# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jonathan Michael Jeremy Williams' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down BATH BA2 7AY UNITED KINGDOM ; _publ_contact_author_email J.M.J.WILLIAMS@BATH.AC.UK _publ_section_title ; Ruthenium Xantphos Complexes in Hydrogen Transfer Processes: Reactivity and Mechanistic Studies ; loop_ _publ_author_name J.Williams 'Araminta E. W. Ledger' 'John P. Lowe' 'Mary F. Mahon' P.Slatford M.Whittlesey # Attachment '18_20_22.cif' data_Compound_18_k05jmjw1 _database_code_depnum_ccdc_archive 'CCDC 678477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H49 O2 P3 Ru' _chemical_formula_weight 971.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0940(1) _cell_length_b 12.9620(1) _cell_length_c 18.1840(2) _cell_angle_alpha 92.599(1) _cell_angle_beta 92.909(1) _cell_angle_gamma 113.854(1) _cell_volume 2382.20(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29836 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.373 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44250 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10813 _reflns_number_gt 9114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.8278P] 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 10813 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 -0.065706(17) -0.172826(14) 0.239271(10) 0.02002(6) Uani 1 1 d . . . P1 P -0.27449(5) -0.29636(5) 0.18886(3) 0.02312(13) Uani 1 1 d . . . P2 P 0.00782(6) -0.29405(5) 0.30645(3) 0.02386(13) Uani 1 1 d . A . P3 P 0.06356(6) 0.00975(5) 0.28388(3) 0.02291(13) Uani 1 1 d . . . O1 O 0.0976(2) -0.17773(19) 0.11061(12) 0.0629(6) Uani 1 1 d . . . O2 O -0.17190(14) -0.46327(12) 0.19451(8) 0.0228(3) Uani 1 1 d . . . C1 C 0.0346(2) -0.1778(2) 0.15880(14) 0.0349(6) Uani 1 1 d . . . C2 C -0.2825(2) -0.39342(18) 0.11032(12) 0.0251(5) Uani 1 1 d . . . C3 C -0.3363(2) -0.3966(2) 0.03895(13) 0.0322(5) Uani 1 1 d . . . H3 H -0.3799 -0.3488 0.0280 0.039 Uiso 1 1 calc R . . C4 C -0.3262(3) -0.4700(2) -0.01658(14) 0.0386(6) Uani 1 1 d . . . H4 H -0.3621 -0.4709 -0.0653 0.046 Uiso 1 1 calc R . . C5 C -0.2647(2) -0.5410(2) -0.00162(14) 0.0367(6) Uani 1 1 d . . . H5 H -0.2586 -0.5901 -0.0403 0.044 Uiso 1 1 calc R . . C6 C -0.2113(2) -0.54232(19) 0.06903(13) 0.0287(5) Uani 1 1 d . . . C7 C -0.1483(2) -0.62137(19) 0.09375(14) 0.0316(5) Uani 1 1 d . . . C8 C -0.0350(2) -0.55305(19) 0.15140(13) 0.0288(5) Uani 1 1 d . . . C9 C 0.0839(2) -0.5645(2) 0.16100(15) 0.0377(6) Uani 1 1 d . . . H9 H 0.1012 -0.6161 0.1290 0.045 Uiso 1 1 calc R . . C10 C 0.1775(3) -0.5010(2) 0.21703(17) 0.0426(7) Uani 1 1 d . . . H10 H 0.2570 -0.5118 0.2242 0.051 Uiso 1 1 calc R . . C11 C 0.1572(2) -0.4223(2) 0.26278(16) 0.0373(6) Uani 1 1 d . . . H11 H 0.2232 -0.3791 0.3005 0.045 Uiso 1 1 calc R . . C12 C 0.0405(2) -0.40541(18) 0.25421(13) 0.0266(5) Uani 1 1 d . . . C13 C -0.0528(2) -0.47476(18) 0.19986(13) 0.0246(5) Uani 1 1 d . . . C14 C -0.2222(2) -0.46704(18) 0.12269(12) 0.0241(5) Uani 1 1 d . . . C15 C -0.1008(3) -0.6704(2) 0.02847(16) 0.0456(7) Uani 1 1 d . . . H15A H -0.0336 -0.6086 0.0049 0.068 Uiso 1 1 calc R . . H15B H -0.1758 -0.7120 -0.0075 0.068 Uiso 1 1 calc R . . H15C H -0.0628 -0.7218 0.0463 0.068 Uiso 1 1 calc R . . C16 C -0.2527(3) -0.7197(2) 0.13037(16) 0.0404(6) Uani 1 1 d . . . H16A H -0.2123 -0.7686 0.1498 0.061 Uiso 1 1 calc R . . H16B H -0.3255 -0.7638 0.0937 0.061 Uiso 1 1 calc R . . H16C H -0.2867 -0.6895 0.1709 0.061 Uiso 1 1 calc R . . C17 C -0.3753(3) -0.2253(2) 0.14934(14) 0.0368(6) Uani 1 1 d . . . C18 C -0.5084(3) -0.2589(3) 0.16194(18) 0.0520(8) Uani 1 1 d . . . H18 H -0.5500 -0.3208 0.1912 0.062 Uiso 1 1 calc R . . C19 C -0.5806(4) -0.2026(4) 0.1320(2) 0.0807(14) Uani 1 1 d . . . H19 H -0.6711 -0.2266 0.1412 0.097 Uiso 1 1 calc R . . C20 C -0.5244(5) -0.1143(4) 0.0900(2) 0.0908(17) Uani 1 1 d . . . H20 H -0.5744 -0.0755 0.0710 0.109 Uiso 1 1 calc R . . C21 C -0.3924(5) -0.0808(3) 0.0750(2) 0.0848(14) Uani 1 1 d . . . H21 H -0.3528 -0.0204 0.0444 0.102 Uiso 1 1 calc R . . C22 C -0.3180(3) -0.1363(3) 0.10532(17) 0.0570(9) Uani 1 1 d . . . H22 H -0.2277 -0.1127 0.0955 0.068 Uiso 1 1 calc R . . C23 C -0.3904(2) -0.3933(2) 0.24878(13) 0.0283(5) Uani 1 1 d . . . C24 C -0.4129(3) -0.3493(3) 0.31441(18) 0.0748(12) Uani 1 1 d . . . H24 H -0.3683 -0.2706 0.3276 0.090 Uiso 1 1 calc R . . C25 C -0.4999(4) -0.4185(4) 0.3614(2) 0.1027(18) Uani 1 1 d . . . H25 H -0.5155 -0.3866 0.4061 0.123 Uiso 1 1 calc R . . C26 C -0.5638(3) -0.5329(3) 0.34374(18) 0.0674(10) Uani 1 1 d . . . H26 H -0.6212 -0.5804 0.3768 0.081 Uiso 1 1 calc R . . C27 C -0.5445(3) -0.5780(2) 0.27853(17) 0.0459(7) Uani 1 1 d . . . H27 H -0.5897 -0.6568 0.2656 0.055 Uiso 1 1 calc R . . C28 C -0.4586(2) -0.5083(2) 0.23111(15) 0.0340(6) Uani 1 1 d . . . H28 H -0.4463 -0.5401 0.1855 0.041 Uiso 1 1 calc R . . C29 C 0.1728(2) -0.2198(2) 0.35443(15) 0.0365(6) Uani 1 1 d . . . C30 C 0.2014(3) -0.2204(2) 0.42972(17) 0.0523(8) Uani 1 1 d . . . H30 H 0.1337 -0.2622 0.4600 0.063 Uiso 1 1 calc R . . C31 C 0.3296(4) -0.1596(3) 0.4603(3) 0.0813(14) Uani 1 1 d . . . H31 H 0.3488 -0.1594 0.5118 0.098 Uiso 1 1 calc R . . C32 C 0.4282(4) -0.1003(3) 0.4175(3) 0.0892(16) Uani 1 1 d . . . H32 H 0.5152 -0.0587 0.4394 0.107 Uiso 1 1 calc R . . C33 C 0.4021(3) -0.1005(3) 0.3424(3) 0.0761(12) Uani 1 1 d . . . H33 H 0.4714 -0.0606 0.3124 0.091 Uiso 1 1 calc R . . C34 C 0.2732(3) -0.1597(2) 0.3109(2) 0.0504(8) Uani 1 1 d . . . H34 H 0.2545 -0.1589 0.2594 0.060 Uiso 1 1 calc R . . C35 C -0.0885(3) -0.37278(19) 0.38015(13) 0.0315(5) Uani 1 1 d . . . C36 C -0.1307(11) -0.3162(10) 0.4366(5) 0.041(2) Uani 0.50 1 d P A 1 H36 H -0.1121 -0.2385 0.4331 0.049 Uiso 0.50 1 calc PR A 1 C37 C -0.1971(14) -0.3697(11) 0.4958(6) 0.047(3) Uani 0.50 1 d P A 1 H37 H -0.2129 -0.3280 0.5357 0.056 Uiso 0.50 1 calc PR A 1 C38 C -0.239(2) -0.483(3) 0.4951(17) 0.052(6) Uani 0.50 1 d P A 1 H38 H -0.2936 -0.5218 0.5321 0.062 Uiso 0.50 1 calc PR A 1 C39 C -0.2043(11) -0.5439(10) 0.4432(7) 0.072(4) Uani 0.50 1 d P A 1 H39 H -0.2279 -0.6225 0.4468 