# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_t20201009_hdc104_2_0m
_database_code_depnum_ccdc_archive 'CCDC 2263024'
loop_
_audit_author_name
_audit_author_address
'Ding-Chong Han'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2023-05-15 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(C8 H11 Cl N), 0.5(Br8 Cd2)'
_chemical_formula_sum            'C16 H22 Br4 Cd Cl2 N2'
_chemical_formula_weight         745.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y+1/2, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y-1/2, -z-1/2'
7 '-x-1/2, y-1/2, z'
8 'x, -y, z-1/2'

_cell_length_a                   7.917(3)
_cell_length_b                   7.942(4)
_cell_length_c                   37.185(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2338.1(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.503
_cell_measurement_theta_min      3.287
_exptl_absorpt_coefficient_mu    8.002
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.7006.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            28394
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.80
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2202
_reflns_number_total             2691
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.093
_refine_diff_density_min         -2.301
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0790
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0667P)²+36.4846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2050
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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:
 C8(H8a,H8b), C7(H7a,H7b)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cl1 Cl 0.3044(7) 0.2300(9) 0.07602(17) 0.115(2) Uani 1 d . . 1 . . .
N1 N 0.4725(13) 0.2438(14) 0.1913(3) 0.049(3) Uani 1 d . . 1 . . .
H1A H 0.3812 0.1809 0.1876 0.059 Uiso 1 calc . . 1 GR . .
H1B H 0.4461 0.3295 0.2057 0.059 Uiso 1 calc . . 1 GR . .
H1C H 0.5524 0.1815 0.2017 0.059 Uiso 1 calc . . 1 GR . .
C8 C 0.5358(16) 0.3098(16) 0.1564(3) 0.042(3) Uani 1 d . . 1 . . .
H8A H 0.6339 0.3801 0.1607 0.050 Uiso 1 calc . . 1 R . .
H8B H 0.4491 0.3791 0.1454 0.050 Uiso 1 calc . . 1 R . .
C6 C 0.6335(19) 0.2387(15) 0.0949(3) 0.048(3) Uani 1 d . . 1 . . .
C1 C 0.5157(18) 0.276(2) 0.0685(4) 0.059(4) Uani 1 d . . 1 . . .
