A new supramolecular tecton: the crucial impact of the polycation charge and geometry of H-bonds on the structure and properties of halometallates in the solid state.
Shestimerova, Tatiana A.; Medved'ko, Aleksei V.; Bykov, Mikhail A.; Kalinin, Mikhail A.; Metlin, Mikhail T.; Taydakov, Ilya V.; Gontcharenko, Victoria E.; Wei, Zheng; Dikarev, Evgeny V.; Vatsadze, Sergey Z.; Shevelkov, Andrei V.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6983–6992; doi:10.1039/d5dt00318k

data_7718420
_publ_section_title
;
 A new supramolecular tecton: the crucial impact of the polycation charge
 and geometry of H-bonds on the structure and properties of halometallates
 in the solid state.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6983
_journal_page_last               6992
_journal_paper_doi               10.1039/d5dt00318k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'I6 Sb, 3(H2 O), C10 H22 N3'
_chemical_formula_sum            'C10 H28 I6 N3 O3 Sb'
_chemical_formula_weight         1121.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-05 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3295(6)
_cell_length_b                   8.7843(2)
_cell_length_c                   11.5066(3)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.495
_cell_measurement_theta_min      2.392
_cell_volume                     2560.24(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'phi and omega shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26491
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.326
_exptl_absorpt_correction_T_max  0.4422
_exptl_absorpt_correction_T_min  0.1705
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1223 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.3856.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0219
_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^)+5.9490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3701
_reflns_number_total             3962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00318k2.cif
_cod_data_source_block           sb
_cod_depositor_comments
'Adding full bibliography for 7718420--7718421.cif.'
_cod_database_code               7718420
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H10A(0.5) H10B(0.5)
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              73527
_shelx_hkl_checksum              763
_olex2_submission_special_instructions 'No special instructions were received'