# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_crystal1
_database_code_depnum_ccdc_archive 'CCDC 2486224'
loop_
_audit_author_name
_audit_author_address
'jiahui zhang'
;Beijing institute of technology
China
;
_audit_update_record             
;
2025-09-08 deposited with the CCDC.	2025-11-17 downloaded from the CCDC.
;
_audit_creation_date             2025-09-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C18 H24 Cd6 Cl12 N12)'
_chemical_formula_sum            'C9 H12 Cd3 Cl6 N6'
_chemical_formula_weight         754.15
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   11.0566(10)
_cell_length_b                   3.8319(3)
_cell_length_c                   15.2570(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     646.41(9)
_cell_formula_units_Z            1.333333
_cell_measurement_reflns_used    2081
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2610
_cell_measurement_theta_min      3.9720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3651
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.109
_diffrn_reflns_theta_min         3.920
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00   6.00   0.50    4.00    --    3.60  13.00  53.00   50
  2  ω    -64.00   1.00   0.50    4.00    --    3.60 -82.00-150.00  130
  3  ω    -64.00  23.00   0.50    4.00    --    3.60 -82.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                773
_reflns_number_total             870
_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 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         870
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.248
_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)+3.2359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0720
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 N1, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
3. Others
 Fixed Sof: N1(0.5) N2(0.5) H2(0.5) C1(0.5) H1(0.5) C2(0.5) H2A(0.5) C3(0.5)
 H3(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cd1 Cd 0.60159(5) 0.750000 0.58956(3) 0.02595(17) Uani 1 2 d S T P . .
Cl1 Cl 0.57268(14) 0.750000 0.41602(9) 0.0254(3) Uani 1 2 d S T P A .
Cl2 Cl 0.75934(15) 0.250000 0.57774(10) 0.0274(3) Uani 1 2 d S T P A .
N1 N 0.5968(6) 0.74(3) 0.7357(4) 0.026(4) Uani 0.5 1 d . . P A -1
N2 N 0.6615(8) 0.797(17) 0.8701(4) 0.040(10) Uani 0.5 1 d . . P A -1
H2 H 0.707567 0.843319 0.913988 0.047 Uiso 0.5 1 calc R U P A -1
C1 C 0.6869(9) 0.862(3) 0.7858(5) 0.036(3) Uani 0.5 1 d . . P A -1
H1 H 0.755651 0.975260 0.765223 0.043 Uiso 0.5 1 calc R U P A -1
C2 C 0.5126(9) 0.616(3) 0.7915(6) 0.036(2) Uani 0.5 1 d . . P A -1
H2A H 0.438005 0.526069 0.774882 0.043 Uiso 0.5 1 calc R U P A -1
C3 C 0.5513(11) 0.645(3) 0.8746(6) 0.044(3) Uani 0.5 1 d . . P A -1
H3 H 0.510560 0.574986 0.924995 0.053 Uiso 0.5 1 calc R U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0325(3) 0.0232(3) 0.0222(2) 0.000 -0.0034(2) 0.000
Cl1 0.0283(8) 0.0256(8) 0.0222(7) 0.000 -0.0017(6) 0.000
Cl2 0.0262(8) 0.0262(8) 0.0298(7) 0.000 0.0000(6) 0.000
N1 0.030(3) 0.025(12) 0.024(3) 0.000(8) -0.002(2) 0.006(7)
N2 0.043(4) 0.05(3) 0.023(3) 0.002(6) -0.009(3) 0.004(7)
C1 0.028(4) 0.053(8) 0.028(4) -0.001(4) 0.000(3) -0.002(4)
C2 0.032(5) 0.040(6) 0.036(4) -0.004(4) 0.002(4) -0.004(4)
C3 0.056(7) 0.042(8) 0.033(5) 0.006(4) 0.005(4) -0.015(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 2.7186(12) 5_666 ?
Cd1 Cl1 2.6670(15) . ?
Cd1 Cl1 2.7186(12) 5_676 ?
Cd1 Cl2 2.5973(12) . ?
Cd1 Cl2 2.5973(12) 1_565 ?
Cd1 N1 2.231(6) . ?
N1 C1 1.34(4) . ?
N1 C2 1.34(4) . ?
N2 H2 0.8600 . ?
N2 C1 1.341(16) . ?
N2 C3 1.35(3) . ?
C1 H1 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.343(13) . ?
C3 H3 0.9300 . ?

