# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_aa
_database_code_depnum_ccdc_archive 'CCDC 1935646'
loop_
_audit_author_name
_audit_author_address
'Pengfei Hao'
;School of Chemical and Material Science, Shanxi Normal University
China
;
_audit_update_record             
;
2019-08-18 deposited with the CCDC.	2019-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H15 N6), Cd3 Cl12'
_chemical_formula_sum            'C36 H30 Cd3 Cl12 N12'
_chemical_formula_weight         1393.32

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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1   '
_symmetry_space_group_name_Hall  '-P 1  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8035(15)
_cell_length_b                   9.9473(16)
_cell_length_c                   13.347(2)
_cell_angle_alpha                84.524(3)
_cell_angle_beta                 79.160(3)
_cell_angle_gamma                64.263(3)
_cell_volume                     1151.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4209
_exptl_absorpt_correction_T_max  0.7021
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 'phi and omega scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17891
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         28.33
_reflns_number_total             5655
_reflns_number_gt                5261
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0278P)²+0.8489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5655
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0598
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.0000 1.0000 0.5000 0.02523(5) Uani 1 2 d S . .
Cd2 Cd 0.901843(19) 0.803581(16) 0.767196(12) 0.03181(5) Uani 1 1 d . . .
Cl1 Cl 0.98353(6) 0.77974(5) 0.41882(4) 0.02851(10) Uani 1 1 d . . .
Cl2 Cl 0.81780(7) 1.18142(6) 0.37510(4) 0.03502(11) Uani 1 1 d . . .
Cl3 Cl 0.76802(5) 1.02399(5) 0.64989(3) 0.02736(9) Uani 1 1 d . . .
Cl4 Cl 1.01162(6) 0.54325(6) 0.71782(4) 0.03560(12) Uani 1 1 d . . .
Cl5 Cl 0.64442(7) 0.84655(7) 0.87267(5) 0.04325(13) Uani 1 1 d . . .
Cl6 Cl 1.01707(6) 0.86615(6) 0.89273(4) 0.03330(11) Uani 1 1 d . . .
C1 C 0.4670(2) 0.5220(2) 0.74029(13) 0.0213(3) Uani 1 1 d . . .
C2 C 0.3429(2) 0.5534(2) 0.90213(13) 0.0218(3) Uani 1 1 d . . .
C3 C 0.3494(2) 0.3756(2) 0.80696(13) 0.0215(3) Uani 1 1 d . . .
C4 C 0.5684(2) 0.5586(2) 0.65585(13) 0.0218(3) Uani 1 1 d . . .
C5 C 0.6364(2) 0.4684(2) 0.57119(14) 0.0267(4) Uani 1 1 d . . .
H5 H 0.6137 0.3884 0.5647 0.032 Uiso 1 1 calc R . .
C6 C 0.7381(2) 0.4985(2) 0.49652(15) 0.0297(4) Uani 1 1 d . . .
H6 H 0.7852 0.4384 0.4395 0.036 Uiso 1 1 calc R . .
C7 C 0.7053(3) 0.7038(2) 0.58746(16) 0.0315(4) Uani 1 1 d . . .
H7 H 0.7301 0.7831 0.5917 0.038 Uiso 1 1 calc R . .
C8 C 0.6034(2) 0.6783(2) 0.66413(15) 0.0286(4) Uani 1 1 d . . .
H8 H 0.5586 0.7400 0.7205 0.034 Uiso 1 1 calc R . .
C9 C 0.3005(2) 0.6289(2) 1.00205(13) 0.0221(3) Uani 1 1 d . . .
C10 C 0.3508(2) 0.7361(2) 1.01431(15) 0.0257(4) Uani 1 1 d . . .
H10 H 0.4117 0.7610 0.9606 0.031 Uiso 1 1 calc R . .
C11 C 0.3095(2) 0.8052(2) 1.10697(16) 0.0295(4) Uani 1 1 d . . .
