# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10.50 H6 N6 O4.50 S Zn2'
_chemical_formula_weight         451.01

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'

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

_cell_length_a                   13.518(5)
_cell_length_b                   13.518(5)
_cell_length_c                   26.420(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     4828(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    13839
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      24.98

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    2.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5818
_exptl_absorpt_correction_T_max  0.6333
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD Detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13839
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2174
_reflns_number_gt                1751
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The crystals contain severely disordered molecules of the DMF
 crystallization solvent within the interstitial voids, which could not
 be modeled reliably by discrete atoms. Its contribution to the
 diffraction pattern was thus subtracted by the Squeeze procedure,
 using the PLATON software (Spek, 2009).
 C5 atom was disordered and refined with splitting mode.
 C5A:C5B 0.5:0.5 and the ISOR and EADP instruction was applied.
;
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 -0.210 0.487 0.000 1093 352 ' '
2 -0.012 0.001 0.500 1093 352 ' '
_platon_squeeze_details          
;
;


_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)+(0.0603P)²+83.9749P] 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         2174
_refine_ls_number_parameters     113
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1709
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.65982(6) -0.22793(6) 0.30357(3) 0.0308(3) Uani 1 1 d . . .
S1 S 0.6316(3) -0.2679(3) 0.5000 0.0702(10) Uani 1 2 d S . .
N2 N 0.3713(4) -0.2109(4) 0.2471(2) 0.0319(12) Uani 1 1 d . . .
N1 N 0.3585(4) -0.2761(4) 0.2861(2) 0.0318(13) Uani 1 1 d . . .
N3 N 0.5154(4) -0.2350(4) 0.2852(2) 0.0353(13) Uani 1 1 d . . .
O1 O 0.6148(7) -0.2932(7) 0.3884(2) 0.088(2) Uani 1 1 d . . .
O2 O 0.7065(6) -0.1692(5) 0.3675(2) 0.0713(19) Uani 1 1 d . . .
C2 C 0.4669(5) -0.1860(6) 0.2487(3) 0.0398(17) Uani 1 1 d . . .
H2 H 0.4962 -0.1402 0.2271 0.048 Uiso 1 1 calc R . .
C1 C 0.4428(5) -0.2917(6) 0.3074(3) 0.0379(17) Uani 1 1 d . . .
H1 H 0.4532 -0.3353 0.3341 0.046 Uiso 1 1 calc R . .
C3 C 0.6682(8) -0.2228(8) 0.3995(3) 0.064(3) Uani 1 1 d . . .
C4 C 0.6917(9) -0.2000(8) 0.4542(3) 0.071(3) Uani 1 1 d . . .
C5A C 0.7727(17) -0.1496(17) 0.4718(9) 0.062(4) Uani 0.50 1 d PU . 1
H5AA H 0.8205 -0.1198 0.4516 0.074 Uiso 0.50 1 calc PR . 1
C5B C 0.7355(17) -0.1244(18) 0.4714(9) 0.062(4) Uani 0.50 1 d PU . 2
H5BA H 0.7640 -0.0753 0.4514 0.074 Uiso 0.50 1 calc PR . 2
O01 O 0.5000 -0.5000 0.3783(7) 0.128(6) Uani 1 4 d S . .
C01 C 0.5000 -0.5000 0.4266(12) 0.128(6) Uani 1 4 d S . .

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
Zn1 0.0290(5) 0.0364(5) 0.0271(4) 0.0037(3) 0.0032(3) 0.0032(3)
S1 0.085(3) 0.092(3) 0.0339(15) 0.000 0.000 0.011(2)
N2 0.033(3) 0.031(3) 0.032(3) 0.006(2) -0.002(2) 0.000(2)
N1 0.040(3) 0.027(3) 0.029(3) 0.006(2) 0.000(2) -0.003(2)
N3 0.030(3) 0.041(3) 0.035(3) 0.014(3) -0.002(2) 0.000(3)
O1 0.109(6) 0.120(7) 0.036(3) -0.017(4) -0.004(4) 0.018(5)
O2 0.102(5) 0.087(5) 0.025(3) -0.001(3) 0.003(3) 0.000(4)
C2 0.035(4) 0.048(4) 0.037(4) 0.012(3) -0.001(3) -0.003(3)
C1 0.027(3) 0.054(5) 0.033(4) 0.016(3) -0.005(3) -0.001(3)
C3 0.079(7) 0.076(7) 0.038(5) -0.002(5) -0.002(5) 0.026(6)
C4 0.099(8) 0.087(7) 0.028(4) -0.001(4) 0.010(5) 0.016(6)
C5A 0.069(8) 0.067(7) 0.049(5) 0.004(5) 0.004(6) 0.006(6)
C5B 0.069(8) 0.067(7) 0.049(5) 0.004(5) 0.004(6) 0.006(6)
O01 0.150(9) 0.150(9) 0.084(10) 0.000 0.000 0.000
C01 0.150(9) 0.150(9) 0.084(10) 0.000 0.000 0.000

