# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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 
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#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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data_20_1
_database_code_depnum_ccdc_archive 'CCDC 917345'
#TrackingRef '1.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H8 N4 O2 Zn '
_chemical_formula_sum            'C9 H8 N4 O2 Zn '
_chemical_formula_weight         269.58
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
_cell_length_a                   9.639(4)
_cell_length_b                   10.219(5)
_cell_length_c                   21.866(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2153.8(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_process_details   SADABS,Bruker(2002)
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9597
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.39
_reflns_number_total             1980
_reflns_number_gt                1436
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0000P)^2^+27.9734P] 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_number_reflns         1977
_refine_ls_number_parameters     145
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.1818
_refine_ls_wR_factor_gt          0.1670
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_restrained_S_all      1.286
_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 0.41623(11) 0.12020(9) 0.44508(5) 0.0327(3) Uani 1 1 d . . .
O1 O 0.3696(11) 0.0859(10) 0.3565(4) 0.085(3) Uani 1 1 d U . .
N1 N 0.2831(8) 0.2625(7) 0.4728(4) 0.0350(19) Uani 1 1 d . . .
N4 N 0.3650(11) 0.4461(10) 0.4153(6) 0.086(4) Uani 1 1 d . . .
H2 H 0.3551 0.5271 0.4056 0.104 Uiso 1 1 calc R . .
H3 H 0.4349 0.4025 0.4017 0.104 Uiso 1 1 calc R . .
C2 C 0.2715(10) 0.3876(10) 0.4518(5) 0.043(2) Uani 1 1 d . . .
C4 C 0.4255(13) 0.1729(12) 0.2602(6) 0.055(3) Uani 1 1 d . . .
C5 C 0.3408(18) 0.0942(19) 0.2293(7) 0.102(6) Uani 1 1 d . . .
H4 H 0.2852 0.0359 0.2508 0.122 Uiso 1 1 calc R . .
C9 C 0.508(2) 0.257(2) 0.2289(8) 0.115(7) Uani 1 1 d . . .
H8 H 0.5688 0.3120 0.2498 0.138 Uiso 1 1 calc R . .
C8 C 0.501(3) 0.261(3) 0.1663(11) 0.155(13) Uani 1 1 d . . .
H7 H 0.5565 0.3204 0.1452 0.185 Uiso 1 1 calc R . .
C7 C 0.417(3) 0.182(3) 0.1349(9) 0.144(14) Uani 1 1 d . . .
H6 H 0.4152 0.1853 0.0924 0.172 Uiso 1 1 calc R . .
C6 C 0.333(2) 0.096(3) 0.1655(9) 0.135(9) Uani 1 1 d . . .
H5 H 0.2724 0.0413 0.1446 0.162 Uiso 1 1 calc R . .
C1 C 0.1756(10) 0.2501(9) 0.5110(5) 0.041(3) Uani 1 1 d . . .
H1 H 0.1575 0.1751 0.5337 0.049 Uiso 1 1 calc R . .
N3 N 0.1612(7) 0.4474(7) 0.4747(4) 0.0329(18) Uani 1 1 d . . .
N2 N 0.0983(7) 0.3561(6) 0.5129(3) 0.0326(17) Uani 1 1 d . . .
C3 C 0.4354(15) 0.1687(13) 0.3283(7) 0.068(4) Uani 1 1 d . . .
O2 O 0.5116(11) 0.2477(13) 0.3562(5) 0.098(3) 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 0.0335(5) 0.0205(5) 0.0441(6) 0.0065(5) -0.0002(5) 0.0005(5)
O1 0.110(7) 0.077(6) 0.069(5) 0.014(5) 0.019(5) 0.008(5)
N1 0.029(4) 0.022(4) 0.054(5) 0.007(4) 0.003(4) 0.002(3)
N4 0.073(8) 0.041(6) 0.144(11) 0.027(7) 0.056(8) 0.010(5)
C2 0.043(5) 0.032(5) 0.054(6) 0.016(5) 0.007(5) 0.003(5)
C4 0.059(7) 0.058(7) 0.050(7) 0.011(6) 0.007(6) 0.019(6)
C5 0.104(13) 0.132(17) 0.069(11) -0.011(10) 0.001(10) 0.016(13)
C9 0.139(17) 0.109(14) 0.096(15) 0.016(11) 0.050(13) -0.014(13)
C8 0.23(3) 0.14(2) 0.094(18) 0.051(16) 0.09(2) 0.06(2)
C7 0.18(3) 0.20(3) 0.044(11) 0.023(14) 0.022(14) 0.12(2)
C6 0.127(17) 0.20(3) 0.078(14) -0.029(16) -0.027(12) 0.070(18)
C1 0.033(5) 0.019(4) 0.070(8) 0.010(5) 0.003(5) 0.002(4)
N3 0.025(4) 0.018(3) 0.056(5) 0.008(4) 0.003(4) -0.002(3)
N2 0.031(4) 0.019(4) 0.048(5) 0.007(3) 0.004(4) 0.002(3)
C3 0.068(9) 0.057(8) 0.078(10) 0.003(7) 0.020(8) 0.017(7)
O2 0.091(6) 0.116(7) 0.088(6) -0.025(6) 0.003(5) 0.006(6)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 1.996(7) 3_556 ?
Zn1 O1 2.020(10) . ?
Zn1 N3 2.023(7) 7_655 ?
Zn1 N1 2.032(7) . ?
O1 C3 1.224(15) . ?
N1 C1 1.338(12) . ?
N1 C2 1.363(12) . ?
N4 C2 1.344(13) . ?
N4 H2 0.8600 . ?
N4 H3 0.8600 . ?
C2 N3 1.324(12) . ?
C4 C5 1.33(2) . ?
C4 C9 1.357(19) . ?
C4 C3 1.492(18) . ?
C5 C6 1.40(2) . ?
C5 H4 0.9300 . ?
C9 C8 1.37(3) . ?
C9 H8 0.9300 . ?
C8 C7 1.34(4) . ?
C8 H7 0.9300 . ?
C7 C6 1.37(3) . ?
C7 H6 0.9300 . ?
C6 H5 0.9300 . ?
C1 N2 1.315(11) . ?
C1 H1 0.9300 . ?
N3 N2 1.392(10) . ?
N3 Zn1 2.023(7) 7_665 ?
N2 Zn1 1.996(7) 3_456 ?
C3 O2 1.251(17) . ?
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 Zn1 O1 131.2(4) 3_556 . ?
N2 Zn1 N3 106.4(3) 3_556 7_655 ?
O1 Zn1 N3 94.2(4) . 7_655 ?
N2 Zn1 N1 109.3(3) 3_556 . ?
O1 Zn1 N1 105.6(4) . . ?
N3 Zn1 N1 107.2(3) 7_655 . ?
C3 O1 Zn1 104.3(10) . . ?
C1 N1 C2 103.6(8) . . ?
C1 N1 Zn1 127.5(6) . . ?
C2 N1 Zn1 128.5(7) . . ?
C2 N4 H2 120.0 . . ?
C2 N4 H3 120.0 . . ?
H2 N4 H3 120.0 . . ?
N3 C2 N4 123.9(9) . . ?
N3 C2 N1 111.8(8) . . ?
N4 C2 N1 124.2(10) . . ?
C5 C4 C9 119.1(15) . . ?
C5 C4 C3 121.9(13) . . ?
C9 C4 C3 118.9(15) . . ?
C4 C5 C6 122(2) . . ?
C4 C5 H4 118.9 . . ?
C6 C5 H4 118.9 . . ?
C4 C9 C8 120(2) . . ?
C4 C9 H8 120.2 . . ?
C8 C9 H8 120.2 . . ?
C7 C8 C9 122(3) . . ?
C7 C8 H7 119.2 . . ?
C9 C8 H7 119.2 . . ?
C8 C7 C6 120(2) . . ?
C8 C7 H6 120.1 . . ?
C6 C7 H6 120.1 . . ?
C7 C6 C5 118(2) . . ?
C7 C6 H5 121.1 . . ?
C5 C6 H5 121.1 . . ?
N2 C1 N1 112.4(8) . . ?
