# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdIBr
_database_code_depnum_ccdc_archive 'CCDC 2381799'
loop_
_audit_author_name
_audit_author_address
'jieru Yang'
;Fujian Normal University
China
;
_audit_update_record             
;
2024-09-04 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br1.57 Cd I2.43, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Br1.57 Cd I2.43 N2'
_chemical_formula_weight         634.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.8562(2)
_cell_length_b                   12.0536(2)
_cell_length_c                   12.7689(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1363.07(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    6165
_cell_measurement_theta_min      4.9940
_cell_measurement_theta_max      76.0100

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_F_000             1127
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    61.109
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.15620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7716
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         5.046
_diffrn_reflns_theta_max         78.045
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             2695
_reflns_number_gt                2544
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.666
_reflns_Friedel_fraction_max     0.873
_reflns_Friedel_fraction_full    0.948

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0970P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2695
_refine_ls_number_parameters     113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1305
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.25698(12) 0.67411(7) 0.42090(8) 0.0404(3) Uani 1 1 d . . . . .
I2 I 0.4561(9) 0.3798(4) 0.5949(6) 0.0333(8) Uani 0.588(14) 1 d . . P A 1
I3 I 0.2388(13) 0.6554(8) 0.7823(9) 0.0332(11) Uani 0.510(13) 1 d . . P A 1
I4 I -0.037(2) 0.4136(17) 0.5985(17) 0.0377(14) Uani 0.328(14) 1 d . . P A 1
Br2 Br 0.459(2) 0.4001(11) 0.5941(16) 0.0333(8) Uani 0.412(14) 1 d . . P A 2
Br3 Br 0.241(2) 0.6417(14) 0.7704(16) 0.0332(11) Uani 0.490(13) 1 d . . P A 2
Br4 Br -0.0240(18) 0.4321(12) 0.5990(13) 0.0377(14) Uani 0.672(14) 1 d . . P A
2
Cd1 Cd 0.23206(12) 0.53967(7) 0.59439(8) 0.0338(3) Uani 1 1 d . . . . .
N1 N 0.9193(14) 0.4866(10) 0.3377(11) 0.033(3) Uani 1 1 d . . . . .
H1A H 0.947237 0.461731 0.400384 0.039 Uiso 1 1 calc R U . . .
H1B H 1.002393 0.502715 0.301592 0.039 Uiso 1 1 calc R U . . .
N2 N 0.5975(15) 0.4765(12) 0.3504(12) 0.041(3) Uani 1 1 d . . . . .
H2A H 0.513947 0.461280 0.386401 0.049 Uiso 1 1 calc R U . . .
H2B H 0.570027 0.500342 0.287264 0.049 Uiso 1 1 calc R U . . .
C2 C 0.688(2) 0.3736(13) 0.3390(17) 0.047(4) Uani 1 1 d . . . . .
H2C H 0.630812 0.318704 0.300220 0.056 Uiso 1 1 calc R U . . .
H2D H 0.710634 0.343295 0.407618 0.056 Uiso 1 1 calc R U . . .
C4 C 0.8286(19) 0.5865(12) 0.3503(16) 0.042(4) Uani 1 1 d . . . . .
H4A H 0.808001 0.617750 0.281735 0.050 Uiso 1 1 calc R U . . .
H4B H 0.886231 0.640781 0.389650 0.050 Uiso 1 1 calc R U . . .
C3 C 0.6827(17) 0.5660(12) 0.4050(15) 0.038(3) Uani 1 1 d . . . . .
H3A H 0.623165 0.633559 0.405806 0.046 Uiso 1 1 calc R U . . .
H3B H 0.701943 0.544344 0.476980 0.046 Uiso 1 1 calc R U . . .
C1 C 0.8334(18) 0.3984(12) 0.2820(13) 0.037(3) Uani 1 1 d . . . . .
H1C H 0.894177 0.331599 0.277848 0.045 Uiso 1 1 calc R U . . .
H1D H 0.811040 0.422527 0.211220 0.045 Uiso 1 1 calc R U . . .

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 0.0488(6) 0.0318(4) 0.0404(5) 0.0092(3) 0.0012(4) 0.0019(4)
I2 0.0402(7) 0.024(2) 0.0358(6) 0.0063(16) 0.0000(5) 0.0046(16)
I3 0.0331(7) 0.023(2) 0.043(3) -0.0045(15) 0.0037(13) -0.0039(14)
I4 0.034(2) 0.040(4) 0.0391(8) 0.002(2) -0.0024(13) -0.019(2)
Br2 0.0402(7) 0.024(2) 0.0358(6) 0.0063(16) 0.0000(5) 0.0046(16)
Br3 0.0331(7) 0.023(2) 0.043(3) -0.0045(15) 0.0037(13) -0.0039(14)
Br4 0.034(2) 0.040(4) 0.0391(8) 0.002(2) -0.0024(13) -0.019(2)
Cd1 0.0330(5) 0.0301(5) 0.0383(5) 0.0038(4) -0.0007(5) -0.0016(4)
N1 0.026(5) 0.036(6) 0.036(7) -0.002(5) 0.003(5) -0.002(5)
N2 0.032(6) 0.042(6) 0.048(9) -0.005(6) 0.002(6) -0.003(6)
C2 0.045(9) 0.030(7) 0.065(11) -0.013(8) 0.003(8) -0.007(7)
C4 0.046(8) 0.023(6) 0.056(10) -0.005(6) -0.012(7) 0.002(6)
C3 0.034(7) 0.030(6) 0.050(9) -0.012(7) -0.004(7) -0.003(6)
C1 0.045(8) 0.029(6) 0.037(8) -0.003(6) 0.005(7) 0.000(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 Cd1 2.7535(13) . ?
I2 Cd1 2.766(7) . ?
I3 Cd1 2.776(10) . ?
I4 Cd1 2.824(17) . ?
Br2 Cd1 2.618(18) . ?
Br3 Cd1 2.564(18) . ?
Br4 Cd1 2.612(12) . ?
N1 C4 1.457(19) . ?
N1 C1 1.488(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C2 1.49(2) . ?
N2 C3 1.490(19) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C2 C1 1.51(2) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C4 C3 1.49(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?

