Osmium-Promoted Dehydrogenation of Amine‒Boranes and B‒H Bond Activation of the Resulting Amino‒Boranes
Esteruelas, Miguel A.; Fernández, Israel; López, Ana M.; Mora, Malka; Oñate, Enrique; Organometallics 33 (2014) 1104–; doi:10.1021/om500027p

data_4082697
_publ_section_title
;
 Osmium-Promoted Dehydrogenation of Amine--Boranes and B--H Bond
 Activation of the Resulting Amino--Boranes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1104
_journal_paper_doi               10.1021/om500027p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C19 H46 B N O Os P2 S'
_chemical_formula_weight         599.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   48.907(4)
_cell_length_b                   18.9148(17)
_cell_length_c                   8.3417(8)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     7716.6(12)
_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 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.956
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            90674
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         0.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.172
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.547
_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            colorless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.628
_refine_diff_density_min         -1.954
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         18377
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+31.8195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                16214
_reflns_number_total             18377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500027p_si_002.cif
_cod_data_source_block           enrique108
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4082697
_shelx_f_squared_multiplier      1.000