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_4321439
_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            'C77 H118 B Cl3 O2 Os P4'
_chemical_formula_weight         1506.95
_chemical_name_common            '[OsCl(O2)(dcpe)2]BPh4'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.9880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.585(4)
_cell_length_b                   12.764(2)
_cell_length_c                   25.587(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7474(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART PLATFORM with CCD detector'
_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  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61602
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.765
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.973
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         18573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1181
_refine_ls_wR_factor_obs         0.0999
_reflns_number_observed          11786
_reflns_number_total             18573
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0002420_3.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7474.5(19)
_cod_database_code               4321439