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_2004480
_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         'C11 H12 Cl4 F2 N2 Os'
_chemical_formula_structural     trans-[(C~5~H~5~N)~2~CH~2~][OsF~2~Cl~4~]
_chemical_formula_sum            'C11 H12 Cl4 F2 N2 Os'
_chemical_formula_weight         542.23
_chemical_name_systematic
;
 N,N'-methylenedipyridinium trans-difluorotetrachloroosmate(IV)
;
_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                89.649(7)
_cell_angle_beta                 70.346(6)
_cell_angle_gamma                75.112(6)
_cell_formula_units_Z            2
_cell_length_a                   7.7562(5)
_cell_length_b                   10.0127(8)
_cell_length_c                   11.0057(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.85
_cell_measurement_theta_min      4.01
_cell_volume                     774.86(11)
_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  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3007
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  240min
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.928
_exptl_absorpt_correction_T_max  1.0
_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    2.324
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .69
_refine_diff_density_min         -.46
_refine_ls_extinction_coef       0.0183(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.132
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_obs          0.0148
_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^(F~o~^2^) + (0.018P)^2^ + 0.31P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0389
_refine_ls_wR_factor_obs         0.0343
_reflns_number_observed          2354
_reflns_number_total             2795
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1027.cif
_cod_data_source_block           II
_cod_original_cell_volume        774.76(14)
_cod_database_code               2004480