#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:18:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179747 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/43/7004372.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_7004372
loop_
_publ_author_name
'Gutsulyak, Dmitry V.'
'Osipov, Alexandr L.'
'Kuzmina, Lyudmila G.'
'Howard, Judith A. K.'
'Nikonov, Georgii I.'
_publ_section_title
;
 Unexpected effect of the ring on the extent of Si⋯H interligand
 interactions in half-sandwich silyl hydrides of ruthenium
;
_journal_issue                   47
_journal_name_full               'Dalton Transactions'
_journal_page_first              6843
_journal_page_last               6850
_journal_paper_doi               10.1039/b806447d
_journal_year                    2008
_chemical_formula_moiety         'C25 H28 Cl P Ru Si'
_chemical_formula_sum            'C25 H28 Cl P Ru Si'
_chemical_formula_weight         524.05
_chemical_name_common
;(cyclopentadienyl)(triphenylphosphine)(dimethylchlorosilyl)
ruthenium dihydride
;
_chemical_name_systematic
;(cyclopentadienyl)(triphenylphosphine)(dimethylchlorosilyl)
ruthenium dihydride
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.7570(10)
_cell_angle_beta                 86.0050(10)
_cell_angle_gamma                82.2760(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7357(2)
_cell_length_b                   11.5961(2)
_cell_length_c                   11.9794(2)
_cell_measurement_reflns_used    5340
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.506
_cell_measurement_theta_min      2.811
_cell_volume                     1153.85(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART-6K'
_diffrn_measurement_method       ω
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11526
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7198
_exptl_absorpt_correction_T_min  0.6753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0263P)²+0.5628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                5783
_reflns_number_total             6037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b806447d.txt
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004372
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.320714(11) 0.833635(8) 0.297149(8) 0.01443(4) Uani 1 1 d . . .
P1 P 0.40831(4) 0.71435(3) 0.17855(3) 0.01331(7) Uani 1 1 d . . .
Si1 Si 0.11340(4) 0.74350(3) 0.40846(3) 0.01578(7) Uani 1 1 d . . .
Cl1 Cl -0.08207(4) 0.87939(3) 0.40171(3) 0.02653(8) Uani 1 1 d . . .
C1 C 0.2787(2) 0.98291(14) 0.38430(14) 0.0285(3) Uani 1 1 d . . .
H1A H 0.1943 0.9924 0.4430 0.034 Uiso 1 1 calc R . .
C2 C 0.4308(2) 0.92401(14) 0.40870(14) 0.0290(3) Uani 1 1 d . . .
H2A H 0.4713 0.8836 0.4880 0.035 Uiso 1 1 calc R . .
C3 C 0.51794(18) 0.93807(13) 0.30274(15) 0.0266(3) Uani 1 1 d . . .
H3A H 0.6304 0.9100 0.2941 0.032 Uiso 1 1 calc R . .
C4 C 0.41949(19) 1.00893(13) 0.21117(14) 0.0251(3) Uani 1 1 d . . .
H4A H 0.4509 1.0383 0.1271 0.030 Uiso 1 1 calc R . .
C5 C 0.27322(19) 1.03626(13) 0.26181(14) 0.0257(3) Uani 1 1 d . . .
H5A H 0.1830 1.0885 0.2195 0.031 Uiso 1 1 calc R . .
C6 C 0.02066(18) 0.62567(13) 0.36833(13) 0.0235(3) Uani 1 1 d . . .
H6A H -0.0628 0.5997 0.4251 0.035 Uiso 1 1 calc R . .
H6B H 0.0979 0.5561 0.3681 0.035 Uiso 1 1 calc R . .
H6C H -0.0218 0.6593 0.2907 0.035 Uiso 1 1 calc R . .
C7 C 0.14472(17) 0.68974(14) 0.57154(12) 0.0230(3) Uani 1 1 d . . .
H7A H 0.0539 0.6535 0.6116 0.034 Uiso 1 1 calc R . .
