# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mary F. Mahon' _publ_contact_author_email chsmfm@bath.ac.uk loop_ _publ_author_name 'Michael J. Page' 'Mary F. Mahon' 'Michael K. Whittlesey' data_h10mkw5 _database_code_depnum_ccdc_archive 'CCDC 810318' #TrackingRef '- bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 N2 O P2 Ru' _chemical_formula_weight 759.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9920(2) _cell_length_b 16.7110(3) _cell_length_c 18.6240(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.524(1) _cell_angle_gamma 90.00 _cell_volume 3708.05(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 72667 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 1.119 _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 66272 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 30.06 _reflns_number_total 10843 _reflns_number_gt 8547 _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. H1 located and refined at a diatnce of 1.6 Angstroms from Ru1. H12 included at a calculated position - with refinement of Uiso in the final least-squares cycles. ; _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^)+(0.0307P)^2^+1.9170P] 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 10843 _refine_ls_number_parameters 435 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _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 0.802928(11) 0.264187(8) 0.090601(7) 0.01815(4) Uani 1 1 d D . . H1 H 0.8125(19) 0.2335(13) 0.1729(5) 0.041(6) Uiso 1 1 d D . . P1 P 0.66900(4) 0.16601(3) 0.07907(2) 0.02126(9) Uani 1 1 d . . . P2 P 0.92737(4) 0.15893(3) 0.07804(2) 0.01998(9) Uani 1 1 d . . . O1 O 0.78865(14) 0.32368(10) -0.06498(7) 0.0424(4) Uani 1 1 d . . . N1 N 1.00439(13) 0.39107(9) 0.13277(8) 0.0251(3) Uani 1 1 d . . . N2 N 0.84904(13) 0.40879(9) 0.17769(8) 0.0231(3) Uani 1 1 d . . . C1 C 0.79319(15) 0.30144(11) -0.00599(9) 0.0246(4) Uani 1 1 d . . . C2 C 0.90092(14) 0.35858(10) 0.13428(9) 0.0213(3) Uani 1 1 d . . . C3 C 1.01463(17) 0.46129(11) 0.17338(11) 0.0317(4) Uani 1 1 d . . . H3 H 1.0783 0.4954 0.1798 0.038 Uiso 1 1 calc R . . C4 C 0.91781(17) 0.47171(11) 0.20174(10) 0.0293(4) Uani 1 1 d . . . H4 H 0.9000 0.5141 0.2324 0.035 Uiso 1 1 calc R . . C5 C 1.08991(15) 0.36053(11) 0.08956(10) 0.0250(4) Uani 1 1 d . . . H5 H 1.0700 0.3039 0.0763 0.030 Uiso 1 1 calc R . . C6 C 1.08865(17) 0.40805(12) 0.01955(11) 0.0318(4) Uani 1 1 d . . . H6A H 1.1035 0.4652 0.0310 0.038 Uiso 1 1 calc R . . H6B H 1.0135 0.4040 -0.0084 0.038 Uiso 1 1 calc R . . C7 C 1.17727(19) 0.37652(14) -0.02606(12) 0.0397(5) Uani 1 1 d . . . H7A H 1.1584 0.3210 -0.0415 0.048 Uiso 1 1 calc R . . H7B H 1.1777 0.4099 -0.0700 0.048 Uiso 1 1 calc R . . C8 C 1.29329(18) 0.37821(14) 0.01698(14) 0.0441(5) Uani 1 1 d . . . H8A H 1.3491 0.3558 -0.0128 0.053 Uiso 1 1 calc R . . H8B H 1.3147 0.4343 0.0289 0.053 Uiso 1 1 calc R . . C9 C 1.29470(16) 0.33022(13) 0.08622(12) 0.0386(5) Uani 1 1 d . . . H9A H 1.3698 0.3343 0.1141 0.046 Uiso 1 1 calc R . . H9B H 1.2805 0.2732 0.0741 0.046 Uiso 1 1 calc R . . C10 C 1.20621(16) 0.36011(13) 0.13250(11) 0.0339(4) Uani 1 1 d . . . H10A H 1.2256 0.4150 0.1497 0.041 Uiso 1 1 calc R . . H10B H 1.2054 0.3251 0.1753 0.041 Uiso 1 1 calc R . . C11 C 0.73496(15) 0.38774(11) 0.19282(9) 0.0247(4) Uani 1 1 d . . . H11 H 0.7417 0.3450 0.2307 0.030 Uiso 1 1 calc R . . C12 C 0.67920(15) 0.35043(10) 0.12271(9) 0.0230(3) Uani 1 1 d . . . H12 H 0.6108 0.3206 0.1335 0.034(6) Uiso 1 1 calc R . . C13 C 0.64349(16) 0.41730(11) 0.06837(10) 0.0268(4) Uani 1 1 d . . . H13A H 0.7115 0.4427 0.0530 0.032 Uiso 1 1 calc R . . H13B H 0.6005 0.3936 0.0251 0.032 Uiso 1 1 calc R . . C14 C 0.57148(17) 0.48176(12) 0.09952(11) 0.0314(4) Uani 1 1 d . . . H14A H 0.5497 0.5228 0.0622 0.038 Uiso 1 1 calc R . . H14B H 0.5021 0.4572 0.1136 0.038 Uiso 1 1 calc R . . C15 C 0.63657(17) 0.52111(11) 0.16527(11) 0.0314(4) Uani 1 1 d . . . H15A H 0.7036 0.5486 0.1507 0.038 Uiso 1 1 calc R . . H15B H 0.5888 0.5616 0.1857 0.038 Uiso 1 1 calc R . . C16 C 0.67261(17) 0.45823(12) 0.22203(10) 0.0313(4) Uani 1 1 d . . . H16A H 0.6053 0.4378 0.2423 0.038 Uiso 1 1 calc R . . H16B H 0.7218 0.4836 0.2619 0.038 Uiso 1 1 calc R . . C17 C 0.73846(15) 0.06809(10) 0.09237(10) 0.0261(4) Uani 1 1 d . . . H17A H 0.7597 0.0583 0.1446 0.031 Uiso 1 1 calc R . . H17B H 0.6866 0.0251 0.0733 0.031 Uiso 1 1 calc R . . C18 C 0.84283(15) 0.06777(10) 0.05275(10) 0.0255(4) Uani 1 1 d . . . H18A H 0.8207 0.0670 -0.0001 0.031 Uiso 1 1 calc R . . H18B H 0.8881 0.0193 0.0660 0.031 Uiso 1 1 calc R . . C19 C 0.56721(15) 0.16087(11) 0.14582(10) 0.0257(4) Uani 1 1 d . . . C20 C 0.60458(18) 0.17830(12) 0.21824(10) 0.0328(4) Uani 1 1 d . . . H20 H 0.6806 0.1934 0.2313 0.039 Uiso 1 1 calc R . . C21 C 0.5322(2) 0.17387(12) 0.27111(11) 0.0373(5) Uani 1 1 d . . . H21 H 0.5592 0.1851 0.3200 0.045 Uiso 1 1 calc R . . C22 C 0.42168(19) 0.15332(14) 0.25290(13) 0.0426(5) Uani 1 1 d . . . H22 H 0.3717 0.1517 0.2889 0.051 Uiso 1 1 calc R . . C23 C 0.38388(19) 0.13519(18) 0.18273(13) 0.0526(7) Uani 1 1 d . . . H23 H 0.3077 0.1201 0.1703 0.063 Uiso 1 1 calc R . . C24 C 0.45670(17) 0.13870(15) 0.12900(12) 0.0416(5) Uani 1 1 d . . . H24 H 0.4295 0.1257 0.0805 0.050 Uiso 1 1 calc R . . C25 C 0.58112(15) 0.15741(11) -0.00758(9) 0.0257(4) Uani 1 1 d . . . C26 C 0.5750(2) 0.08921(14) -0.05011(12) 0.0414(5) Uani 1 1 d . . . H26 H 0.6114 0.0415 -0.0323 0.050 Uiso 1 1 calc R . . C27 C 0.5156(2) 0.09020(16) -0.11923(12) 0.0507(6) Uani 1 1 d . . . H27 H 0.5128 0.0435 -0.1485 0.061 Uiso 1 1 calc R . . C28 C 0.46111(19) 0.15856(15) -0.14501(11) 0.0422(5) Uani 1 1 d . . . H28 H 0.4219 0.1593 -0.1923 0.051 Uiso 1 1 calc R . . C29 C 0.46350(18) 0.22586(14) -0.10236(11) 0.0374(5) Uani 1 1 d . . . H29 H 0.4240 0.2726 -0.1195 0.045 Uiso 1 1 calc R . . C30 C 0.52401(17) 0.22536(12) -0.03393(10) 0.0316(4) Uani 1 1 d . . . H30 H 0.5262 0.2722 -0.0049 0.038 Uiso 1 1 calc R . . C31 C 1.02234(15) 0.15433(10) 0.00699(9) 0.0229(3) Uani 1 1 d . . . C32 C 0.97539(17) 0.16194(11) -0.06506(10) 0.0289(4) Uani 1 1 d . . . H32 H 0.8967 0.1695 -0.0757 0.035 Uiso 1 1 calc R . . C33 C 1.04223(19) 0.15861(12) -0.12105(10) 0.0336(4) Uani 1 1 d . . . H33 H 1.0089 0.1620 -0.1697 0.040 Uiso 1 1 calc R . . C34 C 1.15725(19) 0.15032(12) -0.10614(11) 0.0347(5) Uani 1 1 d . . . H34 H 1.2031 0.1491 -0.1445 0.042 Uiso 1 1 calc R . . C35 C 1.20531(17) 0.14389(12) -0.03554(11) 0.0316(4) Uani 1 1 d . . . H35 H 1.2844 0.1385 -0.0252 0.038 Uiso 1 1 calc R . . C36 C 1.13790(16) 0.14529(11) 0.02063(10) 0.0265(4) Uani 1 1 d . . . H36 H 1.1716 0.1400 0.0691 0.032 Uiso 1 1 calc R . . C37 C 1.01886(14) 0.12525(10) 0.15834(9) 0.0223(3) Uani 1 1 d . . . C38 C 1.04531(15) 0.17856(11) 0.21517(9) 0.0262(4) Uani 1 1 d . . . H38 H 1.0173 0.2317 0.2113 0.031 Uiso 1 1 calc R . . C39 C 1.11220(16) 0.15509(13) 0.27755(10) 0.0306(4) Uani 1 1 d . . . H39 H 1.1310 0.1925 0.3154 0.037 Uiso 1 1 calc R . . C40 C 1.15129(17) 0.07738(13) 0.28462(10) 0.0339(4) Uani 1 1 d . . . H40 H 1.1951 0.0609 0.3278 0.041 Uiso 1 1 calc R . . C41 C 1.12648(18) 0.02389(13) 0.22871(11) 0.0364(5) Uani 1 1 d . . . H41 H 1.1535 -0.0295 0.2334 0.044 Uiso 1 1 calc R . . C42 C 1.06199(17) 0.04775(11) 0.16550(10) 0.0300(4) Uani 1 1 d . . . H42 H 1.0472 0.0109 0.1268 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02062(7) 0.01563(6) 0.01772(6) 0.00016(5) 0.00013(4) -0.00072(5) P1 0.0225(2) 0.0191(2) 0.0216(2) 0.00067(16) 0.00040(16) -0.00268(17) P2 0.0230(2) 0.0166(2) 0.02013(19) -0.00080(16) 0.00138(16) -0.00071(16) O1 0.0532(10) 0.0498(9) 0.0239(7) 0.0100(6) 0.0031(6) 0.0046(8) N1 0.0284(8) 0.0197(7) 0.0268(7) -0.0035(6) 0.0010(6) -0.0047(6) N2 0.0292(8) 0.0191(7) 0.0203(7) -0.0021(6) -0.0001(6) -0.0004(6) C1 0.0266(9) 0.0235(9) 0.0232(8) -0.0014(7) 0.0002(7) -0.0001(7) C2 0.0250(8) 0.0180(8) 0.0199(8) 0.0016(6) -0.0019(6) -0.0001(7) C3 0.0363(11) 0.0216(9) 0.0360(10) -0.0070(8) -0.0003(8) -0.0090(8) C4 0.0389(11) 0.0206(9) 0.0275(9) -0.0055(7) 0.0000(8) -0.0024(8) C5 0.0238(9) 0.0197(8) 0.0312(9) -0.0004(7) 0.0022(7) -0.0030(7) C6 0.0305(10) 0.0308(10) 0.0343(10) 0.0060(8) 0.0045(8) 0.0015(8) C7 0.0419(12) 0.0405(12) 0.0389(11) 0.0062(9) 0.0133(9) 0.0011(10) C8 0.0313(11) 0.0377(12) 0.0658(15) 0.0070(11) 0.0168(10) 0.0004(9) C9 0.0240(10) 0.0298(10) 0.0610(14) 0.0018(10) -0.0001(9) -0.0023(8) C10 0.0284(10) 0.0308(10) 0.0410(11) 0.0030(9) -0.0034(8) -0.0028(8) C11 0.0297(9) 0.0241(9) 0.0206(8) 0.0004(7) 0.0043(7) 0.0018(7) C12 0.0244(9) 0.0210(8) 0.0237(8) 0.0007(7) 0.0030(6) 0.0003(7) C13 0.0309(10) 0.0232(9) 0.0255(9) 0.0010(7) 0.0000(7) 0.0038(7) C14 0.0317(10) 0.0267(10) 0.0356(10) 0.0035(8) 0.0021(8) 0.0062(8) C15 0.0347(10) 0.0236(9) 0.0376(10) -0.0020(8) 0.0108(8) 0.0042(8) C16 0.0383(11) 0.0294(10) 0.0275(9) -0.0037(8) 0.0092(8) 0.0011(8) C17 0.0289(9) 0.0189(8) 0.0302(9) 0.0023(7) 0.0019(7) -0.0030(7) C18 0.0285(9) 0.0188(8) 0.0290(9) -0.0041(7) 0.0021(7) -0.0021(7) C19 0.0272(9) 0.0205(8) 0.0300(9) 0.0050(7) 0.0055(7) -0.0001(7) C20 0.0385(11) 0.0303(10) 0.0308(10) -0.0032(8) 0.0084(8) -0.0087(9) C21 0.0540(14) 0.0285(10) 0.0318(10) -0.0004(8) 0.0153(9) -0.0041(9) C22 0.0411(12) 0.0439(13) 0.0458(13) 0.0169(10) 0.0187(10) 0.0119(10) C23 0.0258(11) 0.0814(19) 0.0507(14) 0.0244(13) 0.0051(9) -0.0018(12) C24 0.0297(11) 0.0607(15) 0.0336(11) 0.0146(10) -0.0004(8) -0.0082(10) C25 0.0234(9) 0.0290(9) 0.0241(8) -0.0017(7) 0.0004(7) -0.0060(7) C26 0.0464(13) 0.0368(12) 0.0377(11) -0.0098(9) -0.0087(9) -0.0002(10) C27 0.0561(15) 0.0552(15) 0.0371(12) -0.0193(11) -0.0107(10) -0.0020(12) C28 0.0374(12) 0.0643(16) 0.0233(9) -0.0032(10) -0.0040(8) -0.0114(11) C29 0.0329(11) 0.0462(13) 0.0310(10) 0.0084(9) -0.0055(8) -0.0056(9) C30 0.0335(10) 0.0323(11) 0.0274(9) 0.0018(8) -0.0037(7) -0.0035(8) C31 0.0296(9) 0.0165(8) 0.0229(8) -0.0024(6) 0.0046(7) -0.0009(7) C32 0.0347(10) 0.0255(9) 0.0263(9) -0.0006(7) 0.0029(7) 0.0016(8) C33 0.0507(13) 0.0289(10) 0.0218(8) -0.0017(7) 0.0073(8) -0.0033(9) C34 0.0480(12) 0.0269(10) 0.0324(10) -0.0042(8) 0.0185(9) -0.0057(9) C35 0.0316(10) 0.0279(10) 0.0370(10) -0.0045(8) 0.0105(8) -0.0025(8) C36 0.0293(9) 0.0243(9) 0.0263(9) -0.0018(7) 0.0046(7) -0.0022(7) C37 0.0228(8) 0.0214(8) 0.0228(8) 0.0029(7) 0.0033(6) -0.0007(7) C38 0.0262(9) 0.0252(9) 0.0269(9) -0.0002(7) 0.0012(7) 0.0021(7) C39 0.0279(10) 0.0396(11) 0.0236(8) -0.0034(8) 0.0004(7) 0.0014(8) C40 0.0292(10) 0.0434(12) 0.0284(9) 0.0109(9) 0.0000(7) 0.0039(9) C41 0.0377(11) 0.0290(10) 0.0415(11) 0.0099(9) -0.0001(9) 0.0052(9) C42 0.0340(10) 0.0226(9) 0.0324(9) 0.0004(7) 0.0002(8) 0.0011(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 1.8947(17) . ? Ru1 C2 2.0770(17) . ? Ru1 C12 2.1996(17) . ? Ru1 P1 2.2889(5) . ? Ru1 P2 2.3356(5) . ? Ru1 H1 1.608(5) . ? P1 C25 1.8301(18) . ? P1 C17 1.8400(18) . ? P1 C19 1.8406(19) . ? P2 C37 1.8397(17) . ? P2 C31 1.8429(18) . ? P2 C18 1.8606(18) . ? O1 C1 1.155(2) . ? N1 C2 1.358(2) . ? N1 C3 1.394(2) . ? N1 C5 1.465(2) . ? N2 C2 1.363(2) . ? N2 C4 1.379(2) . ? N2 C11 1.470(2) . ? C3 C4 1.340(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.525(3) . ? C5 C10 1.527(3) . ? C5 H5 1.0000 . ? C6 C7 1.528(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.525(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.517(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.525(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.528(3) . ? C11 C12 1.530(2) . ? C11 H11 1.0000 . ? C12 C13 1.536(2) . ? C12 H12 1.0000 . ? C13 C14 1.535(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.518(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.377(3) . ? C19 C20 1.403(3) . ? C20 C21 1.386(3) . ? C20 H20 0.9500 . ? C21 C22 1.374(3) . ? C21 H21 0.9500 . ? C22 C23 1.368(3) . ? C22 H22 0.9500 . ? C23 C24 1.402(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.385(3) . ? C25 C30 1.387(3) . ? C26 C27 1.399(3) . ? C26 H26 0.9500 . ? C27 C28 1.375(4) . ? C27 H27 0.9500 . ? C28 C29 1.375(3) . ? C28 H28 0.9500 . ? C29 C30 1.393(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.388(3) . ? C31 C32 1.401(2) . