# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Crochet, Pascale' _publ_contact_author_email crochetpascale@uniovi.es _publ_section_title ; Chiral phosphonite, phosphite and phosphoramidite \"I 6-arene-ruthenium(II) complexes: application to the kinetic resolution of allylic alcohols ; loop_ _publ_author_name M.Fernandez-Zumel B.Lastra-Barreira J.Diez P.Crochet J.Gimeno # Attachment '- 1a_1b_3b_3c.cif' # Chiral phosphonite, phosphite and phosphoramidite \h^6^ arene-ruthenium(II)complexes: # application to the kinetic resolution of allylic alcohols. # Mariano A. Fern\'andez- Zum\'el, Beatriz Lastra-Barreira, Marcus Scheele, # Josefina D\'iez, Pascale Crochet* and Jos\'e Gimeno*. # Departamento de Qu\'imica Org\'anica e Inorg\'anica, Instituto Universitario # de Qu\'imica Organomet\'alica Enrique Moles (Unidad Asociada al CSIC), # Facultad de Qu\'imica, Universidad de Oviedo, E-33071 Oviedo, Spain. # Fax: (+34)-985 10 34 46. E-mail: pascale@fq.uniovi.es (P.C.). #=============================================================================== data_1a _database_code_depnum_ccdc_archive 'CCDC 769455' #TrackingRef '- 1a_1b_3b_3c.cif' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H23 Cl2 O2 P Ru, 0.25(C H2 Cl2)' _chemical_formula_sum 'C32.25 H23.50 Cl2.50 O2 P Ru' _chemical_formula_weight 663.68 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5207(2) _cell_length_b 14.5067(3) _cell_length_c 16.9585(3) _cell_angle_alpha 80.385(1) _cell_angle_beta 89.625(2) _cell_angle_gamma 84.368(1) _cell_volume 2780.79(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8241 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 70.0 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 7.552 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 1.104 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39888 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 70.14 _reflns_number_total 10255 _reflns_number_gt 8729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1004P)^2^+4.9948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10255 _refine_ls_number_parameters 703 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 C1 C 0.2444(4) 0.6786(3) 0.4920(2) 0.0245(9) Uani 1 1 d . . . C2 C 0.3525(4) 0.6328(3) 0.5128(2) 0.0237(8) Uani 1 1 d . . . C3 C 0.3718(4) 0.5442(3) 0.5617(3) 0.0274(9) Uani 1 1 d . . . H3 H 0.4486 0.5145 0.5725 0.033 Uiso 1 1 calc R . . C4 C 0.2772(4) 0.5020(3) 0.5931(3) 0.0295(10) Uani 1 1 d . . . H4 H 0.2882 0.4414 0.6250 0.035 Uiso 1 1 calc R . . C5 C 0.1626(4) 0.5474(3) 0.5788(3) 0.0262(9) Uani 1 1 d . . . C6 C 0.0643(4) 0.5058(3) 0.6135(3) 0.0320(10) Uani 1 1 d . . . H6 H 0.0751 0.4452 0.6455 0.038 Uiso 1 1 calc R . . C7 C -0.0456(4) 0.5505(4) 0.6024(3) 0.0353(11) Uani 1 1 d . . . H7 H -0.1103 0.5212 0.6264 0.042 Uiso 1 1 calc R . . C8 C -0.0628(4) 0.6401(3) 0.5551(3) 0.0317(10) Uani 1 1 d . . . H8 H -0.1391 0.6719 0.5482 0.038 Uiso 1 1 calc R . . C9 C 0.0298(4) 0.6820(3) 0.5190(3) 0.0287(9) Uani 1 1 d . . . H9 H 0.0165 0.7425 0.4871 0.034 Uiso 1 1 calc R . . C10 C 0.1453(4) 0.6370(3) 0.5283(2) 0.0260(9) Uani 1 1 d . . . C11 C 0.2340(4) 0.7694(3) 0.4347(2) 0.0240(9) Uani 1 1 d . . . C12 C 0.2952(4) 0.8428(3) 0.4473(2) 0.0248(9) Uani 1 1 d . . . C13 C 0.2851(4) 0.9309(3) 0.3973(3) 0.0304(10) Uani 1 1 d . . . H13 H 0.3270 0.9801 0.4094 0.036 Uiso 1 1 calc R . . C14 C 0.2142(4) 0.9452(3) 0.3309(3) 0.0311(10) Uani 1 1 d . . . H14 H 0.2062 1.0048 0.2973 0.037 Uiso 1 1 calc R . . C15 C 0.1527(4) 0.8715(3) 0.3119(3) 0.0265(9) Uani 1 1 d . . . C16 C 0.0837(4) 0.8852(3) 0.2419(3) 0.0280(9) Uani 1 1 d . . . H16 H 0.0763 0.9450 0.2085 0.034 Uiso 1 1 calc R . . C17 C 0.0274(4) 0.8141(4) 0.2213(3) 0.0335(11) Uani 1 1 d . . . H17 H -0.0201 0.8247 0.1745 0.040 Uiso 1 1 calc R . . C18 C 0.0404(4) 0.7247(4) 0.2700(3) 0.0317(10) Uani 1 1 d . . . H18 H 0.0032 0.6745 0.2550 0.038 Uiso 1 1 calc R . . C19 C 0.1068(4) 0.7096(3) 0.3396(3) 0.0290(10) Uani 1 1 d . . . H19 H 0.1149 0.6490 0.3717 0.035 Uiso 1 1 calc R . . C20 C 0.1623(4) 0.7825(3) 0.3634(2) 0.0236(8) Uani 1 1 d . . . C21 C 0.5881(4) 0.8072(3) 0.4577(3) 0.0294(9) Uani 1 1 d . . . C22 C 0.5866(5) 0.9027(4) 0.4288(4) 0.0471(13) Uani 1 1 d . . . H22 H 0.5273 0.9459 0.4449 0.057 Uiso 1 1 calc R . . C23 C 0.6727(6) 0.9345(4) 0.3762(4) 0.0599(18) Uani 1 1 d . . . H23 H 0.6724 0.9998 0.3568 0.072 Uiso 1 1 calc R . . C24 C 0.7584(6) 0.8726(5) 0.3517(4) 0.0579(17) Uani 1 1 d . . . H24 H 0.8156 0.8951 0.3147 0.069 Uiso 1 1 calc R . . C25 C 0.7609(5) 0.7780(4) 0.3811(3) 0.0442(13) Uani 1 1 d . . . H25 H 0.8208 0.7353 0.3652 0.053 Uiso 1 1 calc R . . C26 C 0.6768(4) 0.7452(4) 0.4334(3) 0.0318(10) Uani 1 1 d . . . H26 H 0.6789 0.6798 0.4533 0.038 Uiso 1 1 calc R . . C27 C 0.3607(5) 0.7912(4) 0.6991(3) 0.0451(13) Uani 1 1 d . . . H27 H 0.3058 0.8371 0.6698 0.054 Uiso 1 1 calc R . . C28 C 0.4508(5) 0.8192(4) 0.7416(3) 0.0486(15) Uani 1 1 d . . . H28 H 0.4595 0.8841 0.7385 0.058 Uiso 1 1 calc R . . C29 C 0.5299(5) 0.7509(4) 0.7894(3) 0.0477(14) Uani 1 1 d . . . H29 H 0.5876 0.7709 0.8209 0.057 Uiso 1 1 calc R . . C30 C 0.5235(5) 0.6570(4) 0.7906(3) 0.0413(12) Uani 1 1 d . . . H30 H 0.5768 0.6119 0.8224 0.050 Uiso 1 1 calc R . . C31 C 0.4362(5) 0.6269(4) 0.7437(3) 0.0406(12) Uani 1 1 d . . . H31 H 0.4353 0.5620 0.7417 0.049 Uiso 1 1 calc R . . C32 C 0.3505(4) 0.6932(4) 0.6998(3) 0.0400(12) Uani 1 1 d . . . H32 H 0.2889 0.6732 0.6720 0.048 Uiso 1 1 calc R . . C33 C 0.7658(4) 0.2566(3) -0.0780(2) 0.0248(9) Uani 1 1 d . . . C34 C 0.8245(4) 0.3339(3) -0.0735(2) 0.0253(9) Uani 1 1 d . . . C35 C 0.8067(4) 0.4185(3) -0.1283(3) 0.0301(10) Uani 1 1 d . . . H35 H 0.8456 0.4713 -0.1211 0.036 Uiso 1 1 calc R . . C36 C 0.7329(4) 0.4238(4) -0.1919(3) 0.0358(11) Uani 1 1 d . . . H36 H 0.7191 0.4812 -0.2283 0.043 Uiso 1 1 calc R . . C37 C 0.6771(4) 0.3452(3) -0.2043(3) 0.0297(10) Uani 1 1 d . . . C38 C 0.6054(4) 0.3495(4) -0.2722(3) 0.0343(11) Uani 1 1 d . . . H38 H 0.5920 0.4066 -0.3091 0.041 Uiso 1 1 calc R . . C39 C 0.5546(4) 0.2710(4) -0.2851(3) 0.0378(12) Uani 1 1 d . . . H39 H 0.5056 0.2745 -0.3305 0.045 Uiso 1 1 calc R . . C40 C 0.5749(4) 0.1859(4) -0.2316(3) 0.0342(11) Uani 1 1 d . . . H40 H 0.5410 0.1319 -0.2417 0.041 Uiso 1 1 calc R . . C41 C 0.6433(4) 0.1806(3) -0.1648(3) 0.0281(9) Uani 1 1 d . . . H41 H 0.6565 0.1226 -0.1292 0.034 Uiso 1 1 calc R . . C42 C 0.6945(4) 0.2599(3) -0.1483(2) 0.0269(9) Uani 1 1 d . . . C43 C 0.7772(4) 0.1730(3) -0.0135(2) 0.0242(9) Uani 1 1 d . . . C44 C 0.8859(4) 0.1306(3) 0.0117(2) 0.0219(8) Uani 1 1 d . . . C45 C 0.9048(4) 0.0491(3) 0.0692(3) 0.0262(9) Uani 1 1 d . . . H45 H 0.9817 0.0219 0.0833 0.031 Uiso 1 1 calc R . . C46 C 0.8106(4) 0.0096(3) 0.1045(3) 0.0285(9) Uani 1 1 d . . . H46 H 0.8221 -0.0463 0.1429 0.034 Uiso 1 1 calc R . . C47 C 0.6952(4) 0.0514(3) 0.0842(3) 0.0276(9) Uani 1 1 d . . . C48 C 0.5963(4) 0.0129(3) 0.1228(3) 0.0322(10) Uani 1 1 d . . . H48 H 0.6071 -0.0432 0.1610 0.039 Uiso 1 1 calc R . . C49 C 0.4867(4) 0.0554(3) 0.1056(3) 0.0318(10) Uani 1 1 d . . . H49 H 0.4215 0.0281 0.1309 0.038 Uiso 1 1 calc R . . C50 C 0.4700(4) 0.1394(3) 0.0505(3) 0.0298(10) Uani 1 1 d . . . H50 H 0.3934 0.1697 0.0404 0.036 Uiso 1 1 calc R . . C51 C 0.5612(4) 0.1782(3) 0.0115(3) 0.0284(9) Uani 1 1 d . . . H51 H 0.5475 0.2349 -0.0258 0.034 Uiso 1 1 calc R . . C52 C 0.6780(4) 0.1348(3) 0.0260(2) 0.0236(8) Uani 1 1 d . . . C53 C 1.1197(4) 0.2997(3) -0.0654(3) 0.0263(9) Uani 1 1 d . . . C54 C 1.1156(4) 0.3913(4) -0.1054(3) 0.0355(11) Uani 1 1 d . . . H54 H 1.0564 0.4372 -0.0937 0.043 Uiso 1 1 calc R . . C55 C 1.1997(5) 0.4157(4) -0.1635(3) 0.0414(12) Uani 1 1 d . . . H55 H 1.1960 0.4781 -0.1922 0.050 Uiso 1 1 calc R . . C56 C 1.2876(5) 0.3497(4) -0.1790(3) 0.0423(12) Uani 1 1 d . . . H56 H 1.3446 0.3666 -0.2181 0.051 Uiso 1 1 calc R . . C57 C 1.2927(4) 0.2584(4) -0.1373(3) 0.0370(11) Uani 1 1 d . . . H57 H 1.3535 0.2130 -0.1477 0.044 Uiso 1 1 calc R . . C58 C 1.2094(4) 0.2332(3) -0.0805(3) 0.0289(9) Uani 1 1 d . . . H58 H 1.2134 0.1708 -0.0519 0.035 Uiso 1 1 calc R . . C59 C 0.9015(4) 0.3334(4) 0.1719(3) 0.0362(11) Uani 1 1 d . . . H59 H 0.8514 0.3797 0.1387 0.043 Uiso 1 1 calc R . . C60 C 0.9961(5) 0.3597(4) 0.2124(3) 0.0381(11) Uani 1 1 d . . . H60 H 1.0125 0.4235 0.2037 0.046 Uiso 1 1 calc R . . C61 C 1.0676(5) 0.2916(4) 0.2664(3) 0.0366(11) Uani 1 1 d . . . H61 H 1.1284 0.3105 0.2958 0.044 Uiso 1 1 calc R . . C62 C 1.0480(4) 0.1984(4) 0.2754(2) 0.0340(11) Uani 1 1 d . . . H62 H 1.0948 0.1532 0.3119 0.041 Uiso 1 1 calc R . . C63 C 0.9581(4) 0.1690(4) 0.2306(3) 0.0356(11) Uani 1 1 d . . . H63 H 0.9498 0.1040 0.2340 0.043 Uiso 1 1 calc R . . C64 C 0.8814(4) 0.2358(4) 0.1812(3) 0.0387(12) Uani 1 1 d . . . H64 H 0.8177 0.2167 0.1547 0.046 Uiso 1 1 calc R . . C65 C 0.9551(12) -0.0440(9) 0.4855(10) 0.090(6) Uani 0.50 1 d PD . . H65A H 0.9798 -0.0901 0.4502 0.108 Uiso 0.50 1 calc PR . . H65B H 0.8813 -0.0623 0.5109 0.108 Uiso 0.50 1 calc PR . . Cl1 Cl 0.68104(13) 0.82739(9) 0.63006(8) 0.0478(3) Uani 1 1 d . . . Cl2 Cl 0.65515(9) 0.60143(8) 0.62436(6) 0.0308(2) Uani 1 1 d . . . Cl3 Cl 1.22045(11) 0.34239(8) 0.09911(7) 0.0359(3) Uani 1 1 d . . . Cl4 Cl 1.18424(9) 0.11364(7) 0.12396(6) 0.0292(2) Uani 1 1 d . . . Cl5 Cl 0.9291(2) 0.05475(19) 0.43197(13) 0.0928(7) Uani 1 1 d D . . O1 O 0.4512(3) 0.6762(2) 0.48399(17) 0.0235(6) Uani 1 1 d . . . O2 O 0.3666(3) 0.8335(2) 0.51498(17) 0.0261(6) Uani 1 1 d . . . O3 O 0.8983(3) 0.3350(2) -0.00757(17) 0.0253(6) Uani 1 1 d . . . O4 O 0.9842(2) 0.1708(2) -0.02137(17) 0.0226(6) Uani 1 1 d . . . P1 P 0.48343(9) 0.76137(8) 0.52859(6) 0.0233(2) Uani 1 1 d . . . P2 P 1.01599(9) 0.26447(7) 0.01126(6) 0.0219(2) Uani 1 1 d . . . Ru1 Ru 0.52764(3) 0.72796(2) 0.66093(2) 0.02820(13) Uani 1 1 d . . . Ru2 Ru 1.06183(3) 0.25177(2) 0.142588(18) 0.02467(13) Uani 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 C1 0.030(2) 0.027(2) 0.0155(19) -0.0013(16) -0.0033(16) -0.0012(17) C2 0.026(2) 0.025(2) 0.020(2) -0.0025(16) 0.0013(16) -0.0024(16) C3 0.033(2) 0.026(2) 0.023(2) -0.0064(17) -0.0006(18) 0.0000(18) C4 0.038(2) 0.025(2) 0.023(2) 0.0006(17) 0.0043(18) -0.0028(18) C5 0.033(2) 0.027(2) 0.021(2) -0.0079(17) 0.0018(17) -0.0088(18) C6 0.039(3) 0.029(2) 0.029(2) -0.0030(19) 0.003(2) -0.0109(19) C7 0.033(2) 0.043(3) 0.034(3) -0.013(2) 0.008(2) -0.013(2) C8 0.026(2) 0.042(3) 0.029(2) -0.009(2) 0.0015(18) -0.0018(19) C9 0.031(2) 0.034(2) 0.021(2) -0.0048(18) -0.0031(18) -0.0037(19) C10 0.031(2) 0.030(2) 0.017(2) -0.0050(17) 0.0016(17) 0.0000(18) C11 0.024(2) 0.025(2) 0.021(2) -0.0035(17) -0.0021(16) 0.0012(16) C12 0.031(2) 0.026(2) 0.018(2) -0.0048(16) -0.0054(17) -0.0018(17) C13 0.032(2) 0.027(2) 0.031(2) -0.0008(18) -0.0014(19) -0.0030(18) C14 0.034(2) 0.027(2) 0.029(2) 0.0033(18) -0.0041(19) 0.0016(18) C15 0.024(2) 0.032(2) 0.022(2) -0.0022(17) -0.0041(17) 0.0007(17) C16 0.025(2) 0.037(2) 0.020(2) 0.0001(18) -0.0038(17) -0.0027(18) C17 0.028(2) 0.052(3) 0.018(2) -0.002(2) -0.0026(17) 0.006(2) C18 0.028(2) 0.045(3) 0.024(2) -0.010(2) 0.0052(18) -0.009(2) C19 0.033(2) 0.035(2) 0.019(2) -0.0010(18) 0.0000(18) -0.0060(19) C20 0.023(2) 0.030(2) 0.0179(19) -0.0039(17) 0.0018(16) -0.0028(16) C21 0.029(2) 0.033(2) 0.025(2) -0.0008(18) -0.0064(18) -0.0063(18) C22 0.041(3) 0.036(3) 0.061(4) 0.007(3) -0.001(3) -0.007(2) C23 0.051(4) 0.043(3) 0.076(5) 0.023(3) 0.000(3) -0.015(3) C24 0.050(3) 0.074(4) 0.046(3) 0.010(3) 0.008(3) -0.023(3) C25 0.036(3) 0.062(4) 0.035(3) -0.002(3) 0.006(2) -0.014(2) C26 0.028(2) 0.038(3) 0.033(2) -0.011(2) 0.0015(19) -0.0089(19) C27 0.044(3) 0.062(4) 0.029(3) -0.017(2) 0.001(2) 0.013(3) C28 0.066(4) 0.050(3) 0.033(3) -0.026(2) -0.011(3) 0.015(3) C29 0.058(3) 0.062(4) 0.025(3) -0.023(2) -0.012(2) 0.011(3) C30 0.052(3) 0.054(3) 0.013(2) -0.003(2) -0.004(2) 0.009(2) C31 0.043(3) 0.052(3) 0.024(2) 0.002(2) 0.016(2) -0.005(2) C32 0.033(3) 0.061(3) 0.027(2) -0.012(2) 0.003(2) 0.001(2) C33 0.025(2) 0.030(2) 0.019(2) -0.0044(17) -0.0019(16) 0.0006(17) C34 0.030(2) 0.027(2) 0.018(2) -0.0046(17) -0.0039(17) -0.0008(17) C35 0.034(2) 0.027(2) 0.028(2) -0.0026(18) -0.0023(18) 0.0020(18) C36 0.036(3) 0.037(3) 0.028(2) 0.008(2) 0.002(2) 0.003(2) C37 0.029(2) 0.039(3) 0.018(2) 0.0007(18) 0.0022(17) 0.0017(19) C38 0.029(2) 0.053(3) 0.019(2) -0.002(2) 0.0006(18) -0.002(2) C39 0.025(2) 0.068(4) 0.021(2) -0.011(2) -0.0002(18) -0.005(2) C40 0.020(2) 0.059(3) 0.028(2) -0.015(2) 0.0015(18) -0.013(2) C41 0.026(2) 0.038(3) 0.021(2) -0.0060(18) 0.0013(17) -0.0063(18) C42 0.024(2) 0.038(2) 0.017(2) -0.0022(18) 0.0043(16) 0.0002(18) C43 0.027(2) 0.027(2) 0.018(2) -0.0053(16) -0.0039(16) -0.0010(17) C44 0.023(2) 0.025(2) 0.0188(19) -0.0041(16) 0.0011(16) -0.0071(16) C45 0.020(2) 0.029(2) 0.029(2) -0.0063(18) -0.0043(17) -0.0007(17) C46 0.024(2) 0.030(2) 0.030(2) 0.0003(18) -0.0004(18) -0.0011(17) C47 0.033(2) 0.028(2) 0.023(2) -0.0063(18) 0.0034(18) -0.0064(18) C48 0.039(3) 0.026(2) 0.033(2) -0.0051(19) 