# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1413432'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H16 N6 O6 Zn'
_chemical_formula_weight         477.74

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.519(2)
_cell_length_b                   9.8960(17)
_cell_length_c                   14.609(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.259(3)
_cell_angle_gamma                90.00
_cell_volume                     1808.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle-like
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_T_max  0.8954
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3830
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1754
_reflns_number_gt                1478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'

_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)+(0.0602P)²+2.4780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1754
_refine_ls_number_parameters     150
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn 0.0000 0.41884(5) 0.2500 0.0375(2) Uani 1 2 d S . .
N3 N 0.64479(19) 0.4359(2) 0.40392(18) 0.0288(6) Uani 1 1 d . . .
N2 N 0.80885(19) 0.3808(3) 0.4255(2) 0.0379(6) Uani 1 1 d . . .
N1 N 0.8082(2) 0.5124(3) 0.4564(2) 0.0406(7) Uani 1 1 d . . .
C1 C 0.1955(2) 0.4226(3) 0.3087(2) 0.0309(7) Uani 1 1 d . . .
C2 C 0.3145(2) 0.4261(3) 0.3355(2) 0.0300(7) Uani 1 1 d . . .
C3 C 0.3658(2) 0.5471(3) 0.3376(2) 0.0344(7) Uani 1 1 d . . .
H3A H 0.3270 0.6272 0.3246 0.041 Uiso 1 1 calc R . .
C4 C 0.4748(2) 0.5500(3) 0.3589(3) 0.0348(7) Uani 1 1 d . . .
H4A H 0.5090 0.6315 0.3589 0.042 Uiso 1 1 calc R . .
C5 C 0.5320(2) 0.4309(3) 0.3800(2) 0.0273(6) Uani 1 1 d . . .
C6 C 0.4820(2) 0.3084(3) 0.3783(2) 0.0332(7) Uani 1 1 d . . .
H6A H 0.5212 0.2285 0.3927 0.040 Uiso 1 1 calc R . .
C7 C 0.3727(2) 0.3064(3) 0.3551(2) 0.0329(7) Uani 1 1 d . . .
H7A H 0.3381 0.2245 0.3525 0.039 Uiso 1 1 calc R . .
C8 C 0.7116(2) 0.5427(4) 0.4430(3) 0.0384(7) Uani 1 1 d . . .
H8A H 0.6898 0.6262 0.4578 0.046 Uiso 1 1 calc R . .
C9 C 0.7112(2) 0.3375(3) 0.3945(2) 0.0343(7) Uani 1 1 d . . .
H9A H 0.6893 0.2515 0.3693 0.041 Uiso 1 1 calc R . .
O1 O 0.14389(16) 0.5320(2) 0.29495(18) 0.0392(5) Uani 1 1 d U . .
O2 O 0.14964(16) 0.3105(2) 0.29931(17) 0.0370(5) Uani 1 1 d . . .
O1W' O 0.0017(14) 0.4096(19) 0.3993(13) 0.046(3) Uani 0.50 1 d P . .
O1W O 0.0086(15) 0.3793(15) 0.3878(13) 0.036(2) Uani 0.50 1 d P . .
H1WA H 0.0503 0.4168 0.4407 0.043 Uiso 1 1 d R . .
H1WB H -0.0544 0.3813 0.3970 0.043 Uiso 1 1 d 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
Zn1 O1W 2.010(16) 2 ?
Zn1 O1W 2.010(16) . ?
Zn1 O1 2.121(2) . ?
Zn1 O1 2.121(2) 2 ?
Zn1 O2 2.158(2) 2 ?
Zn1 O2 2.158(2) . ?
Zn1 O1W' 2.174(17) . ?
Zn1 O1W' 2.174(17) 2 ?
Zn1 C1 2.451(3) . ?
Zn1 C1 2.451(3) 2 ?
N3 C9 1.366(4) . ?
N3 C8 1.367(4) . ?
N3 C5 1.431(4) . ?
N2 C9 1.296(4) . ?
N2 N1 1.380(4) . ?
N1 C8 1.280(4) . ?
C1 O2 1.253(3) . ?
C1 O1 1.262(4) . ?
C1 C2 1.506(4) . ?
C2 C3 1.378(4) . ?
C2 C7 1.390(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.384(4) . ?
C6 C7 1.385(4) . ?

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
O1W Zn1 O1W 157.5(8) 2 . ?
O1W Zn1 O1 96.4(5) 2 . ?
O1W Zn1 O1 95.4(5) . . ?
O1W Zn1 O1 95.4(5) 2 2 ?
O1W Zn1 O1 96.4(5) . 2 ?
O1 Zn1 O1 116.31(12) . 2 ?
O1W Zn1 O2 83.0(5) 2 2 ?
O1W Zn1 O2 85.9(5) . 2 ?
O1 Zn1 O2 177.72(8) . 2 ?
O1 Zn1 O2 61.65(9) 2 2 ?
O1W Zn1 O2 85.9(5) 2 . ?
O1W Zn1 O2 83.0(5) . . ?
O1 Zn1 O2 61.65(9) . . ?
O1 Zn1 O2 177.72(8) 2 . ?
O2 Zn1 O2 120.41(11) 2 . ?
O1W Zn1 O1W' 166.1(3) 2 . ?
O1W Zn1 O1W' 9.2(8) . . ?
O1 Zn1 O1W' 93.0(5) . . ?
O1 Zn1 O1W' 89.6(4) 2 . ?
O2 Zn1 O1W' 88.1(5) 2 . ?
O2 Zn1 O1W' 89.5(4) . . ?
O1W Zn1 O1W' 9.2(8) 2 2 ?
O1W Zn1 O1W' 166.1(3) . 2 ?
O1 Zn1 O1W' 89.6(5) . 2 ?
O1 Zn1 O1W' 93.0(5) 2 2 ?
O2 Zn1 O1W' 89.5(4) 2 2 ?
O2 Zn1 O1W' 88.1(5) . 2 ?
O1W' Zn1 O1W' 175.2(10) . 2 ?
O1W Zn1 C1 89.9(5) 2 . ?
O1W Zn1 C1 90.4(5) . . ?
O1 Zn1 C1 30.98(9) . . ?
O1 Zn1 C1 147.26(9) 2 . ?
O2 Zn1 C1 151.03(9) 2 . ?
O2 Zn1 C1 30.73(8) . . ?
O1W' Zn1 C1 92.8(5) . . ?
O1W' Zn1 C1 87.2(5) 2 . ?
O1W Zn1 C1 90.4(5) 2 2 ?
O1W Zn1 C1 89.9(5) . 2 ?
O1 Zn1 C1 147.26(9) . 2 ?
O1 Zn1 C1 30.98(9) 2 2 ?
O2 Zn1 C1 30.73(8) 2 2 ?
O2 Zn1 C1 151.03(9) . 2 ?
O1W' Zn1 C1 87.2(5) . 2 ?
O1W' Zn1 C1 92.8(5) 2 2 ?
C1 Zn1 C1 178.24(14) . 2 ?
C9 N3 C8 103.8(3) . . ?
C9 N3 C5 129.2(2) . . ?
C8 N3 C5 127.1(3) . . ?
C9 N2 N1 107.1(2) . . ?
C8 N1 N2 107.7(3) . . ?
O2 C1 O1 121.4(3) . . ?
O2 C1 C2 119.0(3) . . ?
O1 C1 C2 119.6(3) . . ?
O2 C1 Zn1 61.62(15) . . ?
O1 C1 Zn1 59.94(15) . . ?
C2 C1 Zn1 175.0(2) . . ?
C3 C2 C7 119.7(3) . . ?
C3 C2 C1 120.3(3) . . ?
C7 C2 C1 120.0(3) . . ?
C2 C3 C4 120.4(3) . . ?
C5 C4 C3 119.4(3) . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 N3 118.7(3) . . ?
C6 C5 N3 120.2(3) . . ?
C5 C6 C7 119.0(3) . . ?
C6 C7 C2 120.4(3) . . ?
N1 C8 N3 110.9(3) . . ?
N2 C9 N3 110.5(3) . . ?
C1 O1 Zn1 89.08(18) . . ?
C1 O2 Zn1 87.65(17) . . ?

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
O1W' H1WA N1 0.71 2.06 2.746(17) 164.5 5_666
O1W' H1WB N2 0.80 2.04 2.790(17) 155.8 1_455
C4 H4A O1W 0.93 2.49 3.295(15) 145.3 3
C9 H9A O1 0.93 2.40 3.329(4) 174.3 3_545

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1413435'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_2                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......  0.96 Note  
RESPONSE: Because the sample is thin and long (0.32, 0.04 0.03), the 
diffraction pattern quality was poor at high angle.  
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Cl N3 O3 Zn'
_chemical_formula_weight         321.03

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.097(3)
_cell_length_b                   17.622(5)
_cell_length_c                   7.464(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.337(6)
_cell_angle_gamma                90.00
_cell_volume                     1195.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle-like
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    2.280
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5290
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4902
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2017
_reflns_number_gt                1681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'

_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)+(0.0664P)²+1.1544P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2017
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn -0.17575(6) 0.04815(3) 0.11942(8) 0.0258(2) Uani 1 1 d . . .
N1 N 0.0477(4) 0.0706(2) 0.1505(6) 0.0261(9) Uani 1 1 d . . .
N2 N 0.1664(4) 0.0286(2) 0.0916(6) 0.0274(10) Uani 1 1 d . . .
N3 N 0.2502(4) 0.1235(2) 0.2524(5) 0.0230(9) Uani 1 1 d . . .
O1 O 0.6114(4) 0.4171(2) 0.4980(6) 0.0474(11) Uani 1 1 d . . .
O3 O 0.9809(5) 0.2864(3) 0.0664(6) 0.0531(12) Uani 1 1 d . . .
H3 H 0.9163 0.2544 0.0756 0.080 Uiso 1 1 calc R . .
O2 O 0.7736(4) 0.3326(2) 0.5834(6) 0.0451(11) Uani 1 1 d . . .
C1 C 0.6500(6) 0.3492(3) 0.5143(7) 0.0349(13) Uani 1 1 d . . .
C2 C 0.5463(5) 0.2880(3) 0.4503(7) 0.0273(11) Uani 1 1 d . . .
C3 C 0.5789(5) 0.2119(3) 0.4702(7) 0.0310(12) Uani 1 1 d . . .
H3A H 0.6682 0.1976 0.5251 0.037 Uiso 1 1 calc R . .
C4 C 0.4816(5) 0.1570(3) 0.4103(7) 0.0278(11) Uani 1 1 d . . .
H4A H 0.5036 0.1058 0.4249 0.033 Uiso 1 1 calc R . .
C5 C 0.3508(5) 0.1798(3) 0.3281(6) 0.0221(10) Uani 1 1 d . . .
C6 C 0.3151(5) 0.2550(3) 0.3025(7) 0.0267(11) Uani 1 1 d . . .
H6A H 0.2269 0.2687 0.2441 0.032 Uiso 1 1 calc R . .
C7 C 0.4135(5) 0.3097(3) 0.3657(7) 0.0293(12) Uani 1 1 d . . .
H7A H 0.3909 0.3608 0.3517 0.035 Uiso 1 1 calc R . .
C8 C 0.1020(5) 0.1261(3) 0.2472(7) 0.0274(11) Uani 1 1 d . . .
H8A H 0.0465 0.1624 0.3047 0.033 Uiso 1 1 calc R . .
C9 C 0.2852(5) 0.0618(3) 0.1557(7) 0.0294(12) Uani 1 1 d . . .
H9A H 0.3805 0.0453 0.1374 0.035 Uiso 1 1 calc R . .
C10 C 0.9518(8) 0.3485(4) 0.1780(11) 0.064(2) Uani 1 1 d . . .
H10A H 0.9341 0.3306 0.2967 0.095 Uiso 1 1 calc R . .
H10B H 0.8666 0.3752 0.1312 0.095 Uiso 1 1 calc R . .
H10C H 1.0349 0.3822 0.1824 0.095 Uiso 1 1 calc R . .
Cl1 Cl -0.25019(17) -0.00443(9) 0.3694(2) 0.0522(4) Uani 1 1 d . . .