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(3) . ? C33 H33 0.9500 . ? C34 C35 1.378(3) . ? C34 H34 0.9500 . ? C35 C36 1.393(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.392(2) . ? C37 C42 1.395(3) . ? C38 C39 1.391(2) . ? C38 H38 0.9500 . ? C39 C40 1.382(3) . ? C39 H39 0.9500 . ? C40 C41 1.379(3) . ? C40 H40 0.9500 . ? C41 C42 1.391(3) . ? C41 H41 0.9500 . ? C42 H42 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 95.36(7) . . ? C1 Ru1 C12 94.14(7) . . ? C2 Ru1 C12 76.41(7) . . ? C1 Ru1 P1 100.35(6) . . ? C2 Ru1 P1 160.20(5) . . ? C12 Ru1 P1 90.42(5) . . ? C1 Ru1 P2 97.09(6) . . ? C2 Ru1 P2 105.77(5) . . ? C12 Ru1 P2 168.28(5) . . ? P1 Ru1 P2 84.277(17) . . ? C1 Ru1 H1 179.2(9) . . ? C2 Ru1 H1 83.8(8) . . ? C12 Ru1 H1 85.8(8) . . ? P1 Ru1 H1 80.5(8) . . ? P2 Ru1 H1 83.0(8) . . ? C25 P1 C17 104.80(9) . . ? C25 P1 C19 103.43(8) . . ? C17 P1 C19 101.10(8) . . ? C25 P1 Ru1 117.81(6) . . ? C17 P1 Ru1 108.83(6) . . ? C19 P1 Ru1 118.83(6) . . ? C37 P2 C31 102.17(8) . . ? C37 P2 C18 102.28(8) . . ? C31 P2 C18 98.48(8) . . ? C37 P2 Ru1 118.54(6) . . ? C31 P2 Ru1 123.88(6) . . ? C18 P2 Ru1 107.82(6) . . ? C2 N1 C3 110.47(15) . . ? C2 N1 C5 124.78(14) . . ? C3 N1 C5 124.56(15) . . ? C2 N2 C4 111.43(15) . . ? C2 N2 C11 117.62(14) . . ? C4 N2 C11 130.93(15) . . ? O1 C1 Ru1 179.06(17) . . ? N1 C2 N2 104.24(14) . . ? N1 C2 Ru1 140.66(13) . . ? N2 C2 Ru1 115.06(12) . . ? C4 C3 N1 107.24(16) . . ? C4 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? C3 C4 N2 106.61(16) . . ? C3 C4 H4 126.7 . . ? N2 C4 H4 126.7 . . ? N1 C5 C6 110.40(15) . . ? N1 C5 C10 111.63(15) . . ? C6 C5 C10 111.70(15) . . ? N1 C5 H5 107.6 . . ? C6 C5 H5 107.6 . . ? C10 C5 H5 107.6 . . ? C5 C6 C7 110.85(16) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 110.62(19) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 111.00(17) . . ? 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 111.46(17) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C5 111.00(17) . . ? 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 C16 112.79(15) . . ? N2 C11 C12 105.06(13) . . ? C16 C11 C12 115.70(15) . . ? N2 C11 H11 107.6 . . ? C16 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C11 C12 C13 109.14(14) . . ? C11 C12 Ru1 104.83(11) . . ? C13 C12 Ru1 116.35(12) . . ? C11 C12 H12 108.8 . . ? C13 C12 H12 108.8 . . ? Ru1 C12 H12 108.8 . . ? C14 C13 C12 112.85(15) . . ? C14 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? C14 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 110.34(16) . . ? 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 . . ? C16 C15 C14 109.89(16) . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C15 C16 C11 113.43(15) . . ? C15 C16 H16A 108.9 . . ? C11 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C11 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 P1 108.79(12) . . ? C18 C17 H17A 109.9 . . ? P1 C17 H17A 109.9 . . ? C18 C17 H17B 109.9 . . ? P1 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 P2 109.18(12) . . ? C17 C18 H18A 109.8 . . ? P2 C18 H18A 109.8 . . ? C17 C18 H18B 109.8 . . ? P2 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? C24 C19 C20 117.94(18) . . ? C24 C19 P1 123.63(15) . . ? C20 C19 P1 118.41(14) . . ? C21 C20 C19 120.96(19) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.8(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 120.7(2) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C30 118.65(17) . . ? C26 C25 P1 123.82(15) . . ? C30 C25 P1 117.36(14) . . ? C25 C26 C27 120.3(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 119.99(19) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 119.9(2) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 120.91(19) . . ? C25 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C36 C31 C32 118.00(17) . . ? C36 C31 P2 123.96(13) . . ? C32 C31 P2 118.04(14) . . ? C33 C32 C31 120.86(19) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.11(18) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.92(18) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 119.97(19) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 C35 121.11(17) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C38 C37 C42 118.12(16) . . ? C38 C37 P2 119.05(13) . . ? C42 C37 P2 122.82(14) . . ? C39 C38 C37 120.96(17) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 120.10(18) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.71(18) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.31(19) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.74(18) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? 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 C25 -7.58(9) . . . . ? C2 Ru1 P1 C25 134.36(15) . . . . ? C12 Ru1 P1 C25 86.70(8) . . . . ? P2 Ru1 P1 C25 -103.78(7) . . . . ? C1 Ru1 P1 C17 111.43(8) . . . . ? C2 Ru1 P1 C17 -106.62(15) . . . . ? C12 Ru1 P1 C17 -154.29(8) . . . . ? P2 Ru1 P1 C17 15.24(6) . . . . ? C1 Ru1 P1 C19 -133.75(9) . . . . ? C2 Ru1 P1 C19 8.20(16) . . . . ? C12 Ru1 P1 C19 -39.46(8) . . . . ? P2 Ru1 P1 C19 130.06(7) . . . . ? C1 Ru1 P2 C37 153.50(8) . . . . ? C2 Ru1 P2 C37 55.86(8) . . . . ? C12 Ru1 P2 C37 -43.3(2) . . . . ? P1 Ru1 P2 C37 -106.75(7) . . . . ? C1 Ru1 P2 C31 22.64(9) . . . . ? C2 Ru1 P2 C31 -75.00(8) . . . . ? C12 Ru1 P2 C31 -174.1(2) . . . . ? P1 Ru1 P2 C31 122.40(7) . . . . ? C1 Ru1 P2 C18 -91.09(8) . . . . ? C2 Ru1 P2 C18 171.28(8) . . . . ? C12 Ru1 P2 C18 72.1(2) . . . . ? P1 Ru1 P2 C18 8.67(6) . . . . ? C2 Ru1 C1 O1 84(12) . . . . ? C12 Ru1 C1 O1 161(12) . . . . ? P1 Ru1 C1 O1 -108(12) . . . . ? P2 Ru1 C1 O1 -23(12) . . . . ? C3 N1 C2 N2 -1.39(19) . . . . ? C5 N1 C2 N2 -176.51(15) . . . . ? C3 N1 C2 Ru1 175.96(15) . . . . ? C5 N1 C2 Ru1 0.8(3) . . . . ? C4 N2 C2 N1 0.93(19) . . . . ? C11 N2 C2 N1 -177.50(14) . . . . ? C4 N2 C2 Ru1 -177.22(11) . . . . ? C11 N2 C2 Ru1 4.36(19) . . . . ? C1 Ru1 C2 N1 -65.1(2) . . . . ? C12 Ru1 C2 N1 -158.1(2) . . . . ? P1 Ru1 C2 N1 152.38(13) . . . . ? P2 Ru1 C2 N1 33.8(2) . . . . ? C1 Ru1 C2 N2 112.02(13) . . . . ? C12 Ru1 C2 N2 19.05(12) . . . . ? P1 Ru1 C2 N2 -30.5(2) . . . . ? P2 Ru1 C2 N2 -149.04(11) . . . . ? C2 N1 C3 C4 1.4(2) . . . . ? C5 N1 C3 C4 176.51(16) . . . . ? N1 C3 C4 N2 -0.7(2) . . . . ? C2 N2 C4 C3 -0.1(2) . . . . ? C11 N2 C4 C3 178.04(17) . . . . ? C2 N1 C5 C6 97.97(19) . . . . ? C3 N1 C5 C6 -76.5(2) . . . . ? C2 N1 C5 C10 -137.14(17) . . . . ? C3 N1 C5 C10 48.4(2) . . . . ? N1 C5 C6 C7 -179.81(16) . . . . ? C10 C5 C6 C7 55.3(2) . . . . ? C5 C6 C7 C8 -56.3(2) . . . . ? C6 C7 C8 C9 57.0(2) . . . . ? C7 C8 C9 C10 -56.5(2) . . . . ? C8 C9 C10 C5 54.9(2) . . . . ? N1 C5 C10 C9 -178.54(16) . . . . ? C6 C5 C10 C9 -54.4(2) . . . . ? C2 N2 C11 C16 -162.86(15) . . . . ? C4 N2 C11 C16 19.1(3) . . . . ? C2 N2 C11 C12 -35.98(19) . . . . ? C4 N2 C11 C12 145.96(17) . . . . ? N2 C11 C12 C13 -78.00(17) . . . . ? C16 C11 C12 C13 47.1(2) . . . . ? N2 C11 C12 Ru1 47.31(14) . . . . ? C16 C11 C12 Ru1 172.39(13) . . . . ? C1 Ru1 C12 C11 -130.92(12) . . . . ? C2 Ru1 C12 C11 -36.40(11) . . . . ? P1 Ru1 C12 C11 128.68(11) . . . . ? P2 Ru1 C12 C11 65.8(3) . . . . ? C1 Ru1 C12 C13 -10.27(14) . . . . ? C2 Ru1 C12 C13 84.25(13) . . . . ? P1 Ru1 C12 C13 -110.68(13) . . . . ? P2 Ru1 C12 C13 -173.59(16) . . . . ? C11 C12 C13 C14 -52.9(2) . . . . ? Ru1 C12 C13 C14 -171.18(12) . . . . ? C12 C13 C14 C15 60.2(2) . . . . ? C13 C14 C15 C16 -57.9(2) . . . . ? C14 C15 C16 C11 52.3(2) . . . . ? N2 C11 C16 C15 72.4(2) . . . . ? C12 C11 C16 C15 -48.6(2) . . . . ? C25 P1 C17 C18 84.53(13) . . . . ? C19 P1 C17 C18 -168.22(12) . . . . ? Ru1 P1 C17 C18 -42.34(13) . . . . ? P1 C17 C18 P2 50.02(14) . . . . ? C37 P2 C18 C17 89.02(13) . . . . ? C31 P2 C18 C17 -166.47(12) . . . . ? Ru1 P2 C18 C17 -36.68(13) . . . . ? C25 P1 C19 C24 11.7(2) . . . . ? C17 P1 C19 C24 -96.60(19) . . . . ? Ru1 P1 C19 C24 144.49(16) . . . . ? C25 P1 C19 C20 -170.11(15) . . . . ? C17 P1 C19 C20 81.56(16) . . . . ? Ru1 P1 C19 C20 -37.34(17) . . . . ? C24 C19 C20 C21 -0.4(3) . . . . ? P1 C19 C20 C21 -178.71(16) . . . . ? C19 C20 C21 C22 -1.0(3) . . . . ? C20 C21 C22 C23 1.7(3) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? C20 C19 C24 C23 1.1(3) . . . . ? P1 C19 C24 C23 179.28(19) . . . . ? C22 C23 C24 C19 -0.4(4) . . . . ? C17 P1 C25 C26 -0.5(2) . . . . ? C19 P1 C25 C26 -105.98(19) . . . . ? Ru1 P1 C25 C26 120.66(17) . . . . ? C17 P1 C25 C30 -175.71(15) . . . . ? C19 P1 C25 C30 78.76(16) . . . . ? Ru1 P1 C25 C30 -54.59(17) . . . . ? C30 C25 C26 C27 2.3(3) . . . . ? P1 C25 C26 C27 -172.94(19) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C30 2.0(3) . . . . ? C26 C25 C30 C29 -1.3(3) . . . . ? P1 C25 C30 C29 174.19(16) . . . . ? C28 C29 C30 C25 -0.8(3) . . . . ? C37 P2 C31 C36 -12.88(17) . . . . ? C18 P2 C31 C36 -117.49(16) . . . . ? Ru1 P2 C31 C36 124.30(14) . . . . ? C37 P2 C31 C32 168.40(14) . . . . ? C18 P2 C31 C32 63.79(15) . . . . ? Ru1 P2 C31 C32 -54.42(16) . . . . ? C36 C31 C32 C33 1.5(3) . . . . ? P2 C31 C32 C33 -179.69(15) . . . . ? C31 C32 C33 C34 -2.2(3) . . . . ? C32 C33 C34 C35 1.2(3) . . . . ? C33 C34 C35 C36 0.4(3) . . . . ? C32 C31 C36 C35 0.1(3) . . . . ? P2 C31 C36 C35 -178.66(14) . . . . ? C34 C35 C36 C31 -1.0(3) . . . . ? C31 P2 C37 C38 115.23(15) . . . . ? C18 P2 C37 C38 -143.16(15) . . . . ? Ru1 P2 C37 C38 -24.80(17) . . . . ? C31 P2 C37 C42 -65.78(17) . . . . ? C18 P2 C37 C42 35.84(17) . . . . ? Ru1 P2 C37 C42 154.19(14) . . . . ? C42 C37 C38 C39 -0.4(3) . . . . ? P2 C37 C38 C39 178.60(14) . . . . ? C37 C38 C39 C40 -1.6(3) . . . . ? C38 C39 C40 C41 1.9(3) . . . . ? C39 C40 C41 C42 -0.3(3) . . . . ? C40 C41 C42 C37 -1.8(3) . . . . ? C38 C37 C42 C41 2.1(3) . . . . ? P2 C37 C42 C41 -176.90(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.612 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.084 #===end data_k08mkw26 _database_code_depnum_ccdc_archive 'CCDC 810319' #TrackingRef '- bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H43 Cl N2 O P2 Ru' _chemical_formula_weight 742.