# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_cc
_database_code_depnum_ccdc_archive 'CCDC 901623'
_audit_update_record             
;
2012-09-16 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

#============================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H5 Cd N9, O'
_chemical_formula_sum            'C4 H5 Cd N9 O'
_chemical_formula_weight         307.58

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  -R3

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

_cell_length_a                   20.8197(13)
_cell_length_b                   20.8197(13)
_cell_length_c                   11.5581(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4338.8(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       rodlike
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_process_details   'Apex2 (Bruker, 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7453
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.19
_reflns_number_total             1733
_reflns_number_gt                1649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_cell_refinement       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'Apex2 (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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)+(0.0480P)²+14.0629P] 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         1737
_refine_ls_number_parameters     136
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0789
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.002
_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
C1 C 0.1889(2) 0.9646(2) 0.1081(3) 0.0317(9) Uani 1 1 d U . .
H1A H 0.2258 1.0101 0.1450 0.038 Uiso 1 1 calc R . .
H1B H 0.1415 0.9627 0.1130 0.038 Uiso 1 1 calc R . .
C2 C 0.2537(2) 0.9168(2) 0.2279(3) 0.0322(9) Uani 1 1 d U . .
H2A H 0.2423 0.8918 0.3021 0.039 Uiso 1 1 calc R . .
H2B H 0.2834 0.9697 0.2422 0.039 Uiso 1 1 calc R . .
C3 C 0.2091(2) 0.96605(19) -0.0170(3) 0.0224(7) Uani 1 1 d U . .
C4 C 0.29769(18) 0.89246(19) 0.1573(3) 0.0222(7) Uani 1 1 d U . .
Cd1 Cd 0.462625(12) 0.983782(13) 0.30224(2) 0.01863(13) Uani 1 1 d U . .
N1 N 0.18426(15) 0.90099(16) 0.1706(2) 0.0213(6) Uani 1 1 d U . .
H1 H 0.1484 0.8867 0.2257 0.026 Uiso 1 1 calc R . .
N2 N 0.25481(17) 1.02608(16) -0.0758(3) 0.0239(6) Uani 1 1 d U . .
N3 N 0.25285(18) 1.00393(16) -0.1857(3) 0.0272(7) Uani 1 1 d U . .
N4 N 0.20840(16) 0.93254(15) -0.1898(2) 0.0226(6) Uani 1 1 d U . .
N5 N 0.17908(17) 0.90622(16) -0.0840(3) 0.0239(6) Uani 1 1 d U . .
N6 N 0.26981(16) 0.84697(17) 0.0670(3) 0.0240(6) Uani 1 1 d U . .
N7 N 0.32421(18) 0.83470(18) 0.0299(3) 0.0306(7) Uani 1 1 d U . .
N8 N 0.38271(18) 0.87177(19) 0.0949(3) 0.0310(7) Uani 1 1 d U . .
N9 N 0.36736(16) 0.90907(17) 0.1769(3) 0.0257(7) Uani 1 1 d U . .
O1W O 0.4199(12) 0.6603(13) 0.4001(16) 0.414(12) Uani 1 1 d U . .


_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
C1 N1 1.469(5) . ?
C1 C3 1.501(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.470(5) . ?
C2 C4 1.492(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.319(5) . ?
C3 N5 1.328(4) . ?
C4 N6 1.331(5) . ?
C4 N9 1.332(5) . ?
Cd1 N6 2.291(3) 14_455 ?
Cd1 N4 2.316(3) 8_665 ?
Cd1 N9 2.316(3) . ?
Cd1 N2 2.331(3) 6_465 ?
Cd1 N5 2.433(3) 14_455 ?
Cd1 N1 2.504(3) 14_455 ?
N1 Cd1 2.504(3) 15 ?
N1 H1 0.9100 . ?
N2 N3 1.345(4) . ?
N2 Cd1 2.331(3) 8_664 ?
N3 N4 1.301(4) . ?
N4 N5 1.355(4) . ?
N4 Cd1 2.315(3) 6_464 ?
N5 Cd1 2.433(3) 15 ?
N6 N7 1.350(4) . ?
N6 Cd1 2.291(3) 15 ?
N7 N8 1.305(5) . ?
N8 N9 1.361(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 C1 C3 112.5(3) . . ?
N1 C1 H1A 109.1 . . ?
C3 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C3 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N1 C2 C4 112.2(3) . . ?
N1 C2 H2A 109.2 . . ?
C4 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C4 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 N5 111.5(3) . . ?
N2 C3 C1 125.2(3) . . ?
N5 C3 C1 123.2(3) . . ?
N6 C4 N9 110.4(3) . . ?
N6 C4 C2 123.2(3) . . ?
N9 C4 C2 126.3(3) . . ?
N6 Cd1 N4 105.53(11) 14_455 8_665 ?
N6 Cd1 N9 88.04(11) 14_455 . ?
N4 Cd1 N9 99.52(11) 8_665 . ?
N6 Cd1 N2 153.51(11) 14_455 6_465 ?
N4 Cd1 N2 100.95(10) 8_665 6_465 ?
N9 Cd1 N2 87.29(10) . 6_465 ?
N6 Cd1 N5 86.37(10) 14_455 14_455 ?
N4 Cd1 N5 86.23(10) 8_665 14_455 ?
N9 Cd1 N5 172.89(10) . 14_455 ?
N2 Cd1 N5 95.77(10) 6_465 14_455 ?
N6 Cd1 N1 71.48(10) 14_455 14_455 ?
N4 Cd1 N1 159.41(10) 8_665 14_455 ?
N9 Cd1 N1 100.72(10) . 14_455 ?
N2 Cd1 N1 83.82(10) 6_465 14_455 ?
N5 Cd1 N1 73.32(10) 14_455 14_455 ?
C1 N1 C2 113.9(3) . . ?
C1 N1 Cd1 108.5(2) . 15 ?
C2 N1 Cd1 109.7(2) . 15 ?
C1 N1 H1 108.2 . . ?
C2 N1 H1 108.2 . . ?
Cd1 N1 H1 108.2 15 . ?
C3 N2 N3 106.1(3) . . ?
C3 N2 Cd1 136.2(2) . 8_664 ?
N3 N2 Cd1 116.1(2) . 8_664 ?
N4 N3 N2 108.0(3) . . ?
N3 N4 N5 110.4(3) . . ?
N3 N4 Cd1 119.7(2) . 6_464 ?
N5 N4 Cd1 129.9(2) . 6_464 ?
C3 N5 N4 104.0(3) . . ?
C3 N5 Cd1 110.2(2) . 15 ?
N4 N5 Cd1 137.2(2) . 15 ?
C4 N6 N7 106.0(3) . . ?
C4 N6 Cd1 117.5(2) . 15 ?
N7 N6 Cd1 135.6(2) . 15 ?
N8 N7 N6 109.2(3) . . ?
N7 N8 N9 108.8(3) . . ?
C4 N9 N8 105.6(3) . . ?
C4 N9 Cd1 137.5(2) . . ?
N8 N9 Cd1 116.9(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.135
####################################################################### 
# 
# 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_v6
_database_code_depnum_ccdc_archive 'CCDC 901624'
_audit_update_record             
;
2012-09-16 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

#============================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 Cd2 N13 O'
_chemical_formula_sum            'C6 H7 Cd2 N13 O'
_chemical_formula_weight         502.07

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           monoclinic
_symmetry_space_group_name_H-M   p21/n
_symmetry_space_group_name_Hall  -p2yn