_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
Zn1 N1 2.075(4) . ?
Zn1 N2 2.080(4) 3 ?
Zn1 O2 2.167(4) 4_465 ?
Zn1 O1 2.192(4) 4_465 ?
Zn1 Cl1 2.2140(17) . ?
Zn1 C1 2.510(5) 4_465 ?
N1 C8 1.301(6) . ?
N1 N2 1.395(5) . ?
N2 C9 1.302(6) . ?
N2 Zn1 2.080(4) 3 ?
N3 C8 1.347(6) . ?
N3 C9 1.351(6) . ?
N3 C5 1.449(6) . ?
O1 C1 1.251(7) . ?
O1 Zn1 2.192(4) 4_666 ?
O3 C10 1.408(8) . ?
O2 C1 1.253(7) . ?
O2 Zn1 2.167(4) 4_666 ?
C1 C2 1.499(7) . ?
C1 Zn1 2.510(5) 4_666 ?
C2 C3 1.380(7) . ?
C2 C7 1.393(7) . ?
C3 C4 1.373(7) . ?
C4 C5 1.376(7) . ?
C5 C6 1.376(7) . ?
C6 C7 1.385(7) . ?

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
N1 Zn1 N2 97.97(16) . 3 ?
N1 Zn1 O2 91.78(15) . 4_465 ?
N2 Zn1 O2 123.49(17) 3 4_465 ?
N1 Zn1 O1 146.93(17) . 4_465 ?
N2 Zn1 O1 86.06(16) 3 4_465 ?
O2 Zn1 O1 59.84(15) 4_465 4_465 ?
N1 Zn1 Cl1 108.52(13) . . ?
N2 Zn1 Cl1 112.91(13) 3 . ?
O2 Zn1 Cl1 116.10(12) 4_465 . ?
O1 Zn1 Cl1 99.79(13) 4_465 . ?
N1 Zn1 C1 120.06(17) . 4_465 ?
N2 Zn1 C1 106.06(18) 3 4_465 ?
O2 Zn1 C1 29.95(17) 4_465 4_465 ?
O1 Zn1 C1 29.90(17) 4_465 4_465 ?
Cl1 Zn1 C1 110.74(13) . 4_465 ?
C8 N1 N2 107.0(4) . . ?
C8 N1 Zn1 123.6(3) . . ?
N2 N1 Zn1 129.1(3) . . ?
C9 N2 N1 106.7(4) . . ?
C9 N2 Zn1 120.7(3) . 3 ?
N1 N2 Zn1 129.8(3) . 3 ?
C8 N3 C9 105.6(4) . . ?
C8 N3 C5 127.1(4) . . ?
C9 N3 C5 126.9(4) . . ?
C1 O1 Zn1 89.3(3) . 4_666 ?
C1 O2 Zn1 90.4(3) . 4_666 ?
O1 C1 O2 120.5(5) . . ?
O1 C1 C2 119.1(5) . . ?
O2 C1 C2 120.4(5) . . ?
O1 C1 Zn1 60.8(3) . 4_666 ?
O2 C1 Zn1 59.7(3) . 4_666 ?
C2 C1 Zn1 179.6(4) . 4_666 ?
C3 C2 C7 119.6(4) . . ?
C3 C2 C1 122.4(5) . . ?
C7 C2 C1 118.0(5) . . ?
C4 C3 C2 121.1(5) . . ?
C3 C4 C5 118.3(5) . . ?
C6 C5 C4 122.5(4) . . ?
C6 C5 N3 117.6(4) . . ?
C4 C5 N3 119.7(4) . . ?
C5 C6 C7 118.5(5) . . ?
C6 C7 C2 120.0(5) . . ?
N1 C8 N3 110.3(4) . . ?
N2 C9 N3 110.4(4) . . ?

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
O3 H3 O2 0.82 2.01 2.826(6) 173.3 4_565
C6 H6A O3 0.93 2.57 3.496(7) 171.5 1_455
C8 H8A O3 0.93 2.25 3.079(7) 147.4 4_466
C9 H9A O1 0.93 2.48 2.965(6) 112.8 2_645
C9 H9A O1 0.93 2.47 3.259(7) 142.3 4_565

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.137
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1413438'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 N6 O4 Zn'
_chemical_formula_weight         441.71

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   13.664(2)
_cell_length_b                   7.8616(13)
_cell_length_c                   8.2311(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.400(3)
_cell_angle_gamma                90.00
_cell_volume                     883.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8034
_exptl_absorpt_correction_T_max  0.9065
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2798
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1564
_reflns_number_gt                1510
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'

_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)+(0.0256P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.056(18)
_refine_ls_number_reflns         1564
_refine_ls_number_parameters     132
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn 1.0000 0.58456(6) -0.5000 0.02969(18) Uani 1 2 d S . .
O1 O 0.9382(2) 1.4293(4) -1.3541(3) 0.0538(9) Uani 1 1 d . . .
O2 O 0.9110(3) 1.6326(4) -1.1718(5) 0.0612(13) Uani 1 1 d . . .
N1 N 0.9019(2) 0.7499(4) -0.6033(4) 0.0377(8) Uani 1 1 d . . .
N2 N 0.8287(3) 0.8302(5) -0.5188(4) 0.0466(9) Uani 1 1 d . . .
N3 N 0.8543(3) 0.9676(5) -0.7463(4) 0.0350(8) Uani 1 1 d . . .
C1 C 0.9114(4) 1.4840(7) -1.2148(6) 0.0437(13) Uani 1 1 d . . .
C2 C 0.8828(3) 1.3466(5) -1.0982(5) 0.0349(9) Uani 1 1 d . . .
C3 C 0.8605(3) 1.3895(5) -0.9406(5) 0.0391(10) Uani 1 1 d . . .
H3A H 0.8538 1.5035 -0.9128 0.047 Uiso 1 1 calc R . .
C4 C 0.8479(3) 1.2645(6) -0.8224(5) 0.0373(10) Uani 1 1 d . . .
H4A H 0.8351 1.2935 -0.7154 0.045 Uiso 1 1 calc R . .
C5 C 0.8549(2) 1.0977(8) -0.8691(4) 0.0312(8) Uani 1 1 d . . .
C6 C 0.8701(3) 1.0499(5) -1.0298(4) 0.0369(11) Uani 1 1 d . . .
H6A H 0.8702 0.9359 -1.0599 0.044 Uiso 1 1 calc R . .
C7 C 0.8848(3) 1.1753(5) -1.1423(5) 0.0392(10) Uani 1 1 d . . .
H7A H 0.8963 1.1457 -1.2496 0.047 Uiso 1 1 calc R . .
C8 C 0.8024(3) 0.9601(6) -0.6063(5) 0.0421(11) Uani 1 1 d . . .
H8A H 0.7546 1.0380 -0.5778 0.050 Uiso 1 1 calc R . .
C9 C 0.9141(3) 0.8322(5) -0.7368(5) 0.0386(10) Uani 1 1 d . . .
H9A H 0.9584 0.8019 -0.8158 0.046 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
Zn1 O1 1.922(3) 2_743 ?
Zn1 O1 1.922(3) 1_546 ?
Zn1 N1 2.038(3) 2_754 ?
Zn1 N1 2.038(3) . ?
O1 C1 1.286(6) . ?
O1 Zn1 1.922(3) 1_564 ?
O2 C1 1.221(6) . ?
N1 C9 1.290(5) . ?
N1 N2 1.384(5) . ?
N2 C8 1.295(5) . ?
N3 C9 1.343(5) . ?
N3 C8 1.369(5) . ?
N3 C5 1.438(6) . ?
C1 C2 1.503(6) . ?
C2 C3 1.382(6) . ?
C2 C7 1.396(5) . ?
C3 C4 1.397(5) . ?
C4 C5 1.371(8) . ?
C5 C6 1.396(5) . ?
C6 C7 1.371(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
O1 Zn1 O1 101.2(2) 2_743 1_546 ?
O1 Zn1 N1 111.78(13) 2_743 2_754 ?
O1 Zn1 N1 116.05(13) 1_546 2_754 ?
O1 Zn1 N1 116.05(13) 2_743 . ?
O1 Zn1 N1 111.78(13) 1_546 . ?
N1 Zn1 N1 100.7(2) 2_754 . ?
C1 O1 Zn1 118.9(3) . 1_564 ?
C9 N1 N2 108.0(3) . . ?
C9 N1 Zn1 125.3(3) . . ?
N2 N1 Zn1 123.9(2) . . ?
C8 N2 N1 105.9(3) . . ?
C9 N3 C8 104.1(3) . . ?
C9 N3 C5 126.2(3) . . ?
C8 N3 C5 129.3(4) . . ?
O2 C1 O1 125.6(5) . . ?
O2 C1 C2 120.0(5) . . ?
O1 C1 C2 114.4(4) . . ?
C3 C2 C7 119.1(4) . . ?
C3 C2 C1 119.4(4) . . ?
C7 C2 C1 121.3(4) . . ?
C2 C3 C4 121.1(4) . . ?
C5 C4 C3 117.9(4) . . ?
C4 C5 C6 122.4(5) . . ?
C4 C5 N3 118.8(4) . . ?
C6 C5 N3 118.6(5) . . ?
C7 C6 C5 118.3(4) . . ?
C6 C7 C2 120.9(4) . . ?
N2 C8 N3 111.1(4) . . ?
N1 C9 N3 110.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1413443'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.026 0.000 -0.201 319 21 ' '
2 -0.026 0.500 0.299 319 21 ' '
_platon_squeeze_details          
;
Highly Disordered solvent (DMF and H₂O) molecules were not determined and 
the contributions of these disordered solvent molecules to 
the scattering values have been removed by using the PLATON SQUEEZE 
program. TGA and elemental analyses reveal that it contains one DMF and 
3.6 water molecules per molecular unit. Then, the formula can be get 
as [Cd(C₁₈H₁₂N₆O₄)].DMF.3.6H₂O. 



