.2064 0.064 Uiso 1 calc R . . H67B H 0.8583 0.8685 0.2567 0.064 Uiso 1 calc R . . C68 C 0.7175(5) 0.9974(3) 0.2972(4) 0.108(2) Uani 1 d . . . C69 C 0.7984(6) 1.0278(4) 0.3536(5) 0.168(4) Uani 1 d . . . H69A H 0.8316 1.0508 0.3237 0.251 Uiso 1 calc R . . H69B H 0.8333 0.9926 0.3846 0.251 Uiso 1 calc R . . H69C H 0.7817 1.0592 0.3883 0.251 Uiso 1 calc R . . C70 C 0.6453(5) 1.0465(4) 0.2631(5) 0.179(3) Uani 1 d . . . H70A H 0.6117 1.0311 0.2117 0.269 Uiso 1 calc R . . H70B H 0.6697 1.0899 0.2580 0.269 Uiso 1 calc R . . H70C H 0.6083 1.0499 0.2976 0.269 Uiso 1 calc R . . C71 C 0.8845(2) 0.97580(16) 0.15372(18) 0.0725(19) Uani 1 d G . . C72 C 0.8410(2) 1.03698(18) 0.1355(2) 0.075(2) Uani 1 d G . . H72 H 0.7839 1.0380 0.1031 0.089 Uiso 1 calc R . . C73 C 0.8830(3) 1.09666(16) 0.1657(3) 0.098(3) Uani 1 d G . . H73 H 0.8539 1.1376 0.1535 0.118 Uiso 1 calc R . . C74 C 0.9684(3) 1.0952(2) 0.2142(3) 0.136(4) Uani 1 d G . . H74 H 0.9965 1.1351 0.2344 0.164 Uiso 1 calc R . . C75 C 1.0119(3) 1.0340(3) 0.2324(3) 0.162(4) Uani 1 d G . . H75 H 1.0690 1.0330 0.2648 0.194 Uiso 1 calc R . . C76 C 0.9699(2) 0.9743(2) 0.2022(2) 0.130(3) Uani 1 d G . . H76 H 0.9990 0.9334 0.2144 0.156 Uiso 1 calc R . . C77 C 0.91747(18) 0.84284(17) 0.11356(19) 0.0624(17) Uani 1 d G . . C78 C 0.9369(2) 0.78162(17) 0.1532(2) 0.0633(17) Uani 1 d G . . H78 H 0.9048 0.7672 0.1869 0.076 Uiso 1 calc R . . C79 C 1.0044(3) 0.74191(18) 0.1423(3) 0.089(2) Uani 1 d G . . H79 H 1.0174 0.7009 0.1688 0.106 Uiso 1 calc R . . C80 C 1.0524(3) 0.7634(2) 0.0919(3) 0.109(3) Uani 1 d G . . H80 H 1.0976 0.7368 0.0846 0.131 Uiso 1 calc R . . C81 C 1.0330(3) 0.8246(3) 0.0523(3) 0.153(3) Uani 1 d G . . H81 H 1.0651 0.8390 0.0185 0.183 Uiso 1 calc R . . C82 C 0.9655(3) 0.8643(2) 0.0631(2) 0.141(3) Uani 1 d G . . H82 H 0.9525 0.9053 0.0366 0.170 Uiso 1 calc R . . C83 C 1.0006(10) 0.5212(6) 0.4981(7) 0.222 Uiso 0.728(4) d PD . . H83A H 0.9559 0.5373 0.5206 0.332 Uiso 0.728(4) calc PR . . H83B H 1.0340 0.5587 0.4880 0.332 Uiso 0.728(4) calc PR . . H83C H 1.0382 0.4908 0.5347 0.332 Uiso 0.728(4) calc PR . . C84 C 0.9582(9) 0.4843(5) 0.4200(7) 0.202 Uiso 0.728(4) d PD . . H84A H 0.9054 0.5081 0.3920 0.243 Uiso 0.728(4) calc PR . . H84B H 0.9978 0.4857 0.3869 0.243 Uiso 0.728(4) calc PR . . C85 C 0.9367(8) 0.4153(5) 0.4306(7) 0.201 Uiso 0.728(4) d PD . . H85A H 0.9153 0.4136 0.4772 0.242 Uiso 0.728(4) calc PR . . H85B H 0.9909 0.3900 0.4435 0.242 Uiso 0.728(4) calc PR . . C86 C 0.8742(9) 0.3789(5) 0.3674(8) 0.228 Uiso 0.728(4) d PD . . H86A H 0.8940 0.3802 0.3200 0.274 Uiso 0.728(4) calc PR . . H86B H 0.8184 0.4019 0.3556 0.274 Uiso 0.728(4) calc PR . . C87 C 0.8618(10) 0.3087(5) 0.3867(8) 0.237 Uiso 0.728(4) d PD . . H87A H 0.8222 0.3088 0.4198 0.284 Uiso 0.728(4) calc PR . . H87B H 0.9176 0.2926 0.4197 0.284 Uiso 0.728(4) calc PR . . C88 C 0.8290(10) 0.2574(6) 0.3245(8) 0.238 Uiso 0.728(4) d PD . . H88A H 0.8581 0.2624 0.2837 0.358 Uiso 0.728(4) calc PR . . H88B H 0.7673 0.2631 0.3018 0.358 Uiso 0.728(4) calc PR . . H88C H 0.8404 0.2132 0.3475 0.358 Uiso 0.728(4) calc PR . . C89 C 0.0477(8) 0.1108(5) 1.0479(7) 0.236 Uiso 0.864(4) d PD . . H89A H -0.0077 0.0971 1.0542 0.353 Uiso 0.864(4) calc PR . . H89B H 0.0387 0.1442 1.0068 0.353 Uiso 0.864(4) calc PR . . H89C H 0.0830 0.1293 1.0969 0.353 Uiso 0.864(4) calc PR . . C90 C 0.0930(7) 0.0509(6) 1.0255(6) 0.204 Uiso 0.864(4) d PD . . H90A H 0.0944 0.0142 1.0624 0.245 Uiso 0.864(4) calc PR . . H90B H 0.1526 0.0625 1.0275 0.245 Uiso 0.864(4) calc PR . . C91 C 0.0434(8) 0.0300(5) 0.9426(6) 0.214 Uiso 0.864(4) d PD . . H91A H -0.0156 0.0179 0.9421 0.257 Uiso 0.864(4) calc PR . . H91B H 0.0398 0.0681 0.9072 0.257 Uiso 0.864(4) calc PR . . C92 C 0.0815(8) -0.0245(5) 0.9138(6) 0.217 Uiso 0.864(4) d PD . . H92A H 0.0908 -0.0587 0.9549 0.260 Uiso 0.864(4) calc PR . . H92B H 0.1392 -0.0090 0.9139 0.260 Uiso 0.864(4) calc PR . . C93 C 0.0496(9) -0.0596(5) 0.8417(6) 0.224 Uiso 0.864(4) d PD . . H93A H 0.0679 -0.0345 0.8017 0.269 Uiso 0.864(4) calc PR . . H93B H -0.0136 -0.0567 0.8276 0.269 Uiso 0.864(4) calc PR . . C94 C 0.0716(8) -0.1306(5) 0.8333(8) 0.235 Uiso 0.864(4) d PD . . H94A H 0.0837 -0.1369 0.7832 0.352 Uiso 0.864(4) calc PR . . H94B H 0.0233 -0.1586 0.8356 0.352 Uiso 0.864(4) calc PR . . H94C H 0.1221 -0.1426 0.8756 0.352 Uiso 0.864(4) calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0462(2) 0.0410(2) 0.03824(19) -0.00188(17) 0.01515(16) -0.00160(19) Ru2 0.0488(2) 0.0416(2) 0.04306(19) 0.00477(18) 0.01853(16) 0.0018(2) Ru3 0.0544(2) 0.0595(3) 0.03707(19) 0.00978(19) 0.01218(17) -0.0076(2) Ru4 0.0552(2) 0.0398(2) 0.0500(2) 0.00699(18) 0.01754(18) -0.0029(2) Ru5 0.0610(2) 0.0446(2) 0.0409(2) 0.00277(18) 0.01957(18) -0.0027(2) Ru6 0.0593(2) 0.0467(2) 0.0430(2) 0.00349(18) 0.02110(18) -0.0043(2) Ru7 0.0729(3) 0.0553(3) 0.0376(2) 0.00507(19) 0.02016(19) -0.0002(2) Ru8 0.0741(3) 0.0540(3) 0.0527(2) -0.0021(2) 0.0289(2) 0.0037(2) P1 0.0488(7) 0.0412(7) 0.0393(6) -0.0044(5) 0.0149(5) -0.0016(6) P2 0.0579(8) 0.0444(7) 0.0388(7) 0.0025(6) 0.0151(6) -0.0039(7) P3 0.0488(7) 0.0478(7) 0.0452(7) 0.0074(6) 0.0192(5) 0.0002(6) P4 0.0559(8) 0.0548(8) 0.0475(7) 0.0093(7) 0.0172(6) -0.0030(7) C1 0.065(3) 0.060(3) 0.060(3) -0.006(3) 0.019(3) 0.023(3) O1 0.082(3) 0.042(2) 0.117(3) -0.010(2) 0.013(2) -0.006(2) C2 0.053(3) 0.076(4) 0.059(3) 0.001(3) 0.011(3) 0.012(3) O2 0.071(2) 0.141(4) 0.078(2) -0.011(3) 0.0435(19) 0.016(3) C3 0.072(3) 0.062(4) 0.096(4) 0.009(3) 0.038(3) 0.001(3) O3 0.096(3) 0.078(3) 0.241(5) 0.052(3) 0.083(3) 0.040(3) C4 0.081(4) 0.062(4) 0.074(3) -0.003(3) 0.041(3) -0.009(3) O4 0.128(3) 0.154(4) 0.047(2) -0.027(2) 0.038(2) -0.057(3) C5 0.069(3) 0.103(5) 