0.087 Uiso 0.50 1 calc PR A 1 C40 C -0.1340(8) -0.4883(8) 0.3850(5) 0.050(2) Uani 0.50 1 d P A 1 H40 H -0.1165 -0.5319 0.3469 0.060 Uiso 0.50 1 calc PR A 1 C41 C -0.0305(2) 0.09789(19) 0.30007(13) 0.0274(5) Uani 1 1 d . . . C42 C -0.1658(3) 0.0553(2) 0.29064(17) 0.0451(7) Uani 1 1 d . . . H42 H -0.2146 -0.0221 0.2746 0.054 Uiso 1 1 calc R . . C43 C -0.2323(3) 0.1237(3) 0.3042(2) 0.0616(10) Uani 1 1 d . . . H43 H -0.3260 0.0926 0.2970 0.074 Uiso 1 1 calc R . . C44 C -0.1656(3) 0.2346(3) 0.32767(16) 0.0495(7) Uani 1 1 d . . . H44 H -0.2119 0.2808 0.3376 0.059 Uiso 1 1 calc R . . C45 C -0.0312(4) 0.2784(3) 0.3367(2) 0.0710(11) Uani 1 1 d . . . H45 H 0.0169 0.3559 0.3525 0.085 Uiso 1 1 calc R . . C46 C 0.0356(3) 0.2107(2) 0.3231(2) 0.0616(10) Uani 1 1 d . . . H46 H 0.1294 0.2427 0.3297 0.074 Uiso 1 1 calc R . . C47 C 0.1662(2) 0.0505(2) 0.37254(14) 0.0345(6) Uani 1 1 d . . . C48 C 0.1122(3) -0.0093(3) 0.43187(14) 0.0446(7) Uani 1 1 d . . . H48 H 0.0315 -0.0748 0.4244 0.053 Uiso 1 1 calc R . . C49 C 0.1737(4) 0.0243(4) 0.50252(17) 0.0691(11) Uani 1 1 d . . . H49 H 0.1344 -0.0177 0.5429 0.083 Uiso 1 1 calc R . . C50 C 0.2903(5) 0.1173(4) 0.5142(2) 0.0875(16) Uani 1 1 d . . . H50 H 0.3312 0.1413 0.5627 0.105 Uiso 1 1 calc R . . C51 C 0.3481(4) 0.1760(3) 0.4556(3) 0.0821(14) Uani 1 1 d . . . H51 H 0.4307 0.2393 0.4635 0.098 Uiso 1 1 calc R . . C52 C 0.2870(3) 0.1439(3) 0.3845(2) 0.0578(9) Uani 1 1 d . . . H52 H 0.3275 0.1855 0.3443 0.069 Uiso 1 1 calc R . . C53 C 0.1785(2) 0.08966(19) 0.21724(14) 0.0307(5) Uani 1 1 d . . . C54 C 0.1407(3) 0.1455(2) 0.16389(16) 0.0440(7) Uani 1 1 d . . . H54 H 0.0569 0.1492 0.1644 0.053 Uiso 1 1 calc R . . C55 C 0.2240(3) 0.1962(3) 0.10951(18) 0.0606(9) Uani 1 1 d . . . H55 H 0.1967 0.2340 0.0730 0.073 Uiso 1 1 calc R . . C56 C 0.3460(3) 0.1921(3) 0.10817(19) 0.0586(9) Uani 1 1 d . . . H56 H 0.4037 0.2285 0.0716 0.070 Uiso 1 1 calc R . . C57 C 0.3839(3) 0.1352(2) 0.16001(19) 0.0557(9) Uani 1 1 d . . . H57 H 0.4674 0.1311 0.1591 0.067 Uiso 1 1 calc R . . C58 C 0.3001(3) 0.0838(2) 0.21349(18) 0.0463(7) Uani 1 1 d . . . H58 H 0.3264 0.0434 0.2486 0.056 Uiso 1 1 calc R . . H1 H -0.108(3) -0.085(2) 0.1977(15) 0.055(8) Uiso 1 1 d . . . H2 H -0.153(2) -0.1595(19) 0.3098(12) 0.026(6) Uiso 1 1 d . . . C36A C -0.1690(11) -0.3397(10) 0.4126(6) 0.041(2) Uani 0.50 1 d P A 2 H36A H -0.1838 -0.2769 0.3964 0.049 Uiso 0.50 1 calc PR A 2 C37A C -0.2332(15) -0.3968(13) 0.4711(6) 0.056(3) Uani 0.50 1 d P A 2 H37A H -0.2967 -0.3757 0.4930 0.067 Uiso 0.50 1 calc PR A 2 C38A C -0.206(2) -0.487(3) 0.4994(17) 0.057(6) Uani 0.50 1 d P A 2 H38A H -0.2462 -0.5242 0.5413 0.068 Uiso 0.50 1 calc PR A 2 C39A C -0.1209(14) -0.5172(10) 0.4642(7) 0.096(5) Uani 0.50 1 d P A 2 H39A H -0.1045 -0.5796 0.4798 0.115 Uiso 0.50 1 calc PR A 2 C40A C -0.0564(12) -0.4610(8) 0.4060(5) 0.077(4) Uani 0.50 1 d P A 2 H40A H 0.0078 -0.4805 0.3837 0.092 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02274(9) 0.01630(9) 0.01871(9) 0.00041(6) 0.00203(7) 0.00560(7) P1 0.0238(3) 0.0205(3) 0.0233(3) -0.0024(2) -0.0007(2) 0.0078(2) P2 0.0263(3) 0.0188(3) 0.0257(3) -0.0009(2) -0.0005(2) 0.0089(2) P3 0.0242(3) 0.0176(3) 0.0246(3) 0.0004(2) 0.0036(2) 0.0061(2) O1 0.0686(14) 0.0723(15) 0.0441(13) -0.0114(11) 0.0276(11) 0.0240(12) O2 0.0237(8) 0.0223(8) 0.0221(8) -0.0015(6) 0.0054(6) 0.0090(6) C1 0.0384(14) 0.0295(13) 0.0310(14) -0.0043(10) 0.0040(11) 0.0085(11) C2 0.0245(11) 0.0214(11) 0.0241(12) -0.0016(9) 0.0036(9) 0.0040(9) C3 0.0328(13) 0.0315(13) 0.0270(13) 0.0006(10) -0.0003(10) 0.0080(11) C4 0.0399(14) 0.0443(15) 0.0223(13) -0.0030(11) -0.0002(11) 0.0083(12) C5 0.0375(14) 0.0350(14) 0.0280(13) -0.0093(11) 0.0093(11) 0.0054(11) C6 0.0261(12) 0.0249(12) 0.0275(12) -0.0039(9) 0.0096(10) 0.0023(10) C7 0.0327(13) 0.0249(12) 0.0348(14) -0.0054(10) 0.0124(11) 0.0088(10) C8 0.0299(12) 0.0224(11) 0.0336(13) 0.0013(10) 0.0141(10) 0.0090(10) C9 0.0371(14) 0.0283(13) 0.0513(17) -0.0020(11) 0.0145(12) 0.0164(11) C10 0.0315(14) 0.0368(14) 0.0652(19) -0.0022(13) 0.0051(13) 0.0202(12) C11 0.0316(13) 0.0291(13) 0.0518(17) -0.0016(12) -0.0001(12) 0.0140(11) C12 0.0275(12) 0.0206(11) 0.0336(13) 0.0018(9) 0.0045(10) 0.0116(9) C13 0.0235(11) 0.0199(11) 0.0319(13) 0.0051(9) 0.0096(9) 0.0090(9) C14 0.0217(11) 0.0231(11) 0.0214(11) -0.0010(9) 0.0057(9) 0.0027(9) C15 0.0468(16) 0.0436(16) 0.0460(17) -0.0146(13) 0.0131(13) 0.0186(13) C16 0.0402(15) 0.0259(13) 0.0500(17) -0.0016(11) 0.0136(13) 0.0074(11) C17 0.0440(15) 0.0302(13) 0.0374(15) -0.0130(11) -0.0160(12) 0.0201(12) C18 0.0485(17) 0.0566(19) 0.060(2) -0.0208(15) -0.0136(15) 0.0359(15) C19 0.081(3) 0.099(3) 0.088(3) -0.048(3) -0.040(2) 0.074(3) C20 0.125(4) 0.083(3) 0.092(3) -0.046(2) -0.072(3) 0.085(3) C21 0.129(4) 0.052(2) 0.073(3) -0.0066(18) -0.059(3) 0.045(2) C22 0.067(2) 0.0438(17) 0.0554(19) 0.0009(14) -0.0312(16) 0.0223(16) C23 0.0190(11) 0.0345(13) 0.0268(12) -0.0034(10) 0.0015(9) 0.0066(10) C24 0.0535(19) 0.066(2) 0.055(2) -0.0344(17) 0.0292(16) -0.0264(16) C25 0.066(2) 0.113(3) 0.056(2) -0.042(2) 0.0408(19) -0.038(2) C26 0.0439(18) 0.081(2) 0.0456(19) 0.0072(17) 0.0174(15) -0.0087(17) C27 0.0398(15) 0.0401(15) 0.0580(19) 0.0123(14) 0.0196(14) 0.0136(13) C28 0.0313(13) 0.0306(13) 0.0421(15) 0.0049(11) 0.0132(11) 0.0133(11) C29 0.0340(14) 0.0231(12) 0.0522(17) -0.0077(11) -0.0151(12) 0.0144(11) C30 0.065(2) 0.0381(16) 0.0569(19) -0.0116(14) -0.0293(16) 0.0294(15) C31 0.087(3) 0.059(2) 0.097(3) -0.030(2) -0.063(3) 0.041(2) C32 0.058(2) 0.050(2) 0.153(5) -0.035(3) -0.066(3) 0.029(2) C33 0.0362(17) 0.0357(17) 0.149(4) -0.004(2) -0.018(2) 0.0109(14) C34 0.0303(14) 0.0341(15) 0.082(2) 0.0005(15) -0.0107(14) 0.0108(12) C35 0.0468(15) 0.0239(12) 0.0250(12) 0.0044(9) 0.0029(11) 0.0153(11) C36 0.064(8) 0.030(4) 0.039(6) 0.010(4) 0.021(4) 0.025(5) C37 0.078(8) 0.043(5) 0.029(6) 0.010(4) 0.029(5) 0.031(6) C38 0.071(10) 0.054(6) 0.055(12) 0.035(7) 0.048(9) 0.042(7) C39 0.120(9) 0.035(4) 0.076(8) 0.030(5) 0.066(7) 0.036(6) C40 0.085(6) 0.031(4) 0.047(5) 0.017(3) 0.043(5) 0.031(4) C41 0.0336(13) 