#------------------------------------------------------------------------------
#$Date: 2016-02-03 16:44:42 +0200 (Wed, 03 Feb 2016) $
#$Revision: 175475 $
#$URL: svn://www.crystallography.net/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
loop_
_publ_author_name
'Huang, Dejian'
'Heyn, Richard H.'
'Bollinger, John C.'
'Caulton, Kenneth G.'
_publ_section_title
;
 Oxidative Addition of a Si--C(sp) Bond to Ruthenium: Synthesis and
 Reactivity of Ru(SiMe₃)(C⋮ CSiMe₃)(CO)(PtBu₂Me)₂}
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              292
_journal_page_last               293
_journal_paper_doi               10.1021/om9609776
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C27 H60 O P2 Ru Si2'
_chemical_formula_weight         619.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.168(2)
_cell_length_b                   18.043(4)
_cell_length_c                   17.746(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3400.5(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.1269
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8495
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_F_000             1328
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00005(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.956
_refine_ls_goodness_of_fit_obs   1.002
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_restrained_S_obs      1.002
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_obs          0.0462
_refine_ls_shift/esd_max         -1.455
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_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^
;
_refine_ls_wR_factor_all         0.0916
_refine_ls_wR_factor_obs         0.0737
_reflns_number_observed          2823
_reflns_number_total             4432
_reflns_observed_criterion       >2sigma(I)
_cod_database_code               5000401
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'
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_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'
Si Si 0.0817 0.0704 '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'
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) . . ?
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) . ?
