Dipyridiniomethane <i>cis</i>- and <i>trans</i>-Difluorotetrachloroosmate(IV), <i>cis</i>- and <i>trans</i>-[(C~5~H~5~N)~2~CH~2~][OsCl~4~F~2~]
Bruhn, C.; Preetz, W.; Acta Crystallographica Section C 52 (1996) 321–325; doi:10.1107/S0108270195010717

data_2004479
_publ_section_title
;
 Dipyridiniomethane <i>cis</i>- and
 <i>trans</i>-Difluorotetrachloroosmate(IV), <i>cis</i>- and
 <i>trans</i>-[(C~5~H~5~N)~2~CH~2~][OsCl~4~F~2~]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              321
_journal_page_last               325
_journal_paper_doi               10.1107/S0108270195010717
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C22 H24 Cl8 F4 N4 Os2'
_chemical_formula_structural     cis-[(C~5~H~5~N)~2~CH~2~][OsF~2~Cl~4~]
_chemical_formula_sum            'C22 H24 Cl8 F4 N4 Os2'
_chemical_formula_weight         542.23
_chemical_name_systematic
;
N,N'-methylenedipyridinium cis-difluorotetrachloroosmate(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.80(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.269(4)
_cell_length_b                   19.958(3)
_cell_length_c                   15.066(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.68
_cell_measurement_theta_min      3.19
_cell_volume                     2998.6(14)
_computing_cell_refinement       CAD-4-PC
_computing_data_collection       'CAD-4-PC (Enraf-Nonius, 1993)'
_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    'SIR92 (Altomare et al., 1992)'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4995
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.228
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type
'empirical via \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.09
_refine_diff_density_min         -1.55
_refine_ls_extinction_coef       0.00363(10)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.182
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_hydrogen_treatment
;
All H atoms refined freely with isotropic thermal parameters except for H1B
which was placed in a calculated position
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         4707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_obs          0.0290
_refine_ls_shift/esd_max         -0.7
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.031P)^2^ + 6.61P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0756
_refine_ls_wR_factor_obs         0.0642
_reflns_number_observed          3751
_reflns_number_total             4707
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1027.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2004479