N2 C1 H1 123.8 . . ?
N1 C1 H1 123.8 . . ?
C2 N3 N2 105.5(7) . . ?
C2 N3 Zn1 125.3(6) . 7_665 ?
N2 N3 Zn1 128.0(5) . 7_665 ?
C1 N2 N3 106.7(7) . . ?
C1 N2 Zn1 127.8(6) . 3_456 ?
N3 N2 Zn1 125.3(5) . 3_456 ?
O1 C3 O2 120.3(15) . . ?
O1 C3 C4 119.3(14) . . ?
O2 C3 C4 120.4(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
N4 H3 O2 0.86 2.01 2.789(16) 150.1 .
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.125


data_15
_database_code_depnum_ccdc_archive 'CCDC 917346'
#TrackingRef '2.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C6 H5 N4 O2 Zn), O '
_chemical_formula_sum            'C12 H10 N8 O5 Zn2 '
_chemical_formula_weight         477.06
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           tetragonal
_symmetry_space_group_name_H-M   ' P 4/n n c '
_symmetry_space_group_name_Hall  '-P 4a 2bc '
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+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'
_cell_length_a                   12.700(3)
_cell_length_b                   12.700(3)
_cell_length_c                   25.364(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4091(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904.0
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_process_details   SADABS,Bruker(2002)
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17697
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         24.50
_reflns_number_total             1716
_reflns_number_gt                1261
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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^)+(0.0875P)^2^+25.7865P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1715
_refine_ls_number_parameters     115
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1833
_refine_ls_wR_factor_gt          0.1628
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.8096(3) -0.0046(4) 0.41755(12) 0.0340(17) Uani 1 1 d G . .
N2 N 0.9026(2) -0.0016(4) 0.44860(15) 0.0316(14) Uani 1 1 d G . .
N1 N 0.8738(3) 0.0268(4) 0.50079(13) 0.0326(14) Uani 1 1 d G . .
C1 C 0.7630(3) 0.0414(4) 0.50199(14) 0.0412(19) Uani 1 1 d G . .
H1 H 0.7233 0.0603 0.5313 0.049 Uiso 1 1 calc R . .
N4 N 0.7233(2) 0.0220(4) 0.45055(16) 0.0369(16) Uani 1 1 d G . .
Zn1 Zn 0.96145(6) 0.06926(6) 0.56247(3) 0.0287(3) Uani 1 1 d . . .
O1 O 0.8536(5) 0.0505(6) 0.6162(2) 0.0649(19) Uani 1 1 d . . .
C4 C 0.8180(7) 0.0694(7) 0.7073(3) 0.045(2) Uani 1 1 d . . .
O2 O 0.9875(5) 0.0881(5) 0.6671(3) 0.0571(17) Uani 1 1 d U . .
C5 C 0.8563(7) 0.0709(9) 0.7572(4) 0.065(3) Uani 1 1 d . . .
H4 H 0.9287 0.0730 0.7626 0.078 Uiso 1 1 calc R . .
C6 C 0.7890(8) 0.0693(10) 0.8004(3) 0.071(3) Uani 1 1 d . . .
H5 H 0.8164 0.0683 0.8344 0.085 Uiso 1 1 calc R . .
N3 N 0.8041(5) -0.0299(7) 0.3698(2) 0.061(2) Uani 1 1 d . . .
H3 H 0.7440 -0.0323 0.3543 0.073 Uiso 1 1 calc R . .
H2 H 0.8605 -0.0449 0.3526 0.073 Uiso 1 1 calc R . .
C3 C 0.8925(8) 0.0689(7) 0.6612(4) 0.052(2) Uani 1 1 d . . .
O1W O 0.7500 0.7500 0.696(3) 0.85(11) Uani 1 4 d S . .
O2W O 0.7500 0.7500 0.478(4) 1.4(2) 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
C2 0.026(4) 0.037(4) 0.039(4) 0.001(3) 0.001(3) 0.002(3)
N2 0.032(3) 0.038(4) 0.025(3) -0.006(3) 0.000(2) -0.002(3)
N1 0.032(4) 0.043(4) 0.022(3) -0.009(3) 0.003(3) -0.001(3)
C1 0.034(4) 0.057(5) 0.032(4) -0.007(4) -0.003(4) 0.000(4)
N4 0.030(4) 0.050(4) 0.030(3) -0.009(3) 0.004(3) 0.000(3)
Zn1 0.0301(5) 0.0329(5) 0.0229(5) -0.0023(3) 0.0018(3) 0.0016(3)
O1 0.072(5) 0.084(5) 0.039(4) -0.005(3) 0.023(3) -0.007(4)
C4 0.048(5) 0.059(6) 0.028(4) -0.002(4) 0.010(4) 0.001(4)
O2 0.046(4) 0.063(4) 0.062(4) 0.008(3) 0.026(3) 0.006(3)
C5 0.037(5) 0.113(9) 0.044(5) -0.002(5) 0.005(4) 0.003(5)
C6 0.050(6) 0.138(11) 0.025(4) -0.005(5) 0.006(4) 0.001(6)
N3 0.036(4) 0.120(7) 0.028(4) -0.030(4) -0.005(3) 0.012(4)
C3 0.065(7) 0.048(6) 0.043(6) 0.002(4) 0.020(5) -0.002(5)
O1W 1.06(17) 1.06(17) 0.43(12) 0.000 0.000 0.000
O2W 1.9(3) 1.9(3) 0.34(11) 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
C2 N3 1.256(7) . ?
C2 N4 1.4200 . ?
C2 N2 1.4200 . ?
N2 N1 1.4200 . ?
N2 Zn1 1.948(3) 9_756 ?
N1 C1 1.4200 . ?
N1 Zn1 1.995(3) . ?
C1 N4 1.4200 . ?
N4 Zn1 1.995(3) 11_666 ?
Zn1 O1 1.947(6) . ?
Zn1 N2 1.948(8) 9_756 ?
Zn1 N4 1.995(10) 12_656 ?
O1 C3 1.266(11) . ?
C4 C5 1.356(12) . ?
C4 C6 1.373(13) 5_656 ?
C4 C3 1.504(11) . ?
O2 C3 1.239(11) . ?
C5 C6 1.390(12) . ?
C6 C4 1.373(13) 5_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
N3 C2 N4 125.9(4) . . ?
N3 C2 N2 126.0(4) . . ?
N4 C2 N2 108.0 . . ?
N1 N2 C2 108.0 . . ?
N1 N2 Zn1 118.4(2) . 9_756 ?
C2 N2 Zn1 130.2(2) . 9_756 ?
N2 N1 C1 108.0 . . ?
N2 N1 Zn1 131.0(2) . . ?
C1 N1 Zn1 120.1(2) . . ?
N4 C1 N1 108.0 . . ?
C1 N4 C2 108.0 . . ?
C1 N4 Zn1 118.8(2) . 11_666 ?
C2 N4 Zn1 133.2(2) . 11_666 ?
O1 Zn1 N2 132.1(4) . 9_756 ?
O1 Zn1 N1 97.1(2) . . ?
N2 Zn1 N1 105.20(17) 9_756 . ?
O1 Zn1 N4 108.0(4) . 12_656 ?
N2 Zn1 N4 108.4(7) 9_756 12_656 ?
N1 Zn1 N4 101.2(2) . 12_656 ?
C3 O1 Zn1 109.5(6) . . ?
C5 C4 C6 119.3(8) . 5_656 ?
C5 C4 C3 119.9(8) . . ?
C6 C4 C3 120.8(8) 5_656 . ?
C4 C5 C6 121.0(8) . . ?
C4 C6 C5 119.7(8) 5_656 . ?
O2 C3 O1 121.6(8) . . ?
O2 C3 C4 121.2(8) . . ?
