# 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_27febam
_database_code_depnum_ccdc_archive 'CCDC 1027616'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'LIGAND ZWITTER ION'
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H8 N2 O4'
_chemical_formula_sum            'C7 H8 N2 O4'
_chemical_formula_weight         184.15

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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_HALL  '-P 2yn'

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                   7.052(2)
_cell_length_b                   8.324(3)
_cell_length_c                   13.410(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.299(6)
_cell_angle_gamma                90.00
_cell_volume                     769.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1460
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      28.24

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             384
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4130
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1504
_reflns_number_gt                1287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1012P)²+0.0585P] 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         1504
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_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 0.5051(3) 0.3612(2) 0.21482(14) 0.0173(5) Uani 1 1 d . . .
H1 H 0.5828 0.3165 0.2750 0.021 Uiso 1 1 calc R . .
C2 C 0.3292(3) 0.5309(2) 0.10813(14) 0.0158(5) Uani 1 1 d . . .
C3 C 0.3401(3) 0.3893(2) 0.05670(14) 0.0157(5) Uani 1 1 d . . .
C4 C 0.2665(3) 0.3430(3) -0.05327(15) 0.0197(5) Uani 1 1 d . . .
C5 C 0.2262(3) 0.6866(2) 0.07562(15) 0.0190(5) Uani 1 1 d . . .
C6 C 0.4999(3) 0.1146(2) 0.11396(16) 0.0215(5) Uani 1 1 d . . .
H6A H 0.5613 0.0694 0.1805 0.032 Uiso 1 1 calc R . .
H6B H 0.5898 0.1072 0.0676 0.032 Uiso 1 1 calc R . .
H6C H 0.3814 0.0544 0.0855 0.032 Uiso 1 1 calc R . .
C7 C 0.4762(3) 0.6225(3) 0.29201(15) 0.0220(5) Uani 1 1 d . . .
H7A H 0.5501 0.5682 0.3529 0.033 Uiso 1 1 calc R . .
H7B H 0.3538 0.6627 0.3058 0.033 Uiso 1 1 calc R . .
H7C H 0.5522 0.7127 0.2744 0.033 Uiso 1 1 calc R . .
N1 N 0.4507(2) 0.28434(18) 0.12656(12) 0.0160(4) Uani 1 1 d . . .
N2 N 0.4353(2) 0.50865(19) 0.20660(11) 0.0163(4) Uani 1 1 d . . .
O1 O 0.3048(2) 0.20863(17) -0.08116(11) 0.0259(4) Uani 1 1 d . . .
O2 O 0.1722(2) 0.45117(18) -0.11158(10) 0.0230(4) Uani 1 1 d . . .
O3 O 0.1384(2) 0.69648(17) -0.01927(11) 0.0250(4) Uani 1 1 d . . .
H3 H 0.1509 0.6094 -0.0489 0.038 Uiso 1 1 calc R . .
O4 O 0.2302(2) 0.79381(16) 0.13764(12) 0.0244(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0154(10) 0.0201(11) 0.0155(10) 0.0015(7) 0.0017(8) -0.0011(7)
C2 0.0138(10) 0.0183(10) 0.0156(10) 0.0006(7) 0.0036(8) -0.0013(8)
C3 0.0124(10) 0.0186(10) 0.0158(10) 0.0020(7) 0.0026(8) -0.0018(7)
C4 0.0157(10) 0.0260(12) 0.0172(10) -0.0014(8) 0.0027(8) -0.0038(8)
C5 0.0152(10) 0.0194(11) 0.0229(11) 0.0040(8) 0.0056(8) -0.0008(8)
C6 0.0265(12) 0.0133(10) 0.0243(11) 0.0008(8) 0.0047(9) 0.0026(8)
C7 0.0233(11) 0.0230(11) 0.0188(10) -0.0069(8) 0.0025(8) 0.0000(8)
N1 0.0156(9) 0.0142(9) 0.0174(8) 0.0000(6) 0.0016(7) -0.0001(6)
N2 0.0164(9) 0.0187(9) 0.0136(9) -0.0008(6) 0.0028(7) -0.0011(7)
O1 0.0282(9) 0.0251(9) 0.0225(8) -0.0078(6) 0.0013(6) 0.0028(6)
O2 0.0241(9) 0.0271(9) 0.0163(8) 0.0026(6) 0.0008(6) 0.0007(6)
O3 0.0294(9) 0.0230(9) 0.0217(8) 0.0043(6) 0.0033(7) 0.0062(6)
O4 0.0270(9) 0.0175(8) 0.0295(9) -0.0026(6) 0.0080(7) 0.0018(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.318(3) . ?
C1 N1 1.328(3) . ?
C2 C3 1.376(3) . ?
C2 N2 1.385(2) . ?
C2 C5 1.504(3) . ?
C3 N1 1.392(2) . ?
C3 C4 1.506(3) . ?
C4 O1 1.227(3) . ?
C4 O2 1.282(3) . ?
C5 O4 1.216(2) . ?
C5 O3 1.294(2) . ?
C6 N1 1.473(2) . ?
C7 N2 1.467(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 110.01(17) . . ?
C3 C2 N2 106.65(16) . . ?
C3 C2 C5 131.91(18) . . ?
N2 C2 C5 121.43(17) . . ?
C2 C3 N1 106.48(16) . . ?
C2 C3 C4 131.74(17) . . ?
N1 C3 C4 121.68(17) . . ?
O1 C4 O2 124.99(19) . . ?
O1 C4 C3 118.67(18) . . ?
O2 C4 C3 116.31(18) . . ?
O4 C5 O3 124.22(19) . . ?
O4 C5 C2 119.65(18) . . ?
O3 C5 C2 116.14(18) . . ?
C1 N1 C3 108.14(16) . . ?
C1 N1 C6 122.27(16) . . ?
C3 N1 C6 129.54(16) . . ?
C1 N2 C2 108.71(16) . . ?
C1 N2 C7 121.89(17) . . ?
C2 N2 C7 129.39(17) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_3aprb
_database_code_depnum_ccdc_archive 'CCDC 1027617'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Zn monomer'
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H11 Cl N2 O6 Zn, H2 O'
_chemical_formula_sum            'C7 H13 Cl N2 O7 Zn'
_chemical_formula_weight         338.01

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'
Cl Cl 0.1484 0.1585 '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   'p 21/n'
_symmetry_space_group_name_hall  '-p 2yn'

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                   8.4910(17)
_cell_length_b                   8.0410(16)
_cell_length_c                   18.847(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.16(3)
_cell_angle_gamma                90.00
_cell_volume                     1262.5(4)
_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       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?


