An unusual single-crystal-to-single-crystal [2 + 2] photocyclisation reaction of a TTF-arylnitrile derivative
Hayward, John J.; Gumbau-Brisa, Roger; Alberola, Antonio; Clarke, Caroline S.; Rawson, Jeremy M.; Pilkington, Melanie; CrystEngComm 16 (2014) 7268–; doi:10.1039/C4CE00346B

data_7217437
_publ_section_title
;
 An unusual single-crystal-to-single-crystal [2 + 2] photocyclisation
 reaction of a TTF-arylnitrile derivative
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7268
_journal_paper_doi               10.1039/C4CE00346B
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         '0.8(C26 H14 N2 S8), 0.4 (C13 H7 N S4)'
_chemical_formula_sum            'C13 H7 N S4'
_chemical_formula_weight         305.44
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.274(2)
_cell_length_b                   8.2761(17)
_cell_length_c                   27.958(6)
_cell_measurement_reflns_used    50685
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     2596.7(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'thin slice omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12885
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.864
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related equivalents
Sortv (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0027(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         4165
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+14.2266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3460
_reflns_number_total             4165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7215216
_cod_data_source_file            c4ce00346b2.cif
_cod_data_source_block           cmpnd1
_cod_database_code               7217437
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-3
_shelx_res_checksum              77133