O1 C3 C4 117.1(9) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.136


data_30_3
_database_code_depnum_ccdc_archive 'CCDC 917347'
#TrackingRef '3.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H14 N8 O4 Zn2 '
_chemical_formula_sum            'C14 H14 N8 O4 Zn2 '
_chemical_formula_weight         489.11
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   10.203(6)
_cell_length_b                   10.005(6)
_cell_length_c                   18.287(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.560(8)
_cell_angle_gamma                90.00
_cell_volume                     1866.7(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_process_details   SADABS,Bruker(2002)
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8328
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0766
_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       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         24.25
_reflns_number_total             3016
_reflns_number_gt                2330
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.1311P)^2^+0.0000P] 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_number_reflns         3013
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1860
_refine_ls_wR_factor_gt          0.1727
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_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 0.8837(6) -0.1397(7) 0.1991(4) 0.0405(17) Uani 1 1 d . . .
H1 H 0.8496 -0.2007 0.1656 0.049 Uiso 1 1 calc R . .
C3 C 0.6141(6) 0.3719(6) 0.3241(4) 0.0333(15) Uani 1 1 d . . .
C4 C 0.4769(6) 0.2470(6) 0.2658(4) 0.0371(16) Uani 1 1 d . . .
H6 H 0.4012 0.2163 0.2426 0.045 Uiso 1 1 calc R . .
C5 C 0.6453(6) 0.2178(7) 0.0957(4) 0.0378(16) Uani 1 1 d . . .
C6 C 0.5924(8) 0.2985(8) 0.0309(5) 0.056(2) Uani 1 1 d . . .
H8 H 0.6196 0.3909 0.0361 0.068 Uiso 1 1 calc R . .
H7 H 0.6297 0.2641 -0.0139 0.068 Uiso 1 1 calc R . .
C7 C 0.4433(7) 0.2923(7) 0.0255(4) 0.0443(18) Uani 1 1 d . . .
C8 C 0.3625(8) 0.3851(8) 0.0609(4) 0.052(2) Uani 1 1 d . . .
H9 H 0.4009 0.4571 0.0851 0.063 Uiso 1 1 calc R . .
C9 C 0.2266(8) 0.3725(9) 0.0607(5) 0.058(2) Uani 1 1 d . . .
H10 H 0.1762 0.4370 0.0838 0.070 Uiso 1 1 calc R . .
C10 C 0.1653(7) 0.2655(8) 0.0268(4) 0.0429(18) Uani 1 1 d . . .
C13 C 0.2440(7) 0.1723(7) -0.0087(4) 0.0453(18) Uani 1 1 d . . .
H13 H 0.2046 0.0997 -0.0318 0.054 Uiso 1 1 calc R . .
C14 C 0.3805(8) 0.1850(7) -0.0104(4) 0.0459(18) Uani 1 1 d . . .
H14 H 0.4301 0.1222 -0.0354 0.055 Uiso 1 1 calc R . .
C11 C 0.0174(8) 0.2442(11) 0.0311(4) 0.065(2) Uani 1 1 d . . .
H12 H 0.0010 0.1652 0.0604 0.078 Uiso 1 1 calc R . .
H11 H -0.0208 0.3198 0.0564 0.078 Uiso 1 1 calc R . .
C12 C -0.0519(7) 0.2278(8) -0.0418(4) 0.0454(18) Uani 1 1 d . . .
C2 C 1.0140(6) -0.0424(6) 0.2744(4) 0.0330(15) Uani 1 1 d . . .
N5 N 0.6777(5) 0.2573(5) 0.3094(3) 0.0336(13) Uani 1 1 d . . .
N6 N 0.5861(5) 0.1761(5) 0.2719(3) 0.0373(14) Uani 1 1 d . . .
N4 N 0.9029(5) 0.0300(5) 0.2722(3) 0.0336(13) Uani 1 1 d . . .
N1 N 0.8181(5) -0.0345(5) 0.2229(3) 0.0368(14) Uani 1 1 d . . .
N2 N 1.0060(5) -0.1497(5) 0.2286(3) 0.0390(14) Uani 1 1 d . . .
N7 N 0.4878(5) 0.3704(5) 0.2975(3) 0.0344(13) Uani 1 1 d . . .
N8 N 0.6676(6) 0.4780(6) 0.3590(4) 0.0479(16) Uani 1 1 d . . .
H4 H 0.7480 0.4752 0.3736 0.057 Uiso 1 1 calc R . .
H5 H 0.6213 0.5484 0.3667 0.057 Uiso 1 1 calc R . .
N3 N 1.1200(6) -0.0106(6) 0.3168(4) 0.0489(17) Uani 1 1 d . . .
H3 H 1.1182 0.0592 0.3442 0.059 Uiso 1 1 calc R . .
H2 H 1.1887 -0.0603 0.3162 0.059 Uiso 1 1 calc R . .
O1 O 0.5904(4) 0.1023(5) 0.1057(3) 0.0444(12) Uani 1 1 d . . .
O2 O 0.7336(5) 0.2602(6) 0.1358(3) 0.0566(15) Uani 1 1 d . . .
O4 O -0.0360(5) 0.3233(5) -0.0892(3) 0.0470(13) Uani 1 1 d . . .
O3 O -0.1195(7) 0.1301(7) -0.0550(4) 0.085(2) Uani 1 1 d . . .
Zn1 Zn 0.63782(7) 0.02753(7) 0.20143(4) 0.0324(3) Uani 1 1 d . . .
Zn2 Zn 0.86883(7) 0.21402(7) 0.31655(4) 0.0318(3) 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 0.029(4) 0.032(4) 0.061(5) -0.015(3) 0.000(3) 0.001(3)
C3 0.025(3) 0.029(4) 0.046(4) -0.001(3) 0.004(3) 0.003(3)
C4 0.026(4) 0.026(3) 0.059(5) -0.009(3) 0.000(3) -0.003(3)
C5 0.025(4) 0.037(4) 0.052(4) 0.004(3) 0.007(3) -0.001(3)
C6 0.042(5) 0.049(5) 0.079(6) 0.024(4) 0.008(4) -0.006(4)
C7 0.041(4) 0.039(4) 0.054(5) 0.010(3) 0.002(3) 0.000(3)
C8 0.057(5) 0.038(4) 0.062(5) -0.004(4) -0.005(4) 0.001(4)
C9 0.052(5) 0.064(6) 0.060(5) -0.015(4) -0.003(4) 0.019(4)
C10 0.035(4) 0.059(5) 0.035(4) 0.006(4) 0.000(3) 0.000(4)
C13 0.047(5) 0.045(4) 0.044(4) -0.003(4) -0.007(3) -0.011(4)
C14 0.044(4) 0.046(5) 0.047(4) -0.004(4) 0.004(3) 0.009(4)
C11 0.039(5) 0.104(7) 0.051(5) 0.013(5) 0.004(4) -0.008(5)
C12 0.029(4) 0.052(5) 0.056(5) 0.012(4) 0.011(3) 0.002(4)
C2 0.029(4) 0.019(3) 0.051(4) 0.002(3) 0.006(3) 0.005(3)
N5 0.026(3) 0.027(3) 0.048(3) -0.003(3) 0.003(2) 0.003(2)
N6 0.020(3) 0.033(3) 0.059(4) -0.005(3) 0.005(2) -0.001(2)
N4 0.024(3) 0.029(3) 0.048(3) -0.001(3) 0.004(2) 0.002(2)
N1 0.027(3) 0.026(3) 0.057(4) -0.008(3) 0.000(3) 0.000(2)
N2 0.032(3) 0.030(3) 0.056(4) -0.004(3) 0.002(3) 0.004(2)
N7 0.028(3) 0.024(3) 0.051(3) -0.005(2) 0.002(2) 0.004(2)
N8 0.032(3) 0.034(3) 0.078(5) -0.018(3) -0.008(3) 0.001(3)
N3 0.032(3) 0.034(3) 0.080(5) -0.011(3) -0.013(3) 0.005(3)
O1 0.038(3) 0.036(3) 0.059(3) 0.005(2) 0.002(2) -0.010(2)
O2 0.049(3) 0.053(3) 0.068(4) 0.009(3) -0.005(3) -0.019(3)
O4 0.047(3) 0.045(3) 0.049(3) -0.001(2) -0.003(2) 0.001(2)
O3 0.081(5) 0.073(4) 0.099(5) 0.024(4) -0.020(4) -0.041(4)
Zn1 0.0225(5) 0.0257(5) 0.0490(5) -0.0020(3) 0.0015(3) 0.0001(3)
Zn2 0.0218(5) 0.0242(5) 0.0496(5) -0.0005(3) 0.0042(3) -0.0003(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.323(8) . ?
