# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Stuart James'
_publ_contact_author_email       S.JAMES@QUEENS-BELFAST.AC.UK

_publ_section_title              
;
Chemoenzymatic synthesis of chiral 4,4'-bipyridyls and
their metal-organic frameworks
;
loop_
_publ_author_name
'Stuart James'
'David C Apperley'
'Derek R Boyd'
'William Clegg'
'Ross W Harrington'
;
P.N.Horton
;
'Mike Hursthouse'
'Lenuta Sbircea'
'Narain Sharma'

# Attachment 'chiral_MOF.cif'

data_2007src0241
_database_code_depnum_ccdc_archive 'CCDC 695604'

#Dr. S. L. James
#CBiPy + FMA + DMF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 N2 O20 Zn5'
_chemical_formula_weight         963.28

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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.1586(4)
_cell_length_b                   9.7969(4)
_cell_length_c                   9.8730(5)
_cell_angle_alpha                77.598(2)
_cell_angle_beta                 89.947(3)
_cell_angle_gamma                88.060(3)
_cell_volume                     864.68(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    39227
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       'Cut blade'
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_absorpt_coefficient_mu    3.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, 2003)'

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 13842 reflections reduced R(int) from 0.0738 to 0.0497
Ratio of minimum to maximum apparent transmission: 0.639262
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18415
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3950
_reflns_number_gt                3253
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0321P)^2^+8.2011P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0176(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3950
_refine_ls_number_parameters     274
_refine_ls_number_restraints     282
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1346
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.068
_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
O101 O 0.2213(4) 0.4702(4) 0.0343(4) 0.0175(7) Uani 1 1 d U A .
H101 H 0.2714 0.4517 -0.0504 0.021 Uiso 1 1 calc R . .
Zn1 Zn 0.0000 0.5000 0.0000 0.0169(2) Uani 1 2 d SU . .
Zn2 Zn 0.22020(7) 0.28676(6) 0.19110(6) 0.01634(19) Uani 1 1 d DU . .
Zn3 Zn 0.30280(7) 0.62976(6) 0.08942(7) 0.01767(19) Uani 1 1 d U . .
C1 C -0.0152(6) 0.5257(6) -0.3107(6) 0.0188(10) Uani 1 1 d U . .
C2 C 0.0284(6) 0.4731(6) -0.4378(6) 0.0233(11) Uani 1 1 d U . .
H2 H 0.0993 0.3986 -0.4287 0.028 Uiso 1 1 calc R . .
O1 O 0.0330(4) 0.4571(4) -0.1963(4) 0.0234(8) Uani 1 1 d U . .
O2 O -0.0970(5) 0.6336(4) -0.3282(4) 0.0243(9) Uani 1 1 d U . .
C11 C -0.0501(6) 0.1891(5) 0.0152(5) 0.0162(10) Uani 1 1 d U . .
C12 C 0.0225(6) 0.0466(5) 0.0333(6) 0.0194(11) Uani 1 1 d U . .
H12 H 0.1035 0.0232 0.0949 0.023 Uiso 1 1 calc R . .
O11 O 0.0053(4) 0.2758(4) 0.0760(4) 0.0180(7) Uani 1 1 d U A .
O12 O -0.1650(4) 0.2109(4) -0.0585(4) 0.0221(8) Uani 1 1 d U . .
C21 C 0.4062(6) 0.4526(6) 0.3419(6) 0.0238(12) Uani 1 1 d U . .
C22 C 0.4838(6) 0.4443(6) 0.4774(6) 0.0251(12) Uani 1 1 d U . .
H22 H 0.5103 0.3548 0.5323 0.030 Uiso 1 1 calc R . .
O21 O 0.3985(4) 0.3418(4) 0.2992(4) 0.0246(9) Uani 1 1 d U A .
O22 O 0.3545(5) 0.5728(4) 0.2840(4) 0.0279(9) Uani 1 1 d U A .
C31 C 0.4519(6) 0.1882(6) 0.0193(6) 0.0211(11) Uani 1 1 d U . .
C32 C 0.5260(6) 0.0647(6) -0.0181(6) 0.0222(11) Uani 1 1 d U . .
H32 H 0.6139 0.0775 -0.0698 0.027 Uiso 1 1 calc R . .
O31 O 0.3286(4) 0.1708(4) 0.0751(4) 0.0232(8) Uani 1 1 d U A .
O32 O 0.5140(5) 0.3045(4) -0.0029(5) 0.0298(10) Uani 1 1 d U . .
C41 C 0.223(3) 0.062(2) 0.446(3) 0.030(3) Uani 0.54(5) 1 d PDU A 1
H41 H 0.2561 0.1341 0.4884 0.036 Uiso 0.54(5) 1 calc PR A 1
C42 C 0.168(3) -0.179(2) 0.459(3) 0.046(5) Uani 0.54(5) 1 d PDU A 1
H42A H 0.0650 -0.1965 0.4822 0.069 Uiso 0.54(5) 1 calc PR A 1
H42B H 0.2268 -0.2651 0.4936 0.069 Uiso 0.54(5) 1 calc PR A 1
H42C H 0.1777 -0.1515 0.3579 0.069 Uiso 0.54(5) 1 calc PR A 1
C43 C 0.250(5) -0.096(3) 0.669(2) 0.064(6) Uani 0.54(5) 1 d PDU A 1
H43A H 0.3290 -0.1675 0.6908 0.097 Uiso 0.54(5) 1 calc PR A 1
H43B H 0.1625 -0.1299 0.7214 0.097 Uiso 0.54(5) 1 calc PR A 1
H43C H 0.2804 -0.0103 0.6958 0.097 Uiso 0.54(5) 1 calc PR A 1
N41 N 0.218(3) -0.067(2) 0.523(2) 0.035(3) Uani 0.54(5) 1 d PDU A 1
O41 O 0.187(6) 0.092(3) 0.321(3) 0.028(4) Uani 0.54(5) 1 d PDU A 1
C46 C 0.259(4) 0.069(3) 0.448(3) 0.031(4) Uani 0.46(5) 1 d PDU A 2
H46 H 0.3101 0.1416 0.4749 0.037 Uiso 0.46(5) 1 calc PR A 2
C47 C 0.168(4) -0.166(3) 0.508(4) 0.055(6) Uani 0.46(5) 1 d PDU A 2
H47A H 0.1186 -0.1343 0.4183 0.083 Uiso 0.46(5) 1 calc PR A 2
H47B H 0.0959 -0.1962 0.5803 0.083 Uiso 0.46(5) 1 calc PR A 2
H47C H 0.2363 -0.2442 0.5034 0.083 Uiso 0.46(5) 1 calc PR A 2
C48 C 0.316(4) -0.072(3) 0.676(2) 0.056(6) Uani 0.46(5) 1 d PDU A 2
H48A H 0.3768 0.0080 0.6811 0.084 Uiso 0.46(5) 1 calc PR A 2
H48B H 0.3776 -0.1576 0.6933 0.084 Uiso 0.46(5) 1 calc PR A 2
H48C H 0.2400 -0.0796 0.7470 0.084 Uiso 0.46(5) 1 calc PR A 2
N46 N 0.250(4) -0.050(3) 0.541(2) 0.039(4) Uani 0.46(5) 1 d PDU A 2
O46 O 0.205(6) 0.093(3) 0.329(3) 0.026(3) Uani 0.46(5) 1 d PDU A 2

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
O101 0.0228(18) 0.0141(17) 0.0158(18) -0.0038(14) -0.0010(14) 0.0015(14)
Zn1 0.0217(4) 0.0123(4) 0.0164(4) -0.0028(3) -0.0060(3) 0.0017(3)
Zn2 0.0225(3) 0.0113(3) 0.0145(3) -0.0018(2) -0.0024(2) 0.0023(2)
Zn3 0.0198(3) 0.0112(3) 0.0212(3) -0.0016(2) -0.0043(2) 0.0003(2)
C1 0.020(3) 0.018(2) 0.019(2) -0.004(2) -0.001(2) -0.003(2)
C2 0.026(3) 0.024(3) 0.020(3) -0.005(2) 0.003(2) 0.001(2)
O1 0.030(2) 0.022(2) 0.0176(19) -0.0047(15) -0.0043(16) 0.0040(16)
O2 0.034(2) 0.022(2) 0.0170(19) -0.0042(16) -0.0004(16) 0.0048(16)
C11 0.020(2) 0.012(2) 0.018(3) -0.0042(19) -0.0021(19) 0.0005(19)
C12 0.018(2) 0.011(2) 0.027(3) 0.001(2) -0.004(2) 0.0011(19)
O11 0.0227(18) 0.0113(16) 0.0205(19) -0.0047(14) -0.0036(14) 0.0007(14)
O12 0.0206(19) 0.0138(18) 0.033(2) -0.0071(16) -0.0087(16) 0.0025(14)
C21 0.028(3) 0.022(3) 0.022(3) -0.005(2) -0.008(2) 0.001(2)
C22 0.029(3) 0.024(3) 0.022(3) -0.005(2) -0.010(2) 0.002(2)
O21 0.031(2) 0.0175(19) 0.025(2) -0.0058(16) -0.0112(16) 0.0021(16)
O22 0.039(2) 0.020(2) 0.024(2) -0.0051(16) -0.0120(18) 0.0025(17)
C31 0.018(2) 0.016(2) 0.029(3) -0.006(2) 0.000(2) -0.002(2)
C32 0.022(3) 0.017(3) 0.028(3) -0.006(2) 0.002(2) 0.001(2)
O31 0.0230(19) 0.0161(18) 0.033(2) -0.0103(16) 0.0044(16) -0.0024(15)
O32 0.029(2) 0.0146(19) 0.047(3) -0.0095(18) 0.0087(19) -0.0016(16)
C41 0.041(9) 0.023(4) 0.025(4) 0.001(4) -0.003(6) -0.003(5)
C42 0.056(9) 0.021(6) 0.058(12) 0.000(8) 0.003(11) -0.006(6)
C43 0.096(15) 0.048(9) 0.039(7) 0.015(6) -0.011(10) -0.009(11)
N41 0.049(9) 0.026(5) 0.026(5) 0.003(4) 0.000(5) -0.003(5)
O41 0.038(10) 0.022(4) 0.022(4) 0.002(4) -0.005(4) -0.001(4)
C46 0.042(10) 0.022(5) 0.024(5) 0.007(4) 0.003(6) -0.003(5)
C47 0.058(10) 0.026(9) 0.068(14) 0.023(10) -0.002(12) -0.011(8)
C48 0.062(15) 0.054(12) 0.038(8) 0.021(8) -0.004(9) 0.003(10)
N46 0.048(10) 0.032(6) 0.030(6) 0.010(5) 0.006(6) -0.002(6)
O46 0.035(10) 0.017(5) 0.024(5) -0.001(4) -0.002(5) 0.003(4)