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

_cell_length_a                   9.8747(8)
_cell_length_b                   6.7895(6)
_cell_length_c                   17.9044(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9580(10)
_cell_angle_gamma                90.00
_cell_volume                     1174.34(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismy
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    3.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_T_max  0.334
_exptl_absorpt_process_details   'Apex2 (Bruker, 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5401
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.20
_reflns_number_total             2109
_reflns_number_gt                1692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_cell_refinement       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'Apex2 (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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)+(0.0243P)²+25.0525P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2099
_refine_ls_number_parameters     204
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1183
_refine_ls_wR_factor_gt          0.1028
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_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
C1 C 0.6262(10) -0.0637(15) 0.9201(5) 0.026(2) Uani 1 1 d . . .
C2 C 0.4843(11) -0.0515(16) 0.8699(6) 0.034(3) Uani 1 1 d . . .
H2A H 0.4655 -0.1685 0.8384 0.040 Uiso 1 1 calc R . .
H2B H 0.4147 -0.0413 0.9008 0.040 Uiso 1 1 calc R . .
C3 C 0.5768(12) 0.3158(16) 0.7344(6) 0.034(3) Uani 1 1 d . . .
C4 C 0.5587(12) 0.1095(16) 0.7620(6) 0.033(3) Uani 1 1 d . . .
H4A H 0.5093 0.0290 0.7205 0.039 Uiso 1 1 calc R . .
H4B H 0.6483 0.0496 0.7816 0.039 Uiso 1 1 calc R . .
C5 C 0.3139(11) 0.3506(17) 0.8534(6) 0.033(3) Uani 1 1 d . . .
C6 C 0.3406(12) 0.2050(19) 0.7958(8) 0.044(3) Uani 1 1 d . . .
H6A H 0.2729 0.0996 0.7903 0.053 Uiso 1 1 calc R . .
H6B H 0.3330 0.2686 0.7466 0.053 Uiso 1 1 calc R . .
Cd1 Cd 0.97631(8) 0.29535(11) 1.04981(4) 0.0264(3) Uani 1 1 d . . .
Cd2 Cd 0.65207(8) 0.42838(11) 0.91373(4) 0.0259(3) Uani 1 1 d . . .
N1 N 0.6941(10) 0.0960(12) 0.9501(5) 0.033(2) Uani 1 1 d . . .
N2 N 0.8155(9) 0.0286(13) 0.9911(5) 0.028(2) Uani 1 1 d . . .
N3 N 0.8181(9) -0.1622(13) 0.9859(5) 0.029(2) Uani 1 1 d . . .
N4 N 0.6964(9) -0.2278(13) 0.9411(5) 0.030(2) Uani 1 1 d . . .
N5 N 0.4810(9) 0.1244(13) 0.8216(5) 0.033(2) Uani 1 1 d . . .
N6 N 0.6112(9) 0.4664(13) 0.7826(5) 0.031(2) Uani 1 1 d . . .
N7 N 0.6089(10) 0.6267(14) 0.7375(5) 0.037(2) Uani 1 1 d . . .
N8 N 0.5717(11) 0.5755(14) 0.6661(5) 0.039(2) Uani 1 1 d . . .
N9 N 0.5490(9) 0.3769(12) 0.6623(5) 0.029(2) Uani 1 1 d . . .
N10 N 0.4107(10) 0.4371(14) 0.9073(5) 0.036(2) Uani 1 1 d . . .
N11 N 0.3396(10) 0.5606(14) 0.9435(6) 0.041(2) Uani 1 1 d . . .
N12 N 0.2114(9) 0.5512(13) 0.9112(5) 0.030(2) Uani 1 1 d . . .
N13 N 0.1880(10) 0.4207(15) 0.8544(6) 0.041(2) Uani 1 1 d . . .
O1 O 1.1105(7) 0.5711(10) 1.0674(4) 0.0241(15) Uani 1 1 d D . .
H1 H 1.073(11) 0.652(13) 1.091(6) 0.04(4) Uiso 1 1 d 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
C1 N4 1.325(13) . ?
C1 N1 1.328(13) . ?
C1 C2 1.502(13) . ?
C2 N5 1.470(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N9 1.329(14) . ?
C3 N6 1.336(14) . ?
C3 C4 1.509(15) . ?
C4 N5 1.441(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N13 1.335(14) . ?
C5 N10 1.344(14) . ?
C5 C6 1.491(16) . ?
C6 N5 1.473(14) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
Cd1 O1 2.277(7) . ?
Cd1 O1 2.284(7) 3_767 ?
Cd1 N9 2.311(9) 4_666 ?
Cd1 N12 2.355(9) 3_667 ?
Cd1 N3 2.426(8) 3_757 ?
Cd1 N2 2.493(9) . ?
Cd1 Cd1 3.3866(15) 3_767 ?
Cd2 O1 2.298(7) 3_767 ?
Cd2 N6 2.313(9) . ?
Cd2 N1 2.361(9) . ?
Cd2 N10 2.363(9) . ?
Cd2 N4 2.407(9) 1_565 ?
Cd2 N11 2.542(10) 3_667 ?
N1 N2 1.349(12) . ?
N2 N3 1.300(12) . ?
N3 N4 1.373(12) . ?
N3 Cd1 2.426(8) 3_757 ?
N4 Cd2 2.407(9) 1_545 ?
N6 N7 1.353(12) . ?
N7 N8 1.303(13) . ?
N8 N9 1.366(12) . ?
N9 Cd1 2.311(9) 4_565 ?
N10 N11 1.343(13) . ?
N11 N12 1.280(13) . ?
N11 Cd2 2.542(10) 3_667 ?
N12 N13 1.332(12) . ?
N12 Cd1 2.355(9) 3_667 ?
O1 Cd1 2.284(7) 3_767 ?
O1 Cd2 2.298(7) 3_767 ?
O1 H1 0.819(11) . ?

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
N4 C1 N1 112.4(9) . . ?
N4 C1 C2 125.8(10) . . ?
N1 C1 C2 121.8(9) . . ?
N5 C2 C1 107.6(9) . . ?
N5 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
N5 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
N9 C3 N6 111.3(9) . . ?
N9 C3 C4 126.4(10) . . ?
N6 C3 C4 122.0(10) . . ?
N5 C4 C3 107.2(9) . . ?
N5 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
N5 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.5 . . ?
N13 C5 N10 111.1(10) . . ?
N13 C5 C6 123.0(10) . . ?
N10 C5 C6 125.8(10) . . ?
N5 C6 C5 108.6(9) . . ?
N5 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N5 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 Cd1 O1 84.1(2) . 3_767 ?
O1 Cd1 N9 103.2(3) . 4_666 ?
O1 Cd1 N9 172.5(3) 3_767 4_666 ?
O1 Cd1 N12 93.8(3) . 3_667 ?
O1 Cd1 N12 85.9(3) 3_767 3_667 ?
N9 Cd1 N12 95.0(3) 4_666 3_667 ?
O1 Cd1 N3 81.3(3) . 3_757 ?
O1 Cd1 N3 94.6(3) 3_767 3_757 ?
N9 Cd1 N3 85.2(3) 4_666 3_757 ?
N12 Cd1 N3 175.0(3) 3_667 3_757 ?
O1 Cd1 N2 163.1(3) . . ?
O1 Cd1 N2 79.4(3) 3_767 . ?
N9 Cd1 N2 93.2(3) 4_666 . ?
N12 Cd1 N2 88.5(3) 3_667 . ?
N3 Cd1 N2 96.5(3) 3_757 . ?
O1 Cd1 Cd1 42.14(17) . 3_767 ?
O1 Cd1 Cd1 41.99(17) 3_767 3_767 ?
N9 Cd1 Cd1 145.3(2) 4_666 3_767 ?
N12 Cd1 Cd1 89.8(2) 3_667 3_767 ?
N3 Cd1 Cd1 87.3(2) 3_757 3_767 ?
N2 Cd1 Cd1 121.28(19) . 3_767 ?
O1 Cd2 N6 96.2(3) 3_767 . ?
O1 Cd2 N1 81.1(3) 3_767 . ?
N6 Cd2 N1 111.7(3) . . ?
O1 Cd2 N10 174.3(3) 3_767 . ?
N6 Cd2 N10 89.2(3) . . ?
N1 Cd2 N10 98.9(3) . . ?
O1 Cd2 N4 80.3(3) 3_767 1_565 ?
N6 Cd2 N4 94.9(3) . 1_565 ?
N1 Cd2 N4 148.9(3) . 1_565 ?
N10 Cd2 N4 97.2(3) . 1_565 ?
O1 Cd2 N11 91.9(3) 3_767 3_667 ?
N6 Cd2 N11 168.6(3) . 3_667 ?
N1 Cd2 N11 77.5(3) . 3_667 ?
N10 Cd2 N11 82.6(3) . 3_667 ?
N4 Cd2 N11 78.5(3) 1_565 3_667 ?
C1 N1 N2 105.1(8) . . ?
C1 N1 Cd2 128.6(7) . . ?
N2 N1 Cd2 124.0(7) . . ?
N3 N2 N1 109.2(8) . . ?
N3 N2 Cd1 137.2(6) . . ?
N1 N2 Cd1 113.6(6) . . ?
N2 N3 N4 109.6(8) . . ?
N2 N3 Cd1 114.8(7) . 3_757 ?
N4 N3 Cd1 113.8(6) . 3_757 ?
C1 N4 N3 103.7(8) . . ?
C1 N4 Cd2 134.0(7) . 1_545 ?
N3 N4 Cd2 122.2(6) . 1_545 ?
C4 N5 C2 115.3(9) . . ?
C4 N5 C6 113.9(9) . . ?
C2 N5 C6 113.0(9) . . ?
C3 N6 N7 105.0(8) . . ?
C3 N6 Cd2 122.6(7) . . ?
N7 N6 Cd2 132.3(7) . . ?
N8 N7 N6 109.8(9) . . ?
N7 N8 N9 108.8(9) . . ?
C3 N9 N8 105.1(9) . . ?
C3 N9 Cd1 130.7(7) . 4_565 ?
N8 N9 Cd1 124.1(6) . 4_565 ?
N11 N10 C5 104.7(9) . . ?
N11 N10 Cd2 127.9(7) . . ?
C5 N10 Cd2 125.7(8) . . ?
N12 N11 N10 108.5(9) . . ?
N12 N11 Cd2 106.1(7) . 3_667 ?
N10 N11 Cd2 126.3(7) . 3_667 ?
N11 N12 N13 112.2(9) . . ?
N11 N12 Cd1 127.6(7) . 3_667 ?
N13 N12 Cd1 119.8(7) . 3_667 ?
N12 N13 C5 103.4(9) . . ?
Cd1 O1 Cd1 95.9(2) . 3_767 ?
Cd1 O1 Cd2 124.6(3) . 3_767 ?
Cd1 O1 Cd2 108.2(3) 3_767 3_767 ?
Cd1 O1 H1 108(9) . . ?
Cd1 O1 H1 95(9) 3_767 . ?
Cd2 O1 H1 118(9) 3_767 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.014
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.254