C1 N2 1.357(9) . ?
C3 N5 1.346(8) . ?
C3 N8 1.351(8) . ?
C3 N7 1.374(8) . ?
C4 N6 1.324(8) . ?
C4 N7 1.368(8) . ?
C5 O2 1.232(9) . ?
C5 O1 1.298(8) . ?
C5 C6 1.527(11) . ?
C6 C7 1.525(11) . ?
C7 C8 1.404(11) . ?
C7 C14 1.409(10) . ?
C8 C9 1.392(11) . ?
C9 C10 1.384(11) . ?
C10 C13 1.394(10) . ?
C10 C11 1.527(10) . ?
C13 C14 1.399(11) . ?
C11 C12 1.512(11) . ?
C12 O3 1.220(9) . ?
C12 O4 1.301(9) . ?
C2 N4 1.345(8) . ?
C2 N3 1.362(9) . ?
C2 N2 1.364(8) . ?
N5 N6 1.412(8) . ?
N5 Zn2 2.001(5) . ?
N6 Zn1 2.040(6) . ?
N4 N1 1.401(7) . ?
N4 Zn2 2.043(5) . ?
N1 Zn1 1.977(5) . ?
N2 Zn2 2.048(5) 2_745 ?
N7 Zn1 2.029(5) 2_655 ?
O1 Zn1 1.960(5) . ?
O4 Zn2 2.004(5) 4_465 ?
Zn1 N7 2.029(5) 2_645 ?
Zn2 O4 2.004(5) 4_666 ?
Zn2 N2 2.048(5) 2_755 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 113.2(6) . . ?
N5 C3 N8 124.8(6) . . ?
N5 C3 N7 111.8(6) . . ?
N8 C3 N7 123.3(6) . . ?
N6 C4 N7 112.5(6) . . ?
O2 C5 O1 122.4(7) . . ?
O2 C5 C6 122.0(7) . . ?
O1 C5 C6 115.5(6) . . ?
C7 C6 C5 111.9(6) . . ?
C8 C7 C14 116.9(7) . . ?
C8 C7 C6 122.2(7) . . ?
C14 C7 C6 120.7(7) . . ?
C9 C8 C7 121.9(7) . . ?
C10 C9 C8 121.2(7) . . ?
C9 C10 C13 117.8(7) . . ?
C9 C10 C11 121.8(7) . . ?
C13 C10 C11 120.3(7) . . ?
C10 C13 C14 121.9(7) . . ?
C13 C14 C7 120.4(7) . . ?
C12 C11 C10 115.0(6) . . ?
O3 C12 O4 122.0(7) . . ?
O3 C12 C11 121.3(7) . . ?
O4 C12 C11 116.7(7) . . ?
N4 C2 N3 123.7(6) . . ?
N4 C2 N2 111.1(6) . . ?
N3 C2 N2 125.2(6) . . ?
C3 N5 N6 105.7(5) . . ?
C3 N5 Zn2 130.0(5) . . ?
N6 N5 Zn2 123.2(4) . . ?
C4 N6 N5 106.5(5) . . ?
C4 N6 Zn1 124.1(5) . . ?
N5 N6 Zn1 123.5(4) . . ?
C2 N4 N1 106.6(5) . . ?
C2 N4 Zn2 128.3(4) . . ?
N1 N4 Zn2 124.3(4) . . ?
C1 N1 N4 105.5(5) . . ?
C1 N1 Zn1 131.1(5) . . ?
N4 N1 Zn1 123.4(4) . . ?
C1 N2 C2 103.6(5) . . ?
C1 N2 Zn2 117.6(4) . 2_745 ?
C2 N2 Zn2 137.5(4) . 2_745 ?
C4 N7 C3 103.4(5) . . ?
C4 N7 Zn1 130.9(4) . 2_655 ?
C3 N7 Zn1 125.4(4) . 2_655 ?
C5 O1 Zn1 111.3(5) . . ?
C12 O4 Zn2 112.0(5) . 4_465 ?
O1 Zn1 N1 121.2(2) . . ?
O1 Zn1 N7 98.9(2) . 2_645 ?
N1 Zn1 N7 110.0(2) . 2_645 ?
O1 Zn1 N6 102.9(2) . . ?
N1 Zn1 N6 110.5(2) . . ?
N7 Zn1 N6 113.0(2) 2_645 . ?
N5 Zn2 O4 124.1(2) . 4_666 ?
N5 Zn2 N4 109.8(2) . . ?
O4 Zn2 N4 95.2(2) 4_666 . ?
N5 Zn2 N2 116.2(2) . 2_755 ?
O4 Zn2 N2 99.9(2) 4_666 2_755 ?
N4 Zn2 N2 109.3(2) . 2_755 ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.976
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.166


data_20_4
_database_code_depnum_ccdc_archive 'CCDC 917348'
#TrackingRef '4.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 N8 O15 Zn4 '
_chemical_formula_sum            'C22 H18 N8 O15 Zn4 '
_chemical_formula_weight         896.00
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   22.579(3)
_cell_length_b                   18.542(3)
_cell_length_c                   13.6018(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.614(2)
_cell_angle_gamma                90.00
_cell_volume                     5688.6(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3568
_exptl_absorpt_coefficient_mu    3.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_process_details   SADABS,Bruker(2002)
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14224
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5013
_reflns_number_gt                3478
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0404P)^2^+0.0000P] 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_number_reflns         5004
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
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
Zn3 Zn 0.22577(2) 0.10637(3) 0.43341(4) 0.02571(16) Uani 1 1 d . . .
Zn2 Zn 0.06608(2) 0.10167(3) 0.40870(5) 0.03183(18) Uani 1 1 d . . .
Zn1 Zn 0.13506(2) 0.40624(3) 0.33395(5) 0.02761(17) Uani 1 1 d . . .
Zn4 Zn 0.15303(2) -0.19857(3) 0.33865(5) 0.03275(18) Uani 1 1 d . . .
N3 N 0.11514(16) 0.1900(2) 0.3903(3) 0.0294(10) Uani 1 1 d . . .
N1 N 0.14217(16) 0.30475(18) 0.3779(3) 0.0238(9) Uani 1 1 d . . .
N2 N 0.17671(15) 0.19404(19) 0.4036(3) 0.0261(10) Uani 1 1 d . . .
N4 N 0.04005(17) 0.2760(2) 0.3552(3) 0.0446(13) Uani 1 1 d . . .
H3 H 0.0129 0.2435 0.3524 0.053 Uiso 1 1 calc R . .
H2 H 0.0308 0.3205 0.3457 0.053 Uiso 1 1 calc R . .
C2 C 0.0967(2) 0.2574(2) 0.3745(4) 0.0252(11) Uani 1 1 d . . .
C5 C 0.3388(2) 0.1291(3) 0.3995(4) 0.0254(11) Uani 1 1 d . . .
C6 C 0.4041(2) 0.1219(2) 0.3913(4) 0.0229(11) Uani 1 1 d . . .
C11 C 0.4914(2) 0.0470(2) 0.3788(3) 0.0227(11) Uani 1 1 d . . .
C13 C 0.4303(2) 0.0537(2) 0.3881(3) 0.0254(11) Uani 1 1 d . . .
H9 H 0.4070 0.0126 0.3923 0.031 Uiso 1 1 calc R . .
C10 C 0.5261(2) 0.1089(2) 0.3753(3) 0.0259(11) Uani 1 1 d . . .
H8 H 0.5669 0.1046 0.3700 0.031 Uiso 1 1 calc R . .
C7 C 0.4397(2) 0.1827(2) 0.3882(4) 0.0282(12) Uani 1 1 d . . .
H7 H 0.4226 0.2282 0.3920 0.034 Uiso 1 1 calc R . .
O2 O 0.31356(14) 0.18933(18) 0.3930(3) 0.0395(9) Uani 1 1 d . . .