_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6839
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2461
_reflns_number_gt                2135
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
H55 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O1W H55 was given to fix with O1W atom.
H66 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O2W H66 was given to fix with O2W atom.
H5 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O1W H5 was given to fix with O1W atom.
H6 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O2W H6 was given to fix with O2W atom.
H77 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O3W H77 was given to fix with O3W atom.
H78 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O3W H78 was given to fix with O3W atom.
;

_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+0.7638P] 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         2461
_refine_ls_number_parameters     183
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.1079
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

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 0.9416(4) 0.7239(4) -0.02000(16) 0.0139(7) Uani 1 1 d . . .
H1 H 0.9453 0.6703 -0.0634 0.017 Uiso 1 1 calc R . .
C2 C 1.0158(4) 0.8503(4) 0.08543(16) 0.0122(6) Uani 1 1 d . . .
C3 C 0.8528(4) 0.8381(4) 0.07159(16) 0.0132(6) Uani 1 1 d . . .
C4 C 1.1339(4) 0.9206(4) 0.14967(17) 0.0120(6) Uani 1 1 d . . .
C5 C 0.7383(4) 0.8900(4) 0.11775(16) 0.0132(6) Uani 1 1 d . . .
C6 C 0.6472(4) 0.7149(4) -0.03298(17) 0.0179(7) Uani 1 1 d . . .
H6A H 0.6529 0.6595 -0.0775 0.027 Uiso 1 1 calc R . .
H6B H 0.5844 0.8144 -0.0431 0.027 Uiso 1 1 calc R . .
H6C H 0.5981 0.6425 -0.0031 0.027 Uiso 1 1 calc R . .
C7 C 1.2369(4) 0.7622(4) 0.02103(18) 0.0187(7) Uani 1 1 d . . .
H7A H 1.2891 0.6825 0.0557 0.028 Uiso 1 1 calc R . .
H7B H 1.2897 0.8678 0.0300 0.028 Uiso 1 1 calc R . .
H7C H 1.2424 0.7252 -0.0269 0.028 Uiso 1 1 calc R . .
Cl1 Cl 0.79110(10) 0.96128(9) 0.36076(4) 0.0159(2) Uani 1 1 d . . .
N1 N 0.8100(3) 0.7582(3) 0.00488(14) 0.0134(6) Uani 1 1 d . . .
N2 N 1.0682(3) 0.7790(3) 0.02757(13) 0.0126(6) Uani 1 1 d . . .
O1 O 0.8058(3) 0.9229(3) 0.18337(12) 0.0130(5) Uani 1 1 d . . .
O2 O 0.5938(3) 0.8997(3) 0.09249(12) 0.0181(5) Uani 1 1 d . . .
O3 O 1.1685(3) 1.0692(3) 0.14693(13) 0.0184(5) Uani 1 1 d . . .
O4 O 1.1856(3) 0.8173(3) 0.19839(11) 0.0152(5) Uani 1 1 d . . .
O1W O 0.5238(3) 0.7252(3) 0.23671(14) 0.0297(6) Uani 1 1 d D . .
H5 H 0.5467 0.6727 0.2746 0.045 Uiso 1 1 calc RD . .
O2W O 0.5156(3) 1.1471(3) 0.21473(14) 0.0277(6) Uani 1 1 d D . .
H6 H 0.4256 1.1209 0.1932 0.042 Uiso 1 1 calc RD . .
O3W O 0.1797(3) 0.4731(3) 0.16321(13) 0.0229(6) Uani 1 1 d D . .
Zn1 Zn 0.64217(4) 0.94183(4) 0.246974(18) 0.01264(16) Uani 1 1 d . . .
H55 H 0.421(3) 0.742(7) 0.234(3) 0.08(2) Uiso 1 1 d D . .
H66 H 0.550(5) 1.205(5) 0.1806(19) 0.060(16) Uiso 1 1 d D . .
H77 H 0.169(5) 0.573(2) 0.1726(18) 0.019(10) Uiso 1 1 d D . .
H78 H 0.208(6) 0.433(4) 0.2037(14) 0.045(15) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0179(16) 0.0160(16) 0.0082(15) 0.0029(12) 0.0035(12) 0.0023(13)
C2 0.0145(15) 0.0134(15) 0.0098(14) 0.0000(12) 0.0046(12) 0.0002(12)
C3 0.0137(16) 0.0143(16) 0.0116(15) 0.0008(12) 0.0022(12) -0.0010(12)
C4 0.0067(15) 0.0177(17) 0.0131(16) -0.0042(12) 0.0061(12) 0.0010(12)
C5 0.0144(16) 0.0129(15) 0.0125(15) 0.0012(12) 0.0030(12) -0.0014(12)
C6 0.0153(17) 0.0230(18) 0.0139(16) -0.0025(13) -0.0009(13) -0.0023(13)
C7 0.0132(16) 0.0284(19) 0.0153(16) -0.0045(14) 0.0046(13) 0.0010(14)
Cl1 0.0189(4) 0.0186(4) 0.0101(4) 0.0003(3) 0.0023(3) 0.0004(3)
N1 0.0149(13) 0.0163(14) 0.0087(12) 0.0003(10) 0.0013(10) -0.0015(10)
N2 0.0153(14) 0.0160(14) 0.0073(12) -0.0012(10) 0.0040(10) 0.0023(11)
O1 0.0111(11) 0.0175(12) 0.0108(11) -0.0027(8) 0.0028(9) -0.0006(8)
O2 0.0121(12) 0.0273(13) 0.0146(12) -0.0012(10) 0.0019(9) 0.0025(10)
O3 0.0198(13) 0.0162(13) 0.0175(12) 0.0006(9) -0.0002(10) -0.0028(9)
O4 0.0166(12) 0.0168(11) 0.0111(11) 0.0014(9) -0.0004(9) 0.0009(9)
O1W 0.0256(15) 0.0335(15) 0.0301(15) 0.0042(12) 0.0052(12) 0.0010(12)
O2W 0.0249(14) 0.0284(15) 0.0303(15) 0.0020(12) 0.0066(11) 0.0001(11)
O3W 0.0341(15) 0.0171(13) 0.0160(13) -0.0025(10) 0.0009(11) 0.0012(11)
Zn1 0.0125(2) 0.0147(2) 0.0113(2) 0.00014(13) 0.00365(16) 0.00042(13)

_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 1.322(4) . ?
C1 N2 1.335(4) . ?
C2 C3 1.361(4) . ?
C2 N2 1.380(4) . ?
C2 C4 1.524(4) . ?
C3 N1 1.396(4) . ?
C3 C5 1.485(4) . ?
C4 O3 1.233(4) . ?
C4 O4 1.253(4) . ?
C5 O2 1.230(4) . ?
C5 O1 1.286(4) . ?
C6 N1 1.469(4) . ?
C7 N2 1.468(4) . ?
Cl1 Zn1 2.2743(11) . ?
O1 Zn1 2.009(2) . ?
O1W Zn1 2.002(3) . ?
O2W Zn1 1.999(3) . ?