####################################################################### 
# 
# 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_1a
_audit_block_doi                 10.5517/cc13xqmc
_database_code_depnum_ccdc_archive 'CCDC 1040503'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C5.91 H6 N8 O2 Zn2), H1.98 O, 0.267(C)'
_chemical_formula_sum            'C18 H20 N24 O7 Zn6'
_chemical_formula_weight         1076.90

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           hexagonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   30.095(5)
_cell_length_b                   30.095(5)
_cell_length_c                   6.7707(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5310.7(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    10907
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.93

_exptl_crystal_description       rodlike
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3192
_exptl_absorpt_coefficient_mu    4.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_T_max  0.443
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10907
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         27.93
_reflns_number_total             2768
_reflns_number_gt                2070
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0474P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2768
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
C6A C 0.20062(17) 0.29965(15) 0.2988(6) 0.0177(11) Uani 0.911(10) 1 d P A 1
C6B C 0.1779(19) 0.2981(16) 0.367(7) 0.0177(11) Uani 0.089(10) 1 d P A 2
Zn1 Zn 0.181087(15) 0.217638(15) 0.57502(6) 0.01661(13) Uani 1 1 d . . .
Zn2 Zn 0.220944(16) 0.227153(16) 1.07339(6) 0.01840(14) Uani 1 1 d . . .
O1 O 0.18156(10) 0.18628(9) 0.8468(4) 0.0202(6) Uani 1 1 d . . .
O2 O 0.19858(10) 0.25167(9) 0.2988(4) 0.0188(6) Uani 1 1 d . . .
N1 N 0.18983(12) 0.16001(12) 0.4580(5) 0.0219(7) Uani 1 1 d . . .
N2 N 0.20517(13) 0.16068(12) 0.2701(5) 0.0226(7) Uani 1 1 d . . .
N3 N 0.21440(13) 0.12346(13) 0.2404(5) 0.0264(8) Uani 1 1 d . . .
N4 N 0.20446(12) 0.09693(12) 0.4122(5) 0.0218(7) Uani 1 1 d . A .
N5 N 0.28440(12) 0.36863(12) 0.7386(5) 0.0236(7) Uani 1 1 d . . .
N6 N 0.27619(13) 0.34376(13) 0.9122(5) 0.0304(8) Uani 1 1 d . . .
N7 N 0.24402(12) 0.29525(12) 0.8812(5) 0.0242(7) Uani 1 1 d . A .
N8 N 0.23050(12) 0.28784(11) 0.6896(5) 0.0216(7) Uani 1 1 d . . .
C1 C 0.18969(14) 0.12026(14) 0.5429(6) 0.0205(8) Uani 1 1 d . A .
C2 C 0.17548(17) 0.10506(15) 0.7548(6) 0.0288(10) Uani 1 1 d . . .
H2A H 0.2062 0.1131 0.8291 0.035 Uiso 1 1 calc R A .
H2B H 0.1524 0.0683 0.7621 0.035 Uiso 1 1 calc R . .
C3 C 0.14962(15) 0.13253(14) 0.8480(6) 0.0243(9) Uani 1 1 d . A .
H3A H 0.1183 0.1235 0.7763 0.029 Uiso 1 1 calc R . .
H3B H 0.1403 0.1209 0.9833 0.029 Uiso 1 1 calc R . .
C4 C 0.25605(15) 0.33389(14) 0.6046(6) 0.0219(8) Uani 1 1 d . A .
C5 C 0.25111(17) 0.34190(15) 0.3888(6) 0.0287(10) Uani 1 1 d . . .
H5A H 0.2797 0.3429 0.3185 0.034 Uiso 1 1 calc R A 1
H5B H 0.2531 0.3748 0.3709 0.034 Uiso 1 1 calc R A 1
O3 O 1.0000 1.0000 0.243(10) 1.4(3) Uani 1 3 d S . .
H3WA H 0.9767 1.0059 0.2837 2.067 Uiso 0.33 1 d PR . .
H3WB H 0.9965 0.9941 0.1195 2.067 Uiso 0.33 1 d PR . .


_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
C6A O2 1.414(4) . ?
C6A C5 1.538(6) . ?
C6B O2 1.85(5) . ?
C6B C5 1.93(5) . ?
Zn1 N8 2.033(3) . ?
Zn1 N1 2.040(3) . ?
Zn1 N4 2.047(3) 12_556 ?
Zn1 O2 2.070(2) . ?
Zn1 O1 2.071(2) . ?
Zn2 O1 1.953(2) . ?
Zn2 O2 1.955(2) 1_556 ?
Zn2 N5 2.070(3) 5 ?
Zn2 N7 2.226(3) . ?
Zn2 N2 2.248(3) 1_556 ?
O1 C3 1.409(4) . ?
O2 Zn2 1.955(2) 1_554 ?
N1 C1 1.325(4) . ?
N1 N2 1.350(4) . ?
N2 N3 1.298(4) . ?
N2 Zn2 2.247(3) 1_554 ?
N3 N4 1.357(4) . ?
N4 C1 1.336(5) . ?
N4 Zn1 2.046(3) 11_556 ?
N5 C4 1.324(5) . ?
N5 N6 1.348(4) . ?
N5 Zn2 2.070(3) 9_554 ?
N6 N7 1.303(4) . ?
N7 N8 1.344(4) . ?
N8 C4 1.333(5) . ?
C1 C2 1.502(5) . ?
C2 C3 1.527(5) . ?
C4 C5 1.500(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
O2 C6A C5 111.4(3) . . ?
O2 C6B C5 80.5(19) . . ?
N8 Zn1 N1 133.89(13) . . ?
N8 Zn1 N4 110.09(13) . 12_556 ?
N1 Zn1 N4 116.01(13) . 12_556 ?
N8 Zn1 O2 87.57(11) . . ?
N1 Zn1 O2 87.76(11) . . ?
N4 Zn1 O2 96.71(11) 12_556 . ?
N8 Zn1 O1 88.08(11) . . ?
N1 Zn1 O1 85.66(11) . . ?
N4 Zn1 O1 97.32(11) 12_556 . ?
O2 Zn1 O1 165.96(10) . . ?
O1 Zn2 O2 129.48(11) . 1_556 ?
O1 Zn2 N5 115.32(12) . 5 ?
O2 Zn2 N5 115.18(12) 1_556 5 ?
O1 Zn2 N7 86.12(11) . . ?
O2 Zn2 N7 96.70(11) 1_556 . ?
N5 Zn2 N7 85.37(12) 5 . ?
O1 Zn2 N2 96.50(11) . 1_556 ?
O2 Zn2 N2 85.07(11) 1_556 1_556 ?
N5 Zn2 N2 89.50(12) 5 1_556 ?
N7 Zn2 N2 174.85(12) . 1_556 ?
C3 O1 Zn2 124.7(2) . . ?
C3 O1 Zn1 111.8(2) . . ?
Zn2 O1 Zn1 123.45(12) . . ?
C6A O2 C6B 24.2(15) . . ?
C6A O2 Zn2 122.5(2) . 1_554 ?
C6B O2 Zn2 142.1(15) . 1_554 ?
C6A O2 Zn1 112.1(2) . . ?
C6B O2 Zn1 92.9(15) . . ?
Zn2 O2 Zn1 124.67(12) 1_554 . ?
C1 N1 N2 105.6(3) . . ?
C1 N1 Zn1 131.0(3) . . ?
N2 N1 Zn1 122.8(2) . . ?
N3 N2 N1 110.6(3) . . ?
N3 N2 Zn2 129.5(2) . 1_554 ?
N1 N2 Zn2 119.4(2) . 1_554 ?
N2 N3 N4 107.2(3) . . ?
C1 N4 N3 107.0(3) . . ?
C1 N4 Zn1 134.6(3) . 11_556 ?
N3 N4 Zn1 118.4(2) . 11_556 ?
C4 N5 N6 107.0(3) . . ?
C4 N5 Zn2 136.7(3) . 9_554 ?
N6 N5 Zn2 116.1(2) . 9_554 ?
N7 N6 N5 108.0(3) . . ?
N6 N7 N8 109.6(3) . . ?
N6 N7 Zn2 130.7(3) . . ?
N8 N7 Zn2 118.8(2) . . ?
C4 N8 N7 105.9(3) . . ?
C4 N8 Zn1 131.1(3) . . ?
N7 N8 Zn1 123.0(2) . . ?
N1 C1 N4 109.6(3) . . ?
N1 C1 C2 124.2(3) . . ?
N4 C1 C2 126.3(3) . . ?
C1 C2 C3 112.0(3) . . ?
O1 C3 C2 112.3(3) . . ?
N5 C4 N8 109.5(3) . . ?
N5 C4 C5 128.1(3) . . ?
N8 C4 C5 122.4(3) . . ?
C4 C5 C6A 112.9(3) . . ?
C4 C5 C6B 97.8(14) . . ?
C6A C5 C6B 23.7(14) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.93
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.121
####################################################################### 
# 
# 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_1b
_audit_block_doi                 10.5517/cc13xqnd
_database_code_depnum_ccdc_archive 'CCDC 1040504'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2.57 H7 Cd2 N4 O7.43 S'
_chemical_formula_sum            'C2.57 H7 Cd2 N4 O7.43 S'
_chemical_formula_weight         469.72