0.008(2) -0.0061(19) C49 0.026(2) 0.040(3) 0.031(2) -0.005(2) 0.0057(18) -0.0138(19) C50 0.023(2) 0.043(3) 0.025(2) -0.0103(19) 0.0025(17) -0.0039(18) C51 0.028(2) 0.035(2) 0.022(2) -0.0064(18) -0.0028(17) 0.0002(18) C52 0.028(2) 0.024(2) 0.019(2) -0.0040(16) -0.0002(16) -0.0031(16) C53 0.025(2) 0.031(2) 0.025(2) -0.0063(18) -0.0016(17) -0.0055(17) C54 0.035(3) 0.034(3) 0.036(3) -0.002(2) 0.006(2) -0.002(2) C55 0.044(3) 0.030(3) 0.048(3) 0.002(2) 0.015(2) -0.007(2) C56 0.044(3) 0.043(3) 0.038(3) -0.001(2) 0.014(2) -0.007(2) C57 0.037(3) 0.039(3) 0.035(3) -0.009(2) 0.007(2) 0.002(2) C58 0.027(2) 0.032(2) 0.028(2) -0.0046(18) 0.0004(18) -0.0062(18) C59 0.028(2) 0.049(3) 0.031(2) -0.012(2) 0.0021(19) 0.011(2) C60 0.050(3) 0.040(3) 0.028(2) -0.018(2) 0.003(2) 0.004(2) C61 0.050(3) 0.044(3) 0.018(2) -0.012(2) -0.003(2) -0.002(2) C62 0.040(3) 0.050(3) 0.0101(19) -0.0012(19) 0.0010(18) -0.002(2) C63 0.035(3) 0.047(3) 0.025(2) -0.005(2) 0.015(2) -0.010(2) C64 0.035(3) 0.058(3) 0.025(2) -0.013(2) 0.008(2) 0.000(2) C65 0.054(8) 0.089(11) 0.159(17) -0.102(12) -0.001(9) -0.026(7) Cl1 0.0602(8) 0.0397(7) 0.0439(7) 0.0019(5) -0.0238(6) -0.0203(6) Cl2 0.0299(5) 0.0314(5) 0.0278(5) 0.0013(4) 0.0025(4) 0.0026(4) Cl3 0.0423(6) 0.0375(6) 0.0304(6) -0.0062(5) -0.0046(5) -0.0151(5) Cl4 0.0278(5) 0.0295(5) 0.0281(5) -0.0010(4) 0.0014(4) 0.0020(4) Cl5 0.0928(15) 0.1215(19) 0.0655(12) -0.0100(12) 0.0201(11) -0.0292(13) O1 0.0270(15) 0.0233(15) 0.0208(14) -0.0034(11) 0.0007(12) -0.0054(12) O2 0.0289(15) 0.0261(15) 0.0232(15) -0.0051(12) -0.0094(12) 0.0001(12) O3 0.0291(15) 0.0278(16) 0.0185(14) -0.0030(12) -0.0046(12) -0.0007(12) O4 0.0192(14) 0.0245(15) 0.0246(15) -0.0044(12) 0.0018(11) -0.0038(11) P1 0.0248(5) 0.0254(5) 0.0200(5) -0.0038(4) -0.0053(4) -0.0028(4) P2 0.0240(5) 0.0248(5) 0.0171(5) -0.0035(4) -0.0016(4) -0.0031(4) Ru1 0.0332(2) 0.0301(2) 0.0213(2) -0.00634(14) -0.00771(14) 0.00080(15) Ru2 0.0277(2) 0.0285(2) 0.01791(19) -0.00510(13) -0.00223(13) -0.00140(14) _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 C1 C2 1.372(6) . ? C1 C10 1.432(6) . ? C1 C11 1.496(6) . ? C2 O1 1.399(5) . ? C2 C3 1.407(6) . ? C3 C4 1.363(7) . ? C3 H3 0.9500 . ? C4 C5 1.420(7) . ? C4 H4 0.9500 . ? C5 C6 1.414(6) . ? C5 C10 1.429(6) . ? C6 C7 1.364(7) . ? C6 H6 0.9500 . ? C7 C8 1.405(7) . ? C7 H7 0.9500 . ? C8 C9 1.370(7) . ? C8 H8 0.9500 . ? C9 C10 1.421(6) . ? C9 H9 0.9500 . ? C11 C12 1.379(6) . ? C11 C20 1.443(6) . ? C12 O2 1.397(5) . ? C12 C13 1.406(6) . ? C13 C14 1.371(6) . ? C13 H13 0.9500 . ? C14 C15 1.419(7) . ? C14 H14 0.9500 . ? C15 C16 1.408(6) . ? C15 C20 1.428(6) . ? C16 C17 1.365(7) . ? C16 H16 0.9500 . ? C17 C18 1.411(7) . ? C17 H17 0.9500 . ? C18 C19 1.385(6) . ? C18 H18 0.9500 . ? C19 C20 1.403(6) . ? C19 H19 0.9500 . ? C21 C22 1.389(7) . ? C21 C26 1.400(7) . ? C21 P1 1.793(5) . ? C22 C23 1.390(9) . ? C22 H22 0.9500 . ? C23 C24 1.378(10) . ? C23 H23 0.9500 . ? C24 C25 1.377(9) . ? C24 H24 0.9500 . ? C25 C26 1.374(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.397(8) . ? C27 C32 1.435(8) . ? C27 Ru1 2.190(5) . ? C27 H27 0.9500 . ? C28 C29 1.426(8) . ? C28 Ru1 2.182(5) . ? C28 H28 0.9500 . ? C29 C30 1.369(8) . ? C29 Ru1 2.260(5) . ? C29 H29 0.9500 . ? C30 C31 1.430(8) . ? C30 Ru1 2.269(5) . ? C30 H30 0.9500 . ? C31 C32 1.427(7) . ? C31 Ru1 2.196(5) . ? C31 H31 0.9500 . ? C32 Ru1 2.219(5) . ? C32 H32 0.9500 . ? C33 C34 1.379(6) . ? C33 C42 1.443(6) . ? C33 C43 1.488(6) . ? C34 C35 1.408(6) . ? C34 O3 1.412(5) . ? C35 C36 1.365(7) . ? C35 H35 0.9500 . ? C36 C37 1.409(7) . ? C36 H36 0.9500 . ? C37 C38 1.411(6) . ? C37 C42 1.427(6) . ? C38 C39 1.379(8) . ? C38 H38 0.9500 . ? C39 C40 1.405(7) . ? C39 H39 0.9500 . ? C40 C41 1.371(6) . ? C40 H40 0.9500 . ? C41 C42 1.411(7) . ? C41 H41 0.9500 . ? C43 C44 1.377(6) . ? C43 C52 1.433(6) . ? C44 O4 1.397(5) . ? C44 C45 1.400(6) . ? C45 C46 1.365(6) . ? C45 H45 0.9500 . ? C46 C47 1.426(6) . ? C46 H46 0.9500 . ? C47 C48 1.425(7) . ? C47 C52 1.426(6) . ? C48 C49 1.361(7) . ? C48 H48 0.9500 . ? C49 C50 1.404(7) . ? C49 H49 0.9500 . ? C50 C51 1.357(7) . ? C50 H50 0.9500 . ? C51 C52 1.433(6) . ? C51 H51 0.9500 . ? C53 C54 1.384(7) . ? C53 C58 1.396(6) . ? C53 P2 1.804(4) . ? C54 C55 1.404(7) . ? C54 H54 0.9500 . ? C55 C56 1.380(7) . ? C55 H55 0.9500 . ? C56 C57 1.390(7) . ? C56 H56 0.9500 . ? C57 C58 1.386(7) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.408(7) . ? C59 C64 1.441(8) . ? C59 Ru2 2.195(4) . ? C59 H59 0.9500 . ? C60 C61 1.430(7) . ? C60 Ru2 2.191(5) . ? C60 H60 0.9500 . ? C61 C62 1.375(7) . ? C61 Ru2 2.272(4) . ? C61 H61 0.9500 . ? C62 C63 1.428(7) . ? C62 Ru2 2.266(4) . ? C62 H62 0.9500 . ? C63 C64 1.410(7) . ? C63 Ru2 2.181(5) . ? C63 H63 0.9500 . ? C64 Ru2 2.198(5) . ? C64 H64 0.9500 . ? C65 Cl5 1.566(14) . ? C65 Cl5 1.917(14) 2_756 ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? Cl1 Ru1 2.3904(14) . ? Cl2 Ru1 2.3980(11) . ? Cl3 Ru2 2.3962(12) . ? Cl4 Ru2 2.3989(10) . ? Cl5 C65 1.917(14) 2_756 ? O1 P1 1.625(3) . ? O2 P1 1.615(3) . ? O3 P2 1.616(3) . ? O4 P2 1.624(3) . ? P1 Ru1 2.2659(11) . ? P2 Ru2 2.2655(10) . ? 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 C1 C10 117.4(4) . . ? C2 C1 C11 119.9(4) . . ? C10 C1 C11 122.7(4) . . ? C1 C2 O1 118.6(4) . . ? C1 C2 C3 124.4(4) . . ? O1 C2 C3 117.0(4) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.0(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 121.4(4) . . ? C6 C5 C10 118.9(4) . . ? C4 C5 C10 119.7(4) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.4(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 121.4(4) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C5 117.8(4) . . ? C9 C10 C1 123.1(4) . . ? C5 C10 C1 119.1(4) . . ? C12 C11 C20 117.7(4) . . ? C12 C11 C1 120.8(4) . . ? C20 C11 C1 121.4(4) . . ? C11 C12 O2 120.1(4) . . ? C11 C12 C13 123.3(4) . . ? O2 C12 C13 116.5(4) . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 C20 119.8(4) . . ? C14 C15 C20 119.8(4) . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.0(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 118.0(4) . . ? C19 C20 C11 122.8(4) . . ? C15 C20 C11 119.1(4) . . ? C22 C21 C26 119.1(5) . . ? C22 C21 P1 121.9(4) . . ? C26 C21 P1 119.0(4) . . ? C21 C22 C23 119.3(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 121.0(6) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.2(6) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 120.7(5) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 120.3(5) . . ? C28 C27 Ru1 71.1(3) . . ? C32 C27 Ru1 72.1(3) . . ? C28 C27 H27 119.9 . . ? C32 C27 H27 119.9 . . ? Ru1 C27 H27 129.4 . . ? C27 C28 C29 120.5(6) . . ? C27 C28 Ru1 71.7(3) . . ? C29 C28 Ru1 74.3(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? Ru1 C28 H28 126.1 . . ? C30 C29 C28 120.6(5) . . ? C30 C29 Ru1 72.8(3) . . ? C28 C29 Ru1 68.3(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? Ru1 C29 H29 132.2 . . ? C29 C30 C31 119.7(5) . . ? C29 C30 Ru1 72.0(3) . . ? C31 C30 Ru1 68.6(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? Ru1 C30 H30 132.1 . . ? C32 C31 C30 120.9(5) . . ? C32 C31 Ru1 72.0(3) . . ? C30 C31 Ru1 74.1(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? Ru1 C31 H31 126.2 . . ? C31 C32 C27 117.7(5) . . ? C31 C32 Ru1 70.3(3) . . ? C27 C32 Ru1 69.9(3) . . ? C31 C32 H32 121.1 . . ? C27 C32 H32 121.1 . . ? Ru1 C32 H32 131.2 . . ? C34 C33 C42 117.2(4) . . ? C34 C33 C43 121.1(4) . . ? C42 C33 C43 121.7(4) . . ? C33 C34 C35 123.2(4) . . ? C33 C34 O3 120.5(4) . . ? C35 C34 O3 116.0(4) . . ? C36 C35 C34 119.3(4) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.8(4) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 120.7(4) . . ? C36 C37 C42 119.7(4) . . ? C38 C37 C42 119.6(5) . . ? C39 C38 C37 120.1(5) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.6(4) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C41 C40 C39 120.2(5) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 121.1(5) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C41 C42 C37 118.4(4) . . ? C41 C42 C33 122.3(4) . . ? C37 C42 C33 119.3(4) . . ? C44 C43 C52 117.4(4) . . ? C44 C43 C33 120.2(4) . . ? C52 C43 C33 122.3(4) . . ? C43 C44 O4 118.6(4) . . ? C43 C44 C45 124.1(4) . . ? O4 C44 C45 117.3(4) . . ? C46 C45 C44 118.8(4) . . ? C46 C45 H45 120.6 . . ? C44 C45 H45 120.6 . . ? C45 C46 C47 120.5(4) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 121.2(4) . . ? C48 C47 C52 119.1(4) . . ? C46 C47 C52 119.7(4) . . ? C49 C48 C47 120.9(4) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 120.0(4) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 121.3(4) . . ? C51 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C50 C51 C52 120.7(4) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 117.9(4) . . ? C47 C52 C43 119.2(4) . . ? C51 C52 C43 122.9(4) . . ? C54 C53 C58 120.1(4) . . ? C54 C53 P2 121.6(3) . . ? C58 C53 P2 118.2(3) . . ? C53 C54 C55 119.5(4) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 120.3(5) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 119.8(5) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C58 C57 C56 120.3(5) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C57 C58 C53 119.9(4) . . ? C57 C58 H58 120.1 . . ? C53 C58 H58 120.1 . . ? C60 C59 C64 119.4(5) . . ? C60 C59 Ru2 71.1(3) . . ? C64 C59 Ru2 71.0(3) . . ? C60 C59 H59 120.3 . . ? C64 C59 H59 120.3 . . ? Ru2 C59 H59 130.1 . . ? C59 C60 C61 120.8(5) . . ? C59 C60 Ru2 71.4(3) . . ? C61 C60 Ru2 74.4(3) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? Ru2 C60 H60 126.5 . . ? C62 C61 C60 119.6(5) . . ? C62 C61 Ru2 72.1(3) . . ? C60 C61 Ru2 68.3(2) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? Ru2 C61 H61 132.2 . . ? C61 C62 C63 120.7(5) . . ? C61 C62 Ru2 72.6(3) . . ? C63 C62 Ru2 68.0(2) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? Ru2 C62 H62 132.9 . . ? C64 C63 C62 120.6(5) . . ? C64 C63 Ru2 71.9(3) . . ? C62 C63 Ru2 74.5(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? Ru2 C63 H63 125.6 . . ? C63 C64 C59 118.7(5) . . ? C63 C64 Ru2 70.5(3) . . ? C59 C64 Ru2 70.7(3) . . ? C63 C64 H64 120.7 . . ? C59 C64 H64 120.7 . . ? Ru2 C64 H64 130.6 . . ? Cl5 C65 Cl5 116.8(7) . 2_756 ? Cl5 C65 H65A 108.1 . . ? Cl5 C65 H65A 108.1 2_756 . ? Cl5 C65 H65B 108.1 . . ? Cl5 C65 H65B 108.1 2_756 . ? H65A C65 H65B 107.3 . . ? C65 Cl5 C65 63.2(7) . 2_756 ? C2 O1 P1 115.3(3) . . ? C12 O2 P1 122.6(3) . . ? C34 O3 P2 122.7(3) . . ? C44 O4 P2 116.2(3) . . ? O2 P1 O1 102.57(16) . . ? O2 P1 C21 106.91(19) . . ? O1 P1 C21 97.25(19) . . ? O2 P1 Ru1 109.21(12) . . ? O1 P1 Ru1 118.23(11) . . ? C21 P1 Ru1 120.64(15) . . ? O3 P2 O4 102.94(15) . . ? O3 P2 C53 107.37(18) . . ? O4 P2 C53 96.73(18) . . ? O3 P2 Ru2 108.62(11) . . ? O4 P2 Ru2 118.14(11) . . ? C53 P2 Ru2 121.11(14) . . ? C28 Ru1 C27 37.3(2) . . ? C28 Ru1 C31 79.7(2) . . ? C27 Ru1 C31 67.9(2) . . ? C28 Ru1 C32 67.8(2) . . ? C27 Ru1 C32 38.0(2) . . ? C31 Ru1 C32 37.7(2) . . ? C28 Ru1 C29 37.4(2) . . ? C27 Ru1 C29 66.8(2) . . ? C31 Ru1 C29 65.8(2) . . ? C32 Ru1 C29 78.8(2) . . ? C28 Ru1 P1 119.86(15) . . ? C27 Ru1 P1 95.00(14) . . ? C31 Ru1 P1 121.86(15) . . ? C32 Ru1 P1 95.55(13) . . ? C29 Ru1 P1 157.03(15) . . ? C28 Ru1 C30 66.1(2) . . ? C27 Ru1 C30 78.9(2) . . ? C31 Ru1 C30 37.3(2) . . ? C32 Ru1 C30 67.3(2) . . ? C29 Ru1 C30 35.2(2) . . ? P1 Ru1 C30 159.08(16) . . ? C28 Ru1 Cl1 90.38(19) . . ? C27 Ru1 Cl1 117.77(18) . . ? C31 Ru1 Cl1 151.81(15) . . ? C32 Ru1 Cl1 155.75(15) . . ? C29 Ru1 Cl1 90.33(18) . . ? P1 Ru1 Cl1 85.99(4) . . ? C30 Ru1 Cl1 114.64(16) . . ? C28 Ru1 Cl2 155.60(15) . . ? C27 Ru1 Cl2 153.78(17) . . ? C31 Ru1 Cl2 90.11(14) . . ? C32 Ru1 Cl2 115.86(15) . . ? C29 Ru1 Cl2 118.23(14) . . ? P1 Ru1 Cl2 84.37(4) . . ? C30 Ru1 Cl2 92.42(14) . . ? Cl1 Ru1 Cl2 88.38(5) . . ? C63 Ru2 C60 80.0(2) . . ? C63 Ru2 C59 68.2(2) . . ? C60 Ru2 C59 37.45(19) . . ? C63 Ru2 C64 37.57(19) . . ? C60 Ru2 C64 68.2(2) . . ? C59 Ru2 C64 38.3(2) . . ? C63 Ru2 P2 118.63(14) . . ? C60 Ru2 P2 121.32(14) . . ? C59 Ru2 P2 94.70(13) . . ? C64 Ru2 P2 93.41(13) . . ? C63 Ru2 C62 37.41(19) . . ? C60 Ru2 C62 65.87(19) . . ? C59 Ru2 C62 78.74(18) . . ? C64 Ru2 C62 67.01(18) . . ? P2 Ru2 C62 155.90(14) . . ? C63 Ru2 C61 66.31(19) . . ? C60 Ru2 C61 37.32(18) . . ? C59 Ru2 C61 67.05(18) . . ? C64 Ru2 C61 79.18(19) . . ? P2 Ru2 C61 158.62(13) . . ? C62 Ru2 C61 35.28(19) . . ? C63 Ru2 Cl3 154.93(14) . . ? C60 Ru2 Cl3 89.23(15) . . ? C59 Ru2 Cl3 115.11(15) . . ? C64 Ru2 Cl3 153.34(15) . . ? P2 Ru2 Cl3 86.32(4) . . ? C62 Ru2 Cl3 117.54(14) . . ? C61 Ru2 Cl3 91.47(14) . . ? C63 Ru2 Cl4 91.13(14) . . ? C60 Ru2 Cl4 152.94(14) . . ? C59 Ru2 Cl4 156.52(15) . . ? C64 Ru2 Cl4 118.23(15) . . ? P2 Ru2 Cl4 85.41(4) . . ? C62 Ru2 Cl4 91.62(13) . . ? C61 Ru2 Cl4 115.82(13) . . ? Cl3 Ru2 Cl4 88.35(4) . . ? 