0.040(3) -0.001(3) 0.017(2) -0.023(4) O5 0.114(3) 0.096(3) 0.073(3) -0.027(2) 0.035(2) -0.036(3) C6 0.082(4) 0.074(4) 0.061(3) 0.028(3) 0.018(3) -0.018(4) O6 0.112(3) 0.110(3) 0.081(2) 0.026(3) 0.050(2) -0.014(3) C7 0.089(4) 0.093(4) 0.053(3) 0.027(3) 0.010(3) -0.027(4) O7 0.105(4) 0.149(4) 0.101(4) 0.049(3) 0.002(3) 0.004(4) C8 0.054(3) 0.049(3) 0.066(3) 0.000(3) 0.024(3) 0.003(3) O8 0.098(3) 0.113(3) 0.067(3) -0.029(2) 0.023(2) 0.007(3) C9 0.075(4) 0.047(3) 0.077(4) 0.015(3) 0.010(3) -0.004(3) O9 0.106(3) 0.106(3) 0.117(3) 0.033(3) 0.061(2) -0.027(3) C10 0.056(3) 0.073(4) 0.080(4) 0.007(3) 0.013(3) -0.010(3) O10 0.111(3) 0.057(3) 0.155(4) 0.010(3) 0.051(3) 0.028(3) C11 0.086(4) 0.072(4) 0.069(4) -0.010(3) 0.035(3) -0.008(3) O11 0.154(4) 0.118(4) 0.121(3) -0.069(3) 0.060(3) -0.057(3) C12 0.077(3) 0.076(4) 0.071(3) 0.007(3) 0.038(3) -0.001(3) O12 0.103(3) 0.111(3) 0.101(3) 0.059(2) 0.048(2) 0.020(3) C13 0.081(4) 0.064(3) 0.042(3) -0.005(3) 0.009(3) 0.006(3) O13 0.120(3) 0.097(3) 0.083(3) 0.028(2) 0.035(2) -0.051(3) C14 0.079(4) 0.075(4) 0.043(3) -0.006(3) 0.017(3) -0.017(3) O14 0.106(3) 0.077(3) 0.089(3) -0.031(2) 0.026(2) 0.020(3) C15 0.089(4) 0.056(3) 0.054(3) -0.008(3) 0.013(3) -0.010(3) O15 0.122(3) 0.086(3) 0.097(3) -0.001(2) 0.068(2) -0.023(3) C16 0.092(4) 0.070(4) 0.040(3) 0.017(3) 0.024(3) 0.007(3) O16 0.105(3) 0.063(3) 0.082(3) 0.018(2) 0.031(2) 0.007(2) C17 0.086(4) 0.069(4) 0.069(4) 0.012(3) 0.035(3) 0.007(3) O17 0.118(4) 0.133(4) 0.085(3) -0.017(3) -0.023(3) -0.011(4) C18 0.117(5) 0.082(4) 0.063(4) 0.000(3) 0.029(3) 0.045(4) O18 0.156(5) 0.082(3) 0.115(4) -0.051(3) 0.007(3) 0.014(3) C19 0.082(4) 0.054(3) 0.096(4) -0.005(3) 0.051(3) -0.001(3) O19 0.100(3) 0.079(3) 0.099(3) 0.034(3) 0.023(2) 0.011(3) C20 0.121(5) 0.095(5) 0.082(4) 0.012(4) 0.036(4) 0.021(5) O20 0.171(4) 0.219(7) 0.212(5) -0.009(5) 0.150(3) -0.011(5) C21 0.037(3) 0.050(3) 0.055(3) 0.000(3) 0.001(2) -0.002(3) C22 0.068(3) 0.065(4) 0.058(3) 0.004(3) 0.023(3) -0.014(3) C23 0.076(4) 0.082(4) 0.081(4) 0.024(4) 0.012(3) -0.017(4) C24 0.060(4) 0.055(4) 0.145(6) -0.003(4) 0.017(4) -0.006(3) C25 0.071(4) 0.063(4) 0.103(5) -0.032(3) 0.018(3) -0.011(3) C26 0.058(3) 0.051(3) 0.079(4) -0.028(3) 0.019(3) -0.003(3) C27 0.058(3) 0.043(3) 0.047(3) -0.002(2) 0.013(2) 0.003(3) C28 0.056(3) 0.065(3) 0.056(3) -0.016(3) 0.012(2) 0.016(3) C29 0.076(4) 0.092(4) 0.066(4) -0.036(3) 0.011(3) 0.001(4) C30 0.080(4) 0.088(5) 0.110(5) -0.011(4) 0.022(4) 0.039(4) C31 0.066(4) 0.097(5) 0.107(5) -0.022(4) -0.003(4) 0.024(4) C32 0.065(4) 0.059(4) 0.088(4) -0.016(3) 0.003(3) 0.014(3) C33 0.060(3) 0.037(3) 0.047(3) -0.006(2) 0.016(2) -0.001(2) C34 0.074(3) 0.049(3) 0.034(3) -0.002(2) 0.016(2) -0.010(3) C35 0.076(3) 0.043(3) 0.046(3) 0.001(2) 0.018(3) -0.002(3) O34 0.189(4) 0.042(2) 0.065(2) -0.0161(18) 0.068(2) -0.019(2) O35 0.141(3) 0.036(2) 0.069(2) -0.0060(17) 0.050(2) -0.010(2) C36 0.064(3) 0.053(3) 0.046(3) -0.010(2) 0.020(2) -0.017(3) C37 0.131(5) 0.050(3) 0.048(3) -0.009(3) 0.046(3) -0.002(3) C38 0.206(7) 0.047(3) 0.080(4) -0.019(3) 0.070(4) -0.031(4) C39 0.145(7) 0.119(6) 0.101(6) -0.016(5) 0.029(5) 0.017(6) C40 0.058(3) 0.058(3) 0.040(2) -0.004(2) 0.020(2) -0.001(3) C41 0.071(4) 0.067(4) 0.070(4) -0.011(3) 0.019(3) -0.007(3) C42 0.070(4) 0.072(4) 0.086(4) -0.005(3) 0.019(3) -0.006(4) C43 0.078(4) 0.082(4) 0.079(4) -0.029(3) 0.036(3) -0.028(4) C44 0.069(4) 0.061(4) 0.076(4) 0.012(3) 0.020(3) -0.018(3) C45 0.055(3) 0.054(3) 0.073(3) -0.004(3) 0.023(3) -0.005(3) C46 0.068(3) 0.071(4) 0.043(3) 0.017(3) 0.020(2) 0.011(3) C47 0.099(4) 0.051(3) 0.076(4) 0.016(3) 0.034(3) 0.014(3) C48 0.143(6) 0.054(4) 0.130(6) 0.019(4) 0.068(5) 0.016(4) C49 0.112(5) 0.122(6) 0.104(5) 0.046(4) 0.040(4) 0.065(5) C50 0.084(4) 0.119(5) 0.052(3) 0.036(4) 0.011(3) 0.020(4) C51 0.064(4) 0.094(5) 0.066(4) 0.019(4) 0.015(3) 0.010(4) C52 0.050(3) 0.076(4) 0.036(3) 0.008(3) 0.007(2) -0.005(3) C53 0.060(3) 0.070(4) 0.067(3) 0.003(3) 0.009(3) -0.010(3) C54 0.061(4) 0.135(6) 0.045(3) 0.008(4) 0.008(3) 0.012(4) C55 0.072(4) 0.113(5) 0.058(4) -0.026(4) 0.009(3) -0.019(4) C56 0.097(4) 0.098(5) 0.076(4) -0.016(4) 0.031(3) -0.014(4) C57 0.084(3) 0.060(3) 0.058(3) -0.002(3) 0.035(3) -0.020(3) C58 0.051(3) 0.048(3) 0.057(3) 0.018(2) 0.013(2) -0.004(3) C59 0.045(3) 0.126(6) 0.074(4) -0.005(4) 0.011(3) -0.001(4) C60 0.055(3) 0.159(7) 0.090(4) 0.016(4) 0.041(3) -0.002(4) C61 0.095(4) 0.131(6) 0.109(4) 0.046(4) 0.076(3) 0.050(4) C62 0.083(4) 0.097(5) 0.117(5) 0.012(4) 0.062(3) 0.016(4) C63 0.061(3) 0.077(4) 0.076(4) -0.008(3) 0.028(3) 0.012(3) C64 0.062(3) 0.046(3) 0.042(3) 0.007(2) 0.014(2) 0.002(3) C65 0.073(3) 0.054(3) 0.049(3) 0.011(2) 0.031(2) 0.001(3) C66 0.071(3) 0.056(3) 0.047(3) 0.023(2) 0.026(2) 0.017(3) O65 0.152(3) 0.040(2) 0.100(3) 0.0069(18) 0.088(2) 0.010(2) O66 0.181(3) 0.041(2) 0.137(3) 0.038(2) 0.120(2) 0.026(2) C67 0.059(3) 0.047(3) 0.053(3) 0.006(2) 0.016(2) 0.001(3) C68 0.172(6) 0.063(4) 0.128(5) 0.007(4) 0.105(4) 0.004(4) C69 0.219(8) 0.139(7) 0.176(8) -0.032(6) 0.109(7) -0.087(7) C70 0.296(7) 0.102(5) 0.220(7) 0.085(5) 0.204(5) 0.120(5) C71 0.081(4) 0.074(4) 0.060(3) 0.020(3) 0.015(3) -0.027(3) C72 0.107(5) 0.052(3) 0.059(3) 0.003(3) 0.013(3) -0.014(4) C73 0.136(6) 0.073(4) 0.075(4) 0.004(4) 0.012(4) -0.033(5) C74 0.167(7) 0.094(5) 0.115(6) 0.003(5) -0.015(6) -0.059(6) C75 0.135(7) 0.116(7) 0.176(9) 0.020(7) -0.050(7) -0.049(6) C76 0.109(6) 0.108(6) 0.126(6) 0.048(5) -0.045(5) -0.045(5) C77 0.073(3) 0.073(4) 0.047(3) 0.015(3) 0.026(3) -0.004(3) C78 0.066(3) 0.062(4) 0.069(3) 0.002(3) 0.031(3) 0.003(3) C79 0.074(4) 0.112(5) 0.082(4) -0.014(4) 0.024(3) 0.019(4) C80 0.075(4) 0.159(7) 0.104(5) 0.004(5) 0.046(4) 