Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mike Whittlesey' _publ_contact_author_email M.K.WHITTLESEY@BATH.AC.UK _publ_section_title ; Stoichiometric and Catalytic Reactivity of the N-Heterocyclic Carbene Ruthenium Hydride Complexes [Ru(NHC)(L)(CO)HCl] and [Ru(NHC)(L)(CO)H(eta2-BH4)] (L = NHC, PPh3) ; loop_ _publ_author_name 'M Whittlesey' 'Victoria L. Chantler' 'Sarah L. Chatwin' 'Rodolphe F R Jazzar' 'Mary Mahon' ; O.Saker ; data_c:\x-ray\helix\h05mkw21\maxus\h05mkw21 _database_code_depnum_ccdc_archive 'CCDC 607121' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H48 N4 O3 Ru' _chemical_formula_weight 793.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 18.7240(1) _cell_length_b 10.8140(1) _cell_length_c 20.9130(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.651(1) _cell_angle_gamma 90.00 _cell_volume 4012.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 60581 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84494 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11676 _reflns_number_gt 9160 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+2.7141P] 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 11676 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.445259(8) 0.417288(13) 0.753812(8) 0.02290(6) Uani 1 1 d . . . O1 O 0.53588(14) 0.1789(2) 0.80490(13) 0.0712(6) Uani 1 1 d . . . O2 O 0.49293(12) 0.6102(2) 0.86754(11) 0.0598(6) Uani 1 1 d . . . O3 O 0.32682(11) 0.5292(2) 0.63110(12) 0.0661(6) Uani 1 1 d . . . N1 N 0.53986(9) 0.41053(14) 0.65479(8) 0.0232(3) Uani 1 1 d . . . N2 N 0.59546(9) 0.52905(15) 0.73781(8) 0.0253(3) Uani 1 1 d . . . N3 N 0.31056(10) 0.41343(16) 0.81500(9) 0.0287(3) Uani 1 1 d . . . N4 N 0.30367(9) 0.25894(16) 0.74951(8) 0.0292(3) Uani 1 1 d . . . C1 C 0.49937(16) 0.2639(2) 0.78486(17) 0.0518(7) Uani 1 1 d . . . C2 C 0.47526(13) 0.5380(2) 0.82523(13) 0.0385(5) Uani 1 1 d . . . C3 C 0.37257(13) 0.4833(3) 0.67565(13) 0.0448(6) Uani 1 1 d . . . C4 C 0.53187(10) 0.45851(17) 0.71288(9) 0.0232(4) Uani 1 1 d . . . C5 C 0.60601(11) 0.45016(19) 0.64484(10) 0.0271(4) Uani 1 1 d . . . H5 H 0.6232 0.4287 0.6082 0.032 Uiso 1 1 calc R . . C6 C 0.64116(11) 0.52436(19) 0.69673(11) 0.0287(4) Uani 1 1 d . . . H6 H 0.6879 0.5655 0.7040 0.034 Uiso 1 1 calc R . . C7 C 0.48542(11) 0.3423(2) 0.60174(10) 0.0287(4) Uani 1 1 d . . . C8 C 0.49123(13) 0.2139(2) 0.59855(12) 0.0372(5) Uani 1 1 d . . . C9 C 0.44267(16) 0.1547(2) 0.54165(14) 0.0471(6) Uani 1 1 d . . . H9 H 0.4459 0.0675 0.5380 0.057 Uiso 1 1 calc R . . C10 C 0.39044(15) 0.2182(3) 0.49079(13) 0.0503(7) Uani 1 1 d . . . C11 C 0.38646(13) 0.3456(3) 0.49560(12) 0.0427(6) Uani 1 1 d . . . H11 H 0.3499 0.3896 0.4610 0.051 Uiso 1 1 calc R . . C12 C 0.43465(12) 0.4110(2) 0.54984(11) 0.0325(4) Uani 1 1 d . . . C13 C 0.54705(18) 0.1408(2) 0.65241(16) 0.0538(7) Uani 1 1 d . . . H13A H 0.5930 0.1898 0.6715 0.081 Uiso 1 1 calc R . . H13B H 0.5593 0.0644 0.6330 0.081 Uiso 1 1 calc R . . H13C H 0.5255 0.1205 0.6881 0.081 Uiso 1 1 calc R . . C14 C 0.3387(2) 0.1505(4) 0.42999(17) 0.0756(11) Uani 1 1 d . . . H14A H 0.3634 0.0747 0.4223 0.113 Uiso 1 1 calc R . . H14B H 0.3277 0.2038 0.3901 0.113 Uiso 1 1 calc R . . H14C H 0.2915 0.1293 0.4384 0.113 Uiso 1 1 calc R . . C15 C 0.43420(14) 0.5497(2) 0.54946(12) 0.0384(5) Uani 1 1 d . . . H15A H 0.4701 0.5800 0.5277 0.058 Uiso 1 1 calc R . . H15B H 0.4487 0.5803 0.5960 0.058 Uiso 1 1 calc R . . H15C H 0.3835 0.5794 0.5244 0.058 Uiso 1 1 calc R . . C16 C 0.61078(12) 0.6183(2) 0.79195(11) 0.0324(4) Uani 1 1 d . . . C17 C 0.65392(13) 0.5842(2) 0.85713(13) 0.0416(6) Uani 1 1 d . . . C18 C 0.67093(15) 0.6779(3) 0.90595(14) 0.0575(8) Uani 1 1 d . . . H18 H 0.7001 0.6578 0.9509 0.069 Uiso 1 1 calc R . . C19 C 0.64690(18) 0.7980(3) 0.89116(18) 0.0627(9) Uani 1 1 d . . . C20 C 0.60342(18) 0.8267(3) 0.82650(18) 0.0584(8) Uani 1 1 d . . . H20 H 0.5856 0.9090 0.8165 0.070 Uiso 1 1 calc R . . C21 C 0.58464(14) 0.7382(2) 0.77493(14) 0.0424(6) Uani 1 1 d . . . C22 C 0.67992(16) 0.4540(3) 0.87495(13) 0.0532(7) Uani 1 1 d . . . H22A H 0.6386 0.3968 0.8534 0.080 Uiso 1 1 calc R . . H22B H 0.6953 0.4435 0.9240 0.080 Uiso 1 1 calc R . . H22C H 0.7228 0.4365 0.8591 0.080 Uiso 1 1 calc R . . C23 C 0.6689(3) 0.8972(4) 0.9449(2) 0.0935(15) Uani 1 1 d . . . H23A H 0.6714 0.8614 0.9886 0.140 Uiso 1 1 calc R . . H23B H 0.6312 0.9634 0.9334 0.140 Uiso 1 1 calc R . . H23C H 0.7182 0.9311 0.9474 0.140 Uiso 1 1 calc R . . C24 C 0.53703(18) 0.7704(2) 0.70482(16) 0.0558(7) Uani 1 1 d . . . H24A H 0.5645 0.7508 0.6733 0.084 Uiso 1 1 calc R . . H24B H 0.5253 0.8589 0.7023 0.084 Uiso 1 1 calc R . . H24C H 0.4901 0.7226 0.6928 0.084 Uiso 1 1 calc R . . C25 C 0.34943(11) 0.35725(18) 0.77768(10) 0.0252(4) Uani 1 1 d . . . C26 C 0.24308(12) 0.3534(2) 0.80934(12) 0.0376(5) Uani 1 1 d . . . H26 H 0.2070 0.3765 0.8304 0.045 Uiso 1 1 calc R . . C27 C 0.23895(12) 0.2568(2) 0.76831(12) 0.0368(5) Uani 1 1 d . . . H27 H 0.1993 0.1979 0.7547 0.044 Uiso 1 1 calc R . . C28 C 0.33604(12) 0.5129(2) 0.86246(12) 0.0329(4) Uani 1 1 d . . . C29 C 0.37726(14) 0.4819(2) 0.92863(12) 0.0390(5) Uani 1 1 d . . . C30 C 0.39865(18) 0.5778(3) 0.97587(16) 0.0526(7) Uani 1 1 d . . . H30 H 0.4270 0.5592 1.0213 0.063 Uiso 1 1 calc R . . C31 C 0.37935(18) 0.6988(3) 0.95761(19) 0.0608(8) Uani 1 1 d . . . C32 C 0.33823(17) 0.7250(2) 0.8915(2) 0.0593(9) Uani 1 1 d . . . H32 H 0.3252 0.8086 0.8791 0.071 Uiso 1 1 calc R . . C33 C 0.31504(14) 0.6337(2) 0.84210(15) 0.0437(6) Uani 1 1 d . . . C34 C 0.40037(17) 0.3507(2) 0.94799(13) 0.0488(6) Uani 1 1 d . . . H34A H 0.3555 0.2979 0.9366 0.073 Uiso 1 1 calc R . . H34B H 0.4268 0.3462 0.9966 0.073 Uiso 1 1 calc R . . H34C H 0.4339 0.3222 0.9234 0.073 Uiso 1 1 calc R . . C35 C 0.4026(3) 0.8015(4) 1.0094(3) 0.1010(16) Uani 1 1 d . . . H35A H 0.3935 0.8818 0.9865 0.152 Uiso 1 1 calc R . . H35B H 0.4563 0.7934 1.0349 0.152 Uiso 1 1 calc R . . H35C H 0.3730 0.7959 1.0404 0.152 Uiso 1 1 calc R . . C36 C 0.27086(18) 0.6636(3) 0.77020(18) 0.0635(9) Uani 1 1 d . . . H36A H 0.3000 0.6396 0.7408 0.095 Uiso 1 1 calc R . . H36B H 0.2606 0.7525 0.7658 0.095 Uiso 1 1 calc R . . H36C H 0.2231 0.6180 0.7571 0.095 Uiso 1 1 calc R . . C37 C 0.31792(12) 0.1597(2) 0.70923(11) 0.0324(4) Uani 1 1 d . . . C38 C 0.28632(13) 0.1639(2) 0.63911(12) 0.0388(5) Uani 1 1 d . . . C39 C 0.29628(16) 0.0609(3) 0.60300(15) 0.0516(7) Uani 1 1 d . . . H39 H 0.2759 0.0622 0.5552 0.062 Uiso 1 1 calc R . . C40 C 0.33451(16) -0.0426(3) 0.63391(17) 0.0564(8) Uani 1 1 d . . . C41 C 0.36321(16) -0.0454(2) 0.70359(17) 0.0516(7) Uani 1 1 d . . . H41 H 0.3889 -0.1173 0.7253 0.062 Uiso 1 1 calc R . . C42 C 0.35540(14) 0.0550(2) 0.74290(14) 0.0401(5) Uani 1 1 d . . . C43 C 0.24313(16) 0.2725(3) 0.60301(13) 0.0526(7) Uani 1 1 d . . . H43A H 0.2258 0.3220 0.6345 0.079 Uiso 1 1 calc R . . H43B H 0.1995 0.2439 0.5659 0.079 Uiso 1 1 calc R . . H43C H 0.2756 0.3232 0.5849 0.079 Uiso 1 1 calc R . . C44 C 0.3454(2) -0.1522(4) 0.5918(2) 0.0860(13) Uani 1 1 d . . . H44A H 0.3056 -0.1515 0.5479 0.129 Uiso 1 1 calc R . . H44B H 0.3428 -0.2294 0.6155 0.129 Uiso 1 1 calc R . . H44C H 0.3947 -0.1458 0.5851 0.129 Uiso 1 1 calc R . . C45 C 0.38396(17) 0.0476(3) 0.81866(15) 0.0498(6) Uani 1 1 d . . . H45A H 0.4146 0.1207 0.8369 0.075 Uiso 1 1 calc R . . H45B H 0.4148 -0.0270 0.8325 0.075 Uiso 1 1 calc R . . H45C H 0.3411 0.0442 0.8359 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02138(8) 0.02323(8) 0.02637(9) -0.00130(6) 0.01084(6) -0.00078(5) O1 0.0715(15) 0.0623(14) 0.0860(16) 0.0259(12) 0.0340(13) 0.0227(12) O2 0.0547(12) 0.0722(13) 0.0670(13) -0.0383(11) 0.0397(10) -0.0263(10) O3 0.0408(11) 0.0867(16) 0.0713(14) 0.0384(13) 0.0187(10) 0.0154(10) N1 0.0214(7) 0.0253(8) 0.0240(8) -0.0017(6) 0.0086(6) -0.0007(6) N2 0.0222(8) 0.0280(8) 0.0276(8) -0.0054(7) 0.0105(6) -0.0036(6) N3 0.0257(8) 0.0316(9) 0.0326(9) -0.0016(7) 0.0147(7) -0.0017(6) N4 0.0273(8) 0.0325(9) 0.0310(9) -0.0022(7) 0.0137(7) -0.0054(7) C1 0.0527(15) 0.0344(12) 0.087(2) 0.0127(13) 0.0480(15) 0.0042(11) C2 0.0337(11) 0.0454(12) 0.0443(13) -0.0094(11) 0.0237(10) -0.0089(10) C3 0.0279(11) 0.0632(16) 0.0463(14) 0.0156(12) 0.0163(10) 0.0004(10) C4 0.0235(9) 0.0212(8) 0.0253(9) 0.0005(7) 0.0084(7) 0.0010(7) C5 0.0244(9) 0.0334(10) 0.0268(9) -0.0009(8) 0.0129(8) -0.0006(7) C6 0.0223(9) 0.0332(10) 0.0339(10) -0.0042(8) 0.0135(8) -0.0031(7) C7 0.0259(9) 0.0362(11) 0.0254(9) -0.0065(8) 0.0101(8) -0.0055(8) C8 0.0399(12) 0.0351(11) 0.0405(12) -0.0093(9) 0.0182(10) -0.0081(9) C9 0.0529(15) 0.0430(13) 0.0520(15) -0.0196(11) 0.0261(12) -0.0184(11) C10 0.0403(13) 0.0759(19) 0.0368(13) -0.0201(13) 0.0153(11) -0.0243(13) C11 0.0294(11) 0.0681(17) 0.0292(11) -0.0057(11) 0.0072(9) -0.0097(11) C12 0.0269(10) 0.0466(12) 0.0254(10) -0.0033(9) 0.0106(8) -0.0025(8) C13 0.0667(18) 0.0285(12) 0.0636(18) -0.0026(11) 0.0171(14) 0.0044(11) C14 0.068(2) 0.100(3) 0.0530(18) -0.0352(18) 0.0117(16) -0.038(2) C15 0.0358(12) 0.0471(13) 0.0317(11) 0.0050(10) 0.0102(9) 0.0076(10) C16 0.0265(10) 0.0361(10) 0.0388(11) -0.0153(9) 0.0165(9) -0.0093(8) C17 0.0248(10) 0.0630(16) 0.0385(12) -0.0203(11) 0.0123(9) -0.0059(10) C18 0.0343(13) 0.094(2) 0.0462(15) -0.0380(15) 0.0157(11) -0.0173(14) C19 0.0559(17) 0.069(2) 0.076(2) -0.0477(17) 0.0394(16) -0.0309(15) C20 0.0650(18) 0.0412(14) 0.087(2) -0.0303(15) 0.0495(18) -0.0214(13) C21 0.0443(13) 0.0320(11) 0.0612(16) -0.0147(11) 0.0313(12) -0.0125(10) C22 0.0414(14) 0.082(2) 0.0316(12) -0.0085(13) 0.0051(10) 0.0171(13) C23 0.093(3) 0.097(3) 0.107(3) -0.077(3) 0.055(3) -0.046(2) C24 0.0696(19) 0.0311(13) 0.073(2) 0.0032(12) 0.0312(16) 0.0065(12) C25 0.0255(9) 0.0263(9) 0.0256(9) 0.0029(7) 0.0106(7) -0.0003(7) C26 0.0307(11) 0.0476(13) 0.0417(12) -0.0041(10) 0.0217(10) -0.0057(9) C27 0.0318(11) 0.0441(12) 0.0397(12) -0.0051(10) 0.0188(9) -0.0111(9) C28 0.0343(11) 0.0288(10) 0.0442(12) -0.0050(9) 0.0245(10) -0.0012(8) C29 0.0457(13) 0.0384(12) 0.0402(12) -0.0093(10) 0.0241(10) -0.0062(10) C30 0.0589(17) 0.0562(17) 0.0514(16) -0.0233(13) 0.0300(14) -0.0102(13) C31 0.0593(18) 0.0483(16) 0.089(2) -0.0332(16) 0.0432(18) -0.0093(13) C32 0.0579(17) 0.0300(12) 0.109(3) -0.0102(14) 0.0539(19) 0.0034(11) C33 0.0386(12) 0.0345(12) 0.0699(17) 0.0014(11) 0.0341(12) 0.0060(9) C34 0.0683(18) 0.0445(14) 0.0321(12) 0.0018(10) 0.0138(12) -0.0028(12) C35 0.101(3) 0.072(2) 0.143(4) -0.070(3) 0.056(3) -0.017(2) C36 0.0543(17) 0.0529(17) 0.090(2) 0.0274(16) 0.0330(17) 0.0245(14) C37 0.0312(10) 0.0320(10) 0.0383(11) -0.0085(9) 0.0170(9) -0.0103(8) C38 0.0326(11) 0.0490(13) 0.0383(12) -0.0084(10) 0.0161(9) -0.0144(10) C39 0.0432(14) 0.0684(18) 0.0472(15) -0.0272(13) 0.0203(12) -0.0222(13) C40 0.0444(15) 0.0519(16) 0.079(2) -0.0349(15) 0.0286(15) -0.0166(12) C41 0.0458(15) 0.0348(12) 0.079(2) -0.0136(13) 0.0263(14) -0.0085(11) C42 0.0361(12) 0.0339(11) 0.0539(15) -0.0046(10) 0.0196(11) -0.0096(9) C43 0.0511(15) 0.0701(19) 0.0339(13) 0.0016(12) 0.0097(11) -0.0081(13) C44 0.077(2) 0.074(2) 0.111(3) -0.060(2) 0.036(2) -0.0142(19) C45 0.0552(16) 0.0387(13) 0.0567(16) 0.0104(12) 0.0194(13) -0.0004(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C3 1.900(3) . ? Ru1 C2 1.927(2) . ? Ru1 C1 1.944(3) . ? Ru1 C4 2.1093(19) . ? Ru1 C25 2.1125(19) . ? O1 C1 1.141(3) . ? O2 C2 1.147(3) . ? O3 C3 1.157(3) . ? N1 C4 1.372(2) . ? N1 C5 1.388(2) . ? N1 C7 1.446(2) . ? N2 C4 1.369(2) . ? N2 C6 1.394(2) . ? N2 C16 1.445(3) . ? N3 C25 1.368(3) . ? N3 C26 1.391(3) . ? N3 C28 1.438(3) . ? N4 C25 1.374(3) . ? N4 C27 1.389(3) . ? N4 C37 1.441(3) . ? C5 C6 1.341(3) . ? C7 C8 1.395(3) . ? C7 C12 1.405(3) . ? C8 C9 1.400(3) . ? C8 C13 1.494(4) . ? C9 C10 1.376(4) . ? C10 C11 1.384(4) . ? C10 C14 1.518(4) . ? C11 C12 1.395(3) . ? C12 C15 1.500(3) . ? C16 C21 1.392(3) . ? C16 C17 1.393(3) . ? C17 C18 1.401(3) . ? C17 C22 1.498(4) . ? C18 C19 1.377(5) . ? C19 C20 1.372(5) . ? C19 C23 1.512(4) . ? C20 C21 1.400(3) . ? C21 C24 1.493(4) . ? C26 C27 1.339(3) . ? C28 C33 1.391(3) . ? C28 C29 1.393(3) . ? C29 C30 1.400(3) . ? C29 C34 1.501(4) . ? C30 C31 1.379(5) . ? C31 C32 1.380(5) . ? C31 C35 1.515(4) . ? C32 C33 1.394(4) . ? C33 C36 1.501(4) . ? C37 C38 1.395(3) . ? C37 C42 1.398(3) . ? C38 C39 1.391(4) . ? C38 C43 1.488(4) . ? C39 C40 1.373(5) . ? C40 C41 1.383(5) . ? C40 C44 1.528(4) . ? C41 C42 1.397(4) . ? C42 C45 1.504(4) . ? 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 C3 Ru1 C2 111.32(12) . . ? C3 Ru1 C1 139.56(14) . . ? C2 Ru1 C1 109.12(13) . . ? C3 Ru1 C4 90.21(9) . . ? C2 Ru1 C4 95.74(8) . . ? C1 Ru1 C4 85.97(9) . . ? C3 Ru1 C25 83.67(9) . . ? C2 Ru1 C25 94.82(8) . . ? C1 Ru1 C25 92.87(9) . . ? C4 Ru1 C25 169.16(7) . . ? C4 N1 C5 111.79(16) . . ? C4 N1 C7 128.49(16) . . ? C5 N1 C7 119.11(16) . . ? C4 N2 C6 112.06(16) . . ? C4 N2 C16 126.94(16) . . ? C6 N2 C16 120.01(16) . . ? C25 N3 C26 112.25(17) . . ? C25 N3 C28 127.34(17) . . ? C26 N3 C28 119.97(17) . . ? C25 N4 C27 111.87(17) . . ? C25 N4 C37 128.32(16) . . ? C27 N4 C37 119.65(17) . . ? O1 C1 Ru1 174.9(3) . . ? O2 C2 Ru1 179.7(3) . . ? O3 C3 Ru1 175.1(3) . . ? N2 C4 N1 102.70(15) . . ? N2 C4 Ru1 130.63(14) . . ? N1 C4 Ru1 126.50(13) . . ? C6 C5 N1 107.10(17) . . ? C5 C6 N2 106.34(17) . . ? C8 C7 C12 122.2(2) . . ? C8 C7 N1 119.86(19) . . ? C12 C7 N1 117.35(18) . . ? C7 C8 C9 117.1(2) . . ? C7 C8 C13 122.4(2) . . ? C9 C8 C13 120.4(2) . . ? C10 C9 C8 122.5(2) . . ? C9 C10 C11 118.8(2) . . ? C9 C10 C14 120.8(3) . . ? C11 C10 C14 120.4(3) . . ? C10 C11 C12 121.8(2) . . ? C11 C12 C7 117.5(2) . . ? C11 C12 C15 120.1(2) . . ? C7 C12 C15 122.3(2) . . ? C21 C16 C17 122.9(2) . . ? C21 C16 N2 117.2(2) . . ? C17 C16 N2 119.9(2) . . ? C16 C17 C18 116.6(3) . . ? C16 C17 C22 122.2(2) . . ? C18 C17 C22 121.2(3) . . ? C19 C18 C17 122.5(3) . . ? C20 C19 C18 118.9(2) . . ? C20 C19 C23 120.4(4) . . ? C18 C19 C23 120.7(4) . . ? C19 C20 C21 121.9(3) . . ? C16 C21 C20 117.3(3) . . ? C16 C21 C24 121.3(2) . . ? C20 C21 C24 121.4(3) . . ? N3 C25 N4 102.45(16) . . ? N3 C25 Ru1 130.19(14) . . ? N4 C25 Ru1 126.64(14) . . ? C27 C26 N3 106.46(19) . . ? C26 C27 N4 106.96(19) . . ? C33 C28 C29 122.9(2) . . ? C33 C28 N3 119.5(2) . . ? C29 C28 N3 117.49(19) . . ? C28 C29 C30 117.7(2) . . ? C28 C29 C34 121.1(2) . . ? C30 C29 C34 121.2(2) . . ? C31 C30 C29 121.2(3) . . ? C30 C31 C32 119.0(3) . . ? C30 C31 C35 120.5(4) . . ? C32 C31 C35 120.4(3) . . ? C31 C32 C33 122.6(3) . . ? C28 C33 C32 116.6(3) . . ? C28 C33 C36 121.3(2) . . ? C32 C33 C36 122.1(3) . . ? C38 C37 C42 122.1(2) . . ? C38 C37 N4 119.7(2) . . ? C42 C37 N4 117.8(2) . . ? C39 C38 C37 117.3(3) . . ? C39 C38 C43 120.1(2) . . ? C37 C38 C43 122.5(2) . . ? C40 C39 C38 122.5(3) . . ? C39 C40 C41 118.8(2) . . ? C39 C40 C44 120.4(3) . . ? C41 C40 C44 120.8(3) . . ? C40 C41 C42 121.7(3) . . ? C41 C42 C37 117.6(3) . . ? C41 C42 C45 120.7(3) . . ? C37 C42 C45 121.7(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.943 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.077 data_c:\backup\helix\h03rfrj3\maxus\h02rfrj3 _database_code_depnum_ccdc_archive 'CCDC 668486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.20 H51.20 Cl N4 O Ru' _chemical_formula_weight 791.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8640(5) _cell_length_b 20.8610(7) _cell_length_c 19.3630(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.281(2) _cell_angle_gamma 90.00 _cell_volume 7954.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 67372 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.733 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3307 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9288 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33547 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.76 _reflns_number_total 8457 _reflns_number_gt 4707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo & Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+5.8110*P+(0.0428P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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 8457 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.076024(18) 0.7500 0.02368(13) Uani 1 2 d S . . Ru2 Ru 0.0000 -0.074575(18) 0.2500 0.02368(13) Uani 1 2 d S . . Cl1 Cl 0.38397(17) 0.0751(2) 0.7519(2) 0.0327(10) Uani 0.50 1 d P A 2 Cl2A Cl 0.0000 0.0426(2) 0.2500 0.0263(15) Uani 0.50 2 d SP B 1 Cl2B Cl 0.0000 -0.1932(4) 0.2500 0.0529(16) Uani 0.50 2 d SP B 2 O1 O 0.3590(5) 0.0755(8) 0.7532(9) 0.046(3) Uani 0.50 1 d P A 1 O8 O 0.0000 0.0667(6) 0.2500 0.040(5) Uani 0.50 2 d SP B 2 O9 O 0.0000 -0.2139(10) 0.2500 0.092(10) Uiso 0.50 2 d SP B 1 N1 N 0.42500(16) 0.03074(13) 0.59068(16) 0.0293(8) Uani 1 1 d . . . N2 N 0.47063(16) 0.12236(13) 0.58933(16) 0.0287(8) Uani 1 1 d . . . N3 N 0.00171(16) -0.09967(14) 0.40902(16) 0.0281(7) Uani 1 1 d . . . N4 N 0.09399(17) -0.05378(14) 0.41085(16) 0.0303(8) Uani 1 1 d . . . C1 C 0.46366(19) 0.07621(16) 0.63648(19) 0.0255(9) Uani 1 1 d . A . C2 C 0.4369(2) 0.10544(19) 0.5173(2) 0.0384(11) Uani 1 1 d . A . H2 H 0.4344 0.1301 0.4753 0.046 Uiso 1 1 calc R . . C3 C 0.4085(2) 0.04841(18) 0.5176(2) 0.0360(10) Uani 1 1 d . A . H3 H 0.3822 0.0245 0.4762 0.043 Uiso 1 1 calc R . . C4 C 0.4023(2) -0.02853(16) 0.61412(19) 0.0278(9) Uani 1 1 d . A . C5 C 0.3332(2) -0.03336(17) 0.6060(2) 0.0324(10) Uani 1 1 d . . . C6 C 0.3118(2) -0.09045(18) 0.6278(2) 0.0416(11) Uani 1 1 d . A . H6 H 0.2653 -0.0953 0.6232 0.050 Uiso 1 1 calc R . . C7 C 0.3564(2) -0.14102(17) 0.6563(2) 0.0438(11) Uani 1 1 d . . . C8 C 0.4236(2) -0.13400(17) 0.6624(2) 0.0351(10) Uani 1 1 d . A . H8 H 0.4540 -0.1685 0.6815 0.042 Uiso 1 1 calc R . . C9 C 0.4485(2) -0.07788(17) 0.64166(19) 0.0300(9) Uani 1 1 d . . . C10 C 0.2844(2) 0.02055(17) 0.5758(2) 0.0383(10) Uani 1 1 d . A . H10A H 0.2731 0.0222 0.5226 0.057 Uiso 1 1 calc R . . H10B H 0.3053 0.0612 0.5973 0.057 Uiso 1 1 calc R . . H10C H 0.2429 0.0135 0.5880 0.057 Uiso 1 1 calc R . . C11 C 0.3305(3) -0.20323(19) 0.6791(3) 0.0686(16) Uani 1 1 d . A . H11A H 0.3578 -0.2393 0.6719 0.103 Uiso 1 1 calc R . . H11B H 0.2829 -0.2097 0.6493 0.103 Uiso 1 1 calc R . . H11C H 0.3343 -0.2007 0.7309 0.103 Uiso 1 1 calc R . . C12 C 0.5218(2) -0.07216(17) 0.6487(2) 0.0361(10) Uani 1 1 d . A . H12A H 0.5258 -0.0516 0.6048 0.054 Uiso 1 1 calc R . . H12B H 0.5423 -0.1149 0.6542 0.054 Uiso 1 1 calc R . . H12C H 0.5454 -0.0462 0.6918 0.054 Uiso 1 1 calc R . . C13 C 0.5101(2) 0.18022(16) 0.61115(19) 0.0276(9) Uani 1 1 d . A . C14 C 0.5741(2) 0.18287(17) 0.6027(2) 0.0316(10) Uani 1 1 d . . . C15 C 0.6112(2) 0.23883(17) 0.6241(2) 0.0353(10) Uani 1 1 d . A . H15 H 0.6547 0.2419 0.6184 0.042 Uiso 1 1 calc R . . C16 C 0.5871(2) 0.29076(17) 0.6536(2) 0.0350(10) Uani 1 1 d . . . C17 C 0.5229(2) 0.28619(17) 0.6599(2) 0.0342(10) Uani 1 1 d . A . H17 H 0.5054 0.3215 0.6790 0.041 Uiso 1 1 calc R . . C18 C 0.4834(2) 0.23098(17) 0.6389(2) 0.0331(10) Uani 1 1 d . . . C19 C 0.6010(2) 0.12768(18) 0.5703(2) 0.0412(11) Uani 1 1 d . A . H19A H 0.5755 0.1244 0.5179 0.062 Uiso 1 1 calc R . . H19B H 0.5961 0.0878 0.5948 0.062 Uiso 1 1 calc R . . H19C H 0.6492 0.1349 0.5771 0.062 Uiso 1 1 calc R . . C20 C 0.6294(2) 0.34995(17) 0.6785(2) 0.0426(11) Uani 1 1 d . A . H20A H 0.6644 0.3417 0.7258 0.064 Uiso 