0.0254(12) 0.0250(12) 0.0001(9) 0.0051(10) 0.0138(10) C42 0.0361(14) 0.0267(13) 0.075(2) 0.0073(13) 0.0076(14) 0.0143(12) C43 0.0410(17) 0.0428(18) 0.113(3) 0.0217(18) 0.0235(18) 0.0261(14) C44 0.066(2) 0.0510(18) 0.0509(18) 0.0053(14) 0.0158(15) 0.0422(17) C45 0.069(2) 0.0443(19) 0.104(3) -0.0346(19) -0.011(2) 0.0338(18) C46 0.0421(17) 0.0356(16) 0.105(3) -0.0266(17) -0.0076(17) 0.0180(14) C47 0.0379(14) 0.0333(13) 0.0354(14) -0.0115(11) -0.0080(11) 0.0202(12) C48 0.0513(17) 0.0655(19) 0.0291(14) -0.0054(13) -0.0016(12) 0.0378(15) C49 0.086(3) 0.120(3) 0.0323(17) -0.0151(19) -0.0086(17) 0.078(3) C50 0.106(3) 0.129(4) 0.062(3) -0.055(3) -0.049(2) 0.095(3) C51 0.073(3) 0.072(3) 0.100(3) -0.051(2) -0.055(2) 0.040(2) C52 0.0511(18) 0.0407(17) 0.071(2) -0.0162(15) -0.0248(16) 0.0136(14) C53 0.0319(13) 0.0192(11) 0.0382(14) 0.0037(10) 0.0112(11) 0.0062(10) C54 0.0447(16) 0.0496(17) 0.0454(17) 0.0197(13) 0.0193(13) 0.0235(14) C55 0.071(2) 0.067(2) 0.055(2) 0.0346(17) 0.0286(17) 0.0340(18) C56 0.064(2) 0.0510(18) 0.068(2) 0.0250(16) 0.0414(18) 0.0241(16) C57 0.0433(16) 0.0430(17) 0.088(3) 0.0241(16) 0.0377(17) 0.0187(14) C58 0.0374(15) 0.0350(15) 0.070(2) 0.0196(14) 0.0208(14) 0.0149(12) C36A 0.039(5) 0.050(6) 0.037(6) 0.019(4) 0.012(4) 0.018(4) C37A 0.067(8) 0.073(9) 0.040(7) 0.021(5) 0.022(5) 0.038(7) C38A 0.090(14) 0.047(6) 0.040(7) 0.025(5) 0.008(9) 0.032(9) C39A 0.208(15) 0.054(7) 0.064(7) 0.037(6) 0.065(10) 0.084(10) C40A 0.163(11) 0.051(6) 0.053(6) 0.028(4) 0.053(7) 0.073(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 H1 1.60(3) . ? Ru1 H2 1.69(2) . ? Ru1 C1 1.897(3) . ? Ru1 P3 2.2973(6) . ? Ru1 P1 2.3283(6) . ? Ru1 P2 2.3950(6) . ? P1 C2 1.834(2) . ? P1 C23 1.838(2) . ? P1 C17 1.851(2) . ? P2 C35 1.835(2) . ? P2 C29 1.837(2) . ? P2 C12 1.857(2) . ? P3 C53 1.836(2) . ? P3 C47 1.851(2) . ? P3 C41 1.856(2) . ? O1 C1 1.148(3) . ? O2 C14 1.385(3) . ? O2 C13 1.387(3) . ? C2 C14 1.389(3) . ? C2 C3 1.392(3) . ? C3 C4 1.395(3) . ? C4 C5 1.378(4) . ? C5 C6 1.391(3) . ? C6 C14 1.392(3) . ? C6 C7 1.526(3) . ? C7 C8 1.531(3) . ? C7 C15 1.535(3) . ? C7 C16 1.540(3) . ? C8 C9 1.390(3) . ? C8 C13 1.394(3) . ? C9 C10 1.385(4) . ? C10 C11 1.383(4) . ? C11 C12 1.400(3) . ? C12 C13 1.385(3) . ? C17 C22 1.385(4) . ? C17 C18 1.394(4) . ? C18 C19 1.392(4) . ? C19 C20 1.353(6) . ? C20 C21 1.395(6) . ? C21 C22 1.405(4) . ? C23 C24 1.377(4) . ? C23 C28 1.384(3) . ? C24 C25 1.385(4) . ? C25 C26 1.375(5) . ? C26 C27 1.363(4) . ? C27 C28 1.388(3) . ? C29 C34 1.385(4) . ? C29 C30 1.391(4) . ? C30 C31 1.387(5) . ? C31 C32 1.361(6) . ? C32 C33 1.381(6) . ? C33 C34 1.397(4) . ? C35 C36A 1.292(13) . ? C35 C40 1.382(9) . ? C35 C40A 1.419(10) . ? C35 C36 1.438(12) . ? C36 C37 1.385(19) . ? C37 C38 1.35(3) . ? C38 C39 1.37(3) . ? C39 C40 1.396(14) . ? C41 C42 1.372(3) . ? C41 C46 1.378(4) . ? C42 C43 1.385(4) . ? C43 C44 1.359(4) . ? C44 C45 1.362(4) . ? C45 C46 1.380(4) . ? C47 C48 1.375(4) . ? C47 C52 1.394(4) . ? C48 C49 1.387(4) . ? C49 C50 1.364(6) . ? C50 C51 1.369(6) . ? C51 C52 1.391(5) . ? C53 C54 1.382(4) . ? C53 C58 1.387(3) . ? C54 C55 1.387(4) . ? C55 C56 1.378(4) . ? C56 C57 1.373(4) . ? C57 C58 1.379(4) . ? C36A C37A 1.38(2) . ? C37A C38A 1.44(3) . ? C38A C39A 1.34(3) . ? C39A C40A 1.373(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1 Ru1 H2 87.9(12) . . ? H1 Ru1 C1 88.8(10) . . ? H2 Ru1 C1 176.2(8) . . ? H1 Ru1 P3 69.2(10) . . ? H2 Ru1 P3 79.8(7) . . ? C1 Ru1 P3 97.28(7) . . ? H1 Ru1 P1 80.6(10) . . ? H2 Ru1 P1 82.2(7) . . ? C1 Ru1 P1 99.13(8) . . ? P3 Ru1 P1 145.16(2) . . ? H1 Ru1 P2 176.4(10) . . ? H2 Ru1 P2 91.1(7) . . ? C1 Ru1 P2 92.00(8) . . ? P3 Ru1 P2 107.16(2) . . ? P1 Ru1 P2 102.76(2) . . ? C2 P1 C23 101.42(10) . . ? C2 P1 C17 100.77(11) . . ? C23 P1 C17 101.22(12) . . ? C2 P1 Ru1 117.41(7) . . ? C23 P1 Ru1 119.04(7) . . ? C17 P1 Ru1 114.15(8) . . ? C35 P2 C29 101.85(12) . . ? C35 P2 C12 101.73(10) . . ? C29 P2 C12 97.70(11) . . ? C35 P2 Ru1 119.90(8) . . ? C29 P2 Ru1 113.46(8) . . ? C12 P2 Ru1 118.73(8) . . ? C53 P3 C47 103.36(12) . . ? C53 P3 C41 101.68(11) . . ? C47 P3 C41 97.28(10) . . ? C53 P3 Ru1 112.35(8) . . ? C47 P3 Ru1 124.99(8) . . ? C41 P3 Ru1 113.94(8) . . ? C14 O2 C13 114.03(16) . . ? O1 C1 Ru1 178.1(2) . . ? C14 C2 C3 116.9(2) . . ? C14 C2 P1 116.24(17) . . ? C3 C2 P1 126.76(18) . . ? C2 C3 C4 120.1(2) . . ? C5 C4 C3 120.8(2) . . ? C4 C5 C6 121.3(2) . . ? C5 C6 C14 116.2(2) . . ? C5 C6 C7 126.4(2) . . ? C14 C6 C7 117.4(2) . . ? C6 C7 C8 106.85(18) . . ? C6 C7 C15 111.8(2) . . ? C8 C7 C15 112.1(2) . . ? C6 C7 C16 108.26(19) . . ? C8 C7 C16 109.1(2) . . ? C15 C7 C16 108.6(2) . . ? C9 C8 C13 116.7(2) . . ? C9 C8 C7 125.4(2) . . ? C13 C8 C7 117.9(2) . . ? C10 C9 C8 120.3(2) . . ? C11 C10 C9 121.1(2) . . ? C10 C11 C12 120.8(2) . . ? C13 C12 C11 115.9(2) . . ? C13 C12 P2 119.18(16) . . ? C11 C12 P2 124.81(18) . . ? C12 C13 O2 116.01(18) . . ? C12 C13 C8 125.0(2) . . ? O2 C13 C8 119.0(2) . . ? O2 C14 C2 115.49(18) . . ? O2 C14 C6 119.8(2) . . ? C2 C14 C6 124.7(2) . . ? C22 C17 C18 118.5(3) . . ? C22 C17 P1 119.4(2) . . ? C18 C17 P1 122.1(2) . . ? C19 C18 C17 120.5(4) . . ? C20 C19 C18 121.3(4) . . ? C19 C20 C21 119.3(3) . . ? C20 C21 C22 120.0(4) . . ? C17 C22 C21 120.4(4) . . ? C24 C23 C28 117.8(2) . . ? C24 C23 P1 118.5(2) . . ? C28 C23 P1 123.70(18) . . ? C23 C24 C25 120.9(3) . . ? C26 C25 C24 120.4(3) . . ? C27 C26 C25 119.7(3) . . ? C26 C27 C28 119.7(3) . . ? C23 C28 C27 121.4(2) . . ? C34 C29 C30 119.4(3) . . ? C34 C29 P2 116.0(2) . . ? C30 C29 P2 124.6(2) . . ? C31 C30 C29 119.6(4) . . ? C32 C31 C30 121.0(4) . . ? C31 C32 C33 120.2(3) . . ? C32 C33 C34 119.6(4) . . ? C29 C34 C33 120.1(3) . . ? C36A C35 C40 107.4(7) . . ? C36A C35 C40A 122.0(7) . . ? C40 C35 C40A 35.2(5) . . ? C36A C35 C36 23.5(5) . . ? C40 C35 C36 114.0(6) . . ? C40A C35 C36 113.5(6) . . ? C36A C35 P2 120.9(6) . . ? C40 C35 P2 125.3(4) . . ? C40A C35 P2 116.5(5) . . ? C36 C35 P2 120.6(5) . . ? C37 C36 C35 123.2(10) . . ? C38 C37 C36 117.9(14) . . ? C37 C38 C39 122(2) . . ? C38 C39 C40 118.7(15) . . ? C35 C40 C39 