0.028(5) C81 0.165(6) 0.175(8) 0.162(6) 0.066(6) 0.116(5) 0.064(6) C82 0.118(4) 0.179(7) 0.167(6) 0.093(5) 0.105(4) 0.063(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.869(6) . ? Ru1 C1 1.880(6) . ? Ru1 P1 2.3486(12) . ? Ru1 Ru3 2.7941(5) . ? Ru1 Ru4 2.9808(6) . ? Ru1 Ru2 2.9839(6) . ? Ru1 H1 1.786(15) . ? Ru1 H3 1.791(13) . ? Ru2 C3 1.835(6) . ? Ru2 C4 1.854(5) . ? Ru2 P3 2.3517(14) . ? Ru2 Ru4 2.7857(6) . ? Ru2 Ru3 2.9719(5) . ? Ru2 H1 1.773(14) . ? Ru2 H2 1.807(14) . ? Ru3 C5 1.876(6) . ? Ru3 C7 1.877(6) . ? Ru3 C6 1.879(6) . ? Ru3 Ru4 2.9616(6) . ? Ru3 H2 1.790(15) . ? Ru3 H4 1.780(15) . ? Ru4 C8 1.876(5) . ? Ru4 C10 1.898(6) . ? Ru4 C9 1.922(6) . ? Ru4 H3 1.799(14) . ? Ru4 H4 1.793(15) . ? Ru5 C12 1.834(6) . ? Ru5 C11 1.854(6) . ? Ru5 P2 2.3550(15) . ? Ru5 Ru8 2.7918(6) . ? Ru5 Ru7 2.9790(6) . ? Ru5 Ru6 2.9914(6) . ? Ru5 H5 1.795(14) . ? Ru5 H7 1.790(15) . ? Ru6 C13 1.884(6) . ? Ru6 C14 1.937(6) . ? Ru6 P4 2.3563(13) . ? Ru6 Ru7 2.7941(5) . ? Ru6 Ru8 2.9931(6) . ? Ru6 H5 1.798(15) . ? Ru6 H6 1.797(15) . ? Ru7 C16 1.861(6) . ? Ru7 C15 1.906(6) . ? Ru7 C17 1.936(6) . ? Ru7 Ru8 2.9476(6) . ? Ru7 H7 1.774(15) . ? Ru7 H8 1.785(16) . ? Ru8 C19 1.845(6) . ? Ru8 C18 1.890(6) . ? Ru8 C20 1.915(7) . ? Ru8 H6 1.773(15) . ? Ru8 H8 1.776(14) . ? P1 C21 1.834(3) . ? P1 C27 1.838(3) . ? P1 C33 1.848(5) . ? P2 C46 1.822(3) . ? P2 C36 1.824(5) . ? P2 C40 1.843(3) . ? P3 C52 1.832(3) . ? P3 C58 1.844(3) . ? P3 C64 1.853(5) . ? P4 C77 1.827(3) . ? P4 C71 1.844(3) . ? P4 C67 1.845(5) . ? C1 O1 1.146(6) . ? C2 O2 1.124(6) . ? C3 O3 1.169(7) . ? C4 O4 1.153(6) . ? C5 O5 1.138(7) . ? C6 O6 1.146(7) . ? C7 O7 1.166(7) . ? C8 O8 1.151(6) . ? C9 O9 1.115(7) . ? C10 O10 1.139(7) . ? C11 O11 1.146(7) . ? C12 O12 1.164(6) . ? C13 O13 1.142(7) . ? C14 O14 1.082(7) . ? C15 O15 1.146(7) . ? C16 O16 1.172(7) . ? C17 O17 1.114(7) . ? C18 O18 1.160(7) . ? C19 O19 1.179(6) . ? C20 O20 1.141(8) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.506(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O34 1.417(6) . ? C34 C35 1.537(6) . ? C34 H34 0.9800 . ? C35 O35 1.445(6) . ? C35 C36 1.533(7) . ? C35 H35 0.9800 . ? O34 C37 1.428(6) . ? O35 C37 1.407(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.468(8) . ? C37 C39 1.532(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 C50 1.3900 . ? C49 H49 0.9300 . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 C55 1.3900 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 H55 0.9300 . ? C56 C57 1.3900 . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.3900 . ? C58 C63 1.3900 . ? C59 C60 1.3900 . ? C59 H59 0.9300 . ? C60 C61 1.3900 . ? C60 H60 0.9300 . ? C61 C62 1.3900 . ? C61 H61 0.9300 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 C65 1.524(7) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O65 1.435(6) . ? C65 C66 1.517(6) . ? C65 H65 0.9800 . ? C66 O66 1.422(6) . ? C66 C67 1.504(7) . ? C66 H66 0.9800 . ? O65 C68 1.411(8) . ? O66 C68 1.411(8) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C70 1.499(10) . ? C68 C69 1.515(10) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72 0.9300 . ? C73 C74 1.3900 . ? C73 H73 0.9300 . ? C74 C75 1.3900 . ? C74 H74 0.9300 . ? C75 C76 1.3900 . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78 0.9300 . ? C79 C80 1.3900 . ? C79 H79 0.9300 . ? C80 C81 1.3900 . ? C80 H80 0.9300 . ? C81 C82 1.3900 . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? C83 C84 1.532(13) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C85 1.437(11) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C86 1.458(12) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C87 1.460(12) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 C88 1.476(13) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 C90 1.498(12) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 C91 1.505(11) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.403(11) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C93 1.407(11) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.469(12) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? 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 C2 Ru1 C1 93.7(2) . . ? C2 Ru1 P1 90.35(15) . . ? C1 Ru1 P1 96.96(15) . . ? C2 Ru1 Ru3 89.19(15) . . ? C1 Ru1 Ru3 98.10(15) . . ? P1 Ru1 Ru3 164.94(4) . . ? C2 Ru1 Ru4 104.17(18) . . ? C1 Ru1 Ru4 152.13(16) . . ? P1 Ru1 Ru4 104.01(3) . . ? Ru3 Ru1 Ru4 61.606(14) . . ? C2 Ru1 Ru2 149.65(16) . . ? C1 Ru1 Ru2 98.79(17) . . ? P1 Ru1 Ru2 115.20(3) . . ? Ru3 Ru1 Ru2 61.805(14) . . ? Ru4 Ru1 Ru2 55.683(13) . . ? C2 Ru1 H1 174.5(7) . . ? C1 Ru1 H1 80.8(7) . . ? P1 Ru1 H1 90.4(5) . . ? Ru3 Ru1 H1 91.5(5) . . ? Ru4 Ru1 H1 80.9(6) . . ? Ru2 Ru1 H1 32.9(5) . . ? C2 Ru1 H3 84.6(12) . . ? C1 Ru1 H3 173.4(7) . . ? P1 Ru1 H3 76.7(9) . . ? Ru3 Ru1 H3 88.3(9) . . ? Ru4 Ru1 H3 33.9(5) . . ? Ru2 Ru1 H3 85.7(8) . . ? H1 Ru1 H3 100.9(14) . . ? C3 Ru2 C4 95.1(3) . . ? C3 Ru2 P3 92.24(18) . . ? C4 Ru2 P3 95.73(18) . . ? C3 Ru2 Ru4 91.86(18) . . ? C4 Ru2 Ru4 94.29(18) . . ? P3 Ru2 Ru4 168.80(4) . . ? C3 Ru2 Ru3 98.15(19) . . ? C4 Ru2 Ru3 152.89(17) . . ? P3 Ru2 Ru3 107.25(3) . . ? Ru4 Ru2 Ru3 61.812(14) . . ? C3 Ru2 Ru1 149.03(19) . . ? C4 Ru2 Ru1 102.88(17) . . ? P3 Ru2 Ru1 110.56(4) . . ? Ru4 Ru2 Ru1 62.103(14) . . ? Ru3 Ru2 Ru1 55.956(13) . . ? C3 Ru2 H1 174.5(6) . . ? C4 Ru2 H1 79.7(6) . . ? P3 Ru2 H1 89.9(6) . . ? Ru4 Ru2 H1 87.0(6) . . ? Ru3 Ru2 H1 86.1(6) . . ? Ru1 Ru2 H1 33.2(5) . . ? C3 Ru2 H2 84.6(10) . . ? C4 Ru2 H2 172.4(8) . . ? P3 Ru2 H2 76.7(8) . . ? Ru4 Ru2 H2 93.3(7) . . ? Ru3 Ru2 H2 34.1(5) . . ? Ru1 Ru2 H2 80.8(7) . . ? H1 Ru2 H2 100.8(12) . . ? C5 Ru3 C7 97.8(2) . . ? C5 Ru3 C6 89.2(3) . . ? C7 Ru3 C6 