Synthesis and Characterization of Chelating Bis(silane) Complexes [RuH2{(η2-HSiMe2)2X}(PCy3)2] (X = C6H4, O) Containing Two Ru-(η2-Si-H) Bonds
Fabien Delpech; Sylviane Sabo-Etienne; Bruno Chaudret; Jean-Claude Daran; Journal of the American Chemical Society 119 (1997) 3167–3168; doi:10.1021/ja963933x

data_4116947
_publ_contact_author
;
 Daran Jean-Claude
 Laboratoire de Chimie de Coordination du CNRS
 205, route de Narbonne
 31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' 33 (0)5 61 55 30 03  '
_publ_contact_author_phone       ' 33 (0)5 61 33 31 74 '
_publ_section_title
;
 Synthesis and Characterization of Chelating Bis(silane) Complexes
 [RuH2{(\h2-HSiMe2)2X}(PCy3)2] (X = C6H4, O) Containing Two Ru-(\h2-Si-H)
 Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3167
_journal_page_last               3168
_journal_paper_doi               10.1021/ja963933x
_journal_volume                  119
_journal_year                    1997
_chemical_compound_source
;
 synthetic route
;
_chemical_formula_moiety         ' C52 H92 Ru1 P2 Si2 '
_chemical_formula_sum            'C52 H92 P2 Ru Si2'
_chemical_formula_weight         936.49
_chemical_name_systematic
;
 dihydride [\h2-1,2-bis(dimethylsilyl)benzene] 
 bis(tricyclohexyl)phosphine ruthenium(II). benzene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             97-01-20
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90.00
_cell_angle_beta                 90.01(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.033(4)
_cell_length_b                   19.714(2)
_cell_length_c                   25.336(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48.4
_cell_measurement_theta_min      2.9
_cell_volume                     10505(3)
_computing_cell_refinement       'CAD-4 software (Stoe, 2.75, 1996)'
_computing_data_collection       'IPDS Stoe (Stoe, 2.75, 1996)'
_computing_data_reduction
;
 XRED (Stoe, 1.08, 1996)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '  Stoe IPDS '
_diffrn_measurement_method       \w
_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  0.10
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40046
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.43
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    1.18
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             4039.60
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.0706
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
 Coordinates of H hydride were refined with equivalent 
 isotropic thermal parameter
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         4856
_refine_ls_R_factor_obs          0.0446
_refine_ls_shift/esd_max         0.362266
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0403
_reflns_number_observed          4856
_reflns_number_total             8185
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ja963933x.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        10505.6(30)
_cod_original_sg_symbol_H-M      'I 1 2/a 1 '
_cod_original_formula_sum        ' C52 H92 Ru1 P2 Si2 '
_cod_database_code               4116947