O1 O 0.30839(14) 0.07365(18) 0.4167(3) 0.0422(10) Uani 1 1 d . . .
N7 N 0.15103(17) -0.09422(19) 0.3681(3) 0.0287(10) Uani 1 1 d . . .
N6 N 0.11673(17) 0.0166(2) 0.3823(3) 0.0317(11) Uani 1 1 d . . .
N5 N 0.17828(16) 0.02036(19) 0.3891(3) 0.0265(10) Uani 1 1 d . . .
C4 C 0.1966(2) -0.0474(2) 0.3810(4) 0.0270(12) Uani 1 1 d . . .
C3 C 0.1030(2) -0.0516(3) 0.3697(4) 0.0375(14) Uani 1 1 d . . .
H4 H 0.0642 -0.0686 0.3628 0.045 Uiso 1 1 calc R . .
O7 O 0.22632(14) 0.08975(16) 0.5843(3) 0.0309(8) Uani 1 1 d . . .
C14 C 0.2474(2) 0.0323(2) 0.6234(4) 0.0253(11) Uani 1 1 d . . .
C15 C 0.2091(2) -0.0330(2) 0.6293(4) 0.0258(11) Uani 1 1 d . . .
C22 C 0.1482(2) -0.0271(2) 0.6279(4) 0.0276(12) Uani 1 1 d . . .
H12 H 0.1307 0.0183 0.6236 0.033 Uiso 1 1 calc R . .
C16 C 0.2350(2) -0.1020(2) 0.6327(4) 0.0306(12) Uani 1 1 d . . .
H10 H 0.2760 -0.1065 0.6337 0.037 Uiso 1 1 calc R . .
C17 C 0.1998(2) -0.1637(2) 0.6346(4) 0.0295(12) Uani 1 1 d . . .
C12 C 0.5208(2) -0.0259(3) 0.3728(3) 0.0268(12) Uani 1 1 d . . .
O6 O 0.49112(14) -0.08186(16) 0.3700(3) 0.0347(9) Uani 1 1 d . . .
O8 O 0.29890(14) 0.02672(17) 0.6607(3) 0.0369(9) Uani 1 1 d . . .
C9 C 0.5390(2) 0.2430(3) 0.3740(4) 0.0326(13) Uani 1 1 d . . .
C8 C 0.5006(2) 0.1768(2) 0.3797(4) 0.0251(11) Uani 1 1 d . . .
O5 O 0.57726(14) -0.02402(17) 0.3704(3) 0.0355(9) Uani 1 1 d . . .
O3 O 0.51867(17) 0.30405(19) 0.3830(4) 0.0695(15) Uani 1 1 d . . .
N8 N 0.25346(19) -0.0669(2) 0.3797(4) 0.0568(15) Uani 1 1 d . . .
H6 H 0.2809 -0.0347 0.3842 0.068 Uiso 1 1 calc R . .
H5 H 0.2627 -0.1117 0.3743 0.068 Uiso 1 1 calc R . .
C1 C 0.1902(2) 0.2622(2) 0.3956(4) 0.0269(12) Uani 1 1 d . . .
H1 H 0.2288 0.2797 0.4014 0.032 Uiso 1 1 calc R . .
C19 C 0.1385(2) -0.1565(3) 0.6358(4) 0.0314(12) Uani 1 1 d . . .
H11 H 0.1149 -0.1975 0.6387 0.038 Uiso 1 1 calc R . .
C18 C 0.2283(2) -0.2374(3) 0.6354(4) 0.0348(13) Uani 1 1 d . . .
O10 O 0.19812(16) -0.29095(18) 0.6507(3) 0.0521(11) Uani 1 1 d . . .
O4 O 0.59273(15) 0.23122(18) 0.3577(3) 0.0506(11) Uani 1 1 d . . .
O9 O 0.28328(15) -0.23770(18) 0.6216(3) 0.0477(11) Uani 1 1 d . . .
C21 C 0.0461(2) -0.0800(3) 0.6294(4) 0.0306(12) Uani 1 1 d . . .
C20 C 0.1120(2) -0.0886(2) 0.6327(4) 0.0279(12) Uani 1 1 d . . .
O11 O 0.01466(15) -0.13654(18) 0.6360(3) 0.0462(11) Uani 1 1 d . . .
O12 O 0.02230(7) -0.02003(9) 0.61629(13) 0.0469(11) Uani 1 1 d . . .
O2W O 0.05892(7) 0.10555(9) 0.55499(13) 0.0424(10) Uani 1 1 d R . .
H2B H 0.0444 0.0659 0.5738 0.051 Uiso 1 1 d R . .
H2A H 0.0344 0.1377 0.5707 0.051 Uiso 1 1 d R . .
O1W O 0.11847(7) 0.39077(9) 0.18963(13) 0.0409(10) Uani 1 1 d R . .
H1B H 0.0833 0.4037 0.1731 0.049 Uiso 1 1 d R . .
H1A H 0.1269 0.3546 0.1533 0.049 Uiso 1 1 d R . .
O3W O 0.15944(7) -0.19012(9) 0.19227(13) 0.0487(10) Uani 1 1 d R . .
H3A H 0.1844 -0.1619 0.1675 0.058 Uiso 1 1 d R . .
H3B H 0.1698 -0.2325 0.1759 0.058 Uiso 1 1 d R . .
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
Zn3 0.0150(3) 0.0139(3) 0.0483(4) 0.0007(3) 0.0031(3) 0.0011(2)
Zn2 0.0155(3) 0.0157(3) 0.0645(5) 0.0019(3) 0.0049(3) 0.0003(2)
Zn1 0.0156(3) 0.0144(3) 0.0528(4) 0.0031(3) 0.0021(3) 0.0006(2)
Zn4 0.0192(3) 0.0147(3) 0.0647(5) -0.0015(3) 0.0058(3) -0.0011(2)
N3 0.014(2) 0.017(2) 0.057(3) 0.0014(19) 0.0013(19) 0.0042(17)
N1 0.014(2) 0.012(2) 0.046(3) 0.0041(18) 0.0025(18) -0.0007(16)
N2 0.008(2) 0.018(2) 0.053(3) 0.0001(19) 0.0028(18) 0.0004(17)
N4 0.014(2) 0.016(2) 0.102(4) 0.006(2) -0.007(2) -0.0027(18)
C2 0.020(3) 0.016(3) 0.039(3) 0.000(2) -0.001(2) 0.001(2)
C5 0.021(3) 0.021(3) 0.035(3) -0.001(2) 0.006(2) -0.005(2)
C6 0.016(3) 0.017(3) 0.036(3) 0.001(2) 0.000(2) 0.000(2)
C11 0.017(3) 0.018(3) 0.032(3) 0.000(2) 0.000(2) 0.000(2)
C13 0.022(3) 0.020(3) 0.035(3) 0.004(2) 0.004(2) -0.005(2)
C10 0.012(2) 0.028(3) 0.038(3) -0.003(2) 0.002(2) 0.001(2)
C7 0.024(3) 0.019(3) 0.042(3) -0.003(2) 0.006(2) 0.004(2)
O2 0.0217(19) 0.029(2) 0.068(3) 0.0055(18) 0.0066(18) 0.0086(17)
O1 0.0130(18) 0.026(2) 0.088(3) 0.0011(19) 0.0094(18) -0.0029(16)
N7 0.019(2) 0.014(2) 0.054(3) -0.0058(19) 0.003(2) -0.0016(18)
N6 0.015(2) 0.019(2) 0.061(3) -0.005(2) 0.000(2) -0.0017(18)
N5 0.017(2) 0.015(2) 0.047(3) -0.0014(18) 0.0041(19) 0.0018(17)
C4 0.018(3) 0.022(3) 0.042(3) 0.000(2) 0.005(2) 0.001(2)
C3 0.016(3) 0.020(3) 0.077(4) -0.003(3) 0.010(3) -0.001(2)