H11 H 0.3414 0.8780 1.1162 0.035 Uiso 1 1 calc R . .
C12 C 0.1749(3) 0.6621(2) 1.17540(15) 0.0316(4) Uani 1 1 d . . .
H12 H 0.1160 0.6381 1.2310 0.038 Uiso 1 1 calc R . .
C13 C 0.2129(2) 0.5898(2) 1.08423(15) 0.0289(4) Uani 1 1 d . . .
H13 H 0.1807 0.5163 1.0776 0.035 Uiso 1 1 calc R . .
C14 C 0.3132(2) 0.2479(2) 0.79670(14) 0.0225(3) Uani 1 1 d . . .
C15 C 0.2324(3) 0.2017(2) 0.87900(16) 0.0327(4) Uani 1 1 d . . .
H15 H 0.2042 0.2476 0.9419 0.039 Uiso 1 1 calc R . .
C16 C 0.1951(3) 0.0871(3) 0.86569(17) 0.0363(5) Uani 1 1 d . . .
H16 H 0.1408 0.0551 0.9198 0.044 Uiso 1 1 calc R . .
C17 C 0.3176(2) 0.0600(2) 0.69562(16) 0.0306(4) Uani 1 1 d . . .
H17 H 0.3452 0.0109 0.6341 0.037 Uiso 1 1 calc R . .
C18 C 0.3602(2) 0.1725(2) 0.70509(15) 0.0264(4) Uani 1 1 d . . .
H18 H 0.4198 0.1978 0.6507 0.032 Uiso 1 1 calc R . .
N1 N 0.42471(19) 0.59830(18) 0.82651(12) 0.0245(3) Uani 1 1 d . . .
N2 N 0.30141(18) 0.44333(18) 0.89681(12) 0.0241(3) Uani 1 1 d . . .
N3 N 0.43284(18) 0.40991(18) 0.72609(12) 0.0237(3) Uani 1 1 d . . .
N4 N 0.2363(2) 0.0221(2) 0.77567(14) 0.0312(4) Uani 1 1 d . . .
H4 H 0.2094 -0.0476 0.7686 0.037 Uiso 1 1 calc R . .
N5 N 0.2230(2) 0.76681(19) 1.18361(13) 0.0301(4) Uani 1 1 d . . .
H5A H 0.1972 0.8116 1.2408 0.036 Uiso 1 1 calc R . .
N6 N 0.76838(19) 0.6142(2) 0.50681(13) 0.0286(3) Uani 1 1 d . . .
H6A H 0.8313 0.6321 0.4595 0.034 Uiso 1 1 calc R . .


_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 2.6128(5) 2_776 ?
Cd1 Cl1 2.6128(6) . ?
Cd1 Cl2 2.6406(6) 2_776 ?
Cd1 Cl2 2.6406(6) . ?
Cd1 Cl3 2.6721(5) . ?
Cd1 Cl3 2.6721(5) 2_776 ?
Cd2 Cl4 2.4367(6) . ?
Cd2 Cl6 2.4479(6) . ?
Cd2 Cl5 2.5249(7) . ?
Cd2 Cl3 2.5688(6) . ?
C1 N3 1.335(2) . ?
C1 N1 1.336(2) . ?
C1 C4 1.485(2) . ?
C2 N1 1.335(2) . ?
C2 N2 1.335(2) . ?
C2 C9 1.492(2) . ?
C3 N2 1.334(2) . ?
C3 N3 1.338(2) . ?
C3 C14 1.484(2) . ?
C4 C5 1.385(3) . ?
C4 C8 1.393(3) . ?
C5 C6 1.381(3) . ?
C5 H5 0.9300 . ?
C6 N6 1.331(3) . ?
C6 H6 0.9300 . ?
C7 N6 1.338(3) . ?
C7 C8 1.377(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.390(3) . ?
C9 C13 1.395(3) . ?
C10 C11 1.378(3) . ?
