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_4070841
_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_moiety         'C57 H76 N5 Os P, 2(B F4)'
_chemical_formula_sum            'C57 H76 B2 F8 N5 Os P'
_chemical_formula_weight         1226.02
_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                 132.683(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.156(5)
_cell_length_b                   25.895(4)
_cell_length_c                   20.849(3)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     11571(3)
_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      105(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.935
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1142
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63841
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.298
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.701
_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            'dark brown'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.443
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         14445
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                9133
_reflns_number_total             14445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7010694-file002.cif
_cod_data_source_block           mae2711s
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4070841