#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/60/4116022.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_4116022
loop_
_publ_author_name
'Isabelle Atheaux'
'Bruno Donnadieu'
'V. Rodriguez'
'Sylviane Sabo-Etienne'
'Bruno Chaudret'
'Khansaa Hussein'
'Jean-Claude Barthelat'
_publ_section_title
;
 A Unique Coordination of SiH4: Isolation, Characterization, and
 Theoretical Study of (PR3)2H2Ru(SiH4)RuH2(PR3)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5664
_journal_page_last               5665
_journal_paper_doi               10.1021/ja000223p
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C36 H80 P4 Ru2 Si'
_chemical_formula_weight         433.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.025(15)
_cell_angle_beta                 98.066(15)
_cell_angle_gamma                89.960(15)
_cell_formula_units_Z            8
_cell_length_a                   19.588(2)
_cell_length_b                   12.1805(15)
_cell_length_c                   19.823(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      51.9
_cell_measurement_theta_min      4.1
_cell_volume                     4682.8(10)
_computing_cell_refinement
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_data_collection
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_data_reduction
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_computing_molecular_graphics
;
Zsolnai,L.(1997). ZORTEP.Molecular Graphics 
Program.University of Heidelberg, Germany.
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Altomare, A., Cascarano, G., Giacovazzo G., 
Guagliardi A., Burla M.C., Polidori, G.  & Camalli, M. (1994) SIR92 - a 
program for automatic solution of crystal structures by direct methods.
 J. Appl. Cryst. (27), 435
;
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany
;
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16605
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.28
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+0.8989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                2849
_reflns_number_total             3287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000223p.cif
_cod_data_source_block           C36H80SiP4Ru2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4682.7(10)
_cod_original_formula_sum        C36H80SiP4Ru2
_cod_database_code               4116022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.070420(10) 0.177706(14) 0.673564(9) 0.01891(9) Uani 1 1 d .
P1 P 0.01133(3) 0.28194(5) 0.58690(3) 0.02272(16) Uani 1 1 d .
P2 P 0.15983(3) 0.06839(5) 0.72412(3) 0.02167(15) Uani 1 1 d .
Si1 Si 0.0000 0.17865(7) 0.7500 0.0183(2) Uani 1 2 d S
C1 C -0.00583(14) 0.42990(19) 0.60492(13) 0.0305(6) Uani 1 1 d .
C2 C 0.05246(17) 0.2976(2) 0.50789(14) 0.0378(7) Uani 1 1 d .
C3 C -0.07753(15) 0.2330(2) 0.55529(14) 0.0331(6) Uani 1 1 d .
C4 C 0.23791(14) 0.0568(2) 0.67937(14) 0.0315(6) Uani 1 1 d .
C5 C 0.14026(13) -0.08026(19) 0.73575(13) 0.0272(6) Uani 1 1 d .
C6 C 0.19539(14) 0.1058(2) 0.81328(13) 0.0306(6) Uani 1 1 d .
C11 C 0.05615(18) 0.4845(2) 0.64668(18) 0.0473(8) Uani 1 1 d .
H11A H 0.0976 0.4697 0.6257 0.071 Uiso 1 1 calc R
H11B H 0.0622 0.4551 0.6931 0.071 Uiso 1 1 calc R
H11C H 0.0485 0.5640 0.6481 0.071 Uiso 1 1 calc R
C12 C -0.06816(17) 0.4467(2) 0.64162(16) 0.0422(7) Uani 1 1 d .
H12A H -0.1102 0.4285 0.6108 0.063 Uiso 1 1 calc R
H12B H -0.0701 0.5235 0.6560 0.063 Uiso 1 1 calc R
H12C H -0.0643 0.3989 0.6817 0.063 Uiso 1 1 calc R
C21 C 0.1216(2) 0.3519(3) 0.51896(18) 0.0564(9) Uani 1 1 d .
H21A H 0.1167 0.4268 0.5358 0.085 Uiso 1 1 calc R
H21B H 0.1406 0.3545 0.4758 0.085 Uiso 1 1 calc R
H21C H 0.1527 0.3101 0.5525 0.085 Uiso 1 1 calc R
C22 C 0.0586(2) 0.1890(3) 0.47054(16) 0.0525(9) Uani 1 1 d .