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 89.62(5) 5_666 5_676 ?
Cl1 Cd1 Cl1 83.33(4) . 5_676 ?
Cl1 Cd1 Cl1 83.33(4) . 5_666 ?
Cl2 Cd1 Cl1 90.66(4) . . ?
Cl2 Cd1 Cl1 87.36(4) . 5_666 ?
Cl2 Cd1 Cl1 90.66(4) 1_565 . ?
Cl2 Cd1 Cl1 173.56(5) . 5_676 ?
Cl2 Cd1 Cl1 87.36(4) 1_565 5_676 ?
Cl2 Cd1 Cl1 173.56(5) 1_565 5_666 ?
Cl2 Cd1 Cl2 95.07(6) . 1_565 ?
N1 Cd1 Cl1 171.7(6) . . ?
N1 Cd1 Cl1 90(2) . 5_666 ?
N1 Cd1 Cl1 91.8(19) . 5_676 ?
N1 Cd1 Cl2 94(2) . . ?
N1 Cd1 Cl2 96(2) . 1_565 ?
Cd1 Cl1 Cd1 96.66(4) . 5_666 ?
Cd1 Cl1 Cd1 89.62(5) 5_666 5_676 ?
Cd1 Cl1 Cd1 96.66(4) . 5_676 ?
Cd1 Cl2 Cd1 95.07(6) 1_545 . ?
C1 N1 Cd1 123(3) . . ?
C2 N1 Cd1 131(3) . . ?
C2 N1 C1 106.1(7) . . ?
C1 N2 H2 125.7 . . ?
C1 N2 C3 108.5(12) . . ?
C3 N2 H2 125.7 . . ?
N1 C1 H1 125.6 . . ?
N2 C1 N1 109(2) . . ?
N2 C1 H1 125.6 . . ?
N1 C2 H2A 124.8 . . ?
N1 C2 C3 110.5(14) . . ?
C3 C2 H2A 124.8 . . ?
N2 C3 H3 127.1 . . ?
C2 C3 N2 105.9(9) . . ?
C2 C3 H3 127.1 . . ?

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
Cd1 N1 C1 N2 -176(5) . . . . ?
Cd1 N1 C2 C3 177(5) . . . . ?
N1 C2 C3 N2 2(5) . . . . ?
C1 N1 C2 C3 -4(7) . . . . ?
C1 N2 C3 C2 1(4) . . . . ?
C2 N1 C1 N2 4(7) . . . . ?
C3 N2 C1 N1 -3(6) . . . . ?

_shelx_res_file                  
;
TITL crystal1_a.res in Pnma
    crystal1.res
    created by SHELXL-2018/3 at 09:24:40 on 06-Sep-2025
REM Old TITL crystal1_a.res in Pnma
REM SHELXT solution in Pnma: R1 0.096, Rweak 0.003, Alpha 0.011
REM <I/s> 0.630 for 67 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N Cd Cl2
CELL 0.71073 11.0566 3.8319 15.257 90 90 90
ZERR 1.333333 0.001 0.0003 0.001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cd Cl N
UNIT 12 16 4 8 8
RIGU 0.004 0.008 N1 C1 C2

L.S. 24 0 0
PLAN  1
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\crystal1.hkl">
REM </olex2.extras>

