Structure determination of seven phases and solvates of Pigment Yellow 183 and Pigment Yellow 191 from X-ray powder and single-crystal data
Ivashevskaya, Svetlana N.; van de Streek, Jacco; Djanhan, Juste E.; Brüning, Jürgen; Alig, Edith; Bolte, Michael; Schmidt, Martin U.; Blaschka, Peter; Höffken, Hans Wolfgang; Erk, Peter; Acta Crystallographica Section B 65 (2009) 212–222; doi:10.1107/S0108768109001827

data_2104323
_publ_section_title
;
 Structure determination of seven phases and solvates of Pigment Yellow
 183 and Pigment Yellow 191 from X-ray powder and single-crystal data
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              212
_journal_page_last               222
_journal_paper_doi               10.1107/S0108768109001827
_journal_volume                  65
_journal_year                    2009
_chemical_formula_sum            'C16 H16 Ca Cl2 N4 O10 S2'
_chemical_formula_weight         599.43
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.605(19)
_cell_angle_beta                 92.35(3)
_cell_angle_gamma                102.77(3)
_cell_formula_units_Z            2
_cell_length_a                   5.574(3)
_cell_length_b                   10.925(3)
_cell_length_c                   18.801(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      115
_cell_measurement_theta_min      2
_cell_volume                     1100.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3144
_diffrn_reflns_theta_full        55.42
_diffrn_reflns_theta_max         55.42
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    7.087
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_type   DifabsEmpirical(SHELXA)
_exptl_absorpt_process_details   'theta/2theta scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.475
_refine_ls_extinction_coef       0.0004(3)
_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   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         2790
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                1925
_reflns_number_total             2790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5036.cif
_cod_data_source_block           PY183beta
_cod_original_cell_volume        1100.8(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2104323