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_4081334
_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         'C37 H73 B1 P2 Ru1'
_chemical_formula_sum            'C37 H73 B P2 Ru'
_chemical_formula_weight         691.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 106.080(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5088(11)
_cell_length_b                   16.8599(15)
_cell_length_c                   18.2807(17)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      2.6
_cell_measurement_wavelength     0.71073
_cell_volume                     3704.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0529
_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       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31143
_diffrn_reflns_theta_full        23.46
_diffrn_reflns_theta_max         23.46
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0768P)^2^+0.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                3981
_reflns_number_total             5415
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400610k_si_002.cif
_cod_data_source_block           gao130508(bis-sigma-methyl)
_cod_database_code               4081334