#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:22:05 +0100 (lun 21 de mar de 2016) $
#$Revision: 178622 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/33/4073366.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_4073366
loop_
_publ_author_name
'Lachaize, Sébastien'
'Caballero, Ana'
'Vendier, Laure'
'Sabo-Etienne, Sylviane'
_publ_contact_author
;
Sylviane Sabo-Etienne
;
_publ_section_title
;
 Activation of Chlorosilanes at Ruthenium:  A Route to Silyl
 σ-Dihydrogen Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3713
_journal_paper_doi               10.1021/om700295g
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H69 Cl P2 Ru'
_chemical_formula_sum            'C36 H69 Cl P2 Ru'
_chemical_formula_weight         700.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                114.273(11)
_cell_angle_beta                 107.889(11)
_cell_angle_gamma                90.735(13)
_cell_formula_units_Z            1
_cell_length_a                   9.7161(10)
_cell_length_b                   10.1762(11)
_cell_length_c                   10.6933(10)
_cell_measurement_reflns_used    7521
_cell_measurement_temperature    160
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.65
_cell_measurement_wavelength     0.71073
_cell_volume                     905.3(2)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9001
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0401P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                2678
_reflns_number_total             3324
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om700295g-file001.cif
_cod_data_source_block           global
_cod_original_cell_volume        905.4(2)
_cod_database_code               4073366
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
C111 C 0.2577(3) -0.1462(3) 0.2014(3) 0.0216(6) Uani 1 1 d .
H111 H 0.3488 -0.1224 0.284 0.026 Uiso 1 1 calc R
C112 C 0.1451(4) -0.2386(3) 0.2182(4) 0.0283(7) Uani 1 1 d .
H11A H 0.1304 -0.1837 0.3105 0.034 Uiso 1 1 calc R
H11B H 0.0521 -0.26 0.1404 0.034 Uiso 1 1 calc R
C113 C 0.1957(4) -0.3813(4) 0.2133(4) 0.0321(7) Uani 1 1 d .
H11C H 0.1205 -0.4394 0.2199 0.039 Uiso 1 1 calc R
H11D H 0.2839 -0.3602 0.2964 0.039 Uiso 1 1 calc R
C114 C 0.2265(4) -0.4683(3) 0.0722(4) 0.0318(7) Uani 1 1 d .
H11E H 0.2615 -0.5569 0.0729 0.038 Uiso 1 1 calc R
H11F H 0.1366 -0.4959 -0.0107 0.038 Uiso 1 1 calc R
C115 C 0.3404(4) -0.3781(4) 0.0569(4) 0.0309(7) Uani 1 1 d .
H11G H 0.3561 -0.4334 -0.0347 0.037 Uiso 1 1 calc R
H11H H 0.4325 -0.3571 0.1357 0.037 Uiso 1 1 calc R
C116 C 0.2908(4) -0.2347(3) 0.0611(3) 0.0269(7) Uani 1 1 d .
H11I H 0.2035 -0.2557 -0.023 0.032 Uiso 1 1 calc R
H11J H 0.367 -0.1771 0.0554 0.032 Uiso 1 1 calc R
C121 C 0.3750(3) 0.1280(3) 0.2230(3) 0.0239(6) Uani 1 1 d .
H121 H 0.376 0.0914 0.123 0.029 Uiso 1 1 calc R
C122 C 0.5212(3) 0.1027(4) 0.3098(4) 0.0326(7) Uani 1 1 d .
H12A H 0.5331 0.1463 0.4128 0.039 Uiso 1 1 calc R
H12B H 0.5219 -0.0013 0.2778 0.039 Uiso 1 1 calc R
C123 C 0.6476(4) 0.1702(4) 0.2875(5) 0.0407(9) Uani 1 1 d .
H12C H 0.7396 0.1549 0.3445 0.049 Uiso 1 1 calc R
H12D H 0.6387 0.1216 0.1854 0.049 Uiso 1 1 calc R
C124 C 0.6492(4) 0.3318(4) 0.3325(5) 0.0447(9) Uani 1 1 d .
H12E H 0.7262 0.3694 0.3101 0.054 Uiso 1 1 calc R
H12F H 0.6703 0.3823 0.4371 0.054 Uiso 1 1 calc R
C125 C 0.5029(4) 0.3616(4) 0.2536(5) 0.0405(9) Uani 1 1 d .
H12G H 0.4885 0.3228 0.1503 0.049 Uiso 1 1 calc R
H12H H 0.5042 0.4663 0.2907 0.049 Uiso 1 1 calc R
C126 C 0.3749(3) 0.2927(4) 0.2735(4) 0.0307(7) Uani 1 1 d .
H12I H 0.2832 0.309 0.2173 0.037 Uiso 1 1 calc R
H12J H 0.3833 0.3384 0.3756 0.037 Uiso 1 1 calc R
C131 C 0.1665(3) 0.1143(3) 0.3804(3) 0.0224(6) Uani 1 1 d .
H131 H 0.0883 0.045 0.3704 0.027 Uiso 1 1 calc R
C132 C 0.1021(4) 0.2561(4) 0.4046(3) 0.0281(7) Uani 1 1 d .