C10 H10 0.9300 . ?
C11 N5 1.339(3) . ?
C11 H11 0.9300 . ?
C12 N5 1.337(3) . ?
C12 C13 1.378(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C18 1.390(3) . ?
C14 C15 1.391(3) . ?
C15 C16 1.375(3) . ?
C15 H15 0.9300 . ?
C16 N4 1.328(3) . ?
C16 H16 0.9300 . ?
C17 N4 1.335(3) . ?
C17 C18 1.376(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
N4 H4 0.8600 . ?
N5 H5A 0.8600 . ?
N6 H6A 0.8600 . ?

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 180.000(1) 2_776 . ?
Cl1 Cd1 Cl2 87.589(19) 2_776 2_776 ?
Cl1 Cd1 Cl2 92.411(19) . 2_776 ?
Cl1 Cd1 Cl2 92.411(19) 2_776 . ?
Cl1 Cd1 Cl2 87.589(18) . . ?
Cl2 Cd1 Cl2 180.000(1) 2_776 . ?
Cl1 Cd1 Cl3 88.222(16) 2_776 . ?
Cl1 Cd1 Cl3 91.778(16) . . ?
Cl2 Cd1 Cl3 86.25(2) 2_776 . ?
Cl2 Cd1 Cl3 93.75(2) . . ?
Cl1 Cd1 Cl3 91.778(16) 2_776 2_776 ?
Cl1 Cd1 Cl3 88.222(16) . 2_776 ?
Cl2 Cd1 Cl3 93.75(2) 2_776 2_776 ?
Cl2 Cd1 Cl3 86.25(2) . 2_776 ?
Cl3 Cd1 Cl3 180.000(1) . 2_776 ?
Cl4 Cd2 Cl6 117.28(2) . . ?
Cl4 Cd2 Cl5 104.02(2) . . ?
Cl6 Cd2 Cl5 99.71(2) . . ?
Cl4 Cd2 Cl3 123.59(2) . . ?
Cl6 Cd2 Cl3 113.51(2) . . ?
Cl5 Cd2 Cl3 89.79(2) . . ?
Cd2 Cl3 Cd1 101.493(19) . . ?
N3 C1 N1 125.22(16) . . ?
N3 C1 C4 117.36(15) . . ?
N1 C1 C4 117.30(16) . . ?
N1 C2 N2 125.50(16) . . ?
N1 C2 C9 116.84(16) . . ?
N2 C2 C9 117.61(15) . . ?
N2 C3 N3 125.26(16) . . ?
N2 C3 C14 117.67(15) . . ?
N3 C3 C14 117.03(16) . . ?
C5 C4 C8 119.55(17) . . ?
C5 C4 C1 120.11(16) . . ?
C8 C4 C1 120.22(16) . . ?
C6 C5 C4 119.32(18) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
N6 C6 C5 119.48(18) . . ?
N6 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N6 C7 C8 119.77(18) . . ?
N6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C4 118.88(18) . . ?
C7 C8 H8 120.6 . . ?
C4 C8 H8 120.6 . . ?
C10 C9 C13 119.66(17) . . ?
C10 C9 C2 120.12(16) . . ?
C13 C9 C2 120.20(16) . . ?
C11 C10 C9 119.20(18) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
N5 C11 C10 119.48(18) . . ?
N5 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N5 C12 C13 119.71(18) . . ?
N5 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C9 118.85(18) . . ?
C12 C13 H13 120.6 . . ?
C9 C13 H13 120.6 . . ?
C18 C14 C15 119.27(17) . . ?
C18 C14 C3 120.46(16) . . ?
C15 C14 C3 120.27(17) . . ?
C16 C15 C14 118.80(19) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
N4 C16 C15 120.11(19) . . ?
N4 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
N4 C17 C18 119.33(18) . . ?
N4 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C14 119.35(18) . . ?
C17 C18 H18 120.3 . . ?
C14 C18 H18 120.3 . . ?