WGHT    0.000000    3.235900
FVAR       0.40699
CD1   3    0.601590    0.750000    0.589563    10.50000    0.03248    0.02322 =
         0.02217    0.00000   -0.00339    0.00000
CL1   4    0.572678    0.750000    0.416018    10.50000    0.02827    0.02558 =
         0.02221    0.00000   -0.00173    0.00000
CL2   4    0.759345    0.250000    0.577744    10.50000    0.02623    0.02625 =
         0.02983    0.00000    0.00004    0.00000
PART -1
N1    5    0.596845    0.736456    0.735741    10.50000    0.02952    0.02506 =
         0.02438    0.00012   -0.00221    0.00602
N2    5    0.661482    0.796572    0.870124    10.50000    0.04302    0.05240 =
         0.02329    0.00160   -0.00864    0.00379
AFIX  43
H2    2    0.707567    0.843319    0.913988    10.50000   -1.20000
AFIX   0
C1    1    0.686904    0.861795    0.785752    10.50000    0.02757    0.05262 =
         0.02752   -0.00106   -0.00041   -0.00186
AFIX  43
H1    2    0.755651    0.975260    0.765223    10.50000   -1.20000
AFIX   0
C2    1    0.512632    0.616398    0.791498    10.50000    0.03211    0.04026 =
         0.03555   -0.00371    0.00191   -0.00434
AFIX  43
H2A   2    0.438005    0.526069    0.774882    10.50000   -1.20000
AFIX   0
C3    1    0.551278    0.645044    0.874643    10.50000    0.05624    0.04197 =
         0.03310    0.00554    0.00486   -0.01455
AFIX  43
H3    2    0.510560    0.574986    0.924995    10.50000   -1.20000
AFIX   0
HKLF 4




REM  crystal1_a.res in Pnma
REM wR2 = 0.0720, GooF = S = 1.255, Restrained GooF = 1.248 for all data
REM R1 = 0.0285 for 773 Fo > 4sig(Fo) and 0.0340 for all 870 data
REM 64 parameters refined using 9 restraints

END

WGHT      0.0000      3.2358

REM Highest difference peak  0.719,  deepest hole -0.612,  1-sigma level  0.133
Q1    1   0.5005  0.7500  0.9114  10.50000  0.05    0.72
;
_shelx_res_checksum              40487
_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
;
####################################################################### 
# 
# 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_crystal3
_database_code_depnum_ccdc_archive 'CCDC 2486225'
loop_
_audit_author_name
_audit_author_address
'jiahui zhang'
;Beijing institute of technology
China
;
_audit_update_record             
;
2025-09-08 deposited with the CCDC.	2025-11-17 downloaded from the CCDC.
;
_audit_creation_date             2025-09-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C10 H16 Cd2 Cl4 N4)'
_chemical_formula_sum            'C5 H8 Cd Cl2 N2'
_chemical_formula_weight         279.43
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 1 2/m 1'
_space_group_name_Hall           '-I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   13.164(3)
_cell_length_b                   3.9649(6)
_cell_length_c                   16.918(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.14(2)
_cell_angle_gamma                90
_cell_volume                     829.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3870
_cell_measurement_theta_min      4.5820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.203
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1408
_diffrn_reflns_av_unetI/netI     0.1230
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3382
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.190
_diffrn_reflns_theta_min         3.627
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                856
_reflns_number_total             1090
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      0.937
_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)+(0.0184P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1122
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 2A
3. Others
 Fixed Sof: N1(0.5) N2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cd1 Cd 0.38283(4) 0.500000 0.24992(3) 0.0268(2) Uani 1 2 d S T P . .
Cl1 Cl 0.17819(14) 0.500000 0.16059(10) 0.0236(4) Uani 1 2 d S T P A .
Cl2 Cl 0.42880(15) 0.000000 0.16570(11) 0.0288(4) Uani 1 2 d S T P A .
N1 N 0.5460(5) 0.52(2) 0.3519(4) 0.026(5) Uani 0.5 1 d . U P A -1
N2 N 0.7130(6) 0.335(2) 0.4228(5) 0.0297(19) Uani 0.5 1 d . U P A -1
C1 C 0.6317(8) 0.328(3) 0.3475(6) 0.028(2) Uani 0.5 1 d . U P A -1
H1 H 0.633296 0.212645 0.300066 0.033 Uiso 0.5 1 calc R U P A -1
C2 C 0.5748(8) 0.605(2) 0.4339(6) 0.029(3) Uani 0.5 1 d . U P A -1
H2 H 0.533598 0.733006 0.457585 0.035 Uiso 0.5 1 calc R U P A -1
C3 C 0.6761(7) 0.470(13) 0.4768(5) 0.031(5) Uani 0.5 1 d . U P A -1
H3 H 0.711497 0.476172 0.534757 0.037 Uiso 0.5 1 calc R U P A -1
C4 C 0.8215(9) 0.184(3) 0.4445(8) 0.045(3) Uani 0.5 1 d . U P A -1
H4A H 0.830841 0.020774 0.489242 0.054 Uiso 0.5 1 calc R U P A -1
H4B H 0.875084 0.359558 0.466349 0.054 Uiso 0.5 1 calc R U P A -1
C5 C 0.8440(8) 0.005(13) 0.3701(7) 0.066(4) Uani 0.5 1 d . U P A -1
H5A H 0.840961 0.167651 0.327350 0.100 Uiso 0.5 1 calc R U P A -1
H5B H 0.790357 -0.166117 0.346977 0.100 Uiso 0.5 1 calc R U P A -1
H5C H 0.914469 -0.096546 0.390284 0.100 Uiso 0.5 1 calc R U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0220(3) 0.0274(4) 0.0282(4) 0.000 0.0050(3) 0.000
Cl1 0.0231(9) 0.0229(10) 0.0233(8) 0.000 0.0059(7) 0.000
Cl2 0.0320(9) 0.0290(11) 0.0273(9) 0.000 0.0126(8) 0.000
N1 0.024(3) 0.023(13) 0.027(3) 0.002(9) 0.003(3) -0.006(10)
N2 0.021(4) 0.037(5) 0.029(4) 0.008(3) 0.006(4) 0.003(3)
C1 0.025(5) 0.026(5) 0.029(5) -0.004(4) 0.006(4) -0.003(4)
C2 0.030(5) 0.031(7) 0.028(5) -0.002(3) 0.012(4) -0.003(4)
C3 0.037(4) 0.030(14) 0.022(4) 0.011(8) 0.006(3) 0.003(8)
C4 0.027(6) 0.046(7) 0.057(7) -0.002(6) 0.008(6) 0.005(5)
C5 0.045(6) 0.092(10) 0.068(7) 0.02(2) 0.027(6) -0.019(19)

