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_7215218
_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         'C12 H6 N2 S4'
_chemical_formula_sum            'C12 H6 N2 S4'
_chemical_formula_weight         306.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.393(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9337(4)
_cell_length_b                   11.3951(9)
_cell_length_c                   27.644(2)
_cell_measurement_reflns_used    3915
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.84
_cell_volume                     1238.77(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 1.004
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.004
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17919
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.004
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.787
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0849
_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^)+(0.1541P)^2^+9.6439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2579
_refine_ls_wR_factor_ref         0.2704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1908
_reflns_number_total             2213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00346b2.cif
_cod_data_source_block           cmpnd3
_cod_depositor_comments
'Adding full bibliography for 7215216--7215218.cif.'
_cod_database_code               7215218
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2013-3
_shelx_res_checksum              74329