From Tetrahydroborate- to Aminoborylvinylidene-Osmium Complexes via Alkynyl-Aminoboryl Intermediates
María L. Buil; Miguel A. Esteruelas; Karin Garcés; Enrique Oñate; Journal of the American Chemical Society 133 (2011) 2250–2263; doi:10.1021/ja109691v

data_4105652
_publ_contact_author
;
  Dr. Enrique O\~nate Rodr\'iguez
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@posta.unizar.es
_publ_section_title
;
 From Tetrahydroborate- to Aminoborylvinylidene-Osmium Complexes via
 Alkynyl-Aminoboryl Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2250
_journal_page_last               2263
_journal_paper_doi               10.1021/ja109691v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C31 H53 B N2 O Os P2'
_chemical_formula_weight         732.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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   calc
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.393(2)
_cell_angle_beta                 88.068(2)
_cell_angle_gamma                89.455(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1135(11)
_cell_length_b                   17.243(2)
_cell_length_c                   19.003(2)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     3265.5(6)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (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 0.990
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker SMART APEX CCD 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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.1470
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48461
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.028
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.532
_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            orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.670
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1359
_refine_ls_number_reflns         29604
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.7151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                21841
_reflns_number_total             29604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109691v_si_001_2.cif
_cod_data_source_block           mae447bs
_cod_original_cell_volume        3265.6(6)
_cod_database_code               4105652