Crystallographic and molecular mechanics investigation of an order–disorder transition and dimorphism in 5<i>H</i>,10<i>H</i>-dithiolo[2,3-<i>b</i>]-2,5-benzodithiocine-2-thione
Chohan, Zahid H.; Harrison, William T. A.; Howie, R. Alan; Milne, Bruce F.; Wardell, James L.; Acta Crystallographica Section B 56 (2000) 1011–1017; doi:10.1107/S0108768100010636

data_2102168
_publ_section_title
;
 Crystallographic and molecular mechanics investigation of an
 order--disorder transition and dimorphism in
 5<i>H</i>,10<i>H</i>-dithiolo[2,3-<i>b</i>]-2,5-benzodithiocine-2-thione
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1011
_journal_page_last               1017
_journal_paper_doi               10.1107/S0108768100010636
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C11 H8 S5'
_chemical_formula_sum            'C11 H8 S5'
_chemical_formula_weight         300.47
_chemical_melting_point          479
_chemical_name_systematic
;5H,10H-Dithiolo[2,3-b][2,5]benzodithiocine-2-thione (C-centred monoclinic
 form)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 102.80(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.075(8)
_cell_length_b                   11.825(8)
_cell_length_c                   9.063(6)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.9
_cell_measurement_theta_min      10.8
_cell_volume                     1261.9(15)
_computing_cell_refinement       'Nicolet P3 software (Nicolet, 1980)'
_computing_data_collection       'Nicolet P3 software (Nicolet, 1980)'
_computing_data_reduction        'RDNIC (Howie, 1980)'
_computing_molecular_graphics    'ORTEX (McArdle, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.498
_diffrn_measured_fraction_theta_max 0.498
_diffrn_measurement_device_type  'Nicolet P3'
_diffrn_measurement_method       \q--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2034
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   \y
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.95
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0535P)^2^+8.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2153
_reflns_number_gt                1166
_reflns_number_total             1932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm0027.cif
_cod_data_source_block           alphaprime-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+8.1837P] 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^)+(0.0535P)^2^+8.1837P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2102168
_cod_database_fobs_code          2102168