# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_2_293k
_database_code_depnum_ccdc_archive 'CCDC 2204247'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-30 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-12-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd Cl4, 2(C8 F N)'
_chemical_formula_sum            'C16 Cd Cl4 F2 N2'
_chemical_formula_weight         512.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd Cl C H N F'
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'
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'
F F 0.0171 0.0103 '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                   19.0475(14)
_cell_length_b                   7.4870(5)
_cell_length_c                   7.5538(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.033(6)
_cell_angle_gamma                90
_cell_volume                     1071.27(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4404
_cell_measurement_temperature    292.97(10)
_cell_measurement_theta_max      29.0080
_cell_measurement_theta_min      2.1340
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.867
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.769
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.769
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.033
_diffrn_reflns_theta_min         2.150
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.769
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     12.00  60.00   0.50    0.05    --    5.00  77.00 -93.00   96
  2  ω    -16.00  27.00   0.50    0.05    --   -5.46 -99.00 -30.00   86
  3  ω    -10.00  23.00   0.50    0.05    --   -5.46 -99.00   0.00   66
  4  ω      2.00  27.00   0.50    0.05    --   -5.46 -99.00 120.00   50
  5  ω    -68.00  28.00   0.50    0.05    --    5.00 -77.00 141.00  192
;
_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      -0.0195279000
_diffrn_orient_matrix_UB_12      0.0727540000
_diffrn_orient_matrix_UB_13      -0.0402579000
_diffrn_orient_matrix_UB_21      -0.0059487000
_diffrn_orient_matrix_UB_22      0.0325224000
_diffrn_orient_matrix_UB_23      0.0852510000
_diffrn_orient_matrix_UB_31      0.0314011000
_diffrn_orient_matrix_UB_32      0.0513585000
_diffrn_orient_matrix_UB_33      0.0029558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2094
_reflns_number_total             3432
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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         7.735
_refine_diff_density_min         -2.454
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0959
_refine_ls_restrained_S_all      1.126
_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)+(0.1793P)²+4.4961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2710
_refine_ls_wR_factor_ref         0.2856
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
C6 \\sim N1 \\sim C2 \\sim C3 \\sim C1 \\sim C4 \\sim C5 \\sim C7 \\sim C11
\\sim C10 \\sim C8 \\sim C9 \\sim C13 \\sim C12 \\sim F2 \\sim F1: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
2. Others
 Fixed Sof: C6(0.5) C10(0.5) C12(0.5) C8(0.5) F2(0.5) C3(0.5) C1(0.5) C7(0.5)
 F1(0.5) C9(0.5) C13(0.5) C11(0.5)
3.a Fitted hexagon refined as free rotating group:
 C4(C6,C10,C12,C8,C5)
;
_atom_sites_solution_hydrogens   .
_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 0.500000 0.000000 0.500000 0.0303(3) Uani 1 2 d S . P A 1
Cl2 Cl 0.48405(14) 0.2504(2) 0.2464(3) 0.0438(6) Uani 1 1 d . . . . .
Cl1 Cl 0.63233(12) 0.0505(4) 0.5346(4) 0.0491(6) Uani 1 1 d . . . . .
N1 N 0.6159(5) 0.4722(12) 0.5278(18) 0.061(3) Uani 1 1 d . U . . .
C4 C 0.8085(6) 0.6142(16) 0.5819(17) 0.081(3) Uani 1 1 d G U . . .
C6 C 0.8625(9) 0.5007(16) 0.543(3) 0.089(4) Uani 0.5 1 d G U P . .
C10 C 0.9264(7) 0.571(3) 0.502(3) 0.093(4) Uani 0.5 1 d G U P . .
C12 C 0.9363(6) 0.755(3) 0.500(3) 0.093(3) Uani 0.5 1 d G U P . .
C8 C 0.8823(8) 0.8685(19) 0.539(2) 0.088(3) Uani 0.5 1 d G U P . .
C5 C 0.8184(6) 0.7982(15) 0.5802(16) 0.080(3) Uani 1 1 d G U . . .
C2 C 0.6803(9) 0.550(3) 0.541(3) 0.092(3) Uani 1 1 d . U . . .
F2 F 0.8905(15) 1.040(3) 0.536(4) 0.104(5) Uani 0.5 1 d . U P . .
C3 C 0.7389(18) 0.530(4) 0.652(6) 0.086(4) Uani 0.5 1 d . U P . .
C1 C 0.7408(19) 0.519(4) 0.475(6) 0.086(4) Uani 0.5 1 d . U P . .
C7 C 0.858(2) 0.496(4) 0.624(6) 0.090(4) Uani 0.5 1 d . U P . .
F1 F 0.8868(16) 1.032(3) 0.649(4) 0.110(5) Uani 0.5 1 d . U P . .
C9 C 0.8820(18) 0.854(6) 0.648(4) 0.090(3) Uani 0.5 1 d . U P . .
C13 C 0.9301(19) 0.757(5) 0.724(5) 0.093(4) Uani 0.5 1 d . U P . .
C11 C 0.9230(18) 0.583(6) 0.694(5) 0.093(4) Uani 0.5 1 d . U P . .

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 0.0445(5) 0.0239(5) 0.0231(5) -0.0002(2) 0.0053(3) -0.0005(3)
Cl2 0.0661(13) 0.0359(11) 0.0306(10) 0.0129(8) 0.0103(9) -0.0001(8)
Cl1 0.0474(11) 0.0432(11) 0.0568(14) -0.0007(11) 0.0061(10) 0.0001(9)
N1 0.053(5) 0.046(4) 0.082(7) 0.001(4) -0.001(5) -0.018(4)
C4 0.065(5) 0.110(6) 0.070(5) -0.002(5) 0.012(4) -0.008(5)
C6 0.077(7) 0.118(8) 0.072(7) 0.000(7) 0.012(7) -0.001(6)
C10 0.081(7) 0.121(8) 0.077(7) 0.001(7) 0.010(7) -0.004(7)
C12 0.087(6) 0.118(7) 0.074(6) 0.003(7) 0.014(6) -0.010(6)
C8 0.089(6) 0.111(7) 0.067(6) 0.004(7) 0.014(6) -0.014(6)
C5 0.076(5) 0.105(6) 0.059(5) -0.001(5) 0.013(5) -0.013(5)
C2 0.067(6) 0.096(7) 0.111(8) -0.003(7) -0.002(6) -0.014(6)
F2 0.133(11) 0.102(9) 0.079(10) 0.006(10) 0.014(10) -0.028(9)
C3 0.068(7) 0.105(8) 0.086(8) 0.000(7) 0.008(7) -0.014(7)
C1 0.067(7) 0.105(8) 0.087(8) -0.006(7) 0.006(7) -0.014(7)
C7 0.077(7) 0.119(8) 0.075(7) -0.002(7) 0.015(7) 0.001(6)
F1 0.131(11) 0.116(10) 0.086(10) 0.004(10) 0.025(10) -0.033(9)
C9 0.090(6) 0.111(7) 0.069(6) 0.001(7) 0.016(6) -0.013(6)
C13 0.088(7) 0.119(7) 0.073(7) 0.001(7) 0.013(7) -0.011(7)
C11 0.083(6) 0.121(7) 0.078(7) 0.001(7) 0.014(6) -0.004(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
Cd1 Cl2 2.6746(17) 3_656 ?
Cd1 Cl2 2.6774(17) 2_645 ?
Cd1 Cl2 2.6774(17) 4_566 ?
Cd1 Cl2 2.6746(17) . ?
Cd1 Cl1 2.535(2) 3_656 ?
Cd1 Cl1 2.535(2) . ?
N1 C2 1.353(18) . ?
C4 C6 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.61(3) . ?
C4 C1 1.61(4) . ?
C4 C7 1.30(4) . ?
C6 C10 1.3900 . ?
C10 C12 1.3900 . ?
C12 C8 1.3900 . ?
C8 C5 1.3900 . ?
C8 F2 1.30(3) . ?
C5 C9 1.33(4) . ?
C2 C3 1.33(4) . ?
C2 C1 1.32(4) . ?
C7 C11 1.45(5) . ?
F1 C9 1.34(4) . ?
C9 C13 1.26(5) . ?
C13 C11 1.32(5) . ?

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
Cl2 Cd1 Cl2 180.0 3_656 . ?
Cl2 Cd1 Cl2 90.228(14) . 2_645 ?
Cl2 Cd1 Cl2 89.772(14) 3_656 2_645 ?
Cl2 Cd1 Cl2 90.228(14) 3_656 4_566 ?
Cl2 Cd1 Cl2 180.00(6) 2_645 4_566 ?
Cl2 Cd1 Cl2 89.772(14) . 4_566 ?
Cl1 Cd1 Cl2 89.65(8) 3_656 . ?
Cl1 Cd1 Cl2 89.65(8) . 3_656 ?
Cl1 Cd1 Cl2 89.51(8) 3_656 4_566 ?
Cl1 Cd1 Cl2 90.35(8) . . ?
Cl1 Cd1 Cl2 90.35(8) 3_656 3_656 ?
Cl1 Cd1 Cl2 90.49(8) 3_656 2_645 ?
Cl1 Cd1 Cl2 89.51(8) . 2_645 ?
Cl1 Cd1 Cl2 90.49(8) . 4_566 ?
Cl1 Cd1 Cl1 180.0 3_656 . ?
Cd1 Cl2 Cd1 167.03(11) . 2_655 ?
C6 C4 C5 120.0 . . ?
C6 C4 C3 119.1(15) . . ?
C6 C4 C1 101.2(15) . . ?
C5 C4 C3 120.5(15) . . ?
C5 C4 C1 122.3(15) . . ?
C1 C4 C3 49(2) . . ?
C7 C4 C6 27(2) . . ?
C7 C4 C5 125(2) . . ?
C7 C4 C3 105(2) . . ?
C7 C4 C1 110(2) . . ?
C4 C6 C10 120.0 . . ?
C12 C10 C6 120.0 . . ?
C8 C12 C10 120.0 . . ?
C12 C8 C5 120.0 . . ?
F2 C8 C12 120.7(17) . . ?
F2 C8 C5 119.3(17) . . ?
C8 C5 C4 120.0 . . ?
C9 C5 C4 115(2) . . ?
C9 C5 C8 35.5(15) . . ?
C3 C2 N1 134(2) . . ?
C1 C2 N1 135(2) . . ?
C1 C2 C3 61(3) . . ?
C2 C3 C4 114(3) . . ?
C2 C1 C4 115(3) . . ?
C4 C7 C11 111(3) . . ?
F1 C9 C5 112(3) . . ?
C13 C9 C5 126(4) . . ?
C13 C9 F1 122(3) . . ?
C9 C13 C11 116(4) . . ?
C13 C11 C7 125(4) . . ?

