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#$Date: 2026-03-05 13:42:49 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304898 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/15/7251502.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7251502
loop_
_publ_author_name
'Korobeynikov, Nikita A.'
'Usoltsev, Andrey N.'
'Sokolov, Maxim N.'
'Novikov, Alexander S.'
'Adonin, Sergey A.'
_publ_section_title
;
 Supramolecular diiodo-chlorometalates(iii) of group 15 elements with
 halogen-substituted pyridiniums: an interplay of cation⋯anion and
 I2⋯halometalate halogen bonds
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1197
_journal_page_last               1205
_journal_paper_doi               10.1039/D5CE01065A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'Cl4 Sb, I2, 2(C5 H5 Br N), Cl'
_chemical_formula_sum            'C10 H10 Br2 Cl5 I2 N2 Sb'
_chemical_formula_weight         870.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-10-07 deposited with the CCDC.	2026-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9208(3)
_cell_length_b                   7.09130(10)
_cell_length_c                   20.9159(4)
_cell_measurement_reflns_used    8348
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.75
_cell_volume                     2194.66(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.584
_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    8.317
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7281.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_description       plank
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         6700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0335
_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/[σ²(Fo²)+(0.0197P)²+1.1494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4944
_reflns_number_total             6700
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce01065a2.cif
_cod_data_source_block           nk1146
_cod_depositor_comments
'Adding full bibliography for 7251502--7251505.cif.'
_cod_database_code               7251502
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C8(H8), C9(H9), C1(H1A), C10(H10), C5(H5), C3(H3),
 C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.74070(2) 0.73992(3) 0.64473(2) 0.01743(6) Uani 1 1 d . . . . .
I1 I 0.35027(2) 0.72601(3) 0.61200(2) 0.02331(6) Uani 1 1 d . . . . .
I2 I 0.16598(2) 0.71757(4) 0.59968(2) 0.03761(8) Uani 1 1 d . . . . .
Br1 Br 1.06941(3) 0.23407(6) 0.50286(2) 0.03682(11) Uani 1 1 d . . . . .
Br2 Br 0.35530(3) 0.21878(7) 0.72019(2) 0.04165(12) Uani 1 1 d . . . . .
Cl2 Cl 0.73370(6) 0.53007(11) 0.55370(4) 0.02009(18) Uani 1 1 d . . . . .
Cl4 Cl 0.73861(6) 1.01221(12) 0.56986(5) 0.0249(2) Uani 1 1 d . . . . .
Cl5 Cl 0.90676(6) 0.74120(13) 0.65755(4) 0.02504(19) Uani 1 1 d . . . . .
Cl3 Cl 0.74377(6) 0.39642(14) 0.71321(4) 0.0270(2) Uani 1 1 d . . . . .
Cl1 Cl 0.54330(7) 0.74673(14) 0.62885(5) 0.0319(2) Uani 1 1 d . . . . .
N1 N 0.9118(2) 0.2596(4) 0.64668(16) 0.0292(8) Uani 1 1 d . . . . .
H1 H 0.853905 0.276364 0.649061 0.035 Uiso 1 1 calc R U . . .
N2 N 0.5700(2) 0.2588(4) 0.62051(16) 0.0269(7) Uani 1 1 d . . . . .
H2 H 0.628608 0.273769 0.630685 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4271(3) 0.2275(5) 0.65249(18) 0.0237(8) Uani 1 1 d . . . . .
C6 C 0.5185(3) 0.2505(5) 0.66827(19) 0.0255(8) Uani 1 1 d . . . . .
H6 H 0.544626 0.260405 0.712027 0.031 Uiso 1 1 calc R U . . .
C8 C 0.3894(3) 0.2157(5) 0.58870(19) 0.0253(8) Uani 1 1 d . . . . .
H8 H 0.325942 0.202165 0.577807 0.030 Uiso 1 1 calc R U . . .
C9 C 0.4455(3) 0.2239(5) 0.54087(19) 0.0252(8) Uani 1 1 d . . . . .
H9 H 0.420871 0.214560 0.496774 0.030 Uiso 1 1 calc R U . . .
C2 C 1.0295(3) 0.2329(5) 0.58459(18) 0.0225(8) Uani 1 1 d . . . . .
C1 C 0.9393(3) 0.2571(5) 0.58838(19) 0.0254(8) Uani 1 1 d . . . . .