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
Br3 Cd1 Br4 104.2(6) . . ?
Br3 Cd1 Br2 106.5(6) . . ?
Br4 Cd1 Br2 110.3(5) . . ?
Br3 Cd1 I1 114.9(5) . . ?
Br4 Cd1 I1 112.3(4) . . ?
Br2 Cd1 I1 108.4(4) . . ?
I1 Cd1 I2 110.76(16) . . ?
I1 Cd1 I3 113.4(2) . . ?
I2 Cd1 I3 109.4(3) . . ?
I1 Cd1 I4 113.5(5) . . ?
I2 Cd1 I4 103.3(5) . . ?
I3 Cd1 I4 105.8(5) . . ?
C4 N1 C1 111.2(12) . . ?
C4 N1 H1A 109.4 . . ?
C1 N1 H1A 109.4 . . ?
C4 N1 H1B 109.4 . . ?
C1 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
C2 N2 C3 112.1(13) . . ?
C2 N2 H2A 109.2 . . ?
C3 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
C3 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
N2 C2 C1 110.1(14) . . ?
N2 C2 H2C 109.6 . . ?
C1 C2 H2C 109.6 . . ?
N2 C2 H2D 109.6 . . ?
C1 C2 H2D 109.6 . . ?
H2C C2 H2D 108.2 . . ?
N1 C4 C3 113.1(12) . . ?
N1 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C4 C3 N2 109.9(13) . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
N2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N1 C1 C2 110.3(13) . . ?
N1 C1 H1C 109.6 . . ?
C2 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
C2 C1 H1D 109.6 . . ?
H1C C1 H1D 108.1 . . ?

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
C3 N2 C2 C1 -57(2) . . . . ?
C1 N1 C4 C3 56.0(19) . . . . ?
N1 C4 C3 N2 -54.3(19) . . . . ?
C2 N2 C3 C4 54.6(19) . . . . ?
C4 N1 C1 C2 -56.3(18) . . . . ?
N2 C2 C1 N1 56(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A I4^a 0.89 2.60 3.47(3) 165.0 1_655 yes
N1 H1A Br4^b 0.89 2.57 3.44(2) 163.9 1_655 yes
N1 H1B I2^a 0.89 3.02 3.664(15) 131.0 2_664 yes
N1 H1B I3^a 0.89 2.99 3.549(17) 122.5 2_664 yes
N1 H1B Br2^b 0.89 2.92 3.56(2) 131.0 2_664 yes
N1 H1B Br3^b 0.89 2.89 3.49(2) 126.1 2_664 yes
N2 H2A I2^a 0.89 2.88 3.560(17) 134.0 . yes
N2 H2A I3^a 0.89 2.96 3.487(18) 119.7 2_564 yes
N2 H2A Br2^b 0.89 2.80 3.47(3) 133.6 . yes
N2 H2A Br3^b 0.89 2.97 3.47(2) 117.4 2_564 yes
N2 H2B I4^a 0.89 2.64 3.52(3) 169.9 2_564 yes
N2 H2B Br4^b 0.89 2.57 3.46(2) 173.2 2_564 yes
C2 H2C I3^a 0.97 3.30 3.87(2) 119.4 2_564 yes
C2 H2D I2^a 0.97 3.32 3.86(2) 117.6 . yes
C4 H4A I2^a 0.97 3.17 3.80(2) 124.0 2_664 yes
C4 H4A I3^a 0.97 2.92 3.63(2) 131.0 4_566 yes
C4 H4A Br3^b 0.97 3.03 3.70(3) 127.3 4_566 yes
C4 H4B I1 0.97 3.33 4.040(17) 131.4 1_655 yes
C3 H3B I2^a 0.97 3.31 3.866(19) 118.5 . yes
C3 H3B I4^a 0.97 3.20 3.96(3) 135.9 1_655 yes
C3 H3A I1 0.97 3.29 3.994(15) 131.5 . yes
C1 H1C I2^a 0.97 3.07 3.859(17) 139.3 4_556 yes
C1 H1C I3^a 0.97 3.25 3.84(2) 120.9 2_664 yes

_refine_diff_density_max         1.764
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.315

_shelx_res_file                  
;
TITL jr1-4c_autored_a.res in P2(1)2(1)2(1)
    x.res
    created by SHELXL-2018/3 at 16:51:42 on 30-Jan-2024
REM Old TITL jr1-4c_autored_a.res in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1): R1 0.124, Rweak 0.021, Alpha 0.002
REM <I/s> 0.977 for 20 systematic absences, Orientation as input
REM Flack x = 0.394 ( 0.020 ) from 991 Parsons' quotients
REM Formula found by SHELXT: C2 I4 N3 Br
CELL 1.54184 8.8562 12.0536 12.7689 90 90 90
ZERR 4 0.0002 0.0002 0.0003 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N Br Cd
UNIT 16 48 9.72 8 6.28 4

twin
eadp i2 br2
eadp i3 br3
eadp i4 br4
rem exyz i2 br2
rem exyz i3 br3
rem exyz i4 br4
omit 0 0 6
omit 0 1 6
omit 1 2 8
omit 0 1 4
omit 1 2 7
omit 0 0 4
omit 0 2 8
omit 1 3 7
omit -1 2 7
omit 1 3 6
L.S. 40
PLAN  11
TEMP 0
CONF
BOND $H
htab
rem simu 0.02 0.04 3.8 $n $c
list 4
fmap 2 53
acta
MORE -1
BOND $H

EQIV $1 x+1, y, z
HTAB N1 I4_$1
HTAB N1 Br4_$1
EQIV $2 -x+3/2, -y+1, z-1/2
HTAB N1 I2_$2
HTAB N1 I3_$2
HTAB N1 Br2_$2
HTAB N1 Br3_$2
HTAB N2 I2
EQIV $3 -x+1/2, -y+1, z-1/2
HTAB N2 I3_$3
HTAB N2 Br2
HTAB N2 Br3_$3
HTAB N2 I4_$3
HTAB N2 Br4_$3
HTAB C2 I3_$3
HTAB C2 I2
HTAB C4 I2_$2
EQIV $4 x+1/2, -y+3/2, -z+1
HTAB C4 I3_$4
HTAB C4 Br3_$4
HTAB C4 I1_$1
HTAB C3 I2
HTAB C3 I4_$1
HTAB C3 I1
EQIV $5 x+1/2, -y+1/2, -z+1
HTAB C1 I2_$5
HTAB C1 I3_$2
WGHT    0.097000
BASF   0.13052
FVAR       0.20674   0.58773   0.50976   0.32816
mole 1
I1    3    0.256978    0.674109    0.420901    11.00000    0.04883    0.03180 =
         0.04045    0.00920    0.00119    0.00191
PART   1
I2    3    0.456088    0.379773    0.594895    21.00000    0.04015    0.02408 =
         0.03579    0.00632   -0.00005    0.00464
I3    3    0.238846    0.655430    0.782305    31.00000    0.03310    0.02305 =
         0.04337   -0.00446    0.00366   -0.00389
I4    3   -0.036588    0.413575    0.598530    41.00000    0.03361    0.04040 =
         0.03913    0.00167   -0.00241   -0.01855
PART   2
BR2   5    0.458624    0.400127    0.594124   -21.00000    0.04015    0.02408 =
         0.03579    0.00632   -0.00005    0.00464
BR3   5    0.241325    0.641670    0.770439   -31.00000    0.03310    0.02305 =
         0.04337   -0.00446    0.00366   -0.00389
BR4   5   -0.023954    0.432114    0.598967   -41.00000    0.03361    0.04040 =
         0.03913    0.00167   -0.00241   -0.01855
PART   0
CD1   6    0.232062    0.539670    0.594388    11.00000    0.03297    0.03010 =
         0.03825    0.00383   -0.00071   -0.00156
mole 2
N1    4    0.919271    0.486553    0.337671    11.00000    0.02582    0.03630 =
         0.03634   -0.00167    0.00323   -0.00153
AFIX  23
H1A   2    0.947237    0.461731    0.400384    11.00000   -1.20000
H1B   2    1.002393    0.502715    0.301592    11.00000   -1.20000
AFIX   0
N2    4    0.597488    0.476487    0.350418    11.00000    0.03214    0.04164 =
         0.04831   -0.00493    0.00177   -0.00266
AFIX  23
H2A   2    0.513947    0.461280    0.386401    11.00000   -1.20000
H2B   2    0.570027    0.500342    0.287264    11.00000   -1.20000
AFIX   0
C2    1    0.688217    0.373581    0.338976    11.00000    0.04506    0.02983 =
         0.06520   -0.01328    0.00254   -0.00709
AFIX  23
H2C   2    0.630812    0.318704    0.300220    11.00000   -1.20000
H2D   2    0.710634    0.343295    0.407618    11.00000   -1.20000
AFIX   0
C4    1    0.828599    0.586529    0.350277    11.00000    0.04622    0.02268 =
         0.05592   -0.00530   -0.01189    0.00223
AFIX  23
H4A   2    0.808001    0.617750    0.281735    11.00000   -1.20000
H4B   2    0.886231    0.640781    0.389650    11.00000   -1.20000
AFIX   0
C3    1    0.682718    0.566025    0.405049    11.00000    0.03367    0.03027 =
         0.05035   -0.01180   -0.00412   -0.00343
AFIX  23
H3A   2    0.623165    0.633559    0.405806    11.00000   -1.20000
H3B   2    0.701943    0.544344    0.476980    11.00000   -1.20000
AFIX   0
C1    1    0.833381    0.398391    0.282013    11.00000    0.04512    0.02921 =
         0.03714   -0.00281    0.00536   -0.00003
AFIX  23
H1C   2    0.894177    0.331599    0.277848    11.00000   -1.20000
H1D   2    0.811040    0.422527    0.211220    11.00000   -1.20000
AFIX   0
HKLF 4