123.0(9) . . ? C42 C41 C46 117.3(2) . . ? C42 C41 P3 122.69(18) . . ? C46 C41 P3 120.0(2) . . ? C41 C42 C43 120.8(3) . . ? C44 C43 C42 121.1(3) . . ? C43 C44 C45 118.8(3) . . ? C44 C45 C46 120.4(3) . . ? C41 C46 C45 121.5(3) . . ? C48 C47 C52 118.4(3) . . ? C48 C47 P3 116.9(2) . . ? C52 C47 P3 124.4(2) . . ? C47 C48 C49 121.1(3) . . ? C50 C49 C48 120.2(4) . . ? C49 C50 C51 119.6(3) . . ? C50 C51 C52 120.7(4) . . ? C51 C52 C47 119.9(4) . . ? C54 C53 C58 118.0(2) . . ? C54 C53 P3 121.23(19) . . ? C58 C53 P3 120.3(2) . . ? C53 C54 C55 120.5(3) . . ? C56 C55 C54 120.4(3) . . ? C57 C56 C55 119.6(3) . . ? C56 C57 C58 119.7(3) . . ? C57 C58 C53 121.7(3) . . ? C35 C36A C37A 119.3(12) . . ? C36A C37A C38A 121.2(16) . . ? C39A C38A C37A 117(2) . . ? C38A C39A C40A 122.3(16) . . ? C39A C40A C35 118.1(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.466 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.087 #===END data_Compound_20_h07mkw4 _database_code_depnum_ccdc_archive 'CCDC 678478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H34 O3 P2 Ru' _chemical_formula_weight 737.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0620(2) _cell_length_b 10.6710(2) _cell_length_c 18.1510(4) _cell_angle_alpha 73.413(1) _cell_angle_beta 73.881(1) _cell_angle_gamma 73.441(1) _cell_volume 1749.00(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16400 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25664 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7924 _reflns_number_gt 5643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+2.3758P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7924 _refine_ls_number_parameters 435 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.76543(3) 0.56365(3) 0.727269(15) 0.02494(10) Uani 1 1 d D . . P1 P 0.87712(9) 0.73306(8) 0.63155(5) 0.0237(2) Uani 1 1 d . . . P2 P 0.86803(9) 0.52924(8) 0.83689(5) 0.02196(19) Uani 1 1 d . . . O1 O 0.5071(3) 0.7757(3) 0.77833(15) 0.0430(7) Uani 1 1 d . . . O2 O 0.6845(3) 0.4702(3) 0.60678(15) 0.0473(7) Uani 1 1 d . . . O3 O 0.8699(2) 0.8056(2) 0.77235(11) 0.0231(5) Uani 1 1 d . . . C1 C 0.5974(4) 0.6984(4) 0.7604(2) 0.0351(9) Uani 1 1 d . . . C2 C 0.7119(4) 0.5136(3) 0.6504(2) 0.0313(8) Uani 1 1 d . . . C3 C 0.8106(3) 0.9205(3) 0.72278(17) 0.0230(7) Uani 1 1 d . . . C4 C 0.8171(3) 0.9038(3) 0.64830(18) 0.0244(7) Uani 1 1 d . . . C5 C 0.7667(4) 1.0190(3) 0.59431(19) 0.0301(8) Uani 1 1 d . . . H5 H 0.7706 1.0138 0.5423 0.036 Uiso 1 1 calc R . . C6 C 0.7114(4) 1.1400(3) 0.6165(2) 0.0351(9) Uani 1 1 d . . . H6 H 0.6792 1.2178 0.5790 0.042 Uiso 1 1 calc R . . C7 C 0.7018(4) 1.1505(3) 0.69218(19) 0.0325(8) Uani 1 1 d . . . H7 H 0.6606 1.2346 0.7063 0.039 Uiso 1 1 calc R . . C8 C 0.7518(3) 1.0394(3) 0.74790(18) 0.0257(7) Uani 1 1 d . . . C9 C 0.7492(4) 1.0442(3) 0.83155(18) 0.0262(7) Uani 1 1 d . . . C10 C 0.7513(3) 0.9034(3) 0.88406(18) 0.0237(7) Uani 1 1 d . . . C11 C 0.7022(3) 0.8785(3) 0.96571(18) 0.0281(8) Uani 1 1 d . . . H11 H 0.6624 0.9516 0.9909 0.034 Uiso 1 1 calc R . . C12 C 0.7109(4) 0.7476(3) 1.01060(18) 0.0298(8) Uani 1 1 d . . . H12 H 0.6809 0.7323 1.0662 0.036 Uiso 1 1 calc R . . C13 C 0.7629(3) 0.6400(3) 0.97486(18) 0.0262(7) Uani 1 1 d . . . H13 H 0.7658 0.5514 1.0061 0.031 Uiso 1 1 calc R . . C14 C 0.8111(3) 0.6598(3) 0.89361(17) 0.0225(7) Uani 1 1 d . . . C15 C 0.8078(3) 0.7926(3) 0.85176(17) 0.0234(7) Uani 1 1 d . . . C16 C 0.6163(4) 1.1439(4) 0.8615(2) 0.0389(9) Uani 1 1 d . . . H16A H 0.5322 1.1211 0.8562 0.058 Uiso 1 1 calc R . . H16B H 0.6215 1.2347 0.8305 0.058 Uiso 1 1 calc R . . H16C H 0.6100 1.1398 0.9169 0.058 Uiso 1 1 calc R . . C17 C 0.8822(4) 1.0876(3) 0.8318(2) 0.0360(9) Uani 1 1 d . . . H17A H 0.8816 1.0892 0.8856 0.054 Uiso 1 1 calc R . . H17B H 0.8825 1.1774 0.7979 0.054 Uiso 1 1 calc R . . H17C H 0.9673 1.0239 0.8121 0.054 Uiso 1 1 calc R . . C18 C 0.8391(4) 0.7660(3) 0.53351(18) 0.0289(8) Uani 1 1 d . . . C19 C 0.9441(4) 0.7657(4) 0.46507(19) 0.0420(10) Uani 1 1 d . . . H19 H 1.0412 0.7442 0.4678 0.050 Uiso 1 1 calc R . . C20 C 0.9068(5) 0.7969(5) 0.3927(2) 0.0559(12) Uani 1 1 d . . . H20 H 0.9792 0.7964 0.3462 0.067 Uiso 1 1 calc R . . C21 C 0.7682(5) 0.8283(4) 0.3874(2) 0.0530(12) Uani 1 1 d . . . H21 H 0.7444 0.8495 0.3375 0.064 Uiso 1 1 calc R . . C22 C 0.6614(5) 0.8292(4) 0.4556(2) 0.0467(10) Uani 1 1 d . . . H22 H 0.5645 0.8521 0.4522 0.056 Uiso 1 1 calc R . . C23 C 0.6974(4) 0.7965(4) 0.5281(2) 0.0368(9) Uani 1 1 d . . . H23 H 0.6248 0.7949 0.5746 0.044 Uiso 1 1 calc R . . C24 C 1.0705(4) 0.7043(3) 0.61085(17) 0.0284(8) Uani 1 1 d . . . C25 C 1.1512(4) 0.5846(4) 0.5918(2) 0.0410(9) Uani 1 1 d . . . H25 H 1.1056 0.5189 0.5905 0.049 Uiso 1 1 calc R . . C26 C 1.2997(4) 0.5598(4) 0.5744(2) 0.0468(11) Uani 1 1 d . . . H26 H 1.3547 0.4785 0.5600 0.056 Uiso 1 1 calc R . . C27 C 1.3650(4) 0.6533(5) 0.5781(2) 0.0486(11) Uani 1 1 d . . . H27 H 1.4657 0.6364 0.5663 0.058 Uiso 1 1 calc R . . C28 C 1.2869(4) 0.7708(5) 0.5987(2) 0.0463(10) Uani 1 1 d . . . H28 H 1.3335 0.8342 0.6022 0.056 Uiso 1 1 calc R . . C29 C 1.1394(4) 0.7977(4) 0.61457(19) 0.0353(9) Uani 1 1 d . . . H29 H 1.0856 0.8800 0.6280 0.042 Uiso 1 1 calc R . . C30 C 0.8296(4) 0.3862(3) 0.91828(17) 0.0244(7) Uani 1 1 d . . . C31 C 0.9334(4) 0.2971(3) 0.95577(19) 0.0303(8) Uani 1 1 d . . . H31 H 1.0297 0.3035 0.9364 0.036 Uiso 1 1 calc R . . C32 C 0.8971(4) 0.1981(4) 1.0219(2) 0.0395(9) Uani 1 1 d . . . H32 H 0.9694 0.1357 1.0463 0.047 Uiso 1 1 calc R . . C33 C 0.7584(4) 0.1897(4) 1.0520(2) 0.0395(9) Uani 1 1 d . . . H33 H 0.7342 0.1232 1.0978 0.047 Uiso 1 1 calc R . . C34 C 0.6537(4) 0.2792(4) 1.0152(2) 0.0372(9) Uani 1 1 d . . . H34 H 0.5572 0.2742 1.0361 0.045 Uiso 1 1 calc R . . C35 C 0.6886(4) 0.3757(3) 0.94837(18) 0.0298(8) Uani 1 1 d . . . H35 H 0.6163 0.4351 0.9228 0.036 Uiso 1 1 calc R . . C36 C 1.0619(3) 0.4987(3) 0.81612(17) 0.0247(7) Uani 1 1 d . . . C37 C 1.1429(4) 0.3971(4) 0.7782(2) 0.0358(9) Uani 1 1 d . . . H37 H 1.0976 0.3439 0.7635 0.043 Uiso 1 1 calc R . . C38 C 1.2905(4) 0.3727(4) 0.7616(2) 0.0425(10) Uani 1 1 d . . . H38 H 1.3454 0.3023 0.7361 0.051 Uiso 1 1 calc R . . C39 C 1.3571(4) 0.4499(4) 0.7818(2) 0.0390(9) Uani 1 1 d . . . H39 H 1.4578 0.4338 0.7698 0.047 Uiso 1 1 calc R . . C40 C 1.2777(4) 0.5501(4) 0.8194(2) 0.0390(9) Uani 1 1 d . . . H40 H 1.3239 0.6032 0.8335 0.047 Uiso 1 1 calc R . . C41 C 1.1309(4) 0.5751(3) 0.8371(2) 0.0302(8) Uani 1 1 d . . . H41 H 1.0772 0.6446 0.8635 0.036 Uiso 1 1 calc R . . H1 H 0.699(3) 0.441(2) 0.7834(15) 0.034(9) Uiso 1 1 d D . . H2 H 0.895(2) 0.448(2) 0.6984(19) 0.046(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 0.02901(17) 0.02658(16) 0.02158(14) -0.00316(11) -0.00704(11) -0.01047(12) P1 0.0269(5) 0.0261(5) 0.0192(4) -0.0057(4) -0.0039(3) -0.0080(4) P2 0.0236(5) 0.0211(4) 0.0209(4) -0.0043(3) -0.0046(3) -0.0052(4) O1 0.0314(16) 0.0423(16) 0.0503(16) -0.0160(14) -0.0005(13) -0.0029(13) O2 0.071(2) 0.0406(16) 0.0430(15) -0.0079(13) -0.0295(14) -0.0168(15) O3 0.0269(12) 0.0224(11) 0.0174(10) -0.0041(9) -0.0041(9) -0.0024(10) C1 0.040(2) 0.046(2) 0.0267(18) 0.0026(17) -0.0094(17) -0.029(2) C2 0.036(2) 0.0283(19) 0.0295(18) -0.0018(16) -0.0123(16) -0.0072(16) C3 0.0210(17) 0.0251(17) 0.0226(16) -0.0028(14) -0.0041(13) -0.0076(14) C4 0.0250(18) 0.0260(17) 0.0229(16) -0.0034(14) -0.0037(13) -0.0101(15) C5 0.037(2) 0.0293(19) 0.0245(17) -0.0035(15) -0.0077(15) -0.0100(17) C6 0.042(2) 0.0271(19) 0.0327(19) 0.0029(16) -0.0170(17) -0.0035(17) C7 0.039(2) 0.0249(18) 0.0318(18) -0.0078(15) -0.0073(16) -0.0032(16) C8 0.0266(18) 0.0251(18) 0.0266(17) -0.0073(14) -0.0059(14) -0.0060(15) C9 0.035(2) 0.0206(17) 0.0233(16) -0.0040(14) -0.0064(14) -0.0070(15) C10 0.0242(18) 0.0222(17) 0.0258(16) -0.0077(14) -0.0062(13) -0.0037(14) C11 0.0273(19) 0.0293(18) 0.0272(17) -0.0121(15) -0.0055(14) -0.0003(15) C12 0.034(2) 0.0325(19) 0.0203(16) -0.0070(15) -0.0037(14) -0.0051(16) C13 0.0267(18) 0.0267(18) 0.0242(16) -0.0038(14) -0.0055(14) -0.0062(15) C14 0.0209(17) 0.0253(17) 0.0224(16) -0.0060(14) -0.0057(13) -0.0052(14) C15 0.0227(17) 0.0302(18) 0.0168(15) -0.0048(14) -0.0040(13) -0.0055(15) C16 0.049(2) 0.031(2) 0.0302(19) -0.0100(16) -0.0033(17) -0.0008(18) C17 0.052(2) 0.0286(19) 0.0317(19) -0.0036(16) -0.0126(17) -0.0149(18) C18 0.043(2) 0.0243(17) 0.0234(17) -0.0055(14) -0.0062(15) -0.0141(16) C19 0.047(2) 0.055(2) 0.0233(18) -0.0062(18) -0.0025(17) -0.018(2) C20 0.072(3) 0.077(3) 0.0230(19) -0.010(2) -0.007(2) -0.028(3) C21 0.081(4) 0.063(3) 0.027(2) -0.0013(19) -0.025(2) -0.030(3) C22 0.058(3) 0.051(2) 0.042(2) 0.004(2) -0.028(2) -0.026(2) C23 0.047(2) 0.041(2) 0.0279(18) -0.0005(16) -0.0111(17) -0.0223(19) C24 0.0274(19) 0.0330(19) 0.0192(16) -0.0018(14) -0.0020(14) -0.0052(16) C25 0.041(2) 0.037(2) 0.037(2) -0.0051(17) 0.0001(17) -0.0082(19) C26 0.037(2) 0.044(2) 0.038(2) 0.0016(19) 0.0020(18) 0.005(2) C27 0.029(2) 0.066(3) 0.037(2) 0.009(2) -0.0072(17) -0.010(2) C28 0.036(2) 0.068(3) 0.035(2) -0.003(2) -0.0070(17) -0.021(2) C29 0.030(2) 0.048(2) 0.0262(18) -0.0058(17) -0.0045(15) -0.0108(18) C30 0.033(2) 0.0217(17) 0.0217(16) -0.0050(14) -0.0085(14) -0.0086(15) C31 0.035(2) 0.0297(19) 0.0274(17) -0.0034(15) -0.0091(15) -0.0097(16) C32 0.050(3) 0.031(2) 0.035(2) -0.0008(17) -0.0190(18) -0.0029(18) C33 0.057(3) 0.035(2) 0.0258(18) 0.0028(16) -0.0080(18) -0.019(2) C34 0.041(2) 0.045(2) 0.0299(19) -0.0061(17) -0.0030(16) -0.0236(19) C35 0.032(2) 0.0316(19) 0.0263(17) -0.0032(15) -0.0072(15) -0.0101(16) C36 0.0245(18) 0.0286(18) 0.0193(15) -0.0017(14) -0.0053(13) -0.0065(15) C37 0.032(2) 0.045(2) 0.0354(19) -0.0200(17) -0.0094(16) -0.0036(18) C38 0.030(2) 0.055(3) 0.035(2) -0.0150(19) -0.0056(17) 0.0062(19) C39 0.025(2) 0.053(2) 0.0292(19) 0.0050(18) -0.0029(16) -0.0111(19) C40 0.034(2) 0.039(2) 0.044(2) 0.0021(18) -0.0113(17) -0.0154(18) C41 0.0261(19) 0.0272(18) 0.0367(19) -0.0046(15) -0.0093(15) -0.0052(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.878(4) . ? Ru1 C1 1.958(5) . ? Ru1 P2 2.3805(9) . ? Ru1 P1 2.4146(8) . ? Ru1 H1 1.598(5) . ? Ru1 H2 1.605(5) . ? P1 C24 1.828(3) . ? P1 C4 1.834(3) . ? P1 C18 1.839(3) . ? P2 C36 1.831(3) . ? P2 C14 1.835(3) . ? P2 C30 1.842(3) . ? O1 C1 1.083(4) . ? O2 C2 1.150(4) . ? O3 C15 1.386(3) . ? O3 C3 1.385(4) . ? C3 C8 1.386(4) . ? C3 C4 1.395(4) . ? C4 C5 1.401(4) . ? C5 C6 1.379(5) . ? C5 H5 0.9500 . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 C8 1.393(5) . ? C7 H7 0.9500 . ? C8 C9 1.526(4) . ? C9 C16 1.527(5) . ? C9 C10 1.530(4) . ? C9 C17 1.538(5) . ? C10 C15 1.376(4) . ? C10 C11 1.398(4) . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.392(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.389(5) . ? C18 C23 1.394(5) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.362(6) . ? C20 H20 0.9500 . ? C21 C22 1.396(6) . ? C21 H21 0.9500 . ? C22 C23 1.384(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.384(5) . ? C24 C29 1.391(5) . ? C25 C26 1.401(5) . ? C25 H25 0.9500 . ? C26 C27 1.367(6) . ? C26 H26 0.9500 . ? C27 C28 1.369(6) . ? C27 H27 0.9500 . ? C28 C29 1.391(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.384(5) . ? C30 C35 1.397(5) . ? C31 C32 1.394(5) . ? C31 H31 0.9500 . ? C32 C33 1.369(5) . ? C32 H32 0.9500 . ? C33 C34 1.386(5) . ? C33 H33 0.9500 . ? C34 C35 1.383(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.387(5) . ? C36 C41 1.392(5) . ? C37 C38 1.393(5) . ? C37 H37 0.9500 . ? C38 C39 1.373(5) . ? C38 H38 0.9500 . ? C39 C40 1.370(5) . ? C39 H39 0.9500 . ? C40 C41 1.384(5) . ? C40 H40 0.9500 . ? C41 H41 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 C2 Ru1 C1 101.92(15) . . ? C2 Ru1 P2 156.18(10) . . ? C1 Ru1 P2 95.98(10) . . ? C2 Ru1 P1 92.86(10) . . ? C1 Ru1 P1 91.89(10) . . ? P2 Ru1 P1 102.20(3) . . ? C2 Ru1 H1 82.1(12) . . ? C1 Ru1 H1 93.2(11) . . ? P2 Ru1 H1 81.3(12) . . ? P1 Ru1 H1 173.5(11) . . ? C2 Ru1 H2 74.2(13) . . ? C1 Ru1 H2 175.6(13) . . ? P2 Ru1 H2 87.2(12) . . ? P1 Ru1 H2 90.4(12) . . ? H1 Ru1 H2 84.3(16) . . ? C24 P1 C4 103.44(15) . . ? C24 P1 C18 103.05(15) . . ? C4 P1 C18 99.53(15) . . ? C24 P1 Ru1 118.29(11) . . ? C4 P1 Ru1 116.83(10) . . ? C18 P1 Ru1 