Preparation and Characterization of a Monocyclopentadienyl Osmium−Allenylcarbene Complex
Esteruelas, Miguel A.; Hernández, Yohar A.; López, Ana M.; Oñate, Enrique; Organometallics 26 (2007) 6009–; doi:10.1021/om700722e

data_4073916
_publ_section_title
;
 Preparation and Characterization of a Monocyclopentadienyl
 Osmium&#x2212;Allenylcarbene Complex
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6009
_journal_paper_doi               10.1021/om700722e
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C30 H38 B F4 Os P'
_chemical_formula_weight         706.58
_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                 98.652(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2901(15)
_cell_length_b                   17.239(3)
_cell_length_c                   15.961(2)
_cell_measurement_reflns_used    933
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2.3
_cell_volume                     2799.1(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.940
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33796
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    4.657
_exptl_absorpt_correction_T_max  0.653
_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    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+22.5398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                5248
_reflns_number_total             6841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700722e.cif
_cod_data_source_block           mae191bs
_cod_original_cell_volume        2799.2(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073916