_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
O101 Zn3 1.934(4) . ?
O101 Zn1 2.056(4) . ?
O101 Zn2 2.106(4) . ?
O101 H101 1.000 . ?
Zn1 O101 2.056(4) 2_565 ?
Zn1 O1 2.089(4) . ?
Zn1 O1 2.089(4) 2_565 ?
Zn1 O11 2.162(4) . ?
Zn1 O11 2.162(4) 2_565 ?
Zn2 O31 2.017(4) . ?
Zn2 O2 2.026(4) 2_565 ?
Zn2 O41 2.090(10) . ?
Zn2 O46 2.092(11) . ?
Zn2 O21 2.099(4) . ?
Zn2 O11 2.291(4) . ?
Zn3 O22 1.936(4) . ?
Zn3 O12 1.945(4) 2_565 ?
Zn3 O32 1.948(4) 2_665 ?
C1 O1 1.255(7) . ?
C1 O2 1.256(7) . ?
C1 C2 1.504(8) . ?
C2 C2 1.327(12) 2_564 ?
C2 H2 0.950 . ?
O2 Zn2 2.026(4) 2_565 ?
C11 O11 1.260(6) . ?
C11 O12 1.266(6) . ?
C11 C12 1.501(7) . ?
C12 C12 1.311(11) 2 ?
C12 H12 0.950 . ?
O12 Zn3 1.945(4) 2_565 ?
C21 O21 1.250(7) . ?
C21 O22 1.269(7) . ?
C21 C22 1.501(8) . ?
C22 C22 1.308(12) 2_666 ?
C22 H22 0.950 . ?
C31 O31 1.257(7) . ?
C31 O32 1.267(7) . ?
C31 C32 1.482(8) . ?
C32 C32 1.345(11) 2_655 ?
C32 H32 0.950 . ?
O32 Zn3 1.948(4) 2_665 ?
C41 O41 1.249(13) . ?
C41 N41 1.329(13) . ?
C41 H41 0.950 . ?
C42 N41 1.471(17) . ?
C42 H42A 0.980 . ?
C42 H42B 0.980 . ?
C42 H42C 0.980 . ?
C43 N41 1.439(16) . ?
C43 H43A 0.980 . ?
C43 H43B 0.980 . ?
C43 H43C 0.980 . ?
C46 O46 1.249(14) . ?
C46 N46 1.321(13) . ?
C46 H46 0.950 . ?
C47 N46 1.469(18) . ?
C47 H47A 0.980 . ?
C47 H47B 0.980 . ?
C47 H47C 0.980 . ?
C48 N46 1.445(17) . ?
C48 H48A 0.980 . ?
C48 H48B 0.980 . ?
C48 H48C 0.980 . ?

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
Zn3 O101 Zn1 110.95(17) . . ?
Zn3 O101 Zn2 114.81(18) . . ?
Zn1 O101 Zn2 99.04(16) . . ?
Zn3 O101 H101 110.5 . . ?
Zn1 O101 H101 110.5 . . ?
Zn2 O101 H101 110.5 . . ?
O101 Zn1 O101 180.0 . 2_565 ?
O101 Zn1 O1 88.20(15) . . ?
O101 Zn1 O1 91.80(15) 2_565 . ?
O101 Zn1 O1 91.80(15) . 2_565 ?
O101 Zn1 O1 88.20(15) 2_565 2_565 ?
O1 Zn1 O1 180.0 . 2_565 ?
O101 Zn1 O11 81.77(14) . . ?
O101 Zn1 O11 98.23(14) 2_565 . ?
O1 Zn1 O11 86.11(15) . . ?
O1 Zn1 O11 93.89(15) 2_565 . ?
O101 Zn1 O11 98.23(14) . 2_565 ?
O101 Zn1 O11 81.77(14) 2_565 2_565 ?
O1 Zn1 O11 93.89(15) . 2_565 ?
O1 Zn1 O11 86.11(15) 2_565 2_565 ?
O11 Zn1 O11 180.00(6) . 2_565 ?
O31 Zn2 O2 168.66(16) . 2_565 ?
O31 Zn2 O41 83.2(15) . . ?
O2 Zn2 O41 85.7(16) 2_565 . ?
O31 Zn2 O46 82.6(16) . . ?
O2 Zn2 O46 86.5(17) 2_565 . ?
O41 Zn2 O46 5(2) . . ?
O31 Zn2 O21 98.86(16) . . ?
O2 Zn2 O21 84.86(17) 2_565 . ?
O41 Zn2 O21 97.2(9) . . ?
O46 Zn2 O21 92.3(10) . . ?
O31 Zn2 O101 93.56(16) . . ?
O2 Zn2 O101 96.85(15) 2_565 . ?
O41 Zn2 O101 168.4(8) . . ?
O46 Zn2 O101 172.8(9) . . ?
O21 Zn2 O101 94.37(15) . . ?
O31 Zn2 O11 91.90(15) . . ?
O2 Zn2 O11 85.95(15) 2_565 . ?
O41 Zn2 O11 91.2(10) . . ?
O46 Zn2 O11 96.2(11) . . ?
O21 Zn2 O11 167.06(14) . . ?
O101 Zn2 O11 77.70(13) . . ?
O101 Zn3 O22 107.38(16) . . ?
O101 Zn3 O12 111.56(15) . 2_565 ?
O22 Zn3 O12 110.65(18) . 2_565 ?
O101 Zn3 O32 116.61(17) . 2_665 ?
O22 Zn3 O32 103.1(2) . 2_665 ?
O12 Zn3 O32 107.16(17) 2_565 2_665 ?
O1 C1 O2 125.8(5) . . ?
O1 C1 C2 116.9(5) . . ?
O2 C1 C2 117.3(5) . . ?
C2 C2 C1 122.5(7) 2_564 . ?
C2 C2 H2 118.7 2_564 . ?
C1 C2 H2 118.7 . . ?
C1 O1 Zn1 127.8(4) . . ?
C1 O2 Zn2 130.6(4) . 2_565 ?
O11 C11 O12 125.3(5) . . ?
O11 C11 C12 118.2(5) . . ?
O12 C11 C12 116.5(4) . . ?
C12 C12 C11 122.0(6) 2 . ?
C12 C12 H12 119.0 2 . ?
C11 C12 H12 119.0 . . ?
C11 O11 Zn1 125.3(3) . . ?
C11 O11 Zn2 135.3(3) . . ?
Zn1 O11 Zn2 90.56(13) . . ?
C11 O12 Zn3 129.4(3) . 2_565 ?
O21 C21 O22 127.3(5) . . ?
O21 C21 C22 117.1(5) . . ?
O22 C21 C22 115.5(5) . . ?
C22 C22 C21 122.4(7) 2_666 . ?
C22 C22 H22 118.8 2_666 . ?
C21 C22 H22 118.8 . . ?
C21 O21 Zn2 125.1(4) . . ?
C21 O22 Zn3 124.7(4) . . ?
O31 C31 O32 122.7(5) . . ?
O31 C31 C32 117.2(5) . . ?
O32 C31 C32 120.1(5) . . ?
C32 C32 C31 122.7(7) 2_655 . ?
C32 C32 H32 118.6 2_655 . ?
C31 C32 H32 118.6 . . ?
C31 O31 Zn2 129.5(4) . . ?
C31 O32 Zn3 133.9(4) . 2_665 ?
O41 C41 N41 122.7(15) . . ?
O41 C41 H41 118.6 . . ?
N41 C41 H41 118.6 . . ?
C41 N41 C43 121.1(15) . . ?
C41 N41 C42 118.9(13) . . ?
C43 N41 C42 119.8(13) . . ?
C41 O41 Zn2 123.6(17) . . ?
O46 C46 N46 125.3(17) . . ?
O46 C46 H46 117.4 . . ?
N46 C46 H46 117.4 . . ?
N46 C47 H47A 109.5 . . ?
N46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N46 C48 H48A 109.5 . . ?
N46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 N46 C48 122.2(16) . . ?
C46 N46 C47 120.3(15) . . ?
C48 N46 C47 117.5(15) . . ?
C46 O46 Zn2 122.7(18) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.164

#===END

data_2007src0262sq
_database_code_depnum_ccdc_archive 'CCDC 695605'

#Dr. S. L. James

#There was some highly disordered solvent in the unit
#cell that was removed from the calculations using the
#SQUEEZE program resulting in a calculated void space of
#443.1 A3 per unit cell.

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H22 N2 O10 Zn2'
_chemical_formula_weight         629.18