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 C2 C3 C4 164(2) . . . . ?
N1 C2 C1 C4 -161(2) . . . . ?
C4 C6 C10 C12 0.0 . . . . ?
C4 C5 C9 F1 -178(2) . . . . ?
C4 C5 C9 C13 -6(4) . . . . ?
C4 C7 C11 C13 5(6) . . . . ?
C6 C4 C5 C8 0.0 . . . . ?
C6 C4 C5 C9 -39.8(16) . . . . ?
C6 C4 C3 C2 -114(2) . . . . ?
C6 C4 C1 C2 154(2) . . . . ?
C6 C4 C7 C11 96(5) . . . . ?
C6 C10 C12 C8 0.0 . . . . ?
C10 C12 C8 C5 0.0 . . . . ?
C10 C12 C8 F2 -179(2) . . . . ?
C12 C8 C5 C4 0.0 . . . . ?
C12 C8 C5 C9 92(3) . . . . ?
C8 C5 C9 F1 75(3) . . . . ?
C8 C5 C9 C13 -113(5) . . . . ?
C5 C4 C6 C10 0.0 . . . . ?
C5 C4 C3 C2 74(3) . . . . ?
C5 C4 C1 C2 -70(3) . . . . ?
C5 C4 C7 C11 8(4) . . . . ?
C5 C9 C13 C11 17(5) . . . . ?
F2 C8 C5 C4 179(2) . . . . ?
F2 C8 C5 C9 -89(4) . . . . ?
C3 C4 C6 C10 -172(2) . . . . ?
C3 C4 C5 C8 172(2) . . . . ?
C3 C4 C5 C9 132(2) . . . . ?
C3 C4 C1 C2 35(3) . . . . ?
C3 C4 C7 C11 -138(3) . . . . ?
C3 C2 C1 C4 -37(3) . . . . ?
C1 C4 C6 C10 138.0(18) . . . . ?
C1 C4 C5 C8 -129(2) . . . . ?
C1 C4 C5 C9 -169(2) . . . . ?
C1 C4 C3 C2 -35(2) . . . . ?
C1 C4 C7 C11 171(3) . . . . ?
C1 C2 C3 C4 37(2) . . . . ?
C7 C4 C6 C10 -110(4) . . . . ?
C7 C4 C5 C8 31(3) . . . . ?
C7 C4 C5 C9 -9(3) . . . . ?
C7 C4 C3 C2 -138(3) . . . . ?
C7 C4 C1 C2 128(3) . . . . ?
F1 C9 C13 C11 -171(3) . . . . ?
C9 C13 C11 C7 -17(6) . . . . ?

_shelx_res_file                  
;
TITL zy3f_rt_auto_a.res in P2(1)/c
    2_293k.res
    created by SHELXL-2018/3 at 13:11:12 on 27-Dec-2022
REM Old TITL zy3f_rt_auto_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.165, Rweak 0.003, Alpha 0.029
REM <I/s> 1.120 for 169 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 Cd Cl4 F O2
CELL 0.71073 19.0475 7.487 7.5538 90 96.033 90
ZERR 4 0.0014 0.0005 0.0005 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C Cd Cl F N
UNIT 32 1.87 8 4 4
SIMU 0.01 0.02 2 C6 N1 C2 C3 C1 C4 C5 C7 C11 C10 C8 C9 C13 C12 F2 F1

L.S. 20
PLAN  14
SIZE 0.1 0.1 0.1
TEMP 20
CONF
FREE C9 C12
FREE C9 C8
FREE C12 C11
FREE C3 C1
FREE C11 C10
FREE F2 C9
FREE F1 C8
FREE F1 F2
FREE C6 C11
FREE C8 C13
FREE C13 C12
FREE C7 C10
FREE C7 C6
list 4
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\ZY3F_RT_auto.hkl">
REM </olex2.extras>

WGHT    0.179300    4.496100
FVAR       0.47847
PART 1
CD1   2    0.500000    0.000000    0.500000    10.50000    0.04445    0.02387 =
         0.02307   -0.00016    0.00528   -0.00055
PART 0
CL2   3    0.484053    0.250371    0.246403    11.00000    0.06608    0.03590 =
         0.03062    0.01289    0.01032   -0.00009
CL1   3    0.632334    0.050501    0.534560    11.00000    0.04745    0.04325 =
         0.05681   -0.00074    0.00613    0.00014

N1    5    0.615927    0.472175    0.527811    11.00000    0.05329    0.04558 =
         0.08155    0.00101   -0.00086   -0.01770
AFIX  66
C4    1    0.808508    0.614239    0.581913    11.00000    0.06523    0.11023 =
         0.06990   -0.00163    0.01217   -0.00801
C6    1    0.862513    0.500659    0.542864    10.50000    0.07702    0.11784 =
         0.07249    0.00018    0.01159   -0.00084
C10   1    0.926414    0.570986    0.502132    10.50000    0.08093    0.12091 =
         0.07719    0.00093    0.00986   -0.00356
C12   1    0.936310    0.754893    0.500448    10.50000    0.08663    0.11825 =
         0.07400    0.00259    0.01423   -0.01030
C8    1    0.882305    0.868475    0.539497    10.50000    0.08922    0.11067 =
         0.06685    0.00355    0.01416   -0.01379
C5    1    0.818404    0.798150    0.580230    11.00000    0.07615    0.10522 =
         0.05918   -0.00078    0.01296   -0.01338
AFIX   0
C2    1    0.680297    0.550394    0.541225    11.00000    0.06658    0.09578 =
         0.11115   -0.00347   -0.00181   -0.01375
F2    4    0.890467    1.040361    0.536320    10.50000    0.13276    0.10242 =
         0.07853    0.00601    0.01363   -0.02809
C3    1    0.738854    0.530353    0.652486    10.50000    0.06763    0.10483 =
         0.08646   -0.00021    0.00804   -0.01370
C1    1    0.740820    0.519191    0.475031    10.50000    0.06677    0.10457 =
         0.08713   -0.00644    0.00564   -0.01414
C7    1    0.857944    0.496347    0.623511    10.50000    0.07711    0.11852 =
         0.07499   -0.00169    0.01489    0.00079
F1    4    0.886757    1.032127    0.648818    10.50000    0.13103    0.11601 =
         0.08625    0.00391    0.02470   -0.03272
C9    1    0.882018    0.853703    0.648415    10.50000    0.09046    0.11140 =
         0.06912    0.00141    0.01646   -0.01299
C13   1    0.930102    0.757005    0.723750    10.50000    0.08790    0.11873 =
         0.07317    0.00087    0.01335   -0.01075
C11   1    0.922976    0.583455    0.693507    10.50000    0.08294    0.12129 =
         0.07752    0.00123    0.01430   -0.00438
HKLF 4




REM  zy3f_rt_auto_a.res in P2(1)/c
REM wR2 = 0.2856, GooF = S = 1.149, Restrained GooF = 1.126 for all data
REM R1 = 0.0959 for 2094 Fo > 4sig(Fo) and 0.1095 for all 2639 data
REM 157 parameters refined using 186 restraints

END

WGHT      0.1751      5.4565

REM Highest difference peak  7.735,  deepest hole -2.454,  1-sigma level  0.294
Q1    1   0.5000  0.5000  0.5000  10.50000  0.05    7.73
Q2    1   0.5046  0.2529  0.2482  11.00000  0.05    2.62
Q3    1   0.5434  0.0004  0.4580  11.00000  0.05    1.62
Q4    1   0.6785  0.5361  0.6265  11.00000  0.05    1.13
Q5    1   0.8715  0.5014  0.6829  11.00000  0.05    1.03
Q6    1   0.5946  0.4234  0.5170  11.00000  0.05    0.82
Q7    1   0.9185  0.9884  0.7163  11.00000  0.05    0.82
Q8    1   0.5443  0.0113  0.5806  11.00000  0.05    0.80
Q9    1   0.5637  0.4660  0.5172  11.00000  0.05    0.75
Q10   1   0.6293 -0.0182  0.4564  11.00000  0.05    0.72
Q11   1   0.9009  0.5369  0.5797  11.00000  0.05    0.70
Q12   1   0.9123  0.4917  0.7369  11.00000  0.05    0.68
Q13   1   0.6816  0.5469  0.4599  11.00000  0.05    0.68
Q14   1   0.8702  0.3677  0.6024  11.00000  0.05    0.63
;
_shelx_res_checksum              16209
# end Validation Reply Form
_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 2.680
_oxdiff_exptl_absorpt_empirical_full_min 0.420
# start Validation Reply Form
_vrf_PLAT097_2_293k              
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       7.74 eA-3  
RESPONSE: In order to deal with disorder, more limit instructions have been added.
;
####################################################################### 
# 
# 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_2_403k
_database_code_depnum_ccdc_archive 'CCDC 2204248'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 F N), 4(Cd0.25 Cl)'
_chemical_formula_sum            'C16 Cd Cl4 F2 N2'
_chemical_formula_weight         512.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd Cl C H N F'
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'
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'
F F 0.0171 0.0103 '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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.3186(4)
_cell_length_b                   5.3186(4)
_cell_length_c                   40.261(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1138.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    403.02(10)
_cell_measurement_theta_max      28.0470
_cell_measurement_theta_min      3.0110
_shelx_estimated_absorpt_T_max   0.869
_shelx_estimated_absorpt_T_min   0.869
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            2465
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.718
_diffrn_reflns_theta_min         2.023
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      403.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00   5.22   0.38    0.06    --   -5.54  84.00  -6.00   69
  2  ω      1.76  39.00   0.38    0.06    --    5.07 -99.00 150.00   98
  3  ω    -14.00  27.04   0.38    0.06    --    5.07 -99.00  30.00  108
  4  ω     -6.00  20.22   0.38    0.06    --   -5.54 -99.00-180.00   69
;
_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      -0.1029036000
_diffrn_orient_matrix_UB_12      -0.0498230000
_diffrn_orient_matrix_UB_13      -0.0090601000
_diffrn_orient_matrix_UB_21      -0.0721352000
_diffrn_orient_matrix_UB_22      0.1079986000
_diffrn_orient_matrix_UB_23      0.0039485000
_diffrn_orient_matrix_UB_31      0.0443223000
_diffrn_orient_matrix_UB_32      0.0602427000
_diffrn_orient_matrix_UB_33      -0.0145916000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                460
_reflns_number_total             614
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         614
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.359
_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)+(0.0964P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1353
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C6-C7 = C7-C8 = C8-N1
 1.48 with sigma of 0.001
 N1-C7 = C8-C6
 2.3 with sigma of 0.001
 C7-C1 = C7-C5
 2.3 with sigma of 0.02
 N1-C6
 3.8 with sigma of 0.02
 C2-F1
 1.3 with sigma of 0.02
2. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, F1
 with sigma of 0.1
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
C4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C8(0.125) C7(0.125) C1(0.125) C2(0.125) C3(0.125) C4(0.125)
 C5(0.125) C6(0.125) F1(0.125)
6.a Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
;
_atom_sites_solution_hydrogens   .
_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 1.000000 1.000000 0.500000 0.0589(4) Uani 1 16 d S T P . .
Cl1 Cl 0.500000 1.000000 0.500000 0.1026(10) Uani 1 8 d S TU P . .
Cl2 Cl 1.000000 1.000000 0.43765(9) 0.1318(17) Uani 1 8 d S T P . .
N1 N 0.500000 0.500000 0.4449(2) 0.111(4) Uani 1 8 d DS TU P . .
C8 C 0.585(6) 0.541(6) 0.4103(2) 0.101(9) Uani 0.125 1 d D U P A -1
C7 C 0.450(8) 0.339(5) 0.3923(3) 0.228(6) Uani 0.125 1 d D U P A -1
C1 C 0.345(6) 0.488(9) 0.3361(5) 0.228(6) Uani 0.125 1 d DG U P A -1
C2 C 0.383(8) 0.478(10) 0.3019(4) 0.228(6) Uani 0.125 1 d DG U P A -1
C3 C 0.600(10) 0.369(14) 0.2892(3) 0.228(6) Uani 0.125 1 d G U P A -1
C4 C 0.779(12) 0.269(17) 0.3106(7) 0.228(6) Uani 0.125 1 d G U P A -1
C5 C 0.741(10) 0.278(13) 0.3448(6) 0.228(6) Uani 0.125 1 d DG U P A -1
C6 C 0.524(7) 0.388(6) 0.3575(2) 0.228(6) Uani 0.125 1 d DG U P A -1
F1 F 0.175(7) 0.587(15) 0.2917(12) 0.33(4) Uani 0.125 1 d D 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 0.0427(4) 0.0427(4) 0.0914(7) 0.000 0.000 0.000
Cl1 0.0388(12) 0.0751(18) 0.194(3) 0.000 0.000 0.000
Cl2 0.156(3) 0.156(3) 0.0824(17) 0.000 0.000 0.000
N1 0.113(6) 0.113(6) 0.107(7) 0.000 0.000 0.000
C8 0.106(14) 0.096(14) 0.103(9) 0.000(10) 0.003(8) 0.006(10)
C7 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C1 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C2 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C3 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C4 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C5 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
C6 0.228(7) 0.228(7) 0.226(7) -0.003(4) 0.001(4) -0.001(4)
F1 0.33(4) 0.34(5) 0.33(4) 0.00(2) -0.024(19) 0.00(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 2.6593(2) . ?
Cd1 Cl1 2.6593(2) 3_765 ?
Cd1 Cl1 2.6593(2) 3_755 ?
Cd1 Cl1 2.6593(2) 1_655 ?
Cd1 Cl2 2.510(4) . ?
Cd1 Cl2 2.510(4) 17_776 ?
N1 C8 1.4801(11) . ?
C8 C7 1.4797(12) . ?
C7 C6 1.4795(11) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 F1 1.31(2) . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?