C7 C 0.5834(19) 0.1680(16) 0.1307(3) 0.052(3) Uani 1 d . . 1 . . .
H7A H 0.6766 0.1039 0.1406 0.062 Uiso 1 calc . . 1 R . .
H7B H 0.4881 0.0926 0.1277 0.062 Uiso 1 calc . . 1 R . .
C5 C 0.8000(18) 0.2738(17) 0.0863(4) 0.055(3) Uani 1 d . . 1 . . .
H5 H 0.8835 0.2514 0.1032 0.066 Uiso 1 calc . . 1 R . .
C3 C 0.729(2) 0.368(2) 0.0283(4) 0.065(4) Uani 1 d . . 1 . . .
H3 H 0.7625 0.4068 0.0058 0.078 Uiso 1 calc . . 1 R . .
C2 C 0.562(2) 0.339(2) 0.0348(4) 0.067(4) Uani 1 d . . 1 . . .
H2 H 0.4811 0.3614 0.0172 0.080 Uiso 1 calc . . 1 R . .
C4 C 0.847(2) 0.340(2) 0.0538(4) 0.066(4) Uani 1 d . . 1 . . .
H4 H 0.9593 0.3658 0.0493 0.079 Uiso 1 calc . . 1 R . .
Cd1 Cd 0.0000 0.25788(11) 0.2500 0.0234(3) Uani 1 d . . 2 S T P
Br1 Br 0.24343(11) 0.00424(12) 0.25961(3) 0.0338(3) Uani 1 d . . 1 . . .
Br2 Br 0.05427(14) 0.26487(13) 0.17971(3) 0.0354(3) Uani 1 d . . 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
Cl1 0.060(3) 0.185(7) 0.100(4) 0.007(4) -0.010(3) -0.020(3)
N1 0.042(6) 0.076(8) 0.028(5) -0.007(5) -0.003(4) -0.004(5)
C8 0.049(7) 0.045(6) 0.032(6) 0.000(5) 0.010(5) -0.001(5)
C6 0.065(8) 0.047(7) 0.033(6) -0.007(5) -0.002(6) 0.007(6)
C1 0.051(8) 0.076(10) 0.051(8) -0.010(7) -0.003(6) 0.004(7)
C7 0.069(9) 0.044(7) 0.043(7) -0.004(6) 0.003(6) 0.010(6)
C5 0.053(8) 0.069(9) 0.042(7) -0.003(6) -0.008(6) 0.009(7)
C3 0.088(12) 0.069(10) 0.038(7) 0.009(7) 0.010(8) -0.002(9)
C2 0.086(11) 0.079(10) 0.035(7) 0.012(7) -0.013(7) 0.009(9)
C4 0.056(9) 0.083(11) 0.059(9) -0.010(8) 0.021(7) 0.000(8)
Cd1 0.0206(5) 0.0197(4) 0.0299(5) 0.000 0.0019(3) 0.000
Br1 0.0246(5) 0.0265(5) 0.0503(7) -0.0006(4) 0.0026(5) 0.0120(4)
Br2 0.0343(6) 0.0434(6) 0.0284(5) 0.0017(4) -0.0006(4) 0.0004(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
Cl1 C1 1.735(16) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C8 1.487(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.525(17) . ?
C6 C1 1.386(19) . ?
C6 C7 1.496(18) . ?
C6 C5 1.39(2) . ?
C1 C2 1.40(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 H5 0.9300 . ?
C5 C4 1.37(2) . ?
C3 H3 0.9300 . ?
C3 C2 1.36(2) . ?
C3 C4 1.35(2) . ?
C2 H2 0.9300 . ?
C4 H4 0.9300 . ?
Cd1 Br1 2.8107(14) 4 ?
Cd1 Br1 2.8429(14) 7_665 ?
Cd1 Br1 2.8429(14) 6_566 ?
Cd1 Br1 2.8107(14) . ?
Cd1 Br2 2.6495(14) 4 ?
Cd1 Br2 2.6495(14) . ?
Br1 Cd1 2.8429(14) 6_656 ?

