#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/00/04/5000401.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_5000401 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H60 O P2 Ru Si2' _chemical_formula_weight 619.94 _chemical_melting_point ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8495 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1269 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4432 _reflns_number_observed 2823 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] where P = 1.00000Fo^2^ + 0.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4432 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_obs 0.0462 _refine_ls_wR_factor_all 0.0916 _refine_ls_wR_factor_obs 0.0737 _refine_ls_goodness_of_fit_all 0.956 _refine_ls_goodness_of_fit_obs 1.002 _refine_ls_restrained_S_all 0.956 _refine_ls_restrained_S_obs 1.002 _refine_ls_shift/esd_max -1.455 _refine_ls_shift/esd_mean 0.029 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.57111(5) 0.37226(3) 0.21678(3) 0.0136(2) Uani 1 d . . P2 P 0.3695(2) 0.43475(10) 0.16193(10) 0.0154(4) Uani 1 d . . C3 C 0.2529(7) 0.4192(5) 0.2140(5) 0.021(2) Uani 1 d . . C4 C 0.2714(6) 0.4220(4) 0.0549(4) 0.020(2) Uani 1 d . . C5 C 0.3281(8) 0.4632(5) -0.0023(5) 0.027(2) Uani 1 d . . C6 C 0.1352(7) 0.4454(5) 0.0380(5) 0.030(2) Uani 1 d . . C7 C 0.2705(7) 0.3388(4) 0.0354(5) 0.021(2) Uani 1 d . . C8 C 0.4012(6) 0.5376(4) 0.1790(4) 0.020(2) Uani 1 d . . C9 C 0.5019(8) 0.5620(5) 0.1422(5) 0.028(2) Uani 1 d . . C10 C 0.4524(7) 0.5470(5) 0.2700(4) 0.023(2) Uani 1 d . . C11 C 0.2875(8) 0.5888(5) 0.1479(5) 0.030(2) Uani 1 d . . P12 P 0.7896(2) 0.35082(10) 0.29079(10) 0.0170(5) Uani 1 d . . C13 C 0.8300(8) 0.2942(5) 0.3804(5) 0.024(2) Uani 1 d . . C14 C 0.8543(6) 0.4446(4) 0.3346(4) 0.021(2) Uani 1 d . . C15 C 0.7987(8) 0.5041(4) 0.2709(5) 0.028(2) Uani 1 d . . C16 C 0.9971(7) 0.4515(5) 0.3623(6) 0.035(2) Uani 1 d . . C17 C 0.8092(8) 0.4594(5) 0.4057(5) 0.030(2) Uani 1 d . . C18 C 0.8973(6) 0.3113(4) 0.2358(4) 0.021(2) Uani 1 d . . C19 C 1.0264(7) 0.2869(5) 0.2906(5) 0.028(2) Uani 1 d . . C20 C 0.9107(7) 0.3658(6) 0.1740(5) 0.030(2) Uani 1 d . . C21 C 0.8314(9) 0.2411(5) 0.1930(5) 0.027(2) Uani 1 d . . Si22 Si 0.4976(2) 0.24803(11) 0.21389(11) 0.0177(5) Uani 1 d . . C23 C 0.4914(9) 0.1921(5) 0.1230(5) 0.025(2) Uani 1 d . . C24 C 0.3359(7) 0.2375(5) 0.2256(5) 0.022(2) Uani 1 d . . C25 C 0.5887(9) 0.1852(5) 0.2963(5) 0.028(2) Uani 1 d . . C26 C 0.5348(5) 0.3692(4) 0.3230(4) 0.015(2) Uani 1 d . . C27 C 0.5076(6) 0.3641(4) 0.3841(4) 0.021(2) Uani 1 d . . Si28 Si 0.4666(2) 0.34695(11) 0.47438(11) 0.0224(5) Uani 1 d . . C29 C 0.3502(10) 0.4154(6) 0.4861(7) 0.044(3) Uani 1 d . . C30 C 0.6109(9) 0.3539(5) 0.5596(5) 0.031(2) Uani 1 d . . C31 C 0.3965(11) 0.2533(6) 0.4688(6) 