Photoinduced electron transfer in porous organic salt crystals impregnated with fullerenes
Tetsuya; Hasegawa; Kei; Ohkubo; Ichiro; Hisaki; Mikiji; Miyata; Norimitsu; Tohnai; Shunichi; Fukuzumi; Chem.Commun. 52 (2016) 7928–; doi:

data_7119441
_publ_section_title
;
 Photoinduced electron transfer in porous organic salt crystals
 impregnated with fullerenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7928
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C20 H13 O3 S, C19 H18 N'
_chemical_formula_sum            'C39 H31 N O3 S'
_chemical_formula_weight         593.74
_chemical_name_systematic        SPA/TPMA/DCB
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c'
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-04-28 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   25.9455(3)
_cell_length_b                   25.9455(3)
_cell_length_c                   24.2457(2)
_cell_measurement_reflns_used    87845
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.245
_cell_measurement_theta_min      1.656
_cell_volume                     16321.5(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       DENZO
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement.details
' 1.00 degrees, 10.0 sec, detector distance 96.00 mm'
_diffrn_measurement_device_type  'SPring-8 BL26B1'
_diffrn_measurement.method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75000
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_Laue_measured_fraction_full 0.840
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            87845
_diffrn_reflns_point_group_measured_fraction_full 0.840
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         27.245
_diffrn_reflns_theta_min         1.656
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4992.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as guest
atoms were unsuccessful, although this crystal includ ortho_dichlorobenzene.
The data were corrected for disordered
electron density through use of the
SQUEEZE procedure (Sluis, P. van der;
Spek, A. L. Acta Crystallogr. 1990,
A46, 194-201) as implemented in PLATON
(Spek, A.L. Acta Crystallogr. 1990, A46, C34.
PLATON C a multipurpose crystallographic tool.
Utrecht University, Utrecht, The Netherlands).
A total solvent-accessible
void volume of 5540.0 A^3^ with a total electron count of 1295
(consistent with ca. one molecule of oDCB per formula
characterized by thermo-gravimetric analysis) was found in the unit cell.
;
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6314
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1063P)^2^+9.6595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4466
_reflns_number_total             6314
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6cc02377k2.cif
_cod_data_source_block           oDCB
_cod_database_code               7119441
_shelx_res_checksum              58433
_platon_squeeze_void_probe_radius 1.20