# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


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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. 
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data_la1
_database_code_depnum_ccdc_archive 'CCDC 869773'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 La N6 O13.25 Zn3'
_chemical_formula_weight         816.77

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.3969(2)
_cell_length_b                   16.3969(2)
_cell_length_c                   16.3969(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4408.44(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1267
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      24.46

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3124
_exptl_absorpt_coefficient_mu    5.209
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8187
_exptl_absorpt_correction_T_max  0.8187
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13402
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         29.15
_reflns_number_total             1983
_reflns_number_gt                1533
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0400P)^2^+13.4237P] 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         1983
_refine_ls_number_parameters     118
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.758937(17) 0.258937(17) 0.241063(17) 0.00522(13) Uani 1 3 d S . .
Zn1 Zn 0.48624(4) 0.31713(4) 0.20367(4) 0.01230(17) Uani 1 1 d . . .
C1 C 0.4452(4) 0.2462(4) -0.1262(4) 0.0169(12) Uani 1 1 d . . .
C2 C 0.4822(3) 0.2513(4) -0.0428(3) 0.0153(12) Uani 1 1 d . . .
C3 C 0.5589(4) 0.2272(4) -0.0182(4) 0.0207(14) Uani 1 1 d . . .
H3 H 0.6012 0.2034 -0.0498 0.025 Uiso 1 1 calc R . .
C4 C 0.5591(3) 0.2462(3) 0.0630(3) 0.0119(11) Uani 1 1 d . . .
C5 C 0.6216(3) 0.2368(4) 0.1271(3) 0.0138(11) Uani 1 1 d . . .
N1 N 0.4390(3) 0.2827(3) 0.0189(3) 0.0111(10) Uani 1 1 d . . .
N2 N 0.4871(3) 0.2805(3) 0.0852(3) 0.0111(9) Uani 1 1 d . . .
O1 O 0.3691(2) 0.2641(2) -0.1301(2) 0.0142(8) Uani 1 1 d . . .
O2 O 0.4908(3) 0.2256(3) -0.1818(3) 0.0289(12) Uani 1 1 d . . .
O3 O 0.6054(2) 0.2673(2) 0.1967(2) 0.0144(9) Uani 1 1 d . . .
O4 O 0.6876(2) 0.2001(3) 0.1139(2) 0.0167(9) Uani 1 1 d . . .
O5 O 0.6690(3) 0.1690(3) 0.3310(3) 0.056(3) Uani 1 3 d SDU . .
H5A H 0.6618 0.1270 0.3014 0.068 Uiso 0.33 1 d PRD . .
H5B H 0.6907 0.1512 0.3746 0.068 Uiso 0.33 1 d PRD . .
O6 O 0.553(3) 0.053(3) 0.447(3) 0.15(4) Uani 0.25 3 d SP . .
H6A H 0.5234 0.0234 0.4766 0.183 Uiso 0.25 3 d SPR . .
H6B H 0.5448 0.0296 0.3904 0.183 Uiso 0.08 1 d 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
La1 0.00522(13) 0.00522(13) 0.00522(13) -0.00012(10) -0.00012(10) 0.00012(10)
Zn1 0.0120(3) 0.0145(3) 0.0104(3) -0.0010(2) 0.0004(3) 0.0022(3)
C1 0.012(3) 0.027(3) 0.012(3) -0.005(2) -0.001(2) 0.003(2)
C2 0.010(3) 0.028(3) 0.008(2) -0.005(2) -0.006(2) 0.005(2)
C3 0.012(3) 0.034(4) 0.016(3) -0.010(3) 0.001(2) 0.008(3)
C4 0.011(3) 0.015(3) 0.009(3) -0.003(2) -0.006(2) 0.001(2)
C5 0.013(3) 0.017(3) 0.012(3) -0.001(2) -0.007(2) 0.001(2)
N1 0.011(2) 0.014(2) 0.009(2) -0.0052(18) -0.0036(18) 0.0016(18)
N2 0.010(2) 0.013(2) 0.010(2) -0.0023(18) -0.0044(18) 0.0013(18)
O1 0.0084(18) 0.021(2) 0.013(2) -0.0033(17) -0.0035(15) 0.0050(16)
O2 0.013(2) 0.056(3) 0.017(2) -0.014(2) -0.0005(18) 0.008(2)
O3 0.0125(19) 0.021(2) 0.0093(19) -0.0001(17) -0.0028(15) 0.0042(17)
O4 0.013(2) 0.020(2) 0.017(2) -0.0063(17) -0.0083(17) 0.0059(17)
O5 0.056(3) 0.056(3) 0.056(3) 0.014(2) 0.014(2) -0.014(2)
O6 0.15(4) 0.15(4) 0.15(4) -0.12(4) -0.12(4) 0.12(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
La1 O5 2.554(10) . ?