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           triclinic
_symmetry_space_group_name_H-M   'P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   8.7651(3)
_cell_length_b                   8.7941(4)
_cell_length_c                   13.6911(6)
_cell_angle_alpha                73.567(2)
_cell_angle_beta                 73.048(2)
_cell_angle_gamma                81.472(2)
_cell_volume                     965.74(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4334
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       'Cut block'
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             320
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 16282 reflections reduced R(int) from 0.1137 to 0.0515
Ratio of minimum to maximum apparent transmission: 0.831825
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16843
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8315
_reflns_number_gt                7371
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0506P)^2^+1.1183P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(17)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         8315
_refine_ls_number_parameters     345
_refine_ls_number_restraints     322
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1222
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.004
_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 0.49606(4) 0.84875(4) 0.85522(3) 0.01658(16) Uani 1 1 d U . .
Zn2 Zn 0.62406(4) 0.89932(4) 0.62001(3) 0.01594(16) Uani 1 1 d U . .
C1 C 0.7386(5) 0.9809(6) 0.3807(3) 0.0224(9) Uani 1 1 d U . .
C2 C 0.8482(6) 0.9838(6) 0.2818(4) 0.0265(9) Uani 1 1 d U . .
C3 C 0.9916(8) 0.8882(9) 0.2832(5) 0.0289(13) Uani 1 1 d U . .
C4 C 1.0187(7) 0.8046(8) 0.3779(4) 0.0471(14) Uani 1 1 d U . .
H4 H 1.1150 0.7394 0.3798 0.057 Uiso 1 1 calc R . .
C5 C 0.9066(7) 0.8149(7) 0.4702(4) 0.0418(13) Uani 1 1 d U . .
H5 H 0.9277 0.7568 0.5354 0.050 Uiso 1 1 calc R . .
C6 C 1.3508(6) 0.9635(7) 0.0480(4) 0.0375(12) Uani 1 1 d U . .
H6 H 1.4319 1.0365 0.0175 0.045 Uiso 1 1 calc R . .
C7 C 1.2345(6) 0.9828(7) 0.1383(4) 0.0368(12) Uani 1 1 d U . .
H7 H 1.2349 1.0680 0.1681 0.044 Uiso 1 1 calc R . .
C8 C 1.1175(8) 0.8742(9) 0.1839(5) 0.0302(14) Uani 1 1 d U . .
C9 C 1.1192(6) 0.7559(7) 0.1366(4) 0.0371(12) Uani 1 1 d U . .
H9 H 1.0382 0.6827 0.1648 0.044 Uiso 1 1 calc R . .
C10 C 1.2391(6) 0.7442(6) 0.0480(4) 0.0308(10) Uani 1 1 d U . .
H10 H 1.2416 0.6593 0.0172 0.037 Uiso 1 1 calc R . .
C11 C 0.8048(7) 1.0705(8) 0.1801(4) 0.0445(13) Uani 1 1 d U . .
H11 H 0.8998 1.1233 0.1279 0.053 Uiso 1 1 calc R . .
C12 C 0.6648(8) 1.1923(9) 0.1940(4) 0.0543(15) Uani 1 1 d U . .
H12 H 0.6997 1.2830 0.2108 0.065 Uiso 1 1 calc R . .
C13 C 0.5266(8) 1.1253(9) 0.2827(5) 0.0582(17) Uani 1 1 d U . .
H13A H 0.4954 1.0292 0.2713 0.070 Uiso 1 1 calc R . .
H13B H 0.4335 1.2045 0.2864 0.070 Uiso 1 1 calc R . .
C14 C 0.5791(7) 1.0820(8) 0.3875(4) 0.0470(14) Uani 1 1 d U . .
H14A H 0.5891 1.1813 0.4050 0.056 Uiso 1 1 calc R . .
H14B H 0.4951 1.0231 0.4454 0.056 Uiso 1 1 calc R . .
C15 C 0.8078(10) 0.9812(12) 0.0287(5) 0.079(3) Uani 1 1 d U . .
H15A H 0.7465 1.0773 -0.0004 0.118 Uiso 1 1 calc R . .
H15B H 0.7838 0.8908 0.0084 0.118 Uiso 1 1 calc R . .
H15C H 0.9223 0.9968 0.0009 0.118 Uiso 1 1 calc R . .
C16 C 0.5190(13) 1.3924(13) 0.0924(7) 0.114(4) Uani 1 1 d U . .
H16A H 0.5382 1.4534 0.1370 0.171 Uiso 1 1 calc R . .
H16B H 0.4074 1.3651 0.1170 0.171 Uiso 1 1 calc R . .
H16C H 0.5405 1.4565 0.0191 0.171 Uiso 1 1 calc R . .
N1 N 0.7692(6) 0.9035(7) 0.4715(4) 0.0199(11) Uani 1 1 d U . .
N2 N 1.3544(6) 0.8490(7) 0.0025(4) 0.0217(12) Uani 1 1 d U . .
O1 O 0.7646(5) 0.9498(6) 0.1421(3) 0.0546(11) Uani 1 1 d U . .
O2 O 0.6228(7) 1.2495(7) 0.0983(3) 0.0828(17) Uani 1 1 d U . .
C21 C 0.2853(9) 0.8857(13) 0.7067(7) 0.0469(18) Uani 1 1 d U . .
C22 C 0.1155(8) 0.8819(11) 0.6987(6) 0.0462(18) Uani 1 1 d U . .
H22 H 0.0973 0.9019 0.6309 0.055 Uiso 1 1 calc R . .
C23 C -0.0051(8) 0.8520(11) 0.7824(6) 0.0401(16) Uani 1 1 d U . .
H23 H 0.0140 0.8281 0.8502 0.048 Uiso 1 1 calc R . .
C24 C -0.1685(8) 0.8541(10) 0.7752(6) 0.0307(13) Uani 1 1 d U . .
O21 O 0.3958(6) 0.8945(8) 0.6214(4) 0.0517(15) Uani 1 1 d U . .
O22 O 0.3039(6) 0.8863(8) 0.7928(4) 0.0466(14) Uani 1 1 d U . .
O23 O -0.1910(6) 0.8900(8) 0.6849(4) 0.0417(13) Uani 1 1 d U . .
O24 O -0.2739(6) 0.8196(7) 0.8609(4) 0.0419(13) Uani 1 1 d U . .
C31 C 0.5638(11) 0.5699(10) 0.7664(6) 0.0423(17) Uani 1 1 d U . .
C32 C 0.5506(11) 0.4048(10) 0.7753(7) 0.0495(18) Uani 1 1 d U . .
H32 H 0.5239 0.3355 0.8441 0.059 Uiso 1 1 calc R . .
C33 C 0.5728(11) 0.3444(10) 0.6952(6) 0.0460(17) Uani 1 1 d U . .
H33 H 0.5973 0.4124 0.6259 0.055 Uiso 1 1 calc R . .
C34 C 0.5607(10) 0.1675(9) 0.7093(6) 0.0381(16) Uani 1 1 d U . .
O31 O 0.6283(7) 0.6590(6) 0.6749(5) 0.0495(15) Uani 1 1 d U . .
O32 O 0.5063(7) 0.6190(6) 0.8492(5) 0.0483(14) Uani 1 1 d U . .
O33 O 0.5842(7) 0.1255(6) 0.6255(4) 0.0437(13) Uani 1 1 d U . .
O34 O 0.5292(7) 0.0837(6) 0.7997(4) 0.0411(12) 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
Zn1 0.0162(3) 0.0197(4) 0.0132(3) -0.0057(3) 0.0002(3) -0.0048(3)
Zn2 0.0146(3) 0.0203(4) 0.0125(3) -0.0065(3) 0.0002(3) -0.0033(3)
C1 0.020(2) 0.035(2) 0.0114(18) -0.0076(17) -0.0016(15) -0.0047(17)
C2 0.026(2) 0.036(2) 0.0164(19) -0.0084(18) -0.0027(16) -0.0030(18)
C3 0.028(3) 0.045(3) 0.014(2) -0.014(2) 0.0019(19) -0.007(2)
C4 0.035(3) 0.071(4) 0.024(2) -0.012(2) -0.002(2) 0.020(3)
C5 0.040(3) 0.059(3) 0.017(2) -0.010(2) -0.0048(19) 0.021(2)
C6 0.036(3) 0.043(3) 0.033(3) -0.022(2) 0.014(2) -0.023(2)
C7 0.041(3) 0.043(3) 0.030(2) -0.025(2) 0.010(2) -0.019(2)
C8 0.020(3) 0.041(3) 0.027(3) -0.014(2) 0.005(2) -0.006(2)
C9 0.040(3) 0.037(3) 0.029(2) -0.014(2) 0.012(2) -0.020(2)
C10 0.036(3) 0.031(2) 0.023(2) -0.0105(19) 0.0056(19) -0.012(2)
C11 0.046(3) 0.062(3) 0.020(2) -0.010(2) -0.008(2) 0.010(2)
C12 0.062(3) 0.070(3) 0.019(2) -0.006(2) -0.010(2) 0.023(3)
C13 0.049(3) 0.082(4) 0.028(3) -0.005(3) -0.011(2) 0.027(3)
C14 0.042(3) 0.070(4) 0.018(2) -0.008(2) -0.003(2) 0.013(3)
C15 0.078(5) 0.129(7) 0.042(4) -0.055(4) -0.021(4) 0.030(5)
C16 0.140(8) 0.131(8) 0.045(4) -0.016(5) -0.038(5) 0.089(6)
N1 0.017(2) 0.029(3) 0.014(2) -0.007(2) -0.0037(19) -0.001(2)
N2 0.022(3) 0.028(3) 0.013(2) -0.010(2) 0.005(2) -0.008(2)
O1 0.049(2) 0.090(3) 0.033(2) -0.035(2) -0.0127(18) 0.010(2)
O2 0.097(4) 0.109(4) 0.023(2) -0.010(2) -0.016(2) 0.041(3)
C21 0.019(3) 0.092(5) 0.029(3) -0.018(3) -0.001(2) -0.006(3)
C22 0.021(3) 0.099(5) 0.024(3) -0.019(3) -0.009(2) -0.008(3)
C23 0.014(2) 0.086(4) 0.023(3) -0.021(3) 0.000(2) -0.007(3)
C24 0.013(2) 0.061(4) 0.021(3) -0.012(3) -0.007(2) -0.004(3)
O21 0.016(2) 0.113(4) 0.031(2) -0.026(3) -0.0004(19) -0.017(2)
O22 0.015(2) 0.099(4) 0.031(3) -0.021(3) -0.0086(19) -0.005(2)
O23 0.020(2) 0.087(4) 0.021(2) -0.020(2) -0.0024(18) -0.007(2)
O24 0.019(2) 0.080(3) 0.023(2) -0.012(2) -0.0015(17) -0.002(2)
C31 0.074(4) 0.025(3) 0.023(3) -0.007(2) 0.000(3) -0.011(3)
C32 0.093(4) 0.018(3) 0.028(3) -0.007(2) 0.004(3) -0.015(3)
C33 0.089(4) 0.019(3) 0.019(3) -0.003(2) 0.001(3) -0.007(3)
C34 0.067(4) 0.015(3) 0.025(3) -0.006(2) -0.003(3) 0.002(3)
O31 0.078(3) 0.019(2) 0.034(3) -0.008(2) 0.018(2) -0.010(2)
O32 0.085(4) 0.025(3) 0.034(3) -0.015(2) 0.004(2) -0.020(2)
O33 0.083(3) 0.023(3) 0.022(2) -0.006(2) -0.010(2) 0.000(2)
O34 0.072(3) 0.024(2) 0.024(2) -0.0098(19) 0.001(2) -0.012(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
Zn1 O24 2.015(5) 1_655 ?
Zn1 O34 2.023(5) 1_565 ?
Zn1 O32 2.033(5) . ?
Zn1 N2 2.037(5) 1_456 ?
Zn1 O22 2.047(5) . ?
Zn1 Zn2 3.0096(5) . ?
Zn2 O33 1.987(5) 1_565 ?
Zn2 O21 2.002(5) . ?
Zn2 O31 2.031(5) . ?
Zn2 O23 2.045(5) 1_655 ?
Zn2 N1 2.053(5) . ?
C1 N1 1.321(7) . ?
C1 C2 1.409(6) . ?
C1 C14 1.535(7) . ?
C2 C3 1.406(9) . ?
C2 C11 1.513(7) . ?
C3 C4 1.366(9) . ?
C3 C8 1.504(5) . ?
C4 C5 1.374(7) . ?
C4 H4 0.950 . ?
C5 N1 1.332(7) . ?
C5 H5 0.950 . ?
C6 N2 1.317(7) . ?
C6 C7 1.388(6) . ?
C6 H6 0.950 . ?
C7 C8 1.390(9) . ?
C7 H7 0.950 . ?
C8 C9 1.369(9) . ?
C9 C10 1.372(7) . ?
C9 H9 0.950 . ?
C10 N2 1.358(7) . ?
C10 H10 0.950 . ?
C11 O1 1.432(8) . ?
C11 C12 1.510(8) . ?
C11 H11 1.000 . ?
C12 O2 1.399(7) . ?
C12 C13 1.496(9) . ?
C12 H12 1.000 . ?
C13 C14 1.562(8) . ?
C13 H13A 0.990 . ?
C13 H13B 0.990 . ?
C14 H14A 0.990 . ?
C14 H14B 0.990 . ?
C15 O1 1.441(7) . ?
C15 H15A 0.980 . ?
C15 H15B 0.980 . ?
C15 H15C 0.980 . ?
C16 O2 1.436(9) . ?
C16 H16A 0.980 . ?
C16 H16B 0.980 . ?
C16 H16C 0.980 . ?
N2 Zn1 2.037(5) 1_654 ?
C21 O22 1.238(10) . ?
C21 O21 1.272(9) . ?
C21 C22 1.529(10) . ?
C22 C23 1.306(6) . ?
C22 H22 0.950 . ?
C23 C24 1.461(9) . ?
C23 H23 0.950 . ?
C24 O23 1.253(9) . ?
C24 O24 1.253(9) . ?
O23 Zn2 2.045(5) 1_455 ?
O24 Zn1 2.015(5) 1_455 ?
C31 O32 1.267(9) . ?
C31 O31 1.291(9) . ?
C31 C32 1.441(10) . ?
C32 C33 1.304(6) . ?
C32 H32 0.950 . ?
C33 C34 1.528(10) . ?
C33 H33 0.950 . ?
C34 O34 1.223(9) . ?
C34 O33 1.255(9) . ?
O33 Zn2 1.987(5) 1_545 ?
O34 Zn1 2.023(5) 1_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
O24 Zn1 O34 86.3(2) 1_655 1_565 ?
O24 Zn1 O32 90.0(3) 1_655 . ?
O34 Zn1 O32 157.00(19) 1_565 . ?
O24 Zn1 N2 108.3(2) 1_655 1_456 ?
O34 Zn1 N2 99.0(2) 1_565 1_456 ?
O32 Zn1 N2 103.7(2) . 1_456 ?
O24 Zn1 O22 159.08(19) 1_655 . ?
O34 Zn1 O22 89.0(3) 1_565 . ?
O32 Zn1 O22 86.4(3) . . ?
N2 Zn1 O22 92.6(2) 1_456 . ?
O24 Zn1 Zn2 86.55(15) 1_655 . ?
O34 Zn1 Zn2 75.17(15) 1_565 . ?
O32 Zn1 Zn2 81.96(16) . . ?
N2 Zn1 Zn2 163.88(16) 1_456 . ?
O22 Zn1 Zn2 72.55(15) . . ?
O33 Zn2 O21 90.1(3) 1_565 . ?
O33 Zn2 O31 157.83(19) 1_565 . ?
O21 Zn2 O31 87.2(3) . . ?
O33 Zn2 O23 86.3(3) 1_565 1_655 ?
O21 Zn2 O23 155.59(19) . 1_655 ?
O31 Zn2 O23 87.1(3) . 1_655 ?
O33 Zn2 N1 105.0(2) 1_565 . ?
O21 Zn2 N1 109.7(2) . . ?
O31 Zn2 N1 96.6(2) . . ?
O23 Zn2 N1 94.5(2) 1_655 . ?
O33 Zn2 Zn1 81.44(15) 1_565 . ?
O21 Zn2 Zn1 84.86(16) . . ?
O31 Zn2 Zn1 76.41(16) . . ?
O23 Zn2 Zn1 70.73(14) 1_655 . ?
N1 Zn2 Zn1 163.71(15) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 C14 116.1(4) . . ?
C2 C1 C14 120.2(4) . . ?
C3 C2 C1 116.3(5) . . ?
C3 C2 C11 122.2(5) . . ?
C1 C2 C11 121.2(4) . . ?
C4 C3 C2 119.3(5) . . ?
C4 C3 C8 118.3(5) . . ?
C2 C3 C8 122.5(5) . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 122.3(5) . . ?
N1 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
N2 C6 C7 123.3(5) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C6 C7 C8 118.3(5) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
C9 C8 C7 118.8(6) . . ?
C9 C8 C3 121.1(4) . . ?
C7 C8 C3 120.1(4) . . ?
C8 C9 C10 119.3(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 122.6(5) . . ?
N2 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
O1 C11 C12 109.3(5) . . ?
O1 C11 C2 105.4(5) . . ?
C12 C11 C2 113.7(4) . . ?
O1 C11 H11 109.4 . . ?
C12 C11 H11 109.4 . . ?
C2 C11 H11 109.4 . . ?
O2 C12 C13 111.8(6) . . ?
O2 C12 C11 108.5(5) . . ?
C13 C12 C11 111.7(6) . . ?
O2 C12 H12 108.2 . . ?
C13 C12 H12 108.2 . . ?
C11 C12 H12 108.2 . . ?
C12 C13 C14 108.0(6) . . ?
C12 C13 H13A 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C12 C13 H13B 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C1 C14 C13 112.8(4) . . ?
C1 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C1 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
O1 C15 H15A 109.5 . . ?
O1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C5 118.7(5) . . ?
C1 N1 Zn2 127.0(4) . . ?
C5 N1 Zn2 114.3(4) . . ?
C6 N2 C10 117.6(5) . . ?
C6 N2 Zn1 122.5(4) . 1_654 ?
C10 N2 Zn1 118.8(4) . 1_654 ?
C11 O1 C15 113.9(6) . . ?
C12 O2 C16 114.0(6) . . ?
O22 C21 O21 125.5(8) . . ?
O22 C21 C22 118.5(7) . . ?
O21 C21 C22 116.0(7) . . ?
C23 C22 C21 121.8(5) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C24 122.1(5) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
O23 C24 O24 125.9(6) . . ?
O23 C24 C23 117.7(7) . . ?
O24 C24 C23 116.4(6) . . ?
C21 O21 Zn2 120.5(5) . . ?
C21 O22 Zn1 134.8(5) . . ?
C24 O23 Zn2 137.7(5) . 1_455 ?
C24 O24 Zn1 117.7(5) . 1_455 ?
O32 C31 O31 124.2(7) . . ?
O32 C31 C32 117.3(7) . . ?
O31 C31 C32 118.5(7) . . ?
C33 C32 C31 124.3(6) . . ?
C33 C32 H32 117.8 . . ?
C31 C32 H32 117.8 . . ?
C32 C33 C34 122.0(5) . . ?
C32 C33 H33 119.0 . . ?
C34 C33 H33 119.0 . . ?
O34 C34 O33 127.6(7) . . ?
O34 C34 C33 117.1(6) . . ?
O33 C34 C33 115.4(7) . . ?
C31 O31 Zn2 131.1(5) . . ?
C31 O32 Zn1 124.8(5) . . ?
C34 O33 Zn2 122.6(5) . 1_545 ?
C34 O34 Zn1 130.7(5) . 1_545 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.088