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
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N1 H1A 109.5 . . ?
C8 N1 H1B 109.5 . . ?
C8 N1 H1C 109.5 . . ?
N1 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
N1 C8 C7 111.8(10) . . ?
H8A C8 H8B 107.9 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C1 C6 C7 122.1(14) . . ?
C5 C6 C1 115.6(13) . . ?
C5 C6 C7 122.2(13) . . ?
C6 C1 Cl1 119.3(12) . . ?
C6 C1 C2 122.4(14) . . ?
C2 C1 Cl1 118.2(12) . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C6 C7 C8 110.2(10) . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C6 C5 H5 118.7 . . ?
C4 C5 C6 122.6(13) . . ?
C4 C5 H5 118.7 . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C4 C3 C2 121.3(14) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.1(14) . . ?
C3 C2 H2 120.9 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.9(15) . . ?
C3 C4 H4 120.1 . . ?
Br1 Cd1 Br1 177.68(5) . 6_566 ?
Br1 Cd1 Br1 93.02(6) 7_665 6_566 ?
Br1 Cd1 Br1 88.43(6) 4 . ?
Br1 Cd1 Br1 89.28(4) 4 6_566 ?
Br1 Cd1 Br1 177.68(5) 4 7_665 ?
Br1 Cd1 Br1 89.28(4) . 7_665 ?
Br2 Cd1 Br1 90.04(4) 4 . ?
Br2 Cd1 Br1 88.71(4) . 6_566 ?
Br2 Cd1 Br1 91.68(4) . . ?
Br2 Cd1 Br1 89.64(4) . 7_665 ?
Br2 Cd1 Br1 91.68(4) 4 4 ?
Br2 Cd1 Br1 89.64(4) 4 6_566 ?
Br2 Cd1 Br1 90.04(4) . 4 ?
Br2 Cd1 Br1 88.71(4) 4 7_665 ?
Br2 Cd1 Br2 177.60(6) . 4 ?
Cd1 Br1 Cd1 165.29(5) . 6_656 ?