_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 O2 1.971(6) . ?
Zn1 N3 2.014(6) . ?
Zn1 N2 2.017(5) 16_545 ?
Zn1 N1 2.020(6) 4_655 ?
Zn1 O1 2.485(8) . ?
Zn1 C3 2.539(9) . ?
S1 C4 1.723(11) 10_556 ?
S1 C4 1.723(11) . ?
N2 C2 1.335(9) . ?
N2 N1 1.368(7) . ?
N2 Zn1 2.017(5) 15 ?
N1 C1 1.288(9) . ?
N1 Zn1 2.020(6) 3_545 ?
N3 C2 1.342(9) . ?
N3 C1 1.377(9) . ?
O1 C3 1.229(13) . ?
O2 C3 1.228(12) . ?
C3 C4 1.509(13) . ?
C4 C5B 1.27(3) . ?
C4 C5A 1.37(3) . ?
C5A C5A 1.49(5) 10_556 ?
C5B C5B 1.51(5) 10_556 ?
O01 C01 1.28(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
O2 Zn1 N3 122.4(3) . . ?
O2 Zn1 N2 101.0(3) . 16_545 ?
N3 Zn1 N2 101.7(2) . 16_545 ?
O2 Zn1 N1 114.3(3) . 4_655 ?
N3 Zn1 N1 108.6(2) . 4_655 ?
N2 Zn1 N1 106.5(2) 16_545 4_655 ?
O2 Zn1 O1 56.5(3) . . ?
N3 Zn1 O1 87.9(3) . . ?
N2 Zn1 O1 156.7(3) 16_545 . ?
N1 Zn1 O1 90.1(2) 4_655 . ?
O2 Zn1 C3 28.2(3) . . ?
N3 Zn1 C3 106.6(3) . . ?
N2 Zn1 C3 129.0(3) 16_545 . ?
N1 Zn1 C3 103.5(3) 4_655 . ?
O1 Zn1 C3 28.3(3) . . ?
C4 S1 C4 89.3(8) 10_556 . ?
C2 N2 N1 105.1(5) . . ?
C2 N2 Zn1 125.3(5) . 15 ?
N1 N2 Zn1 129.5(4) . 15 ?
C1 N1 N2 108.9(5) . . ?
C1 N1 Zn1 127.1(5) . 3_545 ?
N2 N1 Zn1 124.0(4) . 3_545 ?
C2 N3 C1 103.5(6) . . ?
C2 N3 Zn1 128.6(5) . . ?
C1 N3 Zn1 127.9(4) . . ?
C3 O1 Zn1 78.3(6) . . ?
C3 O2 Zn1 102.6(7) . . ?
N2 C2 N3 111.8(6) . . ?
N1 C1 N3 110.7(6) . . ?
O2 C3 O1 122.7(9) . . ?
O2 C3 C4 116.7(11) . . ?
O1 C3 C4 120.6(10) . . ?
O2 C3 Zn1 49.3(5) . . ?
O1 C3 Zn1 73.4(6) . . ?
C4 C3 Zn1 165.8(9) . . ?
C5B C4 C5A 26.2(12) . . ?
C5B C4 C3 127.4(14) . . ?
C5A C4 C3 126.5(14) . . ?
C5B C4 S1 113.5(13) . . ?
C5A C4 S1 113.7(12) . . ?
C3 C4 S1 117.7(9) . . ?
C4 C5A C5A 109.9(11) . 10_556 ?
C4 C5B C5B 111.0(12) . 10_556 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.124

_database_code_depnum_ccdc_archive 'CCDC 1025511'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 N6 O4 Zn2'
_chemical_formula_weight         507.08

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_H-M_alt        'P 4/n c c'
_space_group_name_Hall           '-P 4a 2ac'

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

_cell_length_a                   13.642(3)
_cell_length_b                   13.642(3)
_cell_length_c                   35.545(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6615(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    31110
_cell_measurement_theta_min      1.88
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_T_max  0.7096
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD Detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31110
_diffrn_reflns_av_R_equivalents  0.1383
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2921
_reflns_number_gt                1852
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The crystals contain severely disordered molecules of the DMF
 crystallization solvent within the interstitial voids, which could not
 be modeled reliably by discrete atoms. Its contribution to the
 diffraction pattern was thus subtracted by the Squeeze procedure,
 using the PLATON software (Spek, 2009).
 C3-C8 atoms were disordered and refined with splitting mode with 0.5:0.5.
 The ISOR and EADP instruction was applied.
;
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 0.001 0.172 0.250 1449 434 ' '
2 0.001 0.324 0.750 1445 433 ' '
_platon_squeeze_details          
;
;

