Tetraphenylphosphonium <i>trans</i>-Aquatetrabromo(carbonyl)osmate(III), <i>trans</i>-[(C~6~H~5~)~4~P][OsBr~4~(CO)(H~2~O)]
Höhling, M.; Preetz, W.; Acta Crystallographica Section C 52 (1996) 863–865; doi:10.1107/S0108270195014259

data_2004764
_publ_section_title
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 Tetraphenylphosphonium
 <i>trans</i>-Aquatetrabromo(carbonyl)osmate(III),
 <i>trans</i>-[(C~6~H~5~)~4~P][OsBr~4~(CO)(H~2~O)]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              863
_journal_page_last               865
_journal_paper_doi               10.1107/S0108270195014259
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C24 H20 P) [Os Br4 (C O) (H2 O)]'
_chemical_formula_structural
;
'trans-[(C~6~H~5~)~4~P][OsBr~4~(CO)(H~2~O)]'
;
_chemical_formula_sum            'C25 H22 Br4 O2 Os P'
_chemical_formula_weight         895.24
_chemical_name_systematic
;
Tetraphenylphosphonium trans-Tetrabromoaquacarbonylosmate(III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                65.749(9)
_cell_angle_beta                 85.167(8)
_cell_angle_gamma                68.828(7)
_cell_formula_units_Z            2
_cell_length_a                   10.5458(9)
_cell_length_b                   12.4347(10)
_cell_length_c                   12.5963(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.263
_cell_measurement_theta_min      5.827
_cell_volume                     1400.4(2)
_computing_cell_refinement       CAD4-PC
_computing_data_collection       'CAD4-PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
;
Enraf-Nonius CAD4-Turbo four-cycle diffractometer
;
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5203
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        3.9
_diffrn_standards_interval_time  '240 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.337
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type
'empirical, \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .880
_refine_diff_density_min         -.516
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.162
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4912
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.163
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_obs          0.0298
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0189P)^2^+2.6281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0725
_refine_ls_wR_factor_obs         0.0556
_reflns_number_observed          3507
_reflns_number_total             4913
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1098.cif
_cod_data_source_block           br4coaq
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0189P)^2^+2.6281P] 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^)+(0.0189P)^2^+2.6281P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               2004764