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 N2 108.6(3) . . ?
C3 C2 N2 106.9(3) . . ?
C3 C2 C4 131.8(3) . . ?
N2 C2 C4 121.3(3) . . ?
C2 C3 N1 106.5(3) . . ?
C2 C3 C5 128.7(3) . . ?
N1 C3 C5 124.8(3) . . ?
O3 C4 O4 128.3(3) . . ?
O3 C4 C2 116.9(3) . . ?
O4 C4 C2 114.8(3) . . ?
O2 C5 O1 125.8(3) . . ?
O2 C5 C3 120.6(3) . . ?
O1 C5 C3 113.6(3) . . ?
C1 N1 C3 109.0(3) . . ?
C1 N1 C6 123.9(3) . . ?
C3 N1 C6 127.1(3) . . ?
C1 N2 C2 109.1(3) . . ?
C1 N2 C7 125.8(3) . . ?
C2 N2 C7 125.0(3) . . ?
C5 O1 Zn1 110.98(19) . . ?
O2W Zn1 O1W 117.30(11) . . ?
O2W Zn1 O1 105.94(10) . . ?
O1W Zn1 O1 105.59(10) . . ?
O2W Zn1 Cl1 113.46(8) . . ?
O1W Zn1 Cl1 109.16(8) . . ?
O1 Zn1 Cl1 104.20(7) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.118
####################################################################### 
# 
# 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_24jula
_database_code_depnum_ccdc_archive 'CCDC 1027618'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            Zinc-herringbone
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H25 N6 O14 Zn2, I'
_chemical_formula_sum            'C21 H25 I N6 O14 Zn2'
_chemical_formula_weight         843.11

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ORTHORHOMBIC
_symmetry_space_group_name_H-M   Pccn
_symmetry_space_group_name_HALL  '-P 2ab 2ac'

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

_cell_length_a                   22.552(5)
_cell_length_b                   10.123(2)
_cell_length_c                   13.594(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3103.4(11)
_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       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    2.614
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.9301
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_process_details   sadabs

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16258
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3049
_reflns_number_gt                2396
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 H15 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5 H15 was given to fix with O5 atom.
 H16 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5 H16 was given to fix with O5 atom.
;

_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)+(0.0999P)²+3.5886P] 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         3049
_refine_ls_number_parameters     208
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1418
_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 0.0307(2) 0.2258(5) 0.6055(4) 0.0211(11) Uani 1 1 d . . .
H1 H 0.0317 0.2380 0.6733 0.025 Uiso 1 1 calc R . .
C2 C 0.0046(2) 0.2441(5) 0.4491(4) 0.0195(11) Uani 1 1 d . . .
C3 C 0.0508(2) 0.1510(5) 0.4571(4) 0.0167(10) Uani 1 1 d . . .
C4 C -0.0320(2) 0.2886(5) 0.3627(4) 0.0189(11) Uani 1 1 d . . .
C5 C 0.0780(2) 0.0640(5) 0.3794(4) 0.0187(11) Uani 1 1 d . . .
C6 C -0.0571(2) 0.3768(5) 0.5745(4) 0.0239(12) Uani 1 1 d . . .
H6A H -0.0937 0.3307 0.5638 0.036 Uiso 1 1 calc R . .
H6B H -0.0567 0.4563 0.5360 0.036 Uiso 1 1 calc R . .
H6C H -0.0534 0.3986 0.6429 0.036 Uiso 1 1 calc R . .
C7 C 0.1142(2) 0.0585(6) 0.5995(4) 0.0256(12) Uani 1 1 d . . .
H7A H 0.1397 0.1132 0.6388 0.038 Uiso 1 1 calc R . .
H7B H 0.1369 0.0183 0.5478 0.038 Uiso 1 1 calc R . .
H7C H 0.0971 -0.0092 0.6400 0.038 Uiso 1 1 calc R . .
C8 C 0.2286(2) 0.1984(5) 0.0112(4) 0.0194(11) Uani 1 1 d . . .
C9 C 0.1746(3) 0.0691(5) -0.1263(4) 0.0251(12) Uani 1 1 d . . .
H9A H 0.1347 0.1017 -0.1206 0.038 Uiso 1 1 calc R . .
H9B H 0.1784 -0.0113 -0.0894 0.038 Uiso 1 1 calc R . .
H9C H 0.1835 0.0524 -0.1942 0.038 Uiso 1 1 calc R . .
C10 C 0.2500 0.2500 -0.1434(5) 0.0212(16) Uani 1 2 d S . .
H10 H 0.2500 0.2500 -0.2118 0.025 Uiso 1 2 calc SR . .
C11 C 0.2018(2) 0.1254(5) 0.0965(4) 0.0200(11) Uani 1 1 d . . .
I1 I 0.2500 0.7500 0.49474(4) 0.0364(2) Uani 1 2 d S . .
N1 N 0.06589(18) 0.1412(4) 0.5557(3) 0.0182(9) Uani 1 1 d . . .
N2 N -0.00610(19) 0.2900(4) 0.5442(3) 0.0203(9) Uani 1 1 d . . .
N3 N 0.21681(19) 0.1699(4) -0.0866(3) 0.0192(9) Uani 1 1 d . . .
O1 O -0.04766(17) 0.2068(4) 0.3013(3) 0.0255(9) Uani 1 1 d . . .
O2 O -0.04417(16) 0.4125(3) 0.3622(3) 0.0224(8) Uani 1 1 d . . .
O3 O 0.09234(17) 0.1230(3) 0.2993(2) 0.0231(8) Uani 1 1 d . . .
O4 O 0.08370(18) -0.0538(4) 0.3959(3) 0.0306(9) Uani 1 1 d . . .
O1W O 0.1725(2) -0.1662(5) 0.2383(4) 0.0443(12) Uani 1 1 d D . .
H16 H 0.1527 -0.2332 0.2461 0.066 Uiso 1 1 calc RD . .
O6 O 0.23552(16) 0.1037(3) 0.1679(3) 0.0240(8) Uani 1 1 d . . .
O7 O 0.14533(15) 0.0904(3) 0.0855(2) 0.0220(8) Uani 1 1 d . . .
Zn1 Zn 0.11811(3) -0.01234(6) 0.20271(4) 0.0180(2) Uani 1 1 d . . .
H15 H 0.197(3) -0.191(6) 0.193(4) 0.07(3) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.027(3) 0.028(3) 0.008(2) 0.001(2) -0.002(2) -0.003(2)
C2 0.027(3) 0.022(3) 0.010(3) -0.0041(19) 0.000(2) -0.007(2)
C3 0.026(3) 0.015(2) 0.009(2) 0.0035(19) -0.001(2) -0.002(2)
C4 0.023(3) 0.024(3) 0.009(2) 0.002(2) 0.000(2) -0.001(2)
C5 0.020(3) 0.023(3) 0.013(2) -0.004(2) -0.005(2) -0.002(2)
C6 0.031(3) 0.026(3) 0.014(3) -0.005(2) 0.004(2) 0.007(2)
C7 0.031(3) 0.031(3) 0.015(3) 0.004(2) -0.005(2) 0.005(2)
C8 0.026(3) 0.022(3) 0.010(2) -0.006(2) 0.000(2) -0.001(2)
C9 0.036(3) 0.029(3) 0.010(2) -0.004(2) -0.001(2) -0.010(2)
C10 0.030(4) 0.026(4) 0.008(3) 0.000 0.000 -0.004(3)
C11 0.033(3) 0.017(3) 0.011(2) -0.0027(19) 0.002(2) 0.000(2)
I1 0.0462(4) 0.0417(4) 0.0213(3) 0.000 0.000 -0.0100(3)
N1 0.024(2) 0.022(2) 0.009(2) 0.0039(17) -0.0018(17) -0.0010(18)
N2 0.024(2) 0.027(2) 0.010(2) -0.0034(18) 0.0012(18) -0.0018(19)
N3 0.031(2) 0.021(2) 0.005(2) 0.0004(16) -0.0027(17) -0.0026(18)
O1 0.040(2) 0.024(2) 0.0122(19) -0.0017(15) -0.0078(17) 0.0012(17)
O2 0.030(2) 0.0209(19) 0.0165(19) -0.0001(14) -0.0015(15) 0.0000(15)
O3 0.035(2) 0.0207(19) 0.0141(19) -0.0009(15) 0.0039(16) 0.0017(16)
O4 0.048(3) 0.0193(19) 0.024(2) -0.0003(16) 0.0096(19) 0.0071(17)
O1W 0.048(3) 0.043(3) 0.041(3) 0.000(2) 0.007(2) 0.011(2)
O6 0.037(2) 0.026(2) 0.0092(18) 0.0012(15) 0.0003(16) -0.0035(16)
O7 0.029(2) 0.0243(19) 0.0130(18) 0.0015(14) 0.0010(15) -0.0019(15)
Zn1 0.0260(4) 0.0197(3) 0.0082(3) -0.0007(2) 0.0014(2) -0.0005(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.344(7) . ?
C1 N1 1.350(7) . ?
C2 N2 1.394(7) . ?
C2 C3 1.409(7) . ?
C2 C4 1.505(7) . ?
C3 N1 1.387(6) . ?
C3 C5 1.506(7) . ?
C4 O1 1.227(6) . ?
C4 O2 1.284(6) . ?
C5 O4 1.220(6) . ?
C5 O3 1.283(6) . ?
C6 N2 1.504(6) . ?
C7 N1 1.498(6) . ?
C8 N3 1.387(6) . ?
C8 C8 1.422(11) 2 ?
C8 C11 1.502(7) . ?
C9 N3 1.496(6) . ?
C10 N3 1.347(6) . ?
C10 N3 1.347(6) 2 ?
C11 O6 1.253(6) . ?
C11 O7 1.330(6) . ?
O2 Zn1 2.034(4) 4 ?
O3 Zn1 1.985(3) . ?
O1W Zn1 2.041(5) . ?
O7 Zn1 1.999(3) . ?
Zn1 O2 2.034(4) 4_545 ?

