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_4067427
_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            'C37.5 H52 B2 Cl F8 N7 Os'
_chemical_formula_weight         1000.13
_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                 100.657(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0654(19)
_cell_length_b                   12.944(2)
_cell_length_c                   31.086(5)
_cell_measurement_reflns_used    941
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      2
_cell_volume                     4771.1(13)
_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      293(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49170
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.757
_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    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+4.4735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                5686
_reflns_number_total             8804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900949j_si_001.cif
_cod_data_source_block           mae283as
_cod_original_cell_volume        4771.0(13)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C37.50 H52 B2 Cl F8 N7 Os'
_cod_database_code               4067427