Monosubstituted Borane Ruthenium Complexes RuH2(η2:η2-H2BR)(PR′3)2: A General Approach to the Geminal Bis(σ-B‒H) Coordination Mode
Gloaguen, Yann; Bénac-Lestrille, Gaëtan; Vendier, Laure; Helmstedt, Ulrike; Clot, Eric; Alcaraz, Gilles; Sabo-Etienne, Sylviane; Organometallics 32 (2013) 4868–; doi:10.1021/om400610k

data_4081337
_publ_section_title
;
 Monosubstituted Borane Ruthenium Complexes
 RuH2(\h2:\h2-H2BR)(PR&#x2032;3)2: A General Approach to the Geminal
 Bis(\s-B--H) Coordination Mode
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4868
_journal_paper_doi               10.1021/om400610k
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H57 B P2 Ru'
_chemical_formula_sum            'C27 H57 B P2 Ru'
_chemical_formula_weight         555.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.7989(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9752(14)
_cell_length_b                   16.3783(2)
_cell_length_c                   10.1876(13)
_cell_measurement_reflns_used    8726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2422
_cell_measurement_theta_min      3.1854
_cell_measurement_wavelength     0.71073
_cell_volume                     1497.4(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0209528
_diffrn_orient_matrix_UB_12      -0.0040977
_diffrn_orient_matrix_UB_13      0.0670609
_diffrn_orient_matrix_UB_21      -0.0718863
_diffrn_orient_matrix_UB_22      -0.0153754
_diffrn_orient_matrix_UB_23      0.0141436
_diffrn_orient_matrix_UB_31      0.0253536
_diffrn_orient_matrix_UB_32      -0.0402772
_diffrn_orient_matrix_UB_33      -0.0122252
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13346
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.5836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0439
_reflns_number_gt                2978
_reflns_number_total             3122
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400610k_si_002.cif
_cod_data_source_block           gbl280212(bis-sigma-MesIPr)
_cod_database_code               4081337