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 C10 C1 C2 O1 -174.2(4) . . . . ? C11 C1 C2 O1 4.6(6) . . . . ? C10 C1 C2 C3 5.9(6) . . . . ? C11 C1 C2 C3 -175.4(4) . . . . ? C1 C2 C3 C4 -2.6(7) . . . . ? O1 C2 C3 C4 177.5(4) . . . . ? C2 C3 C4 C5 -1.7(7) . . . . ? C3 C4 C5 C6 -177.6(4) . . . . ? C3 C4 C5 C10 2.3(7) . . . . ? C4 C5 C6 C7 177.6(4) . . . . ? C10 C5 C6 C7 -2.3(7) . . . . ? C5 C6 C7 C8 0.1(7) . . . . ? C6 C7 C8 C9 1.3(7) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C5 -1.9(6) . . . . ? C8 C9 C10 C1 -179.6(4) . . . . ? C6 C5 C10 C9 3.2(6) . . . . ? C4 C5 C10 C9 -176.7(4) . . . . ? C6 C5 C10 C1 -179.0(4) . . . . ? C4 C5 C10 C1 1.1(6) . . . . ? C2 C1 C10 C9 172.7(4) . . . . ? C11 C1 C10 C9 -6.0(7) . . . . ? C2 C1 C10 C5 -4.9(6) . . . . ? C11 C1 C10 C5 176.3(4) . . . . ? C2 C1 C11 C12 -52.6(6) . . . . ? C10 C1 C11 C12 126.1(5) . . . . ? C2 C1 C11 C20 125.8(5) . . . . ? C10 C1 C11 C20 -55.5(6) . . . . ? C20 C11 C12 O2 -179.5(4) . . . . ? C1 C11 C12 O2 -1.0(6) . . . . ? C20 C11 C12 C13 4.2(6) . . . . ? C1 C11 C12 C13 -177.3(4) . . . . ? C11 C12 C13 C14 -2.2(7) . . . . ? O2 C12 C13 C14 -178.5(4) . . . . ? C12 C13 C14 C15 -0.9(7) . . . . ? C13 C14 C15 C16 -177.4(4) . . . . ? C13 C14 C15 C20 1.5(7) . . . . ? C14 C15 C16 C17 177.6(4) . . . . ? C20 C15 C16 C17 -1.4(7) . . . . ? C15 C16 C17 C18 -1.3(7) . . . . ? C16 C17 C18 C19 1.9(7) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? C18 C19 C20 C15 -2.8(6) . . . . ? C18 C19 C20 C11 -178.9(4) . . . . ? C16 C15 C20 C19 3.4(6) . . . . ? C14 C15 C20 C19 -175.5(4) . . . . ? C16 C15 C20 C11 179.6(4) . . . . ? C14 C15 C20 C11 0.6(6) . . . . ? C12 C11 C20 C19 172.6(4) . . . . ? C1 C11 C20 C19 -5.9(6) . . . . ? C12 C11 C20 C15 -3.4(6) . . . . ? C1 C11 C20 C15 178.1(4) . . . . ? C26 C21 C22 C23 0.4(8) . . . . ? P1 C21 C22 C23 177.6(5) . . . . ? C21 C22 C23 C24 0.7(10) . . . . ? C22 C23 C24 C25 -1.6(11) . . . . ? C23 C24 C25 C26 1.3(10) . . . . ? C24 C25 C26 C21 -0.2(8) . . . . ? C22 C21 C26 C25 -0.6(7) . . . . ? P1 C21 C26 C25 -177.9(4) . . . . ? C32 C27 C28 C29 -3.4(8) . . . . ? Ru1 C27 C28 C29 -58.2(5) . . . . ? C32 C27 C28 Ru1 54.8(4) . . . . ? C27 C28 C29 C30 4.2(9) . . . . ? Ru1 C28 C29 C30 -52.8(5) . . . . ? C27 C28 C29 Ru1 57.0(5) . . . . ? C28 C29 C30 C31 -0.4(8) . . . . ? Ru1 C29 C30 C31 -51.2(4) . . . . ? C28 C29 C30 Ru1 50.8(5) . . . . ? C29 C30 C31 C32 -4.3(7) . . . . ? Ru1 C30 C31 C32 -57.0(4) . . . . ? C29 C30 C31 Ru1 52.7(5) . . . . ? C30 C31 C32 C27 4.9(7) . . . . ? Ru1 C31 C32 C27 -53.1(4) . . . . ? C30 C31 C32 Ru1 58.0(4) . . . . ? C28 C27 C32 C31 -1.1(7) . . . . ? Ru1 C27 C32 C31 53.2(4) . . . . ? C28 C27 C32 Ru1 -54.3(5) . . . . ? C42 C33 C34 C35 8.1(6) . . . . ? C43 C33 C34 C35 -172.7(4) . . . . ? C42 C33 C34 O3 -178.4(4) . . . . ? C43 C33 C34 O3 0.8(6) . . . . ? C33 C34 C35 C36 -3.8(7) . . . . ? O3 C34 C35 C36 -177.6(4) . . . . ? C34 C35 C36 C37 -1.6(7) . . . . ? C35 C36 C37 C38 -176.9(4) . . . . ? C35 C36 C37 C42 2.2(7) . . . . ? C36 C37 C38 C39 177.7(4) . . . . ? C42 C37 C38 C39 -1.5(7) . . . . ? C37 C38 C39 C40 -0.8(7) . . . . ? C38 C39 C40 C41 1.5(7) . . . . ? C39 C40 C41 C42 0.1(7) . . . . ? C40 C41 C42 C37 -2.4(6) . . . . ? C40 C41 C42 C33 179.3(4) . . . . ? C36 C37 C42 C41 -176.1(4) . . . . ? C38 C37 C42 C41 3.0(6) . . . . ? C36 C37 C42 C33 2.3(6) . . . . ? C38 C37 C42 C33 -178.6(4) . . . . ? C34 C33 C42 C41 171.2(4) . . . . ? C43 C33 C42 C41 -8.1(6) . . . . ? C34 C33 C42 C37 -7.1(6) . . . . ? C43 C33 C42 C37 173.6(4) . . . . ? C34 C33 C43 C44 -52.6(6) . . . . ? C42 C33 C43 C44 126.6(4) . . . . ? C34 C33 C43 C52 126.0(5) . . . . ? C42 C33 C43 C52 -54.8(6) . . . . ? C52 C43 C44 O4 -175.0(4) . . . . ? C33 C43 C44 O4 3.6(6) . . . . ? C52 C43 C44 C45 4.6(6) . . . . ? C33 C43 C44 C45 -176.7(4) . . . . ? C43 C44 C45 C46 -1.6(7) . . . . ? O4 C44 C45 C46 178.0(4) . . . . ? C44 C45 C46 C47 -1.1(7) . . . . ? C45 C46 C47 C48 -177.6(4) . . . . ? C45 C46 C47 C52 0.6(7) . . . . ? C46 C47 C48 C49 177.2(4) . . . . ? C52 C47 C48 C49 -1.0(7) . . . . ? C47 C48 C49 C50 -1.4(7) . . . . ? C48 C49 C50 C51 2.2(7) . . . . ? C49 C50 C51 C52 -0.5(7) . . . . ? C48 C47 C52 C51 2.6(6) . . . . ? C46 C47 C52 C51 -175.7(4) . . . . ? C48 C47 C52 C43 -179.3(4) . . . . ? C46 C47 C52 C43 2.5(6) . . . . ? C50 C51 C52 C47 -1.8(6) . . . . ? C50 C51 C52 C43 -179.9(4) . . . . ? C44 C43 C52 C47 -4.9(6) . . . . ? C33 C43 C52 C47 176.5(4) . . . . ? C44 C43 C52 C51 173.1(4) . . . . ? C33 C43 C52 C51 -5.5(6) . . . . ? C58 C53 C54 C55 2.5(7) . . . . ? P2 C53 C54 C55 178.7(4) . . . . ? C53 C54 C55 C56 -1.8(9) . . . . ? C54 C55 C56 C57 0.3(9) . . . . ? C55 C56 C57 C58 0.4(9) . . . . ? C56 C57 C58 C53 0.3(8) . . . . ? C54 C53 C58 C57 -1.8(7) . . . . ? P2 C53 C58 C57 -178.1(4) . . . . ? C64 C59 C60 C61 -4.0(7) . . . . ? Ru2 C59 C60 C61 -57.9(4) . . . . ? C64 C59 C60 Ru2 54.0(4) . . . . ? C59 C60 C61 C62 3.8(7) . . . . ? Ru2 C60 C61 C62 -52.8(4) . . . . ? C59 C60 C61 Ru2 56.5(4) . . . . ? C60 C61 C62 C63 0.9(7) . . . . ? Ru2 C61 C62 C63 -50.1(4) . . . . ? C60 C61 C62 Ru2 51.0(4) . . . . ? C61 C62 C63 C64 -5.4(7) . . . . ? Ru2 C62 C63 C64 -57.5(4) . . . . ? C61 C62 C63 Ru2 52.1(4) . . . . ? C62 C63 C64 C59 5.1(6) . . . . ? Ru2 C63 C64 C59 -53.7(4) . . . . ? C62 C63 C64 Ru2 58.8(4) . . . . ? C60 C59 C64 C63 -0.5(7) . . . . ? Ru2 C59 C64 C63 53.6(4) . . . . ? C60 C59 C64 Ru2 -54.1(4) . . . . ? Cl5 C65 Cl5 C65 0.000(1) 2_756 . . 2_756 ? C1 C2 O1 P1 76.1(4) . . . . ? C3 C2 O1 P1 -103.9(4) . . . . ? C11 C12 O2 P1 66.7(5) . . . . ? C13 C12 O2 P1 -116.9(4) . . . . ? C33 C34 O3 P2 64.9(5) . . . . ? C35 C34 O3 P2 -121.2(4) . . . . ? C43 C44 O4 P2 76.1(4) . . . . ? C45 C44 O4 P2 -103.5(4) . . . . ? C12 O2 P1 O1 -31.2(3) . . . . ? C12 O2 P1 C21 70.5(4) . . . . ? C12 O2 P1 Ru1 -157.5(3) . . . . ? C2 O1 P1 O2 -58.5(3) . . . . ? C2 O1 P1 C21 -167.7(3) . . . . ? C2 O1 P1 Ru1 61.7(3) . . . . ? C22 C21 P1 O2 27.8(5) . . . . ? C26 C21 P1 O2 -155.0(3) . . . . ? C22 C21 P1 O1 133.4(4) . . . . ? C26 C21 P1 O1 -49.4(4) . . . . ? C22 C21 P1 Ru1 -97.6(4) . . . . ? C26 C21 P1 Ru1 79.6(4) . . . . ? C34 O3 P2 O4 -31.5(3) . . . . ? C34 O3 P2 C53 69.9(4) . . . . ? C34 O3 P2 Ru2 -157.6(3) . . . . ? C44 O4 P2 O3 -57.2(3) . . . . ? C44 O4 P2 C53 -166.8(3) . . . . ? C44 O4 P2 Ru2 62.5(3) . . . . ? C54 C53 P2 O3 26.6(4) . . . . ? C58 C53 P2 O3 -157.2(3) . . . . ? C54 C53 P2 O4 132.4(4) . . . . ? C58 C53 P2 O4 -51.4(4) . . . . ? C54 C53 P2 Ru2 -98.8(4) . . . . ? C58 C53 P2 Ru2 77.4(4) . . . . ? C29 C28 Ru1 C27 130.4(6) . . . . ? C27 C28 Ru1 C31 -67.0(4) . . . . ? C29 C28 Ru1 C31 63.4(4) . . . . ? C27 C28 Ru1 C32 -29.5(4) . . . . ? C29 C28 Ru1 C32 100.9(4) . . . . ? C27 C28 Ru1 C29 -130.4(6) . . . . ? C27 C28 Ru1 P1 53.9(4) . . . . ? C29 C28 Ru1 P1 -175.6(3) . . . . ? C27 C28 Ru1 C30 -103.5(4) . . . . ? C29 C28 Ru1 C30 26.9(4) . . . . ? C27 C28 Ru1 Cl1 139.5(3) . . . . ? C29 C28 Ru1 Cl1 -90.0(4) . . . . ? C27 C28 Ru1 Cl2 -133.5(4) . . . . ? C29 C28 Ru1 Cl2 -3.1(7) . . . . ? C32 C27 Ru1 C28 -132.1(5) . . . . ? C28 C27 Ru1 C31 102.3(4) . . . . ? C32 C27 Ru1 C31 -29.8(3) . . . . ? C28 C27 Ru1 C32 132.1(5) . . . . ? C28 C27 Ru1 C29 30.2(4) . . . . ? C32 C27 Ru1 C29 -101.9(4) . . . . ? C28 C27 Ru1 P1 -135.3(3) . . . . ? C32 C27 Ru1 P1 92.6(3) . . . . ? C28 C27 Ru1 C30 64.9(4) . . . . ? C32 C27 Ru1 C30 -67.2(3) . . . . ? C28 C27 Ru1 Cl1 -47.2(4) . . . . ? C32 C27 Ru1 Cl1 -179.3(2) . . . . ? C28 C27 Ru1 Cl2 137.3(4) . . . . ? C32 C27 Ru1 Cl2 5.2(5) . . . . ? C32 C31 Ru1 C28 67.0(3) . . . . ? C30 C31 Ru1 C28 -63.9(3) . . . . ? C32 C31 Ru1 C27 30.0(3) . . . . ? C30 C31 Ru1 C27 -100.8(3) . . . . ? C30 C31 Ru1 C32 -130.9(5) . . . . ? C32 C31 Ru1 C29 103.5(3) . . . . ? C30 C31 Ru1 C29 -27.3(3) . . . . ? C32 C31 Ru1 P1 -51.9(3) . . . . ? C30 C31 Ru1 P1 177.3(2) . . . . ? C32 C31 Ru1 C30 130.9(5) . . . . ? C32 C31 Ru1 Cl1 137.9(3) . . . . ? C30 C31 Ru1 Cl1 7.1(5) . . . . ? C32 C31 Ru1 Cl2 -135.3(3) . . . . ? C30 C31 Ru1 Cl2 93.9(3) . . . . ? C31 C32 Ru1 C28 -102.1(3) . . . . ? C27 C32 Ru1 C28 29.0(3) . . . . ? C31 C32 Ru1 C27 -131.1(5) . . . . ? C27 C32 Ru1 C31 131.1(5) . . . . ? C31 C32 Ru1 C29 -64.7(3) . . . . ? C27 C32 Ru1 C29 66.5(3) . . . . ? C31 C32 Ru1 P1 137.8(3) . . . . ? C27 C32 Ru1 P1 -91.0(3) . . . . ? C31 C32 Ru1 C30 -29.8(3) . . . . ? C27 C32 Ru1 C30 101.3(3) . . . . ? C31 C32 Ru1 Cl1 -129.6(3) . . . . ? C27 C32 Ru1 Cl1 1.5(5) . . . . ? C31 C32 Ru1 Cl2 51.4(3) . . . . ? C27 C32 Ru1 Cl2 -177.4(2) . . . . ? C30 C29 Ru1 C28 134.1(6) . . . . ? C30 C29 Ru1 C27 104.0(4) . . . . ? C28 C29 Ru1 C27 -30.1(4) . . . . ? C30 C29 Ru1 C31 28.9(3) . . . . ? C28 C29 Ru1 C31 -105.3(4) . . . . ? C30 C29 Ru1 C32 66.2(4) . . . . ? C28 C29 Ru1 C32 -68.0(4) . . . . ? C30 C29 Ru1 P1 143.9(4) . . . . ? C28 C29 Ru1 P1 9.7(7) . . . . ? C28 C29 Ru1 C30 -134.1(6) . . . . ? C30 C29 Ru1 Cl1 -135.7(3) . . . . ? C28 C29 Ru1 Cl1 90.2(4) . . . . ? C30 C29 Ru1 Cl2 -47.3(4) . . . . ? C28 C29 Ru1 Cl2 178.5(3) . . . . ? O2 P1 Ru1 C28 -17.7(3) . . . . ? O1 P1 Ru1 C28 -134.3(2) . . . . ? C21 P1 Ru1 C28 106.7(3) . . . . ? O2 P1 Ru1 C27 11.7(2) . . . . ? O1 P1 Ru1 C27 -104.9(2) . . . . ? C21 P1 Ru1 C27 136.1(3) . . . . ? O2 P1 Ru1 C31 78.8(2) . . . . ? O1 P1 Ru1 C31 -37.9(2) . . . . ? C21 P1 Ru1 C31 -156.8(2) . . . . ? O2 P1 Ru1 C32 49.90(19) . . . . ? O1 P1 Ru1 C32 -66.8(2) . . . . ? C21 P1 Ru1 C32 174.3(2) . . . . ? O2 P1 Ru1 C29 -24.5(5) . . . . ? O1 P1 Ru1 C29 -141.1(5) . . . . ? C21 P1 Ru1 C29 99.9(5) . . . . ? O2 P1 Ru1 C30 83.4(4) . . . . ? O1 P1 Ru1 C30 -33.2(4) . . . . ? C21 P1 Ru1 C30 -152.2(4) . . . . ? O2 P1 Ru1 Cl1 -105.82(13) . . . . ? O1 P1 Ru1 Cl1 137.53(13) . . . . ? C21 P1 Ru1 Cl1 18.54(19) . . . . ? O2 P1 Ru1 Cl2 165.42(13) . . . . ? O1 P1 Ru1 Cl2 48.76(13) . . . . ? C21 P1 Ru1 Cl2 -70.22(19) . . . . ? C29 C30 Ru1 C28 -28.5(4) . . . . ? C31 C30 Ru1 C28 104.9(4) . . . . ? C29 C30 Ru1 C27 -65.3(4) . . . . ? C31 C30 Ru1 C27 68.1(3) . . . . ? C29 C30 Ru1 C31 -133.4(5) . . . . ? C29 C30 Ru1 C32 -103.3(4) . . . . ? C31 C30 Ru1 C32 30.1(3) . . . . ? C31 C30 Ru1 C29 133.4(5) . . . . ? C29 C30 Ru1 P1 -139.9(4) . . . . ? C31 C30 Ru1 P1 -6.5(6) . . . . ? C29 C30 Ru1 Cl1 50.3(4) . . . . ? C31 C30 Ru1 Cl1 -176.3(3) . . . . ? C29 C30 Ru1 Cl2 139.6(3) . . . . ? C31 C30 Ru1 Cl2 -87.0(3) . . . . ? C64 C63 Ru2 C60 67.1(3) . . . . ? C62 C63 Ru2 C60 -63.1(3) . . . . ? C64 C63 Ru2 C59 30.0(3) . . . . ? C62 C63 Ru2 C59 -100.2(3) . . . . ? C62 C63 Ru2 C64 -130.2(5) . . . . ? C64 C63 Ru2 P2 -53.2(3) . . . . ? C62 C63 Ru2 P2 176.6(2) . . . . ? C64 C63 Ru2 C62 130.2(5) . . . . ? C64 C63 Ru2 C61 103.5(3) . . . . ? C62 C63 Ru2 C61 -26.7(3) . . . . ? C64 C63 Ru2 Cl3 132.9(3) . . . . ? C62 C63 Ru2 Cl3 2.7(5) . . . . ? C64 C63 Ru2 Cl4 -138.6(3) . . . . ? C62 C63 Ru2 Cl4 91.2(3) . . . . ? C59 C60 Ru2 C63 -67.1(3) . . . . ? C61 C60 Ru2 C63 63.8(3) . . . . ? C61 C60 Ru2 C59 130.9(5) . . . . ? C59 C60 Ru2 C64 -29.8(3) . . . . ? C61 C60 Ru2 C64 101.1(4) . . . . ? C59 C60 Ru2 P2 50.5(3) . . . . ? C61 C60 Ru2 P2 -178.7(3) . . . . ? C59 C60 Ru2 C62 -103.5(3) . . . . ? C61 C60 Ru2 C62 27.4(3) . . . . ? C59 C60 Ru2 C61 -130.9(5) . . . . ? C59 C60 Ru2 Cl3 135.7(3) . . . . ? C61 C60 Ru2 Cl3 -93.4(3) . . . . ? C59 C60 Ru2 Cl4 -139.5(3) . . . . ? C61 C60 Ru2 Cl4 -8.6(6) . . . . ? C60 C59 Ru2 C63 102.4(3) . . . . ? C64 C59 Ru2 C63 -29.5(3) . . . . ? C64 C59 Ru2 C60 -131.8(4) . . . . ? C60 C59 Ru2 C64 131.8(4) . . . . ? C60 C59 Ru2 P2 -138.6(3) . . . . ? C64 C59 Ru2 P2 89.6(3) . . . . ? C60 C59 Ru2 C62 64.8(3) . . . . ? C64 C59 Ru2 C62 -67.0(3) . . . . ? C60 C59 Ru2 C61 29.8(3) . . . . ? C64 C59 Ru2 C61 -102.0(3) . . . . ? C60 C59 Ru2 Cl3 -50.5(3) . . . . ? C64 C59 Ru2 Cl3 177.7(2) . . . . ? C60 C59 Ru2 Cl4 132.1(3) . . . . ? C64 C59 Ru2 Cl4 0.3(5) . . . . ? C59 C64 Ru2 C63 131.5(4) . . . . ? C63 C64 Ru2 C60 -102.3(3) . . . . ? C59 C64 Ru2 C60 29.2(3) . . . . ? C63 C64 Ru2 C59 -131.5(4) . . . . ? C63 C64 Ru2 P2 135.2(3) . . . . ? C59 C64 Ru2 P2 -93.3(3) . . . . ? C63 C64 Ru2 C62 -30.3(3) . . . . ? C59 C64 Ru2 C62 101.2(3) . . . . ? C63 C64 Ru2 C61 -65.0(3) . . . . ? C59 C64 Ru2 C61 66.5(3) . . . . ? C63 C64 Ru2 Cl3 -136.2(3) . . . . ? C59 C64 Ru2 Cl3 -4.7(5) . . . . ? C63 C64 Ru2 Cl4 48.6(3) . . . . ? C59 C64 Ru2 Cl4 -179.9(2) . . . . ? O3 P2 Ru2 C63 74.1(2) . . . . ? O4 P2 Ru2 C63 -42.5(2) . . . . ? C53 P2 Ru2 C63 -161.1(2) . . . . ? O3 P2 Ru2 C60 -21.7(2) . . . . ? O4 P2 Ru2 C60 -138.3(2) . . . . ? C53 P2 Ru2 C60 103.2(2) . . . . ? O3 P2 Ru2 C59 6.41(19) . . . . ? O4 P2 Ru2 C59 -110.21(19) . . . . ? C53 P2 Ru2 C59 131.2(2) . . . . ? O3 P2 Ru2 C64 44.78(19) . . . . ? O4 P2 Ru2 C64 -71.84(19) . . . . ? C53 P2 Ru2 C64 169.6(2) . . . . ? O3 P2 Ru2 C62 79.2(3) . . . . ? O4 P2 Ru2 C62 -37.4(3) . . . . ? C53 P2 Ru2 C62 -156.0(4) . . . . ? O3 P2 Ru2 C61 -23.9(4) . . . . ? O4 P2 Ru2 C61 -140.5(4) . . . . ? C53 P2 Ru2 C61 100.9(4) . . . . ? O3 P2 Ru2 Cl3 -108.51(13) . . . . ? O4 P2 Ru2 Cl3 134.87(13) . . . . ? C53 P2 Ru2 Cl3 16.32(18) . . . . ? O3 P2 Ru2 Cl4 162.85(13) . . . . ? O4 P2 Ru2 Cl4 46.23(13) . . . . ? C53 P2 Ru2 Cl4 -72.31(18) . . . . ? C61 C62 Ru2 C63 -134.7(5) . . . . ? C61 C62 Ru2 C60 -28.9(3) . . . . ? C63 C62 Ru2 C60 105.8(3) . . . . ? C61 C62 Ru2 C59 -66.0(3) . . . . ? C63 C62 Ru2 C59 68.7(3) . . . . ? C61 C62 Ru2 C64 -104.3(3) . . . . ? C63 C62 Ru2 C64 30.4(3) . . . . ? C61 C62 Ru2 P2 -142.1(3) . . . . ? C63 C62 Ru2 P2 -7.4(5) . . . . ? C63 C62 Ru2 C61 134.7(5) . . . . ? C61 C62 Ru2 Cl3 46.6(3) . . . . ? C63 C62 Ru2 Cl3 -178.7(3) . . . . ? C61 C62 Ru2 Cl4 135.6(3) . . . . ? C63 C62 Ru2 Cl4 -89.7(3) . . . . ? C62 C61 Ru2 C63 28.2(3) . . . . ? C60 C61 Ru2 C63 -105.2(4) . . . . ? C62 C61 Ru2 C60 133.3(5) . . . . ? C62 C61 Ru2 C59 103.4(4) . . . . ? C60 C61 Ru2 C59 -29.9(3) . . . . ? C62 C61 Ru2 C64 65.3(3) . . . . ? C60 C61 Ru2 C64 -68.1(3) . . . . ? C62 C61 Ru2 P2 136.5(3) . . . . ? C60 C61 Ru2 P2 3.2(6) . . . . ? C60 C61 Ru2 C62 -133.3(5) . . . . ? C62 C61 Ru2 Cl3 -139.9(3) . . . . ? C60 C61 Ru2 Cl3 86.8(3) . . . . ? C62 C61 Ru2 Cl4 -51.0(3) . . . . ? C60 C61 Ru2 Cl4 175.