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 180.0 . 1_655 ?
Cl1 Cd1 Cl1 90.0 1_655 3_755 ?
Cl1 Cd1 Cl1 90.0 . 3_755 ?
Cl1 Cd1 Cl1 90.0 . 3_765 ?
Cl1 Cd1 Cl1 180.0 3_755 3_765 ?
Cl1 Cd1 Cl1 90.0 1_655 3_765 ?
Cl2 Cd1 Cl1 90.0 17_776 1_655 ?
Cl2 Cd1 Cl1 90.0 . . ?
Cl2 Cd1 Cl1 90.0 . 3_765 ?
Cl2 Cd1 Cl1 90.0 . 1_655 ?
Cl2 Cd1 Cl1 90.0 17_776 . ?
Cl2 Cd1 Cl1 90.0 17_776 3_755 ?
Cl2 Cd1 Cl1 90.0 . 3_755 ?
Cl2 Cd1 Cl1 90.0 17_776 3_765 ?
Cl2 Cd1 Cl2 180.0 17_776 . ?
Cd1 Cl1 Cd1 180.0 1_455 . ?
C7 C8 N1 102.02(10) . . ?
C6 C7 C8 102.05(11) . . ?
C2 C1 C6 120.0 . . ?
C3 C2 C1 120.0 . . ?
F1 C2 C1 100(3) . . ?
F1 C2 C3 140(3) . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 120.0 . . ?
C1 C6 C7 118.3(11) . . ?
C5 C6 C7 119.7(12) . . ?
C5 C6 C1 120.0 . . ?

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
N1 C8 C7 C6 177(2) . . . . ?
C8 C7 C6 C1 -108(3) . . . . ?
C8 C7 C6 C5 89(3) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C1 C6 C7 -163.8(16) . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 163.6(15) . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C1 C2 F1 179(3) . . . . ?
F1 C2 C3 C4 -179(4) . . . . ?

_shelx_res_file                  
;
TITL 2_403.res in I4/mmm
    2_403k.res
    created by SHELXL-2018/3 at 09:32:20 on 15-Dec-2022
REM Old TITL ZY3F_403K_auto in I-42m #121
REM SHELXT solution in I4/mmm
REM R1 0.233, Rweak 0.166, Alpha 0.054, Orientation as input
REM Formula found by SHELXT: Cd Cl4 C4
CELL 0.71073 5.3186 5.3186 40.2606 90 90 90
ZERR 8 0.0004 0.0004 0.008 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC C Cd Cl F N
UNIT 32 2 8 4 4
DFIX 1.48 0.001 C6 C7 C7 C8 C8 N1
DFIX 2.3 0.001 N1 C7 C8 C6
DFIX 2.3 C7 C1 C7 C5
DFIX 3.8 N1 C6
DFIX 1.3 C2 F1
FLAT C1 C2 C3 C4 C5 C6 C7 F1
SIMU 0.001 0.002 2 C1 C2 C3 C4 C5 C6 C7
DELU C1 C2 C3 C4 C5 C6 C7
SIMU 0.001 0.002 2 C4
ISOR 0.01 0.02 C7 N1 C8 C6 C1 C5 C2 C4 C3 F1
ISOR 0.01 0.02 Cl1

L.S. 30
PLAN  9
SIZE 0.1 0.1 0.1
TEMP 129.87(10)
CONF
list 4
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.096400
FVAR       0.59844
CD1   2    1.000000    1.000000    0.500000    10.06250    0.04268    0.04268 =
         0.09139    0.00000    0.00000    0.00000
CL1   3    0.500000    1.000000    0.500000    10.12500    0.03880    0.07506 =
         0.19401    0.00000    0.00000    0.00000
CL2   3    1.000000    1.000000    0.437650    10.12500    0.15648    0.15648 =
         0.08240    0.00000    0.00000    0.00000
N1    5    0.500000    0.500000    0.444937    10.12500    0.11334    0.11334 =
         0.10744    0.00000    0.00000    0.00000
PART -1
C8    1    0.584712    0.540568    0.410331    10.12500    0.10605    0.09571 =
         0.10272    0.00011    0.00349    0.00619
C7    1    0.450017    0.338898    0.392321    10.12500    0.22814    0.22849 =
         0.22623   -0.00269    0.00081   -0.00064
AFIX  66
C1    1    0.344750    0.487779    0.336069    10.12500    0.22817    0.22848 =
         0.22630   -0.00260    0.00086   -0.00062
C2    1    0.382650    0.478266    0.301933    10.12500    0.22818    0.22849 =
         0.22636   -0.00259    0.00084   -0.00062
C3    1    0.599539    0.368797    0.289209    10.12500    0.22817    0.22849 =
         0.22638   -0.00260    0.00086   -0.00063
C4    1    0.778529    0.268840    0.310621    10.12500    0.22817    0.22849 =
         0.22636   -0.00260    0.00085   -0.00063
C5    1    0.740633    0.278351    0.344758    10.12500    0.22816    0.22848 =
         0.22631   -0.00261    0.00084   -0.00065
C6    1    0.523745    0.387820    0.357483    10.12500    0.22815    0.22848 =
         0.22628   -0.00265    0.00084   -0.00063
AFIX   0
F1    4    0.175430    0.587000    0.291698    10.12500    0.33037    0.33636 =
         0.33301    0.00014   -0.02383    0.00101
HKLF 4




REM  zy3f_403k_auto_a.res in I4/mmm
REM wR2 = 0.1353, GooF = S = 1.138, Restrained GooF = 1.359 for all data
REM R1 = 0.0483 for 460 Fo > 4sig(Fo) and 0.0525 for all 519 data
REM 81 parameters refined using 137 restraints