_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 2.5955(19) . ?
Cd1 Cl1 2.7758(12) 7 ?
Cd1 Cl1 2.7758(12) 7_565 ?
Cd1 Cl2 2.6307(11) . ?
Cd1 Cl2 2.6307(12) 1_565 ?
Cd1 N1 2.246(7) . ?
N1 C1 1.38(5) . ?
N1 C2 1.35(3) . ?
N2 C1 1.352(12) . ?
N2 C3 1.29(2) . ?
N2 C4 1.474(13) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.39(2) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.56(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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 83.12(5) . 7_565 ?
Cl1 Cd1 Cl1 91.15(5) 7_565 7 ?
Cl1 Cd1 Cl1 83.12(5) . 7 ?
Cl1 Cd1 Cl2 94.06(5) . . ?
Cl1 Cd1 Cl2 94.06(5) . 1_565 ?
Cl2 Cd1 Cl1 85.47(4) . 7 ?
Cl2 Cd1 Cl1 85.47(4) 1_565 7_565 ?
Cl2 Cd1 Cl1 175.85(4) . 7_565 ?
Cl2 Cd1 Cl1 175.85(4) 1_565 7 ?
Cl2 Cd1 Cl2 97.80(6) 1_565 . ?
N1 Cd1 Cl1 86.4(16) . 7_565 ?
N1 Cd1 Cl1 89.1(16) . 7 ?
N1 Cd1 Cl1 166.8(4) . . ?
N1 Cd1 Cl2 93.1(17) . 1_565 ?
N1 Cd1 Cl2 95.9(17) . . ?
Cd1 Cl1 Cd1 96.87(5) . 7 ?
Cd1 Cl1 Cd1 91.16(5) 7_565 7 ?
Cd1 Cl1 Cd1 96.87(5) . 7_565 ?
Cd1 Cl2 Cd1 97.80(6) . 1_545 ?
C1 N1 Cd1 122(3) . . ?
C2 N1 Cd1 130.8(16) . . ?
C2 N1 C1 104.4(17) . . ?
C1 N2 C4 127.7(9) . . ?
C3 N2 C1 107.9(8) . . ?
C3 N2 C4 124.1(10) . . ?
N1 C1 H1 125.2 . . ?
N2 C1 N1 109.5(11) . . ?
N2 C1 H1 125.2 . . ?
N1 C2 H2 125.7 . . ?
N1 C2 C3 109(2) . . ?
C3 C2 H2 125.7 . . ?
N2 C3 C2 108.5(8) . . ?
N2 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
N2 C4 H4A 108.6 . . ?
N2 C4 H4B 108.6 . . ?
N2 C4 C5 114.9(11) . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 N1 C1 N2 -168(3) . . . . ?
Cd1 N1 C2 C3 160(5) . . . . ?
N1 C2 C3 N2 6(5) . . . . ?
C1 N1 C2 C3 1(5) . . . . ?
C1 N2 C3 C2 -10(3) . . . . ?
C1 N2 C4 C5 2(2) . . . . ?
C2 N1 C1 N2 -7(5) . . . . ?
C3 N2 C1 N1 11(4) . . . . ?
C3 N2 C4 C5 174(3) . . . . ?
C4 N2 C1 N1 -176(3) . . . . ?
C4 N2 C3 C2 176.3(16) . . . . ?