0.046(3) Uani 1 d . . C32 C 0.5919(6) 0.3611(4) 0.1178(4) 0.018(2) Uani 1 d . . O33 O 0.5989(4) 0.3483(3) 0.0539(3) 0.0231(12) Uani 1 d . . H34 H 0.1943(59) 0.4669(36) 0.2030(35) 0.026(19) Uiso 1 d . . H35 H 0.2102(71) 0.3753(48) 0.1924(44) 0.064(28) Uiso 1 d . . H36 H 0.2990(60) 0.4125(35) 0.2669(40) 0.027(21) Uiso 1 d . . H37 H 0.4247(63) 0.4448(35) 0.0122(36) 0.034(20) Uiso 1 d . . H38 H 0.2967(49) 0.4489(30) -0.0493(32) 0.000(17) Uiso 1 d . . H39 H 0.3063(60) 0.5191(39) 0.0012(37) 0.034(21) Uiso 1 d . . H40 H 0.0909(70) 0.4061(41) 0.0652(43) 0.061(27) Uiso 1 d . . H41 H 0.0969(55) 0.4424(33) -0.0155(37) 0.015(19) Uiso 1 d . . H42 H 0.1137(61) 0.4964(39) 0.0407(38) 0.026(22) Uiso 1 d . . H43 H 0.2234(52) 0.3284(31) -0.0146(34) 0.010(18) Uiso 1 d . . H44 H 0.2345(51) 0.3075(30) 0.0674(31) 0.004(16) Uiso 1 d . . H45 H 0.3676(62) 0.3201(33) 0.0393(34) 0.026(19) Uiso 1 d . . H46 H 0.5697(70) 0.5165(43) 0.1438(41) 0.059(25) Uiso 1 d . . H47 H 0.5416(54) 0.6000(31) 0.1630(33) 0.004(18) Uiso 1 d . . H48 H 0.4653(63) 0.5795(37) 0.0845(41) 0.042(22) Uiso 1 d . . H49 H 0.5323(59) 0.5112(34) 0.2957(35) 0.026(18) Uiso 1 d . . H50 H 0.3769(49) 0.5409(28) 0.2948(29) 0.003(15) Uiso 1 d . . H51 H 0.4760(51) 0.5977(32) 0.2775(33) 0.014(18) Uiso 1 d . . H52 H 0.3183(52) 0.6401(34) 0.1647(31) 0.013(17) Uiso 1 d . . H53 H 0.2222(55) 0.5733(32) 0.1651(33) 0.012(18) Uiso 1 d . . H54 H 0.2523(49) 0.5921(28) 0.0841(34) 0.006(15) Uiso 1 d . . H55 H 0.9127(64) 0.3019(35) 0.4168(37) 0.028(21) Uiso 1 d . . H56 H 0.8410(62) 0.2443(39) 0.3682(39) 0.036(23) Uiso 1 d . . H57 H 0.7757(54) 0.2991(31) 0.4035(32) 0.000(18) Uiso 1 d . . H58 H 0.8271(60) 0.4903(35) 0.2195(37) 0.035(21) Uiso 1 d . . H59 H 0.7097(58) 0.5045(31) 0.2582(33) 0.014(18) Uiso 1 d . . H60 H 0.8370(55) 0.5628(36) 0.3000(35) 0.030(19) Uiso 1 d . . H61 H 1.0023(50) 0.4989(32) 0.3783(32) 0.000(17) Uiso 1 d . . H62 H 1.0362(50) 0.4126(31) 0.4000(31) 0.000(15) Uiso 1 d . . H63 H 1.0414(69) 0.4445(41) 0.3182(43) 0.058(27) Uiso 1 d . . H64 H 0.7245(61) 0.4542(32) 0.4008(34) 0.019(20) Uiso 1 d . . H65 H 0.8574(58) 0.4271(35) 0.4512(37) 0.026(21) Uiso 1 d . . H66 H 0.8302(50) 0.5057(31) 0.4227(31) 0.000(16) Uiso 1 d . . H67 H 1.0734(48) 0.3302(30) 0.3244(30) 0.000(15) Uiso 1 d . . H68 H 1.0142(60) 0.2485(38) 0.3284(38) 0.031(22) Uiso 1 d . . H69 H 1.0661(60) 0.2646(35) 0.2651(36) 0.017(21) Uiso 1 d . . H70 H 0.9497(64) 0.3427(37) 0.1414(39) 0.035(23) Uiso 1 d . . H71 H 0.8240(60) 0.3818(35) 0.1268(36) 0.032(19) Uiso 1 d . . H72 H 0.9590(66) 0.4043(40) 0.1871(41) 0.031(24) Uiso 1 d . . H73 H 0.8279(51) 0.2050(31) 0.2368(34) 0.008(16) Uiso 1 d . . H74 H 0.7694(72) 0.2509(43) 0.1626(45) 0.044(30) Uiso 1 d . . H75 H 0.8886(67) 0.2184(38) 0.1630(40) 0.045(23) Uiso 1 d . . H76 H 0.5697(60) 0.1807(32) 0.1185(33) 