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
N2 C1 N1 111.1(4) . . ?
N2 C2 C3 106.2(5) . . ?
N2 C2 C4 121.9(5) . . ?
C3 C2 C4 131.7(5) . . ?
N1 C3 C2 107.7(4) . . ?
N1 C3 C5 122.4(4) . . ?
C2 C3 C5 129.6(4) . . ?
O1 C4 O2 126.5(5) . . ?
O1 C4 C2 119.1(5) . . ?
O2 C4 C2 114.4(4) . . ?
O4 C5 O3 125.7(5) . . ?
O4 C5 C3 119.0(4) . . ?
O3 C5 C3 115.2(4) . . ?
N3 C8 C8 106.4(3) . 2 ?
N3 C8 C11 124.1(5) . . ?
C8 C8 C11 129.4(3) 2 . ?
N3 C10 N3 110.1(6) . 2 ?
O6 C11 O7 128.4(5) . . ?
O6 C11 C8 116.1(5) . . ?
O7 C11 C8 115.5(4) . . ?
C1 N1 C3 107.1(4) . . ?
C1 N1 C7 125.7(4) . . ?
C3 N1 C7 127.1(4) . . ?
C1 N2 C2 107.8(4) . . ?
C1 N2 C6 125.8(4) . . ?
C2 N2 C6 125.5(4) . . ?
C10 N3 C8 108.5(5) . . ?
C10 N3 C9 123.9(4) . . ?
C8 N3 C9 127.6(4) . . ?
C4 O2 Zn1 122.9(3) . 4 ?
C5 O3 Zn1 108.3(3) . . ?
C11 O7 Zn1 110.1(3) . . ?
O3 Zn1 O7 104.95(14) . . ?
O3 Zn1 O2 107.77(15) . 4_545 ?
O7 Zn1 O2 95.76(14) . 4_545 ?
O3 Zn1 O1W 123.09(17) . . ?
O7 Zn1 O1W 113.66(18) . . ?
O2 Zn1 O1W 108.08(17) 4_545 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.317
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.185
####################################################################### 
# 
# 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_2octbm
_database_code_depnum_ccdc_archive 'CCDC 1027619'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            'ZN DIMER'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H14 N4 O8 Zn2, I, 2(H2 O)'
_chemical_formula_sum            'C14 H18 I N4 O10 Zn2'
_chemical_formula_weight         659.96

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'
I I -0.4742 1.8119 '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                   7.9324(13)
_cell_length_b                   8.4897(14)
_cell_length_c                   10.8444(18)
_cell_angle_alpha                80.027(3)
_cell_angle_beta                 72.510(3)
_cell_angle_gamma                64.679(2)
_cell_volume                     628.78(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2012
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.30

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            WHITE
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             323
_exptl_absorpt_coefficient_mu    3.185
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.9301
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3533
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2413
_reflns_number_gt                2161
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
 H55 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5 H55 was given to fix with O5 atom.
 H56 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5 H56 was given to fix with O5 atom.
;

