#------------------------------------------------------------------------------
#$Date: 2026-04-29 00:57:27 +0200 (Wed, 29 Apr 2026) $
#$Revision: 305646 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/72/09/7720937.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_7720937
loop_
_publ_author_name
'Yang, Bo'
'Chen, Ziqi'
'Lu, Zhenjiang'
'Lu, Juanjuan'
_publ_section_title
;
 Broadband infrared-transparent crystals enabled by heterologous
 isomorphic substitution.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d6dt00568c
_journal_year                    2026
_chemical_formula_moiety         'I, 2(Cl2 Zn0.5), H6 N2, H6 N'
_chemical_formula_sum            'Cl4 H12 I N3 Zn'
_chemical_formula_weight         388.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2026-02-04 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1178(5)
_cell_length_b                   16.7739(9)
_cell_length_c                   9.9227(5)
_cell_measurement_reflns_used    7288
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.11
_cell_volume                     1184.70(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11595
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         3.109
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.527
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4975
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1227 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.6672.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         778
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      2.047
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0194
_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)+(0.0288P)²+2.0436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                749
_reflns_number_total             778
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00568c2.cif
_cod_data_source_block           nhzncli111
_cod_database_code               7720937
_shelx_shelxl_version_number     2019/3
_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.
;
_olex2_refinement_description
;
1. Restrained distances
 N1-H1B_$1 = N1-H1B = N1-H1A = N1-H1C
 0.95 with sigma of 0.02
 N2-H2A = N2-H2B = N2-H2C = N2-H2D
 1.42 with sigma of 0.02
 N2-H2B = N2-H2D = N2-H2A = N2-H2C
 0.95 with sigma of 0.02
 H1B_$1-H1C
 1.55 with sigma of 0.02
 N2-H2D = N2-H2C = N2-H2A
 0.95 with sigma of 0.02
 H2D-H2C
 1.55 with sigma of 0.02
 H2B-H2C
 1.55 with sigma of 0.02
 H2B-H2D
 1.55 with sigma of 0.02
 H2C-H2B
 1.55 with sigma of 0.02
 H2D-H2A
 1.55 with sigma of 0.02
 H2B-N2
 0.95 with sigma of 0.02
 H2B-H2A
 1.55 with sigma of 0.02
 H1C-H1A
 1.55 with sigma of 0.02
 H2A-H2C
 1.55 with sigma of 0.02
 H1B_$1-H1B
 1.55 with sigma of 0.02
 H1B-H1A
 1.55 with sigma of 0.02
 H2A-H2B \\sim H2B-H2C \\sim H2C-H2D \\sim H2D-H2A \\sim H2B-H2D \\sim H2A-H2C
 with sigma of 0.04
 N2-H2A \\sim N2-H2B \\sim N2-H2C \\sim N2-H2D
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N2 \\sim H2A \\sim H2B \\sim H2C \\sim H2D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 N2, H2A, H2B, H2C, H2D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1B(0.5) H2A(0.25) H2C(0.25)
;
_shelx_res_file
;
TITL nhzncli111_a.res in Cmcm
    nhzncli111.res
    created by SHELXL-2019/3 at 18:00:01 on 11-Dec-2025
REM Old TITL NHZnClI111 in Cmcm
REM SHELXT solution in Cmcm: R1 0.087, Rweak 0.005, Alpha 0.011
REM <I/s> 2.741 for 26 systematic absences, Orientation as input
REM Formula found by SHELXT: N3 Cl4 Zn I
CELL 0.71073 7.1178 16.7739 9.9227 90 90 90
ZERR 4 0.0005 0.0009 0.0005 0 0 0
LATT 7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC Cl H I N Zn
UNIT 16 48 4 12 4
EQIV $1 1-X,+Y,+Z
DFIX 0.95 N1 H1b_$1 N1 H1b N1 H1a N1 H1c
SIMU N2 H2a H2b H2c H2d
SADI 0.04 H2a H2b H2b H2c H2c H2d H2d H2a H2b H2d H2a H2c
SADI N2 H2a N2 H2b N2 H2c N2 H2d
RIGU N2 H2a H2b H2c H2d
DFIX 1.42 N2 H2a N2 H2b N2 H2c N2 H2d
DFIX 0.95 N2 H2b N2 H2d N2 H2a N2 H2c
DFIX 1.55 H1b_$1 H1c
DFIX 0.95 N2 H2d N2 H2c N2 H2a
DFIX 1.55 H2d H2c
DFIX 1.55 H2b H2c
DFIX 1.55 H2b H2d
DFIX 1.55 H2c H2b
DFIX 1.55 H2d H2a
DFIX 0.95 H2b N2
DFIX 1.55 H2b H2a
DFIX 1.55 H1c H1a
DFIX 1.55 H2a H2c
DFIX 1.55 H1b_$1 H1b
DFIX 1.55 H1b H1a

L.S. 20 0 0
PLAN  2
TEMP -100.15
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT 0 2 0
REM <olex2.extras>
REM <HklSrc "%.\\NHZnClI111.hkl">
REM </olex2.extras>