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.6170(1) _cell_length_b 29.6300(3) _cell_length_c 11.8350(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.223(1) _cell_angle_gamma 90.00 _cell_volume 3446.52(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41839 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description colorless _exptl_crystal_colour block _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 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.84 _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 44189 _diffrn_reflns_av_R_equivalents 0.0858 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7870 _reflns_number_gt 5198 _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. H5, H6a and H6b located and refined at a distance of 0.9\%A from the parent carbons. ; _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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7870 _refine_ls_number_parameters 423 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.71687(3) 0.114296(8) 0.56135(2) 0.02162(10) Uani 1 1 d . . . Cl1 Cl 0.91631(9) 0.08591(3) 0.73964(8) 0.0399(2) Uani 1 1 d . . . P1 P 0.55522(8) 0.14868(3) 0.40056(8) 0.0217(2) Uani 1 1 d . . . P2 P 0.61547(9) 0.15192(3) 0.67920(8) 0.0238(2) Uani 1 1 d . . . O1 O 0.5693(3) 0.03137(8) 0.5996(2) 0.0495(7) Uani 1 1 d . . . N1 N 0.8998(3) 0.11961(8) 0.4260(3) 0.0272(7) Uani 1 1 d . . . N2 N 0.8092(3) 0.05389(9) 0.3804(2) 0.0270(6) Uani 1 1 d . . . C1 C 0.6224(4) 0.06191(11) 0.5785(3) 0.0301(8) Uani 1 1 d . . . C2 C 0.8135(3) 0.09088(10) 0.4489(3) 0.0224(7) Uani 1 1 d . . . C3 C 0.9484(3) 0.10149(12) 0.3418(3) 0.0308(8) Uani 1 1 d . . . C4 C 0.8944(3) 0.06012(11) 0.3134(3) 0.0297(8) Uani 1 1 d . . . C5 C 0.9345(4) 0.16360(11) 0.4880(4) 0.0322(9) Uani 1 1 d D . . C6 C 0.8451(4) 0.17186(11) 0.5619(3) 0.0272(8) Uani 1 1 d D . . C7 C 1.0852(4) 0.16417(14) 0.5664(4) 0.0523(12) Uani 1 1 d . . . H7A H 1.1048 0.1414 0.6308 0.078 Uiso 1 1 calc R . . H7B H 1.1107 0.1941 0.6034 0.078 Uiso 1 1 calc R . . H7C H 1.1374 0.1574 0.5156 0.078 Uiso 1 1 calc R . . C8 C 1.0371(4) 0.12705(13) 0.2905(4) 0.0459(10) Uani 1 1 d . . . H8A H 1.1329 0.1224 0.3427 0.069 Uiso 1 1 calc R . . H8B H 1.0156 0.1593 0.2873 0.069 Uiso 1 1 calc R . . H8C H 1.0206 0.1161 0.2079 0.069 Uiso 1 1 calc R . . C9 C 0.9224(4) 0.02592(12) 0.2338(3) 0.0401(9) Uani 1 1 d . . . H9A H 0.8380 0.0190 0.1647 0.060 Uiso 1 1 calc R . . H9B H 0.9579 -0.0016 0.2809 0.060 Uiso 1 1 calc R . . H9C H 0.9897 0.0379 0.2035 0.060 Uiso 1 1 calc R . . C10 C 0.7274(3) 0.01348(11) 0.3785(3) 0.0304(8) Uani 1 1 d . . . H10 H 0.6698 0.0215 0.4257 0.037 Uiso 1 1 calc R . . C11 C 0.6303(4) 0.00200(15) 0.2514(4) 0.0543(12) Uani 1 1 d . . . H11A H 0.5789 0.0290 0.2126 0.082 Uiso 1 1 calc R . . H11B H 0.5673 -0.0215 0.2554 0.082 Uiso 1 1 calc R . . H11C H 0.6818 -0.0090 0.2034 0.082 Uiso 1 1 calc R . . C12 C 0.8133(5) -0.02594(14) 0.4434(5) 0.0736(16) Uani 1 1 d . . . H12A H 0.8674 -0.0364 0.3974 0.110 Uiso 1 1 calc R . . H12B H 0.7543 -0.0504 0.4498 0.110 Uiso 1 1 calc R . . H12C H 0.8742 -0.0167 0.5254 0.110 Uiso 1 1 calc R . . C13 C 0.4750(4) 0.19280(11) 0.4608(3) 0.0310(8) Uani 1 1 d . . . H13A H 0.5347 0.2197 0.4845 0.037 Uiso 1 1 calc R . . H13B H 0.3871 0.2019 0.3971 0.037 Uiso 1 1 calc R . . C14 C 0.4517(3) 0.17446(12) 0.5713(3) 0.0307(8) Uani 1 1 d . . . H14A H 0.3823 0.1502 0.5461 0.037 Uiso 1 1 calc R . . H14B H 0.4189 0.1988 0.6106 0.037 Uiso 1 1 calc R . . C15 C 0.6124(3) 0.18019(11) 0.2942(3) 0.0252(7) Uani 1 1 d . . . C16 C 0.6524(3) 0.15519(12) 0.2143(3) 0.0289(8) Uani 1 1 d . . . H16 H 0.6443 0.1232 0.2125 0.035 Uiso 1 1 calc R . . C17 C 0.7041(4) 0.17661(14) 0.1372(3) 0.0386(9) Uani 1 1 d . . . H17 H 0.7308 0.1594 0.0824 0.046 Uiso 1 1 calc R . . C18 C 0.7167(4) 0.22293(15) 0.1398(4) 0.0446(10) Uani 1 1 d . . . H18 H 0.7548 0.2376 0.0886 0.054 Uiso 1 1 calc R . . C19 C 0.6741(4) 0.24786(13) 0.2166(4) 0.0430(10) Uani 1 1 d . . . H19 H 0.6794 0.2799 0.2160 0.052 Uiso 1 1 calc R . . C20 C 0.6236(4) 0.22669(11) 0.2948(3) 0.0330(8) Uani 1 1 d . . . H20 H 0.5965 0.2442 0.3490 0.040 Uiso 1 1 calc R . . C21 C 0.4091(3) 0.11891(10) 0.2859(3) 0.0243(7) Uani 1 1 d . . . C22 C 0.3278(3) 0.14164(12) 0.1799(3) 0.0306(8) Uani 1 1 d . . . H22 H 0.3459 0.1725 0.1696 0.037 Uiso 1 1 calc R . . C23 C 0.2222(4) 0.12011(14) 0.0903(3) 0.0393(10) Uani 1 1 d . . . H23 H 0.1665 0.1363 0.0198 0.047 Uiso 1 1 calc R . . C24 C 0.1969(4) 0.07507(14) 0.1025(4) 0.0429(10) Uani 1 1 d . . . H24 H 0.1258 0.0599 0.0394 0.051 Uiso 1 1 calc R . . C25 C 0.2753(4) 0.05220(13) 0.2065(4) 0.0438(10) Uani 1 1 d . . . H25 H 0.2572 0.0213 0.2157 0.053 Uiso 1 1 calc R . . C26 C 0.3811(4) 0.07414(12) 0.2987(3) 0.0360(9) Uani 1 1 d . . . H26 H 0.4343 0.0582 0.3705 0.043 Uiso 1 1 calc R . . C27 C 0.5626(4) 0.12192(11) 0.7889(3) 0.0300(8) Uani 1 1 d . . . C28 C 0.4402(4) 0.13046(13) 0.8012(4) 0.0424(10) Uani 1 1 d . . . H28 H 0.3794 0.1520 0.7493 0.051 Uiso 1 1 calc R . . C29 C 0.4044(5) 0.10812(13) 0.8882(4) 0.0497(11) Uani 1 1 d . . . H29 H 0.3191 0.1141 0.8938 0.060 Uiso 1 1 calc R . . C30 C 0.4897(5) 0.07826(14) 0.9640(4) 0.0517(11) Uani 1 1 d . . . H30 H 0.4654 0.0635 1.0241 0.062 Uiso 1 1 calc R . . C31 C 0.6134(5) 0.06882(15) 0.9551(4) 0.0537(12) Uani 1 1 d . . . H31 H 0.6737 0.0477 1.0092 0.064 Uiso 1 1 calc R . . C32 C 0.6499(4) 0.09042(13) 0.8663(3) 0.0433(10) Uani 1 1 d . . . H32 H 0.7340 0.0835 0.8592 0.052 Uiso 1 1 calc R . . C33 C 0.7060(3) 0.19968(10) 0.7732(3) 0.0253(7) Uani 1 1 d . . . C34 C 0.8417(4) 0.19264(12) 0.8489(3) 0.0324(8) Uani 1 1 d . . . H34 H 0.8825 0.1641 0.8488 0.039 Uiso 1 1 calc R . . C35 C 0.9173(4) 0.22645(12) 0.9239(3) 0.0394(9) Uani 1 1 d . . . H35 H 1.0092 0.2211 0.9758 0.047 Uiso 1 1 calc R . . C36 C 0.8583(4) 0.26863(12) 0.9233(3) 0.0379(9) Uani 1 1 d . . . H36 H 0.9103 0.2922 0.9739 0.045 Uiso 1 1 calc R . . C37 C 0.7256(4) 0.27567(12) 0.8497(3) 0.0392(9) Uani 1 1 d . . . H37 H 0.6855 0.3044 0.8492 0.047 Uiso 1 1 calc R . . C38 C 0.6487(4) 0.24161(11) 0.7758(3) 0.0335(9) Uani 1 1 d . . . H38 H 0.5558 0.2469 0.7264 0.040 Uiso 1 1 calc R . . H6A H 0.898(3) 0.1747(11) 0.6415(8) 0.032(10) Uiso 1 1 d D . . H6B H 0.808(3) 0.1995(4) 0.554(3) 0.020(8) Uiso 1 1 d D . . H5 H 0.917(3) 0.1836(9) 0.427(2) 0.039(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 0.02233(16) 0.01939(14) 0.02333(17) -0.00055(11) 0.00885(12) 0.00200(11) Cl1 0.0401(5) 0.0393(5) 0.0332(5) 0.0003(4) 0.0055(4) 0.0165(4) P1 0.0239(5) 0.0196(4) 0.0232(5) 0.0009(4) 0.0108(4) 0.0020(3) P2 0.0245(5) 0.0256(4) 0.0213(5) -0.0006(4) 0.0088(4) 0.0019(4) O1 0.080(2) 0.0281(14) 0.0534(18) -0.0016(13) 0.0400(17) -0.0150(14) N1 0.0253(16) 0.0268(15) 0.0335(17) -0.0053(13) 0.0154(14) -0.0020(12) N2 0.0276(16) 0.0224(14) 0.0318(17) -0.0054(13) 0.0121(14) 0.0007(12) C1 0.039(2) 0.0270(18) 0.027(2) 0.0007(16) 0.0148(17) 0.0007(16) C2 0.0223(18) 0.0199(16) 0.0267(19) -0.0007(14) 0.0113(15) -0.0021(13) C3 0.0259(19) 0.0322(19) 0.041(2) -0.0037(17) 0.0200(18) 0.0018(15) C4 0.0274(19) 0.0336(19) 0.032(2) -0.0053(16) 0.0151(17) 0.0017(15) C5 0.030(2) 0.0254(18) 0.047(2) -0.0087(18) 0.0212(19) -0.0024(16) C6 0.026(2) 0.0245(18) 0.031(2) -0.0053(16) 0.0114(17) -0.0018(15) C7 0.026(2) 0.060(3) 0.073(3) -0.033(2) 0.020(2) -0.0078(19) C8 0.040(2) 0.046(2) 0.066(3) -0.006(2) 0.036(2) -0.0042(19) C9 0.044(2) 0.036(2) 0.047(2) -0.0128(19) 0.025(2) 0.0020(18) C10 0.033(2) 0.0245(18) 0.036(2) -0.0031(16) 0.0153(17) -0.0019(15) C11 0.057(3) 0.063(3) 0.045(3) -0.016(2) 0.021(2) -0.030(2) C12 0.055(3) 0.039(3) 0.115(5) 0.028(3) 0.018(3) -0.001(2) C13 0.037(2) 0.0317(19) 0.0252(19) 0.0015(15) 0.0121(16) 0.0101(16) C14 0.0275(19) 0.0355(19) 0.030(2) -0.0012(16) 0.0117(16) 0.0040(16) C15 0.0265(18) 0.0261(17) 0.0211(18) 0.0013(14) 0.0070(15) -0.0038(14) C16 0.032(2) 0.0329(18) 0.0229(19) -0.0013(16) 0.0121(16) -0.0036(15) C17 0.037(2) 0.054(2) 0.029(2) 0.0046(19) 0.0167(18) -0.0030(18) C18 0.034(2) 0.063(3) 0.037(2) 0.022(2) 0.0137(19) -0.008(2) C19 0.047(2) 0.036(2) 0.039(2) 0.0157(19) 0.008(2) -0.0121(19) C20 0.042(2) 0.0270(18) 0.026(2) 0.0022(15) 0.0085(17) -0.0060(16) C21 0.0212(17) 0.0297(18) 0.0252(19) 0.0004(15) 0.0122(15) 0.0032(14) C22 0.0256(19) 0.040(2) 0.029(2) 0.0014(17) 0.0137(17) -0.0006(16) C23 0.031(2) 0.061(3) 0.029(2) 0.0032(19) 0.0151(18) 0.0056(19) C24 0.023(2) 0.062(3) 0.041(2) -0.020(2) 0.0094(18) -0.0016(19) C25 0.033(2) 0.032(2) 0.061(3) -0.010(2) 0.012(2) -0.0031(18) C26 0.029(2) 0.032(2) 0.040(2) -0.0018(17) 0.0055(18) 0.0012(16) C27 0.038(2) 0.0290(18) 0.0203(19) -0.0060(15) 0.0085(16) -0.0053(16) C28 0.059(3) 0.0307(19) 0.052(3) -0.0018(19) 0.037(2) 0.0005(19) C29 0.069(3) 0.044(2) 0.057(3) -0.004(2) 0.046(3) -0.009(2) C30 0.071(3) 0.056(3) 0.037(2) -0.011(2) 0.031(2) -0.023(2) C31 0.054(3) 0.062(3) 0.036(2) 0.015(2) 0.006(2) -0.010(2) C32 0.039(2) 0.052(2) 0.035(2) 0.008(2) 0.0102(19) -0.002(2) C33 0.032(2) 0.0262(17) 0.0219(18) -0.0007(14) 0.0153(16) 0.0005(15) C34 0.034(2) 0.0322(19) 0.032(2) -0.0072(16) 0.0134(18) 0.0018(16) C35 0.036(2) 0.046(2) 0.037(2) -0.0081(19) 0.0151(18) -0.0079(19) C36 0.054(3) 0.033(2) 0.033(2) -0.0103(17) 0.024(2) -0.0176(18) C37 0.053(3) 0.0236(18) 0.041(2) -0.0021(17) 0.017(2) 0.0009(18) C38 0.040(2) 0.0273(18) 0.033(2) -0.0001(16) 0.0133(18) 0.0010(16) _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 1.900(4) . ? Ru1 C2 2.083(3) . ? Ru1 C6 2.181(3) . ? Ru1 P1 2.2659(9) . ? Ru1 P2 2.3416(9) . ? Ru1 Cl1 2.5028(9) . ? P1 C13 1.845(3) . ? P1 C15 1.845(3) . ? P1 C21 1.853(3) . ? P2 C27 1.828(4) . ? P2 C33 1.832(3) . ? P2 C14 1.850(3) . ? O1 C1 1.143(4) . ? N1 C2 1.351(4) . ? N1 C3 1.392(4) . ? N1 C5 1.473(4) . ? N2 C2 1.354(4) . ? N2 C4 1.422(4) . ? N2 C10 1.475(4) . ? C3 C4 1.341(5) . ? C3 C8 1.505(5) . ? C4 C9 1.488(4) . ? C5 C7 1.516(5) . ? C5 C6 1.534(5) . ? C5 H5 