La1 O4 2.579(4) 8_645 ?
La1 O4 2.579(4) . ?
La1 O4 2.579(4) 11_556 ?
La1 O1 2.592(4) 4 ?
La1 O1 2.592(4) 5_655 ?
La1 O1 2.592(4) 10_655 ?
La1 O3 2.623(4) 8_645 ?
La1 O3 2.623(4) 11_556 ?
La1 O3 2.623(4) . ?
La1 C5 2.948(5) . ?
La1 C5 2.948(5) 8_645 ?
Zn1 O2 2.007(4) 15_566 ?
Zn1 N2 2.033(5) . ?
Zn1 N1 2.081(5) 19_656 ?
Zn1 O3 2.122(4) . ?
Zn1 O1 2.156(4) 19_656 ?
C1 O2 1.225(7) . ?
C1 O1 1.283(7) . ?
C1 C2 1.499(8) . ?
C2 N1 1.338(7) . ?
C2 C3 1.380(8) . ?
C3 C4 1.367(8) . ?
C3 H3 0.9500 . ?
C4 N2 1.358(7) . ?
C4 C5 1.476(7) . ?
C5 O4 1.256(7) . ?
C5 O3 1.274(7) . ?
N1 N2 1.344(6) . ?
N1 Zn1 2.081(5) 22_565 ?
O1 Zn1 2.156(4) 22_565 ?
O1 La1 2.591(4) 4_455 ?
O2 Zn1 2.007(4) 15_565 ?
O5 H5A 0.8508 . ?
O5 H5B 0.8513 . ?
O6 H6A 0.8495 . ?
O6 H6B 1.0107 . ?

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
O5 La1 O4 89.38(10) . 8_645 ?
O5 La1 O4 89.38(10) . . ?
O4 La1 O4 119.989(4) 8_645 . ?
O5 La1 O4 89.38(10) . 11_556 ?
O4 La1 O4 119.988(4) 8_645 11_556 ?
O4 La1 O4 119.988(4) . 11_556 ?
O5 La1 O1 136.36(9) . 4 ?
O4 La1 O1 68.44(13) 8_645 4 ?
O4 La1 O1 72.19(12) . 4 ?
O4 La1 O1 134.19(14) 11_556 4 ?
O5 La1 O1 136.36(9) . 5_655 ?
O4 La1 O1 72.19(12) 8_645 5_655 ?
O4 La1 O1 134.18(13) . 5_655 ?
O4 La1 O1 68.44(13) 11_556 5_655 ?
O1 La1 O1 73.40(14) 4 5_655 ?
O5 La1 O1 136.36(9) . 10_655 ?
O4 La1 O1 134.19(14) 8_645 10_655 ?
O4 La1 O1 68.44(13) . 10_655 ?
O4 La1 O1 72.19(12) 11_556 10_655 ?
O1 La1 O1 73.40(14) 4 10_655 ?
O1 La1 O1 73.40(14) 5_655 10_655 ?
O5 La1 O3 68.67(9) . 8_645 ?
O4 La1 O3 50.21(12) 8_645 8_645 ?
O4 La1 O3 74.02(13) . 8_645 ?
O4 La1 O3 154.61(13) 11_556 8_645 ?