C2 N1 C1 114.64(16) . . ?
C3 N2 C2 114.62(15) . . ?
C1 N3 C3 114.77(15) . . ?
C16 N4 C17 123.01(18) . . ?
C16 N4 H4 118.5 . . ?
C17 N4 H4 118.5 . . ?
C12 N5 C11 123.07(17) . . ?
C12 N5 H5A 118.5 . . ?
C11 N5 H5A 118.5 . . ?
C6 N6 C7 123.00(17) . . ?
C6 N6 H6A 118.5 . . ?
C7 N6 H6A 118.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C6 H6 Cl2 0.93 2.64 3.398(2) 138.8 1_545
C6 H6 Cl4 0.93 2.66 3.328(2) 129.3 2_766
C7 H7 Cl3 0.93 2.78 3.690(2) 166.8 .
C8 H8 Cl5 0.93 2.79 3.550(2) 139.7 .
C10 H10 Cl5 0.93 2.79 3.656(2) 155.1 .
C11 H11 Cl5 0.93 2.82 3.723(2) 163.4 2_677
C12 H12 Cl1 0.93 2.80 3.460(2) 129.2 1_456
C12 H12 Cl4 0.93 2.59 3.354(2) 140.3 2_667
C15 H15 Cl5 0.93 2.99 3.657(2) 129.9 2_667
C16 H16 Cl6 0.93 2.72 3.309(2) 121.9 1_445
C16 H16 Cl6 0.93 2.67 3.444(2) 141.0 2_667
N4 H4 Cl2 0.86 2.55 3.2468(18) 138.6 2_666
N4 H4 Cl6 0.86 2.64 3.2616(18) 129.7 1_445
N5 H5A Cl1 0.86 2.95 3.5250(18) 126.2 1_456
N5 H5A Cl3 0.86 2.46 3.2237(18) 148.5 2_677
N6 H6A Cl1 0.86 2.47 3.2026(17) 142.9 .
N6 H6A Cl4 0.86 2.85 3.4093(18) 124.7 2_766

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.088
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_aa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1947057'
loop_
_audit_author_name
_audit_author_address
'Pengfei Hao'
;School of Chemical and Material Science, Shanxi Normal University
China
;
_audit_update_record             
;
2019-08-18 deposited with the CCDC.	2019-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H15 N6), Cd3 Cl12'
_chemical_formula_sum            'C36 H30 Cd3 Cl12 N12'
_chemical_formula_weight         1393.32

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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1   '
_symmetry_space_group_name_Hall  '-P 1  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.819(4)
_cell_length_b                   9.940(4)
_cell_length_c                   13.353(6)
_cell_angle_alpha                84.328(8)
_cell_angle_beta                 79.004(7)
_cell_angle_gamma                64.141(7)
_cell_volume                     1151.0(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9718
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3941
_exptl_absorpt_correction_T_max  0.6783
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16637
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         28.33
_reflns_number_total             5510
_reflns_number_gt                5305
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0247P)²+1.3816P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5510
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.0000 1.0000 0.5000 0.02390(6) Uani 1 2 d S . .
Cd2 Cd 0.90272(2) 0.803331(18) 0.766905(13) 0.03017(6) Uani 1 1 d . . .
Cl1 Cl 1.01639(7) 1.22026(6) 0.58082(4) 0.02716(11) Uani 1 1 d . . .
Cl2 Cl 0.81815(8) 1.18140(6) 0.37495(5) 0.03347(13) Uani 1 1 d . . .
Cl3 Cl 0.76807(6) 1.02415(6) 0.65020(4) 0.02615(11) Uani 1 1 d . . .
Cl4 Cl 1.01207(7) 0.54285(6) 0.71752(5) 0.03415(13) Uani 1 1 d . . .
Cl5 Cl 0.64516(8) 0.84618(9) 0.87249(5) 0.04152(15) Uani 1 1 d . . .