WGHT    0.028800    2.043600
EXTI    0.001177
FVAR       0.27896
I1    3    0.500000    0.506241    0.250000    10.25000    0.04653    0.03517 =
         0.04305    0.00000    0.00000    0.00000
ZN1   5    1.000000    0.314539    0.250000    10.25000    0.02861    0.02875 =
         0.02518    0.00000    0.00000    0.00000
CL1   1    0.745498    0.232929    0.250000    10.50000    0.02761    0.03857 =
         0.05865    0.00000    0.00000   -0.00534
CL2   1    1.000000    0.386201    0.440846    10.50000    0.07535    0.05200 =
         0.02454   -0.00957    0.00000    0.00000
N1    4    0.500000    0.344048    0.480666    10.50000    0.05409    0.04545 =
         0.03580    0.00214    0.00000    0.00000
H1A   2    0.500000    0.395824    0.441240    10.50000    0.08014
H1B   2    0.608554    0.339302    0.534783    10.50000    0.10723
H1C   2    0.500000    0.305995    0.410826    10.50000    0.22847
PART 1
N2    4    1.000000    0.553880    0.250000    10.25000    0.04546    0.03409 =
         0.03104    0.00000    0.00000    0.00000
H2A   2    1.043864    0.542396    0.343756    10.25000   -1.50000
H2B   2    0.865402    0.575444    0.250000    10.50000    0.11500
H2C   2    1.074687    0.598702    0.206243    10.25000    0.07572
H2D   2    1.000000    0.505789    0.188054    10.50000    0.10648
HKLF 4




REM  nhzncli111_a.res in Cmcm
REM wR2 = 0.0566, GooF = S = 1.147, Restrained GooF = 2.047 for all data
REM R1 = 0.0194 for 749 Fo > 4sig(Fo) and 0.0203 for all 778 data
REM 55 parameters refined using 78 restraints

END

WGHT      0.0288      2.0436

REM Highest difference peak  0.577,  deepest hole -0.517,  1-sigma level  0.089
Q1    1   1.0000  0.3542  0.4665  10.50000  0.05    0.58
Q2    1   1.0788  0.4010  0.4242  11.00000  0.05    0.53
;
_shelx_res_checksum              14051
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, 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 0.500000 0.50624(2) 0.250000 0.04158(15) Uani 1 4 d S T P . .
Zn1 Zn 1.000000 0.31454(3) 0.250000 0.02751(16) Uani 1 4 d S T P . .
Cl1 Cl 0.74550(12) 0.23293(5) 0.250000 0.0416(2) Uani 1 2 d S T P . .
Cl2 Cl 1.000000 0.38620(6) 0.44085(8) 0.0506(3) Uani 1 2 d S T P . .
N1 N 0.500000 0.34405(19) 0.4807(3) 0.0451(8) Uani 1 2 d DS T P . .
H1A H 0.500000 0.3958(17) 0.441(5) 0.080(18) Uiso 1 2 d DS . P . .
H1B H 0.6086(14) 0.339(3) 0.535(2) 0.11(4) Uiso 0.5 1 d D . P . .
H1C H 0.500000 0.306(3) 0.411(5) 0.23(6) Uiso 1 2 d DS . P . .
N2 N 1.000000 0.5539(3) 0.250000 0.0369(9) Uani 1 4 d DS TU P A 1
H2A H 1.044(5) 0.542(3) 0.3438(15) 0.055 Uiso 0.25 1 d D U P B 1
H2B H 0.865(2) 0.5754(18) 0.250000 0.115(14) Uiso 1 2 d DS U P C 1
H2C H 1.075(5) 0.5987(15) 0.206(5) 0.076(16) Uiso 0.25 1 d D U P D 1
H2D H 1.000000 0.5058(17) 0.188(4) 0.106(15) Uiso 1 2 d DS U P E 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0465(2) 0.0352(2) 0.0430(2) 0.000 0.000 0.000
Zn1 0.0286(3) 0.0287(3) 0.0252(3) 0.000 0.000 0.000
Cl1 0.0276(4) 0.0386(4) 0.0587(5) 0.000 0.000 -0.0053(3)
Cl2 0.0754(7) 0.0520(5) 0.0245(4) -0.0096(3) 0.000 0.000
N1 0.054(2) 0.0455(19) 0.0358(16) 0.0021(14) 0.000 0.000
N2 0.045(2) 0.034(2) 0.0310(19) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'
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'
Zn Zn 0.2839 1.4301 '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 Zn1 Cl1 105.85(5) 3_755 . ?
Cl2 Zn1 Cl1 108.851(18) . . ?
Cl2 Zn1 Cl1 108.850(18) . 3_755 ?
Cl2 Zn1 Cl1 108.850(18) 10_556 3_755 ?
Cl2 Zn1 Cl1 108.851(17) 10_556 . ?
Cl2 Zn1 Cl2 115.19(6) 10_556 . ?
H1A N1 H1B 108(2) . 12_655 ?
H1A N1 H1B 108(2) . . ?
H1A N1 H1C 108(3) . . ?
H1B N1 H1B 110(3) . 12_655 ?
H1B N1 H1C 111.2(19) . . ?
H1C N1 H1B 111(2) . 12_655 ?
H2A N2 H2B 111.1(17) . . ?
H2A N2 H2C 112.1(17) . . ?
H2A N2 H2D 114.2(17) . . ?
H2B N2 H2C 103.2(13) . . ?
H2B N2 H2D 106.3(15) . . ?
H2C N2 H2D 109.2(16) . . ?
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
Zn1 Cl1 2.2706(9) . ?
Zn1 Cl1 2.2705(9) 3_755 ?
Zn1 Cl2 2.2430(9) . ?
Zn1 Cl2 2.2430(9) 10_556 ?
N1 H1A 0.953(18) . ?
N1 H1B 0.944(11) 12_655 ?
N1 H1B 0.944(11) . ?
N1 H1C 0.942(18) . ?
N2 H2A 1.000(9) . ?
N2 H2B 1.024(9) . ?
N2 H2C 1.018(9) . ?
N2 H2D 1.014(9) . ?