O7 0.026(2) 0.0175(19) 0.049(2) -0.0013(15) 0.0001(17) 0.0006(15)
C14 0.024(3) 0.015(3) 0.038(3) -0.001(2) 0.008(2) -0.001(2)
C15 0.022(3) 0.017(3) 0.038(3) 0.001(2) -0.002(2) 0.001(2)
C22 0.024(3) 0.016(3) 0.043(3) 0.004(2) 0.005(2) 0.001(2)
C16 0.013(3) 0.030(3) 0.050(3) 0.006(2) 0.001(2) 0.002(2)
C17 0.017(3) 0.020(3) 0.051(4) 0.007(2) 0.000(2) 0.001(2)
C12 0.029(3) 0.024(3) 0.027(3) -0.006(2) 0.005(2) 0.005(2)
O6 0.0220(19) 0.0146(18) 0.067(3) -0.0007(17) -0.0021(17) 0.0008(15)
O8 0.0165(19) 0.028(2) 0.066(3) 0.0083(17) -0.0050(18) -0.0054(15)
C9 0.023(3) 0.024(3) 0.052(4) 0.000(2) 0.012(2) -0.003(2)
C8 0.017(3) 0.016(3) 0.043(3) -0.002(2) 0.006(2) 0.002(2)
O5 0.0146(19) 0.0242(19) 0.068(3) 0.0003(17) 0.0065(17) 0.0069(15)
O3 0.037(2) 0.019(2) 0.155(5) -0.009(2) 0.034(3) -0.0032(19)
N8 0.030(3) 0.022(3) 0.120(5) -0.008(3) 0.014(3) 0.000(2)
C1 0.017(3) 0.017(3) 0.047(3) -0.002(2) 0.006(2) -0.006(2)
C19 0.021(3) 0.021(3) 0.052(4) 0.003(2) 0.002(2) -0.001(2)
C18 0.031(3) 0.022(3) 0.052(4) 0.004(2) 0.001(3) 0.005(2)
O10 0.032(2) 0.020(2) 0.107(4) 0.008(2) 0.022(2) -0.0014(17)
O4 0.018(2) 0.026(2) 0.109(4) -0.004(2) 0.011(2) -0.0047(17)
O9 0.022(2) 0.026(2) 0.097(3) 0.010(2) 0.012(2) 0.0062(17)
C21 0.020(3) 0.029(3) 0.042(3) 0.002(2) 0.002(2) -0.002(2)
C20 0.020(3) 0.021(3) 0.043(3) -0.002(2) 0.005(2) -0.003(2)
O11 0.0155(19) 0.027(2) 0.096(3) 0.010(2) -0.0018(19) -0.0068(16)
O12 0.022(2) 0.027(2) 0.092(3) 0.010(2) 0.006(2) 0.0089(17)
O2W 0.034(2) 0.024(2) 0.070(3) 0.0038(18) 0.012(2) 0.0043(16)
O1W 0.033(2) 0.032(2) 0.057(3) -0.0103(17) -0.0006(19) 0.0088(17)
O3W 0.055(3) 0.029(2) 0.063(3) -0.0045(19) 0.021(2) -0.0091(19)
_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
Zn3 O1 1.984(3) . ?
Zn3 N2 1.998(4) . ?
Zn3 N5 2.000(4) . ?
Zn3 O7 2.075(4) . ?
Zn2 N6 1.991(4) . ?
Zn2 N3 1.999(4) . ?
Zn2 O11 2.002(3) 5_556 ?
Zn2 O2W 2.005(2) . ?
Zn2 C21 2.594(5) 5_556 ?
Zn1 O5 1.918(3) 3_455 ?
Zn1 O8 1.940(3) 7_556 ?
Zn1 N1 1.979(3) . ?
Zn1 O1W 2.0023(19) . ?
Zn4 O4 1.910(3) 3_445 ?
Zn4 O9 1.920(3) 7_546 ?
Zn4 N7 1.977(4) . ?
Zn4 O3W 2.0090(19) . ?
N3 C2 1.332(5) . ?
N3 N2 1.396(5) . ?
N1 C2 1.350(5) . ?
N1 C1 1.353(5) . ?
N2 C1 1.305(5) . ?
N4 C2 1.340(6) . ?
N4 H3 0.8600 . ?
N4 H2 0.8600 . ?
C5 O2 1.254(5) . ?
C5 O1 1.264(5) . ?
C5 C6 1.490(6) . ?
C6 C7 1.387(6) . ?
C6 C13 1.398(6) . ?
C11 C10 1.392(6) . ?
C11 C13 1.395(6) . ?
C11 C12 1.510(6) . ?
C13 H9 0.9300 . ?
C10 C8 1.388(6) . ?
C10 H8 0.9300 . ?
C7 C8 1.388(6) . ?
C7 H7 0.9300 . ?
N7 C3 1.343(6) . ?
N7 C4 1.352(5) . ?
N6 C3 1.312(6) . ?
N6 N5 1.390(5) . ?
N5 C4 1.328(5) . ?
C4 N8 1.335(6) . ?
C3 H4 0.9300 . ?
O7 C14 1.273(5) . ?
C14 O8 1.253(5) . ?
C14 C15 1.491(6) . ?
C15 C22 1.381(6) . ?
C15 C16 1.406(6) . ?
C22 C20 1.407(6) . ?
C22 H12 0.9300 . ?
C16 C17 1.394(6) . ?
C16 H10 0.9300 . ?
C17 C19 1.392(6) . ?
C17 C18 1.512(6) . ?
C12 O6 1.235(5) . ?
C12 O5 1.276(5) . ?
O8 Zn1 1.940(3) 7_556 ?
C9 O3 1.231(5) . ?
C9 O4 1.262(6) . ?
C9 C8 1.506(6) . ?
O5 Zn1 1.918(3) 3_545 ?
N8 H6 0.8600 . ?
N8 H5 0.8600 . ?
C1 H1 0.9300 . ?
C19 C20 1.392(6) . ?
C19 H11 0.9300 . ?
C18 O10 1.227(6) . ?
C18 O9 1.264(6) . ?
O4 Zn4 1.910(3) 3 ?
O9 Zn4 1.920(3) 7_546 ?
C21 O12 1.245(5) . ?
C21 O11 1.272(6) . ?
C21 C20 1.494(7) . ?
C21 Zn2 2.594(5) 5_556 ?
O11 Zn2 2.002(3) 5_556 ?
O2W H2B 0.8483 . ?
O2W H2A 0.8484 . ?
O1W H1B 0.8491 . ?
O1W H1A 0.8601 . ?
O3W H3A 0.8499 . ?
O3W H3B 0.8519 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn3 N2 137.81(15) . . ?
O1 Zn3 N5 102.46(14) . . ?
N2 Zn3 N5 107.64(15) . . ?
O1 Zn3 O7 95.99(14) . . ?
N2 Zn3 O7 107.43(15) . . ?
N5 Zn3 O7 99.14(14) . . ?
N6 Zn2 N3 107.47(16) . . ?
N6 Zn2 O11 136.37(16) . 5_556 ?
N3 Zn2 O11 101.52(14) . 5_556 ?
N6 Zn2 O2W 106.26(13) . . ?
N3 Zn2 O2W 99.50(13) . . ?
O11 Zn2 O2W 100.14(13) 5_556 . ?
N6 Zn2 C21 113.90(16) . 5_556 ?
N3 Zn2 C21 130.08(15) . 5_556 ?
O11 Zn2 C21 28.60(14) 5_556 5_556 ?
O2W Zn2 C21 94.67(13) . 5_556 ?
O5 Zn1 O8 95.11(14) 3_455 7_556 ?
O5 Zn1 N1 127.57(15) 3_455 . ?
O8 Zn1 N1 123.13(14) 7_556 . ?
O5 Zn1 O1W 104.53(12) 3_455 . ?
O8 Zn1 O1W 103.74(12) 7_556 . ?
N1 Zn1 O1W 99.72(12) . . ?
O4 Zn4 O9 94.12(15) 3_445 7_546 ?
O4 Zn4 N7 128.09(16) 3_445 . ?
O9 Zn4 N7 124.69(16) 7_546 . ?
O4 Zn4 O3W 105.74(14) 3_445 . ?
O9 Zn4 O3W 103.90(14) 7_546 . ?
N7 Zn4 O3W 97.33(13) . . ?
C2 N3 N2 105.8(4) . . ?
