Preparation and crystal structures of oxoosmium(VI) diolato complexes
Lehtonen, Ari; Jokela, Jukka; Edwards, Peter G.; Sillanpää, Reijo; Journal of the Chemical Society, Dalton Transactions  (1999) 2785–2788; doi:10.1039/a903042e

data_7027469
_publ_section_title
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 Preparation and crystal structures of oxoosmium(VI) diolato complexes
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2785
_journal_page_last               2788
_journal_paper_doi               10.1039/a903042e
_journal_year                    1999
_chemical_formula_sum            'C24 H40 O5 Os'
_chemical_formula_weight         598.76
_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                107.61(3)
_cell_angle_beta                 96.28(4)
_cell_angle_gamma                67.01(3)
_cell_formula_units_Z            5
_cell_length_a                   16.421(8)
_cell_length_b                   17.103(5)
_cell_length_c                   12.299(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      6.5
_cell_measurement_theta_min      5.4
_cell_volume                     3031(2)
_computing_cell_refinement
;
MSC/AFC5S Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_collection
; 
MSC/AFC Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_reduction
;
TEXSAN for WINDOWS(Molecular Structure Corporation, 1997)
;
_computing_molecular_graphics    'ORTEP-3 for WINDOWS (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11092
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        -1.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.290
_exptl_absorpt_correction_T_max  0.4494
_exptl_absorpt_correction_T_min  0.3891
_exptl_absorpt_correction_type
;
empirical via \y scans (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       black
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.679
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.3230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                7331
_reflns_number_total             10686
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            903042esup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
Changing the '_atom_site_refinement_flags' tag value for atom 'H32A' 
from 'Z' to 'R' after consulting the original paper.

Antanas Vaitkus,
2015-03-25
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_cod_database_code               7027469