97.7(2) . . ? C5 Ru3 Ru1 85.48(15) . . ? C7 Ru3 Ru1 168.18(19) . . ? C6 Ru3 Ru1 93.68(16) . . ? C5 Ru3 Ru4 147.42(15) . . ? C7 Ru3 Ru4 112.85(19) . . ? C6 Ru3 Ru4 97.08(17) . . ? Ru1 Ru3 Ru4 62.302(13) . . ? C5 Ru3 Ru2 106.19(16) . . ? C7 Ru3 Ru2 105.97(19) . . ? C6 Ru3 Ru2 149.36(16) . . ? Ru1 Ru3 Ru2 62.238(13) . . ? Ru4 Ru3 Ru2 56.001(13) . . ? C5 Ru3 H2 85.3(11) . . ? C7 Ru3 H2 82.2(8) . . ? C6 Ru3 H2 174.5(10) . . ? Ru1 Ru3 H2 86.8(7) . . ? Ru4 Ru3 H2 88.0(7) . . ? Ru2 Ru3 H2 34.5(5) . . ? C5 Ru3 H4 173.2(11) . . ? C7 Ru3 H4 83.6(8) . . ? C6 Ru3 H4 84.0(11) . . ? Ru1 Ru3 H4 94.5(6) . . ? Ru4 Ru3 H4 34.2(5) . . ? Ru2 Ru3 H4 79.7(8) . . ? H2 Ru3 H4 101.4(15) . . ? C8 Ru4 C10 89.3(2) . . ? C8 Ru4 C9 97.1(2) . . ? C10 Ru4 C9 96.4(2) . . ? C8 Ru4 Ru2 92.08(16) . . ? C10 Ru4 Ru2 92.80(18) . . ? C9 Ru4 Ru2 167.01(17) . . ? C8 Ru4 Ru3 149.99(16) . . ? C10 Ru4 Ru3 106.14(17) . . ? C9 Ru4 Ru3 106.26(17) . . ? Ru2 Ru4 Ru3 62.187(14) . . ? C8 Ru4 Ru1 99.48(15) . . ? C10 Ru4 Ru1 153.58(17) . . ? C9 Ru4 Ru1 107.02(17) . . ? Ru2 Ru4 Ru1 62.214(14) . . ? Ru3 Ru4 Ru1 56.092(13) . . ? C8 Ru4 H3 82.7(13) . . ? C10 Ru4 H3 170.8(9) . . ? C9 Ru4 H3 80.3(10) . . ? Ru2 Ru4 H3 91.8(8) . . ? Ru3 Ru4 H3 83.0(9) . . ? Ru1 Ru4 H3 33.8(5) . . ? C8 Ru4 H4 169.4(10) . . ? C10 Ru4 H4 80.7(8) . . ? C9 Ru4 H4 87.5(10) . . ? Ru2 Ru4 H4 85.0(9) . . ? Ru3 Ru4 H4 33.9(5) . . ? Ru1 Ru4 H4 88.2(6) . . ? H3 Ru4 H4 107.5(15) . . ? C12 Ru5 C11 95.7(2) . . ? C12 Ru5 P2 93.90(18) . . ? C11 Ru5 P2 91.57(19) . . ? C12 Ru5 Ru8 93.99(18) . . ? C11 Ru5 Ru8 92.53(19) . . ? P2 Ru5 Ru8 170.70(4) . . ? C12 Ru5 Ru7 152.65(18) . . ? C11 Ru5 Ru7 96.94(18) . . ? P2 Ru5 Ru7 109.86(4) . . ? Ru8 Ru5 Ru7 61.331(15) . . ? C12 Ru5 Ru6 103.73(18) . . ? C11 Ru5 Ru6 148.73(19) . . ? P2 Ru5 Ru6 110.99(4) . . ? Ru8 Ru5 Ru6 62.223(15) . . ? Ru7 Ru5 Ru6 55.807(13) . . ? C12 Ru5 H5 79.5(6) . . ? C11 Ru5 H5 175.0(6) . . ? P2 Ru5 H5 89.9(6) . . ? Ru8 Ru5 H5 86.7(6) . . ? Ru7 Ru5 H5 87.0(5) . . ? Ru6 Ru5 H5 33.7(5) . . ? C12 Ru5 H7 173.2(6) . . ? C11 Ru5 H7 78.2(7) . . ? P2 Ru5 H7 83.2(7) . . ? Ru8 Ru5 H7 89.5(6) . . ? Ru7 Ru5 H7 33.1(5) . . ? Ru6 Ru5 H7 83.1(6) . . ? H5 Ru5 H7 106.6(9) . . ? C13 Ru6 C14 93.5(2) . . ? C13 Ru6 P4 90.73(16) . . ? C14 Ru6 P4 96.52(15) . . ? C13 Ru6 Ru7 87.60(15) . . ? C14 Ru6 Ru7 97.37(15) . . ? P4 Ru6 Ru7 166.08(4) . . ? C13 Ru6 Ru5 148.65(15) . . ? C14 Ru6 Ru5 97.18(17) . . ? P4 Ru6 Ru5 117.05(4) . . ? Ru7 Ru6 Ru5 61.870(14) . . ? C13 Ru6 Ru8 104.88(17) . . ? C14 Ru6 Ru8 150.36(17) . . ? P4 Ru6 Ru8 106.14(4) . . ? Ru7 Ru6 Ru8 61.125(14) . . ? Ru5 Ru6 Ru8 55.615(14) . . ? C13 Ru6 H5 173.8(7) . . ? C14 Ru6 H5 80.4(7) . . ? P4 Ru6 H5 90.3(5) . . ? Ru7 Ru6 H5 92.8(5) . . ? Ru5 Ru6 H5 33.6(5) . . ? Ru8 Ru6 H5 80.7(6) . . ? C13 Ru6 H6 90.5(9) . . ? C14 Ru6 H6 172.6(9) . . ? P4 Ru6 H6 77.1(7) . . ? Ru7 Ru6 H6 89.1(7) . . ? Ru5 Ru6 H6 82.6(6) . . ? Ru8 Ru6 H6 32.8(5) . . ? H5 Ru6 H6 95.7(11) . . ? C16 Ru7 C15 93.0(2) . . ? C16 Ru7 C17 95.5(2) . . ? C15 Ru7 C17 94.8(2) . . ? C16 Ru7 Ru6 86.44(15) . . ? C15 Ru7 Ru6 95.52(15) . . ? C17 Ru7 Ru6 169.36(18) . . ? C16 Ru7 Ru8 148.81(15) . . ? C15 Ru7 Ru8 94.79(17) . . ? C17 Ru7 Ru8 113.83(17) . . ? Ru6 Ru7 Ru8 62.770(14) . . ? C16 Ru7 Ru5 106.46(17) . . ? C15 Ru7 Ru5 148.66(16) . . ? C17 Ru7 Ru5 107.18(18) . . ? Ru6 Ru7 Ru5 62.322(14) . . ? Ru8 Ru7 Ru5 56.203(14) . . ? C16 Ru7 H7 90.3(8) . . ? C15 Ru7 H7 174.2(8) . . ? C17 Ru7 H7 80.1(6) . . ? Ru6 Ru7 H7 89.5(6) . . ? Ru8 Ru7 H7 84.9(6) . . ? Ru5 Ru7 H7 33.5(5) . . ? C16 Ru7 H8 171.2(8) . . ? C15 Ru7 H8 78.2(8) . . ? C17 Ru7 H8 85.7(6) . . ? Ru6 Ru7 H8 94.0(5) . . ? Ru8 Ru7 H8 34.0(5) . . ? Ru5 Ru7 H8 81.4(7) . . ? H7 Ru7 H8 98.6(11) . . ? C19 Ru8 C18 89.4(2) . . ? C19 Ru8 C20 98.2(3) . . ? C18 Ru8 C20 95.0(3) . . ? C19 Ru8 Ru5 90.67(18) . . ? C18 Ru8 Ru5 92.4(2) . . ? C20 Ru8 Ru5 168.5(2) . . ? C19 Ru8 Ru7 149.94(18) . . ? C18 Ru8 Ru7 104.04(18) . . ? C20 Ru8 Ru7 107.1(2) . . ? Ru5 Ru8 Ru7 62.466(15) . . ? C19 Ru8 Ru6 100.73(17) . . ? C18 Ru8 Ru6 152.4(2) . . ? C20 Ru8 Ru6 108.6(2) . . ? Ru5 Ru8 Ru6 62.163(15) . . ? Ru7 Ru8 Ru6 56.105(13) . . ? C19 Ru8 H6 81.4(8) . . ? C18 Ru8 H6 170.7(8) . . ? C20 Ru8 H6 84.9(8) . . ? Ru5 Ru8 H6 89.1(7) . . ? Ru7 Ru8 H6 84.8(6) . . ? Ru6 Ru8 H6 33.3(5) . . ? C19 Ru8 H8 169.1(8) . . ? C18 Ru8 H8 80.0(7) . . ? C20 Ru8 H8 85.4(8) . . ? Ru5 Ru8 H8 87.3(7) . . ? Ru7 Ru8 H8 34.2(5) . . ? Ru6 Ru8 H8 87.7(6) . . ? H6 Ru8 H8 109.2(10) . . ? C21 P1 C27 98.64(13) . . ? C21 P1 C33 102.21(17) . . ? C27 P1 C33 104.64(18) . . ? C21 P1 Ru1 113.55(10) . . ? C27 P1 Ru1 115.57(10) . . ? C33 P1 Ru1 119.45(16) . . ? C46 P2 C36 108.0(2) . . ? C46 P2 C40 104.97(14) . . ? C36 P2 C40 98.48(19) . . ? C46 P2 Ru5 115.05(11) . . ? C36 P2 Ru5 113.37(17) . . ? C40 P2 Ru5 115.41(11) . . ? C52 P3 C58 103.00(13) . . ? C52 P3 C64 106.30(19) . . ? C58 P3 C64 102.23(19) . . ? C52 P3 Ru2 114.75(11) . . ? C58 P3 Ru2 115.33(11) . . ? C64 P3 Ru2 113.82(16) . . ? C77 P4 C71 100.28(16) . . ? C77 P4 C67 101.76(19) . . ? C71 P4 C67 103.59(19) . . ? C77 P4 Ru6 112.73(11) . . ? C71 P4 Ru6 117.06(11) . . ? C67 P4 Ru6 118.81(16) . . ? O1 C1 Ru1 178.1(5) . . ? O2 C2 Ru1 179.4(4) . . ? O3 C3 Ru2 178.2(6) . . ? O4 C4 Ru2 177.4(5) . . ? O5 C5 Ru3 175.9(5) . . ? O6 C6 Ru3 178.1(5) . . ? O7 C7 Ru3 173.2(6) . . ? O8 C8 Ru4 177.6(5) . . ? O9 C9 Ru4 179.7(6) . . ? O10 C10 Ru4 175.2(5) . . ? O11 C11 Ru5 179.1(6) . . ? O12 C12 Ru5 179.6(6) . . ? O13 C13 Ru6 176.7(5) . . ? O14 C14 Ru6 178.4(5) . . ? O15 C15 Ru7 176.6(5) . . ? O16 C16 Ru7 176.9(5) . . ? O17 C17 Ru7 173.9(6) . . ? O18 C18 Ru8 175.8(5) . . ? O19 C19 Ru8 178.1(5) . . ? O20 C20 Ru8 177.4(7) . