Preparation and Structure of Alkylidene−Osmium and Hydride−Alkylidyne−Osmium Complexes Containing an N-Heterocyclic Carbene Ligand
Castarlenas, Ricardo; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 26 (2007) 2129–; doi:10.1021/om070065b

data_4073096
_publ_section_title
;
 Preparation and Structure of Alkylidene&#x2212;Osmium and
 Hydride&#x2212;Alkylidyne&#x2212;Osmium Complexes Containing an
 N-Heterocyclic Carbene Ligand
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2129
_journal_paper_doi               10.1021/om070065b
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C44H54N6S2F6O6Os 0.5C2H3N'
_chemical_formula_sum            'C45 H55.5 Cl0 F6 N6.5 O6 Os S2'
_chemical_formula_weight         1151.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.5690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.430(3)
_cell_length_b                   16.0307(9)
_cell_length_c                   12.9022(7)
_cell_measurement_reflns_used    5222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     10175.4(10)
_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 0.987
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34193
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.740
_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            blue
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.804
_refine_diff_density_min         -2.260
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         12129
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                8430
_reflns_number_total             12129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070065bsi20070122_043945.cif
_cod_data_source_block           mae207as
_cod_original_cell_volume        10175.5(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C45 H55.50 Cl0 F6 N6.50 O6 Os S2'
_cod_database_code               4073096