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 70.14 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.071 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.157 #===END #=============================================================================== data_1b _database_code_depnum_ccdc_archive 'CCDC 769456' #TrackingRef '- 1a_1b_3b_3c.cif' #=============================================================================== _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H23 Cl2 O3 P Ru, C H2 Cl2' _chemical_formula_sum 'C33 H25 Cl4 O3 P Ru' _chemical_formula_weight 743.37 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8464(4) _cell_length_b 11.4973(3) _cell_length_c 15.3719(5) _cell_angle_alpha 70.902(3) _cell_angle_beta 81.985(3) _cell_angle_gamma 65.405(3) _cell_volume 1495.22(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11080 _cell_measurement_theta_min 3.0420 _cell_measurement_theta_max 73.6011 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 8.325 _exptl_absorpt_correction_T_min 0.72169 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur Nova ; _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15171 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 73.99 _reflns_number_total 5575 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlisPro RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlisPro RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1266P)^2^+2.7167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5575 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1289(6) 0.2668(5) 0.2962(3) 0.0264(10) Uani 1 1 d . . . C2 C 0.0209(6) 0.1870(5) 0.2911(3) 0.0262(10) Uani 1 1 d . . . C3 C 0.1355(6) 0.2303(6) 0.2880(4) 0.0320(11) Uani 1 1 d . . . H3 H 0.2359 0.1728 0.2841 0.038 Uiso 1 1 calc R . . C4 C 0.0992(6) 0.3567(6) 0.2909(4) 0.0330(11) Uani 1 1 d . . . H4 H 0.1755 0.3849 0.2924 0.040 Uiso 1 1 calc R . . C5 C -0.0524(6) 0.4468(5) 0.2914(4) 0.0294(11) Uani 1 1 d . . . C6 C -0.0919(7) 0.5814(6) 0.2902(4) 0.0343(12) Uani 1 1 d . . . H6 H -0.0165 0.6105 0.2919 0.041 Uiso 1 1 calc R . . C7 C -0.2373(7) 0.6683(6) 0.2864(4) 0.0364(12) Uani 1 1 d . . . H7 H -0.2614 0.7573 0.2845 0.044 Uiso 1 1 calc R . . C8 C -0.3525(7) 0.6259(6) 0.2854(4) 0.0376(12) Uani 1 1 d . . . H8 H -0.4528 0.6869 0.2821 0.045 Uiso 1 1 calc R . . C9 C -0.3181(7) 0.4960(6) 0.2891(4) 0.0359(12) Uani 1 1 d . . . H9 H -0.3955 0.4685 0.2885 0.043 Uiso 1 1 calc R . . C10 C -0.1677(6) 0.4022(5) 0.2939(4) 0.0288(11) Uani 1 1 d . . . C11 C -0.2414(5) 0.2099(5) 0.3003(3) 0.0254(10) Uani 1 1 d . . . C12 C -0.2393(6) 0.1536(5) 0.2339(4) 0.0274(10) Uani 1 1 d . . . C13 C -0.3434(6) 0.1000(5) 0.2318(4) 0.0289(10) Uani 1 1 d . . . H13 H -0.3393 0.0630 0.1848 0.035 Uiso 1 1 calc R . . C14 C -0.4503(6) 0.1023(5) 0.2987(4) 0.0309(11) Uani 1 1 d . . . H14 H -0.5208 0.0676 0.2971 0.037 Uiso 1 1 calc R . . C15 C -0.4569(6) 0.1560(5) 0.3701(4) 0.0310(11) Uani 1 1 d . . . C16 C -0.5662(6) 0.1568(6) 0.4416(4) 0.0366(12) Uani 1 1 d . . . H16 H -0.6392 0.1248 0.4400 0.044 Uiso 1 1 calc R . . C17 C -0.5655(7) 0.2035(6) 0.5119(4) 0.0398(13) Uani 1 1 d . . . H17 H -0.6400 0.2061 0.5576 0.048 Uiso 1 1 calc R . . C18 C -0.4556(7) 0.2478(7) 0.5174(4) 0.0410(13) Uani 1 1 d . . . H18 H -0.4544 0.2760 0.5681 0.049 Uiso 1 1 calc R . . C19 C -0.3492(7) 0.2504(6) 0.4496(4) 0.0357(12) Uani 1 1 d . . . H19 H -0.2758 0.2805 0.4541 0.043 Uiso 1 1 calc R . . C20 C -0.3497(6) 0.2078(5) 0.3726(4) 0.0281(10) Uani 1 1 d . . . C21 C 0.0745(6) -0.2004(5) 0.3067(3) 0.0267(10) Uani 1 1 d . . . C22 C 0.2107(6) -0.3035(6) 0.3046(4) 0.0349(12) Uani 1 1 d . . . H22 H 0.2718 -0.3003 0.2519 0.042 Uiso 1 1 calc R . . C23 C 0.2548(7) -0.4131(6) 0.3839(5) 0.0423(14) Uani 1 1 d . . . H23 H 0.3467 -0.4856 0.3847 0.051 Uiso 1 1 calc R . . C24 C 0.1645(8) -0.4159(6) 0.4613(4) 0.0433(14) Uani 1 1 d . . . H24 H 0.1953 -0.4900 0.5144 0.052 Uiso 1 1 calc R . . C25 C 0.0277(8) -0.3086(7) 0.4606(4) 0.0427(14) Uani 1 1 d . . . H25 H -0.0340 -0.3104 0.5131 0.051 Uiso 1 1 calc R . . C26 C -0.0167(7) -0.2000(6) 0.3824(4) 0.0368(12) Uani 1 1 d . . . H26 H -0.1082 -0.1268 0.3813 0.044 Uiso 1 1 calc R . . C27 C 0.2728(7) 0.1603(6) -0.0712(4) 0.0375(12) Uani 1 1 d . . . H27 H 0.3353 0.1168 -0.1129 0.045 Uiso 1 1 calc R . . C28 C 0.1172(7) 0.1870(6) -0.0672(4) 0.0358(12) Uani 1 1 d . . . H28 H 0.0786 0.1550 -0.1028 0.043 Uiso 1 1 calc R . . C29 C 0.0212(6) 0.2618(5) -0.0095(4) 0.0339(12) Uani 1 1 d . . . H29 H -0.0824 0.2860 -0.0106 0.041 Uiso 1 1 calc R . . C30 C 0.0804(7) 0.2995(5) 0.0489(4) 0.0356(12) Uani 1 1 d . . . H30 H 0.0169 0.3483 0.0877 0.043 Uiso 1 1 calc R . . C31 C 0.2362(8) 0.2642(6) 0.0496(4) 0.0397(13) Uani 1 1 d . . . H31 H 0.2767 0.2842 0.0920 0.048 Uiso 1 1 calc R . . C32 C 0.3319(6) 0.1989(6) -0.0133(4) 0.0366(13) Uani 1 1 d . . . H32 H 0.4342 0.1817 -0.0158 0.044 Uiso 1 1 calc R . . C33 C 0.4943(12) 0.5649(10) 0.0952(8) 0.084(3) Uani 1 1 d . . . H33A H 0.4448 0.6191 0.0357 0.101 Uiso 1 1 calc R . . H33B H 0.4935 0.6263 0.1272 0.101 Uiso 1 1 calc R . . Cl1 Cl 0.24316(16) -0.12447(13) 0.04809(10) 0.0360(3) Uani 1 1 d . . . Cl2 Cl 0.38586(14) -0.04245(13) 0.19040(9) 0.0336(3) Uani 1 1 d . . . Cl3 Cl 0.3936(3) 0.4701(3) 0.1608(2) 0.0867(7) Uani 1 1 d . . . Cl4 Cl 0.6779(3) 0.4647(3) 0.07660(18) 0.0815(6) Uani 1 1 d . . . O1 O 0.0607(4) 0.0569(3) 0.2873(2) 0.0267(7) Uani 1 1 d . . . O2 O -0.1311(4) 0.1494(4) 0.1640(2) 0.0264(7) Uani 1 1 d . . . O3 O 0.0226(4) -0.0954(4) 0.2232(2) 0.0285(7) Uani 1 1 d . . . P1 P 0.03777(14) 0.04413(12) 0.18976(8) 0.0241(3) Uani 1 1 d . . . Ru1 Ru 0.19646(4) 0.08332(3) 0.07438(2) 0.02488(17) Uani 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 C1 0.028(2) 0.028(2) 0.031(2) -0.015(2) 0.009(2) -0.016(2) C2 0.029(2) 0.030(2) 0.027(2) -0.013(2) 0.0074(19) -0.019(2) C3 0.027(3) 0.040(3) 0.036(3) -0.018(2) 0.004(2) -0.016(2) C4 0.033(3) 0.041(3) 0.036(3) -0.016(2) 0.006(2) -0.025(2) C5 0.038(3) 0.031(3) 0.029(2) -0.012(2) 0.005(2) -0.021(2) C6 0.049(3) 0.035(3) 0.030(3) -0.012(2) 0.006(2) -0.028(3) C7 0.056(4) 0.026(3) 0.032(3) -0.013(2) 0.006(3) -0.020(2) C8 0.044(3) 0.032(3) 0.036(3) -0.015(2) 0.008(2) -0.014(2) C9 0.036(3) 0.035(3) 0.043(3) -0.021(2) 0.007(2) -0.015(2) C10 0.036(3) 0.029(3) 0.027(2) -0.013(2) 0.009(2) -0.017(2) C11 0.024(2) 0.026(2) 0.030(2) -0.014(2) 0.0083(19) -0.0128(19) C12 0.024(2) 0.026(2) 0.032(3) -0.012(2) 0.007(2) -0.0090(19) C13 0.025(2) 0.032(3) 0.037(3) -0.016(2) 0.002(2) -0.015(2) C14 0.022(2) 0.034(3) 0.043(3) -0.016(2) 0.004(2) -0.014(2) C15 0.025(2) 0.028(2) 0.040(3) -0.015(2) 0.006(2) -0.009(2) C16 0.029(3) 0.035(3) 0.044(3) -0.012(2) 0.009(2) -0.014(2) C17 0.040(3) 0.045(3) 0.038(3) -0.019(3) 0.015(3) -0.020(3) C18 0.045(3) 0.051(3) 0.035(3) -0.026(3) 0.019(3) -0.023(3) C19 0.039(3) 0.039(3) 0.039(3) -0.017(2) 0.006(2) -0.023(2) C20 0.027(2) 0.026(2) 0.035(3) -0.013(2) 0.007(2) -0.013(2) C21 0.030(2) 0.028(2) 0.028(2) -0.012(2) 0.005(2) -0.017(2) C22 0.036(3) 0.032(3) 0.039(3) -0.012(2) 0.008(2) -0.017(2) C23 0.037(3) 0.036(3) 0.050(4) -0.009(3) -0.004(3) -0.012(2) C24 0.054(4) 0.040(3) 0.039(3) -0.007(3) -0.003(3) -0.024(3) C25 0.057(4) 0.047(3) 0.031(3) -0.011(3) 0.008(3) -0.031(3) C26 0.041(3) 0.036(3) 0.039(3) -0.013(2) 0.003(2) -0.020(2) C27 0.042(3) 0.035(3) 0.033(3) -0.010(2) 0.012(2) -0.017(2) C28 0.042(3) 0.037(3) 0.028(3) -0.008(2) 0.003(2) -0.017(2) C29 0.030(3) 0.028(3) 0.036(3) -0.004(2) 0.002(2) -0.009(2) C30 0.038(3) 0.028(3) 0.037(3) -0.010(2) 0.013(2) -0.014(2) C31 0.053(4) 0.029(3) 0.043(3) -0.013(2) 0.005(3) -0.022(3) C32 0.031(3) 0.035(3) 0.045(3) -0.007(2) 0.013(2) -0.021(2) C33 0.070(6) 0.067(6) 0.103(8) -0.008(5) -0.005(5) -0.027(5) Cl1 0.0416(7) 0.0324(6) 0.0419(7) -0.0220(5) 0.0118(6) -0.0174(5) Cl2 0.0266(6) 0.0363(6) 0.0374(7) -0.0135(5) 0.0019(5) -0.0107(5) Cl3 0.0867(16) 0.0846(16) 0.0997(18) -0.0319(14) 0.0265(14) -0.0494(14) Cl4 0.0826(15) 0.0726(14) 0.0803(15) -0.0256(11) 0.0130(12) -0.0240(12) O1 0.0289(18) 0.0265(17) 0.0289(17) -0.0135(14) 0.0035(14) -0.0122(14) O2 0.0238(17) 0.0311(18) 0.0263(17) -0.0137(14) 0.0065(13) -0.0111(14) O3 0.0341(19) 0.0289(18) 0.0279(17) -0.0135(15) 0.0053(15) -0.0155(15) P1 0.0247(6) 0.0243(6) 0.0271(6) -0.0129(5) 0.0063(5) -0.0114(5) Ru1 0.0242(2) 0.0253(2) 0.0284(3) -0.01263(17) 0.00729(16) -0.01174(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 C1 C2 1.382(7) . ? C1 C10 1.429(7) . ? C1 C11 1.488(7) . ? C2 O1 1.399(6) . ? C2 C3 1.400(7) . ? C3 C4 1.359(8) . ? C4 C5 1.420(8) . ? C5 C10 1.419(7) . ? C5 C6 1.424(7) . ? C6 C7 1.358(9) . ? C7 C8 1.412(9) . ? C8 C9 1.371(8) . ? C9 C10 1.418(8) . ? C11 C12 1.370(7) . ? C11 C20 1.431(7) . ? C12 O2 1.401(6) . ? C12 C13 1.408(7) . ? C13 C14 1.364(8) . ? C14 C15 1.406(8) . ? C15 C20 1.421(7) . ? C15 C16 1.426(8) . ? C16 C17 1.358(9) . ? C17 C18 1.396(9) . ? C18 C19 1.373(8) . ? C19 C20 1.423(8) . ? C21 C26 1.368(8) . ? C21 C22 1.376(8) . ? C21 O3 1.421(6) . ? C22 C23 1.396(9) . ? C23 C24 1.382(10) . ? C24 C25 1.396(10) . ? C25 C26 1.380(9) . ? C27 C32 1.395(9) . ? C27 C28 1.428(9) . ? C27 Ru1 2.269(6) . ? C28 C29 1.418(9) . ? C28 Ru1 2.184(6) . ? C29 C30 1.394(9) . ? C29 Ru1 2.189(5) . ? C30 C31 1.415(9) . ? C30 Ru1 2.182(6) . ? C31 C32 1.421(9) . ? C31 Ru1 2.177(6) . ? C32 Ru1 2.272(5) . ? C33 Cl4 1.736(11) . ? C33 Cl3 1.758(10) . ? Cl1 Ru1 2.3975(13) . ? Cl2 Ru1 2.3968(13) . ? O1 P1 1.609(4) . ? O2 P1 1.607(4) . ? O3 P1 1.580(4) . ? P1 Ru1 2.2540(13) . ? 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 C1 C10 117.7(4) . . ? C2 C1 C11 118.9(4) . . ? C10 C1 C11 123.3(5) . . ? C1 C2 O1 118.6(4) . . ? C1 C2 C3 123.4(5) . . ? O1 C2 C3 118.0(5) . . ? C4 C3 C2 118.9(5) . . ? C3 C4 C5 120.9(5) . . ? C10 C5 C4 119.6(5) . . ? C10 C5 C6 118.9(5) . . ? C4 C5 C6 121.5(5) . . ? C7 C6 C5 120.9(5) . . ? C6 C7 C8 120.4(5) . . ? C9 C8 C7 120.0(6) . . ? C8 C9 C10 121.1(5) . . ? C9 C10 C5 118.6(5) . . ? C9 C10 C1 122.1(5) . . ? C5 C10 C1 119.3(5) . . ? C12 C11 C20 118.2(5) . . ? C12 C11 C1 119.1(4) . . ? C20 C11 C1 122.7(4) . . ? C11 C12 O2 119.7(4) . . ? C11 C12 C13 122.7(5) . . ? O2 C12 C13 117.6(5) . . ? C14 C13 C12 119.2(5) . . ? C13 C14 C15 121.1(5) . . ? C14 C15 C20 119.3(5) . . ? C14 C15 C16 121.8(5) . . ? C20 C15 C16 118.9(5) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 120.9(5) . . ? C19 C18 C17 120.7(6) . . ? C18 C19 C20 120.2(5) . . ? C15 C20 C19 118.7(5) . . ? C15 C20 C11 119.4(5) . . ? C19 C20 C11 121.8(5) . . ? C26 C21 C22 123.2(5) . . ? C26 C21 O3 119.1(5) . . ? C22 C21 O3 117.5(5) . . ? C21 C22 C23 117.5(5) . . ? C24 C23 C22 120.6(6) . . ? C23 C24 C25 120.0(6) . . ? C26 C25 C24 119.7(6) . . ? C21 C26 C25 119.0(6) . . ? C32 C27 C28 120.0(6) . . ? C32 C27 Ru1 72.2(3) . . ? C28 C27 Ru1 68.1(3) . . ? C29 C28 C27 119.8(6) . . ? C29 C28 Ru1 71.3(3) . . ? C27 C28 Ru1 74.5(3) . . ? C30 C29 C28 120.1(5) . . ? C30 C29 Ru1 71.1(3) . . ? C28 C29 Ru1 70.9(3) . . ? C29 C30 C31 119.8(6) . . ? C29 C30 Ru1 71.7(3) . . ? C31 C30 Ru1 70.9(3) . . ? C30 C31 C32 120.6(6) . . ? C30 C31 Ru1 71.2(3) . . ? C32 C31 Ru1 75.0(3) . . ? C27 C32 C31 119.4(5) . . ? C27 C32 Ru1 72.0(3) . . ? C31 C32 Ru1 67.8(3) . . ? Cl4 C33 Cl3 112.2(6) . . ? C2 O1 P1 116.1(3) . . ? C12 O2 P1 118.2(3) . . ? C21 O3 P1 128.2(3) . . ? O3 P1 O2 102.78(19) . . ? O3 P1 O1 99.86(19) . . ? O2 P1 O1 102.62(19) . . ? O3 P1 Ru1 120.06(15) . . ? O2 P1 Ru1 111.23(14) . . ? O1 P1 Ru1 117.88(14) . . ? C31 Ru1 C30 37.9(2) . . ? C31 Ru1 C28 80.1(2) . . ? C30 Ru1 C28 67.8(2) . . ? C31 Ru1 C29 67.6(2) . . ? C30 Ru1 C29 37.2(2) . . ? C28 Ru1 C29 37.8(2) . . ? C31 Ru1 P1 116.73(17) . . ? C30 Ru1 P1 91.49(15) . . ? C28 Ru1 P1 120.70(16) . . ? C29 Ru1 P1 93.38(15) . . ? C31 Ru1 C27 66.3(2) . . ? C30 Ru1 C27 78.9(2) . . ? C28 Ru1 C27 37.4(2) . . ? C29 Ru1 C27 67.0(2) . . ? P1 Ru1 C27 158.04(17) . . ? C31 Ru1 C32 37.2(2) . . ? C30 Ru1 C32 67.1(2) . . ? C28 Ru1 C32 66.5(2) . . ? C29 Ru1 C32 78.8(2) . . ? P1 Ru1 C32 153.78(17) . . ? C27 Ru1 C32 35.8(2) . . ? C31 Ru1 Cl2 92.05(18) . . ? C30 Ru1 Cl2 119.28(17) . . ? C28 Ru1 Cl2 153.90(16) . . ? C29 Ru1 Cl2 156.47(17) . . ? P1 Ru1 Cl2 85.10(5) . . ? C27 Ru1 Cl2 116.85(16) . . ? C32 Ru1 Cl2 92.25(16) . . ? C31 Ru1 Cl1 152.96(18) . . ? C30 Ru1 Cl1 153.38(17) . . ? C28 Ru1 Cl1 88.61(16) . . ? C29 Ru1 Cl1 116.17(16) . . ? P1 Ru1 Cl1 90.17(5) . . ? C27 Ru1 Cl1 89.95(16) . . ? C32 Ru1 Cl1 115.80(16) . . ? Cl2 Ru1 Cl1 87.34(5) . . ? 