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
Cl1 C1 C2 C3 -176.7(13) . . . . ?
N1 C8 C7 C6 175.6(11) . . . . ?
C6 C1 C2 C3 -2(2) . . . . ?
C6 C5 C4 C3 -2(2) . . . . ?
C1 C6 C7 C8 -85.3(16) . . . . ?
C1 C6 C5 C4 -1(2) . . . . ?
C7 C6 C1 Cl1 -3.6(19) . . . . ?
C7 C6 C1 C2 -178.7(13) . . . . ?
C7 C6 C5 C4 -179.4(13) . . . . ?
C5 C6 C1 Cl1 177.6(11) . . . . ?
C5 C6 C1 C2 3(2) . . . . ?
C5 C6 C7 C8 93.5(15) . . . . ?
C2 C3 C4 C5 4(3) . . . . ?
C4 C3 C2 C1 -2(3) . . . . ?
Br1 Cd1 Br1 Cd1 -88.01(19) 7_665 . . 6_656 ?
Br1 Cd1 Br1 Cd1 101.08(16) 6_566 . . 6_656 ?
Br1 Cd1 Br1 Cd1 91.60(19) 4 . . 6_656 ?
Br2 Cd1 Br1 Cd1 -176.72(18) 4 . . 6_656 ?
Br2 Cd1 Br1 Cd1 1.61(19) . . . 6_656 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cd
_database_code_depnum_ccdc_archive 'CCDC 2263054'
loop_
_audit_author_name
_audit_author_address
'Ding-Chong Han'
;Jiangxi University of Science and Technology
China
;
_audit_update_record             
;
2023-05-15 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Cd2 Cl8), 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Cd Cl6 N2'
_chemical_formula_weight         567.45
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.8581(14)
_cell_length_b                   7.6030(6)
_cell_length_c                   7.6418(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.102(2)
_cell_angle_gamma                90
_cell_volume                     1081.87(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.567
_cell_measurement_theta_min      2.894
_shelx_estimated_absorpt_T_max   0.844
_shelx_estimated_absorpt_T_min   0.743
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15000
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_min         2.894
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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                2230
_reflns_number_total             2470
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.934
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.153
_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)+(0.0452P)²+3.2626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1125
_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:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.0000 0.5000 0.02352(14) Uani 1 2 d S T P . .
Cl3 Cl 0.48304(6) -0.24706(12) 0.74585(12) 0.0348(2) Uani 1 1 d . . . . .
Cl2 Cl 0.36784(5) 0.05189(15) 0.44739(16) 0.0399(2) Uani 1 1 d . . . . .
Cl1 Cl 0.15889(14) 0.2856(2) 0.2842(4) 0.1025(7) Uani 1 1 d . . . . .
N1 N 0.3881(2) 0.4693(5) 0.4542(6) 0.0435(9) Uani 1 1 d . . . . .
H1A H 0.3846 0.3719 0.3887 0.052 Uiso 1 1 calc GR . . . .
H1B H 0.4146 0.4477 0.5590 0.052 Uiso 1 1 calc GR . . . .
H1C H 0.4087 0.5538 0.3991 0.052 Uiso 1 1 calc GR . . . .
C1 C 0.1417(3) 0.5019(7) 0.3382(9) 0.0558(14) Uani 1 1 d . . . . .
C6 C 0.1953(3) 0.6274(7) 0.3415(7) 0.0476(11) Uani 1 1 d . . . . .
C7 C 0.2708(3) 0.5830(9) 0.3127(7) 0.0544(13) Uani 1 1 d . . . . .
H7A H 0.2689 0.4896 0.2256 0.065 Uiso 1 1 calc R . . . .
H7B H 0.2922 0.6854 0.2663 0.065 Uiso 1 1 calc R . . . .
C5 C 0.1773(3) 0.7993(7) 0.3729(7) 0.0510(12) Uani 1 1 d . . . . .
H5 H 0.2121 0.8864 0.3765 0.061 Uiso 1 1 calc R . . . .
C3 C 0.0578(3) 0.7175(10) 0.3965(10) 0.0741(19) Uani 1 1 d . . . . .
H3 H 0.0123 0.7470 0.4193 0.089 Uiso 1 1 calc R . . . .
C2 C 0.0733(3) 0.5464(10) 0.3604(10) 0.0696(17) Uani 1 1 d . . . . .
H2 H 0.0376 0.4611 0.3510 0.083 Uiso 1 1 calc R . . . .
C8 C 0.3163(3) 0.5260(8) 0.4800(8) 0.0551(13) Uani 1 1 d . . . . .
H8A H 0.3209 0.6227 0.5638 0.066 Uiso 1 1 calc R . . . .
H8B H 0.2927 0.4297 0.5309 0.066 Uiso 1 1 calc R . . . .
C4 C 0.1093(4) 0.8450(9) 0.3989(9) 0.0684(16) Uani 1 1 d . . . . .
H4 H 0.0983 0.9619 0.4181 0.082 Uiso 1 1 calc R . . . .

