First crystal structure of a Pigment Red 52 compound: DMSO solvate hydrate of the monosodium salt
Tapmeyer, Lukas; Eisenbeil, Daniel; Bolte, Michael; Schmidt, Martin U.; Acta Crystallographica Section E 77 (2021) 402–405; doi:10.1107/S2056989021002577

data_2243784
_publ_section_title
;
 First crystal structure of a Pigment Red 52 compound: DMSO solvate
 hydrate of the monosodium salt
;
_journal_coeditor_code           YK2145
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              402
_journal_page_last               405
_journal_paper_doi               10.1107/S2056989021002577
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'Na +, C18 H12 Cl N2 O6 S -, C2 H6 O S, H2 O'
_chemical_formula_sum            'C20 H20 Cl N2 Na O8 S2'
_chemical_formula_weight         538.94
_chemical_name_common
'P.R.52 monosodium DMSO-monosolvate monohydrate'
_chemical_name_systematic
;Monosodium
2-[2-(3-carboxy-2-oxo-1,2-dihydronaphthalen-1-ylidene)hydrazin-1-yl]-5-chloro-4-methylbenzenesulfonate
dimethyl sulfoxide monosolvate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                104.844(5)
_cell_angle_beta                 97.478(5)
_cell_angle_gamma                95.404(6)
_cell_formula_units_Z            2
_cell_length_a                   5.7347(4)
_cell_length_b                   10.9336(8)
_cell_length_c                   18.4692(12)
_cell_measurement_reflns_used    12767
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.4
_cell_volume                     1100.00(14)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2001)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2001)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2001)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2015b) and Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCif (Westrip, 2010)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.402
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-Area; Stoe & Cie, 2001)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0429P)^2^+0.0815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                2992
_reflns_number_total             3864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2145sup1.cif
_cod_data_source_block           I
_cod_database_code               2243784
_cod_database_fobs_code          2243784
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              13950
_shelx_res_checksum              8317