Crystal structures of two unexpected products of vicinal diamines left to crystallize in acetone.
Dival, Bruno; Pitinato, Leonardo; Develly, Letícia; Oliveira, Willian X. C.; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624007320

data_2312588
_publ_section_title
;
 Crystal structures of two unexpected products of vicinal diamines left to
 crystallize in acetone.
;
_journal_coeditor_code           EF3057
_journal_issue                   9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624007320
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C26 H31 N4 O4 S2 +, Cl 1, 0.3H2 O1'
_chemical_formula_moiety         'C26 H31 N4 O4 S2 +, Cl 1, 0.3(H2 O1)'
_chemical_formula_sum            'C26 H31.6 Cl N4 O4.3 S2'
_chemical_formula_weight         568.52
_chemical_name_systematic
'2,2,4-Trimethyl-8,9-bis(4-methylbenzenesulfonamido)-2,3-dihydro-5<i>H</i>-1,5-benzodiazepin-1-ium chloride 0.3-hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 103.667(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0993(2)
_cell_length_b                   13.4307(2)
_cell_length_c                   17.3586(3)
_cell_measurement_reflns_used    11735
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.1200
_cell_measurement_theta_min      3.7270
_cell_volume                     2740.94(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
SHELXL2019 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus et al., 2007)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24340
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.676
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.997
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                4787
_reflns_number_total             5837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3057sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C26 H31.60 Cl N4 O4.30 S2'
_cod_database_code               2312588
_shelx_hkl_checksum              6509
_shelx_res_checksum              71596
_cod_database_fobs_code 2312588