END

WGHT      0.0964      0.0000

REM Highest difference peak  0.597,  deepest hole -0.530,  1-sigma level  0.134
Q1    1   1.0000  0.0000  0.3144  10.12500  0.05    0.60
Q2    1   0.5000  0.8151  0.5000  10.25000  0.05    0.47
Q3    1   0.7090  0.7090  0.5000  10.25000  0.05    0.46
Q4    1   0.5000  0.3849  0.3871  10.50000  0.05    0.46
Q5    1   0.5000  0.5000  0.3473  10.12500  0.05    0.45
Q6    1   0.3295  0.8889  0.5000  10.50000  0.05    0.42
Q7    1   0.5000  0.5000  0.3323  10.12500  0.05    0.41
Q8    1   0.5000  0.5000  0.5000  10.06250  0.05    0.40
Q9    1   1.0000  0.8054  0.5000  10.25000  0.05    0.38
;
_shelx_res_checksum              48822
_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 3.956
_oxdiff_exptl_absorpt_empirical_full_min 0.453
# start Validation Reply Form
_vrf_PLAT088_2_403k              
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.41 Note  
RESPONSE: In order to deal with disorder, more limit instructions have been added.
;
_vrf_PLAT242_2_403k              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cd1 Check 
RESPONSE: Cd is heavy element, this alert is common for compound of such molecule type.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1_403k
_database_code_depnum_ccdc_archive 'CCDC 2204250'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-30 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-12-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd Cl4, 2(C8 N)'
_chemical_formula_sum            'C16 Cd Cl4 N2'
_chemical_formula_weight         474.39
_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'
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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.30910(10)
_cell_length_b                   5.30910(10)
_cell_length_c                   39.5281(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1114.16(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6901
_cell_measurement_temperature    403.00(10)
_cell_measurement_theta_max      31.0010
_cell_measurement_theta_min      2.0450
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.868
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             452
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            9586
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.807
_diffrn_reflns_theta_min         2.061
_diffrn_ambient_temperature      403.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  77.00   0.50    0.39    --    4.92  53.00 156.00  124
  2  ω    -18.00  38.00   0.50    0.39    --    4.92 -99.00  90.00  112
  3  ω    -67.00  19.00   0.50    0.39    --    4.92 -53.00  11.00  172
  4  ω    -14.00  12.00   0.50    0.39    --    4.92 -99.00-120.00   52
  5  ω    -53.00 -23.00   0.50    0.39    --   -5.39 -19.00   0.00   60
  6  ω    -77.00   6.00   0.50    0.39    --   -5.39 -37.00 -90.00  166
  7  ω     -8.00  17.00   0.50    0.39    --   -5.39 -99.00-120.00   50
  8  ω    -12.00  26.00   0.50    0.39    --   -5.39 -99.00-150.00   76
  9  ω    -74.00   2.00   0.50    0.39    --   -5.39 -37.00-180.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_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                531
_reflns_number_total             603
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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         0.346
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         603
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0313
_refine_ls_restrained_S_all      1.091
_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)+(0.0638P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0842
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C4-C2 = C5-C3
 1.4 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C6 \\sim C1 \\sim C4 \\sim C2 \\sim C3: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cd1(0.0625) N1(0.125) C1(0.125) C6(0.125) C3(0.125) C5(0.25)
 C2(0.25) C4(0.125)
;
_atom_sites_solution_hydrogens   .
_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 1.000000 1.000000 0.49610(12) 0.0472(7) Uani 0.5 8 d S T P . .
Cl1 Cl 0.500000 1.000000 0.500000 0.0973(6) Uani 1 8 d S T P . .
Cl2 Cl 1.000000 1.000000 0.43646(5) 0.1229(9) Uani 1 8 d S T P . .
N1 N 0.471(4) 0.529(4) 0.44397(19) 0.086(5) Uani 0.25 2 d S TU P A 3
C1 C 0.340(4) 0.447(6) 0.3854(5) 0.114(7) Uani 0.125 1 d . U P B -1
C6 C 0.554(2) 0.446(2) 0.4090(3) 0.091(4) Uani 0.25 2 d S TU P A 3
C3 C 0.596(16) 0.54(3) 0.2846(7) 0.179(10) Uani 0.125 1 d . U P C -1
C5 C 0.602(8) 0.759(4) 0.2972(6) 0.187(9) Uani 0.25 1 d . U P D 3
C2 C 0.597(6) 0.722(4) 0.3326(6) 0.176(8) Uani 0.25 1 d D U P B -1
C4 C 0.434(6) 0.555(6) 0.3492(5) 0.131(7) Uani 0.125 1 d D U P B -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 0.0378(2) 0.0378(2) 0.066(2) 0.000 0.000 0.000
Cl1 0.0338(6) 0.0719(10) 0.1863(17) 0.000 0.000 0.000
Cl2 0.1427(15) 0.1427(15) 0.0833(10) 0.000 0.000 0.000
N1 0.087(7) 0.087(7) 0.084(3) -0.002(3) 0.002(3) 0.008(7)
C1 0.125(11) 0.111(13) 0.105(7) -0.011(8) -0.022(8) 0.005(11)
C6 0.091(6) 0.091(6) 0.090(4) -0.008(3) 0.008(3) 0.010(5)
C3 0.183(15) 0.188(15) 0.166(11) 0.025(11) 0.002(10) -0.003(11)
C5 0.186(12) 0.190(12) 0.184(10) 0.032(7) 0.006(8) -0.003(8)
C2 0.176(14) 0.174(13) 0.178(10) 0.023(9) 0.012(10) 0.014(9)
C4 0.139(11) 0.135(11) 0.117(7) 0.007(8) -0.008(8) 0.009(8)

_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 Cd1 0.309(10) 17_776 ?
Cd1 Cl1 2.6590(3) 3_755 ?
Cd1 Cl1 2.6590(3) 3_765 ?
Cd1 Cl1 2.6590(3) 1_655 ?
Cd1 Cl1 2.6590(3) . ?
Cd1 Cl2 2.357(5) . ?
Cd1 Cl2 2.666(5) 17_776 ?
N1 N1 0.31(4) 4_565 ?
N1 N1 0.31(4) 3_655 ?
N1 N1 0.44(6) 2_665 ?
N1 C6 1.52(2) . ?
N1 C6 1.395(16) 2_665 ?
N1 C6 1.456(16) 3_655 ?
N1 C6 1.456(16) 4_565 ?
C1 C4 1.62(3) . ?
C6 C6 0.57(2) 3_655 ?
C6 C6 0.57(2) 4_565 ?
C6 C6 0.81(3) 2_665 ?
C5 C5 1.09(8) 22_655 ?
C5 C5 1.17(6) 24 ?
C2 C4 1.40(2) . ?

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
Cd1 Cd1 Cl1 86.67(10) 17_776 3_765 ?
Cd1 Cd1 Cl1 86.67(11) 17_776 3_755 ?
Cd1 Cd1 Cl1 86.67(11) 17_776 . ?
Cd1 Cd1 Cl1 86.67(10) 17_776 1_655 ?
Cd1 Cd1 Cl2 180.0 17_776 . ?
Cd1 Cd1 Cl2 0.000(3) 17_776 17_776 ?
Cl1 Cd1 Cl1 89.807(13) 3_765 1_655 ?
Cl1 Cd1 Cl1 89.807(13) 1_655 3_755 ?
Cl1 Cd1 Cl1 173.3(2) 3_765 3_755 ?
Cl1 Cd1 Cl1 89.807(13) 3_765 . ?
Cl1 Cd1 Cl1 89.807(13) . 3_755 ?
Cl1 Cd1 Cl1 173.3(2) 1_655 . ?
Cl1 Cd1 Cl2 86.67(11) 3_765 17_776 ?
Cl1 Cd1 Cl2 86.67(11) 1_655 17_776 ?
Cl1 Cd1 Cl2 86.67(11) 3_755 17_776 ?
Cl1 Cd1 Cl2 86.67(11) . 17_776 ?
Cl2 Cd1 Cl1 93.33(11) . 3_765 ?
Cl2 Cd1 Cl1 93.33(11) . 1_655 ?
Cl2 Cd1 Cl1 93.33(11) . 3_755 ?
Cl2 Cd1 Cl1 93.33(11) . . ?
Cl2 Cd1 Cl2 180.0 . 17_776 ?
Cd1 Cl1 Cd1 180.0 17_776 1_455 ?
Cd1 Cl1 Cd1 6.7(2) 1_455 17_676 ?
Cd1 Cl1 Cd1 6.7(2) 17_776 . ?
Cd1 Cl1 Cd1 173.3(2) 17_776 17_676 ?
Cd1 Cl1 Cd1 173.3(2) 1_455 . ?
Cd1 Cl1 Cd1 180.0 17_676 . ?
Cd1 Cl2 Cd1 0.0 . 17_776 ?
N1 N1 N1 45.00(10) 3_655 2_665 ?
N1 N1 N1 90.00(10) 4_565 3_655 ?
N1 N1 N1 45.00(9) 4_565 2_665 ?
N1 N1 C6 65.8(12) 2_665 . ?
N1 N1 C6 73.1(8) 3_655 . ?
N1 N1 C6 72.4(10) 4_565 3_655 ?
N1 N1 C6 73.1(8) 4_565 . ?
N1 N1 C6 97.7(12) 2_665 2_665 ?
N1 N1 C6 81.4(11) 2_665 3_655 ?
N1 N1 C6 95.5(9) 4_565 2_665 ?
N1 N1 C6 95.5(9) 3_655 2_665 ?
N1 N1 C6 95.2(8) 3_655 3_655 ?
C6 N1 C6 23.0(9) 2_665 3_655 ?
C6 N1 C6 22.1(8) 4_565 . ?
C6 N1 C6 32.3(13) 4_565 3_655 ?
C6 N1 C6 31.9(12) 2_665 . ?
C6 N1 C6 22.1(8) 3_655 . ?
N1 C6 N1 11.7(15) 4_565 . ?
N1 C6 N1 17(2) 2_665 . ?
N1 C6 N1 11.7(15) 3_655 . ?
N1 C6 N1 17(2) 4_565 3_655 ?
N1 C6 N1 12.1(16) 2_665 3_655 ?
C6 C6 N1 84.6(9) 4_565 2_665 ?
C6 C6 N1 73.1(8) 3_655 . ?
C6 C6 N1 84.8(8) 3_655 3_655 ?
C6 C6 N1 73.9(6) 2_665 3_655 ?
C6 C6 N1 73.1(8) 4_565 . ?
C6 C6 N1 82.3(12) 2_665 2_665 ?
C6 C6 N1 72.4(10) 4_565 3_655 ?
C6 C6 N1 84.6(9) 3_655 2_665 ?
C6 C6 N1 65.8(12) 2_665 . ?
C6 C6 C6 45.00(2) 4_565 2_665 ?
C6 C6 C6 45.00(3) 3_655 2_665 ?
C5 C5 C5 135.00(5) 22_655 24 ?
C2 C4 C1 146(2) . . ?

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 N1 C6 N1 47.6(2) 4_565 . . 2_665 ?
N1 N1 C6 N1 -95.3(6) 3_655 . . 4_565 ?
N1 N1 C6 N1 -47.6(2) 3_655 . . 2_665 ?
N1 N1 C6 N1 47.6(3) 2_665 . . 3_655 ?
N1 N1 C6 N1 95.3(6) 4_565 . . 3_655 ?
N1 N1 C6 N1 -47.6(3) 2_665 . . 4_565 ?
N1 N1 C6 C6 -132.4(3) 2_665 . . 3_655 ?
N1 N1 C6 C6 -84.7(6) 4_565 . . 3_655 ?
N1 N1 C6 C6 132.4(3) 2_665 . . 4_565 ?
N1 N1 C6 C6 180.000(7) 2_665 . . 2_665 ?
N1 N1 C6 C6 -132.4(3) 4_565 . . 2_665 ?
N1 N1 C6 C6 180.00(3) 3_655 . . 3_655 ?
N1 N1 C6 C6 132.4(3) 3_655 . . 2_665 ?
N1 N1 C6 C6 84.7(6) 3_655 . . 4_565 ?
N1 N1 C6 C6 180.00(2) 4_565 . . 4_565 ?
C6 N1 C6 N1 132.4(3) 3_655 . . 2_665 ?
C6 N1 C6 N1 84.7(6) 3_655 . . 4_565 ?
C6 N1 C6 N1 132.4(3) 2_665 . . 4_565 ?
C6 N1 C6 N1 180.00(9) 4_565 . . 4_565 ?
C6 N1 C6 N1 180.00(11) 3_655 . . 3_655 ?
C6 N1 C6 N1 -84.7(6) 4_565 . . 3_655 ?
C6 N1 C6 N1 180.000(5) 2_665 . . 2_665 ?
C6 N1 C6 N1 -132.4(4) 2_665 . . 3_655 ?
C6 N1 C6 N1 -132.4(3) 4_565 . . 2_665 ?
C6 N1 C6 C6 -47.6(3) 2_665 . . 4_565 ?
C6 N1 C6 C6 -95.3(6) 3_655 . . 4_565 ?
C6 N1 C6 C6 47.6(3) 2_665 . . 3_655 ?
C6 N1 C6 C6 -47.6(3) 3_655 . . 2_665 ?
C6 N1 C6 C6 95.3(6) 4_565 . . 3_655 ?
C6 N1 C6 C6 47.6(3) 4_565 . . 2_665 ?