_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)+(0.1087P)²+2.8251P] 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         2413
_refine_ls_number_parameters     164
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1627
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 0.7676(8) 0.9482(7) 0.8822(5) 0.0233(11) Uani 1 1 d . . .
H1 H 0.7724 0.9618 0.9660 0.028 Uiso 1 1 calc R . .
C2 C 0.7604(7) 0.9976(7) 0.6767(5) 0.0186(10) Uani 1 1 d . . .
C3 C 0.7556(8) 0.8389(7) 0.7165(5) 0.0193(11) Uani 1 1 d . . .
C4 C 0.7361(7) 0.7097(7) 0.6484(5) 0.0188(11) Uani 1 1 d . . .
C5 C 0.7437(7) 1.0959(7) 0.5501(5) 0.0188(10) Uani 1 1 d . . .
C6 C 0.7571(10) 0.6542(8) 0.9288(6) 0.0305(13) Uani 1 1 d . . .
H6A H 0.8762 0.5532 0.8969 0.046 Uiso 1 1 calc R . .
H6B H 0.6460 0.6327 0.9268 0.046 Uiso 1 1 calc R . .
H6C H 0.7473 0.6726 1.0179 0.046 Uiso 1 1 calc R . .
C7 C 0.7752(9) 1.2336(7) 0.7876(6) 0.0247(12) Uani 1 1 d . . .
H7A H 0.7960 1.2397 0.8710 0.037 Uiso 1 1 calc R . .
H7B H 0.6532 1.3284 0.7779 0.037 Uiso 1 1 calc R . .
H7C H 0.8815 1.2452 0.7173 0.037 Uiso 1 1 calc R . .
I1 I 0.2381(2) 0.69761(17) 0.83754(13) 0.0200(3) Uani 0.25 1 d P . .
I2 I 0.2738(2) 1.12849(16) 0.79379(12) 0.0188(3) Uani 0.25 1 d P . .
N1 N 0.7597(7) 0.8106(6) 0.8458(4) 0.0214(10) Uani 1 1 d . . .
N2 N 0.7676(6) 1.0642(6) 0.7824(4) 0.0197(9) Uani 1 1 d . . .
O1 O 0.5897(5) 0.7655(5) 0.6034(4) 0.0221(8) Uani 1 1 d . . .
O2 O 0.8619(5) 0.5604(5) 0.6410(4) 0.0246(9) Uani 1 1 d . . .
O3 O 0.6724(5) 1.2572(5) 0.5488(4) 0.0228(8) Uani 1 1 d . . .
O4 O 0.8019(5) 1.0004(5) 0.4548(4) 0.0215(8) Uani 1 1 d . . .
O5 O 0.7408(7) 0.5317(6) 0.3995(5) 0.0357(10) Uani 1 1 d D . .
Zn1 Zn 0.31495(8) 0.89927(7) 0.69217(6) 0.0193(3) Uani 1 1 d . . .
H56 H 0.735(11) 0.434(6) 0.424(9) 0.06(3) Uiso 1 1 d D . .
H55 H 0.863(4) 0.500(10) 0.373(10) 0.07(3) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.031(3) 0.023(3) 0.019(3) 0.000(2) -0.012(2) -0.011(2)
C2 0.018(2) 0.017(2) 0.022(3) -0.002(2) -0.007(2) -0.007(2)
C3 0.021(3) 0.020(3) 0.018(3) 0.002(2) -0.008(2) -0.008(2)
C4 0.018(2) 0.022(3) 0.016(2) -0.003(2) 0.001(2) -0.011(2)
C5 0.018(2) 0.022(3) 0.021(3) 0.002(2) -0.009(2) -0.010(2)
C6 0.046(4) 0.027(3) 0.024(3) 0.006(2) -0.014(3) -0.019(3)
C7 0.030(3) 0.024(3) 0.029(3) -0.003(2) -0.011(2) -0.016(2)
I1 0.0263(7) 0.0172(7) 0.0195(7) 0.0019(5) -0.0053(5) -0.0128(5)
I2 0.0265(7) 0.0163(7) 0.0149(6) -0.0039(5) -0.0052(5) -0.0087(5)
N1 0.028(2) 0.022(2) 0.017(2) 0.0021(18) -0.0098(19) -0.011(2)
N2 0.023(2) 0.019(2) 0.020(2) -0.0019(18) -0.0103(18) -0.0074(18)
O1 0.0183(18) 0.0226(19) 0.025(2) -0.0091(16) -0.0054(15) -0.0053(15)
O2 0.0215(19) 0.019(2) 0.032(2) -0.0036(16) -0.0075(17) -0.0051(16)
O3 0.0238(19) 0.0187(19) 0.029(2) 0.0005(15) -0.0105(16) -0.0096(16)
O4 0.0249(19) 0.0210(19) 0.0186(19) -0.0021(15) -0.0093(15) -0.0064(16)
O5 0.041(3) 0.031(2) 0.036(3) 0.001(2) -0.013(2) -0.014(2)
Zn1 0.0209(4) 0.0193(4) 0.0184(4) -0.0022(2) -0.0064(3) -0.0075(3)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.327(7) . ?
C1 N2 1.331(7) . ?
C2 C3 1.354(7) . ?
C2 N2 1.389(7) . ?
C2 C5 1.489(7) . ?
C3 N1 1.389(7) . ?
C3 C4 1.506(7) . ?
C4 O2 1.230(7) . ?
C4 O1 1.265(7) . ?
C5 O3 1.237(7) . ?
C5 O4 1.274(7) . ?
C6 N1 1.474(7) . ?
C7 N2 1.476(7) . ?
I1 Zn1 2.2733(14) . ?
I2 Zn1 2.2562(14) . ?
O1 Zn1 1.992(4) . ?
O4 Zn1 1.967(4) 2_676 ?
Zn1 O4 1.967(4) 2_676 ?

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 N2 109.1(5) . . ?
C3 C2 N2 106.8(5) . . ?
C3 C2 C5 129.0(5) . . ?
N2 C2 C5 124.1(5) . . ?
C2 C3 N1 107.2(5) . . ?
C2 C3 C4 131.5(5) . . ?
N1 C3 C4 121.2(5) . . ?
O2 C4 O1 125.6(5) . . ?
O2 C4 C3 118.0(5) . . ?
O1 C4 C3 116.3(5) . . ?
O3 C5 O4 127.6(5) . . ?
O3 C5 C2 118.0(5) . . ?
O4 C5 C2 114.4(5) . . ?
C1 N1 C3 108.4(5) . . ?
C1 N1 C6 125.6(5) . . ?
C3 N1 C6 126.0(5) . . ?
C1 N2 C2 108.5(4) . . ?
C1 N2 C7 124.1(5) . . ?
C2 N2 C7 127.4(5) . . ?
C4 O1 Zn1 128.3(3) . . ?
C5 O4 Zn1 117.5(3) . 2_676 ?
O4 Zn1 O1 101.97(16) 2_676 . ?
O4 Zn1 I2 105.84(12) 2_676 . ?
O1 Zn1 I2 112.71(11) . . ?
O4 Zn1 I1 122.35(12) 2_676 . ?
O1 Zn1 I1 102.99(12) . . ?
I2 Zn1 I1 110.73(5) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.969
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.185
####################################################################### 
# 
# 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_17febam
_database_code_depnum_ccdc_archive 'CCDC 1027620'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'zINC NITRATE MONOMER'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H24 N4 O13 Zn'
_chemical_formula_sum            'C14 H24 N4 O13 Zn'
_chemical_formula_weight         521.74

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   'P 21/C'
_symmetry_space_group_name_HALL  '-P 2ybc'

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                   15.075(2)
_cell_length_b                   8.3079(12)
_cell_length_c                   16.676(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.800(3)
_cell_angle_gamma                90.00
_cell_volume                     2086.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2804
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.82

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11326
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4082
_reflns_number_gt                3145
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
H9 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O1W H9 was given to fix with O1W atom.
H10 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O1W H10 was given to fix with O1W atom.
H100 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O2W H100 was given to fix with O2W atom.
H101 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O2W H101 was given to fix with O2W atom.
H11 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O3W H11 was given to fix with O3W atom.
H12 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O3W H12 was given to fix with O3W atom.
H120 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O4W H120 was given to fix with O4W atom.
H121 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O4W H121 was given to fix with O4W atom.
H130 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5W H130 was given to fix with O5W atom.
H131 atom was located in difference map positions and refined positionally with DFIX restraint and DFIX 0.84 O5W H131 was given to fix with O5W atom.
;

