# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. Whittlesey' _publ_contact_author_email M.K.WHITTLESEY@BATH.AC.UK _publ_section_title ; Ru(NHC)(xantphos)(CO)H2] Complexes: Intramolecular C-H Activation and Applications in C-C Bond Formation ; loop_ _publ_author_name 'M. Whittlesey' 'Araminta E. W. Ledger' 'Mary Mahon' 'Jonathan M. J. Williams' # Attachment 'bigcif.cif' data_k08mkw6 _database_code_depnum_ccdc_archive 'CCDC 723435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H52 N2 O2 P2 Ru' _chemical_formula_weight 887.96 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' Ru Ru -1.2594 0.8363 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2910(3) _cell_length_b 13.4770(3) _cell_length_c 13.7930(3) _cell_angle_alpha 86.559(1) _cell_angle_beta 89.898(2) _cell_angle_gamma 71.091(1) _cell_volume 2157.18(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59810 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 42117 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9787 _reflns_number_gt 7945 _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^)+(0.0236P)^2^+2.1650P] 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 9787 _refine_ls_number_parameters 550 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.715040(16) 0.272063(15) 0.801327(14) 0.02163(6) Uani 1 1 d D . . P1 P 0.52472(5) 0.27639(5) 0.77901(4) 0.02140(13) Uani 1 1 d . . . O1 O 0.64642(17) 0.49737(14) 0.71937(14) 0.0391(5) Uani 1 1 d . . . N1 N 0.94213(17) 0.32456(16) 0.85941(15) 0.0261(4) Uani 1 1 d . . . C1 C 0.6759(2) 0.4081(2) 0.74344(18) 0.0275(5) Uani 1 1 d . . . H1 H 0.670(2) 0.3268(17) 0.9002(10) 0.026(6) Uiso 1 1 d D . . P2 P 0.81788(5) 0.16241(5) 0.67260(4) 0.02191(13) Uani 1 1 d . . . O2 O 0.62021(13) 0.08351(12) 0.69301(11) 0.0238(3) Uani 1 1 d . . . N2 N 0.89786(17) 0.20959(16) 0.95137(14) 0.0271(4) Uani 1 1 d . . . C2 C 0.8641(2) 0.27167(18) 0.86905(17) 0.0248(5) Uani 1 1 d . . . C3 C 1.0227(2) 0.2949(2) 0.93663(19) 0.0317(6) Uani 1 1 d . . . C4 C 0.9949(2) 0.2226(2) 0.99435(19) 0.0314(6) Uani 1 1 d . . . C5 C 1.1193(3) 0.3373(3) 0.9502(2) 0.0450(7) Uani 1 1 d . . . H5A H 1.1561 0.3119 1.0140 0.068 Uiso 1 1 calc R . . H5B H 1.0895 0.4142 0.9462 0.068 Uiso 1 1 calc R . . H5C H 1.1759 0.3134 0.8992 0.068 Uiso 1 1 calc R . . C6 C 1.0519(3) 0.1614(3) 1.0839(2) 0.0501(8) Uani 1 1 d . . . H6A H 1.1191 0.1815 1.1003 0.075 Uiso 1 1 calc R . . H6B H 1.0765 0.0862 1.0731 0.075 Uiso 1 1 calc R . . H6C H 0.9977 0.1761 1.1375 0.075 Uiso 1 1 calc R . . C7 C 0.9378(2) 0.4007(2) 0.77718(19) 0.0303(6) Uani 1 1 d D . . C8 C 0.8944(3) 0.5135(2) 0.8075(2) 0.0410(7) Uani 1 1 d . . . H8A H 0.8195 0.5269 0.8381 0.061 Uiso 1 1 calc R . . H8B H 0.8866 0.5620 0.7500 0.061 Uiso 1 1 calc R . . H8C H 0.9494 0.5244 0.8537 0.061 Uiso 1 1 calc R . . C9 C 1.0505(2) 0.3776(2) 0.7233(2) 0.0388(7) Uani 1 1 d . . . H9A H 1.1054 0.3992 0.7612 0.058 Uiso 1 1 calc R . . H9B H 1.0368 0.4165 0.6598 0.058 Uiso 1 1 calc R . . H9C H 1.0820 0.3021 0.7143 0.058 Uiso 1 1 calc R . . C10 C 0.8286(2) 0.1441(2) 0.98864(18) 0.0304(6) Uani 1 1 d D . . C11 C 0.7606(3) 0.1924(2) 1.07523(19) 0.0378(6) Uani 1 1 d . . . H11A H 0.8131 0.2023 1.1244 0.057 Uiso 1 1 calc R . . H11B H 0.7203 0.1457 1.1029 0.057 Uiso 1 1 calc R . . H11C H 0.7045 0.2606 1.0545 0.057 Uiso 1 1 calc R . . C12 C 0.7539(2) 0.1332(2) 0.90351(18) 0.0287(5) Uani 1 1 d D . . C13 C 0.4908(2) 0.15639(19) 0.81497(17) 0.0233(5) Uani 1 1 d . . . C14 C 0.4174(2) 0.1435(2) 0.88885(17) 0.0269(5) Uani 1 1 d . . . H14 H 0.3757 0.2019 0.9241 0.032 Uiso 1 1 calc R . . C15 C 0.4052(2) 0.0458(2) 0.91094(18) 0.0305(6) Uani 1 1 d . . . H15 H 0.3562 0.0377 0.9620 0.037 Uiso 1 1 calc R . . C16 C 0.4642(2) -0.0405(2) 0.85888(19) 0.0302(6) Uani 1 1 d . . . H16 H 0.4550 -0.1068 0.8750 0.036 Uiso 1 1 calc R . . C17 C 0.5362(2) -0.03049(19) 0.78369(18) 0.0267(5) Uani 1 1 d . . . C18 C 0.5473(2) 0.06839(19) 0.76510(17) 0.0235(5) Uani 1 1 d . . . C19 C 0.5990(2) -0.11664(19) 0.71692(19) 0.0297(6) Uani 1 1 d . . . C20 C 0.6107(3) -0.2261(2) 0.7629(2) 0.0434(7) Uani 1 1 d . . . H20A H 0.6535 -0.2373 0.8247 0.065 Uiso 1 1 calc R . . H20B H 0.6521 -0.2796 0.7189 0.065 Uiso 1 1 calc R . . H20C H 0.5341 -0.2314 0.7746 0.065 Uiso 1 1 calc R . . C21 C 0.5305(2) -0.0985(2) 0.6204(2) 0.0399(7) Uani 1 1 d . . . H21A H 0.4545 -0.1050 0.6325 0.060 Uiso 1 1 calc R . . H21B H 0.5719 -0.1509 0.5755 0.060 Uiso 1 1 calc R . . H21C H 0.5216 -0.0279 0.5917 0.060 Uiso 1 1 calc R . . C22 C 0.7157(2) -0.10258(19) 0.69585(17) 0.0258(5) Uani 1 1 d . . . C23 C 0.8177(2) -0.18418(19) 0.68271(18) 0.0297(6) Uani 1 1 d . . . H23 H 0.8181 -0.2549 0.6889 0.036 Uiso 1 1 calc R . . C24 C 0.9182(2) -0.1633(2) 0.66079(18) 0.0301(6) Uani 1 1 d . . . H24 H 0.9864 -0.2196 0.6500 0.036 Uiso 1 1 calc R . . C25 C 0.9206(2) -0.06066(19) 0.65445(17) 0.0272(5) Uani 1 1 d . . . H25 H 0.9908 -0.0478 0.6407 0.033 Uiso 1 1 calc R . . C26 C 0.8206(2) 0.02424(18) 0.66807(17) 0.0237(5) Uani 1 1 d . . . C27 C 0.7203(2) -0.00075(18) 0.68585(16) 0.0235(5) Uani 1 1 d . . . C28 C 0.7840(2) 0.21187(19) 0.54526(17) 0.0248(5) Uani 1 1 d . . . C29 C 0.7782(2) 0.3155(2) 0.52010(18) 0.0309(6) Uani 1 1 d . . . H29 H 0.7910 0.3577 0.5687 0.037 Uiso 1 1 calc R . . C30 C 0.7539(2) 0.3575(2) 0.42543(19) 0.0345(6) Uani 1 1 d . . . H30 H 0.7502 0.4280 0.4092 0.041 Uiso 1 1 calc R . . C31 C 0.7348(2) 0.2959(2) 0.35417(19) 0.0378(6) Uani 1 1 d . . . H31 H 0.7168 0.3247 0.2894 0.045 Uiso 1 1 calc R . . C32 C 0.7420(2) 0.1932(2) 0.37752(19) 0.0374(6) Uani 1 1 d . . . H32 H 0.7305 0.1508 0.3285 0.045 Uiso 1 1 calc R . . C33 C 0.7661(2) 0.1516(2) 0.47233(18) 0.0309(6) Uani 1 1 d . . . H33 H 0.7703 0.0808 0.4878 0.037 Uiso 1 1 calc R . . C34 C 0.9754(2) 0.13448(19) 0.67561(17) 0.0244(5) Uani 1 1 d . . . C35 C 1.0339(2) 0.09472(19) 0.76311(19) 0.0288(5) Uani 1 1 d . . . H35 H 0.9922 0.0846 0.8187 0.035 Uiso 1 1 calc R . . C36 C 1.1528(2) 0.0697(2) 0.7701(2) 0.0333(6) Uani 1 1 d . . . H36 H 1.1916 0.0432 0.8305 0.040 Uiso 1 1 calc R . . C37 C 1.2148(2) 0.0832(2) 0.6892(2) 0.0355(6) Uani 1 1 d . . . H37 H 1.2958 0.0672 0.6942 0.043 Uiso 1 1 calc R . . C38 C 1.1584(2) 0.1200(2) 0.6015(2) 0.0343(6) Uani 1 1 d . . . H38 H 1.2011 0.1273 0.5456 0.041 Uiso 1 1 calc R . . C39 C 1.0393(2) 0.1467(2) 0.59427(19) 0.0298(6) Uani 1 1 d . . . H39 H 1.0011 0.1734 0.5337 0.036 Uiso 1 1 calc R . . C40 C 0.4510(2) 0.30851(18) 0.65986(17) 0.0222(5) Uani 1 1 d . . . C41 C 0.4958(2) 0.35654(19) 0.58446(18) 0.0274(5) Uani 1 1 d . . . H41 H 0.5669 0.3685 0.5942 0.033 Uiso 1 1 calc R . . C42 C 0.4384(2) 0.3870(2) 0.49584(18) 0.0300(6) Uani 1 1 d . . . H42 H 0.4708 0.4183 0.4450 0.036 Uiso 1 1 calc R . . C43 C 0.3338(2) 0.3718(2) 0.48139(18) 0.0309(6) Uani 1 1 d . . . H43 H 0.2930 0.3949 0.4214 0.037 Uiso 1 1 calc R . . C44 C 0.2890(2) 0.3229(2) 0.55440(19) 0.0329(6) Uani 1 1 d . . . H44 H 0.2179 0.3111 0.5440 0.040 Uiso 1 1 calc R . . C45 C 0.3469(2) 0.29100(19) 0.64252(18) 0.0279(5) Uani 1 1 d . . . H45 H 0.3156 0.2567 0.6919 0.034 Uiso 1 1 calc R . . C46 C 0.4228(2) 0.37395(19) 0.85266(17) 0.0249(5) Uani 1 1 d . . . C47 C 0.3290(2) 0.4541(2) 0.81305(19) 0.0304(6) Uani 1 1 d . . . H47 H 0.3129 0.4586 0.7453 0.036 Uiso 1 1 calc R . . C48 C 0.2579(2) 0.5282(2) 0.8718(2) 0.0380(7) Uani 1 1 d . . . H48 H 0.1944 0.5834 0.8437 0.046 Uiso 1 1 calc R . . C49 C 0.2793(3) 0.5217(2) 0.9702(2) 0.0398(7) Uani 1 1 d . . . H49 H 0.2303 0.5718 1.0101 0.048 Uiso 1 1 calc R . . C50 C 0.3726(2) 0.4417(2) 1.0109(2) 0.0395(7) Uani 1 1 d . . . H50 H 0.3878 0.4374 1.0788 0.047 Uiso 1 1 calc R . . C51 C 0.4431(2) 0.3686(2) 0.95314(19) 0.0344(6) Uani 1 1 d . . . H51 H 0.5066 0.3138 0.9818 0.041 Uiso 1 1 calc R . . H7 H 0.8761(16) 0.397(2) 0.7318(15) 0.034(7) Uiso 1 1 d D . . H10 H 0.8872(16) 0.0766(11) 1.0127(17) 0.026(7) Uiso 1 1 d D . . H12A H 0.7925(19) 0.0679(11) 0.8696(16) 0.025(6) Uiso 1 1 d D . . H12B H 0.6818(14) 0.127(2) 0.9331(19) 0.041(8) 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 0.02210(10) 0.02186(11) 0.02099(10) -0.00031(7) 0.00139(7) -0.00742(7) P1 0.0214(3) 0.0213(3) 0.0210(3) -0.0012(2) 0.0021(2) -0.0062(2) O1 0.0502(12) 0.0250(10) 0.0407(11) 0.0056(8) -0.0052(9) -0.0114(9) N1 0.0252(10) 0.0263(11) 0.0281(11) -0.0033(8) 0.0003(9) -0.0102(9) C1 0.0278(13) 0.0302(14) 0.0254(13) -0.0012(10) -0.0002(10) -0.0106(11) P2 0.0223(3) 0.0222(3) 0.0216(3) -0.0001(2) 0.0015(2) -0.0079(2) O2 0.0236(8) 0.0210(8) 0.0255(9) -0.0004(6) 0.0033(7) -0.0059(7) N2 0.0287(11) 0.0282(11) 0.0240(11) 0.0009(8) -0.0013(9) -0.0092(9) C2 0.0263(12) 0.0228(12) 0.0255(12) -0.0039(9) 0.0049(10) -0.0077(10) C3 0.0271(13) 0.0348(15) 0.0337(14) -0.0079(11) -0.0007(11) -0.0098(11) C4 0.0275(13) 0.0336(14) 0.0315(14) -0.0035(11) -0.0038(11) -0.0072(11) C5 0.0366(16) 0.0506(19) 0.0525(19) -0.0037(14) -0.0055(14) -0.0204(14) C6 0.055(2) 0.053(2) 0.0420(18) 0.0068(14) -0.0179(15) -0.0183(16) C7 0.0319(14) 0.0313(14) 0.0301(14) -0.0003(11) 0.0043(11) -0.0137(11) C8 0.0439(17) 0.0293(15) 0.0491(17) -0.0011(12) 0.0096(14) -0.0113(13) C9 0.0401(16) 0.0422(17) 0.0395(16) -0.0062(12) 0.0126(13) -0.0203(13) C10 0.0333(14) 0.0296(14) 0.0280(13) 0.0060(10) -0.0045(11) -0.0110(11) C11 0.0473(17) 0.0447(17) 0.0265(14) 0.0023(12) 0.0015(12) -0.0229(14) C12 0.0292(13) 0.0291(14) 0.0283(13) 0.0027(10) -0.0024(11) -0.0109(11) C13 0.0214(12) 0.0263(13) 0.0230(12) 0.0016(9) -0.0023(9) -0.0092(10) C14 0.0241(12) 0.0318(14) 0.0249(12) -0.0011(10) 0.0017(10) -0.0093(10) C15 0.0264(13) 0.0399(15) 0.0270(13) 0.0059(11) 0.0017(11) -0.0146(11) C16 0.0296(13) 0.0283(14) 0.0352(14) 0.0071(11) -0.0037(11) -0.0144(11) C17 0.0238(12) 0.0252(13) 0.0317(13) 0.0005(10) -0.0032(10) -0.0094(10) C18 0.0201(11) 0.0262(13) 0.0246(12) 0.0014(9) -0.0008(9) -0.0087(10) C19 0.0303(13) 0.0210(12) 0.0396(15) -0.0028(10) 0.0013(11) -0.0105(10) C20 0.0457(17) 0.0231(14) 0.063(2) -0.0018(13) 0.0121(15) -0.0128(13) C21 0.0365(15) 0.0397(16) 0.0474(17) -0.0144(13) -0.0002(13) -0.0156(13) C22 0.0294(13) 0.0237(12) 0.0247(12) -0.0011(9) -0.0005(10) -0.0092(10) C23 0.0365(14) 0.0206(13) 0.0308(13) -0.0021(10) 0.0026(11) -0.0074(11) C24 0.0307(13) 0.0245(13) 0.0285(13) -0.0029(10) 0.0022(11) 0.0002(10) C25 0.0252(12) 0.0281(13) 0.0266(13) -0.0012(10) 0.0033(10) -0.0065(10) C26 0.0263(12) 0.0229(12) 0.0214(12) -0.0009(9) 0.0014(10) -0.0072(10) C27 0.0243(12) 0.0224(12) 0.0209(12) -0.0005(9) -0.0005(9) -0.0036(10) C28 0.0211(12) 0.0280(13) 0.0241(12) -0.0004(10) 0.0000(10) -0.0066(10) C29 0.0381(15) 0.0272(14) 0.0266(13) -0.0031(10) 0.0059(11) -0.0095(11) C30 0.0434(16) 0.0275(14) 0.0298(14) 0.0036(11) 0.0047(12) -0.0083(12) C31 0.0458(17) 0.0391(16) 0.0245(13) 0.0060(11) 0.0002(12) -0.0095(13) C32 0.0453(16) 0.0415(16) 0.0276(14) -0.0038(12) -0.0036(12) -0.0170(13) C33 0.0368(14) 0.0292(14) 0.0279(13) 0.0019(10) -0.0020(11) -0.0128(11) C34 0.0215(12) 0.0235(12) 0.0286(13) -0.0054(10) 0.0029(10) -0.0069(10) C35 0.0291(13) 0.0253(13) 0.0309(14) -0.0031(10) 0.0016(11) -0.0071(10) C36 0.0297(14) 0.0275(14) 0.0407(15) -0.0031(11) -0.0072(12) -0.0062(11) C37 0.0221(13) 0.0300(14) 0.0540(18) -0.0096(12) 0.0003(12) -0.0065(11) C38 0.0306(14) 0.0318(14) 0.0437(16) -0.0095(12) 0.0115(12) -0.0132(11) C39 0.0271(13) 0.0302(14) 0.0309(14) -0.0011(10) 0.0028(11) -0.0077(11) C40 0.0229(12) 0.0188(12) 0.0231(12) -0.0024(9) 0.0013(9) -0.0040(9) C41 0.0268(13) 0.0262(13) 0.0292(13) -0.0009(10) 0.0032(10) -0.0087(10) C42 0.0357(14) 0.0314(14) 0.0238(13) 0.0006(10) 0.0033(11) -0.0123(11) C43 0.0351(14) 0.0311(14) 0.0255(13) -0.0009(10) -0.0064(11) -0.0096(11) C44 0.0313(14) 0.0361(15) 0.0339(14) -0.0023(11) -0.0065(11) -0.0143(12) C45 0.0283(13) 0.0285(13) 0.0279(13) 0.0013(10) -0.0001(10) -0.0110(11) C46 0.0254(12) 0.0248(13) 0.0276(13) -0.0057(10) 0.0069(10) -0.0118(10) C47 0.0337(14) 0.0264(13) 0.0311(14) -0.0027(10) 0.0067(11) -0.0096(11) C48 0.0389(15) 0.0241(14) 0.0473(17) -0.0023(12) 