#===END

data_ssg1356
_database_code_depnum_ccdc_archive 'CCDC 695606'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 N2 O10 Zn2, 4 C3 H7 N O'
_chemical_formula_sum            'C34 H46 N6 O14 Zn2'
_chemical_formula_weight         893.51
_chemical_absolute_configuration ad

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'

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

_cell_length_a                   8.7994(6)
_cell_length_b                   53.888(3)
_cell_length_c                   8.8039(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.111(2)
_cell_angle_gamma                90.00
_cell_volume                     4174.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6893
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            31223
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         24.22
_reflns_number_total             14545
_reflns_number_gt                14227
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

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

Group site occupancy factors were refined for all DMF solvent molecules.
Six of them gave values significantly lower than 1, indicating partial
occupancy, but the positions appear to be ordered. The other two gave
values essentially equal to 1 (one below 1 and one above 1, but the
deviations are only about 1sigma, so they are insignificant), indicating
full occupancy and ordered molecules. An occupancy factor >1 is physically
unrealistic, but since the excess is statistically insignificantly different
from zero this is acceptable, and we prefer to leave the refined value in
the result rather than fixing the occupancy at exactly 1 in order to
provide clear evidence from the experimental data of the occupancy of
all four sites.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+4.1691P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.095(19)
_refine_ls_number_reflns         14545
_refine_ls_number_parameters     1018
_refine_ls_number_restraints     1501
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1514
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.013
_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
Zn1 Zn 0.26565(16) 0.253511(15) 0.17697(9) 0.0431(3) Uani 1 1 d . . .
Zn2 Zn 0.22756(17) 0.197880(15) 0.21188(9) 0.0504(3) Uani 1 1 d . . .
Zn3 Zn 0.56839(13) 0.451517(14) 0.33714(9) 0.0323(2) Uani 1 1 d . . .
Zn4 Zn 0.60378(12) 0.505930(14) 0.37088(9) 0.0321(2) Uani 1 1 d . . .
N1 N 0.3142(11) 0.29088(11) 0.1707(7) 0.049(2) Uani 1 1 d DU . .
N2 N 0.5261(9) 0.41544(12) 0.2923(7) 0.0360(16) Uani 1 1 d DU . .
C1 C 0.3085(10) 0.30632(13) 0.0475(8) 0.0327(17) Uani 1 1 d DU . .
C2 C 0.2340(14) 0.29528(15) -0.0845(10) 0.048(2) Uani 1 1 d DU . .
H2A H 0.1270 0.2931 -0.0619 0.058 Uiso 1 1 calc R . .
H2B H 0.2771 0.2790 -0.1020 0.058 Uiso 1 1 calc R . .
C3 C 0.2496(13) 0.31128(14) -0.2368(9) 0.044(2) Uani 1 1 d DU . .
H3A H 0.3484 0.3085 -0.2824 0.053 Uiso 1 1 calc R . .
H3B H 0.1720 0.3064 -0.3091 0.053 Uiso 1 1 calc R . .
C4 C 0.2318(11) 0.33786(14) -0.1978(8) 0.0394(18) Uani 1 1 d DU . .
H4 H 0.1311 0.3403 -0.1529 0.047 Uiso 1 1 calc R . .
C5 C 0.3527(10) 0.34693(15) -0.0841(8) 0.0351(17) Uani 1 1 d DU . .
H5 H 0.3311 0.3642 -0.0561 0.042 Uiso 1 1 calc R . .
C6 C 0.3548(10) 0.33098(12) 0.0583(7) 0.0313(17) Uani 1 1 d DU . .
C7 C 0.4109(11) 0.34006(13) 0.1955(9) 0.0373(18) Uani 1 1 d DU . .
C8 C 0.4198(12) 0.32362(15) 0.3183(9) 0.045(2) Uani 1 1 d DU . .
H8 H 0.4558 0.3291 0.4118 0.054 Uiso 1 1 calc R . .
C9 C 0.3750(14) 0.29929(14) 0.3004(9) 0.047(2) Uani 1 1 d DU . .
H9 H 0.3873 0.2883 0.3811 0.057 Uiso 1 1 calc R . .
C10 C 0.4275(13) 0.40249(15) 0.3805(9) 0.043(2) Uani 1 1 d DU . .
H10 H 0.3850 0.4103 0.4644 0.052 Uiso 1 1 calc R . .
C11 C 0.3880(13) 0.37832(16) 0.3508(9) 0.048(2) Uani 1 1 d DU . .
H11 H 0.3190 0.3701 0.4129 0.057 Uiso 1 1 calc R . .
C12 C 0.4532(11) 0.36604(13) 0.2248(8) 0.0347(16) Uani 1 1 d DU . .
C13 C 0.5536(12) 0.37931(15) 0.1372(10) 0.044(2) Uani 1 1 d DU . .
H13 H 0.6007 0.3718 0.0547 0.053 Uiso 1 1 calc R . .
C14 C 0.5845(13) 0.40376(16) 0.1720(10) 0.044(2) Uani 1 1 d DU . .
H14 H 0.6493 0.4126 0.1083 0.052 Uiso 1 1 calc R . .
O1 O 0.2395(10) 0.35149(11) -0.3354(6) 0.056(2) Uani 1 1 d DU . .
H1 H 0.2299 0.3663 -0.3172 0.084 Uiso 1 1 calc R . .
O2 O 0.5013(9) 0.34543(13) -0.1478(7) 0.0515(17) Uani 1 1 d DU . .
H2 H 0.5050 0.3539 -0.2253 0.077 Uiso 1 1 calc R . .
N3 N 0.2272(11) 0.16084(13) 0.2773(8) 0.059(2) Uani 1 1 d DU . .
N4 N 0.3557(10) 0.04165(11) 0.5672(7) 0.0392(18) Uani 1 1 d DU . .
C15 C 0.1126(12) 0.14494(17) 0.2659(12) 0.059(2) Uani 1 1 d DU . .
C16 C -0.0133(16) 0.1535(3) 0.177(2) 0.100(4) Uani 1 1 d DU . .
H16A H 0.0030 0.1494 0.0708 0.120 Uiso 1 1 calc R . .
H16B H -0.0225 0.1713 0.1856 0.120 Uiso 1 1 calc R . .
C17 C -0.1709(16) 0.1400(2) 0.2378(17) 0.086(3) Uani 1 1 d DU . .
H17A H -0.1929 0.1446 0.3420 0.104 Uiso 1 1 calc R . .
H17B H -0.2571 0.1443 0.1741 0.104 Uiso 1 1 calc R . .
C18 C -0.1315(14) 0.1127(2) 0.2247(16) 0.081(3) Uani 1 1 d DU . .
H18 H -0.0949 0.1078 0.1240 0.097 Uiso 1 1 calc R . .
C19 C -0.0171(14) 0.1064(2) 0.3583(13) 0.076(3) Uani 1 1 d DU . .
H19 H 0.0089 0.0888 0.3528 0.092 Uiso 1 1 calc R . .
C20 C 0.1263(12) 0.12153(17) 0.3273(13) 0.061(2) Uani 1 1 d DU . .
C21 C 0.2560(12) 0.11416(14) 0.3996(9) 0.049(2) Uani 1 1 d DU . .
C22 C 0.3758(17) 0.1305(2) 0.4075(19) 0.091(4) Uani 1 1 d DU . .
H22 H 0.4704 0.1255 0.4440 0.110 Uiso 1 1 calc R . .
C23 C 0.3493(19) 0.1550(2) 0.358(2) 0.102(4) Uani 1 1 d DU . .
H23 H 0.4192 0.1673 0.3822 0.123 Uiso 1 1 calc R . .
C24 C 0.419(2) 0.0504(2) 0.4421(15) 0.087(4) Uani 1 1 d DU . .
H24 H 0.4699 0.0393 0.3795 0.105 Uiso 1 1 calc R . .
C25 C 0.4137(17) 0.0754(2) 0.3979(13) 0.075(3) Uani 1 1 d DU . .
H25 H 0.4862 0.0829 0.3362 0.090 Uiso 1 1 calc R . .
C26 C 0.2830(12) 0.08830(14) 0.4588(9) 0.046(2) Uani 1 1 d DU . .
C27 C 0.2167(12) 0.07943(17) 0.5864(11) 0.051(2) Uani 1 1 d DU . .
H27 H 0.1402 0.0884 0.6346 0.061 Uiso 1 1 calc R . .
C28 C 0.2658(14) 0.05637(17) 0.6452(12) 0.054(3) Uani 1 1 d DU . .
H28 H 0.2338 0.0515 0.7413 0.065 Uiso 1 1 calc R . .
O3 O -0.2672(14) 0.1007(3) 0.2687(18) 0.131(5) Uani 1 1 d DU . .
H3 H -0.2555 0.0856 0.2643 0.197 Uiso 1 1 calc R . .
O4 O -0.0602(16) 0.1122(2) 0.5126(13) 0.133(5) Uani 1 1 d DU . .
H4A H -0.1371 0.1044 0.5348 0.199 Uiso 1 1 calc R . .
O5 O 0.4824(12) 0.24364(12) 0.2070(8) 0.065(2) Uani 1 1 d U . .
O6 O 0.4609(11) 0.20194(13) 0.1930(8) 0.066(2) Uani 1 1 d U . .
O7 O 1.0420(10) 0.25418(12) 0.1570(7) 0.0579(18) Uani 1 1 d U . .
O8 O 1.0227(14) 0.21371(14) 0.2130(11) 0.083(3) Uani 1 1 d U . .
C29 C 0.5390(15) 0.22160(16) 0.1981(11) 0.050(2) Uani 1 1 d U . .
C30 C 0.7013(16) 0.2182(2) 0.2009(11) 0.059(2) Uani 1 1 d U . .
H30 H 0.7403 0.2023 0.2091 0.071 Uiso 1 1 calc R . .
C31 C 0.7977(16) 0.23737(18) 0.1919(11) 0.055(2) Uani 1 1 d U . .
H31 H 0.7578 0.2533 0.1864 0.066 Uiso 1 1 calc R . .
C32 C 0.9635(17) 0.2344(2) 0.1904(12) 0.062(2) Uani 1 1 d U . .
O9 O 0.2759(11) 0.23661(12) -0.0313(7) 0.059(2) Uani 1 1 d U . .
O10 O 0.2208(9) 0.19626(12) -0.0155(6) 0.0478(16) Uani 1 1 d U . .
O11 O 0.2427(10) 0.24973(12) -0.5924(6) 0.056(2) Uani 1 1 d U . .
O12 O 0.2471(14) 0.20947(12) -0.5689(7) 0.079(3) Uani 1 1 d U . .
C33 C 0.2446(13) 0.21603(14) -0.0882(9) 0.038(2) Uani 1 1 d U . .
C34 C 0.2512(13) 0.21383(16) -0.2561(9) 0.043(2) Uani 1 1 d U . .
H34 H 0.2615 0.1981 -0.2980 0.051 Uiso 1 1 calc R . .
C35 C 0.2432(14) 0.23330(16) -0.3508(10) 0.047(2) Uani 1 1 d U . .
H35 H 0.2347 0.2492 -0.3099 0.056 Uiso 1 1 calc R . .
C36 C 0.2473(14) 0.23049(16) -0.5146(10) 0.047(2) Uani 1 1 d U . .