H13A H 0.1759 0.3325 0.4216 0.034 Uiso 1 1 calc R
H13B H 0.0202 0.241 0.318 0.034 Uiso 1 1 calc R
C133 C 0.0504(4) 0.3027(4) 0.5362(4) 0.0335(8) Uani 1 1 d .
H13C H 0.0162 0.3958 0.5547 0.04 Uiso 1 1 calc R
H13D H -0.0315 0.2313 0.5137 0.04 Uiso 1 1 calc R
C134 C 0.1710(4) 0.3166(4) 0.6722(3) 0.0329(8) Uani 1 1 d .
H13E H 0.1319 0.3394 0.7507 0.039 Uiso 1 1 calc R
H13F H 0.2475 0.3964 0.702 0.039 Uiso 1 1 calc R
C135 C 0.2362(4) 0.1764(4) 0.6465(3) 0.0341(8) Uani 1 1 d .
H13G H 0.1626 0.0987 0.627 0.041 Uiso 1 1 calc R
H13H H 0.3171 0.1908 0.7335 0.041 Uiso 1 1 calc R
C136 C 0.2909(4) 0.1326(4) 0.5174(3) 0.0292(7) Uani 1 1 d .
H13I H 0.3697 0.2071 0.5398 0.035 Uiso 1 1 calc R
H13J H 0.3291 0.0416 0.5004 0.035 Uiso 1 1 calc R
P1 P 0.20198(8) 0.02914(8) 0.20490(7) 0.01894(18) Uani 1 1 d .
Cl1 Cl 0.15273(15) 0.08401(18) -0.09731(15) 0.0262(3) Uani 0.5 1 d P
Ru1 Ru 0 0 0 0.02098(12) Uani 1 2 d S
H1 H -0.0993 -0.0423 0.056 0.025 Uiso 0.5 1 d P
H2 H -0.0779 0.0597 0.0993 0.025 Uiso 0.5 1 d P
H1A H 0.0373 0.1549 0.0736 0.025 Uiso 0.5 1 d P
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 0 '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
C112 C111 C116 110.4(2) . .
C112 C111 P1 113.5(2) . .
C116 C111 P1 110.3(2) . .
C112 C111 H111 107.5 . .
C116 C111 H111 107.5 . .
P1 C111 H111 107.5 . .
C113 C112 C111 111.2(2) . .
C113 C112 H11A 109.4 . .
C111 C112 H11A 109.4 . .
C113 C112 H11B 109.4 . .
C111 C112 H11B 109.4 . .
H11A C112 H11B 108 . .
C112 C113 C114 111.0(3) . .
C112 C113 H11C 109.4 . .
C114 C113 H11C 109.4 . .
C112 C113 H11D 109.4 . .
C114 C113 H11D 109.4 . .
H11C C113 H11D 108 . .
C115 C114 C113 110.5(3) . .
C115 C114 H11E 109.5 . .
C113 C114 H11E 109.5 . .
C115 C114 H11F 109.5 . .
C113 C114 H11F 109.5 . .
H11E C114 H11F 108.1 . .
C114 C115 C116 110.8(3) . .
C114 C115 H11G 109.5 . .
C116 C115 H11G 109.5 . .
C114 C115 H11H 109.5 . .
C116 C115 H11H 109.5 . .
H11G C115 H11H 108.1 . .
C115 C116 C111 111.4(3) . .
C115 C116 H11I 109.3 . .
C111 C116 H11I 109.3 . .
C115 C116 H11J 109.3 . .
C111 C116 H11J 109.3 . .
H11I C116 H11J 108 . .
C122 C121 C126 109.4(3) . .
C122 C121 P1 118.7(2) . .
C126 C121 P1 112.98(19) . .
C122 C121 H121 104.8 . .
C126 C121 H121 104.8 . .
P1 C121 H121 104.8 . .
C123 C122 C121 110.1(3) . .
C123 C122 H12A 109.6 . .
C121 C122 H12A 109.6 . .
C123 C122 H12B 109.6 . .
C121 C122 H12B 109.6 . .
H12A C122 H12B 108.2 . .
C124 C123 C122 111.7(3) . .
C124 C123 H12C 109.3 . .
C122 C123 H12C 109.3 . .
C124 C123 H12D 109.3 . .
C122 C123 H12D 109.3 . .
H12C C123 H12D 107.9 . .
C123 C124 C125 111.1(3) . .
C123 C124 H12E 109.4 . .
C125 C124 H12E 109.4 . .
C123 C124 H12F 109.4 . .
C125 C124 H12F 109.4 . .
H12E C124 H12F 108 . .
C124 C125 C126 111.9(3) . .
C124 C125 H12G 109.2 . .
C126 C125 H12G 109.2 . .
C124 C125 H12H 109.2 . .
C126 C125 H12H 109.2 . .
H12G C125 H12H 107.9 . .
C125 C126 C121 110.3(3) . .
C125 C126 H12I 109.6 . .
C121 C126 H12I 109.6 . .
C125 C126 H12J 109.6 . .
C121 C126 H12J 109.6 . .
H12I C126 H12J 108.1 . .