0.0125(13) -0.0052(12) C49 0.0454(17) 0.0340(15) 0.0452(17) -0.0170(13) 0.0233(14) -0.0178(13) C50 0.0417(16) 0.0529(19) 0.0313(15) -0.0158(13) 0.0105(13) -0.0232(14) C51 0.0296(14) 0.0414(16) 0.0321(14) -0.0093(12) 0.0049(11) -0.0102(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 C1 1.866(3) . ? Ru1 C2 2.056(2) . ? Ru1 C12 2.196(2) . ? Ru1 P1 2.3414(6) . ? Ru1 P2 2.4558(6) . ? P1 C40 1.837(2) . ? P1 C13 1.837(2) . ? P1 C46 1.849(2) . ? O1 C1 1.166(3) . ? N1 C2 1.370(3) . ? N1 C3 1.404(3) . ? N1 C7 1.472(3) . ? P2 C28 1.840(2) . ? P2 C34 1.848(2) . ? P2 C26 1.856(2) . ? O2 C27 1.386(3) . ? O2 C18 1.387(3) . ? N2 C2 1.351(3) . ? N2 C4 1.399(3) . ? N2 C10 1.483(3) . ? C3 C4 1.350(4) . ? C3 C5 1.492(4) . ? C4 C6 1.484(4) . ? C7 C9 1.521(4) . ? C7 C8 1.523(4) . ? C10 C11 1.512(4) . ? C10 C12 1.535(4) . ? C13 C18 1.387(3) . ? C13 C14 1.399(3) . ? C14 C15 1.388(4) . ? C15 C16 1.395(4) . ? C16 C17 1.391(3) . ? C17 C18 1.392(3) . ? C17 C19 1.529(3) . ? C19 C22 1.532(3) . ? C19 C20 1.533(4) . ? C19 C21 1.540(4) . ? C22 C27 1.390(3) . ? C22 C23 1.393(3) . ? C23 C24 1.383(4) . ? C24 C25 1.390(4) . ? C25 C26 1.403(3) . ? C26 C27 1.396(3) . ? C28 C33 1.391(3) . ? C28 C29 1.397(3) . ? C29 C30 1.385(4) . ? C30 C31 1.391(4) . ? C31 C32 1.376(4) . ? C32 C33 1.385(4) . ? C34 C35 1.392(3) . ? C34 C39 1.401(3) . ? C35 C36 1.391(4) . ? C36 C37 1.387(4) . ? C37 C38 1.377(4) . ? C38 C39 1.392(4) . ? C40 C41 1.397(3) . ? C40 C45 1.398(3) . ? C41 C42 1.384(3) . ? C42 C43 1.382(4) . ? C43 C44 1.381(4) . ? C44 C45 1.383(4) . ? C46 C47 1.385(4) . ? C46 C51 1.402(4) . ? C47 C48 1.396(4) . ? C48 C49 1.374(4) . ? C49 C50 1.385(4) . ? C50 C51 1.377(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 C1 Ru1 C2 96.69(10) . . ? C1 Ru1 C12 165.44(10) . . ? C2 Ru1 C12 77.35(9) . . ? C1 Ru1 P1 89.40(8) . . ? C2 Ru1 P1 160.43(7) . . ? C12 Ru1 P1 92.21(7) . . ? C1 Ru1 P2 103.15(8) . . ? C2 Ru1 P2 93.41(7) . . ? C12 Ru1 P2 90.56(7) . . ? P1 Ru1 P2 103.32(2) . . ? C40 P1 C13 99.34(11) . . ? C40 P1 C46 100.67(11) . . ? C13 P1 C46 101.58(11) . . ? C40 P1 Ru1 122.30(8) . . ? C13 P1 Ru1 117.36(8) . . ? C46 P1 Ru1 112.41(8) . . ? C2 N1 C3 110.6(2) . . ? C2 N1 C7 122.3(2) . . ? C3 N1 C7 127.0(2) . . ? O1 C1 Ru1 170.9(2) . . ? C28 P2 C34 100.59(11) . . ? C28 P2 C26 101.72(11) . . ? C34 P2 C26 96.92(11) . . ? C28 P2 Ru1 118.59(8) . . ? C34 P2 Ru1 114.44(8) . . ? C26 P2 Ru1 120.73(8) . . ? C27 O2 C18 114.11(18) . . ? C2 N2 C4 112.0(2) . . ? C2 N2 C10 119.8(2) . . ? C4 N2 C10 128.1(2) . . ? N2 C2 N1 104.3(2) . . ? N2 C2 Ru1 117.56(17) . . ? N1 C2 Ru1 137.95(18) . . ? C4 C3 N1 106.9(2) . . ? C4 C3 C5 127.8(3) . . ? N1 C3 C5 125.3(2) . . ? C3 C4 N2 106.2(2) . . ? C3 C4 C6 130.7(3) . . ? N2 C4 C6 123.0(2) . . ? N1 C7 C9 113.3(2) . . ? N1 C7 C8 111.9(2) . . ? C9 C7 C8 111.8(2) . . ? N2 C10 C11 109.9(2) . . ? N2 C10 C12 107.1(2) . . ? C11 C10 C12 113.9(2) . . ? C10 C12 Ru1 110.28(17) . . ? C18 C13 C14 116.8(2) . . ? C18 C13 P1 115.96(17) . . ? C14 C13 P1 127.17(19) . . ? C15 C14 C13 120.4(2) . . ? C14 C15 C16 120.6(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 116.7(2) . . ? C16 C17 C19 125.8(2) . . ? C18 C17 C19 117.4(2) . . ? O2 C18 C13 115.4(2) . . ? O2 C18 C17 119.9(2) . . ? C13 C18 C17 124.7(2) . . ? C17 C19 C22 106.61(19) . . ? C17 C19 C20 111.4(2) . . ? C22 C19 C20 112.5(2) . . ? C17 C19 C21 108.6(2) . . ? C22 C19 C21 108.1(2) . . ? C20 C19 C21 109.5(2) . . ? C27 C22 C23 117.1(2) . . ? C27 C22 C19 117.9(2) . . ? C23 C22 C19 125.0(2) . . ? C24 C23 C22 120.7(2) . . ? C23 C24 C25 120.7(2) . . ? C24 C25 C26 120.9(2) . . ? C27 C26 C25 116.2(2) . . ? C27 C26 P2 119.71(17) . . ? C25 C26 P2 123.94(18) . . ? O2 C27 C22 119.5(2) . . ? O2 C27 C26 116.1(2) . . ? C22 C27 C26 124.4(2) . . ? C33 C28 C29 118.1(2) . . ? C33 C28 P2 123.87(19) . . ? C29 C28 P2 117.98(18) . . ? C30 C29 C28 121.0(2) . . ? C29 C30 C31 119.6(2) . . ? C32 C31 C30 120.0(2) . . ? C31 C32 C33 120.1(3) . . ? C32 C33 C28 121.1(2) . . ? C35 C34 C39 118.4(2) . . ? C35 C34 P2 117.72(18) . . ? C39 C34 P2 123.85(19) . . ? C36 C35 C34 120.8(2) . . ? C37 C36 C35 120.1(3) . . ? C38 C37 C36 119.8(2) . . ? C37 C38 C39 120.5(2) . . ? C38 C39 C34 120.4(2) . . ? C41 C40 C45 117.8(2) . . ? C41 C40 P1 120.12(18) . . ? C45 C40 P1 122.01(18) . . ? C42 C41 C40 121.2(2) . . ? C43 C42 C41 120.0(2) . . ? C44 C43 C42 119.8(2) . . ? C43 C44 C45 120.4(2) . . ? C44 C45 C40 120.9(2) . . ? C47 C46 C51 118.3(2) . . ? C47 C46 P1 123.18(19) . . ? C51 C46 P1 118.53(19) . . ? C46 C47 C48 120.6(3) . . ? C49 C48 C47 120.3(3) . . ? C48 C49 C50 119.8(3) . . ? C51 C50 C49 120.1(3) . . ? C50 C51 C46 121.0(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.583 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.073 #===END data_k08mkw35 _database_code_depnum_ccdc_archive 'CCDC 723436' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H58 N2 O2 P2 Ru' _chemical_formula_weight 942.04 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8270(1) _cell_length_b 11.6570(2) _cell_length_c 20.7780(4) _cell_angle_alpha 81.022(1) _cell_angle_beta 85.197(1) _cell_angle_gamma 65.431(1) _cell_volume 2355.23(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51282 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 46023 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.45 _reflns_number_total 10691 _reflns_number_gt 7679 _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^)+(0.0589P)^2^+0.8829P] 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 0.0026(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10691 _refine_ls_number_parameters 570 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.74445(3) 0.00283(2) 0.284332(13) 0.02365(10) Uani 1 1 d D . . P1 P 0.82524(9) 0.12926(8) 0.20554(4) 0.0254(2) Uani 1 1 d . . . P2 P 0.51934(8) 0.13812(8) 0.29933(4) 0.02344(19) Uani 1 1 d . . . O1 O 0.8270(3) 0.1045(2) 0.39245(13) 0.0439(7) Uani 1 1 d . . . O2 O 0.6204(2) 0.3342(2) 0.26529(10) 0.0248(5) Uani 1 1 d . . . N1 N 0.9557(3) -0.2364(3) 0.22200(13) 0.0281(6) Uani 1 1 d . . . N2 N 1.0052(3) -0.2475(2) 0.32153(14) 0.0275(6) Uani 1 1 d . . . C1 C 0.8018(4) 0.0594(3) 0.35211(17) 0.0299(8) Uani 1 1 d . . . C2 C 0.9138(3) -0.1697(3) 0.27517(16) 0.0254(7) Uani 1 1 d . . . C3 C 1.0675(4) -0.3496(3) 0.23689(19) 0.0352(8) Uani 1 1 d . . . H3 H 1.1136 -0.4110 0.2082 0.042 Uiso 1 1 calc R . . C4 C 1.0992(4) -0.3576(3) 0.29817(18) 0.0339(8) Uani 1 1 d . . . H4 H 1.1717 -0.4251 0.3216 0.041 Uiso 1 1 calc R . . C5 C 0.8797(4) -0.2041(3) 0.16172(16) 0.0335(8) Uani 1 1 d . . . H5 H 0.8335 -0.1092 0.1524 0.040 Uiso 1 1 calc R . . C6 C 0.9713(5) -0.2527(4) 0.10324(18) 0.0450(10) Uani 1 1 d . . . H6A H 1.0165 -0.3468 0.1104 0.054 Uiso 1 1 calc R . . H6B H 1.0423 -0.2190 0.0974 0.054 Uiso 1 1 calc R . . C7 C 0.8841(6) -0.2083(5) 0.0423(2) 0.0645(14) Uani 1 1 d . . . H7A H 0.8445 -0.1142 0.0339 0.077 Uiso 1 1 calc R . . H7B H 0.9425 -0.2412 0.0043 0.077 Uiso 1 1 calc R . . C8 C 0.7703(6) -0.2541(5) 0.0499(2) 0.0695(15) Uani 1 1 d . . . H8A H 0.7127 -0.2186 0.0110 0.083 Uiso 1 1 calc R . . H8B H 0.8098 -0.3480 0.0530 0.083 Uiso 1 1 calc R . . C9 C 0.6835(5) -0.2135(5) 0.1103(2) 0.0565(12) Uani 1 1 d . . . H9A H 0.6159 -0.2513 0.1163 0.068 Uiso 1 1 calc R . . H9B H 0.6337 -0.1197 0.1046 0.068 Uiso 1 1 calc R . . C10 C 0.7710(4) -0.2562(4) 0.17014(19) 0.0418(9) Uani 1 1 d . . . H10A H 0.8148 -0.3503 0.1778 0.050 Uiso 1 1 calc R . . H10B H 0.7130 -0.2261 0.2087 0.050 Uiso 1 1 calc R . . C11 C 0.9943(4) -0.2348(3) 0.39149(16) 0.0288(7) Uani 1 1 d . . . H11 H 0.9319 -0.1448 0.3964 0.035 Uiso 1 1 calc R . . C12 C 1.1294(4) -0.2615(4) 0.41959(18) 0.0350(8) Uani 1 1 d . . . H12A H 1.1654 -0.2004 0.3966 0.042 Uiso 1 1 calc R . . H12B H 1.1952 -0.3485 0.4130 0.042 Uiso 1 1 calc R . . C13 C 1.1134(4) -0.2495(4) 0.49220(19) 0.0406(9) Uani 1 1 d . . . H13A H 1.2036 -0.2720 0.5103 0.049 Uiso 1 1 calc R . . H13B H 1.0553 -0.1601 0.4983 0.049 Uiso 1 1 calc R . . C14 C 1.0502(4) -0.3361(4) 0.52923(19) 0.0427(9) Uani 1 1 d . . . H14A H 1.1126 -0.4261 0.5270 0.051 Uiso 1 1 calc R . . H14B H 1.0365 -0.3226 0.5756 0.051 Uiso 1 1 calc R . . C15 C 0.9147(4) -0.3086(4) 0.50043(19) 0.0411(9) Uani 1 1 d . . . H15A H 0.8494 -0.2214 0.5069 0.049 Uiso 1 1 calc R . . H15B H 0.8779 -0.3690 0.5236 0.049 Uiso 1 1 calc R . . C16 C 0.9291(4) -0.3207(4) 0.42811(18) 0.0358(8) Uani 1 1 d . . . H16A H 0.8385 -0.2967 0.4102 0.043 Uiso 1 1 calc R . . H16B H 0.9860 -0.4103 0.4219 0.043 Uiso 1 1 calc R . . C17 C 0.7408(3) 0.3495(3) 0.26397(16) 0.0261(7) Uani 1 1 d . . . C18 C 0.8504(3) 0.2609(3) 0.23323(16) 0.0264(7) Uani 1 1 d . . . C19 C 0.9717(4) 0.2783(3) 0.22965(18) 0.0327(8) Uani 1 1 d . . . H19 H 1.0494 0.2222 0.2083 0.039 Uiso 1 1 calc R . . C20 C 0.9794(4) 0.3762(3) 0.25677(19) 0.0358(9) Uani 1 1 d . . . H20 H 1.0625 0.3862 0.2539 0.043 Uiso 1 1 calc R . . C21 C 0.8682(4) 0.4597(3) 0.28796(18) 0.0313(8) Uani 1 1 d . . . H21 H 0.8762 0.5253 0.3070 0.038 Uiso 1 1 calc R . . C22 C 0.7444(3) 0.4485(3) 0.29173(17) 0.0287(7) Uani 1 1 d . . . C23 C 0.6127(4) 0.5361(3) 0.32257(18) 0.0310(8) Uani 1 1 d . . . C24 C 0.5440(3) 0.4507(3) 0.35650(17) 0.0273(7) Uani 1 1 d . . . C25 C 0.4707(4) 0.4659(3) 0.41513(18) 0.0335(8) Uani 1 1 d . . . H25 H 0.4665 0.5298 0.4397 0.040 Uiso 1 1 calc R . . C26 C 0.4038(4) 0.3884(3) 0.43789(17) 0.0345(8) Uani 1 1 d . . . H26 H 0.3541 0.3996 0.4780 0.041 Uiso 1 1 calc R . . C27 C 0.4081(4) 0.2946(3) 0.40297(17) 0.0311(8) Uani 1 1 d . . . H27 H 0.3594 0.2441 0.4189 0.037 Uiso 1 1 calc R . . C28 C 0.4832(3) 0.2735(3) 0.34474(16) 0.0250(7) Uani 1 1 d . . . C29 C 0.5473(3) 0.3546(3) 0.32351(16) 0.0261(7) Uani 1 1 d . . . C30 C 0.5172(4) 0.6279(3) 0.2685(2) 0.0408(9) Uani 1 1 d . . . H30A H 0.5564 0.6861 0.2464 0.061 Uiso 1 1 calc R . . H30B H 0.4285 0.6771 0.2878 0.061 Uiso 1 1 calc R . . H30C H 0.5058 0.5790 0.2369 0.061 Uiso 1 1 calc R . . C31 C 0.6364(4) 0.6138(4) 0.3691(2) 0.0449(10) Uani 1 1 d . . . H31A H 0.6948 0.5562 0.4044 0.067 Uiso 1 1 calc R . . H31B H 0.5490 0.6686 0.3875 0.067 Uiso 1 1 calc R . . H31C H 0.6804 0.6666 0.3454 0.067 Uiso 1 1 calc R . . C32 C 0.9991(3) 0.0382(3) 0.17566(18) 0.0302(8) Uani 1 1 d . . . C33 C 1.0327(4) 0.0231(3) 0.1102(2) 0.0392(9) Uani 1 1 d . . . H33 H 0.9658 0.0656 0.0778 0.047 Uiso 1 1 calc R . . C34 C 1.1647(5) -0.0542(4) 0.0927(2) 0.0538(12) Uani 1 1 d . . . H34 H 1.1869 -0.0658 0.0483 0.065 Uiso 1 1 calc R . . C35 C 1.2634(5) -0.1142(4) 0.1386(3) 0.0599(14) Uani 1 1 d . . . H35 H 1.3534 -0.1666 0.1261 0.072 Uiso 1 1 calc R . . C36 C 1.2305(4) -0.0977(4) 0.2034(3) 0.0574(13) Uani 1 1 d . . . H36 H 1.2990 -0.1376 0.2352 0.069 Uiso 1 1 calc R . . C37 C 1.0992(4) -0.0238(3) 0.2223(2) 0.0392(9) Uani 1 1 d . . . H37 H 1.0772 -0.0154 0.2671 0.047 Uiso 1 1 calc R . . C38 C 0.7379(3) 0.2106(3) 0.12844(17) 0.0305(8) Uani 1 1 d . . . C39 C 0.6568(4) 0.1639(4) 0.10301(17) 0.0341(8) Uani 1 1 d . . . H39 H 0.6428 0.0937 0.1268 0.041 Uiso 1 1 calc R . . C40 C 0.5956(4) 0.2181(4) 0.04323(19) 0.0455(10) Uani 1 1 d . . . H40 H 0.5410 0.1842 0.0261 0.055 Uiso 1 1 calc R . . C41 C 0.6140(5) 0.3212(4) 0.0086(2) 0.0531(12) Uani 1 1 d . . . H41 H 0.5715 0.3589 -0.0321 0.064 Uiso 1 1 calc R . . C42 C 0.6940(5) 0.3691(4) 0.0333(2) 0.0583(13) Uani 1 1 d . . . H42 H 0.7069 0.4399 0.0094 0.070 Uiso 1 1 calc R . . C43 C 0.7558(5) 0.3149(4) 0.09268(19) 0.0451(10) Uani 1 1 d . . . H43 H 0.8109 0.3487 0.1093 0.054 Uiso 1 1 calc R . . C44 C 0.4134(4) 0.0676(3) 0.35002(16) 0.0278(7) Uani 1 1 d . . . C45 C 0.4689(4) -0.0190(3) 0.40495(18) 0.0348(8) Uani 1 1 d . . . H45 H 0.5635 -0.0505 0.4124 0.042 Uiso 1 1 calc R . . C46 C 0.3862(4) -0.0599(4) 0.44933(19) 0.0420(10) Uani 1 1 d . . . H46 H 0.4247 -0.1177 0.4872 0.050 Uiso 1 1 calc R . . C47 C 0.2503(4) -0.0173(4) 0.4387(2) 0.0432(10) Uani 1 1 d . . . H47 H 0.1950 -0.0457 0.4690 0.052 Uiso 1 1 calc R . . C48 C 0.1936(4) 0.0671(4) 0.38379(19) 0.0422(10) Uani 