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_1571978
_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         'C4 H10 O, 2(C16 H18 I), 2(C16 H36 N), Mo8 O26'
_chemical_formula_sum            'C68 H118 I2 Mo8 N2 O27'
_chemical_formula_weight         2416.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 98.520(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9198(3)
_cell_length_b                   19.5787(4)
_cell_length_c                   14.9460(3)
_cell_measurement_reflns_used    12603
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8990
_cell_measurement_theta_min      2.5180
_cell_volume                     4607.09(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.191
_diffrn_reflns_theta_min         2.080
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       block
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0341P)^2^+8.3975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9065
_reflns_number_total             10435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01695e2.cif
_cod_data_source_block           Xy_DMF
_cod_depositor_comments
'Adding full bibliography for 1571977--1571981.cif.'
_cod_database_code               1571978
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.616
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
 H2SC(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
 O1S(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C3S(H3SA,H3SB), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA,
 H3BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB), C13B(H13A,H13B),
 C14B(H14A,H14B), C15B(H15A,H15B), C9B(H9BA,H9BB), C10B(H10A,H10B), C11B(H11A,
 H11B)
2.b Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C16A(H16D,H16E,H16F), C15A(H15C,
 H15D,H15E), C13A(H13C,H13D,H13E), C14A(H14C,H14D,H14E), C4B(H4BA,H4BB,H4BC),
 C8B(H8BA,H8BB,H8BC), C16B(H16A,H16B,H16C), C12B(H12A,H12B,H12C)
2.c Aromatic/amide H refined with riding coordinates:
 C11A(H11C), C10A(H10C), C8A(H8A), C3A(H3A), C4A(H4A), C6A(H6A)
;
_shelx_res_checksum              34831
_shelx_hkl_checksum              52152
_olex2_submission_special_instructions 'No special instructions were received'