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_1571977
_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), 0.14(I), Mo8 O26, 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H54 I4 Mo8 N2 O28'
_chemical_formula_weight         2454.11
_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                69.875(2)
_cell_angle_beta                 64.408(2)
_cell_angle_gamma                68.367(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7533(3)
_cell_length_b                   12.7583(3)
_cell_length_c                   13.1803(3)
_cell_measurement_reflns_used    8572
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8010
_cell_measurement_theta_min      2.7600
_cell_volume                     1753.70(8)
_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 0.832
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.049
_diffrn_reflns_theta_min         1.833
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91751
_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    2.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.451
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+4.4419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6488
_reflns_number_total             7792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01695e2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 1571977--1571981.cif.'
_cod_original_cell_volume        1753.71(8)
_cod_database_code               1571977
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.445
_olex2_refinement_description
;
1. Others
 Fixed Sof: I1B(0.93) I1C(0.07)
2.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C8A(H8A), C6A(H6A), C5A(H5A),
 C4A(H4A), C3A(H3A), C2A(H2A), C12B(H12B), C11B(H11B), C10B(H10B), C9B(H9B),
 C8B(H8B), C6B(H6B), C5B(H5B), C4B(H4B), C3B(H3B), C2B(H2B), C1S(H1S)
2.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              1417
_shelx_hkl_checksum              95491
_olex2_submission_special_instructions 'No special instructions were received'