1 1 calc R . . H20B H 0.6003 0.3853 0.6837 0.064 Uiso 1 1 calc R . . H20C H 0.6510 0.3615 0.6424 0.064 Uiso 1 1 calc R . . C21 C 0.4136(2) 0.22860(19) 0.6450(3) 0.0531(13) Uani 1 1 d . A . H21A H 0.4128 0.1973 0.6824 0.080 Uiso 1 1 calc R . . H21B H 0.3807 0.2160 0.5978 0.080 Uiso 1 1 calc R . . H21C H 0.4015 0.2710 0.6587 0.080 Uiso 1 1 calc R . . C22 C 0.0337(2) -0.07547(16) 0.36359(19) 0.0264(9) Uani 1 1 d . B . C23 C 0.0414(2) -0.09346(19) 0.4814(2) 0.0372(10) Uani 1 1 d . B . H23 H 0.0298 -0.1070 0.5226 0.045 Uiso 1 1 calc R . . C24 C 0.0989(2) -0.06504(19) 0.4831(2) 0.0400(11) Uani 1 1 d . B . H24 H 0.1361 -0.0545 0.5254 0.048 Uiso 1 1 calc R . . C25 C -0.0639(2) -0.12948(17) 0.38552(19) 0.0292(9) Uani 1 1 d . B . C26 C -0.0665(2) -0.19634(18) 0.3940(2) 0.0345(10) Uani 1 1 d . . . C27 C -0.1295(2) -0.2250(2) 0.3721(3) 0.0492(12) Uani 1 1 d . B . H27 H -0.1324 -0.2700 0.3782 0.059 Uiso 1 1 calc R . . C28 C -0.1895(2) -0.18986(19) 0.3411(3) 0.0456(11) Uani 1 1 d . . . C29 C -0.1846(2) -0.12404(18) 0.3337(2) 0.0371(10) Uani 1 1 d . B . H29 H -0.2249 -0.0997 0.3130 0.044 Uiso 1 1 calc R . . C30 C -0.1221(2) -0.09295(16) 0.3558(2) 0.0299(9) Uani 1 1 d . . . C31 C -0.1186(2) -0.02121(16) 0.3469(2) 0.0373(10) Uani 1 1 d . B . H31A H -0.0856 -0.0029 0.3909 0.056 Uiso 1 1 calc R . . H31B H -0.1634 -0.0024 0.3396 0.056 Uiso 1 1 calc R . . H31C H -0.1046 -0.0118 0.3044 0.056 Uiso 1 1 calc R . . C32 C -0.2584(2) -0.2220(2) 0.3168(3) 0.0677(15) Uani 1 1 d . B . H32A H -0.2937 -0.1900 0.2955 0.102 Uiso 1 1 calc R . . H32B H -0.2663 -0.2421 0.3591 0.102 Uiso 1 1 calc R . . H32C H -0.2598 -0.2549 0.2802 0.102 Uiso 1 1 calc R . . C33 C -0.0034(2) -0.23563(18) 0.4249(2) 0.0440(11) Uani 1 1 d . B . H33A H 0.0140 -0.2306 0.4782 0.066 Uiso 1 1 calc R . . H33B H 0.0310 -0.2212 0.4041 0.066 Uiso 1 1 calc R . . H33C H -0.0139 -0.2809 0.4127 0.066 Uiso 1 1 calc R . . C34 C 0.14564(19) -0.02158(17) 0.38969(18) 0.0280(9) Uani 1 1 d . B . C35 C 0.1511(2) 0.04485(17) 0.3969(2) 0.0316(10) Uani 1 1 d . . . C36 C 0.2003(2) 0.07481(18) 0.3749(2) 0.0351(10) Uani 1 1 d . B . H36 H 0.2046 0.1201 0.3791 0.042 Uiso 1 1 calc R . . C37 C 0.2433(2) 0.04157(17) 0.3471(2) 0.0322(9) Uani 1 1 d . . . C38 C 0.23818(19) -0.02483(18) 0.3429(2) 0.0331(9) Uani 1 1 d . B . H38 H 0.2684 -0.0485 0.3252 0.040 Uiso 1 1 calc R . . C39 C 0.1894(2) -0.05724(17) 0.3641(2) 0.0319(9) Uani 1 1 d . . . C40 C 0.1049(2) 0.08253(18) 0.4278(2) 0.0425(11) Uani 1 1 d . B . H40A H 0.1124 0.1285 0.4233 0.064 Uiso 1 1 calc R . . H40B H 0.1149 0.0715 0.4795 0.064 Uiso 1 1 calc R . . H40C H 0.0575 0.0720 0.4005 0.064 Uiso 1 1 calc R . . C41 C 0.2961(2) 0.07572(18) 0.3225(2) 0.0401(10) Uani 1 1 d . B . H41A H 0.2738 0.0977 0.2760 0.060 Uiso 1 1 calc R . . H41B H 0.3286 0.0444 0.3159 0.060 Uiso 1 1 calc R . . H41C H 0.3202 0.1071 0.3596 0.060 Uiso 1 1 calc R . . C42 C 0.1855(2) -0.12956(17) 0.3598(3) 0.0517(12) Uani 1 1 d . B . H42A H 0.1895 -0.1471 0.4079 0.078 Uiso 1 1 calc R . . H42B H 0.2226 -0.1460 0.3443 0.078 Uiso 1 1 calc R . . H42C H 0.1419 -0.1425 0.3242 0.078 Uiso 1 1 calc R . . C101 C 0.2210(15) 0.1979(11) 0.5135(11) 0.053(7) Uani 0.20 1 d P . . H101 H 0.1996 0.1601 0.5222 0.064 Uiso 0.20 1 calc PR . . C102 C 0.2794(15) 0.1919(10) 0.5047(11) 0.050(7) Uani 0.20 1 d P . . H102 H 0.2998 0.1507 0.5091 0.060 Uiso 0.20 1 calc PR . . C103 C 0.3129(12) 0.2443(12) 0.4888(12) 0.059(7) Uani 0.20 1 d P . . H103 H 0.3550 0.2411 0.4802 0.071 Uiso 0.20 1 calc PR . . C201 C 0.1917(15) 0.281(2) -0.0090(16) 0.086(10) Uani 0.20 1 d P . . H201 H 0.1496 0.3013 -0.0146 0.103 Uiso 0.20 1 calc PR . . C202 C 0.1951(17) 0.2165(17) -0.0030(15) 0.079(9) Uani 0.20 1 d P . . H202 H 0.1550 0.1933 -0.0061 0.095 Uiso 0.20 1 calc PR . . C203 C 0.255(2) 0.1827(15) 0.0074(16) 0.093(11) Uani 0.20 1 d P . . H203 H 0.2582 0.1374 0.0130 0.112 Uiso 0.20 1 calc PR . . C1A C 0.4149(7) 0.0750(8) 0.7500(8) 0.034(3) Uani 0.50 1 d P A 1 C2A C 0.0000 0.0132(7) 0.2500 0.023(4) Uani 0.50 2 d SP B 2 C2B C 0.0000 -0.1605(8) 0.2500 0.047(6) Uani 0.50 2 d SP B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0196(3) 0.0235(2) 0.0281(2) 0.000 0.0081(2) 0.000 Ru2 0.0197(3) 0.0246(2) 0.0281(2) 0.000 0.0097(2) 0.000 Cl1 0.018(3) 0.0451(15) 0.0371(14) -0.0002(12) 0.013(3) 0.005(3) Cl2A 0.032(2) 0.013(5) 0.036(2) 0.000 0.0122(17) 0.000 Cl2B 0.059(4) 0.065(6) 0.036(3) 0.000 0.017(2) 0.000 O1 0.007(6) 0.085(5) 0.052(4) -0.004(4) 0.016(5) 0.009(6) O8 0.056(8) 0.017(9) 0.046(6) 0.000 0.015(5) 0.000 N1 0.033(2) 0.0248(16) 0.0313(18) -0.0017(14) 0.0118(16) -0.0059(15) N2 0.029(2) 0.0248(16) 0.0314(18) 0.0015(14) 0.0092(16) -0.0057(15) N3 0.019(2) 0.0349(17) 0.0303(18) -0.0001(14) 0.0083(16) -0.0052(15) N4 0.024(2) 0.0376(18) 0.0301(18) 0.0008(14) 0.0096(16) -0.0069(15) C1 0.023(2) 0.0231(18) 0.031(2) 0.0010(17) 0.0109(19) 0.0015(18) C2 0.044(3) 0.041(2) 0.028(2) 0.0062(18) 0.009(2) -0.008(2) C3 0.043(3) 0.037(2) 0.025(2) -0.0025(17) 0.008(2) -0.009(2) C4 0.034(3) 0.0229(18) 0.028(2) -0.0044(16) 0.0120(19) -0.0068(18) C5 0.031(3) 0.028(2) 0.038(2) -0.0040(17) 0.011(2) -0.0011(19) C6 0.032(3) 0.038(2) 0.061(3) -0.003(2) 0.023(2) -0.005(2) C7 0.048(3) 0.026(2) 0.068(3) 0.004(2) 0.034(3) -0.003(2) C8 0.036(3) 0.024(2) 0.050(2) 0.0017(18) 0.020(2) 0.0012(19) C9 0.034(3) 0.030(2) 0.029(2) -0.0056(17) 0.0148(19) -0.005(2) C10 0.028(3) 0.035(2) 0.049(3) -0.0028(19) 0.009(2) -0.0051(19) C11 0.059(4) 0.036(2) 0.128(5) 0.015(3) 0.053(4) -0.007(2) C12 0.035(3) 0.033(2) 0.045(2) -0.0010(19) 0.019(2) 0.002(2) C13 0.027(2) 0.0219(19) 0.030(2) 0.0037(16) 0.0044(18) -0.0039(18) C14 0.029(3) 0.031(2) 0.035(2) 0.0003(17) 0.012(2) 0.0003(19) C15 0.025(3) 0.039(2) 0.043(2) -0.0017(19) 0.013(2) -0.006(2) C16 0.038(3) 0.026(2) 0.040(2) 0.0029(17) 0.012(2) -0.0044(19) C17 0.035(3) 0.024(2) 0.047(2) -0.0010(17) 0.017(2) 0.0000(19) C18 0.025(3) 0.030(2) 0.047(2) 0.0051(18) 0.015(2) -0.0033(19) C19 0.034(3) 0.041(2) 0.051(3) -0.007(2) 0.018(2) 0.000(2) C20 0.037(3) 0.035(2) 0.054(3) 0.001(2) 0.013(2) -0.009(2) C21 0.034(3) 0.037(2) 0.094(4) -0.004(2) 0.030(3) -0.006(2) C22 0.022(2) 0.0264(19) 0.033(2) -0.0010(17) 0.011(2) -0.0005(18) C23 0.029(3) 0.053(2) 0.031(2) 0.0035(19) 0.012(2) -0.011(2) C24 0.028(3) 0.061(3) 0.026(2) 0.000(2) 0.0026(19) -0.011(2) C25 0.024(3) 0.038(2) 0.029(2) -0.0010(17) 0.0145(19) -0.0047(19) C26 0.026(3) 0.035(2) 0.045(3) 0.0028(19) 0.016(2) -0.001(2) C27 0.039(3) 0.031(2) 0.083(4) 0.004(2) 0.028(3) -0.001(2) C28 0.024(3) 0.038(2) 0.078(3) -0.006(2) 0.020(3) -0.007(2) C29 0.021(2) 0.038(2) 0.053(3) -0.005(2) 0.014(2) 0.0015(19) C30 0.027(3) 0.032(2) 0.036(2) -0.0033(17) 0.017(2) -0.0013(18) C31 0.030(3) 0.038(2) 0.047(2) -0.0067(19) 0.017(2) 0.000(2) C32 0.029(3) 0.051(3) 0.125(5) -0.009(3) 0.027(3) -0.007(2) C33 0.036(3) 0.038(2) 0.063(3) 0.011(2) 0.024(2) 0.004(2) C34 0.017(2) 0.038(2) 0.028(2) 0.0056(17) 0.0047(17) -0.0029(18) C35 0.028(3) 0.035(2) 0.034(2) 0.0017(17) 0.012(2) -0.0030(19) C36 0.036(3) 0.028(2) 0.040(2) 0.0028(18) 0.011(2) -0.006(2) C37 0.021(2) 0.038(2) 0.038(2) 0.0046(18) 0.0104(19) -0.0024(19) C38 0.019(2) 0.039(2) 0.044(2) 0.0002(18) 0.0135(19) 0.0001(19) C39 0.022(2) 0.034(2) 0.038(2) 0.0036(17) 0.0077(19) -0.0005(18) C40 0.040(3) 0.043(2) 0.048(3) -0.001(2) 0.020(2) 0.002(2) C41 0.029(3) 0.042(2) 0.052(3) 0.007(2) 0.016(2) -0.006(2) C42 0.042(3) 0.034(2) 0.087(3) -0.003(2) 0.032(3) -0.004(2) C101 0.07(2) 0.043(14) 0.034(13) 0.013(10) 0.006(14) -0.024(14) C102 0.08(2) 0.029(12) 0.035(13) -0.006(9) 0.015(14) 0.013(13) C103 0.044(17) 0.084(18) 0.068(17) 0.039(14) 0.043(14) 0.022(15) C201 0.035(19) 0.13(3) 0.09(2) -0.05(2) 0.014(17) -0.01(2) C202 0.08(3) 0.09(2) 0.08(2) 0.005(18) 0.04(2) -0.02(2) C203 0.07(3) 0.09(2) 0.09(2) 0.031(18) -0.01(2) 0.03(2) C1A 0.035(9) 0.038(5) 0.036(5) -0.003(4) 0.020(8) 0.002(8) C2A 0.021(7) 0.026(11) 0.022(6) 0.000 0.007(5) 0.000 C2B 0.043(11) 0.059(13) 0.042(9) 0.000 0.016(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1A 1.776(12) 2_656 ? Ru1 C1A 1.776(12) . ? Ru1 C1 2.075(3) 2_656 ? Ru1 C1 2.075(3) . ? Ru1 Cl1 2.433(3) . ? Ru1 Cl1 2.433(3) 2_656 ? Ru2 C2B 1.793(17) . ? Ru2 C2A 1.832(14) . ? Ru2 C22 2.076(4) . ? Ru2 C22 2.076(4) 2 ? Ru2 Cl2A 2.445(5) . ? Ru2 Cl2B 2.474(9) . ? O1 C1A 1.189(13) . ? O8 C2A 1.11(2) . ? O9 C2B 1.11(3) . ? N1 C1 1.366(4) . ? N1 C3 1.391(4) . ? N1 C4 1.449(4) . ? N2 C1 1.367(4) . ? N2 C2 1.384(4) . ? N2 C13 1.444(4) . ? N3 C22 1.365(4) . ? N3 C23 1.379(5) . ? N3 C25 1.435(5) . ? N4 C22 1.365(4) . ? N4 C24 1.388(4) . ? N4 C34 1.439(4) . ? C2 C3 1.329(5) . ? C4 C9 1.390(5) . ? C4 C5 1.401(5) . ? C5 C6 1.386(5) . ? C5 C10 1.500(5) . ? C6 C7 1.394(6) . ? C7 C8 1.375(6) . ? C7 C11 1.526(5) . ? C8 C9 1.393(5) . ? C9 C12 1.495(5) . ? C13 C18 1.386(5) . ? C13 C14 1.398(5) . ? C14 C15 1.387(5) . ? C14 C19 1.506(5) . ? C15 C16 1.395(5) . ? C16 C17 1.388(5) . ? C16 C20 1.501(5) . ? C17 C18 1.396(5) . ? C18 C21 1.500(5) . ? C23 C24 1.329(5) . ? C25 C30 1.387(5) . ? C25 C26 1.407(5) . ? C26 C27 1.378(6) . ? C26 C33 1.497(5) . ? C27 C28 1.403(6) . ? C28 C29 1.388(5) . ? C28 C32 1.515(6) . ? C29 C30 1.392(5) . ? C30 C31 1.511(5) . ? C34 C39 1.389(5) . ? C34 C35 1.394(5) . ? C35 C36 1.384(5) . ? C35 C40 1.511(5) . ? C36 C37 1.377(5) . ? C37 C38 1.390(5) . ? C37 C41 1.515(5) . ? C38 C39 1.393(5) . ? C39 C42 1.512(5) . ? C101 C102 1.29(3) . ? C101 C103 1.39(3) 7_556 ? C102 C103 1.39(3) . ? C103 C101 1.39(3) 7_556 ? C201 C203 1.33(4) 7 ? C201 C202 1.35(4) . ? C202 C203 1.39(4) . ? C203 C201 1.33(4) 7 ? 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 C1A Ru1 C1A 178.6(11) 2_656 . ? C1A Ru1 C1 89.1(5) 2_656 2_656 ? C1A Ru1 C1 90.9(5) . 2_656 ? C1A Ru1 C1 90.9(5) 2_656 . ? C1A Ru1 C1 89.1(5) . . ? C1 Ru1 C1 179.78(19) 2_656 . ? C1A Ru1 Cl1 178.6(5) 2_656 . ? C1A Ru1 Cl1 0.9(5) . . ? C1 Ru1 Cl1 90.08(14) 2_656 . ? C1 Ru1 Cl1 89.92(14) . . ? C1A Ru1 Cl1 0.9(5) 2_656 2_656 ? C1A Ru1 Cl1 178.6(5) . 2_656 ? C1 Ru1 Cl1 89.92(14) 2_656 2_656 ? C1 Ru1 Cl1 90.08(14) . 2_656 ? Cl1 Ru1 Cl1 179.1(2) . 2_656 ? C2B Ru2 C2A 180.000(1) . . ? C2B Ru2 C22 89.49(9) . . ? C2A Ru2 C22 90.51(9) . . ? C2B Ru2 C22 89.49(9) . 2 ? C2A Ru2 C22 90.51(9) . 2 ? C22 Ru2 C22 178.97(19) . 2 ? C2B Ru2 Cl2A 180.0 . . ? C2A Ru2 Cl2A 0.0 . . ? C22 Ru2 Cl2A 90.51(9) . . ? C22 Ru2 Cl2A 90.51(9) 2 . ? C2B Ru2 Cl2B 0.0 . . ? C2A Ru2 Cl2B 180.000(1) . . ? C22 Ru2 Cl2B 89.49(9) . . ? C22 Ru2 Cl2B 89.49(9) 2 . ? Cl2A Ru2 Cl2B 180.0 . . ? C1 N1 C3 111.8(3) . . ? C1 N1 C4 125.0(3) . . ? C3 N1 C4 123.2(3) . . ? C1 N2 C2 111.2(3) . . ? C1 N2 C13 124.7(3) . . ? C2 N2 C13 124.0(3) . . ? C22 N3 C23 111.2(3) . . ? C22 N3 C25 125.1(3) . . ? C23 N3 C25 123.6(3) . . ? C22 N4 C24 111.4(3) . . ? C22 N4 C34 125.0(3) . . ? C24 N4 C34 123.5(3) . . ? N1 C1 N2 103.0(3) . . ? N1 C1 Ru1 128.1(2) . . ? N2 C1 Ru1 128.8(3) . . ? C3 C2 N2 107.6(3) . . ? C2 C3 N1 106.3(3) . . ? C9 C4 C5 123.1(3) . . ? C9 C4 N1 119.7(3) . . ? C5 C4 N1 117.2(3) . . ? C6 C5 C4 116.8(4) . . ? C6 C5 C10 121.1(4) . . ? C4 C5 C10 122.1(3) . . ? C5 C6 C7 122.1(4) . . ? C8 C7 C6 118.8(4) . . ? C8 C7 C11 120.9(4) . . ? C6 C7 C11 120.3(4) . . ? C7 C8 C9 122.1(4) . . ? C4 C9 C8 117.1(4) . . ? C4 C9 C12 122.3(3) . . ? C8 C9 C12 120.6(4) . . ? C18 C13 C14 122.5(3) . . ? C18 C13 N2 119.2(3) . . ? C14 C13 N2 118.3(3) . . ? C15 C14 C13 117.3(3) . . ? C15 C14 C19 121.3(4) . . ? C13 C14 C19 121.4(3) . . ? C14 C15 C16 122.3(4) . . ? C17 C16 C15 118.2(4) . . ? C17 C16 C20 120.7(3) . . ? C15 C16 C20 121.1(4) . . ? C16 C17 C18 121.7(3) . . ? C13 C18 C17 117.9(4) . . ? C13 C18 C21 122.1(3) . . ? C17 C18 C21 119.9(3) . . ? N4 C22 N3 103.2(3) . . ? N4 C22 Ru2 128.5(3) . . ? N3 C22 Ru2 128.2(3) . . ? C24 C23 N3 107.5(3) . . ? C23 C24 N4 106.6(4) . . ? C30 C25 C26 122.1(4) . . ? C30 C25 N3 120.4(3) . . ? C26 C25 N3 117.4(4) . . ? C27 C26 C25 117.6(4) . . ? C27 C26 C33 120.6(4) . . ? C25 C26 C33 121.9(4) . . ? C26 C27 C28 122.0(4) . . ? C29 C28 C27 118.5(4) . . ? C29 C28 C32 120.0(4) . . ? C27 C28 C32 121.5(4) . . ? C28 C29 C30 121.5(4) . . ? C25 C30 C29 118.3(3) . . ? C25 C30 C31 121.5(4) . . ? C29 C30 C31 120.1(4) . . ? C39 C34 C35 121.8(3) . . ? C39 C34 N4 119.5(3) . . ? C35 C34 N4 118.6(3) . . ? C36 C35 C34 117.5(4) . . ? C36 C35 C40 121.4(3) . . ? C34 C35 C40 121.0(3) . . ? C37 C36 C35 122.6(3) . . ? C36 C37 C38 118.5(3) . . ? C36 C37 C41 121.5(3) . . ? C38 C37 C41 120.0(3) . . ? C37 C38 C39 121.1(4) . . ? C34 C39 C38 118.4(3) . . ? C34 C39 C42 121.7(3) . . ? C38 C39 C42 119.9(3) . . ? C102 C101 C103 125(2) . 7_556 ? C101 C102 C103 121(2) . . ? C102 C103 C101 114(2) . 7_556 ? C203 C201 C202 123(3) 7 . ? C201 C202 C203 122(3) . . ? C201 C203 C202 115(3) 7 . ? O1 C1A Ru1 176.9(19) . . ? O8 C2A Ru2 180.000(1) . . ? O9 C2B Ru2 180.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.563 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.075 data_c:\x-ray\kappa\k06mkw6\maxus\k06mkw6 _database_code_depnum_ccdc_archive 'CCDC 668487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H93 Cl N4 O Ru' _chemical_formula_weight 1046.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P22121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6170(1) _cell_length_b 13.0050(1) _cell_length_c 20.6750(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2854.68(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 77547 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.364 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58230 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8352 _reflns_number_gt 7900 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+1.1316P] 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 SHELXL _refine_ls_extinction_coef 0.0031(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(04) _refine_ls_number_reflns 8352 _refine_ls_number_parameters 361 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.092977(15) 0.0000 0.0000 0.01713(5) Uani 1 2 d S . . Cl1 Cl 0.31432(18) 0.0000 0.0000 0.0328(3) Uani 0.60 2 d SP A 1 Cl1A Cl -0.1280(3) 0.0000 0.0000 0.0318(5) Uani 0.40 2 d SP A 2 O1 O -0.1902(4) 0.0000 0.0000 0.0479(11) Uani 0.60 2 d SP A 1 O1A O 0.3801(7) 0.0000 0.0000 0.0560(19) Uani 0.40 2 d SP A 2 N1 N 0.05689(16) -0.04134(12) -0.14681(7) 0.0238(3) Uani 1 1 d . . . N2 N 0.14431(16) 0.10678(11) -0.13084(7) 0.0232(3) Uani 1 1 d . . . C30A C 0.6504(8) 0.4608(5) 0.0618(3) 0.0656(13) Uani 0.50 1 d PDU B 2 H30A H 0.6881 0.3926 0.0530 0.079 Uiso 0.50 1 calc PR B 2 H30B H 0.7196 0.5084 0.0733 0.079 Uiso 0.50 1 calc PR B 2 C31A C 0.5670(10) 0.4520(7) 0.1156(4) 0.0639(12) Uani 0.50 1 d PDU B 2 H31A H 0.5505 0.3781 0.1233 0.077 Uiso 0.50 1 calc PR B 2 H31B H 0.4858 0.4843 0.1037 0.077 Uiso 0.50 1 calc PR B 2 C32A C 0.6096(6) 0.4969(6) 0.1746(3) 0.0620(12) Uani 0.50 1 d PDU B 2 H32A H 0.5421 0.4937 0.2069 0.093 Uiso 0.50 1 calc PR B 2 H32B H 0.6329 0.5688 0.1670 0.093 Uiso 0.50 1 calc PR B 2 H32C H 0.6832 0.4589 0.1905 0.093 Uiso 0.50 1 calc PR B 2 C1 C -0.0823(6) 0.0000 0.0000 0.0278(13) Uani 0.60 2 d SP A 1 C2 C 0.09709(16) 0.02370(11) -0.09991(7) 0.0185(3) Uani 1 1 d . A . C3 C 0.0913(3) -0.0059(2) -0.21243(8) 0.0519(7) Uani 1 1 d . A . H3A H 0.0192 -0.0115 -0.2426 0.062 Uiso 1 1 calc R . . H3B H 0.1633 -0.0456 -0.2299 0.062 Uiso 1 1 calc R . . C4 C 0.1262(3) 0.10286(16) -0.20127(9) 0.0384(5) Uani 1 1 d . A . H4A H 0.2047 0.1210 -0.2245 0.046 Uiso 1 1 calc R . . H4B H 0.0580 0.1499 -0.2152 0.046 Uiso 1 1 calc R . . C5 C 0.01840(18) -0.14690(13) -0.14014(8) 0.0221(3) Uani 1 1 d . A . C6 C 0.11065(18) -0.22302(14) -0.13303(9) 0.0257(4) Uani 1 1 d . . . C7 C 0.0718(2) -0.32559(15) -0.13227(10) 0.0305(4) Uani 1 1 d . A . H7 H 0.1326 -0.3786 -0.1272 0.037 Uiso 1 1 calc R . . C8 C -0.0539(2) -0.35101(15) -0.13873(10) 0.0316(4) Uani 1 1 d . . . H8 H -0.0789 -0.4212 -0.1381 0.038 Uiso 1 1 calc R A . C9 C -0.1436(2) -0.27476(16) -0.14607(11) 0.0295(5) Uani 1 1 d . A . H9 H -0.2298 -0.2933 -0.1502 0.035 Uiso 1 1 calc R . . C10 C -0.10986(18) -0.17093(13) -0.14756(8) 0.0251(3) Uani 1 1 d . . . C11 C 0.25059(19) -0.19883(18) -0.12904(10) 0.0307(4) Uani 1 1 d . A . H11 H 0.2610 -0.1228 -0.1241 0.037 Uiso 1 1 calc R . . C12 C 0.3196(3) -0.2331(3) -0.19105(13) 0.0615(9) Uani 1 1 d . . . H12A H 0.3067 -0.3070 -0.1977 0.092 Uiso 1 1 calc R A . H12B H 0.4098 -0.2189 -0.1867 0.092 Uiso 1 1 calc R . . H12C H 0.2860 -0.1952 -0.2282 0.092 Uiso 1 1 calc R . . C13 C 0.3128(2) -0.2516(2) -0.07169(14) 0.0423(5) Uani 1 1 d . . . H13A H 0.2653 -0.2361 -0.0322 0.063 Uiso 1 1 calc R A . H13B H 0.3994 -0.2265 -0.0671 0.063 Uiso 1 1 calc R . . H13C H 0.3138 -0.3261 -0.0788 0.063 Uiso 1 1 calc R . . C14 C -0.2112(2) -0.08969(17) -0.15824(12) 0.0368(5) Uani 1 1 d . A . H14 H -0.1773 -0.0215 -0.1442 0.044 Uiso 1 1 calc R . . C15 C -0.2438(3) -0.0837 -0.2309 0.0675(9) Uani 1 1 d . . . H15A H -0.2726 -0.1512 -0.2459 0.101 Uiso 1 1 calc R A . H15B H -0.1688 -0.0632 -0.2553 0.101 Uiso 1 1 calc R . . H15C H -0.3107 -0.0329 -0.2376 0.101 Uiso 1 1 calc R . . C16 C -0.3313(2) -0.1119(2) -0.12005(15) 0.0485(6) Uani 1 1 d . . . H16A H -0.3711 -0.1744 -0.1369 0.073 Uiso 1 1 calc R A . H16B H -0.3896 -0.0539 -0.1245 0.073 Uiso 1 1 calc R . . H16C H -0.3103 -0.1216 -0.0743 0.073 Uiso 1 1 calc R . . C17 C 0.17629(18) 0.20600(13) -0.10479(9) 0.0227(3) Uani 1 1 d . A . C18 C 0.07908(19) 0.27386(14) -0.08753(9) 0.0252(3) Uani 1 1 d . . . C19 C 0.1118(2) 0.37477(14) -0.07044(10) 0.0315(4) Uani 1 1 d . A . H19 H 0.0478 0.4218 -0.0579 0.038 Uiso 1 1 calc R . . C20 C 0.2357(2) 0.40664(15) -0.07159(11) 0.0337(4) Uani 1 1 d . . . H20 H 0.2565 0.4755 -0.0605 0.040 Uiso 1 1 calc R A . C21 C 0.3303(2) 0.33799(15) -0.08897(10) 0.0323(4) Uani 1 1 d . A . H21 H 0.4153 0.3608 -0.0897 0.039 Uiso 1 1 calc R . . C22 C 0.3029(2) 0.23635(14) -0.10530(10) 0.0265(4) Uani 1 1 d . . . C23 C -0.05933(19) 0.24390(16) -0.08944(10) 0.0288(4) Uani 1 1 d . A . H23 H -0.0641 0.1680 -0.0967 0.035 Uiso 1 1 calc R . . C24 C -0.1251(2) 0.26743(18) -0.02563(11) 0.0375(5) Uani 1 1 d . . . H24A H -0.0822 0.2311 0.0096 0.056 Uiso 1 1 calc R A . H24B H -0.2130 0.2447 -0.0280 0.056 Uiso 1 1 calc R . . H24C H -0.1225 0.3416 -0.0175 0.056 Uiso 1 1 calc R . . C25 C -0.1266(3) 0.2973(2) -0.14636(13) 0.0432(6) Uani 1 1 d . . . H25A H -0.1224 0.3720 -0.1406 0.065 Uiso 1 1 calc R A . H25B H -0.2150 0.2755 -0.1476 0.065 Uiso 1 1 calc R . . H25C H -0.0853 0.2783 -0.1870 0.065 Uiso 1 1 calc R . . C26 C 0.4110(2) 0.16474(15) -0.12364(11) 0.0341(4) Uani 1 1 d . A . H26 H 0.3782 0.0927 -0.1246 0.041 Uiso 1 1 calc R . . C27 C 0.4619(3) 0.1917(3) -0.19144(16) 0.0596(8) Uani 1 1 d . . . H27A H 0.3932 0.1883 -0.2230 0.089 Uiso 1 1 calc R A . H27B H 0.5279 0.1426 -0.2035 0.089 Uiso 1 1 calc R . . H27C H 0.4971 0.2614 -0.1909 0.089 Uiso 1 1 calc R . . C28 C 0.5199(2) 0.1697(2) -0.07513(15) 0.0463(6) Uani 1 1 d . . . H28A H 0.5535 0.2399 -0.0738 0.070 Uiso 1 1 calc R A . H28B H 0.5865 0.1221 -0.0885 0.070 Uiso 1 1 calc R . . H28C H 0.4893 0.1505 -0.0321 0.070 Uiso 1 1 calc R . . C29 C 0.5858(4) 0.5000 0.0000 0.129(3) Uani 1 2 d SD . . C30 C 0.6451(6) 0.5024 0.0519 0.0570(11) Uani 0.50 1 d PDU B 1 H30C H 0.6477 0.5722 0.0710 0.068 Uiso 0.50 1 calc PR B 1 H30D H 0.7317 0.4749 0.0475 0.068 