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 0.0300(2) 0.0192(2) 0.0217(2) 0.00041(11) 0.00502(14) 0.00203(12)
Cl3 0.0523(6) 0.0247(4) 0.0281(5) 0.0086(3) 0.0082(4) 0.0001(4)
Cl2 0.0286(4) 0.0364(5) 0.0540(6) -0.0006(5) 0.0046(4) 0.0000(4)
Cl1 0.1232(18) 0.0516(10) 0.133(2) -0.0101(10) 0.0193(15) -0.0051(10)
N1 0.038(2) 0.0350(19) 0.055(2) 0.0009(17) 0.0017(17) 0.0049(15)
C1 0.056(3) 0.048(3) 0.064(4) 0.005(2) 0.009(3) -0.004(2)
C6 0.038(2) 0.052(3) 0.051(3) 0.007(2) 0.0028(19) 0.001(2)
C7 0.047(3) 0.074(4) 0.044(3) 0.013(3) 0.015(2) 0.006(3)
C5 0.048(3) 0.050(3) 0.053(3) 0.005(2) 0.002(2) -0.005(2)
C3 0.047(3) 0.093(5) 0.085(5) 0.014(4) 0.018(3) 0.012(3)
C2 0.045(3) 0.075(4) 0.090(5) 0.010(4) 0.013(3) -0.018(3)
C8 0.049(3) 0.064(3) 0.052(3) -0.002(2) 0.007(2) 0.014(2)
C4 0.070(4) 0.062(4) 0.072(4) 0.006(3) 0.008(3) 0.015(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 Cl3 2.7111(9) . ?
Cd1 Cl3 2.7159(9) 2_656 ?
Cd1 Cl3 2.7111(9) 3_656 ?
Cd1 Cl3 2.7159(9) 4 ?
Cd1 Cl2 2.4922(10) 3_656 ?
Cd1 Cl2 2.4923(10) . ?
Cl3 Cd1 2.7159(9) 2_646 ?
Cl1 C1 1.738(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C8 1.463(7) . ?
C1 C6 1.387(7) . ?
C1 C2 1.370(9) . ?
C6 C7 1.512(7) . ?
C6 C5 1.381(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.487(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.372(8) . ?
C3 H3 0.9300 . ?
C3 C2 1.370(10) . ?
C3 C4 1.370(10) . ?
C2 H2 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4 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
Cl3 Cd1 Cl3 180.0 . 3_656 ?
Cl3 Cd1 Cl3 180.0 2_656 4 ?
Cl3 Cd1 Cl3 90.487(8) 3_656 4 ?
Cl3 Cd1 Cl3 90.487(8) . 2_656 ?
Cl3 Cd1 Cl3 89.513(8) 3_656 2_656 ?
Cl3 Cd1 Cl3 89.513(8) . 4 ?
Cl2 Cd1 Cl3 89.72(3) 3_656 2_656 ?
Cl2 Cd1 Cl3 89.72(3) . 4 ?
Cl2 Cd1 Cl3 90.18(4) . 3_656 ?
Cl2 Cd1 Cl3 90.28(3) . 2_656 ?
Cl2 Cd1 Cl3 89.82(4) 3_656 3_656 ?
Cl2 Cd1 Cl3 90.18(4) 3_656 . ?
Cl2 Cd1 Cl3 89.82(4) . . ?
Cl2 Cd1 Cl3 90.28(3) 3_656 4 ?
Cl2 Cd1 Cl2 180.0 3_656 . ?
Cd1 Cl3 Cd1 166.58(5) . 2_646 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N1 H1A 109.5 . . ?
C8 N1 H1B 109.5 . . ?
C8 N1 H1C 109.5 . . ?
C6 C1 Cl1 119.5(5) . . ?
C2 C1 Cl1 118.5(5) . . ?
C2 C1 C6 121.7(5) . . ?
C1 C6 C7 122.9(5) . . ?
C5 C6 C1 117.0(5) . . ?
C5 C6 C7 120.0(5) . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 C6 111.7(4) . . ?
C8 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C5 H5 119.1 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 H5 119.1 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C4 C3 C2 120.0(6) . . ?
C1 C2 C3 119.6(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
N1 C8 C7 113.0(5) . . ?
N1 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4 120.2 . . ?