O1 La1 O3 68.31(13) 4 8_645 ?
O1 La1 O3 118.82(12) 5_655 8_645 ?
O1 La1 O3 132.63(12) 10_655 8_645 ?
O5 La1 O3 68.67(9) . 11_556 ?
O4 La1 O3 74.02(13) 8_645 11_556 ?
O4 La1 O3 154.61(13) . 11_556 ?
O4 La1 O3 50.21(12) 11_556 11_556 ?
O1 La1 O3 132.63(12) 4 11_556 ?
O1 La1 O3 68.31(13) 5_655 11_556 ?
O1 La1 O3 118.82(12) 10_655 11_556 ?
O3 La1 O3 107.55(9) 8_645 11_556 ?
O5 La1 O3 68.67(9) . . ?
O4 La1 O3 154.61(13) 8_645 . ?
O4 La1 O3 50.21(13) . . ?
O4 La1 O3 74.02(13) 11_556 . ?
O1 La1 O3 118.82(12) 4 . ?
O1 La1 O3 132.63(12) 5_655 . ?
O1 La1 O3 68.31(13) 10_655 . ?
O3 La1 O3 107.55(10) 8_645 . ?
O3 La1 O3 107.55(10) 11_556 . ?
O5 La1 C5 81.59(12) . . ?
O4 La1 C5 143.01(14) 8_645 . ?
O4 La1 C5 25.15(14) . . ?
O4 La1 C5 95.84(14) 11_556 . ?
O1 La1 C5 94.00(14) 4 . ?
O1 La1 C5 135.58(14) 5_655 . ?
O1 La1 C5 62.19(15) 10_655 . ?
O3 La1 C5 93.45(14) 8_645 . ?
O3 La1 C5 133.01(14) 11_556 . ?
O3 La1 C5 25.60(14) . . ?
O5 La1 C5 81.59(12) . 8_645 ?
O4 La1 C5 25.15(14) 8_645 8_645 ?
O4 La1 C5 95.84(14) . 8_645 ?
O4 La1 C5 143.01(14) 11_556 8_645 ?
O1 La1 C5 62.19(15) 4 8_645 ?
O1 La1 C5 94.00(14) 5_655 8_645 ?
O1 La1 C5 135.58(14) 10_655 8_645 ?
O3 La1 C5 25.60(14) 8_645 8_645 ?
O3 La1 C5 93.45(14) 11_556 8_645 ?
O3 La1 C5 133.01(14) . 8_645 ?
C5 La1 C5 117.90(6) . 8_645 ?
O2 Zn1 N2 142.3(2) 15_566 . ?
O2 Zn1 N1 103.0(2) 15_566 19_656 ?
N2 Zn1 N1 112.61(18) . 19_656 ?
O2 Zn1 O3 83.17(17) 15_566 . ?
N2 Zn1 O3 80.14(17) . . ?
N1 Zn1 O3 97.95(17) 19_656 . ?
O2 Zn1 O1 86.66(18) 15_566 19_656 ?
N2 Zn1 O1 110.93(17) . 19_656 ?
N1 Zn1 O1 79.73(16) 19_656 19_656 ?
O3 Zn1 O1 168.79(15) . 19_656 ?
O2 C1 O1 128.3(6) . . ?
O2 C1 C2 116.5(5) . . ?
O1 C1 C2 115.2(5) . . ?
N1 C2 C3 111.8(5) . . ?
N1 C2 C1 119.9(5) . . ?
C3 C2 C1 128.3(5) . . ?
C4 C3 C2 102.8(5) . . ?
C4 C3 H3 128.6 . . ?
C2 C3 H3 128.6 . . ?
N2 C4 C3 110.7(5) . . ?
N2 C4 C5 117.2(5) . . ?
C3 C4 C5 132.2(5) . . ?
O4 C5 O3 121.5(5) . . ?
O4 C5 C4 121.6(5) . . ?
O3 C5 C4 116.9(5) . . ?
O4 C5 La1 60.8(3) . . ?
O3 C5 La1 62.8(3) . . ?