Cl6 Cl 1.01734(7) 0.86594(7) 0.89253(4) 0.03178(12) Uani 1 1 d . . .
C1 C 0.4670(2) 0.5222(2) 0.74092(15) 0.0205(4) Uani 1 1 d . . .
C2 C 0.3422(2) 0.5538(2) 0.90258(15) 0.0206(4) Uani 1 1 d . . .
C3 C 0.3492(2) 0.3757(2) 0.80745(15) 0.0204(4) Uani 1 1 d . . .
C4 C 0.5684(2) 0.5588(2) 0.65629(15) 0.0202(4) Uani 1 1 d . . .
C5 C 0.6358(3) 0.4687(2) 0.57160(16) 0.0249(4) Uani 1 1 d . . .
H5 H 0.6127 0.3889 0.5652 0.030 Uiso 1 1 calc R . .
C6 C 0.7378(3) 0.4985(3) 0.49674(17) 0.0284(5) Uani 1 1 d . . .
H6 H 0.7848 0.4384 0.4397 0.034 Uiso 1 1 calc R . .
C7 C 0.7055(3) 0.7036(3) 0.58783(18) 0.0302(5) Uani 1 1 d . . .
H7 H 0.7306 0.7827 0.5920 0.036 Uiso 1 1 calc R . .
C8 C 0.6039(3) 0.6781(3) 0.66463(17) 0.0279(5) Uani 1 1 d . . .
H8 H 0.5596 0.7395 0.7212 0.033 Uiso 1 1 calc R . .
C9 C 0.3003(2) 0.6289(2) 1.00230(15) 0.0207(4) Uani 1 1 d . . .
C10 C 0.3510(3) 0.7363(2) 1.01443(17) 0.0247(4) Uani 1 1 d . . .
H10 H 0.4121 0.7610 0.9607 0.030 Uiso 1 1 calc R . .
C11 C 0.3093(3) 0.8054(3) 1.10714(18) 0.0279(4) Uani 1 1 d . . .
H11 H 0.3408 0.8783 1.1163 0.033 Uiso 1 1 calc R . .
C12 C 0.1748(3) 0.6623(3) 1.17559(17) 0.0303(5) Uani 1 1 d . . .
H12 H 0.1157 0.6386 1.2312 0.036 Uiso 1 1 calc R . .
C13 C 0.2128(3) 0.5898(3) 1.08445(17) 0.0272(4) Uani 1 1 d . . .
H13 H 0.1806 0.5163 1.0780 0.033 Uiso 1 1 calc R . .
C14 C 0.3128(2) 0.2482(2) 0.79720(16) 0.0216(4) Uani 1 1 d . . .
C15 C 0.2322(3) 0.2021(3) 0.87944(18) 0.0313(5) Uani 1 1 d . . .
H15 H 0.2041 0.2479 0.9423 0.038 Uiso 1 1 calc R . .
C16 C 0.1947(3) 0.0874(3) 0.8663(2) 0.0352(5) Uani 1 1 d . . .
H16 H 0.1405 0.0552 0.9205 0.042 Uiso 1 1 calc R . .
C17 C 0.3168(3) 0.0606(3) 0.69625(19) 0.0297(5) Uani 1 1 d . . .
H17 H 0.3442 0.0117 0.6347 0.036 Uiso 1 1 calc R . .
C18 C 0.3599(3) 0.1729(3) 0.70536(17) 0.0255(4) Uani 1 1 d . . .
H18 H 0.4197 0.1981 0.6509 0.031 Uiso 1 1 calc R . .
N1 N 0.4245(2) 0.5985(2) 0.82687(14) 0.0236(4) Uani 1 1 d . . .
N2 N 0.3010(2) 0.4439(2) 0.89727(13) 0.0228(3) Uani 1 1 d . . .
N3 N 0.4325(2) 0.4102(2) 0.72656(14) 0.0225(3) Uani 1 1 d . . .