H7B H 0.1602 0.7587 0.5999 0.034 Uiso 1 1 calc R . .
H7C H 0.2361 0.6293 0.5870 0.034 Uiso 1 1 calc R . .
C8 C 0.33627(15) 0.76372(11) 0.02967(11) 0.0149(2) Uani 1 1 d . . .
C9 C 0.22876(15) 0.86655(12) -0.00369(12) 0.0170(2) Uani 1 1 d . . .
H9A H 0.1906 0.9092 0.0516 0.020 Uiso 1 1 calc R . .
C10 C 0.17673(16) 0.90742(12) -0.11714(12) 0.0197(3) Uani 1 1 d . . .
H10A H 0.1041 0.9779 -0.1390 0.024 Uiso 1 1 calc R . .
C11 C 0.23125(18) 0.84507(12) -0.19803(12) 0.0215(3) Uani 1 1 d . . .
H11A H 0.1941 0.8716 -0.2748 0.026 Uiso 1 1 calc R . .
C12 C 0.34049(18) 0.74342(13) -0.16659(12) 0.0220(3) Uani 1 1 d . . .
H12A H 0.3786 0.7012 -0.2222 0.026 Uiso 1 1 calc R . .
C13 C 0.39378(16) 0.70370(12) -0.05393(12) 0.0190(2) Uani 1 1 d . . .
H13A H 0.4698 0.6353 -0.0334 0.023 Uiso 1 1 calc R . .
C14 C 0.61612(15) 0.69654(11) 0.13953(11) 0.0157(2) Uani 1 1 d . . .
C15 C 0.68733(16) 0.80141(12) 0.09058(13) 0.0206(3) Uani 1 1 d . . .
H15A H 0.6321 0.8783 0.0885 0.025 Uiso 1 1 calc R . .
C16 C 0.83759(16) 0.79412(13) 0.04508(13) 0.0229(3) Uani 1 1 d . . .
H16A H 0.8840 0.8660 0.0115 0.027 Uiso 1 1 calc R . .
C17 C 0.92064(16) 0.68250(13) 0.04819(13) 0.0223(3) Uani 1 1 d . . .
H17A H 1.0227 0.6779 0.0153 0.027 Uiso 1 1 calc R . .
C18 C 0.85315(16) 0.57762(13) 0.09987(14) 0.0230(3) Uani 1 1 d . . .
H18A H 0.9104 0.5008 0.1046 0.028 Uiso 1 1 calc R . .
C19 C 0.70172(16) 0.58477(12) 0.14476(13) 0.0207(3) Uani 1 1 d . . .
H19A H 0.6563 0.5126 0.1794 0.025 Uiso 1 1 calc R . .
C20 C 0.36911(15) 0.55632(11) 0.23434(11) 0.0154(2) Uani 1 1 d . . .
C21 C 0.42148(16) 0.49194(12) 0.34529(12) 0.0195(3) Uani 1 1 d . . .
H21A H 0.4815 0.5290 0.3855 0.023 Uiso 1 1 calc R . .
C22 C 0.38696(18) 0.37498(12) 0.39714(13) 0.0230(3) Uani 1 1 d . . .
H22A H 0.4223 0.3330 0.4726 0.028 Uiso 1 1 calc R . .
C23 C 0.30057(18) 0.31928(12) 0.33843(13) 0.0240(3) Uani 1 1 d . . .
H23A H 0.2752 0.2398 0.3742 0.029 Uiso 1 1 calc R . .
C24 C 0.25195(17) 0.38058(12) 0.22757(13) 0.0222(3) Uani 1 1 d . . .
H24A H 0.1950 0.3421 0.1866 0.027 Uiso 1 1 calc R . .
C25 C 0.28592(16) 0.49858(12) 0.17540(12) 0.0180(2) Uani 1 1 d . . .
H25A H 0.2521 0.5396 0.0993 0.022 Uiso 1 1 calc R . .