_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)+(0.0886P)²+2.4251P] 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         4082
_refine_ls_number_parameters     324
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1726
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.143
_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
C1 C 1.1021(3) 0.1348(6) 0.8770(3) 0.0254(10) Uani 1 1 d . . .
H1 H 1.1618 0.1631 0.8780 0.031 Uiso 1 1 calc R . .
C2 C 0.9781(3) -0.0091(6) 0.8776(3) 0.0196(9) Uani 1 1 d . . .
C3 C 0.9563(3) 0.1508(5) 0.8729(3) 0.0195(9) Uani 1 1 d . . .
C4 C 0.8668(3) 0.2297(5) 0.8715(3) 0.0200(9) Uani 1 1 d . . .
C5 C 0.9192(3) -0.1559(5) 0.8795(3) 0.0208(10) Uani 1 1 d . . .
C6 C 1.1250(3) -0.1625(6) 0.8803(3) 0.0279(11) Uani 1 1 d . . .
H6A H 1.1851 -0.1344 0.8697 0.042 Uiso 1 1 calc R . .
H6B H 1.1021 -0.2353 0.8397 0.042 Uiso 1 1 calc R . .
H6C H 1.1237 -0.2133 0.9319 0.042 Uiso 1 1 calc R . .
C7 C 1.0444(3) 0.4141(5) 0.8749(3) 0.0262(11) Uani 1 1 d . . .
H7A H 1.1057 0.4423 0.8847 0.039 Uiso 1 1 calc R . .
H7B H 1.0101 0.4568 0.9170 0.039 Uiso 1 1 calc R . .
H7C H 1.0232 0.4583 0.8243 0.039 Uiso 1 1 calc R . .
C8 C 0.4816(3) 0.1542(5) 1.0898(3) 0.0216(10) Uani 1 1 d . . .
H8 H 0.4908 0.1089 1.1405 0.026 Uiso 1 1 calc R . .
C9 C 0.4174(3) 0.2281(5) 0.9739(2) 0.0155(9) Uani 1 1 d . . .
C10 C 0.5025(3) 0.2858(5) 0.9773(2) 0.0182(9) Uani 1 1 d . . .
C11 C 0.5473(3) 0.3835(5) 0.9167(3) 0.0178(9) Uani 1 1 d . . .
C12 C 0.3457(3) 0.2327(5) 0.9070(3) 0.0186(9) Uani 1 1 d . . .
C13 C 0.3249(3) 0.0628(6) 1.0674(3) 0.0267(11) Uani 1 1 d . . .
H13A H 0.3358 0.0111 1.1184 0.040 Uiso 1 1 calc R . .
H13B H 0.3086 -0.0166 1.0275 0.040 Uiso 1 1 calc R . .
H13C H 0.2776 0.1393 1.0711 0.040 Uiso 1 1 calc R . .
C14 C 0.6312(3) 0.2717(6) 1.0842(3) 0.0226(10) Uani 1 1 d . . .
H14A H 0.6359 0.3842 1.0969 0.034 Uiso 1 1 calc R . .
H14B H 0.6736 0.2444 1.0454 0.034 Uiso 1 1 calc R . .
H14C H 0.6428 0.2094 1.1321 0.034 Uiso 1 1 calc R . .
N1 N 1.0705(2) -0.0170(5) 0.8797(2) 0.0220(8) Uani 1 1 d . . .
N2 N 1.0354(2) 0.2359(4) 0.8727(2) 0.0201(8) Uani 1 1 d . . .
N3 N 0.4061(2) 0.1466(4) 1.0445(2) 0.0185(8) Uani 1 1 d . . .
N4 N 0.5412(2) 0.2365(4) 1.0512(2) 0.0181(8) Uani 1 1 d . . .
O1 O 0.8577(2) 0.3532(4) 0.82691(18) 0.0232(7) Uani 1 1 d . . .
O2 O 0.8104(2) 0.1728(4) 0.9139(2) 0.0275(8) Uani 1 1 d . . .
O3 O 0.8599(2) -0.1638(4) 0.82345(19) 0.0255(7) Uani 1 1 d . . .
O4 O 0.9343(2) -0.2523(4) 0.93450(19) 0.0260(7) Uani 1 1 d . . .
O5 O 0.6288(2) 0.4060(4) 0.92937(19) 0.0271(8) Uani 1 1 d . . .
O6 O 0.4987(2) 0.4289(4) 0.85845(19) 0.0244(7) Uani 1 1 d . . .
O7 O 0.2828(2) 0.3289(4) 0.91379(18) 0.0219(7) Uani 1 1 d . . .
O8 O 0.3557(2) 0.1349(4) 0.8514(2) 0.0304(8) Uani 1 1 d . . .
O1W O 0.7985(2) 0.5379(4) 0.95780(18) 0.0222(7) Uani 1 1 d D . .
H9 H 0.7619 0.5711 0.9886 0.033 Uiso 1 1 calc RD . .
O2W O 0.7217(2) 0.6361(4) 0.79866(19) 0.0242(7) Uani 1 1 d D . .
H100 H 0.7134 0.6173 0.7506 0.036 Uiso 1 1 calc RD . .
O3W O 0.6744(2) 0.2817(4) 0.77237(19) 0.0230(7) Uani 1 1 d D . .
H11 H 0.7080 0.2076 0.7624 0.034 Uiso 1 1 calc RD . .
O4W O 0.4793(2) 0.6121(4) 0.7267(2) 0.0252(7) Uani 1 1 d D . .
O5W O 0.7719(2) 0.0399(4) 0.7164(2) 0.0250(7) Uani 1 1 d D . .
Zn1 Zn 0.73311(3) 0.42616(6) 0.85977(3) 0.0199(2) Uani 1 1 d . . .
H120 H 0.493(3) 0.565(5) 0.7683(18) 0.017(13) Uiso 1 1 d D . .
H121 H 0.529(2) 0.642(7) 0.711(3) 0.05(2) Uiso 1 1 d D . .
H12 H 0.6261(15) 0.242(5) 0.779(3) 0.018(13) Uiso 1 1 d D . .
H10 H 0.832(3) 0.615(4) 0.951(3) 0.043(18) Uiso 1 1 d D . .
H101 H 0.768(3) 0.688(7) 0.803(3) 0.05(2) Uiso 1 1 d D . .
H131 H 0.754(4) -0.018(5) 0.679(2) 0.038(17) Uiso 1 1 d D . .
H130 H 0.801(3) -0.020(5) 0.747(2) 0.018(13) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.026(3) 0.024(2) 0.026(2) 0.0039(19) 0.003(2) -0.003(2)
C2 0.016(2) 0.025(2) 0.018(2) -0.0006(18) 0.0032(17) -0.0021(19)
C3 0.014(2) 0.025(2) 0.019(2) -0.0031(18) -0.0012(18) -0.0019(18)
C4 0.021(2) 0.019(2) 0.020(2) -0.0039(17) -0.0013(19) -0.0042(18)
C5 0.020(2) 0.016(2) 0.026(2) -0.0007(18) 0.003(2) -0.0017(18)
C6 0.022(2) 0.026(3) 0.036(3) -0.001(2) 0.000(2) 0.005(2)
C7 0.032(3) 0.015(2) 0.031(3) 0.0020(18) -0.002(2) -0.0057(19)
C8 0.030(3) 0.019(2) 0.016(2) -0.0031(17) 0.0024(19) -0.0029(19)
C9 0.016(2) 0.015(2) 0.016(2) -0.0013(16) 0.0039(17) -0.0013(17)
C10 0.024(2) 0.016(2) 0.014(2) 0.0002(16) -0.0017(18) 0.0035(18)
C11 0.022(2) 0.016(2) 0.015(2) -0.0034(16) 0.0048(18) -0.0014(18)
C12 0.021(2) 0.017(2) 0.019(2) -0.0011(17) 0.0008(18) -0.0048(18)
C13 0.030(3) 0.028(3) 0.022(2) 0.0026(19) 0.002(2) -0.010(2)
C14 0.021(2) 0.024(2) 0.022(2) -0.0047(18) -0.0043(19) -0.0007(19)
N1 0.0181(19) 0.023(2) 0.024(2) -0.0003(16) -0.0024(16) 0.0001(16)
N2 0.0180(19) 0.022(2) 0.0203(19) 0.0005(15) -0.0005(15) -0.0033(16)
N3 0.022(2) 0.0171(19) 0.0170(18) 0.0029(14) 0.0031(16) -0.0056(15)
N4 0.0217(19) 0.0166(18) 0.0157(17) -0.0045(14) 0.0001(15) 0.0017(15)
O1 0.0244(17) 0.0216(17) 0.0234(16) -0.0026(13) -0.0019(14) 0.0037(13)
O2 0.0215(18) 0.0251(18) 0.0363(19) -0.0026(14) 0.0058(15) -0.0012(14)
O3 0.0268(18) 0.0212(17) 0.0277(17) 0.0044(13) -0.0071(15) -0.0068(14)
O4 0.0294(19) 0.0224(17) 0.0256(17) 0.0033(14) -0.0037(14) -0.0041(14)
O5 0.0213(18) 0.043(2) 0.0175(16) -0.0052(14) 0.0064(14) -0.0114(15)
O6 0.0265(18) 0.0258(18) 0.0209(17) 0.0062(13) 0.0027(14) 0.0029(14)
O7 0.0200(16) 0.0245(17) 0.0210(16) -0.0039(13) -0.0005(13) 0.0018(13)
O8 0.0297(19) 0.035(2) 0.0257(17) -0.0123(15) -0.0046(15) 0.0081(16)
O1W 0.0246(18) 0.0222(17) 0.0198(16) -0.0012(13) 0.0023(14) -0.0054(14)
O2W 0.030(2) 0.0204(17) 0.0213(16) 0.0068(13) -0.0069(14) -0.0030(15)
O3W 0.0227(18) 0.0237(17) 0.0229(16) -0.0047(13) 0.0037(14) -0.0035(14)
O4W 0.0248(18) 0.0293(19) 0.0214(17) 0.0112(14) 0.0005(14) 0.0012(15)
O5W 0.0285(19) 0.0233(17) 0.0225(17) 0.0022(14) -0.0041(15) 0.0030(15)
Zn1 0.0203(3) 0.0210(3) 0.0184(3) -0.00022(19) 0.0013(2) -0.0021(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.310(6) . ?
C1 N1 1.349(6) . ?
C2 C3 1.370(7) . ?
C2 N1 1.393(6) . ?
C2 C5 1.510(6) . ?
C3 N2 1.386(6) . ?
C3 C4 1.498(6) . ?
C4 O2 1.228(5) . ?
C4 O1 1.270(5) . ?
C5 O4 1.231(5) . ?
C5 O3 1.263(5) . ?
C6 N1 1.462(6) . ?
C7 N2 1.487(6) . ?
C8 N4 1.321(6) . ?
C8 N3 1.337(6) . ?
C9 C10 1.369(6) . ?
C9 N3 1.376(5) . ?
C9 C12 1.515(6) . ?
C10 N4 1.398(5) . ?
C10 C11 1.485(6) . ?
C11 O6 1.246(6) . ?
C11 O5 1.249(5) . ?
C12 O8 1.248(5) . ?
C12 O7 1.249(5) . ?
C13 N3 1.474(6) . ?
C14 N4 1.469(6) . ?
O1 Zn1 2.073(3) . ?
O5 Zn1 2.007(3) . ?
O1W Zn1 2.086(3) . ?
O2W Zn1 2.023(3) . ?
O3W Zn1 2.055(3) . ?