REM  jr1-4c_autored_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1323, GooF = S = 1.055, Restrained GooF = 1.055 for all data
REM R1 = 0.0509 for 2544 Fo > 4sig(Fo) and 0.0535 for all 2695 data
REM 113 parameters refined using 0 restraints

END

WGHT      0.0974      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 I4_$1
HTAB N1 Br4_$1
HTAB N1 I2_$2
HTAB N1 I3_$2
HTAB N1 Br2_$2
HTAB N1 Br3_$2
HTAB N2 I2
HTAB N2 I3_$3
HTAB N2 Br2
HTAB N2 Br3_$3
HTAB N2 I4_$3
HTAB N2 Br4_$3
HTAB C2 I3_$3
HTAB C2 I2
HTAB C4 I2_$2
HTAB C4 I3_$4
HTAB C4 Br3_$4
HTAB C3 I1
HTAB C3 I2
HTAB C3 I4_$1
HTAB C1 I2_$5
HTAB C1 I3_$2

REM Highest difference peak  1.764,  deepest hole -1.997,  1-sigma level  0.315
Q1    1   0.2408  0.6600  0.5873  11.00000  0.05    1.76
Q2    1   0.2569  0.6819  0.4926  11.00000  0.05    1.63
Q3    1   0.4716  0.3815  0.6636  11.00000  0.05    1.41
Q4    1   0.2566  0.6737  0.3413  11.00000  0.05    1.35
Q5    1   0.2532  0.6649  0.7084  11.00000  0.05    1.27
Q6    1   0.0093  0.4187  0.5353  11.00000  0.05    1.18
Q7    1   0.2271  0.5335  0.5185  11.00000  0.05    1.18
Q8    1   0.4660  0.3825  0.5255  11.00000  0.05    1.14
Q9    1   0.2494  0.6521  0.8571  11.00000  0.05    1.13
Q10   1  -0.0027  0.4094  0.6667  11.00000  0.05    1.13
Q11   1   0.2605  0.7880  0.4190  11.00000  0.05    1.13
;
_shelx_res_checksum              48869
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdICl
_database_code_depnum_ccdc_archive 'CCDC 2381800'
loop_
_audit_author_name
_audit_author_address
'jieru Yang'
;Fujian Normal University
China
;
_audit_update_record             
;
2024-09-04 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 N2, Cd Cl2 I2'
_chemical_formula_sum            'C4 H12 Cd Cl2 I2 N2'
_chemical_formula_weight         525.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.3343(2)
_cell_length_b                   12.0155(2)
_cell_length_c                   10.0864(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.087(2)
_cell_angle_gamma                90
_cell_volume                     1290.08(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7322
_cell_measurement_theta_min      5.5240
_cell_measurement_theta_max      77.4410

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.704
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    54.599
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9382
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         5.552
_diffrn_reflns_theta_max         78.118
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1384
_reflns_number_gt                1313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0379P)²+13.3384P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00053(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1384
_refine_ls_number_parameters     53
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0825
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cd1 Cd 0.500000 0.18488(5) 0.750000 0.03654(19) Uani 1 2 d S T P . .
I1 I 0.31647(4) 0.07219(3) 0.54412(4) 0.04329(18) Uani 1 1 d . . . . .
Cl1 Cl 0.39221(13) 0.30931(13) 0.87291(14) 0.0433(3) Uani 1 1 d . . . . .
N1 N 0.5936(5) 0.2919(5) 0.1851(6) 0.0514(14) Uani 1 1 d . . . . .
H1A H 0.548038 0.291670 0.093553 0.062 Uiso 1 1 calc R U . . .
H1B H 0.674368 0.290674 0.193404 0.062 Uiso 1 1 calc R U . . .
C1 C 0.5642(7) 0.1925(6) 0.2520(8) 0.0533(17) Uani 1 1 d . . . . .
H1C H 0.578763 0.126781 0.203920 0.064 Uiso 1 1 calc R U . . .
H1D H 0.620065 0.189035 0.349418 0.064 Uiso 1 1 calc R U . . .
C2 C 0.5671(11) 0.3948(7) 0.2508(10) 0.083(3) Uani 1 1 d . . . . .
H2A H 0.580464 0.459094 0.199600 0.100 Uiso 1 1 calc R U . . .
H2B H 0.624425 0.399936 0.347407 0.100 Uiso 1 1 calc R U . . .

