Bis[bis(triphenylphosphoranylidene)ammonium] Pentachlorofluoroosmate(IV) Hydrate, [(C~6~H~5~)~3~P= N= P(C~6~H~5~)~3~]~2~[OsFCl~5~].H~2~O
Bruhn, C.; Preetz, W.; Acta Crystallographica Section C 53 (1997) 63–66; doi:10.1107/S010827019601061X

data_2005872
_publ_section_title
;
 Bis[bis(triphenylphosphoranylidene)ammonium]
 Pentachlorofluoroosmate(IV) Hydrate, [(C~6~H~5~)~3~P= N=
 P(C~6~H~5~)~3~]~2~[OsFCl~5~].H~2~O
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              63
_journal_page_last               66
_journal_paper_doi               10.1107/S010827019601061X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '(C36 H30 N1 P2)2 [Os1 Cl5 F1], H2 O1'
_chemical_formula_structural
'[(C~6~H~5~)~3~P=N=P(C~6~H~5~)~3~]~2~[OsFCl~5~](H~2~O)'
_chemical_formula_sum            'C72 H62 Cl5 F N2 O Os P4'
_chemical_formula_weight         1481.653
_chemical_name_systematic
;
Di-[bis-(triphenylphosphoranylidene)-ammonium Fluoropentachloroosmate(IV)
Hydrate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 105.11(3)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   21.374(6)
_cell_length_b                   13.072(8)
_cell_length_c                   23.771(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      10.10
_cell_measurement_theta_min      1.77
_cell_volume                     6412(5)
_computing_cell_refinement       CAD-4-PC
_computing_data_collection       'CAD-4-PC (Enraf-Nonius, 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11596
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.349
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type
'empirical via \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.728
_refine_ls_extinction_coef       0.00034(2)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.162
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment
'Water H atoms were refined with bond-length restraints, other H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11268
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(Fo^2^) + (0.0135P)^2^ + 22.6947P]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.1060
_refine_ls_wR_factor_obs         0.0760
_reflns_number_observed          6705
_reflns_number_total             11272
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            jz1142.cif
_cod_data_source_block           osfcl5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005872