_shelx_res_file                  
;
TITL crystal3re_a.res in I2/m
    crystal3.res
    created by SHELXL-2018/3 at 09:33:26 on 06-Sep-2025
REM Old TITL crystal3re_a.res in Im
REM SHELXT solution in I2/m: R1 0.111, Rweak 0.006, Alpha 0.034
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 N2 Cd Cl2
CELL 0.71073 13.1637 3.9649 16.9181 90 110.145 90
ZERR 4 0.0025 0.0006 0.003 0 0.021 0
LATT 2
SYMM -X,+Y,-Z
SFAC C H Cd Cl N
UNIT 20 32 4 8 8
SIMU 0.02 0.04 2 N1 > C5

L.S. 14 0 0
PLAN  1
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\crystal3.hkl">
REM </olex2.extras>

WGHT    0.018400
FVAR       0.34807
CD1   3    0.382832    0.500000    0.249924    10.50000    0.02201    0.02736 =
         0.02820    0.00000    0.00499    0.00000
CL1   4    0.178193    0.500000    0.160592    10.50000    0.02310    0.02289 =
         0.02330    0.00000    0.00588    0.00000
CL2   4    0.428804    0.000000    0.165702    10.50000    0.03200    0.02902 =
         0.02728    0.00000    0.01256    0.00000
PART -1
N1    5    0.546030    0.518124    0.351936    10.50000    0.02429    0.02290 =
         0.02682    0.00199    0.00288   -0.00560
N2    5    0.713006    0.335005    0.422764    10.50000    0.02061    0.03692 =
         0.02947    0.00819    0.00612    0.00304
C1    1    0.631712    0.327919    0.347502    10.50000    0.02526    0.02649 =
         0.02908   -0.00363    0.00583   -0.00322
AFIX  43
H1    2    0.633296    0.212645    0.300066    10.50000   -1.20000
AFIX   0
C2    1    0.574819    0.604584    0.433857    10.50000    0.03025    0.03074 =
         0.02785   -0.00242    0.01172   -0.00309
AFIX  43
H2    2    0.533598    0.733006    0.457585    10.50000   -1.20000
AFIX   0
C3    1    0.676119    0.470048    0.476781    10.50000    0.03687    0.03047 =
         0.02160    0.01128    0.00552    0.00300
AFIX  43
H3    2    0.711497    0.476172    0.534757    10.50000   -1.20000
AFIX   0
C4    1    0.821458    0.183769    0.444524    10.50000    0.02695    0.04608 =
         0.05670   -0.00163    0.00795    0.00519
AFIX  23
H4A   2    0.830841    0.020774    0.489242    10.50000   -1.20000
H4B   2    0.875084    0.359558    0.466349    10.50000   -1.20000
AFIX   0
C5    1    0.843974    0.005017    0.370138    10.50000    0.04491    0.09196 =
         0.06827    0.02400    0.02685   -0.01900
AFIX 137
H5A   2    0.840961    0.167651    0.327350    10.50000   -1.50000
H5B   2    0.790357   -0.166117    0.346977    10.50000   -1.50000
H5C   2    0.914469   -0.096546    0.390284    10.50000   -1.50000
AFIX   0
HKLF 4




