Osmium−Allenylidene Complexes Containing an N-Heterocyclic Carbene Ligand
Castarlenas, Ricardo; Esteruelas, Miguel A.; Lalrempuia, Ralte; Oliván, Montserrat; Oñate, Enrique; Organometallics 27 (2008) 795–; doi:10.1021/om7010694

data_4070840
_publ_section_title
;
 Osmium&#x2212;Allenylidene Complexes Containing an N-Heterocyclic Carbene
 Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              795
_journal_paper_doi               10.1021/om7010694
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C53 H66 Cl F3 N2 O6 Os S'
_chemical_formula_weight         1141.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 97.237(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.657(2)
_cell_length_b                   18.140(2)
_cell_length_c                   16.2916(19)
_cell_measurement_reflns_used    3886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     5176.6(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      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24004
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.62
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.509
_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    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.248
_refine_diff_density_min         -2.290
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11846
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+15.5305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                10479
_reflns_number_total             11846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7010694-file002.cif
_cod_data_source_block           mae2231s
_cod_original_cell_volume        5176.5(10)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4070840