Uiso 0.50 1 calc PR B 1 C31 C 0.5733(12) 0.4421(9) 0.0829(6) 0.211(12) Uani 0.50 1 d PD B 1 H31C H 0.5989 0.3692 0.0786 0.253 Uiso 0.50 1 calc PR B 1 H31D H 0.4838 0.4501 0.0706 0.253 Uiso 0.50 1 calc PR B 1 C32 C 0.5969(7) 0.4788(5) 0.1404(4) 0.0602(13) Uani 0.50 1 d PDU B 1 H32D H 0.5427 0.4447 0.1722 0.090 Uiso 0.50 1 calc PR B 1 H32E H 0.5802 0.5529 0.1408 0.090 Uiso 0.50 1 calc PR B 1 H32F H 0.6854 0.4664 0.1513 0.090 Uiso 0.50 1 calc PR B 1 C1A C 0.2653(11) 0.0000 0.0000 0.043(3) Uani 0.40 2 d SP A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02160(8) 0.01620(7) 0.01359(7) -0.00013(8) 0.000 0.000 Cl1 0.0268(8) 0.0445(6) 0.0272(5) 0.0051(10) 0.000 0.000 Cl1A 0.0229(13) 0.0469(10) 0.0257(7) 0.0046(18) 0.000 0.000 O1 0.0230(19) 0.072(3) 0.048(2) -0.006(4) 0.000 0.000 O1A 0.021(3) 0.089(5) 0.058(4) 0.020(6) 0.000 0.000 N1 0.0347(8) 0.0211(6) 0.0157(6) 0.0009(5) -0.0008(6) -0.0091(6) N2 0.0351(8) 0.0190(6) 0.0154(6) -0.0011(5) 0.0018(6) -0.0072(6) C30A 0.063(2) 0.047(3) 0.087(3) -0.030(2) -0.015(2) 0.014(3) C31A 0.062(2) 0.044(2) 0.086(3) -0.020(2) -0.020(2) 0.015(2) C32A 0.063(3) 0.058(3) 0.065(3) -0.017(3) -0.011(2) 0.014(3) C1 0.032(4) 0.036(2) 0.0163(18) 0.002(4) 0.000 0.000 C2 0.0214(7) 0.0190(7) 0.0151(6) 0.0000(5) 0.0005(6) -0.0011(5) C3 0.101(2) 0.0403(11) 0.0143(7) 0.0000(9) 0.0022(9) -0.032(2) C4 0.0704(16) 0.0276(9) 0.0172(8) 0.0013(7) 0.0009(9) -0.0169(10) C5 0.0312(9) 0.0202(8) 0.0150(7) -0.0016(6) 0.0001(6) -0.0053(6) C6 0.0300(9) 0.0284(8) 0.0185(7) -0.0030(6) 0.0010(7) -0.0029(7) C7 0.0410(11) 0.0239(8) 0.0266(9) -0.0016(7) 0.0010(8) 0.0025(8) C8 0.0459(11) 0.0190(8) 0.0298(9) -0.0040(7) 0.0011(8) -0.0074(8) C9 0.0345(11) 0.0287(10) 0.0253(9) -0.0068(8) 0.0014(8) -0.0099(8) C10 0.0308(9) 0.0235(8) 0.0211(8) -0.0038(6) -0.0010(7) -0.0043(7) C11 0.0280(10) 0.0409(11) 0.0232(9) -0.0042(8) 0.0019(8) -0.0014(8) C12 0.0375(13) 0.111(3) 0.0364(13) -0.0202(15) 0.0103(11) -0.0088(15) C13 0.0372(12) 0.0439(13) 0.0457(14) -0.0009(11) -0.0085(11) 0.0051(10) C14 0.0346(11) 0.0287(10) 0.0472(12) -0.0052(9) -0.0098(9) -0.0019(8) C15 0.070(2) 0.074(2) 0.0590(18) 0.0158(16) -0.0196(16) 0.0160(17) C16 0.0291(11) 0.0452(13) 0.0714(18) -0.0150(13) -0.0022(11) -0.0008(10) C17 0.0320(9) 0.0167(7) 0.0194(8) 0.0002(6) 0.0015(7) -0.0060(6) C18 0.0300(9) 0.0238(8) 0.0220(8) 0.0015(6) -0.0022(7) -0.0019(7) C19 0.0389(11) 0.0224(8) 0.0333(10) -0.0016(7) -0.0028(8) 0.0031(8) C20 0.0445(12) 0.0172(8) 0.0393(11) -0.0012(7) -0.0029(9) -0.0059(8) C21 0.0356(10) 0.0242(9) 0.0370(10) -0.0001(8) 0.0023(8) -0.0106(8) C22 0.0339(10) 0.0231(8) 0.0225(8) 0.0001(7) 0.0054(8) -0.0050(7) C23 0.0291(9) 0.0311(9) 0.0261(9) 0.0040(7) -0.0038(7) 0.0001(7) C24 0.0351(11) 0.0424(12) 0.0349(10) 0.0033(9) 0.0029(9) 0.0036(9) C25 0.0400(14) 0.0529(15) 0.0367(12) 0.0120(11) -0.0082(10) 0.0043(11) C26 0.0340(10) 0.0281(9) 0.0402(11) -0.0030(8) 0.0120(9) -0.0039(8) C27 0.0607(18) 0.0630(18) 0.0550(16) 0.0006(14) 0.0290(14) 0.0045(15) C28 0.0312(11) 0.0381(12) 0.0697(17) -0.0057(12) 0.0041(11) -0.0030(9) C29 0.0337(19) 0.122(5) 0.231(9) 0.114(6) 0.000 0.000 C30 0.0558(19) 0.031(2) 0.084(3) -0.023(3) -0.0261(18) 0.011(3) C31 0.086(7) 0.101(9) 0.44(3) 0.171(15) -0.098(14) -0.055(7) C32 0.064(2) 0.048(3) 0.068(3) -0.028(2) -0.024(2) 0.021(2) C1A 0.042(6) 0.060(5) 0.027(4) 0.013(7) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1A 1.829(12) . ? Ru1 C1 1.861(7) . ? Ru1 C2 2.0889(15) . ? Ru1 C2 2.0889(15) 3 ? Ru1 Cl1A 2.346(3) . ? Ru1 Cl1 2.3500(19) . ? O1 C1 1.146(6) . ? O1A C1A 1.220(10) . ? N1 C2 1.356(2) . ? N1 C5 1.439(2) . ? N1 C3 1.479(2) . ? N2 C2 1.352(2) . ? N2 C17 1.439(2) . ? N2 C4 1.470(2) . ? C30A C31A 1.426(11) . ? C30A C29 1.537(7) . ? C31A C32A 1.427(9) . ? C3 C4 1.480(3) . ? C5 C6 1.400(3) . ? C5 C10 1.406(3) . ? C6 C7 1.396(3) . ? C6 C11 1.521(3) . ? C7 C8 1.382(3) . ? C8 C9 1.383(3) . ? C9 C10 1.397(3) . ? C10 C14 1.524(3) . ? C11 C13 1.521(3) . ? C11 C12 1.542(3) . ? C14 C16 1.527(3) . ? C14 C15 1.544(3) . ? C17 C22 1.401(3) . ? C17 C18 1.404(3) . ? C18 C19 1.403(3) . ? C18 C23 1.521(3) . ? C19 C20 1.380(3) . ? C20 C21 1.391(3) . ? C21 C22 1.395(3) . ? C22 C26 1.525(3) . ? C23 C24 1.524(3) . ? C23 C25 1.542(3) . ? C26 C28 1.532(3) . ? C26 C27 1.543(3) . ? C29 C30 1.244(4) . ? C29 C30 1.244(4) 3_565 ? C29 C30A 1.537(7) 3_565 ? C29 C31 1.878(11) . ? C29 C31 1.878(11) 3_565 ? C30 C31 1.268(10) . ? C30 C32 1.924(8) . ? C31 C32 1.304(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 C1A Ru1 C1 180.0 . . ? C1A Ru1 C2 88.80(5) . . ? C1 Ru1 C2 91.20(5) . . ? C1A Ru1 C2 88.80(5) . 3 ? C1 Ru1 C2 91.20(5) . 3 ? C2 Ru1 C2 177.60(9) . 3 ? C1A Ru1 Cl1A 180.0 . . ? C1 Ru1 Cl1A 0.0 . . ? C2 Ru1 Cl1A 91.20(5) . . ? C2 Ru1 Cl1A 91.20(5) 3 . ? C1A Ru1 Cl1 0.0 . . ? C1 Ru1 Cl1 180.0 . . ? C2 Ru1 Cl1 88.80(5) . . ? C2 Ru1 Cl1 88.80(5) 3 . ? Cl1A Ru1 Cl1 180.0 . . ? C2 N1 C5 128.03(14) . . ? C2 N1 C3 112.56(15) . . ? C5 N1 C3 117.11(16) . . ? C2 N2 C17 128.84(14) . . ? C2 N2 C4 113.11(14) . . ? C17 N2 C4 115.64(14) . . ? C31A C30A C29 113.4(7) . . ? C30A C31A C32A 115.9(9) . . ? O1 C1 Ru1 180.0 . . ? N2 C2 N1 106.09(14) . . ? N2 C2 Ru1 126.40(11) . . ? N1 C2 Ru1 127.49(11) . . ? N1 C3 C4 102.53(16) . . ? N2 C4 C3 102.72(15) . . ? C6 C5 C10 122.14(16) . . ? C6 C5 N1 119.07(17) . . ? C10 C5 N1 118.48(16) . . ? C7 C6 C5 118.02(18) . . ? C7 C6 C11 119.06(18) . . ? C5 C6 C11 122.87(17) . . ? C8 C7 C6 120.87(19) . . ? C7 C8 C9 120.27(18) . . ? C8 C9 C10 121.2(2) . . ? C9 C10 C5 117.45(19) . . ? C9 C10 C14 119.47(19) . . ? C5 C10 C14 123.07(16) . . ? C13 C11 C6 111.92(18) . . ? C13 C11 C12 108.1(2) . . ? C6 C11 C12 111.04(18) . . ? C10 C14 C16 112.55(19) . . ? C10 C14 C15 109.54(18) . . ? C16 C14 C15 109.0(2) . . ? C22 C17 C18 122.02(16) . . ? C22 C17 N2 118.44(17) . . ? C18 C17 N2 119.03(17) . . ? C19 C18 C17 118.04(18) . . ? C19 C18 C23 119.05(18) . . ? C17 C18 C23 122.86(16) . . ? C20 C19 C18 120.85(19) . . ? C19 C20 C21 120.00(18) . . ? C20 C21 C22 121.4(2) . . ? C21 C22 C17 117.70(18) . . ? C21 C22 C26 118.83(19) . . ? C17 C22 C26 123.46(17) . . ? C18 C23 C24 111.66(17) . . ? C18 C23 C25 110.61(18) . . ? C24 C23 C25 110.96(19) . . ? C22 C26 C28 112.27(18) . . ? C22 C26 C27 110.5(2) . . ? C28 C26 C27 108.7(2) . . ? C30 C29 C30 119.2(6) . 3_565 ? C30 C29 C30A 20.9(3) . . ? C30 C29 C30A 118.9(4) 3_565 . ? C30 C29 C30A 118.9(4) . 3_565 ? C30 C29 C30A 20.9(3) 3_565 3_565 ? C30A C29 C30A 127.1(7) . 3_565 ? C30 C29 C31 42.1(4) . . ? C30 C29 C31 144.4(6) 3_565 . ? C30A C29 C31 30.6(5) . . ? C30A C29 C31 157.5(6) 3_565 . ? C30 C29 C31 144.4(6) . 3_565 ? C30 C29 C31 42.1(4) 3_565 3_565 ? C30A C29 C31 157.5(6) . 3_565 ? C30A C29 C31 30.6(5) 3_565 3_565 ? C31 C29 C31 171.9(9) . 3_565 ? C29 C30 C31 96.7(7) . . ? C29 C30 C32 132.9(5) . . ? C31 C30 C32 42.3(6) . . ? C30 C31 C32 96.8(9) . . ? C30 C31 C29 41.2(4) . . ? C32 C31 C29 132.2(8) . . ? C31 C32 C30 40.9(5) . . ? O1A C1A Ru1 180.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.644 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.060 data_c:\x-ray\kappa\k06mkw10\maxus\k06mkw10 _database_code_depnum_ccdc_archive 'CCDC 668488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H49 Cl N4 O2 Ru' _chemical_formula_weight 802.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 18.5500(1) _cell_length_b 10.8650(1) _cell_length_c 21.1290(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.646(1) _cell_angle_gamma 90.00 _cell_volume 4034.94(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 69290 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.508 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56500 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.50 _reflns_number_total 12272 _reflns_number_gt 10523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+2.4215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12272 _refine_ls_number_parameters 511 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.063087(7) 0.086806(12) -0.252128(6) 0.01981(4) Uani 1 1 d D . . Cl1 Cl -0.02165(7) 0.23627(14) -0.32400(7) 0.0361(2) Uani 0.60 1 d P A 1 Cl1A Cl 0.14586(14) -0.0527(2) -0.17559(14) 0.0352(5) Uani 0.40 1 d P A 2 O1 O 0.01892(9) -0.11177(16) -0.36469(9) 0.0521(5) Uani 1 1 d . . . O2 O 0.17241(19) -0.0782(4) -0.14828(19) 0.0562(11) Uani 0.60 1 d P A 1 O2A O -0.0412(3) 0.2924(5) -0.3331(3) 0.0574(15) Uani 0.40 1 d P A 2 N1 N 0.19540(8) 0.10512(13) -0.31699(7) 0.0228(3) Uani 1 1 d . . . N2 N 0.20010(7) 0.25714(12) -0.25161(7) 0.0216(3) Uani 1 1 d . . . N3 N -0.08554(7) -0.03344(12) -0.23509(7) 0.0216(3) Uani 1 1 d . . . N4 N -0.03577(7) 0.09571(12) -0.15655(7) 0.0200(3) Uani 1 1 d . . . C1 C 0.03478(10) -0.03949(18) -0.32367(10) 0.0301(4) Uani 1 1 d . A . C2 C 0.1293(4) -0.0165(6) -0.1896(4) 0.0362(13) Uani 0.60 1 d P A 1 C3 C 0.15723(9) 0.15514(15) -0.27726(8) 0.0192(3) Uani 1 1 d . A . C4 C 0.25914(10) 0.17303(18) -0.31544(10) 0.0309(4) Uani 1 1 d . A . H4 H 0.2939 0.1555 -0.3389 0.037 Uiso 1 1 calc R . . C5 C 0.26226(10) 0.26796(17) -0.27447(9) 0.0291(4) Uani 1 1 d . A . H5 H 0.2998 0.3309 -0.2631 0.035 Uiso 1 1 calc R . . C6 C 0.17294(9) 0.00113(16) -0.36104(9) 0.0246(3) Uani 1 1 d . A . C7 C 0.20159(10) -0.11466(17) -0.33865(10) 0.0297(4) Uani 1 1 d . . . C8 C 0.18010(12) -0.21153(19) -0.38390(11) 0.0385(5) Uani 1 1 d . A . H8 H 0.1976 -0.2922 -0.3695 0.046 Uiso 1 1 calc R . . C9 C 0.13414(12) -0.1942(2) -0.44900(12) 0.0424(5) Uani 1 1 d . . . C10 C 0.10846(12) -0.0758(2) -0.47032(10) 0.0382(5) Uani 1 1 d . A . H10 H 0.0777 -0.0631 -0.5153 0.046 Uiso 1 1 calc R . . C11 C 0.12709(11) 0.02372(18) -0.42689(9) 0.0302(4) Uani 1 1 d . . . C12 C 0.25350(12) -0.1371(2) -0.26856(11) 0.0420(5) Uani 1 1 d . A . H12A H 0.2810 -0.0611 -0.2507 0.063 Uiso 1 1 calc R . . H12B H 0.2900 -0.2019 -0.2690 0.063 Uiso 1 1 calc R . . H12C H 0.2233 -0.1628 -0.2404 0.063 Uiso 1 1 calc R . . C13 C 0.11221(17) -0.3025(3) -0.49630(15) 0.0687(8) Uani 1 1 d . A . H13A H 0.1431 -0.3741 -0.4761 0.103 Uiso 1 1 calc R . . H13B H 0.1211 -0.2818 -0.5384 0.103 Uiso 1 1 calc R . . H13C H 0.0583 -0.3217 -0.5051 0.103 Uiso 1 1 calc R . . C14 C 0.09708(13) 0.1512(2) -0.44873(10) 0.0404(5) Uani 1 1 d . A . H14A H 0.0671 0.1499 -0.4962 0.061 Uiso 1 1 calc R . . H14B H 0.1398 0.2084 -0.4416 0.061 Uiso 1 1 calc R . . H14C H 0.0648 0.1781 -0.4226 0.061 Uiso 1 1 calc R . . C15 C 0.18811(9) 0.35047(15) -0.20730(8) 0.0226(3) Uani 1 1 d . A . C16 C 0.15330(10) 0.46064(16) -0.23529(9) 0.0265(3) Uani 1 1 d . . . C17 C 0.15103(11) 0.55566(17) -0.19165(10) 0.0328(4) Uani 1 1 d . A . H17 H 0.1282 0.6318 -0.2095 0.039 Uiso 1 1 calc R . . C18 C 0.18135(11) 0.54214(19) -0.12242(10) 0.0345(4) Uani 1 1 d . . . C19 C 0.21541(11) 0.43126(18) -0.09727(9) 0.0321(4) Uani 1 1 d . A . H19 H 0.2360 0.4212 -0.0503 0.039 Uiso 1 1 calc R . . C20 C 0.22041(9) 0.33408(16) -0.13866(9) 0.0260(3) Uani 1 1 d . . . C21 C 0.12009(12) 0.47787(19) -0.30972(10) 0.0358(4) Uani 1 1 d . A . H21A H 0.1602 0.4681 -0.3302 0.054 Uiso 1 1 calc R . . H21B H 0.0981 0.5605 -0.3193 0.054 Uiso 1 1 calc R . . H21C H 0.0803 0.4162 -0.3281 0.054 Uiso 1 1 calc R . . C22 C 0.17704(14) 0.6461(2) -0.07586(13) 0.0507(6) Uani 1 1 d . A . H22A H 0.1284 0.6420 -0.0670 0.076 Uiso 1 1 calc R . . H22B H 0.1811 0.7252 -0.0968 0.076 Uiso 1 1 calc R . . H22C H 0.2189 0.6382 -0.0337 0.076 Uiso 1 1 calc R . . C23 C 0.25975(12) 0.21646(19) -0.10933(10) 0.0366(4) Uani 1 1 d . A . H23A H 0.3006 0.2346 -0.0677 0.055 Uiso 1 1 calc R . . H23B H 0.2813 0.1777 -0.1411 0.055 Uiso 1 1 calc R . . H23C H 0.2230 0.1604 -0.1000 0.055 Uiso 1 1 calc R . . C24 C -0.02427(9) 0.04429(15) -0.21199(8) 0.0196(3) Uani 1 1 d . A . C25 C -0.13247(9) -0.03040(15) -0.19530(9) 0.0241(3) Uani 1 1 d . A . H25 H -0.1776 -0.0768 -0.2016 0.029 Uiso 1 1 calc R . . C26 C -0.10160(9) 0.05056(16) -0.14653(9) 0.0235(3) Uani 1 1 d . A . H26 H -0.1209 0.0731 -0.1116 0.028 Uiso 1 1 calc R . . C27 C -0.09531(10) -0.12895(17) -0.28496(10) 0.0288(4) Uani 1 1 d . A . C28 C -0.14039(10) -0.10751(19) -0.35066(11) 0.0359(5) Uani 1 1 d . . . C29 C -0.15040(12) -0.2063(2) -0.39516(12) 0.0486(6) Uani 1 1 d . A . H29 H -0.1808 -0.1950 -0.4404 0.058 Uiso 1 1 calc R . . C30 C -0.11725(15) -0.3205(2) -0.37517(15) 0.0553(7) Uani 1 1 d . . . C31 C -0.07355(14) -0.3376(2) -0.30965(15) 0.0506(6) Uani 1 1 d . A . H31 H -0.0508 -0.4157 -0.2961 0.061 Uiso 1 1 calc R . . C32 C -0.06175(11) -0.24309(18) -0.26244(12) 0.0380(5) Uani 1 1 d . . . C33 C -0.17669(12) 0.0146(2) -0.37386(10) 0.0421(5) Uani 1 1 d . A . H33A H -0.2207 0.0255 -0.3583 0.063 Uiso 1 1 calc R . . H33B H -0.1933 0.0177 -0.4228 0.063 Uiso 1 1 calc R . . H33C H -0.1398 0.0804 -0.3557 0.063 Uiso 1 1 calc R . . C34 C -0.1314(2) -0.4251(3) -0.42564(18) 0.0865(12) Uani 1 1 d . A . H34A H -0.1020 -0.4975 -0.4045 0.130 Uiso 1 1 calc R . . H34B H -0.1157 -0.3995 -0.4637 0.130 Uiso 1 1 calc R . . H34C H -0.1857 -0.4456 -0.4412 0.130 Uiso 1 1 calc R . . C35 C -0.01627(13) -0.26433(19) -0.19087(13) 0.0445(5) Uani 1 1 d . A . H35A H 0.0275 -0.2085 -0.1781 0.067 Uiso 1 1 calc R . . H35B H 0.0016 -0.3497 -0.1850 0.067 Uiso 1 1 calc R . . H35C H -0.0482 -0.2486 -0.1626 0.067 Uiso 1 1 calc R . . C36 C 0.01421(9) 0.17373(17) -0.10570(8) 0.0247(3) Uani 1 1 d . A . C37 C 0.00498(10) 0.30142(18) -0.11047(10) 0.0306(4) Uani 1 1 d . . . C38 C 0.04744(12) 0.3711(2) -0.05571(11) 0.0404(5) Uani 1 1 d . A . H38 H 0.0420 0.4581 -0.0577 0.048 Uiso 1 1 calc R . . C39 C 0.09706(12) 0.3186(2) 0.00125(11) 0.0447(6) Uani 1 1 d . . . C40 C 0.10522(11) 0.1914(2) 0.00317(10) 0.0420(5) Uani 1 1 d . A . H40 H 0.1400 0.1544 0.0416 0.050 Uiso 1 1 calc R . . C41 C 0.06395(10) 0.11611(19) -0.04952(9) 0.0309(4) Uani 1 1 d . . . C42 C -0.04758(13) 0.36188(19) -0.17162(11) 0.0405(5) Uani 1 1 d . A . H42A H -0.0265 0.3544 -0.2085 0.061 Uiso 1 1 calc R . . H42B H -0.0532 0.4491 -0.1624 0.061 Uiso 1 1 calc R . . H42C H -0.0975 0.3217 -0.1840 0.061 Uiso 1 1 calc R . . C43 C 0.14150(16) 0.3979(3) 0.05981(13) 0.0666(8) Uani 1 1 d . A . H43A H 0.1736 0.3453 0.0954 0.100 Uiso 1 1 calc R . . H43B H 0.1060 0.4440 0.0766 0.100 Uiso 1 1 calc R . . H43C H 0.1736 0.4556 0.0452 0.100 Uiso 1 1 calc R . . C44 C 0.07185(11) -0.0217(2) -0.04424(10) 0.0380(5) Uani 1 1 d . A . H44A H 0.0263 -0.0571 -0.0374 0.057 Uiso 1 1 calc R . . H44B H 0.1167 -0.0431 -0.0064 0.057 Uiso 1 1 calc R . . H44C H 0.0776 -0.0547 -0.0855 0.057 Uiso 1 1 calc R . . C2A C 0.0006(4) 0.2128(9) -0.3028(4) 0.0409(19) Uani 0.40 1 d P A 2 H1 H 0.0846(13) 0.1892(16) -0.1952(9) 0.050(7) Uiso 1 1 d D A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01709(6) 0.02124(7) 0.02373(7) -0.00445(5) 0.01020(5) -0.00362(5) Cl1 0.0283(7) 0.0398(7) 0.0401(8) 0.0098(6) 0.0108(5) 0.0040(5) Cl1A 0.0305(14) 0.0390(14) 0.0411(15) 0.0080(9) 0.0185(11) 0.0023(8) O1 0.0449(9) 0.0652(11) 0.0594(10) -0.0386(9) 0.0351(8) -0.0289(8) O2 0.0327(18) 0.080(3) 0.056(2) 0.0381(18) 0.0142(15) 0.0181(15) O2A 0.046(3) 0.058(3) 0.066(3) 0.031(3) 0.015(2) 0.022(2) N1 0.0210(6) 0.0254(7) 0.0255(7) -0.0029(6) 0.0123(5) -0.0023(5) N2 0.0213(6) 0.0227(7) 0.0231(7) -0.0010(5) 0.0104(5) -0.0039(5) N3 0.0186(6) 0.0194(7) 0.0296(7) -0.0056(6) 0.0119(5) -0.0030(5) N4 0.0179(6) 0.0218(7) 0.0218(6) -0.0008(5) 0.0083(5) -0.0016(5) C1 0.0245(8) 0.0356(10) 0.0356(10) -0.0082(8) 0.0171(7) -0.0072(7) C2 0.024(3) 0.046(4) 0.044(3) 0.008(3) 0.018(2) -0.002(2) C3 0.0180(7) 0.0211(7) 0.0190(7) 0.0004(6) 0.0065(6) -0.0002(5) C4 0.0263(8) 0.0371(10) 0.0361(10) -0.0070(8) 0.0195(8) -0.0079(7) C5 0.0263(8) 0.0337(9) 0.0328(9) -0.0044(8) 0.0169(7) -0.0106(7) C6 0.0226(8) 0.0264(8) 0.0287(9) -0.0057(7) 0.0136(7) -0.0017(6) C7 0.0246(8) 0.0306(9) 0.0377(10) -0.0028(8) 0.0154(7) 0.0035(7) C8 0.0373(10) 0.0288(10) 0.0543(13) -0.0080(9) 0.0216(10) 0.0057(8) C9 0.0417(11) 0.0406(12) 0.0488(13) -0.0214(10) 0.0201(10) -0.0021(9) C10 0.0393(11) 0.0470(12) 0.0292(10) -0.0129(9) 0.0121(8) -0.0025(9) C11 0.0312(9) 0.0340(10) 0.0286(9) -0.0037(8) 0.0143(7) -0.0018(7) C12 0.0372(11) 0.0427(12) 0.0457(12) 0.0048(10) 0.0128(9) 0.0146(9) C13 0.0727(19) 0.0544(16) 0.0737(19) -0.0390(15) 0.0161(15) 0.0012(14) C14 0.0490(12) 0.0404(12) 0.0298(10) 0.0025(9) 0.0100(9) 0.0034(9) C15 0.0205(7) 0.0237(8) 0.0253(8) -0.0040(6) 0.0097(6) -0.0060(6) C16 0.0247(8) 0.0259(8) 0.0303(9) -0.0012(7) 0.0107(7) -0.0039(6) C17 0.0299(9) 0.0264(9) 0.0438(11) -0.0046(8) 0.0144(8) -0.0021(7) C18 0.0313(9) 0.0348(10) 0.0411(11) -0.0149(9) 0.0169(8) -0.0094(8) C19 0.0294(9) 0.0411(11) 0.0259(9) -0.0090(8) 0.0090(7) -0.0095(8) C20 0.0223(8) 0.0308(9) 0.0262(8) -0.0012(7) 0.0094(7) -0.0065(6) C21 0.0396(11) 0.0309(10) 0.0362(10) 0.0054(8) 0.0111(8) 0.0020(8) C22 0.0561(14) 0.0444(13) 0.0543(14) -0.0252(11) 0.0216(12) -0.0092(11) C23 0.0389(10) 0.0414(11) 0.0268(9) 0.0033(8) 0.0066(8) -0.0004(8) C24 0.0174(7) 0.0186(7) 0.0243(8) -0.0021(6) 0.0086(6) -0.0005(5) C25 0.0194(7) 0.0235(8) 0.0332(9) -0.0006(7) 0.0138(7) -0.0016(6) C26 0.0202(7) 0.0276(8) 0.0266(8) 0.0022(7) 0.0129(6) 0.0001(6) C27 0.0234(8) 0.0256(8) 0.0441(11) -0.0162(8) 0.0202(8) -0.0102(7) C28 0.0233(8) 0.0446(12) 0.0450(11) -0.0211(9) 0.0183(8) -0.0098(8) C29 0.0367(11) 0.0635(15) 0.0526(13) -0.0332(12) 0.0242(10) -0.0209(10) C30 0.0571(15) 0.0432(13) 0.0832(19) -0.0390(13) 0.0470(14) -0.0250(11) C31 0.0543(14) 0.0278(10) 0.0869(19) -0.0232(11) 0.0469(14) -0.0138(9) C32 0.0347(10) 0.0246(9) 0.0667(14) -0.0127(9) 0.0330(10) -0.0101(7) C33 0.0313(10) 0.0605(14) 0.0328(11) -0.0137(10) 0.0079(8) 0.0023(9) C34 0.118(3) 0.0605(19) 0.104(3) -0.0567(18) 0.067(2) -0.0354(18) C35 0.0437(12) 0.0244(10) 0.0730(16) 0.0039(10) 0.0293(11) 0.0030(8) C36 0.0210(7) 0.0342(9) 0.0217(8) -0.0062(7) 0.0107(6) -0.0057(6) C37 0.0291(9) 0.0323(10) 0.0347(10) -0.0094(8) 0.0161(8) -0.0085(7) C38 0.0409(11) 0.0415(11) 0.0450(12) -0.0192(10) 0.0226(10) -0.0181(9) C39 0.0352(11) 0.0693(16) 0.0336(11) -0.0210(11) 0.0165(9) -0.0233(10) C40 0.0285(9) 0.0731(16) 0.0241(9) -0.0057(10) 0.0079(7) -0.0106(10) C41 0.0234(8) 0.0476(11) 0.0244(9) -0.0013(8) 0.0115(7) -0.0035(7) C42 0.0473(12) 0.0253(10) 0.0471(12) -0.0045(9) 0.0126(10) -0.0016(8) C43 0.0588(16) 0.096(2) 0.0448(14) -0.0376(14) 0.0165(12) -0.0354(15) C44 0.0330(10) 0.0540(13) 0.0270(9) 0.0079(9) 0.0098(8) 0.0098(9) C2A 0.023(4) 0.056(5) 0.044(5) 0.013(4) 0.013(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.594(9) . ? Ru1 C2 1.864(6) . ? Ru1 C2A 1.890(8) . ? Ru1 C1 1.9840(19) . ? Ru1 C24 2.1064(15) . ? Ru1 C3 2.1158(15) . ? Ru1 Cl1A 2.384(2) . ? Ru1 Cl1 2.4264(15) . ? O1 C1 1.136(2) . ? O2 C2 1.186(5) . ? O2A C2A 1.200(8) . ? N1 C3 1.372(2) . ? N1 C4 1.385(2) . ? N1 C6 1.438(2) . ? N2 C3 1.371(2) . ? N2 C5 1.390(2) . ? N2 C15 1.445(2) . ? N3 C24 1.374(2) . ? N3 C25 1.390(2) . ? N3 C27 1.448(2) . ? N4 C24 1.375(2) . ? N4 C26 1.3935(19) . ? N4 C36 1.447(2) . ? C4 C5 1.336(3) . ? C6 C7 1.389(3) . ? C6 C11 1.401(3) . ? C7 C8 1.392(3) . ? C7 C12 1.506(3) . ? C8 C9 1.380(3) . ? C9 C10 1.396(3) . ? C9 C13 1.513(3) . ? C10 C11 1.389(3) . ? C11 C14 1.509(3) . ? C15 C20 1.392(2) . ? C15 C16 1.398(2) . ? C16 C17 1.394(3) . ? C16 C21 1.506(3) . ? C17 C18 1.397(3) . ? C18 C19 1.385(3) . ? C18 C22 1.517(3) . ? C19 C20 1.393(3) . ? C20 C23 