H1A H 0.897331 0.271692 0.550519 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5369(3) 0.2455(5) 0.5578(2) 0.0277(9) Uani 1 1 d . . . . .
H10 H 0.576269 0.251039 0.525609 0.033 Uiso 1 1 calc R U . . .
C5 C 0.9672(3) 0.2380(5) 0.7014(2) 0.0360(10) Uani 1 1 d . . . . .
H5 H 0.944166 0.238825 0.741678 0.043 Uiso 1 1 calc R U . . .
C3 C 1.0890(3) 0.2124(6) 0.6397(2) 0.0381(11) Uani 1 1 d . . . . .
H3 H 1.151667 0.196519 0.637304 0.046 Uiso 1 1 calc R U . . .
C4 C 1.0568(3) 0.2149(6) 0.6990(2) 0.0408(11) Uani 1 1 d . . . . .
H4 H 1.097295 0.200478 0.737597 0.049 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Sb1 Cl4 89.21(3) . . ?
Cl2 Sb1 Cl5 91.66(3) . . ?
Cl2 Sb1 Cl3 82.19(3) . . ?
Cl4 Sb1 Cl3 171.38(3) . . ?
Cl5 Sb1 Cl4 89.80(3) . . ?
Cl5 Sb1 Cl3 89.86(3) . . ?
C1 N1 H1 118.2 . . ?
C5 N1 H1 118.2 . . ?
C5 N1 C1 123.6(4) . . ?
C6 N2 H2 118.2 . . ?
C6 N2 C10 123.5(4) . . ?
C10 N2 H2 118.2 . . ?
C6 C7 Br2 117.9(3) . . ?
C6 C7 C8 120.5(4) . . ?
C8 C7 Br2 121.6(3) . . ?
N2 C6 C7 118.3(4) . . ?
N2 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.1(4) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(4) . . ?
C10 C9 H9 120.3 . . ?
C1 C2 Br1 118.7(3) . . ?
C3 C2 Br1 121.3(3) . . ?
C3 C2 C1 120.0(4) . . ?
N1 C1 C2 118.3(4) . . ?
N1 C1 H1A 120.8 . . ?
C2 C1 H1A 120.8 . . ?
N2 C10 C9 119.2(4) . . ?
N2 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
N1 C5 H5 120.4 . . ?
N1 C5 C4 119.2(4) . . ?
C4 C5 H5 120.4 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 Cl2 2.4083(9) . ?
Sb1 Cl4 2.4837(9) . ?
Sb1 Cl5 2.4577(9) . ?
Sb1 Cl3 2.8231(9) . ?
I1 I2 2.7293(4) . ?
Br1 C2 1.881(4) . ?
Br2 C7 1.883(4) . ?
N1 H1 0.8800 . ?
N1 C1 1.336(5) . ?
N1 C5 1.332(5) . ?
N2 H2 0.8800 . ?
N2 C6 1.337(5) . ?
N2 C10 1.344(5) . ?
C7 C6 1.371(5) . ?
C7 C8 1.382(5) . ?
C6 H6 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.385(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.373(5) . ?
C2 C1 1.369(5) . ?
C2 C3 1.368(6) . ?
C1 H1A 0.9500 . ?
C10 H10 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.354(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(6) . ?
C4 H4 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C2 C1 N1 -178.8(3) . . . . ?
Br1 C2 C3 C4 179.1(3) . . . . ?
Br2 C7 C6 N2 -179.3(3) . . . . ?
Br2 C7 C8 C9 179.7(3) . . . . ?
N1 C5 C4 C3 -0.6(6) . . . . ?
C7 C8 C9 C10 -0.7(5) . . . . ?
C6 N2 C10 C9 0.6(5) . . . . ?
C6 C7 C8 C9 1.2(6) . . . . ?
C8 C7 C6 N2 -0.9(5) . . . . ?
C8 C9 C10 N2 -0.2(5) . . . . ?
C2 C3 C4 C5 -0.1(7) . . . . ?
C1 N1 C5 C4 1.0(6) . . . . ?
C1 C2 C3 C4 0.5(6) . . . . ?
C10 N2 C6 C7 -0.1(5) . . . . ?
C5 N1 C1 C2 -0.7(6) . . . . ?
C3 C2 C1 N1 -0.1(5) . . . . ?