1 1 d . . . H48 H 0.0996 0.0956 0.3759 0.051 Uiso 1 1 calc R . . C49 C 0.2749(4) 0.1102(4) 0.34008(18) 0.0356(8) Uani 1 1 d . . . H49 H 0.2352 0.1696 0.3029 0.043 Uiso 1 1 calc R . . C50 C 0.4146(3) 0.2145(3) 0.22650(16) 0.0265(7) Uani 1 1 d . . . C51 C 0.3823(4) 0.1381(3) 0.19157(17) 0.0317(8) Uani 1 1 d . . . H51 H 0.4143 0.0494 0.2060 0.038 Uiso 1 1 calc R . . C52 C 0.3046(4) 0.1894(4) 0.13631(18) 0.0382(9) Uani 1 1 d . . . H52 H 0.2801 0.1368 0.1142 0.046 Uiso 1 1 calc R . . C53 C 0.2623(4) 0.3182(4) 0.11321(18) 0.0411(9) Uani 1 1 d . . . H53 H 0.2099 0.3535 0.0750 0.049 Uiso 1 1 calc R . . C54 C 0.2966(4) 0.3943(4) 0.14585(17) 0.0351(8) Uani 1 1 d . . . H54 H 0.2699 0.4818 0.1294 0.042 Uiso 1 1 calc R . . C55 C 0.3702(3) 0.3439(3) 0.20291(17) 0.0306(8) Uani 1 1 d . . . H55 H 0.3903 0.3979 0.2260 0.037 Uiso 1 1 calc R . . H1 H 0.677(3) -0.040(3) 0.2319(10) 0.027(9) Uiso 1 1 d D . . H2 H 0.710(4) -0.097(3) 0.3364(10) 0.053(12) 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 0.02299(16) 0.02450(15) 0.02237(16) -0.00315(10) 0.00098(10) -0.00891(11) P1 0.0228(4) 0.0258(4) 0.0247(5) -0.0017(3) 0.0018(3) -0.0081(4) P2 0.0224(4) 0.0265(4) 0.0213(4) -0.0037(3) 0.0014(3) -0.0101(4) O1 0.0565(19) 0.0412(15) 0.0375(16) -0.0098(12) -0.0116(13) -0.0199(14) O2 0.0229(12) 0.0297(12) 0.0233(12) -0.0052(9) 0.0020(9) -0.0121(10) N1 0.0291(16) 0.0294(15) 0.0257(15) -0.0065(12) 0.0022(12) -0.0113(13) N2 0.0267(15) 0.0219(14) 0.0307(16) -0.0047(11) -0.0018(12) -0.0063(12) C1 0.0290(19) 0.0243(17) 0.0300(19) 0.0028(14) 0.0009(15) -0.0071(15) C2 0.0265(18) 0.0285(17) 0.0224(17) -0.0044(13) 0.0006(13) -0.0125(14) C3 0.033(2) 0.0287(18) 0.039(2) -0.0112(15) 0.0050(16) -0.0066(16) C4 0.030(2) 0.0252(17) 0.041(2) -0.0099(15) -0.0012(16) -0.0035(15) C5 0.044(2) 0.0329(19) 0.0229(18) -0.0070(14) 0.0037(16) -0.0149(17) C6 0.058(3) 0.042(2) 0.030(2) -0.0093(17) 0.0109(19) -0.016(2) C7 0.088(4) 0.059(3) 0.027(2) -0.008(2) 0.008(2) -0.013(3) C8 0.082(4) 0.082(4) 0.039(3) -0.021(2) -0.016(2) -0.021(3) C9 0.056(3) 0.074(3) 0.040(3) -0.014(2) -0.010(2) -0.023(2) C10 0.047(2) 0.049(2) 0.034(2) -0.0108(17) -0.0027(18) -0.021(2) C11 0.033(2) 0.0247(17) 0.0284(19) -0.0035(14) -0.0021(15) -0.0116(15) C12 0.033(2) 0.038(2) 0.036(2) -0.0030(16) -0.0045(16) -0.0175(17) C13 0.042(2) 0.044(2) 0.038(2) -0.0023(17) -0.0102(17) -0.0196(19) C14 0.056(3) 0.042(2) 0.028(2) 0.0033(16) -0.0047(18) -0.019(2) C15 0.047(2) 0.037(2) 0.041(2) -0.0022(17) 0.0036(18) -0.0203(19) C16 0.038(2) 0.037(2) 0.036(2) -0.0039(16) -0.0019(16) -0.0186(17) C17 0.0248(18) 0.0270(17) 0.0243(17) 0.0031(13) -0.0036(13) -0.0102(14) C18 0.0268(18) 0.0262(17) 0.0242(17) 0.0028(13) -0.0005(13) -0.0110(14) C19 0.0249(18) 0.0298(18) 0.039(2) 0.0029(15) 0.0023(15) -0.0102(15) C20 0.0265(19) 0.036(2) 0.047(2) 0.0043(16) -0.0020(16) -0.0180(16) C21 0.032(2) 0.0254(17) 0.037(2) 0.0031(14) -0.0068(15) -0.0131(15) C22 0.0288(19) 0.0251(17) 0.0300(19) 0.0038(14) -0.0063(14) -0.0105(14) C23 0.0263(19) 0.0246(17) 0.040(2) -0.0049(15) -0.0037(15) -0.0076(15) C24 0.0243(18) 0.0234(16) 0.0309(19) -0.0061(14) -0.0021(14) -0.0054(14) C25 0.032(2) 0.0298(18) 0.037(2) -0.0131(15) -0.0023(16) -0.0070(16) C26 0.037(2) 0.041(2) 0.0243(19) -0.0105(15) 0.0064(15) -0.0137(17) C27 0.0285(19) 0.0337(18) 0.0303(19) -0.0058(15) 0.0053(15) -0.0125(15) C28 0.0229(17) 0.0265(17) 0.0228(17) -0.0026(13) -0.0009(13) -0.0076(14) C29 0.0230(17) 0.0258(17) 0.0244(17) -0.0018(13) -0.0016(13) -0.0053(14) C30 0.034(2) 0.0294(19) 0.053(3) 0.0064(17) -0.0057(18) -0.0103(17) C31 0.041(2) 0.039(2) 0.060(3) -0.0197(19) 0.003(2) -0.0186(19) C32 0.0269(19) 0.0234(16) 0.038(2) -0.0027(14) 0.0080(15) -0.0103(14) C33 0.037(2) 0.033(2) 0.043(2) -0.0059(16) 0.0127(17) -0.0127(17) C34 0.051(3) 0.041(2) 0.063(3) -0.014(2) 0.030(2) -0.015(2) C35 0.035(3) 0.035(2) 0.094(4) -0.008(2) 0.026(3) -0.0049(19) C36 0.027(2) 0.034(2) 0.098(4) 0.013(2) -0.002(2) -0.0058(18) C37 0.032(2) 0.0300(19) 0.048(2) 0.0078(17) -0.0004(17) -0.0097(16) C38 0.0252(18) 0.0283(17) 0.0282(19) -0.0027(14) 0.0016(14) -0.0021(14) C39 0.0291(19) 0.040(2) 0.0263(19) -0.0059(15) 0.0018(15) -0.0070(16) C40 0.036(2) 0.057(3) 0.033(2) -0.0136(19) 0.0005(17) -0.0073(19) C41 0.051(3) 0.060(3) 0.027(2) -0.0035(19) -0.0093(19) -0.001(2) C42 0.075(3) 0.047(3) 0.038(3) 0.0120(19) -0.009(2) -0.015(2) C43 0.058(3) 0.042(2) 0.031(2) 0.0038(17) -0.0030(19) -0.019(2) C44 0.034(2) 0.0272(17) 0.0252(18) -0.0071(14) 0.0062(14) -0.0149(15) C45 0.035(2) 0.0338(19) 0.032(2) -0.0029(15) 0.0054(16) -0.0114(16) C46 0.050(3) 0.037(2) 0.035(2) 0.0009(16) 0.0099(18) -0.0169(19) C47 0.056(3) 0.045(2) 0.040(2) -0.0099(18) 0.0161(19) -0.034(2) C48 0.037(2) 0.062(3) 0.040(2) -0.017(2) 0.0086(18) -0.031(2) C49 0.036(2) 0.045(2) 0.030(2) -0.0075(16) 0.0038(16) -0.0203(18) C50 0.0193(16) 0.0375(19) 0.0222(17) -0.0054(14) 0.0031(13) -0.0112(14) C51 0.032(2) 0.039(2) 0.0261(19) -0.0051(15) 0.0001(15) -0.0161(16) C52 0.039(2) 0.054(2) 0.028(2) -0.0132(17) 0.0002(16) -0.0236(19) C53 0.034(2) 0.054(2) 0.027(2) -0.0070(17) -0.0046(16) -0.0074(18) C54 0.0281(19) 0.038(2) 0.0271(19) -0.0044(15) 0.0011(15) -0.0017(16) C55 0.0275(19) 0.0329(19) 0.0280(19) -0.0063(15) 0.0004(15) -0.0083(15) _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 1.892(4) . ? Ru1 C2 2.106(3) . ? Ru1 P2 2.3140(9) . ? Ru1 P1 2.3867(8) . ? Ru1 H1 1.61(3) . ? Ru1 H2 1.61(3) . ? P1 C38 1.842(4) . ? P1 C32 1.845(3) . ? P1 C18 1.847(3) . ? P2 C50 1.843(3) . ? P2 C44 1.848(3) . ? P2 C28 1.851(3) . ? O1 C1 1.161(4) . ? O2 C29 1.385(4) . ? O2 C17 1.385(4) . ? N1 C3 1.382(5) . ? N1 C2 1.386(4) . ? N1 C5 1.468(5) . ? N2 C2 1.368(4) . ? N2 C4 1.394(4) . ? N2 C11 1.474(4) . ? C3 C4 1.325(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C10 1.521(5) . ? C5 C6 1.525(5) . ? C5 H5 1.0000 . ? C6 C7 1.533(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.516(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.518(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.512(5) . ? C11 C16 1.529(5) . ? C11 H11 1.0000 . ? C12 C13 1.526(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.525(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.520(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.520(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.384(5) . ? C17 C18 1.394(5) . ? C18 C19 1.404(5) . ? C19 C20 1.383(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 C22 1.395(5) . ? C21 H21 0.9500 . ? C22 C23 1.525(5) . ? C23 C31 1.527(5) . ? C23 C24 1.533(5) . ? C23 C30 1.542(5) . ? C24 C29 1.389(5) . ? C24 C25 1.391(5) . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 C27 1.386(5) . ? C26 H26 0.9500 . ? C27 C28 1.395(5) . ? C27 H27 0.9500 . ? C28 C29 1.390(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.394(5) . ? C32 C33 1.397(5) . ? C33 C34 1.389(6) . ? C33 H33 0.9500 . ? C34 C35 1.372(7) . ? C34 H34 0.9500 . ? C35 C36 1.386(7) . ? C35 H35 0.9500 . ? C36 C37 1.382(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.383(5) . ? C38 C43 1.400(5) . ? C39 C40 1.388(5) . ? C39 H39 0.9500 . ? C40 C41 1.381(6) . ? C40 H40 0.9500 . ? C41 C42 1.376(7) . ? C41 H41 0.9500 . ? C42 C43 1.383(6) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.391(5) . ? C44 C49 1.392(5) . ? C45 C46 1.400(5) . ? C45 H45 0.9500 . ? C46 C47 1.369(6) . ? C46 H46 0.9500 . ? C47 C48 1.382(6) . ? C47 H47 0.9500 . ? C48 C49 1.395(5) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.395(5) . ? C50 C55 1.397(5) . ? C51 C52 1.383(5) . ? C51 H51 0.9500 . ? C52 C53 1.391(6) . ? C52 H52 0.9500 . ? C53 C54 1.374(5) . ? C53 H53 0.9500 . ? C54 C55 1.392(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 100.52(13) . . ? C1 Ru1 P2 92.46(10) . . ? C2 Ru1 P2 157.94(9) . . ? C1 Ru1 P1 89.96(10) . . ? C2 Ru1 P1 95.15(9) . . ? P2 Ru1 P1 102.68(3) . . ? C1 Ru1 H1 172.6(11) . . ? C2 Ru1 H1 84.7(12) . . ? P2 Ru1 H1 81.0(12) . . ? P1 Ru1 H1 94.8(9) . . ? C1 Ru1 H2 90.2(10) . . ? C2 Ru1 H2 77.1(14) . . ? P2 Ru1 H2 85.1(14) . . ? P1 Ru1 H2 172.2(15) . . ? H1 Ru1 H2 85.9(5) . . ? C38 P1 C32 101.22(16) . . ? C38 P1 C18 100.18(16) . . ? C32 P1 C18 99.46(15) . . ? C38 P1 Ru1 122.47(12) . . ? C32 P1 Ru1 112.58(11) . . ? C18 P1 Ru1 117.41(11) . . ? C50 P2 C44 101.46(15) . . ? C50 P2 C28 102.70(15) . . ? C44 P2 C28 97.76(14) . . ? C50 P2 Ru1 117.98(10) . . ? C44 P2 Ru1 116.14(11) . . ? C28 P2 Ru1 117.64(11) . . ? C29 O2 C17 114.1(2) . . ? C3 N1 C2 110.9(3) . . ? C3 N1 C5 123.2(3) . . ? C2 N1 C5 125.1(3) . . ? C2 N2 C4 111.8(3) . . ? C2 N2 C11 125.9(3) . . ? C4 N2 C11 121.2(3) . . ? O1 C1 Ru1 173.9(3) . . ? N2 C2 N1 102.7(3) . . ? N2 C2 Ru1 128.5(2) . . ? N1 C2 Ru1 128.7(2) . . ? C4 C3 N1 108.1(3) . . ? C4 C3 H3 126.0 . . ? N1 C3 H3 126.0 . . ? C3 C4 N2 106.5(3) . . ? C3 C4 H4 126.7 . . ? N2 C4 H4 126.7 . . ? N1 C5 C10 110.6(3) . . ? N1 C5 C6 112.6(3) . . ? C10 C5 C6 109.5(3) . . ? N1 C5 H5 108.0 . . ? C10 C5 H5 108.0 . . ? C6 C5 H5 108.0 . . ? C5 C6 C7 108.7(4) . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8 C7 C6 111.8(4) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 111.3(4) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 110.6(4) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 C5 111.1(3) . . ? C9 C10 H10A 109.4 . . ? C5 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C5 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 112.4(3) . . ? N2 C11 C16 109.3(3) . . ? C12 C11 C16 112.0(3) . . ? N2 C11 H11 107.7 . . ? C12 C11 H11 107.7 . . ? C16 C11 H11 107.7 . . ? C11 C12 C13 110.5(3) . . ? C11 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 111.5(3) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 110.7(3) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.5(3) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 110.6(3) . . ? C15 C16 H16A 109.5 . . ? C11 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C22 C17 O2 119.5(3) . . ? C22 C17 C18 125.3(3) . . ? O2 C17 C18 115.2(3) . . ? C17 C18 C19 115.7(3) . . ? C17 C18 P1 117.6(2) . . ? C19 C18 P1 126.7(3) . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C17 C22 C21 116.6(3) . . ? C17 C22 C23 117.2(3) . . ? C21 C22 C23 126.2(3) . . ? C22 C23 C31 112.6(3) . . ? C22 C23 C24 106.4(3) . . ? C31 C23 C24 112.4(3) . . ? C22 C23 C30 109.4(3) . . ? C31 C23 C30 108.9(3) . . ? C24 C23 C30 107.0(3) . . ? C29 C24 C25 116.9(3) . . ? C29 C24 C23 117.0(3) . . ? C25 C24 C23 126.0(3) . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 116.1(3) . . ? C29 C28 P2 117.9(2) . . ? C27 C28 P2 125.6(3) . . ? O2 C29 C24 119.3(3) . . ? O2 C29 C28 115.8(3) . . ? C24 C29 C28 124.9(3) . . ? C23 C30 H30A 109.5 . . ? C23 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C23 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C31 H31A 109.5 . . ? C23 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C23 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 119.3(3) . . ? C37 C32 P1 117.0(3) . . ? C33 C32 P1 123.7(3) . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C35 C34 C33 120.9(4) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.4(4) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 120.7(5) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C32 119.9(4) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C43 118.3(4) . . ? C39 C38 P1 119.3(3) . . ? C43 C38 P1 122.3(3) . . ? C38 C39 C40 121.0(4) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 119.9(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 119.8(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.4(4) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C38 120.5(4) . . ? C42 C43 H43 119.8 . . ? C38 C43 H43 119.8 . . ? C45 C44 C49 118.3(3) . . ? C45 C44 P2 119.1(3) . . ? C49 C44 P2 122.1(3) . . ? C44 C45 C46 120.3(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 120.6(4) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 120.0(3) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 119.7(4) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C44 C49 C48 121.1(4) . . ? C44 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C51 C50 C55 118.1(3) . . ? C51 C50 P2 118.2(3) . . ? C55 C50 P2 123.6(3) . . ? C52 C51 C50 121.1(4) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 119.9(4) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 119.8(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 120.3(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C50 120.6(3) . . ? C54 C55 H55 119.7 . . ? C50 C55 H55 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 P1 C38 -144.20(16) . . . . ? C2 Ru1 P1 C38 115.24(16) . . . . ? P2 Ru1 P1 C38 -51.69(13) . . . . ? C1 Ru1 P1 C32 94.85(17) . . . . ? C2 Ru1 P1 C32 -5.71(16) . . . . ? P2 Ru1 P1 C32 -172.63(13) . . . . ? C1 Ru1 P1 C18 -19.74(16) . . . . ? C2 Ru1 P1 C18 -120.30(15) . . . . ? P2 Ru1 P1 C18 72.78(13) . . . . ? C1 Ru1 P2 C50 142.21(16) . . . . ? C2 Ru1 P2 C50 -91.5(3) . . . . ? P1 Ru1 P2 C50 51.69(13) . . . . ? C1 Ru1 P2 C44 -97.05(16) . . . . ? C2 Ru1 P2 C44 29.3(3) . . . . ? P1 Ru1 P2 C44 172.43(12) . . . . ? C1 Ru1 P2 C28 18.21(15) . . . . ? C2 Ru1 P2 C28 144.5(3) . . . . ? P1 Ru1 P2 C28 -72.30(12) . . . . ? C2 Ru1 C1 O1 170(3) . . . . ? P2 Ru1 C1 O1 -28(3) . . . . ? P1 Ru1 C1 O1 74(3) . . . . ? C4 N2 C2 N1 -0.2(4) . . . . ? C11 N2 C2 N1 -168.2(3) . . . . ? C4 N2 C2 Ru1 176.4(2) . . . . ? C11 N2 C2 Ru1 8.4(5) . . . . ? C3 N1 C2 N2 0.3(3) . . . . ? C5 N1 C2 N2 170.3(3) . . . . ? C3 N1 C2 Ru1 -176.4(2) . . . . ? C5 N1 C2 Ru1 -6.3(5) . . . . ? C1 Ru1 C2 N2 27.2(3) . . . . ? P2 Ru1 C2 N2 -97.8(3) . . . . ? P1 Ru1 C2 N2 118.1(3) . . . . ? C1 Ru1 C2 N1 -157.0(3) . . . . ? P2 Ru1 C2 N1 78.0(4) . . . . ? P1 Ru1 C2 N1 -66.1(3) . . . . ? C2 N1 C3 C4 -0.2(4) . . . . ? C5 N1 C3 C4 -170.5(3) . . . . ? N1 C3 C4 N2 0.1(4) . . . . ? C2 N2 C4 C3 0.1(4) . . . . ? C11 N2 C4 C3 168.8(3) . . . . ? C3 N1 C5 C10 86.6(4) . . . . ? C2 N1 C5 C10 -82.3(4) . . . . ? C3 N1 C5 C6 -36.3(4) . . . . ? C2 N1 C5 C6 154.8(3) . . . . ? N1 C5 C6 C7 -177.0(3) . . . . ? C10 C5 C6 C7 59.5(4) . . . . ? C5 C6 C7 C8 -57.6(5) . . . . ? C6 C7 C8 C9 55.1(6) . . . . ? C7 C8 C9 C10 -53.9(6) . . . . ? C8 C9 C10 C5 57.0(5) . . . . ? N1 C5 C10 C9 174.9(3) . . . . ? C6 C5 C10 C9 -60.4(4) . . . . ? C2 N2 C11 C12 -140.1(3) . . . . ? C4 N2 C11 C12 53.0(4) . . . . ? C2 N2 C11 C16 95.0(4) . . . . ? C4 N2 C11 C16 -72.0(4) . . . . ? N2 C11 C12 C13 -179.0(3) . . . . ? C16 C11 C12 C13 -55.5(4) . . . . ? C11 C12 C13 C14 55.8(4) . . . . ? C12 C13 C14 C15 -56.1(4) . . . . ? C13 C14 C15 C16 55.9(4) . . . . ? C14 C15 C16 C11 -55.4(4) . . . . ? N2 C11 C16 C15 -179.3(3) . . . . ? C12 C11 C16 C15 55.5(4) . . . . ? C29 O2 C17 C22 -40.5(4) . . . . ? C29 O2 C17 C18 139.9(3) . . . . ? C22 C17 C18 C19 -1.6(5) . . . . ? O2 C17 C18 C19 177.9(3) . . . . ? C22 C17 C18 P1 175.2(3) . . . . ? O2 C17 C18 P1 -5.2(4) . . . . ? C38 P1 C18 C17 80.8(3) . . . . ? C32 P1 C18 C17 -175.9(3) . . . . ? Ru1 P1 C18 C17 -54.3(3) . . . . ? C38 P1 C18 C19 -102.8(3) . . . . ? C32 P1 C18 C19 0.6(3) . . . . ? Ru1 P1 C18 C19 122.2(3) . . . . ? C17 C18 C19 C20 1.5(5) . . . . ? P1 C18 C19 C20 -175.0(3) . . . . ? C18 C19 C20 C21 -0.1(6) . . . . ? C19 C20 C21 C22 -1.2(5) . . . . ? O2 C17 C22 C21 -179.2(3) . . . . ? C18 C17 C22 C21 0.4(5) . . . . ? O2 C17 C22 C23 0.0(5) . . . . ? C18 C17 C22 C23 179.5(3) . . . . ? C20 C21 C22 C17 1.1(5) . . . . ? C20 C21 C22 C23 -177.9(3) . . . . ? C17 C22 C23 C31 162.2(3) . . . . ? C21 C22 C23 C31 -18.8(5) . . . . ? C17 C22 C23 C24 38.6(4) . . . . ? C21 C22 C23 C24 -142.3(3) . . . . ? C17 C22 C23 C30 -76.6(4) . . . . ? C21 C22 C23 C30 102.4(4) . . . . ? C22 C23 C24 C29 -41.2(4) . . . . ? C31 C23 C24 C29 -164.8(3) . . . . ? C30 C23 C24 C29 75.7(4) . . . . ? C22 C23 C24 C25 143.5(4) . . . . ? C31 C23 C24 C25 19.8(5) . . . . ? C30 C23 C24 C25 -99.6(4) . . . . ? C29 C24 C25 C26 -0.8(5) . . . . ? C23 C24 C25 C26 174.5(3) . . . . ? C24 C25 C26 C27 -0.1(6) . . . . ? C25 C26 C27 C28 1.8(6) . . . . ? C26 C27 C28 C29 -2.4(5) . . . . ? C26 C27 C28 P2 170.5(3) . . . . ? C50 P2 C28 C29 -77.8(3) . . . . ? C44 P2 C28 C29 178.5(3) . . . . ? Ru1 P2 C28 C29 53.6(3) . . . . ? C50 P2 C28 C27 109.5(3) . . . . ? C44 P2 C28 C27 5.8(3) . . . . ? Ru1 P2 C28 C27 -119.2(3) . . . . ? C17 O2 C29 C24 37.6(4) . . . . ? C17 O2 C29 C28 -141.7(3) . . . . ? C25 C24 C29 O2 -179.2(3) . . . . ? C23 C24 C29 O2 5.1(5) . . . . ? C25 C24 C29 C28 0.1(5) . . . . ? C23 C24 C29 C28 -175.7(3) . . . . ? C27 C28 C29 O2 -179.3(3) . . . . ? P2 C28 C29 O2 7.3(4) . . . . ? C27 C28 C29 C24 1.5(5) . . . . ? P2 C28 C29 C24 -171.9(3) . . . . ? C38 P1 C32 C37 172.1(3) . . . . ? C18 P1 C32 C37 69.6(3) . . . . ? Ru1 P1 C32 C37 -55.4(3) . . . . ? C38 P1 C32 C33 -11.5(3) . . . . ? C18 P1 C32 C33 -113.9(3) . . . . ? Ru1 P1 C32 C33 121.0(3) . . . . ? C37 C32 C33 C34 0.7(5) . . . . ? P1 C32 C33 C34 -175.7(3) . . . . ? C32 C33 C34 C35 -1.3(6) . . . . ? C33 C34 C35 C36 0.3(7) . . . . ? C34 C35 C36 C37 1.4(6) . . . . ? C35 C36 C37 C32 -2.0(6) . . . . ? C33 C32 C37 C36 1.0(5) . . . . ? P1 C32 C37 C36 177.5(3) . . . . ? C32 P1 C38 C39 101.6(3) . . . . ? C18 P1 C38 C39 -156.5(3) . . . . ? Ru1 P1 C38 C39 -24.5(3) . . . . ? C32 P1 C38 C43 -75.2(3) . . . . ? C18 P1 C38 C43 26.7(3) . . . . ? Ru1 P1 C38 C43 158.7(3) . . . . ? C43 C38 C39 C40 0.6(5) . . . . ? P1 C38 C39 C40 -176.3(3) . . . . ? C38 C39 C40 C41 -0.8(6) . . . . ? C39 C40 C41 C42 0.6(6) . . . . ? C40 C41 C42 C43 -0.2(7) . . . . ? C41 C42 C43 C38 0.0(7) . . . . ? C39 C38 C43 C42 -0.2(6) . . . . ? P1 C38 C43 C42 176.6(3) . . . . ? C50 P2 C44 C45 168.4(3) . . . . ? C28 P2 C44 C45 -86.9(3) . . . . ? Ru1 P2 C44 C45 39.1(3) . . . . ? C50 P2 C44 C49 -20.2(3) . . . . ? C28 P2 C44 C49 84.5(3) . . . . ? Ru1 P2 C44 C49 -149.4(2) . . . . ? C49 C44 C45 C46 -1.1(5) . . . . ? P2 C44 C45 C46 170.7(3) . . . . ? C44 C45 C46 C47 1.3(6) . . . . ? C45 C46 C47 C48 -0.2(6) . . . . ? C46 C47 C48 C49 -1.1(6) . . . . ? C45 C44 C49 C48 -0.3(5) . . . . ? P2 C44 C49 C48 -171.8(3) . . . . ? C47 C48 C49 C44 1.4(6) . . . . ? C44 P2 C50 C51 -59.2(3) . . . . ? C28 P2 C50 C51 -159.9(3) . . . . ? Ru1 P2 C50 C51 68.9(3) . . . . ? C44 P2 C50 C55 123.4(3) . . . . ? C28 P2 C50 C55 22.6(3) . . . . ? Ru1 P2 C50 C55 -108.5(3) . . . . ? C55 C50 C51 C52 -2.2(5) . . . . ? P2 C50 C51 C52 -179.7(3) . . . . ? C50 C51 C52 C53 2.8(5) . . . . ? C51 C52 C53 C54 -0.8(6) . . . . ? C52 C53 C54 C55 -1.8(5) . . . . ? C53 C54 C55 C50 2.4(5) . . . . ? C51 C50 C55 C54 -0.5(5) . . . . ? P2 C50 C55 C54 177.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.943 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.117 #===END data_k08mkw37 _database_code_depnum_ccdc_archive 'CCDC 723437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H63 N2 O2 P2 Ru' _chemical_formula_weight 983.11 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5450(2) _cell_length_b 12.4830(2) _cell_length_c 19.4880(3) _cell_angle_alpha 103.1740(10) _cell_angle_beta 95.7910(10) _cell_angle_gamma 114.2760(10) _cell_volume 2432.16(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 49059 _diffrn_reflns_av_R_equivalents 0.0982 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.54 _reflns_number_total 11115 _reflns_number_gt 7952 _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^)+(0.0211P)^2^+2.9743P] 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 11115 _refine_ls_number_parameters 600 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0853 _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 0.83621(2) 0.45533(2) 0.192710(13) 0.01875(7) Uani 1 1 d D . . P1 P 0.61109(8) 0.32814(7) 0.16771(4) 0.01938(17) Uani 1 1 d . . . P2 P 0.89368(8) 0.47595(7) 0.31880(4) 0.01911(17) Uani 1 1 d . . . O1 O 0.7871(2) 0.6790(2) 0.20683(13) 0.0346(6) Uani 1 1 d . . . O2 O 0.68358(19) 0.23165(18) 0.27948(10) 0.0204(5) Uani 1 1 d . . . N1 N 1.0768(2) 0.4478(2) 0.15852(13) 0.0227(6) Uani 1 1 d . . . N2 N 1.1076(2) 0.6316(2) 0.16351(14) 0.0249(6) Uani 1 1 d . . . C1 C 0.8091(3) 0.5951(3) 0.20508(16) 0.0223(7) Uani 1 1 d . . . C2 C 1.0218(3) 0.5256(3) 0.17473(15) 0.0210(7) Uani 1 1 d . . . C3 C 1.1913(3) 0.5015(3) 0.13629(18) 0.0298(8) Uani 1 1 d . . . H3 H 1.2457 0.4645 0.1218 0.036 Uiso 1 1 calc R . . C4 C 1.2107(3) 0.6162(3) 0.13927(19) 0.0319(8) Uani 1 1 d . . . H4 H 1.2817 0.6759 0.1271 0.038 Uiso 1 1 calc R . . C5 C 1.0155(3) 0.3312(3) 0.17689(17) 0.0221(7) Uani 1 1 d D . . C6 C 0.8687(3) 0.2910(3) 0.15651(16) 0.0213(7) Uani 1 1 d D . . C7 C 0.8188(3) 0.2241(3) 0.07514(16) 0.0258(7) Uani 1 1 d . . . H7A H 0.7229 0.1913 0.0630 0.031 Uiso 1 1 calc R . . H7B H 0.8557 0.2842 0.0482 0.031 Uiso 1 1 calc R . . C8 C 0.8541(3) 0.1184(3) 0.05030(19) 0.0324(8) Uani 1 1 d . . . H8A H 0.8171 0.0769 -0.0020 0.039 Uiso 1 1 calc R . . H8B H 0.8174 0.0572 0.0765 0.039 Uiso 1 1 calc R . . C9 C 1.0023(3) 0.1700(3) 0.06548(19) 0.0338(8) Uani 1 1 d . . . H9A H 1.0262 0.1021 0.0501 0.041 Uiso 1 1 calc R . . H9B H 1.0380 0.2281 0.0373 0.041 Uiso 1 1 calc R . . C10 C 1.0607(3) 0.2359(3) 0.14522(18) 0.0304(8) Uani 1 1 d . . . H10A H 1.1567 0.2771 0.1526 0.036 Uiso 1 1 calc R . . H10B H 1.0379 0.1741 0.1720 0.036 Uiso 1 1 calc R . . C11 C 1.0974(3) 0.7478(3) 0.18152(18) 0.0274(7) Uani 1 1 d . . . H11 H 1.0289 0.7381 0.2105 0.033 Uiso 1 1 calc R . . C12 C 1.2238(3) 0.8536(3) 0.22836(19) 0.0343(8) Uani 1 1 d . . . H12A H 1.2473 0.8342 0.2727 0.041 Uiso 1 1 calc R . . H12B H 1.2945 0.8644 0.2018 0.041 Uiso 1 1 calc R . . C13 C 1.2105(4) 0.9719(3) 0.2489(2) 0.0392(9) Uani 1 1 d . . . H13A H 1.2947 1.0402 0.2780 0.047 Uiso 1 1 calc R . . H13B H 1.1446 0.9633 0.2788 0.047 Uiso 1 1 calc R . . C14 C 1.1697(4) 1.0022(3) 0.1817(2) 0.0393(9) Uani 1 1 d . . . H14A H 1.1585 1.0781 0.1962 0.047 Uiso 1 1 calc R . . H14B H 1.2386 1.0171 0.1536 0.047 Uiso 1 1 calc R . . C15 C 1.0423(4) 0.8962(3) 0.1349(2) 0.0405(9) Uani 1 1 d . . . H15A H 1.0190 0.9157 0.0906 0.049 Uiso 1 1 calc R . . H15B H 0.9719 0.8865 0.1616 0.049 Uiso 1 1 calc R . . C16 C 1.0534(4) 0.7751(3) 0.11394(19) 0.0362(8) Uani 1 1 d . . . H16A H 0.9679 0.7071 0.0864 0.043 Uiso 1 1 calc R . . H16B H 1.1169 0.7814 0.0827 0.043 Uiso 1 1 calc R . . C17 C 0.5597(3) 0.1637(3) 0.16007(16) 0.0205(6) Uani 1 1 d . . . C18 C 0.4882(3) 0.0656(3) 0.09723(16) 0.0237(7) Uani 1 1 d . . . H18 H 0.4491 0.0798 0.0571 0.028 Uiso 1 1 calc R . . C19 C 0.4736(3) -0.0515(3) 0.09276(17) 0.0268(7) Uani 1 1 d . . . H19 H 0.4245 -0.1168 0.0497 0.032 Uiso 1 1 calc R . . C20 C 0.5296(3) -0.0749(3) 0.15024(17) 0.0261(7) Uani 1 1 d . . . H20 H 0.5201 -0.1556 0.1458 0.031 Uiso 1 1 calc R . . C21 C 0.5996(3) 0.0187(3) 0.21442(17) 0.0241(7) Uani 1 1 d . . . C22 C 0.6634(3) 0.0023(3) 0.28179(17) 0.0269(7) Uani 1 1 d . . . C23 C 0.7923(3) 0.1182(3) 0.31334(16) 0.0224(7) Uani 1 1 d . . . C24 C 0.9075(3) 0.1221(3) 0.34639(17) 0.0274(7) Uani 1 1 d . . . H24 H 0.9110 0.0478 0.3474 0.033 Uiso 1 1 calc R . . C25 C 1.0176(3) 0.2343(3) 0.37796(17) 0.0279(7) Uani 1 1 d . . . H25 H 1.0946 0.2358 0.4016 0.034 Uiso 1 1 calc R . . C26 C 1.0161(3) 0.3440(3) 0.37524(16) 0.0240(7) Uani 1 1 d . . . H26 H 1.0919 0.4197 0.3973 0.029 Uiso 1 1 calc R . . C27 C 0.9042(3) 0.3441(3) 0.34031(15) 0.0203(6) Uani 1 1 d . . . C28 C 0.7949(3) 0.2297(3) 0.31202(15) 0.0206(6) Uani 1 1 d . . . C29 C 0.6120(3) 0.1351(3) 0.21700(16) 0.0207(6) Uani 1 1 d . . . C30 C 0.6818(4) -0.1146(3) 0.2640(2) 0.0455(10) Uani 1 1 d . . . H30A H 0.7367 -0.1112 0.2286 0.068 Uiso 1 1 calc R . . H30B H 0.5967 -0.1865 0.2439 0.068 Uiso 1 1 calc R . . H30C H 0.7237 -0.1211 0.3081 0.068 Uiso 1 1 calc R . . C31 C 0.5755(3) -0.0041(3) 0.33730(18) 0.0373(9) Uani 1 1 d . . . H31A H 0.6175 -0.0096 0.3817 0.056 Uiso 1 1 calc R . . H31B H 0.4912 -0.0768 0.3171 0.056 Uiso 1 1 calc R . . H31C H 0.5622 0.0701 0.3482 0.056 Uiso 1 1 calc R . . C32 C 0.5153(3) 0.3160(3) 0.08116(15) 0.0212(7) Uani 1 1 d . . . C33 C 0.5738(3) 