C2 N3 Zn2 128.2(3) . . ?
N2 N3 Zn2 125.6(3) . . ?
C2 N1 C1 103.2(4) . . ?
C2 N1 Zn1 123.9(3) . . ?
C1 N1 Zn1 131.4(3) . . ?
C1 N2 N3 106.0(4) . . ?
C1 N2 Zn3 132.5(3) . . ?
N3 N2 Zn3 121.5(3) . . ?
C2 N4 H3 120.0 . . ?
C2 N4 H2 120.0 . . ?
H3 N4 H2 120.0 . . ?
N3 C2 N4 124.2(4) . . ?
N3 C2 N1 112.0(4) . . ?
N4 C2 N1 123.8(4) . . ?
O2 C5 O1 119.3(4) . . ?
O2 C5 C6 121.5(4) . . ?
O1 C5 C6 119.2(4) . . ?
C7 C6 C13 119.1(4) . . ?
C7 C6 C5 120.4(4) . . ?
C13 C6 C5 120.4(4) . . ?
C10 C11 C13 119.3(4) . . ?
C10 C11 C12 119.0(4) . . ?
C13 C11 C12 121.6(4) . . ?
C11 C13 C6 120.4(4) . . ?
C11 C13 H9 119.8 . . ?
C6 C13 H9 119.8 . . ?
C8 C10 C11 120.8(4) . . ?
C8 C10 H8 119.6 . . ?
C11 C10 H8 119.6 . . ?
C6 C7 C8 121.1(4) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C5 O1 Zn3 107.0(3) . . ?
C3 N7 C4 103.3(4) . . ?
C3 N7 Zn4 127.2(3) . . ?
C4 N7 Zn4 129.1(3) . . ?
C3 N6 N5 106.7(4) . . ?
C3 N6 Zn2 130.8(3) . . ?
N5 N6 Zn2 121.9(3) . . ?
C4 N5 N6 105.1(4) . . ?
C4 N5 Zn3 127.9(3) . . ?
N6 N5 Zn3 125.5(3) . . ?
N5 C4 N8 124.1(4) . . ?
N5 C4 N7 112.4(4) . . ?
N8 C4 N7 123.4(4) . . ?
N6 C3 N7 112.5(4) . . ?
N6 C3 H4 123.8 . . ?
N7 C3 H4 123.8 . . ?
C14 O7 Zn3 121.5(3) . . ?
O8 C14 O7 124.0(4) . . ?
O8 C14 C15 116.2(4) . . ?
O7 C14 C15 119.8(4) . . ?
C22 C15 C16 119.1(4) . . ?
C22 C15 C14 120.9(4) . . ?
C16 C15 C14 120.0(4) . . ?
C15 C22 C20 121.0(4) . . ?
C15 C22 H12 119.5 . . ?
C20 C22 H12 119.5 . . ?
C17 C16 C15 120.7(4) . . ?
C17 C16 H10 119.6 . . ?
C15 C16 H10 119.6 . . ?
C19 C17 C16 119.3(4) . . ?
C19 C17 C18 120.7(4) . . ?
C16 C17 C18 120.0(4) . . ?
O6 C12 O5 124.3(4) . . ?
O6 C12 C11 120.9(4) . . ?
O5 C12 C11 114.8(4) . . ?
C14 O8 Zn1 131.4(3) . 7_556 ?
O3 C9 O4 122.9(5) . . ?
O3 C9 C8 121.7(5) . . ?
O4 C9 C8 115.4(4) . . ?
C10 C8 C7 119.3(4) . . ?
C10 C8 C9 119.7(4) . . ?
C7 C8 C9 121.0(4) . . ?
C12 O5 Zn1 132.8(3) . 3_545 ?
C4 N8 H6 120.0 . . ?
C4 N8 H5 120.0 . . ?
H6 N8 H5 120.0 . . ?
N2 C1 N1 113.1(4) . . ?
N2 C1 H1 123.5 . . ?
N1 C1 H1 123.5 . . ?
C17 C19 C20 120.8(4) . . ?
C17 C19 H11 119.6 . . ?
C20 C19 H11 119.6 . . ?
O10 C18 O9 125.4(5) . . ?
O10 C18 C17 119.6(5) . . ?
O9 C18 C17 115.1(4) . . ?
C9 O4 Zn4 127.1(3) . 3 ?
C18 O9 Zn4 133.5(3) . 7_546 ?
O12 C21 O11 120.5(4) . . ?
O12 C21 C20 121.5(4) . . ?
O11 C21 C20 117.9(4) . . ?
O12 C21 Zn2 72.4(2) . 5_556 ?
O11 C21 Zn2 48.9(2) . 5_556 ?
C20 C21 Zn2 162.0(4) . 5_556 ?
C19 C20 C22 119.0(4) . . ?
C19 C20 C21 121.6(4) . . ?
C22 C20 C21 119.4(4) . . ?
C21 O11 Zn2 102.5(3) . 5_556 ?
Zn2 O2W H2B 108.5 . . ?
Zn2 O2W H2A 111.0 . . ?
H2B O2W H2A 105.5 . . ?
Zn1 O1W H1B 110.5 . . ?
Zn1 O1W H1A 129.7 . . ?
H1B O1W H1A 107.3 . . ?
Zn4 O3W H3A 121.3 . . ?
Zn4 O3W H3B 102.7 . . ?
H3A O3W H3B 105.6 . . ?
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
N8 H6 O1 0.86 2.14 2.921(5) 150.0 .
O2W H2B O12 0.85 1.78 2.620 173.6 .
N8 H5 O10 0.86 2.05 2.890(5) 167.0 7_546
O1W H1B O6 0.85 1.78 2.618(4) 171.6 4
O1W H1A O10 0.86 2.00 2.651(4) 132.2 6
O3W H3A O7 0.85 2.02 2.847(4) 165.4 6
O3W H3B O2 0.85 1.78 2.603(4) 163.3 4_545
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.102


data_30_5
_database_code_depnum_ccdc_archive 'CCDC 917349'
#TrackingRef '5.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N8 O10 Zn3, 3(O) '
_chemical_formula_sum            'C14 H12 N8 O13 Zn3 '
_chemical_formula_weight         696.49
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   7.9770(9)
_cell_length_b                   16.763(2)
_cell_length_c                   15.8519(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.788(2)
_cell_angle_gamma                90.00
_cell_volume                     2082.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    3.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_process_details   SADABS,Bruker(2002)
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5203
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1838
_reflns_number_gt                1608
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0907P)^2^+83.5788P] 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_number_reflns         1835
_refine_ls_number_parameters     169
_refine_ls_number_restraints     611
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0781
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1936
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 0.06447(9) 0.2500 0.0201(4) Uani 1 2 d SU . .
Zn2 Zn 0.57382(15) 0.17562(7) 0.50431(8) 0.0276(4) Uani 1 1 d U . .
C3 C 0.3042(12) 0.0950(6) 0.5014(6) 0.025(2) Uani 1 1 d U . .
O1 O 0.4062(8) 0.0779(4) 0.4528(4) 0.0279(12) Uani 1 1 d U . .
O2 O 0.3325(8) 0.1528(4) 0.5518(4) 0.0265(11) Uani 1 1 d U . .
C5 C 0.0385(11) 0.0622(5) 0.5562(5) 0.0184(18) Uani 1 1 d U . .
H4 H 0.0654 0.1044 0.5945 0.022 Uiso 1 1 calc R . .
C6 C 0.1070(11) -0.0184(5) 0.4419(5) 0.0182(18) Uani 1 1 d U . .
C4 C 0.1470(11) 0.0454(5) 0.4988(5) 0.0188(18) Uani 1 1 d U . .
N1 N 0.7387(9) 0.1709(4) 0.4237(4) 0.0153(15) Uani 1 1 d U . .
N4 N 0.6436(10) 0.0550(5) 0.3402(5) 0.0264(18) Uani 1 1 d U . .
H2 H 0.5578 0.0482 0.3652 0.032 Uiso 1 1 calc R . .
H3 H 0.6606 0.0225 0.3006 0.032 Uiso 1 1 calc R . .