1.504(3) . ? C25 C26 1.337(2) . ? C27 C28 1.392(3) . ? C27 C32 1.401(3) . ? C28 C29 1.400(3) . ? C28 C33 1.497(3) . ? C29 C30 1.389(4) . ? C30 C31 1.375(4) . ? C30 C34 1.523(3) . ? C31 C32 1.399(3) . ? C32 C35 1.495(3) . ? C36 C41 1.397(3) . ? C36 C37 1.398(3) . ? C37 C38 1.396(3) . ? C37 C42 1.499(3) . ? C38 C39 1.383(3) . ? C39 C40 1.390(4) . ? C39 C43 1.516(3) . ? C40 C41 1.396(3) . ? C41 C44 1.505(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1 Ru1 C2 86.3(9) . . ? H1 Ru1 C2A 83.2(9) . . ? C2 Ru1 C2A 169.6(4) . . ? H1 Ru1 C1 179.1(9) . . ? C2 Ru1 C1 94.4(3) . . ? C2A Ru1 C1 96.0(3) . . ? H1 Ru1 C24 83.5(8) . . ? C2 Ru1 C24 90.0(2) . . ? C2A Ru1 C24 88.6(3) . . ? C1 Ru1 C24 96.02(7) . . ? H1 Ru1 C3 85.3(8) . . ? C2 Ru1 C3 88.8(2) . . ? C2A Ru1 C3 90.5(3) . . ? C1 Ru1 C3 95.17(6) . . ? C24 Ru1 C3 168.81(6) . . ? H1 Ru1 Cl1A 88.9(8) . . ? C2 Ru1 Cl1A 2.5(3) . . ? C2A Ru1 Cl1A 172.1(3) . . ? C1 Ru1 Cl1A 91.91(9) . . ? C24 Ru1 Cl1A 89.94(7) . . ? C3 Ru1 Cl1A 89.38(7) . . ? H1 Ru1 Cl1 87.8(8) . . ? C2 Ru1 Cl1 174.0(3) . . ? C2A Ru1 Cl1 4.6(3) . . ? C1 Ru1 Cl1 91.45(7) . . ? C24 Ru1 Cl1 88.33(5) . . ? C3 Ru1 Cl1 91.70(5) . . ? Cl1A Ru1 Cl1 176.37(8) . . ? C3 N1 C4 112.22(14) . . ? C3 N1 C6 127.44(13) . . ? C4 N1 C6 120.15(14) . . ? C3 N2 C5 111.82(13) . . ? C3 N2 C15 129.33(13) . . ? C5 N2 C15 118.84(13) . . ? C24 N3 C25 112.17(13) . . ? C24 N3 C27 126.55(13) . . ? C25 N3 C27 119.99(13) . . ? C24 N4 C26 111.63(13) . . ? C24 N4 C36 129.30(13) . . ? C26 N4 C36 118.55(13) . . ? O1 C1 Ru1 179.65(16) . . ? O2 C2 Ru1 177.4(8) . . ? N2 C3 N1 102.40(13) . . ? N2 C3 Ru1 127.27(11) . . ? N1 C3 Ru1 130.06(11) . . ? C5 C4 N1 106.64(15) . . ? C4 C5 N2 106.92(15) . . ? C7 C6 C11 122.80(17) . . ? C7 C6 N1 119.42(16) . . ? C11 C6 N1 117.60(16) . . ? C6 C7 C8 117.18(18) . . ? C6 C7 C12 122.43(17) . . ? C8 C7 C12 120.39(18) . . ? C9 C8 C7 122.12(19) . . ? C8 C9 C10 119.06(18) . . ? C8 C9 C13 120.2(2) . . ? C10 C9 C13 120.8(2) . . ? C11 C10 C9 121.2(2) . . ? C10 C11 C6 117.62(18) . . ? C10 C11 C14 121.55(18) . . ? C6 C11 C14 120.80(17) . . ? C20 C15 C16 122.47(16) . . ? C20 C15 N2 118.76(15) . . ? C16 C15 N2 118.21(15) . . ? C17 C16 C15 117.50(17) . . ? C17 C16 C21 120.66(17) . . ? C15 C16 C21 121.83(16) . . ? C16 C17 C18 121.85(18) . . ? C19 C18 C17 118.35(17) . . ? C19 C18 C22 120.7(2) . . ? C17 C18 C22 120.9(2) . . ? C18 C19 C20 122.16(18) . . ? C15 C20 C19 117.66(17) . . ? C15 C20 C23 121.91(16) . . ? C19 C20 C23 120.43(17) . . ? N3 C24 N4 102.49(13) . . ? N3 C24 Ru1 130.33(11) . . ? N4 C24 Ru1 127.08(11) . . ? C26 C25 N3 106.56(14) . . ? C25 C26 N4 107.15(14) . . ? C28 C27 C32 123.15(17) . . ? C28 C27 N3 120.07(17) . . ? C32 C27 N3 116.65(18) . . ? C27 C28 C29 116.7(2) . . ? C27 C28 C33 122.59(17) . . ? C29 C28 C33 120.7(2) . . ? C30 C29 C28 122.0(2) . . ? C31 C30 C29 119.2(2) . . ? C31 C30 C34 121.2(3) . . ? C29 C30 C34 119.5(3) . . ? C30 C31 C32 121.7(2) . . ? C31 C32 C27 117.2(2) . . ? C31 C32 C35 121.1(2) . . ? C27 C32 C35 121.73(18) . . ? C41 C36 C37 122.58(17) . . ? C41 C36 N4 117.42(16) . . ? C37 C36 N4 119.55(16) . . ? C38 C37 C36 117.07(19) . . ? C38 C37 C42 121.05(19) . . ? C36 C37 C42 121.88(16) . . ? C39 C38 C37 122.7(2) . . ? C38 C39 C40 118.13(19) . . ? C38 C39 C43 120.9(2) . . ? C40 C39 C43 121.0(2) . . ? C39 C40 C41 122.2(2) . . ? C40 C41 C36 117.38(19) . . ? C40 C41 C44 120.53(19) . . ? C36 C41 C44 122.07(17) . . ? O2A C2A Ru1 176.9(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.408 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.075 data_c:\x-ray\helix\h06mkw7\maxus\h06mkw7 _database_code_depnum_ccdc_archive 'CCDC 668489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H73 Cl N4 O2 Ru' _chemical_formula_weight 970.70 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' N N 0.0061 0.0033 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.8060(2) _cell_length_b 15.1130(2) _cell_length_c 35.3110(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.646(1) _cell_angle_gamma 90.00 _cell_volume 10568.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 105938 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54374 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.59 _reflns_number_total 11933 _reflns_number_gt 8979 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+8.4576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11933 _refine_ls_number_parameters 624 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.734293(9) -0.008416(11) 0.619972(5) 0.02514(6) Uani 1 1 d D . . Cl1 Cl 0.6741(2) -0.0929(2) 0.57381(9) 0.0400(6) Uani 0.50 1 d P A 2 O1 O 0.8050(4) 0.0810(4) 0.68689(16) 0.0484(15) Uani 0.50 1 d P A 2 O2 O 0.79278(9) 0.12147(12) 0.56027(5) 0.0526(5) Uani 1 1 d . . . N1 N 0.82250(9) -0.18011(12) 0.63443(5) 0.0311(4) Uani 1 1 d . . . N2 N 0.85810(9) -0.11361(12) 0.58521(5) 0.0317(4) Uani 1 1 d . . . N3 N 0.63485(9) 0.15671(11) 0.62241(5) 0.0271(4) Uani 1 1 d . . . N4 N 0.59603(9) 0.05157(12) 0.65588(5) 0.0320(4) Uani 1 1 d . . . C1 C 0.7794(11) 0.0518(14) 0.6609(4) 0.033(3) Uani 0.50 1 d P A 2 C2 C 0.77150(12) 0.07394(15) 0.58213(7) 0.0345(5) Uani 1 1 d . A . C3 C 0.81214(11) -0.10407(14) 0.61389(6) 0.0265(5) Uani 1 1 d . A . C4 C 0.87047(13) -0.23468(16) 0.61809(7) 0.0427(6) Uani 1 1 d . A . H4 H 0.8847 -0.2911 0.6270 0.051 Uiso 1 1 calc R . . C5 C 0.89273(13) -0.19269(16) 0.58751(7) 0.0423(6) Uani 1 1 d . A . H5 H 0.9261 -0.2133 0.5705 0.051 Uiso 1 1 calc R . . C6 C 0.79441(12) -0.20793(15) 0.67044(6) 0.0341(5) Uani 1 1 d . A . C7 C 0.74116(13) -0.26784(15) 0.66975(7) 0.0380(6) Uani 1 1 d . . . C8 C 0.72022(15) -0.30186(17) 0.70479(7) 0.0479(7) Uani 1 1 d . A . H8 H 0.6826 -0.3409 0.7056 0.057 Uiso 1 1 calc R . . C9 C 0.75309(16) -0.27968(18) 0.73783(8) 0.0524(7) Uani 1 1 d . . . H9 H 0.7388 -0.3044 0.7611 0.063 Uiso 1 1 calc R A . C10 C 0.80643(15) -0.22209(18) 0.73736(7) 0.0493(7) Uani 1 1 d . A . H10 H 0.8287 -0.2078 0.7605 0.059 Uiso 1 1 calc R . . C11 C 0.82903(13) -0.18369(16) 0.70368(7) 0.0389(6) Uani 1 1 d . . . C12 C 0.70885(15) -0.30129(17) 0.63328(7) 0.0479(7) Uani 1 1 d . A . H12 H 0.7279 -0.2662 0.6119 0.057 Uiso 1 1 calc R . . C13 C 0.7279(2) -0.3982(2) 0.62716(10) 0.0929(14) Uani 1 1 d . . . H13A H 0.7771 -0.4034 0.6257 0.139 Uiso 1 1 calc R A . H13B H 0.7073 -0.4194 0.6035 0.139 Uiso 1 1 calc R . . H13C H 0.7116 -0.4338 0.6484 0.139 Uiso 1 1 calc R . . C14 C 0.63287(16) -0.2885(3) 0.63276(9) 0.0763(10) Uani 1 1 d . . . H14A H 0.6127 -0.3239 0.6530 0.114 Uiso 1 1 calc R A . H14B H 0.6144 -0.3074 0.6082 0.114 Uiso 1 1 calc R . . H14C H 0.6224 -0.2258 0.6368 0.114 Uiso 1 1 calc R . . C15 C 0.88986(13) -0.12357(19) 0.70313(7) 0.0481(7) Uani 1 1 d . A . H15 H 0.8866 -0.0865 0.6797 0.058 Uiso 1 1 calc R . . C16 C 0.95506(15) -0.1787(3) 0.70070(10) 0.0766(11) Uani 1 1 d . . . H16A H 0.9588 -0.2172 0.7229 0.115 Uiso 1 1 calc R A . H16B H 0.9941 -0.1389 0.6999 0.115 Uiso 1 1 calc R . . H16C H 0.9537 -0.2149 0.6777 0.115 Uiso 1 1 calc R . . C17 C 0.89443(15) -0.0608(2) 0.73723(8) 0.0571(8) Uani 1 1 d . . . H17A H 0.8524 -0.0270 0.7392 0.086 Uiso 1 1 calc R A . H17B H 0.9323 -0.0199 0.7339 0.086 Uiso 1 1 calc R . . H17C H 0.9015 -0.0953 0.7604 0.086 Uiso 1 1 calc R . . C18 C 0.87981(12) -0.04798(15) 0.55805(7) 0.0359(6) Uani 1 1 d . A . C19 C 0.92731(13) 0.01464(16) 0.57034(8) 0.0434(6) Uani 1 1 d . . . C20 C 0.95122(14) 0.07379(18) 0.54329(10) 0.0560(8) Uani 1 1 d . A . H20 H 0.9831 0.1177 0.5506 0.067 Uiso 1 1 calc R . . C21 C 0.92954(17) 0.0697(2) 0.50631(10) 0.0634(9) Uani 1 1 d . . . H21 H 0.9459 0.1115 0.4885 0.076 Uiso 1 1 calc R A . C22 C 0.88455(16) 0.0060(2) 0.49480(8) 0.0556(8) Uani 1 1 d . A . H22 H 0.8709 0.0036 0.4690 0.067 Uiso 1 1 calc R . . C23 C 0.85832(14) -0.05574(17) 0.52037(7) 0.0432(6) Uani 1 1 d . . . C24 C 0.95470(15) 0.0165(2) 0.61053(9) 0.0563(8) Uani 1 1 d . A . H24 H 0.9246 -0.0211 0.6264 0.068 Uiso 1 1 calc R . . C25 C 1.02579(18) -0.0240(3) 0.61216(11) 0.0812(11) Uani 1 1 d . . . H25A H 1.0242 -0.0845 0.6023 0.122 Uiso 1 1 calc R A . H25B H 1.0421 -0.0248 0.6385 0.122 Uiso 1 1 calc R . . H25C H 1.0564 0.0117 0.5968 0.122 Uiso 1 1 calc R . . C26 C 0.95545(17) 0.1095(2) 0.62765(11) 0.0809(11) Uani 1 1 d . . . H26A H 0.9868 0.1470 0.6135 0.121 Uiso 1 1 calc R A . H26B H 0.9701 0.1063 0.6542 0.121 Uiso 1 1 calc R . . H26C H 0.9100 0.1349 0.6262 0.121 Uiso 1 1 calc R . . C27 C 0.81266(15) -0.1294(2) 0.50641(7) 0.0527(7) Uani 1 1 d . A . H27 H 0.7943 -0.1606 0.5290 0.063 Uiso 1 1 calc R . . C28 C 0.85424(19) -0.1967(2) 0.48359(9) 0.0809(11) Uani 1 1 d . . . H28A H 0.8730 -0.1675 0.4613 0.121 Uiso 1 1 calc R A . H28B H 0.8250 -0.2456 0.4755 0.121 Uiso 1 1 calc R . . H28C H 0.8911 -0.2197 0.4995 0.121 Uiso 1 1 calc R . . C29 C 0.75280(17) -0.0956(3) 0.48266(9) 0.0767(10) Uani 1 1 d . . . H29A H 0.7262 -0.0541 0.4978 0.115 Uiso 1 1 calc R A . H29B H 0.7243 -0.1456 0.4749 0.115 Uiso 1 1 calc R . . H29C H 0.7696 -0.0653 0.4601 0.115 Uiso 1 1 calc R . . C30 C 0.64841(10) 0.07073(14) 0.63220(5) 0.0248(4) Uani 1 1 d . A . C31 C 0.57818(12) 0.18940(16) 0.64030(7) 0.0390(6) Uani 1 1 d . A . H31 H 0.5600 0.2473 0.6380 0.047 Uiso 1 1 calc R . . C32 C 0.55419(12) 0.12366(16) 0.66139(7) 0.0424(6) Uani 1 1 d . A . H32 H 0.5157 0.1259 0.6772 0.051 Uiso 1 1 calc R . . C33 C 0.66743(12) 0.21101(14) 0.59410(6) 0.0303(5) Uani 1 1 d . A . C34 C 0.71278(12) 0.27552(15) 0.60609(7) 0.0356(5) Uani 1 1 d . . . C35 C 0.73863(14) 0.33204(17) 0.57837(8) 0.0472(7) Uani 1 1 d . A . H35 H 0.7703 0.3765 0.5854 0.057 Uiso 1 1 calc R . . C36 C 0.71888(16) 0.32413(18) 0.54118(8) 0.0544(8) Uani 1 1 d . . . H36 H 0.7365 0.3637 0.5229 0.065 Uiso 1 1 calc R A . C37 C 0.67417(15) 0.25999(18) 0.53011(7) 0.0482(7) Uani 1 1 d . A . H37 H 0.6617 0.2553 0.5041 0.058 Uiso 1 1 calc R . . C38 C 0.64627(13) 0.20099(16) 0.55627(6) 0.0379(6) Uani 1 1 d . . . C39 C 0.73249(13) 0.28767(16) 0.64754(7) 0.0383(6) Uani 1 1 d . A . H39 H 0.7165 0.2346 0.6618 0.046 Uiso 1 1 calc R . . C40 C 0.80878(15) 0.2948(2) 0.65347(9) 0.0624(8) Uani 1 1 d . . . H40A H 0.8310 0.2449 0.6410 0.094 Uiso 1 1 calc R A . H40B H 0.8194 0.2936 0.6806 0.094 Uiso 1 1 calc R . . H40C H 0.8249 0.3504 0.6426 0.094 Uiso 1 1 calc R . . C41 C 0.69691(17) 0.36872(19) 0.66363(8) 0.0610(8) Uani 1 1 d . . . H41A H 0.7078 0.4208 0.6483 0.091 Uiso 1 1 calc R A . H41B H 0.7121 0.3785 0.6898 0.091 Uiso 1 1 calc R . . H41C H 0.6480 0.3590 0.6631 0.091 Uiso 1 1 calc R . . C42 C 0.59631(14) 0.13062(19) 0.54404(7) 0.0482(7) Uani 1 1 d . A . H42 H 0.5955 0.0848 0.5644 0.058 Uiso 1 1 calc R . . C43 C 0.61602(17) 0.0842(2) 0.50747(9) 0.0698(9) Uani 1 1 d . . . H43A H 0.6134 0.1262 0.4864 0.105 Uiso 1 1 calc R A . H43B H 0.5851 0.0347 0.5026 0.105 Uiso 1 1 calc R . . H43C H 0.6623 0.0616 0.5099 0.105 Uiso 1 1 calc R . . C44 C 0.52530(17) 0.1680(3) 0.54041(12) 0.0935(13) Uani 1 1 d . . . H44A H 0.5121 0.1944 0.5646 0.140 Uiso 1 1 calc R A . H44B H 0.4938 0.1204 0.5337 0.140 Uiso 1 1 calc R . . H44C H 0.5242 0.2134 0.5206 0.140 Uiso 1 1 calc R . . C45 C 0.57616(12) -0.03308(15) 0.67169(7) 0.0349(5) Uani 1 1 d . A . C46 C 0.59758(12) -0.05416(15) 0.70835(7) 0.0372(6) Uani 1 1 d . . . C47 C 0.57431(14) -0.13398(17) 0.72333(7) 0.0476(7) Uani 1 1 d . A . H47 H 0.5894 -0.1522 0.7478 0.057 Uiso 1 1 calc R . . C48 C 0.52997(16) -0.18659(18) 0.70327(8) 0.0561(8) Uani 1 1 d . . . H48 H 0.5152 -0.2409 0.7139 0.067 Uiso 1 1 calc R A . C49 C 0.50656(15) -0.16159(18) 0.66778(8) 0.0520(7) Uani 1 1 d . A . H49 H 0.4743 -0.1974 0.6549 0.062 Uiso 1 1 calc R . . C50 C 0.52993(13) -0.08425(17) 0.65080(7) 0.0436(6) Uani 1 1 d . . . C51 C 0.64044(13) 0.00798(16) 0.73221(7) 0.0386(6) Uani 1 1 d . A . H51 H 0.6587 0.0545 0.7150 0.046 Uiso 1 1 calc R . . C52 C 0.70004(16) -0.0384(2) 0.75076(9) 0.0607(8) Uani 1 1 d . . . H52A H 0.6836 -0.0825 0.7688 0.091 Uiso 1 1 calc R A . H52B H 0.7281 0.0051 0.7642 0.091 Uiso 1 1 calc R . . H52C H 0.7269 -0.0679 0.7313 0.091 Uiso 1 1 calc R . . C53 C 0.59713(16) 0.0546(2) 0.76200(9) 0.0638(9) Uani 1 1 d . . . H53A H 0.5772 0.0103 0.7788 0.096 Uiso 1 1 calc R A . H53B H 0.5611 0.0881 0.7493 0.096 Uiso 1 1 calc R . . H53C H 0.6255 0.0951 0.7769 0.096 Uiso 1 1 calc R . . C54 C 0.50425(15) -0.0577(2) 0.61189(9) 0.0596(8) Uani 1 1 d . A . H54 H 0.5384 -0.0168 0.6007 0.071 Uiso 1 1 calc R . . C55 C 0.49568(18) -0.1358(2) 0.58465(9) 0.0777(11) Uani 1 1 d . . . H55A H 0.5364 -0.1726 0.5855 0.117 Uiso 1 1 calc R A . H55B H 0.4885 -0.1135 0.5588 0.117 Uiso 1 1 calc R . . H55C H 0.4566 -0.1712 0.5922 0.117 Uiso 1 1 calc R . . C56 C 0.43701(17) -0.0061(2) 0.61468(13) 0.0883(13) Uani 1 1 d . . . H56A H 0.4024 -0.0444 0.6256 0.132 Uiso 1 1 calc R A . H56B H 0.4225 0.0130 0.5893 0.132 Uiso 1 1 calc R . . H56C H 0.4436 0.0459 0.6309 0.132 Uiso 1 1 calc R . . Cl1A Cl 0.7906(2) 0.0627(3) 0.67175(10) 0.0365(8) Uani 0.50 1 d P A 1 O1A O 0.6521(3) -0.1128(4) 0.56192(17) 0.0579(16) Uani 0.50 1 d P A 1 C1A C 0.6814(8) -0.0730(9) 0.5838(3) 0.032(2) Uani 0.50 1 d P A 1 H1 H 0.7041(11) -0.0761(13) 0.6503(5) 0.048(7) Uiso 1 1 d D A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02869(11) 0.02345(10) 0.02338(9) 0.00077(7) 0.00487(7) 0.00156(8) Cl1 0.0428(14) 0.0432(19) 0.034(2) -0.0170(11) -0.0056(13) -0.0021(12) O1 0.051(3) 0.054(3) 0.040(4) -0.014(3) -0.008(3) 0.002(2) O2 0.0538(12) 0.0457(11) 0.0591(12) 0.0227(9) 0.0294(10) 0.0157(9) N1 0.0349(11) 0.0268(10) 0.0316(10) 0.0004(8) 0.0046(8) 0.0049(8) N2 0.0347(11) 0.0263(10) 0.0342(10) -0.0026(8) 0.0085(8) 0.0028(8) N3 0.0271(10) 0.0257(9) 0.0287(9) 0.0035(7) 0.0045(8) 0.0030(8) N4 0.0290(10) 0.0294(10) 0.0378(11) 0.0075(8) 0.0076(8) 0.0004(8) C1 0.022(6) 0.040(7) 0.036(8) 0.011(6) -0.004(5) 0.006(4) C2 0.0345(14) 0.0321(12) 0.0368(13) 0.0001(10) 0.0051(11) 0.0075(11) C3 0.0278(12) 0.0255(11) 0.0260(11) -0.0043(8) -0.0004(9) -0.0023(9) C4 0.0488(16) 0.0300(13) 0.0494(15) 0.0010(11) 0.0093(12) 0.0136(12) C5 0.0449(16) 0.0332(13) 0.0490(15) -0.0018(11) 0.0156(12) 0.0117(12) C6 0.0421(14) 0.0289(12) 0.0316(12) 0.0074(9) 0.0061(10) 0.0102(11) C7 0.0486(16) 0.0280(12) 0.0376(13) 0.0051(10) 0.0061(11) 0.0034(11) C8 0.0623(18) 0.0340(14) 0.0476(16) 0.0086(11) 0.0144(13) -0.0012(13) C9 0.076(2) 0.0431(16) 0.0388(15) 0.0137(12) 0.0142(14) 0.0135(15) C10 0.0642(19) 0.0503(17) 0.0333(14) 0.0059(11) -0.0029(13) 0.0167(15) C11 0.0423(15) 0.0387(14) 0.0358(13) 0.0028(10) -0.0010(11) 0.0138(12) C12 0.0634(19) 0.0374(15) 0.0430(15) 0.0042(11) 0.0086(13) -0.0119(13) C13 0.173(4) 0.0411(18) 0.065(2) -0.0099(15) 0.006(2) -0.005(2) C14 0.059(2) 0.110(3) 0.060(2) -0.0046(19) 0.0030(16) -0.033(2) C15 0.0412(16) 0.0636(18) 0.0394(14) -0.0021(12) -0.0062(12) 0.0057(14) C16 0.0447(19) 0.108(3) 0.077(2) -0.029(2) -0.0062(16) 0.0176(19) C17 0.0525(18) 0.065(2) 0.0536(18) -0.0054(14) -0.0153(14) 0.0023(15) C18 0.0380(14) 0.0307(12) 0.0395(13) 0.0023(10) 0.0172(11) 0.0074(11) C19 0.0355(14) 0.0370(14) 0.0581(17) -0.0005(12) 0.0176(12) 0.0038(12) C20 0.0430(17) 0.0408(16) 0.085(2) 0.0063(15) 0.0286(16) -0.0015(13) C21 0.065(2) 0.0508(18) 0.075(2) 0.0269(16) 0.0383(18) 0.0175(17) C22 0.064(2) 0.0581(19) 0.0457(16) 0.0137(13) 0.0238(14) 0.0210(17) C23 0.0507(16) 0.0420(15) 0.0372(14) 0.0002(11) 0.0167(12) 0.0127(13) C24 0.0469(17) 0.0598(19) 0.0624(19) -0.0063(14) 0.0098(14) -0.0188(15) C25 0.070(2) 0.080(3) 0.094(3) -0.003(2) -0.018(2) 0.010(2) C26 0.051(2) 0.089(3) 0.103(3) -0.039(2) 0.0121(19) -0.0131(19) C27 0.0635(19) 0.0608(18) 0.0339(14) -0.0075(12) 0.0049(13) 0.0055(15) C28 0.104(3) 0.074(2) 0.065(2) -0.0307(18) 0.015(2) 0.009(2) C29 0.078(2) 0.109(3) 0.0439(18) -0.0021(18) -0.0034(16) 0.005(2) C30 0.0242(11) 0.0282(11) 0.0221(10) 0.0019(8) -0.0002(8) -0.0026(9) C31 0.0333(14) 0.0345(13) 0.0495(15) 0.0064(11) 0.0120(11) 0.0112(11) C32 0.0313(14) 0.0395(14) 0.0569(16) 0.0111(12) 0.0177(12) 0.0098(11) C33 0.0349(13) 0.0248(11) 0.0313(12) 0.0090(9) 0.0096(10) 0.0075(10) C34 0.0415(14) 0.0258(12) 0.0398(13) 0.0041(10) 0.0103(11) 0.0046(11) C35 0.0581(18) 0.0315(13) 0.0522(16) 0.0088(11) 0.0166(13) -0.0044(13) C36 0.075(2) 0.0397(15) 0.0495(17) 0.0187(13) 0.0259(15) 0.0069(15) C37 0.0661(19) 0.0488(16) 0.0299(13) 0.0120(11) 0.0091(12) 0.0177(15) C38 0.0436(15) 0.0374(13) 0.0326(12) 0.0054(10) 0.0027(11) 0.0115(12) C39 0.0451(15) 0.0308(12) 0.0390(13) 0.0038(10) 0.0034(11) -0.0040(11) C40 0.0540(19) 0.063(2) 0.071(2) -0.0039(16) 0.0010(15) -0.0174(16) C41 0.091(2) 0.0464(17) 0.0455(16) -0.0063(13) 0.0050(16) 0.0094(17) C42 0.0509(17) 0.0548(17) 0.0387(14) 0.0044(12) -0.0058(12) 0.0053(14) C43 0.073(2) 0.078(2) 0.059(2) -0.0179(16) -0.0153(17) 0.0088(19) C44 0.048(2) 0.098(3) 0.134(4) -0.034(3) -0.012(2) 0.015(2) C45 0.0326(13) 0.0298(12) 0.0424(14) 0.0071(10) 0.0134(11) -0.0002(10) C46 0.0379(14) 0.0326(13) 0.0415(14) 0.0049(10) 0.0148(11) 0.0026(11) C47 0.0626(19) 0.0387(14) 0.0419(14) 0.0080(11) 0.0182(13) -0.0047(14) C48 0.079(2) 0.0366(15) 0.0538(17) 0.0039(13) 0.0315(16) -0.0150(15) C49 0.0562(18) 0.0453(16) 0.0548(17) -0.0024(13) 0.0169(14) -0.0196(14) C50 0.0364(15) 0.0444(15) 0.0502(16) 0.0056(12) 0.0103(12) -0.0077(12) C51 0.0394(14) 0.0366(13) 0.0400(13) 0.0082(10) 0.0098(11) 0.0019(11) C52 0.063(2) 0.0558(18) 0.063(2) 0.0135(15) -0.0052(16) 0.0085(16) C53 0.0570(19) 0.065(2) 0.070(2) -0.0203(16) 0.0218(16) -0.0049(16) C54 0.0483(18) 0.064(2) 0.066(2) 0.0184(16) -0.0074(15) -0.0211(16) C55 0.071(2) 0.095(3) 0.066(2) 0.0048(19) -0.0209(18) -0.031(2) C56 0.050(2) 0.079(3) 0.136(4) 0.032(2) -0.017(2) -0.0098(19) Cl1A 0.035(2) 0.0407(15) 0.033(3) -0.0035(17) -0.0057(16) 0.0048(14) O1A 0.063(4) 0.061(3) 0.050(4) -0.027(2) -0.005(3) -0.005(3) C1A 0.036(5) 0.036(6) 0.023(6) -0.010(3) 0.003(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.601(9) . ? Ru1 C1A 1.912(10) . ? Ru1 C1 1.920(11) . ? Ru1 C2 1.975(2) . ? Ru1 C3 2.126(2) . ? Ru1 C30 2.128(2) . ? Ru1 Cl1 2.379(2) . ? Ru1 Cl1A 2.387(3) . ? O1 C1 1.134(11) . ? O2 C2 1.139(3) . ? N1 C3 1.373(3) . ? N1 C4 1.389(3) . ? N1 C6 1.456(3) . ? N2 C3 1.377(3) . ? N2 C5 1.380(3) . ? N2 C18 1.448(3) . ? N3 C30 1.370(3) . ? N3 C31 1.385(3) . ? N3 C33 1.450(3) . ? N4 C30 1.371(3) . ? N4 C32 1.384(3) . ? N4 C45 1.452(3) . ? C4 C5 1.332(3) . ? C6 C7 1.390(3) . ? C6 C11 1.401(3) . ? C7 C8 1.407(3) . ? C7 C12 1.518(4) . ? C8 C9 1.371(4) . ? C9 C10 1.369(4) . ? C10 C11 1.401(3) . ? C11 C15 1.509(4) . ? C12 C14 1.517(4) . ? C12 C13 1.528(4) . ? C15 C17 1.535(4) . ? C15 C16 1.540(4) . ? C18 C23 1.397(3) . ? C18 C19 1.400(4) . ? C19 C20 1.395(4) . ? C19 C24 1.514(4) . ? C20 C21 1.371(4) . ? C21 C22 1.371(4) . ? C22 C23 1.402(4) . ? C23 C27 1.513(4) . ? C24 C26 1.530(4) . ? C24 C25 1.535(4) . ? C27 C29 1.533(4) . ? C27 C28 1.541(4) . ? C31 C32 1.332(3) . ? C33 C34 1.389(3) . ? C33 C38 1.404(3) . ? C34 C35 1.401(3) . ? C34 C39 1.522(3) . ? C35 C36 1.371(4) . ? C36 C37 1.367(4) . ? C37 C38 1.402(3) . ? C38 C42 1.512(4) . ? C39 C41 1.526(3) . ? C39 C40 1.527(4) . ? C42 C44 1.520(4) . ? C42 C43 1.525(4) . ? C45 C46 1.395(3) . ? C45 C50 1.402(4) . ? C46 C47 1.398(3) . ? C46 C51 1.515(4) . ? C47 C48 1.375(4) . ? C48 C49 1.384(4) . ? C49 C50 1.395(3) . ? C50 C54 1.514(4) . ? C51 C52 1.516(4) . ? C51 C53 1.536(3) . ? C54 C55 1.530(4) . ? C54 