0.90(2) . ? C6 H6A 0.900(13) . ? C6 H6B 0.898(18) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.502(5) . ? C10 C11 1.506(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.520(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.383(4) . ? C15 C16 1.388(4) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.378(5) . ? C17 H17 0.9500 . ? C18 C19 1.374(5) . ? C18 H18 0.9500 . ? C19 C20 1.383(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.380(4) . ? C21 C22 1.398(4) . ? C22 C23 1.374(5) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.376(5) . ? C24 H24 0.9500 . ? C25 C26 1.396(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.385(5) . ? C27 C32 1.388(5) . ? C28 C29 1.392(5) . ? C28 H28 0.9500 . ? C29 C30 1.339(6) . ? C29 H29 0.9500 . ? C30 C31 1.385(6) . ? C30 H30 0.9500 . ? C31 C32 1.405(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.389(4) . ? C33 C34 1.394(5) . ? C34 C35 1.377(5) . ? C34 H34 0.9500 . ? C35 C36 1.396(5) . ? C35 H35 0.9500 . ? C36 C37 1.364(5) . ? C36 H36 0.9500 . ? C37 C38 1.382(5) . ? C37 H37 0.9500 . ? C38 H38 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 101.73(13) . . ? C1 Ru1 C6 173.08(14) . . ? C2 Ru1 C6 78.73(12) . . ? C1 Ru1 P1 101.20(11) . . ? C2 Ru1 P1 90.73(9) . . ? C6 Ru1 P1 85.68(10) . . ? C1 Ru1 P2 86.87(10) . . ? C2 Ru1 P2 171.03(9) . . ? C6 Ru1 P2 93.04(9) . . ? P1 Ru1 P2 85.03(3) . . ? C1 Ru1 Cl1 87.01(11) . . ? C2 Ru1 Cl1 87.86(9) . . ? C6 Ru1 Cl1 86.11(10) . . ? P1 Ru1 Cl1 171.78(3) . . ? P2 Ru1 Cl1 95.21(3) . . ? C13 P1 C15 102.98(15) . . ? C13 P1 C21 103.84(15) . . ? C15 P1 C21 98.15(14) . . ? C13 P1 Ru1 107.92(11) . . ? C15 P1 Ru1 117.41(11) . . ? C21 P1 Ru1 124.01(11) . . ? C27 P2 C33 100.15(14) . . ? C27 P2 C14 101.83(16) . . ? C33 P2 C14 106.31(15) . . ? C27 P2 Ru1 121.68(11) . . ? C33 P2 Ru1 118.39(11) . . ? C14 P2 Ru1 106.54(11) . . ? C2 N1 C3 111.3(3) . . ? C2 N1 C5 121.3(3) . . ? C3 N1 C5 127.4(3) . . ? C2 N2 C4 110.1(3) . . ? C2 N2 C10 123.5(3) . . ? C4 N2 C10 126.3(3) . . ? O1 C1 Ru1 173.8(3) . . ? N1 C2 N2 105.2(3) . . ? N1 C2 Ru1 117.0(2) . . ? N2 C2 Ru1 137.7(2) . . ? C4 C3 N1 107.0(3) . . ? C4 C3 C8 129.2(3) . . ? N1 C3 C8 123.6(3) . . ? C3 C4 N2 106.3(3) . . ? C3 C4 C9 127.8(3) . . ? N2 C4 C9 125.9(3) . . ? N1 C5 C7 108.8(3) . . ? N1 C5 C6 109.4(3) . . ? C7 C5 C6 112.7(3) . . ? N1 C5 H5 104(2) . . ? C7 C5 H5 110(2) . . ? C6 C5 H5 112(2) . . ? C5 C6 Ru1 113.2(2) . . ? C5 C6 H6A 110(2) . . ? Ru1 C6 H6A 103(2) . . ? C5 C6 H6B 115(2) . . ? Ru1 C6 H6B 117.6(19) . . ? H6A C6 H6B 96(3) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C12 112.5(3) . . ? N2 C10 C11 112.0(3) . . ? C12 C10 C11 112.9(3) . . ? N2 C10 H10 106.3 . . ? C12 C10 H10 106.3 . . ? C11 C10 H10 106.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 109.2(2) . . ? C14 C13 H13A 109.8 . . ? P1 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? P1 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C13 C14 P2 107.9(2) . . ? C13 C14 H14A 110.1 . . ? P2 C14 H14A 110.1 . . ? C13 C14 H14B 110.1 . . ? P2 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C20 C15 C16 119.2(3) . . ? C20 C15 P1 123.4(3) . . ? C16 C15 P1 117.3(2) . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 120.2(4) . . ? C15 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C26 C21 C22 118.5(3) . . ? C26 C21 P1 122.2(3) . . ? C22 C21 P1 119.3(2) . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.2(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 120.3(3) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P2 122.6(3) . . ? C32 C27 P2 119.2(3) . . ? C27 C28 C29 121.4(4) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 120.2(4) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C32 120.2(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C32 C31 119.8(4) . . ? C27 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C38 C33 C34 118.3(3) . . ? C38 C33 P2 124.8(3) . . ? C34 C33 P2 116.9(2) . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 119.5(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.9(3) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 120.5(3) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 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 C13 98.52(16) . . . . ? C2 Ru1 P1 C13 -159.36(15) . . . . ? C6 Ru1 P1 C13 -80.72(15) . . . . ? P2 Ru1 P1 C13 12.72(12) . . . . ? Cl1 Ru1 P1 C13 -79.3(2) . . . . ? C1 Ru1 P1 C15 -145.77(16) . . . . ? C2 Ru1 P1 C15 -43.66(14) . . . . ? C6 Ru1 P1 C15 34.98(15) . . . . ? P2 Ru1 P1 C15 128.42(12) . . . . ? Cl1 Ru1 P1 C15 36.4(3) . . . . ? C1 Ru1 P1 C21 -22.91(16) . . . . ? C2 Ru1 P1 C21 79.20(15) . . . . ? C6 Ru1 P1 C21 157.84(15) . . . . ? P2 Ru1 P1 C21 -108.72(13) . . . . ? Cl1 Ru1 P1 C21 159.3(2) . . . . ? C1 Ru1 P2 C27 26.49(17) . . . . ? C2 Ru1 P2 C27 -169.9(6) . . . . ? C6 Ru1 P2 C27 -146.59(17) . . . . ? P1 Ru1 P2 C27 128.02(14) . . . . ? Cl1 Ru1 P2 C27 -60.23(14) . . . . ? C1 Ru1 P2 C33 151.16(16) . . . . ? C2 Ru1 P2 C33 -45.2(6) . . . . ? C6 Ru1 P2 C33 -21.92(16) . . . . ? P1 Ru1 P2 C33 -107.30(12) . . . . ? Cl1 Ru1 P2 C33 64.45(13) . . . . ? C1 Ru1 P2 C14 -89.27(16) . . . . ? C2 Ru1 P2 C14 74.3(6) . . . . ? C6 Ru1 P2 C14 97.65(15) . . . . ? P1 Ru1 P2 C14 12.27(12) . . . . ? Cl1 Ru1 P2 C14 -175.98(12) . . . . ? C2 Ru1 C1 O1 137(3) . . . . ? C6 Ru1 C1 O1 44(4) . . . . ? P1 Ru1 C1 O1 -130(3) . . . . ? P2 Ru1 C1 O1 -45(3) . . . . ? Cl1 Ru1 C1 O1 50(3) . . . . ? C3 N1 C2 N2 1.1(4) . . . . ? C5 N1 C2 N2 -177.9(3) . . . . ? C3 N1 C2 Ru1 -174.8(2) . . . . ? C5 N1 C2 Ru1 6.2(4) . . . . ? C4 N2 C2 N1 -0.3(3) . . . . ? C10 N2 C2 N1 179.4(3) . . . . ? C4 N2 C2 Ru1 174.3(3) . . . . ? C10 N2 C2 Ru1 -6.0(5) . . . . ? C1 Ru1 C2 N1 -175.0(2) . . . . ? C6 Ru1 C2 N1 -2.0(2) . . . . ? P1 Ru1 C2 N1 83.4(2) . . . . ? P2 Ru1 C2 N1 21.8(7) . . . . ? Cl1 Ru1 C2 N1 -88.5(2) . . . . ? C1 Ru1 C2 N2 10.9(4) . . . . ? C6 Ru1 C2 N2 -176.2(4) . . . . ? P1 Ru1 C2 N2 -90.7(3) . . . . ? P2 Ru1 C2 N2 -152.4(4) . . . . ? Cl1 Ru1 C2 N2 97.4(3) . . . . ? C2 N1 C3 C4 -1.5(4) . . . . ? C5 N1 C3 C4 177.4(3) . . . . ? C2 N1 C3 C8 174.8(3) . . . . ? C5 N1 C3 C8 -6.3(6) . . . . ? N1 C3 C4 N2 1.3(4) . . . . ? C8 C3 C4 N2 -174.8(4) . . . . ? N1 C3 C4 C9 -175.5(3) . . . . ? C8 C3 C4 C9 8.5(6) . . . . ? C2 N2 C4 C3 -0.7(4) . . . . ? C10 N2 C4 C3 179.7(3) . . . . ? C2 N2 C4 C9 176.2(3) . . . . ? C10 N2 C4 C9 -3.4(5) . . . . ? C2 N1 C5 C7 116.1(4) . . . . ? C3 N1 C5 C7 -62.7(5) . . . . ? C2 N1 C5 C6 -7.5(4) . . . . ? C3 N1 C5 C6 173.7(3) . . . . ? N1 C5 C6 Ru1 5.2(4) . . . . ? C7 C5 C6 Ru1 -116.0(3) . . . . ? C1 Ru1 C6 C5 92.5(11) . . . . ? C2 Ru1 C6 C5 -2.0(3) . . . . ? P1 Ru1 C6 C5 -93.6(3) . . . . ? P2 Ru1 C6 C5 -178.4(2) . . . . ? Cl1 Ru1 C6 C5 86.6(3) . . . . ? C2 N2 C10 C12 -107.8(4) . . . . ? C4 N2 C10 C12 71.8(5) . . . . ? C2 N2 C10 C11 123.8(4) . . . . ? C4 N2 C10 C11 -56.6(4) . . . . ? C15 P1 C13 C14 -167.0(2) . . . . ? C21 P1 C13 C14 91.1(3) . . . . ? Ru1 P1 C13 C14 -42.2(3) . . . . ? P1 C13 C14 P2 53.0(3) . . . . ? C27 P2 C14 C13 -169.3(2) . . . . ? C33 P2 C14 C13 86.3(2) . . . . ? Ru1 P2 C14 C13 -40.8(2) . . . . ? C13 P1 C15 C20 16.4(3) . . . . ? C21 P1 C15 C20 122.7(3) . . . . ? Ru1 P1 C15 C20 -102.0(3) . . . . ? C13 P1 C15 C16 -167.0(3) . . . . ? C21 P1 C15 C16 -60.7(3) . . . . ? Ru1 P1 C15 C16 74.6(3) . . . . ? C20 C15 C16 C17 0.7(5) . . . . ? P1 C15 C16 C17 -176.1(3) . . . . ? C15 C16 C17 C18 0.3(5) . . . . ? C16 C17 C18 C19 -1.9(6) . . . . ? C17 C18 C19 C20 2.6(6) . . . . ? C16 C15 C20 C19 0.0(5) . . . . ? P1 C15 C20 C19 176.5(3) . . . . ? C18 C19 C20 C15 -1.6(5) . . . . ? C13 P1 C21 C26 -116.1(3) . . . . ? C15 P1 C21 C26 138.3(3) . . . . ? Ru1 P1 C21 C26 7.2(3) . . . . ? C13 P1 C21 C22 67.1(3) . . . . ? C15 P1 C21 C22 -38.5(3) . . . . ? Ru1 P1 C21 C22 -169.7(2) . . . . ? C26 C21 C22 C23 0.2(5) . . . . ? P1 C21 C22 C23 177.1(3) . . . . ? C21 C22 C23 C24 -1.7(5) . . . . ? C22 C23 C24 C25 2.0(5) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C22 C21 C26 C25 0.9(5) . . . . ? P1 C21 C26 C25 -175.9(3) . . . . ? C24 C25 C26 C21 -0.5(6) . . . . ? C33 P2 C27 C28 89.9(3) . . . . ? C14 P2 C27 C28 -19.4(3) . . . . ? Ru1 P2 C27 C28 -137.5(3) . . . . ? C33 P2 C27 C32 -87.8(3) . . . . ? C14 P2 C27 C32 163.0(3) . . . . ? Ru1 P2 C27 C32 44.9(3) . . . . ? C32 C27 C28 C29 -0.3(6) . . . . ? P2 C27 C28 C29 -177.9(3) . . . . ? C27 C28 C29 C30 1.3(6) . . . . ? C28 C29 C30 C31 -1.1(6) . . . . ? C29 C30 C31 C32 -0.2(6) . . . . ? C28 C27 C32 C31 -0.9(5) . . . . ? P2 C27 C32 C31 176.8(3) . . . . ? C30 C31 C32 C27 1.2(6) . . . . ? C27 P2 C33 C38 -94.5(3) . . . . ? C14 P2 C33 C38 11.1(3) . . . . ? Ru1 P2 C33 C38 130.8(3) . . . . ? C27 P2 C33 C34 84.1(3) . . . . ? C14 P2 C33 C34 -170.2(3) . . . . ? Ru1 P2 C33 C34 -50.5(3) . . . . ? C38 C33 C34 C35 -0.5(5) . . . . ? P2 C33 C34 C35 -179.2(3) . . . . ? C33 C34 C35 C36 -0.8(5) . . . . ? C34 C35 C36 C37 0.9(5) . . . . ? C35 C36 C37 C38 0.1(6) . . . . ? C36 C37 C38 C33 -1.4(6) . . . . ? C34 C33 C38 C37 1.5(5) . . . . ? P2 C33 C38 C37 -179.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.278 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.144 #===end data_h08mkw11 _database_code_depnum_ccdc_archive 'CCDC 810320' #TrackingRef '- bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H43 Cl N2 O P2 Ru' _chemical_formula_weight 742.