#------------------------------------------------------------------------------
#$Date: 2026-03-13 23:55:27 +0100 (Fri 13 de Mar de 2026) $
#$Revision: 305079 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/56/7135625.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_7135625
loop_
_publ_author_name
'Liu, Yi-Chen'
'Zhang, Ming-Zhi'
'Hu, Chun-Li'
'Mao, Jiang-Gao'
_publ_section_title
;
 [ICl4]-: A Large Anisotropic Planar Anion Group Produces Giant
 Birefringence
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D6CC00713A
_journal_year                    2026
_chemical_formula_moiety         'Cl4 I, C5 H7 N2'
_chemical_formula_sum            'C5 H7 Cl4 I N2'
_chemical_formula_weight         363.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-14 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.656(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0937(5)
_cell_length_b                   11.9204(15)
_cell_length_c                   11.0250(16)
_cell_measurement_reflns_used    1950
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4150
_cell_measurement_theta_min      3.6620
_cell_volume                     536.91(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3762
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.071
_diffrn_reflns_theta_min         2.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_description       needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0364
_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)+(0.0393P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1096
_reflns_number_total             1317
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6cc00713a2.cif
_cod_data_source_block           1
_cod_database_code               7135625
_shelx_shelxl_version_number     2018/3
_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   0.996
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1), N2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.31317(10) 0.250000 0.75061(4) 0.01736(16) Uani 1 2 d S T P . .
Cl1 Cl 0.5198(3) 0.10501(9) 0.90012(11) 0.0274(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1141(3) 0.09737(10) 0.60787(11) 0.0281(3) Uani 1 1 d . . . . .
N1 N -0.0269(14) 0.250000 0.1171(6) 0.0317(14) Uani 1 2 d S T P . .
H1 H -0.161394 0.250000 0.053934 0.038 Uiso 1 2 d R U P . .
N2 N 0.6078(15) 0.250000 0.4145(6) 0.0394(16) Uani 1 2 d S T P . .
H2 H 0.680376 0.314510 0.445594 0.047 Uiso 1 1 d R U . . .
C1 C 0.0724(13) 0.1506(4) 0.1661(5) 0.0324(12) Uani 1 1 d . . . . .
H1A H -0.004941 0.083863 0.131268 0.039 Uiso 1 1 calc R U . . .
C2 C 0.2857(12) 0.1478(4) 0.2666(5) 0.0307(12) Uani 1 1 d . . . . .
H2A H 0.355174 0.079474 0.299658 0.037 Uiso 1 1 calc R U . . .
C3 C 0.4010(17) 0.250000 0.3203(7) 0.0294(16) Uani 1 2 d S T P . .
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 87.54(6) . 4_565 ?
Cl1 I1 Cl2 89.71(4) 4_565 4_565 ?
Cl1 I1 Cl2 177.25(4) . 4_565 ?
Cl1 I1 Cl2 177.25(4) 4_565 . ?
Cl1 I1 Cl2 89.71(4) . . ?
Cl2 I1 Cl2 93.04(6) 4_565 . ?
C1 N1 H1 118.9 . . ?
C1 N1 H1 118.9 4_565 . ?
C1 N1 C1 122.1(7) . 4_565 ?
H2 N2 H2 120.6 . 4_565 ?
C3 N2 H2 119.703(12) . 4_565 ?
C3 N2 H2 119.7 . . ?
N1 C1 H1A 119.9 . . ?
N1 C1 C2 120.3(5) . . ?
C2 C1 H1A 119.9 . . ?
C1 C2 H2A 120.2 . . ?
C1 C2 C3 119.7(5) . . ?
C3 C2 H2A 120.2 . . ?
N2 C3 C2 121.1(3) . 4_565 ?
N2 C3 C2 121.1(3) . . ?
C2 C3 C2 117.9(7) 4_565 . ?
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 2.4984(12) . ?
I1 Cl1 2.4985(12) 4_565 ?
I1 Cl2 2.5074(12) . ?
I1 Cl2 2.5074(12) 4_565 ?
N1 H1 0.8600 . ?
N1 C1 1.354(6) 4_565 ?
N1 C1 1.354(6) . ?
N2 H2 0.8855 . ?
N2 H2 0.8854 4_565 ?
N2 C3 1.297(9) . ?
C1 H1A 0.9300 . ?
C1 C2 1.366(7) . ?
C2 H2A 0.9300 . ?
C2 C3 1.421(6) . ?
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
N1 C1 C2 C3 0.6(8) . . . . ?
C1 N1 C1 C2 -1.6(10) 4_565 . . . ?
C1 C2 C3 N2 -178.8(6) . . . . ?
C1 C2 C3 C2 0.3(9) . . . 4_565 ?