REM  crystal3re_a.res in I2/m
REM wR2 = 0.1122, GooF = S = 0.952, Restrained GooF = 0.937 for all data
REM R1 = 0.0532 for 856 Fo > 4sig(Fo) and 0.0671 for all 1090 data
REM 83 parameters refined using 42 restraints

END

WGHT      0.0183      0.0000

REM Highest difference peak  1.121,  deepest hole -1.309,  1-sigma level  0.246
Q1    1   0.1626  0.0000  0.1448  10.50000  0.05    1.12
;
_shelx_res_checksum              10666
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_crystal2
_database_code_depnum_ccdc_archive 'CCDC 2486226'
loop_
_audit_author_name
_audit_author_address
'jiahui zhang'
;Beijing institute of technology
China
;
_audit_update_record             
;
2025-09-08 deposited with the CCDC.	2025-11-17 downloaded from the CCDC.
;
_audit_creation_date             2025-09-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H6 Cd Cl2 N2'
_chemical_formula_sum            'C4 H6 Cd Cl2 N2'
_chemical_formula_weight         265.41
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   3.8859(4)
_cell_length_b                   17.1403(15)
_cell_length_c                   11.2169(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.796(8)
_cell_angle_gamma                90
_cell_volume                     743.29(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9270
_cell_measurement_theta_min      3.8550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7873
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.697
_diffrn_reflns_theta_min         3.840
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -30.00   0.50    8.00    --    0.30 -68.00-127.00   50
  2  ω    -16.00  65.00   0.50    8.00    --    0.30  68.00   5.00  162
  3  ω    -53.00   0.00   0.50    8.00    --    0.30 -82.00 -30.00  106
  4  ω    -40.00   7.00   0.50    8.00    --    0.30 -82.00-180.00   94
  5  ω    -63.00  20.00   0.50    8.00    --    0.30 -82.00  60.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1498
_reflns_number_total             1860
_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 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1860
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      0.990
_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)+(0.0226P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cd1 Cd 0.79846(8) 0.56651(2) 0.61771(2) 0.02710(11) Uani 1 1 d . . . . .
Cl1 Cl 0.7628(3) 0.41961(5) 0.55409(8) 0.0288(2) Uani 1 1 d . . . . .
Cl2 Cl 0.3490(3) 0.54545(6) 0.76943(8) 0.0314(2) Uani 1 1 d . . . . .
N1 N 0.7922(9) 0.69743(19) 0.6351(3) 0.0297(8) Uani 1 1 d . . . . .
N2 N 0.8787(10) 0.8220(2) 0.6025(3) 0.0327(8) Uani 1 1 d . . . . .
C1 C 0.9116(12) 0.7489(2) 0.5624(4) 0.0320(9) Uani 1 1 d . . . . .
H1 H 1.006708 0.736151 0.492115 0.038 Uiso 1 1 calc R U . . .
C2 C 0.6787(13) 0.7403(2) 0.7269(4) 0.0343(10) Uani 1 1 d . . . . .
