Sequential and Selective Hydrogenation of the Cα-Cβ and M-Cα Double Bonds of an Allenylidene Ligand Coordinated to Osmium: New Reaction Patterns between an Allenylidene Complex and Alcohols
Tamara Bolaño; Ricardo Castarlenas; Miguel A. Esteruelas; Enrique Oñate; Journal of the American Chemical Society 129 (2007) 8850–8859; doi:10.1021/ja071972a

data_4109666
_publ_contact_author
;
  Dr. Enrique O\~nate Rodr\'iguez
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@posta.unizar.es
_publ_section_title
;
 Sequential and Selective Hydrogenation of the C\a-C\b and M-C\a Double
 Bonds of an Allenylidene Ligand Coordinated to Osmium: New Reaction
 Patterns between an Allenylidene Complex and Alcohols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8850
_journal_page_last               8859
_journal_paper_doi               10.1021/ja071972a
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C41 H62 N P2 O Os; B F4; O0.5 c2 H5'
_chemical_formula_sum            'C43 H67 B F4 N O1.5 Os P2'
_chemical_formula_weight         960.93
_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                 90.816(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6813(19)
_cell_length_b                   13.9813(17)
_cell_length_c                   21.656(3)
_cell_measurement_reflns_used    858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     4444.7(10)
_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 0.992
_diffrn_measured_fraction_theta_max 0.910
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28234
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         1.39
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    2.991
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.621
_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    1.436
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.847
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                7469
_reflns_number_total             10722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071972asi20070507_012156_2.cif
_cod_data_source_block           mae205as
_cod_original_cell_volume        4444.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C43 H67 B F4 N O1.50 Os P2'
_cod_database_code               4109666