RuH3(SiCl2Me)(PPh3)3: A Trihydridosilylruthenium Complex with Three Nonclassical Ru−H···Si Interactions
Yardy, Nicholas M.; Lemke, Frederick R.; Brammer, Lee; Organometallics 20 (2001) 5670–; doi:10.1021/om010654w

data_4077431
_publ_section_title
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 RuH3(SiCl2Me)(PPh3)3:&#x00A0; A Trihydridosilylruthenium Complex with
 Three Nonclassical Ru&#x2212;H&#x00B7;&#x00B7;&#x00B7;Si Interactions
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_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5670
_journal_paper_doi               10.1021/om010654w
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C55 H51 Cl2 P3 Ru Si'
_chemical_formula_weight         1004.93
_chemical_name_systematic
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 ? 
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_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.7603(4)
_cell_length_b                   14.6024(3)
_cell_length_c                   13.9643(3)
_cell_measurement_reflns_used    55344
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      61.236
_cell_measurement_theta_min      4.383
_cell_volume                     4845.02(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Omega Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            84251
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.8193
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   'empirical: SADABS'
_exptl_absorpt_process_details
;
absorption correction was based upon symmetry equivalent and 
repeated intensity measurements using the program SADABS 
(Sheldrick, 1995), which is based upon the method of 
Blessing (Blessing, R. H. Acta Cryst., 1995, A51, 33-38).  
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multifacetted block'
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(12)
_refine_ls_extinction_coef       0.00117(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         14197
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                13399
_reflns_number_total             14197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010654w.cif
_cod_data_source_block           l8000sd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom + difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4077431