# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2264014'
loop_
_audit_author_name
_audit_author_address
'Jin Chen'
;Fujian Normal University
China
;
_audit_update_record             
;
2023-05-19 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-04-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd I4, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cd I4 N2'
_chemical_formula_weight         708.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         (H12C4N2)CdI4
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'
Cd Cd -0.8075 1.2024 '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'

_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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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                   9.0318(5)
_cell_length_b                   12.2358(6)
_cell_length_c                   13.0518(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1442.37(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5740
_cell_measurement_theta_min      3.6720
_shelx_estimated_absorpt_T_max   0.132
_shelx_estimated_absorpt_T_min   0.042
_exptl_absorpt_coefficient_mu    10.037
_exptl_absorpt_correction_T_max  0.109
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 6 -16 0.2195
-2 8 -16 0.1795
-6 -5 16 0.1703
0 -8 17 0.2222
-1 3 -18 0.1730
-6 1 16 0.1541
-1 -3 -18 0.1564
-4 5 17 0.1654
1 13 12 0.1619
-12 -2 -6 0.3452
-2 -17 -2 0.1899
-3 16 -4 0.2485
-1 17 -4 0.1979
0 -15 9 0.2030
-8 -8 11 0.1648
12 -6 3 0.3836
-4 10 14 0.1666
0 -13 -12 0.1787
-2 16 6 0.1974
-2 -16 -7 0.1792
2 -16 -6 0.2219

_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.34
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.9308 5.9842 -16.2813 -0.2329 -0.9725 -0.0090
-1.7332 8.2095 -15.9793 -0.2085 -0.8721 0.4428
-5.8293 -4.8296 15.5101 0.2294 0.9571 0.1770
-0.4067 -7.5660 16.5144 0.2234 0.9336 -0.2801
-0.7807 2.8657 -18.1013 0.0761 -0.9571 0.2795
-6.4672 1.1100 15.7868 -0.0738 0.9350 0.3469
-0.6025 -2.9092 -18.1110 0.3793 -0.9140 0.1438
-3.9085 5.2830 16.5667 -0.3713 0.8956 0.2449
0.7676 12.9028 12.1715 -0.8476 0.5189 0.1105
-11.8763 -1.5649 -6.4621 0.4651 -0.1106 0.8783
-2.0578 -16.9435 -1.8597 0.9775 0.0773 -0.1963
-3.1482 16.2041 -4.3643 -0.7317 -0.3029 0.6106
-0.9465 16.7434 -4.2144 -0.8191 -0.3393 0.4625
-0.4429 -15.0044 9.0514 0.7067 0.6037 -0.3690
-8.4428 -7.5076 11.1962 0.4894 0.8002 0.3465
11.6762 -6.3243 2.8895 0.0016 -0.0089 -1.0000
-3.9364 10.2504 13.6513 -0.6017 0.7032 0.3789
-0.3647 -13.0659 -12.0102 0.8440 -0.5165 -0.1444
-2.1496 16.1346 5.7254 -0.8701 0.2080 0.4469
-1.5175 -15.6937 -7.3426 0.9601 -0.2298 -0.1594
2.3823 -16.1122 -5.6017 0.8615 -0.2059 -0.4642