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'

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                   17.501(3)
_cell_length_b                   33.436(6)
_cell_length_c                   7.1042(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4157.0(12)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1872
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3549.8
_exptl_absorpt_coefficient_mu    4.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5328
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         25.40
_reflns_number_total             1872
_reflns_number_gt                1783
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0228P)²+43.9670P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(5)
_refine_ls_number_reflns         1872
_refine_ls_number_parameters     150
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
C1 C 0.4550(3) 0.94913(17) 0.2625(18) 0.042(2) Uani 0.57(4) 1 d P . 1
O1B O 0.4550(3) 0.94913(17) 0.2625(18) 0.042(2) Uani 0.43(4) 1 d P . 2
C2 C 0.5335(3) 0.92689(17) 0.2609(13) 0.0266(12) Uani 1 1 d . . .
H2A H 0.5652 0.9380 0.1618 0.032 Uiso 1 1 calc R . 1
H2B H 0.5593 0.9316 0.3799 0.032 Uiso 1 1 calc R . 1
C3 C 0.5256(4) 0.8823(2) 0.2305(14) 0.043(2) Uani 1 1 d . . .
H3A H 0.4992 0.8775 0.1126 0.052 Uiso 1 1 calc R . .
H3B H 0.5760 0.8704 0.2213 0.052 Uiso 1 1 calc R . .
Cd1 Cd 0.25134(2) 1.001973(14) 0.5092(3) 0.02075(11) Uani 1 1 d . . .
Cd2 Cd 0.42669(2) 0.959753(12) 0.76084(9) 0.02072(11) Uani 1 1 d . . .
N1 N 0.4202(4) 0.95861(17) 0.4162(14) 0.023(2) Uani 1 1 d . . .
N2 N 0.3543(4) 0.9746(2) 0.3504(9) 0.0258(7) Uani 1 1 d . . .
N3 N 0.3543(4) 0.9733(2) 0.1685(9) 0.0258(7) Uani 1 1 d . . .
N4 N 0.4200(4) 0.95718(17) 0.1060(13) 0.0196(18) Uani 1 1 d . . .
O2 O 0.4850(4) 0.8637(2) 0.3777(10) 0.0616(18) Uani 1 1 d . . .
H2 H 0.5081 0.8669 0.4771 0.092 Uiso 1 1 calc R . .
O7 O 0.20252(19) 1.03378(11) 0.2564(11) 0.0213(8) Uani 1 1 d . . .
O8 O 0.4242(3) 0.89367(13) 0.7463(15) 0.0502(14) Uani 1 1 d . . .
H8A H 0.4167 0.8703 0.7025 0.060 Uiso 1 1 d R . .
H8B H 0.4428 0.8911 0.8562 0.060 Uiso 1 1 d R . .
O4 O 0.1708(4) 0.94684(16) 0.0950(7) 0.0335(13) Uani 1 1 d . . .
O3 O 0.1685(3) 0.94981(15) 0.4344(7) 0.0307(12) Uani 1 1 d . . .
O6 O 0.0925(2) 0.90097(12) 0.2691(10) 0.0333(10) Uani 1 1 d . . .
O5 O 0.0582(2) 0.97067(11) 0.2607(13) 0.0274(9) Uani 1 1 d . . .
S1 S 0.12326(7) 0.94130(4) 0.2641(3) 0.0208(3) 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
C1 N1 1.290(15) . ?
C1 N4 1.297(15) . ?
C1 C2 1.563(8) . ?
C2 C3 1.514(9) . ?
C3 O2 1.408(10) . ?
Cd1 O7 2.255(7) . ?
Cd1 O4 2.271(5) 10_575 ?
Cd1 O7 2.273(6) 10_575 ?
Cd1 N2 2.315(7) . ?
Cd1 N3 2.320(7) 10_575 ?
Cd1 O3 2.329(5) . ?
Cd2 O8 2.212(5) . ?
Cd2 O7 2.272(3) 10_575 ?
Cd2 O5 2.331(4) 9 ?
Cd2 O5 2.341(4) 10_575 ?
Cd2 N1 2.451(10) . ?
Cd2 N4 2.456(9) 1_556 ?
N1 N2 1.355(9) . ?
N2 N3 1.293(6) . ?
N3 N4 1.345(9) . ?
N3 Cd1 2.320(7) 10_574 ?
N4 Cd2 2.456(9) 1_554 ?
O7 Cd2 2.272(3) 10_574 ?
O7 Cd1 2.273(6) 10_574 ?
O4 S1 1.473(5) . ?
O4 Cd1 2.271(5) 10_574 ?
O3 S1 1.474(5) . ?
O6 S1 1.453(4) . ?
O5 S1 1.503(4) . ?
O5 Cd2 2.331(4) 9_454 ?
O5 Cd2 2.341(4) 10_574 ?

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 C1 N4 116.8(6) . . ?
N1 C1 C2 122.5(10) . . ?
N4 C1 C2 120.5(10) . . ?
C3 C2 C1 112.9(5) . . ?
O2 C3 C2 112.0(7) . . ?
O7 Cd1 O4 94.92(17) . 10_575 ?
O7 Cd1 O7 176.34(15) . 10_575 ?
O4 Cd1 O7 88.61(18) 10_575 10_575 ?
O7 Cd1 N2 95.4(2) . . ?
O4 Cd1 N2 87.8(2) 10_575 . ?
O7 Cd1 N2 83.8(2) 10_575 . ?
O7 Cd1 N3 85.3(2) . 10_575 ?
O4 Cd1 N3 94.5(2) 10_575 10_575 ?
O7 Cd1 N3 95.4(2) 10_575 10_575 ?
N2 Cd1 N3 177.5(3) . 10_575 ?
O7 Cd1 O3 86.31(18) . . ?
O4 Cd1 O3 177.4(3) 10_575 . ?
O7 Cd1 O3 90.21(17) 10_575 . ?
N2 Cd1 O3 94.4(2) . . ?
N3 Cd1 O3 83.2(2) 10_575 . ?
O8 Cd2 O7 94.28(17) . 10_575 ?
O8 Cd2 O5 100.13(17) . 9 ?
O7 Cd2 O5 165.51(13) 10_575 9 ?
O8 Cd2 O5 174.0(2) . 10_575 ?
O7 Cd2 O5 91.01(13) 10_575 10_575 ?
O5 Cd2 O5 74.53(14) 9 10_575 ?
O8 Cd2 N1 86.4(3) . . ?
O7 Cd2 N1 86.7(2) 10_575 . ?
O5 Cd2 N1 92.7(3) 9 . ?
O5 Cd2 N1 91.2(3) 10_575 . ?
O8 Cd2 N4 90.6(3) . 1_556 ?
O7 Cd2 N4 88.3(2) 10_575 1_556 ?
O5 Cd2 N4 93.0(3) 9 1_556 ?
O5 Cd2 N4 92.3(3) 10_575 1_556 ?
N1 Cd2 N4 173.88(15) . 1_556 ?
C1 N1 N2 101.9(8) . . ?
C1 N1 Cd2 145.9(6) . . ?
N2 N1 Cd2 112.2(6) . . ?
N3 N2 N1 109.3(8) . . ?
N3 N2 Cd1 120.1(6) . . ?
N1 N2 Cd1 130.6(6) . . ?
N2 N3 N4 110.1(7) . . ?
N2 N3 Cd1 118.4(6) . 10_574 ?
N4 N3 Cd1 131.5(6) . 10_574 ?
C1 N4 N3 101.8(8) . . ?
C1 N4 Cd2 147.1(6) . 1_554 ?
N3 N4 Cd2 110.9(5) . 1_554 ?
Cd1 O7 Cd2 114.3(3) . 10_574 ?
Cd1 O7 Cd1 103.45(14) . 10_574 ?
Cd2 O7 Cd1 114.5(3) 10_574 10_574 ?
S1 O4 Cd1 130.7(3) . 10_574 ?
S1 O3 Cd1 131.8(3) . . ?
S1 O5 Cd2 130.2(2) . 9_454 ?
S1 O5 Cd2 124.3(2) . 10_574 ?
Cd2 O5 Cd2 105.47(14) 9_454 10_574 ?
O6 S1 O4 110.3(3) . . ?
O6 S1 O3 111.0(4) . . ?
O4 S1 O3 110.0(2) . . ?
O6 S1 O5 109.0(2) . . ?
O4 S1 O5 109.4(4) . . ?
O3 S1 O5 107.1(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.111
####################################################################### 
# 
# 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_2a
_audit_block_doi                 10.5517/cc13xqpf
_database_code_depnum_ccdc_archive 'CCDC 1040505'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 N10 O8 Zn3'
_chemical_formula_sum            'C18 H12 N10 O8 Zn3'
_chemical_formula_weight         692.49