0.3688(3) 0.03070(16) 0.0253(7) Uani 1 1 d . . . H33 H 0.6661 0.4105 0.0395 0.030 Uiso 1 1 calc R . . C34 C 0.4999(3) 0.3617(3) -0.03233(17) 0.0301(8) Uani 1 1 d . . . H34 H 0.5421 0.3999 -0.0657 0.036 Uiso 1 1 calc R . . C35 C 0.3663(3) 0.2999(3) -0.04711(18) 0.0333(8) Uani 1 1 d . . . H35 H 0.3160 0.2946 -0.0906 0.040 Uiso 1 1 calc R . . C36 C 0.3057(3) 0.2451(3) 0.00256(18) 0.0339(8) Uani 1 1 d . . . H36 H 0.2135 0.2014 -0.0072 0.041 Uiso 1 1 calc R . . C37 C 0.3796(3) 0.2541(3) 0.06624(17) 0.0286(7) Uani 1 1 d . . . H37 H 0.3372 0.2177 0.1002 0.034 Uiso 1 1 calc R . . C38 C 0.5107(3) 0.3679(3) 0.22709(16) 0.0211(7) Uani 1 1 d . . . C39 C 0.4521(3) 0.3009(3) 0.27260(17) 0.0269(7) Uani 1 1 d . . . H39 H 0.4642 0.2308 0.2746 0.032 Uiso 1 1 calc R . . C40 C 0.3758(3) 0.3352(3) 0.31524(18) 0.0325(8) Uani 1 1 d . . . H40 H 0.3369 0.2887 0.3462 0.039 Uiso 1 1 calc R . . C41 C 0.3568(3) 0.4364(3) 0.31273(18) 0.0334(8) Uani 1 1 d . . . H41 H 0.3037 0.4591 0.3412 0.040 Uiso 1 1 calc R . . C42 C 0.4163(3) 0.5051(3) 0.26801(18) 0.0319(8) Uani 1 1 d . . . H42 H 0.4046 0.5757 0.2666 0.038 Uiso 1 1 calc R . . C43 C 0.4920(3) 0.4714(3) 0.22578(16) 0.0266(7) Uani 1 1 d . . . H43 H 0.5318 0.5190 0.1955 0.032 Uiso 1 1 calc R . . C44 C 1.0538(3) 0.5998(3) 0.37275(16) 0.0208(7) Uani 1 1 d . . . C45 C 1.1649(3) 0.6224(3) 0.34373(17) 0.0270(7) Uani 1 1 d . . . H45 H 1.1562 0.5760 0.2959 0.032 Uiso 1 1 calc R . . C46 C 1.2872(3) 0.7109(3) 0.38350(18) 0.0294(8) Uani 1 1 d . . . H46 H 1.3613 0.7240 0.3630 0.035 Uiso 1 1 calc R . . C47 C 1.3017(3) 0.7803(3) 0.45295(18) 0.0316(8) Uani 1 1 d . . . H47 H 1.3852 0.8417 0.4801 0.038 Uiso 1 1 calc R . . C48 C 1.1929(3) 0.7593(3) 0.48242(18) 0.0326(8) Uani 1 1 d . . . H48 H 1.2021 0.8064 0.5302 0.039 Uiso 1 1 calc R . . C49 C 1.0707(3) 0.6701(3) 0.44289(17) 0.0277(7) Uani 1 1 d . . . H49 H 0.9972 0.6568 0.4640 0.033 Uiso 1 1 calc R . . C50 C 0.7893(3) 0.5061(3) 0.37793(15) 0.0217(7) Uani 1 1 d . . . C51 C 0.7537(3) 0.4494(3) 0.43142(17) 0.0274(7) Uani 1 1 d . . . H51 H 0.7788 0.3875 0.4361 0.033 Uiso 1 1 calc R . . C52 C 0.6823(3) 0.4820(3) 0.47795(18) 0.0330(8) Uani 1 1 d . . . H52 H 0.6580 0.4416 0.5137 0.040 Uiso 1 1 calc R . . C53 C 0.6466(3) 0.5724(3) 0.47231(18) 0.0337(8) Uani 1 1 d . . . H53 H 0.5998 0.5963 0.5050 0.040 Uiso 1 1 calc R . . C54 C 0.6792(3) 0.6287(3) 0.41867(18) 0.0349(8) Uani 1 1 d . . . H54 H 0.6533 0.6903 0.4142 0.042 Uiso 1 1 calc R . . C55 C 0.7492(3) 0.5954(3) 0.37175(17) 0.0310(8) Uani 1 1 d . . . H55 H 0.7702 0.6339 0.3349 0.037 Uiso 1 1 calc R . . C56 C 1.2730(6) 1.0665(5) 0.4517(3) 0.0888(19) Uani 1 1 d . . . H56A H 1.3008 1.0337 0.4093 0.133 Uiso 1 1 calc R . . H56B H 1.3154 1.0573 0.4947 0.133 Uiso 1 1 calc R . . H56C H 1.2975 1.1538 0.4582 0.133 Uiso 1 1 calc R . . C57 C 1.1210(6) 0.9936(5) 0.4403(3) 0.0739(16) Uani 1 1 d . . . H57A H 1.0781 1.0029 0.3970 0.089 Uiso 1 1 calc R . . H57B H 1.0959 0.9050 0.4322 0.089 Uiso 1 1 calc R . . C58 C 1.0758(5) 1.0408(5) 0.5053(3) 0.0774(16) Uani 1 1 d . . . H58A H 1.0944 1.1276 0.5113 0.093 Uiso 1 1 calc R . . H58B H 1.1231 1.0372 0.5493 0.093 Uiso 1 1 calc R . . H5 H 1.047(3) 0.353(2) 0.2303(3) 0.014(7) Uiso 1 1 d D . . H6 H 0.829(3) 0.228(2) 0.1816(14) 0.024(8) Uiso 1 1 d D . . H1 H 0.808(4) 0.437(3) 0.1078(4) 0.047(11) 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 0.01623(13) 0.02135(13) 0.01882(13) 0.00585(10) 0.00364(9) 0.00866(10) P1 0.0171(4) 0.0225(4) 0.0190(4) 0.0059(3) 0.0039(3) 0.0095(3) P2 0.0180(4) 0.0202(4) 0.0187(4) 0.0048(3) 0.0030(3) 0.0090(3) O1 0.0352(14) 0.0335(14) 0.0479(15) 0.0186(12) 0.0147(11) 0.0226(12) O2 0.0183(11) 0.0205(11) 0.0196(11) 0.0030(9) 0.0002(8) 0.0086(9) N1 0.0154(13) 0.0258(14) 0.0257(14) 0.0071(11) 0.0055(11) 0.0081(11) N2 0.0193(14) 0.0266(15) 0.0320(15) 0.0123(12) 0.0083(11) 0.0110(12) C1 0.0160(16) 0.0274(17) 0.0219(16) 0.0079(13) 0.0045(12) 0.0077(14) C2 0.0199(16) 0.0232(16) 0.0195(15) 0.0067(13) 0.0014(12) 0.0095(13) C3 0.0215(17) 0.036(2) 0.0365(19) 0.0124(16) 0.0114(14) 0.0146(16) C4 0.0188(17) 0.036(2) 0.044(2) 0.0165(17) 0.0146(15) 0.0108(15) C5 0.0199(16) 0.0240(17) 0.0250(17) 0.0077(13) 0.0055(13) 0.0120(14) C6 0.0199(16) 0.0254(17) 0.0206(15) 0.0088(13) 0.0068(12) 0.0105(14) C7 0.0221(17) 0.0279(17) 0.0235(17) 0.0017(14) 0.0052(13) 0.0104(14) C8 0.033(2) 0.0284(18) 0.0306(19) 0.0025(15) 0.0073(15) 0.0118(16) C9 0.035(2) 0.0322(19) 0.039(2) 0.0072(16) 0.0136(16) 0.0195(17) C10 0.0281(18) 0.0292(18) 0.0369(19) 0.0085(15) 0.0087(15) 0.0159(15) C11 0.0206(17) 0.0203(16) 0.0394(19) 0.0108(14) 0.0069(14) 0.0063(14) C12 0.0284(19) 0.0307(19) 0.040(2) 0.0154(16) 0.0013(15) 0.0085(16) C13 0.039(2) 0.0254(19) 0.044(2) 0.0070(16) 0.0026(17) 0.0081(17) C14 0.035(2) 0.031(2) 0.052(2) 0.0163(18) 0.0057(18) 0.0132(17) C15 0.040(2) 0.039(2) 0.046(2) 0.0135(18) 0.0012(18) 0.0218(18) C16 0.034(2) 0.034(2) 0.038(2) 0.0108(16) 0.0013(16) 0.0141(17) C17 0.0145(15) 0.0236(16) 0.0228(16) 0.0065(13) 0.0053(12) 0.0079(13) C18 0.0199(16) 0.0294(18) 0.0192(16) 0.0044(13) 0.0057(12) 0.0097(14) C19 0.0247(17) 0.0253(17) 0.0202(16) -0.0028(13) 0.0022(13) 0.0070(14) C20 0.0255(18) 0.0206(16) 0.0280(17) 0.0019(14) 0.0073(14) 0.0087(14) C21 0.0192(16) 0.0245(17) 0.0294(17) 0.0092(14) 0.0080(13) 0.0092(14) C22 0.0274(18) 0.0213(17) 0.0294(18) 0.0077(14) 0.0029(14) 0.0091(14) C23 0.0232(17) 0.0227(16) 0.0228(16) 0.0077(13) 0.0060(13) 0.0110(14) C24 0.0313(19) 0.0279(18) 0.0293(18) 0.0108(14) 0.0068(14) 0.0180(15) C25 0.0228(17) 0.0325(19) 0.0318(18) 0.0126(15) 0.0039(14) 0.0144(15) C26 0.0198(16) 0.0283(17) 0.0226(16) 0.0091(14) 0.0041(13) 0.0089(14) C27 0.0215(16) 0.0239(16) 0.0169(15) 0.0064(12) 0.0059(12) 0.0108(14) C28 0.0224(16) 0.0252(16) 0.0150(14) 0.0051(12) 0.0035(12) 0.0119(14) C29 0.0161(15) 0.0213(16) 0.0205(15) 0.0028(13) 0.0048(12) 0.0061(13) C30 0.054(3) 0.0241(19) 0.053(2) 0.0079(17) -0.0101(19) 0.0184(18) C31 0.030(2) 0.039(2) 0.0324(19) 0.0172(17) 0.0051(15) 0.0022(16) C32 0.0226(16) 0.0235(16) 0.0187(15) 0.0024(13) 0.0026(12) 0.0140(14) C33 0.0216(17) 0.0263(17) 0.0274(17) 0.0064(14) 0.0042(13) 0.0114(14) C34 0.033(2) 0.0330(19) 0.0243(17) 0.0094(15) 0.0039(14) 0.0152(16) C35 0.038(2) 0.041(2) 0.0241(17) 0.0035(15) -0.0017(15) 0.0254(18) C36 0.0225(18) 0.044(2) 0.0311(19) 0.0045(16) 0.0010(15) 0.0153(16) C37 0.0232(17) 0.039(2) 0.0256(17) 0.0099(15) 0.0052(13) 0.0155(16) C38 0.0158(15) 0.0241(16) 0.0198(15) 0.0030(13) 0.0018(12) 0.0078(13) C39 0.0231(17) 0.0301(18) 0.0272(17) 0.0079(14) 0.0067(14) 0.0116(15) C40 0.0281(19) 0.038(2) 0.0298(18) 0.0096(16) 0.0124(15) 0.0124(16) C41 0.0262(18) 0.043(2) 0.0317(19) 0.0031(16) 0.0089(15) 0.0200(17) C42 0.0319(19) 0.0324(19) 0.0341(19) 0.0066(16) 0.0033(15) 0.0196(16) C43 0.0290(18) 0.0322(18) 0.0220(16) 0.0073(14) 0.0061(13) 0.0170(15) C44 0.0203(16) 0.0192(15) 0.0220(16) 0.0079(13) 0.0028(12) 0.0075(13) C45 0.0306(19) 0.0286(18) 0.0212(16) 0.0064(14) 0.0022(14) 0.0138(15) C46 0.0193(17) 0.0321(19) 0.0342(19) 0.0110(15) 0.0051(14) 0.0086(15) C47 0.0247(18) 0.0268(18) 0.0327(19) 0.0058(15) -0.0036(15) 0.0053(15) C48 0.034(2) 0.0270(18) 0.0241(17) -0.0011(14) -0.0002(15) 0.0072(16) C49 0.0240(17) 0.0275(18) 0.0264(17) 0.0056(14) 0.0046(14) 0.0079(15) C50 0.0173(15) 0.0242(16) 0.0182(15) 0.0015(13) 0.0024(12) 0.0071(13) C51 0.0244(17) 0.0311(18) 0.0263(17) 0.0074(14) 0.0066(14) 0.0126(15) C52 0.0270(19) 0.038(2) 0.0284(18) 0.0100(15) 0.0114(15) 0.0082(16) C53 0.0270(19) 0.040(2) 0.0264(18) -0.0015(15) 0.0082(14) 0.0133(16) C54 0.034(2) 0.043(2) 0.0340(19) 0.0052(16) 0.0074(16) 0.0265(18) C55 0.038(2) 0.0333(19) 0.0246(17) 0.0066(15) 0.0067(15) 0.0200(17) C56 0.120(6) 0.076(4) 0.071(4) 0.019(3) 0.005(3) 0.048(4) C57 0.109(5) 0.058(3) 0.059(3) 0.016(3) -0.008(3) 0.048(3) C58 0.107(5) 0.067(4) 0.062(3) 0.036(3) 0.010(3) 0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.864(3) . ? Ru1 C2 2.057(3) . ? Ru1 C6 2.207(3) . ? Ru1 P1 2.3477(8) . ? Ru1 P2 2.4055(8) . ? Ru1 H1 1.600(3) . ? P1 C38 1.847(3) . ? P1 C17 1.851(3) . ? P1 C32 1.860(3) . ? P2 C27 1.836(3) . ? P2 C50 1.838(3) . ? P2 C44 1.852(3) . ? O1 C1 1.169(4) . ? O2 C28 1.386(3) . ? O2 C29 1.389(3) . ? N1 C2 1.361(4) . ? N1 C3 1.380(4) . ? N1 C5 1.479(4) . ? N2 C2 1.370(4) . ? N2 C4 1.392(4) . ? N2 C11 1.469(4) . ? C3 C4 1.341(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C10 1.520(4) . ? C5 C6 1.535(4) . ? C5 H5 1.000(3) . ? C6 C7 1.536(4) . ? C6 H6 1.00(3) . ? C7 C8 1.527(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.528(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.515(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.518(4) . ? C11 C16 1.524(5) . ? C11 H11 1.0000 . ? C12 C13 1.515(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.535(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C29 1.395(4) . ? C17 C18 1.401(4) . ? C18 C19 1.382(4) . ? C18 H18 0.9500 . ? C19 C20 1.384(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(4) . ? C20 H20 0.9500 . ? C21 C29 1.388(4) . ? C21 C22 1.536(4) . ? C22 C23 1.525(4) . ? C22 C30 1.528(5) . ? C22 C31 1.549(5) . ? C23 C28 1.386(4) . ? C23 C24 1.395(4) . ? C24 C25 1.393(5) . ? C24 H24 0.9500 . ? C25 C26 1.389(4) . ? C25 H25 0.9500 . ? C26 C27 1.399(4) . ? C26 H26 0.9500 . ? C27 C28 1.398(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.386(4) . ? C32 C37 1.396(4) . ? C33 C34 1.386(4) . ? C33 H33 0.9500 . ? C34 C35 1.374(5) . ? C34 H34 0.9500 . ? C35 C36 1.392(5) . ? C35 H35 0.9500 . ? C36 C37 1.387(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.392(4) . ? C38 C43 1.400(4) . ? C39 C40 1.394(5) . ? C39 H39 0.9500 . ? C40 C41 1.379(5) . ? C40 H40 0.9500 . ? C41 C42 1.394(5) . ? C41 H41 0.9500 . ? C42 C43 1.381(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.391(4) . ? C44 C45 1.402(4) . ? C45 C46 1.386(4) . ? C45 H45 0.9500 . ? C46 C47 1.382(5) . ? C46 H46 0.9500 . ? C47 C48 1.385(5) . ? C47 H47 0.9500 . ? C48 C49 1.386(4) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.392(4) . ? C50 C55 1.395(4) . ? C51 C52 1.388(5) . ? C51 H51 0.9500 . ? C52 C53 1.373(5) . ? C52 H52 0.9500 . ? C53 C54 1.388(5) . ? C53 H53 0.9500 . ? C54 C55 1.384(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.573(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.506(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C58 1.584(11) 2_776 ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 99.32(13) . . ? C1 Ru1 C6 168.97(12) . . ? C2 Ru1 C6 76.41(12) . . ? C1 Ru1 P1 91.13(10) . . ? C2 Ru1 P1 157.81(8) . . ? C6 Ru1 P1 89.67(8) . . ? C1 Ru1 P2 96.90(9) . . ? C2 Ru1 P2 97.64(8) . . ? C6 Ru1 P2 93.77(8) . . ? P1 Ru1 P2 100.48(3) . . ? C1 Ru1 H1 87.3(13) . . ? C2 Ru1 H1 78.3(13) . . ? C6 Ru1 H1 81.9(13) . . ? P1 Ru1 H1 82.7(13) . . ? P2 Ru1 H1 174.6(13) . . ? C38 P1 C17 102.69(14) . . ? C38 P1 C32 97.19(13) . . ? C17 P1 C32 101.10(13) . . ? C38 P1 Ru1 119.79(10) . . ? C17 P1 Ru1 116.54(10) . . ? C32 P1 Ru1 116.20(11) . . ? C27 P2 C50 101.71(14) . . ? C27 P2 C44 99.31(13) . . ? C50 P2 C44 99.09(14) . . ? C27 P2 Ru1 116.38(10) . . ? C50 P2 Ru1 118.31(10) . . ? C44 P2 Ru1 118.63(10) . . ? C28 O2 C29 114.5(2) . . ? C2 N1 C3 111.9(3) . . ? C2 N1 C5 115.8(2) . . ? C3 N1 C5 131.6(3) . . ? C2 N2 C4 110.3(3) . . ? C2 N2 C11 124.2(3) . . ? C4 N2 C11 125.3(3) . . ? O1 C1 Ru1 174.4(3) . . ? N1 C2 N2 103.8(3) . . ? N1 C2 Ru1 118.2(2) . . ? N2 C2 Ru1 137.2(2) . . ? C4 C3 N1 106.4(3) . . ? C4 C3 H3 126.8 . . ? N1 C3 H3 126.8 . . ? C3 C4 N2 107.5(3) . . ? C3 C4 H4 126.3 . . ? N2 C4 H4 126.3 . . ? N1 C5 C10 114.6(3) . . ? N1 C5 C6 104.5(2) . . ? C10 C5 C6 116.1(3) . . ? N1 C5 H5 105.5(17) . . ? C10 C5 H5 104.2(16) . . ? C6 C5 H5 111.5(17) . . ? C5 C6 C7 109.1(3) . . ? C5 C6 Ru1 108.0(2) . . ? C7 C6 Ru1 114.5(2) . . ? C5 C6 H6 104.2(18) . . ? C7 C6 H6 106.4(18) . . ? Ru1 C6 H6 114.1(18) . . ? C8 C7 C6 113.4(3) . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 108.9(3) . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C8 110.6(3) . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 C5 114.0(3) . . ? C9 C10 H10A 108.8 . . ? C5 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C5 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C12 111.3(3) . . ? N2 C11 C16 111.5(3) . . ? C12 C11 C16 111.7(3) . . ? N2 C11 H11 107.3 . . ? C12 C11 H11 107.3 . . ? C16 C11 H11 107.3 . . ? C13 C12 C11 110.8(3) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C12 C13 C14 110.8(3) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 110.3(3) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.4(3) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C11 C16 C15 110.1(3) . . ? C11 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? C11 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? C29 C17 C18 116.1(3) . . ? C29 C17 P1 118.1(2) . . ? C18 C17 P1 125.1(2) . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.8(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.6(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C29 C21 C20 116.9(3) . . ? C29 C21 C22 118.2(3) . . ? C20 C21 C22 124.9(3) . . ? C23 C22 C30 112.3(3) . . ? C23 C22 C21 106.1(3) . . ? C30 C22 C21 112.0(3) . . ? C23 C22 C31 108.6(3) . . ? C30 C22 C31 109.3(3) . . ? C21 C22 C31 108.6(3) . . ? C28 C23 C24 116.8(3) . . ? C28 C23 C22 117.8(3) . . ? C24 C23 C22 125.3(3) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 116.3(3) . . ? C28 C27 P2 117.2(2) . . ? C26 C27 P2 126.1(2) . . ? O2 C28 C23 119.5(3) . . ? O2 C28 C27 115.7(3) . . ? C23 C28 C27 124.8(3) . . ? C21 C29 O2 118.8(3) . . ? C21 C29 C17 124.6(3) . . ? O2 C29 C17 116.6(3) . . ? C22 C30 H30A 109.5 . . ? C22 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C22 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 C31 H31A 109.5 . . ? C22 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C22 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 118.0(3) . . ? C33 C32 P1 122.3(2) . . ? C37 C32 P1 119.7(2) . . ? C32 C33 C34 121.1(3) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120.8(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 119.0(3) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C32 120.9(3) . . ? C36 C37 H37 119.6 . . ? C32 C37 H37 119.6 . . ? C39 C38 C43 118.2(3) . . ? C39 C38 P1 124.0(2) . . ? C43 C38 P1 117.8(2) . . ? C38 C39 C40 120.9(3) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 119.3(3) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C43 C42 C41 120.5(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C38 120.8(3) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? C49 C44 C45 117.6(3) . . ? C49 C44 P2 122.8(2) . . ? C45 C44 P2 119.6(2) . . ? C46 C45 C44 121.3(3) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C47 C46 C45 120.2(3) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.2(3) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C49 120.7(3) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C48 C49 C44 121.1(3) . . ? C48 C49 H49 119.5 . . ? C44 C49 H49 119.5 . . ? C51 C50 C55 118.0(3) . . ? C51 C50 P2 123.5(2) . . ? C55 C50 P2 118.4(2) . . ? C52 C51 C50 121.1(3) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C53 C52 C51 120.1(3) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 119.7(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C55 C54 C53 120.2(3) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C50 120.8(3) . . ? C54 C55 H55 119.6 . . ? C50 C55 H55 119.6 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C56 110.6(4) . . ? C58 C57 H57A 109.5 . . ? C56 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? C57 C58 C58 109.4(6) . 2_776 ? C57 C58 H58A 109.8 . . ? C58 C58 H58A 109.8 2_776 . ? C57 C58 H58B 109.8 . . ? C58 C58 H58B 109.8 2_776 . ? H58A C58 H58B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 P1 C38 -47.58(15) . . . . ? C2 Ru1 P1 C38 -166.1(2) . . . . ? C6 Ru1 P1 C38 143.42(14) . . . . ? P2 Ru1 P1 C38 49.65(12) . . . . ? C1 Ru1 P1 C17 -172.26(14) . . . . ? C2 Ru1 P1 C17 69.2(2) . . . . ? C6 Ru1 P1 C17 18.74(13) . . . . ? P2 Ru1 P1 C17 -75.03(11) . . . . ? C1 Ru1 P1 C32 68.68(14) . . . . ? C2 Ru1 P1 C32 -49.8(3) . . . . ? C6 Ru1 P1 C32 -100.32(13) . . . . ? P2 Ru1 P1 C32 165.91(11) . . . . ? C1 Ru1 P2 C27 169.56(15) . . . . ? C2 Ru1 P2 C27 -90.03(14) . . . . ? C6 Ru1 P2 C27 -13.25(14) . . . . ? P1 Ru1 P2 C27 77.11(12) . . . . ? C1 Ru1 P2 C50 47.93(15) . . . . ? C2 Ru1 P2 C50 148.34(14) . . . . ? C6 Ru1 P2 C50 -134.88(14) . . . . ? P1 Ru1 P2 C50 -44.52(12) . . . . ? C1 Ru1 P2 C44 -71.98(15) . . . . ? C2 Ru1 P2 C44 28.44(14) . . . . ? C6 Ru1 P2 C44 105.21(14) . . . . ? P1 Ru1 P2 C44 -164.42(11) . . . . ? C2 Ru1 C1 O1 95(3) . . . . ? C6 Ru1 C1 O1 29(3) . . . . ? P1 Ru1 C1 O1 -65(3) . . . . ? P2 Ru1 C1 O1 -166(3) . . . . ? C3 N1 C2 N2 -1.3(3) . . . . ? C5 N1 C2 N2 170.7(2) . . . . ? C3 N1 C2 Ru1 170.1(2) . . . . ? C5 N1 C2 Ru1 -17.9(3) . . . . ? C4 N2 C2 N1 1.4(3) . . . . ? C11 N2 C2 N1 -173.1(3) . . . . ? C4 N2 C2 Ru1 -167.4(3) . . . . ? C11 N2 C2 Ru1 18.1(5) . . . . ? C1 Ru1 C2 N1 -176.2(2) . . . . ? C6 Ru1 C2 N1 -6.5(2) . . . . ? P1 Ru1 C2 N1 -59.1(3) . . . . ? P2 Ru1 C2 N1 85.5(2) . . . . ? C1 Ru1 C2 N2 -8.5(3) . . . . ? C6 Ru1 C2 N2 161.1(3) . . . . ? P1 Ru1 C2 N2 108.6(3) . . . . ? P2 Ru1 C2 N2 -106.8(3) . . . . ? C2 N1 C3 C4 0.8(4) . . . . ? C5 N1 C3 C4 -169.6(3) . . . . ? N1 C3 C4 N2 0.1(4) . . . . ? C2 N2 C4 C3 -1.0(4) . . . . ? C11 N2 C4 C3 173.4(3) . . . . ? C2 N1 C5 C10 168.5(3) . . . . ? C3 N1 C5 C10 -21.4(4) . . . . ? C2 N1 C5 C6 40.3(3) . . . . ? C3 N1 C5 C6 -149.7(3) . . . . ? N1 C5 C6 C7 82.6(3) . . . . ? C10 C5 C6 C7 -44.8(4) . . . . ? N1 C5 C6 Ru1 -42.4(3) . . . . ? C10 C5 C6 Ru1 -169.8(2) . . . . ? C1 Ru1 C6 C5 96.0(7) . . . . ? C2 Ru1 C6 C5 27.64(19) . . . . ? P1 Ru1 C6 C5 -169.80(19) . . . . ? P2 Ru1 C6 C5 -69.32(19) . . . . ? C1 Ru1 C6 C7 -25.8(8) . . . . ? C2 Ru1 C6 C7 -94.1(2) . . . . ? P1 Ru1 C6 C7 68.4(2) . . . . ? P2 Ru1 C6 C7 168.9(2) . . . . ? C5 C6 C7 C8 53.2(4) . . . . ? Ru1 C6 C7 C8 174.4(2) . . . . ? C6 C7 C8 C9 -61.5(4) . . . . ? C7 C8 C9 C10 58.5(4) . . . . ? C8 C9 C10 C5 -51.6(4) . . . . ? N1 C5 C10 C9 -76.4(4) . . . . ? C6 C5 C10 C9 45.8(4) . . . . ? C2 N2 C11 C12 127.1(3) . . . . ? C4 N2 C11 C12 -46.5(4) . . . . ? C2 N2 C11 C16 -107.3(3) . . . . ? C4 N2 C11 C16 79.0(4) . . . . ? N2 C11 C12 C13 -177.8(3) . . . . ? C16 C11 C12 C13 56.7(4) . . . . ? C11 C12 C13 C14 -57.2(4) . . . . ? C12 C13 C14 C15 57.3(4) . . . . ? C13 C14 C15 C16 -56.7(4) . . . . ? N2 C11 C16 C15 179.3(3) . . . . ? C12 C11 C16 C15 -55.4(4) . . . . ? C14 C15 C16 C11 55.5(4) . . . . ? C38 P1 C17 C29 -79.4(3) . . . . ? C32 P1 C17 C29 -179.5(2) . . . . ? Ru1 P1 C17 C29 53.6(3) . . . . ? C38 P1 C17 C18 111.0(3) . . . . ? C32 P1 C17 C18 11.0(3) . . . . ? Ru1 P1 C17 C18 -116.0(3) . . . . ? C29 C17 C18 C19 -1.1(4) . . . . ? P1 C17 C18 C19 168.6(2) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 1.3(5) . . . . ? C19 C20 C21 C29 -1.2(5) . . . . ? C19 C20 C21 C22 178.8(3) . . . . ? C29 C21 C22 C23 -38.1(4) . . . . ? C20 C21 C22 C23 141.9(3) . . . . ? C29 C21 C22 C30 -160.9(3) . . . . ? C20 C21 C22 C30 19.2(5) . . . . ? C29 C21 C22 C31 78.4(4) . . . . ? C20 C21 C22 C31 -101.5(4) . . . . ? C30 C22 C23 C28 161.4(3) . . . . ? C21 C22 C23 C28 38.8(4) . . . . ? C31 C22 C23 C28 -77.7(3) . . . . ? C30 C22 C23 C24 -21.5(5) . . . . ? C21 C22 C23 C24 -144.1(3) . . . . ? C31 C22 C23 C24 99.4(4) . . . . ? C28 C23 C24 C25 1.7(5) . . . . ? C22 C23 C24 C25 -175.5(3) . . . . ? C23 C24 C25 C26 -2.0(5) . . . . ? C24 C25 C26 C27 -0.4(5) . . . . ? C25 C26 C27 C28 2.8(5) . . . . ? C25 C26 C27 P2 -169.3(2) . . . . ? C50 P2 C27 C28 75.1(3) . . . . ? C44 P2 C27 C28 176.4(2) . . . . ? Ru1 P2 C27 C28 -55.0(3) . . . . ? C50 P2 C27 C26 -112.9(3) . . . . ? C44 P2 C27 C26 -11.5(3) . . . . ? Ru1 P2 C27 C26 117.0(3) . . . . ? C29 O2 C28 C23 -38.3(4) . . . . ? C29 O2 C28 C27 140.5(3) . . . . ? C24 C23 C28 O2 179.6(3) . . . . ? C22 C23 C28 O2 -3.0(4) . . . . ? C24 C23 C28 C27 0.9(5) . . . . ? C22 C23 C28 C27 178.3(3) . . . . ? C26 C27 C28 O2 178.1(3) . . . . ? P2 C27 C28 O2 -9.0(4) . . . . ? C26 C27 C28 C23 -3.2(5) . . . . ? P2 C27 C28 C23 169.6(2) . . . . ? C20 C21 C29 O2 -178.6(3) . . . . ? C22 C21 C29 O2 1.5(4) . . . . ? C20 C21 C29 C17 -0.2(5) . . . . ? C22 C21 C29 C17 179.8(3) . . . . ? C28 O2 C29 C21 38.9(4) . . . . ? C28 O2 C29 C17 -139.6(3) . . . . ? C18 C17 C29 C21 1.3(5) . . . . ? P1 C17 C29 C21 -169.2(3) . . . . ? C18 C17 C29 O2 179.7(3) . . . . ? P1 C17 C29 O2 9.2(4) . . . . ? C38 P1 C32 C33 134.4(3) . . . . ? C17 P1 C32 C33 -121.1(3) . . . . ? Ru1 P1 C32 C33 6.1(3) . . . . ? C38 P1 C32 C37 -44.2(3) . . . . ? C17 P1 C32 C37 60.3(3) . . . . ? Ru1 P1 C32 C37 -172.5(2) . . . . ? C37 C32 C33 C34 0.7(5) . . . . ? P1 C32 C33 C34 -177.9(2) . . . . ? C32 C33 C34 C35 -1.2(5) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C34 C35 C36 C37 0.6(5) . . . . ? C35 C36 C37 C32 -1.1(5) . . . . ? C33 C32 C37 C36 0.5(5) . . . . ? P1 C32 C37 C36 179.1(3) . . . . ? C17 P1 C38 C39 20.2(3) . . . . ? C32 P1 C38 C39 123.3(3) . . . . ? Ru1 P1 C38 C39 -110.9(2) . . . . ? C17 P1 C38 C43 -159.4(2) . . . . ? C32 P1 C38 C43 -56.3(3) . . . . ? Ru1 P1 C38 C43 69.5(2) . . . . ? C43 C38 C39 C40 0.6(5) . . . . ? P1 C38 C39 C40 -179.0(2) . . . . ? C38 C39 C40 C41 0.3(5) . . . . ? C39 C40 C41 C42 -1.0(5) . . . . ? C40 C41 C42 C43 0.9(5) . . . . ? C41 C42 C43 C38 -0.1(5) . . . . ? C39 C38 C43 C42 -0.7(5) . . . . ? P1 C38 C43 C42 179.0(2) . . . . ? C27 P2 C44 C49 -93.6(3) . . . . ? C50 P2 C44 C49 10.0(3) . . . . ? Ru1 P2 C44 C49 139.4(2) . . . . ? C27 P2 C44 C45 84.0(3) . . . . ? C50 P2 C44 C45 -172.4(2) . . . . ? Ru1 P2 C44 C45 -43.0(3) . . . . ? C49 C44 C45 C46 0.3(5) . . . . ? P2 C44 C45 C46 -177.4(2) . . . . ? C44 C45 C46 C47 -0.7(5) . . . . ? C45 C46 C47 C48 0.7(5) . . . . ? C46 C47 C48 C49 -0.2(5) . . . . ? C47 C48 C49 C44 -0.2(5) . . . . ? C45 C44 C49 C48 0.1(5) . . . . ? P2 C44 C49 C48 177.8(3) . . . . ? C27 P2 C50 C51 9.4(3) . . . . ? C44 P2 C50 C51 -92.2(3) . . . . ? Ru1 P2 C50 C51 138.2(2) . . . . ? C27 P2 C50 C55 -174.3(2) . . . . ? C44 P2 C50 C55 84.1(3) . . . . ? Ru1 P2 C50 C55 -45.5(3) . . . . ? C55 C50 C51 C52 -0.9(5) . . . . ? P2 C50 C51 C52 175.4(2) . . . . ? C50 C51 C52 C53 -0.7(5) . . . . ? C51 C52 C53 C54 1.8(5) . . . . ? C52 C53 C54 C55 -1.1(5) . . . . ? C53 C54 C55 C50 -0.7(5) . . . . ? C51 C50 C55 C54 1.6(5) . . . . ? P2 C50 C55 C54 -174.9(3) . . . . ? C56 C57 C58 C58 -175.7(5) . . . 2_776 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.641 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.101 #===END data_k09mkw5 _database_code_depnum_ccdc_archive 'CCDC 723438' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H47 Cl2 O2 P3 Ru' _chemical_formula_weight 1016.