C4 C5 La1 165.6(4) . . ?
C2 N1 N2 106.9(4) . . ?
C2 N1 Zn1 110.8(3) . 22_565 ?
N2 N1 Zn1 140.8(4) . 22_565 ?
N1 N2 C4 107.7(4) . . ?
N1 N2 Zn1 139.6(4) . . ?
C4 N2 Zn1 112.6(3) . . ?
C1 O1 Zn1 113.4(3) . 22_565 ?
C1 O1 La1 132.8(4) . 4_455 ?
Zn1 O1 La1 112.41(16) 22_565 4_455 ?
C1 O2 Zn1 140.2(4) . 15_565 ?
C5 O3 Zn1 113.0(3) . . ?
C5 O3 La1 91.6(3) . . ?
Zn1 O3 La1 152.77(19) . . ?
C5 O4 La1 94.1(3) . . ?
La1 O5 H5A 102.7 . . ?
La1 O5 H5B 116.3 . . ?
H5A O5 H5B 105.0 . . ?
H6A O6 H6B 102.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 171.9(6) . . . . ?
O1 C1 C2 N1 -8.0(9) . . . . ?
O2 C1 C2 C3 -8.0(10) . . . . ?
O1 C1 C2 C3 172.0(6) . . . . ?
N1 C2 C3 C4 0.0(7) . . . . ?
C1 C2 C3 C4 180.0(6) . . . . ?
C2 C3 C4 N2 -0.7(7) . . . . ?
C2 C3 C4 C5 179.8(6) . . . . ?
N2 C4 C5 O4 174.4(5) . . . . ?
C3 C4 C5 O4 -6.1(11) . . . . ?
N2 C4 C5 O3 -5.3(8) . . . . ?
C3 C4 C5 O3 174.1(7) . . . . ?
N2 C4 C5 La1 -90.4(16) . . . . ?
C3 C4 C5 La1 89.1(17) . . . . ?
O5 La1 C5 O4 -106.8(3) . . . . ?
O4 La1 C5 O4 -29.2(4) 8_645 . . . ?
O4 La1 C5 O4 164.7(4) 11_556 . . . ?
O1 La1 C5 O4 29.5(4) 4 . . . ?
O1 La1 C5 O4 99.8(4) 5_655 . . . ?
O1 La1 C5 O4 98.4(4) 10_655 . . . ?
O3 La1 C5 O4 -39.0(4) 8_645 . . . ?
O3 La1 C5 O4 -157.0(3) 11_556 . . . ?
O3 La1 C5 O4 -163.9(6) . . . . ?
C5 La1 C5 O4 -31.0(5) 8_645 . . . ?
O5 La1 C5 O3 57.1(3) . . . . ?
O4 La1 C5 O3 134.8(3) 8_645 . . . ?
O4 La1 C5 O3 163.9(6) . . . . ?
O4 La1 C5 O3 -31.4(3) 11_556 . . . ?
O1 La1 C5 O3 -166.5(3) 4 . . . ?
O1 La1 C5 O3 -96.3(4) 5_655 . . . ?
O1 La1 C5 O3 -97.7(3) 10_655 . . . ?
O3 La1 C5 O3 125.0(4) 8_645 . . . ?
O3 La1 C5 O3 7.0(4) 11_556 . . . ?
C5 La1 C5 O3 132.9(2) 8_645 . . . ?
O5 La1 C5 C4 149.6(16) . . . . ?
O4 La1 C5 C4 -132.8(15) 8_645 . . . ?
O4 La1 C5 C4 -103.6(17) . . . . ?
O4 La1 C5 C4 61.1(16) 11_556 . . . ?
O1 La1 C5 C4 -74.1(16) 4 . . . ?
O1 La1 C5 C4 -3.8(17) 5_655 . . . ?
O1 La1 C5 C4 -5.2(15) 10_655 . . . ?
O3 La1 C5 C4 -142.6(16) 8_645 . . . ?
O3 La1 C5 C4 99.4(16) 11_556 . . . ?
