Key-to-lock halogen bond-based tetragonal pyramidal association of iodonium cations with the lacune rims of beta-octamolybdate.
Soldatova, Natalia S.; Radzhabov, Amirbek D.; Ivanov, Daniil M.; Burguera, Sergi; Frontera, Antonio; Abramov, Pavel A.; Postnikov, Pavel S.; Kukushkin, Vadim Yu; Chemical science 15 (2024) 12459–12472; doi:10.1039/d4sc01695e

data_1571980
_publ_section_title
;
 Key-to-lock halogen bond-based tetragonal pyramidal association of
 iodonium cations with the lacune rims of beta-octamolybdate.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              12459
_journal_page_last               12472
_journal_paper_doi               10.1039/d4sc01695e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '4(C12 H10 I), 2(C2 H6 O S), 2(Mo4 O13)'
_chemical_formula_sum            'C52 H52 I4 Mo8 O28 S2'
_chemical_formula_weight         2464.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-21 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                100.4640(10)
_cell_angle_beta                 98.6000(10)
_cell_angle_gamma                115.2890(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0495(3)
_cell_length_b                   14.4726(3)
_cell_length_c                   20.8666(5)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5971
_cell_measurement_theta_min      2.2755
_cell_volume                     3387.69(14)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54964
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.597
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_description       plate
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.550
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         18461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0285P)^2^+5.1147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15472
_reflns_number_total             18461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01695e2.cif
_cod_data_source_block           Ph_DMSO
_cod_depositor_comments
'Adding full bibliography for 1571977--1571981.cif.'
_cod_database_code               1571980
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.630
_olex2_refinement_description
;
1. Others
 Fixed Sof: S2S(0.3) O3S(0.3) C4S(0.3) H4SA(0.3) H4SB(0.3) H4SC(0.3) C3S(0.3)
 H3SA(0.3) H3SB(0.3) H3SC(0.3) S3S(0.7) O2S(0.7) C6S(0.7) H6SA(0.7) H6SB(0.7)
 H6SC(0.7) C5S(0.7) H5SA(0.7) H5SB(0.7) H5SC(0.7)
2.a Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C3S(H3SA,H3SB,
 H3SC), C6S(H6SA,H6SB,H6SC), C5S(H5SA,H5SB,H5SC)
2.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C2D(H2D), C3A(H3A), C3B(H3B), C3D(H3D), C2E(H2E),
 C4A(H4A), C4B(H4B), C4D(H4D), C3E(H3E), C5A(H5A), C5B(H5B), C5D(H5D), C4E(H4E),
  C6A(H6A), C6B(H6B), C6D(H6D), C5E(H5E), C6E(H6E), C8A(H8A), C8B(H8B),
 C8D(H8D), C9A(H9A), C9B(H9B), C9D(H9D), C8E(H8E), C10A(H10A), C10B(H10B),
 C10D(H10D), C9E(H9E), C11A(H11A), C11B(H11B), C11D(H11D), C10E(H10E),
 C12A(H12A), C12B(H12B), C12D(H12D), C11E(H11E), C12E(H12E)
;
_shelx_res_checksum              49127
_shelx_hkl_checksum              45977
_olex2_submission_special_instructions 'No special instructions were received'