O13 O 0.7968(10) 0.45298(14) 0.3474(11) 0.065(2) Uani 1 1 d U . .
O14 O 0.8195(10) 0.49326(15) 0.3641(10) 0.060(2) Uani 1 1 d U . .
O15 O 1.3519(11) 0.46474(14) 0.3469(11) 0.067(2) Uani 1 1 d U . .
O16 O 1.3738(10) 0.50548(16) 0.3594(11) 0.073(2) Uani 1 1 d U . .
C37 C 0.8666(13) 0.47205(17) 0.3582(10) 0.0393(19) Uani 1 1 d U . .
C38 C 1.0429(13) 0.46949(18) 0.3570(11) 0.046(2) Uani 1 1 d U . .
H38 H 1.0853 0.4537 0.3539 0.056 Uiso 1 1 calc R . .
C39 C 1.1306(13) 0.48811(17) 0.3601(12) 0.049(2) Uani 1 1 d U . .
H39 H 1.0877 0.5038 0.3669 0.058 Uiso 1 1 calc R . .
C40 C 1.2983(13) 0.48607(19) 0.3535(11) 0.048(2) Uani 1 1 d U . .
O17 O 0.5818(12) 0.46478(14) 0.1229(7) 0.061(2) Uani 1 1 d U . .
O18 O 0.6030(11) 0.50538(13) 0.1416(6) 0.062(2) Uani 1 1 d U . .
O19 O 0.5648(10) 0.45112(12) -0.4333(6) 0.060(2) Uani 1 1 d U . .
O20 O 0.5890(12) 0.49270(12) -0.4158(7) 0.065(3) Uani 1 1 d U . .
C41 C 0.5966(12) 0.48574(17) 0.0695(9) 0.038(2) Uani 1 1 d U . .
C42 C 0.5865(12) 0.48791(16) -0.1006(10) 0.041(2) Uani 1 1 d U . .
H42 H 0.5819 0.5037 -0.1435 0.050 Uiso 1 1 calc R . .
C43 C 0.5840(13) 0.46864(15) -0.1905(9) 0.043(2) Uani 1 1 d U . .
H43 H 0.5815 0.4529 -0.1476 0.052 Uiso 1 1 calc R . .
C44 C 0.5849(13) 0.47094(17) -0.3576(10) 0.044(2) Uani 1 1 d U . .
O21 O 0.6050(12) 0.39132(16) 0.7675(9) 0.078(3) Uani 1.013(14) 1 d PDU . .
N5 N 0.7950(12) 0.38402(17) 0.5948(12) 0.071(3) Uani 1.013(14) 1 d PDU . .
C45 C 0.6918(12) 0.3985(2) 0.6656(11) 0.057(3) Uani 1.013(14) 1 d PDU . .
H45 H 0.6853 0.4150 0.6358 0.069 Uiso 1.013(14) 1 calc PR . .
C46 C 0.800(2) 0.3576(2) 0.623(2) 0.117(6) Uani 1.013(14) 1 d PDU . .
H46A H 0.8808 0.3504 0.5641 0.176 Uiso 1.013(14) 1 calc PR . .
H46B H 0.7052 0.3503 0.5935 0.176 Uiso 1.013(14) 1 calc PR . .
H46C H 0.8182 0.3546 0.7286 0.176 Uiso 1.013(14) 1 calc PR . .
C47 C 0.8848(16) 0.3935(3) 0.4712(13) 0.073(3) Uani 1.013(14) 1 d PDU . .
H47A H 0.9516 0.3808 0.4349 0.109 Uiso 1.013(14) 1 calc PR . .
H47B H 0.9437 0.4074 0.5060 0.109 Uiso 1.013(14) 1 calc PR . .
H47C H 0.8188 0.3988 0.3903 0.109 Uiso 1.013(14) 1 calc PR . .
O22 O -0.008(2) 0.3598(3) 0.1115(14) 0.150(7) Uani 0.988(16) 1 d PDU . .
N6 N -0.0602(16) 0.3241(2) 0.2335(15) 0.104(4) Uani 0.988(16) 1 d PDU . .
C48 C 0.019(2) 0.3460(3) 0.215(2) 0.115(5) Uani 0.988(16) 1 d PDU . .
H48 H 0.0953 0.3501 0.2845 0.138 Uiso 0.988(16) 1 calc PR . .
C49 C -0.166(2) 0.3152(4) 0.120(2) 0.125(6) Uani 0.988(16) 1 d PDU . .
H49A H -0.2090 0.2997 0.1537 0.187 Uiso 0.988(16) 1 calc PR . .
H49B H -0.1136 0.3127 0.0261 0.187 Uiso 0.988(16) 1 calc PR . .
H49C H -0.2456 0.3272 0.1065 0.187 Uiso 0.988(16) 1 calc PR . .
C50 C -0.039(3) 0.3096(4) 0.3676(19) 0.126(6) Uani 0.988(16) 1 d PDU . .
H50A H -0.1020 0.2951 0.3621 0.189 Uiso 0.988(16) 1 calc PR . .
H50B H -0.0675 0.3193 0.4549 0.189 Uiso 0.988(16) 1 calc PR . .
H50C H 0.0653 0.3048 0.3759 0.189 Uiso 0.988(16) 1 calc PR . .
O23 O 0.657(3) 0.2967(4) 0.5346(15) 0.166(9) Uani 0.89(2) 1 d PDU . .
N7 N 0.661(3) 0.2684(3) 0.7069(16) 0.130(7) Uani 0.89(2) 1 d PDU . .
C51 C 0.651(3) 0.2937(3) 0.6719(19) 0.122(6) Uani 0.89(2) 1 d PDU . .
H51 H 0.6417 0.3064 0.7429 0.146 Uiso 0.89(2) 1 calc PR . .
C52 C 0.666(3) 0.2519(4) 0.583(2) 0.132(7) Uani 0.89(2) 1 d PDU . .
H52A H 0.6769 0.2611 0.4904 0.198 Uiso 0.89(2) 1 calc PR . .
H52B H 0.5740 0.2424 0.5797 0.198 Uiso 0.89(2) 1 calc PR . .
H52C H 0.7513 0.2409 0.5946 0.198 Uiso 0.89(2) 1 calc PR . .
C53 C 0.639(3) 0.2631(4) 0.8593(19) 0.132(7) Uani 0.89(2) 1 d PDU . .
H53A H 0.6400 0.2454 0.8737 0.198 Uiso 0.89(2) 1 calc PR . .
H53B H 0.5426 0.2696 0.8910 0.198 Uiso 0.89(2) 1 calc PR . .
H53C H 0.7186 0.2705 0.9185 0.198 Uiso 0.89(2) 1 calc PR . .
O24 O 0.623(3) 0.2037(4) 0.856(2) 0.096(8) Uani 0.433(15) 1 d PDU . .
N8 N 0.7751(18) 0.1820(3) 0.6932(17) 0.051(4) Uani 0.433(15) 1 d PDU . .
C54 C 0.751(3) 0.1955(5) 0.823(2) 0.070(6) Uani 0.433(15) 1 d PDU . .
H54 H 0.8324 0.1987 0.8877 0.084 Uiso 0.433(15) 1 calc PR . .
C55 C 0.656(2) 0.1776(5) 0.585(2) 0.053(6) Uani 0.433(15) 1 d PDU . .
H55A H 0.6965 0.1686 0.4997 0.080 Uiso 0.433(15) 1 calc PR . .
H55B H 0.6158 0.1931 0.5502 0.080 Uiso 0.433(15) 1 calc PR . .
H55C H 0.5769 0.1680 0.6314 0.080 Uiso 0.433(15) 1 calc PR . .
C56 C 0.925(2) 0.1743(5) 0.659(3) 0.074(7) Uani 0.433(15) 1 d PDU . .
H56A H 0.9260 0.1658 0.5633 0.111 Uiso 0.433(15) 1 calc PR . .
H56B H 0.9610 0.1633 0.7373 0.111 Uiso 0.433(15) 1 calc PR . .
H56C H 0.9905 0.1885 0.6539 0.111 Uiso 0.433(15) 1 calc PR . .
O25 O 0.285(2) 0.0927(2) -0.0011(15) 0.076(5) Uani 0.553(17) 1 d PDU . .
N9 N 0.386(2) 0.1303(3) -0.0590(17) 0.084(6) Uani 0.553(17) 1 d PDU . .
C57 C 0.400(3) 0.1049(4) -0.028(4) 0.124(8) Uani 0.553(17) 1 d PDU . .
H57 H 0.4949 0.0974 -0.0272 0.149 Uiso 0.553(17) 1 calc PR . .
C58 C 0.494(3) 0.1477(5) 0.004(3) 0.100(8) Uani 0.553(17) 1 d PDU . .
H58A H 0.4742 0.1640 -0.0368 0.150 Uiso 0.553(17) 1 calc PR . .
H58B H 0.5952 0.1427 -0.0220 0.150 Uiso 0.553(17) 1 calc PR . .
H58C H 0.4835 0.1482 0.1125 0.150 Uiso 0.553(17) 1 calc PR . .
C59 C 0.286(3) 0.1375(5) -0.176(3) 0.091(7) Uani 0.553(17) 1 d PDU . .
H59A H 0.2934 0.1551 -0.1909 0.137 Uiso 0.553(17) 1 calc PR . .
H59B H 0.1836 0.1334 -0.1478 0.137 Uiso 0.553(17) 1 calc PR . .
H59C H 0.3122 0.1291 -0.2681 0.137 Uiso 0.553(17) 1 calc PR . .
O26 O 0.219(2) 0.5481(3) -0.262(2) 0.120(8) Uani 0.68(2) 1 d PDU . .
N10 N 0.102(3) 0.5112(4) -0.239(3) 0.151(9) Uani 0.68(2) 1 d PDU . .
C60 C 0.105(3) 0.5365(5) -0.225(5) 0.158(10) Uani 0.68(2) 1 d PDU . .
H60 H 0.0212 0.5449 -0.1868 0.190 Uiso 0.68(2) 1 calc PR . .
C61 C 0.233(3) 0.4970(6) -0.189(4) 0.156(11) Uani 0.68(2) 1 d PDU . .
H61A H 0.2130 0.4796 -0.2006 0.234 Uiso 0.68(2) 1 calc PR . .
H61B H 0.2539 0.5006 -0.0843 0.234 Uiso 0.68(2) 1 calc PR . .
H61C H 0.3202 0.5014 -0.2494 0.234 Uiso 0.68(2) 1 calc PR . .
C62 C -0.040(3) 0.4986(6) -0.226(4) 0.156(10) Uani 0.68(2) 1 d PDU . .
H62A H -0.0241 0.4810 -0.2310 0.233 Uiso 0.68(2) 1 calc PR . .
H62B H -0.1057 0.5036 -0.3084 0.233 Uiso 0.68(2) 1 calc PR . .
H62C H -0.0868 0.5028 -0.1313 0.233 Uiso 0.68(2) 1 calc PR . .
O27 O 0.339(2) 0.5994(6) 0.377(3) 0.217(15) Uani 0.726(16) 1 d PDU . .
N11 N 0.3111(19) 0.5719(3) 0.1858(18) 0.100(5) Uani 0.726(16) 1 d PDU . .
C63 C 0.398(2) 0.5886(3) 0.2650(17) 0.079(5) Uani 0.726(16) 1 d PDU . .
H63 H 0.4975 0.5919 0.2367 0.095 Uiso 0.726(16) 1 calc PR . .
C64 C 0.383(3) 0.5537(4) 0.087(3) 0.105(7) Uani 0.726(16) 1 d PDU . .
H64A H 0.3065 0.5433 0.0420 0.158 Uiso 0.726(16) 1 calc PR . .
H64B H 0.4515 0.5436 0.1457 0.158 Uiso 0.726(16) 1 calc PR . .
H64C H 0.4384 0.5621 0.0087 0.158 Uiso 0.726(16) 1 calc PR . .
C65 C 0.157(2) 0.5672(6) 0.224(3) 0.127(8) Uani 0.726(16) 1 d PDU . .
H65A H 0.1149 0.5551 0.1558 0.190 Uiso 0.726(16) 1 calc PR . .
H65B H 0.0994 0.5823 0.2172 0.190 Uiso 0.726(16) 1 calc PR . .
H65C H 0.1513 0.5609 0.3265 0.190 Uiso 0.726(16) 1 calc PR . .
O28 O 1.2025(13) 0.40173(15) 0.6892(10) 0.053(3) Uani 0.762(13) 1 d PDU . .
N12 N 1.1645(14) 0.4220(2) 0.9107(11) 0.067(3) Uani 0.762(13) 1 d PDU . .
C66 C 1.2525(18) 0.4128(3) 0.7955(15) 0.067(4) Uani 0.762(13) 1 d PDU . .
H66 H 1.3569 0.4153 0.8005 0.081 Uiso 0.762(13) 1 calc PR . .
C67 C 1.234(2) 0.4344(3) 1.0350(16) 0.075(4) Uani 0.762(13) 1 d PDU . .
H67A H 1.1572 0.4401 1.1037 0.112 Uiso 0.762(13) 1 calc PR . .
H67B H 1.2916 0.4483 0.9983 0.112 Uiso 0.762(13) 1 calc PR . .
H67C H 1.3006 0.4231 1.0870 0.112 Uiso 0.762(13) 1 calc PR . .
C68 C 1.013(2) 0.4130(5) 0.932(3) 0.112(6) Uani 0.762(13) 1 d PDU . .
H68A H 0.9670 0.4216 1.0156 0.167 Uiso 0.762(13) 1 calc PR . .
H68B H 1.0167 0.3955 0.9537 0.167 Uiso 0.762(13) 1 calc PR . .
H68C H 0.9550 0.4158 0.8415 0.167 Uiso 0.762(13) 1 calc PR . .