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
Cd1 0.0324(3) 0.0384(3) 0.0381(3) 0.000 0.0113(2) 0.000
I1 0.0418(3) 0.0370(2) 0.0460(3) -0.00297(14) 0.00857(17) -0.00731(14)
Cl1 0.0404(7) 0.0542(8) 0.0341(6) -0.0023(5) 0.0112(5) 0.0160(6)
N1 0.040(3) 0.068(4) 0.049(3) 0.003(3) 0.019(2) -0.012(3)
C1 0.064(4) 0.047(4) 0.058(4) 0.010(3) 0.032(4) 0.018(3)
C2 0.143(9) 0.054(4) 0.060(5) -0.007(4) 0.044(6) -0.053(5)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cd1 Cl1 2.5110(13) . ?
Cd1 Cl1 2.5110(13) 2_656 ?
Cd1 I1 2.7396(5) 2_656 ?
Cd1 I1 2.7396(5) . ?
N1 C1 1.465(9) . ?
N1 C2 1.481(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C1 1.443(15) 2_655 ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C2 1.52(2) 2_655 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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 Cd1 Cl1 106.92(8) . 2_656 ?
Cl1 Cd1 I1 106.95(3) . 2_656 ?
Cl1 Cd1 I1 107.28(4) 2_656 2_656 ?
Cl1 Cd1 I1 107.28(4) . . ?
Cl1 Cd1 I1 106.95(3) 2_656 . ?
I1 Cd1 I1 120.76(3) 2_656 . ?
C1 N1 C2 111.2(5) . . ?
C1 N1 H1A 109.4 . . ?
C2 N1 H1A 109.4 . . ?
C1 N1 H1B 109.4 . . ?
C2 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
C1 C1 N1 112.0(5) 2_655 . ?
C1 C1 H1C 109.2 2_655 . ?
N1 C1 H1C 109.2 . . ?
C1 C1 H1D 109.2 2_655 . ?
N1 C1 H1D 109.2 . . ?
H1C C1 H1D 107.9 . . ?
N1 C2 C2 110.6(6) . 2_655 ?
N1 C2 H2A 109.5 . . ?
C2 C2 H2A 109.5 2_655 . ?
N1 C2 H2B 109.5 . . ?
C2 C2 H2B 109.5 2_655 . ?
H2A C2 H2B 108.1 . . ?

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
C2 N1 C1 C1 56.2(10) . . . 2_655 ?
C1 N1 C2 C2 -54.4(11) . . . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Cl1 0.89 2.33 3.199(6) 166.3 1_554 yes
N1 H1B I1 0.89 3.04 3.679(5) 130.3 8 yes
N1 H1B Cl1 0.89 2.78 3.481(6) 136.2 8 yes
C1 H1C I1 0.97 3.18 3.951(7) 137.2 2_655 yes
C1 H1D I1 0.97 3.32 3.777(7) 111.3 5_656 yes
C2 H2A Cl1 0.97 2.92 3.848(8) 160.4 5_666 yes
C2 H2B I1 0.97 3.16 3.943(9) 138.8 3 yes

_refine_diff_density_max         1.193
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.167

_shelx_res_file                  
;
TITL w0331-39_auto_a.res in C2/c
    x.res
    created by SHELXL-2018/3 at 17:05:36 on 30-Jan-2024
REM Old TITL W0331-39_auto in C2/c
REM SHELXT solution in C2/c
REM R1 0.092, Rweak 0.012, Alpha 0.007, Orientation as input
REM Formula found by SHELXT: C4 C2 Cl2 I3
CELL 1.54184 11.3343 12.0155 10.0864 90 110.087 90
ZERR 4 0.0002 0.0002 0.0002 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cd Cl I N
UNIT 16 48 4 8 8 8
list 4

L.S. 14
PLAN  5
CONF
MORE -1
BOND $H
fmap 2
acta
htab

EQIV $3 x, y, z-1
HTAB N1 Cl1_$3
EQIV $4 x+1/2, -y+1/2, z-1/2
HTAB N1 I1_$4
HTAB N1 Cl1_$4
EQIV $2 -x+1, y, -z+1/2
HTAB C1 I1_$2
EQIV $5 -x+1, -y, -z+1
HTAB C1 I1_$5
EQIV $6 -x+1, -y+1, -z+1
HTAB C2 Cl1_$6
EQIV $7 x+1/2, y+1/2, z
HTAB C2 I1_$7
WGHT    0.037900   13.338400
EXTI    0.000533
FVAR       0.24250   1.00914
mole 1
CD1   3    0.500000    0.184879    0.750000    10.50000    0.03241    0.03845 =
         0.03810    0.00000    0.01126    0.00000
I1    5    0.316475    0.072190    0.544125    11.00000    0.04181    0.03700 =
         0.04601   -0.00297    0.00857   -0.00731
CL1   4    0.392212    0.309307    0.872912    11.00000    0.04037    0.05419 =
         0.03408   -0.00226    0.01119    0.01604
mole 2
N1    6    0.593628    0.291915    0.185113    11.00000    0.03988    0.06827 =
         0.04915    0.00341    0.01927   -0.01243
AFIX  23
H1A   2    0.548038    0.291670    0.093553    11.00000   -1.20000
H1B   2    0.674368    0.290674    0.193404    11.00000   -1.20000
AFIX   0
C1    1    0.564227    0.192518    0.251983    11.00000    0.06379    0.04701 =
         0.05772    0.00998    0.03194    0.01791
AFIX  23
H1C   2    0.578763    0.126781    0.203920    11.00000   -1.20000
H1D   2    0.620065    0.189035    0.349418    11.00000   -1.20000
AFIX   0
C2    1    0.567094    0.394753    0.250786    11.00000    0.14338    0.05436 =
         0.05972   -0.00713    0.04430   -0.05316
AFIX  23
H2A   2    0.580464    0.459094    0.199600    11.00000   -1.20000
H2B   2    0.624425    0.399936    0.347407    11.00000   -1.20000

AFIX   0
HKLF 4




REM  w0331-39_auto_a.res in C2/c
REM wR2 = 0.0825, GooF = S = 1.062, Restrained GooF = 1.062 for all data
REM R1 = 0.0325 for 1313 Fo > 4sig(Fo) and 0.0342 for all 1384 data
REM 53 parameters refined using 0 restraints

END

WGHT      0.0379     13.3384

REM Instructions for potential hydrogen bonds
HTAB N1 Cl1_$3
HTAB N1 I1_$4
HTAB N1 Cl1_$4
HTAB C1 I1_$2
HTAB C1 I1_$5
HTAB C2 Cl1_$6
HTAB C2 I1_$7

