Redox-active tubular frameworks with TTF: self-assemblies by complementary hydrogen-bonds and π-stacks of TTF-phenyluracil
Murata, Tsuyoshi; Maki, Suguru; Ohmoto, Makoto; Miyazaki, Eigo; Umemoto, Yoshikazu; Nakasuji, Kazuhiro; Morita, Yasushi; CrystEngComm 13 (2011) 6880–; doi:10.1039/c1ce05794d

data_7206743
_publ_section_title
;
 Redox-active tubular frameworks with TTF: self-assemblies by
 complementary hydrogen-bonds and \p-stacks of TTF-phenyluracil
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              6880
_journal_paper_doi               10.1039/c1ce05794d
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C18.96 H15.92 N2 O2.74 S4'
_chemical_formula_weight         443.90
_chemical_name_common            TTFPhU-THF
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.863(8)
_cell_length_b                   5.722(3)
_cell_length_c                   21.510(9)
_cell_measurement_reflns_used    10935
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.06
_cell_volume                     2069.4(17)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15488
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.7454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             918.5
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                2597
_reflns_number_total             4269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05794d.txt
_cod_data_source_block           TTF-PhU_THF
_cod_original_cell_volume        2069.4(16)
_cod_database_code               7206743