N4 N 0.2358(2) 0.0226(2) 0.77612(16) 0.0304(4) Uani 1 1 d . . .
H4 H 0.2088 -0.0470 0.7691 0.036 Uiso 1 1 calc R . .
N5 N 0.2231(2) 0.7667(2) 1.18363(15) 0.0288(4) Uani 1 1 d . . .
H5A H 0.1975 0.8111 1.2409 0.035 Uiso 1 1 calc R . .
N6 N 0.7681(2) 0.6145(2) 0.50710(15) 0.0272(4) Uani 1 1 d . . .
H6A H 0.8308 0.6327 0.4596 0.033 Uiso 1 1 calc R . .


_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 2.6124(10) 2_776 ?
Cd1 Cl1 2.6124(10) . ?
Cd1 Cl2 2.6385(9) . ?
Cd1 Cl2 2.6385(9) 2_776 ?
Cd1 Cl3 2.6724(10) 2_776 ?
Cd1 Cl3 2.6724(10) . ?
Cd2 Cl4 2.4360(11) . ?
Cd2 Cl6 2.4506(9) . ?
Cd2 Cl5 2.5266(11) . ?
Cd2 Cl3 2.5638(9) . ?
C1 N1 1.334(3) . ?
C1 N3 1.336(3) . ?
C1 C4 1.485(3) . ?
C2 N2 1.332(3) . ?
C2 N1 1.336(3) . ?
C2 C9 1.490(3) . ?
C3 N2 1.337(3) . ?
C3 N3 1.337(3) . ?
C3 C14 1.484(3) . ?
C4 C5 1.385(3) . ?
C4 C8 1.394(3) . ?
C5 C6 1.381(3) . ?
C5 H5 0.9300 . ?
C6 N6 1.335(3) . ?
C6 H6 0.9300 . ?
C7 N6 1.336(3) . ?
C7 C8 1.375(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.393(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.379(3) . ?
C10 H10 0.9300 . ?
C11 N5 1.336(3) . ?
C11 H11 0.9300 . ?
C12 N5 1.335(3) . ?
C12 C13 1.380(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.388(3) . ?
C14 C18 1.393(3) . ?
C15 C16 1.378(3) . ?
C15 H15 0.9300 . ?
C16 N4 1.330(3) . ?
C16 H16 0.9300 . ?
C17 N4 1.332(3) . ?
C17 C18 1.377(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
N4 H4 0.8600 . ?
N5 H5A 0.8600 . ?
N6 H6A 0.8600 . ?

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 2_776 . ?
Cl1 Cd1 Cl2 87.44(3) 2_776 . ?
Cl1 Cd1 Cl2 92.56(3) . . ?
Cl1 Cd1 Cl2 92.56(3) 2_776 2_776 ?
Cl1 Cd1 Cl2 87.44(3) . 2_776 ?
Cl2 Cd1 Cl2 180.0 . 2_776 ?
Cl1 Cd1 Cl3 88.21(3) 2_776 2_776 ?
Cl1 Cd1 Cl3 91.79(3) . 2_776 ?
Cl2 Cd1 Cl3 86.19(4) . 2_776 ?
Cl2 Cd1 Cl3 93.81(4) 2_776 2_776 ?
Cl1 Cd1 Cl3 91.79(3) 2_776 . ?
Cl1 Cd1 Cl3 88.21(3) . . ?
Cl2 Cd1 Cl3 93.81(4) . . ?
Cl2 Cd1 Cl3 86.19(4) 2_776 . ?
Cl3 Cd1 Cl3 180.0 2_776 . ?
Cl4 Cd2 Cl6 117.50(3) . . ?
Cl4 Cd2 Cl5 103.86(3) . . ?
Cl6 Cd2 Cl5 99.69(4) . . ?
Cl4 Cd2 Cl3 123.54(3) . . ?
Cl6 Cd2 Cl3 113.52(3) . . ?