H22A H 0.0125 0.1587 0.4564 0.079 Uiso 1 1 calc R
H22B H 0.0858 0.1370 0.5010 0.079 Uiso 1 1 calc R
H22C H 0.0814 0.2017 0.4303 0.079 Uiso 1 1 calc R
C31 C -0.11550(18) 0.2973(3) 0.49471(16) 0.0485(8) Uani 1 1 d .
H31A H -0.1122 0.3762 0.5045 0.073 Uiso 1 1 calc R
H31B H -0.1641 0.2754 0.4872 0.073 Uiso 1 1 calc R
H31C H -0.0944 0.2815 0.4538 0.073 Uiso 1 1 calc R
C32 C -0.08392(17) 0.1100(2) 0.54116(14) 0.0414(7) Uani 1 1 d .
H32A H -0.0567 0.0696 0.5784 0.062 Uiso 1 1 calc R
H32B H -0.0667 0.0933 0.4982 0.062 Uiso 1 1 calc R
H32C H -0.1324 0.0881 0.5378 0.062 Uiso 1 1 calc R
C41 C 0.27906(18) 0.1632(2) 0.6814(2) 0.0521(9) Uani 1 1 d .
H41A H 0.3005 0.1777 0.7282 0.078 Uiso 1 1 calc R
H41B H 0.2482 0.2239 0.6654 0.078 Uiso 1 1 calc R
H41C H 0.3150 0.1562 0.6518 0.078 Uiso 1 1 calc R
C42 C 0.22197(17) 0.0189(3) 0.60597(16) 0.0488(8) Uani 1 1 d .
H42A H 0.2017 -0.0548 0.6046 0.073 Uiso 1 1 calc R
H42B H 0.2646 0.0169 0.5854 0.073 Uiso 1 1 calc R
H42C H 0.1893 0.0699 0.5805 0.073 Uiso 1 1 calc R
C51 C 0.09853(18) -0.1304(2) 0.67302(15) 0.0405(7) Uani 1 1 d .
H51A H 0.1230 -0.1202 0.6336 0.061 Uiso 1 1 calc R
H51B H 0.0534 -0.0944 0.6643 0.061 Uiso 1 1 calc R
H51C H 0.0922 -0.2090 0.6806 0.061 Uiso 1 1 calc R
C52 C 0.10189(17) -0.1003(2) 0.79637(15) 0.0388(7) Uani 1 1 d .
H52A H 0.1323 -0.0835 0.8387 0.058 Uiso 1 1 calc R
H52B H 0.0876 -0.1774 0.7968 0.058 Uiso 1 1 calc R
H52C H 0.0611 -0.0529 0.7927 0.058 Uiso 1 1 calc R
C61 C 0.25644(17) 0.0367(3) 0.84558(17) 0.0512(8) Uani 1 1 d .
H61A H 0.2453 -0.0413 0.8393 0.077 Uiso 1 1 calc R
H61B H 0.2661 0.0532 0.8944 0.077 Uiso 1 1 calc R
H61C H 0.2971 0.0541 0.8238 0.077 Uiso 1 1 calc R
C62 C 0.21270(15) 0.2279(2) 0.82432(15) 0.0369(6) Uani 1 1 d .
H62A H 0.1769 0.2725 0.7978 0.055 Uiso 1 1 calc R
H62B H 0.2573 0.2434 0.8094 0.055 Uiso 1 1 calc R
H62C H 0.2149 0.2457 0.8728 0.055 Uiso 1 1 calc R
H1 H 0.0836(14) 0.110(2) 0.6141(13) 0.028(7) Uiso 1 1 d .
H2 H 0.1284(15) 0.251(2) 0.6571(14) 0.038(7) Uiso 1 1 d .
H3 H 0.0091(16) 0.094(2) 0.6844(15) 0.047(8) Uiso 1 1 d .
H4 H 0.0671(14) 0.263(2) 0.7355(13) 0.033(7) 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'
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
Si1 Ru1 P1 102.34(2) . .
Si1 Ru1 P2 102.43(2) . .
P1 Ru1 P2 155.18(2) . .
Si1 Ru1 H1 138.2(10) . .
P1 Ru1 H1 80.8(10) . .
P2 Ru1 H1 79.6(10) . .
Si1 Ru1 H2 135.2(10) . .
P1 Ru1 H2 80.0(11) . .
P2 Ru1 H2 83.7(11) . .
H1 Ru1 H2 86.6(15) . .
Si1 Ru1 H3 50.1(10) . .
P1 Ru1 H3 98.2(11) . .
P2 Ru1 H3 96.3(11) . .