_shelx_res_file                  
;
TITL zybya_403k1_auto_d.res in I4/mmm
    1_403k.res
    created by SHELXL-2018/3 at 12:12:20 on 29-Dec-2022
REM Old TITL zybya_403k1_auto_a.res in I4/mmm
REM SHELXT solution in I4/mmm: R1 0.410, Rweak 0.695, Alpha 0.052
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: Cd Cl4 C4
CELL 0.71073 5.3091 5.3091 39.5281 90 90 90
ZERR 64 0.0001 0.0001 0.0018 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC C Cd Cl N
UNIT 32 2 8 4
ISOR 0.01 0.02 C1 N1 C6 C4 C2 C5 C3
SIMU 0.01 0.02 2 C5 N1 C6 C1 C4 C2 C3
DFIX 1.4 C4 C2 C5 C3

L.S. 20
PLAN  2
SIZE 0.1 0.1 0.1
TEMP 130
CONF
BIND C6 C1
BIND C5 C3
BIND C2 C5
LIST 6
MORE -1
fmap 2
acta
OMIT 0 0 8
REM <olex2.extras>
REM <HklSrc "%.\\1_403K.hkl">
REM </olex2.extras>

WGHT    0.063800
FVAR       0.54061
CD1   2    1.000000    1.000000    0.496097    10.06250    0.03784    0.03784 =
         0.06590    0.00000    0.00000    0.00000
CL1   3    0.500000    1.000000    0.500000    10.12500    0.03380    0.07190 =
         0.18629    0.00000    0.00000    0.00000
CL2   3    1.000000    1.000000    0.436461    10.12500    0.14274    0.14274 =
         0.08335    0.00000    0.00000    0.00000
PART 3
N1    4    0.471016    0.528984    0.443973    10.12500    0.08739    0.08739 =
         0.08369   -0.00206    0.00206    0.00808
PART -1
C1    1    0.339611    0.446935    0.385430    10.12500    0.12520    0.11061 =
         0.10502   -0.01066   -0.02248    0.00453
PART 3
C6    1    0.553887    0.446113    0.409014    10.12500    0.09119    0.09119 =
         0.08990   -0.00805    0.00805    0.00970
PART -1
C3    1    0.596003    0.538501    0.284615    10.12500    0.18318    0.18809 =
         0.16617    0.02492    0.00223   -0.00315
PART 3
C5    1    0.602310    0.758573    0.297209    10.25000    0.18577    0.19014 =
         0.18385    0.03196    0.00649   -0.00325
PART -1
C2    1    0.597024    0.722166    0.332574    10.25000    0.17565    0.17387 =
         0.17785    0.02256    0.01231    0.01411
C4    1    0.433938    0.554866    0.349157    10.12500    0.13926    0.13542 =
         0.11742    0.00695   -0.00774    0.00901
HKLF 4




REM  zybya_403k1_auto_d.res in I4/mmm
REM wR2 = 0.0842, GooF = S = 1.116, Restrained GooF = 1.091 for all data
REM R1 = 0.0313 for 531 Fo > 4sig(Fo) and 0.0331 for all 568 data
REM 67 parameters refined using 79 restraints

END

WGHT      0.0638      0.0000

REM Highest difference peak  0.346,  deepest hole -0.366,  1-sigma level  0.085
Q1    1   0.4171  0.4171  0.3900  10.50000  0.05    0.35
Q2    1   0.5000  0.5000  0.3221  10.12500  0.05    0.32
;
_shelx_res_checksum              59915
_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_3_293k
_database_code_depnum_ccdc_archive 'CCDC 2204251'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-09-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd Cl4, 2(C8 H11 F N)'
_chemical_formula_sum            'C16 H22 Cd Cl4 F2 N2'
_chemical_formula_weight         534.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'F Cd Cl C H N'
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'
F F 0.0171 0.0103 '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                   20.0721(17)
_cell_length_b                   7.3523(6)
_cell_length_c                   7.4427(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.274(7)
_cell_angle_gamma                90
_cell_volume                     1095.31(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6091
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      31.0210
_cell_measurement_theta_min      2.9690
_shelx_estimated_absorpt_T_max   0.864
_shelx_estimated_absorpt_T_min   0.864
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.034
_diffrn_reflns_theta_min         2.035
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  10.00   0.50    0.06    --    5.00  91.00 122.00   68
  2  ω     -9.00  36.00   0.50    0.06    --    5.00 -99.00 150.00   90
  3  ω    -33.00  -7.00   0.50    0.06    --    5.00 -91.00   8.00   52
  4  ω      1.00  28.00   0.50    0.06    --    5.00 -91.00   8.00   54
  5  ω    -17.00  33.00   0.50    0.06    --    5.00 -99.00-120.00  100
  6  ω    -17.00  28.00   0.50    0.06    --   -5.46 -99.00 -30.00   90
  7  ω    -78.00   1.00   0.50    0.06    --   -5.46 -37.00 120.00  158
;
_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      -0.0215743000
_diffrn_orient_matrix_UB_12      0.0358629000
_diffrn_orient_matrix_UB_13      -0.0711423000
_diffrn_orient_matrix_UB_21      0.0193226000
_diffrn_orient_matrix_UB_22      0.0807388000
_diffrn_orient_matrix_UB_23      0.0007889000
_diffrn_orient_matrix_UB_31      0.0203323000
_diffrn_orient_matrix_UB_32      -0.0387295000
_diffrn_orient_matrix_UB_33      -0.0640108000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2324
_reflns_number_total             3498
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      0.993
_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)+(0.0706P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1133
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 N12(H12A,H12B,H12C)
;
_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 0.500000 1.000000 0.500000 0.02945(13) Uani 1 2 d S . P . .
Cl2 Cl 0.48470(4) 0.72413(10) 0.27243(9) 0.0422(2) Uani 1 1 d . . . . .
Cl3 Cl 0.62630(4) 0.95299(13) 0.53796(11) 0.0451(2) Uani 1 1 d . . . . .
N12 N 0.38465(17) 0.4888(3) 0.5064(5) 0.0479(8) Uani 1 1 d . . . . .
H12A H 0.415320 0.553311 0.453927 0.058 Uiso 1 1 calc R U . . .
H12B H 0.390920 0.370983 0.486242 0.058 Uiso 1 1 calc R U . . .
H12C H 0.388229 0.509842 0.624492 0.058 Uiso 1 1 calc R U . . .
C11 C 0.3172(2) 0.5428(5) 0.4307(6) 0.0541(8) Uani 1 1 d . . . . .
H11A H 0.310647 0.501437 0.306895 0.065 Uiso 1 1 calc R U . . .
H11B H 0.313576 0.674336 0.430953 0.065 Uiso 1 1 calc R U . . .
C4 C 0.1949(2) 0.4897(5) 0.4489(7) 0.0596(12) Uani 1 1 d . . . . .
C10 C 0.2639(2) 0.4630(7) 0.5381(7) 0.0688(12) Uani 1 1 d . . . . .
H10A H 0.266283 0.519275 0.656319 0.083 Uiso 1 1 calc R U . . .
H10B H 0.272157 0.333913 0.554557 0.083 Uiso 1 1 calc R U . . .
F13 F 0.00414(19) 0.5511(6) 0.2154(7) 0.1283(14) Uani 1 1 d . . . . .
C9 C 0.1683(2) 0.3755(8) 0.3164(8) 0.0978(17) Uani 1 1 d . . . . .
H9 H 0.194052 0.279421 0.279215 0.117 Uiso 1 1 calc R U . . .
C7 C 0.0678(3) 0.5319(9) 0.2926(9) 0.0840(16) Uani 1 1 d . . . . .
C8 C 0.1053(3) 0.3984(9) 0.2376(8) 0.1026(19) Uani 1 1 d . . . . .
H8 H 0.088966 0.320756 0.145962 0.123 Uiso 1 1 calc R U . . .
C5 C 0.1548(2) 0.6297(8) 0.4969(7) 0.0957(17) Uani 1 1 d . . . . .
H5 H 0.171122 0.713611 0.582834 0.115 Uiso 1 1 calc R U . . .
C6 C 0.0906(3) 0.6477(9) 0.4194(8) 0.108(2) Uani 1 1 d . . . . .
H6 H 0.063271 0.740833 0.455938 0.130 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 0.0413(2) 0.02393(19) 0.02293(18) 0.00010(7) 0.00117(12) 0.00093(8)
Cl2 0.0615(5) 0.0323(3) 0.0327(3) -0.0108(2) 0.0024(3) 0.0015(3)
Cl3 0.0408(4) 0.0482(4) 0.0462(4) -0.0011(3) 0.0028(3) 0.0008(3)
N12 0.0424(18) 0.0508(19) 0.050(2) 0.0039(10) -0.0002(14) -0.0035(10)
C11 0.054(2) 0.0538(17) 0.054(2) 0.0057(18) 0.0011(17) -0.0006(18)
C4 0.050(2) 0.074(3) 0.056(3) 0.0018(15) 0.011(2) 0.0076(15)
C10 0.047(2) 0.098(3) 0.062(3) 0.018(2) 0.0074(19) 0.011(2)
F13 0.0545(17) 0.194(3) 0.133(3) 0.001(3) -0.021(2) 0.006(2)
C9 0.065(3) 0.107(4) 0.122(5) -0.045(4) 0.011(3) 0.002(3)
C7 0.047(3) 0.119(4) 0.084(4) -0.002(3) -0.004(2) 0.001(3)
C8 0.066(3) 0.132(5) 0.108(4) -0.042(4) -0.004(3) -0.013(3)
C5 0.077(3) 0.118(4) 0.088(3) -0.041(3) -0.017(3) 0.033(3)
C6 0.071(3) 0.137(5) 0.114(4) -0.032(4) -0.010(3) 0.043(3)