;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H26.2 Cd N7 O8.6'
_chemical_formula_weight         626.69

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnc2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'

_cell_length_a                   8.3848(17)
_cell_length_b                   14.808(3)
_cell_length_c                   11.494(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1427.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_T_max  0.8090
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11581
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2797
_reflns_number_gt                2393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0519P)²+0.0538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(8)
_refine_ls_number_reflns         2797
_refine_ls_number_parameters     132
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.235
_refine_ls_shift/su_max          0.000
_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 0.5000 0.0000 0.3207(2) 0.03611(12) Uani 1 2 d S . .
N1 N 0.4090(3) -0.11125(17) 0.4387(3) 0.0646(8) Uani 1 1 d U . .
N2 N 0.5024(3) -0.1823(5) 0.4696(10) 0.1228(18) Uani 1 1 d U . .
N3 N 0.2594(3) -0.2098(2) 0.5269(3) 0.0748(11) Uani 1 1 d . . .
C1 C 0.4118(5) -0.2367(4) 0.5250(7) 0.143(2) Uani 1 1 d U . .
H1A H 0.4478 -0.2894 0.5603 0.171 Uiso 1 1 calc R . .
C2 C 0.2647(4) -0.1314(2) 0.4718(3) 0.0576(8) Uani 1 1 d U . .
H2A H 0.1762 -0.0951 0.4583 0.069 Uiso 1 1 calc R . .
C3 C 0.1260(4) -0.2555(3) 0.5759(5) 0.0669(11) Uani 1 1 d . . .
C4 C -0.0264(5) -0.2345(5) 0.5411(7) 0.091(2) Uani 1 1 d . . .
H4A H -0.0435 -0.1895 0.4861 0.110 Uiso 1 1 calc R . .
C5 C -0.1549(5) -0.2809(3) 0.5888(5) 0.0795(15) Uani 1 1 d . . .
H5A H -0.2580 -0.2657 0.5664 0.095 Uiso 1 1 calc R . .
C6 C -0.1319(5) -0.3489(3) 0.6685(4) 0.0565(9) Uani 1 1 d . . .
C7 C 0.0213(4) -0.3700(4) 0.7029(5) 0.0616(12) Uani 1 1 d . . .
H7A H 0.0381 -0.4162 0.7563 0.074 Uiso 1 1 calc R . .
C8 C 0.1513(5) -0.3224(3) 0.6579(5) 0.0749(14) Uani 1 1 d . . .
H8A H 0.2542 -0.3355 0.6829 0.090 Uiso 1 1 calc R . .
C9 C -0.2683(3) -0.4022(2) 0.7179(3) 0.0552(8) Uani 1 1 d . . .
O1 O -0.2404(2) -0.45887(16) 0.7957(2) 0.0625(6) Uani 1 1 d . . .
O2 O -0.4074(2) -0.38880(16) 0.6805(2) 0.0726(7) Uani 1 1 d . . .


_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 N1 2.266(3) 2_655 ?
Cd1 N1 2.266(3) . ?
Cd1 O1 2.278(2) 4_554 ?
Cd1 O1 2.278(2) 3_644 ?
Cd1 O2 2.431(3) 3_644 ?
Cd1 O2 2.431(3) 4_554 ?
Cd1 C9 2.696(3) 4_554 ?
Cd1 C9 2.696(3) 3_644 ?
N1 C2 1.303(4) . ?
N1 N2 1.359(6) . ?
N2 C1 1.277(8) . ?
N3 C2 1.323(4) . ?
N3 C1 1.339(4) . ?
N3 C3 1.424(4) . ?
C3 C4 1.374(5) . ?
C3 C8 1.384(6) . ?
C4 C5 1.390(6) . ?
C5 C6 1.375(6) . ?
C6 C7 1.380(5) . ?
C6 C9 1.500(5) . ?
C7 C8 1.398(6) . ?
C9 O1 1.249(4) . ?
C9 O2 1.259(4) . ?
C9 Cd1 2.696(3) 3_445 ?
O1 Cd1 2.278(2) 3_445 ?
O2 Cd1 2.431(3) 3_445 ?

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
N1 Cd1 N1 106.5(2) 2_655 . ?
N1 Cd1 O1 101.70(10) 2_655 4_554 ?
N1 Cd1 O1 87.03(9) . 4_554 ?
N1 Cd1 O1 87.03(9) 2_655 3_644 ?
N1 Cd1 O1 101.70(10) . 3_644 ?
O1 Cd1 O1 165.52(18) 4_554 3_644 ?
N1 Cd1 O2 141.40(9) 2_655 3_644 ?
N1 Cd1 O2 90.68(10) . 3_644 ?
O1 Cd1 O2 113.74(11) 4_554 3_644 ?
O1 Cd1 O2 55.27(8) 3_644 3_644 ?
N1 Cd1 O2 90.68(10) 2_655 4_554 ?
N1 Cd1 O2 141.40(9) . 4_554 ?
O1 Cd1 O2 55.27(8) 4_554 4_554 ?
O1 Cd1 O2 113.74(11) 3_644 4_554 ?
O2 Cd1 O2 96.97(17) 3_644 4_554 ?
N1 Cd1 C9 96.57(10) 2_655 4_554 ?
N1 Cd1 C9 114.22(10) . 4_554 ?
O1 Cd1 C9 27.47(9) 4_554 4_554 ?
O1 Cd1 C9 140.97(14) 3_644 4_554 ?
O2 Cd1 C9 107.66(13) 3_644 4_554 ?
O2 Cd1 C9 27.81(9) 4_554 4_554 ?
N1 Cd1 C9 114.22(10) 2_655 3_644 ?
N1 Cd1 C9 96.57(10) . 3_644 ?
O1 Cd1 C9 140.97(14) 4_554 3_644 ?
O1 Cd1 C9 27.47(9) 3_644 3_644 ?
O2 Cd1 C9 27.81(9) 3_644 3_644 ?
O2 Cd1 C9 107.66(13) 4_554 3_644 ?
C9 Cd1 C9 128.00(18) 4_554 3_644 ?
C2 N1 N2 106.3(3) . . ?
C2 N1 Cd1 130.8(2) . . ?
N2 N1 Cd1 121.7(3) . . ?
C1 N2 N1 106.0(3) . . ?
C2 N3 C1 102.8(3) . . ?
C2 N3 C3 129.3(3) . . ?
C1 N3 C3 128.0(4) . . ?
N2 C1 N3 112.8(4) . . ?
N1 C2 N3 111.8(3) . . ?
C4 C3 C8 120.2(4) . . ?
C4 C3 N3 120.5(5) . . ?
C8 C3 N3 119.3(4) . . ?
C3 C4 C5 119.6(5) . . ?
C6 C5 C4 121.1(4) . . ?
C5 C6 C7 119.1(4) . . ?
C5 C6 C9 122.0(4) . . ?
C7 C6 C9 118.9(4) . . ?
C6 C7 C8 120.4(5) . . ?
C3 C8 C7 119.5(4) . . ?
O1 C9 O2 121.6(3) . . ?
O1 C9 C6 118.8(3) . . ?
O2 C9 C6 119.6(3) . . ?
O1 C9 Cd1 57.29(15) . 3_445 ?
O2 C9 Cd1 64.31(17) . 3_445 ?
C6 C9 Cd1 175.7(3) . 3_445 ?
C9 O1 Cd1 95.23(18) . 3_445 ?
C9 O2 Cd1 87.9(2) . 3_445 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1413445'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 Cd N6 O4'
_chemical_formula_weight         488.74

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.680(3)
_cell_length_b                   32.764(7)
_cell_length_c                   6.5537(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3581.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7353
_exptl_absorpt_correction_T_max  0.7867
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8456
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         27.44
_reflns_number_total             1926
_reflns_number_gt                1848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0188P)²+6.3646P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_number_reflns         1926
_refine_ls_number_parameters     132
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0406
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.199
_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 0.0000 0.0000 0.58538(6) 0.03494(8) Uani 1 2 d S . .
O1 O 0.1703(2) 0.22109(7) 1.5849(6) 0.0817(10) Uani 1 1 d . . .
O2 O 0.22093(18) 0.17870(7) 1.8039(4) 0.0641(7) Uani 1 1 d . . .
N1 N 0.09346(14) 0.02076(7) 0.8177(6) 0.0403(6) Uani 1 1 d . . .
N2 N 0.16771(17) 0.00563(7) 0.8650(5) 0.0474(6) Uani 1 1 d . . .
N3 N 0.14058(13) 0.05671(6) 1.0698(4) 0.0371(5) Uani 1 1 d . . .
C1 C 0.18586(19) 0.18582(9) 1.6411(5) 0.0445(7) Uani 1 1 d . . .
C2 C 0.16678(17) 0.15069(8) 1.4995(5) 0.0386(6) Uani 1 1 d . . .
C3 C 0.13649(19) 0.15881(8) 1.3062(6) 0.0456(7) Uani 1 1 d . . .
H3A H 0.1218 0.1853 1.2714 0.055 Uiso 1 1 calc R . .
C4 C 0.1280(2) 0.12761(9) 1.1649(5) 0.0446(8) Uani 1 1 d . . .
H4A H 0.1090 0.1331 1.0344 0.054 Uiso 1 1 calc R . .
C5 C 0.14812(17) 0.08838(8) 1.2205(5) 0.0375(6) Uani 1 1 d . . .
C6 C 0.1754(2) 0.07936(9) 1.4137(5) 0.0451(7) Uani 1 1 d . . .
H6A H 0.1869 0.0525 1.4497 0.054 Uiso 1 1 calc R . .
C7 C 0.18571(19) 0.11066(9) 1.5545(5) 0.0454(7) Uani 1 1 d . . .
H7A H 0.2051 0.1050 1.6844 0.054 Uiso 1 1 calc R . .
C8 C 0.07918(19) 0.05110(10) 0.9413(6) 0.0518(8) Uani 1 1 d . . .
H8A H 0.0326 0.0667 0.9403 0.062 Uiso 1 1 calc R . .
C9 C 0.1943(2) 0.02768(9) 1.0160(5) 0.0492(8) Uani 1 1 d . . .
H9A H 0.2438 0.0240 1.0786 0.059 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 N1 2.283(3) . ?
Cd1 N1 2.283(3) 2 ?
Cd1 O1 2.315(3) 11_453 ?
Cd1 O1 2.315(3) 8_543 ?
Cd1 O2 2.395(2) 11_453 ?
Cd1 O2 2.395(2) 8_543 ?
Cd1 C1 2.681(3) 8_543 ?
Cd1 C1 2.681(3) 11_453 ?
O1 C1 1.240(4) . ?
O1 Cd1 2.315(3) 3_556 ?
O2 C1 1.239(4) . ?
O2 Cd1 2.395(2) 3_556 ?
N1 C8 1.304(4) . ?
N1 N2 1.370(4) . ?
N2 C9 1.303(4) . ?
N3 C8 1.338(4) . ?
N3 C9 1.354(4) . ?
N3 C5 1.439(3) . ?
C1 C2 1.512(4) . ?
C1 Cd1 2.681(3) 3_556 ?
C2 C3 1.390(5) . ?
C2 C7 1.396(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.377(4) . ?
C5 C6 1.378(4) . ?
C6 C7 1.390(4) . ?