O3 La1 C5 C4 92.5(16) . . . . ?
C5 La1 C5 C4 -134.6(15) 8_645 . . . ?
C3 C2 N1 N2 0.6(7) . . . . ?
C1 C2 N1 N2 -179.3(5) . . . . ?
C3 C2 N1 Zn1 -168.4(5) . . . 22_565 ?
C1 C2 N1 Zn1 11.6(7) . . . 22_565 ?
C2 N1 N2 C4 -1.0(6) . . . . ?
Zn1 N1 N2 C4 162.7(5) 22_565 . . . ?
C2 N1 N2 Zn1 175.1(5) . . . . ?
Zn1 N1 N2 Zn1 -21.2(10) 22_565 . . . ?
C3 C4 N2 N1 1.1(7) . . . . ?
C5 C4 N2 N1 -179.3(5) . . . . ?
C3 C4 N2 Zn1 -176.2(4) . . . . ?
C5 C4 N2 Zn1 3.4(6) . . . . ?
O2 Zn1 N2 N1 118.1(6) 15_566 . . . ?
N1 Zn1 N2 N1 -82.3(6) 19_656 . . . ?
O3 Zn1 N2 N1 -176.9(6) . . . . ?
O1 Zn1 N2 N1 5.0(6) 19_656 . . . ?
O2 Zn1 N2 C4 -66.0(5) 15_566 . . . ?
N1 Zn1 N2 C4 93.7(4) 19_656 . . . ?
O3 Zn1 N2 C4 -0.9(4) . . . . ?
O1 Zn1 N2 C4 -179.1(4) 19_656 . . . ?
O2 C1 O1 Zn1 179.9(6) . . . 22_565 ?
C2 C1 O1 Zn1 -0.1(7) . . . 22_565 ?
O2 C1 O1 La1 14.9(10) . . . 4_455 ?
C2 C1 O1 La1 -165.1(4) . . . 4_455 ?
O1 C1 O2 Zn1 -17.4(13) . . . 15_565 ?
C2 C1 O2 Zn1 162.6(5) . . . 15_565 ?
O4 C5 O3 Zn1 -175.5(4) . . . . ?
C4 C5 O3 Zn1 4.3(7) . . . . ?
La1 C5 O3 Zn1 168.1(3) . . . . ?
O4 C5 O3 La1 16.4(6) . . . . ?
C4 C5 O3 La1 -163.8(5) . . . . ?
O2 Zn1 O3 C5 144.1(4) 15_566 . . . ?
N2 Zn1 O3 C5 -2.0(4) . . . . ?
N1 Zn1 O3 C5 -113.7(4) 19_656 . . . ?
O1 Zn1 O3 C5 169.1(7) 19_656 . . . ?
O2 Zn1 O3 La1 -62.8(4) 15_566 . . . ?
N2 Zn1 O3 La1 151.2(4) . . . . ?
N1 Zn1 O3 La1 39.5(4) 19_656 . . . ?
O1 Zn1 O3 La1 -37.7(11) 19_656 . . . ?
O5 La1 O3 C5 -116.9(3) . . . . ?
O4 La1 O3 C5 -85.1(5) 8_645 . . . ?
O4 La1 O3 C5 -8.8(3) . . . . ?
O4 La1 O3 C5 147.4(4) 11_556 . . . ?
O1 La1 O3 C5 15.4(4) 4 . . . ?
O1 La1 O3 C5 109.0(3) 5_655 . . . ?
O1 La1 O3 C5 70.6(3) 10_655 . . . ?
O3 La1 O3 C5 -59.1(4) 8_645 . . . ?
O3 La1 O3 C5 -174.6(3) 11_556 . . . ?
C5 La1 O3 C5 -62.2(3) 8_645 . . . ?
O5 La1 O3 Zn1 87.7(4) . . . . ?
O4 La1 O3 Zn1 119.5(4) 8_645 . . . ?
O4 La1 O3 Zn1 -164.2(5) . . . . ?
O4 La1 O3 Zn1 -8.0(4) 11_556 . . . ?