_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 Cl2 2.6483(6) 4_576 ?
Cd1 Cl2 2.6483(6) 2_655 ?
Cd1 Cl2 2.6457(6) 3_676 ?
Cd1 Cl2 2.6457(6) . ?
Cd1 Cl3 2.5534(8) . ?
Cd1 Cl3 2.5534(8) 3_676 ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N12 H12C 0.8900 . ?
N12 C11 1.482(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.502(6) . ?
C4 C10 1.503(7) . ?
C4 C9 1.372(7) . ?
C4 C5 1.370(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
F13 C7 1.369(6) . ?
C9 H9 0.9300 . ?
C9 C8 1.364(7) . ?
C7 C8 1.321(8) . ?
C7 C6 1.327(8) . ?
C8 H8 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.379(6) . ?
C6 H6 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
Cl2 Cd1 Cl2 180.0 . 3_676 ?
Cl2 Cd1 Cl2 89.918(8) 3_676 2_655 ?
Cl2 Cd1 Cl2 90.082(7) . 2_655 ?
Cl2 Cd1 Cl2 89.918(7) . 4_576 ?
Cl2 Cd1 Cl2 180.0 2_655 4_576 ?
Cl2 Cd1 Cl2 90.082(8) 3_676 4_576 ?
Cl3 Cd1 Cl2 88.05(3) . 3_676 ?
Cl3 Cd1 Cl2 88.05(3) 3_676 . ?
Cl3 Cd1 Cl2 90.11(3) . 4_576 ?
Cl3 Cd1 Cl2 91.95(3) 3_676 3_676 ?
Cl3 Cd1 Cl2 91.95(3) . . ?
Cl3 Cd1 Cl2 89.89(3) . 2_655 ?
Cl3 Cd1 Cl2 90.11(3) 3_676 2_655 ?
Cl3 Cd1 Cl2 89.89(3) 3_676 4_576 ?
Cl3 Cd1 Cl3 180.0 . 3_676 ?
Cd1 Cl2 Cd1 162.29(4) . 2_645 ?
H12A N12 H12B 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
C11 N12 H12A 109.5 . . ?
C11 N12 H12B 109.5 . . ?
C11 N12 H12C 109.5 . . ?
N12 C11 H11A 109.4 . . ?
N12 C11 H11B 109.4 . . ?
N12 C11 C10 111.1(3) . . ?
H11A C11 H11B 108.0 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C9 C4 C10 122.3(4) . . ?
C5 C4 C10 121.5(4) . . ?
C5 C4 C9 116.3(5) . . ?
C11 C10 C4 112.5(4) . . ?
C11 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C4 C10 H10A 109.1 . . ?
C4 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C4 C9 H9 118.9 . . ?
C8 C9 C4 122.2(5) . . ?
C8 C9 H9 118.9 . . ?
C8 C7 F13 118.8(6) . . ?
C8 C7 C6 121.6(5) . . ?
C6 C7 F13 119.6(5) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 C9 119.3(5) . . ?
C7 C8 H8 120.3 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.8(5) . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 119.9(5) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?

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
N12 C11 C10 C4 -170.8(3) . . . . ?
C4 C9 C8 C7 -1.6(10) . . . . ?
C4 C5 C6 C7 -2.2(10) . . . . ?
C10 C4 C9 C8 179.0(5) . . . . ?
C10 C4 C5 C6 -177.2(5) . . . . ?
F13 C7 C8 C9 -178.5(6) . . . . ?
F13 C7 C6 C5 -179.6(6) . . . . ?
C9 C4 C10 C11 83.1(6) . . . . ?
C9 C4 C5 C6 2.4(9) . . . . ?
C8 C7 C6 C5 -0.1(11) . . . . ?
C5 C4 C10 C11 -97.3(6) . . . . ?
C5 C4 C9 C8 -0.6(9) . . . . ?
C6 C7 C8 C9 1.9(11) . . . . ?

_shelx_res_file                  
;
TITL zy4f_rt_auto_a.res in P2(1)/c
    3_293k.res
    created by SHELXL-2018/3 at 19:20:20 on 24-Sep-2022
REM Old TITL ZY4F_RT_auto in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.116, Rweak 0.017, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: C18 F2 Cl4 Cd
CELL 0.71073 20.0721 7.3523 7.4427 90 94.274 90
ZERR 4 0.0017 0.0006 0.0005 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cd Cl F N
UNIT 32 44 2 8 4 4

L.S. 20
PLAN  5
SIZE 0.1 0.1 0.1
TEMP 20
CONF
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\zy4f_rt_auto.hkl">
REM </olex2.extras>

WGHT    0.070600
FVAR       0.51821
CD1   3    0.500000    1.000000    0.500000    10.50000    0.04128    0.02393 =
         0.02293    0.00010    0.00117    0.00093
CL2   4    0.484698    0.724126    0.272426    11.00000    0.06151    0.03233 =
         0.03272   -0.01081    0.00240    0.00148
CL3   4    0.626305    0.952986    0.537958    11.00000    0.04080    0.04821 =
         0.04624   -0.00111    0.00284    0.00076
N12   6    0.384645    0.488844    0.506400    11.00000    0.04244    0.05075 =
         0.05006    0.00389   -0.00019   -0.00346
AFIX 137
H12A  2    0.415320    0.553311    0.453927    11.00000   -1.20000
H12B  2    0.390920    0.370983    0.486242    11.00000   -1.20000
H12C  2    0.388229    0.509842    0.624492    11.00000   -1.20000
AFIX   0
C11   1    0.317174    0.542772    0.430723    11.00000    0.05408    0.05384 =
         0.05381    0.00570    0.00114   -0.00056
AFIX  23
H11A  2    0.310647    0.501437    0.306895    11.00000   -1.20000
H11B  2    0.313576    0.674336    0.430953    11.00000   -1.20000
AFIX   0
C4    1    0.194885    0.489705    0.448922    11.00000    0.04978    0.07423 =
         0.05588    0.00180    0.01088    0.00761
C10   1    0.263871    0.463039    0.538116    11.00000    0.04714    0.09773 =
         0.06205    0.01768    0.00740    0.01119
AFIX  23
H10A  2    0.266283    0.519275    0.656319    11.00000   -1.20000
H10B  2    0.272157    0.333913    0.554557    11.00000   -1.20000
AFIX   0
F13   5    0.004144    0.551076    0.215360    11.00000    0.05454    0.19353 =
         0.13271    0.00071   -0.02111    0.00551
C9    1    0.168286    0.375535    0.316428    11.00000    0.06503    0.10673 =
         0.12231   -0.04473    0.01052    0.00196
AFIX  43
H9    2    0.194052    0.279421    0.279215    11.00000   -1.20000
AFIX   0
C7    1    0.067800    0.531927    0.292573    11.00000    0.04733    0.11928 =
         0.08403   -0.00164   -0.00428    0.00099
C8    1    0.105322    0.398390    0.237552    11.00000    0.06554    0.13219 =
         0.10843   -0.04190   -0.00366   -0.01253
AFIX  43
H8    2    0.088966    0.320756    0.145962    11.00000   -1.20000
AFIX   0
C5    1    0.154813    0.629730    0.496950    11.00000    0.07747    0.11828 =
         0.08789   -0.04147   -0.01742    0.03302
AFIX  43
H5    2    0.171122    0.713611    0.582834    11.00000   -1.20000
AFIX   0
C6    1    0.090568    0.647732    0.419405    11.00000    0.07097    0.13676 =
         0.11377   -0.03227   -0.00961    0.04314
AFIX  43
H6    2    0.063271    0.740833    0.455938    11.00000   -1.20000
AFIX   0
HKLF 4




REM  zy4f_rt_auto_a.res in P2(1)/c
REM wR2 = 0.1133, GooF = S = 0.993, Restrained GooF = 0.993 for all data
REM R1 = 0.0419 for 2324 Fo > 4sig(Fo) and 0.0514 for all 2825 data
REM 116 parameters refined using 0 restraints

END

WGHT      0.0706      0.0000

REM Highest difference peak  0.928,  deepest hole -1.145,  1-sigma level  0.139
Q1    1   0.5138  0.7809  0.2303  11.00000  0.05    0.93
Q2    1   0.4995  0.7990  0.5003  11.00000  0.05    0.64
Q3    1   0.5385  1.0824  0.4733  11.00000  0.05    0.64
Q4    1   0.5193  1.1063  0.5898  11.00000  0.05    0.60
Q5    1   0.5381  0.9151  0.4775  11.00000  0.05    0.58
;
_shelx_res_checksum              56004
_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 5.557
_oxdiff_exptl_absorpt_empirical_full_min 0.168
####################################################################### 
# 
# 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_3_408k
_database_code_depnum_ccdc_archive 'CCDC 2204252'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-30 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-12-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(Cd0.25 Cl), 2(C8 F N)'
_chemical_formula_sum            'C16 Cd Cl4 F2 N2'
_chemical_formula_weight         512.39
_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'
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'
F F 0.0171 0.0103 '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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.2977(2)
_cell_length_b                   5.2977(2)
_cell_length_c                   40.592(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1139.23(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4273
_cell_measurement_temperature    408.01(10)
_cell_measurement_theta_max      30.2470
_cell_measurement_theta_min      2.9950
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.869
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            5062
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.793
_diffrn_reflns_theta_min         2.007
_diffrn_ambient_temperature      408.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  66.00   0.50    0.53    --   -5.39  77.00-128.00  102
  2  ω    -16.00  34.00   0.50    0.53    --    4.92 -99.00 -90.00  100
  3  ω    -12.00  37.00   0.50    0.53    --    4.92 -99.00 -30.00   98
  4  ω    -62.00  17.00   0.50    0.53    --   -5.39 -77.00 105.00  158
  5  ω    -18.00   7.00   0.50    0.53    --    4.92 -99.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_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                522
_reflns_number_total             618
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         618
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      1.407
_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)+(0.1048P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1362
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C1-C2 = C2-C3
 1.4 with sigma of 0.02
 C1-C3
 2.425 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C4 \\sim C6 \\sim N1 \\sim C5 \\sim C3 \\sim C2 \\sim C1 \\sim F1: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(F1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3. Others
 Fixed Sof: C6(0.125) C4(0.125) N1(0.125) C1(0.125) F1(0.125) C2(0.25)
 C5(0.125) C3(0.25)
;
_atom_sites_solution_hydrogens   .
_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 1.000000 1.000000 0.500000 0.0554(4) Uani 1 16 d S TU P . .
Cl2 Cl 1.000000 0.500000 0.500000 0.0992(10) Uani 1 8 d S T P . .
Cl1 Cl 1.000000 1.000000 0.43814(7) 0.1222(16) Uani 1 8 d S T P . .
C6 C 0.54(5) 0.56(4) 0.4099(5) 0.096(8) Uani 0.125 1 d . U P A -1
C4 C 0.597(11) 0.47(3) 0.3539(8) 0.130(7) Uani 0.125 1 d . U P A -1
N1 N 0.468(15) 0.500000 0.4449(3) 0.090(10) Uani 0.25 2 d S TU P B 3
C1 C 0.733(10) 0.38(2) 0.2901(14) 0.169(8) Uani 0.125 1 d D U P A -1
F1 F 0.913(9) 0.444(12) 0.2627(6) 0.180(12) Uani 0.125 1 d . U P A -1
C2 C 0.473(9) 0.359(7) 0.2981(5) 0.166(7) Uani 0.25 1 d D U P A -1
C5 C 0.554(11) 0.365(9) 0.3882(7) 0.114(7) Uani 0.125 1 d . U P A -1
C3 C 0.433(7) 0.354(8) 0.3333(5) 0.150(6) Uani 0.25 1 d D 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 0.0378(4) 0.0378(4) 0.0904(6) 0.000 0.000 0.000
Cl2 0.0711(18) 0.0334(12) 0.193(3) 0.000 0.000 0.000
Cl1 0.143(3) 0.143(3) 0.0796(13) 0.000 0.000 0.000
C6 0.101(16) 0.094(15) 0.093(7) 0.003(10) 0.005(12) -0.005(12)
C4 0.134(10) 0.134(10) 0.121(8) -0.005(7) 0.001(7) 0.005(7)
N1 0.096(19) 0.090(18) 0.084(5) 0.000 0.012(11) 0.000
C1 0.170(11) 0.170(11) 0.168(10) -0.009(8) 0.003(8) 0.005(8)
F1 0.186(18) 0.175(19) 0.181(14) -0.003(14) 0.022(13) 0.012(14)
C2 0.164(10) 0.170(9) 0.162(8) -0.014(7) -0.002(7) 0.006(7)
C5 0.121(11) 0.115(10) 0.106(8) -0.001(7) 0.000(7) 0.006(8)
C3 0.151(10) 0.157(9) 0.143(7) -0.013(7) -0.004(7) 0.009(7)

_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 Cl2 2.64885(10) . ?
Cd1 Cl2 2.64885(10) 3_755 ?
Cd1 Cl2 2.64885(10) 3_655 ?
Cd1 Cl2 2.64885(10) 1_565 ?
Cd1 Cl1 2.511(3) 17_776 ?
Cd1 Cl1 2.511(3) . ?
C6 C5 1.35(17) . ?
C4 C5 1.52(8) . ?
C4 C3 1.36(11) . ?
C1 F1 1.50(5) . ?
C1 C2 1.42(2) . ?
C2 C3 1.447(18) . ?