_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)+(0.0891P)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         2921
_refine_ls_number_parameters     141
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1689
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.020
_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 0.4583(4) 0.3051(4) 0.46019(16) 0.0395(13) Uani 1 1 d U . .
H1A H 0.4163 0.2945 0.4400 0.047 Uiso 1 1 calc R . .
C2 C 0.5609(4) 0.2833(4) 0.50277(16) 0.0400(14) Uani 1 1 d . . .
H2A H 0.6058 0.2536 0.5188 0.048 Uiso 1 1 calc R . .
C3A C 0.4924(11) 0.0572(11) 0.3481(4) 0.099(5) Uani 0.50 1 d PGDU A 1
C4A C 0.5644(11) -0.0053(11) 0.3346(4) 0.112(5) Uani 0.50 1 d PGDU A 1
H4A H 0.6063 -0.0369 0.3512 0.134 Uiso 0.50 1 calc PR A 1
C5A C 0.5738(11) -0.0206(12) 0.2962(4) 0.122(6) Uani 0.50 1 d PGU A 1
H5A H 0.6221 -0.0625 0.2871 0.147 Uiso 0.50 1 calc PR A 1
C6A C 0.5113(13) 0.0265(13) 0.2714(4) 0.120(6) Uani 0.50 1 d PGU A 1
C7A C 0.4393(12) 0.0890(12) 0.2849(4) 0.135(6) Uani 0.50 1 d PGU A 1
H7A H 0.3973 0.1206 0.2682 0.163 Uiso 0.50 1 calc PR A 1
C8A C 0.4299(11) 0.1043(11) 0.3233(4) 0.114(5) Uani 0.50 1 d PGDU A 1
H8A H 0.3816 0.1462 0.3323 0.137 Uiso 0.50 1 calc PR A 1
C9A C 0.4855(12) 0.0975(13) 0.3903(7) 0.084(4) Uani 0.50 1 d PDU A 1
O1A O 0.5539(16) 0.0717(14) 0.4110(7) 0.081(3) Uani 0.50 1 d PDU A 1
O2A O 0.4161(12) 0.1484(18) 0.4006(8) 0.083(3) Uani 0.50 1 d PDU A 1
C3B C 0.5373(11) 0.1009(11) 0.3488(4) 0.099(5) Uani 0.50 1 d PGDU A 2
C4B C 0.6092(11) 0.0370(11) 0.3347(4) 0.112(5) Uani 0.50 1 d PGDU A 2
H4AA H 0.6461 -0.0011 0.3511 0.134 Uiso 0.50 1 calc PR A 2
C5B C 0.6253(11) 0.0306(11) 0.2957(4) 0.122(6) Uani 0.50 1 d PGU A 2
H5AA H 0.6728 -0.0117 0.2864 0.147 Uiso 0.50 1 calc PR A 2
C6B C 0.5695(12) 0.0882(12) 0.2709(4) 0.120(6) Uani 0.50 1 d PGU A 2
C7B C 0.4976(12) 0.1521(12) 0.2850(4) 0.135(6) Uani 0.50 1 d PGU A 2
H7AA H 0.4606 0.1902 0.2686 0.163 Uiso 0.50 1 calc PR A 2
C8B C 0.4815(11) 0.1585(11) 0.3240(4) 0.114(5) Uani 0.50 1 d PGDU A 2
H8AA H 0.4339 0.2008 0.3334 0.137 Uiso 0.50 1 calc PR A 2
C9B C 0.5182(12) 0.0932(12) 0.3907(7) 0.084(4) Uani 0.50 1 d PDU A 2
O1B O 0.5712(16) 0.0414(13) 0.4108(7) 0.081(3) Uani 0.50 1 d PDU A 2
O2B O 0.4499(13) 0.1439(18) 0.4021(8) 0.083(3) Uani 0.50 1 d PDU A 2
N1 N 0.5113(3) 0.2343(3) 0.47607(13) 0.0385(12) Uani 1 1 d . A .
N2 N 0.4714(3) 0.3918(3) 0.47595(13) 0.0375(11) Uani 1 1 d U . .
N3 N 0.5395(3) 0.3779(3) 0.50397(12) 0.0361(11) Uani 1 1 d . . .
