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_7250412
_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 Na3 O13 S3, 2(C H6 N3), O'
_chemical_formula_sum            'C8 H19 N6 Na3 O14 S3'
_chemical_formula_weight         585.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-01
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8318(9)
_cell_length_b                   12.1850(9)
_cell_length_c                   25.4468(18)
_cell_measurement_reflns_used    2116
_cell_measurement_temperature    296.15(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.44
_cell_volume                     3978.7(5)
_computing_cell_refinement       'ShelXL (Sheldrick, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14758
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9158
_exptl_absorpt_correction_T_min  0.9020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_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    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2116
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+11.5810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                1792
_reflns_number_total             2116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5ce00320b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7250411--7250413.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               7250412
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Rigid bond restraints
 C6A, N3A, N4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C6A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(N4A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6A) = Uanis(C6B)
Uanis(N3A) = Uanis(N4B)
Uanis(N4A) = Uanis(N3B)
4. Same fragment restrains
{C5, N1, N2} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C6B, N4B, N3B}
{C5, N1, N2} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C6A, N3A, N4A}
5. Others
 Sof(N3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(C6B)=Sof(N4B)=Sof(H4BA)=Sof(H4BB)=0.5*(1-FVAR(2))
 Sof(C6A)=Sof(N3A)=Sof(H3AA)=Sof(H3AB)=0.5*FVAR(2)
 Sof(N4A)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
 Fixed Sof: O1W(0.5)
6.a Everything fixed:
 H1A
6.b Ternary CH refined with riding coordinates:
 C1(H1)
6.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3A(H3AA,H3AB), N4A(H4AA,H4AB), N4B(H4BA,H4BB), N3B(H3BA,H3BB)
;
_shelx_res_checksum              99309
_olex2_submission_special_instructions 'No special instructions were received'