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_1571981
_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         '2(C16 H36 N), 2(C16 H18 I), Mo8 O26'
_chemical_formula_sum            'C64 H108 I2 Mo8 N2 O26'
_chemical_formula_weight         2342.84
_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                 110.5660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7278(3)
_cell_length_b                   16.3027(3)
_cell_length_c                   18.7455(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.4625
_cell_measurement_theta_min      2.4389
_cell_volume                     4500.13(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         2.439
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6435
_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    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         13758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+2.0609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11673
_reflns_number_total             13758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01695e2.cif
_cod_data_source_block           1_a_sq
_cod_depositor_comments
'Adding full bibliography for 1571977--1571981.cif.'
_cod_database_code               1571981
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C5B(H5BA,H5BB), C9B(H9B1,H9B2), C6B(H6BA,H6BB), C15B(H15D,
 H15E), C13B(H13A,H13B), C11B(H11B,H11C), C3B(H3BA,H3BB), C2B(H2BA,H2BB),
 C10B(H10A,H10B), C14B(H14D,H14E), C7B(H7BA,H7BB)
1.b Me refined with riding coordinates:
 C8B(H8BA,H8BB,H8BC), C12B(H12A,H12B,H12C), C14A(H14A,H14B,H14C), C16B(H16D,
 H16E,H16F), C4B(H4BA,H4BB,H4BC)
1.c Aromatic/amide H refined with riding coordinates:
 C8A(H8AA), C3A(H3AA), C6A(H6AA), C11A(H11A), C10A(H10C), C4A(H4AA)
1.d Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C13A(H13C,H13D,H13E), C16A(H16A,H16B,H16C)
;
_shelx_res_checksum              45572
_shelx_hkl_checksum              47068
_shelx_fab_checksum              6727
_olex2_submission_special_instructions 'No special instructions were received'