REM Highest difference peak  1.193,  deepest hole -1.212,  1-sigma level  0.167
Q1    1   0.3555  0.0491  0.5094  11.00000  0.05    1.19
Q2    1   0.3820  0.2630  0.8908  11.00000  0.05    0.87
Q3    1   0.3136  0.0422  0.6125  11.00000  0.05    0.82
Q4    1   0.3650  0.3085  0.6593  11.00000  0.05    0.80
Q5    1   0.5378  0.1956  0.8978  11.00000  0.05    0.62
;
_shelx_res_checksum              34579
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jr1-44a_autored
_database_code_depnum_ccdc_archive 'CCDC 2404363'
loop_
_audit_author_name
_audit_author_address
'Ke-Zhao DU'
;Fujian Normal University
China
;
_audit_update_record             
;
2024-11-21 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd I4, 2(I), 2(C4 H12 N2)'
_chemical_formula_sum            'C8 H24 Cd I6 N4'
_chemical_formula_weight         1050.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd I C N H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.2216(2)
_cell_length_b                   9.7456(2)
_cell_length_c                   23.3106(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.911(2)
_cell_angle_gamma                90
_cell_volume                     2316.69(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.6660
_cell_measurement_theta_min      3.7680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    70.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       bloke
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.792
_diffrn_reflns_theta_min         3.801
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  80.00   0.50    0.30    --   47.60 -97.00  30.00  206
  2  ω     38.00 112.00   0.50    0.80    --  108.08-125.00-120.00  148
  3  ω    -23.00  80.00   0.50    0.30    --   47.60 -97.00  30.00  206
  4  ω     65.00  97.00   0.50    0.80    --  108.08 -97.00  30.00   64
  5  ω     35.00 105.00   0.50    0.80    --  108.08 -77.00  30.00  140
  6  ω     41.00  70.00   0.50    0.80    --  108.08 -61.00  60.00   58
  7  ω     35.00  71.00   0.50    0.80    --  108.08 -61.00  30.00   72
  8  ω     36.00  70.00   0.50    0.80    --  108.08 -61.00 120.00   68
  9  ω     35.00  71.00   0.50    0.80    --  108.08 -61.00   0.00   72
 10  ω    -28.00  26.00   0.50    0.30    --   47.60 -19.00-120.00  108
 11  ω    -28.00  26.00   0.50    0.30    --   47.60 -19.00 -60.00  108
 12  ω     35.00  71.00   0.50    0.80    --  108.08 -61.00-180.00   72
 13  ω     36.00  61.00   0.50    0.80    --  108.08 -61.00 -60.00   50
 14  ω     94.00 132.00   0.50    0.80    --  108.08  30.00  90.00   76
 15  ω    114.00 175.00   0.50    0.80    --  108.08  30.00  90.00  122
 16  ω     85.00 176.00   0.50    0.80    --  108.08  97.00 138.00  182
 17  ω    -26.00  28.00   0.50    0.30    --  -47.60  19.00 150.00  108
 18  ω    -71.00 -32.00   0.50    0.80    -- -105.00  61.00 -60.00   78
 19  ω    -71.00 -32.00   0.50    0.80    -- -105.00  61.00 -90.00   78
 20  ω    -71.00 -32.00   0.50    0.80    -- -105.00  61.00 -30.00   78
 21  ω    -71.00 -32.00   0.50    0.80    -- -105.00  61.00   0.00   78
 22  ω    -80.00  23.00   0.50    0.30    --  -47.60  97.00 138.00  206
 23  ω   -105.00 -34.00   0.50    0.80    -- -105.00  97.00 138.00  142
 24  ω   -105.00 -34.00   0.50    0.80    -- -105.00  97.00 138.00  142
 25  ω    -80.00  23.00   0.50    0.30    --  -47.60  97.00 138.00  206
 26  ω   -175.00 -85.00   0.50    0.80    -- -105.00 -97.00  30.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1223707000
_diffrn_orient_matrix_UB_12      0.0155867000
_diffrn_orient_matrix_UB_13      -0.0418639000
_diffrn_orient_matrix_UB_21      0.0417224000
_diffrn_orient_matrix_UB_22      0.1475938000
_diffrn_orient_matrix_UB_23      -0.0137521000
_diffrn_orient_matrix_UB_31      0.0781615000
_diffrn_orient_matrix_UB_32      -0.0543631000
_diffrn_orient_matrix_UB_33      -0.0494674000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2114
_reflns_number_total             2372
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0804P)²+17.0557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1237
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
I3 I 0.28389(5) 0.40066(5) 0.25954(2) 0.02835(18) Uani 1 1 d . . . . .
I1 I 0.72840(5) -0.02884(6) 0.48554(2) 0.03188(19) Uani 1 1 d . . . . .
I2 I 0.51305(5) 0.69636(6) 0.35817(2) 0.03349(19) Uani 1 1 d . . . . .
Cd1 Cd 0.500000 0.58286(9) 0.250000 0.0288(2) Uani 1 2 d S T P . .
N1 N 0.6431(7) 0.1597(8) 0.3644(3) 0.0294(15) Uani 1 1 d . . . . .
H1A H 0.669866 0.097310 0.390508 0.035 Uiso 1 1 calc R U . . .
H1B H 0.705008 0.167975 0.339593 0.035 Uiso 1 1 calc R U . . .
N2 N 0.3928(7) 0.2362(8) 0.4030(3) 0.0333(16) Uani 1 1 d . . . . .
H2A H 0.332066 0.226739 0.428364 0.040 Uiso 1 1 calc R U . . .
H2B H 0.364015 0.298209 0.377135 0.040 Uiso 1 1 calc R U . . .
C1 C 0.5192(8) 0.1112(10) 0.3331(4) 0.0311(18) Uani 1 1 d . . . . .
H1C H 0.533249 0.021430 0.316633 0.037 Uiso 1 1 calc R U . . .
H1D H 0.494196 0.174029 0.302050 0.037 Uiso 1 1 calc R U . . .
C2 C 0.4110(9) 0.1029(10) 0.3738(4) 0.0356(19) Uani 1 1 d . . . . .
H2C H 0.329816 0.077056 0.352577 0.043 Uiso 1 1 calc R U . . .
H2D H 0.432043 0.032577 0.402406 0.043 Uiso 1 1 calc R U . . .
C3 C 0.5169(9) 0.2865(9) 0.4333(4) 0.0318(18) Uani 1 1 d . . . . .
H3A H 0.541893 0.225391 0.465052 0.038 Uiso 1 1 calc R U . . .
H3B H 0.502365 0.376916 0.449077 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6262(10) 0.2937(10) 0.3936(4) 0.040(2) Uani 1 1 d . . . . .
H4A H 0.606975 0.364376 0.364938 0.048 Uiso 1 1 calc R U . . .
H4B H 0.707148 0.318199 0.415300 0.048 Uiso 1 1 calc R U . . .

