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_7251356
_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
'(Bi2 I11), 2(Bi I8), 2(I3), 6(C13 H16 N2),[H3O], 3[H2O]'
_chemical_formula_sum            'C78 H105 Bi4 I33 N12 O4'
_chemical_formula_weight         6298.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 91.534(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.913(2)
_cell_length_b                   14.4492(17)
_cell_length_c                   56.667(7)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.16
_cell_volume                     13843(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            76995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.524
_diffrn_reflns_theta_min         1.854
_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    12.471
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0938 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.7050.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_description       plate
_exptl_crystal_F_000             11080
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         22931
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+172.0072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16449
_reflns_number_total             22931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00992h2.cif
_cod_data_source_block           nk39_a
_cod_database_code               7251356
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.421
_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. Restrained distances
 Bi2-I11A \\sim Bi2-I11B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I14A) = Uanis(I14B)
Uanis(I9B) = Uanis(I9A)
Uanis(I11A) = Uanis(I11B)
4. Others
 Sof(I9B)=1-FVAR(1)
 Sof(I9A)=FVAR(1)
 Sof(I10B)=0.5*(1-FVAR(3))
 Sof(I10A)=0.5*FVAR(3)
 Sof(I14B)=1-FVAR(3)
 Sof(I14A)=FVAR(3)
 Sof(I11B)=1-FVAR(4)
 Sof(I11A)=FVAR(4)
 Fixed Sof: H1A(0.5) H1B(0.5) O3(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
5.a Riding coordinates:
 O3(H3A,H3B,H3C)
5.b Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
5.c Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
5.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_shelx_res_checksum              80758
_olex2_submission_special_instructions 'No special instructions were received'