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_1571979
_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(C3 H7 N O), 4(C18 H22 I), C1.8 N0.6 O0.6, Mo8 O26'
_chemical_formula_sum            'C79.8 H106.2 I4 Mo8 N2.6 O28.6'
_chemical_formula_weight         2834.59
_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                61.0800(10)
_cell_angle_beta                 81.7340(10)
_cell_angle_gamma                65.7040(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9442(4)
_cell_length_b                   14.7482(4)
_cell_length_c                   14.7605(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.7108
_cell_measurement_theta_min      2.3299
_cell_volume                     2415.85(12)
_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 0.992
_diffrn_measured_fraction_theta_max 0.978
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35741
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.711
_diffrn_reflns_theta_min         2.702
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6561
_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    1.948
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         12209
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0250P)^2^+3.6283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11019
_reflns_number_total             12209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01695e2.cif
_cod_data_source_block           Mes_DMF
_cod_depositor_comments
'Adding full bibliography for 1571977--1571981.cif.'
_cod_original_formula_sum        'C79.80 H106.20 I4 Mo8 N2.60 O28.60'
_cod_database_code               1571979
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Restrained distances
 O3S-C6S
 1.2 with sigma of 0.02
2. Others
 Fixed Sof: C6S(0.3) C5S(0.3) C7S(0.3) N2S(0.3) O2S(0.2) O3S(0.1) C3A(0.5)
 H3A(0.5) C4A(0.5) C14A(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C5A(0.5) H5A(0.5)
 C3C(0.5) H3C(0.5) C4C(0.5) C14C(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C5C(0.5)
 H5C(0.5) C2S(0.2) H2SA(0.2) H2SB(0.2) H2SC(0.2) C4S(0.8) H4SA(0.8) H4SB(0.8)
 H4SC(0.8)
3.a Me refined with riding coordinates:
 C3S(H3SA,H3SB,H3SC), C13B(H13D,H13E,H13F), C15B(H15D,H15E,H15F), C14B(H14G,
 H14H,H14I), C18B(H18D,H18E,H18F), C17B(H17D,H17E,H17F), C13A(H13A,H13B,H13C),
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C14A(H14A,H14B,H14C), C14C(H14D,
 H14E,H14F)
3.b Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C5B(H5B), C3B(H3B), C11B(H11B), C9B(H9B), C9A(H9A), C11A(H11A),
 C3A(H3A), C5A(H5A), C3C(H3C), C5C(H5C)
3.c Idealised Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
3.d Idealised Me refined as rotating group:
 C16B(H16D,H16E,H16F), C15A(H15A,H15B,H15C), C18A(H18A,H18B,H18C)
;
_shelx_res_checksum              14154
_shelx_hkl_checksum              27315
_olex2_submission_special_instructions 'No special instructions were received'