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
I3 0.0248(3) 0.0335(3) 0.0272(3) 0.00049(19) 0.0054(2) -0.00242(19)
I1 0.0417(3) 0.0330(3) 0.0215(3) 0.00168(18) 0.0058(2) 0.0099(2)
I2 0.0352(3) 0.0407(3) 0.0246(3) -0.0064(2) 0.0023(2) 0.0002(2)
Cd1 0.0295(4) 0.0349(4) 0.0223(4) 0.000 0.0047(3) 0.000
N1 0.028(3) 0.041(4) 0.020(3) 0.003(3) 0.012(3) 0.004(3)
N2 0.027(3) 0.047(4) 0.026(3) -0.012(3) 0.006(3) 0.010(3)
C1 0.028(4) 0.040(5) 0.025(4) -0.006(3) 0.000(3) 0.009(4)
C2 0.036(5) 0.039(5) 0.032(4) -0.007(4) 0.009(4) 0.001(4)
C3 0.032(4) 0.034(4) 0.030(4) -0.014(3) 0.006(3) 0.002(4)
C4 0.049(6) 0.035(5) 0.037(5) -0.006(4) 0.009(4) -0.002(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
I3 Cd1 2.8547(7) . ?
I2 Cd1 2.7484(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.494(11) . ?
N1 C4 1.487(12) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.484(11) . ?
N2 C3 1.492(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.507(12) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.501(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
I3 Cd1 I3 103.07(3) . 2_655 ?
I2 Cd1 I3 109.415(16) . 2_655 ?
I2 Cd1 I3 109.417(16) 2_655 . ?
I2 Cd1 I3 99.687(16) . . ?
I2 Cd1 I3 99.688(16) 2_655 2_655 ?
I2 Cd1 I2 132.53(4) 2_655 . ?
H1A N1 H1B 107.9 . . ?
C1 N1 H1A 109.1 . . ?
C1 N1 H1B 109.1 . . ?
C4 N1 H1A 109.1 . . ?
C4 N1 H1B 109.1 . . ?
C4 N1 C1 112.4(7) . . ?
H2A N2 H2B 107.9 . . ?
C2 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
C2 N2 C3 112.1(7) . . ?
C3 N2 H2A 109.2 . . ?
C3 N2 H2B 109.2 . . ?
N1 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
N1 C1 C2 110.1(7) . . ?
H1C C1 H1D 108.2 . . ?
C2 C1 H1C 109.6 . . ?
C2 C1 H1D 109.6 . . ?
N2 C2 C1 111.2(8) . . ?
N2 C2 H2C 109.4 . . ?
N2 C2 H2D 109.4 . . ?
C1 C2 H2C 109.4 . . ?
C1 C2 H2D 109.4 . . ?
H2C C2 H2D 108.0 . . ?
N2 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
N2 C3 C4 111.6(7) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N1 C4 C3 110.8(8) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?

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 N2 55.4(10) . . . . ?
N2 C3 C4 N1 -53.7(11) . . . . ?
C1 N1 C4 C3 55.4(10) . . . . ?
C2 N2 C3 C4 54.3(10) . . . . ?
C3 N2 C2 C1 -55.2(10) . . . . ?
C4 N1 C1 C2 -56.1(10) . . . . ?

_shelx_res_file                  
;
TITL jr1-44a_autored_a.res in C2/c
    jr1-44a_autored.res
    created by SHELXL-2019/2 at 16:47:29 on 20-Nov-2024
REM Old TITL JR1-44A_autored in C2/c
REM SHELXT solution in C2/c: R1 0.099, Rweak 0.003, Alpha 0.008
REM <I/s> 0.591 for 147 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N4 I7
CELL 1.54184 10.2216 9.7456 23.3106 90 93.911 90
ZERR 4 0.0002 0.0002 0.0004 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cd I N
UNIT 32 96 4 24 16

L.S. 20 0 0
PLAN  10
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\JR1-44A_autored.hkl">
REM </olex2.extras>

WGHT    0.080400   17.055698
FVAR       0.10142
I3    4    0.283889    0.400658    0.259540    11.00000    0.02476    0.03355 =
         0.02725    0.00049    0.00541   -0.00242
I1    4    0.728400   -0.028840    0.485537    11.00000    0.04165    0.03297 =
         0.02153    0.00168    0.00584    0.00995
I2    4    0.513048    0.696363    0.358173    11.00000    0.03519    0.04074 =
         0.02457   -0.00642    0.00229    0.00022
CD1   3    0.500000    0.582858    0.250000    10.50000    0.02948    0.03492 =
         0.02230    0.00000    0.00466    0.00000
N1    5    0.643082    0.159736    0.364423    11.00000    0.02848    0.04112 =
         0.02012    0.00251    0.01220    0.00422
AFIX  23
H1A   2    0.669866    0.097310    0.390508    11.00000   -1.20000
H1B   2    0.705008    0.167975    0.339593    11.00000   -1.20000
AFIX   0
N2    5    0.392776    0.236190    0.403038    11.00000    0.02720    0.04667 =
         0.02649   -0.01172    0.00618    0.00971
AFIX  23
H2A   2    0.332066    0.226739    0.428364    11.00000   -1.20000
H2B   2    0.364015    0.298209    0.377135    11.00000   -1.20000
AFIX   0
C1    1    0.519230    0.111161    0.333144    11.00000    0.02791    0.04007 =
         0.02507   -0.00618    0.00020    0.00886
AFIX  23
H1C   2    0.533249    0.021430    0.316633    11.00000   -1.20000
H1D   2    0.494196    0.174029    0.302050    11.00000   -1.20000
AFIX   0
C2    1    0.410987    0.102912    0.373812    11.00000    0.03635    0.03888 =
         0.03233   -0.00719    0.00886    0.00109
AFIX  23
H2C   2    0.329816    0.077056    0.352577    11.00000   -1.20000
H2D   2    0.432043    0.032577    0.402406    11.00000   -1.20000
AFIX   0
C3    1    0.516874    0.286484    0.433329    11.00000    0.03225    0.03429 =
         0.02950   -0.01384    0.00625    0.00245
AFIX  23
H3A   2    0.541893    0.225391    0.465052    11.00000   -1.20000
H3B   2    0.502365    0.376916    0.449077    11.00000   -1.20000
AFIX   0
C4    1    0.626211    0.293682    0.393571    11.00000    0.04906    0.03506 =
         0.03656   -0.00570    0.00889   -0.00220
AFIX  23
H4A   2    0.606975    0.364376    0.364938    11.00000   -1.20000
H4B   2    0.707148    0.318199    0.415300    11.00000   -1.20000
AFIX   0
HKLF 4




REM  jr1-44a_autored_a.res in C2/c
REM wR2 = 0.1237, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0443 for 2114 Fo > 4sig(Fo) and 0.0492 for all 2372 data
REM 87 parameters refined using 0 restraints