C136 C131 C132 110.9(2) . .
C136 C131 P1 116.7(2) . .
C132 C131 P1 113.7(2) . .
C136 C131 H131 104.7 . .
C132 C131 H131 104.7 . .
P1 C131 H131 104.7 . .
C133 C132 C131 109.9(3) . .
C133 C132 H13A 109.7 . .
C131 C132 H13A 109.7 . .
C133 C132 H13B 109.7 . .
C131 C132 H13B 109.7 . .
H13A C132 H13B 108.2 . .
C134 C133 C132 112.0(3) . .
C134 C133 H13C 109.2 . .
C132 C133 H13C 109.2 . .
C134 C133 H13D 109.2 . .
C132 C133 H13D 109.2 . .
H13C C133 H13D 107.9 . .
C133 C134 C135 111.6(3) . .
C133 C134 H13E 109.3 . .
C135 C134 H13E 109.3 . .
C133 C134 H13F 109.3 . .
C135 C134 H13F 109.3 . .
H13E C134 H13F 108 . .
C134 C135 C136 110.6(3) . .
C134 C135 H13G 109.5 . .
C136 C135 H13G 109.5 . .
C134 C135 H13H 109.5 . .
C136 C135 H13H 109.5 . .
H13G C135 H13H 108.1 . .
C131 C136 C135 110.4(3) . .
C131 C136 H13I 109.6 . .
C135 C136 H13I 109.6 . .
C131 C136 H13J 109.6 . .
C135 C136 H13J 109.6 . .
H13I C136 H13J 108.1 . .
C111 P1 C131 102.41(13) . .
C111 P1 C121 101.92(13) . .
C131 P1 C121 109.42(14) . .
C111 P1 Ru1 113.73(10) . .
C131 P1 Ru1 113.74(10) . .
C121 P1 Ru1 114.37(10) . .
P1 Ru1 P1 180.00(3) . 2
P1 Ru1 Cl1 88.40(4) . 2
P1 Ru1 Cl1 91.60(4) 2 2
P1 Ru1 Cl1 91.60(4) . .
P1 Ru1 Cl1 88.40(4) 2 .
Cl1 Ru1 Cl1 180.00(5) 2 .
P1 Ru1 H1 91.559(18) . .
P1 Ru1 H1 88.441(18) 2 .
Cl1 Ru1 H1 4.70(4) 2 .
Cl1 Ru1 H1 175.30(4) . .
P1 Ru1 H2 86.564(19) . .
P1 Ru1 H2 93.436(19) 2 .
Cl1 Ru1 H2 41.43(4) 2 .
Cl1 Ru1 H2 138.57(4) . .
H1 Ru1 H2 38.257(7) . .
P1 Ru1 H1A 79.21(2) . .
P1 Ru1 H1A 100.79(2) 2 .
Cl1 Ru1 H1A 110.52(4) 2 .
Cl1 Ru1 H1A 69.48(4) . .
H1 Ru1 H1A 107.727(12) . .
H2 Ru1 H1A 69.529(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C111 C112 1.533(4) .
C111 C116 1.535(4) .
C111 P1 1.860(3) .
C111 H111 0.98 .
C112 C113 1.524(5) .
C112 H11A 0.97 .
C112 H11B 0.97 .
C113 C114 1.529(4) .
C113 H11C 0.97 .
C113 H11D 0.97 .
C114 C115 1.517(4) .
C114 H11E 0.97 .
C114 H11F 0.97 .
C115 C116 1.530(5) .
C115 H11G 0.97 .
C115 H11H 0.97 .
C116 H11I 0.97 .
C116 H11J 0.97 .
C121 C122 1.530(4) .
C121 C126 1.535(4) .
C121 P1 1.863(3) .
C121 H121 0.98 .
C122 C123 1.527(4) .
C122 H12A 0.97 .
C122 H12B 0.97 .
C123 C124 1.511(5) .
C123 H12C 0.97 .
C123 H12D 0.97 .
C124 C125 1.520(5) .
C124 H12E 0.97 .
C124 H12F 0.97 .
C125 C126 1.532(4) .
C125 H12G 0.97 .
C125 H12H 0.97 .
C126 H12I 0.97 .
C126 H12J 0.97 .
C131 C136 1.524(4) .
C131 C132 1.534(4) .
C131 P1 1.860(3) .
C131 H131 0.98 .
C132 C133 1.534(4) .
C132 H13A 0.97 .
C132 H13B 0.97 .
C133 C134 1.512(5) .
C133 H13C 0.97 .
C133 H13D 0.97 .
C134 C135 1.523(5) .
C134 H13E 0.97 .
C134 H13F 0.97 .
C135 C136 1.528(4) .
C135 H13G 0.97 .
C135 H13H 0.97 .
C136 H13I 0.97 .
C136 H13J 0.97 .
P1 Ru1 2.3557(8) .
Cl1 Ru1 2.3797(12) .
Ru1 P1 2.3557(8) 2
Ru1 Cl1 2.3797(12) 2
Ru1 H1 1.42512(14) .
Ru1 H2 1.43025(18) .
Ru1 H1A 1.4233(2) .
