Oxo Complexes of Osmium(IV) Formed via Dioxygen Activation. X-ray Structures of [OsX(dcpe)2]PF6 (X = Cl, Br), [OsCl(η2-O2)(dcpe)2]BPh4, and [OsCl(O)(dcpe)2]BPh4 (dcpe = 1,2-Bis(dicyclohexylphosphino)ethane)
Peter Barthazy; Michael Wörle; Heinz Rüegger; Antonio Mezzetti; Inorganic Chemistry 39 (2000) 4903–4912; doi:10.1021/ic0002420

data_4321438
_publ_section_title
;
 Oxo Complexes of Osmium(IV) Formed via Dioxygen Activation. X-ray
 Structures of [OsX(dcpe)2]PF6 (X = Cl, Br), [OsCl(\h2-O2)(dcpe)2]BPh4,
 and [OsCl(O)(dcpe)2]BPh4 (dcpe = 1,2-Bis(dicyclohexylphosphino)ethane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4912
_journal_paper_doi               10.1021/ic0002420
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C52 H96 Br F6 Os P5'
_chemical_formula_weight         1260.25
_chemical_name_common            '[OsBr(dcpe)2]PF6'
_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                 100.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.546(6)
_cell_length_b                   14.682(7)
_cell_length_c                   26.171(12)
_cell_measurement_temperature    293(2)
_cell_volume                     5492(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Synthex P21'
_diffrn_measurement_method       '\w scans'
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5383
_diffrn_reflns_theta_full        20.05
_diffrn_reflns_theta_max         20.05
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_refine_diff_density_max         3.834
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                3897
_reflns_number_total             5117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002420_2.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4321438