Structures of six industrial benzimidazolone pigments from laboratory powder diffraction data
van de Streek, Jacco; Brüning, Jürgen; Ivashevskaya, Svetlana N.; Ermrich, Martin; Paulus, Erich F.; Bolte, Michael; Schmidt, Martin U.; Acta Crystallographica Section B 65 (2009) 200–211; doi:10.1107/S0108768108041529

data_2104315
_publ_section_title
;
 Structures of six industrial benzimidazolone pigments from laboratory
 powder diffraction data
;
_journal_coeditor_code           OG5035
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              200
_journal_page_last               211
_journal_paper_doi               10.1107/S0108768108041529
_journal_volume                  65
_journal_year                    2009
_chemical_formula_sum            'C18 H16 Cl N5 O4'
_chemical_formula_weight         401.81
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 replaces BIRZIL'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.126(2)
_cell_length_b                   5.036(2)
_cell_length_c                   42.450(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3631.0(17)
_computing_cell_refinement       'Nicolet software'
_computing_data_collection       'Nicolet software'
_computing_data_reduction        'Nicolet software'
_computing_molecular_graphics    'SHELX-97  (Sheldrick, 1997)'
_computing_publication_material  'SHELX-97  (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
  Nicolet R3 computer-controlled four circle diffractometer
;
_diffrn_measurement_method       '2theta/theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.1270
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            2394
_diffrn_reflns_theta_full        55.17
_diffrn_reflns_theta_max         55.17
_diffrn_reflns_theta_min         4.20
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 40
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.247
_refine_ls_extinction_coef       0.00042(8)
_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   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1647
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                971
_reflns_number_total             2303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5035.cif
_cod_data_source_block           BIRZIL
_cod_original_cell_volume        3631(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2104315
_cod_database_fobs_code          2104315