C−C Bond Activation of the NHC Ligand of an Osmium−Amido Complex
Bolaño, Tamara; Buil, María L.; Esteruelas, Miguel A.; Izquierdo, Susana; Lalrempuia, Ralte; Oliván, Montserrat; Oñate, Enrique; Organometallics 29 (2010) 4517–; doi:10.1021/om100684a

data_4066872
_publ_section_title
;
 C&#x2212;C Bond Activation of the NHC Ligand of an Osmium&#x2212;Amido
 Complex
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4517
_journal_paper_doi               10.1021/om100684a
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C41 H56 N4 Os x 2(B F4) x 0.5 (N C2 H3)'
_chemical_formula_sum            'C42 H57.5 B2 F8 N4.5 Os'
_chemical_formula_weight         989.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.531(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.288(3)
_cell_length_b                   19.507(5)
_cell_length_c                   20.839(6)
_cell_measurement_reflns_used    1833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      2
_cell_volume                     4525(2)
_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 0.998
_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  0.1308
_diffrn_reflns_av_sigmaI/netI    0.2149
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45816
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.710
_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            brown
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         11151
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.719
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                5669
_reflns_number_total             11151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100684a_si_001.cif
_cod_data_source_block           mae264as
_cod_original_cell_volume        4526(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C42 H57.50 B2 F8 N4.50 Os'
_cod_database_code               4066872