Zn1 Zn 0.51884(5) 0.09311(4) 0.461153(17) 0.0351(2) 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 0.032(3) 0.043(3) 0.043(3) 0.000(3) -0.012(3) 0.000(3)
C2 0.044(3) 0.032(3) 0.044(4) 0.000(3) -0.012(3) 0.010(3)
C3A 0.107(8) 0.105(7) 0.085(6) -0.005(6) 0.000(6) -0.004(6)
C4A 0.120(8) 0.122(8) 0.093(6) -0.004(6) 0.000(6) 0.000(6)
C5A 0.133(8) 0.128(8) 0.105(7) 0.000(6) 0.003(6) 0.002(6)
C6A 0.126(8) 0.126(8) 0.108(7) -0.005(6) 0.003(6) 0.003(6)
C7A 0.144(9) 0.147(9) 0.116(7) -0.001(6) -0.003(6) 0.008(6)
C8A 0.124(8) 0.127(8) 0.090(6) -0.004(6) 0.004(6) 0.005(6)
C9A 0.086(7) 0.092(6) 0.074(5) 0.001(5) 0.002(6) 0.008(5)
O1A 0.098(6) 0.094(8) 0.051(3) 0.002(6) 0.006(4) 0.018(6)
O2A 0.086(8) 0.099(4) 0.064(4) -0.009(3) -0.002(7) 0.001(6)
C3B 0.107(8) 0.105(7) 0.085(6) -0.005(6) 0.000(6) -0.004(6)
C4B 0.120(8) 0.122(8) 0.093(6) -0.004(6) 0.000(6) 0.000(6)
C5B 0.133(8) 0.128(8) 0.105(7) 0.000(6) 0.003(6) 0.002(6)
C6B 0.126(8) 0.126(8) 0.108(7) -0.005(6) 0.003(6) 0.003(6)
C7B 0.144(9) 0.147(9) 0.116(7) -0.001(6) -0.003(6) 0.008(6)
C8B 0.124(8) 0.127(8) 0.090(6) -0.004(6) 0.004(6) 0.005(6)
C9B 0.086(7) 0.092(6) 0.074(5) 0.001(5) 0.002(6) 0.008(5)
O1B 0.098(6) 0.094(8) 0.051(3) 0.002(6) 0.006(4) 0.018(6)
O2B 0.086(8) 0.099(4) 0.064(4) -0.009(3) -0.002(7) 0.001(6)
N1 0.038(3) 0.032(3) 0.046(3) -0.003(2) -0.010(2) -0.003(2)
N2 0.039(3) 0.039(2) 0.035(3) -0.001(2) -0.006(2) 0.009(2)
N3 0.035(3) 0.039(3) 0.034(3) -0.001(2) -0.008(2) 0.002(2)
Zn1 0.0379(4) 0.0344(4) 0.0329(4) 0.0024(3) -0.0026(3) -0.0024(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 N2 1.322(7) . ?
C1 N1 1.331(7) . ?
C1 H1A 0.9300 . ?
C2 N3 1.324(7) . ?
C2 N1 1.344(6) . ?
C2 H2A 0.9300 . ?
C3A C8A 1.386(8) . ?
C3A C4A 1.386(8) . ?
C3A C9A 1.60(3) . ?
C4A C5A 1.386(8) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.386(8) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.386(8) . ?
C6A C6A 1.55(3) 7_545 ?
C7A C8A 1.386(8) . ?
C7A H7A 0.9300 . ?
C8A H8A 0.9300 . ?
C9A O2A 1.232(9) . ?
C9A O1A 1.240(9) . ?
C9A Zn1 2.56(2) . ?
O1A Zn1 1.87(3) . ?
C3B C4B 1.405(8) . ?
C3B C8B 1.405(8) . ?
C3B C9B 1.51(3) . ?
C4B C5B 1.406(8) . ?
C4B H4AA 0.9300 . ?
C5B C6B 1.405(8) . ?
C5B H5AA 0.9300 . ?
C6B C7B 1.406(8) . ?
C6B C6B 1.53(3) 7_545 ?
C7B C8B 1.405(8) . ?
C7B H7AA 0.9300 . ?
C8B H8AA 0.9300 . ?
C9B O2B 1.230(9) . ?
C9B O1B 1.239(9) . ?
C9B Zn1 2.51(2) . ?
O1B Zn1 2.05(2) . ?
O2B Zn1 2.40(3) . ?
N1 Zn1 2.000(5) . ?
N2 N3 1.376(6) . ?
N2 Zn1 2.013(4) 3 ?
N3 Zn1 2.014(4) 11_666 ?
Zn1 N2 2.013(4) 4 ?
