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_4081338
_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         'C39 H69 B P2 Ru'
_chemical_formula_sum            'C39 H69 B P2 Ru'
_chemical_formula_weight         711.76
_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                94.553(5)
_cell_angle_beta                 94.383(3)
_cell_angle_gamma                111.545(6)
_cell_formula_units_Z            4
_cell_length_a                   11.1641(8)
_cell_length_b                   14.5855(7)
_cell_length_c                   26.5827(9)
_cell_measurement_reflns_used    13599
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.1628
_cell_measurement_theta_min      3.2771
_cell_measurement_wavelength     0.71073
_cell_volume                     3987.3(4)
_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    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0171503
_diffrn_orient_matrix_UB_12      0.0427509
_diffrn_orient_matrix_UB_13      -0.0130739
_diffrn_orient_matrix_UB_21      -0.015887
_diffrn_orient_matrix_UB_22      0.0261508
_diffrn_orient_matrix_UB_23      0.0204203
_diffrn_orient_matrix_UB_31      0.0646575
_diffrn_orient_matrix_UB_32      0.0161092
_diffrn_orient_matrix_UB_33      0.0117477
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49505
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.9558
_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            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.45
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         16248
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0768
_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^)+(0.0587P)^2^+3.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                11696
_reflns_number_total             16248
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400610k_si_002.cif
_cod_data_source_block           gbl03031(bis-sigma-MesCyp)
_cod_database_code               4081338