Hydroboration and Hydrogenation of an Osmium‒Carbon Triple Bond: Osmium Chemistry of a Bis-σ-Borane
Buil, Mar\?ía L.; Cardo, Juan J. F.; Esteruelas, Miguel A.; Fernández, Israel; Oñate, Enrique; Organometallics 34 (2015) 547–; doi:10.1021/om501274x

data_4085323
_publ_section_title
;
 Hydroboration and Hydrogenation of an Osmium--Carbon Triple Bond: Osmium
 Chemistry of a Bis-\s-Borane
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              547
_journal_paper_doi               10.1021/om501274x
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C43 H64 N2 O Os P, C F3 O3 S'
_chemical_formula_sum            'C44 H64 F3 N2 O4 Os P S'
_chemical_formula_weight         995.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.267(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.291(4)
_cell_length_b                   10.4349(19)
_cell_length_c                   22.176(4)
_cell_measurement_reflns_used    4772
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4455.5(14)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39825
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.000
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.994
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10548
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+8.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                7339
_reflns_number_total             10548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501274x_si_001.cif
_cod_data_source_block           2-enrique95
_cod_depositor_comments
'Adding full bibliography for 4085323--4085325.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4085323