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7400(2) _cell_length_b 10.6990(2) _cell_length_c 22.8980(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.509(1) _cell_angle_gamma 90.00 _cell_volume 3443.79(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 73187 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.103 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.88 _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 47231 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.08 _reflns_number_total 7542 _reflns_number_gt 5771 _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. Hydrogens attached to C7 and C8 located and refined at a distance of 0.9\%A from the parent atoms. ; _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^)+(0.0412P)^2^+4.3252P] 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 7542 _refine_ls_number_parameters 420 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.243210(17) 0.21810(2) 0.334364(11) 0.02303(8) Uani 1 1 d . . . Cl1 Cl 0.41136(6) 0.28442(8) 0.38179(4) 0.03363(19) Uani 1 1 d . . . P1 P 0.19814(6) 0.39072(7) 0.26769(4) 0.02504(18) Uani 1 1 d . . . P2 P 0.20407(6) 0.35540(8) 0.40622(4) 0.02537(18) Uani 1 1 d . . . O1 O 0.04626(18) 0.1234(2) 0.28453(11) 0.0389(6) Uani 1 1 d . . . N1 N 0.30661(19) -0.0058(2) 0.43506(11) 0.0280(6) Uani 1 1 d . . . N2 N 0.31019(18) -0.0426(2) 0.34350(12) 0.0266(6) Uani 1 1 d . . . C1 C 0.1216(3) 0.1593(3) 0.30328(14) 0.0291(7) Uani 1 1 d . . . C2 C 0.2873(2) 0.0469(3) 0.37862(14) 0.0262(7) Uani 1 1 d . . . C3 C 0.3434(2) -0.1275(3) 0.43481(15) 0.0319(7) Uani 1 1 d . . . C4 C 0.3454(2) -0.1492(3) 0.37677(15) 0.0309(7) Uani 1 1 d . . . C5 C 0.2912(2) -0.0227(3) 0.27725(14) 0.0296(7) Uani 1 1 d . . . H5 H 0.3453 -0.0587 0.2649 0.036 Uiso 1 1 calc R . . C6 C 0.2010(3) -0.0873(3) 0.24118(16) 0.0376(8) Uani 1 1 d . . . H6A H 0.2026 -0.1747 0.2544 0.056 Uiso 1 1 calc R . . H6B H 0.1955 -0.0843 0.1975 0.056 Uiso 1 1 calc R . . H6C H 0.1462 -0.0451 0.2482 0.056 Uiso 1 1 calc R . . C7 C 0.2892(3) 0.1177(3) 0.26675(15) 0.0302(7) Uani 1 1 d D . . C8 C 0.3017(3) 0.0650(3) 0.48894(15) 0.0328(8) Uani 1 1 d D . . C9 C 0.4004(3) 0.0979(4) 0.53086(16) 0.0434(9) Uani 1 1 d . . . H9A H 0.4346 0.0210 0.5475 0.065 Uiso 1 1 calc R . . H9B H 0.3943 0.1504 0.5646 0.065 Uiso 1 1 calc R . . H9C H 0.4356 0.1434 0.5075 0.065 Uiso 1 1 calc R . . C10 C 0.2386(3) 0.0024(4) 0.52268(17) 0.0430(9) Uani 1 1 d . . . H10A H 0.1776 -0.0205 0.4932 0.065 Uiso 1 1 calc R . . H10B H 0.2277 0.0605 0.5529 0.065 Uiso 1 1 calc R . . H10C H 0.2703 -0.0730 0.5435 0.065 Uiso 1 1 calc R . . C11 C 0.3707(3) -0.2144(3) 0.48872(16) 0.0408(9) Uani 1 1 d . . . H11A H 0.3133 -0.2436 0.4976 0.061 Uiso 1 1 calc R . . H11B H 0.4116 -0.1701 0.5245 0.061 Uiso 1 1 calc R . . H11C H 0.4052 -0.2861 0.4793 0.061 Uiso 1 1 calc R . . C12 C 0.3843(3) -0.2572(3) 0.35078(17) 0.0388(8) Uani 1 1 d . . . H12A H 0.4128 -0.3174 0.3834 0.058 Uiso 1 1 calc R . . H12B H 0.4329 -0.2275 0.3328 0.058 Uiso 1 1 calc R . . H12C H 0.3328 -0.2978 0.3190 0.058 Uiso 1 1 calc R . . C13 C 0.2815(2) 0.4761(3) 0.23678(14) 0.0306(7) Uani 1 1 d . . . C14 C 0.3732(3) 0.4331(4) 0.24557(17) 0.0405(9) Uani 1 1 d . . . H14 H 0.3942 0.3587 0.2683 0.049 Uiso 1 1 calc R . . C15 C 0.4350(3) 0.4994(4) 0.22094(19) 0.0508(10) Uani 1 1 d . . . H15 H 0.4976 0.4688 0.2268 0.061 Uiso 1 1 calc R . . C16 C 0.4068(3) 0.6081(4) 0.18840(17) 0.0472(10) Uani 1 1 d . . . H16 H 0.4497 0.6529 0.1725 0.057 Uiso 1 1 calc R . . C17 C 0.3153(3) 0.6508(4) 0.17928(16) 0.0426(9) Uani 1 1 d . . . H17 H 0.2949 0.7257 0.1569 0.051 Uiso 1 1 calc R . . C18 C 0.2528(3) 0.5851(3) 0.20261(15) 0.0341(8) Uani 1 1 d . . . H18 H 0.1895 0.6145 0.1952 0.041 Uiso 1 1 calc R . . C19 C 0.1011(2) 0.3595(3) 0.19705(14) 0.0268(7) Uani 1 1 d . . . C20 C 0.1197(3) 0.3387(3) 0.14193(15) 0.0344(8) Uani 1 1 d . . . H20 H 0.1832 0.3433 0.1402 0.041 Uiso 1 1 calc R . . C21 C 0.0464(3) 0.3113(3) 0.08954(16) 0.0396(9) Uani 1 1 d . . . H21 H 0.0599 0.2980 0.0520 0.048 Uiso 1 1 calc R . . C22 C -0.0464(3) 0.3031(3) 0.09139(17) 0.0409(9) Uani 1 1 d . . . H22 H -0.0962 0.2832 0.0553 0.049 Uiso 1 1 calc R . . C23 C -0.0667(3) 0.3235(3) 0.14516(17) 0.0375(8) Uani 1 1 d . . . H23 H -0.1305 0.3199 0.1463 0.045 Uiso 1 1 calc R . . C24 C 0.0073(2) 0.3498(3) 0.19831(16) 0.0328(7) Uani 1 1 d . . . H24 H -0.0064 0.3613 0.2359 0.039 Uiso 1 1 calc R . . C25 C 0.1498(2) 0.5144(3) 0.30636(14) 0.0300(7) Uani 1 1 d . . . H25A H 0.1560 0.5969 0.2884 0.036 Uiso 1 1 calc R . . H25B H 0.0815 0.4988 0.3008 0.036 Uiso 1 1 calc R . . C26 C 0.2054(2) 0.5134(3) 0.37445(14) 0.0294(7) Uani 1 1 d . . . H26A H 0.1766 0.5735 0.3966 0.035 Uiso 1 1 calc R . . H26B H 0.2719 0.5395 0.3800 0.035 Uiso 1 1 calc R . . C27 C 0.0840(2) 0.3385(3) 0.41301(14) 0.0319(7) Uani 1 1 d . . . C28 C 0.0277(3) 0.4402(4) 0.41890(17) 0.0424(9) Uani 1 1 d . . . H28 H 0.0504 0.5228 0.4175 0.051 Uiso 1 1 calc R . . C29 C -0.0603(3) 0.4217(5) 0.42674(18) 0.0533(11) Uani 1 1 d . . . H29 H -0.0975 0.4919 0.4307 0.064 Uiso 1 1 calc R . . C30 C -0.0951(3) 0.3028(5) 0.42887(17) 0.0541(12) Uani 1 1 d . . . H30 H -0.1560 0.2913 0.4343 0.065 Uiso 1 1 calc R . . C31 C -0.0416(3) 0.2005(5) 0.42307(16) 0.0492(11) Uani 1 1 d . . . H31 H -0.0651 0.1184 0.4248 0.059 Uiso 1 1 calc R . . C32 C 0.0477(2) 0.2186(4) 0.41465(15) 0.0364(8) Uani 1 1 d . . . H32 H 0.0842 0.1481 0.4100 0.044 Uiso 1 1 calc R . . C33 C 0.2726(2) 0.3874(3) 0.48649(14) 0.0280(7) Uani 1 1 d . . . C34 C 0.3626(2) 0.4431(3) 0.50049(15) 0.0331(7) Uani 1 1 d . . . H34 H 0.3896 0.4607 0.4686 0.040 Uiso 1 1 calc R . . C35 C 0.4125(3) 0.4728(3) 0.56033(17) 0.0402(9) Uani 1 1 d . . . H35 H 0.4723 0.5137 0.5689 0.048 Uiso 1 1 calc R . . C36 C 0.3765(3) 0.4438(4) 0.60777(17) 0.0476(10) Uani 1 1 d . . . H36 H 0.4111 0.4642 0.6488 0.057 Uiso 1 1 calc R . . C37 C 0.2902(3) 0.3850(4) 0.59484(16) 0.0484(10) Uani 1 1 d . . . H37 H 0.2658 0.3626 0.6274 0.058 Uiso 1 1 calc R . . C38 C 0.2376(3) 0.3576(4) 0.53474(15) 0.0393(8) Uani 1 1 d . . . H38 H 0.1774 0.3181 0.5267 0.047 Uiso 1 1 calc R . . H7A H 0.2536(18) 0.131(3) 0.2277(5) 0.020(8) Uiso 1 1 d D . . H7B H 0.3476(10) 0.149(3) 0.2714(14) 0.024(9) Uiso 1 1 d D . . H8 H 0.272(2) 0.1363(18) 0.4729(15) 0.041(10) 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 0.02396(14) 0.02308(13) 0.02128(13) -0.00031(10) 0.00562(10) 0.00087(10) Cl1 0.0289(4) 0.0374(4) 0.0326(4) -0.0020(3) 0.0061(3) -0.0019(3) P1 0.0252(4) 0.0253(4) 0.0239(4) 0.0012(3) 0.0064(3) 0.0018(3) P2 0.0266(4) 0.0256(4) 0.0239(4) -0.0013(3) 0.0076(3) 0.0002(3) O1 0.0356(14) 0.0377(14) 0.0388(14) -0.0017(11) 0.0042(11) -0.0042(11) N1 0.0299(15) 0.0271(14) 0.0248(13) 0.0007(11) 0.0047(11) -0.0012(11) N2 0.0258(14) 0.0255(13) 0.0276(13) -0.0007(11) 0.0065(11) 0.0004(11) C1 0.037(2) 0.0270(16) 0.0241(16) 0.0018(13) 0.0111(15) 0.0052(15) C2 0.0261(16) 0.0252(16) 0.0268(16) -0.0009(13) 0.0072(13) -0.0009(13) C3 0.0297(18) 0.0268(17) 0.0343(18) 0.0018(14) 0.0020(14) 0.0011(13) C4 0.0304(18) 0.0234(16) 0.0361(18) -0.0001(14) 0.0057(15) -0.0013(13) C5 0.0336(18) 0.0314(17) 0.0245(16) -0.0022(13) 0.0097(14) 0.0039(14) C6 0.043(2) 0.0340(19) 0.0328(18) -0.0059(15) 0.0073(16) -0.0007(16) C7 0.0332(19) 0.0311(17) 0.0263(16) 0.0010(14) 0.0089(15) 0.0012(15) C8 0.041(2) 0.0326(18) 0.0239(16) -0.0013(14) 0.0083(15) 0.0017(16) C9 0.048(2) 0.043(2) 0.0341(19) -0.0046(16) 0.0052(17) -0.0035(18) C10 0.054(2) 0.043(2) 0.0359(19) 0.0022(16) 0.0199(18) -0.0032(18) C11 0.049(2) 0.0344(19) 0.0352(19) 0.0083(16) 0.0066(17) 0.0017(17) C12 0.043(2) 0.0305(18) 0.041(2) -0.0013(15) 0.0104(17) 0.0049(15) C13 0.0316(18) 0.0332(18) 0.0259(16) -0.0019(14) 0.0068(14) -0.0034(14) C14 0.035(2) 0.046(2) 0.043(2) 0.0087(17) 0.0149(16) -0.0001(16) C15 0.030(2) 0.068(3) 0.057(3) 0.010(2) 0.0168(19) 0.0009(19) C16 0.044(2) 0.061(3) 0.038(2) 0.0051(19) 0.0154(18) -0.017(2) C17 0.054(2) 0.043(2) 0.0316(18) 0.0028(16) 0.0137(17) -0.0084(18) C18 0.0372(19) 0.0337(18) 0.0309(17) 0.0002(14) 0.0094(15) -0.0025(15) C19 0.0291(17) 0.0229(15) 0.0257(15) 0.0012(12) 0.0041(13) 0.0028(13) C20 0.0366(19) 0.0360(18) 0.0315(18) 0.0006(15) 0.0115(15) -0.0004(15) C21 0.047(2) 0.044(2) 0.0268(17) -0.0059(15) 0.0095(16) 0.0002(17) C22 0.040(2) 0.039(2) 0.0354(19) -0.0009(16) -0.0015(16) 0.0003(16) C23 0.0345(19) 0.0315(18) 0.044(2) -0.0028(15) 0.0088(16) 0.0002(15) C24 0.0304(18) 0.0340(18) 0.0335(18) -0.0018(14) 0.0085(15) 0.0037(14) C25 0.0339(18) 0.0266(16) 0.0288(16) 0.0002(13) 0.0084(14) 0.0060(14) C26 0.0361(18) 0.0257(16) 0.0262(16) -0.0016(13) 0.0093(14) 0.0016(14) C27 0.0287(18) 0.044(2) 0.0219(16) -0.0035(14) 0.0064(14) 0.0002(15) C28 0.038(2) 0.048(2) 0.040(2) -0.0100(17) 0.0107(17) 0.0025(17) C29 0.035(2) 0.084(3) 0.040(2) -0.014(2) 0.0097(17) 0.015(2) C30 0.030(2) 0.100(4) 0.032(2) -0.004(2) 0.0088(17) -0.006(2) C31 0.038(2) 0.076(3) 0.0306(19) 0.0039(19) 0.0062(17) -0.018(2) C32 0.0323(18) 0.047(2) 0.0298(17) 0.0005(16) 0.0094(15) -0.0045(17) C33 0.0297(17) 0.0267(16) 0.0267(16) -0.0036(13) 0.0074(14) 0.0029(13) C34 0.0339(19) 0.0314(18) 0.0338(18) -0.0023(14) 0.0098(15) -0.0035(14) C35 0.035(2) 0.0363(19) 0.042(2) -0.0034(16) 0.0013(16) -0.0026(16) C36 0.054(3) 0.052(2) 0.0297(19) -0.0112(17) 0.0016(18) 0.001(2) C37 0.053(2) 0.067(3) 0.0281(18) -0.0054(18) 0.0153(17) 0.001(2) C38 0.037(2) 0.049(2) 0.0308(18) -0.0036(16) 0.0094(16) -0.0028(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.830(4) . ? Ru1 C2 2.100(3) . ? Ru1 C7 2.154(3) . ? Ru1 P1 2.3606(8) . ? Ru1 P2 2.4018(8) . ? Ru1 Cl1 2.4913(8) . ? P1 C13 1.836(3) . ? P1 C19 1.839(3) . ? P1 C25 1.850(3) . ? P2 C27 1.832(3) . ? P2 C26 1.843(3) . ? P2 C33 1.843(3) . ? O1 C1 1.130(4) . ? N1 C2 1.359(4) . ? N1 C3 1.412(4) . ? N1 C8 1.468(4) . ? N2 C2 1.356(4) . ? N2 C4 1.383(4) . ? N2 C5 1.473(4) . ? C3 C4 1.358(5) . ? C3 C11 1.500(5) . ? C4 C12 1.492(5) . ? C5 C6 1.506(5) . ? C5 C7 1.521(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.902(14) . ? C7 H7B 0.90(2) . ? C8 C9 1.523(5) . ? C8 C10 1.530(5) . ? C8 H8 0.90(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.384(5) . ? C13 C18 1.397(5) . ? C14 C15 1.400(5) . ? C14 H14 0.9500 . ? C15 C16 1.375(6) . ? C15 H15 0.9500 . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.388(5) . ? C19 C24 1.394(5) . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.369(5) . ? C22 H22 0.9500 . ? C23 C24 1.397(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.528(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.395(5) . ? C27 C28 1.399(5) . ? C28 C29 1.375(6) . ? C28 H28 0.9500 . ? C29 C30 1.379(7) . ? C29 H29 0.9500 . ? C30 C31 1.379(6) . ? C30 H30 0.9500 . ? C31 C32 1.400(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.389(5) . ? C33 C34 1.401(5) . ? C34 C35 1.383(5) . ? C34 H34 0.9500 . ? C35 C36 1.380(6) . ? C35 H35 0.9500 . ? C36 C37 1.369(6) . ? C36 H36 0.9500 . ? C37 C38 1.392(5) . ? C37 H37 0.9500 . ? C38 H38 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 90.73(13) . . ? C1 Ru1 C7 91.86(14) . . ? C2 Ru1 C7 78.07(12) . . ? C1 Ru1 P1 88.01(10) . . ? C2 Ru1 P1 168.72(9) . . ? C7 Ru1 P1 90.76(9) . . ? C1 Ru1 P2 93.87(10) . . ? C2 Ru1 P2 107.84(9) . . ? C7 Ru1 P2 171.70(10) . . ? P1 Ru1 P2 83.43(3) . . ? C1 Ru1 Cl1 175.75(10) . . ? C2 Ru1 Cl1 85.13(9) . . ? C7 Ru1 Cl1 88.19(10) . . ? P1 Ru1 Cl1 96.23(3) . . ? P2 Ru1 Cl1 86.54(3) . . ? C13 P1 C19 100.67(14) . . ? C13 P1 C25 103.15(15) . . ? C19 P1 C25 103.95(15) . . ? C13 P1 Ru1 123.23(11) . . ? C19 P1 Ru1 114.82(10) . . ? C25 P1 Ru1 108.91(10) . . ? C27 P2 C26 104.45(16) . . ? C27 P2 C33 100.77(14) . . ? C26 P2 C33 98.96(14) . . ? C27 P2 Ru1 115.80(11) . . ? C26 P2 Ru1 104.91(11) . . ? C33 P2 Ru1 128.62(11) . . ? C2 N1 C3 110.4(3) . . ? C2 N1 C8 122.4(3) . . ? C3 N1 C8 126.6(3) . . ? C2 N2 C4 112.0(3) . . ? C2 N2 C5 120.3(3) . . ? C4 N2 C5 127.6(3) . . ? O1 C1 Ru1 179.4(3) . . ? N2 C2 N1 104.7(3) . . ? N2 C2 Ru1 115.2(2) . . ? N1 C2 Ru1 140.0(2) . . ? C4 C3 N1 106.4(3) . . ? C4 C3 C11 128.3(3) . . ? N1 C3 C11 125.2(3) . . ? C3 C4 N2 106.5(3) . . ? C3 C4 C12 130.3(3) . . ? N2 C4 C12 123.0(3) . . ? N2 C5 C6 111.2(3) . . ? N2 C5 C7 107.1(3) . . ? C6 C5 C7 113.3(3) . . ? N2 C5 H5 108.4 . . ? C6 C5 H5 108.4 . . ? C7 C5 H5 108.