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 0.0962(9) 0.0135(4) 0.0197(4) 0.0010(3) -0.0056(4) -0.0028(5)
Zn2 0.1219(11) 0.0121(4) 0.0171(4) 0.0024(3) 0.0000(4) -0.0020(5)
Zn3 0.0564(7) 0.0175(4) 0.0231(4) -0.0031(3) -0.0005(3) -0.0081(4)
Zn4 0.0546(6) 0.0184(4) 0.0232(4) -0.0024(3) 0.0014(3) -0.0073(4)
N1 0.113(7) 0.012(3) 0.023(3) 0.006(2) -0.003(3) -0.003(4)
N2 0.046(5) 0.033(3) 0.028(3) -0.008(3) 0.000(3) -0.022(3)
C1 0.048(5) 0.018(3) 0.032(3) 0.002(3) -0.004(3) -0.010(3)
C2 0.084(7) 0.019(3) 0.041(4) 0.004(3) -0.010(4) -0.010(4)
C3 0.075(6) 0.027(3) 0.031(3) 0.002(3) -0.001(3) -0.004(4)
C4 0.067(5) 0.031(4) 0.020(3) 0.004(3) -0.003(3) -0.005(4)
C5 0.047(5) 0.028(3) 0.030(3) 0.005(3) 0.005(3) -0.004(3)
C6 0.050(5) 0.018(3) 0.025(3) 0.007(2) -0.001(3) -0.009(3)
C7 0.048(5) 0.029(3) 0.035(3) 0.001(3) -0.004(3) -0.001(3)
C8 0.064(6) 0.032(4) 0.040(4) -0.002(3) -0.006(4) -0.016(4)
C9 0.085(7) 0.021(3) 0.036(4) 0.005(3) -0.017(4) -0.002(4)
C10 0.075(6) 0.031(4) 0.023(3) 0.000(3) 0.008(3) -0.004(4)
C11 0.071(6) 0.037(4) 0.035(4) -0.001(3) 0.008(4) -0.020(4)
C12 0.047(5) 0.028(3) 0.029(3) 0.004(3) -0.006(3) -0.005(3)
C13 0.057(6) 0.027(4) 0.048(4) -0.015(3) 0.012(4) -0.005(4)
C14 0.068(6) 0.027(4) 0.036(4) -0.008(3) 0.007(4) -0.007(4)
O1 0.117(7) 0.028(3) 0.023(3) 0.012(2) -0.015(3) -0.010(4)
O2 0.063(5) 0.048(4) 0.044(3) -0.006(3) 0.016(3) -0.007(3)
N3 0.133(7) 0.018(3) 0.026(3) 0.005(3) -0.020(4) -0.007(4)
N4 0.070(6) 0.020(3) 0.028(3) -0.008(2) 0.011(3) -0.001(3)
C15 0.074(5) 0.031(4) 0.074(5) 0.013(4) 0.020(4) 0.019(4)
C16 0.090(7) 0.077(7) 0.133(9) 0.034(6) -0.010(6) 0.001(6)
C17 0.085(6) 0.092(6) 0.082(7) 0.004(6) 0.003(6) 0.029(5)
C18 0.061(6) 0.059(5) 0.122(7) 0.028(6) 0.013(5) 0.012(5)
C19 0.093(6) 0.047(5) 0.089(6) 0.024(5) 0.018(5) 0.001(5)
C20 0.066(5) 0.041(4) 0.075(6) 0.015(4) 0.023(4) 0.002(4)
C21 0.097(5) 0.018(3) 0.033(4) -0.005(3) -0.007(4) 0.003(3)
C22 0.105(7) 0.050(5) 0.118(8) 0.029(6) -0.062(6) -0.017(5)
C23 0.135(8) 0.058(5) 0.113(8) 0.046(6) -0.058(7) -0.012(6)
C24 0.140(9) 0.049(5) 0.073(6) 0.016(5) 0.045(6) 0.027(6)
C25 0.107(8) 0.055(5) 0.063(5) 0.013(4) 0.029(5) 0.027(5)
C26 0.078(6) 0.027(3) 0.034(4) 0.001(3) 0.004(4) -0.002(4)
C27 0.052(6) 0.040(4) 0.059(5) 0.022(4) 0.012(4) 0.013(4)
C28 0.058(6) 0.041(4) 0.065(5) 0.018(4) 0.018(4) 0.014(4)
O3 0.081(8) 0.139(10) 0.174(13) 0.078(10) 0.009(7) -0.006(7)
O4 0.157(12) 0.133(10) 0.109(6) 0.048(7) 0.072(7) 0.087(9)
O5 0.114(7) 0.024(3) 0.056(4) 0.001(3) -0.014(4) 0.001(4)
O6 0.113(7) 0.025(3) 0.058(4) 0.010(3) -0.028(4) -0.009(4)
O7 0.100(6) 0.024(3) 0.050(3) 0.005(3) 0.005(3) 0.002(4)
O8 0.136(9) 0.025(3) 0.088(6) 0.014(4) 0.030(6) 0.025(4)
C29 0.083(5) 0.021(4) 0.045(4) 0.004(3) -0.014(4) 0.002(4)
C30 0.091(5) 0.034(4) 0.052(5) -0.005(4) -0.013(5) -0.002(4)
C31 0.087(5) 0.026(4) 0.053(5) 0.003(4) 0.002(4) 0.002(4)
C32 0.091(6) 0.045(4) 0.049(5) 0.002(4) -0.006(4) 0.003(4)
O9 0.122(7) 0.025(3) 0.030(3) 0.000(2) -0.005(3) -0.008(4)
O10 0.084(5) 0.036(3) 0.023(2) 0.008(3) 0.001(2) -0.014(3)
O11 0.110(6) 0.028(3) 0.029(3) 0.004(2) 0.001(3) -0.032(4)
O12 0.197(11) 0.024(3) 0.017(3) 0.002(2) -0.007(4) -0.024(4)
C33 0.075(6) 0.014(3) 0.025(3) -0.004(3) -0.007(3) -0.003(3)
C34 0.075(6) 0.030(4) 0.023(3) 0.006(3) -0.006(3) 0.002(4)
C35 0.084(6) 0.023(4) 0.034(3) -0.010(3) 0.000(4) -0.007(4)
C36 0.083(6) 0.030(4) 0.028(3) 0.011(3) -0.006(4) -0.005(4)
O13 0.050(5) 0.031(3) 0.113(6) 0.002(4) -0.012(4) -0.021(4)
O14 0.048(5) 0.036(4) 0.094(6) -0.025(4) -0.007(4) 0.003(3)
O15 0.056(5) 0.040(4) 0.104(6) -0.021(4) -0.016(4) -0.007(4)
O16 0.055(5) 0.050(4) 0.115(7) 0.008(5) -0.008(4) -0.022(4)
C37 0.047(5) 0.028(4) 0.042(4) 0.001(3) -0.002(4) -0.004(4)
C38 0.050(4) 0.030(4) 0.059(5) -0.008(4) 0.004(4) -0.003(3)
C39 0.054(4) 0.033(4) 0.060(5) 0.000(4) 0.002(4) -0.005(3)
C40 0.049(5) 0.045(4) 0.050(4) -0.004(4) 0.011(4) -0.012(4)
O17 0.121(8) 0.042(4) 0.019(3) 0.005(2) 0.000(3) -0.015(4)
O18 0.137(8) 0.031(3) 0.019(2) -0.008(3) 0.002(3) -0.008(4)
O19 0.139(7) 0.021(3) 0.021(2) -0.002(2) -0.015(3) -0.004(4)
O20 0.145(8) 0.028(3) 0.022(3) 0.002(2) 0.009(3) -0.024(4)
C41 0.050(5) 0.031(4) 0.032(3) -0.003(3) 0.005(3) -0.012(4)
C42 0.064(6) 0.027(4) 0.034(3) 0.001(3) 0.003(3) -0.007(4)
C43 0.072(6) 0.027(4) 0.029(3) 0.002(3) 0.005(3) -0.022(4)
C44 0.066(6) 0.029(4) 0.035(4) 0.001(3) 0.003(4) -0.010(4)
O21 0.106(8) 0.059(5) 0.069(5) -0.002(4) 0.030(4) -0.002(5)
N5 0.079(8) 0.053(5) 0.083(6) 0.005(4) 0.025(5) -0.004(5)
C45 0.050(6) 0.058(5) 0.064(5) 0.008(4) -0.001(4) -0.011(4)
C46 0.135(10) 0.077(6) 0.140(10) 0.028(7) 0.037(8) 0.013(7)
C47 0.086(8) 0.070(6) 0.063(5) 0.001(5) 0.007(5) -0.003(6)
O22 0.205(18) 0.162(11) 0.082(7) -0.002(7) 0.063(9) 0.048(11)
N6 0.099(10) 0.094(8) 0.118(8) -0.044(6) 0.016(7) 0.030(7)
C48 0.125(10) 0.114(8) 0.106(8) -0.024(6) 0.031(7) 0.013(7)
C49 0.127(10) 0.113(9) 0.135(9) -0.010(8) -0.012(7) 0.027(7)
C50 0.143(11) 0.113(9) 0.121(8) -0.016(7) 0.015(7) 0.033(8)
O23 0.21(2) 0.209(18) 0.077(7) 0.018(9) -0.041(10) 0.073(15)
N7 0.177(18) 0.121(10) 0.093(8) -0.010(7) 0.010(10) 0.062(13)
C51 0.137(11) 0.117(8) 0.112(8) 0.005(7) 0.000(8) -0.003(8)
C52 0.149(12) 0.126(9) 0.120(9) -0.008(8) 0.001(8) -0.014(9)
C53 0.142(12) 0.141(11) 0.112(7) 0.010(7) -0.004(8) 0.004(9)
O24 0.123(17) 0.082(14) 0.082(13) -0.003(11) -0.020(11) 0.068(14)
N8 0.046(9) 0.056(11) 0.050(8) 0.017(6) -0.005(6) -0.018(8)
C54 0.075(10) 0.069(10) 0.067(8) -0.009(7) -0.003(7) -0.012(8)
C55 0.056(9) 0.056(9) 0.048(8) -0.008(7) -0.002(7) 0.006(8)
C56 0.067(8) 0.068(10) 0.087(11) -0.010(8) -0.003(7) -0.001(8)
O25 0.134(14) 0.049(8) 0.046(7) -0.002(6) -0.019(8) 0.009(7)
N9 0.140(17) 0.067(9) 0.045(8) -0.008(7) 0.023(8) -0.008(9)
C57 0.137(12) 0.104(9) 0.132(12) 0.016(8) -0.008(9) -0.005(8)
C58 0.092(11) 0.109(10) 0.099(11) 0.001(9) 0.003(8) -0.004(8)
C59 0.105(11) 0.097(11) 0.073(9) 0.009(8) 0.008(7) -0.025(8)
O26 0.154(16) 0.047(7) 0.158(17) 0.035(9) 0.058(14) 0.039(8)
N10 0.149(15) 0.159(12) 0.146(18) 0.043(15) -0.064(15) -0.072(11)
C60 0.151(13) 0.157(11) 0.168(14) 0.013(9) 0.011(9) -0.004(8)
C61 0.152(12) 0.160(13) 0.156(14) -0.003(10) 0.000(9) -0.003(9)
C62 0.139(11) 0.171(13) 0.157(14) 0.013(10) -0.001(9) -0.022(9)
O27 0.077(13) 0.38(3) 0.19(2) -0.20(2) 0.005(12) 0.055(17)
N11 0.108(10) 0.107(12) 0.084(10) -0.014(8) -0.033(8) 0.032(8)
C63 0.086(8) 0.087(8) 0.065(7) -0.002(6) 0.022(6) -0.004(7)
C64 0.115(10) 0.095(10) 0.106(10) -0.029(7) -0.014(8) 0.003(8)
C65 0.119(9) 0.136(12) 0.126(11) -0.024(9) 0.005(8) -0.024(8)
O28 0.081(8) 0.025(4) 0.052(5) -0.001(3) -0.014(4) 0.008(4)
N12 0.073(8) 0.087(9) 0.042(5) -0.002(5) -0.004(5) -0.018(7)
C66 0.067(8) 0.063(7) 0.073(6) -0.005(5) -0.006(5) 0.001(6)
C67 0.084(8) 0.081(8) 0.059(6) -0.010(6) -0.014(6) 0.014(7)
C68 0.094(8) 0.130(11) 0.111(10) 0.014(8) -0.003(7) -0.025(8)

