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_4085325
_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 H66 N2 Os P, C F3 O3 S, 0.625(C4 H10 O),0.375(C H2 Cl2)'
_chemical_formula_sum            'C46.88 H73 Cl0.75 F3 N2 O3.63 Os P S'
_chemical_formula_weight         1059.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.728(3)
_cell_angle_beta                 86.522(3)
_cell_angle_gamma                74.427(3)
_cell_formula_units_Z            4
_cell_length_a                   12.112(2)
_cell_length_b                   12.152(2)
_cell_length_c                   35.128(7)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4927.4(15)
_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 0.993
_diffrn_measured_fraction_theta_max 0.894
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            53946
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.756
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.522
_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            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.697
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.131
_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     1099
_refine_ls_number_reflns         24713
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.3798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                18452
_reflns_number_total             24713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501274x_si_001.cif
_cod_data_source_block           5-enriquen77
_cod_depositor_comments
'Adding full bibliography for 4085323--4085325.cif.'
_cod_original_cell_volume        4927.2(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085325