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
Cl2 Cd1 Cl2 180.0 . 1_565 ?
Cl2 Cd1 Cl2 180.0 3_655 3_755 ?
Cl2 Cd1 Cl2 90.0 . 3_755 ?
Cl2 Cd1 Cl2 90.0 1_565 3_655 ?
Cl2 Cd1 Cl2 90.0 . 3_655 ?
Cl2 Cd1 Cl2 90.0 1_565 3_755 ?
Cl1 Cd1 Cl2 90.0 17_776 3_755 ?
Cl1 Cd1 Cl2 90.0 17_776 3_655 ?
Cl1 Cd1 Cl2 90.0 . 1_565 ?
Cl1 Cd1 Cl2 90.0 . . ?
Cl1 Cd1 Cl2 90.0 . 3_655 ?
Cl1 Cd1 Cl2 90.0 . 3_755 ?
Cl1 Cd1 Cl2 90.0 17_776 1_565 ?
Cl1 Cd1 Cl2 90.0 17_776 . ?
Cl1 Cd1 Cl1 180.0 17_776 . ?
Cd1 Cl2 Cd1 180.0 1_545 . ?
C3 C4 C5 107(10) . . ?
C2 C1 F1 143(6) . . ?
C1 C2 C3 112(3) . . ?
C6 C5 C4 108(8) . . ?
C4 C3 C2 120(4) . . ?

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
C1 C2 C3 C4 29(9) . . . . ?
F1 C1 C2 C3 -165(13) . . . . ?
C5 C4 C3 C2 -162(4) . . . . ?
C3 C4 C5 C6 -134(14) . . . . ?

_shelx_res_file                  
;
TITL zy4f_408k_auto_a.res in I4/mmm
    3_408k.res
    created by SHELXL-2018/3 at 12:03:04 on 29-Dec-2022
REM Old TITL zy4f_408k_auto_a.res in I4/mmm
REM SHELXT solution in I4/mmm
REM R1 0.220, Rweak 0.039, Alpha 0.056, Orientation as input
REM Formula found by SHELXT: Cd Cl4 C1
CELL 0.71073 5.2977 5.2977 40.5917 90 90 90
ZERR 4 0.0002 0.0002 0.0027 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC C Cd Cl F N
UNIT 32 2 8 4 4
ISOR 0.01 0.02 C4 C6 N1 C5 C3 C2 C1 F1
SIMU 0.01 0.02 2 C4 C6 N1 C5 C3 C2 C1 F1
ISOR 0.003 0.006 Cd1
DANG 2.425 C1 C3
DFIX 1.4 C1 C2 C2 C3

L.S. 20
PLAN  6
SIZE 0.1 0.1 0.02
TEMP 135
CONF
BIND N1 C6
list 4
MORE -1
fmap 2
acta
OMIT 1 1 6
REM <olex2.extras>
REM <HklSrc "%.\\3_408k.hkl">
REM </olex2.extras>

WGHT    0.104800
FVAR       0.54550
CD1   2    1.000000    1.000000    0.500000    10.06250    0.03784    0.03784 =
         0.09039    0.00000    0.00000    0.00000
CL2   3    1.000000    0.500000    0.500000    10.12500    0.07114    0.03341 =
         0.19310    0.00000    0.00000    0.00000
CL1   3    1.000000    1.000000    0.438137    10.12500    0.14344    0.14344 =
         0.07964    0.00000    0.00000    0.00000
PART -1
C6    1    0.542552    0.559006    0.409855    10.12500    0.10104    0.09441 =
         0.09287    0.00256    0.00536   -0.00498
C4    1    0.596607    0.474215    0.353894    10.12500    0.13446    0.13404 =
         0.12056   -0.00522    0.00121    0.00457
PART 3
N1    5    0.467635    0.500000    0.444914    10.12500    0.09643    0.09023 =
         0.08377    0.00000    0.01245    0.00000
PART -1
C1    1    0.732929    0.382131    0.290107    10.12500    0.16999    0.17041 =
         0.16797   -0.00857    0.00326    0.00510
F1    4    0.912559    0.444258    0.262702    10.12500    0.18559    0.17491 =
         0.18089   -0.00263    0.02199    0.01223
C2    1    0.473470    0.359303    0.298085    10.25000    0.16440    0.16966 =
         0.16247   -0.01367   -0.00237    0.00612
C5    1    0.553749    0.365012    0.388153    10.12500    0.12069    0.11486 =
         0.10610   -0.00112    0.00034    0.00575
C3    1    0.433398    0.354106    0.333336    10.25000    0.15085    0.15748 =
         0.14305   -0.01318   -0.00404    0.00876
HKLF 4




REM  zy4f_408k_auto_a.res in I4/mmm
REM wR2 = 0.1362, GooF = S = 1.270, Restrained GooF = 1.407 for all data
REM R1 = 0.0505 for 522 Fo > 4sig(Fo) and 0.0510 for all 528 data
REM 78 parameters refined using 99 restraints