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
N2 C1 N1 109.3(4) . . ?
C3 C2 N1 106.5(4) . . ?
C3 C2 C5 130.2(4) . . ?
N1 C2 C5 123.4(4) . . ?
C2 C3 N2 106.9(4) . . ?
C2 C3 C4 129.7(4) . . ?
N2 C3 C4 123.4(4) . . ?
O2 C4 O1 126.2(4) . . ?
O2 C4 C3 118.1(4) . . ?
O1 C4 C3 115.7(4) . . ?
O4 C5 O3 128.1(4) . . ?
O4 C5 C2 116.9(4) . . ?
O3 C5 C2 115.0(4) . . ?
N4 C8 N3 109.2(4) . . ?
C10 C9 N3 106.9(4) . . ?
C10 C9 C12 131.0(4) . . ?
N3 C9 C12 121.9(4) . . ?
C9 C10 N4 106.5(4) . . ?
C9 C10 C11 128.3(4) . . ?
N4 C10 C11 125.2(4) . . ?
O6 C11 O5 128.5(4) . . ?
O6 C11 C10 115.2(4) . . ?
O5 C11 C10 116.3(4) . . ?
O8 C12 O7 127.1(4) . . ?
O8 C12 C9 115.0(4) . . ?
O7 C12 C9 117.9(4) . . ?
C1 N1 C2 108.0(4) . . ?
C1 N1 C6 125.0(4) . . ?
C2 N1 C6 126.9(4) . . ?
C1 N2 C3 109.3(4) . . ?
C1 N2 C7 124.6(4) . . ?
C3 N2 C7 125.8(4) . . ?
C8 N3 C9 108.8(4) . . ?
C8 N3 C13 124.8(4) . . ?
C9 N3 C13 126.3(4) . . ?
C8 N4 C10 108.5(4) . . ?
C8 N4 C14 123.9(4) . . ?
C10 N4 C14 127.6(4) . . ?
C4 O1 Zn1 98.9(3) . . ?
C11 O5 Zn1 134.9(3) . . ?
O5 Zn1 O2W 108.26(14) . . ?
O5 Zn1 O3W 92.23(13) . . ?
O2W Zn1 O3W 97.06(13) . . ?
O5 Zn1 O1 150.98(14) . . ?
O2W Zn1 O1 100.08(13) . . ?
O3W Zn1 O1 90.36(13) . . ?
O5 Zn1 O1W 86.43(13) . . ?
O2W Zn1 O1W 92.09(13) . . ?
O3W Zn1 O1W 170.70(13) . . ?
O1 Zn1 O1W 86.41(12) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.141
####################################################################### 
# 
# 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_12augc
_database_code_depnum_ccdc_archive 'CCDC 1027621'
_audit_update_record             
;
2015-01-30 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Cd DDII'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H14 Cd N4 O8'
_chemical_formula_sum            'C14 H14 Cd N4 O8'
_chemical_formula_weight         478.69

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           MONOCLINIC
_symmetry_space_group_name_H-M   C2/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                   8.8373(8)
_cell_length_b                   13.3995(8)
_cell_length_c                   13.4110(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.947(2)
_cell_angle_gamma                90.00
_cell_volume                     1587.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2369
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      27.86

_exptl_crystal_description       NEEDLES
_exptl_crystal_colour            WHITE
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4288
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1532
_reflns_number_gt                1431
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 ISOR command used for C5 and tha value given as 0.01. 
;