END

WGHT      0.0804     17.0556

REM Highest difference peak  1.622,  deepest hole -1.749,  1-sigma level  0.320
Q1    1   0.5838  0.6982  0.3569  11.00000  0.05    1.62
Q2    1   0.3576  0.3977  0.2581  11.00000  0.05    1.51
Q3    1   0.2155  0.3981  0.2603  11.00000  0.05    1.37
Q4    1   0.5026  0.6045  0.3573  11.00000  0.05    1.30
Q5    1   0.4359  0.7111  0.3595  11.00000  0.05    1.24
Q6    1   0.5303  0.7032  0.4224  11.00000  0.05    1.23
Q7    1   0.2861  0.2985  0.2575  11.00000  0.05    1.17
Q8    1   0.7998 -0.0155  0.4801  11.00000  0.05    1.17
Q9    1   0.4983  0.6602  0.2015  11.00000  0.05    1.16
Q10   1   0.6455 -0.0372  0.4836  11.00000  0.05    1.13
;
_shelx_res_checksum              56492
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.805
_oxdiff_exptl_absorpt_empirical_full_min 0.392
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CdI-P
_database_code_depnum_ccdc_archive 'CCDC 2381801'
loop_
_audit_author_name
_audit_author_address
'jieru Yang'
;Fujian Normal University
China
;
_audit_update_record             
;
2024-09-04 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C4 H12 N2), Cd I4, 2(Cl)'
_chemical_formula_sum            'C8 H24 Cd Cl2 I4 N4'
_chemical_formula_weight         867.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.13180(10)
_cell_length_b                   9.4889(2)
_cell_length_c                   21.8916(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.7510(10)
_cell_angle_gamma                90
_cell_volume                     2100.14(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    274(2)
_cell_measurement_reflns_used    8952
_cell_measurement_theta_min      3.9930
_cell_measurement_theta_max      76.5360

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.743
_exptl_crystal_F_000             1576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    56.797
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      274(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10971
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.047
_diffrn_reflns_theta_max         77.457
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2190
_reflns_number_gt                2075
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0863P)²+2.6882P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2190
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.01288(3) 0.68930(4) 0.36587(2) 0.02804(18) Uani 1 1 d . . . . .
I2 I 0.21886(3) 0.39079(4) 0.24141(2) 0.02645(18) Uani 1 1 d . . . . .
Cd1 Cd 0.000000 0.57399(6) 0.250000 0.02522(19) Uani 1 2 d S T P . .
Cl1 Cl 0.23224(13) -0.03697(15) 0.48153(6) 0.0294(3) Uani 1 1 d . . . . .
N1 N 0.1454(4) 0.1544(6) 0.3736(2) 0.0257(9) Uani 1 1 d . . . . .
H1C H 0.207963 0.166461 0.347429 0.031 Uiso 1 1 calc R U . . .
H1D H 0.172665 0.087994 0.400259 0.031 Uiso 1 1 calc R U . . .
N2 N -0.1075(5) 0.2223(6) 0.4183(2) 0.0339(11) Uani 1 1 d . . . . .
H2C H -0.166855 0.206513 0.445695 0.041 Uiso 1 1 calc R U . . .
H2D H -0.139442 0.289054 0.392851 0.041 Uiso 1 1 calc R U . . .
C1 C 0.0210(5) 0.1075(6) 0.3397(2) 0.0264(12) Uani 1 1 d . . . . .
H1A H 0.035634 0.018006 0.319801 0.032 Uiso 1 1 calc R U . . .
H1B H -0.005135 0.176005 0.308282 0.032 Uiso 1 1 calc R U . . .
C2 C -0.0880(6) 0.0918(7) 0.3833(3) 0.0312(13) Uani 1 1 d . . . . .
H2A H -0.169862 0.067636 0.360242 0.037 Uiso 1 1 calc R U . . .
H2B H -0.065990 0.015386 0.411559 0.037 Uiso 1 1 calc R U . . .
C3 C 0.0184(6) 0.2731(7) 0.4505(2) 0.0300(12) Uani 1 1 d . . . . .
H3A H 0.002713 0.363012 0.469851 0.036 Uiso 1 1 calc R U . . .
H3B H 0.046721 0.206491 0.482268 0.036 Uiso 1 1 calc R U . . .
C4 C 0.1251(6) 0.2897(7) 0.4072(3) 0.0313(12) Uani 1 1 d . . . . .
H4A H 0.206804 0.316625 0.429720 0.038 Uiso 1 1 calc R U . . .
H4B H 0.101253 0.363843 0.378027 0.038 Uiso 1 1 calc R U . . .

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 0.0243(2) 0.0330(3) 0.0263(2) -0.00542(13) -0.00212(15) 0.00103(13)
I2 0.0170(2) 0.0283(3) 0.0340(3) 0.00073(13) 0.00146(15) 0.00216(12)
Cd1 0.0214(3) 0.0302(3) 0.0239(3) 0.000 -0.00036(19) 0.000
Cl1 0.0312(6) 0.0273(7) 0.0292(6) 0.0030(5) -0.0003(5) 0.0091(5)
N1 0.017(2) 0.031(3) 0.029(2) 0.004(2) 0.0033(16) 0.0025(19)
N2 0.021(2) 0.040(3) 0.041(3) -0.010(2) 0.0037(19) 0.008(2)
C1 0.023(3) 0.032(3) 0.023(3) -0.002(2) 0.0002(19) 0.005(2)
C2 0.019(3) 0.040(4) 0.034(3) -0.011(3) 0.004(2) -0.003(2)
C3 0.032(3) 0.029(3) 0.029(3) -0.009(2) -0.001(2) 0.002(2)
C4 0.027(3) 0.025(3) 0.041(3) -0.005(2) -0.001(2) -0.004(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 Cd1 2.7577(4) . ?
I2 Cd1 2.8335(5) . ?
N1 C1 1.489(7) . ?
N1 C4 1.500(8) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N2 C2 1.475(8) . ?
N2 C3 1.496(7) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
C1 C2 1.513(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.492(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
I1 Cd1 I1 133.25(3) 2 . ?
I1 Cd1 I2 108.320(10) 2 2 ?
I1 Cd1 I2 99.933(11) . 2 ?
I1 Cd1 I2 99.934(11) 2 . ?
I1 Cd1 I2 108.320(10) . . ?
I2 Cd1 I2 104.32(2) 2 . ?
C1 N1 C4 111.2(4) . . ?
C1 N1 H1C 109.4 . . ?
C4 N1 H1C 109.4 . . ?
C1 N1 H1D 109.4 . . ?
C4 N1 H1D 109.4 . . ?
H1C N1 H1D 108.0 . . ?
C2 N2 C3 112.1(4) . . ?
C2 N2 H2C 109.2 . . ?
C3 N2 H2C 109.2 . . ?
C2 N2 H2D 109.2 . . ?
C3 N2 H2D 109.2 . . ?
H2C N2 H2D 107.9 . . ?
N1 C1 C2 110.0(4) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 111.9(5) . . ?
N2 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 N2 111.4(4) . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 N1 110.4(5) . . ?
C3 C4 H4A 109.6 . . ?
N1 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
N1 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?