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
N1 Cd1 N1 96.34(17) . 2 ?
N1 Cd1 O1 138.00(9) . 11_453 ?
N1 Cd1 O1 101.69(11) 2 11_453 ?
N1 Cd1 O1 101.69(11) . 8_543 ?
N1 Cd1 O1 138.00(9) 2 8_543 ?
O1 Cd1 O1 89.7(2) 11_453 8_543 ?
N1 Cd1 O2 84.54(9) . 11_453 ?
N1 Cd1 O2 102.11(10) 2 11_453 ?
O1 Cd1 O2 54.80(9) 11_453 11_453 ?
O1 Cd1 O2 117.03(11) 8_543 11_453 ?
N1 Cd1 O2 102.11(10) . 8_543 ?
N1 Cd1 O2 84.54(9) 2 8_543 ?
O1 Cd1 O2 117.03(11) 11_453 8_543 ?
O1 Cd1 O2 54.80(9) 8_543 8_543 ?
O2 Cd1 O2 170.13(14) 11_453 8_543 ?
N1 Cd1 C1 106.14(9) . 8_543 ?
N1 Cd1 C1 110.83(10) 2 8_543 ?
O1 Cd1 C1 102.32(11) 11_453 8_543 ?
O1 Cd1 C1 27.52(10) 8_543 8_543 ?
O2 Cd1 C1 143.62(10) 11_453 8_543 ?
O2 Cd1 C1 27.53(9) 8_543 8_543 ?
N1 Cd1 C1 110.83(10) . 11_453 ?
N1 Cd1 C1 106.14(9) 2 11_453 ?
O1 Cd1 C1 27.52(10) 11_453 11_453 ?
O1 Cd1 C1 102.32(11) 8_543 11_453 ?
O2 Cd1 C1 27.53(9) 11_453 11_453 ?
O2 Cd1 C1 143.62(10) 8_543 11_453 ?
C1 Cd1 C1 123.29(14) 8_543 11_453 ?
C1 O1 Cd1 92.9(2) . 3_556 ?
C1 O2 Cd1 89.2(2) . 3_556 ?
C8 N1 N2 107.5(3) . . ?
C8 N1 Cd1 121.1(2) . . ?
N2 N1 Cd1 131.4(2) . . ?
C9 N2 N1 106.2(3) . . ?
C8 N3 C9 104.3(3) . . ?
C8 N3 C5 126.7(2) . . ?
C9 N3 C5 128.9(3) . . ?
O2 C1 O1 122.0(3) . . ?
O2 C1 C2 119.0(3) . . ?
O1 C1 C2 118.9(3) . . ?
O2 C1 Cd1 63.26(17) . 3_556 ?
O1 C1 Cd1 59.6(2) . 3_556 ?
C2 C1 Cd1 166.5(2) . 3_556 ?
C3 C2 C7 119.8(3) . . ?
C3 C2 C1 119.3(3) . . ?
C7 C2 C1 120.6(3) . . ?
C4 C3 C2 120.3(3) . . ?
C5 C4 C3 119.1(3) . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 N3 118.0(3) . . ?
C6 C5 N3 120.3(3) . . ?
C5 C6 C7 119.5(3) . . ?
C6 C7 C2 119.6(3) . . ?
N1 C8 N3 110.8(3) . . ?
N2 C9 N3 111.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1413448'
_audit_update_record             
;
2015-07-18 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58.50 H54.5 Cd5 Cl4 N19.50 O17.50'
_chemical_formula_weight         2014.55

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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