C56 1.548(5) . ? O1A C1A 1.133(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 H1 Ru1 C1A 85.1(10) . . ? H1 Ru1 C1 88.5(11) . . ? C1A Ru1 C1 172.9(8) . . ? H1 Ru1 C2 179.3(9) . . ? C1A Ru1 C2 94.3(5) . . ? C1 Ru1 C2 92.1(7) . . ? H1 Ru1 C3 84.8(9) . . ? C1A Ru1 C3 88.7(4) . . ? C1 Ru1 C3 93.8(7) . . ? C2 Ru1 C3 94.80(8) . . ? H1 Ru1 C30 85.3(9) . . ? C1A Ru1 C30 89.4(4) . . ? C1 Ru1 C30 87.0(7) . . ? C2 Ru1 C30 95.06(8) . . ? C3 Ru1 C30 170.07(8) . . ? H1 Ru1 Cl1 85.8(9) . . ? C1A Ru1 Cl1 3.2(5) . . ? C1 Ru1 Cl1 174.3(7) . . ? C2 Ru1 Cl1 93.57(12) . . ? C3 Ru1 Cl1 85.65(11) . . ? C30 Ru1 Cl1 92.60(11) . . ? H1 Ru1 Cl1A 87.2(9) . . ? C1A Ru1 Cl1A 171.9(5) . . ? C1 Ru1 Cl1A 1.5(8) . . ? C2 Ru1 Cl1A 93.42(14) . . ? C3 Ru1 Cl1A 92.90(13) . . ? C30 Ru1 Cl1A 87.65(13) . . ? Cl1 Ru1 Cl1A 172.96(16) . . ? C3 N1 C4 112.13(18) . . ? C3 N1 C6 130.30(18) . . ? C4 N1 C6 117.47(18) . . ? C3 N2 C5 112.30(19) . . ? C3 N2 C18 128.24(18) . . ? C5 N2 C18 118.76(18) . . ? C30 N3 C31 112.37(18) . . ? C30 N3 C33 128.53(17) . . ? C31 N3 C33 118.79(18) . . ? C30 N4 C32 112.20(18) . . ? C30 N4 C45 129.11(19) . . ? C32 N4 C45 118.33(18) . . ? O1 C1 Ru1 174(2) . . ? O2 C2 Ru1 179.8(3) . . ? N1 C3 N2 101.82(17) . . ? N1 C3 Ru1 128.32(15) . . ? N2 C3 Ru1 129.16(15) . . ? C5 C4 N1 106.7(2) . . ? C4 C5 N2 107.0(2) . . ? C7 C6 C11 123.3(2) . . ? C7 C6 N1 118.0(2) . . ? C11 C6 N1 117.9(2) . . ? C6 C7 C8 117.0(2) . . ? C6 C7 C12 123.0(2) . . ? C8 C7 C12 119.9(2) . . ? C9 C8 C7 121.1(3) . . ? C10 C9 C8 120.3(2) . . ? C9 C10 C11 121.8(3) . . ? C10 C11 C6 116.4(2) . . ? C10 C11 C15 121.5(2) . . ? C6 C11 C15 122.0(2) . . ? C14 C12 C7 112.1(2) . . ? C14 C12 C13 111.6(3) . . ? C7 C12 C13 109.7(2) . . ? C11 C15 C17 113.7(2) . . ? C11 C15 C16 110.2(2) . . ? C17 C15 C16 109.6(2) . . ? C23 C18 C19 123.3(2) . . ? C23 C18 N2 118.9(2) . . ? C19 C18 N2 117.5(2) . . ? C20 C19 C18 116.9(3) . . ? C20 C19 C24 120.6(3) . . ? C18 C19 C24 122.4(2) . . ? C21 C20 C19 121.2(3) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C23 121.4(3) . . ? C18 C23 C22 116.5(3) . . ? C18 C23 C27 123.1(2) . . ? C22 C23 C27 120.3(3) . . ? C19 C24 C26 112.9(3) . . ? C19 C24 C25 110.3(3) . . ? C26 C24 C25 110.3(3) . . ? C23 C27 C29 112.8(3) . . ? C23 C27 C28 109.6(2) . . ? C29 C27 C28 110.4(3) . . ? N3 C30 N4 101.93(17) . . ? N3 C30 Ru1 129.55(14) . . ? N4 C30 Ru1 128.12(15) . . ? C32 C31 N3 106.5(2) . . ? C31 C32 N4 106.9(2) . . ? C34 C33 C38 123.4(2) . . ? C34 C33 N3 118.6(2) . . ? C38 C33 N3 117.7(2) . . ? C33 C34 C35 117.1(2) . . ? C33 C34 C39 122.4(2) . . ? C35 C34 C39 120.5(2) . . ? C36 C35 C34 120.9(3) . . ? C37 C36 C35 120.8(2) . . ? C36 C37 C38 121.4(2) . . ? C37 C38 C33 116.3(2) . . ? C37 C38 C42 121.4(2) . . ? C33 C38 C42 122.3(2) . . ? C34 C39 C41 109.9(2) . . ? C34 C39 C40 112.5(2) . . ? C41 C39 C40 110.7(2) . . ? C38 C42 C44 111.4(2) . . ? C38 C42 C43 113.1(2) . . ? C44 C42 C43 110.2(3) . . ? C46 C45 C50 123.5(2) . . ? C46 C45 N4 118.5(2) . . ? C50 C45 N4 117.5(2) . . ? C45 C46 C47 116.8(2) . . ? C45 C46 C51 122.5(2) . . ? C47 C46 C51 120.6(2) . . ? C48 C47 C46 121.0(3) . . ? C47 C48 C49 120.9(2) . . ? C48 C49 C50 120.6(3) . . ? C49 C50 C45 117.0(2) . . ? C49 C50 C54 120.2(2) . . ? C45 C50 C54 122.8(2) . . ? C46 C51 C52 112.5(2) . . ? C46 C51 C53 110.6(2) . . ? C52 C51 C53 110.8(2) . . ? C50 C54 C55 113.6(3) . . ? C50 C54 C56 110.9(3) . . ? C55 C54 C56 109.8(3) . . ? O1A C1A Ru1 177.6(14) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.390 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.075 data_c:\x-ray\kappa\k07mkw7\maxus\k07mkw7 _database_code_depnum_ccdc_archive 'CCDC 668490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H77 Cl N4 O2 Ru' _chemical_formula_weight 974.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.6590(3) _cell_length_b 15.1810(2) _cell_length_c 35.1910(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.022(1) _cell_angle_gamma 90.00 _cell_volume 10496.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36723 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33921 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 29.99 _reflns_number_total 12955 _reflns_number_gt 8178 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12955 _refine_ls_number_parameters 625 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.732179(9) -0.007107(11) 0.619344(6) 0.01931(7) Uani 1 1 d D . . Cl1 Cl 0.67014(12) -0.09554(14) 0.57378(7) 0.0288(6) Uani 0.50 1 d P A 2 Cl1A Cl 0.78747(11) 0.06588(14) 0.67278(7) 0.0257(6) Uani 0.50 1 d P A 1 O1 O 0.79160(9) 0.12058(11) 0.55938(6) 0.0407(6) Uani 1 1 d . . . O2 O 0.8033(4) 0.0845(5) 0.6867(2) 0.0359(16) Uani 0.50 1 d PU A 2 O2A O 0.6483(3) -0.1143(4) 0.5616(2) 0.0368(14) Uani 0.50 1 d PU A 1 N1 N 0.85220(9) -0.11419(11) 0.58363(7) 0.0237(5) Uani 1 1 d . . . N2 N 0.81892(9) -0.17877(12) 0.63449(7) 0.0243(5) Uani 1 1 d . . . N3 N 0.59514(9) 0.05351(11) 0.65457(6) 0.0231(5) Uani 1 1 d . . . N4 N 0.63699(9) 0.16054(11) 0.62239(6) 0.0218(5) Uani 1 1 d . . . C1 C 0.76969(11) 0.07409(15) 0.58127(9) 0.0266(7) Uani 1 1 d . A . C2 C 0.7760(7) 0.0485(8) 0.6607(3) 0.0193(19) Uani 0.50 1 d PU A 2 C3 C 0.80977(11) -0.10467(14) 0.61309(8) 0.0208(6) Uani 1 1 d . A . C4 C 0.89507(12) -0.19405(14) 0.58625(9) 0.0310(7) Uani 1 1 d . A . H4A H 0.9424 -0.1796 0.5945 0.037 Uiso 1 1 calc R . . H4B H 0.8953 -0.2258 0.5617 0.037 Uiso 1 1 calc R . . C5 C 0.85997(12) -0.24674(15) 0.61593(8) 0.0316(7) Uani 1 1 d . A . H5A H 0.8308 -0.2933 0.6042 0.038 Uiso 1 1 calc R . . H5B H 0.8932 -0.2741 0.6342 0.038 Uiso 1 1 calc R . . C6 C 0.87551(12) -0.04956(15) 0.55704(9) 0.0266(7) Uani 1 1 d . A . C7 C 0.85392(13) -0.05604(16) 0.51895(10) 0.0315(7) Uani 1 1 d . . . C8 C 0.88058(14) 0.00437(17) 0.49329(10) 0.0408(8) Uani 1 1 d . A . H8 H 0.8659 0.0026 0.4673 0.049 Uiso 1 1 calc R . . C9 C 0.92784(14) 0.06635(18) 0.50537(11) 0.0476(10) Uani 1 1 d . . . H9 H 0.9450 0.1073 0.4877 0.057 Uiso 1 1 calc R A . C10 C 0.95020(13) 0.06936(17) 0.54252(11) 0.0410(9) Uani 1 1 d . A . H10 H 0.9833 0.1121 0.5501 0.049 Uiso 1 1 calc R . . C11 C 0.92585(12) 0.01138(15) 0.56971(10) 0.0320(8) Uani 1 1 d . . . C12 C 0.80759(14) -0.12901(17) 0.50403(9) 0.0379(8) Uani 1 1 d . A . H12 H 0.7905 -0.1621 0.5263 0.045 Uiso 1 1 calc R . . C13 C 0.84792(16) -0.19347(19) 0.47974(10) 0.0527(10) Uani 1 1 d . . . H13A H 0.8622 -0.1635 0.4567 0.079 Uiso 1 1 calc R A . H13B H 0.8191 -0.2439 0.4727 0.079 Uiso 1 1 calc R . . H13C H 0.8882 -0.2141 0.4944 0.079 Uiso 1 1 calc R . . C14 C 0.74582(14) -0.0946(2) 0.48069(10) 0.0524(9) Uani 1 1 d . . . H14A H 0.7200 -0.0537 0.4962 0.079 Uiso 1 1 calc R A . H14B H 0.7166 -0.1441 0.4729 0.079 Uiso 1 1 calc R . . H14C H 0.7613 -0.0638 0.4581 0.079 Uiso 1 1 calc R . . C15 C 0.95516(13) 0.01289(17) 0.60970(11) 0.0408(9) Uani 1 1 d . A . H15 H 0.9295 -0.0308 0.6249 0.049 Uiso 1 1 calc R . . C16 C 1.03072(13) -0.0147(2) 0.61091(11) 0.0567(11) Uani 1 1 d . . . H16A H 1.0350 -0.0736 0.5999 0.085 Uiso 1 1 calc R A . H16B H 1.0482 -0.0153 0.6373 0.085 Uiso 1 1 calc R . . H16C H 1.0570 0.0274 0.5962 0.085 Uiso 1 1 calc R . . C17 C 0.94801(15) 0.10427(18) 0.62868(11) 0.0579(11) Uani 1 1 d . . . H17A H 0.9751 0.1476 0.6152 0.087 Uiso 1 1 calc R A . H17B H 0.9643 0.1009 0.6553 0.087 Uiso 1 1 calc R . . H17C H 0.9001 0.1222 0.6276 0.087 Uiso 1 1 calc R . . C18 C 0.79372(12) -0.20361(15) 0.67091(9) 0.0271(7) Uani 1 1 d . A . C19 C 0.73959(13) -0.26504(15) 0.67145(9) 0.0319(7) Uani 1 1 d . . . C20 C 0.72397(16) -0.29814(18) 0.70731(11) 0.0439(9) Uani 1 1 d . A . H20 H 0.6869 -0.3380 0.7090 0.053 Uiso 1 1 calc R . . C21 C 0.75951(18) -0.27576(19) 0.73976(11) 0.0530(10) Uani 1 1 d . . . H21 H 0.7477 -0.3010 0.7633 0.064 Uiso 1 1 calc R A . C22 C 0.81277(16) -0.21627(19) 0.73854(10) 0.0491(9) Uani 1 1 d . A . H22 H 0.8374 -0.2010 0.7613 0.059 Uiso 1 1 calc R . . C23 C 0.83068(14) -0.17827(17) 0.70383(10) 0.0347(8) Uani 1 1 d . . . C24 C 0.70291(13) -0.29755(15) 0.63603(10) 0.0351(8) Uani 1 1 d . A . H24 H 0.7222 -0.2662 0.6138 0.042 Uiso 1 1 calc R . . C25 C 0.71496(15) -0.39660(16) 0.63083(11) 0.0491(10) Uani 1 1 d . . . H25A H 0.7640 -0.4081 0.6303 0.074 Uiso 1 1 calc R A . H25B H 0.6929 -0.4161 0.6069 0.074 Uiso 1 1 calc R . . H25C H 0.6957 -0.4288 0.6520 0.074 Uiso 1 1 calc R . . C26 C 0.62713(13) -0.27753(18) 0.63635(10) 0.0489(10) Uani 1 1 d . . . H26A H 0.6069 -0.3088 0.6575 0.073 Uiso 1 1 calc R A . H26B H 0.6053 -0.2968 0.6123 0.073 Uiso 1 1 calc R . . H26C H 0.6204 -0.2140 0.6394 0.073 Uiso 1 1 calc R . . C27 C 0.89019(13) -0.11435(19) 0.70221(10) 0.0438(9) Uani 1 1 d . A . H27 H 0.8818 -0.0755 0.6796 0.053 Uiso 1 1 calc R . . C28 C 0.95737(14) -0.1636(2) 0.69639(12) 0.0743(13) Uani 1 1 d . . . H28A H 0.9661 -0.2043 0.7176 0.111 Uiso 1 1 calc R A . H28B H 0.9947 -0.1211 0.6953 0.111 Uiso 1 1 calc R . . H28C H 0.9540 -0.1969 0.6725 0.111 Uiso 1 1 calc R . . C29 C 0.89734(14) -0.0545(2) 0.73727(10) 0.0533(10) Uani 1 1 d . . . H29A H 0.8545 -0.0228 0.7407 0.080 Uiso 1 1 calc R A . H29B H 0.9341 -0.0120 0.7337 0.080 Uiso 1 1 calc R . . H29C H 0.9079 -0.0904 0.7599 0.080 Uiso 1 1 calc R . . C30 C 0.64654(10) 0.07451(14) 0.63150(8) 0.0181(5) Uani 1 1 d . A . C31 C 0.57339(12) 0.19740(15) 0.63688(9) 0.0320(7) Uani 1 1 d . A . H31A H 0.5372 0.2004 0.6167 0.038 Uiso 1 1 calc R . . H31B H 0.5808 0.2568 0.6479 0.038 Uiso 1 1 calc R . . C32 C 0.55662(12) 0.13145(15) 0.66686(9) 0.0327(8) Uani 1 1 d . A . H32A H 0.5723 0.1515 0.6925 0.039 Uiso 1 1 calc R . . H32B H 0.5071 0.1193 0.6669 0.039 Uiso 1 1 calc R . . C33 C 0.66846(11) 0.21245(14) 0.59366(9) 0.0237(7) Uani 1 1 d . A . C34 C 0.71683(12) 0.27620(15) 0.60614(9) 0.0261(7) Uani 1 1 d . . . C35 C 0.74287(13) 0.33075(16) 0.57771(10) 0.0347(8) Uani 1 1 d . A . H35 H 0.7762 0.3737 0.5847 0.042 Uiso 1 1 calc R . . C36 C 0.72171(14) 0.32386(17) 0.54057(10) 0.0396(9) Uani 1 1 d . . . H36 H 0.7406 0.3617 0.5222 0.047 Uiso 1 1 calc R A . C37 C 0.67318(13) 0.26256(16) 0.52923(9) 0.0325(7) Uani 1 1 d . A . H37 H 0.6587 0.2590 0.5032 0.039 Uiso 1 1 calc R . . C38 C 0.64523(12) 0.20551(15) 0.55589(9) 0.0261(7) Uani 1 1 d . . . C39 C 0.73716(12) 0.28904(15) 0.64732(9) 0.0291(7) Uani 1 1 d . A . H39 H 0.7193 0.2382 0.6620 0.035 Uiso 1 1 calc R . . C40 C 0.81477(12) 0.29274(18) 0.65422(10) 0.0437(9) Uani 1 1 d . . . H40A H 0.8358 0.2418 0.6421 0.066 Uiso 1 1 calc R A . H40B H 0.8255 0.2916 0.6816 0.066 Uiso 1 1 calc R . . H40C H 0.8325 0.3471 0.6433 0.066 Uiso 1 1 calc R . . C41 C 0.70518(14) 0.37357(17) 0.66243(10) 0.0455(9) Uani 1 1 d . . . H41A H 0.7211 0.4242 0.6479 0.068 Uiso 1 1 calc R A . H41B H 0.7185 0.3810 0.6893 0.068 Uiso 1 1 calc R . . H41C H 0.6555 0.3696 0.6597 0.068 Uiso 1 1 calc R . . C42 C 0.59091(13) 0.14014(16) 0.54266(9) 0.0333(7) Uani 1 1 d . A . H42 H 0.5787 0.1036 0.5650 0.040 Uiso 1 1 calc R . . C43 C 0.61640(14) 0.07814(18) 0.51203(9) 0.0449(9) Uani 1 1 d . . . H43A H 0.6258 0.1120 0.4891 0.067 Uiso 1 1 calc R A . H43B H 0.5815 0.0337 0.5060 0.067 Uiso 1 1 calc R . . H43C H 0.6582 0.0489 0.5214 0.067 Uiso 1 1 calc R . . C44 C 0.52608(13) 0.18725(19) 0.52782(10) 0.0477(9) Uani 1 1 d . . . H44A H 0.5099 0.2270 0.5475 0.072 Uiso 1 1 calc R A . H44B H 0.4908 0.1435 0.5215 0.072 Uiso 1 1 calc R . . H44C H 0.5362 0.2213 0.5050 0.072 Uiso 1 1 calc R . . C45 C 0.57382(11) -0.02998(15) 0.66990(9) 0.0235(7) Uani 1 1 d . A . C46 C 0.52611(12) -0.08003(15) 0.64791(9) 0.0279(7) Uani 1 1 d . . . C47 C 0.50025(12) -0.15543(16) 0.66493(9) 0.0331(8) Uani 1 1 d . A . H47 H 0.4671 -0.1898 0.6514 0.040 Uiso 1 1 calc R . . C48 C 0.52167(13) -0.18093(16) 0.70069(10) 0.0360(8) Uani 1 1 d . . . H48 H 0.5046 -0.2338 0.7112 0.043 Uiso 1 1 calc R A . C49 C 0.56822(13) -0.13020(16) 0.72183(9) 0.0332(7) Uani 1 1 d . A . H49 H 0.5828 -0.1486 0.7466 0.040 Uiso 1 1 calc R . . C50 C 0.59359(12) -0.05185(15) 0.70661(9) 0.0262(7) Uani 1 1 d . . . C51 C 0.50292(13) -0.05422(17) 0.60817(10) 0.0379(8) Uani 1 1 d . A . H51 H 0.5401 -0.0184 0.5971 0.045 Uiso 1 1 calc R . . C52 C 0.48969(15) -0.1328(2) 0.58188(10) 0.0509(9) Uani 1 1 d . . . H52A H 0.5282 -0.1738 0.5841 0.076 Uiso 1 1 calc R A . H52B H 0.4844 -0.1122 0.5556 0.076 Uiso 1 1 calc R . . H52C H 0.4480 -0.1630 0.5891 0.076 Uiso 1 1 calc R . . C53 C 0.43844(15) 0.00390(19) 0.60813(12) 0.0595(11) Uani 1 1 d . . . H53A H 0.4024 -0.0269 0.6214 0.089 Uiso 1 1 calc R A . H53B H 0.4230 0.0159 0.5818 0.089 Uiso 1 1 calc R . . H53C H 0.4489 0.0596 0.6211 0.089 Uiso 1 1 calc R . . C54 C 0.63950(12) 0.00693(15) 0.73178(9) 0.0291(6) Uani 1 1 d . A . H54 H 0.6558 0.0567 0.7159 0.035 Uiso 1 1 calc R . . C55 C 0.70165(13) -0.04334(19) 0.74732(9) 0.0433(9) Uani 1 1 d . . . H55A H 0.6869 -0.0908 0.7640 0.065 Uiso 1 1 calc R A . H55B H 0.7317 -0.0030 0.7618 0.065 Uiso 1 1 calc R . . H55C H 0.7263 -0.0685 0.7262 0.065 Uiso 1 1 calc R . . C56 C 0.60006(14) 0.04610(19) 0.76480(9) 0.0433(9) Uani 1 1 d . . . H56A H 0.5841 -0.0016 0.7810 0.065 Uiso 1 1 calc R A . H56B H 0.5610 0.0796 0.7546 0.065 Uiso 1 1 calc R . . H56C H 0.6301 0.0852 0.7799 0.065 Uiso 1 1 calc R . . C2A C 0.6816(6) -0.0723(7) 0.5839(3) 0.026(2) Uani 0.50 1 d PU A 1 H1 H 0.6984(10) -0.0711(12) 0.6493(5) 0.031(7) Uiso 1 1 d D A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02015(10) 0.01874(10) 0.01928(14) -0.00023(9) 0.00430(8) 0.00276(8) Cl1 0.0250(16) 0.0353(17) 0.026(2) -0.0116(11) -0.0049(12) -0.0018(12) Cl1A 0.0218(17) 0.0257(19) 0.029(2) -0.0051(13) -0.0086(14) -0.0017(12) O1 0.0393(11) 0.0343(10) 0.0501(18) 0.0166(10) 0.0256(11) 0.0128(8) O2 0.034(3) 0.033(3) 0.041(5) -0.016(3) -0.010(3) -0.005(2) O2A 0.032(3) 0.043(3) 0.035(5) -0.019(2) -0.010(3) 0.000(2) N1 0.0233(10) 0.0208(10) 0.0273(17) -0.0016(9) 0.0066(10) 0.0059(8) N2 0.0251(11) 0.0225(10) 0.0257(18) 0.0006(10) 0.0028(10) 0.0069(8) N3 0.0214(10) 0.0197(10) 0.0286(17) 0.0042(9) 0.0068(10) 0.0038(8) N4 0.0219(10) 0.0220(10) 0.0220(16) 0.0021(9) 0.0055(10) 0.0059(8) C1 0.0215(12) 0.0253(13) 0.033(2) -0.0035(12) 0.0041(13) 0.0066(10) C2 0.015(4) 0.018(4) 0.024(6) -0.012(3) -0.010(3) -0.002(3) C3 0.0195(12) 0.0211(12) 0.0217(19) -0.0052(11) -0.0015(11) -0.0012(9) C4 0.0265(13) 0.0244(13) 0.043(2) -0.0029(13) 0.0073(13) 0.0091(10) C5 0.0345(14) 0.0258(13) 0.035(2) -0.0005(12) 0.0080(14) 0.0100(11) C6 0.0250(13) 0.0221(12) 0.034(2) 0.0009(12) 0.0129(13) 0.0063(10) C7 0.0374(15) 0.0281(14) 0.030(2) -0.0027(13) 0.0146(15) 0.0104(11) C8 0.0481(17) 0.0411(16) 0.034(2) 0.0073(15) 0.0170(16) 0.0144(14) C9 0.0445(18) 0.0360(16) 0.064(3) 0.0163(17) 0.0299(19) 0.0085(14) C10 0.0340(15) 0.0289(14) 0.061(3) 0.0001(16) 0.0192(17) 0.0009(12) C11 0.0252(13) 0.0310(14) 0.041(2) -0.0043(14) 0.0125(14) 0.0053(11) C12 0.0450(17) 0.0389(15) 0.030(2) -0.0044(14) 0.0056(15) 0.0047(13) C13 0.068(2) 0.0498(18) 0.040(3) -0.0168(17) 0.0035(19) 0.0118(15) C14 0.0528(19) 0.066(2) 0.039(3) -0.0052(18) 0.0018(18) 0.0102(16) C15 0.0304(14) 0.0447(17) 0.048(3) -0.0069(15) 0.0082(15) -0.0092(12) C16 0.0361(16) 0.064(2) 0.070(3) -0.0116(19) -0.0033(18) 0.0011(14) C17 0.0437(18) 0.058(2) 0.073(3) -0.028(2) 0.0134(19) -0.0083(15) C18 0.0329(14) 0.0248(13) 0.024(2) 0.0063(12) 0.0052(14) 0.0142(11) C19 0.0423(16) 0.0210(13) 0.033(2) 0.0026(13) 0.0115(15) 0.0097(11) C20 0.062(2) 0.0314(15) 0.040(3) 0.0087(15) 0.0160(19) 0.0094(13) C21 0.082(2) 0.0390(17) 0.039(3) 0.0171(17) 0.023(2) 0.0190(17) C22 0.069(2) 0.0510(19) 0.027(3) 0.0002(16) -0.0058(18) 0.0300(17) C23 0.0409(16) 0.0346(15) 0.029(2) 0.0004(14) 0.0007(15) 0.0179(12) C24 0.0400(15) 0.0234(13) 0.043(3) 0.0004(13) 0.0154(15) -0.0022(11) C25 0.0577(19) 0.0279(15) 0.063(3) -0.0039(15) 0.0170(18) 0.0003(13) C26 0.0395(16) 0.0423(17) 0.066(3) 0.0002(17) 0.0157(17) -0.0011(13) C27 0.0313(15) 0.0609(19) 0.039(3) -0.0097(17) -0.0070(15) 0.0110(13) C28 0.0347(18) 0.113(3) 0.074(4) -0.044(3) -0.0121(19) 0.0214(18) C29 0.0432(18) 0.071(2) 0.044(3) -0.0121(19) -0.0150(17) 0.0118(15) C30 0.0198(11) 0.0209(11) 0.0132(17) -0.0019(10) -0.0034(11) -0.0005(9) C31 0.0279(13) 0.0294(13) 0.040(2) 0.0069(13) 0.0142(14) 0.0125(11) C32 0.0323(14) 0.0298(13) 0.037(2) 0.0047(13) 0.0152(14) 0.0099(11) C33 0.0246(12) 0.0189(11) 0.028(2) 0.0072(11) 0.0105(13) 0.0080(9) C34 0.0292(13) 0.0203(12) 0.029(2) 0.0018(12) 0.0033(13) 0.0064(10) C35 0.0355(15) 0.0272(13) 0.042(3) 0.0086(14) 0.0112(15) -0.0015(11) C36 0.0448(17) 0.0331(15) 0.042(3) 0.0171(15) 0.0173(17) 0.0069(13) C37 0.0386(15) 0.0363(15) 0.023(2) 0.0048(13) 0.0041(14) 0.0133(12) C38 0.0281(13) 0.0276(13) 0.023(2) 0.0052(12) 0.0034(13) 0.0084(10) C39 0.0321(14) 0.0220(12) 0.033(2) 0.0057(12) 0.0008(13) -0.0007(10) C40 0.0356(15) 0.0421(16) 0.053(3) 0.0036(16) -0.0043(16) -0.0056(12) C41 0.0520(18) 0.0397(16) 0.045(3) -0.0071(15) 0.0020(17) 0.0066(13) C42 0.0395(16) 0.0370(15) 0.023(2) 0.0014(13) -0.0023(14) 0.0025(12) C43 0.0520(18) 0.0401(16) 0.041(3) -0.0089(15) -0.0140(17) 0.0152(13) C44 0.0350(16) 0.0600(19) 0.048(3) -0.0118(17) -0.0054(16) 0.0072(14) C45 0.0193(12) 0.0232(12) 0.029(2) 0.0056(12) 0.0077(12) 0.0029(9) C46 0.0254(13) 0.0290(13) 0.030(2) 0.0004(12) 0.0070(13) 0.0018(10) C47 0.0282(14) 0.0321(14) 0.040(3) -0.0055(14) 0.0136(15) -0.0051(11) C48 0.0432(16) 0.0257(14) 0.040(3) 0.0038(14) 0.0197(16) -0.0055(12) C49 0.0422(16) 0.0326(14) 0.026(2) 0.0063(13) 0.0111(14) 0.0009(12) C50 0.0234(12) 0.0287(13) 0.027(2) 0.0031(12) 0.0111(13) 0.0023(10) C51 0.0302(15) 0.0405(16) 0.043(3) 0.0052(15) 0.0003(15) -0.0054(12) C52 0.0457(18) 0.065(2) 0.041(3) -0.0027(18) -0.0103(17) -0.0062(15) C53 0.0479(18) 0.060(2) 0.069(3) 0.0112(19) -0.0184(19) 0.0102(15) C54 0.0295(13) 0.0340(14) 0.0241(19) 0.0040(13) 0.0036(12) 0.0007(11) C55 0.0406(17) 0.0454(16) 0.044(3) 0.0129(16) -0.0034(16) 0.0031(13) C56 0.0429(17) 0.0501(17) 0.037(3) -0.0052(16) 0.0111(16) -0.0052(13) C2A 0.021(4) 0.031(5) 0.026(6) -0.008(3) -0.009(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.595(9) . ? Ru1 C2A 1.855(7) . ? Ru1 C2 1.867(7) . ? Ru1 C1 1.982(3) . ? Ru1 C3 2.143(2) . ? Ru1 C30 2.146(2) . ? Ru1 Cl1 2.3922(19) . ? Ru1 Cl1A 2.4086(19) . ? O1 C1 1.140(3) . ? O2 C2 1.179(8) . ? O2A C2A 1.190(8) . ? N1 C3 1.361(3) . ? N1 C6 1.442(3) . ? N1 C4 1.477(3) . ? N2 C3 1.362(3) . ? N2 C18 1.440(3) . ? N2 C5 1.476(3) . ? N3 C30 1.356(3) . ? N3 C45 1.445(3) . ? N3 C32 1.478(3) . ? N4 C30 1.356(3) . ? N4 C33 1.439(3) . ? N4 C31 1.477(3) . ? C4 C5 1.503(3) . ? C6 C7 1.395(4) . ? C6 C11 1.415(4) . ? C7 C8 1.402(4) . ? C7 C12 1.516(4) . ? C8 C9 1.379(4) . ? C9 C10 1.365(4) . ? C10 C11 1.397(4) . ? C11 C15 1.502(4) . ? C12 C14 1.534(4) . ? C12 C13 1.538(4) . ? C15 C16 1.542(4) . ? C15 C17 1.548(4) . ? C18 C23 1.400(4) . ? C18 C19 1.416(3) . ? C19 C20 1.403(4) . ? C19 C24 1.501(4) . ? C20 C21 1.360(4) . ? C21 C22 1.385(4) . ? C22 C23 1.407(4) . ? C23 C27 1.523(4) . ? C24 C26 1.521(3) . ? C24 C25 1.534(3) . ? C27 C29 1.535(4) . ? C27 C28 1.538(4) . ? C31 C32 1.500(3) . ? C33 C38 1.394(4) . ? C33 C34 1.416(3) . ? C34 C35 1.409(4) . ? C34 C39 1.502(4) . ? C35 C36 1.362(4) . ? C36 C37 1.382(4) . ? C37 C38 1.403(3) . ? C38 C42 1.519(3) . ? C39 C41 1.533(3) . ? C39 C40 1.538(3) . ? C42 C43 1.529(4) . ? C42 C44 1.537(3) . ? C45 C50 1.377(4) . ? C45 C46 1.416(4) . ? C46 C47 1.396(3) . ? C46 C51 1.507(4) . ? C47 C48 1.369(4) . ? C48 C49 1.391(4) . ? C49 C50 1.403(3) . ? C50 C54 1.529(4) . ? C51 C52 1.527(4) . ? C51 C53 1.544(4) . ? C54 C55 1.526(3) . ? C54 C56 1.539(4) . ? 