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 117.15(16) . . ? C26 C21 P1 122.84(16) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 P1 121.24(15) . . ? C32 C27 P1 118.75(15) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C34 C33 P1 112.5(3) . . ? C34 C33 H33A 109.1 . . ? P1 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? P1 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? O34 C34 C33 109.3(4) . . ? O34 C34 C35 103.7(4) . . ? C33 C34 C35 117.5(4) . . ? O34 C34 H34 108.6 . . ? C33 C34 H34 108.7 . . ? C35 C34 H34 108.6 . . ? O35 C35 C36 110.4(4) . . ? O35 C35 C34 102.0(4) . . ? C36 C35 C34 116.5(4) . . ? O35 C35 H35 109.2 . . ? C36 C35 H35 109.2 . . ? C34 C35 H35 109.2 . . ? C34 O34 C37 111.5(4) . . ? C37 O35 C35 108.7(4) . . ? C35 C36 P2 119.1(3) . . ? C35 C36 H36A 107.5 . . ? P2 C36 H36A 107.5 . . ? C35 C36 H36B 107.5 . . ? P2 C36 H36B 107.5 . . ? H36A C36 H36B 107.0 . . ? O35 C37 O34 104.6(4) . . ? O35 C37 C38 109.0(5) . . ? O34 C37 C38 107.8(4) . . ? O35 C37 C39 111.3(5) . . ? O34 C37 C39 109.1(6) . . ? C38 C37 C39 114.6(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 120.0 . . ? C41 C40 P2 122.79(14) . . ? C45 C40 P2 117.14(14) . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C47 C46 C51 120.0 . . ? C47 C46 P2 123.06(17) . . ? C51 C46 P2 116.78(17) . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? C53 C52 C57 120.0 . . ? C53 C52 P3 116.20(16) . . ? C57 C52 P3 123.58(16) . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57 120.0 . . ? C52 C57 H57 120.0 . . ? C59 C58 C63 120.0 . . ? C59 C58 P3 123.17(15) . . ? C63 C58 P3 116.81(15) . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C58 120.0 . . ? C62 C63 H63 120.0 . . ? C58 C63 H63 120.0 . . ? C65 C64 P3 118.7(3) . . ? C65 C64 H64A 107.6 . . ? P3 C64 H64A 107.6 . . ? C65 C64 H64B 107.6 . . ? P3 C64 H64B 107.6 . . ? H64A C64 H64B 107.1 . . ? O65 C65 C66 102.0(4) . . ? O65 C65 C64 107.1(4) . . ? C66 C65 C64 115.2(4) . . ? O65 C65 H65 110.7 . . ? C66 C65 H65 110.7 . . ? C64 C65 H65 110.7 . . ? O66 C66 C67 108.5(4) . . ? O66 C66 C65 102.0(4) . . ? C67 C66 C65 115.5(4) . . ? O66 C66 H66 110.2 . . ? C67 C66 H66 110.2 . . ? C65 C66 H66 110.2 . . ? C68 O65 C65 106.5(4) . . ? C68 O66 C66 110.1(4) . . ? C66 C67 P4 114.1(3) . . ? C66 C67 H67A 108.7 . . ? P4 C67 H67A 108.7 . . ? C66 C67 H67B 108.7 . . ? P4 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? O65 C68 O66 106.2(5) . . ? O65 C68 C70 109.2(6) . . ? O66 C68 C70 109.0(6) . . ? O65 C68 C69 110.4(6) . . ? O66 C68 C69 106.8(6) . . ? C70 C68 C69 114.9(6) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C76 120.0 . . ? C72 C71 P4 120.45(18) . . ? C76 C71 P4 119.33(18) . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? C78 C77 C82 120.0 . . ? C78 C77 P4 122.33(18) . . ? C82 C77 P4 117.61(18) . . ? C77 C78 C79 120.0 . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C80 C79 C78 120.0 . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C79 C80 C81 120.0 . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C82 C81 C80 120.0 . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82 120.0 . . ? C77 C82 H82 120.0 . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 C83 113.6(10) . . ? C85 C84 H84A 108.9 . . ? C83 C84 H84A 108.9 . . ? C85 C84 H84B 108.8 . . ? C83 C84 H84B 108.8 . . ? H84A C84 H84B 107.7 . . ? C84 C85 C86 120.7(10) . . ? C84 C85 H85A 107.1 . . ? C86 C85 H85A 107.1 . . ? C84 C85 H85B 107.2 . . ? C86 C85 H85B 107.2 . . ? H85A C85 H85B 106.8 . . ? C85 C86 C87 113.9(10) . . ? C85 C86 H86A 108.7 . . ? C87 C86 H86A 108.8 . . ? C85 C86 H86B 108.8 . . ? C87 C86 H86B 108.8 . . ? H86A C86 H86B 107.7 . . ? C86 C87 C88 122.0(11) . . ? C86 C87 H87A 106.8 . . ? C88 C87 H87A 106.8 . . ? C86 C87 H87B 106.8 . . ? C88 C87 H87B 106.8 . . ? H87A C87 H87B 106.7 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.4 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C90 C89 H89A 109.5 . . ? C90 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C90 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C89 C90 C91 108.0(8) . . ? C89 C90 H90A 110.1 . . ? C91 C90 H90A 110.1 . . ? C89 C90 H90B 110.1 . . ? C91 C90 H90B 110.1 . . ? H90A C90 H90B 108.4 . . ? C92 C91 C90 113.4(9) . . ? C92 C91 H91A 108.9 . . ? C90 C91 H91A 108.9 . . ? C92 C91 H91B 108.9 . . ? C90 C91 H91B 108.9 . . ? H91A C91 H91B 107.7 . . ? C91 C92 C93 128.3(10) . . ? C91 C92 H92A 105.2 . . ? C93 C92 H92A 105.2 . . ? C91 C92 H92B 105.2 . . ? C93 C92 H92B 105.2 . . ? H92A C92 H92B 105.9 . . ? C92 C93 C94 121.8(10) . . ? C92 C93 H93A 106.9 . . ? C94 C93 H93A 106.9 . . ? C92 C93 H93B 106.9 . . ? C94 C93 H93B 106.9 . . ? H93A C93 H93B 106.7 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.558 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.087 #===END data_[Ru4H4(CO)10(DIPAMP)]_(7) _database_code_depnum_ccdc_archive 'CCDC 287848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 O13 P2 Ru4' _chemical_formula_weight 1162.86 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.8868(4) _cell_length_b 16.0305(6) _cell_length_c 22.8822(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4360.