C2 C 0.7522(11) 0.1169(5) 0.3633(5) 0.0162(17) Uani 1 1 d U . .
N3 N 0.8920(9) 0.1308(4) 0.3277(5) 0.0195(16) Uani 1 1 d U . .
C1 C 0.9620(11) 0.1964(5) 0.3688(5) 0.0209(19) Uani 1 1 d U . .
H1 H 1.0609 0.2204 0.3580 0.025 Uiso 1 1 calc R . .
N2 N 0.8753(7) 0.2227(3) 0.4259(4) 0.0171(15) Uani 1 1 d U . .
O1W O 0.3909(7) 0.2406(3) 0.3992(4) 0.0582(15) Uani 1 1 d RU . .
H1A H 0.3324 0.2408 0.4399 0.070 Uiso 1 1 d R . .
H1B H 0.3360 0.2717 0.3617 0.070 Uiso 1 1 d R . .
O2W O 0.0000(7) 0.1909(3) 0.7500(4) 0.176(12) Uani 1 2 d SRU . .
O3 O 0.6893(10) 0.1007(5) 0.6092(5) 0.0386(12) Uani 1 1 d U . .
C7 C 0.7890(13) 0.0423(6) 0.6242(6) 0.0302(16) Uani 1 1 d U . .
O4 O 0.8171(9) 0.0082(4) 0.6967(4) 0.0296(16) Uani 1 1 d U . .
O3W O 0.151(6) 0.344(3) 0.269(4) 0.42(2) 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 0.0270(7) 0.0176(7) 0.0188(7) 0.000 0.0120(5) 0.000
Zn2 0.0277(6) 0.0244(6) 0.0364(6) -0.0130(4) 0.0206(4) -0.0104(4)
C3 0.025(2) 0.025(2) 0.025(2) 0.0008(11) 0.0046(11) -0.0003(11)
O1 0.0267(14) 0.0277(13) 0.0289(15) -0.0015(10) 0.0046(10) -0.0052(10)
O2 0.0236(13) 0.0282(16) 0.0293(15) 0.0005(10) 0.0087(10) -0.0027(10)
C5 0.018(2) 0.018(2) 0.018(2) 0.0000(10) 0.0035(11) -0.0006(10)
C6 0.018(2) 0.018(2) 0.018(2) 0.0006(10) 0.0032(11) -0.0003(10)
C4 0.0187(19) 0.0189(19) 0.0188(19) 0.0003(8) 0.0036(8) -0.0002(8)
N1 0.0151(17) 0.0155(17) 0.0154(17) 0.0001(10) 0.0035(10) -0.0005(10)
N4 0.027(2) 0.026(2) 0.026(2) -0.0011(10) 0.0056(11) -0.0010(10)
C2 0.0163(19) 0.0160(19) 0.0162(19) -0.0002(10) 0.0030(11) 0.0001(10)
N3 0.0198(18) 0.0196(18) 0.0194(18) -0.0003(10) 0.0044(10) 0.0001(10)
C1 0.021(2) 0.021(2) 0.021(2) -0.0002(11) 0.0046(11) -0.0001(11)
N2 0.0170(17) 0.0170(17) 0.0176(17) -0.0004(10) 0.0037(10) -0.0006(10)
O1W 0.0578(17) 0.0581(17) 0.0580(16) 0.0017(10) 0.0094(9) 0.0014(11)
O2W 0.176(12) 0.176(12) 0.176(12) 0.000 0.033(2) 0.000
O3 0.0374(15) 0.0384(14) 0.0413(14) -0.0047(10) 0.0106(10) 0.0019(10)
C7 0.0306(18) 0.0312(17) 0.0293(19) -0.0002(11) 0.0066(11) -0.0028(10)
O4 0.0303(18) 0.0297(18) 0.0292(18) 0.0009(10) 0.0068(10) 0.0010(10)
O3W 0.42(2) 0.42(2) 0.42(2) 0.0000(11) 0.079(5) -0.0002(11)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.966(7) 6 ?
Zn1 O4 1.966(7) 5_756 ?
Zn1 N3 1.973(7) 2_755 ?
Zn1 N3 1.973(7) . ?
Zn2 N1 2.000(7) . ?
Zn2 N2 2.031(6) 7_656 ?
Zn2 O3 2.148(8) . ?
Zn2 O1 2.175(7) . ?
Zn2 O2 2.228(7) . ?
Zn2 O1W 2.276(6) . ?
C3 O2 1.250(12) . ?
C3 O1 1.253(12) . ?
C3 C4 1.498(13) . ?
C5 C6 1.379(12) 5_556 ?
C5 C4 1.396(12) . ?
C6 C5 1.379(12) 5_556 ?
C6 C4 1.398(12) . ?
C6 C7 1.507(13) 5_656 ?
N1 C2 1.336(11) . ?
N1 N2 1.390(9) . ?
N4 C2 1.358(12) . ?
C2 N3 1.361(11) . ?
N3 C1 1.344(12) . ?
C1 N2 1.314(11) . ?
N2 Zn2 2.031(6) 7_656 ?
O3 C7 1.256(13) . ?
C7 O4 1.266(12) . ?
C7 C6 1.507(13) 5_656 ?
O4 Zn1 1.966(7) 5_756 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O4 103.4(4) 6 5_756 ?
O4 Zn1 N3 117.2(3) 6 2_755 ?
O4 Zn1 N3 104.0(3) 5_756 2_755 ?
O4 Zn1 N3 104.0(3) 6 . ?
O4 Zn1 N3 117.2(3) 5_756 . ?
N3 Zn1 N3 111.3(4) 2_755 . ?
N1 Zn2 N2 107.1(3) . 7_656 ?
N1 Zn2 O3 103.5(3) . . ?
N2 Zn2 O3 93.2(3) 7_656 . ?
N1 Zn2 O1 99.3(3) . . ?
N2 Zn2 O1 152.0(3) 7_656 . ?
O3 Zn2 O1 89.7(3) . . ?
N1 Zn2 O2 157.3(3) . . ?
N2 Zn2 O2 93.3(2) 7_656 . ?
O3 Zn2 O2 84.9(3) . . ?
O1 Zn2 O2 59.2(3) . . ?
N1 Zn2 O1W 87.7(2) . . ?
N2 Zn2 O1W 91.8(2) 7_656 . ?
O3 Zn2 O1W 165.8(3) . . ?
O1 Zn2 O1W 79.7(2) . . ?
O2 Zn2 O1W 81.6(2) . . ?
O2 C3 O1 120.7(9) . . ?
O2 C3 C4 119.8(8) . . ?
O1 C3 C4 119.6(8) . . ?
C3 O1 Zn2 91.3(6) . . ?
C3 O2 Zn2 88.9(6) . . ?
C6 C5 C4 122.2(8) 5_556 . ?
C5 C6 C4 119.0(8) 5_556 . ?
C5 C6 C7 116.7(8) 5_556 5_656 ?
C4 C6 C7 124.3(8) . 5_656 ?
C5 C4 C6 118.7(8) . . ?
C5 C4 C3 119.2(8) . . ?
C6 C4 C3 122.0(8) . . ?
C2 N1 N2 105.9(6) . . ?
C2 N1 Zn2 129.5(6) . . ?
N2 N1 Zn2 124.4(5) . . ?
N1 C2 N4 125.3(8) . . ?
N1 C2 N3 111.3(7) . . ?
N4 C2 N3 123.4(8) . . ?
C1 N3 C2 103.7(7) . . ?
C1 N3 Zn1 125.0(6) . . ?
C2 N3 Zn1 130.5(6) . . ?
N2 C1 N3 112.6(8) . . ?
C1 N2 N1 106.4(6) . . ?
C1 N2 Zn2 125.5(5) . 7_656 ?
N1 N2 Zn2 127.9(5) . 7_656 ?
C7 O3 Zn2 140.1(7) . . ?
O3 C7 O4 121.5(10) . . ?
O3 C7 C6 119.1(9) . 5_656 ?
O4 C7 C6 119.0(9) . 5_656 ?
C7 O4 Zn1 131.4(7) . 5_756 ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.120
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.218