113.20(11) . . ? C36 P2 C14 103.08(14) . . ? C36 P2 C30 102.99(15) . . ? C14 P2 C30 98.43(14) . . ? C36 P2 Ru1 115.95(10) . . ? C14 P2 Ru1 118.40(10) . . ? C30 P2 Ru1 115.39(10) . . ? C15 O3 C3 115.7(2) . . ? O1 C1 Ru1 177.7(3) . . ? O2 C2 Ru1 173.3(3) . . ? O3 C3 C8 120.7(3) . . ? O3 C3 C4 114.2(3) . . ? C8 C3 C4 125.0(3) . . ? C3 C4 C5 116.4(3) . . ? C3 C4 P1 117.9(2) . . ? C5 C4 P1 125.5(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C3 C8 C7 116.1(3) . . ? C3 C8 C9 120.0(3) . . ? C7 C8 C9 123.8(3) . . ? C8 C9 C16 109.8(3) . . ? C8 C9 C10 108.6(3) . . ? C16 C9 C10 110.7(3) . . ? C8 C9 C17 109.3(3) . . ? C16 C9 C17 109.7(3) . . ? C10 C9 C17 108.7(3) . . ? C15 C10 C11 116.3(3) . . ? C15 C10 C9 120.1(3) . . ? C11 C10 C9 123.5(3) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 116.4(3) . . ? C13 C14 P2 125.8(2) . . ? C15 C14 P2 117.7(2) . . ? C10 C15 O3 121.0(3) . . ? C10 C15 C14 125.0(3) . . ? O3 C15 C14 114.1(3) . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 H17A 109.5 . . ? C9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.9(3) . . ? C19 C18 P1 123.2(3) . . ? C23 C18 P1 117.8(2) . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.6(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 120.6(3) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C25 C24 C29 118.9(3) . . ? C25 C24 P1 118.8(3) . . ? C29 C24 P1 122.4(3) . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 120.2(4) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C35 118.8(3) . . ? C31 C30 P2 122.3(3) . . ? C35 C30 P2 118.6(2) . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.4(3) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C30 120.3(3) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C37 C36 C41 118.7(3) . . ? C37 C36 P2 119.4(3) . . ? C41 C36 P2 121.8(3) . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 120.3(4) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.9(4) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C40 C41 C36 120.1(3) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.510 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.090 #===END data_Compound_22_h07jmjw1 _database_code_depnum_ccdc_archive 'CCDC 678479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 N0 O4 P2 Ru' _chemical_formula_weight 841.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 10.7330(1) _cell_length_b 28.5420(2) _cell_length_c 13.0640(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.661(1) _cell_angle_gamma 90.00 _cell_volume 3975.03(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68308 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57366 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9072 _reflns_number_gt 7068 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+2.3773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9072 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.746414(17) 0.109587(6) 0.383399(14) 0.02596(7) Uani 1 1 d . . . P1 P 0.60574(5) 0.16716(2) 0.30038(4) 0.02490(13) Uani 1 1 d . . . P2 P 0.89791(5) 0.102014(19) 0.26322(4) 0.02502(13) Uani 1 1 d . . . O1 O 0.6291(2) 0.08974(8) 0.57997(16) 0.0628(6) Uani 1 1 d . . . O2 O 0.95409(18) 0.16285(7) 0.51585(14) 0.0483(5) Uani 1 1 d . . . O3 O 0.6414(3) 0.01503(9) 0.30633(19) 0.0812(8) Uani 1 1 d . . . O4 O 0.68375(13) 0.12586(5) 0.11845(11) 0.0244(3) Uani 1 1 d . . . C1 C 0.6698(3) 0.09816(9) 0.5048(2) 0.0398(6) Uani 1 1 d . . . C2 C 0.8744(2) 0.14397(9) 0.46637(18) 0.0336(5) Uani 1 1 d . . . C3 C 0.6789(3) 0.05077(9) 0.3322(2) 0.0424(6) Uani 1 1 d . . . C4 C 0.4906(2) 0.19122(9) 0.38044(18) 0.0323(5) Uani 1 1 d . . . C5 C 0.4191(2) 0.16030(11) 0.4309(2) 0.0461(7) Uani 1 1 d . . . H5 H 0.4289 0.1275 0.4233 0.055 Uiso 1 1 calc R . . C6 C 0.3318(3) 0.17795(15) 0.4935(2) 0.0620(9) Uani 1 1 d . . . H6 H 0.2821 0.1570 0.5281 0.074 Uiso 1 1 calc R . . C7 C 0.3184(3) 0.22568(14) 0.5047(2) 0.0619(9) Uani 1 1 d . . . H7 H 0.2606 0.2375 0.5482 0.074 Uiso 1 1 calc R . . C8 C 0.3869(3) 0.25593(12) 0.4540(2) 0.0540(8) Uani 1 1 d . . . H8 H 0.3764 0.2887 0.4617 0.065 Uiso 1 1 calc R . . C9 C 0.4724(2) 0.23913(10) 0.3911(2) 0.0394(6) Uani 1 1 d . . . H9 H 0.5189 0.2606 0.3549 0.047 Uiso 1 1 calc R . . C10 C 0.6756(2) 0.22092(7) 0.25677(17) 0.0261(5) Uani 1 1 d . . . C11 C 0.7708(2) 0.24173(8) 0.32205(19) 0.0321(5) Uani 1 1 d . . . H11 H 0.8023 0.2265 0.3844 0.039 Uiso 1 1 calc R . . C12 C 0.8203(2) 0.28432(9) 0.2974(2) 0.0367(6) Uani 1 1 d . . . H12 H 0.8841 0.2985 0.3436 0.044 Uiso 1 1 calc R . . C13 C 0.7779(2) 0.30635(9) 0.2063(2) 0.0379(6) Uani 1 1 d . . . H13 H 0.8121 0.3357 0.1895 0.045 Uiso 1 1 calc R . . C14 C 0.6855(3) 0.28553(9) 0.1399(2) 0.0471(7) Uani 1 1 d . . . H14 H 0.6566 0.3004 0.0765 0.057 Uiso 1 1 calc R . . C15 C 0.6341(3) 0.24285(9) 0.1648(2) 0.0392(6) Uani 1 1 d . . . H15 H 0.5702 0.2287 0.1184 0.047 Uiso 1 1 calc R . . C16 C 0.5537(2) 0.12677(7) 0.10729(17) 0.0252(5) Uani 1 1 d . . . C17 C 0.5003(2) 0.14897(8) 0.18618(17) 0.0266(5) Uani 1 1 d . . . C18 C 0.3695(2) 0.15338(8) 0.17341(19) 0.0322(5) Uani 1 1 d . . . H18 H 0.3284 0.1693 0.2238 0.039 Uiso 1 1 calc R . . C19 C 0.3002(2) 0.13455(9) 0.08723(19) 0.0346(6) Uani 1 1 d . . . H19 H 0.2117 0.1383 0.0787 0.042 Uiso 1 1 calc R . . C20 C 0.3568(2) 0.11046(8) 0.01330(19) 0.0323(5) Uani 1 1 d . . . H20 H 0.3067 0.0965 -0.0433 0.039 Uiso 1 1 calc R . . C21 C 0.4872(2) 0.10655(8) 0.02145(17) 0.0272(5) Uani 1 1 d . . . C22 C 0.5619(2) 0.08481(8) -0.05932(18) 0.0306(5) Uani 1 1 d . . . C23 C 0.6774(2) 0.06166(8) -0.00073(17) 0.0278(5) Uani 1 1 d . . . C24 C 0.7325(2) 0.01973(8) -0.02654(18) 0.0338(5) Uani 1 1 d . . . H24 H 0.6961 0.0024 -0.0846 0.041 Uiso 1 1 calc R . . C25 C 0.8392(2) 0.00300(8) 0.03103(19) 0.0353(5) Uani 1 1 d . . . H25 H 0.8749 -0.0257 0.0120 0.042 Uiso 1 1 calc R . . C26 C 0.8950(2) 0.02724(8) 0.11583(19) 0.0321(5) Uani 1 1 d . . . H26 H 0.9686 0.0151 0.1542 0.039 Uiso 1 1 calc R . . C27 C 0.8438(2) 0.06940(7) 0.14542(17) 0.0259(5) Uani 1 1 d . . . C28 C 0.7353(2) 0.08486(7) 0.08607(17) 0.0254(5) Uani 1 1 d . . . C29 