Highly bent crystals formed by restrained π-stacked columns connected via alkylene linkers with variable conformations
Chou, Chih-Ming; Nobusue, Shunpei; Saito, Shohei; Inoue, Daishi; Hashizume, Daisuke; Yamaguchi, Shigehiro; Chem. Sci. 6 (2015) 2354–; doi:10.1039/C4SC03849E

data_1518664
_publ_section_title
;
 Highly bent crystals formed by restrained \p-stacked columns connected
 via alkylene linkers with variable conformations
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2354
_journal_paper_doi               10.1039/C4SC03849E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C66 H52 S4'
_chemical_formula_sum            'C66 H52 S4'
_chemical_formula_weight         973.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-15 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.599(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.430(5)
_cell_length_b                   5.2798(12)
_cell_length_c                   24.950(6)
_cell_measurement_reflns_used    2480
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      96.87
_cell_measurement_theta_min      6.83
_cell_volume                     2624.8(11)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32019
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.210
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4770
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2251
_refine_ls_wR_factor_ref         0.2686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1565
_reflns_number_total             4770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03849e2.cif
_cod_data_source_block           1c_high_temp
_cod_depositor_comments
'Adding full bibliography for 1518661--1518665.cif.'
_cod_database_code               1518664
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              15844
_shelx_hkl_checksum              12343