Experimental and theoretical studies into the structural perturbations between neutral, oxidised and reduced forms of 1,4-dithiinoquinoxaline derivatives
Skabara, Peter J.; Berridge, Rory; Prescott, Karen; Goldenberg, Leonid M.; Ortí, Enrique; Viruela, Rafael; Pou-Amérigo, Rosendo; Batsanov, Andrei S.; Howard, Judith A. K.; Coles, Simon J.; Hursthouse, Michael B.; Journal of Materials Chemistry 10 (2000) 2448–; doi:10.1039/b003910l

data_7203991
_publ_section_title
;
 Experimental and theoretical studies into the structural perturbations
 between neutral, oxidised and reduced forms of 1,4-dithiinoquinoxaline
 derivatives
;
_journal_issue                   11
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2448
_journal_paper_doi               10.1039/b003910l
_journal_volume                  10
_journal_year                    2000
_chemical_formula_sum            'C12 H6 N2 S3'
_chemical_formula_weight         274.37
_chemical_melting_point          435.1(10)
_chemical_name_systematic
; 
 thieno[3',4'-d:5,6][1,4]dithiino[2,3-b]quinoxaline 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                101.96(1)
_cell_angle_beta                 95.96(1)
_cell_angle_gamma                104.09(1)
_cell_formula_units_Z            2
_cell_length_a                   6.876(2)
_cell_length_b                   9.361(3)
_cell_length_c                   9.508(3)
_cell_measurement_reflns_used    511
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      12.0
_cell_volume                     573.0(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'SMART 1K 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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3221
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_correction_T_min  0.7644
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       pinakoid
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0185(40)
_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_all   1.121
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_obs          0.0286
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.42P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0819
_refine_ls_wR_factor_obs         0.0764
_reflns_number_observed          1693
_reflns_number_total             1793
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b003910l.txt
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '161-163 deg.C' was changed to
'435.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.42P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.42P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        573.0(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203991