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

_cell_length_a                   12.946(3)
_cell_length_b                   17.321(3)
_cell_length_c                   22.153(4)
_cell_angle_alpha                70.13(3)
_cell_angle_beta                 76.08(3)
_cell_angle_gamma                73.31(3)
_cell_volume                     4418.3(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1964
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6683
_exptl_absorpt_correction_T_max  0.7003
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36654
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.00
_reflns_number_total             17149
_reflns_number_gt                12491
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0898P)²+5.9815P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17149
_refine_ls_number_parameters     1031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1593
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 1.16515(4) 0.54865(3) 0.01310(2) 0.03523(13) Uani 1 1 d . . .
Cd2 Cd 0.17809(3) 0.73405(3) 0.090749(19) 0.02756(12) Uani 1 1 d . . .
Cd3 Cd 0.17465(3) 0.77685(2) 0.248079(19) 0.02693(12) Uani 1 1 d . . .
Cd4 Cd 0.17631(3) 0.81187(3) 0.408313(19) 0.02612(12) Uani 1 1 d . . .
Cd5 Cd -0.83254(4) 1.00526(3) 0.48319(2) 0.02811(12) Uani 1 1 d . . .
Cl1 Cl 0.29231(15) 0.62030(11) 0.03149(9) 0.0457(4) Uani 1 1 d . . .
Cl2 Cl 0.05532(13) 0.83723(10) 0.15491(7) 0.0378(4) Uani 1 1 d . . .
Cl3 Cl 0.27952(15) 0.70458(11) 0.34725(8) 0.0469(4) Uani 1 1 d . . .
Cl4 Cl 0.05536(13) 0.91954(11) 0.46810(9) 0.0434(4) Uani 1 1 d . . .
N1 N 1.1399(7) 0.6360(4) -0.4748(3) 0.064(2) Uani 1 1 d . . .
N2 N 1.1631(5) 0.7130(3) -0.4890(3) 0.0423(14) Uani 1 1 d . . .
N3 N 1.1628(6) 0.6536(4) -0.3857(3) 0.0472(15) Uani 1 1 d . . .
N4 N 1.0168(4) 0.6263(3) 0.0650(3) 0.0364(12) Uani 1 1 d . . .
N5 N 1.0159(4) 0.6898(3) 0.0888(3) 0.0377(12) Uani 1 1 d . . .
N6 N 0.8474(4) 0.6819(4) 0.0978(3) 0.0445(14) Uani 1 1 d . . .
N7 N 0.1874(5) 0.6242(3) 0.1903(2) 0.0369(13) Uani 1 1 d . . .
N8 N 0.1737(5) 0.6428(3) 0.2474(2) 0.0377(13) Uani 1 1 d . . .
N9 N 0.1730(5) 0.5104(3) 0.2702(3) 0.0435(15) Uani 1 1 d . . .
N10 N 0.1809(4) 0.9094(3) 0.2505(2) 0.0321(11) Uani 1 1 d . . .
N11 N 0.1791(5) 0.9253(3) 0.3073(2) 0.0354(12) Uani 1 1 d . . .
N12 N 0.1795(5) 1.0424(3) 0.2280(3) 0.0360(12) Uani 1 1 d . . .
N13 N 0.0112(4) 0.8028(3) 0.3815(2) 0.0324(11) Uani 1 1 d . . .
N14 N 0.0117(4) 0.7923(3) 0.3222(2) 0.0328(11) Uani 1 1 d . . .
N15 N -0.1573(4) 0.8181(3) 0.3719(2) 0.0347(12) Uani 1 1 d . . .
N16 N -0.8591(6) 0.9193(4) 0.9795(3) 0.0499(16) Uani 1 1 d . . .
N17 N -0.8409(5) 0.8325(3) 0.9919(2) 0.0396(13) Uani 1 1 d . . .
N18 N -0.8417(5) 0.8902(3) 0.8882(3) 0.0413(13) Uani 1 1 d . . .
C1 C 1.1420(9) 0.6032(5) -0.4137(4) 0.069(3) Uani 1 1 d . . .
H1A H 1.1303 0.5496 -0.3909 0.083 Uiso 1 1 calc R . .
C2 C 1.1761(6) 0.7222(4) -0.4369(3) 0.0441(17) Uani 1 1 d . . .
H2A H 1.1926 0.7697 -0.4343 0.053 Uiso 1 1 calc R . .
C3 C 1.1673(6) 0.6388(5) -0.3179(3) 0.0447(17) Uani 1 1 d . . .
C4 C 1.1252(6) 0.7038(4) -0.2903(3) 0.0447(17) Uani 1 1 d . . .
H4A H 1.0960 0.7573 -0.3158 0.054 Uiso 1 1 calc R . .
C5 C 1.1258(6) 0.6905(4) -0.2256(3) 0.0428(16) Uani 1 1 d . . .
H5A H 1.0961 0.7344 -0.2070 0.051 Uiso 1 1 calc R . .
C6 C 1.1714(6) 0.6103(4) -0.1882(3) 0.0426(16) Uani 1 1 d . . .
C7 C 1.2138(8) 0.5452(5) -0.2168(4) 0.064(2) Uani 1 1 d . . .
H7A H 1.2439 0.4916 -0.1920 0.077 Uiso 1 1 calc R . .
C8 C 1.2114(8) 0.5598(5) -0.2819(4) 0.066(3) Uani 1 1 d . . .
H8A H 1.2396 0.5163 -0.3010 0.079 Uiso 1 1 calc R . .
C9 C 1.1726(6) 0.5943(5) -0.1170(3) 0.0421(16) Uani 1 1 d . . .
C10 C 0.9152(6) 0.6216(5) 0.0712(4) 0.0461(17) Uani 1 1 d . . .
H10A H 0.8930 0.5830 0.0592 0.055 Uiso 1 1 calc R . .
C11 C 0.9145(5) 0.7218(4) 0.1082(4) 0.0434(16) Uani 1 1 d . . .
H11A H 0.8912 0.7659 0.1268 0.052 Uiso 1 1 calc R . .
C12 C 0.7299(5) 0.7008(5) 0.1078(4) 0.0459(17) Uani 1 1 d . . .
C13 C 0.6722(6) 0.7051(7) 0.1668(4) 0.074(3) Uani 1 1 d . . .
H13A H 0.7078 0.6950 0.2014 0.088 Uiso 1 1 calc R . .
C14 C 0.5592(7) 0.7247(8) 0.1747(5) 0.079(3) Uani 1 1 d . . .
H14A H 0.5185 0.7289 0.2146 0.095 Uiso 1 1 calc R . .
C15 C 0.5065(5) 0.7379(5) 0.1236(4) 0.0457(17) Uani 1 1 d . . .
C16 C 0.5683(6) 0.7242(9) 0.0676(5) 0.096(4) Uani 1 1 d . . .
H16A H 0.5337 0.7246 0.0352 0.115 Uiso 1 1 calc R . .
C17 C 0.6803(7) 0.7098(8) 0.0574(4) 0.090(4) Uani 1 1 d . . .
H17A H 0.7210 0.7063 0.0173 0.108 Uiso 1 1 calc R . .
C18 C 0.3823(5) 0.7576(5) 0.1336(4) 0.0432(16) Uani 1 1 d . . .
C19 C 0.1872(6) 0.5452(4) 0.2040(3) 0.0425(16) Uani 1 1 d . . .
H19A H 0.1954 0.5167 0.1738 0.051 Uiso 1 1 calc R . .
C20 C 0.1656(7) 0.5739(4) 0.2947(3) 0.0450(18) Uani 1 1 d . . .
H20A H 0.1562 0.5691 0.3387 0.054 Uiso 1 1 calc R . .
C21 C 0.1668(7) 0.4247(4) 0.3060(3) 0.0453(18) Uani 1 1 d . . .
C22 C 0.1984(9) 0.3904(5) 0.3658(4) 0.066(3) Uani 1 1 d . . .
H22A H 0.2203 0.4226 0.3844 0.079 Uiso 1 1 calc R . .
C23 C 0.1971(8) 0.3059(4) 0.3987(4) 0.061(2) Uani 1 1 d . . .
H23A H 0.2199 0.2814 0.4391 0.073 Uiso 1 1 calc R . .
C24 C 0.1628(6) 0.2592(4) 0.3723(3) 0.0360(14) Uani 1 1 d . . .
C25 C 0.1274(6) 0.2958(4) 0.3126(3) 0.0440(17) Uani 1 1 d . . .
H25A H 0.1032 0.2642 0.2944 0.053 Uiso 1 1 calc R . .
C26 C 0.1280(7) 0.3793(4) 0.2801(4) 0.054(2) Uani 1 1 d . . .
H26A H 0.1022 0.4047 0.2406 0.065 Uiso 1 1 calc R . .
C27 C 0.1643(6) 0.1677(4) 0.4072(3) 0.0377(15) Uani 1 1 d . . .
C28 C 0.1787(6) 1.0053(4) 0.2930(3) 0.0372(15) Uani 1 1 d . . .
H28A H 0.1779 1.0326 0.3228 0.045 Uiso 1 1 calc R . .
C29 C 0.1801(5) 0.9802(4) 0.2035(3) 0.0345(14) Uani 1 1 d . . .
H29A H 0.1800 0.9868 0.1601 0.041 Uiso 1 1 calc R . .
C30 C 0.1759(6) 1.1297(4) 0.1930(3) 0.0349(14) Uani 1 1 d . . .
C31 C 0.1103(6) 1.1688(4) 0.1465(3) 0.0433(16) Uani 1 1 d . . .
H31A H 0.0684 1.1394 0.1378 0.052 Uiso 1 1 calc R . .
C32 C 0.1067(6) 1.2531(4) 0.1124(3) 0.0468(17) Uani 1 1 d . . .
H32A H 0.0625 1.2801 0.0804 0.056 Uiso 1 1 calc R . .
C33 C 0.1680(6) 1.2971(4) 0.1254(3) 0.0407(16) Uani 1 1 d . . .
C34 C 0.2352(7) 1.2550(4) 0.1724(4) 0.053(2) Uani 1 1 d . . .
H34A H 0.2774 1.2838 0.1815 0.064 Uiso 1 1 calc R . .
C35 C 0.2403(7) 1.1708(4) 0.2060(4) 0.0508(19) Uani 1 1 d . . .
H35A H 0.2865 1.1427 0.2369 0.061 Uiso 1 1 calc R . .
C36 C 0.1598(6) 1.3905(4) 0.0904(3) 0.0436(17) Uani 1 1 d . . .
C37 C -0.0926(5) 0.8033(4) 0.3178(3) 0.0386(15) Uani 1 1 d . . .
H37A H -0.1171 0.8010 0.2825 0.046 Uiso 1 1 calc R . .
C38 C -0.0882(5) 0.8175(4) 0.4098(3) 0.0341(14) Uani 1 1 d . . .
H38A H -0.1101 0.8265 0.4505 0.041 Uiso 1 1 calc R . .
C39 C -0.2750(5) 0.8325(4) 0.3865(3) 0.0350(14) Uani 1 1 d . . .
C40 C -0.3309(5) 0.8898(5) 0.4192(4) 0.0484(18) Uani 1 1 d . . .
H40A H -0.2932 0.9178 0.4325 0.058 Uiso 1 1 calc R . .
C41 C -0.4435(5) 0.9062(5) 0.4324(4) 0.0468(17) Uani 1 1 d . . .
H41A H -0.4819 0.9451 0.4547 0.056 Uiso 1 1 calc R . .
C42 C -0.4993(5) 0.8640(4) 0.4120(3) 0.0382(15) Uani 1 1 d . . .
C43 C -0.4416(6) 0.8074(5) 0.3777(4) 0.0506(19) Uani 1 1 d . . .
H43A H -0.4791 0.7807 0.3629 0.061 Uiso 1 1 calc R . .
C44 C -0.3279(5) 0.7898(5) 0.3649(4) 0.0500(19) Uani 1 1 d . . .
H44A H -0.2887 0.7508 0.3427 0.060 Uiso 1 1 calc R . .
C45 C -0.6227(5) 0.8836(4) 0.4244(3) 0.0366(14) Uani 1 1 d . . .
C46 C -0.8598(7) 0.9504(4) 0.9186(3) 0.052(2) Uani 1 1 d . . .
H46A H -0.8713 1.0078 0.8972 0.063 Uiso 1 1 calc R . .
C47 C -0.8324(6) 0.8178(4) 0.9378(3) 0.0410(16) Uani 1 1 d . . .
H47A H -0.8213 0.7645 0.9333 0.049 Uiso 1 1 calc R . .
C48 C -0.8303(6) 0.8985(4) 0.8207(3) 0.0380(15) Uani 1 1 d . . .
C49 C -0.8950(6) 0.9666(4) 0.7818(3) 0.0408(16) Uani 1 1 d . . .
H49A H -0.9466 1.0063 0.7995 0.049 Uiso 1 1 calc R . .
C50 C -0.8809(6) 0.9744(4) 0.7160(3) 0.0401(15) Uani 1 1 d . . .
H50A H -0.9212 1.0210 0.6888 0.048 Uiso 1 1 calc R . .
C51 C -0.8080(6) 0.9136(4) 0.6908(3) 0.0379(15) Uani 1 1 d . . .
C52 C -0.7449(6) 0.8449(4) 0.7309(3) 0.0453(17) Uani 1 1 d . . .
H52A H -0.6959 0.8037 0.7137 0.054 Uiso 1 1 calc R . .
C53 C -0.7548(6) 0.8376(4) 0.7958(3) 0.0463(18) Uani 1 1 d . . .
H53A H -0.7115 0.7926 0.8224 0.056 Uiso 1 1 calc R . .
C54 C -0.7942(6) 0.9199(5) 0.6195(3) 0.0414(16) Uani 1 1 d . . .
O1 O 1.2025(5) 0.5196(3) -0.0832(2) 0.0502(13) Uani 1 1 d . . .
O2 O 1.1436(5) 0.6548(3) -0.0937(2) 0.0515(13) Uani 1 1 d . . .
O3 O 0.3414(4) 0.7560(4) 0.0888(3) 0.0605(15) Uani 1 1 d . . .
O4 O 0.3360(4) 0.7729(4) 0.1838(3) 0.0689(17) Uani 1 1 d . . .
O5 O 0.1973(4) 0.1374(3) 0.4615(2) 0.0422(11) Uani 1 1 d . . .
O6 O 0.1357(5) 0.1248(3) 0.3817(2) 0.0511(13) Uani 1 1 d . . .
O7 O 0.2142(6) 1.4283(3) 0.1036(3) 0.0733(19) Uani 1 1 d . . .
O8 O 0.0980(5) 1.4247(3) 0.0492(3) 0.0621(16) Uani 1 1 d . . .
O9 O -0.6667(4) 0.8297(3) 0.4231(3) 0.0561(14) Uani 1 1 d . . .
O10 O -0.6690(4) 0.9535(3) 0.4341(3) 0.0565(14) Uani 1 1 d . . .
O11 O -0.7558(6) 0.8570(4) 0.6002(2) 0.0691(17) Uani 1 1 d . . .
O12 O -0.8284(5) 0.9937(3) 0.5837(2) 0.0506(13) Uani 1 1 d . . .
C1E C 0.3455(16) 0.4123(15) 0.5054(11) 0.087(6) Uani 0.50 1 d P . .
H1EA H 0.2772 0.4256 0.5328 0.131 Uiso 0.50 1 calc PR . .
H1EB H 0.3499 0.3620 0.4948 0.131 Uiso 0.50 1 calc PR . .
H1EC H 0.3504 0.4581 0.4662 0.131 Uiso 0.50 1 calc PR . .
C2E C 0.5490(13) 0.3786(11) 0.5056(9) 0.069(5) Uani 0.50 1 d P . .
H2EA H 0.5990 0.3728 0.5334 0.103 Uiso 0.50 1 calc PR . .
H2EB H 0.5601 0.4231 0.4662 0.103 Uiso 0.50 1 calc PR . .
H2EC H 0.5617 0.3268 0.4953 0.103 Uiso 0.50 1 calc PR . .
C3E C 0.4128(17) 0.4026(9) 0.5973(11) 0.064(5) Uani 0.50 1 d P . .
H3EA H 0.4746 0.3950 0.6150 0.077 Uiso 0.50 1 calc PR . .
N1E N 0.4346(11) 0.3990(8) 0.5394(8) 0.059(4) Uani 0.50 1 d P . .
O1E O 0.3352(14) 0.4129(9) 0.6315(8) 0.092(5) Uani 0.50 1 d P . .
C1R C 0.603(2) 0.9938(15) 0.2347(10) 0.111(9) Uani 0.50 1 d P . .
H1RA H 0.6808 0.9862 0.2285 0.166 Uiso 0.50 1 calc PR . .
H1RB H 0.5743 0.9832 0.2803 0.166 Uiso 0.50 1 calc PR . .
H1RC H 0.5712 1.0506 0.2120 0.166 Uiso 0.50 1 calc PR . .
C2R C 0.4709(15) 0.9500(15) 0.2193(12) 0.098(8) Uani 0.50 1 d P . .
H2RA H 0.4303 0.9939 0.2386 0.147 Uiso 0.50 1 calc PR . .
H2RB H 0.4536 0.8973 0.2463 0.147 Uiso 0.50 1 calc PR . .
H2RC H 0.4521 0.9627 0.1771 0.147 Uiso 0.50 1 calc PR . .
C3R C 0.664(2) 0.8921(13) 0.1884(12) 0.099(8) Uani 0.50 1 d P . .
H3RA H 0.6435 0.8600 0.1693 0.118 Uiso 0.50 1 calc PR . .
O1R O 0.7544(9) 0.8797(9) 0.1860(7) 0.071(4) Uani 0.50 1 d P . .
N1R N 0.5804(9) 0.9442(8) 0.2134(7) 0.049(3) Uani 0.50 1 d P . .
C1T C 0.477(2) 0.1249(16) 0.3825(13) 0.120(10) Uani 0.50 1 d P . .
H1TA H 0.4459 0.1032 0.3580 0.179 Uiso 0.50 1 calc PR . .
H1TB H 0.4358 0.1171 0.4257 0.179 Uiso 0.50 1 calc PR . .
H1TC H 0.5513 0.0953 0.3847 0.179 Uiso 0.50 1 calc PR . .
C2T C 0.516(3) 0.260(2) 0.3853(15) 0.19(2) Uani 0.50 1 d P . .
H2TA H 0.5001 0.3190 0.3617 0.281 Uiso 0.50 1 calc PR . .
H2TB H 0.5931 0.2398 0.3842 0.281 Uiso 0.50 1 calc PR . .
H2TC H 0.4802 0.2528 0.4296 0.281 Uiso 0.50 1 calc PR . .
C3T C 0.4477(18) 0.245(2) 0.2925(16) 0.115(9) Uani 0.50 1 d P . .
H3TA H 0.4455 0.3027 0.2744 0.138 Uiso 0.50 1 calc PR . .
N1T N 0.4718(13) 0.2090(14) 0.3529(9) 0.101(7) Uani 0.50 1 d P . .
O1T O 0.4281(16) 0.2076(18) 0.2590(10) 0.146(9) Uani 0.50 1 d P . .
O1W O 0.1359(8) 0.0270(4) 0.0597(3) 0.046(2) Uani 0.60 1 d P . .
O2W O 0.1412(13) 0.0945(8) 0.0068(6) 0.059(4) Uani 0.40 1 d P . .
O3W O 0.091(2) 0.3812(16) 0.7303(12) 0.071(7) Uiso 0.25 1 d P . .
O4W O 0.117(2) 0.3987(16) 0.6667(12) 0.072(7) Uiso 0.25 1 d P . .
O5W O 1.0847(12) 0.5537(8) -0.5524(6) 0.079(4) Uiso 0.50 1 d P . .
O6W O 0.9849(16) 0.5928(12) -0.5537(9) 0.124(6) Uiso 0.50 1 d P . .
O7W O 1.493(3) 0.5139(19) -0.1313(15) 0.092(9) Uiso 0.25 1 d P . .
O8W O 0.490(3) 0.415(2) 0.1233(17) 0.118(11) Uiso 0.25 1 d P . .
O9W O 0.450(3) 0.784(2) -0.0859(19) 0.130(13) Uiso 0.25 1 d P . .
O10W O 1.555(3) 0.530(2) -0.2362(16) 0.107(10) Uiso 0.25 1 d P . .
O11W O 0.416(3) 0.501(2) 0.3373(17) 0.116(11) Uiso 0.25 1 d P . .
O12W O 0.167(3) 0.352(2) 0.7184(15) 0.092(9) Uiso 0.25 1 d P . .