Cl5 Cd2 Cl3 89.55(3) . . ?
Cd2 Cl3 Cd1 101.26(3) . . ?
N1 C1 N3 125.38(19) . . ?
N1 C1 C4 117.28(18) . . ?
N3 C1 C4 117.24(18) . . ?
N2 C2 N1 125.41(19) . . ?
N2 C2 C9 117.78(18) . . ?
N1 C2 C9 116.74(18) . . ?
N2 C3 N3 125.03(19) . . ?
N2 C3 C14 117.88(18) . . ?
N3 C3 C14 117.05(18) . . ?
C5 C4 C8 119.66(19) . . ?
C5 C4 C1 120.02(19) . . ?
C8 C4 C1 120.19(19) . . ?
C6 C5 C4 119.3(2) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
N6 C6 C5 119.3(2) . . ?
N6 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N6 C7 C8 119.8(2) . . ?
N6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C4 118.8(2) . . ?
C7 C8 H8 120.6 . . ?
C4 C8 H8 120.6 . . ?
C13 C9 C10 119.70(19) . . ?
C13 C9 C2 120.10(19) . . ?
C10 C9 C2 120.19(18) . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
N5 C11 C10 119.4(2) . . ?
N5 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N5 C12 C13 119.8(2) . . ?
N5 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C9 118.7(2) . . ?
C12 C13 H13 120.7 . . ?
C9 C13 H13 120.7 . . ?
C15 C14 C18 119.4(2) . . ?
C15 C14 C3 120.20(19) . . ?
C18 C14 C3 120.44(19) . . ?
C16 C15 C14 118.8(2) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
N4 C16 C15 120.1(2) . . ?
N4 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
N4 C17 C18 119.6(2) . . ?
N4 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C14 119.1(2) . . ?
C17 C18 H18 120.4 . . ?
C14 C18 H18 120.4 . . ?
C1 N1 C2 114.58(18) . . ?
C2 N2 C3 114.87(18) . . ?
C1 N3 C3 114.72(18) . . ?
C16 N4 C17 122.9(2) . . ?
C16 N4 H4 118.5 . . ?
C17 N4 H4 118.5 . . ?
C12 N5 C11 123.2(2) . . ?
C12 N5 H5A 118.4 . . ?
C11 N5 H5A 118.4 . . ?
C6 N6 C7 123.07(19) . . ?
C6 N6 H6A 118.5 . . ?
C7 N6 H6A 118.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H6A Cl4 0.86 2.84 3.408(2) 124.6 2_766
N6 H6A Cl1 0.86 2.48 3.203(2) 142.8 2_776
N5 H5A Cl3 0.86 2.46 3.224(2) 148.4 2_677
N5 H5A Cl1 0.86 2.95 3.526(2) 126.3 2_677
N4 H4 Cl6 0.86 2.64 3.256(2) 129.9 1_445
N4 H4 Cl2 0.86 2.56 3.258(2) 138.7 2_666
C16 H16 Cl6 0.93 2.66 3.437(3) 141.0 2_667
C16 H16 Cl6 0.93 2.73 3.310(3) 121.5 1_445
C15 H15 Cl5 0.93 2.99 3.655(3) 130.1 2_667
C12 H12 Cl4 0.93 2.59 3.354(3) 140.1 2_667
C12 H12 Cl1 0.93 2.80 3.461(3) 129.3 2_677
C11 H11 Cl5 0.93 2.82 3.722(3) 163.6 2_677
C10 H10 Cl5 0.93 2.79 3.659(3) 155.1 .
C8 H8 Cl5 0.93 2.79 3.549(3) 139.9 .
C7 H7 Cl3 0.93 2.78 3.695(3) 166.7 .
C6 H6 Cl4 0.93 2.66 3.326(2) 129.2 2_766
C6 H6 Cl2 0.93 2.64 3.399(3) 139.0 1_545

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.083
_chemical_properties_physical    Light-sensitive,Photo-sensitive