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10982
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.538
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00  18.00   1.00    1.00    --   15.65 -57.00 -90.00   61
  2  ω    -21.00  39.00   1.00    1.00    --   15.65 -19.00 -90.00   60
  3  ω    -25.00  21.00   1.00    1.00    --  -16.59 -99.00 -90.00   46
  4  ω    -24.00  14.00   1.00    1.00    --  -16.59 -99.00-180.00   38
  5  ω     36.00  61.00   1.00    1.00    --   15.65-178.00 -60.00   25
  6  ω    -19.00   8.00   1.00    1.00    --  -16.59 -99.00  90.00   27
  7  ω     -1.00  85.00   1.00    1.00    --   15.65  38.00  90.00   86
  8  ω     49.00  88.00   1.00    1.00    --   15.65 178.00-120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0258701000
_diffrn_orient_matrix_UB_12      -0.0532843000
_diffrn_orient_matrix_UB_13      -0.0115237000
_diffrn_orient_matrix_UB_21      -0.0181187000
_diffrn_orient_matrix_UB_22      -0.0081083000
_diffrn_orient_matrix_UB_23      0.0523735000
_diffrn_orient_matrix_UB_31      -0.0718830000
_diffrn_orient_matrix_UB_32      0.0213023000
_diffrn_orient_matrix_UB_33      -0.0089695000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                2643
_reflns_number_total             2902
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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)'
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(12)
_refine_ls_extinction_coef       0.0139(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      1.047
_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)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.55(12)
 0.45(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C1(H1C,H1D), C2(H2C,H2D), C4(H4A,H4B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
I4 I 0.74133(11) 0.64827(7) 0.22314(7) 0.0358(3) Uani 1 1 d . . . . .
I2 I 0.96165(10) 0.38473(7) 0.40660(8) 0.0359(3) Uani 1 1 d . . . . .
I1 I 0.47166(11) 0.41751(8) 0.40387(8) 0.0391(3) Uani 1 1 d . . . . .
Cd1 Cd 0.73526(12) 0.53920(8) 0.40920(8) 0.0360(3) Uani 1 1 d . . . . .
I3 I 0.75859(14) 0.67437(8) 0.57722(8) 0.0487(3) Uani 1 1 d . . . . .
N2 N 0.4013(14) 0.5218(10) 0.1510(10) 0.042(3) Uani 1 1 d . . . . .
H2A H 0.428558 0.496743 0.212184 0.050 Uiso 1 1 calc R U . . .
H2B H 0.482795 0.537116 0.115515 0.050 Uiso 1 1 calc R U . . .
N1 N 0.0846(13) 0.5144(9) 0.1648(10) 0.034(3) Uani 1 1 d . . . . .
H1A H 0.057752 0.540106 0.103772 0.041 Uiso 1 1 calc R U . . .
H1B H 0.002707 0.499609 0.200119 0.041 Uiso 1 1 calc R U . . .
C1 C 0.1718(17) 0.4124(12) 0.1510(14) 0.043(4) Uani 1 1 d . . . . .
H1C H 0.114215 0.360043 0.111883 0.051 Uiso 1 1 calc R U . . .
H1D H 0.193064 0.380486 0.217393 0.051 Uiso 1 1 calc R U . . .
C2 C 0.3141(16) 0.4358(12) 0.0960(14) 0.041(4) Uani 1 1 d . . . . .
H2C H 0.372295 0.369373 0.091509 0.050 Uiso 1 1 calc R U . . .
H2D H 0.292761 0.460322 0.026926 0.050 Uiso 1 1 calc R U . . .
C4 C 0.3116(17) 0.6228(13) 0.1640(14) 0.044(4) Uani 1 1 d . . . . .
H4A H 0.288996 0.653543 0.097328 0.053 Uiso 1 1 calc R U . . .
H4B H 0.368214 0.676442 0.202268 0.053 Uiso 1 1 calc R U . . .
C3 C 0.1713(17) 0.5982(11) 0.2195(12) 0.035(3) Uani 1 1 d . . . . .
H3A H 0.193991 0.572527 0.288003 0.042 Uiso 1 1 calc R U . . .
H3B H 0.112968 0.664489 0.225611 0.042 Uiso 1 1 calc R U . . .


_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
I4 Cd1 2.7714(13) . ?
I2 Cd1 2.7847(14) . ?
I1 Cd1 2.8089(14) . ?
Cd1 I3 2.7548(14) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.496(18) . ?
N2 C4 1.488(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.487(18) . ?
N1 C3 1.474(17) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.50(2) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.49(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 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
I4 Cd1 I2 107.56(5) . . ?
I4 Cd1 I1 104.50(4) . . ?
I2 Cd1 I1 105.21(4) . . ?
I3 Cd1 I4 114.01(4) . . ?
I3 Cd1 I2 111.16(5) . . ?
I3 Cd1 I1 113.75(5) . . ?
H2A N2 H2B 108.1 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 C2 110.6(11) . . ?
H1A N1 H1B 108.0 . . ?
C1 N1 H1A 109.4 . . ?
C1 N1 H1B 109.4 . . ?
C3 N1 H1A 109.4 . . ?
C3 N1 H1B 109.4 . . ?
C3 N1 C1 111.2(11) . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 C2 110.6(12) . . ?
H1C C1 H1D 108.1 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
N2 C2 C1 110.9(13) . . ?
N2 C2 H2C 109.5 . . ?
N2 C2 H2D 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 C3 110.5(12) . . ?
H4A C4 H4B 108.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N1 C3 C4 110.9(12) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.0 . . ?