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 C10 C1 C2 O1 -176.0(4) . . . . ? C11 C1 C2 O1 1.8(7) . . . . ? C10 C1 C2 C3 3.0(8) . . . . ? C11 C1 C2 C3 -179.2(5) . . . . ? C1 C2 C3 C4 0.5(8) . . . . ? O1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C5 -3.6(8) . . . . ? C3 C4 C5 C10 3.2(8) . . . . ? C3 C4 C5 C6 -177.1(5) . . . . ? C10 C5 C6 C7 -3.4(8) . . . . ? C4 C5 C6 C7 176.9(5) . . . . ? C5 C6 C7 C8 1.1(8) . . . . ? C6 C7 C8 C9 0.7(9) . . . . ? C7 C8 C9 C10 -0.2(9) . . . . ? C8 C9 C10 C5 -2.2(8) . . . . ? C8 C9 C10 C1 -178.8(5) . . . . ? C4 C5 C10 C9 -176.5(5) . . . . ? C6 C5 C10 C9 3.9(8) . . . . ? C4 C5 C10 C1 0.3(8) . . . . ? C6 C5 C10 C1 -179.3(5) . . . . ? C2 C1 C10 C9 173.4(5) . . . . ? C11 C1 C10 C9 -4.4(8) . . . . ? C2 C1 C10 C5 -3.3(7) . . . . ? C11 C1 C10 C5 179.0(5) . . . . ? C2 C1 C11 C12 -53.8(7) . . . . ? C10 C1 C11 C12 124.0(6) . . . . ? C2 C1 C11 C20 124.3(5) . . . . ? C10 C1 C11 C20 -58.0(7) . . . . ? C20 C11 C12 O2 -177.6(4) . . . . ? C1 C11 C12 O2 0.5(7) . . . . ? C20 C11 C12 C13 3.1(8) . . . . ? C1 C11 C12 C13 -178.8(5) . . . . ? C11 C12 C13 C14 -0.7(8) . . . . ? O2 C12 C13 C14 180.0(4) . . . . ? C12 C13 C14 C15 -0.7(8) . . . . ? C13 C14 C15 C20 -0.3(8) . . . . ? C13 C14 C15 C16 -178.8(5) . . . . ? C14 C15 C16 C17 176.9(6) . . . . ? C20 C15 C16 C17 -1.5(8) . . . . ? C15 C16 C17 C18 -2.0(9) . . . . ? C16 C17 C18 C19 2.8(10) . . . . ? C17 C18 C19 C20 -0.1(10) . . . . ? C14 C15 C20 C19 -174.3(5) . . . . ? C16 C15 C20 C19 4.1(8) . . . . ? C14 C15 C20 C11 2.8(8) . . . . ? C16 C15 C20 C11 -178.8(5) . . . . ? C18 C19 C20 C15 -3.4(8) . . . . ? C18 C19 C20 C11 179.6(5) . . . . ? C12 C11 C20 C15 -4.1(7) . . . . ? C1 C11 C20 C15 177.8(5) . . . . ? C12 C11 C20 C19 172.9(5) . . . . ? C1 C11 C20 C19 -5.2(8) . . . . ? C26 C21 C22 C23 1.2(8) . . . . ? O3 C21 C22 C23 -173.7(5) . . . . ? C21 C22 C23 C24 -0.6(9) . . . . ? C22 C23 C24 C25 0.2(10) . . . . ? C23 C24 C25 C26 -0.1(10) . . . . ? C22 C21 C26 C25 -1.1(9) . . . . ? O3 C21 C26 C25 173.6(5) . . . . ? C24 C25 C26 C21 0.6(9) . . . . ? C32 C27 C28 C29 4.9(8) . . . . ? Ru1 C27 C28 C29 57.2(5) . . . . ? C32 C27 C28 Ru1 -52.3(5) . . . . ? C27 C28 C29 C30 -5.4(8) . . . . ? Ru1 C28 C29 C30 53.4(5) . . . . ? C27 C28 C29 Ru1 -58.8(5) . . . . ? C28 C29 C30 C31 0.7(8) . . . . ? Ru1 C29 C30 C31 54.0(5) . . . . ? C28 C29 C30 Ru1 -53.3(5) . . . . ? C29 C30 C31 C32 4.5(8) . . . . ? Ru1 C30 C31 C32 58.9(5) . . . . ? C29 C30 C31 Ru1 -54.4(5) . . . . ? C28 C27 C32 C31 0.2(8) . . . . ? Ru1 C27 C32 C31 -50.2(5) . . . . ? C28 C27 C32 Ru1 50.4(5) . . . . ? C30 C31 C32 C27 -4.9(8) . . . . ? Ru1 C31 C32 C27 52.1(5) . . . . ? C30 C31 C32 Ru1 -57.0(5) . . . . ? C1 C2 O1 P1 76.6(5) . . . . ? C3 C2 O1 P1 -102.5(5) . . . . ? C11 C12 O2 P1 73.6(5) . . . . ? C13 C12 O2 P1 -107.0(5) . . . . ? C26 C21 O3 P1 89.0(6) . . . . ? C22 C21 O3 P1 -95.9(5) . . . . ? C21 O3 P1 O2 -127.9(4) . . . . ? C21 O3 P1 O1 -22.4(4) . . . . ? C21 O3 P1 Ru1 108.0(4) . . . . ? C12 O2 P1 O3 61.1(4) . . . . ? C12 O2 P1 O1 -42.2(4) . . . . ? C12 O2 P1 Ru1 -169.1(3) . . . . ? C2 O1 P1 O3 -155.8(3) . . . . ? C2 O1 P1 O2 -50.2(4) . . . . ? C2 O1 P1 Ru1 72.4(3) . . . . ? C32 C31 Ru1 C30 -130.3(6) . . . . ? C30 C31 Ru1 C28 66.4(4) . . . . ? C32 C31 Ru1 C28 -63.9(4) . . . . ? C30 C31 Ru1 C29 29.1(4) . . . . ? C32 C31 Ru1 C29 -101.2(4) . . . . ? C30 C31 Ru1 P1 -53.1(4) . . . . ? C32 C31 Ru1 P1 176.6(3) . . . . ? C30 C31 Ru1 C27 102.8(4) . . . . ? C32 C31 Ru1 C27 -27.5(4) . . . . ? C30 C31 Ru1 C32 130.3(6) . . . . ? C30 C31 Ru1 Cl2 -138.7(3) . . . . ? C32 C31 Ru1 Cl2 91.0(3) . . . . ? C30 C31 Ru1 Cl1 133.2(4) . . . . ? C32 C31 Ru1 Cl1 2.9(6) . . . . ? C29 C30 Ru1 C31 132.0(5) . . . . ? C29 C30 Ru1 C28 29.1(3) . . . . ? C31 C30 Ru1 C28 -102.9(4) . . . . ? C31 C30 Ru1 C29 -132.0(5) . . . . ? C29 C30 Ru1 P1 -93.6(3) . . . . ? C31 C30 Ru1 P1 134.4(3) . . . . ? C29 C30 Ru1 C27 66.5(4) . . . . ? C31 C30 Ru1 C27 -65.5(4) . . . . ? C29 C30 Ru1 C32 102.0(4) . . . . ? C31 C30 Ru1 C32 -30.0(4) . . . . ? C29 C30 Ru1 Cl2 -178.8(3) . . . . ? C31 C30 Ru1 Cl2 49.2(4) . . . . ? C29 C30 Ru1 Cl1 -0.3(6) . . . . ? C31 C30 Ru1 Cl1 -132.3(4) . . . . ? C29 C28 Ru1 C31 -66.1(4) . . . . ? C27 C28 Ru1 C31 63.6(4) . . . . ? C29 C28 Ru1 C30 -28.7(3) . . . . ? C27 C28 Ru1 C30 101.0(4) . . . . ? C27 C28 Ru1 C29 129.6(5) . . . . ? C29 C28 Ru1 P1 49.3(4) . . . . ? C27 C28 Ru1 P1 178.9(3) . . . . ? C29 C28 Ru1 C27 -129.6(5) . . . . ? C29 C28 Ru1 C32 -102.3(4) . . . . ? C27 C28 Ru1 C32 27.3(3) . . . . ? C29 C28 Ru1 Cl2 -140.3(3) . . . . ? C27 C28 Ru1 Cl2 -10.7(6) . . . . ? C29 C28 Ru1 Cl1 138.6(3) . . . . ? C27 C28 Ru1 Cl1 -91.7(3) . . . . ? C30 C29 Ru1 C31 -29.6(3) . . . . ? C28 C29 Ru1 C31 103.2(4) . . . . ? C28 C29 Ru1 C30 132.7(5) . . . . ? C30 C29 Ru1 C28 -132.7(5) . . . . ? C30 C29 Ru1 P1 88.0(3) . . . . ? C28 C29 Ru1 P1 -139.3(3) . . . . ? C30 C29 Ru1 C27 -102.2(4) . . . . ? C28 C29 Ru1 C27 30.5(3) . . . . ? C30 C29 Ru1 C32 -66.7(4) . . . . ? C28 C29 Ru1 C32 66.0(4) . . . . ? C30 C29 Ru1 Cl2 2.5(6) . . . . ? C28 C29 Ru1 Cl2 135.3(4) . . . . ? C30 C29 Ru1 Cl1 179.9(3) . . . . ? C28 C29 Ru1 Cl1 -47.4(4) . . . . ? O3 P1 Ru1 C31 -170.0(3) . . . . ? O2 P1 Ru1 C31 70.1(2) . . . . ? O1 P1 Ru1 C31 -48.0(3) . . . . ? O3 P1 Ru1 C30 160.6(2) . . . . ? O2 P1 Ru1 C30 40.7(2) . . . . ? O1 P1 Ru1 C30 -77.4(2) . . . . ? O3 P1 Ru1 C28 95.6(2) . . . . ? O2 P1 Ru1 C28 -24.3(2) . . . . ? O1 P1 Ru1 C28 -142.4(2) . . . . ? O3 P1 Ru1 C29 123.4(2) . . . . ? O2 P1 Ru1 C29 3.5(2) . . . . ? O1 P1 Ru1 C29 -114.6(2) . . . . ? O3 P1 Ru1 C27 97.5(5) . . . . ? O2 P1 Ru1 C27 -22.5(5) . . . . ? O1 P1 Ru1 C27 -140.5(4) . . . . ? O3 P1 Ru1 C32 -165.3(4) . . . . ? O2 P1 Ru1 C32 74.8(4) . . . . ? O1 P1 Ru1 C32 -43.3(4) . . . . ? O3 P1 Ru1 Cl2 -80.16(17) . . . . ? O2 P1 Ru1 Cl2 159.91(15) . . . . ? O1 P1 Ru1 Cl2 41.84(16) . . . . ? O3 P1 Ru1 Cl1 7.16(17) . . . . ? O2 P1 Ru1 Cl1 -112.77(15) . . . . ? O1 P1 Ru1 Cl1 129.16(16) . . . . ? C32 C27 Ru1 C31 28.5(4) . . . . ? C28 C27 Ru1 C31 -105.5(4) . . . . ? C32 C27 Ru1 C30 66.1(4) . . . . ? C28 C27 Ru1 C30 -67.9(4) . . . . ? C32 C27 Ru1 C28 134.0(5) . . . . ? C32 C27 Ru1 C29 103.2(4) . . . . ? C28 C27 Ru1 C29 -30.9(4) . . . . ? C32 C27 Ru1 P1 131.5(4) . . . . ? C28 C27 Ru1 P1 -2.6(7) . . . . ? C28 C27 Ru1 C32 -134.0(5) . . . . ? C32 C27 Ru1 Cl2 -51.2(4) . . . . ? C28 C27 Ru1 Cl2 174.8(3) . . . . ? C32 C27 Ru1 Cl1 -138.2(3) . . . . ? C28 C27 Ru1 Cl1 87.8(3) . . . . ? C27 C32 Ru1 C31 -133.7(5) . . . . ? C27 C32 Ru1 C30 -103.1(4) . . . . ? C31 C32 Ru1 C30 30.5(4) . . . . ? C27 C32 Ru1 C28 -28.4(4) . . . . ? C31 C32 Ru1 C28 105.3(4) . . . . ? C27 C32 Ru1 C29 -66.0(4) . . . . ? C31 C32 Ru1 C29 67.6(4) . . . . ? C27 C32 Ru1 P1 -140.6(4) . . . . ? C31 C32 Ru1 P1 -7.0(6) . . . . ? C31 C32 Ru1 C27 133.7(5) . . . . ? C27 C32 Ru1 Cl2 135.9(3) . . . . ? C31 C32 Ru1 Cl2 -90.4(4) . . . . ? C27 C32 Ru1 Cl1 47.8(4) . . . . ? C31 C32 Ru1 Cl1 -178.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 73.99 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.191 _refine_diff_density_min -2.214 _refine_diff_density_rms 0.169 #===END #=============================================================================== data_3b _database_code_depnum_ccdc_archive 'CCDC 769457' #TrackingRef '- 1a_1b_3b_3c.cif' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H29 Cl2 O3 P Ru' _chemical_formula_sum 'C35 H29 Cl2 O3 P Ru' _chemical_formula_weight 700.52 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 13.4193(3) _cell_length_b 18.7656(2) _cell_length_c 11.9365(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3005.86(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3071 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18991 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2896 _reflns_number_gt 2505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 2896 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3789(4) 0.0771(3) -0.3002(5) 0.0322(13) Uani 1 1 d . . . C2 C 0.3721(4) 0.0484(3) -0.1945(5) 0.0342(14) Uani 1 1 d . . . C3 C 0.3761(5) -0.0257(4) -0.1749(7) 0.0455(17) Uani 1 1 d . . . H3 H 0.3728 -0.0439 -0.1025 0.055 Uiso 1 1 calc R . . C4 C 0.3847(5) -0.0696(4) -0.2641(8) 0.0472(18) Uani 1 1 d . . . H4 H 0.3909 -0.1183 -0.2517 0.057 Uiso 1 1 calc R . . C5 C 0.3847(5) -0.0444(4) -0.3742(7) 0.0437(18) Uani 1 1 d . . . C6 C 0.3894(6) -0.0900(3) -0.4708(8) 0.050(3) Uani 1 1 d . . . H6 H 0.3990 -0.1386 -0.4606 0.061 Uiso 1 1 calc R . . C7 C 0.3805(6) -0.0645(5) -0.5750(8) 0.055(2) Uani 1 1 d . . . H7 H 0.3811 -0.0960 -0.6352 0.065 Uiso 1 1 calc R . . C8 C 0.3703(5) 0.0088(4) -0.5949(7) 0.047(2) Uani 1 1 d . . . H8 H 0.3639 0.0263 -0.6675 0.057 Uiso 1 1 calc R . . C9 C 0.3699(4) 0.0543(3) -0.5042(8) 0.0414(15) Uani 1 1 d . . . H9 H 0.3634 0.1030 -0.5168 0.050 Uiso 1 1 calc R . . C10 C 0.3788(5) 0.0303(4) -0.3949(6) 0.0377(16) Uani 1 1 d . . . C11 C 0.3833(5) 0.1559(3) -0.3135(5) 0.0343(14) Uani 1 1 d . . . C12 C 0.3132(5) 0.1986(3) -0.2663(5) 0.0374(14) Uani 1 1 d . . . C13 C 0.3102(6) 0.2730(3) -0.2802(6) 0.0472(17) Uani 1 1 d . . . H13 H 0.2602 0.3002 -0.2473 0.057 Uiso 1 1 calc R . . C14 C 0.3832(6) 0.3041(4) -0.3434(7) 0.0519(19) Uani 1 1 d . . . H14 H 0.3795 0.3527 -0.3585 0.062 Uiso 1 1 calc R . . C15 C 0.4633(6) 0.2648(3) -0.3860(6) 0.0468(17) Uani 1 1 d . . . C16 C 0.5463(7) 0.2972(4) -0.4409(7) 0.064(2) Uani 1 1 d . . . H16 H 0.5467 0.3463 -0.4521 0.077 Uiso 1 1 calc R . . C17 C 0.6257(6) 0.2569(5) -0.4775(9) 0.069(3) Uani 1 1 d . . . H17 H 0.6794 0.2791 -0.5123 0.083 Uiso 1 1 calc R . . C18 C 0.6261(5) 0.1845(5) -0.4629(7) 0.059(2) Uani 1 1 d . . . H18 H 0.6798 0.1577 -0.4885 0.071 Uiso 1 1 calc R . . C19 C 0.5482(5) 0.1514(4) -0.4113(6) 0.0451(16) Uani 1 1 d . . . H19 H 0.5505 0.1023 -0.4013 0.054 Uiso 1 1 calc R . . C20 C 0.4647(5) 0.1892(3) -0.3725(5) 0.0390(15) Uani 1 1 d . . . C21 C 0.3324(5) 0.2197(3) 0.0866(5) 0.0342(13) Uani 1 1 d . . . C22 C 0.3790(5) 0.1697(4) 0.1538(6) 0.0442(16) Uani 1 1 d . . . H22 H 0.3928 0.1245 0.1260 0.053 Uiso 1 1 calc R . . C23 C 0.4045(6) 0.1872(4) 0.2617(7) 0.057(2) Uani 1 1 d . . . H23 H 0.4365 0.1540 0.3070 0.069 Uiso 1 1 calc R . . C24 C 0.3826(6) 0.2544(5) 0.3028(7) 0.065(2) Uani 1 1 d . . . H24 H 0.3993 0.2658 0.3763 0.078 Uiso 1 1 calc R . . C25 C 0.3362(6) 0.3046(4) 0.2362(7) 0.058(2) Uani 1 1 d . . . H25 H 0.3214 0.3496 0.2645 0.070 Uiso 1 1 calc R . . C26 C 0.3119(5) 0.2874(4) 0.1271(6) 0.0468(17) Uani 1 1 d . . . H26 H 0.2820 0.3211 0.0809 0.056 Uiso 1 1 calc R . . C27 C 0.0751(5) 0.1307(4) 0.1655(6) 0.0442(15) Uani 1 1 d . . . C28 C 0.0845(5) 0.1859(3) 0.0881(6) 0.0359(14) Uani 1 1 d . . . H28 H 0.1219 0.2258 0.1075 0.043 Uiso 1 1 calc R . . C29 C 0.0388(4) 0.1835(3) -0.0198(6) 0.0381(16) Uani 1 1 d . . . C30 C -0.0173(5) 0.1225(3) -0.0476(7) 0.0456(17) Uani 1 1 d . . . H30 H -0.0421 0.1173 -0.1199 0.055 Uiso 1 1 calc R . . C31 C -0.0369(5) 0.0677(3) 0.0356(7) 0.051(2) Uani 1 1 d . . . C32 C 0.0106(5) 0.0723(4) 0.1377(7) 0.0485(18) Uani 1 1 d . . . H32 H 0.0006 0.0365 0.1903 0.058 Uiso 1 1 calc R . . C33 C 0.1281(6) 0.1358(5) 0.2759(7) 0.067(2) Uani 1 1 d . . . H33A H 0.1626 0.1806 0.2804 0.101 Uiso 1 1 calc R . . H33B H 0.1752 0.0975 0.2822 0.101 Uiso 1 1 calc R . . H33C H 0.0805 0.1327 0.3357 0.101 Uiso 1 1 calc R . . C34 C 0.0498(5) 0.2432(3) -0.1026(6) 0.0502(17) Uani 1 1 d . . . H34A H -0.0049 0.2757 -0.0945 0.075 Uiso 1 1 calc R . . H34B H 0.0502 0.2242 -0.1772 0.075 Uiso 1 1 calc R . . H34C H 0.1113 0.2679 -0.0889 0.075 Uiso 1 1 calc R . . C35 C -0.1050(6) 0.0062(4) 0.0095(13) 0.082(3) Uani 1 1 d . . . H35A H -0.1104 -0.0241 0.0740 0.123 Uiso 1 1 calc R . . H35B H -0.0784 -0.0206 -0.0522 0.123 Uiso 1 1 calc R . . H35C H -0.1698 0.0240 -0.0101 0.123 Uiso 1 1 calc R . . Cl1 Cl 0.24208(14) 0.00747(9) 0.10468(17) 0.0527(5) Uani 1 1 d . . . Cl2 Cl 0.12917(13) -0.00121(12) -0.1415(2) 0.0628(6) Uani 1 1 d . . . O1 O 0.3646(3) 0.0930(2) -0.1016(4) 0.0363(10) Uani 1 1 d . . . O2 O 0.2363(3) 0.1668(2) -0.2015(3) 0.0363(10) Uani 1 1 d . . . O3 O 0.3078(3) 0.2071(2) -0.0253(3) 0.0398(11) Uani 1 1 d . . . P1 P 0.26210(11) 0.13588(8) -0.08011(14) 0.0325(3) Uani 1 1 d . . . Ru1 Ru 0.13093(3) 0.08580(2) 0.00465(5) 0.03172(15) Uani 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 C1 0.032(3) 0.037(3) 0.028(3) -0.001(2) 0.003(2) -0.001(2) C2 0.027(3) 0.041(4) 0.034(3) 0.002(3) 0.003(3) 0.004(2) C3 0.040(4) 0.049(4) 0.048(4) 0.010(3) 0.006(3) 0.009(3) C4 0.045(4) 0.035(3) 0.062(5) 0.004(3) 0.005(4) 0.003(3) C5 0.035(4) 0.045(4) 0.051(4) -0.009(3) 0.006(3) -0.002(3) C6 0.042(4) 0.031(3) 0.078(9) -0.014(3) 