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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   25.319(5)
_cell_length_b                   14.309(3)
_cell_length_c                   7.0137(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.379(3)
_cell_angle_gamma                90.00
_cell_volume                     2525.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4592
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      25.39

_exptl_crystal_description       rod-like
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    2.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4592
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.39
_reflns_number_total             2320
_reflns_number_gt                1852
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0263P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2320
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0730
_refine_ls_wR_factor_gt          0.0691
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Zn1 Zn 0.0000 0.58424(4) 0.7500 0.02225(15) Uani 1 2 d S . .
Zn2 Zn 0.150262(15) 0.71408(3) 0.16257(6) 0.02617(14) Uani 1 1 d . . .
N1 N 0.20531(11) 0.60864(19) 0.1351(4) 0.0272(7) Uani 1 1 d . . .
C4 C 0.22688(14) 0.4464(2) 0.1269(5) 0.0301(8) Uani 1 1 d . . .
H4 H 0.2152 0.3850 0.1115 0.036 Uiso 1 1 calc R . .
C2 C 0.29544(14) 0.5577(2) 0.1799(5) 0.0320(9) Uani 1 1 d . . .
H2 H 0.3313 0.5733 0.1985 0.038 Uiso 1 1 calc R . .
C1 C 0.25783(14) 0.6269(2) 0.1664(5) 0.0321(9) Uani 1 1 d . . .
H1 H 0.2689 0.6888 0.1793 0.038 Uiso 1 1 calc R . .
C5 C 0.19077(14) 0.5189(2) 0.1105(5) 0.0319(9) Uani 1 1 d . . .
H5 H 0.1549 0.5050 0.0813 0.038 Uiso 1 1 calc R . .
C3 C 0.28050(13) 0.4654(2) 0.1660(5) 0.0273(8) Uani 1 1 d . . .
C6 C 0.32068(14) 0.3877(3) 0.2012(5) 0.0337(9) Uani 1 1 d . . .
O1 O 0.36808(11) 0.40553(19) 0.2205(5) 0.0629(9) Uani 1 1 d . . .
O2 O 0.30106(10) 0.30555(17) 0.2117(4) 0.0396(7) Uani 1 1 d . . .
N5 N 0.04130(10) 0.59790(18) 0.5046(4) 0.0219(6) Uani 1 1 d . . .
N4 N 0.04886(10) 0.53470(18) 0.3668(4) 0.0222(6) Uani 1 1 d . . .
N3 N 0.08294(11) 0.56629(18) 0.2575(4) 0.0250(6) Uani 1 1 d . . .
C7 C 0.07259(12) 0.6702(2) 0.4731(5) 0.0218(7) Uani 1 1 d . . .
N2 N 0.09917(10) 0.65237(18) 0.3233(4) 0.0244(6) Uani 1 1 d . . .
O4 O -0.05781(9) 0.67617(17) 0.6198(3) 0.0350(6) Uani 1 1 d . . .
O3 O 0.13186(9) 0.75838(16) -0.1004(3) 0.0334(6) Uani 1 1 d . . .
C8 C 0.07895(14) 0.7552(2) 0.5966(5) 0.0282(8) Uani 1 1 d . . .
H8A H 0.0469 0.7927 0.5770 0.034 Uiso 1 1 calc R . .
H8B H 0.1083 0.7925 0.5607 0.034 Uiso 1 1 calc R . .
C9 C 0.08957(13) 0.7279(2) -0.1933(5) 0.0253(8) 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 O4 2.100(2) . ?
Zn1 O4 2.100(2) 2_556 ?
Zn1 N5 2.120(3) . ?
Zn1 N5 2.120(3) 2_556 ?
Zn1 N4 2.207(3) 5_566 ?
Zn1 N4 2.207(3) 6_566 ?
Zn2 O2 1.941(2) 4 ?
Zn2 O3 1.957(2) . ?
Zn2 N2 2.012(3) . ?
Zn2 N1 2.077(3) . ?
N1 C5 1.342(4) . ?
N1 C1 1.349(4) . ?
C4 C5 1.378(5) . ?
C4 C3 1.382(5) . ?
C4 H4 0.9300 . ?
C2 C1 1.370(5) . ?
C2 C3 1.375(4) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C5 H5 0.9300 . ?
C3 C6 1.509(5) . ?
C6 O1 1.220(4) . ?
C6 O2 1.281(4) . ?
O2 Zn2 1.941(2) 4_545 ?
N5 C7 1.336(4) . ?
N5 N4 1.353(3) . ?
N4 N3 1.298(3) . ?
N4 Zn1 2.207(3) 5_566 ?
N3 N2 1.363(3) . ?
C7 N2 1.334(4) . ?
C7 C8 1.492(4) . ?
O4 C9 1.246(4) 2 ?
O3 C9 1.267(4) . ?
C8 C9 1.519(5) 1_556 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.246(4) 2 ?
C9 C8 1.519(5) 1_554 ?

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
O4 Zn1 O4 102.43(14) . 2_556 ?
O4 Zn1 N5 88.40(9) . . ?
O4 Zn1 N5 84.98(9) 2_556 . ?
O4 Zn1 N5 84.98(9) . 2_556 ?
O4 Zn1 N5 88.40(9) 2_556 2_556 ?
N5 Zn1 N5 169.42(14) . 2_556 ?
O4 Zn1 N4 89.24(10) . 5_566 ?
O4 Zn1 N4 168.28(10) 2_556 5_566 ?
N5 Zn1 N4 94.38(9) . 5_566 ?
N5 Zn1 N4 93.77(10) 2_556 5_566 ?
O4 Zn1 N4 168.28(10) . 6_566 ?
O4 Zn1 N4 89.24(10) 2_556 6_566 ?
N5 Zn1 N4 93.77(10) . 6_566 ?
N5 Zn1 N4 94.38(9) 2_556 6_566 ?
N4 Zn1 N4 79.11(13) 5_566 6_566 ?
O2 Zn2 O3 106.40(10) 4 . ?
O2 Zn2 N2 117.17(11) 4 . ?
O3 Zn2 N2 124.73(10) . . ?
O2 Zn2 N1 97.65(11) 4 . ?
O3 Zn2 N1 103.88(11) . . ?
N2 Zn2 N1 102.29(11) . . ?
C5 N1 C1 117.3(3) . . ?
C5 N1 Zn2 122.0(2) . . ?
C1 N1 Zn2 120.2(2) . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C1 C2 C3 120.4(3) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C2 C3 C4 117.3(3) . . ?
C2 C3 C6 121.4(3) . . ?
C4 C3 C6 121.2(3) . . ?
O1 C6 O2 124.6(3) . . ?
O1 C6 C3 120.1(3) . . ?
O2 C6 C3 115.3(3) . . ?
C6 O2 Zn2 114.5(2) . 4_545 ?
C7 N5 N4 105.4(2) . . ?
C7 N5 Zn1 124.1(2) . . ?
N4 N5 Zn1 129.8(2) . . ?
N3 N4 N5 110.2(2) . . ?
N3 N4 Zn1 115.6(2) . 5_566 ?
N5 N4 Zn1 131.51(19) . 5_566 ?
N4 N3 N2 108.1(2) . . ?
N2 C7 N5 110.1(3) . . ?
N2 C7 C8 125.6(3) . . ?
N5 C7 C8 124.3(3) . . ?
C7 N2 N3 106.2(2) . . ?
C7 N2 Zn2 140.3(2) . . ?
N3 N2 Zn2 113.30(19) . . ?
C9 O4 Zn1 130.0(2) 2 . ?
C9 O3 Zn2 118.2(2) . . ?
C7 C8 C9 110.4(3) . 1_556 ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 1_556 . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 1_556 . ?
H8A C8 H8B 108.1 . . ?
O4 C9 O3 122.6(3) 2 . ?
O4 C9 C8 120.1(3) 2 1_554 ?
O3 C9 C8 117.3(3) . 1_554 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.084