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
N2 C4 C3 N1 -57.5(17) . . . . ?
N1 C1 C2 N2 55.6(17) . . . . ?
C1 N1 C3 C4 57.4(16) . . . . ?
C2 N2 C4 C3 56.8(17) . . . . ?
C4 N2 C2 C1 -56.1(17) . . . . ?
C3 N1 C1 C2 -56.3(17) . . . . ?

_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.699
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.55(12)
2 0.45(12)

####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 2264015'
loop_
_audit_author_name
_audit_author_address
'Jin Chen'
;Fujian Normal University
China
;
_audit_update_record             
;
2023-05-19 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_audit_creation_date             2023-04-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H11 Cd I3 N2'
_chemical_formula_sum            'C4 H11 Cd I3 N2'
_chemical_formula_weight         580.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4N2H11CdI3
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           9
_space_group_name_H-M_alt        'C 1 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'

_cell_length_a                   14.3680(6)
_cell_length_b                   7.13490(10)
_cell_length_c                   13.7778(5)
_cell_angle_alpha                90
_cell_angle_beta                 121.298(5)
_cell_angle_gamma                90
_cell_volume                     1206.88(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    109(3)
_cell_measurement_theta_max      77.6930
_cell_measurement_theta_min      3.7300
_shelx_estimated_absorpt_T_max   0.057
_shelx_estimated_absorpt_T_min   0.022
_exptl_absorpt_coefficient_mu    74.345
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.030
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 2 3 0.0787
5 4 -3 0.0577
-4 -1 -5 0.0688
7 3 -3 0.0546
-7 1 -1 0.0437
-9 0 1 0.0455
8 0 -1 0.0433
9 -1 -4 0.0446
8 2 -6 0.0498
2 4 -6 0.0516
-5 3 -1 0.0445
-9 1 4 0.0428
6 -3 0 0.0432
-7 3 2 0.0465
-4 4 1 0.0489
-2 -4 6 0.0411
5 -3 -7 0.0830
6 0 -9 0.0672
-4 4 3 0.0639
0 1 -7 0.0596
6 3 1 0.0710
-5 1 -4 0.0511
9 0 -5 0.0458
9 -1 -5 0.0524
8 -2 -7 0.0635
-1 5 1 0.0630

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.2581 1.9119 2.8450 -0.5675 0.8233 -0.0090
4.5709 4.0201 -2.9087 -0.3329 0.4784 0.8126
-4.2921 -0.5723 -4.5780 0.5305 -0.7715 0.3512
7.0682 2.9737 -2.6266 -0.6540 0.4981 0.5694
-7.4809 0.9950 -0.5290 0.8836 -0.3127 0.3485
-8.6060 -0.1584 1.3550 0.9427 -0.3324 0.0281
8.2879 -0.2779 -0.6563 -0.9323 0.3292 -0.1502
9.1309 -0.6979 -3.5016 -0.9997 0.0248 -0.0089
8.3737 1.6249 -6.2119 -0.7946 0.0176 0.6069
1.8996 3.5439 -5.6160 -0.0089 -0.0032 1.0000
-5.1133 2.9994 -1.4951 0.7005 -0.0198 0.7133
-9.1309 0.6979 3.5016 0.9997 -0.0248 0.0089
6.2774 -2.6452 0.4615 -0.8041 0.0219 -0.5941
-6.8147 3.0362 1.9419 0.8426 0.2491 0.4774
-4.3628 4.0369 1.0574 0.6143 0.4205 0.6677
-1.8656 -3.5327 5.6313 0.0053 0.0081 -1.0000
5.4620 -2.7594 -6.9191 -0.6076 -0.7942 -0.0090
5.5317 -0.2406 -8.8957 -0.4996 -0.6565 0.5652
-3.7779 4.1675 3.1155 0.5227 0.6800 0.5142
-0.1124 1.4359 -7.2081 0.1682 -0.5542 0.8152
5.5703 3.0093 0.8175 -0.5350 0.7782 0.3288
-4.7176 1.2547 -3.9066 0.6314 -0.4803 0.6088
9.3170 0.2036 -4.7702 -0.9709 0.0249 0.2384
8.7555 -1.4919 -5.2951 -0.9584 -0.2853 0.0096
7.6628 -1.6878 -7.1669 -0.8146 -0.5610 0.1470
-0.8765 4.5906 1.1500 0.2398 0.6866 0.6863