_shelx_res_file                  
;
    cd.res created by SHELXL-2014/7

TITL cd_a.res in P2(1)/c
REM Old TITL Cd in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.099, Rweak 0.001, Alpha 0.032, Orientation as input
REM Formula found by SHELXT: C14 N4 Cl6 Cd
CELL 0.71073 18.8581 7.603 7.6418 90 99.102 90
ZERR 2 0.0014 0.0006 0.0006 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cd Cl N
UNIT 32 44 2 12 4

L.S. 99
PLAN  20 0 0
SIZE 0.18 0.12 0.1
TEMP 20(2)
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\Cd.hkl">
REM </olex2.extras>

WGHT    0.045200    3.262600
FVAR       0.68619
CD1   3    0.500000    0.000000    0.500000    10.50000    0.02996    0.01922 =
         0.02168    0.00041    0.00502    0.00203
CL3   4    0.483043   -0.247058    0.745847    11.00000    0.05233    0.02471 =
         0.02811    0.00862    0.00825    0.00010
CL2   4    0.367845    0.051894    0.447391    11.00000    0.02862    0.03643 =
         0.05397   -0.00059    0.00463   -0.00004
CL1   4    0.158888    0.285641    0.284219    11.00000    0.12324    0.05157 =
         0.13251   -0.01013    0.01931   -0.00515
N1    5    0.388069    0.469305    0.454170    11.00000    0.03838    0.03505 =
         0.05519    0.00086    0.00171    0.00490
AFIX 137
H1A   2    0.384592    0.371943    0.388713    11.00000   -1.20000
H1B   2    0.414607    0.447713    0.558982    11.00000   -1.20000
H1C   2    0.408663    0.553779    0.399103    11.00000   -1.20000
AFIX   0
C1    1    0.141741    0.501941    0.338216    11.00000    0.05556    0.04768 =
         0.06420    0.00488    0.00950   -0.00375
C6    1    0.195334    0.627373    0.341452    11.00000    0.03844    0.05226 =
         0.05083    0.00678    0.00278    0.00134
C7    1    0.270780    0.582958    0.312717    11.00000    0.04693    0.07450 =
         0.04432    0.01296    0.01470    0.00599
AFIX  23
H7A   2    0.268912    0.489628    0.225564    11.00000   -1.20000
H7B   2    0.292236    0.685361    0.266331    11.00000   -1.20000
AFIX   0
C5    1    0.177276    0.799255    0.372883    11.00000    0.04837    0.04987 =
         0.05284    0.00516    0.00191   -0.00525
AFIX  43
H5    2    0.212103    0.886356    0.376517    11.00000   -1.20000
AFIX   0
C3    1    0.057834    0.717478    0.396460    11.00000    0.04747    0.09273 =
         0.08455    0.01359    0.01816    0.01226
AFIX  43
H3    2    0.012328    0.747042    0.419318    11.00000   -1.20000
AFIX   0
C2    1    0.073336    0.546443    0.360367    11.00000    0.04451    0.07529 =
         0.08966    0.00952    0.01295   -0.01788
AFIX  43
H2    2    0.037616    0.461073    0.350967    11.00000   -1.20000
AFIX   0
C8    1    0.316322    0.525977    0.479996    11.00000    0.04926    0.06398 =
         0.05172   -0.00246    0.00703    0.01401
AFIX  23
H8A   2    0.320869    0.622700    0.563801    11.00000   -1.20000
H8B   2    0.292692    0.429700    0.530949    11.00000   -1.20000
AFIX   0
C4    1    0.109341    0.844957    0.398888    11.00000    0.07043    0.06185 =
         0.07184    0.00560    0.00803    0.01478
AFIX  43
H4    2    0.098301    0.961890    0.418072    11.00000   -1.20000
AFIX   0
HKLF 4

REM  cd_a.res in P2(1)/c
REM R1 =  0.0403 for    2230 Fo > 4sig(Fo)  and  0.0447 for all    2470 data
REM    116 parameters refined using      0 restraints

END

WGHT      0.0452      3.2626

REM Highest difference peak  1.934,  deepest hole -0.589,  1-sigma level  0.121
Q1    1   0.5002  0.0010  0.7236  11.00000  0.05    1.93
Q2    1   0.1626  0.2854  0.4431  11.00000  0.05    1.19
Q3    1   0.4840 -0.2505  0.9844  11.00000  0.05    0.91
Q4    1   0.3690  0.0509  0.2331  11.00000  0.05    0.79
Q5    1   0.3169  0.5188  0.3641  11.00000  0.05    0.74
Q6    1   0.3696 -0.0432  0.4463  11.00000  0.05    0.59
Q7    1   0.2669  0.5828  0.5102  11.00000  0.05    0.54
Q8    1   0.1415  0.5195  0.1708  11.00000  0.05    0.43
Q9    1   0.1987  0.6174  0.4490  11.00000  0.05    0.43
Q10   1   0.1109  0.6585  0.5735  11.00000  0.05    0.42
Q11   1   0.0573  0.7196  0.2589  11.00000  0.05    0.42
Q12   1   0.4306 -0.0088  0.4174  11.00000  0.05    0.41
Q13   1   0.4417 -0.1285  0.6232  11.00000  0.05    0.38
Q14   1   0.1956  0.6251  0.1978  11.00000  0.05    0.38
Q15   1   0.0694  0.9477  0.5777  11.00000  0.05    0.37
Q16   1   0.1165  0.8392  0.2926  11.00000  0.05    0.37
Q17   1   0.1830  0.8054  0.1671  11.00000  0.05    0.36
Q18   1   0.5194 -0.2434  0.7593  11.00000  0.05    0.36
Q19   1   0.1773  0.7143  0.4375  11.00000  0.05    0.35
Q20   1   0.3161 -0.0513  0.4402  11.00000  0.05    0.31
;
_shelx_res_checksum              43805
_olex2_submission_special_instructions 'No special instructions were received'
