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_4081336
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H73 B1 P2 Ru1 S1'
_chemical_formula_sum            'C40 H73 B P2 Ru S'
_chemical_formula_weight         759.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8219(3)
_cell_length_b                   16.3983(4)
_cell_length_c                   24.5714(7)
_cell_measurement_reflns_used    12456
_cell_measurement_temperature    108
_cell_measurement_theta_max      29.2929
_cell_measurement_theta_min      3.3344
_cell_measurement_wavelength     0.71073
_cell_volume                     3957.53(19)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
;
_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      108
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.011706
_diffrn_orient_matrix_UB_12      -0.0055001
_diffrn_orient_matrix_UB_13      0.0282445
_diffrn_orient_matrix_UB_21      0.0590144
_diffrn_orient_matrix_UB_22      0.023309
_diffrn_orient_matrix_UB_23      0.0059295
_diffrn_orient_matrix_UB_31      -0.0399383
_diffrn_orient_matrix_UB_32      0.0360259
_diffrn_orient_matrix_UB_33      0.0004749
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30146
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
        (compiled Oct 25 2010,18:11:34)
        Empirical absorption correction using spherical harmonics,
       implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.1763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                6262
_reflns_number_total             7225
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400610k_si_002.cif
_cod_data_source_block           gbl280111(bis-sigma-thienyl)
_cod_database_code               4081336