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4712
_diffrn_reflns_point_group_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.071
_diffrn_reflns_theta_min         7.179
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  24.00   0.50    0.05    --  -45.86  19.00-180.00   88
  2  ω    -22.00  26.00   0.50    0.05    --  -45.86  19.00   0.00   96
  3  ω   -102.00 -77.00   0.50    0.05    -- -104.50 112.00  46.00   50
  4  ω    -75.00 -13.00   0.50    0.05    --  -45.86 112.00  46.00  124
  5  ω     40.00  94.00   0.50    0.05    --  108.75-125.00 120.00  108
  6  ω     52.00  78.00   0.50    0.05    --  108.75 -95.00  90.00   52
  7  ω     86.00 111.00   0.50    0.05    --  108.75-125.00  30.00   50
  8  ω     86.00 112.00   0.50    0.05    --  108.75-125.00   0.00   52
  9  ω     67.00  93.00   0.50    0.05    --  108.75-112.00 -46.00   52
 10  ω     10.00  53.00   0.50    0.05    --   45.86-112.00 -46.00   86
 11  ω     86.00 111.00   0.50    0.05    --  108.75 -86.00 -54.91   50
 12  ω     39.00  70.00   0.50    0.05    --  108.75 -95.00 -30.00   62
 13  ω     36.00  72.00   0.50    0.05    --  108.75 -95.00   0.00   72
 14  ω     79.00 104.00   0.50    0.05    --  108.75 -95.00   0.00   50
 15  ω     39.00  73.00   0.50    0.05    --  108.75 -61.00  30.00   68
 16  ω     39.00  73.00   0.50    0.05    --  108.75 -61.00 120.00   68
 17  ω     78.00 105.00   0.50    0.05    --  108.75 -76.00 -52.94   54
 18  ω     42.00  67.00   0.50    0.05    --  108.75 -61.00   0.00   50
 19  ω     40.00  71.00   0.50    0.05    --  108.75 -61.00 -60.00   62
 20  ω     37.00  72.00   0.50    0.05    --  108.75 -61.00-120.00   70
 21  ω     38.00  70.00   0.50    0.05    --  108.75 -77.00-150.00   64
 22  ω     81.00 106.00   0.50    0.05    --  108.75 -77.00-150.00   50
 23  ω    133.00 158.00   0.50    0.05    --  108.75  15.00-180.00   50
 24  ω    128.00 177.00   0.50    0.05    --  108.75  45.00-150.00   98
 25  ω     91.00 149.00   0.50    0.05    --  108.75  61.00-180.00  116
 26  ω     96.00 126.00   0.50    0.05    --  108.75  15.00-180.00   60
 27  ω    101.00 127.00   0.50    0.05    --  108.75  61.00-120.00   52
 28  ω    130.00 155.00   0.50    0.05    --  108.75  61.00-120.00   50
 29  ω    100.00 129.00   0.50    0.05    --  108.75  30.00  30.00   58
 30  ω    119.00 169.00   0.50    0.05    --  108.75 125.00 150.00  100
 31  ω    109.00 135.00   0.50    0.05    --  108.75 112.00  46.00   52
 32  ω     84.00 132.00   0.50    0.05    --  108.75 125.00-120.00   96
 33  ω    150.00 177.00   0.50    0.05    --  108.75 125.00-120.00   54
 34  ω    -54.00 -28.00   0.50    0.05    --  -45.86 -77.00-120.00   52
 35  ω   -112.00 -58.00   0.50    0.05    --  -45.86 -77.00-120.00  108
 36  ω   -122.00 -83.00   0.50    0.05    -- -104.50-112.00 -46.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1124937000
_diffrn_orient_matrix_UB_12      0.0344454000
_diffrn_orient_matrix_UB_13      -0.0147218000
_diffrn_orient_matrix_UB_21      0.0523365000
_diffrn_orient_matrix_UB_22      0.1338262000
_diffrn_orient_matrix_UB_23      0.1027230000
_diffrn_orient_matrix_UB_31      -0.0188778000
_diffrn_orient_matrix_UB_32      0.1658857000
_diffrn_orient_matrix_UB_33      -0.0797592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.677
_reflns_Friedel_fraction_max     0.624
_reflns_number_gt                2036
_reflns_number_total             2046
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.281
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.060
_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)+(0.0874P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1043
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.01(2)
 -0.01(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
3.a Ternary CH refined with riding coordinates:
 N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C4(H4A,H4B), C1(H1C,H1D), C3(H3A,H3B), C2(H2A,H2B)
;
_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
I2 I 0.47222(6) 0.34349(10) 0.26232(6) 0.0260(2) Uani 1 1 d . . . . .
I1 I 0.67254(6) 0.83938(10) 0.50519(6) 0.0265(2) Uani 1 1 d . . . . .
I3 I 0.31210(6) 0.77654(10) 0.38582(7) 0.0274(2) Uani 1 1 d . . . . .
Cd1 Cd 0.49741(7) 0.60115(10) 0.42288(8) 0.0232(2) Uani 1 1 d . . . . .
N1 N 0.6073(10) 0.0593(17) 0.7009(10) 0.027(2) Uani 1 1 d . . . . .
H1A H 0.614014 -0.017911 0.652312 0.032 Uiso 1 1 calc R U . . .
H1B H 0.623912 -0.008051 0.764011 0.032 Uiso 1 1 calc R U . . .
N2 N 0.5449(9) 0.4080(13) 0.5754(10) 0.024(2) Uani 1 1 d . . . . .
H2 H 0.538712 0.485410 0.632304 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4679(12) 0.2531(19) 0.5449(12) 0.026(3) Uani 1 1 d . . . . .
H4A H 0.469235 0.175885 0.485907 0.032 Uiso 1 1 calc R U . . .
H4B H 0.393550 0.305189 0.511466 0.032 Uiso 1 1 calc R U . . .
C1 C 0.6866(12) 0.220(2) 0.7340(13) 0.033(3) Uani 1 1 d . . . . .
H1C H 0.685168 0.296542 0.793059 0.039 Uiso 1 1 calc R U . . .
H1D H 0.761259 0.169633 0.766365 0.039 Uiso 1 1 calc R U . . .
C3 C 0.4919(11) 0.1270(19) 0.6452(11) 0.025(3) Uani 1 1 d . . . . .
H3A H 0.481410 0.198092 0.700548 0.030 Uiso 1 1 calc R U . . .
H3B H 0.441376 0.018819 0.618175 0.030 Uiso 1 1 calc R U . . .
C2 C 0.6582(12) 0.3394(19) 0.6334(14) 0.030(3) Uani 1 1 d . . . . .
H2A H 0.708314 0.448040 0.658411 0.035 Uiso 1 1 calc R U . . .
H2B H 0.668926 0.266095 0.578962 0.035 Uiso 1 1 calc R U . . .