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.492 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57874 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 30.27 _reflns_number_total 13019 _reflns_number_gt 10601 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT+ _computing_structure_solution 'SIR-97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+7.5109P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 13019 _refine_ls_number_parameters 526 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.085 _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 0.88581(3) 0.51193(3) -0.064521(17) 0.03421(9) Uani 1 1 d D . . Ru2 Ru 0.83673(4) 0.58561(3) 0.052276(18) 0.03814(10) Uani 1 1 d D . . Ru3 Ru 0.71269(4) 0.43500(3) 0.017355(19) 0.04103(10) Uani 1 1 d D . . Ru4 Ru 0.93930(4) 0.42897(3) 0.047506(18) 0.03994(10) Uani 1 1 d D . . P2 P 0.92024(11) 0.42389(10) -0.14201(6) 0.0404(3) Uani 1 1 d . . . P1 P 0.81101(12) 0.60137(10) -0.13440(6) 0.0401(3) Uani 1 1 d . . . C2 C 0.9867(6) 0.6264(4) 0.0599(3) 0.0565(15) Uani 1 1 d . . . C4 C 0.8147(6) 0.5820(5) 0.1340(3) 0.0573(16) Uani 1 1 d . . . C3 C 0.7625(6) 0.6912(4) 0.0418(3) 0.0522(15) Uani 1 1 d . . . C9 C 1.0946(5) 0.4590(4) 0.0506(3) 0.0534(14) Uani 1 1 d . . . C8 C 0.9616(5) 0.3129(4) 0.0358(3) 0.0547(16) Uani 1 1 d . . . C10 C 0.9198(6) 0.4173(5) 0.1282(3) 0.0628(18) Uani 1 1 d . . . C1 C 1.0287(5) 0.5584(4) -0.0710(2) 0.0419(12) Uani 1 1 d . . . C6 C 0.7251(5) 0.3215(4) -0.0045(3) 0.0470(13) Uani 1 1 d . . . C7 C 0.6762(6) 0.4062(5) 0.0944(3) 0.0625(18) Uani 1 1 d . . . C5 C 0.5591(6) 0.4486(4) -0.0064(3) 0.0581(16) Uani 1 1 d . . . C11 C 0.9047(5) 0.4824(4) -0.2116(2) 0.0518(15) Uani 1 1 d . . . H11A H 0.9778 0.5037 -0.2231 0.062 Uiso 1 1 calc R . . H11B H 0.8798 0.4441 -0.2418 0.062 Uiso 1 1 calc R . . C12 C 0.8221(5) 0.5552(4) -0.2086(2) 0.0511(15) Uani 1 1 d . . . H12A H 0.7484 0.5360 -0.2208 0.061 Uiso 1 1 calc R . . H12B H 0.8460 0.5981 -0.2358 0.061 Uiso 1 1 calc R . . C13 C 0.6620(5) 0.6308(4) -0.1326(3) 0.0449(12) Uani 1 1 d . . . C14 C 0.5986(5) 0.6230(4) -0.0828(3) 0.0518(15) Uani 1 1 d . . . H14 H 0.6317 0.6024 -0.0489 0.062 Uiso 1 1 calc R . . C15 C 0.4853(6) 0.6454(5) -0.0822(4) 0.0665(19) Uani 1 1 d . . . H15 H 0.4432 0.6408 -0.0481 0.080 Uiso 1 1 calc R . . C16 C 0.4380(7) 0.6738(6) -0.1314(4) 0.083(3) Uani 1 1 d . . . H16 H 0.3616 0.6862 -0.1319 0.100 Uiso 1 1 calc R . . C17 C 0.5011(8) 0.6849(6) -0.1813(4) 0.088(3) Uani 1 1 d . . . H17 H 0.4677 0.7077 -0.2144 0.105 Uiso 1 1 calc R . . C18 C 0.6126(7) 0.6628(5) -0.1828(3) 0.068(2) Uani 1 1 d . . . H18 H 0.6543 0.6692 -0.2169 0.082 Uiso 1 1 calc R . . C19 C 0.8774(5) 0.7047(4) -0.1353(3) 0.0487(14) Uani 1 1 d . . . C20 C 0.8257(7) 0.7712(4) -0.1058(3) 0.0636(18) Uani 1 1 d . . . H20 H 0.7539 0.7645 -0.0904 0.076 Uiso 1 1 calc R . . C21 C 0.8809(8) 0.8467(5) -0.0996(5) 0.087(3) Uani 1 1 d . . . H21 H 0.8469 0.8903 -0.0795 0.104 Uiso 1 1 calc R . . C22 C 0.9849(10) 0.8567(6) -0.1232(5) 0.098(3) Uani 1 1 d . . . H22 H 1.0216 0.9075 -0.1185 0.118 Uiso 1 1 calc R . . C23 C 1.0372(8) 0.7945(7) -0.1535(4) 0.090(3) Uani 1 1 d . . . H23 H 1.1074 0.8032 -0.1704 0.107 Uiso 1 1 calc R . . C24 C 0.9839(6) 0.7189(5) -0.1585(3) 0.0590(18) Uani 1 1 d . . . C25 C 1.1432(9) 0.6567(11) -0.2072(5) 0.146(6) Uani 1 1 d . . . H25A H 1.1645 0.6056 -0.2260 0.218 Uiso 1 1 calc R . . H25B H 1.1920 0.6668 -0.1745 0.218 Uiso 1 1 calc R . . H25C H 1.1493 0.7019 -0.2345 0.218 Uiso 1 1 calc R . . C26 C 0.8367(6) 0.3290(4) -0.1479(3) 0.0512(15) Uani 1 1 d . . . C27 C 0.8820(7) 0.2515(5) -0.1360(3) 0.069(2) Uani 1 1 d . . . H27 H 0.9576 0.2470 -0.1261 0.083 Uiso 1 1 calc R . . C28 C 0.8160(10) 0.1801(5) -0.1386(4) 0.089(3) Uani 1 1 d . . . H28 H 0.8474 0.1285 -0.1299 0.107 Uiso 1 1 calc R . . C29 C 0.7073(8) 0.1853(7) -0.1535(4) 0.085(3) Uani 1 1 d . . . H29 H 0.6646 0.1368 -0.1564 0.102 Uiso 1 1 calc R . . C30 C 0.6580(7) 0.2611(6) -0.1646(3) 0.074(2) Uani 1 1 d . . . H30 H 0.5823 0.2638 -0.1748 0.089 Uiso 1 1 calc R . . C31 C 0.7208(7) 0.3338(5) -0.1606(3) 0.0627(19) Uani 1 1 d . . . C32 C 0.5630(7) 0.4223(7) -0.1786(5) 0.102(3) Uani 1 1 d . . . H32A H 0.5472 0.4805 -0.1842 0.153 Uiso 1 1 calc R . . H32B H 0.5226 0.4023 -0.1451 0.153 Uiso 1 1 calc R . . H32C H 0.5400 0.3916 -0.2126 0.153 Uiso 1 1 calc R . . C33 C 1.0627(5) 0.3812(4) -0.1510(3) 0.0469(13) Uani 1 1 d . . . C34 C 1.0940(6) 0.3496(6) -0.2054(3) 0.074(2) Uani 1 1 d . . . H34 H 1.0437 0.3527 -0.2365 0.089 Uiso 1 1 calc R . . C35 C 1.1996(9) 0.3133(7) -0.2142(5) 0.106(4) Uani 1 1 d . . . H35 H 1.2172 0.2891 -0.2500 0.127 Uiso 1 1 calc R . . C36 C 1.2775(7) 0.3134(6) -0.1695(4) 0.080(2) Uani 1 1 d . . . H36 H 1.3500 0.2934 -0.1756 0.097 Uiso 1 1 calc R . . C37 C 1.2447(6) 0.3446(5) -0.1142(4) 0.068(2) Uani 1 1 d . . . H37 H 1.2948 0.3416 -0.0830 0.082 Uiso 1 1 calc R . . C38 C 1.1421(5) 0.3788(4) -0.1060(3) 0.0531(15) Uani 1 1 d . . . H38 H 1.1238 0.4010 -0.0697 0.064 Uiso 1 1 calc R . . O2 O 1.0736(4) 0.6532(4) 0.0650(3) 0.0875(18) Uani 1 1 d . . . O4 O 0.7966(6) 0.5848(4) 0.1830(2) 0.095(2) Uani 1 1 d . . . O3 O 0.7225(6) 0.7549(3) 0.0369(3) 0.0876(18) Uani 1 1 d . . . O9 O 1.1885(4) 0.4749(3) 0.0512(3) 0.0827(16) Uani 1 1 d . . . O8 O 0.9756(5) 0.2431(3) 0.0316(3) 0.092(2) Uani 1 1 d . . . O10 O 0.9128(6) 0.4055(5) 0.1780(2) 0.111(3) Uani 1 1 d . . . O1 O 1.1184(4) 0.5856(3) -0.0731(2) 0.0611(12) Uani 1 1 d . . . O6 O 0.7279(4) 0.2519(3) -0.0154(2) 0.0668(13) Uani 1 1 d . . . O7 O 0.6485(6) 0.3899(4) 0.1416(3) 0.100(2) Uani 1 1 d . . . O5 O 0.4653(4) 0.4526(4) -0.0169(3) 0.095(2) Uani 1 1 d . . . O11 O 1.0300(4) 0.6504(4) -0.1872(2) 0.0748(16) Uani 1 1 d . . . O12 O 0.6818(4) 0.4110(4) -0.1694(2) 0.0701(14) Uani 1 1 d . . . H3 H 0.946(5) 0.418(2) -0.0326(8) 0.054(18) Uiso 1 1 d D . . H2 H 0.743(3) 0.468(4) -0.0584(11) 0.07(2) Uiso 1 1 d D . . H4 H 0.6940(18) 0.5435(17) 0.040(3) 0.07(2) Uiso 1 1 d D . . H1 H 0.826(9) 0.603(3) -0.0270(8) 0.16(5) Uiso 1 1 d D . . O1W O 0.1088(16) 0.6201(12) 0.1917(8) 0.115(6) Uiso 0.43 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03254(18) 0.0418(2) 0.02829(18) -0.00014(15) -0.00149(15) -0.00080(17) Ru2 0.0404(2) 0.0416(2) 0.0324(2) -0.00278(17) -0.00008(17) 0.00097(17) Ru3 0.0369(2) 0.0466(2) 0.0397(2) 