Influence of organic and alkali metal cations over a crystal lattice of the benzenetrihydroxy trisulfonate ligand
Tiwari, Ranjay K.; Kumar, Jitendra; Behera, J. N.; CrystEngComm 27 (2025) 4116–4124; doi:10.1039/D5CE00320B

data_7250411
_publ_section_title
;
 Influence of organic and alkali metal cations over a crystal lattice of
 the benzenetrihydroxy trisulfonate ligand
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4116
_journal_page_last               4124
_journal_paper_doi               10.1039/D5CE00320B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C6 H3 O12 S3, C3 H6 N6, 3(C3 H7 N6), 4(H2 O)'
_chemical_formula_sum            'C18 H38 N24 O16 S3'
_chemical_formula_weight         942.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-23 deposited with the CCDC.	2025-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.431(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8237(6)
_cell_length_b                   12.2192(4)
_cell_length_c                   18.3904(7)
_cell_measurement_reflns_used    7406
_cell_measurement_temperature    296.15(3)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2
_cell_volume                     3626.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15(3)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0598P)^2^+2.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5857
_reflns_number_total             7406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00320b2.cif
_cod_data_source_block           adduct1
_cod_depositor_comments
'Adding full bibliography for 7250411--7250413.cif.'
_cod_database_code               7250411
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Restrained distances
 O1W-H1WA
 0.82 with sigma of 0.02
 O1W-H1WB
 0.82 with sigma of 0.02
 O2W-H2WA
 0.82 with sigma of 0.02
 O2W-H2WB
 0.82 with sigma of 0.02
 O3W-H3WB
 0.82 with sigma of 0.02
 O3W-H3WA
 0.82 with sigma of 0.02
 O4W-H4WA
 0.82 with sigma of 0.02
 O4W-H4WB
 0.82 with sigma of 0.02
 H1WA-H1WB
 1.33 with sigma of 0.04
 H2WA-H2WB
 1.33 with sigma of 0.04
 H3WB-H3WA
 1.33 with sigma of 0.04
 H4WA-H4WB
 1.33 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N5B(H5B), N5C(H5C), N6D(H6D)
3.b X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB), N1C(H1CA,H1CB), N1D(H1DA,H1DB), N2A(H2AA,
 H2AB), N2B(H2BA,H2BB), N2C(H2CA,H2CB), N2D(H2DA,H2DB), N3A(H3AA,H3AB),
 N3B(H3BA,H3BB), N3C(H3CA,H3CB), N3D(H3DA,H3DB)
;
_shelx_res_checksum              62696
_olex2_submission_special_instructions 'No special instructions were received'