0.005(4) 0.003(2) C7 0.056(5) 0.054(5) 0.053(5) -0.022(5) 0.007(4) -0.009(4) C8 0.045(4) 0.059(5) 0.038(4) -0.012(4) 0.002(3) -0.012(3) C9 0.042(3) 0.043(3) 0.040(4) -0.004(4) 0.002(3) -0.007(2) C10 0.035(4) 0.039(3) 0.039(4) -0.005(3) 0.005(3) -0.005(3) C11 0.043(3) 0.037(3) 0.023(3) -0.002(3) -0.002(3) -0.008(3) C12 0.048(4) 0.039(3) 0.025(3) -0.001(3) -0.001(3) 0.002(3) C13 0.064(5) 0.044(4) 0.034(4) 0.000(3) -0.009(3) 0.011(3) C14 0.076(5) 0.037(4) 0.043(4) 0.008(3) -0.015(4) -0.009(3) C15 0.066(5) 0.045(4) 0.029(3) 0.009(3) -0.009(3) -0.017(3) C16 0.089(7) 0.057(4) 0.047(4) 0.021(4) -0.019(5) -0.036(4) C17 0.059(5) 0.099(7) 0.048(7) 0.019(5) 0.000(4) -0.028(5) C18 0.049(4) 0.075(5) 0.054(6) -0.002(4) 0.003(3) -0.022(3) C19 0.041(4) 0.059(4) 0.035(4) -0.007(3) 0.000(3) -0.013(3) C20 0.052(4) 0.042(3) 0.024(3) -0.001(3) -0.005(3) -0.012(3) C21 0.029(3) 0.039(3) 0.034(3) -0.003(3) 0.003(3) -0.005(3) C22 0.044(4) 0.045(4) 0.043(4) 0.003(3) 0.001(3) 0.001(3) C23 0.058(5) 0.070(5) 0.045(4) 0.012(4) -0.009(4) -0.001(4) C24 0.064(5) 0.093(7) 0.037(4) -0.010(4) -0.003(4) -0.027(5) C25 0.056(4) 0.058(5) 0.061(5) -0.027(4) 0.013(4) -0.017(4) C26 0.043(4) 0.045(4) 0.052(4) -0.004(3) -0.001(3) -0.003(3) C27 0.045(4) 0.053(4) 0.034(4) -0.005(3) 0.013(3) 0.003(3) C28 0.032(3) 0.034(3) 0.042(4) -0.010(3) 0.008(3) 0.003(2) C29 0.028(3) 0.039(3) 0.048(5) -0.010(3) 0.003(3) 0.005(2) C30 0.029(3) 0.051(4) 0.057(4) -0.017(3) -0.008(3) 0.005(3) C31 0.025(3) 0.045(4) 0.081(7) -0.015(3) 0.009(3) -0.002(3) C32 0.041(4) 0.049(4) 0.055(5) 0.003(3) 0.021(4) -0.006(3) C33 0.085(6) 0.089(6) 0.027(4) -0.002(4) 0.010(4) 0.005(4) C34 0.051(4) 0.049(4) 0.050(4) 0.006(3) 0.002(3) 0.013(3) C35 0.051(4) 0.057(4) 0.136(9) -0.020(7) -0.009(7) -0.018(3) Cl1 0.0560(11) 0.0484(9) 0.0538(11) 0.0100(8) -0.0019(9) 0.0097(8) Cl2 0.0485(10) 0.0688(12) 0.0710(14) -0.0432(11) -0.0032(10) -0.0007(8) O1 0.029(2) 0.051(3) 0.029(2) 0.0017(18) 0.0000(17) 0.0065(17) O2 0.036(2) 0.045(2) 0.028(2) 0.0024(18) -0.0021(18) 0.0050(18) O3 0.046(3) 0.042(2) 0.031(3) -0.0013(17) 0.0008(19) -0.011(2) P1 0.0314(8) 0.0401(8) 0.0261(7) -0.0027(7) 0.0006(7) 0.0003(6) Ru1 0.0296(2) 0.0334(2) 0.0322(2) -0.0049(2) 0.0008(3) -0.00136(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 C1 C2 1.374(9) . ? C1 C10 1.431(10) . ? C1 C11 1.489(8) . ? C2 O1 1.393(8) . ? C2 C3 1.412(9) . ? C3 C4 1.351(12) . ? C3 H3 0.9300 . ? C4 C5 1.397(12) . ? C4 H4 0.9300 . ? C5 C10 1.426(11) . ? C5 C6 1.437(11) . ? C6 C7 1.337(15) . ? C6 H6 0.9300 . ? C7 C8 1.403(12) . ? C7 H7 0.9300 . ? C8 C9 1.380(11) . ? C8 H8 0.9300 . ? C9 C10 1.385(12) . ? C9 H9 0.9300 . ? C11 C12 1.358(9) . ? C11 C20 1.442(9) . ? C12 C13 1.406(9) . ? C12 O2 1.421(8) . ? C13 C14 1.367(10) . ? C13 H13 0.9300 . ? C14 C15 1.400(11) . ? C14 H14 0.9300 . ? C15 C16 1.428(11) . ? C15 C20 1.428(9) . ? C16 C17 1.377(12) . ? C16 H16 0.9300 . ? C17 C18 1.371(11) . ? C17 H17 0.9300 . ? C18 C19 1.363(9) . ? C18 H18 0.9300 . ? C19 C20 1.405(9) . ? C19 H19 0.9300 . ? C21 C22 1.383(10) . ? C21 C26 1.387(9) . ? C21 O3 1.396(8) . ? C22 C23 1.373(12) . ? C22 H22 0.9300 . ? C23 C24 1.384(11) . ? C23 H23 0.9300 . ? C24 C25 1.383(12) . ? C24 H24 0.9300 . ? C25 C26 1.381(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.393(9) . ? C27 C32 1.435(10) . ? C27 C33 1.500(11) . ? C27 Ru1 2.227(6) . ? C28 C29 1.428(10) . ? C28 Ru1 2.216(5) . ? C28 H28 0.9300 . ? C29 C30 1.410(8) . ? C29 C34 1.501(9) . ? C29 Ru1 2.230(6) . ? C30 C31 1.453(11) . ? C30 Ru1 2.196(6) . ? C30 H30 0.9300 . ? C31 C32 1.379(11) . ? C31 C35 1.505(9) . ? C31 Ru1 2.307(6) . ? C32 Ru1 2.279(7) . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? Cl1 Ru1 2.4106(18) . ? Cl2 Ru1 2.3894(18) . ? O1 P1 1.614(4) . ? O2 P1 1.599(4) . ? O3 P1 1.609(4) . ? P1 Ru1 2.2372(16) . ? 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 C1 C10 119.0(6) . . ? C2 C1 C11 119.3(6) . . ? C10 C1 C11 121.7(6) . . ? C1 C2 O1 120.0(5) . . ? C1 C2 C3 122.4(6) . . ? O1 C2 C3 117.6(6) . . ? C4 C3 C2 118.2(7) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 122.4(7) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C10 119.7(7) . . ? C4 C5 C6 123.6(7) . . ? C10 C5 C6 116.6(7) . . ? C7 C6 C5 122.0(6) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 121.1(8) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 118.3(8) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 122.5(7) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C9 C10 C5 119.2(6) . . ? C9 C10 C1 123.0(7) . . ? C5 C10 C1 117.8(7) . . ? C12 C11 C20 118.2(6) . . ? C12 C11 C1 120.9(6) . . ? C20 C11 C1 120.8(6) . . ? C11 C12 C13 123.8(6) . . ? C11 C12 O2 118.8(5) . . ? C13 C12 O2 117.4(6) . . ? C14 C13 C12 118.0(7) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C13 C14 C15 121.7(6) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 122.7(7) . . ? C14 C15 C20 119.5(6) . . ? C16 C15 C20 117.7(7) . . ? C17 C16 C15 121.0(7) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C16 120.5(8) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.4(8) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 122.1(7) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C15 118.3(6) . . ? C19 C20 C11 123.2(6) . . ? C15 C20 C11 118.4(6) . . ? C22 C21 C26 120.6(7) . . ? C22 C21 O3 123.1(6) . . ? C26 C21 O3 116.2(6) . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 119.9(8) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.8(8) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 119.3(7) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 119.7(7) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C28 C27 C32 118.0(7) . . ? C28 C27 C33 119.5(7) . . ? C32 C27 C33 122.5(7) . . ? C28 C27 Ru1 71.3(4) . . ? C32 C27 Ru1 73.4(4) . . ? C33 C27 Ru1 128.4(5) . . ? C27 C28 C29 122.4(6) . . ? C27 C28 Ru1 72.1(3) . . ? C29 C28 Ru1 71.8(3) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? Ru1 C28 H28 130.0 . . ? C30 C29 C28 117.9(6) . . ? C30 C29 C34 120.3(6) . . ? C28 C29 C34 121.8(5) . . ? C30 C29 Ru1 70.1(3) . . ? C28 C29 Ru1 70.7(3) . . ? C34 C29 Ru1 130.2(4) . . ? C29 C30 C31 120.7(7) . . ? C29 C30 Ru1 72.8(3) . . ? C31 C30 Ru1 75.4(4) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? Ru1 C30 H30 123.7 . . ? C32 C31 C30 118.4(6) . . ? C32 C31 C35 120.9(8) . . ? C30 C31 C35 120.7(8) . . ? C32 C31 Ru1 71.4(4) . . ? C30 C31 Ru1 67.0(3) . . ? C35 C31 Ru1 132.3(5) . . ? C31 C32 C27 122.1(7) . . ? C31 C32 Ru1 73.6(4) . . ? C27 C32 Ru1 69.5(4) . . ? C31 C32 H32 118.9 . . ? C27 C32 H32 118.9 . . ? Ru1 C32 H32 130.8 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C2 O1 P1 119.2(4) . . ? C12 O2 P1 119.2(4) . . ? C21 O3 P1 128.3(4) . . ? O2 P1 O3 98.6(2) . . ? O2 P1 O1 102.8(2) . . ? O3 P1 O1 98.8(2) . . ? O2 P1 Ru1 113.06(17) . . ? O3 P1 Ru1 117.70(17) . . ? O1 P1 Ru1 122.20(18) . . ? C30 Ru1 C28 66.9(2) . . ? C30 Ru1 C27 79.7(3) . . ? C28 Ru1 C27 36.6(2) . . ? C30 Ru1 C29 37.1(2) . . ? C28 Ru1 C29 37.5(2) . . ? C27 Ru1 C29 67.4(2) . . ? C30 Ru1 P1 116.9(2) . . ? C28 Ru1 P1 93.93(16) . . ? C27 Ru1 P1 119.71(19) . . ? C29 Ru1 P1 91.81(16) . . ? C30 Ru1 C32 65.9(3) . . ? C28 Ru1 C32 65.3(2) . . ? C27 Ru1 C32 37.1(2) . . ? C29 Ru1 C32 77.9(2) . . ? P1 Ru1 C32 156.80(19) . . ? C30 Ru1 C31 37.6(3) . . ? C28 Ru1 C31 77.2(2) . . ? C27 Ru1 C31 65.8(3) . . ? C29 Ru1 C31 66.5(2) . . ? P1 Ru1 C31 154.4(2) . . ? C32 Ru1 C31 35.0(3) . . ? C30 Ru1 Cl2 89.88(18) . . ? C28 Ru1 Cl2 154.79(19) . . ? C27 Ru1 Cl2 152.24(19) . . ? C29 Ru1 Cl2 117.42(18) . . ? P1 Ru1 Cl2 87.97(7) . . ? C32 Ru1 Cl2 115.23(19) . . ? C31 Ru1 Cl2 90.36(19) . . ? C30 Ru1 Cl1 153.2(2) . . ? C28 Ru1 Cl1 117.92(19) . . ? C27 Ru1 Cl1 90.69(19) . . ? C29 Ru1 Cl1 155.38(17) . . ? P1 Ru1 Cl1 89.62(6) . . ? C32 Ru1 Cl1 91.5(2) . . ? C31 Ru1 Cl1 115.8(2) . . ? Cl2 Ru1 Cl1 87.20(8) . . ? 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 C10 C1 C2 O1 -175.3(5) . . . . ? C11 C1 C2 O1 3.1(9) . . . . ? C10 C1 C2 C3 7.1(9) . . . . ? C11 C1 C2 C3 -174.5(5) . . . . ? C1 C2 C3 C4 -1.5(9) . . . . ? O1 C2 C3 C4 -179.1(6) . . . . ? C2 C3 C4 C5 -3.3(10) . . . . ? C3 C4 C5 C10 2.2(11) . . . . ? C3 C4 C5 C6 -177.2(7) . . . . ? C4 C5 C6 C7 174.0(8) . . . . ? C10 C5 C6 C7 -5.4(11) . . . . ? C5 C6 C7 C8 2.8(13) . . . . ? C6 C7 C8 C9 0.2(12) . . . . ? C7 C8 C9 C10 -0.3(10) . . . . ? C8 C9 C10 C5 -2.5(10) . . . . ? C8 C9 C10 C1 179.8(6) . . . . ? C4 C5 C10 C9 -174.3(6) . . . . ? C6 C5 C10 C9 5.2(9) . . . . ? C4 C5 C10 C1 3.5(10) . . . . ? C6 C5 C10 C1 -177.0(6) . . . . ? C2 C1 C10 C9 169.7(6) . . . . ? C11 C1 C10 C9 -8.6(10) . . . . ? C2 C1 C10 C5 -8.0(9) . . . . ? C11 C1 C10 C5 173.7(6) . . . . ? C2 C1 C11 C12 -53.3(9) . . . . ? C10 C1 C11 C12 125.0(7) . . . . ? C2 C1 C11 C20 123.9(6) . . . . ? C10 C1 C11 C20 -57.8(8) . . . . ? C20 C11 C12 C13 5.9(10) . . . . ? C1 C11 C12 C13 -176.8(6) . . . . ? C20 C11 C12 O2 -175.8(5) . . . . ? C1 C11 C12 O2 1.4(9) . . . . ? C11 C12 C13 C14 -1.0(10) . . . . ? O2 C12 C13 C14 -179.3(6) . . . . ? C12 C13 C14 C15 -5.1(11) . . . . ? C13 C14 C15 C16 -172.4(7) . . . . ? C13 C14 C15 C20 6.0(11) . . . . ? C14 C15 C16 C17 177.2(8) . . . . ? C20 C15 C16 C17 -1.3(11) . . . . ? C15 C16 C17 C18 0.7(14) . . . . ? C16 C17 C18 C19 -0.5(14) . . . . ? C17 C18 C19 C20 0.9(12) . . . . ? C18 C19 C20 C15 -1.5(10) . . . . ? C18 C19 C20 C11 -177.3(7) . . . . ? C14 C15 C20 C19 -176.9(6) . . . . ? C16 C15 C20 C19 1.6(9) . . . . ? C14 C15 C20 C11 -0.9(9) . . . . ? C16 C15 C20 C11 177.6(6) . . . . ? C12 C11 C20 C19 171.0(6) . . . . ? C1 C11 C20 C19 -6.3(9) . . . . ? C12 C11 C20 C15 -4.8(9) . . . . ? C1 C11 C20 C15 177.9(6) . . . . ? C26 C21 C22 C23 0.4(10) . . . . ? O3 C21 C22 C23 177.3(6) . . . . ? C21 C22 C23 C24 0.7(11) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C23 C24 C25 C26 -0.3(12) . . . . ? C24 C25 C26 C21 1.4(11) . . . . ? C22 C21 C26 C25 -1.4(10) . . . . ? O3 C21 C26 C25 -178.5(6) . . . . ? C32 C27 C28 C29 -4.9(9) . . . . ? C33 C27 C28 C29 177.9(6) . . . . ? Ru1 C27 C28 C29 53.6(5) . . . . ? C32 C27 C28 Ru1 -58.6(5) . . . . ? C33 C27 C28 Ru1 124.2(6) . . . . ? C27 C28 C29 C30 -0.2(9) . . . . ? Ru1 C28 C29 C30 53.6(5) . . . . ? C27 C28 C29 C34 -179.8(6) . . . . ? Ru1 C28 C29 C34 -126.0(6) . . . . ? C27 C28 C29 Ru1 -53.8(5) . . . . ? C28 C29 C30 C31 6.6(8) . . . . ? C34 C29 C30 C31 -173.7(6) . . . . ? Ru1 C29 C30 C31 60.6(5) . . . . ? C28 C29 C30 Ru1 -54.0(5) . . . . ? C34 C29 C30 Ru1 125.7(5) . . . . ? C29 C30 C31 C32 -7.8(9) . . . . ? Ru1 C30 C31 C32 51.5(6) . . . . ? C29 C30 C31 C35 174.0(6) . . . . ? Ru1 C30 C31 C35 -126.8(6) . . . . ? C29 C30 C31 Ru1 -59.3(5) . . . . ? C30 C31 C32 C27 2.5(10) . . . . ? C35 C31 C32 C27 -179.3(7) . . . . ? Ru1 C31 C32 C27 52.0(6) . . . . ? C30 C31 C32 Ru1 -49.5(5) . . . . ? C35 C31 C32 Ru1 128.7(7) . . . . ? C28 C27 C32 C31 3.7(10) . . . . ? C33 C27 C32 C31 -179.2(7) . . . . ? Ru1 C27 C32 C31 -53.8(6) . . . . ? C28 C27 C32 Ru1 57.5(5) . . . . ? C33 C27 C32 Ru1 -125.4(7) . . . . ? C1 C2 O1 P1 71.7(7) . . . . ? C3 C2 O1 P1 -110.5(5) . . . . ? C11 C12 O2 P1 73.0(7) . . . . ? C13 C12 O2 P1 -108.6(6) . . . . ? C22 C21 O3 P1 41.2(8) . . . . ? C26 C21 O3 P1 -141.7(5) . . . . ? C12 O2 P1 O3 56.4(4) . . . . ? C12 O2 P1 O1 -44.8(4) . . . . ? C12 O2 P1 Ru1 -178.5(4) . . . . ? C21 O3 P1 O2 169.9(5) . . . . ? C21 O3 P1 O1 -85.6(5) . . . . ? C21 O3 P1 Ru1 48.1(6) . . . . ? C2 O1 P1 O2 -45.6(5) . . . . ? C2 O1 P1 O3 -146.6(4) . . . . ? C2 O1 P1 Ru1 82.6(5) . . . . ? C29 C30 Ru1 C28 30.0(4) . . . . ? C31 C30 Ru1 C28 -99.3(4) . . . . ? C29 C30 Ru1 C27 65.9(4) . . . . ? C31 C30 Ru1 C27 -63.4(4) . . . . ? C31 C30 Ru1 C29 -129.3(6) . . . . ? C29 C30 Ru1 P1 -52.3(4) . . . . ? C31 C30 Ru1 P1 178.4(3) . . . . ? C29 C30 Ru1 C32 102.1(4) . . . . ? C31 C30 Ru1 C32 -27.2(4) . . . . ? C29 C30 Ru1 C31 129.3(6) . . . . ? C29 C30 Ru1 Cl2 -139.9(4) . . . . ? C31 C30 Ru1 Cl2 90.8(4) . . . . ? C29 C30 Ru1 Cl1 136.5(4) . . . . ? C31 C30 Ru1 Cl1 7.2(6) . . . . ? C27 C28 Ru1 C30 104.5(5) . . . . ? C29 C28 Ru1 C30 -29.8(4) . . . . ? C29 C28 Ru1 C27 -134.3(6) . . . . ? C27 C28 Ru1 C29 134.3(6) . . . . ? C27 C28 Ru1 P1 -137.9(4) . . . . ? C29 C28 Ru1 P1 87.8(3) . . . . ? C27 C28 Ru1 C32 31.5(4) . . . . ? C29 C28 Ru1 C32 -102.8(4) . . . . ? C27 C28 Ru1 C31 66.4(4) . . . . ? C29 C28 Ru1 C31 -67.9(4) . . . . ? C27 C28 Ru1 Cl2 128.6(4) . . . . ? C29 C28 Ru1 Cl2 -5.7(6) . . . . ? C27 C28 Ru1 Cl1 -46.2(4) . . . . ? C29 C28 Ru1 Cl1 179.5(3) . . . . ? C28 C27 Ru1 C30 -64.8(4) . . . . ? C32 C27 Ru1 C30 63.3(4) . . . . ? C33 C27 Ru1 C30 -178.0(8) . . . . ? C32 C27 Ru1 C28 128.1(6) . . . . ? C33 C27 Ru1 C28 -113.2(9) . . . . ? C28 C27 Ru1 C29 -28.1(4) . . . . ? C32 C27 Ru1 C29 100.0(5) . . . . ? C33 C27 Ru1 C29 -141.4(8) . . . . ? C28 C27 Ru1 P1 50.4(5) . . . . ? C32 C27 Ru1 P1 178.5(4) . . . . ? C33 C27 Ru1 P1 -62.8(8) . . . . ? C28 C27 Ru1 C32 -128.1(6) . . . . ? C33 C27 Ru1 C32 118.6(9) . . . . ? C28 C27 Ru1 C31 -101.5(5) . . . . ? C32 C27 Ru1 C31 26.6(4) . . . . ? C33 