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 H1 Ru1 C2A 83.9(9) . . ? H1 Ru1 C2 87.3(10) . . ? C2A Ru1 C2 171.1(6) . . ? H1 Ru1 C1 177.2(8) . . ? C2A Ru1 C1 94.6(5) . . ? C2 Ru1 C1 94.2(5) . . ? H1 Ru1 C3 87.8(7) . . ? C2A Ru1 C3 85.9(4) . . ? C2 Ru1 C3 94.7(4) . . ? C1 Ru1 C3 94.43(9) . . ? H1 Ru1 C30 82.6(7) . . ? C2A Ru1 C30 92.1(4) . . ? C2 Ru1 C30 85.8(4) . . ? C1 Ru1 C30 95.10(9) . . ? C3 Ru1 C30 170.39(9) . . ? H1 Ru1 Cl1 83.5(8) . . ? C2A Ru1 Cl1 2.2(4) . . ? C2 Ru1 Cl1 170.7(5) . . ? C1 Ru1 Cl1 95.10(10) . . ? C3 Ru1 Cl1 83.76(9) . . ? C30 Ru1 Cl1 94.17(9) . . ? H1 Ru1 Cl1A 87.2(8) . . ? C2A Ru1 Cl1A 170.9(4) . . ? C2 Ru1 Cl1A 0.7(5) . . ? C1 Ru1 Cl1A 94.21(10) . . ? C3 Ru1 Cl1A 95.44(9) . . ? C30 Ru1 Cl1A 85.08(9) . . ? Cl1 Ru1 Cl1A 170.69(9) . . ? C3 N1 C6 129.75(18) . . ? C3 N1 C4 113.8(2) . . ? C6 N1 C4 113.91(18) . . ? C3 N2 C18 131.70(19) . . ? C3 N2 C5 113.3(2) . . ? C18 N2 C5 114.91(19) . . ? C30 N3 C45 131.41(18) . . ? C30 N3 C32 112.79(18) . . ? C45 N3 C32 115.76(18) . . ? C30 N4 C33 129.36(19) . . ? C30 N4 C31 113.27(18) . . ? C33 N4 C31 115.17(17) . . ? O1 C1 Ru1 179.6(2) . . ? O2 C2 Ru1 179.3(16) . . ? N1 C3 N2 105.12(18) . . ? N1 C3 Ru1 127.53(18) . . ? N2 C3 Ru1 126.49(17) . . ? N1 C4 C5 101.85(18) . . ? N2 C5 C4 101.95(18) . . ? C7 C6 C11 122.3(3) . . ? C7 C6 N1 118.9(2) . . ? C11 C6 N1 118.4(3) . . ? C6 C7 C8 117.7(3) . . ? C6 C7 C12 122.9(3) . . ? C8 C7 C12 119.2(3) . . ? C9 C8 C7 120.7(3) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C11 121.9(3) . . ? C10 C11 C6 116.7(3) . . ? C10 C11 C15 120.2(3) . . ? C6 C11 C15 123.1(3) . . ? C7 C12 C14 113.0(2) . . ? C7 C12 C13 110.0(2) . . ? C14 C12 C13 109.5(3) . . ? C11 C15 C16 111.0(3) . . ? C11 C15 C17 112.4(3) . . ? C16 C15 C17 109.5(2) . . ? C23 C18 C19 122.6(3) . . ? C23 C18 N2 118.7(2) . . ? C19 C18 N2 117.8(3) . . ? C20 C19 C18 115.9(3) . . ? C20 C19 C24 121.0(3) . . ? C18 C19 C24 123.0(3) . . ? C21 C20 C19 122.9(3) . . ? C20 C21 C22 120.2(3) . . ? C21 C22 C23 120.5(3) . . ? C18 C23 C22 117.9(3) . . ? C18 C23 C27 121.4(3) . . ? C22 C23 C27 120.7(3) . . ? C19 C24 C26 111.7(2) . . ? C19 C24 C25 110.5(2) . . ? C26 C24 C25 110.6(2) . . ? C23 C27 C29 113.3(3) . . ? C23 C27 C28 111.1(2) . . ? C29 C27 C28 109.9(2) . . ? N3 C30 N4 105.54(18) . . ? N3 C30 Ru1 126.17(16) . . ? N4 C30 Ru1 127.73(16) . . ? N4 C31 C32 101.53(18) . . ? N3 C32 C31 101.59(19) . . ? C38 C33 C34 122.8(2) . . ? C38 C33 N4 119.6(2) . . ? C34 C33 N4 117.2(3) . . ? C35 C34 C33 116.0(3) . . ? C35 C34 C39 121.2(2) . . ? C33 C34 C39 122.7(2) . . ? C36 C35 C34 122.0(3) . . ? C35 C36 C37 120.9(3) . . ? C36 C37 C38 120.4(3) . . ? C33 C38 C37 117.9(2) . . ? C33 C38 C42 123.0(2) . . ? C37 C38 C42 119.1(3) . . ? C34 C39 C41 110.2(2) . . ? C34 C39 C40 112.7(2) . . ? C41 C39 C40 109.4(2) . . ? C38 C42 C43 112.0(2) . . ? C38 C42 C44 111.5(2) . . ? C43 C42 C44 109.6(3) . . ? C50 C45 C46 122.9(2) . . ? C50 C45 N3 119.1(2) . . ? C46 C45 N3 117.5(3) . . ? C47 C46 C45 116.7(3) . . ? C47 C46 C51 120.6(3) . . ? C45 C46 C51 122.7(2) . . ? C48 C47 C46 121.4(3) . . ? C47 C48 C49 120.7(2) . . ? C48 C49 C50 120.1(3) . . ? C45 C50 C49 118.0(3) . . ? C45 C50 C54 123.0(2) . . ? C49 C50 C54 118.9(3) . . ? C46 C51 C52 113.5(2) . . ? C46 C51 C53 111.8(3) . . ? C52 C51 C53 108.9(3) . . ? C55 C54 C50 111.4(2) . . ? C55 C54 C56 109.9(3) . . ? C50 C54 C56 111.1(2) . . ? O2A C2A Ru1 178.9(14) . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.660 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.077 data_c:\x-ray\kappa\k06mkw11\maxus\k06mkw11 _database_code_depnum_ccdc_archive 'CCDC 668491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H46 Cl N2 O2 P Ru' _chemical_formula_weight 838.35 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0670(1) _cell_length_b 13.8480(2) _cell_length_c 14.0060(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.407(1) _cell_angle_gamma 90.00 _cell_volume 2079.00(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30866 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Pale-yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44617 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11963 _reflns_number_gt 10641 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.2945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.027(13) _refine_ls_number_reflns 11963 _refine_ls_number_parameters 498 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.124075(12) 0.819010(9) 0.304399(9) 0.01761(4) Uani 1 1 d D . . Cl1 Cl -0.05621(5) 0.88900(4) 0.35168(4) 0.02550(11) Uani 1 1 d . . . P1 P 0.07709(5) 0.91940(3) 0.16449(3) 0.01785(10) Uani 1 1 d . . . O1 O 0.28984(17) 0.97698(12) 0.42982(12) 0.0409(4) Uani 1 1 d . . . O2 O 0.31757(18) 0.71318(14) 0.23075(13) 0.0478(5) Uani 1 1 d . . . N1 N 0.03863(16) 0.63930(12) 0.40537(12) 0.0231(4) Uani 1 1 d . . . N2 N 0.20684(16) 0.69631(12) 0.49927(11) 0.0224(4) Uani 1 1 d . . . C1 C 0.2312(2) 0.91541(15) 0.38892(14) 0.0245(4) Uani 1 1 d . . . C2 C 0.2470(2) 0.75516(16) 0.26096(15) 0.0290(5) Uani 1 1 d . . . C3 C 0.12383(18) 0.71210(14) 0.41042(13) 0.0201(4) Uani 1 1 d . . . C4 C 0.0693(2) 0.58067(16) 0.48893(16) 0.0312(5) Uani 1 1 d . . . H4 H 0.0242 0.5259 0.5020 0.037 Uiso 1 1 calc R . . C5 C 0.1745(2) 0.61638(15) 0.54727(16) 0.0310(5) Uani 1 1 d . . . H5 H 0.2185 0.5917 0.6095 0.037 Uiso 1 1 calc R . . C6 C -0.0756(2) 0.62677(14) 0.32979(15) 0.0233(4) Uani 1 1 d . . . C7 C -0.1861(2) 0.66172(16) 0.34775(16) 0.0278(4) Uani 1 1 d . . . C8 C -0.2952(2) 0.65172(17) 0.27334(18) 0.0321(5) Uani 1 1 d . . . H8 H -0.3710 0.6766 0.2836 0.039 Uiso 1 1 calc R . . C9 C -0.2966(2) 0.60651(16) 0.18450(17) 0.0319(5) Uani 1 1 d . . . C10 C -0.1863(2) 0.56809(15) 0.17158(16) 0.0302(5) Uani 1 1 d . . . H10 H -0.1870 0.5348 0.1121 0.036 Uiso 1 1 calc R . . C11 C -0.0739(2) 0.57688(14) 0.24344(15) 0.0264(4) Uani 1 1 d . . . C12 C -0.1904(2) 0.70596(18) 0.44480(17) 0.0367(5) Uani 1 1 d . . . H12A H -0.2001 0.6549 0.4908 0.055 Uiso 1 1 calc R . . H12B H -0.2612 0.7506 0.4349 0.055 Uiso 1 1 calc R . . H12C H -0.1127 0.7413 0.4720 0.055 Uiso 1 1 calc R . . C13 C -0.4175(3) 0.5963(2) 0.1063(2) 0.0490(7) Uani 1 1 d . . . H13A H -0.3997 0.5909 0.0414 0.073 Uiso 1 1 calc R . . H13B H -0.4698 0.6532 0.1075 0.073 Uiso 1 1 calc R . . H13C H -0.4615 0.5383 0.1193 0.073 Uiso 1 1 calc R . . C14 C 0.0442(2) 0.53309(19) 0.2283(2) 0.0387(6) Uani 1 1 d . . . H14A H 0.0979 0.5842 0.2134 0.058 Uiso 1 1 calc R . . H14B H 0.0237 0.4874 0.1732 0.058 Uiso 1 1 calc R . . H14C H 0.0879 0.4991 0.2884 0.058 Uiso 1 1 calc R . . C15 C 0.30973(19) 0.75860(15) 0.54534(14) 0.0226(4) Uani 1 1 d . . . C16 C 0.28722(19) 0.83125(18) 0.60745(13) 0.0278(5) Uani 1 1 d . . . C17 C 0.3860(2) 0.89061(16) 0.65277(16) 0.0315(5) Uani 1 1 d . . . H17 H 0.3722 0.9407 0.6952 0.038 Uiso 1 1 calc R . . C18 C 0.5042(2) 0.87870(16) 0.63769(16) 0.0314(5) Uani 1 1 d . . . C19 C 0.5233(2) 0.80424(18) 0.57688(15) 0.0311(5) Uani 1 1 d . . . H19 H 0.6043 0.7951 0.5669 0.037 Uiso 1 1 calc R . . C20 C 0.4274(2) 0.74230(15) 0.52990(14) 0.0264(4) Uani 1 1 d . . . C21 C 0.1588(2) 0.84729(18) 0.62336(18) 0.0402(6) Uani 1 1 d . . . H21A H 0.1594 0.9054 0.6634 0.060 Uiso 1 1 calc R . . H21B H 0.1350 0.7914 0.6575 0.060 Uiso 1 1 calc R . . H21C H 0.0986 0.8555 0.5595 0.060 Uiso 1 1 calc R . . C22 C 0.6109(3) 0.94424(19) 0.68746(19) 0.0454(7) Uani 1 1 d . . . H22A H 0.5778 1.0073 0.7002 0.068 Uiso 1 1 calc R . . H22B H 0.6677 0.9525 0.6444 0.068 Uiso 1 1 calc R . . H22C H 0.6562 0.9153 0.7500 0.068 Uiso 1 1 calc R . . C23 C 0.4530(2) 0.65963(19) 0.46819(17) 0.0378(6) Uani 1 1 d . . . H23A H 0.3863 0.6116 0.4607 0.057 Uiso 1 1 calc R . . H23B H 0.5331 0.6298 0.5005 0.057 Uiso 1 1 calc R . . H23C H 0.4565 0.6836 0.4031 0.057 Uiso 1 1 calc R . . C24 C -0.08493(18) 0.91656(14) 0.09058(14) 0.0210(4) Uani 1 1 d . . . C25 C -0.16435(19) 0.84124(14) 0.10006(15) 0.0250(5) Uani 1 1 d . . . H25 H -0.1364 0.7919 0.1475 0.030 Uiso 1 1 calc R . . C26 C -0.2853(2) 0.83868(15) 0.03942(15) 0.0287(5) Uani 1 1 d . . . H26 H -0.3396 0.7873 0.0461 0.034 Uiso 1 1 calc R . . C27 C -0.3272(2) 0.90947(17) -0.02986(16) 0.0302(5) Uani 1 1 d . . . H27 H -0.4092 0.9062 -0.0715 0.036 Uiso 1 1 calc R . . C28 C -0.2495(2) 0.98550(17) -0.03879(16) 0.0321(5) Uani 1 1 d . . . H28 H -0.2784 1.0351 -0.0858 0.039 Uiso 1 1 calc R . . C29 C -0.1289(2) 0.98888(16) 0.02151(15) 0.0283(5) Uani 1 1 d . . . H29 H -0.0757 1.0412 0.0155 0.034 Uiso 1 1 calc R . . C30 C 0.16595(19) 0.88804(14) 0.07477(14) 0.0206(4) Uani 1 1 d . . . C31 C 0.1127(2) 0.83808(15) -0.01131(14) 0.0287(5) Uani 1 1 d . . . H31 H 0.0260 0.8239 -0.0278 0.034 Uiso 1 1 calc R . . C32 C 0.1863(2) 0.8088(2) -0.07351(16) 0.0389(6) Uani 1 1 d . . . H32 H 0.1496 0.7744 -0.1323 0.047 Uiso 1 1 calc R . . C33 C 0.3121(2) 0.8292(2) -0.05037(16) 0.0389(5) Uani 1 1 d . . . H33 H 0.3617 0.8097 -0.0935 0.047 Uiso 1 1 calc R . . C34 C 0.3666(2) 0.87866(17) 0.03643(17) 0.0335(5) Uani 1 1 d . . . H34 H 0.4533 0.8926 0.0530 0.040 Uiso 1 1 calc R . . C35 C 0.29318(19) 0.90731(16) 0.09826(15) 0.0266(4) Uani 1 1 d . . . H35 H 0.3303 0.9406 0.1576 0.032 Uiso 1 1 calc R . . C36 C 0.10342(19) 1.04943(14) 0.18442(14) 0.0218(4) Uani 1 1 d . . . C37 C 0.0682(2) 1.09147(17) 0.26271(17) 0.0304(5) Uani 1 1 d . . . H37 H 0.0321 1.0527 0.3042 0.037 Uiso 1 1 calc R . . C38 C 0.0850(3) 1.18990(16) 0.28180(17) 0.0381(6) Uani 1 1 d . . . H38 H 0.0595 1.2179 0.3356 0.046 Uiso 1 1 calc R . . C39 C 0.1383(2) 1.24656(16) 0.22275(19) 0.0392(6) Uani 1 1 d . . . H39 H 0.1508 1.3136 0.2361 0.047 Uiso 1 1 calc R . . C40 C 0.1736(2) 1.20603(17) 0.14452(19) 0.0376(5) Uani 1 1 d . . . H40 H 0.2102 1.2453 0.1036 0.045 Uiso 1 1 calc R . . C41 C 0.1561(2) 1.10790(15) 0.12460(16) 0.0290(5) Uani 1 1 d . . . H41 H 0.1803 1.0806 0.0699 0.035 Uiso 1 1 calc R . . C42 C 0.4713(2) 1.0769(2) 0.2856(2) 0.0443(6) Uani 1 1 d . . . H42 H 0.4047 1.0986 0.3116 0.053 Uiso 1 1 calc R . . C43 C 0.5270(2) 0.9890(2) 0.3150(2) 0.0455(6) Uani 1 1 d . . . H43 H 0.4992 0.9503 0.3614 0.055 Uiso 1 1 calc R . . C44 C 0.6241(3) 0.9576(2) 0.2761(2) 0.0449(7) Uani 1 1 d . . . H44 H 0.6624 0.8969 0.2954 0.054 Uiso 1 1 calc R . . C45 C 0.6650(3) 1.0145(2) 0.2096(2) 0.0451(7) Uani 1 1 d . . . H45 H 0.7325 0.9937 0.1840 0.054 Uiso 1 1 calc R . . C46 C 0.6081(3) 1.1006(2) 0.1809(2) 0.0487(7) Uani 1 1 d . . . H46 H 0.6350 1.1392 0.1340 0.058 Uiso 1 1 calc R . . C47 C 0.5113(3) 1.1324(2) 0.2196(2) 0.0487(7) Uani 1 1 d . . . H47 H 0.4729 1.1930 0.1999 0.058 Uiso 1 1 calc R . . H1 H 0.0398(19) 0.7473(14) 0.2282(14) 0.024(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01809(7) 0.01930(6) 0.01541(6) 0.00184(7) 0.00410(5) 0.00062(7) Cl1 0.0258(3) 0.0267(2) 0.0260(2) 0.00044(19) 0.0101(2) 0.0017(2) P1 0.0173(2) 0.0206(2) 0.0157(2) 0.00122(18) 0.00433(18) -0.00027(19) O1 0.0475(11) 0.0342(9) 0.0333(9) 0.0019(7) -0.0044(8) -0.0152(8) O2 0.0523(12) 0.0528(11) 0.0446(10) 0.0154(9) 0.0240(9) 0.0269(9) N1 0.0259(10) 0.0224(8) 0.0197(8) 0.0034(7) 0.0032(7) -0.0025(7) N2 0.0246(9) 0.0229(8) 0.0176(8) 0.0039(6) 0.0010(7) -0.0006(7) C1 0.0240(11) 0.0291(10) 0.0198(9) 0.0068(8) 0.0042(8) -0.0005(9) C2 0.0330(13) 0.0310(11) 0.0229(10) 0.0109(9) 0.0066(9) 0.0038(10) C3 0.0225(10) 0.0198(9) 0.0180(9) 0.0010(7) 0.0048(8) 0.0005(8) C4 0.0388(13) 0.0268(11) 0.0263(11) 0.0087(9) 0.0047(10) -0.0069(9) C5 0.0393(14) 0.0270(11) 0.0236(10) 0.0084(9) 0.0020(9) 0.0002(9) C6 0.0247(11) 0.0219(9) 0.0220(10) 0.0029(8) 0.0035(8) -0.0052(8) C7 0.0298(12) 0.0273(10) 0.0276(11) 0.0012(9) 0.0099(9) -0.0062(9) C8 0.0239(12) 0.0304(11) 0.0426(13) 0.0042(10) 0.0091(10) -0.0051(9) C9 0.0293(13) 0.0268(11) 0.0344(13) 0.0051(10) -0.0015(10) -0.0098(10) C10 0.0358(13) 0.0250(10) 0.0273(11) -0.0022(8) 0.0033(10) -0.0087(9) C11 0.0288(12) 0.0207(10) 0.0287(11) 0.0018(8) 0.0054(9) -0.0036(8) C12 0.0395(14) 0.0406(13) 0.0352(12) -0.0019(10) 0.0191(10) -0.0068(11) C13 0.0383(16) 0.0443(15) 0.0539(16) 0.0025(13) -0.0082(13) -0.0124(12) C14 0.0379(15) 0.0341(13) 0.0446(15) -0.0111(11) 0.0110(12) 0.0018(11) C15 0.0221(10) 0.0251(10) 0.0175(9) 0.0026(8) -0.0008(8) -0.0004(8) C16 0.0289(10) 0.0338(13) 0.0188(8) 0.0020(9) 0.0022(7) 0.0078(10) C17 0.0417(14) 0.0249(10) 0.0235(10) -0.0026(9) 0.0000(9) 0.0052(10) C18 0.0352(13) 0.0286(11) 0.0240(11) 0.0057(9) -0.0043(9) -0.0033(9) C19 0.0231(10) 0.0399(16) 0.0284(10) 0.0035(10) 0.0028(8) -0.0002(10) C20 0.0276(12) 0.0300(11) 0.0193(9) 0.0014(8) 0.0016(8) 0.0038(9) C21 0.0383(14) 0.0478(16) 0.0353(12) -0.0060(10) 0.0108(10) 0.0084(10) C22 0.0472(16) 0.0397(13) 0.0392(14) 0.0031(11) -0.0082(12) -0.0113(12) C23 0.0318(13) 0.0477(14) 0.0330(12) -0.0081(11) 0.0063(10) 0.0071(11) C24 0.0178(10) 0.0273(10) 0.0180(9) -0.0001(8) 0.0044(7) 0.0015(8) C25 0.0218(10) 0.0269(12) 0.0255(9) 0.0010(8) 0.0044(8) 0.0011(7) C26 0.0214(10) 0.0311(14) 0.0325(10) -0.0014(9) 0.0046(8) -0.0030(8) C27 0.0180(10) 0.0431(13) 0.0280(11) -0.0036(10) 0.0031(8) 0.0033(9) C28 0.0251(12) 0.0422(13) 0.0275(11) 0.0104(10) 0.0038(9) 0.0062(10) C29 0.0219(11) 0.0365(12) 0.0255(10) 0.0080(9) 0.0038(9) -0.0002(9) C30 0.0221(10) 0.0232(9) 0.0175(9) 0.0017(7) 0.0070(7) 0.0003(8) C31 0.0247(10) 0.0365(15) 0.0245(9) -0.0053(8) 0.0055(8) -0.0024(9) C32 0.0414(13) 0.0483(16) 0.0292(10) -0.0147(12) 0.0131(9) -0.0024(13) C33 0.0391(12) 0.0461(15) 0.0394(11) -0.0070(13) 0.0248(10) 0.0022(13) C34 0.0232(12) 0.0419(13) 0.0391(13) 0.0002(10) 0.0147(10) -0.0004(10) C35 0.0223(11) 0.0337(11) 0.0236(10) -0.0011(9) 0.0055(8) -0.0022(9) C36 0.0222(10) 0.0217(9) 0.0192(9) 0.0038(7) 0.0012(8) 0.0014(8) C37 0.0424(15) 0.0246(11) 0.0260(12) 0.0016(9) 0.0117(11) 0.0016(10) C38 0.0532(16) 0.0281(12) 0.0313(12) -0.0041(9) 0.0073(11) 0.0071(11) C39 0.0422(15) 0.0200(10) 0.0485(14) 0.0018(10) -0.0017(11) -0.0001(10) C40 0.0366(14) 0.0269(11) 0.0494(14) 0.0120(10) 0.0110(11) -0.0018(10) C41 0.0302(13) 0.0291(11) 0.0294(11) 0.0057(9) 0.0105(9) 0.0006(9) C42 0.0294(14) 0.0544(16) 0.0466(15) -0.0202(13) 0.0047(11) -0.0023(12) C43 0.0304(14) 0.0561(17) 0.0458(15) -0.0033(13) 0.0015(12) -0.0088(12) C44 0.0305(15) 0.0430(14) 0.0533(16) -0.0109(13) -0.0046(12) 0.0022(11) C45 0.0386(16) 0.0561(17) 0.0384(15) -0.0196(13) 0.0054(12) 0.0038(13) C46 0.0462(17) 0.0545(17) 0.0447(15) -0.0038(13) 0.0103(13) 0.0017(13) C47 0.0433(17) 0.0405(15) 0.0586(17) -0.0094(13) 0.0055(13) 0.0055(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.581(15) . ? Ru1 C2 1.848(2) . ? Ru1 C1 1.973(2) . ? Ru1 C3 2.0974(19) . ? Ru1 P1 2.3529(5) . ? Ru1 Cl1 2.4528(5) . ? P1 C30 1.830(2) . ? P1 C24 1.834(2) . ? P1 C36 1.834(2) . ? O1 C1 1.136(3) . ? O2 C2 1.136(3) . ? N1 C3 1.370(3) . ? N1 C4 1.395(3) . ? N1 C6 1.443(3) . ? N2 C3 1.368(2) . ? N2 C5 1.387(3) . ? N2 C15 1.446(3) . ? C4 C5 1.340(3) . ? C6 C7 1.395(3) . ? C6 C11 1.397(3) . ? C7 C8 1.392(3) . ? C7 C12 1.502(3) . ? C8 C9 1.390(3) . ? C9 C10 1.384(4) . ? C9 C13 1.510(3) . ? C10 C11 1.397(3) . ? C11 C14 1.502(3) . ? C15 C20 1.390(3) . ? C15 C16 1.392(3) . ? C16 C17 1.389(3) . ? C16 C21 1.509(3) . ? C17 C18 1.386(3) . ? C18 C19 1.387(3) . ? C18 C22 1.515(3) . ? C19 C20 1.396(3) . ? C20 C23 1.504(3) . ? C24 C25 1.391(3) . ? C24 C29 1.393(3) . ? C25 C26 1.396(3) . ? C26 C27 1.376(3) . ? C27 C28 1.384(3) . ? C28 C29 1.392(3) . ? C30 C31 1.388(3) . ? C30 C35 1.390(3) . ? C31 C32 1.393(3) . ? C32 C33 1.378(3) . ? C33 C34 1.395(3) . ? C34 C35 1.384(3) . ? C36 C37 1.380(3) . ? C36 C41 1.393(3) . ? C37 C38 1.392(3) . ? C38 C39 1.375(4) . ? C39 C40 1.371(4) . ? C40 C41 1.391(3) . ? C42 C47 1.358(4) . ? C42 C43 1.380(4) . ? C43 C44 1.390(4) . ? C44 C45 1.379(4) . ? C45 C46 1.362(4) . ? C46 C47 1.388(4) . ? 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 H1 Ru1 C2 80.6(8) . . ? H1 Ru1 C1 174.7(8) . . ? C2 Ru1 C1 98.02(10) . . ? H1 Ru1 C3 86.0(8) . . ? C2 Ru1 C3 91.49(8) . . ? C1 Ru1 C3 99.17(8) . . ? H1 Ru1 P1 80.7(8) . . ? C2 Ru1 P1 92.11(6) . . ? C1 Ru1 P1 94.31(6) . . ? C3 Ru1 P1 165.42(5) . . ? H1 Ru1 Cl1 92.7(8) . . ? C2 Ru1 Cl1 173.18(7) . . ? C1 Ru1 Cl1 88.77(6) . . ? C3 Ru1 Cl1 86.75(6) . . ? P1 Ru1 Cl1 88.014(17) . . ? C30 P1 C24 102.96(9) . . ? C30 P1 C36 104.20(9) . . ? C24 P1 C36 101.71(9) . . ? C30 P1 Ru1 112.74(6) . . ? C24 P1 Ru1 116.09(6) . . ? C36 P1 Ru1 117.35(6) . . ? C3 N1 C4 111.37(17) . . ? C3 N1 C6 126.32(16) . . ? C4 N1 C6 122.09(17) . . ? C3 N2 C5 111.87(17) . . ? C3 N2 C15 125.91(16) . . ? C5 N2 C15 121.94(16) . . ? O1 C1 Ru1 173.19(17) . . ? O2 C2 Ru1 176.2(2) . . ? N2 C3 N1 103.13(16) . . ? N2 C3 Ru1 129.64(14) . . ? N1 C3 Ru1 127.22(13) . . ? C5 C4 N1 106.85(18) . . ? C4 C5 N2 106.78(18) . . ? C7 C6 C11 121.92(19) . . ? C7 C6 N1 118.23(18) . . ? C11 C6 N1 119.78(19) . . ? C8 C7 C6 117.8(2) . . ? C8 C7 C12 120.1(2) . . ? C6 C7 C12 122.1(2) . . ? C9 C8 C7 122.0(2) . . ? C10 C9 C8 118.5(2) . . ? C10 C9 C13 121.4(2) . . ? C8 C9 C13 120.1(2) . . ? C9 C10 C11 121.9(2) . . ? C6 C11 C10 117.7(2) . . ? C6 C11 C14 121.4(2) . . ? C10 C11 C14 120.8(2) . . ? C20 C15 C16 122.32(19) . . ? C20 C15 N2 119.84(18) . . ? C16 C15 N2 117.80(19) . . ? C17 C16 C15 118.1(2) . . ? C17 C16 C21 120.6(2) . . ? C15 C16 C21 121.3(2) . . ? C18 C17 C16 121.7(2) . . ? C17 C18 C19 118.4(2) . . ? C17 C18 C22 121.1(2) . . ? C19 C18 C22 120.5(2) . . ? C18 C19 C20 122.2(2) . . ? C15 C20 C19 117.30(19) . . ? C15 C20 C23 122.1(2) . . ? C19 C20 C23 120.6(2) . . ? C25 C24 C29 119.04(18) . . ? C25 C24 P1 120.95(15) . . ? C29 C24 P1 119.98(15) . . ? C24 C25 C26 119.60(18) . . ? C27 C26 C25 120.9(2) . . ? C26 C27 C28 119.9(2) . . ? C27 C28 C29 119.6(2) . . ? C28 C29 C24 120.9(2) . . ? C31 C30 C35 119.19(18) . . ? C31 C30 P1 122.01(15) . . ? C35 C30 P1 118.53(15) . . ? C30 C31 C32 120.0(2) . . ? C33 C32 C31 120.5(2) . . ? C32 C33 C34 119.9(2) . . ? C35 C34 C33 119.5(2) . . ? C34 C35 C30 120.95(19) . . ? C37 C36 C41 118.40(19) . . ? C37 C36 P1 118.00(16) . . ? C41 C36 P1 123.61(16) . . ? C36 C37 C38 121.0(2) . . ? C39 C38 C37 120.0(2) . . ? C40 C39 C38 119.8(2) . . ? C39 C40 C41 120.5(2) . . ? C40 C41 C36 120.3(2) . . ? C47 C42 C43 120.4(3) . . ? C42 C43 C44 119.4(3) . . ? C45 C44 C43 120.1(3) . . ? C46 C45 C44 119.7(3) . . ? C45 C46 C47 120.5(3) . . ? C42 C47 C46 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.849 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.059 data_c:\x-ray\helix\h07mkw3\maxus\h07mkw3 _database_code_depnum_ccdc_archive 'CCDC 668492' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H92 B N4 O Ru' _chemical_formula_weight 1021.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P22121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6630(2) _cell_length_b 13.0470(3) _cell_length_c 20.8400(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2899.26(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 73998 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 0.312 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15736 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6524 _reflns_number_gt 5389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.2231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 6524 _refine_ls_number_parameters 336 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.39977(2) 0.0000 0.0000 0.02783(10) Uani 1 2 d SD . . O1 O 0.1294(7) 0.0525(6) -0.0095(5) 0.057(2) Uiso 0.30 1 d PD . 