_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)+(0.0421P)²+13.2433P] 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         1532
_refine_ls_number_parameters     125
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_restrained_S_all      1.250
_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
C2 C 0.8117(5) 0.0689(4) 0.0478(3) 0.0147(9) Uani 1 1 d . . .
C3 C 0.7337(5) -0.0185(3) 0.0508(3) 0.0127(9) Uani 1 1 d . . .
C6 C 0.6429(6) -0.1469(4) -0.0763(4) 0.0170(10) Uani 1 1 d . . .
H3A H 0.5430 -0.1283 -0.0997 0.025 Uiso 1 1 calc R . .
H3B H 0.6359 -0.1919 -0.0209 0.025 Uiso 1 1 calc R . .
H3C H 0.6950 -0.1790 -0.1291 0.025 Uiso 1 1 calc R . .
C1 C 0.7949(5) 0.0055(3) -0.1053(4) 0.0153(10) Uani 1 1 d . . .
H4 H 0.8038 -0.0031 -0.1736 0.018 Uiso 1 1 calc R . .
C7 C 0.9225(5) 0.1670(4) -0.1001(3) 0.0166(10) Uani 1 1 d . . .
H5A H 1.0301 0.1620 -0.0888 0.025 Uiso 1 1 calc R . .
H5B H 0.8870 0.2284 -0.0723 0.025 Uiso 1 1 calc R . .
H5C H 0.8991 0.1659 -0.1706 0.025 Uiso 1 1 calc R . .
C4 C 0.8572(5) 0.1387(3) 0.1313(3) 0.0135(9) Uani 1 1 d . . .
Cd1 Cd 1.0000 0.29624(3) 0.2500 0.01423(19) Uani 1 2 d S . .
N1 N 0.8477(4) 0.0821(3) -0.0521(3) 0.0139(8) Uani 1 1 d . . .
N2 N 0.7271(4) -0.0568(3) -0.0441(3) 0.0139(8) Uani 1 1 d . . .
O1 O 0.9462(4) 0.2086(2) 0.1103(3) 0.0201(8) Uani 1 1 d . . .
O2 O 0.8016(4) 0.1220(3) 0.2134(3) 0.0249(8) Uani 1 1 d . . .
O3 O 0.7298(4) -0.1319(3) 0.1887(3) 0.0196(8) Uani 1 1 d . . .
O4 O 0.5138(4) -0.0666(3) 0.1313(3) 0.0218(8) Uani 1 1 d . . .
C5 C 0.6537(5) -0.0751(3) 0.1321(3) 0.0119(9) Uani 1 1 d U . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C2 0.016(2) 0.017(2) 0.011(2) -0.0001(18) 0.0041(18) 0.0022(19)
C3 0.018(2) 0.014(2) 0.006(2) -0.0003(17) 0.0031(17) 0.0015(18)
C6 0.024(2) 0.015(2) 0.011(2) -0.0045(18) 0.0017(18) -0.008(2)
C1 0.016(2) 0.014(2) 0.015(2) -0.0042(18) -0.0043(18) -0.0026(18)
C7 0.021(2) 0.019(2) 0.010(2) -0.0008(19) 0.0026(18) -0.011(2)
C4 0.017(2) 0.010(2) 0.013(2) -0.0022(17) -0.0030(18) 0.0059(18)
Cd1 0.0169(3) 0.0150(3) 0.0109(3) 0.000 0.00194(18) 0.000
N1 0.0155(19) 0.014(2) 0.0121(19) 0.0040(15) 0.0006(15) 0.0012(15)
N2 0.0182(19) 0.015(2) 0.0084(18) 0.0009(15) 0.0053(15) -0.0021(16)
O1 0.0285(19) 0.0201(19) 0.0115(17) -0.0024(13) 0.0000(14) -0.0074(15)
O2 0.035(2) 0.0207(19) 0.0191(19) -0.0007(15) 0.0043(15) 0.0001(16)
O3 0.0196(17) 0.0182(18) 0.0212(18) 0.0036(14) 0.0021(14) 0.0008(14)
O4 0.0190(18) 0.0225(19) 0.0242(19) 0.0062(15) 0.0052(14) 0.0007(15)
C5 0.020(2) 0.013(2) 0.0032(19) -0.0018(16) 0.0052(17) 0.0001(18)

_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
C2 C3 1.360(7) . ?
C2 N1 1.398(6) . ?
C2 C4 1.503(6) . ?
C3 N2 1.372(6) . ?
C3 C5 1.522(6) . ?
C6 N2 1.475(6) . ?
C1 N1 1.326(6) . ?
C1 N2 1.328(6) . ?
C7 N1 1.475(6) . ?
C4 O2 1.241(6) . ?
C4 O1 1.261(6) . ?
Cd1 O1 2.248(3) . ?
Cd1 O1 2.248(3) 2_755 ?
Cd1 O3 2.417(3) 3 ?
Cd1 O3 2.417(3) 4_655 ?
Cd1 O4 2.438(3) 3 ?
Cd1 O4 2.438(3) 4_655 ?
Cd1 C5 2.732(4) 3 ?
Cd1 C5 2.732(4) 4_655 ?
O3 C5 1.254(6) . ?
O3 Cd1 2.417(3) 3_445 ?
O4 C5 1.242(6) . ?
O4 Cd1 2.438(3) 3_445 ?
C5 Cd1 2.732(4) 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
C3 C2 N1 105.6(4) . . ?
C3 C2 C4 129.5(4) . . ?
N1 C2 C4 124.8(4) . . ?
C2 C3 N2 107.5(4) . . ?
C2 C3 C5 134.3(4) . . ?
N2 C3 C5 118.2(4) . . ?
N1 C1 N2 108.2(4) . . ?
O2 C4 O1 126.9(4) . . ?
O2 C4 C2 116.4(4) . . ?
O1 C4 C2 116.7(4) . . ?
O1 Cd1 O1 117.04(18) . 2_755 ?
O1 Cd1 O3 94.65(12) . 3 ?
O1 Cd1 O3 109.58(13) 2_755 3 ?
O1 Cd1 O3 109.58(13) . 4_655 ?
O1 Cd1 O3 94.65(12) 2_755 4_655 ?
O3 Cd1 O3 133.04(16) 3 4_655 ?
O1 Cd1 O4 82.13(12) . 3 ?
O1 Cd1 O4 157.57(13) 2_755 3 ?
O3 Cd1 O4 54.28(11) 3 3 ?
O3 Cd1 O4 89.02(11) 4_655 3 ?
O1 Cd1 O4 157.57(13) . 4_655 ?
O1 Cd1 O4 82.13(12) 2_755 4_655 ?
O3 Cd1 O4 89.02(11) 3 4_655 ?
O3 Cd1 O4 54.28(11) 4_655 4_655 ?
O4 Cd1 O4 82.13(17) 3 4_655 ?
O1 Cd1 C5 86.71(13) . 3 ?
O1 Cd1 C5 135.76(13) 2_755 3 ?
O3 Cd1 C5 27.32(13) 3 3 ?
O3 Cd1 C5 112.68(12) 4_655 3 ?
O4 Cd1 C5 27.04(13) 3 3 ?
O4 Cd1 C5 86.51(12) 4_655 3 ?
O1 Cd1 C5 135.76(13) . 4_655 ?
O1 Cd1 C5 86.71(12) 2_755 4_655 ?
O3 Cd1 C5 112.68(12) 3 4_655 ?
O3 Cd1 C5 27.32(13) 4_655 4_655 ?
O4 Cd1 C5 86.51(12) 3 4_655 ?
O4 Cd1 C5 27.04(13) 4_655 4_655 ?
C5 Cd1 C5 101.74(18) 3 4_655 ?
C1 N1 C2 109.3(4) . . ?
C1 N1 C7 121.1(4) . . ?
C2 N1 C7 129.5(4) . . ?
C1 N2 C3 109.4(4) . . ?
C1 N2 C6 124.6(4) . . ?
C3 N2 C6 125.7(4) . . ?
C4 O1 Cd1 108.5(3) . . ?
C5 O3 Cd1 90.5(3) . 3_445 ?
C5 O4 Cd1 89.8(3) . 3_445 ?
O4 C5 O3 125.1(4) . . ?
O4 C5 C3 115.7(4) . . ?
O3 C5 C3 118.9(4) . . ?
O4 C5 Cd1 63.2(2) . 3_445 ?
O3 C5 Cd1 62.2(2) . 3_445 ?
C3 C5 Cd1 168.9(3) . 3_445 ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.168



#===END