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4940(2) _cell_length_b 12.3400(2) _cell_length_c 19.1250(3) _cell_angle_alpha 71.9740(10) _cell_angle_beta 82.1580(10) _cell_angle_gamma 89.6640(10) _cell_volume 2331.29(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22475 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 'horizonally mounted graphite crystal' _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 28901 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.57 _reflns_number_total 10584 _reflns_number_gt 9312 _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-97/2 (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^)+(0.0281P)^2^+2.2389P] 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 10584 _refine_ls_number_parameters 582 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.724145(14) 0.150523(12) 0.294743(8) 0.01372(5) Uani 1 1 d D . . Cl1 Cl 0.39731(8) -0.08322(6) 0.15746(4) 0.05029(18) Uani 1 1 d . . . Cl2 Cl 0.34043(8) 0.06518(7) 0.01468(4) 0.05186(19) Uani 1 1 d . . . P1 P 0.84239(5) 0.16214(4) 0.17615(3) 0.01555(10) Uani 1 1 d . . . P2 P 0.72618(5) 0.33645(4) 0.29533(3) 0.01527(10) Uani 1 1 d . . . P3 P 0.75084(5) -0.03607(4) 0.36535(3) 0.01450(10) Uani 1 1 d . . . O1 O 0.47241(15) 0.15105(15) 0.23160(10) 0.0331(4) Uani 1 1 d . . . O2 O 0.70732(13) 0.39690(11) 0.14143(8) 0.0186(3) Uani 1 1 d . . . C1 C 0.5669(2) 0.14886(17) 0.25642(11) 0.0201(4) Uani 1 1 d . . . C2 C 0.77176(19) 0.36291(17) 0.37846(11) 0.0184(4) Uani 1 1 d . . . C3 C 0.8137(2) 0.27575(18) 0.43564(12) 0.0222(4) Uani 1 1 d . . . H3 H 0.8157 0.2001 0.4330 0.027 Uiso 1 1 calc R . . C4 C 0.8528(2) 0.2986(2) 0.49663(13) 0.0282(5) Uani 1 1 d . . . H4 H 0.8796 0.2383 0.5357 0.034 Uiso 1 1 calc R . . C5 C 0.8526(2) 0.4084(2) 0.50050(12) 0.0283(5) Uani 1 1 d . . . H5 H 0.8828 0.4242 0.5411 0.034 Uiso 1 1 calc R . . C6 C 0.8082(2) 0.49577(19) 0.44505(13) 0.0288(5) Uani 1 1 d . . . H6 H 0.8061 0.5711 0.4482 0.035 Uiso 1 1 calc R . . C7 C 0.7667(2) 0.47275(18) 0.38496(12) 0.0244(4) Uani 1 1 d . . . H7 H 0.7344 0.5325 0.3478 0.029 Uiso 1 1 calc R . . C8 C 0.5724(2) 0.40936(17) 0.28964(11) 0.0190(4) Uani 1 1 d . . . C9 C 0.4641(2) 0.35193(18) 0.33644(13) 0.0257(5) Uani 1 1 d . . . H9 H 0.4714 0.2771 0.3691 0.031 Uiso 1 1 calc R . . C10 C 0.3452(2) 0.4024(2) 0.33618(15) 0.0327(5) Uani 1 1 d . . . H10 H 0.2723 0.3628 0.3691 0.039 Uiso 1 1 calc R . . C11 C 0.3334(2) 0.5106(2) 0.28786(15) 0.0333(5) Uani 1 1 d . . . H11 H 0.2523 0.5452 0.2874 0.040 Uiso 1 1 calc R . . C12 C 0.4395(3) 0.5680(2) 0.24036(14) 0.0344(6) Uani 1 1 d . . . H12 H 0.4309 0.6417 0.2066 0.041 Uiso 1 1 calc R . . C13 C 0.5596(2) 0.51874(18) 0.24143(13) 0.0272(5) Uani 1 1 d . . . H13 H 0.6326 0.5596 0.2094 0.033 Uiso 1 1 calc R . . C14 C 0.83972(19) 0.43406(16) 0.22184(11) 0.0177(4) Uani 1 1 d . . . C15 C 0.9527(2) 0.48179(17) 0.23261(12) 0.0211(4) Uani 1 1 d . . . H15 H 0.9679 0.4751 0.2816 0.025 Uiso 1 1 calc R . . C16 C 1.0437(2) 0.53931(18) 0.17224(12) 0.0246(4) Uani 1 1 d . . . H16 H 1.1203 0.5715 0.1803 0.029 Uiso 1 1 calc R . . C17 C 1.0225(2) 0.54943(17) 0.10081(12) 0.0235(4) Uani 1 1 d . . . H17 H 1.0843 0.5890 0.0598 0.028 Uiso 1 1 calc R . . C18 C 0.9112(2) 0.50204(17) 0.08863(11) 0.0211(4) Uani 1 1 d . . . H18 H 0.8964 0.5087 0.0396 0.025 Uiso 1 1 calc R . . C19 C 0.82245(19) 0.44493(16) 0.14902(11) 0.0171(4) Uani 1 1 d . . . C20 C 0.70884(19) 0.34544(17) 0.08635(11) 0.0178(4) Uani 1 1 d . . . C21 C 0.76679(18) 0.24059(17) 0.09246(11) 0.0175(4) Uani 1 1 d . . . C22 C 0.7594(2) 0.19658(17) 0.03377(11) 0.0213(4) Uani 1 1 d . . . H22 H 0.8004 0.1275 0.0345 0.026 Uiso 1 1 calc R . . C23 C 0.6943(2) 0.25041(19) -0.02538(12) 0.0251(4) Uani 1 1 d . . . H23 H 0.6904 0.2175 -0.0639 0.030 Uiso 1 1 calc R . . C24 C 0.6348(2) 0.35203(19) -0.02843(12) 0.0262(5) Uani 1 1 d . . . H24 H 0.5891 0.3886 -0.0684 0.031 Uiso 1 1 calc R . . C25 C 0.6429(2) 0.39963(18) 0.02787(12) 0.0227(4) Uani 1 1 d . . . H25 H 0.6031 0.4695 0.0263 0.027 Uiso 1 1 calc R . . C26 C 1.00807(19) 0.22436(16) 0.14968(11) 0.0188(4) Uani 1 1 d . . . C27 C 1.07392(19) 0.24318(17) 0.20368(12) 0.0208(4) Uani 1 1 d . . . H27 H 1.0318 0.2267 0.2532 0.025 Uiso 1 1 calc R . . C28 C 1.2008(2) 0.28594(19) 0.18576(13) 0.0270(5) Uani 1 1 d . . . H28 H 1.2449 0.2981 0.2231 0.032 Uiso 1 1 calc R . . C29 C 1.2627(2) 0.31085(19) 0.11340(14) 0.0297(5) Uani 1 1 d . . . H29 H 1.3494 0.3397 0.1011 0.036 Uiso 1 1 calc R . . C30 C 1.1980(2) 0.29357(19) 0.05941(13) 0.0291(5) Uani 1 1 d . . . H30 H 1.2403 0.3114 0.0098 0.035 Uiso 1 1 calc R . . C31 C 1.0714(2) 0.25030(18) 0.07683(12) 0.0250(5) Uani 1 1 d . . . H31 H 1.0280 0.2384 0.0392 0.030 Uiso 1 1 calc R . . C32 C 0.8612(2) 0.02441(17) 0.15735(11) 0.0188(4) Uani 1 1 d . . . C33 C 0.7491(2) -0.04014(18) 0.16448(12) 0.0235(4) Uani 1 1 d . . . H33 H 0.6684 -0.0121 0.1786 0.028 Uiso 1 1 calc R . . C34 C 0.7529(2) -0.14464(19) 0.15132(13) 0.0306(5) Uani 1 1 d . . . H34 H 0.6754 -0.1875 0.1565 0.037 Uiso 1 1 calc R . . C35 C 0.8700(3) -0.1864(2) 0.13055(14) 0.0348(6) Uani 1 1 d . . . H35 H 0.8730 -0.2574 0.1208 0.042 Uiso 1 1 calc R . . C36 C 0.9808(2) -0.12489(15) 0.12416(11) 0.0340(5) Uani 1 1 d . . . H36 H 1.0611 -0.1544 0.1108 0.041 Uiso 1 1 calc R . . C57 C 0.4142(2) 0.05780(15) 0.09301(11) 0.0466(7) Uani 1 1 d R . . H57A H 0.3744 0.1121 0.1174 0.056 Uiso 1 1 calc R . . H57B H 0.5068 0.0799 0.0773 0.056 Uiso 1 1 calc R . . C37 C 0.9784(2) -0.01837(19) 0.13693(12) 0.0264(5) Uani 1 1 d . . . H37 H 1.0564 0.0240 0.1316 0.032 Uiso 1 1 calc R . . C38 C 0.89218(18) -0.10900(16) 0.33656(10) 0.0158(4) Uani 1 1 d . . . C39 C 0.8841(2) -0.21527(17) 0.32611(12) 0.0217(4) Uani 1 1 d . . . H39 H 0.8025 -0.2531 0.3335 0.026 Uiso 1 1 calc R . . C40 C 0.9951(2) -0.26665(18) 0.30490(14) 0.0284(5) Uani 1 1 d . . . H40 H 0.9885 -0.3390 0.2976 0.034 Uiso 1 1 calc R . . C41 C 1.1139(2) -0.21324(19) 0.29454(13) 0.0272(5) Uani 1 1 d . . . H41 H 1.1892 -0.2490 0.2805 0.033 Uiso 1 1 calc R . . C42 C 1.1239(2) -0.10708(18) 0.30458(13) 0.0242(4) Uani 1 1 d . . . H42 H 1.2059 -0.0702 0.2978 0.029 Uiso 1 1 calc R . . C43 C 1.01331(19) -0.05502(17) 0.32462(12) 0.0202(4) Uani 1 1 d . . . H43 H 1.0202 0.0184 0.3303 0.024 Uiso 1 1 calc R . . C44 C 0.62396(18) -0.14838(16) 0.38496(11) 0.0180(4) Uani 1 1 d . . . C45 C 0.6110(2) -0.24081(19) 0.45020(12) 0.0272(5) Uani 1 1 d . . . H45 H 0.6619 -0.2421 0.4878 0.033 Uiso 1 1 calc R . . C46 C 0.5238(2) -0.3314(2) 0.46063(14) 0.0321(5) Uani 1 1 d . . . H46 H 0.5149 -0.3935 0.5054 0.039 Uiso 1 1 calc R . . C47 C 0.4506(2) -0.33049(19) 0.40577(14) 0.0301(5) Uani 1 1 d . . . H47 H 0.3942 -0.3936 0.4116 0.036 Uiso 1 1 calc R . . C48 C 0.4595(2) -0.2377(2) 0.34259(14) 0.0313(5) Uani 1 1 d . . . H48 H 0.4069 -0.2359 0.3056 0.038 Uiso 1 1 calc R . . C49 C 0.5448(2) -0.14673(18) 0.33235(12) 0.0233(4) Uani 1 1 d . . . H49 H 0.5490 -0.0827 0.2888 0.028 Uiso 1 1 calc R . . C50 C 0.77078(19) -0.05031(16) 0.46212(11) 0.0173(4) Uani 1 1 d . . . C51 C 0.8673(2) -0.11264(19) 0.49787(12) 0.0262(5) Uani 1 1 d . . . H51 H 0.9342 -0.1408 0.4702 0.031 Uiso 1 1 calc R . . C52 C 0.8670(2) -0.1341(2) 0.57363(13) 0.0304(5) Uani 1 1 d . . . H52 H 0.9340 -0.1761 0.5971 0.036 Uiso 1 1 calc R . . C53 C 0.7707(2) -0.09526(19) 0.61498(12) 0.0253(5) Uani 1 1 d . . . H53 H 0.7698 -0.1121 0.6670 0.030 Uiso 1 1 calc R . . C54 C 0.6749(2) -0.03137(18) 0.58029(12) 0.0258(5) Uani 1 1 d . . . H54 H 0.6088 -0.0031 0.6083 0.031 Uiso 1 1 calc R . . C55 C 0.6758(2) -0.00884(18) 0.50450(12) 0.0233(4) Uani 1 1 d . . . H55 H 0.6103 0.0357 0.4810 0.028 Uiso 1 1 calc R . . H1 H 0.647(2) 0.146(2) 0.3738(7) 0.034(7) Uiso 1 1 d D . . H2 H 0.8542(13) 0.155(2) 0.3289(13) 0.028(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 0.01573(8) 0.01123(8) 0.01393(8) -0.00362(6) -0.00194(6) 0.00151(5) Cl1 0.0636(5) 0.0504(4) 0.0330(3) -0.0073(3) -0.0063(3) -0.0141(3) Cl2 0.0680(5) 0.0579(4) 0.0427(4) -0.0264(3) -0.0281(3) 0.0264(4) P1 0.0169(2) 0.0152(2) 0.0146(2) -0.00474(19) -0.00232(18) 0.00231(18) P2 0.0194(2) 0.0119(2) 0.0143(2) -0.00390(18) -0.00207(18) 0.00148(18) P3 0.0159(2) 0.0115(2) 0.0158(2) -0.00368(18) -0.00273(18) 0.00046(18) O1 0.0237(8) 0.0433(10) 0.0370(10) -0.0154(8) -0.0141(7) 0.0059(7) O2 0.0195(7) 0.0193(7) 0.0183(7) -0.0077(6) -0.0029(5) 0.0005(5) C1 0.0234(10) 0.0169(9) 0.0196(10) -0.0065(8) 0.0008(8) 0.0028(8) C2 0.0219(10) 0.0181(9) 0.0158(9) -0.0065(8) -0.0016(8) 0.0010(8) C3 0.0265(10) 0.0207(10) 0.0205(10) -0.0075(8) -0.0045(8) 0.0044(8) C4 0.0323(12) 0.0317(12) 0.0217(11) -0.0078(9) -0.0097(9) 0.0087(10) C5 0.0324(12) 0.0358(12) 0.0212(11) -0.0143(10) -0.0061(9) -0.0018(10) C6 0.0421(13) 0.0223(11) 0.0242(11) -0.0105(9) -0.0039(10) -0.0032(10) C7 0.0366(12) 0.0174(10) 0.0189(10) -0.0050(8) -0.0043(9) 0.0012(9) C8 0.0235(10) 0.0177(9) 0.0183(10) -0.0088(8) -0.0045(8) 0.0047(8) C9 0.0257(11) 0.0194(10) 0.0335(12) -0.0104(9) -0.0044(9) 0.0037(8) C10 0.0230(11) 0.0328(12) 0.0473(15) -0.0202(11) -0.0039(10) 0.0037(9) C11 0.0287(12) 0.0363(13) 0.0453(15) -0.0233(11) -0.0163(11) 0.0156(10) C12 0.0469(15) 0.0281(12) 0.0325(13) -0.0120(10) -0.0150(11) 0.0202(11) C13 0.0364(12) 0.0206(10) 0.0236(11) -0.0060(9) -0.0035(9) 0.0099(9) C14 0.0217(9) 0.0124(9) 0.0184(10) -0.0043(7) -0.0016(8) 0.0026(7) C15 0.0270(10) 0.0172(9) 0.0203(10) -0.0073(8) -0.0035(8) -0.0008(8) C16 0.0245(10) 0.0209(10) 0.0284(12) -0.0083(9) -0.0022(9) -0.0040(8) C17 0.0260(10) 0.0179(10) 0.0233(11) -0.0043(8) 0.0029(8) -0.0019(8) C18 0.0277(10) 0.0180(9) 0.0166(10) -0.0045(8) -0.0015(8) 0.0026(8) C19 0.0203(9) 0.0131(9) 0.0182(10) -0.0051(7) -0.0030(8) 0.0021(7) C20 0.0194(9) 0.0189(9) 0.0152(9) -0.0060(8) -0.0015(7) -0.0002(8) C21 0.0179(9) 0.0201(9) 0.0135(9) -0.0039(8) -0.0018(7) 0.0000(8) C22 0.0261(10) 0.0194(10) 0.0186(10) -0.0063(8) -0.0033(8) 0.0013(8) C23 0.0310(11) 0.0274(11) 0.0190(10) -0.0089(9) -0.0063(9) -0.0014(9) C24 0.0279(11) 0.0302(11) 0.0208(11) -0.0057(9) -0.0100(9) 0.0031(9) C25 0.0247(10) 0.0218(10) 0.0217(11) -0.0055(8) -0.0073(8) 0.0047(8) C26 0.0187(9) 0.0157(9) 0.0195(10) -0.0023(8) -0.0018(8) 0.0044(7) C27 0.0209(10) 0.0177(9) 0.0215(10) -0.0029(8) -0.0024(8) 0.0019(8) C28 0.0224(10) 0.0241(11) 0.0325(12) -0.0042(9) -0.0084(9) 0.0009(9) C29 0.0191(10) 0.0244(11) 0.0373(13) 0.0011(10) -0.0003(9) 0.0002(9) C30 0.0248(11) 0.0270(11) 0.0264(12) 0.0008(9) 0.0061(9) 0.0034(9) C31 0.0255(11) 0.0245(11) 0.0217(11) -0.0032(9) -0.0018(8) 0.0043(9) C32 0.0255(10) 0.0186(9) 0.0125(9) -0.0052(7) -0.0030(8) 0.0051(8) C33 0.0278(11) 0.0216(10) 0.0223(11) -0.0080(8) -0.0045(8) 0.0025(8) C34 0.0406(13) 0.0251(11) 0.0306(12) -0.0123(10) -0.0117(10) 0.0013(10) C35 0.0549(16) 0.0243(11) 0.0326(13) -0.0169(10) -0.0128(11) 0.0114(11) C36 0.0401(14) 0.0292(12) 0.0349(13) -0.0145(10) -0.0028(11) 0.0156(10) C57 0.0653(19) 0.0388(15) 0.0430(16) -0.0151(13) -0.0270(14) 0.0089(13) C37 0.0284(11) 0.0256(11) 0.0251(11) -0.0089(9) -0.0015(9) 0.0067(9) C38 0.0197(9) 0.0127(8) 0.0138(9) -0.0021(7) -0.0029(7) 0.0017(7) C39 0.0226(10) 0.0171(9) 0.0252(11) -0.0072(8) -0.0012(8) -0.0012(8) C40 0.0323(12) 0.0186(10) 0.0379(13) -0.0153(9) -0.0023(10) 0.0024(9) C41 0.0220(10) 0.0276(11) 0.0343(13) -0.0137(10) -0.0021(9) 0.0075(9) C42 0.0178(9) 0.0253(11) 0.0310(12) -0.0110(9) -0.0029(8) 0.0018(8) C43 0.0205(10) 0.0164(9) 0.0248(11) -0.0077(8) -0.0040(8) 0.0012(8) C44 0.0166(9) 0.0149(9) 0.0230(10) -0.0076(8) 0.0002(8) 0.0001(7) C45 0.0327(12) 0.0242(11) 0.0223(11) -0.0028(9) -0.0060(9) -0.0056(9) C46 0.0393(13) 0.0228(11) 0.0290(12) -0.0028(9) 0.0016(10) -0.0110(10) C47 0.0259(11) 0.0233(11) 0.0400(14) -0.0104(10) 0.0003(10) -0.0104(9) C48 0.0267(11) 0.0324(12) 0.0384(14) -0.0135(11) -0.0113(10) -0.0027(10) C49 0.0235(10) 0.0193(10) 0.0272(11) -0.0061(9) -0.0066(9) -0.0015(8) C50 0.0196(9) 0.0147(9) 0.0165(9) -0.0035(7) -0.0022(7) -0.0019(7) C51 0.0242(10) 0.0325(12) 0.0224(11) -0.0081(9) -0.0058(8) 0.0085(9) C52 0.0292(11) 0.0392(13) 0.0231(11) -0.0071(10) -0.0109(9) 0.0055(10) C53 0.0315(11) 0.0266(11) 0.0170(10) -0.0049(9) -0.0049(9) -0.0043(9) C54 0.0318(11) 0.0247(11) 0.0190(10) -0.0062(9) 0.0017(9) 0.0039(9) C55 0.0252(10) 0.0217(10) 0.0206(10) -0.0035(8) -0.0032(8) 0.0043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.898(2) . ? Ru1 P2 2.2981(5) . ? Ru1 P3 2.3184(5) . ? Ru1 P1 2.3952(5) . ? Ru1 H1 1.599(3) . ? Ru1 H2 1.600(3) . ? Cl1 C57 1.788(2) . ? Cl2 C57 1.756(2) . ? P1 C26 1.845(2) . ? P1 C32 1.847(2) . ? P1 C21 1.873(2) . ? P2 C14 1.833(2) . ? P2 C2 1.842(2) . ? P2 C8 1.843(2) . ? P3 C38 1.839(2) . ? P3 C44 1.843(2) . ? P3 C50 1.845(2) . ? O1 C1 1.153(3) . ? O2 C20 1.387(2) . ? O2 C19 1.393(2) . ? C2 C3 1.395(3) . ? C2 C7 1.399(3) . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.390(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.391(3) . ? C8 C13 1.397(3) . ? C9 C10 1.391(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C10 H10 0.9500 . ? C11 C12 1.379(4) . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.394(3) . ? C14 C15 1.394(3) . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C17 1.382(3) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C20 C25 1.385(3) . ? C20 C21 1.405(3) . ? C21 C22 1.401(3) . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.394(3) . ? C26 C31 1.400(3) . ? C27 C28 1.393(3) . ? C27 H27 0.9500 . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 C30 1.379(4) . ? C29 H29 0.9500 . ? C30 C31 1.392(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.390(3) . ? C32 C33 1.392(3) . ? C33 C34 1.388(3) . ? C33 H33 0.9500 . ? C34 C35 1.385(4) . ? C34 H34 0.9500 . ? C35 C36 1.362(3) . ? C35 H35 0.9500 . ? C36 C37 1.409(3) . ? C36 H36 0.9500 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C37 H37 0.9500 . ? C38 C39 1.391(3) . ? C38 C43 1.396(3) . ? C39 C40 1.394(3) . ? C39 H39 0.9500 . ? C40 C41 1.375(3) . ? C40 H40 0.9500 . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 C43 1.388(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.385(3) . ? C44 C45 1.397(3) . ? C45 C46 1.397(3) . ? C45 H45 0.9500 . ? C46 C47 1.380(3) . ? C46 H46 0.9500 . ? C47 C48 1.376(3) . ? C47 H47 0.9500 . ? C48 C49 1.389(3) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.393(3) . ? C50 C55 1.394(3) . ? C51 C52 1.389(3) . ? C51 H51 0.9500 . ? C52 C53 1.374(3) . ? C52 H52 0.9500 . ? C53 C54 1.386(3) . ? C53 H53 0.9500 . ? C54 C55 1.388(3) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 P2 98.41(6) . . ? C1 Ru1 P3 105.84(6) . . ? P2 Ru1 P3 143.866(19) . . ? C1 Ru1 P1 90.27(6) . . ? P2 Ru1 P1 103.317(18) . . ? P3 Ru1 P1 102.944(18) . . ? C1 Ru1 H1 90.6(9) . . ? P2 Ru1 H1 75.2(9) . . ? P3 Ru1 H1 78.1(9) . . ? P1 Ru1 H1 178.4(9) . . ? C1 Ru1 H2 177.6(9) . . ? P2 Ru1 H2 79.6(9) . . ? P3 Ru1 H2 75.3(9) . . ? P1 Ru1 H2 91.5(9) . . ? H1 Ru1 H2 87.6(13) . . ? C26 P1 C32 102.09(9) . . ? C26 P1 C21 101.29(9) . . ? C32 P1 C21 98.10(9) . . ? C26 P1 Ru1 120.43(7) . . ? C32 P1 Ru1 114.86(6) . . ? C21 P1 Ru1 116.69(6) . . ? C14 P2 C2 101.07(9) . . ? C14 P2 C8 104.25(9) . . ? C2 P2 C8 99.79(9) . . ? C14 P2 Ru1 115.20(6) . . ? C2 P2 Ru1 116.95(6) . . ? C8 P2 Ru1 117.12(7) . . ? C38 P3 C44 100.74(9) . . ? C38 P3 C50 101.56(9) . . ? C44 P3 C50 98.13(9) . . ? C38 P3 Ru1 117.84(6) . . ? C44 P3 Ru1 121.97(7) . . ? C50 P3 Ru1 113.08(6) . . ? C20 O2 C19 118.08(15) . . ? O1 C1 Ru1 177.92(19) . . ? C3 C2 C7 118.29(19) . . ? C3 C2 P2 121.55(15) . . ? C7 C2 P2 120.15(15) . . ? C4 C3 C2 120.6(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 119.8(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 121.0(2) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 C13 118.73(19) . . ? C9 C8 P2 117.74(15) . . ? C13 C8 P2 123.52(16) . . ? C10 C9 C8 121.0(2) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 119.8(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C12 C11 C10 119.9(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.0(2) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C19 C14 C15 117.52(18) . . ? C19 C14 P2 116.35(15) . . ? C15 C14 P2 125.16(16) . . ? C14 C15 C16 120.8(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.32(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 118.9(2) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 O2 122.41(18) . . ? C18 C19 C14 122.47(19) . . ? O2 C19 C14 115.09(17) . . ? C25 C20 O2 116.06(18) . . ? C25 C20 C21 122.32(19) . . ? O2 C20 C21 121.49(17) . . ? C22 C21 C20 115.86(18) . . ? C22 C21 P1 122.40(15) . . ? C20 C21 P1 121.69(15) . . ? C23 C22 C21 122.3(2) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C24 C23 C22 120.2(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.0(2) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C20 C25 C24 120.2(2) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C31 118.74(19) . . ? C27 C26 P1 119.55(15) . . ? C31 C26 P1 121.68(16) . . ? C28 C27 C26 120.7(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 120.0(2) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 119.7(2) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.7(2) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C26 120.1(2) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C37 C32 C33 118.46(19) . . ? C37 C32 P1 124.68(17) . . ? C33 C32 P1 116.86(15) . . ? C34 C33 C32 121.3(2) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C33 119.9(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 119.5(2) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 121.2(2) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? Cl2 C57 Cl1 110.75(11) . . ? Cl2 C57 H57A 109.5 . . ? Cl1 C57 H57A 109.5 . . ? Cl2 C57 H57B 109.5 . . ? Cl1 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? C32 C37 C36 119.6(2) . . ? C32 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C43 118.49(18) . . ? C39 C38 P3 123.15(15) . . ? C43 C38 P3 118.36(14) . . ? C38 C39 C40 120.43(19) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 120.4(2) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 120.0(2) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 119.7(2) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C42 C43 C38 120.99(19) . . ? C42 C43 H43 119.5 . . ? C38 C43 H43 119.5 . . ? C49 C44 C45 118.39(19) . . ? C49 C44 P3 120.12(15) . . ? C45 C44 P3 121.33(16) . . ? C46 C45 C44 120.6(2) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C47 C46 C45 119.9(2) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C47 C46 119.7(2) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C49 120.6(2) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C44 C49 C48 120.7(2) . . ? C44 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C51 C50 C55 117.88(19) . . ? C51 C50 P3 123.23(16) . . ? C55 C50 P3 118.41(15) . . ? C52 C51 C50 120.7(2) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C53 C52 C51 120.7(2) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 119.6(2) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C55 119.8(2) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C50 121.3(2) . . ? C54 C55 H55 119.4 . . ? C50 C55 H55 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 P1 C26 155.37(9) . . . . ? P2 Ru1 P1 C26 56.66(7) . . . . ? P3 Ru1 P1 C26 -98.30(7) . . . . ? C1 Ru1 P1 C32 -81.96(9) . . . . ? P2 Ru1 P1 C32 179.33(7) . . . . ? P3 Ru1 P1 C32 24.38(7) . . . . ? C1 Ru1 P1 C21 32.04(9) . . . . ? P2 Ru1 P1 C21 -66.67(7) . . . . ? P3 Ru1 P1 C21 138.38(7) . . . . ? C1 Ru1 P2 C14 -105.33(10) . . . . ? P3 Ru1 P2 C14 122.56(8) . . . . ? P1 Ru1 P2 C14 -13.04(8) . . . . ? C1 Ru1 P2 C2 136.15(9) . . . . ? P3 Ru1 P2 C2 4.04(8) . . . . ? P1 Ru1 P2 C2 -131.56(7) . . . . ? C1 Ru1 P2 C8 17.80(10) . . . . ? P3 Ru1 P2 C8 -114.30(8) . . . . ? P1 Ru1 P2 C8 110.09(7) . . . . ? C1 Ru1 P3 C38 117.90(10) . . . . ? P2 Ru1 P3 C38 -111.82(8) . . . . ? P1 Ru1 P3 C38 23.87(7) . . . . ? C1 Ru1 P3 C44 -7.41(10) . . . . ? P2 Ru1 P3 C44 122.87(8) . . . . ? P1 Ru1 P3 C44 -101.44(8) . . . . ? C1 Ru1 P3 C50 -123.97(9) . . . . ? P2 Ru1 P3 C50 6.31(8) . . . . ? P1 Ru1 P3 C50 142.00(7) . . . . ? P2 Ru1 C1 O1 43(5) . . . . ? P3 Ru1 C1 O1 -164(5) . . . . ? P1 Ru1 C1 O1 -61(5) . . . . ? C14 P2 C2 C3 -120.56(18) . . . . ? C8 P2 C2 C3 132.68(18) . . . . ? Ru1 P2 C2 C3 5.3(2) . . . . ? C14 P2 C2 C7 58.47(19) . . . . ? C8 P2 C2 C7 -48.28(19) . . . . ? Ru1 P2 C2 C7 -175.63(15) . . . . ? C7 C2 C3 C4 -1.7(3) . . . . ? P2 C2 C3 C4 177.35(17) . . . . ? C2 C3 C4 C5 -1.2(3) . . . . ? C3 C4 C5 C6 2.8(4) . . . . ? C4 C5 C6 C7 -1.4(4) . . . . ? C5 C6 C7 C2 -1.5(4) . . . . ? C3 C2 C7 C6 3.1(3) . . . . ? P2 C2 C7 C6 -176.01(17) . . . . ? C14 P2 C8 C9 176.13(17) . . . . ? C2 P2 C8 C9 -79.69(18) . . . . ? Ru1 P2 C8 C9 47.55(19) . . . . ? C14 P2 C8 C13 -4.3(2) . . . . ? C2 P2 C8 C13 99.88(19) . . . . ? Ru1 P2 C8 C13 -132.88(17) . . . . ? C13 C8 C9 C10 -0.7(3) . . . . ? P2 C8 C9 C10 178.84(18) . . . . ? C8 C9 C10 C11 1.1(4) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C10 C11 C12 C13 -1.1(4) . . . . ? C11 C12 C13 C8 1.5(4) . . . . ? C9 C8 C13 C12 -0.6(3) . . . . ? P2 C8 C13 C12 179.86(18) . . . . ? C2 P2 C14 C19 -173.28(15) . . . . ? C8 P2 C14 C19 -70.07(16) . . . . ? Ru1 P2 C14 C19 59.66(16) . . . . ? C2 P2 C14 C15 18.35(19) . . . . ? C8 P2 C14 C15 121.56(18) . . . . ? Ru1 P2 C14 C15 -108.71(17) . . . . ? C19 C14 C15 C16 0.7(3) . . . . ? P2 C14 C15 C16 168.98(16) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? C16 C17 C18 C19 0.1(3) . . . . ? C17 C18 C19 O2 178.73(18) . . . . ? C17 C18 C19 C14 0.7(3) . . . . ? C20 O2 C19 C18 38.0(3) . . . . ? C20 O2 C19 C14 -143.83(17) . . . . ? C15 C14 C19 C18 -1.1(3) . . . . ? P2 C14 C19 C18 -170.35(16) . . . . ? C15 C14 C19 O2 -179.26(17) . . . . ? P2 C14 C19 O2 11.5(2) . . . . ? C19 O2 C20 C25 -112.0(2) . . . . ? C19 O2 C20 C21 72.1(2) . . . . ? C25 C20 C21 C22 3.0(3) . . . . ? O2 C20 C21 C22 178.71(17) . . . . ? C25 C20 C21 P1 -174.31(16) . . . . ? O2 C20 C21 P1 1.4(3) . . . . ? C26 P1 C21 C22 94.31(18) . . . . ? C32 P1 C21 C22 -9.83(18) . . . . ? Ru1 P1 C21 C22 -132.97(15) . . . . ? C26 P1 C21 C20 -88.52(17) . . . . ? C32 P1 C21 C20 167.35(16) . . . . ? Ru1 P1 C21 C20 44.20(18) . . . . ? C20 C21 C22 C23 -2.6(3) . . . . ? P1 C21 C22 C23 174.69(16) . . . . ? C21 C22 C23 C24 0.8(3) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? O2 C20 C25 C24 -177.46(18) . . . . ? C21 C20 C25 C24 -1.6(3) . . . . ? C23 C24 C25 C20 -0.5(3) . . . . ? C32 P1 C26 C27 -115.57(16) . . . . ? C21 P1 C26 C27 143.49(16) . . . . ? Ru1 P1 C26 C27 13.07(18) . . . . ? C32 P1 C26 C31 62.50(18) . . . . ? C21 P1 C26 C31 -38.44(19) . . . . ? Ru1 P1 C26 C31 -168.86(14) . . . . ? C31 C26 C27 C28 -0.6(3) . . . . ? P1 C26 C27 C28 177.52(16) . . . . ? C26 C27 C28 C29 0.3(3) . . . . ? C27 C28 C29 C30 0.3(3) . . . . ? C28 C29 C30 C31 -0.6(3) . . . . ? C29 C30 C31 C26 0.3(3) . . . . ? C27 C26 C31 C30 0.3(3) . . . . ? P1 C26 C31 C30 -177.81(16) . . . . ? C26 P1 C32 C37 6.6(2) . . . . ? C21 P1 C32 C37 110.01(19) . . . . ? Ru1 P1 C32 C37 -125.52(17) . . . . ? C26 P1 C32 C33 -173.53(16) . . . . ? C21 P1 C32 C33 -70.08(17) . . . . ? Ru1 P1 C32 C33 54.39(17) . . . . ? C37 C32 C33 C34 -0.3(3) . . . . ? P1 C32 C33 C34 179.78(17) . . . . ? C32 C33 C34 C35 -0.1(3) . . . . ? C33 C34 C35 C36 0.8(4) . . . . ? C34 C35 C36 C37 -1.2(3) . . . . ? C33 C32 C37 C36 -0.1(3) . . . . ? P1 C32 C37 C36 179.86(15) . . . . ? C35 C36 C37 C32 0.8(3) . . . . ? C44 P3 C38 C39 7.12(19) . . . . ? C50 P3 C38 C39 107.82(18) . . . . ? Ru1 P3 C38 C39 -128.08(16) . . . . ? C44 P3 C38 C43 -172.89(16) . . . . ? C50 P3 C38 C43 -72.18(17) . . . . ? Ru1 P3 C38 C43 51.91(17) . . . . ? C43 C38 C39 C40 0.6(3) . . . . ? P3 C38 C39 C40 -179.39(17) . . . . ? C38 C39 C40 C41 0.4(3) . . . . ? C39 C40 C41 C42 -0.5(4) . . . . ? C40 C41 C42 C43 -0.4(4) . . . . ? C41 C42 C43 C38 1.5(3) . . . . ? C39 C38 C43 C42 -1.6(3) . . . . ? P3 C38 C43 C42 178.41(17) . . . . ? C38 P3 C44 C49 -98.44(18) . . . . ? C50 P3 C44 C49 158.08(17) . . . . ? Ru1 P3 C44 C49 34.3(2) . . . . ? C38 P3 C44 C45 76.95(19) . . . . ? C50 P3 C44 C45 -26.53(19) . . . . ? Ru1 P3 C44 C45 -150.30(15) . . . . ? C49 C44 C45 C46 2.5(3) . . . . ? P3 C44 C45 C46 -172.96(18) . . . . ? C44 C45 C46 C47 0.7(4) . . . . ? C45 C46 C47 C48 -3.1(4) . . . . ? C46 C47 C48 C49 2.2(4) . . . . ? C45 C44 C49 C48 -3.4(3) . . . . ? P3 C44 C49 C48 172.16(18) . . . . ? C47 C48 C49 C44 1.0(4) . . . . ? C38 P3 C50 C51 -5.08(19) . . . . ? C44 P3 C50 C51 97.70(18) . . . . ? Ru1 P3 C50 C51 -132.34(16) . . . . ? C38 P3 C50 C55 -176.89(16) . . . . ? C44 P3 C50 C55 -74.10(17) . . . . ? Ru1 P3 C50 C55 55.86(17) . . . . ? C55 C50 C51 C52 1.1(3) . . . . ? P3 C50 C51 C52 -170.73(18) . . . . ? C50 C51 C52 C53 0.6(4) . . . . ? C51 C52 C53 C54 -1.7(4) . . . . ? C52 C53 C54 C55 1.1(3) . . . . ? C53 C54 C55 C50 0.7(3) . . . . ? C51 C50 C55 C54 -1.8(3) . . . . ? P3 C50 C55 C54 170.48(17) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.201 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.071