_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 Zn2 3.0322(12) . ?
Zn1 N1 2.060(6) . ?
Zn1 O5 1.997(10) . ?
Zn1 O7 1.976(9) 1_455 ?
Zn1 O9 2.049(6) . ?
Zn1 O11 2.051(6) 1_556 ?
Zn2 N3 2.077(7) . ?
Zn2 O6 2.072(10) . ?
Zn2 O8 1.994(11) 1_455 ?
Zn2 O10 2.004(5) . ?
Zn2 O12 2.036(6) 1_556 ?
Zn3 Zn4 2.9635(11) . ?
Zn3 N2 2.018(6) . ?
Zn3 O13 2.014(8) . ?
Zn3 O15 2.036(9) 1_455 ?
Zn3 O17 2.021(6) . ?
Zn3 O19 2.021(5) 1_556 ?
Zn4 N4 2.032(6) 2_656 ?
Zn4 O14 2.018(9) . ?
Zn4 O16 2.027(9) 1_455 ?
Zn4 O18 2.019(5) . ?
Zn4 O20 2.013(6) 1_556 ?
N1 C1 1.368(9) . ?
N1 C9 1.339(10) . ?
N2 C10 1.358(11) . ?
N2 C14 1.336(10) . ?
C1 C2 1.459(10) . ?
C1 C6 1.393(9) . ?
C2 C3 1.600(10) . ?
C3 C4 1.481(10) . ?
C4 C5 1.539(11) . ?
C4 O1 1.418(8) . ?
C5 C6 1.520(9) . ?
C5 O2 1.427(11) . ?
C6 C7 1.393(10) . ?
C7 C8 1.400(10) . ?
C7 C12 1.471(9) . ?
C8 C9 1.378(10) . ?
C10 C11 1.373(11) . ?
C11 C12 1.414(11) . ?
C12 C13 1.374(11) . ?
C13 C14 1.380(11) . ?
N3 C15 1.327(12) . ?
N3 C23 1.324(13) . ?
N4 Zn4 2.032(6) 2_646 ?
N4 C24 1.321(12) . ?
N4 C28 1.315(11) . ?
C15 C16 1.432(14) . ?
C15 C20 1.377(11) . ?
C16 C17 1.654(16) . ?
C17 C18 1.520(14) . ?
C18 C19 1.583(15) . ?
C18 O3 1.411(14) . ?
C19 C20 1.526(13) . ?
C19 O4 1.445(14) . ?
C20 C21 1.366(13) . ?
C21 C22 1.374(14) . ?
C21 C26 1.506(10) . ?
C22 C23 1.413(13) . ?
C24 C25 1.402(13) . ?
C25 C26 1.448(13) . ?
C26 C27 1.354(11) . ?
C27 C28 1.414(11) . ?
O5 C29 1.290(12) . ?
O6 C29 1.264(13) . ?
O7 Zn1 1.976(9) 1_655 ?
O7 C32 1.305(15) . ?
O8 Zn2 1.994(11) 1_655 ?
O8 C32 1.245(14) . ?
C29 C30 1.440(18) . ?
C30 C31 1.338(16) . ?
C31 C32 1.468(19) . ?
O9 C33 1.248(10) . ?
O10 C33 1.261(10) . ?
O11 Zn1 2.051(6) 1_554 ?
O11 C36 1.243(11) . ?
O12 Zn2 2.036(6) 1_554 ?
O12 C36 1.229(11) . ?
C33 C34 1.484(11) . ?
C34 C35 1.342(12) . ?
C35 C36 1.451(12) . ?
O13 C37 1.200(13) . ?
O14 C37 1.217(12) . ?
O15 Zn3 2.036(9) 1_655 ?
O15 C40 1.244(14) . ?
O16 Zn4 2.027(9) 1_655 ?
O16 C40 1.240(13) . ?
C37 C38 1.558(16) . ?
C38 C39 1.266(13) . ?
C39 C40 1.480(16) . ?
O17 C41 1.230(11) . ?
O18 C41 1.235(11) . ?
O19 Zn3 2.021(5) 1_554 ?
O19 C44 1.271(11) . ?
O20 Zn4 2.013(6) 1_554 ?
O20 C44 1.280(11) . ?
C41 C42 1.504(11) . ?
C42 C43 1.306(11) . ?
C43 C44 1.476(12) . ?
O21 C45 1.241(11) . ?
N5 C45 1.350(12) . ?
N5 C46 1.445(13) . ?
N5 C47 1.441(12) . ?
O22 C48 1.204(14) . ?
N6 C48 1.379(14) . ?
N6 C49 1.444(14) . ?
N6 C50 1.427(14) . ?
O23 C51 1.221(15) . ?
N7 C51 1.401(15) . ?
N7 C52 1.409(15) . ?
N7 C53 1.386(15) . ?
O24 C54 1.243(16) . ?
N8 C54 1.371(15) . ?
N8 C55 1.435(15) . ?
N8 C56 1.418(16) . ?
O25 C57 1.227(16) . ?
N9 C57 1.398(16) . ?
N9 C58 1.445(16) . ?
N9 C59 1.410(16) . ?
O26 C60 1.226(16) . ?
N10 C60 1.371(17) . ?
N10 C61 1.455(16) . ?
N10 C62 1.427(16) . ?
O27 C63 1.253(14) . ?
N11 C63 1.370(15) . ?
N11 C64 1.456(15) . ?
N11 C65 1.425(16) . ?
O28 C66 1.194(13) . ?
N12 C66 1.371(14) . ?
N12 C67 1.417(13) . ?
N12 C68 1.430(15) . ?

