#------------------------------------------------------------------------------
#$Date: 2023-10-06 03:02:36 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/72/7247288.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_7247288
loop_
_publ_author_name
'Korobeynikov, Nikita A.'
'Usoltsev, Andrey N.'
'Sokolov, Maxim N.'
'Novikov, Alexander S.'
'Sukhikh, Taisiya S.'
'Adonin, Sergey A.'
_publ_section_title
;
 Halogen bonding in chloroiodates(iii)
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              5233
_journal_page_last               5237
_journal_paper_doi               10.1039/D3CE00400G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Cl4 I, C12 H14 N2, Cl'
_chemical_formula_sum            'C12 H14 Cl5 I N2'
_chemical_formula_weight         490.40
_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             2023-04-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                93.199(2)
_cell_angle_beta                 110.363(2)
_cell_angle_gamma                95.058(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4887(5)
_cell_length_b                   7.6756(5)
_cell_length_c                   8.0494(5)
_cell_measurement_reflns_used    5068
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.68
_cell_volume                     430.22(5)
_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 0.988
_diffrn_measured_fraction_theta_max 0.936
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5544
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.579
_diffrn_reflns_theta_min         2.676
_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    2.628
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0823 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.8619.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       plank
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0161P)²+0.7968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2207
_reflns_number_total             2276
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00400g2.cif
_cod_data_source_block           nk770_a
_cod_depositor_comments
'Adding full bibliography for 7247286--7247294.cif.'
_cod_database_code               7247288
_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   0.902
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C2(H2), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
I1 I 0.500000 0.000000 1.000000 0.01924(8) Uani 1 2 d S . P . .
C1 C 0.7161(5) 0.6703(4) 0.5316(4) 0.0280(6) Uani 1 1 d . . . . .
H1 H 0.670893 0.781269 0.506809 0.034 Uiso 1 1 calc R U . . .
N1 N 0.6904(4) 0.5490(3) 0.3986(3) 0.0262(5) Uani 1 1 d . . . . .
H1A H 0.630282 0.572652 0.288564 0.031 Uiso 1 1 calc R U . . .
Cl1 Cl 0.83965(12) -0.00987(12) 1.19737(12) 0.0397(2) Uani 1 1 d . . . . .
Cl2 Cl 0.59871(13) 0.03611(11) 0.73759(10) 0.03378(18) Uani 1 1 d . . . . .
C2 C 0.8073(4) 0.6367(4) 0.7045(4) 0.0257(6) Uani 1 1 d . . . . .
H2 H 0.824548 0.724032 0.798846 0.031 Uiso 1 1 calc R U . . .
Cl3 Cl 0.500000 0.500000 0.000000 0.0302(2) Uani 1 2 d S . P . .
C3 C 0.8748(4) 0.4745(4) 0.7420(4) 0.0213(5) Uani 1 1 d . . . . .
C5 C 0.7539(4) 0.3909(4) 0.4277(4) 0.0250(6) Uani 1 1 d . . . . .
H5 H 0.734632 0.306906 0.330083 0.030 Uiso 1 1 calc R U . . .
C4 C 0.8461(4) 0.3507(4) 0.5979(4) 0.0238(6) Uani 1 1 d . . . . .
H4 H 0.890629 0.238940 0.618187 0.029 Uiso 1 1 calc R U . . .
C6 C 0.9743(5) 0.4247(4) 0.9278(4) 0.0255(6) Uani 1 1 d . . . . .
H6A H 1.093165 0.374853 0.932111 0.031 Uiso 1 1 calc R U . . .
H6B H 0.890092 0.331557 0.953515 0.031 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'
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'
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
Cl1 I1 Cl1 180.0 . 2_657 ?
Cl2 I1 Cl1 88.84(3) 2_657 . ?
Cl2 I1 Cl1 88.84(3) . 2_657 ?
Cl2 I1 Cl1 91.16(3) 2_657 2_657 ?
Cl2 I1 Cl1 91.16(3) . . ?
Cl2 I1 Cl2 180.0 . 2_657 ?
N1 C1 H1 119.7 . . ?
N1 C1 C2 120.5(3) . . ?
C2 C1 H1 119.7 . . ?
C1 N1 H1A 119.2 . . ?
C1 N1 C5 121.6(3) . . ?
C5 N1 H1A 119.2 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 117.6(3) . . ?
C2 C3 C6 123.9(3) . . ?
C4 C3 C6 118.5(3) . . ?
N1 C5 H5 119.9 . . ?
N1 C5 C4 120.1(3) . . ?
C4 C5 H5 119.9 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C6 C6 114.5(3) . 2_767 ?
C3 C6 H6A 108.6 . . ?
C3 C6 H6B 108.6 . . ?
C6 C6 H6A 108.6 2_767 . ?
C6 C6 H6B 108.6 2_767 . ?
H6A C6 H6B 107.6 . . ?
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
I1 Cl1 2.4969(8) 2_657 ?
I1 Cl1 2.4969(8) . ?
I1 Cl2 2.4902(8) 2_657 ?
I1 Cl2 2.4901(8) . ?
C1 H1 0.9500 . ?
C1 N1 1.329(4) . ?
C1 C2 1.371(4) . ?
N1 H1A 0.8800 . ?
N1 C5 1.345(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(4) . ?
C3 C4 1.401(4) . ?
C3 C6 1.508(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.369(4) . ?
C4 H4 0.9500 . ?
C6 C6 1.515(5) 2_767 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
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
C1 N1 C5 C4 0.6(5) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C1 C2 C3 C6 -179.1(3) . . . . ?
N1 C1 C2 C3 0.3(5) . . . . ?
N1 C5 C4 C3 -0.1(4) . . . . ?
C2 C1 N1 C5 -0.7(5) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C2 C3 C6 C6 -9.6(5) . . . 2_767 ?
C4 C3 C6 C6 171.1(3) . . . 2_767 ?
C6 C3 C4 C5 179.1(3) . . . . ?