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 0.000 -0.026 185 52 ' '
2 0.500 0.500 -0.044 185 52 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_2b
_audit_block_doi                 10.5517/cc13xqqg
_database_code_depnum_ccdc_archive 'CCDC 1040506'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 Cd9 N30 O20, 1.828(H2 O)'
_chemical_formula_sum            'C18 H23.65 Cd9 N30 O21.83'
_chemical_formula_weight         2021.26

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3781(13)
_cell_length_b                   13.574(2)
_cell_length_c                   13.578(2)
_cell_angle_alpha                113.181(2)
_cell_angle_beta                 103.841(2)
_cell_angle_gamma                90.952(2)
_cell_volume                     1204.4(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6315
_cell_measurement_theta_min      1.64
_cell_measurement_theta_max      25.40

_exptl_crystal_description       rodlike
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_T_max  0.450
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6315
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.40
_reflns_number_total             4340
_reflns_number_gt                3478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0382P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4340
_refine_ls_number_parameters     377
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
C1 C 0.9589(9) 0.6176(5) 0.4117(5) 0.0206(15) Uani 1 1 d . . .
C2 C 0.8430(9) 0.7086(5) 0.4259(6) 0.0212(15) Uani 1 1 d . . .
H2A H 0.8065 0.7169 0.3563 0.025 Uiso 1 1 calc R . .
H2B H 0.9196 0.7747 0.4815 0.025 Uiso 1 1 calc R . .
C3 C 0.6669(10) 0.6939(5) 0.4604(6) 0.0222(15) Uani 1 1 d . . .
C4 C 0.6284(9) 0.4032(5) -0.1425(5) 0.0200(15) Uani 1 1 d . . .
C5 C 0.8012(9) 0.4346(5) -0.1666(6) 0.0223(15) Uani 1 1 d . . .
H5A H 0.7838 0.4002 -0.2464 0.027 Uiso 1 1 calc R . .
H5B H 0.9046 0.4052 -0.1327 0.027 Uiso 1 1 calc R . .
C6 C 0.8598(9) 0.5551(5) -0.1280(5) 0.0187(14) Uani 1 1 d . . .
C7 C 0.6468(9) -0.0155(5) -0.1860(5) 0.0183(14) Uani 1 1 d . . .
C8 C 0.8309(9) -0.0586(5) -0.1901(6) 0.0206(15) Uani 1 1 d . . .
H8A H 0.9294 0.0008 -0.1654 0.025 Uiso 1 1 calc R . .
H8B H 0.8258 -0.1063 -0.2662 0.025 Uiso 1 1 calc R . .
C9 C 0.8777(11) -0.1206(5) -0.1161(6) 0.0259(16) Uani 1 1 d . . .
N1 N 0.8980(7) 0.5139(4) 0.3514(4) 0.0190(12) Uani 1 1 d . . .
N2 N 1.0429(8) 0.4581(4) 0.3645(5) 0.0227(13) Uani 1 1 d . . .
N3 N 1.1890(8) 0.5275(4) 0.4319(4) 0.0212(12) Uani 1 1 d . . .
N4 N 1.1399(8) 0.6280(4) 0.4626(4) 0.0198(12) Uani 1 1 d . . .
N5 N 0.6146(8) 0.3349(4) -0.0959(5) 0.0225(13) Uani 1 1 d . . .
N6 N 0.4343(8) 0.3308(4) -0.0904(5) 0.0230(13) Uani 1 1 d . . .
N7 N 0.3417(8) 0.3931(5) -0.1320(5) 0.0257(14) Uani 1 1 d . . .
N8 N 0.4621(8) 0.4409(4) -0.1647(5) 0.0228(13) Uani 1 1 d . . .
N9 N 0.6266(7) 0.0822(4) -0.1171(4) 0.0191(12) Uani 1 1 d . . .
N10 N 0.4377(8) 0.0823(4) -0.1313(5) 0.0240(13) Uani 1 1 d . . .
N11 N 0.3483(8) -0.0108(4) -0.2056(5) 0.0277(14) Uani 1 1 d . . .
N12 N 0.4796(8) -0.0736(4) -0.2421(5) 0.0241(13) Uani 1 1 d . . .
N13 N 0.0146(8) 0.2087(5) -0.1154(5) 0.0263(14) Uani 1 1 d . . .
N14 N -0.0481(10) 0.1856(6) -0.2113(6) 0.0420(17) Uani 1 1 d . . .
N15 N -0.1151(17) 0.1665(9) -0.3012(7) 0.110(4) Uani 1 1 d . . .
O1 O 0.5731(7) 0.6010(4) 0.4115(4) 0.0247(11) Uani 1 1 d . . .
O2 O 0.6206(7) 0.7737(4) 0.5304(4) 0.0354(13) Uani 1 1 d D . .
O3 O 1.0299(6) 0.5856(4) -0.0960(4) 0.0305(12) Uani 1 1 d . . .
O4 O 0.7305(6) 0.6153(4) -0.1335(4) 0.0245(11) Uani 1 1 d . . .
O5 O 1.0288(7) -0.1624(4) -0.1150(4) 0.0297(12) Uani 1 1 d . . .
O6 O 0.7651(8) -0.1230(5) -0.0623(5) 0.0451(16) Uani 1 1 d . . .
O7 O 0.4972(6) 0.3589(3) 0.3394(4) 0.0205(10) Uani 1 1 d . . .
O8 O 0.6102(6) 0.2761(4) 0.1080(4) 0.0212(10) Uani 1 1 d . . .
O6W O 0.7635(10) 0.1143(5) 0.4710(5) 0.0529(18) Uani 1 1 d D . .
H6A H 0.779(15) 0.131(8) 0.538(3) 0.079 Uiso 1 1 d D . .
H6B H 0.728(11) 0.049(2) 0.441(7) 0.079 Uiso 1 1 d D . .
O7W O 0.8785(8) 0.2382(4) 0.3126(5) 0.0345(13) Uani 1 1 d D . .
H7A H 0.882(13) 0.201(6) 0.249(3) 0.052 Uiso 1 1 d D . .
H7B H 0.952(10) 0.292(4) 0.332(7) 0.052 Uiso 1 1 d D . .
O8W O 0.5801(14) 0.9045(8) 0.3867(10) 0.096(4) Uani 0.914(18) 1 d PD . .
H8WA H 0.464(4) 0.894(12) 0.358(12) 0.144 Uiso 0.914(18) 1 d PD . .
H8WB H 0.603(18) 0.870(11) 0.428(11) 0.144 Uiso 0.914(18) 1 d PD . .
Cd1 Cd 0.5000 0.5000 0.5000 0.02003(17) Uani 1 2 d S . .
Cd2 Cd 0.60071(7) 0.43771(4) 0.23774(4) 0.01938(13) Uani 1 1 d . . .
Cd3 Cd 0.63427(7) 0.23155(4) 0.39498(4) 0.02055(13) Uani 1 1 d . . .
Cd4 Cd 0.82032(7) 0.24499(4) 0.00416(4) 0.01854(13) Uani 1 1 d . . .
Cd5 Cd 0.31565(6) 0.22785(4) -0.01423(4) 0.01807(13) 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
C1 N1 1.323(8) . ?
C1 N4 1.325(9) . ?
C1 C2 1.490(9) . ?
C2 C3 1.518(9) . ?
C3 O2 1.245(8) . ?
C3 O1 1.266(8) . ?
C4 N5 1.326(8) . ?
C4 N8 1.350(8) . ?
C4 C5 1.486(9) . ?
C5 C6 1.527(9) . ?
C6 O3 1.231(8) . ?
C6 O4 1.274(7) . ?
C7 N9 1.324(8) . ?
C7 N12 1.330(9) . ?
C7 C8 1.493(9) . ?
C8 C9 1.532(8) . ?
C9 O6 1.239(8) . ?
C9 O5 1.260(8) . ?
N1 N2 1.339(7) . ?
N1 Cd2 2.304(5) . ?
N2 N3 1.305(8) . ?
N3 N4 1.345(7) . ?
N3 Cd1 2.354(5) 1_655 ?
N4 Cd3 2.367(6) 2_766 ?
N5 N6 1.351(8) . ?
N5 Cd4 2.454(5) . ?
N6 N7 1.308(7) . ?
N6 Cd5 2.306(5) . ?
N7 N8 1.342(7) . ?
N8 Cd2 2.238(5) 2_665 ?
N9 N10 1.361(7) . ?
N9 Cd4 2.354(5) . ?
N10 N11 1.304(8) . ?
N10 Cd5 2.348(5) . ?
N11 N12 1.355(7) . ?
N12 Cd3 2.284(6) 2_655 ?
N13 N14 1.181(8) . ?
N13 Cd5 2.265(6) . ?
N13 Cd4 2.332(6) 1_455 ?
N14 N15 1.121(10) . ?
O1 Cd1 2.279(4) . ?
O1 Cd2 2.578(5) . ?
O2 Cd3 2.352(5) 2_666 ?
O3 Cd4 2.250(5) 2_765 ?
O4 Cd5 2.379(5) 2_665 ?
O4 Cd2 2.445(5) 2_665 ?
O5 Cd4 2.308(4) 2_755 ?
O6 Cd5 2.211(5) 2_655 ?
O7 Cd1 2.261(4) . ?
O7 Cd2 2.296(4) . ?
O7 Cd3 2.303(4) . ?
O8 Cd2 2.223(4) . ?
O8 Cd4 2.274(4) . ?
O8 Cd5 2.297(5) . ?
O6W Cd3 2.319(5) . ?
O7W Cd3 2.355(5) . ?
Cd1 O7 2.261(4) 2_666 ?
Cd1 O1 2.279(4) 2_666 ?
Cd1 N3 2.354(5) 2_766 ?
Cd1 N3 2.354(5) 1_455 ?
Cd2 N8 2.238(5) 2_665 ?
Cd2 O4 2.445(5) 2_665 ?
Cd3 N12 2.284(6) 2_655 ?
Cd3 O2 2.352(5) 2_666 ?
Cd3 N4 2.367(6) 2_766 ?
Cd4 O3 2.250(5) 2_765 ?
Cd4 O5 2.308(4) 2_755 ?
Cd4 N13 2.332(6) 1_655 ?
Cd5 O6 2.211(5) 2_655 ?
Cd5 O4 2.379(5) 2_665 ?

