Osmium-Acyl Decarbonylation Promoted by Tp-Mediated Allenylidene Abstraction: A New Role of the Tp Ligand
Bajo, Sonia; Esteruelas, Miguel A.; López, Ana M.; Oñate, Enrique; Organometallics 33 (2014) 4057–; doi:10.1021/om500569m

data_4084056
_publ_section_title
;
 Osmium-Acyl Decarbonylation Promoted by Tp-Mediated Allenylidene
 Abstraction: A New Role of the Tp Ligand
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4057
_journal_paper_doi               10.1021/om500569m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         '2(C48 H52 B N6 O Os P), C6 H5 F'
_chemical_formula_sum            'C51 H54.5 B F0.5 N6 O Os P'
_chemical_formula_weight         1008.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.557(2)
_cell_angle_beta                 100.165(2)
_cell_angle_gamma                105.928(2)
_cell_formula_units_Z            4
_cell_length_a                   13.687(2)
_cell_length_b                   17.372(3)
_cell_length_c                   21.600(3)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     4827.9(13)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (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 0.966
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45174
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.686
_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            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.399
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         20830
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+4.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                17921
_reflns_number_total             20830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500569m_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4084056--4084058.cif.'
_cod_original_cell_volume        4827.9(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C51 H54.50 B F0.50 N6 O Os P'
_cod_database_code               4084056
_shelx_f_squared_multiplier      1.000