0.014(19) Uiso 1 d . . H77 H 0.4349(58) 0.2194(34) 0.0697(37) 0.029(19) Uiso 1 d . . H78 H 0.4619(69) 0.1488(43) 0.1276(43) 0.051(30) Uiso 1 d . . H79 H 0.3157(55) 0.1888(35) 0.2327(34) 0.015(19) Uiso 1 d . . H80 H 0.2701(55) 0.2576(31) 0.1838(35) 0.012(17) Uiso 1 d . . H81 H 0.3406(76) 0.2587(46) 0.2782(49) 0.075(31) Uiso 1 d . . H82 H 0.6636(78) 0.1762(43) 0.2939(47) 0.058(32) Uiso 1 d . . H83 H 0.5953(59) 0.2047(36) 0.3409(37) 0.018(21) Uiso 1 d . . H84 H 0.5482(72) 0.1342(51) 0.2939(44) 0.073(28) Uiso 1 d . . H85 H 0.2809(72) 0.4196(42) 0.4406(45) 0.056(30) Uiso 1 d . . H86 H 0.3867(53) 0.4573(32) 0.4934(33) 0.000(19) Uiso 1 d . . H87 H 0.3200(80) 0.4096(45) 0.5299(51) 0.071(33) Uiso 1 d . . H88 H 0.6412(57) 0.4061(38) 0.5732(35) 0.022(19) Uiso 1 d . . H89 H 0.6778(63) 0.3225(37) 0.5583(37) 0.028(22) Uiso 1 d . . H90 H 0.6032(73) 0.3344(44) 0.5973(45) 0.047(30) Uiso 1 d . . H91 H 0.4472(60) 0.2144(36) 0.4598(36) 0.021(21) Uiso 1 d . . H92 H 0.3267(83) 0.2510(48) 0.4254(52) 0.077(37) Uiso 1 d . . H93 H 0.3710(57) 0.2475(34) 0.5168(38) 0.025(19) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0121(3) 0.0160(3) 0.0132(3) 0.0007(3) 0.0047(2) 0.0005(3) P2 0.0114(10) 0.0194(11) 0.0158(10) 0.0003(8) 0.0049(8) 0.0014(8) C3 0.014(4) 0.032(5) 0.016(5) 0.004(4) 0.005(4) 0.001(4) C4 0.019(4) 0.028(5) 0.011(4) 0.000(3) 0.003(3) 0.013(3) C5 0.027(5) 0.035(6) 0.018(5) 0.001(4) 0.006(4) 0.001(4) C6 0.021(5) 0.040(6) 0.025(5) 0.003(4) -0.001(4) 0.005(4) C7 0.021(5) 0.024(5) 0.014(4) -0.002(4) 0.000(4) -0.009(4) C8 0.020(4) 0.014(4) 0.030(4) 0.001(3) 0.015(4) 0.003(3) C9 0.025(5) 0.026(5) 0.028(5) 0.001(4) -0.001(4) -0.003(4) C10 0.012(5) 0.030(5) 0.026(5) -0.003(4) 0.008(4) -0.003(4) C11 0.028(5) 0.025(5) 0.040(6) 0.000(4) 0.014(4) 0.001(4) P12 0.0146(10) 0.0205(11) 0.0151(10) 0.0004(8) 0.0037(8) 0.0002(8) C13 0.018(5) 0.032(6) 0.025(5) -0.001(4) 0.009(4) -0.001(4) C14 0.010(4) 0.026(4) 0.028(4) -0.005(4) 0.007(3) -0.001(3) C15 0.025(5) 0.021(5) 0.041(5) 0.001(4) 0.012(4) 0.000(4) C16 0.023(5) 0.032(6) 0.049(6) -0.003(5) 0.009(5) -0.001(4) C17 0.017(5) 0.035(6) 0.035(6) -0.015(5) 0.003(4) -0.009(4) C18 0.008(4) 0.023(4) 0.028(4) 0.003(4) 0.000(3) 0.005(3) C19 0.013(5) 0.036(6) 0.033(5) -0.009(5) 0.004(4) 0.009(4) C20 0.014(5) 0.050(6) 0.033(5) 0.001(5) 0.017(4) 0.000(5) C21 0.021(5) 0.031(5) 0.027(5) 0.000(4) 0.008(4) 0.006(4) Si22 0.0182(11) 0.0180(11) 0.0167(11) 0.0027(9) 0.0051(9) -0.0010(9) C23 0.025(6) 0.025(5) 0.023(5) 0.002(4) 0.006(4) 0.010(4) C24 0.029(5) 0.021(5) 0.017(5) 0.002(4) 0.005(4) -0.006(4) C25 0.033(6) 0.026(5) 0.024(5) -0.001(4) 0.006(4) -0.002(4) C26 0.009(4) 0.019(4) 0.014(4) 0.000(4) -0.002(3) 0.001(3) C27 0.011(4) 0.028(5) 0.019(4) -0.003(4) -0.002(3) -0.005(3) Si28 0.0242(12) 0.0290(13) 0.0162(11) 0.0018(9) 0.0097(9) 