1 N1 N 0.4311(2) -0.04186(18) 0.14733(12) 0.0327(5) Uani 1 1 d . . . N2 N 0.3668(2) 0.11071(18) 0.13194(12) 0.0325(5) Uani 1 1 d . . . C1 C 0.2347(9) 0.0397(7) -0.0043(10) 0.042(2) Uiso 0.30 1 d PD . 1 C2 C 0.3991(2) 0.02407(17) 0.09898(13) 0.0289(6) Uani 1 1 d . . . C3 C 0.4192(3) 0.0027(3) 0.20701(14) 0.0528(8) Uani 1 1 d . . . H3 H 0.4356 -0.0287 0.2473 0.063 Uiso 1 1 calc R . . C4 C 0.3796(4) 0.0996(3) 0.19702(16) 0.0529(9) Uani 1 1 d . . . H4 H 0.3638 0.1502 0.2288 0.064 Uiso 1 1 calc R . . C5 C 0.4711(3) -0.1474(2) 0.14236(14) 0.0340(6) Uani 1 1 d . . . C6 C 0.6002(3) -0.1698(2) 0.14970(15) 0.0386(6) Uani 1 1 d . . . C7 C 0.6335(4) -0.2733(3) 0.14743(19) 0.0435(10) Uani 1 1 d . . . H7 H 0.7192 -0.2919 0.1517 0.052 Uiso 1 1 calc R . . C8 C 0.5454(3) -0.3489(2) 0.13925(17) 0.0474(8) Uani 1 1 d . . . H8 H 0.5710 -0.4186 0.1381 0.057 Uiso 1 1 calc R . . C9 C 0.4216(3) -0.3251(2) 0.13282(17) 0.0449(8) Uani 1 1 d . . . H9 H 0.3618 -0.3784 0.1275 0.054 Uiso 1 1 calc R . . C10 C 0.3817(3) -0.2233(2) 0.13404(15) 0.0369(7) Uani 1 1 d . . . C11 C 0.6988(3) -0.0882(3) 0.1616(2) 0.0562(10) Uani 1 1 d . . . H11 H 0.6642 -0.0210 0.1468 0.067 Uiso 1 1 calc R . . C12 C 0.7257(5) -0.0801(4) 0.2344(3) 0.1012(19) Uani 1 1 d . . . H12A H 0.6495 -0.0579 0.2568 0.152 Uiso 1 1 calc R . . H12B H 0.7927 -0.0300 0.2417 0.152 Uiso 1 1 calc R . . H12C H 0.7518 -0.1472 0.2508 0.152 Uiso 1 1 calc R . . C13 C 0.8186(3) -0.1096(4) 0.1236(3) 0.096(2) Uani 1 1 d . . . H13A H 0.8572 -0.1730 0.1393 0.144 Uiso 1 1 calc R . . H13B H 0.8773 -0.0525 0.1292 0.144 Uiso 1 1 calc R . . H13C H 0.7981 -0.1170 0.0780 0.144 Uiso 1 1 calc R . . C14 C 0.2417(3) -0.1978(3) 0.13097(18) 0.0480(8) Uani 1 1 d . . . H14 H 0.2338 -0.1250 0.1165 0.058 Uiso 1 1 calc R . . C15 C 0.1830(4) -0.2053(6) 0.1969(3) 0.115(2) Uani 1 1 d . . . H15A H 0.2105 -0.2688 0.2177 0.173 Uiso 1 1 calc R . . H15B H 0.0914 -0.2056 0.1928 0.173 Uiso 1 1 calc R . . H15C H 0.2091 -0.1465 0.2229 0.173 Uiso 1 1 calc R . . C16 C 0.1723(4) -0.2640(4) 0.0829(3) 0.0813(16) Uani 1 1 d . . . H16A H 0.2240 -0.2727 0.0444 0.122 Uiso 1 1 calc R . . H16B H 0.0930 -0.2310 0.0713 0.122 Uiso 1 1 calc R . . H16C H 0.1552 -0.3312 0.1019 0.122 Uiso 1 1 calc R . . C17 C 0.3303(3) 0.2099(2) 0.10637(16) 0.0350(7) Uani 1 1 d . . . C18 C 0.4258(3) 0.2770(2) 0.08851(16) 0.0376(7) Uani 1 1 d . . . C19 C 0.3909(3) 0.3772(2) 0.07044(17) 0.0474(8) Uani 1 1 d . . . H19 H 0.4534 0.4253 0.0581 0.057 Uiso 1 1 calc R . . C20 C 0.2660(4) 0.4055(2) 0.0706(2) 0.0563(10) Uani 1 1 d . . . H20 H 0.2429 0.4730 0.0583 0.068 Uiso 1 1 calc R . . C21 C 0.1756(3) 0.3371(2) 0.0885(2) 0.0520(9) Uani 1 1 d . . . H21 H 0.0904 0.3585 0.0885 0.062 Uiso 1 1 calc R . . C22 C 0.2042(3) 0.2363(2) 0.10671(19) 0.0435(8) Uani 1 1 d . . . C23 C 0.5638(3) 0.2481(3) 0.09087(17) 0.0432(8) Uani 1 1 d . . . H23 H 0.5694 0.1717 0.0936 0.052 Uiso 1 1 calc R . . C24 C 0.6351(3) 0.2823(3) 0.0308(2) 0.0601(10) Uani 1 1 d . . . H24A H 0.5926 0.2560 -0.0075 0.090 Uiso 1 1 calc R . . H24B H 0.7210 0.2556 0.0323 0.090 Uiso 1 1 calc R . . H24C H 0.6375 0.3574 0.0291 0.090 Uiso 1 1 calc R . . C25 C 0.6242(5) 0.2927(4) 0.1513(2) 0.0680(14) Uani 1 1 d . . . H25A H 0.6279 0.3675 0.1477 0.102 Uiso 1 1 calc R . . H25B H 0.7092 0.2653 0.1560 0.102 Uiso 1 1 calc R . . H25C H 0.5740 0.2738 0.1889 0.102 Uiso 1 1 calc R . . C26 C 0.1001(3) 0.1644(3) 0.1260(2) 0.0592(10) Uani 1 1 d . . . H26 H 0.1342 0.0931 0.1244 0.071 Uiso 1 1 calc R . . C27 C 0.0628(6) 0.1866(5) 0.1959(4) 0.128(3) Uani 1 1 d . . . H27A H 0.1307 0.1651 0.2246 0.191 Uiso 1 1 calc R . . H27B H -0.0137 0.1486 0.2064 0.191 Uiso 1 1 calc R . . H27C H 0.0477 0.2602 0.2011 0.191 Uiso 1 1 calc R . . C28 C -0.0130(4) 0.1696(4) 0.0794(4) 0.111(3) Uani 1 1 d . . . H28A H -0.0483 0.2389 0.0798 0.167 Uiso 1 1 calc R . . H28B H -0.0772 0.1204 0.0931 0.167 Uiso 1 1 calc R . . H28C H 0.0150 0.1527 0.0359 0.167 Uiso 1 1 calc R . . C29 C 0.9132(5) 0.5000 0.0000 0.094(2) Uani 1 2 d SD . . C30 C 0.8574(4) 0.5134(8) 0.0587(3) 0.126(3) Uani 1 1 d . . . H30A H 0.8059 0.4512 0.0656 0.151 Uiso 1 1 calc R . . H30B H 0.7973 0.5704 0.0527 0.151 Uiso 1 1 calc R . . C31 C 0.9159(7) 0.5324(6) 0.1179(5) 0.133(3) Uani 1 1 d . . . H31A H 1.0021 0.5055 0.1126 0.160 Uiso 1 1 calc R . . H31B H 0.9246 0.6079 0.1197 0.160 Uiso 1 1 calc R . . C32 C 0.8867(7) 0.5082(7) 0.1709(6) 0.179(5) Uani 1 1 d . . . H32A H 0.9483 0.5351 0.2015 0.268 Uiso 1 1 calc R . . H32B H 0.8840 0.4333 0.1740 0.268 Uiso 1 1 calc R . . H32C H 0.8037 0.5364 0.1809 0.268 Uiso 1 1 calc R . . B1 B 0.6058(8) -0.0236(6) 0.0024(14) 0.031(2) Uiso 0.30 1 d PD . 1 O1A O 0.6731(7) 0.0419(8) 0.0004(13) 0.058(3) Uiso 0.20 1 d PD . 2 C1A C 0.5662(9) 0.0371(11) -0.001(2) 0.043(4) Uiso 0.20 1 d PD . 2 B1A B 0.1931(8) 0.0191(9) 0.000(2) 0.025(3) Uiso 0.20 1 d PD . 2 H29A H 0.9691(7) 0.4405(19) 0.007(6) 0.13(4) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03115(15) 0.02252(14) 0.02981(15) 0.00131(17) 0.000 0.000 N1 0.0387(13) 0.0281(10) 0.0313(13) 0.0032(10) 0.0043(10) 0.0081(10) N2 0.0386(13) 0.0257(11) 0.0331(13) 0.0007(10) 0.0039(10) 0.0076(10) C2 0.0257(11) 0.0242(14) 0.0368(14) 0.0005(9) 0.0015(11) -0.0003(10) C3 0.085(2) 0.0441(15) 0.0294(13) -0.0004(19) 0.0071(13) 0.021(3) C4 0.088(3) 0.0426(17) 0.0284(16) -0.0031(13) 0.0059(17) 0.0231(18) C5 0.0451(17) 0.0259(13) 0.0311(15) 0.0029(12) 0.0064(13) 0.0046(12) C6 0.0401(15) 0.0343(14) 0.0415(17) 0.0071(12) 0.0034(14) 0.0047(14) C7 0.045(2) 0.0408(17) 0.045(2) 0.0073(15) 0.0014(16) 0.0153(15) C8 0.068(2) 0.0270(14) 0.047(2) 0.0031(14) 0.0001(17) 0.0120(15) C9 0.059(2) 0.0293(14) 0.0463(19) 0.0066(13) 0.0003(16) -0.0048(14) C10 0.0414(17) 0.0373(15) 0.0321(16) 0.0049(12) 0.0018(14) 0.0013(14) C11 0.0473(18) 0.0412(18) 0.080(3) 0.0107(18) -0.0094(19) -0.0005(16) C12 0.096(4) 0.091(4) 0.117(5) 0.000(3) -0.040(3) -0.041(3) C13 0.038(2) 0.071(3) 0.177(6) 0.045(3) 0.018(3) 0.007(2) C14 0.0417(19) 0.057(2) 0.045(2) 0.0146(17) -0.0004(16) -0.0023(16) C15 0.051(3) 0.222(7) 0.074(4) 0.057(4) 0.020(2) 0.023(4) C16 0.060(3) 0.061(3) 0.123(5) 0.003(3) -0.036(3) -0.012(2) C17 0.0432(17) 0.0242(13) 0.0376(17) -0.0019(12) 0.0000(14) 0.0062(12) C18 0.0404(17) 0.0326(15) 0.0399(17) -0.0005(13) -0.0042(13) -0.0018(12) C19 0.0557(19) 0.0315(14) 0.055(2) 0.0058(14) -0.0097(17) -0.0124(15) C20 0.064(2) 0.0268(16) 0.078(3) 0.0052(17) -0.014(2) 0.0078(16) C21 0.0442(19) 0.0291(16) 0.083(3) -0.0013(16) -0.0086(18) 0.0122(14) C22 0.0381(18) 0.0320(17) 0.061(2) -0.0050(16) 0.0009(17) 0.0033(14) C23 0.0381(16) 0.0507(19) 0.0408(19) -0.0053(15) -0.0012(13) -0.0055(14) C24 0.053(2) 0.068(2) 0.060(2) -0.001(2) 0.0057(18) -0.0169(18) C25 0.052(3) 0.095(3) 0.057(3) -0.019(2) -0.005(2) -0.013(2) C26 0.0410(18) 0.0386(17) 0.098(3) 0.0036(18) 0.010(2) 0.0019(16) C27 0.115(4) 0.115(5) 0.153(6) -0.026(4) 0.087(4) -0.045(4) C28 0.053(3) 0.051(3) 0.230(8) 0.024(4) -0.032(3) -0.008(2) C29 0.037(3) 0.099(5) 0.145(7) -0.044(7) 0.000 0.000 C30 0.048(2) 0.228(9) 0.103(4) 0.070(6) -0.021(2) -0.041(4) C31 0.115(5) 0.098(4) 0.186(8) -0.074(5) -0.049(6) 0.065(4) C32 0.157(8) 0.173(9) 0.206(11) -0.019(8) 0.042(7) -0.082(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.837(9) 3 ? Ru1 C1 1.837(9) . ? Ru1 C1A 1.840(9) 3 ? Ru1 C1A 1.840(9) . ? Ru1 C2 2.086(3) . ? Ru1 C2 2.086(3) 3 ? Ru1 B1A 2.218(9) 3 ? Ru1 B1A 2.218(9) . ? Ru1 B1 2.219(8) 3 ? Ru1 B1 2.219(8) . ? O1 C1 1.140(11) . ? O1 O1 1.426(16) 3 ? O1 C1 1.671(11) 3 ? N1 C2 1.368(3) . ? N1 C3 1.379(4) . ? N1 C5 1.445(3) . ? N2 C2 1.367(3) . ? N2 C4 1.371(4) . ? N2 C17 1.452(4) . ? C1 C1 1.05(2) 3 ? C1 O1 1.671(11) 3 ? C3 C4 1.349(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C10 1.386(4) . ? C5 C6 1.416(4) . ? C6 C7 1.397(4) . ? C6 C11 1.516(5) . ? C7 C8 1.372(5) . ? C7 H7 0.9500 . ? C8 C9 1.363(5) . ? C8 H8 0.9500 . ? C9 C10 1.395(4) . ? C9 H9 0.9500 . ? C10 C14 1.531(5) . ? C11 C13 1.528(6) . ? C11 C12 1.548(7) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.513(6) . ? C14 C16 1.516(6) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.387(5) . ? C17 C18 1.394(4) . ? C18 C19 1.410(4) . ? C18 C23 1.520(4) . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 C21 1.365(5) . ? C20 H20 0.9500 . ? C21 C22 1.402(4) . ? C21 H21 0.9500 . ? C22 C26 1.508(5) . ? C23 C25 1.529(5) . ? C23 C24 1.532(5) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.536(7) . ? C26 C28 1.550(6) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.371(6) 3_565 ? C29 C30 1.371(6) . ? C29 H29A 0.990(3) . ? C30 C31 1.404(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.192(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? B1 B1 0.623(18) 3 ? O1A O1A 1.09(2) 3 ? O1A C1A 1.141(11) . ? O1A C1A 1.536(14) 3 ? C1A C1A 0.97(3) 3 ? C1A O1A 1.536(14) 3 ? B1A B1A 0.50(2) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C1 33.3(6) 3 . ? C1 Ru1 C1A 148.1(6) 3 3 ? C1 Ru1 C1A 177.6(17) . 3 ? C1 Ru1 C1A 177.6(17) 3 . ? C1 Ru1 C1A 148.1(6) . . ? C1A Ru1 C1A 30.5(9) 3 . ? C1 Ru1 C2 89.5(6) 3 . ? C1 Ru1 C2 90.1(6) . . ? C1A Ru1 C2 91.8(15) 3 . ? C1A Ru1 C2 88.6(15) . . ? C1 Ru1 C2 90.1(6) 3 3 ? C1 Ru1 C2 89.5(6) . 3 ? C1A Ru1 C2 88.6(15) 3 3 ? C1A Ru1 C2 91.8(15) . 3 ? C2 Ru1 C2 179.58(14) . 3 ? C1 Ru1 B1A 10.4(6) 3 3 ? C1 Ru1 B1A 23.0(4) . 3 ? C1A Ru1 B1A 158.3(6) 3 3 ? C1A Ru1 B1A 171.2(5) . 3 ? C2 Ru1 B1A 91.0(11) . 3 ? C2 Ru1 B1A 88.6(11) 3 3 ? C1 Ru1 B1A 23.0(4) 3 . ? C1 Ru1 B1A 10.4(6) . . ? C1A Ru1 B1A 171.2(5) 3 . ? C1A Ru1 B1A 158.3(6) . . ? C2 Ru1 B1A 88.6(11) . . ? C2 Ru1 B1A 91.0(11) 3 . ? B1A Ru1 B1A 12.9(6) 3 . ? C1 Ru1 B1 171.4(4) 3 3 ? C1 Ru1 B1 155.3(4) . 3 ? C1A Ru1 B1 23.3(5) 3 3 ? C1A Ru1 B1 7.3(6) . 3 ? C2 Ru1 B1 90.3(7) . 3 ? C2 Ru1 B1 90.1(7) 3 3 ? B1A Ru1 B1 177.9(12) 3 3 ? B1A Ru1 B1 165.5(4) . 3 ? C1 Ru1 B1 155.3(4) 3 . ? C1 Ru1 B1 171.4(4) . . ? C1A Ru1 B1 7.3(6) 3 . ? C1A Ru1 B1 23.3(5) . . ? C2 Ru1 B1 90.1(7) . . ? C2 Ru1 B1 90.3(7) 3 . ? B1A Ru1 B1 165.5(4) 3 . ? B1A Ru1 B1 177.9(12) . . ? B1 Ru1 B1 16.1(5) 3 . ? C1 O1 O1 80.4(7) . 3 ? C1 O1 C1 38.5(8) . 3 ? O1 O1 C1 42.3(4) 3 3 ? C2 N1 C3 112.1(2) . . ? C2 N1 C5 128.3(2) . . ? C3 N1 C5 119.6(3) . . ? C2 N2 C4 112.6(2) . . ? C2 N2 C17 128.3(3) . . ? C4 N2 C17 118.9(3) . . ? C1 C1 O1 99.2(7) 3 . ? C1 C1 O1 42.3(4) 3 3 ? O1 C1 O1 57.3(8) . 3 ? C1 C1 Ru1 73.4(3) 3 . ? O1 C1 Ru1 171.6(10) . . ? O1 C1 Ru1 115.6(6) 3 . ? N2 C2 N1 102.3(2) . . ? N2 C2 Ru1 128.48(19) . . ? N1 C2 Ru1 129.23(18) . . ? C4 C3 N1 106.6(3) . . ? C4 C3 H3 126.7 . . ? N1 C3 H3 126.7 . . ? C3 C4 N2 106.4(3) . . ? C3 C4 H4 126.8 . . ? N2 C4 H4 126.8 . . ? C10 C5 C6 122.4(3) . . ? C10 C5 N1 119.1(3) . . ? C6 C5 N1 118.4(3) . . ? C7 C6 C5 116.3(3) . . ? C7 C6 C11 120.6(3) . . ? C5 C6 C11 123.1(3) . . ? C8 C7 C6 121.7(3) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.7(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C5 C10 C9 118.2(3) . . ? C5 C10 C14 121.4(3) . . ? C9 C10 C14 120.2(3) . . ? C6 C11 C13 111.5(3) . . ? C6 C11 C12 109.6(3) . . ? C13 C11 C12 111.4(4) . . ? C6 C11 H11 108.0 . . ? C13 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 111.2(4) . . ? C15 C14 C10 110.5(3) . . ? C16 C14 C10 112.3(4) . . ? C15 C14 H14 107.5 . . ? C16 C14 H14 107.5 . . ? C10 C14 H14 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 123.6(3) . . ? C22 C17 N2 118.6(3) . . ? C18 C17 N2 117.5(3) . . ? C17 C18 C19 117.5(3) . . ? C17 C18 C23 122.9(3) . . ? C19 C18 C23 119.6(3) . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 122.2(3) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C17 C22 C21 116.3(3) . . ? C17 C22 C26 124.0(3) . . ? C21 C22 C26 119.7(3) . . ? C18 C23 C25 109.9(3) . . ? C18 C23 C24 112.5(3) . . ? C25 C23 C24 110.7(3) . . ? C18 C23 H23 107.9 . . ? C25 C23 H23 107.9 . . ? C24 C23 H23 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C27 109.1(4) . . ? C22 C26 C28 112.2(4) . . ? C27 C26 C28 112.6(4) . . ? C22 C26 H26 107.6 . . ? C27 C26 H26 107.6 . . ? C28 C26 H26 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C30 128.6(5) 3_565 . ? C30 C29 H29A 107(7) 3_565 . ? C30 C29 H29A 103(7) . . ? C29 C30 C31 127.8(5) . . ? C29 C30 H30A 105.4 . . ? C31 C30 H30A 105.4 . . ? C29 C30 H30B 105.4 . . ? C31 C30 H30B 105.4 . . ? H30A C30 H30B 106.0 . . ? C32 C31 C30 130.7(10) . . ? C32 C31 H31A 104.6 . . ? C30 C31 H31A 104.6 . . ? C32 C31 H31B 104.6 . . ? C30 C31 H31B 104.6 . . ? H31A C31 H31B 105.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? B1 B1 Ru1 81.9(2) 3 . ? O1A O1A C1A 86.8(9) 3 . ? O1A O1A C1A 47.9(6) 3 3 ? C1A O1A C1A 39.0(12) . 3 ? C1A C1A O1A 93.1(9) 3 . ? C1A C1A O1A 47.9(6) 3 3 ? O1A C1A O1A 45.3(9) . 3 ? C1A C1A Ru1 74.7(5) 3 . ? O1A C1A Ru1 167.7(15) . . ? O1A C1A Ru1 122.6(9) 3 . ? B1A B1A Ru1 83.5(3) 3 . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.488 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.061 data_c:\x-ray\kappa\k07mkw10\maxus\k07mkw10 _database_code_depnum_ccdc_archive 'CCDC 668493' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40.90 Cl0.10 N2 O2 P Ru' _chemical_formula_weight 729.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.1750(2) _cell_length_b 14.0430(2) _cell_length_c 17.2770(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.837(1) _cell_angle_gamma 90.00 _cell_volume 3616.11(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40485 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1510 _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68346 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10509 _reflns_number_gt 8530 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+2.4461P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10509 _refine_ls_number_parameters 438 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.193906(8) 0.074056(9) 0.257614(8) 0.01949(5) Uani 1 1 d D . . P1 P 0.09822(3) -0.05576(3) 0.23051(3) 0.01990(9) Uani 1 1 d . A . O1 O 0.10767(9) 0.13534(11) 0.39619(8) 0.0340(3) Uani 1 1 d . . . O2 O 0.08851(11) 0.22298(11) 0.14857(9) 0.0415(3) Uani 1 1 d . . . N1 N 0.34058(10) 0.22366(11) 0.32937(10) 0.0283(3) Uani 1 1 d . . . N2 N 0.38930(10) 0.13318(11) 0.24682(9) 0.0251(3) Uani 1 1 d . . . C1 C 0.14491(11) 0.11474(13) 0.34685(10) 0.0231(3) Uani 1 1 d . A . C2 C 0.12741(12) 0.16748(13) 0.18796(10) 0.0246(3) Uani 1 1 d . A . C3 C 0.31418(11) 0.15020(12) 0.27827(10) 0.0225(3) Uani 1 1 d . A . C4 C 0.42878(13) 0.25068(16) 0.32980(13) 0.0370(5) Uani 1 1 d . A . H4 H 0.4612 0.2997 0.3607 0.044 Uiso 1 1 calc R . . C5 C 0.45898(13) 0.19416(15) 0.27831(13) 0.0336(4) Uani 1 1 d . A . H5 H 0.5172 0.1954 0.2656 0.040 Uiso 1 1 calc R . . C6 C 0.28499(12) 0.27233(14) 0.37574(12) 0.0291(4) Uani 1 1 d . A . C7 C 0.23338(14) 0.34916(14) 0.34248(13) 0.0355(4) Uani 1 1 d . . . C8 C 0.17871(16) 0.39288(16) 0.38874(16) 0.0451(6) Uani 1 1 d . A . H8 H 0.1417 0.4446 0.3673 0.054 Uiso 1 1 calc R . . C9 C 0.17682(16) 0.36311(17) 0.46499(15) 0.0450(6) Uani 1 1 d . . . C10 C 0.23263(15) 0.29029(17) 0.49690(14) 0.0422(5) Uani 1 1 d . A . H10 H 0.2339 0.2720 0.5500 0.051 Uiso 1 1 calc R . . C11 C 0.28715(14) 0.24288(15) 0.45333(12) 0.0346(4) Uiso 1 1 d . . . C12 C 0.23763(19) 0.38481(17) 0.26100(15) 0.0493(6) Uani 1 1 d . A . H12A H 0.2873 0.4301 0.2640 0.074 Uiso 1 1 calc R . . H12B H 0.1811 0.4165 0.2385 0.074 Uiso 1 1 calc R . . H12C H 0.2473 0.3310 0.2275 0.074 Uiso 1 1 calc R . . C13 C 0.1139(2) 0.4084(2) 0.5131(2) 0.0664(9) Uani 1 1 d . A . H13A H 0.0775 0.3588 0.5318 0.100 Uiso 1 1 calc R . . H13B H 0.0744 0.4538 0.4802 0.100 Uiso 1 1 calc R . . H13C H 0.1490 0.4418 0.5584 0.100 Uiso 1 1 calc R . . C14 C 0.34352(18) 0.1606(2) 0.48845(15) 0.0518(6) Uani 1 1 d . A . H14A H 0.3375 0.1525 0.5436 0.078 Uiso 1 1 calc R . . H14B H 0.4065 0.1729 0.4859 0.078 Uiso 1 1 calc R . . H14C H 0.3235 0.1025 0.4589 0.078 Uiso 1 1 calc R . . C15 C 0.39661(11) 0.06706(13) 0.18452(11) 0.0251(4) Uani 1 1 d . A . C16 C 0.37508(12) 0.09908(14) 0.10706(11) 0.0288(4) Uani 1 1 d . . . C17 C 0.38201(13) 0.03490(16) 0.04688(12) 0.0340(4) Uani 1 1 d . A . H17 H 0.3671 0.0555 -0.0063 0.041 Uiso 1 1 calc R . . C18 C 0.41011(14) -0.05824(15) 0.06266(13) 0.0356(5) Uani 1 1 d . . . C19 C 0.43335(13) -0.08656(14) 0.14089(13) 0.0345(4) Uani 1 1 d . A . H19 H 0.4542 -0.1497 0.1523 0.041 Uiso 1 1 calc R . . C20 C 0.42705(12) -0.02536(14) 0.20319(12) 0.0300(4) Uani 1 1 d . . . C21 C 0.34392(17) 0.19967(16) 0.08865(14) 0.0417(5) Uani 1 1 d . A . H21A H 0.2873 0.2102 0.1068 0.063 Uiso 1 1 calc R . . H21B H 0.3349 0.2102 0.0316 0.063 Uiso 1 1 calc R . . H21C H 0.3893 0.2442 0.1155 0.063 Uiso 1 1 calc R . . C22 C 0.41338(18) -0.12752(19) -0.00383(16) 0.0512(6) Uani 1 1 d . A . H22A H 0.3575 -0.1643 -0.0147 0.077 Uiso 1 1 calc R . . H22B H 0.4643 -0.1709 0.0113 0.077 Uiso 1 1 calc R . . H22C H 0.4204 -0.0922 -0.0512 0.077 Uiso 1 1 calc R . . C23 C 0.44752(17) -0.06004(17) 0.28684(14) 0.0436(5) Uani 1 1 d . A . H23A H 0.4678 -0.1263 0.2879 0.065 Uiso 0.50 1 calc PR . . H23B H 0.3933 -0.0560 0.3098 0.065 Uiso 0.50 1 calc PR . . H23C H 0.4948 -0.0204 0.3174 0.065 Uiso 0.50 1 calc PR . . H23D H 0.4361 -0.0088 0.3222 0.065 Uiso 0.50 1 calc PR . . H23E H 0.5106 -0.0792 0.3003 0.065 Uiso 0.50 1 calc PR . . H23F H 0.4092 -0.1147 0.2926 0.065 Uiso 0.50 1 calc PR . . C24 C 0.15158(11) -0.16822(12) 0.20961(10) 0.0242(3) Uani 1 1 d . . . C25 C 0.21602(13) -0.16866(14) 0.16186(12) 0.0324(4) Uani 1 1 d . A . H25 H 0.2355 -0.1102 0.1431 0.039 Uiso 1 1 calc R . . C26 C 0.25220(14) -0.25403(15) 0.14130(13) 0.0378(5) Uani 1 1 d . . . H26 H 0.2956 -0.2534 0.1082 0.045 Uiso 1 1 calc R A . C27 C 0.22552(14) -0.33950(15) 0.16872(14) 0.0400(5) Uani 1 1 d . A . H27 H 0.2499 -0.3977 0.1542 0.048 Uiso 1 1 calc R . . C28 C 0.16335(16) -0.33975(16) 0.21722(17) 0.0488(6) Uani 1 1 d . . . H28 H 0.1453 -0.3984 0.2368 0.059 Uiso 1 1 calc R A . C29 C 0.12663(14) -0.25460(14) 0.23785(14) 0.0387(5) Uani 1 1 d . A . H29 H 0.0840 -0.2557 0.2717 0.046 Uiso 1 1 calc R . . C30 C 0.00588(11) -0.04445(12) 0.14590(10) 0.0220(3) Uani 1 1 d . . . C31 C -0.05448(12) 0.03071(14) 0.14519(12) 0.0294(4) Uani 1 1 d . A . H31 H -0.0456 0.0754 0.1872 0.035 Uiso 1 1 calc R . . C32 C -0.12716(13) 0.04098(15) 0.08394(13) 0.0366(5) Uani 1 1 d . . . H32 H -0.1685 0.0916 0.0849 0.044 Uiso 1 1 calc R A . C33 C -0.13995(14) -0.02210(16) 0.02132(12) 0.0380(5) Uani 1 1 d . A . H33 H -0.1893 -0.0146 -0.0211 0.046 Uiso 1 1 calc R . . C34 C -0.08028(15) -0.09585(17) 0.02127(12) 0.0396(5) Uani 1 1 d . . . H34 H -0.0886 -0.1392 -0.0217 0.048 Uiso 1 1 calc R A . C35 C -0.00794(13) -0.10795(15) 0.08304(11) 0.0307(4) Uani 1 1 d . A . H35 H 0.0322 -0.1598 0.0823 0.037 Uiso 1 1 calc R . . C36 C 0.03711(12) -0.09234(13) 0.30796(10) 0.0237(3) Uani 1 1 d . . . C37 C 0.08009(13) -0.08827(14) 0.38636(11) 0.0294(4) Uani 1 1 d . A . H37 H 0.1407 -0.0675 0.3992 0.035 Uiso 1 1 calc R . . C38 C 0.03525(16) -0.11435(16) 0.44608(12) 0.0382(5) Uani 1 1 d . . . H38 H 