1,1'-[(1,3-Dihydroxypropane-2,2-diyl)dimethylene]dipyridinium bis(hexafluorophosphate)
Yuan, Ai-lin; Zheng, Chun-ling; Zhuang, Ling-hua; Wang, Chang-sheng; Wang, Guo-wei; Acta Crystallographica Section E 67 (2011) o1104–; doi:10.1107/S1600536811013080

data_2230033
_publ_section_title
;
 1,1'-[(1,3-Dihydroxypropane-2,2-diyl)dimethylene]dipyridinium
 bis(hexafluorophosphate)
;
_journal_coeditor_code           IM2266
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1104
_journal_paper_doi               10.1107/S1600536811013080
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C15 H20 N2 O2 2+ , 2 P F6 -'
_chemical_formula_moiety         'C15 H20 N2 O2 2+ , 2(F6 P -)'
_chemical_formula_sum            'C15 H20 F12 N2 O2 P2'
_chemical_formula_weight         550.27
_chemical_melting_point_gt       508
_chemical_melting_point_lt       510
_chemical_name_systematic
;
1,1'-[(1,3-Dihydroxypropane-2,2-diyl)dimethylene]dipyridinium
bis(hexafluorophosphate)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.955(2)
_cell_length_b                   13.796(3)
_cell_length_c                   12.707(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      9
_cell_volume                     2087.3(8)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo,1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4027
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.9072
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.263
_refine_ls_extinction_coef       0.0115(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0676P)^2^+0.8940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                2564
_reflns_number_total             3835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2266.cif
_cod_data_source_block           I
_cod_original_cell_volume        2087.3(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230033
_cod_database_fobs_code          2230033