0.0021(9) C29 0.038(7) 0.043(7) 0.058(8) 0.004(6) 0.026(6) 0.012(5) C30 0.044(6) 0.029(6) 0.019(5) 0.002(4) 0.008(4) 0.012(5) C31 0.063(8) 0.048(7) 0.031(6) 0.006(5) 0.019(6) -0.006(6) C32 0.017(4) 0.016(4) 0.020(4) 0.001(4) 0.006(3) -0.006(3) O33 0.023(3) 0.032(3) 0.015(3) 0.001(2) 0.006(2) 0.003(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 C32 1.852(7) . ? Ru1 C26 2.048(6) . ? Ru1 Si22 2.382(2) . ? Ru1 P12 2.418(2) . ? Ru1 P2 2.435(2) . ? P2 C3 1.837(7) . ? P2 C4 1.890(6) . ? P2 C8 1.895(7) . ? C4 C6 1.516(10) . ? C4 C7 1.540(9) . ? C4 C5 1.544(10) . ? C8 C11 1.529(10) . ? C8 C9 1.530(10) . ? C8 C10 1.546(9) . ? P12 C13 1.824(8) . ? P12 C14 1.908(7) . ? P12 C18 1.906(7) . ? C14 C16 1.521(10) . ? C14 C17 1.520(10) . ? C14 C15 1.544(10) . ? C18 C20 1.515(10) . ? C18 C19 1.533(9) . ? C18 C21 1.541(10) . ? Si22 C25 1.881(8) . ? Si22 C24 1.890(8) . ? Si22 C23 1.886(8) . ? C26 C27 1.216(8) . ? C27 Si28 1.824(7) . ? Si28 C29 1.851(9) . ? Si28 C31 1.852(10) . ? Si28 C30 1.842(9) . ? C32 O33 1.183(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C32 Ru1 C26 171.3(3) . . ? C32 Ru1 Si22 91.2(2) . . ? C26 Ru1 Si22 80.2(2) . . ? C32 Ru1 P12 95.5(2) . . ? C26 Ru1 P12 87.1(2) . . ? Si22 Ru1 P12 98.29(6) . . ? C32 Ru1 P2 92.4(2) . . ? C26 Ru1 P2 87.6(2) . . ? Si22 Ru1 P2 99.06(7) . . ? P12 Ru1 P2 160.73(6) . . ? C3 P2 C4 101.9(3) . . ? C3 P2 C8 101.3(3) . . ? C4 P2 C8 107.5(3) . . ? C3 P2 Ru1 116.1(3) . . ? C4 P2 Ru1 121.5(2) . . ? C8 P2 Ru1 106.6(2) . . ? C6 C4 C7 106.9(7) . . ? C6 C4 C5 109.0(6) . . ? C7 C4 C5 107.3(6) . . ? C6 C4 P2 113.6(5) . . ? C7 C4 P2 107.8(5) . . ? C5 C4 P2 111.9(5) . . ? C11 C8 C9 108.1(6) . . ? C11 C8 C10 107.9(6) . . ? C9 C8 C10 109.3(6) . . ? C11 C8 P2 116.2(5) . . ? C9 C8 P2 109.8(5) . . ? C10 C8 P2 105.4(5) . . ? C13 P12 C14 100.4(4) . . ? C13 P12 C18 102.2(4) . . ? C14 P12 C18 108.7(3) . . ? C13 P12 Ru1 119.9(3) . . ? C14 P12 Ru1 105.7(2) . . ? C18 P12 Ru1 118.2(2) . . ? C16 C14 C17 107.5(6) . . ? C16 C14 C15 108.9(6) . . ? C17 C14 C15 109.0(6) . . ? C16 C14 P12 115.5(5) . . ? C17 C14 P12 108.2(5) . . ? C15 C14 P12 107.6(5) . . ? C20 C18 C19 111.2(6) . . ? C20 C18 C21 108.4(7) . . ? C19 C18 C21 106.8(6) . . ? C20 C18 P12 110.3(5) . . ? C19 C18 P12 113.6(5) . . ? C21 C18 P12 106.2(5) . . ? C25 Si22 C24 99.2(4) . . ? C25 Si22 C23 102.2(4) . . ? C24 Si22 C23 104.8(4) . . ? C25 Si22 Ru1 116.8(3) . . ? C24 Si22 Ru1 115.2(3) . . ? C23 Si22 Ru1 116.3(3) . . ? C27 C26 Ru1 176.0(6) . . ? C26 C27 Si28 174.6(7) . . ? C27 Si28 C29 111.2(4) . . ? C27 Si28 C31 108.9(4) . . ? C29 Si28 C31 108.4(5) . . ? C27 Si28 C30 108.4(4) . . ? C29 Si28 C30 109.2(5) . . ? C31 Si28 C30 110.7(5) . . ? O33 C32 Ru1 174.0(6) . . ? _refine_diff_density_max 0.386 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.095 _cod_database_code 5000401