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_4066876
_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         'C34 H46 N3 Os x B F4 x C H2 Cl2'
_chemical_formula_sum            'C35 H48 B Cl2 F4 N3 Os'
_chemical_formula_weight         858.67
_chemical_name_systematic
; 
 ? 
;
_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                 101.2130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6290(11)
_cell_length_b                   12.2917(11)
_cell_length_c                   23.440(2)
_cell_measurement_reflns_used    7842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2.3
_cell_volume                     3569.2(5)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 4.0 (Bruker AXS, 2008)'
_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 0.968
_diffrn_measured_fraction_theta_max 0.921
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40471
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.484
_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
v. 2008.1 (2008) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         8498
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0409P)^2^+8.3096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                6525
_reflns_number_total             8498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100684a_si_001.cif
_cod_data_source_block           enrique17as-nh3
_cod_original_cell_volume        3569.1(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066876