Zn1 N3 2.014(4) 12_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 113.4(5) . . ?
N2 C1 H1A 123.3 . . ?
N1 C1 H1A 123.3 . . ?
N3 C2 N1 113.4(5) . . ?
N3 C2 H2A 123.3 . . ?
N1 C2 H2A 123.3 . . ?
C8A C3A C4A 120.0 . . ?
C8A C3A C9A 113.7(12) . . ?
C4A C3A C9A 125.3(12) . . ?
C5A C4A C3A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A C7A 120.0 . . ?
C5A C6A C6A 119(2) . 7_545 ?
C7A C6A C6A 121(2) . 7_545 ?
C8A C7A C6A 120.0 . . ?
C8A C7A H7A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C7A C8A C3A 120.0 . . ?
C7A C8A H8A 120.0 . . ?
C3A C8A H8A 120.0 . . ?
O2A C9A O1A 124(2) . . ?
O2A C9A C3A 121(2) . . ?
O1A C9A C3A 114.6(18) . . ?
O2A C9A Zn1 81.7(16) . . ?
O1A C9A Zn1 43.5(13) . . ?
C3A C9A Zn1 154.7(11) . . ?
C9A O1A Zn1 109.3(18) . . ?
C4B C3B C8B 120.0 . . ?
C4B C3B C9B 115.4(12) . . ?
C8B C3B C9B 124.2(12) . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4AA 120.0 . . ?
C5B C4B H4AA 120.0 . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B H5AA 120.0 . . ?
C4B C5B H5AA 120.0 . . ?
C5B C6B C7B 120.0 . . ?
C5B C6B C6B 115(2) . 7_545 ?
C7B C6B C6B 125(2) . 7_545 ?
C8B C7B C6B 120.0 . . ?
C8B C7B H7AA 120.0 . . ?
C6B C7B H7AA 120.0 . . ?
C7B C8B C3B 120.0 . . ?
C7B C8B H8AA 120.0 . . ?
C3B C8B H8AA 120.0 . . ?
O2B C9B O1B 125(2) . . ?
O2B C9B C3B 114.7(19) . . ?
O1B C9B C3B 120.5(19) . . ?
O2B C9B Zn1 70.8(16) . . ?
O1B C9B Zn1 54.5(13) . . ?
C3B C9B Zn1 169.2(10) . . ?
C9B O1B Zn1 96.0(16) . . ?
C9B O2B Zn1 80.3(16) . . ?
C1 N1 C2 102.2(5) . . ?
C1 N1 Zn1 127.9(4) . . ?
C2 N1 Zn1 129.8(4) . . ?
C1 N2 N3 105.9(4) . . ?
C1 N2 Zn1 127.0(4) . 3 ?
N3 N2 Zn1 127.1(3) . 3 ?
C2 N3 N2 105.1(4) . . ?
C2 N3 Zn1 128.5(4) . 11_666 ?
N2 N3 Zn1 126.4(3) . 11_666 ?
O1A Zn1 N1 114.6(6) . . ?
O1A Zn1 N2 113.7(7) . 4 ?
N1 Zn1 N2 107.87(19) . 4 ?
O1A Zn1 N3 110.6(6) . 12_656 ?
N1 Zn1 N3 102.86(18) . 12_656 ?
N2 Zn1 N3 106.43(19) 4 12_656 ?
O1A Zn1 O1B 12.9(9) . . ?
N1 Zn1 O1B 125.5(6) . . ?
N2 Zn1 O1B 112.1(6) 4 . ?
N3 Zn1 O1B 99.7(5) 12_656 . ?
O1A Zn1 O2B 46.5(7) . . ?
N1 Zn1 O2B 86.2(6) . . ?
N2 Zn1 O2B 91.0(5) 4 . ?
N3 Zn1 O2B 156.4(5) 12_656 . ?
O1B Zn1 O2B 58.2(6) . . ?
O1A Zn1 C9B 17.6(8) . . ?
N1 Zn1 C9B 105.3(4) . . ?
N2 Zn1 C9B 105.0(4) 4 . ?
N3 Zn1 C9B 128.2(4) 12_656 . ?
O1B Zn1 C9B 29.4(4) . . ?
O2B Zn1 C9B 28.9(3) . . ?
O1A Zn1 C9A 27.2(6) . . ?
N1 Zn1 C9A 103.3(4) . . ?
N2 Zn1 C9A 96.6(4) 4 . ?
N3 Zn1 C9A 137.6(4) 12_656 . ?
O1B Zn1 C9A 38.0(7) . . ?
O2B Zn1 C9A 20.6(8) . . ?
C9B Zn1 C9A 10.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1025512'
