Crystal structure of tetrabutylammonium sulfanilate – 1-(diaminomethylene)thiourea (1/2)
Xu, Duanjie; Wang, Baiyan; Zhu, Xin; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 59–60; doi:10.1515/ncrs-2021-0361

data_8104960
_publ_section_title
;
 Crystal structure of tetrabutylammonium sulfanilate --
 1-(diaminomethylene)thiourea (1/2)
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              59
_journal_page_last               60
_journal_paper_doi               10.1515/ncrs-2021-0361
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C16 H36 N, C6 H6 N O3 S, 2(C2 H6 N4 S)'
_chemical_formula_sum            'C26 H54 N10 O3 S3'
_chemical_formula_weight         650.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 109.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5247(5)
_cell_length_b                   10.6658(5)
_cell_length_c                   21.2970(10)
_cell_measurement_reflns_used    3814
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.67
_cell_volume                     1825.63(16)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'SHELXL-2014/7 [3]'
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXL-2014/7 [2]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9917
_diffrn_reflns_point_group_measured_fraction_full 0.816
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.260
_diffrn_reflns_theta_min         1.909
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.978
_exptl_transmission_factor_min   0.907
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0500P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.619
_reflns_Friedel_fraction_full    0.636
_reflns_Friedel_fraction_max     0.618
_reflns_number_gt                5012
_reflns_number_total             5952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0361_suppl.cif
_cod_data_source_block           090523b_0m
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               8104960
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.978