X-ray Crystallographic Study on Single-Crystalline Photochromism of Bis(2,5-dimethyl-3-thienyl)perfluorocyclopentene
Taro Yamada; Seiya Kobatake; Keishi Muto; Masahiro Irie; Journal of the American Chemical Society 122 (2000) 1589–1592; doi:10.1021/ja993289x

data_4115937
_publ_contact_author
;
    Prof. Masahiro Irie
    Department of Chemistry and Biochemistry
    Graduate School of Engineering
    Kyushu University
    6-10-1 Hakozaki, Higashi-ku
    Fukuoka  812-8581, Japan
;
_publ_contact_author_email       irie@cstf.kyushu-u.ac.jp
_publ_contact_author_fax         +81-92-642-3568
_publ_contact_author_phone       +81-92-642-3556
_publ_section_title
;
 X-ray Crystallographic Study on Single-Crystalline Photochromism of
 Bis(2,5-dimethyl-3-thienyl)perfluorocyclopentene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1589
_journal_page_last               1592
_journal_paper_doi               10.1021/ja993289x
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C17 H14 F6 S2'
_chemical_formula_weight         396.40
_chemical_name_systematic
;

8,8,9,9,10,10-hexafluoro-trans-1,2,4,14-tetramethyl-3,15-dithiatetracyclo[10
.3.
pentadeca-4,6(7),11(12),13-tetraene

3-(2-(2,5-dimethyl(3-thienyl))-3,3,4,4,5,5-hexafluorocyclopent-1-enyl)-2,5-d
imethylthiophene
;
_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                 103.639(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2674(12)
_cell_length_b                   24.787(5)
_cell_length_c                   11.381(2)
_cell_measurement_reflns_used    4245
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.5
_cell_volume                     1718.2(6)
_computing_cell_refinement       'SAINT v6.0 (Bruker)'
_computing_data_collection       'SMART v5.0 (Bruker)'
_computing_data_reduction        'XPREP v5.1 (Bruekr)'
_computing_molecular_graphics    'XP v5.0 (bruker)'
_computing_publication_material  'XP v5.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9413
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0.7
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.831001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.8191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                2741
_reflns_number_total             3572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993289x_1.cif
_cod_data_source_block           1bprime
_cod_database_code               4115937