Trapping of a 12-Valence-Electron Osmium Intermediate
Buil, María L.; Esteruelas, Miguel A.; Garcés, Karin; García-Raboso, Jorge; Oliván, Montserrat; Organometallics 28 (2009) 4606–; doi:10.1021/om9002544

data_4069539
_publ_section_title
;
 Trapping of a 12-Valence-Electron Osmium Intermediate
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4606
_journal_paper_doi               10.1021/om9002544
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C25 H51 Os P2, B F4 '
_chemical_formula_sum            'C25 H51 B F4 Os P2'
_chemical_formula_weight         690.61
_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                79.513(3)
_cell_angle_beta                 84.033(3)
_cell_angle_gamma                88.269(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5710(3)
_cell_length_b                   10.5741(5)
_cell_length_c                   15.5455(5)
_cell_measurement_reflns_used    14553
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6872
_cell_measurement_theta_min      2.9722
_cell_volume                     1377.77(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_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      150(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur TS, CCD area detector
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26522
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.783
_exptl_absorpt_correction_T_max  1.0904
_exptl_absorpt_correction_T_min  0.7557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.940
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6258
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                5312
_reflns_number_total             6258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9002544_si_001.cif
_cod_data_source_block           est4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069539