C27 Ru1 C31 145.3(8) . . . . ? C28 C27 Ru1 Cl2 -134.3(4) . . . . ? C32 C27 Ru1 Cl2 -6.2(7) . . . . ? C33 C27 Ru1 Cl2 112.4(7) . . . . ? C28 C27 Ru1 Cl1 140.4(4) . . . . ? C32 C27 Ru1 Cl1 -91.5(4) . . . . ? C33 C27 Ru1 Cl1 27.1(7) . . . . ? C28 C29 Ru1 C30 130.8(6) . . . . ? C34 C29 Ru1 C30 -113.3(8) . . . . ? C30 C29 Ru1 C28 -130.8(6) . . . . ? C34 C29 Ru1 C28 115.9(7) . . . . ? C30 C29 Ru1 C27 -103.3(5) . . . . ? C28 C29 Ru1 C27 27.5(4) . . . . ? C34 C29 Ru1 C27 143.4(7) . . . . ? C30 C29 Ru1 P1 135.1(4) . . . . ? C28 C29 Ru1 P1 -94.1(3) . . . . ? C34 C29 Ru1 P1 21.8(6) . . . . ? C30 C29 Ru1 C32 -65.8(4) . . . . ? C28 C29 Ru1 C32 64.9(4) . . . . ? C34 C29 Ru1 C32 -179.2(6) . . . . ? C30 C29 Ru1 C31 -31.0(4) . . . . ? C28 C29 Ru1 C31 99.8(4) . . . . ? C34 C29 Ru1 C31 -144.3(7) . . . . ? C30 C29 Ru1 Cl2 46.5(4) . . . . ? C28 C29 Ru1 Cl2 177.3(3) . . . . ? C34 C29 Ru1 Cl2 -66.9(6) . . . . ? C30 C29 Ru1 Cl1 -131.8(4) . . . . ? C28 C29 Ru1 Cl1 -1.1(6) . . . . ? C34 C29 Ru1 Cl1 114.8(6) . . . . ? O2 P1 Ru1 C30 -24.8(3) . . . . ? O3 P1 Ru1 C30 89.3(3) . . . . ? O1 P1 Ru1 C30 -148.3(3) . . . . ? O2 P1 Ru1 C28 -90.8(2) . . . . ? O3 P1 Ru1 C28 23.3(3) . . . . ? O1 P1 Ru1 C28 145.7(3) . . . . ? O2 P1 Ru1 C27 -118.1(3) . . . . ? O3 P1 Ru1 C27 -4.1(3) . . . . ? O1 P1 Ru1 C27 118.3(3) . . . . ? O2 P1 Ru1 C29 -53.3(2) . . . . ? O3 P1 Ru1 C29 60.8(3) . . . . ? O1 P1 Ru1 C29 -176.9(3) . . . . ? O2 P1 Ru1 C32 -115.9(6) . . . . ? O3 P1 Ru1 C32 -1.8(6) . . . . ? O1 P1 Ru1 C32 120.5(6) . . . . ? O2 P1 Ru1 C31 -22.5(5) . . . . ? O3 P1 Ru1 C31 91.5(5) . . . . ? O1 P1 Ru1 C31 -146.1(5) . . . . ? O2 P1 Ru1 Cl2 64.07(18) . . . . ? O3 P1 Ru1 Cl2 178.1(2) . . . . ? O1 P1 Ru1 Cl2 -59.5(2) . . . . ? O2 P1 Ru1 Cl1 151.28(17) . . . . ? O3 P1 Ru1 Cl1 -94.7(2) . . . . ? O1 P1 Ru1 Cl1 27.7(2) . . . . ? C31 C32 Ru1 C30 29.0(4) . . . . ? C27 C32 Ru1 C30 -105.5(5) . . . . ? C31 C32 Ru1 C28 103.5(5) . . . . ? C27 C32 Ru1 C28 -31.1(4) . . . . ? C31 C32 Ru1 C27 134.6(7) . . . . ? C31 C32 Ru1 C29 66.2(4) . . . . ? C27 C32 Ru1 C29 -68.4(4) . . . . ? C31 C32 Ru1 P1 131.3(5) . . . . ? C27 C32 Ru1 P1 -3.2(8) . . . . ? C27 C32 Ru1 C31 -134.6(7) . . . . ? C31 C32 Ru1 Cl2 -48.6(4) . . . . ? C27 C32 Ru1 Cl2 176.8(4) . . . . ? C31 C32 Ru1 Cl1 -136.2(4) . . . . ? C27 C32 Ru1 Cl1 89.2(4) . . . . ? C32 C31 Ru1 C30 -133.4(6) . . . . ? C35 C31 Ru1 C30 111.4(11) . . . . ? C32 C31 Ru1 C28 -64.9(4) . . . . ? C30 C31 Ru1 C28 68.5(4) . . . . ? C35 C31 Ru1 C28 180.0(10) . . . . ? C32 C31 Ru1 C27 -28.1(4) . . . . ? C30 C31 Ru1 C27 105.3(4) . . . . ? C35 C31 Ru1 C27 -143.3(10) . . . . ? C32 C31 Ru1 C29 -102.8(4) . . . . ? C30 C31 Ru1 C29 30.6(4) . . . . ? C35 C31 Ru1 C29 142.0(11) . . . . ? C32 C31 Ru1 P1 -136.7(5) . . . . ? C30 C31 Ru1 P1 -3.3(7) . . . . ? C35 C31 Ru1 P1 108.1(9) . . . . ? C30 C31 Ru1 C32 133.4(6) . . . . ? C35 C31 Ru1 C32 -115.2(11) . . . . ? C32 C31 Ru1 Cl2 137.2(4) . . . . ? C30 C31 Ru1 Cl2 -89.3(4) . . . . ? C35 C31 Ru1 Cl2 22.1(10) . . . . ? C32 C31 Ru1 Cl1 50.2(4) . . . . ? C30 C31 Ru1 Cl1 -176.4(3) . . . . ? C35 C31 Ru1 Cl1 -65.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.765 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.182 #===END #=============================================================================== data_3c _database_code_depnum_ccdc_archive 'CCDC 769458' #TrackingRef '- 1a_1b_3b_3c.cif' #=============================================================================== _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Cl2 N O2 P Ru' _chemical_formula_sum 'C34 H34 Cl2 N O2 P Ru' _chemical_formula_weight 691.56 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.0637(4) _cell_length_b 8.3804(3) _cell_length_c 15.1019(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.135(3) _cell_angle_gamma 90.00 _cell_volume 1520.65(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5119 _cell_measurement_theta_min 2.9352 _cell_measurement_theta_max 73.6865 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.143 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.017 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 6.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67776 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur Nova ; _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number 11289 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11273 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 74.00 _reflns_number_total 4576 _reflns_number_gt 4016 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlisPro RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlisPro RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0596P)^2^+1.0004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(13) _refine_ls_number_reflns 4576 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 C1 C 1.0197(4) 0.8266(7) 0.6922(4) 0.0378(11) Uani 1 1 d . . . C2 C 0.9965(4) 0.9298(10) 0.7572(3) 0.0391(11) Uani 1 1 d . . . C3 C 1.0745(5) 0.9760(8) 0.8279(4) 0.0463(13) Uani 1 1 d . . . H3 H 1.0542 1.0456 0.8716 0.056 Uiso 1 1 calc R . . C4 C 1.1793(4) 0.9175(13) 0.8309(3) 0.0494(11) Uani 1 1 d . . . H4 H 1.2313 0.9490 0.8767 0.059 Uiso 1 1 calc R . . C5 C 1.2113(5) 0.8096(8) 0.7661(4) 0.0460(13) Uani 1 1 d . . . C6 C 1.3200(5) 0.7468(10) 0.7695(5) 0.0553(16) Uani 1 1 d . . . H6 H 1.3726 0.7811 0.8142 0.066 Uiso 1 1 calc R . . C7 C 1.3505(5) 0.6367(10) 0.7090(5) 0.0580(17) Uani 1 1 d . . . H7 H 1.4233 0.5993 0.7115 0.070 Uiso 1 1 calc R . . C8 C 1.2699(5) 0.5813(9) 0.6430(4) 0.0495(14) Uani 1 1 d . . . H8 H 1.2889 0.5033 0.6032 0.059 Uiso 1 1 calc R . . C9 C 1.1631(5) 0.6412(9) 0.6366(5) 0.0467(15) Uani 1 1 d . . . H9 H 1.1117 0.6047 0.5916 0.056 Uiso 1 1 calc R . . C10 C 1.1300(4) 0.7573(8) 0.6972(4) 0.0405(12) Uani 1 1 d . . . C11 C 0.9304(4) 0.7762(7) 0.6212(4) 0.0391(11) Uani 1 1 d . . . C12 C 0.8281(4) 0.7286(7) 0.6468(4) 0.0405(12) Uani 1 1 d . . . C13 C 0.7434(5) 0.6684(9) 0.5876(4) 0.0476(14) Uani 1 1 d . . . H13 H 0.6766 0.6352 0.6078 0.057 Uiso 1 1 calc R . . C14 C 0.7594(5) 0.6587(9) 0.5000(4) 0.0504(15) Uani 1 1 d . . . H14 H 0.7044 0.6136 0.4607 0.060 Uiso 1 1 calc R . . C15 C 0.8572(5) 0.7153(8) 0.4676(4) 0.0482(14) Uani 1 1 d . . . C16 C 0.8719(6) 0.7129(9) 0.3752(5) 0.0516(17) Uani 1 1 d . . . H16 H 0.8173 0.6683 0.3353 0.062 Uiso 1 1 calc R . . C17 C 0.9661(6) 0.7759(9) 0.3445(5) 0.0556(16) Uani 1 1 d . . . H17 H 0.9754 0.7731 0.2840 0.067 Uiso 1 1 calc R . . C18 C 1.0483(5) 0.8445(8) 0.4038(4) 0.0494(13) Uani 1 1 d . . . H18 H 1.1107 0.8905 0.3822 0.059 Uiso 1 1 calc R . . C19 C 1.0378(5) 0.8445(8) 0.4935(4) 0.0456(13) Uani 1 1 d . . . H19 H 1.0942 0.8888 0.5318 0.055 Uiso 1 1 calc R . . C20 C 0.9435(4) 0.7790(7) 0.5291(4) 0.0391(11) Uani 1 1 d . . . C21 C 0.7238(5) 1.0776(10) 0.6145(4) 0.0532(15) Uani 1 1 d . . . H21A H 0.7066 0.9989 0.5682 0.064 Uiso 1 1 calc R . . H21B H 0.8032 1.0985 0.6180 0.064 Uiso 1 1 calc R . . C22 C 0.6613(6) 1.2291(11) 0.5909(5) 0.0656(19) Uani 1 1 d . . . H22A H 0.6802 1.2664 0.5333 0.079 Uiso 1 1 calc R . . H22B H 0.6834 1.3107 0.6345 0.079 Uiso 1 1 calc R . . C23 C 0.5369(6) 1.2034(14) 0.5880(6) 0.080(3) Uani 1 1 d . . . H23A H 0.5131 1.1314 0.5397 0.096 Uiso 1 1 calc R . . H23B H 0.4986 1.3043 0.5773 0.096 Uiso 1 1 calc R . . C24 C 0.5073(6) 1.1328(14) 0.6763(6) 0.079(3) Uani 1 1 d . . . H24A H 0.5224 1.2109 0.7232 0.095 Uiso 1 1 calc R . . H24B H 0.4284 1.1079 0.6722 0.095 Uiso 1 1 calc R . . C25 C 0.5731(5) 0.9845(10) 0.6987(4) 0.0575(17) Uani 1 1 d . . . H25A H 0.5560 0.9458 0.7565 0.069 Uiso 1 1 calc R . . H25B H 0.5517 0.9026 0.6551 0.069 Uiso 1 1 calc R . . C26 C 0.7670(6) 1.1798(8) 0.9307(5) 0.0566(16) Uani 1 1 d . . . C27 C 0.8232(6) 1.0974(9) 1.0020(5) 0.0621(19) Uani 1 1 d . . . H27 H 0.9000 1.1079 1.0125 0.074 Uiso 1 1 calc R . . C28 C 0.7652(7) 0.9986(10) 1.0584(4) 0.066(2) Uani 1 1 d . . . C29 C 0.6537(7) 0.9715(10) 1.0390(4) 0.0617(18) Uani 1 1 d . . . H29 H 0.6168 0.9036 1.0752 0.074 Uiso 1 1 calc R . . C30 C 0.5929(5) 1.0449(10) 0.9646(5) 0.0558(17) Uani 1 1 d . . . C31 C 0.6507(6) 1.1485(8) 0.9131(5) 0.0514(15) Uani 1 1 d . . . H31 H 0.6119 1.1993 0.8651 0.062 Uiso 1 1 calc R . . C32 C 0.8231(9) 1.2960(10) 0.8751(8) 0.089(3) Uani 1 1 d . . . H32A H 0.7991 1.4021 0.8877 0.134 Uiso 1 1 calc R . . H32B H 0.8040 1.2725 0.8134 0.134 Uiso 1 1 calc R . . H32C H 0.9022 1.2883 0.8882 0.134 Uiso 1 1 calc R . . C33 C 0.8298(9) 0.9177(19) 1.1360(5) 0.098(3) Uani 1 1 d . . . H33A H 0.8217 0.8041 1.1302 0.147 Uiso 1 1 calc R . . H33B H 0.8017 0.9519 1.1904 0.147 Uiso 1 1 calc R . . H33C H 0.9070 0.9456 1.1368 0.147 Uiso 1 1 calc R . . C34 C 0.4704(6) 1.0121(14) 0.9428(6) 0.081(3) Uani 1 1 d . . . H34A H 0.4281 1.0712 0.9826 0.121 Uiso 1 1 calc R . . H34B H 0.4564 0.9001 0.9492 0.121 Uiso 1 1 calc R . . H34C H 0.4487 1.0441 0.8827 0.121 Uiso 1 1 calc R . . N1 N 0.6943(4) 1.0136(7) 0.7003(3) 0.0439(11) Uani 1 1 d . . . O1 O 0.8935(3) 1.0086(5) 0.7527(3) 0.0429(9) Uani 1 1 d . . . O2 O 0.8051(3) 0.7397(5) 0.7363(3) 0.0417(8) Uani 1 1 d . . . P1 P 0.78017(8) 0.9174(3) 0.77287(7) 0.0365(2) Uani 1 1 d . . . Cl1 Cl 0.61493(13) 0.6973(2) 0.86880(11) 0.0522(4) Uani 1 1 d . . . Cl2 Cl 0.88217(14) 0.7266(2) 0.94528(11) 0.0594(4) Uani 1 1 d . . . Ru1 Ru 0.73605(3) 0.91716(5) 0.91532(2) 0.03960(11) Uani 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 C1 0.033(2) 0.039(3) 0.041(3) -0.003(2) -0.003(2) -0.003(2) C2 0.0320(19) 0.040(3) 0.045(2) 0.002(3) -0.0013(16) -0.002(3) C3 0.047(3) 0.049(3) 0.042(3) -0.011(2) -0.001(2) -0.008(2) C4 0.042(2) 0.059(3) 0.045(2) -0.003(4) -0.0109(18) -0.011(4) C5 0.036(3) 0.052(4) 0.048(3) 0.000(3) -0.007(2) -0.005(2) C6 0.035(3) 0.065(4) 0.063(4) -0.003(3) -0.010(3) -0.007(3) C7 0.030(3) 0.068(4) 0.076(4) -0.004(4) -0.001(3) 0.001(3) C8 0.043(3) 0.054(4) 0.051(3) -0.003(3) 0.000(2) 0.000(3) C9 0.040(3) 0.049(4) 0.051(3) 0.001(3) 0.005(3) 0.002(3) C10 0.030(2) 0.048(3) 0.042(3) -0.002(2) -0.004(2) -0.006(2) C11 0.034(2) 0.042(3) 0.040(3) -0.005(2) -0.004(2) -0.003(2) C12 0.037(2) 0.042(3) 0.042(3) -0.007(2) -0.003(2) 0.000(2) C13 0.036(3) 0.050(4) 0.056(3) -0.012(3) -0.003(2) -0.005(3) C14 0.038(3) 0.057(4) 0.053(3) -0.015(3) -0.011(2) 0.002(3) C15 0.043(3) 0.054(4) 0.046(3) -0.014(3) -0.006(2) 0.008(3) C16 0.058(4) 0.054(4) 0.041(3) -0.009(3) -0.008(3) 0.011(3) C17 0.066(4) 0.055(4) 0.045(3) -0.005(3) 0.004(3) 0.015(3) C18 0.052(3) 0.051(3) 0.045(3) -0.001(3) 0.004(2) 0.009(3) C19 0.044(3) 0.048(3) 0.044(3) 0.001(2) -0.001(2) 0.006(2) C20 0.038(2) 0.037(3) 0.040(3) 0.000(2) -0.006(2) 0.006(2) C21 0.051(3) 0.064(4) 0.046(3) 0.010(3) 0.011(3) 0.000(3) C22 0.066(4) 0.064(5) 0.066(4) 0.022(4) -0.002(3) 0.002(4) C23 0.055(4) 0.110(8) 0.074(5) 0.029(5) -0.004(3) 0.017(5) C24 0.042(3) 0.121(8) 0.072(5) 0.031(5) -0.008(3) 0.018(4) C25 0.039(3) 0.080(5) 0.051(3) 0.012(3) -0.007(2) -0.011(3) C26 0.069(4) 0.033(3) 0.067(4) -0.015(3) 0.005(3) -0.002(3) C27 0.054(3) 0.058(4) 0.071(4) -0.032(4) -0.013(3) 0.003(3) C28 0.099(5) 0.064(5) 0.030(3) -0.030(3) -0.021(3) 0.020(4) C29 0.082(5) 0.067(4) 0.039(3) -0.016(3) 0.018(3) 0.001(4) C30 0.043(3) 0.066(4) 0.059(4) -0.029(3) 0.008(3) 0.010(3) C31 0.053(3) 0.043(3) 0.056(4) -0.016(3) -0.009(3) 0.015(3) C32 0.098(6) 0.042(4) 0.132(9) -0.011(5) 0.033(6) -0.007(4) C33 0.131(8) 0.093(6) 0.062(4) -0.010(7) -0.030(5) 0.043(9) C34 0.053(4) 0.109(8) 0.080(5) -0.038(5) 0.006(4) -0.004(4) N1 0.036(2) 0.052(3) 0.044(2) 0.002(2) 0.0042(18) 0.000(2) O1 0.0328(17) 0.042(2) 0.054(2) -0.0076(18) 0.0038(15) -0.0019(16) O2 0.0421(18) 0.043(2) 0.0406(19) -0.0021(17) 0.0081(15) -0.0053(17) P1 0.0319(5) 0.0399(6) 0.0374(5) -0.0009(9) 0.0014(4) -0.0035(9) Cl1 0.0545(8) 0.0508(8) 0.0517(8) -0.0032(7) 0.0066(6) -0.0144(7) Cl2 0.0630(9) 0.0554(9) 0.0565(8) -0.0051(7) -0.0129(7) 0.0194(8) Ru1 0.03993(17) 0.04087(19) 0.03695(18) -0.0037(2) -0.00239(12) 0.0007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.356(9) . ? C1 C10 1.448(8) . ? C1 C11 1.510(7) . ? C2 O1 1.404(7) . ? C2 C3 1.413(7) . ? C3 C4 1.352(9) . ? C3 H3 0.9300 . ? C4 C5 1.411(10) . ? C4 H4 0.9300 . ? C5 C6 1.409(9) . ? C5 C10 1.433(8) . ? C6 C7 1.372(11) . ? C6 H6 0.9300 . ? C7 C8 1.408(9) . ? C7 H7 0.9300 . ? C8 C9 1.377(9) . ? C8 H8 0.9300 . ? C9 C10 1.417(10) . ? C9 H9 0.9300 . ? C11 C12 1.385(8) . ? C11 C20 1.413(8) . ? C12 C13 1.391(8) . ? C12 O2 1.407(7) . ? C13 C14 1.356(10) . ? C13 H13 0.9300 . ? C14 C15 1.399(10) . ? C14 H14 0.9300 . ? C15 C16 1.423(10) . ? C15 C20 1.436(8) . ? C16 C17 1.371(11) . ? C16 H16 0.9300 . ? C17 C18 1.399(10) . ? C17 H17 0.9300 . ? C18 C19 1.371(9) . ? C18 H18 0.9300 . ? C19 C20 1.412(8) . ? C19 H19 0.9300 . ? C21 N1 1.474(8) . ? C21 C22 1.504(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.512(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.530(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.498(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N1 1.481(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.402(11) . ? C26 C31 1.429(10) . ? C26 C32 1.488(12) . ? C26 Ru1 2.241(7) . ? C27 C28 1.417(12) . ? C27 Ru1 2.204(6) . ? C27 H27 0.9300 . ? C28 C29 1.369(12) . ? C28 C33 1.509(10) . ? C28 Ru1 2.263(5) . ? C29 C30 1.424(11) . ? C29 Ru1 2.239(6) . ? C29 H29 0.9300 . ? C30 C31 1.394(11) . ? C30 C34 1.511(9) . ? C30 Ru1 2.216(6) . ? C31 Ru1 2.194(6) . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1 P1 1.650(5) . ? O1 P1 1.619(4) . ? O2 P1 1.625(5) . ? P1 Ru1 2.2618(11) . ? Cl1 Ru1 2.4165(15) . ? Cl2 Ru1 2.3917(16) . ? 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 C1 C10 117.7(5) . . ? C2 C1 C11 120.8(5) . . ? C10 C1 C11 121.3(5) . . ? C1 C2 O1 120.3(4) . . ? C1 C2 C3 123.8(5) . . ? O1 C2 C3 115.7(6) . . ? C4 C3 C2 118.9(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.4(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 121.7(5) . . ? C6 C5 C10 119.1(6) . . ? C4 C5 C10 119.2(5) . . ? C7 C6 C5 122.1(6) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 119.0(6) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 120.7(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 121.4(6) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C5 117.7(5) . . ? C9 C10 C1 123.5(5) . . ? C5 C10 C1 118.8(5) . . ? C12 C11 C20 117.4(5) . . ? C12 C11 C1 118.6(5) . . ? C20 C11 C1 123.9(5) . . ? C11 C12 C13 123.1(6) . . ? C11 C12 O2 120.4(5) . . ? C13 C12 O2 116.4(5) . . ? C14 C13 C12 119.2(6) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 121.4(6) . . ? C14 C15 C20 119.0(6) . . ? C16 C15 C20 119.6(6) . . ? C17 C16 C15 120.4(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 120.7(6) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 121.7(6) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C11 123.1(5) . . ? C19 C20 C15 117.4(5) . . ? C11 C20 C15 119.5(5) . . ? N1 C21 C22 111.1(6) . . ? N1 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? N1 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 111.2(7) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 109.8(6) . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C23 110.9(7) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N1 C25 C24 111.7(6) . . ? N1 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? N1 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C31 116.9(7) . . ? C27 C26 C32 122.9(8) . . ? C31 C26 C32 120.2(8) . . ? C27 C26 Ru1 70.2(4) . . ? C31 C26 Ru1 69.4(4) . . ? C32 C26 Ru1 131.6(6) . . ? C26 C27 C28 121.2(7) . . ? C26 C27 Ru1 73.1(4) . . ? C28 C27 Ru1 73.8(4) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? Ru1 C27 H27 125.5 . . ? C29 C28 C27 119.8(6) . . ? C29 C28 C33 121.4(9) . . ? C27 C28 C33 118.7(8) . . ? C29 C28 Ru1 71.4(3) . . ? C27 C28 Ru1 69.3(3) . . ? C33 C28 Ru1 129.2(6) . . ? C28 C29 C30 121.6(7) . . ? C28 C29 Ru1 73.2(4) . . ? C30 C29 Ru1 70.5(3) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? Ru1 C29 H29 129.6 . . ? C31 C30 C29 117.5(6) . . ? C31 C30 C34 121.3(7) . . ? C29 C30 C34 121.2(8) . . ? C31 C30 Ru1 70.7(3) . . ? C29 C30 Ru1 72.2(4) . . ? C34 C30 Ru1 128.0(5) . . ? C30 C31 C26 122.8(7) . . ? C30 C31 Ru1 72.5(4) . . ? C26 C31 Ru1 73.0(4) . . ? C30 C31 H31 118.6 . . ? C26 C31 H31 118.6 . . ? Ru1 C31 H31 128.3 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C21 N1 C25 111.2(5) . . ? C21 N1 P1 125.1(4) . . ? C25 N1 P1 119.3(4) . . ? C2 O1 P1 121.8(4) . . ? C12 O2 P1 116.4(4) . . ? O1 P1 O2 100.6(2) . . ? O1 P1 N1 97.7(2) . . ? O2 P1 N1 110.3(2) . . ? O1 P1 Ru1 116.97(16) . . ? O2 P1 Ru1 112.88(17) . . ? N1 P1 Ru1 116.44(18) . . ? C31 Ru1 C27 66.5(3) . . ? C31 Ru1 C30 36.8(3) . . ? C27 Ru1 C30 79.3(3) . . ? C31 Ru1 C29 65.8(3) . . ? C27 Ru1 C29 65.7(3) . . ? C30 Ru1 C29 37.3(3) . . ? C31 Ru1 C26 37.6(3) . . ? C27 Ru1 C26 36.8(3) . . ? C30 Ru1 C26 67.6(3) . . ? C29 Ru1 C26 78.2(3) . . ? C31 Ru1 P1 97.7(2) . . ? C27 Ru1 P1 115.1(2) . . ? C30 Ru1 P1 125.2(2) . . ? C29 Ru1 P1 162.3(2) . . ? C26 Ru1 P1 92.7(2) . . ? C31 Ru1 C28 77.3(3) . . ? C27 Ru1 C28 37.0(3) . . ? C30 Ru1 C28 66.0(3) . . ? C29 Ru1 C28 35.4(3) . . ? C26 Ru1 C28 66.1(3) . . ? P1 Ru1 C28 151.4(3) . . ? C31 Ru1 Cl2 158.43(18) . . ? C27 Ru1 Cl2 92.3(2) . . ? C30 Ru1 Cl2 147.4(2) . . ? C29 Ru1 Cl2 110.6(2) . . ? C26 Ru1 Cl2 121.5(2) . . ? P1 Ru1 Cl2 87.03(6) . . ? C28 Ru1 Cl2 88.4(2) . . ? C31 Ru1 Cl1 113.49(19) . . ? C27 Ru1 Cl1 160.0(2) . . ? C30 Ru1 Cl1 89.8(2) . . ? C29 Ru1 Cl1 95.5(2) . . ? C26 Ru1 Cl1 150.4(2) . . ? P1 Ru1 Cl1 84.94(6) . . ? C28 Ru1 Cl1 123.1(3) . . ? Cl2 Ru1 Cl1 87.82(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 C10 C1 C2 O1 175.8(6) . . . . ? C11 C1 C2 O1 -8.9(9) . . . . ? C10 C1 C2 C3 1.7(10) . . . . ? C11 C1 C2 C3 176.9(6) . . . . ? C1 C2 C3 C4 1.3(11) . . . . ? O1 C2 C3 C4 -173.2(7) . . . . ? C2 C3 C4 C5 -1.1(12) . . . . ? C3 C4 C5 C6 -179.3(7) . . . . ? C3 C4 C5 C10 -2.0(12) . . . . ? C4 C5 C6 C7 177.1(8) . . . . ? C10 C5 C6 C7 -0.2(11) . . . . ? C5 C6 C7 C8 -1.9(12) . . . . ? C6 C7 C8 C9 2.7(12) . . . . ? C7 C8 C9 C10 -1.5(11) . . . . ? C8 C9 C10 C5 -0.5(10) . . . . ? C8 C9 C10 C1 178.5(6) . . . . ? C6 C5 C10 C9 1.4(10) . . . . ? C4 C5 C10 C9 -176.0(7) . . . . ? C6 C5 C10 C1 -177.8(6) . . . . ? C4 C5 C10 C1 4.9(10) . . . . ? C2 C1 C10 C9 176.3(7) . . . . ? C11 C1 C10 C9 1.0(9) . . . . ? C2 C1 C10 C5 -4.7(9) . . . . ? C11 C1 C10 C5 -179.9(6) . . . . ? C2 C1 C11 C12 -47.4(9) . . . . ? C10 C1 C11 C12 127.7(6) . . . . ? C2 C1 C11 C20 130.7(7) . . . . ? C10 C1 C11 C20 -54.2(8) . . . . ? C20 C11 C12 C13 7.0(9) . . . . ? C1 C11 C12 C13 -174.9(6) . . . . ? C20 C11 C12 O2 -173.0(5) . . . . ? C1 C11 C12 O2 5.2(9) . . . . ? C11 C12 C13 C14 -1.7(10) . . . . ? O2 C12 C13 C14 178.3(6) . . . . ? C12 C13 C14 C15 -3.2(11) . . . . ? C13 C14 C15 C16 -176.7(7) . . . . ? C13 C14 C15 C20 2.4(10) . . . . ? C14 C15 C16 C17 176.9(7) . . . . ? C20 C15 C16 C17 -2.2(10) . . . . ? C15 C16 C17 C18 -0.5(11) . . . . ? C16 C17 C18 C19 2.4(10) . . . . ? C17 C18 C19 C20 -1.3(10) . . . . ? C18 C19 C20 C11 179.6(6) . . . . ? C18 C19 C20 C15 -1.5(9) . . . . ? C12 C11 C20 C19 171.5(6) . . . . ? C1 C11 C20 C19 -6.6(9) . . . . ? C12 C11 C20 C15 -7.4(8) . . . . ? C1 C11 C20 C15 174.5(6) . . . . ? C14 C15 C20 C19 -175.9(6) . . . . ? C16 C15 C20 C19 3.2(9) . . . . ? C14 C15 C20 C11 3.0(9) . . . . ? C16 C15 C20 C11 -177.8(6) . . . . ? N1 C21 C22 C23 -57.0(9) . . . . ? C21 C22 C23 C24 54.9(11) . . . . ? C22 C23 C24 C25 -54.2(12) . . . . ? C23 C24 C25 N1 55.6(9) . . . . ? C31 C26 C27 C28 -5.3(10) . . . . ? C32 C26 C27 C28 174.3(7) . . . . ? Ru1 C26 C27 C28 -58.3(6) . . . . ? C31 C26 C27 Ru1 53.0(5) . . . . ? C32 C26 C27 Ru1 -127.4(7) . . . . ? C26 C27 C28 C29 5.6(10) . . . . ? Ru1 C27 C28 C29 -52.3(6) . . . . ? C26 C27 C28 C33 -177.8(8) . . . . ? Ru1 C27 C28 C33 124.2(7) . . . . ? C26 C27 C28 Ru1 57.9(6) . . . . ? C27 C28 C29 C30 -2.1(10) . . . . ? C33 C28 C29 C30 -178.6(8) . . . . ? Ru1 C28 C29 C30 -53.5(6) . . . . ? C27 C28 C29 Ru1 51.4(6) . . . . ? C33 C28 C29 Ru1 -125.1(7) . . . . ? C28 C29 C30 C31 -1.3(10) . . . . ? Ru1 C29 C30 C31 -56.1(5) . . . . ? C28 C29 C30 C34 178.9(7) . . . . ? Ru1 C29 C30 C34 124.1(7) . . . . ? C28 C29 C30 Ru1 54.8(6) . . . . ? C29 C30 C31 C26 1.5(9) . . . . ? C34 C30 C31 C26 -178.7(6) . . . . ? Ru1 C30 C31 C26 -55.4(6) . . . . ? C29 C30 C31 Ru1 56.9(5) . . . . ? C34 C30 C31 Ru1 -123.4(6) . . . . ? C27 C26 C31 C30 1.8(9) . . . . ? C32 C26 C31 C30 -177.9(7) . . . . ? Ru1 C26 C31 C30 55.1(6) . . . . ? C27 C26 C31 Ru1 -53.4(5) . . . . ? C32 C26 C31 Ru1 127.0(7) . . . . ? C22 C21 N1 C25 57.4(8) . . . . ? C22 C21 N1 P1 -146.4(5) . . . . ? C24 C25 N1 C21 -57.2(8) . . . . ? C24 C25 N1 P1 145.1(5) . . . . ? C1 C2 O1 P1 74.3(7) . . . . ? C3 C2 O1 P1 -111.1(6) . . . . ? C11 C12 O2 P1 75.1(6) . . . . ? C13 C12 O2 P1 -104.8(6) . . . . ? C2 O1 P1 O2 -32.8(4) . . . . ? C2 O1 P1 N1 -145.2(4) . . . . ? C2 O1 P1 Ru1 89.8(4) . . . . ? C12 O2 P1 O1 -57.5(4) . . . . ? C12 O2 P1 N1 45.0(4) . . . . ? C12 O2 P1 Ru1 177.1(3) . . . . ? C21 N1 P1 O1 31.9(6) . . . . ? C25 N1 P1 O1 -173.6(5) . . . . ? C21 N1 P1 O2 -72.5(6) . . . . ? C25 N1 P1 O2 82.0(5) . . . . ? C21 N1 P1 Ru1 157.2(5) . . . . ? C25 N1 P1 Ru1 -48.3(6) . . . . ? C30 C31 Ru1 C27 -103.9(5) . . . . ? C26 C31 Ru1 C27 29.7(5) . . . . ? C26 C31 Ru1 C30 133.7(6) . . . . ? C30 C31 Ru1 C29 -31.2(4) . . . . ? C26 C31 Ru1 C29 102.5(5) . . . . ? C30 C31 Ru1 C26 -133.7(6) . . . . ? C30 C31 Ru1 P1 142.0(4) . . . . ? C26 C31 Ru1 P1 -84.3(4) . . . . ? C30 C31 Ru1 C28 -66.6(4) . . . . ? C26 C31 Ru1 C28 67.1(5) . . . . ? C30 C31 Ru1 Cl2 -116.4(6) . . . . ? C26 C31 Ru1 Cl2 17.3(8) . . . . ? C30 C31 Ru1 Cl1 54.2(4) . . . . ? C26 C31 Ru1 Cl1 -172.1(4) . . . . ? C26 C27 Ru1 C31 -30.4(4) . . . . ? C28 C27 Ru1 C31 100.4(5) . . . . ? C26 C27 Ru1 C30 -66.7(5) . . . . ? C28 C27 Ru1 C30 64.0(5) . . . . ? C26 C27 Ru1 C29 -103.3(5) . . . . ? C28 C27 Ru1 C29 27.4(4) . . . . ? C28 C27 Ru1 C26 130.7(7) . . . . ? C26 C27 Ru1 P1 57.3(5) . . . . ? C28 C27 Ru1 P1 -172.0(4) . . . . ? C26 C27 Ru1 C28 -130.7(7) . . . . ? C26 C27 Ru1 Cl2 145.1(4) . . . . ? C28 C27 Ru1 Cl2 -84.2(4) . . . . ? C26 C27 Ru1 Cl1 -124.8(6) . . . . ? C28 C27 Ru1 Cl1 5.9(8) . . . . ? C29 C30 Ru1 C31 -128.7(6) . . . . ? C34 C30 Ru1 C31 115.2(9) . . . . ? C31 C30 Ru1 C27 65.0(4) . . . . ? C29 C30 Ru1 C27 -63.8(5) . . . . ? C34 C30 Ru1 C27 -179.8(9) . . . . ? C31 C30 Ru1 C29 128.7(6) . . . . ? C34 C30 Ru1 C29 -116.1(10) . . . . ? C31 C30 Ru1 C26 28.5(4) . . . . ? C29 C30 Ru1 C26 -100.2(5) . . . . ? C34 C30 Ru1 C26 143.7(9) . . . . ? C31 C30 Ru1 P1 -48.3(4) . . . . ? C29 C30 Ru1 P1 -177.0(4) . . . . ? C34 C30 Ru1 P1 66.9(9) . . . . ? C31 C30 Ru1 C28 101.3(5) . . . . ? C29 C30 Ru1 C28 -27.5(5) . . . . ? C34 C30 Ru1 C28 -143.5(9) . . . . ? C31 C30 Ru1 Cl2 142.3(4) . . . . ? C29 C30 Ru1 Cl2 13.6(7) . . . . ? C34 C30 Ru1 Cl2 -102.5(8) . . . . ? C31 C30 Ru1 Cl1 -132.0(4) . . . . ? C29 C30 Ru1 Cl1 99.3(4) . . . . ? C34 C30 Ru1 Cl1 -16.8(8) . . . . ? C28 C29 Ru1 C31 -102.5(5) . . . . ? C30 C29 Ru1 C31 30.8(4) . . . . ? C28 C29 Ru1 C27 -28.6(5) . . . . ? C30 C29 Ru1 C27 104.8(5) . . . . ? C28 C29 Ru1 C30 -133.4(7) . . . . ? C28 C29 Ru1 C26 -65.1(5) . . . . ? C30 C29 Ru1 C26 68.3(5) . . . . ? C28 C29 Ru1 P1 -125.3(7) . . . . ? C30 C29 Ru1 P1 8.1(10) . . . . ? C30 C29 Ru1 C28 133.4(7) . . . . ? C28 C29 Ru1 Cl2 54.4(5) . . . . ? C30 C29 Ru1 Cl2 -172.2(4) . . . . ? C28 C29 Ru1 Cl1 144.2(5) . . . . ? C30 C29 Ru1 Cl1 -82.5(4) . . . . ? C27 C26 Ru1 C31 130.5(7) . . . . ? C32 C26 Ru1 C31 -112.6(10) . . . . ? C31 C26 Ru1 C27 -130.5(7) . . . . ? C32 C26 Ru1 C27 116.9(10) . . . . ? C27 C26 Ru1 C30 102.5(5) . . . . ? C31 C26 Ru1 C30 -28.0(4) . . . . ? C32 C26 Ru1 C30 -140.6(9) . . . . ? C27 C26 Ru1 C29 65.0(5) . . . . ? C31 C26 Ru1 C29 -65.5(4) . . . . ? C32 C26 Ru1 C29 -178.1(9) . . . . ? C27 C26 Ru1 P1 -130.3(4) . . . . ? C31 C26 Ru1 P1 99.2(4) . . . . ? C32 C26 Ru1 P1 -13.4(9) . . . . ? C27 C26 Ru1 C28 29.9(5) . . . . ? C31 C26 Ru1 C28 -100.6(5) . . . . ? C32 C26 Ru1 C28 146.8(9) . . . . ? C27 C26 Ru1 Cl2 -42.1(5) . . . . ? C31 C26 Ru1 Cl2 -172.6(3) . . . . ? C32 C26 Ru1 Cl2 74.7(9) . . . . ? C27 C26 Ru1 Cl1 145.2(4) . . . . ? C31 C26 Ru1 Cl1 14.7(7) . . . . ? C32 C26 Ru1 Cl1 -97.9(9) . . . . ? O1 P1 Ru1 C31 84.9(3) . . . . ? O2 P1 Ru1 C31 -159.1(2) . . . . ? N1 P1 Ru1 C31 -30.0(3) . . . . ? O1 P1 Ru1 C27 17.2(3) . . . . ? O2 P1 Ru1 C27 133.3(3) . . . . ? N1 P1 Ru1 C27 -97.7(3) . . . . ? O1 P1 Ru1 C30 111.8(3) . . . . ? O2 P1 Ru1 C30 -132.2(3) . . . . ? N1 P1 Ru1 C30 -3.2(3) . . . . ? O1 P1 Ru1 C29 105.8(7) . . . . ? O2 P1 Ru1 C29 -138.2(7) . . . . ? N1 P1 Ru1 C29 -9.2(8) . . . . ? O1 P1 Ru1 C26 47.5(3) . . . . ? O2 P1 Ru1 C26 163.5(2) . . . . ? N1 P1 Ru1 C26 -67.4(3) . . . . ? O1 P1 Ru1 C28 7.2(5) . . . . ? O2 P1 Ru1 C28 123.2(4) . . . . ? N1 P1 Ru1 C28 -107.7(5) . . . . ? O1 P1 Ru1 Cl2 -74.0(2) . . . . ? O2 P1 Ru1 Cl2 42.06(16) . . . . ? N1 P1 Ru1 Cl2 171.1(2) . . . . ? O1 P1 Ru1 Cl1 -162.0(2) . . . . ? O2 P1 Ru1 Cl1 -46.01(16) . . . . ? N1 P1 Ru1 Cl1 83.0(2) . . . . ? C29 C28 Ru1 C31 65.9(5) . . . . ? C27 C28 Ru1 C31 -67.6(4) . . . . ? C33 C28 Ru1 C31 -178.4(10) . . . . ? C29 C28 Ru1 C27 133.5(7) . . . . ? C33 C28 Ru1 C27 -110.8(11) . . . . ? C29 C28 Ru1 C30 28.8(5) . . . . ? C27 C28 Ru1 C30 -104.7(5) . . . . ? C33 C28 Ru1 C30 144.5(11) . . . . ? C27 C28 Ru1 C29 -133.5(7) . . . . ? C33 C28 Ru1 C29 115.7(12) . . . . ? C29 C28 Ru1 C26 103.8(5) . . . . ? C27 C28 Ru1 C26 -29.7(4) . . . . ? C33 C28 Ru1 C26 -140.5(11) . . . . ? C29 C28 Ru1 P1 148.8(4) . . . . ? C27 C28 Ru1 P1 15.2(7) . . . . ? C33 C28 Ru1 P1 -95.5(10) . . . . ? C29 C28 Ru1 Cl2 -130.4(5) . . . . ? C27 C28 Ru1 Cl2 96.1(4) . . . . ? C33 C28 Ru1 Cl2 -14.7(10) . . . . ? C29 C28 Ru1 Cl1 -44.1(5) . . . . ? C27 C28 Ru1 Cl1 -177.6(3) . . . . ? C33 C28 Ru1 Cl1 71.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 74.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.619 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.077 #===END