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
C4 N1 C1 C2 -56.9(6) . . . . ?
C3 N2 C2 C1 -53.7(7) . . . . ?
N1 C1 C2 N2 55.0(7) . . . . ?
C2 N2 C3 C4 54.1(7) . . . . ?
N2 C3 C4 N1 -55.4(7) . . . . ?
C1 N1 C4 C3 57.8(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1C I1 0.89 3.10 3.753(4) 132.2 3_545 yes
N1 H1C I2 0.89 3.16 3.775(5) 128.4 . yes
N1 H1D Cl1 0.89 2.19 3.063(5) 166.6 . yes
N2 H2C Cl1 0.89 2.39 3.141(6) 142.4 5_556 yes
N2 H2D I2 0.89 3.15 3.941(6) 149.6 2 yes
C1 H1A I1 0.97 3.29 4.011(6) 132.6 1_545 yes
C1 H1A I2 0.97 3.14 3.865(6) 132.5 4_545 yes
C1 H1B I2 0.97 3.12 3.964(6) 146.8 2 yes
C2 H2A I2 0.97 3.24 4.040(6) 141.5 3_445 yes
C3 H3A Cl1 0.97 2.93 3.517(6) 120.3 3_455 yes
C3 H3B Cl1 0.97 2.98 3.691(7) 131.2 . yes
C4 H4A Cl1 0.97 2.89 3.615(6) 132.0 7_556 yes
C4 H4B I1 0.97 3.22 4.044(7) 143.7 . yes
C4 H4B I2 0.97 3.30 3.930(6) 124.3 . yes

_refine_diff_density_max         2.053
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.288

_shelx_res_file                  
;
TITL jr1-4b_autored_a.res in C2/c
    x.res
    created by SHELXL-2018/3 at 16:12:21 on 30-Jan-2024
REM Old TITL JR1-4B_autored in C2/c
REM SHELXT solution in C2/c: R1 0.088, Rweak 0.007, Alpha 0.011
REM <I/s> 1.186 for 137 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N4 Cl2 I5
CELL 1.54184 10.1318 9.4889 21.8916 90 93.751 90
ZERR 4 0.0001 0.0002 0.0002 0 0.001 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cd Cl I N
UNIT 32 96 4 8 16 16

L.S. 20 0 0
PLAN  7
TEMP 0.95
CONF
BOND $h
list 4
MORE -1
BOND $H
fmap 2 53
acta
htab
EQIV $2 x+1/2, y-1/2, z
HTAB N1 I1_$2
HTAB N1 I2
HTAB N1 Cl1
EQIV $3 -x, -y, -z+1
HTAB N2 Cl1_$3
EQIV $1 -x, y, -z+1/2
HTAB N2 I2_$1
EQIV $4 x, y-1, z
HTAB C1 I1_$4
EQIV $5 -x+1/2, y-1/2, -z+1/2
HTAB C1 I2_$5
HTAB C1 I2_$1
EQIV $6 x-1/2, y-1/2, z
HTAB C2 I2_$6
EQIV $7 x-1/2, y+1/2, z
HTAB C3 Cl1_$7
HTAB C3 Cl1
EQIV $8 -x+1/2, -y+1/2, -z+1
HTAB C4 Cl1_$8
HTAB C4 I1
HTAB C4 I2
WGHT    0.086300    2.688200
EXTI    0.000286
FVAR       0.14872
mole 1
I1    5    0.012885    0.689300    0.365868    11.00000    0.02428    0.03302 =
         0.02634   -0.00542   -0.00212    0.00103
I2    5    0.218858    0.390795    0.241406    11.00000    0.01703    0.02829 =
         0.03401    0.00073    0.00146    0.00216
CD1   3    0.000000    0.573990    0.250000    10.50000    0.02136    0.03018 =
         0.02388    0.00000   -0.00036    0.00000
mole 2
CL1   4    0.232239   -0.036970    0.481532    11.00000    0.03121    0.02734 =
         0.02921    0.00297   -0.00032    0.00915
mole 3
N1    6    0.145370    0.154404    0.373638    11.00000    0.01745    0.03086 =
         0.02898    0.00378    0.00330    0.00251
AFIX  23
H1C   2    0.207963    0.166461    0.347429    11.00000   -1.20000
H1D   2    0.172665    0.087994    0.400259    11.00000   -1.20000
AFIX   0
N2    6   -0.107498    0.222271    0.418257    11.00000    0.02096    0.04035 =
         0.04063   -0.01002    0.00369    0.00802
AFIX  23
H2C   2   -0.166855    0.206513    0.445695    11.00000   -1.20000
H2D   2   -0.139442    0.289054    0.392851    11.00000   -1.20000
AFIX   0
C1    1    0.020984    0.107504    0.339670    11.00000    0.02304    0.03235 =
         0.02349   -0.00201    0.00020    0.00454
AFIX  23
H1A   2    0.035634    0.018006    0.319801    11.00000   -1.20000
H1B   2   -0.005135    0.176005    0.308282    11.00000   -1.20000
AFIX   0
C2    1   -0.087977    0.091844    0.383291    11.00000    0.01935    0.03988 =
         0.03448   -0.01144    0.00354   -0.00319
AFIX  23
H2A   2   -0.169862    0.067636    0.360242    11.00000   -1.20000
H2B   2   -0.065990    0.015386    0.411559    11.00000   -1.20000
AFIX   0
C3    1    0.018351    0.273149    0.450476    11.00000    0.03153    0.02937 =
         0.02869   -0.00897   -0.00071    0.00249
AFIX  23
H3A   2    0.002713    0.363012    0.469851    11.00000   -1.20000
H3B   2    0.046721    0.206491    0.482268    11.00000   -1.20000
AFIX   0
C4    1    0.125076    0.289678    0.407189    11.00000    0.02695    0.02544 =
         0.04116   -0.00505   -0.00122   -0.00449
AFIX  23
H4A   2    0.206804    0.316625    0.429720    11.00000   -1.20000
H4B   2    0.101253    0.363843    0.378027    11.00000   -1.20000

AFIX   0
HKLF 4




REM  jr1-4b_autored_a.res in C2/c
REM wR2 = 0.1146, GooF = S = 1.077, Restrained GooF = 1.077 for all data
REM R1 = 0.0422 for 2075 Fo > 4sig(Fo) and 0.0434 for all 2190 data
REM 88 parameters refined using 0 restraints

END

WGHT      0.0863      2.6882

REM Instructions for potential hydrogen bonds
HTAB N1 I1_$2
HTAB N1 I2
HTAB N1 Cl1
HTAB N2 Cl1_$3
HTAB N2 I2_$1
HTAB C1 I1_$4
HTAB C1 I2_$5
HTAB C1 I2_$1
HTAB C2 I2_$6
HTAB C3 Cl1_$7
HTAB C3 Cl1
HTAB C4 Cl1_$8
HTAB C4 I1
HTAB C4 I2

REM Highest difference peak  2.053,  deepest hole -1.552,  1-sigma level  0.288
Q1    1   0.0978  0.3978  0.2215  11.00000  0.05    2.05
Q2    1   0.1349  0.6949  0.3853  11.00000  0.05    1.90
Q3    1   0.3436  0.3942  0.2602  11.00000  0.05    1.89
Q4    1   0.2120  0.3943  0.2794  11.00000  0.05    1.77
Q5    1   0.0025  0.6962  0.3999  11.00000  0.05    1.70
Q6    1  -0.1129  0.6821  0.3412  11.00000  0.05    1.69
Q7    1   0.2233  0.3805  0.2016  11.00000  0.05    1.64
;
_shelx_res_checksum              95060
