3,3'-Dimethyl-1,1'-[(1,3-dihydroxypropane-2,2-diyl)dimethylidene]diimidazolium bis(hexafluorophosphate)
Yuan, Ai-Lin; Wang, Chang-Sheng; Zhuang, Ling-Hua; Wang, Guo-Wei; Acta Crystallographica Section E 66 (2010) o3282–; doi:10.1107/S1600536810047677

data_2228531
_publ_section_title
;
 3,3'-Dimethyl-1,1'-[(1,3-dihydroxypropane-2,2-diyl)dimethylidene]diimidazolium
 bis(hexafluorophosphate)
;
_journal_coeditor_code           RK2245
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3282
_journal_paper_doi               10.1107/S1600536810047677
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H22 N4 O2 2+, 2P F6 -'
_chemical_formula_moiety         'C13 H22 N4 O2 2+, 2(F6 P -)'
_chemical_formula_sum            'C13 H22 F12 N4 O2 P2'
_chemical_formula_weight         556.29
_chemical_melting_point_gt       497
_chemical_melting_point_lt       500
_chemical_name_systematic
;
3,3'-Dimethyl-1,1'-[(1,3-dihydroxypropane-2,2-diyl)dimethylidene]diimidazolium
bis(hexafluorophosphate)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.622(3)
_cell_length_b                   12.504(3)
_cell_length_c                   12.165(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      9
_cell_volume                     2224.2(8)
_computing_cell_refinement       '<i>CAD-4</i> (Enraf--Nonius, 1989)'
_computing_data_collection       '<i>CAD-4</i> (Enraf--Nonius, 1989)'
_computing_data_reduction        '<i>XCAD4</i> (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4082
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.9399
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.168
_refine_ls_abs_structure_details 'Flack (1983), 1930 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(16)
_refine_ls_extinction_coef       0.105(11)
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                1861
_reflns_number_total             2152
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2245.cif
_cod_data_source_block           I
_cod_database_code               2228531
_cod_database_fobs_code          2228531