0.0651 -0.1107 0.4995 0.046 Uiso 1 1 calc R A . C39 C -0.05282(17) -0.14570(19) 0.42815(13) 0.0460(6) Uani 1 1 d . A . H39 H -0.0836 -0.1627 0.4692 0.055 Uiso 1 1 calc R . . C40 C -0.09536(16) -0.1520(2) 0.35074(14) 0.0508(6) Uani 1 1 d . . . H40 H -0.1553 -0.1747 0.3383 0.061 Uiso 1 1 calc R A . C41 C -0.05105(14) -0.12541(17) 0.29045(12) 0.0380(5) Uani 1 1 d . A . H41 H -0.0810 -0.1298 0.2371 0.046 Uiso 1 1 calc R . . H1 H 0.2294(14) 0.0291(15) 0.1838(9) 0.033(6) Uiso 1 1 d D A . H2 H 0.2541(17) -0.0088(15) 0.3013(16) 0.054(8) Uiso 0.90 1 d PD A 1 Cl1 Cl 0.2837(5) -0.0498(5) 0.3368(5) 0.074(2) Uiso 0.10 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01792(7) 0.02003(8) 0.02138(7) -0.00341(5) 0.00593(5) -0.00224(5) P1 0.01887(19) 0.0204(2) 0.0214(2) -0.00175(15) 0.00613(15) -0.00127(15) O1 0.0308(7) 0.0433(8) 0.0306(7) -0.0092(6) 0.0129(6) -0.0021(6) O2 0.0515(9) 0.0375(8) 0.0357(8) 0.0036(6) 0.0091(7) 0.0054(7) N1 0.0227(7) 0.0282(8) 0.0361(8) -0.0111(6) 0.0113(6) -0.0069(6) N2 0.0216(7) 0.0246(8) 0.0307(8) -0.0049(6) 0.0094(6) -0.0018(6) C1 0.0206(8) 0.0236(8) 0.0246(8) -0.0018(6) 0.0026(6) -0.0022(6) C2 0.0273(8) 0.0266(9) 0.0221(8) -0.0056(7) 0.0101(7) -0.0046(7) C3 0.0212(8) 0.0218(8) 0.0256(8) -0.0024(6) 0.0072(6) -0.0010(6) C4 0.0267(9) 0.0394(11) 0.0467(12) -0.0158(9) 0.0119(8) -0.0147(8) C5 0.0224(8) 0.0366(11) 0.0440(11) -0.0087(9) 0.0119(8) -0.0097(8) C6 0.0252(8) 0.0276(9) 0.0368(10) -0.0139(8) 0.0118(7) -0.0085(7) C7 0.0362(10) 0.0256(10) 0.0469(12) -0.0115(8) 0.0138(9) -0.0067(8) C8 0.0402(12) 0.0279(11) 0.0695(16) -0.0157(10) 0.0161(11) -0.0018(9) C9 0.0417(12) 0.0399(12) 0.0597(14) -0.0264(11) 0.0257(11) -0.0159(10) C10 0.0420(12) 0.0484(13) 0.0400(11) -0.0206(10) 0.0174(9) -0.0174(10) C12 0.0611(15) 0.0313(12) 0.0569(15) 0.0021(10) 0.0145(12) -0.0015(11) C13 0.0637(17) 0.0582(17) 0.090(2) -0.0338(16) 0.0483(17) -0.0112(14) C14 0.0518(14) 0.0599(16) 0.0420(13) -0.0004(11) 0.0044(11) -0.0005(12) C15 0.0205(8) 0.0253(9) 0.0321(9) -0.0046(7) 0.0119(7) -0.0013(6) C16 0.0273(9) 0.0289(9) 0.0328(9) 0.0002(7) 0.0124(7) -0.0005(7) C17 0.0317(10) 0.0423(11) 0.0310(10) -0.0048(8) 0.0131(8) -0.0028(8) C18 0.0293(9) 0.0387(11) 0.0435(11) -0.0137(9) 0.0185(8) -0.0047(8) C19 0.0315(10) 0.0270(10) 0.0484(12) -0.0052(8) 0.0162(9) 0.0034(8) C20 0.0243(8) 0.0309(10) 0.0369(10) -0.0024(8) 0.0113(7) 0.0034(7) C21 0.0511(13) 0.0350(11) 0.0412(12) 0.0059(9) 0.0140(10) 0.0063(10) C22 0.0543(14) 0.0497(15) 0.0554(15) -0.0241(12) 0.0254(12) -0.0075(11) C23 0.0493(13) 0.0410(12) 0.0418(12) 0.0067(9) 0.0121(10) 0.0143(10) C24 0.0223(8) 0.0221(8) 0.0280(9) -0.0021(7) 0.0039(7) 0.0007(6) C25 0.0345(10) 0.0265(10) 0.0393(11) -0.0020(8) 0.0148(8) 0.0020(8) C26 0.0357(10) 0.0344(11) 0.0457(12) -0.0095(9) 0.0137(9) 0.0058(8) C27 0.0330(10) 0.0260(10) 0.0586(14) -0.0120(9) 0.0022(9) 0.0073(8) C28 0.0470(13) 0.0214(10) 0.0812(18) 0.0015(10) 0.0208(12) 0.0010(9) C29 0.0355(10) 0.0238(10) 0.0612(14) 0.0008(9) 0.0201(10) -0.0010(8) C30 0.0218(8) 0.0220(8) 0.0228(8) 0.0002(6) 0.0061(6) -0.0049(6) C31 0.0259(9) 0.0256(9) 0.0359(10) -0.0032(7) 0.0036(7) -0.0007(7) C32 0.0278(9) 0.0303(10) 0.0485(12) 0.0074(9) -0.0005(9) -0.0010(8) C33 0.0342(10) 0.0424(12) 0.0333(10) 0.0105(9) -0.0046(8) -0.0099(9) C34 0.0441(12) 0.0477(13) 0.0245(9) -0.0046(8) -0.0002(8) -0.0080(10) C35 0.0345(10) 0.0313(10) 0.0263(9) -0.0048(7) 0.0057(7) -0.0009(8) C36 0.0244(8) 0.0241(9) 0.0237(8) -0.0001(6) 0.0077(6) -0.0013(6) C37 0.0317(9) 0.0304(10) 0.0255(9) 0.0051(7) 0.0038(7) -0.0016(7) C38 0.0511(12) 0.0401(12) 0.0242(9) 0.0043(8) 0.0088(9) -0.0038(10) C39 0.0510(13) 0.0601(15) 0.0325(11) 0.0046(10) 0.0222(10) -0.0081(11) C40 0.0351(11) 0.0826(19) 0.0382(12) 0.0057(12) 0.0153(9) -0.0193(12) C41 0.0301(10) 0.0585(14) 0.0269(9) 0.0018(9) 0.0093(8) -0.0140(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H2 1.580(10) . ? Ru1 H1 1.604(9) . ? Ru1 C1 1.9202(18) . ? Ru1 C2 1.9315(19) . ? Ru1 C3 2.0874(17) . ? Ru1 P1 2.3228(4) . ? Ru1 Cl1 2.460(3) . ? P1 C30 1.8317(17) . ? P1 C36 1.8387(18) . ? P1 C24 1.8413(18) . ? O1 C1 1.145(2) . ? O2 C2 1.126(2) . ? N1 C3 1.368(2) . ? N1 C4 1.390(2) . ? N1 C6 1.440(2) . ? N2 C3 1.373(2) . ? N2 C5 1.390(2) . ? N2 C15 1.442(2) . ? C4 C5 1.336(3) . ? C6 C7 1.392(3) . ? C6 C11 1.397(3) . ? C7 C8 1.398(3) . ? C7 C12 1.507(3) . ? C8 C9 1.388(4) . ? C9 C10 1.375(4) . ? C9 C13 1.519(3) . ? C10 C11 1.389(3) . ? C11 C14 1.497(3) . ? C15 C16 1.391(3) . ? C15 C20 1.395(3) . ? C16 C17 1.395(3) . ? C16 C21 1.504(3) . ? C17 C18 1.387(3) . ? C18 C19 1.389(3) . ? C18 C22 1.513(3) . ? C19 C20 1.395(3) . ? C20 C23 1.501(3) . ? C24 C29 1.386(3) . ? C24 C25 1.393(3) . ? C25 C26 1.392(3) . ? C26 C27 1.379(3) . ? C27 C28 1.375(3) . ? C28 C29 1.394(3) . ? C30 C35 1.390(2) . ? C30 C31 1.396(3) . ? C31 C32 1.385(3) . ? C32 C33 1.383(3) . ? C33 C34 1.376(3) . ? C34 C35 1.390(3) . ? C36 C37 1.390(2) . ? C36 C41 1.395(3) . ? C37 C38 1.388(3) . ? C38 C39 1.386(3) . ? C39 C40 1.374(3) . ? C40 C41 1.393(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H2 Ru1 H1 80.8(13) . . ? H2 Ru1 C1 96.4(11) . . ? H1 Ru1 C1 173.7(8) . . ? H2 Ru1 C2 170.0(11) . . ? H1 Ru1 C2 89.2(8) . . ? C1 Ru1 C2 93.58(7) . . ? H2 Ru1 C3 83.5(11) . . ? H1 Ru1 C3 85.6(8) . . ? C1 Ru1 C3 99.70(7) . . ? C2 Ru1 C3 95.52(7) . . ? H2 Ru1 P1 78.6(11) . . ? H1 Ru1 P1 79.7(8) . . ? C1 Ru1 P1 94.22(5) . . ? C2 Ru1 P1 100.02(5) . . ? C3 Ru1 P1 158.42(5) . . ? H2 Ru1 Cl1 5.2(11) . . ? H1 Ru1 Cl1 86.0(8) . . ? C1 Ru1 Cl1 91.2(2) . . ? C2 Ru1 Cl1 175.2(2) . . ? C3 Ru1 Cl1 83.8(2) . . ? P1 Ru1 Cl1 79.5(2) . . ? C30 P1 C36 100.97(8) . . ? C30 P1 C24 102.50(8) . . ? C36 P1 C24 101.75(8) . . ? C30 P1 Ru1 116.63(6) . . ? C36 P1 Ru1 117.02(6) . . ? C24 P1 Ru1 115.56(6) . . ? C3 N1 C4 111.97(15) . . ? C3 N1 C6 125.86(14) . . ? C4 N1 C6 122.11(15) . . ? C3 N2 C5 111.42(15) . . ? C3 N2 C15 126.43(14) . . ? C5 N2 C15 121.97(15) . . ? O1 C1 Ru1 173.11(15) . . ? O2 C2 Ru1 178.68(16) . . ? N1 C3 N2 102.86(14) . . ? N1 C3 Ru1 129.58(12) . . ? N2 C3 Ru1 127.42(12) . . ? C5 C4 N1 106.55(16) . . ? C4 C5 N2 107.20(16) . . ? C7 C6 C11 122.36(18) . . ? C7 C6 N1 118.75(18) . . ? C11 C6 N1 118.85(18) . . ? C6 C7 C8 116.9(2) . . ? C6 C7 C12 121.56(19) . . ? C8 C7 C12 121.5(2) . . ? C9 C8 C7 122.1(2) . . ? C10 C9 C8 118.9(2) . . ? C10 C9 C13 119.7(3) . . ? C8 C9 C13 121.4(3) . . ? C9 C10 C11 121.6(2) . . ? C10 C11 C6 118.0(2) . . ? C10 C11 C14 120.3(2) . . ? C6 C11 C14 121.7(2) . . ? C16 C15 C20 122.06(17) . . ? C16 C15 N2 118.23(16) . . ? C20 C15 N2 119.68(17) . . ? C15 C16 C17 118.11(18) . . ? C15 C16 C21 120.96(18) . . ? C17 C16 C21 120.92(19) . . ? C18 C17 C16 121.8(2) . . ? C17 C18 C19 118.27(18) . . ? C17 C18 C22 120.7(2) . . ? C19 C18 C22 121.1(2) . . ? C18 C19 C20 122.20(19) . . ? C19 C20 C15 117.55(18) . . ? C19 C20 C23 120.75(19) . . ? C15 C20 C23 121.61(18) . . ? C29 C24 C25 118.24(17) . . ? C29 C24 P1 121.47(14) . . ? C25 C24 P1 120.24(14) . . ? C26 C25 C24 120.62(19) . . ? C27 C26 C25 120.4(2) . . ? C28 C27 C26 119.42(19) . . ? C27 C28 C29 120.5(2) . . ? C24 C29 C28 120.8(2) . . ? C35 C30 C31 118.40(17) . . ? C35 C30 P1 123.25(14) . . ? C31 C30 P1 118.34(13) . . ? C32 C31 C30 120.83(18) . . ? C33 C32 C31 120.3(2) . . ? C34 C33 C32 119.14(19) . . ? C33 C34 C35 121.1(2) . . ? C34 C35 C30 120.18(19) . . ? C37 C36 C41 118.71(17) . . ? C37 C36 P1 119.30(13) . . ? C41 C36 P1 121.98(14) . . ? C38 C37 C36 120.53(18) . . ? C39 C38 C37 120.32(19) . . ? C40 C39 C38 119.7(2) . . ? C39 C40 C41 120.4(2) . . ? C40 C41 C36 120.36(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.007 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.070 data_c:\x-ray\kappa\k06mkw7\maxus\k06mkw7 _database_code_depnum_ccdc_archive 'CCDC 676387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H87 Cl N4 O Ru' _chemical_formula_weight 1028.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P22121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6270(1) _cell_length_b 13.0200(1) _cell_length_c 20.7530(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2871.46(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 65000 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.361 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50119 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8385 _reflns_number_gt 8009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.5785P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(17) _refine_ls_number_reflns 8385 _refine_ls_number_parameters 333 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.593907(13) 1.0000 0.0000 0.02006(4) Uani 1 2 d SD . . Cl1 Cl 0.3750(2) 1.0000 0.0000 0.0392(5) Uani 0.50 2 d SP A 1 O1 O 0.8709(6) 1.0000 0.0000 0.0595(14) Uani 0.50 2 d SP A 1 N1 N 0.56359(12) 1.04328(10) -0.14779(6) 0.0242(3) Uani 1 1 d . . . N2 N 0.63174(13) 0.89077(10) -0.13252(6) 0.0242(2) Uani 1 1 d . . . C1 C 0.7727(7) 1.0000 0.0000 0.0325(17) Uani 0.50 2 d SP A 1 C2 C 0.59600(13) 0.97677(9) -0.09950(6) 0.0200(3) Uani 1 1 d . A . C3 C 0.57859(16) 0.99934(16) -0.20835(6) 0.0378(3) Uani 1 1 d . A . H3 H 0.5625 1.0311 -0.2487 0.045 Uiso 1 1 calc R . . C4 C 0.6204(2) 0.90298(13) -0.19849(8) 0.0381(4) Uani 1 1 d . A . H4 H 0.6386 0.8531 -0.2306 0.046 Uiso 1 1 calc R . . C5 C 0.52362(15) 1.14897(11) -0.14115(7) 0.0239(3) Uani 1 1 d . A . C6 C 0.61632(16) 1.22425(12) -0.13253(7) 0.0273(3) Uani 1 1 d . . . C7 C 0.57691(18) 1.32667(12) -0.13095(8) 0.0334(3) Uani 1 1 d . A . H7 H 0.6374 1.3796 -0.1251 0.040 Uiso 1 1 calc R . . C8 C 0.45159(18) 1.35199(12) -0.13771(8) 0.0338(4) Uani 1 1 d . . . H8 H 0.4266 1.4220 -0.1366 0.041 Uiso 1 1 calc R A . C9 C 0.36167(19) 1.27584(14) -0.14614(9) 0.0314(4) Uani 1 1 d . A . H9 H 0.2757 1.2945 -0.1507 0.038 Uiso 1 1 calc R . . C10 C 0.39556(16) 1.17195(11) -0.14802(7) 0.0272(3) Uani 1 1 d . . . C11 C 0.75513(16) 1.19771(15) -0.12855(8) 0.0326(3) Uani 1 1 d . A . H11 H 0.7619 1.1232 -0.1174 0.039 Uiso 1 1 calc R . . C12 C 0.8229(2) 1.25826(18) -0.07613(14) 0.0564(6) Uani 1 1 d . . . H12A H 0.8238 1.3313 -0.0876 0.085 Uiso 1 1 calc R A . H12B H 0.9096 1.2333 -0.0721 0.085 Uiso 1 1 calc R . . H12C H 0.7790 1.2491 -0.0350 0.085 Uiso 1 1 calc R . . C13 C 0.8185(2) 1.2134(3) -0.19324(12) 0.0830(11) Uani 1 1 d . . . H13A H 0.7781 1.1695 -0.2256 0.125 Uiso 1 1 calc R A . H13B H 0.9077 1.1953 -0.1898 0.125 Uiso 1 1 calc R . . H13C H 0.8106 1.2855 -0.2062 0.125 Uiso 1 1 calc R . . C14 C 0.29523(17) 1.09023(14) -0.15874(10) 0.0381(4) Uani 1 1 d . A . H14 H 0.3293 1.0233 -0.1427 0.046 Uiso 1 1 calc R . . C15 C 0.2674(3) 1.0784(2) -0.23138(13) 0.0639(7) Uani 1 1 d . . . H15A H 0.2010 1.0271 -0.2375 0.096 Uiso 1 1 calc R A . H15B H 0.3439 1.0561 -0.2538 0.096 Uiso 1 1 calc R . . H15C H 0.2397 1.1445 -0.2490 0.096 Uiso 1 1 calc R . . C16 C 0.17435(19) 1.11303(18) -0.12176(13) 0.0552(6) Uani 1 1 d . . . H16A H 0.1941 1.1235 -0.0761 0.083 Uiso 1 1 calc R A . H16B H 0.1162 1.0550 -0.1262 0.083 Uiso 1 1 calc R . . H16C H 0.1351 1.1752 -0.1392 0.083 Uiso 1 1 calc R . . C17 C 0.66690(15) 0.79200(11) -0.10661(8) 0.0239(3) Uani 1 1 d . A . C18 C 0.79395(16) 0.76362(12) -0.10718(8) 0.0269(3) Uani 1 1 d . . . C19 C 0.82198(17) 0.66274(12) -0.08971(9) 0.0339(4) Uani 1 1 d . A . H19 H 0.9071 0.6404 -0.0905 0.041 Uiso 1 1 calc R . . C20 C 0.72902(19) 0.59435(12) -0.07125(9) 0.0365(4) Uani 1 1 d . . . H20 H 0.7507 0.5260 -0.0596 0.044 Uiso 1 1 calc R A . C21 C 0.60450(18) 0.62542(12) -0.06979(8) 0.0335(3) Uani 1 1 d . A . H21 H 0.5414 0.5783 -0.0564 0.040 Uiso 1 1 calc R . . C22 C 0.57008(15) 0.72512(12) -0.08772(8) 0.0273(3) Uani 1 1 d . . . C23 C 0.89952(17) 0.83590(13) -0.12670(9) 0.0367(4) Uani 1 1 d . A . H23 H 0.8665 0.9078 -0.1250 0.044 Uiso 1 1 calc R . . C24 C 0.9414(3) 0.8138(2) -0.19600(14) 0.0688(8) Uani 1 1 d . . . H24A H 0.9628 0.7409 -0.2002 0.103 Uiso 1 1 calc R A . H24B H 1.0154 0.8557 -0.2063 0.103 Uiso 1 1 calc R . . H24C H 0.8729 0.8307 -0.2258 0.103 Uiso 1 1 calc R . . C25 C 1.01284(18) 0.82900(16) -0.08178(14) 0.0519(6) Uani 1 1 d . . . H25A H 0.9855 0.8406 -0.0373 0.078 Uiso 1 1 calc R A . H25B H 1.0748 0.8813 -0.0939 0.078 Uiso 1 1 calc R . . H25C H 1.0509 0.7607 -0.0853 0.078 Uiso 1 1 calc R . . C26 C 0.43269(15) 0.75640(14) -0.08975(8) 0.0307(3) Uani 1 1 d . A . H26 H 0.4294 0.8329 -0.0936 0.037 Uiso 1 1 calc R . . C27 C 0.3689(2) 0.7110(2) -0.14954(12) 0.0482(6) Uani 1 1 d . . . H27A H 0.4111 0.7364 -0.1884 0.072 Uiso 1 1 calc R A . H27B H 0.2802 0.7316 -0.1503 0.072 Uiso 1 1 calc R . . H27C H 0.3746 0.6359 -0.1481 0.072 Uiso 1 1 calc R . . C28 C 0.36306(19) 0.72645(17) -0.02806(10) 0.0433(4) Uani 1 1 d . . . H28A H 0.3622 0.6515 -0.0238 0.065 Uiso 1 1 calc R A . H28B H 0.2764 0.7520 -0.0300 0.065 Uiso 1 1 calc R . . H28C H 0.4060 0.7566 0.0092 0.065 Uiso 1 1 calc R . . C29 C 0.8927(4) 0.9969(4) -0.3269(2) 0.0549(9) Uiso 0.50 1 d P B 1 C30 C 0.9344(4) 0.9557(3) -0.3915(2) 0.0404(8) Uiso 0.50 1 d P B 1 C31 C 0.8626(3) 1.0089(4) -0.44855(18) 0.0402(7) Uiso 0.50 1 d P B 1 H1 H 0.591(3) 0.8792(9) 0.0149(16) 0.026(9) Uiso 0.50 1 d PD A . Cl1A Cl 0.81329(16) 1.0000 0.0000 0.0282(4) Uani 0.50 2 d SP A 2 O1A O 0.3077(4) 1.0000 0.0000 0.0521(11) Uani 0.50 2 d SP A 2 C1A C 0.4180(7) 1.0000 0.0000 0.0310(15) Uani 0.50 2 d SP A 2 C29A C 0.8981(4) 0.9862(4) -0.3632(3) 0.0569(10) Uiso 0.50 1 d P . 2 C30A C 0.8506(5) 0.9586(4) -0.4311(3) 0.0557(11) Uiso 0.50 1 d P . 2 C31A C 0.9172(3) 1.0161(3) -0.48615(15) 0.0384(8) Uiso 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02718(7) 0.01712(6) 0.01589(6) 0.00043(7) 0.000 0.000 Cl1 0.0323(12) 0.0547(8) 0.0305(6) -0.0054(14) 0.000 0.000 O1 0.050(3) 0.088(3) 0.040(2) -0.013(4) 0.000 0.000 N1 0.0332(7) 0.0211(5) 0.0183(5) -0.0001(4) 0.0002(5) 0.0067(5) N2 0.0328(6) 0.0212(6) 0.0186(5) 0.0008(4) 0.0021(5) 0.0053(5) C1 0.020(4) 0.051(3) 0.027(2) -0.007(4) 0.000 0.000 C2 0.0224(6) 0.0195(6) 0.0181(6) 0.0003(4) 0.0014(5) 0.0008(4) C3 0.0652(10) 0.0316(7) 0.0166(5) 0.0014(8) 0.0018(6) 0.0133(14) C4 0.0639(12) 0.0321(8) 0.0183(7) -0.0016(6) 0.0041(7) 0.0141(8) C5 0.0329(8) 0.0216(6) 0.0174(6) 0.0031(5) 0.0016(5) 0.0041(5) C6 0.0330(8) 0.0276(7) 0.0214(7) 0.0034(6) 0.0014(6) 0.0022(6) C7 0.0439(10) 0.0252(7) 0.0311(8) 0.0022(6) 0.0006(7) -0.0032(7) C8 0.0477(10) 0.0212(7) 0.0326(8) 0.0038(6) 0.0015(7) 0.0078(6) C9 0.0369(10) 0.0307(8) 0.0264(8) 0.0057(7) 0.0010(7) 0.0100(7) C10 0.0336(8) 0.0254(7) 0.0227(7) 0.0049(5) -0.0011(6) 0.0039(6) C11 0.0311(8) 0.0387(9) 0.0281(8) 0.0053(7) -0.0002(6) -0.0005(7) C12 0.0454(12) 0.0509(13) 0.0729(16) -0.0122(12) -0.0169(11) -0.0003(10) C13 0.0394(12) 0.168(3) 0.0416(13) 0.0292(17) 0.0117(10) 0.0206(16) C14 0.0362(9) 0.0298(8) 0.0484(11) 0.0056(7) -0.0109(8) 0.0018(7) C15 0.0716(16) 0.0615(15) 0.0587(15) -0.0101(12) -0.0244(13) -0.0102(13) C16 0.0313(9) 0.0500(12) 0.0844(18) 0.0194(12) -0.0049(10) 0.0009(8) C17 0.0304(7) 0.0181(6) 0.0232(7) -0.0010(5) 0.0003(6) 0.0043(5) C18 0.0305(8) 0.0211(7) 0.0291(8) -0.0024(6) 0.0031(6) 0.0036(6) C19 0.0338(8) 0.0241(7) 0.0438(10) -0.0021(7) -0.0018(7) 0.0095(6) C20 0.0487(10) 0.0188(7) 0.0421(9) 0.0008(6) -0.0050(8) 0.0040(7) C21 0.0396(9) 0.0245(7) 0.0364(8) 0.0025(6) -0.0021(7) -0.0066(7) C22 0.0329(8) 0.0244(7) 0.0246(7) -0.0017(6) -0.0032(6) -0.0006(6) C23 0.0342(8) 0.0261(7) 0.0500(10) 0.0004(7) 0.0127(8) 0.0029(7) C24 0.0753(17) 0.0626(15) 0.0686(16) -0.0079(13) 0.0409(14) -0.0154(13) C25 0.0293(9) 0.0357(10) 0.0908(18) 0.0030(11) 0.0036(10) 0.0010(7) C26 0.0294(8) 0.0334(8) 0.0294(8) -0.0028(6) -0.0017(6) -0.0026(6) C27 0.0393(13) 0.0647(14) 0.0405(12) -0.0135(11) -0.0088(9) -0.0027(10) C28 0.0392(10) 0.0518(11) 0.0389(9) -0.0004(9) 0.0066(8) -0.0048(8) Cl1A 0.0117(9) 0.0472(6) 0.0256(5) -0.0014(10) 0.000 0.000 O1A 0.0235(19) 0.082(3) 0.050(2) 0.007(4) 0.000 0.000 C1A 0.032(4) 0.041(3) 0.020(2) -0.007(4) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1 1.603(10) . ? Ru1 C1A 1.870(7) . ? Ru1 C1 1.900(7) . ? Ru1 C2 2.0872(13) 3_575 ? Ru1 C2 2.0872(13) . ? Ru1 Cl1 2.327(2) . ? Ru1 Cl1A 2.3314(17) . ? O1 C1 1.044(7) . ? N1 C2 1.3685(17) . ? N1 C3 1.3900(19) . ? N1 C5 1.4467(18) . ? N2 C2 1.3666(17) . ? N2 C4 1.384(2) . ? N2 C17 1.4432(18) . ? C3 C4 1.347(3) . ? C5 C10 1.401(2) . ? C5 C6 1.401(2) . ? C6 C7 1.398(2) . ? C6 C11 1.517(2) . ? C7 C8 1.379(3) . ? C8 C9 1.388(3) . ? C9 C10 1.400(2) . ? C10 C14 1.523(2) . ? C11 C13 1.516(3) . ? C11 C12 1.525(3) . ? C14 C16 1.525(3) . ? C14 C15 1.544(3) . ? C17 C18 1.400(2) . ? C17 C22 1.404(2) . ? C18 C19 1.395(2) . ? C18 C23 1.519(2) . ? C19 C20 1.384(3) . ? C20 C21 1.384(3) . ? C21 C22 1.399(2) . ? C22 C26 1.516(2) . ? C23 C25 1.526(3) . ? C23 C24 1.533(3) . ? C26 C28 1.529(2) . ? C26 C27 1.532(3) . ? C29 C30 1.512(6) . ? C30 C31 1.569(6) . ? O1A C1A 1.172(6) . ? C29A C30A 1.540(7) . ? C30A C31A 1.538(6) . ? C30A C31A 1.886(6) 3_574 ? C31A C31A 0.712(6) 3_574 ? C31A C30A 1.886(6) 3_574 ? 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 H1 Ru1 C1A 88.7(12) . . ? H1 Ru1 C1 91.3(12) . . ? C1A Ru1 C1 180.0 . . ? H1 Ru1 C2 87.2(12) . 3_575 ? C1A Ru1 C2 90.61(4) . 3_575 ? C1 Ru1 C2 89.39(4) . 3_575 ? H1 Ru1 C2 92.8(12) . . ? C1A Ru1 C2 90.61(4) . . ? C1 Ru1 C2 89.39(4) . . ? C2 Ru1 C2 178.78(8) 3_575 . ? H1 Ru1 Cl1 88.7(12) . . ? C1A Ru1 Cl1 0.0 . . ? C1 Ru1 Cl1 180.0 . . ? C2 Ru1 Cl1 90.61(4) 3_575 . ? C2 Ru1 Cl1 90.61(4) . . ? H1 Ru1 Cl1A 91.3(12) . . ? C1A Ru1 Cl1A 180.0 . . ? C1 Ru1 Cl1A 0.0 . . ? C2 Ru1 Cl1A 89.39(4) 3_575 . ? C2 Ru1 Cl1A 89.39(4) . . ? Cl1 Ru1 Cl1A 180.0 . . ? C2 N1 C3 111.88(13) . . ? C2 N1 C5 127.30(12) . . ? C3 N1 C5 120.75(13) . . ? C2 N2 C4 112.20(12) . . ? C2 N2 C17 127.97(12) . . ? C4 N2 C17 119.58(13) . . ? O1 C1 Ru1 180.0 . . ? N2 C2 N1 102.79(11) . . ? N2 C2 Ru1 128.15(9) . . ? N1 C2 Ru1 129.06(9) . . ? C4 C3 N1 106.50(13) . . ? C3 C4 N2 106.62(14) . . ? C10 C5 C6 123.14(14) . . ? C10 C5 N1 118.61(14) . . ? C6 C5 N1 118.11(14) . . ? C7 C6 C5 117.36(15) . . ? C7 C6 C11 120.48(16) . . ? C5 C6 C11 122.08(14) . . ? C8 C7 C6 120.99(16) . . ? C7 C8 C9 120.46(15) . . ? C8 C9 C10 121.09(17) . . ? C9 C10 C5 116.96(16) . . ? C9 C10 C14 119.93(16) . . ? C5 C10 C14 123.09(14) . . ? C13 C11 C6 110.66(15) . . ? C13 C11 C12 110.6(2) . . ? C6 C11 C12 112.37(16) . . ? C10 C14 C16 112.35(16) . . ? C10 C14 C15 110.27(17) . . ? C16 C14 C15 110.44(19) . . ? C18 C17 C22 123.07(14) . . ? C18 C17 N2 118.80(14) . . ? C22 C17 N2 117.84(14) . . ? C19 C18 C17 116.89(15) . . ? C19 C18 C23 119.67(15) . . ? C17 C18 C23 123.43(14) . . ? C20 C19 C18 121.70(16) . . ? C19 C20 C21 120.03(15) . . ? C20 C21 C22 121.03(16) . . ? C21 C22 C17 117.26(15) . . ? C21 C22 C26 120.56(15) . . ? C17 C22 C26 122.10(14) . . ? C18 C23 C25 112.54(16) . . ? C18 C23 C24 110.39(17) . . ? C25 C23 C24 109.45(19) . . ? C22 C26 C28 111.97(14) . . ? C22 C26 C27 110.17(15) . . ? C28 C26 C27 111.43(16) . . ? C29 C30 C31 111.8(4) . . ? O1A C1A Ru1 180.0 . . ? C31A C30A C29A 114.5(4) . . ? C31A C30A C31A 21.0(2) . 3_574 ? C29A C30A C31A 132.0(4) . 3_574 ? C31A C31A C30A 108.2(6) 3_574 . ? C31A C31A C30A 50.8(5) 3_574 3_574 ? C30A C31A C30A 126.0(4) . 3_574 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.396 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.045