0.00048(19) 0.00227(18) -0.00489(19) Ru4 0.0399(2) 0.0440(2) 0.0359(2) 0.00470(19) -0.00157(17) 0.00271(18) P2 0.0345(7) 0.0508(8) 0.0358(6) -0.0064(6) -0.0009(5) -0.0036(6) P1 0.0370(7) 0.0520(8) 0.0312(6) 0.0032(6) -0.0021(5) -0.0003(6) C2 0.054(4) 0.062(4) 0.054(4) -0.011(3) -0.001(3) -0.004(3) C4 0.062(4) 0.069(4) 0.040(3) 0.002(3) 0.000(3) 0.009(3) C3 0.059(4) 0.056(4) 0.042(3) -0.008(3) -0.004(3) -0.001(3) C9 0.054(4) 0.054(3) 0.051(3) 0.000(3) -0.005(3) 0.001(3) C8 0.039(3) 0.056(4) 0.069(4) 0.005(3) -0.003(3) 0.001(3) C10 0.066(4) 0.079(5) 0.043(3) 0.011(3) 0.001(3) 0.021(4) C1 0.047(3) 0.043(3) 0.036(3) 0.000(2) -0.002(2) 0.003(2) C6 0.036(3) 0.059(4) 0.046(3) 0.007(3) 0.001(2) -0.007(3) C7 0.066(4) 0.066(4) 0.056(4) 0.000(3) 0.014(3) -0.003(4) C5 0.053(4) 0.053(4) 0.068(4) -0.002(3) 0.002(3) -0.005(3) C11 0.048(3) 0.073(4) 0.034(3) -0.007(3) 0.001(2) 0.006(3) C12 0.051(3) 0.068(4) 0.034(3) 0.001(3) -0.004(2) 0.004(3) C13 0.040(3) 0.051(3) 0.044(3) -0.001(2) -0.006(2) 0.004(3) C14 0.047(3) 0.059(4) 0.050(3) -0.001(3) -0.004(3) 0.009(3) C15 0.039(3) 0.084(5) 0.076(5) -0.011(4) 0.003(3) -0.001(3) C16 0.047(4) 0.108(7) 0.095(6) -0.029(5) -0.018(4) 0.011(4) C17 0.086(6) 0.117(8) 0.061(5) -0.010(5) -0.028(5) 0.038(6) C18 0.064(4) 0.089(5) 0.051(4) 0.000(4) -0.013(4) 0.018(4) C19 0.042(3) 0.062(4) 0.043(3) 0.016(3) -0.010(3) -0.004(3) C20 0.071(5) 0.051(4) 0.068(5) 0.000(3) -0.017(4) 0.004(3) C21 0.076(6) 0.065(5) 0.119(8) 0.000(5) -0.026(6) -0.011(5) C22 0.115(9) 0.063(5) 0.117(8) 0.011(6) -0.042(7) -0.022(6) C23 0.074(6) 0.110(8) 0.085(6) 0.041(6) -0.027(5) -0.042(6) C24 0.052(4) 0.079(5) 0.046(4) 0.021(3) -0.008(3) -0.010(4) C25 0.090(8) 0.252(17) 0.095(8) 0.019(10) 0.040(6) -0.017(10) C26 0.052(3) 0.058(4) 0.043(3) -0.014(3) 0.005(3) -0.014(3) C27 0.073(5) 0.065(5) 0.069(5) -0.009(4) 0.008(4) -0.017(4) C28 0.126(9) 0.062(5) 0.079(6) -0.011(4) 0.011(6) -0.021(5) C29 0.078(6) 0.109(8) 0.067(5) -0.019(5) 0.016(4) -0.052(6) C30 0.067(5) 0.098(6) 0.058(4) -0.014(4) 0.011(4) -0.038(5) C31 0.060(4) 0.086(5) 0.043(3) -0.015(3) 0.005(3) -0.027(4) C32 0.050(4) 0.133(9) 0.122(8) -0.021(7) -0.010(5) -0.014(5) C33 0.041(3) 0.049(3) 0.050(3) -0.014(3) 0.000(3) 0.002(3) C34 0.052(4) 0.101(6) 0.068(5) -0.035(4) -0.003(3) 0.014(4) C35 0.087(7) 0.137(9) 0.094(7) -0.056(6) -0.014(5) 0.047(6) C36 0.043(4) 0.090(6) 0.108(7) -0.020(5) 0.005(4) 0.006(4) C37 0.051(4) 0.079(5) 0.075(5) -0.007(4) -0.010(3) 0.013(4) C38 0.046(4) 0.064(4) 0.049(3) -0.004(3) -0.002(3) 0.002(3) O2 0.053(3) 0.084(4) 0.126(5) -0.024(4) -0.003(3) -0.019(3) O4 0.120(5) 0.130(5) 0.036(2) -0.004(3) 0.008(3) 0.027(4) O3 0.122(5) 0.056(3) 0.085(4) -0.004(3) 0.001(4) 0.035(3) O9 0.044(3) 0.085(4) 0.119(5) 0.007(4) -0.015(3) -0.006(2) O8 0.066(3) 0.047(3) 0.162(7) -0.002(3) 0.009(4) 0.006(2) O10 0.142(6) 0.145(6) 0.045(3) 0.021(3) 0.007(3) 0.047(5) O1 0.045(2) 0.071(3) 0.067(3) 0.003(2) -0.007(2) -0.016(2) O6 0.072(3) 0.054(3) 0.074(3) -0.008(2) 0.006(3) -0.011(2) O7 0.117(5) 0.125(5) 0.058(3) 0.006(3) 0.027(3) -0.030(4) O5 0.040(3) 0.085(4) 0.161(6) 0.002(4) -0.019(3) -0.007(3) O11 0.047(3) 0.121(5) 0.056(3) 0.007(3) 0.009(2) -0.019(3) O12 0.045(3) 0.087(4) 0.078(3) -0.016(3) -0.003(2) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.861(6) . ? Ru1 P2 2.3029(15) . ? Ru1 P1 2.3245(15) . ? Ru1 Ru4 2.9570(6) . ? Ru1 Ru2 2.9796(6) . ? Ru1 Ru3 3.0439(6) . ? Ru1 H3 1.815(19) . ? Ru1 H2 1.843(19) . ? Ru1 H1 1.84(2) . ? Ru2 C4 1.889(6) . ? Ru2 C2 1.906(7) . ? Ru2 C3 1.924(7) . ? Ru2 Ru4 2.7935(6) . ? Ru2 Ru3 2.9396(6) . ? Ru2 H4 1.85(2) . ? Ru2 H1 1.84(2) . ? Ru3 C7 1.873(7) . ? Ru3 C6 1.893(7) . ? Ru3 C5 1.917(7) . ? Ru3 Ru4 2.7823(6) . ? Ru3 H2 1.85(2) . ? Ru3 H4 1.830(19) . ? Ru4 C10 1.870(6) . ? Ru4 C8 1.898(7) . ? Ru4 C9 1.909(7) . ? Ru4 H3 1.842(19) . ? P2 C26 1.822(6) . ? P2 C33 1.838(6) . ? P2 C11 1.858(6) . ? P1 C13 1.834(6) . ? P1 C19 1.834(6) . ? P1 C12 1.857(6) . ? C2 O2 1.125(7) . ? C4 O4 1.142(7) . ? C3 O3 1.131(8) . ? C9 O9 1.145(7) . ? C8 O8 1.135(8) . ? C10 O10 1.159(8) . ? C1 O1 1.153(7) . ? C6 O6 1.143(8) . ? C7 O7 1.159(8) . ? C5 O5 1.143(8) . ? C11 C12 1.526(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.372(9) . ? C13 C18 1.388(9) . ? C14 C15 1.394(9) . ? C14 H14 0.9300 . ? C15 C16 1.337(12) . ? C15 H15 0.9300 . ? C16 C17 1.377(13) . ? C16 H16 0.9300 . ? C17 C18 1.372(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.392(9) . ? C19 C20 1.404(10) . ? C20 C21 1.384(11) . ? C20 H20 0.9300 . ? C21 C22 1.358(14) . ? C21 H21 0.9300 . ? C22 C23 1.364(15) . ? C22 H22 0.9300 . ? C23 C24 1.373(11) . ? C23 H23 0.9300 . ? C24 O11 1.391(10) . ? C25 O11 1.425(11) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.382(11) . ? C26 C31 1.410(10) . ? C27 C28 1.388(11) . ? C27 H27 0.9300 . ? C28 C29 1.339(14) . ? C28 H28 0.9300 . ? C29 C30 1.374(14) . ? C29 H29 0.9300 . ? C30 C31 1.387(10) . ? C30 H30 0.9300 . ? C31 O12 1.337(10) . ? C32 O12 1.439(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.395(9) . ? C33 C38 1.398(9) . ? C34 C35 1.398(11) . ? C34 H34 0.9300 . ? C35 C36 1.379(13) . ? C35 H35 0.9300 . ? C36 C37 1.416(11) . ? C36 H36 0.9300 . ? C37 C38 1.351(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P2 91.26(17) . . ? C1 Ru1 P1 92.72(17) . . ? P2 Ru1 P1 85.20(5) . . ? C1 Ru1 Ru4 93.02(17) . . ? P2 Ru1 Ru4 110.71(4) . . ? P1 Ru1 Ru4 162.94(4) . . ? C1 Ru1 Ru2 95.24(17) . . ? P2 Ru1 Ru2 165.54(4) . . ? P1 Ru1 Ru2 107.31(4) . . ? Ru4 Ru1 Ru2 56.139(14) . . ? C1 Ru1 Ru3 145.92(16) . . ? P2 Ru1 Ru3 110.23(4) . . ? P1 Ru1 Ru3 114.50(4) . . ? Ru4 Ru1 Ru3 55.221(14) . . ? Ru2 Ru1 Ru3 58.409(14) . . ? C1 Ru1 H3 90(2) . . ? P2 Ru1 H3 74.6(7) . . ? P1 Ru1 H3 