Dicationic Alkylidene−, Olefin−, and Alkoxyalkenylcarbene−Osmium Complexes Stabilized by a NHC Ligand
Buil, María L.; Castarlenas, Ricardo; Esteruelas, Miguel A.; Izquierdo, Susana; Lalrempuia, Ralte; Oñate, Enrique; Organometallics 29 (2010) 876–; doi:10.1021/om900949j

data_4067426
_publ_section_title
;
 Dicationic Alkylidene&#x2212;, Olefin&#x2212;, and
 Alkoxyalkenylcarbene&#x2212;Osmium Complexes Stabilized by a NHC Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              876
_journal_paper_doi               10.1021/om900949j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C40.25 H54.5 Cl0.5 F6 N6 O6 Os S2'
_chemical_formula_weight         1104.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.355(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.717(4)
_cell_length_b                   18.141(5)
_cell_length_c                   21.711(6)
_cell_measurement_reflns_used    989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     4852(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48826
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.770
_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            colorless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2226
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.422
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         8556
_refine_ls_number_restraints     1398
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+33.0461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                7058
_reflns_number_total             8556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900949j_si_001.cif
_cod_data_source_block           mae333bs
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C40.25 H54.50 Cl0.50 F6 N6 O6 Os S2'
_cod_database_code               4067426