H1 Ru1 H3 88.2(14) . .
H2 Ru1 H3 174.6(14) . .
Si1 Ru1 H4 51.3(10) . .
P1 Ru1 H4 98.2(9) . .
P2 Ru1 H4 98.6(10) . .
H1 Ru1 H4 170.4(14) . .
H2 Ru1 H4 83.9(14) . .
H3 Ru1 H4 101.4(14) . .
C3 P1 C2 104.08(13) . .
C3 P1 C1 100.82(12) . .
C2 P1 C1 99.82(12) . .
C3 P1 Ru1 114.87(8) . .
C2 P1 Ru1 116.71(9) . .
C1 P1 Ru1 118.05(9) . .
C6 P2 C5 100.10(12) . .
C6 P2 C4 104.20(12) . .
C5 P2 C4 100.41(11) . .
C6 P2 Ru1 115.47(8) . .
C5 P2 Ru1 117.01(9) . .
C4 P2 Ru1 117.09(9) . .
Ru1 Si1 Ru1 179.40(4) . 2_556
Ru1 Si1 H3 47.2(10) . .
Ru1 Si1 H3 132.3(10) 2_556 .
Ru1 Si1 H4 47.0(9) . .
Ru1 Si1 H4 133.5(9) 2_556 .
H3 Si1 H4 94.2(14) . .
C12 C1 C11 108.3(2) . .
C12 C1 P1 113.38(18) . .
C11 C1 P1 111.89(19) . .
C21 C2 C22 108.9(3) . .
C21 C2 P1 114.2(2) . .
C22 C2 P1 112.9(2) . .
C32 C3 C31 109.8(2) . .
C32 C3 P1 115.1(2) . .
C31 C3 P1 115.2(2) . .
C42 C4 C41 108.7(3) . .
C42 C4 P2 113.8(2) . .
C41 C4 P2 112.80(19) . .
C51 C5 C52 108.2(2) . .
C51 C5 P2 112.63(18) . .
C52 C5 P2 112.64(17) . .
C61 C6 C62 109.2(2) . .
C61 C6 P2 115.5(2) . .
C62 C6 P2 114.70(18) . .
C1 C11 H11A 109.5 . .
C1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C1 C12 H12A 109.5 . .
C1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C2 C21 H21A 109.5 . .
C2 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C2 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C2 C22 H22A 109.5 . .
C2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C3 C31 H31A 109.5 . .
C3 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C3 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C3 C32 H32A 109.5 . .
C3 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C3 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C4 C41 H41A 109.5 . .
C4 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C4 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C4 C42 H42A 109.5 . .
C4 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C4 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C5 C51 H51A 109.5 . .
C5 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C5 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
C5 C52 H52A 109.5 . .
C5 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C5 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
C6 C61 H61A 109.5 . .
C6 C61 H61B 109.5 . .
H61A C61 H61B 109.5 . .
C6 C61 H61C 109.5 . .
H61A C61 H61C 109.5 . .
H61B C61 H61C 109.5 . .
C6 C62 H62A 109.5 . .
C6 C62 H62B 109.5 . .
H62A C62 H62B 109.5 . .
C6 C62 H62C 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 Si1 2.1875(4) .
Ru1 P1 2.3119(7) .
Ru1 P2 2.3129(7) .
Ru1 H1 1.49(2) .
Ru1 H2 1.52(3) .
Ru1 H3 1.62(3) .
Ru1 H4 1.62(3) .
P1 C3 1.864(3) .
P1 C2 1.869(3) .
P1 C1 1.876(2) .
P2 C6 1.863(3) .
P2 C5 1.872(2) .
P2 C4 1.878(3) .
Si1 Ru1 2.1875(4) 2_556
Si1 H3 1.69(3) .
Si1 H4 1.73(3) .
C1 C12 1.520(4) .
C1 C11 1.523(4) .
C2 C21 1.495(5) .
C2 C22 1.528(4) .
C3 C32 1.526(4) .
C3 C31 1.536(4) .
C4 C42 1.517(4) .
C4 C41 1.524(4) .
C5 C51 1.517(4) .
C5 C52 1.524(4) .
C6 C61 1.527(4) .
C6 C62 1.534(4) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C61 H61A 0.9800 .
C61 H61B 0.9800 .
C61 H61C 0.9800 .
C62 H62A 0.9800 .
C62 H62B 0.9800 .
C62 H62C 0.9800 .