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 C1 N4 108.9(6) . . ?
N1 C1 C2 126.2(6) . . ?
N4 C1 C2 124.8(6) . . ?
C1 C2 C3 114.0(5) . . ?
O2 C3 O1 124.7(6) . . ?
O2 C3 C2 118.6(6) . . ?
O1 C3 C2 116.7(6) . . ?
N5 C4 N8 110.2(6) . . ?
N5 C4 C5 125.3(6) . . ?
N8 C4 C5 124.5(6) . . ?
C4 C5 C6 117.2(5) . . ?
O3 C6 O4 125.5(6) . . ?
O3 C6 C5 116.6(6) . . ?
O4 C6 C5 117.9(6) . . ?
N9 C7 N12 110.4(6) . . ?
N9 C7 C8 124.6(6) . . ?
N12 C7 C8 124.6(6) . . ?
C7 C8 C9 111.0(5) . . ?
O6 C9 O5 126.6(6) . . ?
O6 C9 C8 117.0(6) . . ?
O5 C9 C8 116.4(6) . . ?
C1 N1 N2 107.8(6) . . ?
C1 N1 Cd2 127.7(4) . . ?
N2 N1 Cd2 124.5(4) . . ?
N3 N2 N1 107.6(5) . . ?
N2 N3 N4 109.4(5) . . ?
N2 N3 Cd1 130.4(4) . 1_655 ?
N4 N3 Cd1 120.2(4) . 1_655 ?
C1 N4 N3 106.3(5) . . ?
C1 N4 Cd3 136.2(4) . 2_766 ?
N3 N4 Cd3 116.6(4) . 2_766 ?
C4 N5 N6 104.8(5) . . ?
C4 N5 Cd4 139.1(5) . . ?
N6 N5 Cd4 115.1(4) . . ?
N7 N6 N5 110.9(5) . . ?
N7 N6 Cd5 126.1(4) . . ?
N5 N6 Cd5 123.0(4) . . ?
N6 N7 N8 107.5(5) . . ?
N7 N8 C4 106.6(5) . . ?
N7 N8 Cd2 126.3(4) . 2_665 ?
C4 N8 Cd2 127.0(4) . 2_665 ?
C7 N9 N10 105.0(5) . . ?
C7 N9 Cd4 137.5(4) . . ?
N10 N9 Cd4 117.4(4) . . ?
N11 N10 N9 110.5(5) . . ?
N11 N10 Cd5 128.2(4) . . ?
N9 N10 Cd5 120.8(4) . . ?
N10 N11 N12 107.1(5) . . ?
C7 N12 N11 107.1(5) . . ?
C7 N12 Cd3 136.4(4) . 2_655 ?
N11 N12 Cd3 115.5(4) . 2_655 ?
N14 N13 Cd5 130.5(5) . . ?
N14 N13 Cd4 121.1(5) . 1_455 ?
Cd5 N13 Cd4 108.4(2) . 1_455 ?
N15 N14 N13 176.4(10) . . ?
C3 O1 Cd1 124.4(4) . . ?
C3 O1 Cd2 129.8(4) . . ?
Cd1 O1 Cd2 94.99(16) . . ?
C3 O2 Cd3 124.7(5) . 2_666 ?
C6 O3 Cd4 128.8(4) . 2_765 ?
C6 O4 Cd5 127.0(4) . 2_665 ?
C6 O4 Cd2 128.5(4) . 2_665 ?
Cd5 O4 Cd2 96.37(16) 2_665 2_665 ?
C9 O5 Cd4 130.1(4) . 2_755 ?
C9 O6 Cd5 137.4(4) . 2_655 ?
Cd1 O7 Cd2 103.81(17) . . ?
Cd1 O7 Cd3 104.36(17) . . ?
Cd2 O7 Cd3 126.92(19) . . ?
Cd2 O8 Cd4 122.9(2) . . ?
Cd2 O8 Cd5 105.39(17) . . ?
Cd4 O8 Cd5 106.76(18) . . ?
O7 Cd1 O7 180.0(2) . 2_666 ?
O7 Cd1 O1 96.11(16) . 2_666 ?
O7 Cd1 O1 83.89(16) 2_666 2_666 ?
O7 Cd1 O1 83.89(16) . . ?
O7 Cd1 O1 96.11(16) 2_666 . ?
O1 Cd1 O1 179.999(1) 2_666 . ?
O7 Cd1 N3 86.75(18) . 2_766 ?
O7 Cd1 N3 93.25(18) 2_666 2_766 ?
O1 Cd1 N3 83.94(17) 2_666 2_766 ?
O1 Cd1 N3 96.06(17) . 2_766 ?
O7 Cd1 N3 93.25(18) . 1_455 ?
O7 Cd1 N3 86.75(18) 2_666 1_455 ?
O1 Cd1 N3 96.06(17) 2_666 1_455 ?
O1 Cd1 N3 83.94(17) . 1_455 ?
N3 Cd1 N3 180.000(1) 2_766 1_455 ?
O8 Cd2 N8 111.36(18) . 2_665 ?
O8 Cd2 O7 90.67(16) . . ?
N8 Cd2 O7 143.06(17) 2_665 . ?
O8 Cd2 N1 110.65(17) . . ?
N8 Cd2 N1 98.9(2) 2_665 . ?
O7 Cd2 N1 100.40(17) . . ?
O8 Cd2 O4 78.48(16) . 2_665 ?
N8 Cd2 O4 76.10(18) 2_665 2_665 ?
O7 Cd2 O4 80.04(16) . 2_665 ?
N1 Cd2 O4 170.80(17) . 2_665 ?
O8 Cd2 O1 167.36(15) . . ?
N8 Cd2 O1 80.26(18) 2_665 . ?
O7 Cd2 O1 76.78(15) . . ?
N1 Cd2 O1 70.94(16) . . ?
O4 Cd2 O1 100.39(15) 2_665 . ?
N12 Cd3 O7 102.98(18) 2_655 . ?
N12 Cd3 O6W 82.1(2) 2_655 . ?
O7 Cd3 O6W 173.1(2) . . ?
N12 Cd3 O2 93.98(19) 2_655 2_666 ?
O7 Cd3 O2 87.22(16) . 2_666 ?
O6W Cd3 O2 87.8(2) . 2_666 ?
N12 Cd3 O7W 84.88(19) 2_655 . ?
O7 Cd3 O7W 90.30(18) . . ?
O6W Cd3 O7W 94.9(2) . . ?
O2 Cd3 O7W 177.0(2) 2_666 . ?
N12 Cd3 N4 157.98(19) 2_655 2_766 ?
O7 Cd3 N4 88.39(17) . 2_766 ?
O6W Cd3 N4 88.4(2) . 2_766 ?
O2 Cd3 N4 105.50(18) 2_666 2_766 ?
O7W Cd3 N4 76.15(18) . 2_766 ?
O3 Cd4 O8 93.65(17) 2_765 . ?
O3 Cd4 O5 101.50(18) 2_765 2_755 ?
O8 Cd4 O5 85.18(15) . 2_755 ?
O3 Cd4 N13 89.0(2) 2_765 1_655 ?
O8 Cd4 N13 175.24(18) . 1_655 ?
O5 Cd4 N13 98.18(18) 2_755 1_655 ?
O3 Cd4 N9 168.04(18) 2_765 . ?
O8 Cd4 N9 86.95(17) . . ?
O5 Cd4 N9 90.46(18) 2_755 . ?
N13 Cd4 N9 89.65(19) 1_655 . ?
O3 Cd4 N5 80.46(18) 2_765 . ?
O8 Cd4 N5 84.31(17) . . ?
O5 Cd4 N5 169.42(17) 2_755 . ?
N13 Cd4 N5 92.24(19) 1_655 . ?
N9 Cd4 N5 87.72(18) . . ?
O6 Cd5 N13 91.1(2) 2_655 . ?
O6 Cd5 O8 91.0(2) 2_655 . ?
N13 Cd5 O8 170.02(19) . . ?
O6 Cd5 N6 173.31(19) 2_655 . ?
N13 Cd5 N6 94.9(2) . . ?
O8 Cd5 N6 83.66(18) . . ?
O6 Cd5 N10 88.98(19) 2_655 . ?
N13 Cd5 N10 102.5(2) . . ?
O8 Cd5 N10 87.30(18) . . ?
N6 Cd5 N10 86.8(2) . . ?
O6 Cd5 O4 91.18(18) 2_655 2_665 ?
N13 Cd5 O4 91.75(19) . 2_665 ?
O8 Cd5 O4 78.44(15) . 2_665 ?
N6 Cd5 O4 91.67(18) . 2_665 ?
N10 Cd5 O4 165.73(18) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.177
####################################################################### 
# 
# 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_2c
_audit_block_doi                 10.5517/cc13xqrh
_database_code_depnum_ccdc_archive 'CCDC 1040507'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H7 N5 O2 Zn, H2 O'
_chemical_formula_sum            'C8 H9 N5 O3 Zn'
_chemical_formula_weight         288.57

