Formation of an Asymmetric Acyclic Osmium−Dienylcarbene Complex
Bolaño, Tamara; Castarlenas, Ricardo; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 27 (2008) 6367–; doi:10.1021/om800535t

data_4072036
_publ_section_title
;
 Formation of an Asymmetric Acyclic Osmium&#x2212;Dienylcarbene Complex
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6367
_journal_paper_doi               10.1021/om800535t
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C47.33 H69.66 B2 Cl0.66 F8 N3 Os P2'
_chemical_formula_weight         1129.41
_chemical_name_systematic
; 
 ? 
;
_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                 116.310(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.522(4)
_cell_length_b                   14.461(3)
_cell_length_c                   19.434(4)
_cell_measurement_reflns_used    1011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     5421.9(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1198
_diffrn_reflns_av_sigmaI/netI    0.2063
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26778
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    2.503
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.692
_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            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2295
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9530
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      0.858
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                4162
_reflns_number_total             9530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800535t_si_001.cif
_cod_data_source_block           mae212bs
_cod_original_cell_volume        5421.9(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072036