H1 H 0.355(2) 0.7106(18) 0.3826(17) 0.032(5) Uiso 1 1 d . . .
H2 H 0.172(2) 0.8252(18) 0.2392(18) 0.034(5) Uiso 1 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'
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'
Cl Cl 0.1484 0.1585 '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
C1 Ru1 C2 36.92(6) . . ?
C1 Ru1 C3 61.72(6) . . ?
C2 Ru1 C3 36.68(6) . . ?
C1 Ru1 C5 37.01(6) . . ?
C2 Ru1 C5 61.30(6) . . ?
C3 Ru1 C5 61.40(6) . . ?
C1 Ru1 C4 61.54(6) . . ?
C2 Ru1 C4 61.32(6) . . ?
C3 Ru1 C4 37.06(6) . . ?
C5 Ru1 C4 36.43(6) . . ?
C1 Ru1 P1 164.66(4) . . ?
C2 Ru1 P1 135.43(5) . . ?
C3 Ru1 P1 104.96(4) . . ?
C5 Ru1 P1 131.50(4) . . ?
C4 Ru1 P1 103.36(4) . . ?
C1 Ru1 Si1 89.43(4) . . ?
C2 Ru1 Si1 106.75(5) . . ?
C3 Ru1 Si1 143.35(4) . . ?
C5 Ru1 Si1 109.46(4) . . ?
C4 Ru1 Si1 145.87(4) . . ?
P1 Ru1 Si1 105.760(12) . . ?
C1 Ru1 H1 112.5(8) . . ?
C2 Ru1 H1 91.9(8) . . ?
C3 Ru1 H1 106.6(8) . . ?
C5 Ru1 H1 149.4(8) . . ?
C4 Ru1 H1 143.3(8) . . ?
P1 Ru1 H1 77.5(8) . . ?
Si1 Ru1 H1 61.9(8) . . ?
C1 Ru1 H2 109.6(8) . . ?
C2 Ru1 H2 146.4(8) . . ?
C3 Ru1 H2 148.7(8) . . ?
C5 Ru1 H2 93.1(8) . . ?
C4 Ru1 H2 111.7(8) . . ?
P1 Ru1 H2 77.5(8) . . ?
Si1 Ru1 H2 59.0(8) . . ?
H1 Ru1 H2 104.4(11) . . ?
C20 P1 C14 101.89(6) . . ?
C20 P1 C8 104.77(6) . . ?
C14 P1 C8 97.57(6) . . ?
C20 P1 Ru1 114.56(4) . . ?
C14 P1 Ru1 119.10(4) . . ?
C8 P1 Ru1 116.42(4) . . ?
C6 Si1 C7 107.60(7) . . ?
C6 Si1 Cl1 100.17(5) . . ?
C7 Si1 Cl1 100.76(5) . . ?
C6 Si1 Ru1 121.87(5) . . ?
C7 Si1 Ru1 114.36(5) . . ?
Cl1 Si1 Ru1 109.091(18) . . ?
C2 C1 C5 107.43(14) . . ?
C2 C1 Ru1 71.83(8) . . ?
C5 C1 Ru1 72.09(8) . . ?
C2 C1 H1A 126.1 . . ?
C5 C1 H1A 126.1 . . ?
Ru1 C1 H1A 126.1 . . ?
C3 C2 C1 108.65(14) . . ?
C3 C2 Ru1 71.83(8) . . ?
C1 C2 Ru1 71.25(8) . . ?
C3 C2 H2A 125.6 . . ?
C1 C2 H2A 125.6 . . ?
Ru1 C2 H2A 125.6 . . ?
C2 C3 C4 107.59(14) . . ?
C2 C3 Ru1 71.49(8) . . ?
C4 C3 Ru1 71.91(8) . . ?
C2 C3 H3A 126.1 . . ?
C4 C3 H3A 126.1 . . ?
Ru1 C3 H3A 126.1 . . ?
C5 C4 C3 107.83(14) . . ?
