The role of sulfur interactions in crystal architecture: experimental and quantum theoretical studies on hydrogen, halogen, and chalcogen bonds in trithiocyanuric acid–pyridine N-oxide co-crystals
Wzgarda-Raj, Kinga; Palusiak, Marcin; Wojtulewski, Sławomir; Rybarczyk-Pirek, Agnieszka J.; CrystEngComm 23 (2021) 324–334; doi:10.1039/D0CE01319F

data_7241493
_publ_section_title
;
 The role of sulfur interactions in crystal architecture: experimental and
 quantum theoretical studies on hydrogen, halogen, and chalcogen bonds in
 trithiocyanuric acid--pyridine N-oxide co-crystals
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              324
_journal_page_last               334
_journal_paper_doi               10.1039/D0CE01319F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '2(C3 H3 N3 S3), C5 H4 Br N O, H2 O'
_chemical_formula_sum            'C11 H12 Br N7 O2 S6'
_chemical_formula_weight         546.54
_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   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-21 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                80.082(2)
_cell_angle_beta                 85.993(2)
_cell_angle_gamma                80.258(2)
_cell_formula_units_Z            4
_cell_length_a                   6.9760(2)
_cell_length_b                   11.2345(2)
_cell_length_c                   26.3305(5)
_cell_measurement_reflns_used    20459
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3420
_cell_measurement_theta_min      3.3690
_cell_volume                     2001.65(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4052
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.499
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.880
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.00020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+1.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6790
_reflns_number_total             7385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01319f2.cif
_cod_data_source_block           structure_III
_cod_depositor_comments
;
Adding full bibliography for 7241492--7241495.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C22 H24 Br2 N14 O4 S12'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1093.09
_cod_database_code               7241493
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              68183