_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 O1 2.266(5) . ?
Cd1 N4 2.307(5) . ?
Cd1 O8 2.361(5) 1_645 ?
Cd1 O7 2.404(5) 1_645 ?
Cd1 O2 2.475(5) . ?
Cd1 Cl1 2.5012(19) 1_655 ?
Cd1 C9 2.702(6) . ?
Cd1 C36 2.702(7) 1_645 ?
Cd2 O3 2.241(5) . ?
Cd2 N17 2.291(5) 1_654 ?
Cd2 N7 2.376(5) . ?
Cd2 N5 2.447(5) 1_455 ?
Cd2 Cl2 2.5979(18) . ?
Cd2 Cl1 2.6349(19) . ?
Cd3 O4 2.225(5) . ?
Cd3 N8 2.331(5) . ?
Cd3 N10 2.340(5) . ?
Cd3 N14 2.351(5) . ?
Cd3 Cl3 2.6127(18) . ?
Cd3 Cl2 2.6227(17) . ?
Cd4 O9 2.255(5) 1_655 ?
Cd4 N2 2.338(5) 1_456 ?
Cd4 N13 2.411(5) . ?
Cd4 N11 2.425(5) . ?
Cd4 Cl3 2.5459(18) . ?
Cd4 Cl4 2.5860(18) . ?
Cd5 O12 2.180(4) . ?
Cd5 O10 2.221(5) . ?
Cd5 O5 2.300(5) 1_465 ?
Cd5 Cl4 2.4962(17) 1_455 ?
Cd5 O6 2.511(5) 1_465 ?
Cd5 C27 2.738(6) 1_465 ?
Cd5 Cl4 2.9124(19) 2_476 ?
Cl1 Cd1 2.5012(19) 1_455 ?
Cl4 Cd5 2.4962(17) 1_655 ?
Cl4 Cd5 2.9123(19) 2_476 ?
N1 C1 1.282(9) . ?
N1 N2 1.367(8) . ?
N2 C2 1.273(8) . ?
N2 Cd4 2.338(5) 1_654 ?
N3 C1 1.341(9) . ?
N3 C2 1.354(8) . ?
N3 C3 1.450(8) . ?
N4 C10 1.314(8) . ?
N4 N5 1.368(7) . ?
N5 C11 1.300(9) . ?
N5 Cd2 2.447(5) 1_655 ?
N6 C11 1.355(8) . ?
N6 C10 1.361(9) . ?
N6 C12 1.439(8) . ?
N7 C19 1.298(8) . ?
N7 N8 1.368(7) . ?
N8 C20 1.304(8) . ?
N9 C20 1.355(8) . ?
N9 C19 1.371(8) . ?
N9 C21 1.441(8) . ?
N10 C29 1.310(7) . ?
N10 N11 1.370(7) . ?
N11 C28 1.311(8) . ?
N12 C29 1.358(8) . ?
N12 C28 1.362(8) . ?
N12 C30 1.438(7) . ?
N13 C38 1.283(8) . ?
N13 N14 1.384(6) . ?
N14 C37 1.331(8) . ?
N15 C37 1.344(8) . ?
N15 C38 1.361(8) . ?
N15 C39 1.444(7) . ?
N16 C46 1.273(9) . ?
N16 N17 1.392(8) . ?
N17 C47 1.279(8) . ?
N17 Cd2 2.291(5) 1_456 ?
N18 C47 1.355(8) . ?
N18 C46 1.363(9) . ?
N18 C48 1.428(8) . ?
C3 C8 1.364(10) . ?
C3 C4 1.375(10) . ?
C4 C5 1.375(9) . ?
C5 C6 1.395(9) . ?
C6 C7 1.392(10) . ?
C6 C9 1.509(9) . ?
C7 C8 1.384(10) . ?
C9 O2 1.245(9) . ?
C9 O1 1.256(8) . ?
C12 C13 1.356(11) . ?
C12 C17 1.360(11) . ?
C13 C14 1.385(11) . ?
C14 C15 1.379(10) . ?
C15 C16 1.360(11) . ?
C15 C18 1.521(9) . ?
C16 C17 1.375(11) . ?
C18 O4 1.205(8) . ?
C18 O3 1.243(8) . ?
C21 C22 1.364(10) . ?
C21 C26 1.368(10) . ?
C22 C23 1.399(9) . ?
C23 C24 1.358(10) . ?
C24 C25 1.385(9) . ?
C24 C27 1.505(8) . ?
C25 C26 1.382(9) . ?
C27 O6 1.247(8) . ?
C27 O5 1.262(8) . ?
C27 Cd5 2.738(6) 1_645 ?
C30 C31 1.363(9) . ?
C30 C35 1.372(10) . ?
C31 C32 1.390(9) . ?
C32 C33 1.378(10) . ?
C33 C34 1.389(10) . ?
C33 C36 1.523(9) . ?
C34 C35 1.383(9) . ?
C36 O7 1.226(9) . ?
C36 O8 1.239(9) . ?
C36 Cd1 2.702(7) 1_465 ?
C39 C40 1.362(9) . ?
C39 C44 1.390(9) . ?
C40 C41 1.380(9) . ?
C41 C42 1.394(9) . ?
C42 C43 1.382(10) . ?
C42 C45 1.511(8) . ?
C43 C44 1.392(9) . ?
C45 O9 1.236(8) . ?
C45 O10 1.254(8) . ?
C48 C53 1.384(10) . ?
C48 C49 1.386(9) . ?
C49 C50 1.390(9) . ?
C50 C51 1.373(10) . ?
C51 C52 1.394(9) . ?
C51 C54 1.515(9) . ?
C52 C53 1.377(9) . ?
C54 O11 1.233(9) . ?
C54 O12 1.270(8) . ?
O5 Cd5 2.300(4) 1_645 ?
O6 Cd5 2.511(5) 1_645 ?
O7 Cd1 2.404(5) 1_465 ?
O8 Cd1 2.361(5) 1_465 ?
O9 Cd4 2.255(4) 1_455 ?
C1E N1E 1.45(2) . ?
C2E N1E 1.49(2) . ?
C3E O1E 1.11(2) . ?
C3E N1E 1.26(2) . ?
C1R N1R 1.24(3) . ?
C2R N1R 1.37(2) . ?
C3R O1R 1.11(3) . ?
C3R N1R 1.34(3) . ?
C1T N1T 1.37(3) . ?
C2T N1T 1.60(4) . ?
C3T O1T 1.25(3) . ?
C3T N1T 1.34(3) . ?
O1W O2W 1.349(14) . ?
O3W O12W 0.99(3) . ?
O3W O4W 1.31(3) . ?
O4W O12W 1.35(4) . ?
O5W O6W 1.28(2) . ?
O7W O8W 1.38(4) 2_765 ?
O8W O7W 1.38(4) 2_765 ?