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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   16.852(2)
_cell_length_b                   17.116(2)
_cell_length_c                   9.7103(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.683(2)
_cell_angle_gamma                90.00
_cell_volume                     2457.2(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2265
_cell_measurement_theta_min      1.82
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6286
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.40
_reflns_number_total             2265
_reflns_number_gt                1976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1081P)²+6.6815P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2265
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1552
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
O1 O 1.1404(2) 0.1891(2) 0.5936(4) 0.0440(8) Uani 1 1 d . . .
C8 C 1.0630(3) 0.1601(3) 0.5028(5) 0.0353(10) Uani 1 1 d . . .
O4W O 0.5937(4) 0.0841(3) 0.3273(7) 0.0301(15) Uani 0.509(7) 1 d P A 1
H4A H 0.5312 0.0759 0.2738 0.036 Uiso 0.509(7) 1 d PR A 1
H4B H 0.6134 0.0573 0.2604 0.036 Uiso 0.509(7) 1 d PR A 1
O3W O 0.6661(5) 0.2319(4) 0.3829(7) 0.046(2) Uani 0.491(7) 1 d P A 2
H3A H 0.6472 0.1854 0.3524 0.055 Uiso 0.491(7) 1 d PR A 2
H3B H 0.6531 0.2563 0.2975 0.055 Uiso 0.491(7) 1 d PR A 2
Zn1 Zn 0.73316(3) 0.39211(3) 0.15579(5) 0.0280(2) Uani 1 1 d . . .
N1 N 0.7453(2) 0.4752(2) 0.3096(4) 0.0321(8) Uani 1 1 d . . .
N5 N 0.8432(2) 0.3202(2) 0.2658(4) 0.0314(8) Uani 1 1 d . . .
C7 C 0.9254(3) 0.3457(3) 0.3630(6) 0.0421(11) Uani 1 1 d . . .
H7 H 0.9340 0.3993 0.3786 0.050 Uiso 1 1 calc R . .
C3 C 0.8309(3) 0.2426(3) 0.2422(5) 0.0370(10) Uani 1 1 d . . .
H3 H 0.7737 0.2237 0.1727 0.044 Uiso 1 1 calc R . .
C4 C 0.9016(3) 0.1901(3) 0.3190(5) 0.0353(10) Uani 1 1 d . . .
H4 H 0.8914 0.1367 0.3018 0.042 Uiso 1 1 calc R . .
C1 C 0.7091(3) 0.4888(2) 0.4006(5) 0.0307(9) Uani 1 1 d . . .
N4 N 0.7463(2) 0.5532(2) 0.4855(4) 0.0312(8) Uani 1 1 d . . .
N2 N 0.8069(3) 0.5328(2) 0.3383(5) 0.0427(10) Uani 1 1 d . . .
N3 N 0.8070(3) 0.5794(2) 0.4438(5) 0.0398(9) Uani 1 1 d . . .
C5 C 0.9865(3) 0.2172(3) 0.4201(5) 0.0327(9) Uani 1 1 d . . .
C2 C 0.6386(4) 0.4403(4) 0.4081(8) 0.0612(17) Uani 1 1 d . . .
H2A H 0.5818 0.4485 0.3151 0.092 Uiso 1 1 calc R . .
H2B H 0.6331 0.4549 0.4986 0.092 Uiso 1 1 calc R . .
H2C H 0.6551 0.3862 0.4156 0.092 Uiso 1 1 calc R . .
C6 C 0.9997(3) 0.2974(3) 0.4432(6) 0.0411(11) Uani 1 1 d . . .
H6 H 1.0565 0.3179 0.5101 0.049 Uiso 1 1 calc R . .
O2 O 1.0483(3) 0.0900(2) 0.4774(6) 0.0657(13) 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
O1 C8 1.274(6) . ?
O1 Zn1 1.958(3) 8_556 ?
C8 O2 1.226(6) . ?
C8 C5 1.506(6) . ?
Zn1 O1 1.958(3) 8_455 ?
Zn1 N1 2.001(4) . ?
Zn1 N4 2.002(4) 6_565 ?
Zn1 N5 2.048(4) . ?
N1 C1 1.313(6) . ?
N1 N2 1.360(5) . ?
N5 C7 1.321(6) . ?
N5 C3 1.347(6) . ?
C7 C6 1.386(7) . ?
C3 C4 1.390(6) . ?
C4 C5 1.370(6) . ?
C1 N4 1.339(6) . ?
C1 C2 1.480(7) . ?
N4 N3 1.345(5) . ?
N4 Zn1 2.002(4) 6_566 ?
N2 N3 1.298(5) . ?
C5 C6 1.392(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
C8 O1 Zn1 109.7(3) . 8_556 ?
O2 C8 O1 124.2(4) . . ?
O2 C8 C5 119.3(4) . . ?
O1 C8 C5 116.5(4) . . ?
O1 Zn1 N1 121.05(15) 8_455 . ?
O1 Zn1 N4 117.72(15) 8_455 6_565 ?
N1 Zn1 N4 105.77(14) . 6_565 ?
O1 Zn1 N5 97.07(15) 8_455 . ?
N1 Zn1 N5 107.16(15) . . ?
N4 Zn1 N5 106.30(14) 6_565 . ?
C1 N1 N2 106.8(3) . . ?
C1 N1 Zn1 135.5(3) . . ?
N2 N1 Zn1 117.6(3) . . ?
C7 N5 C3 118.1(4) . . ?
C7 N5 Zn1 123.4(3) . . ?
C3 N5 Zn1 118.5(3) . . ?
N5 C7 C6 124.0(4) . . ?
N5 C3 C4 121.6(4) . . ?
C5 C4 C3 119.8(4) . . ?
N1 C1 N4 109.2(4) . . ?
N1 C1 C2 125.3(4) . . ?
N4 C1 C2 125.5(4) . . ?
C1 N4 N3 106.7(4) . . ?
C1 N4 Zn1 133.6(3) . 6_566 ?
N3 N4 Zn1 119.6(3) . 6_566 ?
N3 N2 N1 108.5(3) . . ?
N2 N3 N4 108.7(4) . . ?
C4 C5 C6 118.8(4) . . ?
C4 C5 C8 119.6(4) . . ?
C6 C5 C8 121.6(4) . . ?
C7 C6 C5 117.8(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.135