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 Ru1 112.0(2) . . ? C5 C7 H7A 107(2) . . ? Ru1 C7 H7A 115(2) . . ? C5 C7 H7B 112(2) . . ? Ru1 C7 H7B 103(2) . . ? H7A C7 H7B 108(3) . . ? N1 C8 C9 111.7(3) . . ? N1 C8 C10 112.9(3) . . ? C9 C8 C10 113.1(3) . . ? N1 C8 H8 104(2) . . ? C9 C8 H8 108(2) . . ? C10 C8 H8 106(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.5(3) . . ? C14 C13 P1 121.1(3) . . ? C18 C13 P1 120.4(3) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 121.3(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.9(3) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C20 C19 C24 118.4(3) . . ? C20 C19 P1 120.9(3) . . ? C24 C19 P1 120.6(2) . . ? C21 C20 C19 120.4(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.6(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.4(3) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C19 C24 C23 121.1(3) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 P1 108.5(2) . . ? C26 C25 H25A 110.0 . . ? P1 C25 H25A 110.0 . . ? C26 C25 H25B 110.0 . . ? P1 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? C25 C26 P2 110.1(2) . . ? C25 C26 H26A 109.6 . . ? P2 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? P2 C26 H26B 109.6 . . ? H26A C26 H26B 108.2 . . ? C32 C27 C28 118.0(3) . . ? C32 C27 P2 118.8(3) . . ? C28 C27 P2 123.2(3) . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 119.9(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C27 C32 C31 121.0(4) . . ? C27 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C38 C33 C34 117.9(3) . . ? C38 C33 P2 121.8(3) . . ? C34 C33 P2 120.3(2) . . ? C35 C34 C33 120.6(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 120.8(3) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 119.0(3) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 121.0(4) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C33 C38 C37 120.6(4) . . ? C33 C38 H38 119.7 . . ? C37 C38 H38 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 C13 -151.04(16) . . . . ? C2 Ru1 P1 C13 -67.3(5) . . . . ? C7 Ru1 P1 C13 -59.21(16) . . . . ? P2 Ru1 P1 C13 114.83(13) . . . . ? Cl1 Ru1 P1 C13 29.06(13) . . . . ? C1 Ru1 P1 C19 -27.88(15) . . . . ? C2 Ru1 P1 C19 55.9(5) . . . . ? C7 Ru1 P1 C19 63.95(15) . . . . ? P2 Ru1 P1 C19 -122.01(12) . . . . ? Cl1 Ru1 P1 C19 152.22(12) . . . . ? C1 Ru1 P1 C25 88.17(15) . . . . ? C2 Ru1 P1 C25 171.9(5) . . . . ? C7 Ru1 P1 C25 180.00(15) . . . . ? P2 Ru1 P1 C25 -5.96(12) . . . . ? Cl1 Ru1 P1 C25 -91.73(12) . . . . ? C1 Ru1 P2 C27 8.28(16) . . . . ? C2 Ru1 P2 C27 -83.74(15) . . . . ? C7 Ru1 P2 C27 141.7(6) . . . . ? P1 Ru1 P2 C27 95.82(13) . . . . ? Cl1 Ru1 P2 C27 -167.49(13) . . . . ? C1 Ru1 P2 C26 -106.27(15) . . . . ? C2 Ru1 P2 C26 161.72(14) . . . . ? C7 Ru1 P2 C26 27.2(7) . . . . ? P1 Ru1 P2 C26 -18.72(12) . . . . ? Cl1 Ru1 P2 C26 77.96(12) . . . . ? C1 Ru1 P2 C33 138.96(17) . . . . ? C2 Ru1 P2 C33 46.95(17) . . . . ? C7 Ru1 P2 C33 -87.6(7) . . . . ? P1 Ru1 P2 C33 -133.49(14) . . . . ? Cl1 Ru1 P2 C33 -36.80(14) . . . . ? C2 Ru1 C1 O1 90(38) . . . . ? C7 Ru1 C1 O1 169(100) . . . . ? P1 Ru1 C1 O1 -101(38) . . . . ? P2 Ru1 C1 O1 -17(38) . . . . ? Cl1 Ru1 C1 O1 78(38) . . . . ? C4 N2 C2 N1 -1.3(3) . . . . ? C5 N2 C2 N1 175.0(3) . . . . ? C4 N2 C2 Ru1 175.4(2) . . . . ? C5 N2 C2 Ru1 -8.2(4) . . . . ? C3 N1 C2 N2 1.2(3) . . . . ? C8 N1 C2 N2 173.1(3) . . . . ? C3 N1 C2 Ru1 -174.2(3) . . . . ? C8 N1 C2 Ru1 -2.4(5) . . . . ? C1 Ru1 C2 N2 84.3(2) . . . . ? C7 Ru1 C2 N2 -7.4(2) . . . . ? P1 Ru1 C2 N2 0.9(6) . . . . ? P2 Ru1 C2 N2 178.6(2) . . . . ? Cl1 Ru1 C2 N2 -96.6(2) . . . . ? C1 Ru1 C2 N1 -100.6(4) . . . . ? C7 Ru1 C2 N1 167.7(4) . . . . ? P1 Ru1 C2 N1 176.0(2) . . . . ? P2 Ru1 C2 N1 -6.3(4) . . . . ? Cl1 Ru1 C2 N1 78.5(4) . . . . ? C2 N1 C3 C4 -0.7(4) . . . . ? C8 N1 C3 C4 -172.1(3) . . . . ? C2 N1 C3 C11 -178.7(3) . . . . ? C8 N1 C3 C11 9.9(5) . . . . ? N1 C3 C4 N2 -0.2(4) . . . . ? C11 C3 C4 N2 177.8(3) . . . . ? N1 C3 C4 C12 174.4(3) . . . . ? C11 C3 C4 C12 -7.6(6) . . . . ? C2 N2 C4 C3 1.0(4) . . . . ? C5 N2 C4 C3 -175.0(3) . . . . ? C2 N2 C4 C12 -174.1(3) . . . . ? C5 N2 C4 C12 9.9(5) . . . . ? C2 N2 C5 C6 -99.4(3) . . . . ? C4 N2 C5 C6 76.3(4) . . . . ? C2 N2 C5 C7 24.9(4) . . . . ? C4 N2 C5 C7 -159.4(3) . . . . ? N2 C5 C7 Ru1 -29.0(3) . . . . ? C6 C5 C7 Ru1 93.9(3) . . . . ? C1 Ru1 C7 C5 -69.8(2) . . . . ? C2 Ru1 C7 C5 20.6(2) . . . . ? P1 Ru1 C7 C5 -157.8(2) . . . . ? P2 Ru1 C7 C5 156.6(5) . . . . ? Cl1 Ru1 C7 C5 106.0(2) . . . . ? C2 N1 C8 C9 -104.2(4) . . . . ? C3 N1 C8 C9 66.3(4) . . . . ? C2 N1 C8 C10 127.0(3) . . . . ? C3 N1 C8 C10 -62.5(4) . . . . ? C19 P1 C13 C14 -121.4(3) . . . . ? C25 P1 C13 C14 131.3(3) . . . . ? Ru1 P1 C13 C14 7.9(3) . . . . ? C19 P1 C13 C18 57.2(3) . . . . ? C25 P1 C13 C18 -50.0(3) . . . . ? Ru1 P1 C13 C18 -173.5(2) . . . . ? C18 C13 C14 C15 0.7(5) . . . . ? P1 C13 C14 C15 179.4(3) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C14 C15 C16 C17 -1.0(6) . . . . ? C15 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C13 1.4(5) . . . . ? C14 C13 C18 C17 -1.7(5) . . . . ? P1 C13 C18 C17 179.6(3) . . . . ? C13 P1 C19 C20 33.3(3) . . . . ? C25 P1 C19 C20 139.8(3) . . . . ? Ru1 P1 C19 C20 -101.3(3) . . . . ? C13 P1 C19 C24 -150.1(3) . . . . ? C25 P1 C19 C24 -43.5(3) . . . . ? Ru1 P1 C19 C24 75.4(3) . . . . ? C24 C19 C20 C21 1.1(5) . . . . ? P1 C19 C20 C21 177.9(3) . . . . ? C19 C20 C21 C22 -0.6(5) . . . . ? C20 C21 C22 C23 0.8(6) . . . . ? C21 C22 C23 C24 -1.5(5) . . . . ? C20 C19 C24 C23 -1.9(5) . . . . ? P1 C19 C24 C23 -178.6(3) . . . . ? C22 C23 C24 C19 2.1(5) . . . . ? C13 P1 C25 C26 -96.8(2) . . . . ? C19 P1 C25 C26 158.5(2) . . . . ? Ru1 P1 C25 C26 35.7(2) . . . . ? P1 C25 C26 P2 -53.9(3) . . . . ? C27 P2 C26 C25 -75.1(3) . . . . ? C33 P2 C26 C25 -178.7(2) . . . . ? Ru1 P2 C26 C25 47.2(2) . . . . ? C26 P2 C27 C32 157.5(3) . . . . ? C33 P2 C27 C32 -100.2(3) . . . . ? Ru1 P2 C27 C32 42.7(3) . . . . ? C26 P2 C27 C28 -24.9(3) . . . . ? C33 P2 C27 C28 77.4(3) . . . . ? Ru1 P2 C27 C28 -139.7(3) . . . . ? C32 C27 C28 C29 0.7(5) . . . . ? P2 C27 C28 C29 -176.9(3) . . . . ? C27 C28 C29 C30 -0.1(6) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 C32 -0.4(6) . . . . ? C28 C27 C32 C31 -1.1(5) . . . . ? P2 C27 C32 C31 176.6(3) . . . . ? C30 C31 C32 C27 1.0(5) . . . . ? C27 P2 C33 C38 19.3(3) . . . . ? C26 P2 C33 C38 126.0(3) . . . . ? Ru1 P2 C33 C38 -116.7(3) . . . . ? C27 P2 C33 C34 -160.8(3) . . . . ? C26 P2 C33 C34 -54.1(3) . . . . ? Ru1 P2 C33 C34 63.3(3) . . . . ? C38 C33 C34 C35 -3.1(5) . . . . ? P2 C33 C34 C35 176.9(3) . . . . ? C33 C34 C35 C36 2.6(5) . . . . ? C34 C35 C36 C37 -0.1(6) . . . . ? C35 C36 C37 C38 -1.7(6) . . . . ? C34 C33 C38 C37 1.3(5) . . . . ? P2 C33 C38 C37 -178.8(3) . . . . ? C36 C37 C38 C33 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.863 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.088 #===end data_k08mkw34 _database_code_depnum_ccdc_archive 'CCDC 810321' #TrackingRef '- bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H56 B2 F8 N6 O P2 Ru' _chemical_formula_weight 1045.60 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.9663(2) _cell_length_b 13.1062(2) _cell_length_c 30.1835(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5129.35(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 43667 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details '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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30246 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11321 _reflns_number_gt 8883 _reflns_threshold_expression >2sigma(I) _computing_data_collection kappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material ORTEX _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. The asymmetric unit in k08mkw34 contains one ruthenium based dication, two tetrafluoroborate anions one ordered molecule of acetonitrile, and a diffuse region of solvent which was treated using PLATON SQUEEZE. The latter approximates to one molecule of acetonotrile per asymmetric unit and the data presented herein take account of same. All fluorines in the anion based on B2 were found to be disordered in a 60:40 ratio over 2 positions. B-F distance similarity restraints in addition to ADP restraints for the partial occupancy halides were included to assist convergence. ; _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^)+(0.0460P)^2^+0.6132P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 11321 _refine_ls_number_parameters 613 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.87453(2) 0.06042(2) 0.920914(9) 0.02881(8) Uani 1 1 d . . . P1 P 0.77621(7) 0.14694(8) 0.97585(3) 0.0296(2) Uani 1 1 d . . . P2 P 0.86681(8) 0.21745(7) 0.88399(3) 0.0321(2) Uani 1 1 d . . . F1 F 0.4831(3) -0.0118(3) 0.77915(12) 0.1003(13) Uani 1 1 d . . . F2 F 0.3325(3) 0.0286(4) 0.81164(16) 0.1380(18) Uani 1 1 d . . . F3 F 0.4789(3) 0.0347(3) 0.85110(10) 0.0849(10) Uani 1 1 d . . . F4 F 0.4074(3) -0.1140(3) 0.82744(13) 0.1125(14) Uani 1 1 d . . . F5 F 1.0716(4) -0.1170(5) 1.0553(3) 0.091(2) Uani 0.60 1 d PDU A 3 F6 F 1.1745(8) -0.0092(6) 1.0226(3) 0.113(3) Uani 0.60 1 d PDU A 3 F7 F 1.2377(5) -0.1592(7) 1.0519(6) 0.102(3) Uani 0.60 1 d PDU A 3 F8 F 1.1872(10) -0.0217(7) 1.0925(3) 0.077(2) Uani 0.60 1 d PDU A 3 F5A F 1.0791(7) -0.0727(10) 1.0304(4) 0.093(3) Uani 0.40 1 d PDU A 4 F6A F 1.2386(8) -0.0346(10) 1.0286(4) 0.100(3) Uani 0.40 1 d PDU A 4 F7A F 1.1972(11) -0.1812(10) 1.0481(8) 0.105(4) Uani 0.40 1 d PDU A 4 F8A F 1.1636(16) -0.0569(13) 1.0983(4) 0.097(4) Uani 0.40 1 d PDU A 4 O1 O 1.0659(2) 0.1572(2) 0.95733(9) 0.0431(7) Uani 1 1 d . . . N1 N 1.0421(2) -0.0858(2) 0.87683(10) 0.0346(8) Uani 1 1 d . . . N2 N 0.9267(2) -0.0483(3) 0.82827(10) 0.0396(8) Uani 1 1 d . . . N3 N 0.8784(3) -0.0698(2) 0.96227(9) 0.0339(7) Uani 1 1 d . . . N4 N 0.7370(3) -0.0139(3) 0.90107(10) 0.0374(8) Uani 1 1 d . . . N5 N 1.3031(4) -0.4033(4) 0.88068(18) 0.0811(15) Uani 1 1 d . . . C1 C 0.9945(3) 0.1186(3) 0.94314(12) 0.0335(9) Uani 1 1 d . . . C2 C 0.9555(3) -0.0290(3) 0.87093(11) 0.0351(9) Uani 1 1 d . . . C3 C 1.0679(3) -0.1387(3) 0.83837(13) 0.0385(10) Uani 1 1 d . . . C4 C 0.9954(3) -0.1161(4) 0.80805(13) 0.0414(10) Uani 1 1 d . . . C5 C 1.1027(3) -0.0888(3) 0.91871(13) 0.0372(9) Uani 1 1 d . . . H5 H 1.0632 -0.0483 0.9411 0.045 Uiso 1 1 calc R . . C6 C 1.2076(3) -0.0366(4) 0.91346(14) 