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_4081335
_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         'C42 H75 B1 P2 Ru1'
_chemical_formula_sum            'C42 H75 B P2 Ru'
_chemical_formula_weight         753.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                100.430(8)
_cell_angle_beta                 102.772(7)
_cell_angle_gamma                108.026(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5995(8)
_cell_length_b                   12.6765(12)
_cell_length_c                   18.1000(17)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.9967
_cell_measurement_theta_min      2.7451
_cell_measurement_wavelength     0.71073
_cell_volume                     1967.3(4)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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      120(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_orient_matrix_UB_11      -0.0217129738
_diffrn_orient_matrix_UB_12      0.0478334109
_diffrn_orient_matrix_UB_13      0.0115005316
_diffrn_orient_matrix_UB_21      0.0237389749
_diffrn_orient_matrix_UB_22      0.0225635479
_diffrn_orient_matrix_UB_23      -0.030145249
_diffrn_orient_matrix_UB_31      -0.0749897257
_diffrn_orient_matrix_UB_32      -0.0310277963
_diffrn_orient_matrix_UB_33      -0.0265769377
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12900
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+2.6939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                4123
_reflns_number_total             6459
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400610k_si_002.cif
_cod_data_source_block           gbl77(bis-sigma-phenyl)
_cod_original_cell_volume        1967.3(3)
_cod_database_code               4081335