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
Zn2 Zn1 N1 173.0(2) . . ?
Zn2 Zn1 O5 80.2(2) . . ?
Zn2 Zn1 O7 85.2(2) . 1_455 ?
Zn2 Zn1 O9 69.90(18) . . ?
Zn2 Zn1 O11 77.91(17) . 1_556 ?
N1 Zn1 O5 93.8(3) . . ?
N1 Zn1 O7 100.8(3) . 1_455 ?
N1 Zn1 O9 113.6(2) . . ?
N1 Zn1 O11 98.3(2) . 1_556 ?
O5 Zn1 O7 165.3(3) . 1_455 ?
O5 Zn1 O9 87.5(3) . . ?
O5 Zn1 O11 86.5(3) . 1_556 ?
O7 Zn1 O9 88.5(3) 1_455 . ?
O7 Zn1 O11 89.4(3) 1_455 1_556 ?
O9 Zn1 O11 147.8(2) . 1_556 ?
Zn1 Zn2 N3 168.03(19) . . ?
Zn1 Zn2 O6 77.16(19) . . ?
Zn1 Zn2 O8 71.2(3) . 1_455 ?
Zn1 Zn2 O10 86.85(18) . . ?
Zn1 Zn2 O12 77.49(18) . 1_556 ?
N3 Zn2 O6 97.2(3) . . ?
N3 Zn2 O8 114.1(4) . 1_455 ?
N3 Zn2 O10 103.6(3) . . ?
N3 Zn2 O12 91.9(3) . 1_556 ?
O6 Zn2 O8 148.3(3) . 1_455 ?
O6 Zn2 O10 87.3(3) . . ?
O6 Zn2 O12 87.8(4) . 1_556 ?
O8 Zn2 O10 89.9(4) 1_455 . ?
O8 Zn2 O12 86.5(4) 1_455 1_556 ?
O10 Zn2 O12 164.3(2) . 1_556 ?
Zn4 Zn3 N2 172.7(2) . . ?
Zn4 Zn3 O13 81.5(2) . . ?
Zn4 Zn3 O15 75.4(2) . 1_455 ?
Zn4 Zn3 O17 74.8(2) . . ?
Zn4 Zn3 O19 84.96(19) . 1_556 ?
N2 Zn3 O13 103.3(3) . . ?
N2 Zn3 O15 100.0(3) . 1_455 ?
N2 Zn3 O17 99.8(3) . . ?
N2 Zn3 O19 100.5(3) . 1_556 ?
O13 Zn3 O15 156.7(3) . 1_455 ?
O13 Zn3 O17 88.2(4) . . ?
O13 Zn3 O19 88.4(4) . 1_556 ?
O15 Zn3 O17 88.4(4) 1_455 . ?
O15 Zn3 O19 86.9(4) 1_455 1_556 ?
O17 Zn3 O19 159.7(3) . 1_556 ?
Zn3 Zn4 N4 169.3(2) . 2_656 ?
Zn3 Zn4 O14 76.2(2) . . ?
Zn3 Zn4 O16 83.0(3) . 1_455 ?
Zn3 Zn4 O18 83.4(2) . . ?
Zn3 Zn4 O20 74.70(19) . 1_556 ?
N4 Zn4 O14 99.4(3) 2_656 . ?
N4 Zn4 O16 101.5(3) 2_656 1_455 ?
N4 Zn4 O18 106.4(3) 2_656 . ?
N4 Zn4 O20 95.6(3) 2_656 1_556 ?
O14 Zn4 O16 159.0(3) . 1_455 ?
O14 Zn4 O18 88.1(4) . . ?
O14 Zn4 O20 88.3(4) . 1_556 ?
O16 Zn4 O18 87.0(4) 1_455 . ?
O16 Zn4 O20 88.6(4) 1_455 1_556 ?
O18 Zn4 O20 158.0(3) . 1_556 ?
Zn1 N1 C1 127.5(5) . . ?
Zn1 N1 C9 113.0(5) . . ?
C1 N1 C9 119.0(7) . . ?
Zn3 N2 C10 120.1(5) . . ?
Zn3 N2 C14 122.5(6) . . ?
C10 N2 C14 117.3(7) . . ?
N1 C1 C2 113.5(6) . . ?
N1 C1 C6 121.0(6) . . ?
C2 C1 C6 125.0(7) . . ?
C1 C2 C3 114.1(7) . . ?
C2 C3 C4 108.5(6) . . ?
C3 C4 C5 112.6(8) . . ?
C3 C4 O1 107.3(6) . . ?
C5 C4 O1 110.9(7) . . ?
C4 C5 C6 111.4(6) . . ?
C4 C5 O2 111.1(6) . . ?
C6 C5 O2 106.4(7) . . ?
C1 C6 C5 118.7(6) . . ?
C1 C6 C7 119.8(6) . . ?
C5 C6 C7 121.4(6) . . ?
C6 C7 C8 117.8(7) . . ?
C6 C7 C12 125.1(6) . . ?
C8 C7 C12 116.9(6) . . ?
C7 C8 C9 119.9(7) . . ?
N1 C9 C8 122.2(7) . . ?
N2 C10 C11 122.7(8) . . ?
C10 C11 C12 119.4(8) . . ?
C7 C12 C11 118.7(7) . . ?
C7 C12 C13 124.0(7) . . ?
C11 C12 C13 117.3(7) . . ?
C12 C13 C14 120.0(8) . . ?
N2 C14 C13 123.3(8) . . ?
Zn2 N3 C15 127.0(7) . . ?
Zn2 N3 C23 112.0(7) . . ?
C15 N3 C23 120.2(9) . . ?
Zn4 N4 C24 119.3(6) 2_646 . ?
Zn4 N4 C28 122.5(6) 2_646 . ?
C24 N4 C28 118.3(8) . . ?
N3 C15 C16 114.9(9) . . ?
N3 C15 C20 119.7(10) . . ?
C16 C15 C20 125.1(11) . . ?
C15 C16 C17 109.3(10) . . ?
C16 C17 C18 102.0(10) . . ?
C17 C18 C19 107.1(11) . . ?
C17 C18 O3 103.2(11) . . ?
C19 C18 O3 103.7(10) . . ?
C18 C19 C20 106.2(8) . . ?
C18 C19 O4 119.1(11) . . ?
C20 C19 O4 105.8(11) . . ?
C15 C20 C19 119.1(10) . . ?
C15 C20 C21 121.5(10) . . ?
C19 C20 C21 116.9(8) . . ?
C20 C21 C22 118.6(8) . . ?
C20 C21 C26 124.2(9) . . ?
C22 C21 C26 117.0(9) . . ?
C21 C22 C23 117.2(11) . . ?
N3 C23 C22 121.4(12) . . ?
N4 C24 C25 124.2(10) . . ?
C24 C25 C26 112.6(10) . . ?
C21 C26 C25 116.2(8) . . ?
C21 C26 C27 123.1(8) . . ?
C25 C26 C27 118.8(8) . . ?
C26 C27 C28 118.8(9) . . ?
N4 C28 C27 121.5(8) . . ?
Zn1 O5 C29 127.3(8) . . ?
Zn2 O6 C29 128.6(8) . . ?
Zn1 O7 C32 119.5(7) 1_655 . ?
Zn2 O8 C32 139.4(10) 1_655 . ?
O5 C29 O6 124.3(12) . . ?
O5 C29 C30 119.9(10) . . ?
O6 C29 C30 115.7(9) . . ?
C29 C30 C31 122.1(10) . . ?
C30 C31 C32 123.1(10) . . ?
O7 C32 O8 123.1(14) . . ?
O7 C32 C31 116.0(10) . . ?
O8 C32 C31 120.8(12) . . ?
Zn1 O9 C33 138.1(6) . . ?
Zn2 O10 C33 117.7(5) . . ?
Zn1 O11 C36 128.7(6) 1_554 . ?
Zn2 O12 C36 130.7(6) 1_554 . ?
O9 C33 O10 125.7(7) . . ?
O9 C33 C34 117.5(8) . . ?
O10 C33 C34 116.4(7) . . ?
C33 C34 C35 123.6(8) . . ?
C34 C35 C36 122.3(8) . . ?
O11 C36 O12 123.6(8) . . ?
O11 C36 C35 117.4(8) . . ?
O12 C36 C35 118.9(8) . . ?
Zn3 O13 C37 123.2(8) . . ?
Zn4 O14 C37 129.7(8) . . ?
Zn3 O15 C40 132.9(8) 1_655 . ?
Zn4 O16 C40 123.2(8) 1_655 . ?
O13 C37 O14 129.3(11) . . ?
O13 C37 C38 115.7(9) . . ?
O14 C37 C38 115.0(9) . . ?
C37 C38 C39 122.5(9) . . ?
C38 C39 C40 123.2(10) . . ?
O15 C40 O16 125.3(11) . . ?
O15 C40 C39 116.6(9) . . ?
O16 C40 C39 118.0(10) . . ?
Zn3 O17 C41 133.4(6) . . ?
Zn4 O18 C41 121.7(6) . . ?
Zn3 O19 C44 120.9(6) 1_554 . ?
Zn4 O20 C44 134.4(6) 1_554 . ?
O17 C41 O18 126.5(8) . . ?
O17 C41 C42 116.5(7) . . ?
O18 C41 C42 116.5(8) . . ?
C41 C42 C43 122.8(8) . . ?
C42 C43 C44 122.5(8) . . ?
O19 C44 O20 124.3(8) . . ?
O19 C44 C43 116.8(7) . . ?
O20 C44 C43 118.4(8) . . ?
C45 N5 C46 120.8(10) . . ?
C45 N5 C47 120.9(9) . . ?
C46 N5 C47 117.5(11) . . ?
O21 C45 N5 124.7(10) . . ?
C48 N6 C49 122.2(14) . . ?
C48 N6 C50 119.9(14) . . ?
C49 N6 C50 117.9(14) . . ?
O22 C48 N6 120.9(18) . . ?
C51 N7 C52 116.6(14) . . ?
C51 N7 C53 114.0(14) . . ?
C52 N7 C53 128.4(17) . . ?
O23 C51 N7 110.0(16) . . ?
C54 N8 C55 122.0(15) . . ?
C54 N8 C56 118.5(16) . . ?
C55 N8 C56 119.3(16) . . ?
O24 C54 N8 121.6(19) . . ?
C57 N9 C58 120.4(18) . . ?
C57 N9 C59 118.0(17) . . ?
C58 N9 C59 120.5(16) . . ?
O25 C57 N9 119(2) . . ?
C60 N10 C61 118.6(19) . . ?
C60 N10 C62 119(2) . . ?
C61 N10 C62 115.1(19) . . ?
O26 C60 N10 120(2) . . ?
C63 N11 C64 120.3(15) . . ?
C63 N11 C65 121.7(15) . . ?
C64 N11 C65 116.0(15) . . ?
O27 C63 N11 118.4(17) . . ?
C66 N12 C67 119.8(12) . . ?
C66 N12 C68 120.0(13) . . ?
C67 N12 C68 117.3(13) . . ?
O28 C66 N12 123.7(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O28 0.82 1.92 2.735(10) 170 1_454
O2 H2 O21 0.82 2.20 2.740(11) 123 1_554
O3 H3 O26 0.82 2.05 2.87(2) 177 2_545
O4 H4A O27 0.82 1.96 2.73(2) 156 2_546

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.22
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.093

#===END