0.0499(11) Uani 1 1 d . . . H6A H 1.2514 -0.0773 0.8938 0.075 Uiso 1 1 calc R . . H6B H 1.2408 -0.0305 0.9425 0.075 Uiso 1 1 calc R . . H6C H 1.1979 0.0316 0.9007 0.075 Uiso 1 1 calc R . . C7 C 1.1101(4) -0.1975(3) 0.93666(14) 0.0491(11) Uani 1 1 d . . . H7A H 1.0432 -0.2315 0.9335 0.074 Uiso 1 1 calc R . . H7B H 1.1295 -0.1955 0.9680 0.074 Uiso 1 1 calc R . . H7C H 1.1625 -0.2353 0.9200 0.074 Uiso 1 1 calc R . . C8 C 0.8372(3) 0.0000(4) 0.80606(14) 0.0506(12) Uani 1 1 d . . . H8 H 0.8045 0.0460 0.8285 0.061 Uiso 1 1 calc R . . C9 C 0.8696(5) 0.0675(5) 0.76770(13) 0.0751(17) Uani 1 1 d . . . H9A H 0.9226 0.1155 0.7777 0.113 Uiso 1 1 calc R . . H9B H 0.8097 0.1055 0.7568 0.113 Uiso 1 1 calc R . . H9C H 0.8974 0.0250 0.7438 0.113 Uiso 1 1 calc R . . C10 C 0.7547(4) -0.0795(5) 0.79317(17) 0.0713(17) Uani 1 1 d . . . H10A H 0.7707 -0.1075 0.7638 0.107 Uiso 1 1 calc R . . H10B H 0.6867 -0.0468 0.7924 0.107 Uiso 1 1 calc R . . H10C H 0.7542 -0.1348 0.8150 0.107 Uiso 1 1 calc R . . C11 C 1.1559(3) -0.2105(4) 0.83309(15) 0.0552(13) Uani 1 1 d . . . H11A H 1.1449 -0.2705 0.8519 0.083 Uiso 1 1 calc R . . H11B H 1.2200 -0.1764 0.8419 0.083 Uiso 1 1 calc R . . H11C H 1.1609 -0.2318 0.8020 0.083 Uiso 1 1 calc R . . C12 C 0.9832(4) -0.1577(4) 0.76201(14) 0.0614(14) Uani 1 1 d . . . H12A H 1.0367 -0.2088 0.7564 0.092 Uiso 1 1 calc R . . H12B H 0.9898 -0.1020 0.7405 0.092 Uiso 1 1 calc R . . H12C H 0.9150 -0.1893 0.7590 0.092 Uiso 1 1 calc R . . C13 C 0.8765(3) -0.1365(3) 0.98656(12) 0.0376(8) Uani 1 1 d . . . C14 C 0.8758(4) -0.2206(3) 1.01805(14) 0.0520(11) Uani 1 1 d . . . H14A H 0.9461 -0.2464 1.0219 0.078 Uiso 1 1 calc R . . H14B H 0.8315 -0.2755 1.0068 0.078 Uiso 1 1 calc R . . H14C H 0.8491 -0.1966 1.0466 0.078 Uiso 1 1 calc R . . C15 C 0.6711(4) -0.0719(4) 0.89868(15) 0.0534(12) Uani 1 1 d . . . C16 C 0.5857(5) -0.1437(5) 0.8985(3) 0.096(2) Uani 1 1 d . . . H16A H 0.5980 -0.1967 0.9208 0.144 Uiso 1 1 calc R . . H16B H 0.5800 -0.1751 0.8692 0.144 Uiso 1 1 calc R . . H16C H 0.5216 -0.1075 0.9055 0.144 Uiso 1 1 calc R . . C17 C 0.7375(3) 0.2692(3) 0.95204(13) 0.0370(9) Uani 1 1 d . . . H17A H 0.6773 0.2597 0.9323 0.044 Uiso 1 1 calc R . . H17B H 0.7179 0.3173 0.9759 0.044 Uiso 1 1 calc R . . C18 C 0.8279(3) 0.3114(3) 0.92601(13) 0.0374(9) Uani 1 1 d . . . H18A H 0.8863 0.3255 0.9462 0.045 Uiso 1 1 calc R . . H18B H 0.8079 0.3762 0.9115 0.045 Uiso 1 1 calc R . . C19 C 0.8434(3) 0.1767(3) 1.02725(11) 0.0311(9) Uani 1 1 d . . . C20 C 0.9230(3) 0.1149(3) 1.04240(12) 0.0368(9) Uani 1 1 d . . . H20 H 0.9449 0.0582 1.0252 0.044 Uiso 1 1 calc R . . C21 C 0.9710(3) 0.1361(3) 1.08279(13) 0.0408(9) Uani 1 1 d . . . H21 H 1.0247 0.0932 1.0933 0.049 Uiso 1 1 calc R . . C22 C 0.9405(3) 0.2190(4) 1.10739(13) 0.0451(11) Uani 1 1 d . . . H22 H 0.9737 0.2337 1.1347 0.054 Uiso 1 1 calc R . . C23 C 0.8615(3) 0.2810(3) 1.09253(13) 0.0457(10) Uani 1 1 d . . . H23 H 0.8403 0.3381 1.1097 0.055 Uiso 1 1 calc R . . C24 C 0.8135(3) 0.2600(3) 1.05277(13) 0.0387(10) Uani 1 1 d . . . H24 H 0.7593 0.3029 1.0427 0.046 Uiso 1 1 calc R . . C25 C 0.6599(3) 0.0825(3) 0.99459(13) 0.0348(9) Uani 1 1 d . . . C26 C 0.6634(3) 0.0193(3) 1.03180(13) 0.0402(10) Uani 1 1 d . . . H26 H 0.7260 0.0127 1.0479 0.048 Uiso 1 1 calc R . . C27 C 0.5768(4) -0.0338(4) 1.04539(16) 0.0500(12) Uani 1 1 d . . . H27 H 0.5802 -0.0764 1.0708 0.060 Uiso 1 1 calc R . . C28 C 0.4856(4) -0.0253(4) 1.02219(18) 0.0563(13) Uani 1 1 d . . . H28 H 0.4261 -0.0615 1.0316 0.068 Uiso 1 1 calc R . . C29 C 0.4818(3) 0.0351(4) 0.98591(19) 0.0600(14) Uani 1 1 d . . . H29 H 0.4189 0.0404 0.9699 0.072 Uiso 1 1 calc R . . C30 C 0.5667(3) 0.0893(3) 0.97144(16) 0.0506(12) Uani 1 1 d . . . H30 H 0.5618 0.1312 0.9458 0.061 Uiso 1 1 calc R . . C31 C 0.9910(3) 0.2647(4) 0.86316(12) 0.0396(10) Uani 1 1 d . . . C32 C 1.0611(3) 0.1979(4) 0.84429(13) 0.0436(11) Uani 1 1 d . . . H32 H 1.0430 0.1282 0.8406 0.052 Uiso 1 1 calc R . . C33 C 1.1575(3) 0.2313(5) 0.83065(15) 0.0575(14) Uani 1 1 d . . . H33 H 1.2050 0.1846 0.8179 0.069 Uiso 1 1 calc R . . C34 C 1.1841(4) 0.3317(5) 0.83563(15) 0.0644(16) Uani 1 1 d . . . H34 H 1.2503 0.3546 0.8265 0.077 Uiso 1 1 calc R . . C35 C 1.1147(4) 0.3998(4) 0.85393(14) 0.0567(13) Uani 1 1 d . . . H35 H 1.1331 0.4696 0.8570 0.068 Uiso 1 1 calc R . . C36 C 1.0186(3) 0.3667(4) 0.86781(13) 0.0472(11) Uani 1 1 d . . . H36 H 0.9714 0.4138 0.8805 0.057 Uiso 1 1 calc R . . C37 C 0.7738(3) 0.2441(3) 0.83987(12) 0.0336(9) Uani 1 1 d . . . C38 C 0.6826(3) 0.1898(3) 0.83580(12) 0.0363(9) Uani 1 1 d . . . H38 H 0.6674 0.1363 0.8560 0.044 Uiso 1 1 calc R . . C39 C 0.6132(3) 0.2135(3) 0.80216(13) 0.0434(10) Uani 1 1 d . . . H39 H 0.5514 0.1752 0.7992 0.052 Uiso 1 1 calc R . . C40 C 0.6336(4) 0.2920(4) 0.77323(13) 0.0485(11) Uani 1 1 d . . . H40 H 0.5857 0.3076 0.7504 0.058 Uiso 1 1 calc R . . C41 C 0.7224(4) 0.3481(4) 0.77709(14) 0.0530(12) Uani 1 1 d . . . H41 H 0.7357 0.4027 0.7572 0.064 Uiso 1 1 calc R . . C42 C 0.7932(3) 0.3247(4) 0.81028(13) 0.0445(11) Uani 1 1 d . . . H42 H 0.8549 0.3634 0.8129 0.053 Uiso 1 1 calc R . . C43 C 1.3697(5) -0.4091(5) 0.8574(2) 0.0776(16) Uani 1 1 d . . . C44 C 1.4584(7) -0.4120(9) 0.8283(3) 0.154(4) Uani 1 1 d . . . H44A H 1.4815 -0.3422 0.8222 0.231 Uiso 1 1 calc R . . H44B H 1.4395 -0.4456 0.8005 0.231 Uiso 1 1 calc R . . H44C H 1.5143 -0.4502 0.8426 0.231 Uiso 1 1 calc R . . B1 B 0.4244(6) -0.0123(7) 0.8167(2) 0.072(2) Uani 1 1 d . . . B2 B 1.1687(4) -0.0815(4) 1.05513(18) 0.0565(15) Uani 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 0.03313(14) 0.03017(16) 0.02314(12) -0.00152(13) -0.00199(13) 0.00267(14) P1 0.0331(5) 0.0303(6) 0.0253(4) -0.0005(4) -0.0010(4) 0.0021(4) P2 0.0353(5) 0.0348(6) 0.0262(4) 0.0025(4) -0.0006(4) 0.0015(5) F1 0.099(3) 0.118(3) 0.084(2) -0.043(2) 0.034(2) -0.044(2) F2 0.094(3) 0.184(5) 0.136(4) -0.044(3) -0.025(3) 0.056(3) F3 0.108(3) 0.075(2) 0.072(2) -0.0333(18) -0.0007(18) -0.023(2) F4 0.139(4) 0.097(3) 0.102(3) -0.030(2) -0.005(2) -0.055(3) F5 0.053(3) 0.066(4) 0.153(7) 0.000(4) 0.004(4) -0.022(3) F6 0.160(7) 0.087(5) 0.092(4) -0.002(4) 0.009(5) -0.015(5) F7 0.050(4) 0.091(5) 0.165(6) -0.045(5) 0.003(5) 0.004(4) F8 0.111(6) 0.060(5) 0.059(4) 0.001(3) -0.010(3) -0.010(4) F5A 0.072(5) 0.097(7) 0.110(6) -0.037(5) -0.014(5) 0.004(5) F6A 0.081(6) 0.112(8) 0.105(6) -0.002(6) 0.028(6) -0.033(6) F7A 0.106(9) 0.078(7) 0.132(7) -0.016(7) 0.005(10) 0.024(7) F8A 0.133(10) 0.105(10) 0.054(5) 0.002(6) 0.014(5) 0.046(8) O1 0.0368(15) 0.052(2) 0.0403(15) -0.0047(14) -0.0060(13) -0.0027(14) N1 0.0358(17) 0.039(2) 0.0291(16) -0.0019(14) -0.0017(13) 0.0068(15) N2 0.0433(18) 0.044(2) 0.0311(16) -0.0066(17) -0.0017(14) 0.0072(17) N3 0.0375(15) 0.0325(18) 0.0316(14) 0.0015(15) -0.0023(14) 0.0049(19) N4 0.046(2) 0.031(2) 0.0351(17) -0.0028(15) -0.0088(15) -0.0002(17) N5 0.076(3) 0.074(4) 0.093(4) 0.017(3) 0.003(3) 0.008(3) C1 0.040(2) 0.035(2) 0.0248(18) -0.0008(17) 0.0033(17) 0.0027(19) C2 0.044(2) 0.035(2) 0.0260(19) -0.0064(17) 0.0004(17) 0.0042(18) C3 0.041(2) 0.041(3) 0.033(2) -0.006(2) 0.0028(18) 0.011(2) C4 0.049(2) 0.048(3) 0.027(2) -0.0117(19) 0.0051(18) 0.008(2) C5 0.038(2) 0.045(3) 0.0284(17) -0.0043(19) -0.0029(17) 0.0086(16) C6 0.044(2) 0.058(3) 0.048(3) -0.011(2) -0.0050(19) 0.003(2) C7 0.053(3) 0.049(3) 0.046(2) -0.001(2) -0.005(2) 0.017(2) C8 0.053(3) 0.067(3) 0.032(2) -0.009(2) -0.0074(19) 0.022(2) C9 0.106(4) 0.089(4) 0.030(2) 0.006(2) 0.000(3) 0.053(4) C10 0.062(3) 0.089(5) 0.063(3) -0.041(3) -0.022(3) 0.018(3) C11 0.058(3) 0.066(3) 0.041(2) -0.015(2) -0.001(2) 0.023(2) C12 0.066(3) 0.080(4) 0.038(2) -0.017(3) -0.012(2) 0.025(3) C13 0.0362(19) 0.039(2) 0.0381(19) -0.0005(19) 0.000(2) 0.001(2) C14 0.058(2) 0.044(3) 0.054(2) 0.015(2) 0.000(3) -0.002(3) C15 0.072(3) 0.038(3) 0.050(3) 0.004(2) -0.020(2) -0.005(3) C16 0.088(4) 0.064(4) 0.137(6) 0.005(4) -0.028(4) -0.045(3) C17 0.041(2) 0.039(2) 0.0311(19) 0.0020(18) -0.0001(17) 0.0098(19) C18 0.048(2) 0.031(2) 0.032(2) 0.0054(18) -0.0073(18) 0.0031(18) C19 0.0305(19) 0.037(2) 0.0254(17) 0.0011(17) 0.0030(14) -0.0037(16) C20 0.044(2) 0.040(2) 0.0260(19) -0.0045(18) 0.0011(17) 0.0012(19) C21 0.039(2) 0.051(3) 0.032(2) 0.005(2) -0.0060(19) -0.0025(19) C22 0.043(2) 0.064(3) 0.028(2) -0.007(2) 0.0019(18) -0.017(2) C23 0.046(2) 0.052(3) 0.039(2) -0.0168(19) 0.0042(19) -0.003(2) C24 0.038(2) 0.044(3) 0.035(2) -0.008(2) 0.0030(17) -0.0012(19) C25 0.0331(19) 0.033(2) 0.038(2) -0.0058(18) 0.0034(15) 0.0030(16) C26 0.045(2) 0.039(3) 0.036(2) 0.0038(19) -0.0010(17) -0.0009(19) C27 0.056(3) 0.040(3) 0.054(3) 0.002(2) 0.007(2) -0.013(2) C28 0.049(3) 0.042(3) 0.078(4) -0.008(3) 0.011(3) -0.010(2) C29 0.034(2) 0.051(3) 0.095(4) 0.005(3) -0.011(2) -0.007(2) C30 0.041(2) 0.049(3) 0.062(3) 0.012(2) -0.011(2) -0.007(2) C31 0.035(2) 0.056(3) 0.0278(19) 0.008(2) -0.0043(16) -0.011(2) C32 0.033(2) 0.061(3) 0.037(2) 0.012(2) -0.0002(18) 0.003(2) C33 0.045(3) 0.084(4) 0.043(3) 0.019(3) 0.004(2) 0.006(3) C34 0.043(3) 0.109(5) 0.041(3) 0.028(3) -0.006(2) -0.018(3) C35 0.056(3) 0.070(3) 0.044(2) 0.007(2) -0.009(2) -0.026(3) C36 0.052(3) 0.054(3) 0.036(2) 0.002(2) -0.0029(19) -0.014(2) C37 0.035(2) 0.039(2) 0.0267(18) 0.0017(17) 0.0019(16) 0.0068(18) C38 0.044(2) 0.037(2) 0.0282(19) -0.0028(18) 0.0031(17) 0.0044(19) C39 0.039(2) 0.048(3) 0.043(2) -0.005(2) -0.0050(19) 0.007(2) C40 0.045(2) 0.063(3) 0.037(2) 0.011(2) -0.005(2) 0.012(3) C41 0.060(3) 0.055(3) 0.044(2) 0.016(2) -0.002(2) 0.004(3) C42 0.048(2) 0.050(3) 0.035(2) 0.012(2) -0.0049(19) -0.001(2) C43 0.063(3) 0.090(4) 0.080(4) 0.022(3) -0.007(3) -0.003(4) C44 0.109(6) 0.245(13) 0.107(6) 0.041(7) 0.025(5) 0.007(7) B1 0.068(4) 0.077(5) 0.071(4) -0.025(4) 0.005(3) -0.008(4) B2 0.067(4) 0.054(4) 0.049(3) 0.004(3) 0.004(3) 0.000(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 1.858(4) . ? Ru1 N3 2.115(3) . ? Ru1 N4 2.119(4) . ? Ru1 C2 2.180(4) . ? Ru1 P2 2.3425(10) . ? Ru1 P1 2.3793(10) . ? P1 C25 1.819(4) . ? P1 C19 1.822(4) . ? P1 C17 1.827(4) . ? P2 C37 1.830(4) . ? P2 C31 1.836(4) . ? P2 C18 1.839(4) . ? F1 B1 1.366(8) . ? F2 B1 1.315(8) . ? F3 B1 1.399(8) . ? F4 B1 1.389(9) . ? F5 B2 1.342(7) . ? F6 B2 1.366(8) . ? F7 B2 1.360(9) . ? F8 B2 1.393(9) . ? F5A B2 1.387(9) . ? F6A B2 1.356(10) . ? F7A B2 1.375(12) . ? F8A B2 1.345(12) . ? O1 C1 1.139(4) . ? N1 C2 1.359(5) . ? N1 C3 1.393(5) . ? N1 C5 1.489(5) . ? N2 C2 1.364(5) . ? N2 C4 1.398(5) . ? N2 C8 1.483(5) . ? N3 C13 1.141(5) . ? N4 C15 1.146(6) . ? N5 C43 1.116(7) . ? C3 C4 1.345(6) . ? C3 C11 1.488(6) . ? C4 C12 1.501(6) . ? C5 C7 1.527(6) . ? C5 C6 1.531(6) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.516(7) . ? C8 C10 1.543(7) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.455(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.453(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.516(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.389(5) . ? C19 C24 1.391(5) . ? C20 C21 1.396(5) . ? C20 H20 0.9500 . ? C21 C22 1.374(6) . ? C21 H21 0.9500 . ? C22 C23 1.383(6) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.397(5) . ? C25 C30 1.399(6) . ? C26 C27 1.384(6) . ? C26 H26 0.9500 . ? C27 C28 1.378(7) . ? C27 H27 0.9500 . ? C28 C29 1.352(7) . ? C28 H28 0.9500 . ? C29 C30 1.381(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.385(6) . ? C31 C36 1.391(6) . ? C32 C33 1.387(6) . ? C32 H32 0.9500 . ? C33 C34 1.368(8) . ? C33 H33 0.9500 . ? C34 C35 1.383(7) . ? C34 H34 0.9500 . ? C35 C36 1.385(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.386(6) . ? C37 C42 1.407(6) . ? C38 C39 1.391(5) . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 H39 0.9500 . ? C40 C41 1.371(7) . ? C40 H40 0.9500 . ? C41 C42 1.393(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.448(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 N3 95.66(15) . . ? C1 Ru1 N4 174.70(15) . . ? N3 Ru1 N4 79.39(13) . . ? C1 Ru1 C2 93.88(15) . . ? N3 Ru1 C2 87.90(13) . . ? N4 Ru1 C2 87.86(14) . . ? C1 Ru1 P2 81.18(12) . . ? N3 Ru1 P2 172.18(8) . . ? N4 Ru1 P2 103.49(9) . . ? C2 Ru1 P2 99.42(11) . . ? C1 Ru1 P1 90.06(12) . . ? N3 Ru1 P1 89.19(8) . . ? N4 Ru1 P1 88.00(9) . . ? C2 Ru1 P1 175.31(11) . . ? P2 Ru1 P1 83.68(3) . . ? C25 P1 C19 103.38(17) . . ? C25 P1 C17 107.56(18) . . ? C19 P1 C17 106.18(19) . . ? C25 P1 Ru1 116.09(13) . . ? C19 P1 Ru1 116.05(12) . . ? C17 P1 Ru1 106.92(13) . . ? C37 P2 C31 105.33(17) . . ? C37 P2 C18 101.16(18) . . ? C31 P2 C18 104.5(2) . . ? C37 P2 Ru1 122.81(14) . . ? C31 P2 Ru1 114.94(15) . . ? C18 P2 Ru1 105.79(13) . . ? C2 N1 C3 111.2(3) . . ? C2 N1 C5 124.2(3) . . ? C3 N1 C5 124.6(3) . . ? C2 N2 C4 110.8(3) . . ? C2 N2 C8 124.2(3) . . ? C4 N2 C8 124.9(3) . . ? C13 N3 Ru1 175.4(3) . . ? C15 N4 Ru1 161.9(3) . . ? O1 C1 Ru1 177.5(4) . . ? N1 C2 N2 104.4(3) . . ? N1 C2 Ru1 127.0(2) . . ? N2 C2 Ru1 128.4(3) . . ? C4 C3 N1 106.8(3) . . ? C4 C3 C11 127.1(4) . . ? N1 C3 C11 126.1(4) . . ? C3 C4 N2 106.7(3) . . ? C3 C4 C12 128.6(4) . . ? N2 C4 C12 124.6(4) . . ? N1 C5 C7 111.1(3) . . ? N1 C5 C6 111.6(3) . . ? C7 C5 C6 113.4(3) . . ? N1 C5 H5 106.7 . . ? C7 C5 H5 106.7 . . ? C6 C5 H5 106.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 112.2(4) . . ? N2 C8 C10 111.6(4) . . ? C9 C8 C10 113.2(4) . . ? N2 C8 H8 106.5 . . ? C9 C8 H8 106.5 . . ? C10 C8 H8 106.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 178.8(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 C16 176.4(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P1 108.2(3) . . ? C18 C17 H17A 110.1 . . ? P1 C17 H17A 110.1 . . ? C18 C17 H17B 110.1 . . ? P1 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C17 C18 P2 109.0(3) . . ? C17 C18 H18A 109.9 . . ? P2 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? P2 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C20 C19 C24 118.8(3) . . ? C20 C19 P1 120.7(3) . . ? C24 C19 P1 120.4(3) . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 120.8(4) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C26 C25 C30 117.9(4) . . ? C26 C25 P1 119.9(3) . . ? C30 C25 P1 122.1(3) . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.3(4) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 119.4(4) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 121.8(4) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 119.9(4) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C32 C31 C36 118.7(4) . . ? C32 C31 P2 120.2(3) . . ? C36 C31 P2 121.0(3) . . ? C33 C32 C31 121.0(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 119.9(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.1(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.3(5) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 120.1(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 C42 118.8(4) . . ? C38 C37 P2 122.0(3) . . ? C42 C37 P2 119.2(3) . . ? C37 C38 C39 120.1(4) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 120.4(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 120.5(4) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 119.8(4) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C37 120.2(4) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? N5 C43 C44 177.0(9) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? F2 B1 F1 114.0(7) . . ? F2 B1 F4 105.9(6) . . ? F1 B1 F4 106.7(6) . . ? F2 B1 F3 111.4(6) . . ? F1 B1 F3 109.4(5) . . ? F4 B1 F3 109.2(6) . . ? F5 B2 F8A 91.9(10) . . ? F5 B2 F6A 141.8(8) . . ? F8A B2 F6A 119.8(11) . . ? F5 B2 F7 110.9(6) . . ? F8A B2 F7 106.4(12) . . ? F6A B2 F7 81.8(9) . . ? F5 B2 F6 107.1(7) . . ? F8A B2 F6 122.2(9) . . ? F6A B2 F6 39.2(5) . . ? F7 B2 F6 115.6(9) . . ? F5 B2 F7A 85.6(8) . . ? F8A B2 F7A 113.0(13) . . ? F6A B2 F7A 99.2(11) . . ? F7 B2 F7A 25.7(7) . . ? F6 B2 F7A 122.3(11) . . ? F5 B2 F5A 40.9(5) . . ? F8A B2 F5A 117.5(11) . . ? F6A B2 F5A 101.8(8) . . ? F7 B2 F5A 125.0(8) . . ? F6 B2 F5A 66.5(7) . . ? F7A B2 F5A 102.7(10) . . ? F5 B2 F8 110.6(7) . . ? F8A B2 F8 24.4(9) . . ? F6A B2 F8 96.2(8) . . ? F7 B2 F8 111.6(9) . . ? F6 B2 F8 100.5(6) . . ? F7A B2 F8 127.8(11) . . ? F5A B2 F8 122.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 P1 C25 -149.30(19) . . . . ? N3 Ru1 P1 C25 -53.65(17) . . . . ? N4 Ru1 P1 C25 25.77(17) . . . . ? C2 Ru1 P1 C25 -2.0(13) . . . . ? P2 Ru1 P1 C25 129.58(14) . . . . ? C1 Ru1 P1 C19 -27.55(19) . . . . ? N3 Ru1 P1 C19 68.11(17) . . . . ? N4 Ru1 P1 C19 147.52(17) . . . . ? C2 Ru1 P1 C19 119.7(13) . . . . ? P2 Ru1 P1 C19 -108.67(15) . . . . ? C1 Ru1 P1 C17 90.68(18) . . . . ? N3 Ru1 P1 C17 -173.66(16) . . . . ? N4 Ru1 P1 C17 -94.25(17) . . . . ? C2 Ru1 P1 C17 -122.1(13) . . . . ? P2 Ru1 P1 C17 9.56(14) . . . . ? C1 Ru1 P2 C37 170.49(18) . . . . ? N3 Ru1 P2 C37 -122.9(7) . . . . ? N4 Ru1 P2 C37 -12.06(17) . . . . ? C2 Ru1 P2 C37 77.99(18) . . . . ? P1 Ru1 P2 C37 -98.46(15) . . . . ? C1 Ru1 P2 C31 40.19(19) . . . . ? N3 Ru1 P2 C31 106.8(7) . . . . ? N4 Ru1 P2 C31 -142.35(17) . . . . ? C2 Ru1 P2 C31 -52.31(18) . . . . ? P1 Ru1 P2 C31 131.24(15) . . . . ? C1 Ru1 P2 C18 -74.57(18) . . . . ? N3 Ru1 P2 C18 -8.0(7) . . . . ? N4 Ru1 P2 C18 102.88(16) . . . . ? C2 Ru1 P2 C18 -167.07(17) . . . . ? P1 Ru1 P2 C18 16.48(14) . . . . ? C1 Ru1 N3 C13 92(4) . . . . ? N4 Ru1 N3 C13 -86(4) . . . . ? C2 Ru1 N3 C13 -174(4) . . . . ? P2 Ru1 N3 C13 26(5) . . . . ? P1 Ru1 N3 C13 2(4) . . . . ? C1 Ru1 N4 C15 -20(2) . . . . ? N3 Ru1 N4 C15 0.7(12) . . . . ? C2 Ru1 N4 C15 89.0(12) . . . . ? P2 Ru1 N4 C15 -171.8(12) . . . . ? P1 Ru1 N4 C15 -88.8(12) . . . . ? N3 Ru1 C1 O1 -115(8) . . . . ? N4 Ru1 C1 O1 -94(9) . . . . ? C2 Ru1 C1 O1 157(8) . . . . ? P2 Ru1 C1 O1 58(8) . . . . ? P1 Ru1 C1 O1 -26(8) . . . . ? C3 N1 C2 N2 0.7(4) . . . . ? C5 N1 C2 N2 179.4(3) . . . . ? C3 N1 C2 Ru1 175.5(3) . . . . ? C5 N1 C2 Ru1 -5.8(5) . . . . ? C4 N2 C2 N1 -0.2(5) . . . . ? C8 N2 C2 N1 -177.8(4) . . . . ? C4 N2 C2 Ru1 -174.9(3) . . . . ? C8 N2 C2 Ru1 7.5(6) . . . . ? C1 Ru1 C2 N1 45.8(4) . . . . ? N3 Ru1 C2 N1 -49.7(3) . . . . ? N4 Ru1 C2 N1 -129.1(3) . . . . ? P2 Ru1 C2 N1 127.5(3) . . . . ? P1 Ru1 C2 N1 -101.3(13) . . . . ? C1 Ru1 C2 N2 -140.6(4) . . . . ? N3 Ru1 C2 N2 123.9(4) . . . . ? N4 Ru1 C2 N2 44.4(4) . . . . ? P2 Ru1 C2 N2 -58.9(4) . . . . ? P1 Ru1 C2 N2 72.2(14) . . . . ? C2 N1 C3 C4 -1.0(5) . . . . ? C5 N1 C3 C4 -179.7(4) . . . . ? C2 N1 C3 C11 -178.1(4) . . . . ? C5 N1 C3 C11 3.2(7) . . . . ? N1 C3 C4 N2 0.8(5) . . . . ? C11 C3 C4 N2 177.8(4) . . . . ? N1 C3 C4 C12 -176.0(5) . . . . ? C11 C3 C4 C12 1.0(8) . . . . ? C2 N2 C4 C3 -0.4(5) . . . . ? C8 N2 C4 C3 177.2(4) . . . . ? C2 N2 C4 C12 176.6(5) . . . . ? C8 N2 C4 C12 -5.9(7) . . . . ? C2 N1 C5 C7 121.8(4) . . . . ? C3 N1 C5 C7 -59.6(5) . . . . ? C2 N1 C5 C6 -110.5(4) . . . . ? C3 N1 C5 C6 68.1(5) . . . . ? C2 N2 C8 C9 115.1(5) . . . . ? C4 N2 C8 C9 -62.1(6) . . . . ? C2 N2 C8 C10 -116.7(5) . . . . ? C4 N2 C8 C10 66.1(5) . . . . ? Ru1 N3 C13 C14 -82(25) . . . . ? Ru1 N4 C15 C16 65(9) . . . . ? C25 P1 C17 C18 -165.7(3) . . . . ? C19 P1 C17 C18 84.1(3) . . . . ? Ru1 P1 C17 C18 -40.4(3) . . . . ? P1 C17 C18 P2 56.7(3) . . . . ? C37 P2 C18 C17 82.2(3) . . . . ? C31 P2 C18 C17 -168.6(3) . . . . ? Ru1 P2 C18 C17 -46.8(3) . . . . ? C25 P1 C19 C20 98.6(3) . . . . ? C17 P1 C19 C20 -148.3(3) . . . . ? Ru1 P1 C19 C20 -29.7(3) . . . . ? C25 P1 C19 C24 -79.3(3) . . . . ? C17 P1 C19 C24 33.8(3) . . . . ? Ru1 P1 C19 C24 152.5(3) . . . . ? C24 C19 C20 C21 0.6(6) . . . . ? P1 C19 C20 C21 -177.3(3) . . . . ? C19 C20 C21 C22 -0.9(6) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C19 0.1(6) . . . . ? C20 C19 C24 C23 -0.2(6) . . . . ? P1 C19 C24 C23 177.7(3) . . . . ? C19 P1 C25 C26 -35.3(4) . . . . ? C17 P1 C25 C26 -147.3(3) . . . . ? Ru1 P1 C25 C26 93.0(3) . . . . ? C19 P1 C25 C30 148.4(4) . . . . ? C17 P1 C25 C30 36.4(4) . . . . ? Ru1 P1 C25 C30 -83.3(4) . . . . ? C30 C25 C26 C27 -0.7(6) . . . . ? P1 C25 C26 C27 -177.2(3) . . . . ? C25 C26 C27 C28 0.3(7) . . . . ? C26 C27 C28 C29 0.3(7) . . . . ? C27 C28 C29 C30 -0.4(8) . . . . ? C28 C29 C30 C25 -0.1(8) . . . . ? C26 C25 C30 C29 0.6(7) . . . . ? P1 C25 C30 C29 177.0(4) . . . . ? C37 P2 C31 C32 -98.3(3) . . . . ? C18 P2 C31 C32 155.5(3) . . . . ? Ru1 P2 C31 C32 40.0(4) . . . . ? C37 P2 C31 C36 84.7(4) . . . . ? C18 P2 C31 C36 -21.5(4) . . . . ? Ru1 P2 C31 C36 -137.0(3) . . . . ? C36 C31 C32 C33 0.7(6) . . . . ? P2 C31 C32 C33 -176.4(3) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? C32 C33 C34 C35 -0.5(7) . . . . ? C33 C34 C35 C36 0.8(7) . . . . ? C34 C35 C36 C31 -0.4(6) . . . . ? C32 C31 C36 C35 -0.3(6) . . . . ? P2 C31 C36 C35 176.7(3) . . . . ? C31 P2 C37 C38 156.7(3) . . . . ? C18 P2 C37 C38 -94.7(3) . . . . ? Ru1 P2 C37 C38 22.5(4) . . . . ? C31 P2 C37 C42 -26.0(4) . . . . ? C18 P2 C37 C42 82.6(3) . . . . ? Ru1 P2 C37 C42 -160.2(3) . . . . ? C42 C37 C38 C39 1.7(6) . . . . ? P2 C37 C38 C39 179.0(3) . . . . ? C37 C38 C39 C40 -1.2(6) . . . . ? C38 C39 C40 C41 0.0(6) . . . . ? C39 C40 C41 C42 0.6(7) . . . . ? C40 C41 C42 C37 -0.1(7) . . . . ? C38 C37 C42 C41 -1.1(6) . . . . ? P2 C37 C42 C41 -178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.391 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.106 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.207 0.159 0.698 150 24 ' ' 2 -0.207 0.659 0.802 150 24 ' ' 3 0.293 0.841 0.198 150 23 ' ' 4 0.706 0.341 0.302 150 23 ' ' _platon_squeeze_details ; ; #===end