H2 H 0.581426 0.719638 0.792473 0.041 Uiso 1 1 calc R U . . .
C3 C 0.7299(13) 0.8168(2) 0.7073(4) 0.0341(10) Uani 1 1 d . . . . .
H3 H 0.674624 0.857972 0.755856 0.041 Uiso 1 1 calc R U . . .
C4 C 0.9863(15) 0.8927(3) 0.5434(5) 0.0483(13) Uani 1 1 d . . . . .
H4A H 0.785847 0.922864 0.515673 0.073 Uiso 1 1 calc R U . . .
H4B H 1.109156 0.878629 0.476519 0.073 Uiso 1 1 calc R U . . .
H4C H 1.134439 0.923044 0.599267 0.073 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 0.02345(18) 0.02526(17) 0.03305(17) -0.00297(10) 0.00510(12) -0.00071(11)
Cl1 0.0262(5) 0.0276(5) 0.0328(5) -0.0017(3) 0.0039(4) 0.0002(4)
Cl2 0.0254(5) 0.0409(5) 0.0282(4) 0.0025(4) 0.0047(4) -0.0011(4)
N1 0.029(2) 0.0247(18) 0.0362(18) -0.0049(12) 0.0054(15) 0.0027(14)
N2 0.032(2) 0.0279(18) 0.0379(19) 0.0014(13) 0.0040(16) -0.0006(15)
C1 0.032(3) 0.030(2) 0.035(2) -0.0033(16) 0.0076(19) 0.0020(18)
C2 0.039(3) 0.034(2) 0.030(2) -0.0049(16) 0.0054(19) 0.0019(19)
C3 0.037(3) 0.028(2) 0.037(2) -0.0127(16) 0.0056(19) -0.0008(17)
C4 0.047(3) 0.032(3) 0.066(3) 0.012(2) 0.007(3) -0.001(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
Cd1 Cl1 2.7709(11) 3_666 ?
Cd1 Cl1 2.7094(10) 3_766 ?
Cd1 Cl1 2.6169(10) . ?
Cd1 Cl2 2.5840(10) . ?
Cd1 Cl2 2.6207(12) 1_655 ?
Cd1 N1 2.253(3) . ?
N1 C1 1.317(5) . ?
N1 C2 1.373(5) . ?
N2 C1 1.342(5) . ?
N2 C3 1.365(5) . ?
N2 C4 1.462(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.348(6) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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 90.31(3) 3_766 3_666 ?
Cl1 Cd1 Cl1 82.91(3) . 3_666 ?
Cl1 Cd1 Cl1 84.85(3) . 3_766 ?
Cl1 Cd1 Cl2 93.55(3) . 1_655 ?
Cl2 Cd1 Cl1 86.17(3) . 3_666 ?
Cl2 Cd1 Cl1 175.58(3) 1_655 3_666 ?
Cl2 Cd1 Cl1 91.40(3) . . ?
Cl2 Cd1 Cl1 175.16(3) . 3_766 ?
Cl2 Cd1 Cl1 86.73(3) 1_655 3_766 ?
Cl2 Cd1 Cl2 96.59(3) . 1_655 ?
N1 Cd1 Cl1 89.27(9) . 3_766 ?
N1 Cd1 Cl1 87.72(9) . 3_666 ?
N1 Cd1 Cl1 168.90(9) . . ?
N1 Cd1 Cl2 95.52(10) . 1_655 ?
N1 Cd1 Cl2 93.91(9) . . ?
Cd1 Cl1 Cd1 95.15(3) . 3_766 ?
Cd1 Cl1 Cd1 97.09(3) . 3_666 ?
Cd1 Cl1 Cd1 90.31(3) 3_766 3_666 ?
Cd1 Cl2 Cd1 96.59(3) . 1_455 ?
C1 N1 Cd1 127.3(3) . . ?
C1 N1 C2 105.4(4) . . ?
C2 N1 Cd1 127.2(3) . . ?
C1 N2 C3 106.9(3) . . ?
C1 N2 C4 125.5(4) . . ?
C3 N2 C4 127.6(4) . . ?
N1 C1 N2 111.5(4) . . ?
N1 C1 H1 124.2 . . ?
N2 C1 H1 124.2 . . ?
N1 C2 H2 125.2 . . ?
C3 C2 N1 109.5(4) . . ?
C3 C2 H2 125.2 . . ?
N2 C3 H3 126.7 . . ?
C2 C3 N2 106.7(3) . . ?
C2 C3 H3 126.7 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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 N1 C1 N2 -177.4(3) . . . . ?
Cd1 N1 C2 C3 177.5(3) . . . . ?
N1 C2 C3 N2 -0.3(5) . . . . ?
C1 N1 C2 C3 0.4(5) . . . . ?
C1 N2 C3 C2 0.1(5) . . . . ?
C2 N1 C1 N2 -0.3(5) . . . . ?
C3 N2 C1 N1 0.1(5) . . . . ?
C4 N2 C1 N1 179.8(4) . . . . ?
C4 N2 C3 C2 -179.5(5) . . . . ?

