Structural and Physical Properties of a Series of 7,7,8,8-Tetracyanoquinodimethane Salts with Dications Bearing Two Terminal Pyridinium Rings
Kubota, Hiroyuki; Takahashi, Yukihiro; Harada, Jun; Inabe, Tamotsu; Crystal Growth & Design 14 (2014) 5575–; doi:10.1021/cg500820v

data_4512049
_publ_section_title
;
 Structural and Physical Properties of a Series of
 7,7,8,8-Tetracyanoquinodimethane Salts with Dications Bearing Two
 Terminal Pyridinium Rings
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5575
_journal_paper_doi               10.1021/cg500820v
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C12 H14 N2, 3(C12 H4 N4)'
_chemical_formula_sum            'C48 H26 N14'
_chemical_formula_weight         798.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                83.1512(14)
_cell_angle_beta                 76.1582(14)
_cell_angle_gamma                76.0042(14)
_cell_formula_units_Z            1
_cell_length_a                   8.0675(9)
_cell_length_b                   8.0934(9)
_cell_length_c                   15.5631(18)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.494
_cell_measurement_theta_min      2.599
_cell_volume                     955.33(19)
_computing_cell_refinement       'Bruker SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18232
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.350
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1336 before and 0.0702 after correction. The Ratio of minimum to maximum transmission is 0.5428. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.1607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3723
_reflns_number_total             4395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500820v_si_002.cif
_cod_data_source_block           C2BPy_(TCNQ)3
_cod_depositor_comments
'Adding full bibliography for 4512048--4512055.cif.'
_cod_original_cell_volume        955.34(19)
_cod_database_code               4512049
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6B,H7A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H8), C12(H9), C14(H10), C15(H11),
 C23(H12), C24(H13)
;
_shelx_res_checksum              99414
_shelx_hkl_checksum              54964