New iodine-rich Group 15 iodometalates(III): self-assembly of metal halide anions and polyiodides into supramolecular architectures via I···I contacts
Shentseva, Irina; Korobeynikov, Nikita A.; Usoltsev, Andrey N.; Sokolov, Maksim Nailyevich; Adonin, Sergey A.; CrystEngComm  (2025) –; doi:10.1039/D5CE00992H

data_7251355
_publ_section_title
;
 New iodine-rich Group 15 iodometalates(III): self-assembly of metal
 halide anions and polyiodides into supramolecular architectures via
 I&#x00B7;&#x00B7;&#x00B7;I contacts
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00992H
_journal_year                    2025
_chemical_formula_moiety
'(I11 Sb2), 2(I8 Sb), 2(I3), 6(C13 H16 N2), [H3O], 3[H2O]'
_chemical_formula_sum            'C78 H105 I33 N12 O4 Sb4'
_chemical_formula_weight         5949.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-19 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.9204(3)
_cell_length_b                   14.3689(3)
_cell_length_c                   29.1546(7)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.17
_cell_volume                     6839.1(3)
_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, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            74686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.154
_diffrn_reflns_theta_min         1.888
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.273
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.8155.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_description       plate
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Flack x determined using 5884 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         25992
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0167P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                18188
_reflns_number_total             25992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00992h2.cif
_cod_data_source_block           is476
_cod_database_code               7251355
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.595
_diffrn_oxdiff_ac3_digest_hkl    01476d007f094dd519bacf892d9895c4d9a00f
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I13B) = Uanis(I14A)
Uanis(I10) = Uanis(I14B)
3. Others
 Sof(I9B)=1-FVAR(1)
 Sof(I9A)=FVAR(1)
 Sof(I14B)=0.5*(1-FVAR(3))
 Sof(I14A)=0.5*FVAR(3)
 Sof(I13B)=1-FVAR(3)
 Sof(I13A)=FVAR(3)
 Sof(I11B)=1-FVAR(4)
 Sof(I11A)=FVAR(4)
 Fixed Sof: H40A(0.5) H40B(0.5) H7A(0.5) H7B(0.5) O3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) O1(0.5) H1A(0.5) H1B(0.5)
4.a Riding coordinates:
 O3(H3A,H3B,H3C)
4.b Free rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
4.c Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C28(H28A,H28B),
 C14(H14A,H14B), C39(H39A,H39B), C26(H26A,H26B), C15(H15A,H15B), C27(H27A,H27B)
4.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C36(H36), C11(H11), C38(H38), C35(H35), C12(H12), C33(H33), C9(H9),
 C37(H37), C8(H8), C34(H34), C10(H10), C31(H31), C4(H4), C29(H29), C30(H30),
 C16(H16), C19(H19), C18(H18), C1(H1), C20(H20), C32(H32), C2(H2), C17(H17),
 C3(H3), C22(H22), C23(H23), C25(H25), C24(H24), C21(H21)
;
_shelx_res_checksum              68990
_olex2_submission_special_instructions 'No special instructions were received'