159.6(8) . . ? Ru4 Ru1 H3 36.3(7) . . ? Ru2 Ru1 H3 92.5(7) . . ? Ru3 Ru1 H3 71.5(17) . . ? C1 Ru1 H2 179(2) . . ? P2 Ru1 H2 89.2(17) . . ? P1 Ru1 H2 86.4(13) . . ? Ru4 Ru1 H2 87.6(9) . . ? Ru2 Ru1 H2 84.5(14) . . ? Ru3 Ru1 H2 34.4(7) . . ? H3 Ru1 H2 91(3) . . ? C1 Ru1 H1 94(4) . . ? P2 Ru1 H1 156.3(12) . . ? P1 Ru1 H1 71.5(7) . . ? Ru4 Ru1 H1 92.0(7) . . ? Ru2 Ru1 H1 35.9(7) . . ? Ru3 Ru1 H1 77(3) . . ? H3 Ru1 H1 128.4(10) . . ? H2 Ru1 H1 85(4) . . ? C4 Ru2 C2 92.8(3) . . ? C4 Ru2 C3 95.0(3) . . ? C2 Ru2 C3 98.0(3) . . ? C4 Ru2 Ru4 94.1(2) . . ? C2 Ru2 Ru4 84.5(2) . . ? C3 Ru2 Ru4 170.47(18) . . ? C4 Ru2 Ru3 100.0(2) . . ? C2 Ru2 Ru3 140.8(2) . . ? C3 Ru2 Ru3 117.31(19) . . ? Ru4 Ru2 Ru3 57.998(16) . . ? C4 Ru2 Ru1 154.5(2) . . ? C2 Ru2 Ru1 92.0(2) . . ? C3 Ru2 Ru1 109.09(18) . . ? Ru4 Ru2 Ru1 61.522(14) . . ? Ru3 Ru2 Ru1 61.890(14) . . ? C4 Ru2 H4 91(2) . . ? C2 Ru2 H4 176.3(17) . . ? C3 Ru2 H4 83.2(10) . . ? Ru4 Ru2 H4 93.8(8) . . ? Ru3 Ru2 H4 36.7(6) . . ? Ru1 Ru2 H4 84.3(16) . . ? C4 Ru2 H1 166(2) . . ? C2 Ru2 H1 96(3) . . ? C3 Ru2 H1 73.3(7) . . ? Ru4 Ru2 H1 97.4(7) . . ? Ru3 Ru2 H1 80(3) . . ? Ru1 Ru2 H1 35.8(7) . . ? H4 Ru2 H1 81(4) . . ? C7 Ru3 C6 91.7(3) . . ? C7 Ru3 C5 94.3(3) . . ? C6 Ru3 C5 96.2(3) . . ? C7 Ru3 Ru4 89.0(2) . . ? C6 Ru3 Ru4 87.53(18) . . ? C5 Ru3 Ru4 175.0(2) . . ? C7 Ru3 Ru2 93.6(2) . . ? C6 Ru3 Ru2 145.33(18) . . ? C5 Ru3 Ru2 117.5(2) . . ? Ru4 Ru3 Ru2 58.369(15) . . ? C7 Ru3 Ru1 146.7(2) . . ? C6 Ru3 Ru1 100.04(17) . . ? C5 Ru3 Ru1 115.0(2) . . ? Ru4 Ru3 Ru1 60.803(14) . . ? Ru2 Ru3 Ru1 59.701(14) . . ? C7 Ru3 H2 177(2) . . ? C6 Ru3 H2 91(2) . . ? C5 Ru3 H2 83.6(11) . . ? Ru4 Ru3 H2 93.0(10) . . ? Ru2 Ru3 H2 85.6(14) . . ? Ru1 Ru3 H2 34.4(7) . . ? C7 Ru3 H4 86(2) . . ? C6 Ru3 H4 177.1(13) . . ? C5 Ru3 H4 81.8(9) . . ? Ru4 Ru3 H4 94.6(8) . . ? Ru2 Ru3 H4 37.1(7) . . ? Ru1 Ru3 H4 82.7(16) . . ? H2 Ru3 H4 91(3) . . ? C10 Ru4 C8 93.4(3) . . ? C10 Ru4 C9 96.2(3) . . ? C8 Ru4 C9 96.8(3) . . ? C10 Ru4 Ru3 97.4(2) . . ? C8 Ru4 Ru3 97.71(19) . . ? C9 Ru4 Ru3 159.50(19) . . ? C10 Ru4 Ru2 89.8(2) . . ? C8 Ru4 Ru2 161.34(19) . . ? C9 Ru4 Ru2 101.17(19) . . ? Ru3 Ru4 Ru2 63.634(16) . . ? C10 Ru4 Ru1 150.9(2) . . ? C8 Ru4 Ru1 110.4(2) . . ? C9 Ru4 Ru1 97.3(2) . . ? Ru3 Ru4 Ru1 63.975(15) . . ? Ru2 Ru4 Ru1 62.339(15) . . ? C10 Ru4 H3 168.0(15) . . ? C8 Ru4 H3 76.3(9) . . ? C9 Ru4 H3 91.2(19) . . ? Ru3 Ru4 H3 78.3(17) . . ? Ru2 Ru4 H3 98.1(7) . . ? Ru1 Ru4 H3 35.7(7) . . ? C26 P2 C33 100.6(3) . . ? C26 P2 C11 107.7(3) . . ? C33 P2 C11 100.6(3) . . ? C26 P2 Ru1 118.2(2) . . ? C33 P2 Ru1 118.58(19) . . ? C11 P2 Ru1 109.4(2) . . ? C13 P1 C19 100.6(3) . . ? C13 P1 C12 101.0(3) . . ? C19 P1 C12 108.6(3) . . ? C13 P1 Ru1 120.9(2) . . ? C19 P1 Ru1 113.58(19) . . ? C12 P1 Ru1 110.9(2) . . ? O2 C2 Ru2 177.4(6) . . ? O4 C4 Ru2 175.1(7) . . ? O3 C3 Ru2 177.0(6) . . ? O9 C9 Ru4 177.7(7) . . ? O8 C8 Ru4 176.7(7) . . ? O10 C10 Ru4 175.2(7) . . ? O1 C1 Ru1 177.4(5) . . ? O6 C6 Ru3 176.1(5) . . ? O7 C7 Ru3 176.7(8) . . ? O5 C5 Ru3 174.4(7) . . ? C12 C11 P2 114.3(4) . . ? C12 C11 H11A 108.7 . . ? P2 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? P2 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 P1 113.0(4) . . ? C11 C12 H12A 109.0 . . ? P1 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? P1 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C18 119.3(6) . . ? C14 C13 P1 121.7(5) . . ? C18 C13 P1 119.0(5) . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.1(7) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 120.8(8) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 120.9(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C13 118.9(8) . . ? C17 C18 H18 120.6 . . ? C13 C18 H18 120.6 . . ? C24 C19 C20 117.2(7) . . ? C24 C19 P1 122.9(6) . . ? C20 C19 P1 119.5(5) . . ? C21 C20 C19 120.4(8) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 119.6(10) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 122.0(9) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C24 118.5(9) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 O11 123.7(8) . . ? C23 C24 C19 122.1(9) . . ? O11 C24 C19 114.1(6) . . ? O11 C25 H25A 109.5 . . ? O11 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O11 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 118.1(7) . . ? C27 C26 P2 121.6(6) . . ? C31 C26 P2 120.1(6) . . ? C26 C27 C28 120.8(9) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 120.4(10) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.9(8) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C31 120.1(9) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? O12 C31 C30 125.5(8) . . ? O12 C31 C26 114.9(6) . . ? C30 C31 C26 119.6(9) . . ? O12 C32 H32A 109.5 . . ? O12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 117.9(6) . . ? C34 C33 P2 118.8(5) . . ? C38 C33 P2 123.3(5) . . ? C33 C34 C35 121.2(7) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 119.8(8) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 118.5(8) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C38 C37 C36 121.1(7) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C33 121.2(6) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C24 O11 C25 117.9(9) . . ? C31 O12 C32 118.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 P2 Ru1 P1 128.5(2) . . . . ? C26 P2 Ru1 P1 -109.6(3) . . . . ? C19 P1 Ru1 P2 -123.3(2) . . . . ? C13 P1 Ru1 P2 117.1(2) . . . . ? C24 C19 P1 Ru1 74.8(5) . . . . ? C31 C26 P2 Ru1 68.0(6) . . . . ? C18 C13 P1 Ru1 -161.1(5) . . . . ? C34 C33 P2 Ru1 -160.9(6) . . . . ? C20 C19 P1 Ru1 -97.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.952 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.112 #===END