END

WGHT      0.1044      0.0000

REM Highest difference peak  0.651,  deepest hole -0.692,  1-sigma level  0.169
Q1    1   0.5000  0.5000  0.2522  10.12500  0.05    0.65
Q2    1   1.0000  1.0000  0.5083  10.12500  0.05    0.55
Q3    1   0.2642  0.2642  0.3441  10.50000  0.05    0.43
Q4    1   0.5000  0.5000  0.3517  10.12500  0.05    0.39
Q5    1   0.5000  0.3048  0.3921  10.50000  0.05    0.36
Q6    1   0.7587  0.2413  0.3084  10.50000  0.05    0.29
;
_shelx_res_checksum              94214
# end Validation Reply Form
_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
;
# start Validation Reply Form
_vrf_PLAT088_3_408k              
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.92 Note  
RESPONSE: In order to deal with disorder, more limit instructions have been added.
;
_vrf_PLAT242_3_408k              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cd1 Check 
RESPONSE: Cd is heavy element, this alert is common for compound of such molecule type.
;
####################################################################### 
# 
# 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_1_293k
_database_code_depnum_ccdc_archive 'CCDC 2204249'
loop_
_audit_author_name
_audit_author_address
'zhiyuan yue'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_audit_creation_date             2022-12-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd Cl4, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Cd Cl4 N2'
_chemical_formula_weight         498.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd Cl C H N'
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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.3756(5)
_cell_length_b                   7.4398(5)
_cell_length_c                   38.942(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2136.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    293.01(10)
_cell_measurement_theta_max      29.3390
_cell_measurement_theta_min      2.0800
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.863
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            11551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.792
_diffrn_reflns_theta_min         2.092
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  77.00   0.25    0.03    --    4.92  53.00 156.00  320
  2  ω    -18.00  20.00   0.25    0.03    --    4.92 -99.00 -30.00  152
  3  ω    -15.00  33.00   0.25    0.03    --    4.92 -99.00 -60.00  192
;
_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      -0.0935135000
_diffrn_orient_matrix_UB_12      0.0214966000
_diffrn_orient_matrix_UB_13      -0.0011779000
_diffrn_orient_matrix_UB_21      -0.0128556000
_diffrn_orient_matrix_UB_22      -0.0723853000
_diffrn_orient_matrix_UB_23      -0.0115931000
_diffrn_orient_matrix_UB_31      -0.0185326000
_diffrn_orient_matrix_UB_32      -0.0581198000
_diffrn_orient_matrix_UB_33      0.0140062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1931
_reflns_number_total             3350
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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  (Sheldrick, 2015)'
_refine_diff_density_max         0.522
_refine_diff_density_min         -2.703
_refine_diff_density_rms         0.230
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.108
_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)+(0.0640P)²+1.0423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1406
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_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
Cd1 Cd 0.500000 0.000000 0.000000 0.02943(17) Uani 1 2 d S . P . .
Cl2 Cl 0.22474(13) 0.22533(13) 0.00802(3) 0.0414(3) Uani 1 1 d . . . . .
Cl3 Cl 0.54797(18) 0.01308(13) 0.06493(3) 0.0448(3) Uani 1 1 d . . . . .
N1 N 0.9894(5) -0.0281(5) 0.05917(10) 0.0452(10) Uani 1 1 d . . . . .
H1A H 1.057110 0.027299 0.043504 0.054 Uiso 1 1 calc R U . . .
H1B H 0.873019 -0.002834 0.055506 0.054 Uiso 1 1 calc R U . . .
H1C H 1.006260 -0.146322 0.057642 0.054 Uiso 1 1 calc R U . . .
C2 C 0.9871(7) -0.0099(7) 0.15701(15) 0.0586(17) Uani 1 1 d . . . . .
C3 C 1.0422(8) 0.0343(7) 0.09396(12) 0.0545(12) Uani 1 1 d . . . . .
H3A H 1.000430 0.156664 0.097286 0.065 Uiso 1 1 calc R U . . .
H3B H 1.173304 0.033836 0.095910 0.065 Uiso 1 1 calc R U . . .
C4 C 1.1396(11) 0.0009(9) 0.21129(15) 0.089(2) Uani 1 1 d . . . . .
H4 H 1.231633 -0.040981 0.225519 0.107 Uiso 1 1 calc R U . . .
C5 C 1.1250(9) -0.0661(8) 0.17823(13) 0.0753(16) Uani 1 1 d . . . . .
H5 H 1.208956 -0.149634 0.170321 0.090 Uiso 1 1 calc R U . . .
C6 C 0.9631(8) -0.0835(8) 0.12115(12) 0.0665(14) Uani 1 1 d . . . . .
H6A H 1.019767 -0.200937 0.119861 0.080 Uiso 1 1 calc R U . . .
H6B H 0.834688 -0.098941 0.116671 0.080 Uiso 1 1 calc R U . . .
C7 C 0.8721(10) 0.1179(9) 0.16955(15) 0.090(2) Uani 1 1 d . . . . .
H7 H 0.777746 0.160012 0.155892 0.108 Uiso 1 1 calc R U . . .
C8 C 1.0247(11) 0.1239(11) 0.22306(16) 0.092(2) Uani 1 1 d . . . . .
H8 H 1.035288 0.166154 0.245447 0.111 Uiso 1 1 calc R U . . .
C9 C 0.8945(11) 0.1861(10) 0.20262(17) 0.101(2) Uani 1 1 d . . . . .
H9 H 0.817499 0.276115 0.210498 0.121 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 0.0249(3) 0.0237(2) 0.0397(3) -0.00174(12) -0.00056(12) 0.00003(13)
Cl2 0.0338(5) 0.0323(5) 0.0581(5) -0.0020(4) -0.0017(4) 0.0102(4)
Cl3 0.0483(6) 0.0484(6) 0.0378(5) 0.0007(4) -0.0003(5) 0.0009(5)
N1 0.051(3) 0.044(2) 0.040(2) -0.0028(14) 0.0020(13) -0.0023(15)
C2 0.075(5) 0.060(4) 0.041(3) 0.0066(18) -0.0024(19) 0.000(2)
C3 0.057(3) 0.056(3) 0.050(3) -0.004(2) -0.001(2) -0.009(2)
C4 0.111(6) 0.101(5) 0.056(3) 0.009(3) -0.032(4) -0.005(4)
C5 0.095(5) 0.066(4) 0.065(3) 0.000(3) -0.018(3) 0.019(3)
C6 0.094(4) 0.056(3) 0.050(3) 0.003(2) -0.007(2) -0.012(3)
C7 0.101(5) 0.100(5) 0.068(4) 0.001(3) -0.006(3) 0.034(4)
C8 0.134(7) 0.096(6) 0.046(3) -0.006(3) 0.001(3) -0.017(5)
C9 0.130(7) 0.096(5) 0.076(4) -0.019(3) 0.017(4) 0.032(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 Cl2 2.6514(9) . ?
Cd1 Cl2 2.6513(9) 5_655 ?
Cd1 Cl2 2.6497(8) 3 ?
Cd1 Cl2 2.6497(8) 7_655 ?
Cd1 Cl3 2.5549(10) 5_655 ?
Cd1 Cl3 2.5551(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.484(6) . ?
C2 C5 1.375(7) . ?
C2 C6 1.510(8) . ?
C2 C7 1.365(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C6 1.493(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.385(8) . ?
C4 C8 1.329(10) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7 0.9300 . ?
C7 C9 1.394(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.331(9) . ?
C9 H9 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
Cl2 Cd1 Cl2 180.00(7) 7_655 3 ?
Cl2 Cd1 Cl2 180.0 5_655 . ?
Cl2 Cd1 Cl2 89.698(8) 7_655 . ?
Cl2 Cd1 Cl2 90.302(8) 7_655 5_655 ?
Cl2 Cd1 Cl2 89.698(8) 3 5_655 ?
Cl2 Cd1 Cl2 90.302(8) 3 . ?
Cl3 Cd1 Cl2 88.02(3) 5_655 5_655 ?
Cl3 Cd1 Cl2 91.99(3) 5_655 . ?
Cl3 Cd1 Cl2 90.04(3) . 3 ?
Cl3 Cd1 Cl2 91.98(3) . 5_655 ?
Cl3 Cd1 Cl2 88.01(3) . . ?
Cl3 Cd1 Cl2 90.04(3) 5_655 7_655 ?
Cl3 Cd1 Cl2 89.96(3) . 7_655 ?
Cl3 Cd1 Cl2 89.96(3) 5_655 3 ?
Cl3 Cd1 Cl3 180.0 5_655 . ?
Cd1 Cl2 Cd1 162.32(5) 3_455 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
C5 C2 C6 122.2(5) . . ?
C7 C2 C5 117.1(6) . . ?
C7 C2 C6 120.7(5) . . ?
N1 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
N1 C3 C6 111.2(4) . . ?
H3A C3 H3B 108.0 . . ?
C6 C3 H3A 109.4 . . ?
C6 C3 H3B 109.4 . . ?
C5 C4 H4 119.4 . . ?
C8 C4 H4 119.4 . . ?
C8 C4 C5 121.3(6) . . ?
C2 C5 C4 120.5(6) . . ?
C2 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C2 C6 H6A 108.9 . . ?
C2 C6 H6B 108.9 . . ?
C3 C6 C2 113.4(5) . . ?
C3 C6 H6A 108.9 . . ?
C3 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C2 C7 H7 119.7 . . ?
C2 C7 C9 120.7(6) . . ?
C9 C7 H7 119.7 . . ?
C4 C8 H8 120.2 . . ?
C4 C8 C9 119.6(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C9 H9 119.6 . . ?
C8 C9 C7 120.8(6) . . ?
C8 C9 H9 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C3 C6 C2 -170.8(4) . . . . ?
C2 C7 C9 C8 -2.2(12) . . . . ?
C4 C8 C9 C7 2.9(12) . . . . ?
C5 C2 C6 C3 -97.7(7) . . . . ?
C5 C2 C7 C9 -0.5(10) . . . . ?
C5 C4 C8 C9 -1.0(12) . . . . ?
C6 C2 C5 C4 -178.2(6) . . . . ?
C6 C2 C7 C9 -179.9(6) . . . . ?
C7 C2 C5 C4 2.4(9) . . . . ?
C7 C2 C6 C3 81.6(7) . . . . ?
C8 C4 C5 C2 -1.8(11) . . . . ?

_shelx_res_file                  
;
TITL ZYBYA_RT1_auto in Pbca #61
    1_293k.res
    created by SHELXL-2018/3 at 15:49:37 on 13-Dec-2022
REM reset to Pbca #61
CELL 0.71073 7.3756 7.4398 38.9424 90 90 90
ZERR 4 0.0005 0.0005 0.0024 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cd Cl N
UNIT 64 96 4 16 8

L.S. 5
PLAN  5
SIZE 0.1 0.1 0.1
TEMP 20
CONF
BOND
MORE -1
BOND $H
fmap 2
acta
OMIT 2 2 0
OMIT 0 2 0
REM <olex2.extras>
REM <HklSrc "%.\\ZYBYA_RT1_auto.hkl">
REM </olex2.extras>

WGHT    0.064000    1.042300
FVAR       2.36627
CD1   3    0.500000    0.000000    0.000000    10.50000    0.02492    0.02367 =
         0.03972   -0.00174   -0.00056    0.00003
CL2   4    0.224738    0.225329    0.008022    11.00000    0.03380    0.03225 =
         0.05810   -0.00199   -0.00174    0.01019
CL3   4    0.547967    0.013083    0.064931    11.00000    0.04826    0.04840 =
         0.03783    0.00072   -0.00031    0.00085
N1    5    0.989357   -0.028145    0.059171    11.00000    0.05123    0.04433 =
         0.03997   -0.00279    0.00202   -0.00232
AFIX 137
H1A   2    1.057110    0.027299    0.043504    11.00000   -1.20000
H1B   2    0.873019   -0.002834    0.055506    11.00000   -1.20000
H1C   2    1.006260   -0.146322    0.057642    11.00000   -1.20000
AFIX   0
C2    1    0.987135   -0.009903    0.157008    11.00000    0.07506    0.05966 =
         0.04115    0.00663   -0.00237    0.00018
C3    1    1.042193    0.034263    0.093961    11.00000    0.05703    0.05625 =
         0.05037   -0.00433   -0.00122   -0.00932
AFIX  23
H3A   2    1.000430    0.156664    0.097286    11.00000   -1.20000
H3B   2    1.173304    0.033836    0.095910    11.00000   -1.20000
AFIX   0
C4    1    1.139617    0.000905    0.211286    11.00000    0.11144    0.10115 =
         0.05563    0.00918   -0.03245   -0.00490
AFIX  43
H4    2    1.231633   -0.040981    0.225519    11.00000   -1.20000
AFIX   0
C5    1    1.124982   -0.066076    0.178229    11.00000    0.09505    0.06595 =
         0.06496   -0.00039   -0.01780    0.01944
AFIX  43
H5    2    1.208956   -0.149634    0.170321    11.00000   -1.20000
AFIX   0
C6    1    0.963116   -0.083467    0.121147    11.00000    0.09385    0.05553 =
         0.05013    0.00277   -0.00655   -0.01161
AFIX  23
H6A   2    1.019767   -0.200937    0.119861    11.00000   -1.20000
H6B   2    0.834688   -0.098941    0.116671    11.00000   -1.20000
AFIX   0
C7    1    0.872067    0.117947    0.169553    11.00000    0.10108    0.09996 =
         0.06818    0.00146   -0.00551    0.03441
AFIX  43
H7    2    0.777746    0.160012    0.155892    11.00000   -1.20000
AFIX   0
C8    1    1.024742    0.123854    0.223063    11.00000    0.13439    0.09592 =
         0.04644   -0.00594    0.00064   -0.01650
AFIX  43
H8    2    1.035288    0.166154    0.245447    11.00000   -1.20000
AFIX   0
C9    1    0.894479    0.186097    0.202624    11.00000    0.13026    0.09607 =
         0.07643   -0.01872    0.01743    0.03205
AFIX  43
H9    2    0.817499    0.276115    0.210498    11.00000   -1.20000
AFIX   0
HKLF 4




REM  ZYBYA_RT1_auto in Pbca #61
REM wR2 = 0.1406, GooF = S = 1.108, Restrained GooF = 1.108 for all data
REM R1 = 0.0543 for 1931 Fo > 4sig(Fo) and 0.0750 for all 2703 data
REM 107 parameters refined using 0 restraints

END

WGHT      0.0640      1.0423

REM Highest difference peak  0.522,  deepest hole -2.703,  1-sigma level  0.230
Q1    1   0.2012  0.0093  0.0050  11.00000  0.05    0.52
Q2    1   1.0876 -0.4124  0.1129  11.00000  0.05    0.50
Q3    1   0.1876  0.1341  0.0018  11.00000  0.05    0.49
Q4    1   0.5886 -0.0771  0.1382  11.00000  0.05    0.49
Q5    1   0.4986  0.0560  0.1785  11.00000  0.05    0.49
;
_shelx_res_checksum              71461
_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 2.289
_oxdiff_exptl_absorpt_empirical_full_min 0.378