_shelx_res_file                  
;
TITL crystal2_a.res in P2(1)/c
    crystal2.res
    created by SHELXL-2018/3 at 09:29:43 on 06-Sep-2025
REM Old TITL crystal2_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.072, Rweak 0.005, Alpha 0.019
REM <I/s> 0.455 for 59 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 N Cd Cl2
CELL 0.71073 3.8859 17.1403 11.2169 90 95.796 90
ZERR 4 0.0004 0.0015 0.0009 0 0.008 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cd Cl N
UNIT 16 24 4 8 8

L.S. 4 0 0
PLAN  2
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\crystal2.hkl">
REM </olex2.extras>

WGHT    0.022600
FVAR       0.33996
CD1   3    0.798458    0.566513    0.617712    11.00000    0.02345    0.02526 =
         0.03305   -0.00297    0.00510   -0.00071
CL1   4    0.762772    0.419615    0.554088    11.00000    0.02622    0.02758 =
         0.03285   -0.00175    0.00390    0.00025
CL2   4    0.349014    0.545451    0.769428    11.00000    0.02539    0.04094 =
         0.02824    0.00249    0.00466   -0.00106
N1    5    0.792221    0.697432    0.635120    11.00000    0.02853    0.02473 =
         0.03621   -0.00494    0.00540    0.00274
N2    5    0.878682    0.822012    0.602462    11.00000    0.03225    0.02793 =
         0.03793    0.00136    0.00400   -0.00058
C1    1    0.911571    0.748894    0.562406    11.00000    0.03159    0.03028 =
         0.03497   -0.00325    0.00760    0.00199
AFIX  43
H1    2    1.006708    0.736151    0.492115    11.00000   -1.20000
AFIX   0
C2    1    0.678694    0.740253    0.726898    11.00000    0.03948    0.03400 =
         0.02976   -0.00494    0.00544    0.00191
AFIX  43
H2    2    0.581426    0.719638    0.792473    11.00000   -1.20000
AFIX   0
C3    1    0.729902    0.816761    0.707337    11.00000    0.03721    0.02813 =
         0.03721   -0.01266    0.00560   -0.00084
AFIX  43
H3    2    0.674624    0.857972    0.755856    11.00000   -1.20000
AFIX   0
C4    1    0.986267    0.892707    0.543410    11.00000    0.04660    0.03227 =
         0.06646    0.01243    0.00708   -0.00095
AFIX 137
H4A   2    0.785847    0.922864    0.515673    11.00000   -1.50000
H4B   2    1.109156    0.878629    0.476519    11.00000   -1.50000
H4C   2    1.134439    0.923044    0.599267    11.00000   -1.50000
AFIX   0
HKLF 4




REM  crystal2_a.res in P2(1)/c
REM wR2 = 0.0732, GooF = S = 0.990, Restrained GooF = 0.990 for all data
REM R1 = 0.0323 for 1498 Fo > 4sig(Fo) and 0.0500 for all 1860 data
REM 83 parameters refined using 0 restraints

END

WGHT      0.0225      0.0000

REM Highest difference peak  1.134,  deepest hole -1.163,  1-sigma level  0.238
Q1    1   0.8024  0.4610  0.4995  11.00000  0.05    1.13
Q2    1   0.1349  0.5640  0.6911  11.00000  0.05    1.04
;
_shelx_res_checksum              40569
_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
;