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
O1 Cd1 N4 134.23(19) . . ?
O1 Cd1 O8 82.06(19) . 1_645 ?
N4 Cd1 O8 95.6(2) . 1_645 ?
O1 Cd1 O7 114.1(2) . 1_645 ?
N4 Cd1 O7 100.1(2) . 1_645 ?
O8 Cd1 O7 54.1(2) 1_645 1_645 ?
O1 Cd1 O2 54.89(17) . . ?
N4 Cd1 O2 91.80(19) . . ?
O8 Cd1 O2 123.41(18) 1_645 . ?
O7 Cd1 O2 168.0(2) 1_645 . ?
O1 Cd1 Cl1 116.52(15) . 1_655 ?
N4 Cd1 Cl1 91.32(13) . 1_655 ?
O8 Cd1 Cl1 144.74(15) 1_645 1_655 ?
O7 Cd1 Cl1 90.68(16) 1_645 1_655 ?
O2 Cd1 Cl1 90.75(13) . 1_655 ?
O1 Cd1 C9 27.5(2) . . ?
N4 Cd1 C9 113.5(2) . . ?
O8 Cd1 C9 102.7(2) 1_645 . ?
O7 Cd1 C9 141.6(2) 1_645 . ?
O2 Cd1 C9 27.40(19) . . ?
Cl1 Cd1 C9 106.00(15) 1_655 . ?
O1 Cd1 C36 97.0(2) . 1_645 ?
N4 Cd1 C36 101.1(2) . 1_645 ?
O8 Cd1 C36 27.3(2) 1_645 1_645 ?
O7 Cd1 C36 27.0(2) 1_645 1_645 ?
O2 Cd1 C36 148.3(2) . 1_645 ?
Cl1 Cd1 C36 117.50(18) 1_655 1_645 ?
C9 Cd1 C36 122.9(2) . 1_645 ?
O3 Cd2 N17 92.1(2) . 1_654 ?
O3 Cd2 N7 92.9(2) . . ?
N17 Cd2 N7 174.03(19) 1_654 . ?
O3 Cd2 N5 171.1(2) . 1_455 ?
N17 Cd2 N5 90.1(2) 1_654 1_455 ?
N7 Cd2 N5 84.40(19) . 1_455 ?
O3 Cd2 Cl2 99.21(15) . . ?
N17 Cd2 Cl2 93.22(15) 1_654 . ?
N7 Cd2 Cl2 89.13(14) . . ?
N5 Cd2 Cl2 89.28(14) 1_455 . ?
O3 Cd2 Cl1 84.43(16) . . ?
N17 Cd2 Cl1 89.80(15) 1_654 . ?
N7 Cd2 Cl1 87.51(14) . . ?
N5 Cd2 Cl1 86.95(14) 1_455 . ?
Cl2 Cd2 Cl1 175.17(6) . . ?
O4 Cd3 N8 91.3(2) . . ?
O4 Cd3 N10 87.8(2) . . ?
N8 Cd3 N10 178.04(18) . . ?
O4 Cd3 N14 172.2(2) . . ?
N8 Cd3 N14 95.3(2) . . ?
N10 Cd3 N14 85.43(19) . . ?
O4 Cd3 Cl3 87.94(16) . . ?
N8 Cd3 Cl3 87.94(14) . . ?
N10 Cd3 Cl3 90.28(13) . . ?
N14 Cd3 Cl3 88.18(13) . . ?
O4 Cd3 Cl2 96.57(15) . . ?
N8 Cd3 Cl2 87.36(14) . . ?
N10 Cd3 Cl2 94.48(13) . . ?
N14 Cd3 Cl2 87.87(13) . . ?
Cl3 Cd3 Cl2 173.56(6) . . ?
O9 Cd4 N2 90.0(2) 1_655 1_456 ?
O9 Cd4 N13 174.14(19) 1_655 . ?
N2 Cd4 N13 95.9(2) 1_456 . ?
O9 Cd4 N11 90.1(2) 1_655 . ?
N2 Cd4 N11 174.11(19) 1_456 . ?
N13 Cd4 N11 84.08(18) . . ?
O9 Cd4 Cl3 91.74(15) 1_655 . ?
N2 Cd4 Cl3 95.32(15) 1_456 . ?
N13 Cd4 Cl3 87.47(13) . . ?
N11 Cd4 Cl3 90.56(13) . . ?
O9 Cd4 Cl4 93.45(14) 1_655 . ?
N2 Cd4 Cl4 85.01(15) 1_456 . ?
N13 Cd4 Cl4 87.34(13) . . ?
N11 Cd4 Cl4 89.11(13) . . ?
Cl3 Cd4 Cl4 174.80(6) . . ?
O12 Cd5 O10 111.2(2) . . ?
O12 Cd5 O5 84.59(18) . 1_465 ?
O10 Cd5 O5 95.21(19) . 1_465 ?
O12 Cd5 Cl4 115.57(15) . 1_455 ?
O10 Cd5 Cl4 100.90(15) . 1_455 ?
O5 Cd5 Cl4 146.68(13) 1_465 1_455 ?
O12 Cd5 O6 135.70(17) . 1_465 ?
O10 Cd5 O6 90.3(2) . 1_465 ?
O5 Cd5 O6 54.28(16) 1_465 1_465 ?
Cl4 Cd5 O6 96.37(13) 1_455 1_465 ?
O12 Cd5 C27 110.25(19) . 1_465 ?
O10 Cd5 C27 94.0(2) . 1_465 ?
O5 Cd5 C27 27.28(18) 1_465 1_465 ?
Cl4 Cd5 C27 121.69(15) 1_455 1_465 ?
O6 Cd5 C27 27.03(17) 1_465 1_465 ?
O12 Cd5 Cl4 75.82(16) . 2_476 ?
O10 Cd5 Cl4 172.94(16) . 2_476 ?
O5 Cd5 Cl4 84.36(13) 1_465 2_476 ?
Cl4 Cd5 Cl4 76.14(6) 1_455 2_476 ?
O6 Cd5 Cl4 83.67(14) 1_465 2_476 ?
C27 Cd5 Cl4 82.33(15) 1_465 2_476 ?
Cd1 Cl1 Cd2 109.06(7) 1_455 . ?
Cd2 Cl2 Cd3 93.09(5) . . ?
Cd4 Cl3 Cd3 95.04(6) . . ?
Cd5 Cl4 Cd4 110.55(6) 1_655 . ?
Cd5 Cl4 Cd5 103.86(6) 1_655 2_476 ?
Cd4 Cl4 Cd5 145.26(7) . 2_476 ?
C1 N1 N2 104.7(6) . . ?
C2 N2 N1 108.5(5) . . ?
C2 N2 Cd4 125.6(4) . 1_654 ?
N1 N2 Cd4 125.9(4) . 1_654 ?
C1 N3 C2 102.2(6) . . ?
C1 N3 C3 128.7(6) . . ?
C2 N3 C3 129.1(6) . . ?
C10 N4 N5 107.8(5) . . ?
C10 N4 Cd1 124.4(4) . . ?
N5 N4 Cd1 127.5(4) . . ?
C11 N5 N4 107.3(5) . . ?
C11 N5 Cd2 127.7(4) . 1_655 ?
N4 N5 Cd2 125.0(4) . 1_655 ?
C11 N6 C10 105.0(6) . . ?
C11 N6 C12 128.9(6) . . ?
C10 N6 C12 126.0(6) . . ?
C19 N7 N8 108.2(5) . . ?
C19 N7 Cd2 130.7(4) . . ?
N8 N7 Cd2 120.1(3) . . ?
C20 N8 N7 107.5(5) . . ?
C20 N8 Cd3 131.3(4) . . ?
N7 N8 Cd3 121.1(3) . . ?
C20 N9 C19 105.2(5) . . ?
C20 N9 C21 127.4(5) . . ?
C19 N9 C21 127.4(6) . . ?
C29 N10 N11 107.9(5) . . ?
C29 N10 Cd3 130.0(4) . . ?
N11 N10 Cd3 122.0(3) . . ?
C28 N11 N10 107.3(5) . . ?
C28 N11 Cd4 133.2(4) . . ?
N10 N11 Cd4 119.5(3) . . ?
C29 N12 C28 105.3(5) . . ?
C29 N12 C30 127.3(5) . . ?
C28 N12 C30 127.3(5) . . ?
C38 N13 N14 108.1(5) . . ?
C38 N13 Cd4 130.8(4) . . ?
N14 N13 Cd4 120.4(4) . . ?
C37 N14 N13 105.9(5) . . ?
C37 N14 Cd3 133.0(4) . . ?
N13 N14 Cd3 120.7(4) . . ?
C37 N15 C38 105.1(5) . . ?
C37 N15 C39 127.5(5) . . ?
C38 N15 C39 127.4(5) . . ?
C46 N16 N17 105.7(6) . . ?
C47 N17 N16 107.7(5) . . ?
C47 N17 Cd2 126.5(4) . 1_456 ?
N16 N17 Cd2 125.7(4) . 1_456 ?
C47 N18 C46 103.0(5) . . ?
C47 N18 C48 127.2(6) . . ?
C46 N18 C48 129.8(6) . . ?
N1 C1 N3 113.5(7) . . ?
N2 C2 N3 111.0(6) . . ?
C8 C3 C4 121.0(6) . . ?
C8 C3 N3 119.2(6) . . ?
C4 C3 N3 119.8(6) . . ?
C5 C4 C3 120.7(7) . . ?
C4 C5 C6 119.1(7) . . ?
C5 C6 C7 119.5(6) . . ?
C5 C6 C9 120.0(6) . . ?
C7 C6 C9 120.5(6) . . ?
C8 C7 C6 120.4(7) . . ?
C3 C8 C7 119.3(7) . . ?
O2 C9 O1 122.5(6) . . ?
O2 C9 C6 119.4(6) . . ?
O1 C9 C6 118.1(6) . . ?
O2 C9 Cd1 66.1(4) . . ?
O1 C9 Cd1 56.5(3) . . ?
C6 C9 Cd1 172.9(5) . . ?
N4 C10 N6 109.3(6) . . ?
N5 C11 N6 110.6(6) . . ?
C13 C12 C17 121.9(7) . . ?
C13 C12 N6 120.2(6) . . ?
C17 C12 N6 117.8(7) . . ?
C12 C13 C14 118.8(7) . . ?
C15 C14 C13 120.5(8) . . ?
C16 C15 C14 118.1(7) . . ?
C16 C15 C18 121.9(6) . . ?
C14 C15 C18 119.7(7) . . ?
C15 C16 C17 122.0(8) . . ?
C12 C17 C16 118.1(8) . . ?
O4 C18 O3 128.2(7) . . ?
O4 C18 C15 116.1(6) . . ?
O3 C18 C15 115.7(6) . . ?
N7 C19 N9 109.2(6) . . ?
N8 C20 N9 109.9(6) . . ?
C22 C21 C26 120.9(6) . . ?
C22 C21 N9 119.4(6) . . ?
C26 C21 N9 119.7(6) . . ?
C21 C22 C23 118.8(7) . . ?
C24 C23 C22 120.7(7) . . ?
C23 C24 C25 119.8(6) . . ?
C23 C24 C27 120.4(6) . . ?
C25 C24 C27 119.8(6) . . ?
C26 C25 C24 119.6(6) . . ?
C21 C26 C25 120.0(6) . . ?
O6 C27 O5 122.8(6) . . ?
O6 C27 C24 119.9(6) . . ?
O5 C27 C24 117.3(6) . . ?
O6 C27 Cd5 66.3(3) . 1_645 ?
O5 C27 Cd5 56.6(3) . 1_645 ?
C24 C27 Cd5 173.5(5) . 1_645 ?
N11 C28 N12 109.8(6) . . ?
N10 C29 N12 109.6(5) . . ?
C31 C30 C35 121.8(6) . . ?
C31 C30 N12 118.8(6) . . ?
C35 C30 N12 119.4(6) . . ?
C30 C31 C32 119.1(7) . . ?
C33 C32 C31 120.8(6) . . ?
C32 C33 C34 118.6(6) . . ?
C32 C33 C36 120.8(6) . . ?
C34 C33 C36 120.6(7) . . ?
C35 C34 C33 121.0(7) . . ?
C30 C35 C34 118.7(7) . . ?
O7 C36 O8 123.0(6) . . ?
O7 C36 C33 119.3(7) . . ?
O8 C36 C33 117.7(7) . . ?
O7 C36 Cd1 62.8(4) . 1_465 ?
O8 C36 Cd1 60.8(4) . 1_465 ?
C33 C36 Cd1 171.4(5) . 1_465 ?
N14 C37 N15 110.2(6) . . ?
N13 C38 N15 110.7(5) . . ?
C40 C39 C44 122.0(6) . . ?
C40 C39 N15 118.8(6) . . ?
C44 C39 N15 119.2(6) . . ?
C39 C40 C41 119.9(6) . . ?
C40 C41 C42 119.7(6) . . ?
C43 C42 C41 119.8(6) . . ?
C43 C42 C45 120.2(6) . . ?
C41 C42 C45 120.0(6) . . ?
C42 C43 C44 120.8(7) . . ?
C39 C44 C43 117.8(6) . . ?
O9 C45 O10 127.3(6) . . ?
O9 C45 C42 116.8(6) . . ?
O10 C45 C42 115.9(6) . . ?
N16 C46 N18 112.5(6) . . ?
N17 C47 N18 111.1(6) . . ?
C53 C48 C49 121.7(6) . . ?
C53 C48 N18 118.7(6) . . ?
C49 C48 N18 119.6(6) . . ?
C50 C49 C48 118.5(6) . . ?
C51 C50 C49 120.4(6) . . ?
C50 C51 C52 120.0(6) . . ?
C50 C51 C54 121.0(6) . . ?
C52 C51 C54 119.0(6) . . ?
C53 C52 C51 120.4(7) . . ?
C52 C53 C48 118.8(6) . . ?
O11 C54 O12 124.8(6) . . ?
O11 C54 C51 121.1(6) . . ?
O12 C54 C51 114.0(6) . . ?
C9 O1 Cd1 95.9(4) . . ?
C9 O2 Cd1 86.5(4) . . ?
C18 O3 Cd2 130.0(5) . . ?
C18 O4 Cd3 140.6(5) . . ?
C27 O5 Cd5 96.1(4) . 1_645 ?
C27 O6 Cd5 86.7(4) . 1_645 ?
C36 O7 Cd1 90.2(4) . 1_465 ?
C36 O8 Cd1 91.9(5) . 1_465 ?
C45 O9 Cd4 142.7(5) . 1_455 ?
C45 O10 Cd5 134.3(5) . . ?
C54 O12 Cd5 116.3(4) . . ?
O1E C3E N1E 133(2) . . ?
C3E N1E C1E 119.0(16) . . ?
C3E N1E C2E 122.2(16) . . ?
C1E N1E C2E 118.8(16) . . ?
O1R C3R N1R 133(2) . . ?
C1R N1R C3R 117(2) . . ?
C1R N1R C2R 115(2) . . ?
C3R N1R C2R 128.6(19) . . ?
O1T C3T N1T 124(3) . . ?
C1T N1T C3T 121(3) . . ?
C1T N1T C2T 119(2) . . ?
C3T N1T C2T 119(3) . . ?
O12W O3W O4W 70(3) . . ?
O3W O4W O12W 43.6(17) . . ?
O3W O12W O4W 66(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.158
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1422293'
_audit_update_record             
;
2015-09-04 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.100 0.250 532 134 ' '
2 0.500 -0.397 0.250 532 135 ' '
3 0.000 -0.100 0.750 531 133 ' '
4 0.500 0.397 0.750 531 134 ' '
_platon_squeeze_details          
;
Highly Disordered solvent (DMA and H₂O) molecules were not determined
and the contributions of these disordered solvent molecules to 
the scattering values have been removed by using the PLATON SQUEEZE 
program. TGA and elemental analyses reveal that it contains one DMA and 
3.5 water molecules per molecular unit. Then, the formula can be get 
as [Zn(C₁₈H₁₂N₆O₄)]DMA.3.5H₂O.  
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H28 N7 O8.5 Zn'
_chemical_formula_weight         591.89

