Ruthenium Complexes Containing Two Ru-(η2-Si-H) Bonds: Synthesis, Spectroscopic Properties, Structural Data, Theoretical Calculations, and Reactivity Studies
Fabien Delpech; Sylviane Sabo-Etienne; Jean-Claude Daran; Bruno Chaudret; Khansaa Hussein; Colin J. Marsden; Jean-Claude Barthelat; Journal of the American Chemical Society 121 (1999) 6668–6682; doi:10.1021/ja990199j

data_4116442
_publ_contact_author             'Jean-Claude Daran'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_phone       ' (33) 5 61 33 31 74 '
_publ_section_title
;
 Ruthenium Complexes Containing Two Ru-(\h2-Si-H) Bonds: Synthesis,
 Spectroscopic Properties, Structural Data, Theoretical Calculations, and
 Reactivity Studies
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6668
_journal_page_last               6682
_journal_paper_doi               10.1021/ja990199j
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source
;
 synthetic route
;
_chemical_formula_moiety         ' C54 H80 Ru1 P2 SI2 '
_chemical_formula_sum            'C54 H80 I2 P2 Ru S'
_chemical_formula_weight         948.37
_chemical_name_systematic
; 
 ? 
;
_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           CRYSTALS
_cell_angle_alpha                99.037(11)
_cell_angle_beta                 99.503(11)
_cell_angle_gamma                100.280(11)
_cell_formula_units_Z            2
_cell_length_a                   9.9070(10)
_cell_length_b                   10.9279(12)
_cell_length_c                   24.785(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      1.95
_cell_volume                     2555.4(5)
_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    'CAMERON (Watkin, Prout & Pearce,  1996)'
_computing_publication_material  'CRYSTALS Issue 10 (Watkin et al., 1996)'
_computing_structure_refinement  'CRYSTALS Issue 10 (Watkin et al., 1996)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0441
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15829
_diffrn_reflns_theta_full        24.06
_diffrn_reflns_theta_max         24.06
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       needle
_exptl_crystal_F_000             1009.9
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.079
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
; 
 Robust-resistant weighting scheme (Prince E, 1982): 
 w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients 
 Ar(2.22, -0.542, 1.84) for the Chebyshev polynomial ArTr(x) where x 
 was Fc/Fc(max). 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6160
_reflns_number_total             7558
_reflns_observed_criterion       >2.00\s(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja990199j_3.cif
_cod_data_source_block           4Ph
_cod_depositor_comments
;
Adding closing parentheses to _atom_site_aniso_U_12 values.
Adding _atom_site_type_symbol label and values.

 Antanas Vaitkus
 2013-04-03
-------------------------------------------------------------------------------
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'triclinic ' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C54 H80 Ru1 P2 SI2 '
_cod_database_code               4116442