Hydride-Carbyne to Carbene Transformation in an Osmium-Acetate-Bis(triisopropylphosphine) System: Influence of the Coordination Mode of the Carboxylate and the Reaction Solvent
Bolaño, Tamara; Castarlenas, Ricardo; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 26 (2007) 2037–; doi:10.1021/om0611655

data_4072962
_publ_section_title
;
 Hydride-Carbyne to Carbene Transformation in an
 Osmium-Acetate-Bis(triisopropylphosphine) System:&#x00A0; Influence of
 the Coordination Mode of the Carboxylate and the Reaction Solvent
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2037
_journal_paper_doi               10.1021/om0611655
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C42 H69 B F4 N2 O3 Os P2'
_chemical_formula_weight         988.94
_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                 93.378(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.354(2)
_cell_length_b                   9.5203(11)
_cell_length_c                   23.038(3)
_cell_measurement_reflns_used    929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2.5
_cell_volume                     4456.5(9)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54479
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.626
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         11080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                8184
_reflns_number_total             11080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611655si20061221_054942.cif
_cod_data_source_block           mae198as
_cod_original_cell_volume        4456.3(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072962