C5 C4 Ru1 71.48(8) . . ?
C3 C4 Ru1 71.04(8) . . ?
C5 C4 H4A 126.0 . . ?
C3 C4 H4A 126.0 . . ?
Ru1 C4 H4A 126.0 . . ?
C4 C5 C1 108.47(14) . . ?
C4 C5 Ru1 72.09(8) . . ?
C1 C5 Ru1 70.90(8) . . ?
C4 C5 H5A 125.7 . . ?
C1 C5 H5A 125.7 . . ?
Ru1 C5 H5A 125.7 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 118.64(12) . . ?
C9 C8 P1 120.08(10) . . ?
C13 C8 P1 121.19(10) . . ?
C10 C9 C8 120.82(12) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C11 C10 C9 119.89(13) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 119.96(13) . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C13 C12 C11 120.09(13) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C8 120.56(13) . . ?
C12 C13 H13A 119.7 . . ?
C8 C13 H13A 119.7 . . ?
C19 C14 C15 118.36(12) . . ?
C19 C14 P1 123.26(10) . . ?
C15 C14 P1 118.02(10) . . ?
C16 C15 C14 120.69(13) . . ?
C16 C15 H15A 119.7 . . ?
C14 C15 H15A 119.7 . . ?
C15 C16 C17 120.50(13) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C16 C17 C18 119.38(13) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C17 C18 C19 120.20(13) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C18 C19 C14 120.82(12) . . ?
C18 C19 H19A 119.6 . . ?
C14 C19 H19A 119.6 . . ?
C25 C20 C21 118.40(12) . . ?
C25 C20 P1 124.06(10) . . ?
C21 C20 P1 117.48(9) . . ?
C22 C21 C20 121.02(13) . . ?
C22 C21 H21A 119.5 . . ?
C20 C21 H21A 119.5 . . ?
C21 C22 C23 120.00(13) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C24 C23 C22 119.52(13) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C25 120.58(13) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C20 C25 C24 120.43(13) . . ?
C20 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
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 2.2378(14) . ?
Ru1 C2 2.2454(14) . ?
Ru1 C3 2.2499(14) . ?
Ru1 C5 2.2535(14) . ?
Ru1 C4 2.2614(14) . ?
Ru1 P1 2.2762(3) . ?
Ru1 Si1 2.3544(4) . ?
Ru1 H1 1.51(2) . ?
Ru1 H2 1.54(2) . ?
P1 C20 1.8368(13) . ?
P1 C14 1.8416(13) . ?
P1 C8 1.8420(13) . ?
Si1 C6 1.8638(14) . ?
Si1 C7 1.9046(14) . ?
Si1 Cl1 2.1518(5) . ?
C1 C2 1.419(2) . ?
C1 C5 1.426(2) . ?
C1 H1A 1.0000 . ?
C2 C3 1.414(2) . ?
C2 H2A 1.0000 . ?
C3 C4 1.434(2) . ?
C3 H3A 1.0000 . ?
C4 C5 1.411(2) . ?
C4 H4A 1.0000 . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.3958(18) . ?
C8 C13 1.4020(18) . ?
C9 C10 1.3951(19) . ?
C9 H9A 0.9500 . ?
C10 C11 1.387(2) . ?
C10 H10A 0.9500 . ?
C11 C12 1.393(2) . ?
C11 H11A 0.9500 . ?
C12 C13 1.3900(19) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C19 1.3942(18) . ?
C14 C15 1.4012(18) . ?
C15 C16 1.3869(19) . ?
C15 H15A 0.9500 . ?
C16 C17 1.388(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.389(2) . ?
C17 H17A 0.9500 . ?
C18 C19 1.394(2) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 C25 1.3935(17) . ?
C20 C21 1.4040(18) . ?
C21 C22 1.3888(19) . ?
C21 H21A 0.9500 . ?
C22 C23 1.393(2) . ?
C22 H22A 0.9500 . ?
C23 C24 1.385(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.3985(18) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