_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
I2 Cd1 2.7518(11) . ?
I1 Cd1 2.7463(11) . ?
I3 Cd1 2.7393(12) . ?
Cd1 N2 2.300(11) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.509(19) . ?
N1 C3 1.500(18) . ?
N2 H2 1.0000 . ?
N2 C4 1.462(17) . ?
N2 C2 1.476(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.532(17) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C1 C2 1.49(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?

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 I2 117.07(4) . . ?
I3 Cd1 I2 116.50(4) . . ?
I3 Cd1 I1 112.80(3) . . ?
N2 Cd1 I2 100.8(3) . . ?
N2 Cd1 I1 102.7(3) . . ?
N2 Cd1 I3 104.0(3) . . ?
H1A N1 H1B 107.9 . . ?
C1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
C3 N1 H1A 109.3 . . ?
C3 N1 H1B 109.3 . . ?
C3 N1 C1 111.8(11) . . ?
Cd1 N2 H2 106.3 . . ?
C4 N2 Cd1 111.7(8) . . ?
C4 N2 H2 106.3 . . ?
C4 N2 C2 111.2(10) . . ?
C2 N2 Cd1 114.5(9) . . ?
C2 N2 H2 106.3 . . ?
N2 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
N2 C4 C3 113.7(11) . . ?
H4A C4 H4B 107.7 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 108.1 . . ?
C2 C1 N1 110.7(11) . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
N1 C3 C4 108.7(11) . . ?
N1 C3 H3A 109.9 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N2 C2 C1 112.7(13) . . ?
N2 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?

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
Cd1 N2 C4 C3 -176.5(10) . . . . ?
Cd1 N2 C2 C1 178.1(10) . . . . ?
N1 C1 C2 N2 54.9(16) . . . . ?
N2 C4 C3 N1 -54.5(15) . . . . ?
C4 N2 C2 C1 -54.2(16) . . . . ?
C1 N1 C3 C4 54.4(15) . . . . ?
C3 N1 C1 C2 -55.9(15) . . . . ?
C2 N2 C4 C3 54.3(16) . . . . ?

_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 1.693
_oxdiff_exptl_absorpt_empirical_full_min 0.544
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.01(2)
2 -0.01(2)