C 0.6055(2) 0.12497(9) -0.12619(19) 0.0386(6) Uani 1 1 d . . . H29A H 0.6515 0.1483 -0.0816 0.058 Uiso 1 1 calc R . . H29B H 0.5321 0.1397 -0.1649 0.058 Uiso 1 1 calc R . . H29C H 0.6603 0.1123 -0.1744 0.058 Uiso 1 1 calc R . . C30 C 0.4843(3) 0.04977(10) -0.1294(2) 0.0421(6) Uani 1 1 d . . . H30A H 0.5346 0.0381 -0.1820 0.063 Uiso 1 1 calc R . . H30B H 0.4090 0.0654 -0.1630 0.063 Uiso 1 1 calc R . . H30C H 0.4596 0.0234 -0.0881 0.063 Uiso 1 1 calc R . . C31 C 1.0422(2) 0.07088(8) 0.31376(18) 0.0301(5) Uani 1 1 d . . . C32 C 1.0542(3) 0.05058(9) 0.4106(2) 0.0419(6) Uani 1 1 d . . . H32 H 0.9855 0.0512 0.4503 0.050 Uiso 1 1 calc R . . C33 C 1.1662(3) 0.02931(11) 0.4503(2) 0.0543(8) Uani 1 1 d . . . H33 H 1.1738 0.0155 0.5168 0.065 Uiso 1 1 calc R . . C34 C 1.2665(3) 0.02835(10) 0.3927(3) 0.0531(8) Uani 1 1 d . . . H34 H 1.3430 0.0139 0.4199 0.064 Uiso 1 1 calc R . . C35 C 1.2562(2) 0.04822(9) 0.2964(2) 0.0431(6) Uani 1 1 d . . . H35 H 1.3252 0.0474 0.2570 0.052 Uiso 1 1 calc R . . C36 C 1.1447(2) 0.06942(9) 0.2568(2) 0.0363(6) Uani 1 1 d . . . H36 H 1.1378 0.0831 0.1901 0.044 Uiso 1 1 calc R . . C37 C 0.9665(2) 0.15616(8) 0.21818(18) 0.0264(5) Uani 1 1 d . . . C38 C 1.0545(2) 0.17976(8) 0.28673(19) 0.0324(5) Uani 1 1 d . . . H38 H 1.0825 0.1661 0.3516 0.039 Uiso 1 1 calc R . . C39 C 1.1015(2) 0.22285(9) 0.2612(2) 0.0356(6) Uani 1 1 d . . . H39 H 1.1610 0.2385 0.3087 0.043 Uiso 1 1 calc R . . C40 C 1.0625(2) 0.24298(9) 0.1676(2) 0.0361(6) Uani 1 1 d . . . H40 H 1.0933 0.2729 0.1510 0.043 Uiso 1 1 calc R . . C41 C 0.9783(2) 0.21964(9) 0.0978(2) 0.0360(6) Uani 1 1 d . . . H41 H 0.9527 0.2332 0.0323 0.043 Uiso 1 1 calc R . . C42 C 0.9307(2) 0.17636(8) 0.12256(18) 0.0305(5) Uani 1 1 d . . . H42 H 0.8732 0.1605 0.0737 0.037 Uiso 1 1 calc R . . C43 C 1.1115(5) 0.10008(16) 0.6994(3) 0.0927(14) Uani 1 1 d . . . H43 H 1.1615 0.0977 0.6442 0.111 Uiso 1 1 calc R . . C44 C 1.1427(4) 0.13158(15) 0.7784(4) 0.0865(13) Uani 1 1 d . . . H44 H 1.2123 0.1521 0.7779 0.104 Uiso 1 1 calc R . . C45 C 1.0675(4) 0.13206(16) 0.8595(3) 0.0834(14) Uani 1 1 d . . . H45 H 1.0874 0.1529 0.9158 0.100 Uiso 1 1 calc R . . C46 C 0.9672(4) 0.10335(14) 0.8590(3) 0.0739(11) Uani 1 1 d . . . H46 H 0.9180 0.1040 0.9148 0.089 Uiso 1 1 calc R . . C47 C 0.9370(4) 0.07396(12) 0.7796(3) 0.0741(11) Uani 1 1 d . . . H47 H 0.8654 0.0544 0.7790 0.089 Uiso 1 1 calc R . . C48 C 1.0071(5) 0.07208(13) 0.7013(3) 0.0874(13) Uani 1 1 d . . . H48 H 0.9844 0.0510 0.6459 0.105 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 0.02964(11) 0.02417(10) 0.02431(10) 0.00034(7) 0.00411(7) -0.00064(7) P1 0.0235(3) 0.0253(3) 0.0261(3) -0.0021(2) 0.0040(2) -0.0012(2) P2 0.0250(3) 0.0242(3) 0.0257(3) 0.0000(2) 0.0025(2) 0.0003(2) O1 0.0932(17) 0.0572(13) 0.0439(12) 0.0036(10) 0.0335(12) -0.0080(12) O2 0.0486(11) 0.0551(12) 0.0392(11) -0.0119(9) -0.0028(9) -0.0070(9) O3 0.111(2) 0.0644(16) 0.0722(16) -0.0258(13) 0.0260(15) -0.0491(15) O4 0.0203(7) 0.0241(7) 0.0289(8) -0.0052(6) 0.0030(6) -0.0013(6) C1 0.0541(17) 0.0314(13) 0.0350(14) -0.0021(11) 0.0096(13) -0.0034(12) C2 0.0378(14) 0.0360(13) 0.0274(12) -0.0018(10) 0.0052(11) 0.0015(11) C3 0.0555(17) 0.0374(15) 0.0364(14) -0.0070(12) 0.0146(13) -0.0158(13) C4 0.0236(11) 0.0438(14) 0.0297(12) -0.0061(10) 0.0040(10) -0.0004(10) C5 0.0391(15) 0.0596(18) 0.0405(15) -0.0004(13) 0.0093(12) -0.0018(13) C6 0.0407(17) 0.102(3) 0.0471(18) 0.0055(18) 0.0195(14) -0.0059(17) C7 0.0386(17) 0.100(3) 0.0483(18) -0.0227(18) 0.0119(14) 0.0132(17) C8 0.0359(15) 0.070(2) 0.0552(18) -0.0291(16) 0.0008(14) 0.0126(14) C9 0.0309(13) 0.0447(15) 0.0421(15) -0.0133(12) 0.0024(11) 0.0057(11) C10 0.0252(11) 0.0236(11) 0.0296(12) -0.0020(9) 0.0040(9) 0.0023(9) C11 0.0296(12) 0.0310(12) 0.0343(13) 0.0014(10) -0.0021(10) -0.0004(10) C12 0.0318(13) 0.0307(13) 0.0468(15) -0.0041(11) 0.0019(11) -0.0052(10) C13 0.0475(15) 0.0275(12) 0.0403(14) -0.0003(11) 0.0120(12) -0.0070(11) C14 0.0688(19) 0.0354(14) 0.0352(14) 0.0091(12) -0.0026(13) -0.0056(13) C15 0.0451(15) 0.0339(13) 0.0363(14) 0.0017(11) -0.0049(12) -0.0062(11) C16 0.0225(11) 0.0223(10) 0.0306(12) 0.0014(9) 0.0028(9) -0.0032(9) C17 0.0250(11) 0.0257(11) 0.0287(12) 0.0001(9) 0.0018(9) -0.0037(9) C18 0.0266(12) 0.0359(13) 0.0348(13) -0.0004(10) 0.0062(10) -0.0011(10) C19 0.0219(11) 0.0438(15) 0.0374(13) 0.0026(11) 0.0007(10) -0.0048(10) C20 0.0285(12) 0.0346(13) 0.0323(13) 0.0006(10) -0.0029(10) -0.0100(10) C21 0.0278(11) 0.0262(11) 0.0271(11) 0.0007(9) 0.0013(9) -0.0053(9) C22 0.0326(12) 0.0319(13) 0.0271(12) -0.0046(10) 0.0023(10) -0.0056(10) C23 0.0299(12) 0.0282(12) 0.0262(11) -0.0025(9) 0.0067(9) -0.0055(9) C24 0.0409(14) 0.0312(12) 0.0304(13) -0.0090(10) 0.0089(11) -0.0073(10) C25 0.0392(14) 0.0269(12) 0.0415(14) -0.0072(11) 0.0114(11) 0.0010(10) C26 0.0317(13) 0.0288(12) 0.0369(13) 0.0011(10) 0.0079(10) 0.0031(10) C27 0.0285(11) 0.0239(11) 0.0260(11) -0.0017(9) 0.0069(9) -0.0027(9) C28 0.0267(11) 0.0229(11) 0.0278(11) -0.0018(9) 0.0085(9) -0.0043(9) C29 0.0429(15) 0.0442(15) 0.0293(13) 0.0053(11) 0.0064(11) -0.0026(12) C30 0.0444(15) 0.0465(16) 0.0338(14) -0.0130(12) -0.0024(12) -0.0070(12) C31 0.0306(12) 0.0231(11) 0.0362(13) -0.0006(10) 0.0024(10) 0.0025(9) C32 0.0416(15) 0.0391(15) 0.0448(15) 0.0085(12) 0.0044(12) 0.0041(12) C33 0.0522(18) 0.0521(18) 0.0563(19) 0.0186(15) -0.0040(15) 0.0132(14) C34 0.0420(16) 0.0410(16) 0.073(2) 0.0041(15) -0.0080(15) 0.0119(12) C35 0.0332(14) 0.0342(14) 0.0619(18) -0.0060(13) 0.0052(13) 0.0028(11) C36 0.0330(13) 0.0333(13) 0.0420(14) -0.0013(11) 0.0025(11) 0.0026(10) C37 0.0231(11) 0.0248(11) 0.0319(12) -0.0001(9) 0.0065(9) 0.0022(9) C38 0.0270(12) 0.0364(13) 0.0334(13) -0.0017(10) 0.0016(10) -0.0002(10) C39 0.0276(12) 0.0345(13) 0.0447(15) -0.0070(11) 0.0034(11) -0.0048(10) C40 0.0311(13) 0.0295(12) 0.0495(15) 0.0005(11) 0.0117(12) -0.0041(10) C41 0.0338(13) 0.0367(13) 0.0382(14) 0.0078(11) 0.0074(11) -0.0001(11) C42 0.0258(12) 0.0332(12) 0.0325(12) 0.0004(10) 0.0037(10) -0.0033(9) C43 0.143(4) 0.080(3) 0.059(2) 0.015(2) 0.030(3) 0.012(3) C44 0.083(3) 0.078(3) 0.091(3) 0.023(2) -0.022(3) 0.014(2) C45 0.087(3) 0.092(3) 0.063(2) -0.018(2) -0.026(2) 0.057(3) C46 0.074(3) 0.081(3) 0.065(2) 0.006(2) 0.000(2) 0.037(2) C47 0.106(3) 0.048(2) 0.069(2) 0.0141(18) 0.012(2) 0.0198(19) C48 0.156(4) 0.045(2) 0.060(2) 0.0070(17) 0.013(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.897(3) . ? Ru1 C3 1.918(3) . ? Ru1 C2 1.918(3) . ? Ru1 P2 2.3975(6) . ? Ru1 P1 2.4034(6) . ? P1 C10 1.828(2) . ? P1 C17 1.840(2) . ? P1 C4 1.842(2) . ? P2 C27 1.834(2) . ? P2 C37 1.838(2) . ? P2 C31 1.840(2) . ? O1 C1 1.146(3) . ? O2 C2 1.145(3) . ? O3 C3 1.134(3) . ? O4 C28 1.382(3) . ? O4 C16 1.387(2) . ? C4 C5 1.386(4) . ? C4 C9 1.391(4) . ? C5 C6 1.406(4) . ? C5 H5 0.9500 . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 C8 1.355(5) . ? C7 H7 0.9500 . ? C8 C9 1.387(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.382(3) . ? C10 C11 1.386(3) . ? C11 C12 1.380(3) . ? C11 H11 0.9500 . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 C14 1.375(4) . ? C13 H13 0.9500 . ? C14 C15 1.391(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.383(3) . ? C16 C17 1.389(3) . ? C17 C18 1.400(3) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.382(4) . ? C19 H19 0.9500 . ? C20 C21 1.396(3) . ? C20 H20 0.9500 . ? C21 C22 1.529(3) . ? C22 C23 1.529(3) . ? C22 C30 1.535(3) . ? C22 C29 1.546(3) . ? C23 C24 1.394(3) . ? C23 C28 1.395(3) . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 H25 0.9500 . ? C26 C27 1.396(3) . ? C26 H26 0.9500 . ? C27 C28 1.394(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.384(3) . ? C31 C36 1.398(3) . ? C32 C33 1.392(4) . ? C32 H32 0.9500 . ? C33 C34 1.384(4) . ? C33 H33 0.9500 . ? C34 C35 1.372(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.389(3) . ? C37 C38 1.397(3) . ? C38 C39 1.384(3) . ? C38 H38 0.9500 . ? C39 C40 1.372(4) . ? C39 H39 0.9500 . ? C40 C41 1.379(4) . ? C40 H40 0.9500 . ? C41 C42 1.389(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.378(6) . ? C43 C44 1.380(6) . ? C43 H43 0.9500 . ? C44 C45 1.405(6) . ? C44 H44 0.9500 . ? C45 C46 1.352(6) . ? C45 H45 0.9500 . ? C46 C47 1.344(5) . ? C46 H46 0.9500 . ? C47 C48 1.339(6) . ? C47 H47 0.9500 . ? C48 H48 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 C3 87.62(11) . . ? C1 Ru1 C2 88.10(11) . . ? C3 Ru1 C2 149.51(12) . . ? C1 Ru1 P2 157.57(9) . . ? C3 Ru1 P2 87.13(8) . . ? C2 Ru1 P2 85.44(7) . . ? C1 Ru1 P1 100.63(9) . . ? C3 Ru1 P1 104.41(9) . . ? C2 Ru1 P1 106.05(8) . . ? P2 Ru1 P1 101.80(2) . . ? C10 P1 C17 102.72(10) . . ? C10 P1 C4 100.99(11) . . ? C17 P1 C4 100.11(10) . . ? C10 P1 Ru1 117.10(7) . . ? C17 P1 Ru1 117.92(7) . . ? C4 P1 Ru1 115.24(8) . . ? C27 P2 C37 104.94(10) . . ? C27 P2 C31 103.14(10) . . ? C37 P2 C31 99.74(10) . . ? C27 P2 Ru1 114.99(7) . . ? C37 P2 Ru1 117.46(7) . . ? C31 P2 Ru1 114.52(8) . . ? C28 O4 C16 114.69(16) . . ? O1 C1 Ru1 176.3(3) . . ? O2 C2 Ru1 177.1(2) . . ? O3 C3 Ru1 176.6(3) . . ? C5 C4 C9 119.1(2) . . ? C5 C4 P1 118.6(2) . . ? C9 C4 P1 122.32(19) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.2(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C4 120.6(3) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C15 C10 C11 118.8(2) . . ? C15 C10 P1 123.26(18) . . ? C11 C10 P1 117.90(17) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 119.4(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.5(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 120.2(2) . . ? C10 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C21 C16 O4 119.70(19) . . ? C21 C16 C17 125.0(2) . . ? O4 C16 C17 115.32(18) . . ? C16 C17 C18 116.6(2) . . ? C16 C17 P1 117.54(16) . . ? C18 C17 P1 125.83(18) . . ? C19 C18 C17 119.9(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 121.6(2) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 120.3(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 116.5(2) . . ? C16 C21 C22 117.80(19) . . ? C20 C21 C22 125.5(2) . . ? C21 C22 C23 106.82(18) . . ? C21 C22 C30 112.61(19) . . ? C23 C22 C30 111.7(2) . . ? C21 C22 C29 107.82(19) . . ? C23 C22 C29 108.83(19) . . ? C30 C22 C29 108.9(2) . . ? C24 C23 C28 116.3(2) . . ? C24 C23 C22 126.3(2) . . ? C28 C23 C22 117.4(2) . . ? C25 C24 C23 120.9(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 121.3(2) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 120.3(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 116.7(2) . . ? C28 C27 P2 117.96(16) . . ? C26 C27 P2 124.97(18) . . ? O4 C28 C27 115.87(19) . . ? O4 C28 C23 119.62(19) . . ? C27 C28 C23 124.5(2) . . ? C22 C29 H29A 109.5 . . ? C22 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C22 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C22 C30 H30A 109.5 . . ? C22 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C22 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 118.6(2) . . ? C32 C31 P2 121.02(19) . . ? C36 C31 P2 120.29(18) . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119.9(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.8(3) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 120.8(3) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C42 C37 C38 118.2(2) . . ? C42 C37 P2 123.90(17) . . ? C38 C37 P2 117.80(17) . . ? C39 C38 C37 120.8(2) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.3(2) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 119.8(2) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.4(2) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.5(2) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C48 C43 C44 119.5(4) . . ? C48 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 117.3(4) . . ? C43 C44 H44 121.3 . . ? C45 C44 H44 121.3 . . ? C46 C45 C44 121.1(4) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C47 C46 C45 120.2(4) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 120.5(4) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C43 121.3(4) . . ? C47 C48 H48 119.3 . . ? C43 C48 H48 119.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.454 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.086 #===END