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   20.0621(18)
_cell_length_b                   15.5930(14)
_cell_length_c                   17.2349(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5391.6(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7661
_exptl_absorpt_correction_T_max  0.8202
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30975
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5303
_reflns_number_gt                4117
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'

_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)+(0.0656P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5303
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.003
_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
Zn1 Zn 0.288681(13) 0.022949(17) 1.005930(15) 0.02862(11) Uani 1 1 d . . .
N1 N 0.37903(9) 0.07352(13) 1.03332(12) 0.0346(5) Uani 1 1 d . . .
N2 N 0.42489(11) 0.02179(15) 1.07067(15) 0.0541(7) Uani 1 1 d . . .
N3 N 0.47141(9) 0.14512(14) 1.04250(12) 0.0380(5) Uani 1 1 d . . .
N4 N 0.30741(10) -0.03512(13) 0.90142(12) 0.0345(5) Uani 1 1 d . . .
N5 N 0.36010(11) -0.01949(14) 0.85269(12) 0.0431(5) Uani 1 1 d . . .
N6 N 0.30405(10) -0.13131(13) 0.81088(12) 0.0353(5) Uani 1 1 d . . .
C1 C 0.40783(12) 0.14605(18) 1.01731(15) 0.0385(6) Uani 1 1 d . . .
H1A H 0.3875 0.1919 0.9922 0.046 Uiso 1 1 calc R . .
C2 C 0.47897(13) 0.0668(2) 1.07508(18) 0.0560(8) Uani 1 1 d . . .
H2A H 0.5182 0.0476 1.0979 0.067 Uiso 1 1 calc R . .
C3 C 0.52162(12) 0.21106(17) 1.03566(15) 0.0394(6) Uani 1 1 d . . .
C4 C 0.50553(13) 0.29475(18) 1.0499(2) 0.0585(9) Uani 1 1 d . . .
H4A H 0.4621 0.3098 1.0633 0.070 Uiso 1 1 calc R . .
C5 C 0.55461(14) 0.3569(2) 1.0444(2) 0.0620(9) Uani 1 1 d . . .
H5A H 0.5441 0.4141 1.0538 0.074 Uiso 1 1 calc R . .
C6 C 0.61904(13) 0.33452(17) 1.02491(16) 0.0417(6) Uani 1 1 d . . .
C7 C 0.63403(13) 0.24952(19) 1.01032(16) 0.0456(7) Uani 1 1 d . . .
H7A H 0.6773 0.2341 0.9969 0.055 Uiso 1 1 calc R . .
C8 C 0.58516(13) 0.18708(18) 1.01552(16) 0.0459(7) Uani 1 1 d . . .
H8A H 0.5952 0.1299 1.0055 0.055 Uiso 1 1 calc R . .
C9 C 0.67249(14) 0.4027(2) 1.02050(18) 0.0505(7) Uani 1 1 d . . .
C10 C 0.27490(12) -0.10178(17) 0.87553(15) 0.0383(6) Uani 1 1 d . . .
H10A H 0.2371 -0.1253 0.8985 0.046 Uiso 1 1 calc R . .
C11 C 0.35625(14) -0.07748(18) 0.79871(15) 0.0464(7) Uani 1 1 d . . .
H11A H 0.3855 -0.0816 0.7570 0.056 Uiso 1 1 calc R . .
C12 C 0.28521(12) -0.20575(16) 0.76635(14) 0.0370(6) Uani 1 1 d . . .
C13 C 0.29008(13) -0.20263(18) 0.68614(15) 0.0430(6) Uani 1 1 d . . .
H13A H 0.3039 -0.1528 0.6612 0.052 Uiso 1 1 calc R . .
C14 C 0.27397(13) -0.27503(17) 0.64406(15) 0.0418(6) Uani 1 1 d . . .
H14A H 0.2770 -0.2739 0.5902 0.050 Uiso 1 1 calc R . .
C15 C 0.25337(13) -0.34929(16) 0.68099(14) 0.0384(6) Uani 1 1 d . . .
C16 C 0.24851(16) -0.35006(18) 0.76057(15) 0.0500(7) Uani 1 1 d . . .
H16A H 0.2342 -0.3996 0.7856 0.060 Uiso 1 1 calc R . .
C17 C 0.26451(15) -0.27845(18) 0.80398(15) 0.0493(7) Uani 1 1 d . . .
H17A H 0.2613 -0.2796 0.8578 0.059 Uiso 1 1 calc R . .
C18 C 0.23596(13) -0.42877(17) 0.63439(16) 0.0422(6) Uani 1 1 d . . .
O2 O 0.65832(12) 0.47763(15) 1.03259(19) 0.0890(9) Uani 1 1 d . . .
O1 O 0.73053(9) 0.37746(13) 1.00289(10) 0.0475(5) Uani 1 1 d . . .
O3 O 0.22946(9) -0.41796(12) 0.56205(10) 0.0448(5) Uani 1 1 d . . .
O4 O 0.22885(14) -0.49768(14) 0.66693(13) 0.0771(7) Uani 1 1 d . . .


_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
Zn1 O3 1.9360(17) 2_545 ?
Zn1 O1 1.9483(18) 4_457 ?
Zn1 N1 2.0322(18) . ?
Zn1 N4 2.051(2) . ?
N1 C1 1.300(3) . ?
N1 N2 1.383(3) . ?
N2 C2 1.294(3) . ?
N3 C1 1.348(3) . ?
N3 C2 1.353(3) . ?
N3 C3 1.444(3) . ?
N4 C10 1.306(3) . ?
N4 N5 1.372(3) . ?
N5 C11 1.300(3) . ?
N6 C10 1.340(3) . ?
N6 C11 1.358(3) . ?
N6 C12 1.442(3) . ?
C3 C4 1.367(4) . ?
C3 C8 1.373(4) . ?
C4 C5 1.385(4) . ?
C5 C6 1.380(4) . ?
C6 C7 1.382(4) . ?
C6 C9 1.512(4) . ?
C7 C8 1.385(4) . ?
C9 O2 1.221(4) . ?
C9 O1 1.266(4) . ?
C12 C17 1.371(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.380(4) . ?
C14 C15 1.385(3) . ?
C15 C16 1.375(4) . ?
C15 C18 1.518(3) . ?
C16 C17 1.382(4) . ?
C18 O4 1.220(3) . ?
C18 O3 1.265(3) . ?
O1 Zn1 1.9483(18) 4_557 ?
O3 Zn1 1.9360(17) 2_544 ?

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
O3 Zn1 O1 126.90(8) 2_545 4_457 ?
O3 Zn1 N1 112.32(8) 2_545 . ?
O1 Zn1 N1 104.06(9) 4_457 . ?
O3 Zn1 N4 95.73(8) 2_545 . ?
O1 Zn1 N4 113.15(8) 4_457 . ?
N1 Zn1 N4 102.23(8) . . ?
C1 N1 N2 108.10(19) . . ?
C1 N1 Zn1 133.23(17) . . ?
N2 N1 Zn1 118.38(15) . . ?
C2 N2 N1 105.6(2) . . ?
C1 N3 C2 104.4(2) . . ?
C1 N3 C3 128.8(2) . . ?
C2 N3 C3 126.8(2) . . ?
C10 N4 N5 108.5(2) . . ?
C10 N4 Zn1 124.06(18) . . ?
N5 N4 Zn1 126.90(15) . . ?
C11 N5 N4 105.6(2) . . ?
C10 N6 C11 104.6(2) . . ?
C10 N6 C12 127.2(2) . . ?
C11 N6 C12 128.1(2) . . ?
N1 C1 N3 110.1(2) . . ?
N2 C2 N3 111.8(2) . . ?
C4 C3 C8 121.7(2) . . ?
C4 C3 N3 120.0(2) . . ?
C8 C3 N3 118.3(2) . . ?
C3 C4 C5 119.2(3) . . ?
C6 C5 C4 120.3(3) . . ?
C5 C6 C7 119.4(2) . . ?
C5 C6 C9 119.9(3) . . ?
C7 C6 C9 120.7(2) . . ?
C6 C7 C8 120.6(2) . . ?
C3 C8 C7 118.8(3) . . ?
O2 C9 O1 123.5(3) . . ?
O2 C9 C6 120.0(3) . . ?
O1 C9 C6 116.5(3) . . ?
N4 C10 N6 109.9(2) . . ?
N5 C11 N6 111.4(2) . . ?
C17 C12 C13 121.5(2) . . ?
C17 C12 N6 119.6(2) . . ?
C13 C12 N6 118.9(2) . . ?
C14 C13 C12 118.6(3) . . ?
C13 C14 C15 120.8(2) . . ?
C16 C15 C14 119.1(2) . . ?
C16 C15 C18 120.3(2) . . ?
C14 C15 C18 120.6(2) . . ?
C15 C16 C17 121.1(3) . . ?
C12 C17 C16 118.9(2) . . ?
O4 C18 O3 123.9(3) . . ?
O4 C18 C15 120.2(3) . . ?
O3 C18 C15 115.9(2) . . ?
C9 O1 Zn1 108.78(19) . 4_557 ?
C18 O3 Zn1 113.52(17) . 2_544 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.068