O1 La1 O3 Zn1 -140.1(4) 4 . . . ?
O1 La1 O3 Zn1 -46.5(5) 5_655 . . . ?
O1 La1 O3 Zn1 -84.8(4) 10_655 . . . ?
O3 La1 O3 Zn1 145.5(3) 8_645 . . . ?
O3 La1 O3 Zn1 29.9(5) 11_556 . . . ?
C5 La1 O3 Zn1 -155.4(7) . . . . ?
C5 La1 O3 Zn1 142.3(4) 8_645 . . . ?
O3 C5 O4 La1 -16.8(6) . . . . ?
C4 C5 O4 La1 163.5(5) . . . . ?
O5 La1 O4 C5 71.3(3) . . . . ?
O4 La1 O4 C5 160.2(3) 8_645 . . . ?
O4 La1 O4 C5 -17.6(5) 11_556 . . . ?
O1 La1 O4 C5 -148.9(4) 4 . . . ?
O1 La1 O4 C5 -105.9(4) 5_655 . . . ?
O1 La1 O4 C5 -70.2(4) 10_655 . . . ?
O3 La1 O4 C5 139.2(4) 8_645 . . . ?
O3 La1 O4 C5 41.9(5) 11_556 . . . ?
O3 La1 O4 C5 8.9(3) . . . . ?
C5 La1 O4 C5 152.8(4) 8_645 . . . ?

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
O5 H5A O2 0.85 2.58 3.401(5) 163.5 18_655
O5 H5B O2 0.85 2.65 3.401(5) 148.5 21_656
O6 H6A O6 0.85 2.18 3.03(19) 180.0 13_656
O6 H6B N1 1.01 2.53 3.485(7) 156.8 18_655

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.15
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.176


data_0819m
_database_code_depnum_ccdc_archive 'CCDC 869774'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 Ce N6 O13.25 Zn3'
_chemical_formula_weight         817.98

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.3614(5)
_cell_length_b                   16.3614(5)
_cell_length_c                   16.3614(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4379.9(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4505
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      28.96

_exptl_crystal_description       cubic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3132
_exptl_absorpt_coefficient_mu    5.371
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7388
_exptl_absorpt_correction_T_max  0.7388
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26397
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         30.50
_reflns_number_total             2233
_reflns_number_gt                1839
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0219P)^2^+6.3605P] 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         2233
_refine_ls_number_parameters     118
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0563
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.072
_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
Ce1 Ce 0.759726(9) 0.259726(9) 0.240274(9) 0.00533(7) Uani 1 3 d S . .
Zn1 Zn 0.48678(2) 0.31825(2) 0.20320(2) 0.00903(9) Uani 1 1 d . . .
C1 C 0.44616(18) 0.24548(19) -0.12572(19) 0.0149(6) Uani 1 1 d . . .
C2 C 0.48358(18) 0.25083(19) -0.04384(18) 0.0142(6) Uani 1 1 d . . .
C3 C 0.56069(19) 0.2260(2) -0.01863(19) 0.0189(7) Uani 1 1 d . . .
H3 H 0.6029 0.2013 -0.0499 0.023 Uiso 1 1 calc R . .
C4 C 0.56062(17) 0.24626(18) 0.06329(18) 0.0124(6) Uani 1 1 d . . .
C5 C 0.62331(17) 0.23693(18) 0.12697(18) 0.0121(6) Uani 1 1 d . . .
N1 N 0.44021(15) 0.28302(15) 0.01811(14) 0.0106(5) Uani 1 1 d . . .
N2 N 0.48842(14) 0.28099(14) 0.08518(14) 0.0094(5) Uani 1 1 d . . .
O1 O 0.36971(12) 0.26306(13) -0.13037(12) 0.0120(4) Uani 1 1 d . . .
O2 O 0.49180(14) 0.22446(17) -0.18271(14) 0.0251(6) Uani 1 1 d . . .
O3 O 0.60689(12) 0.26840(13) 0.19652(12) 0.0125(4) Uani 1 1 d . . .
O4 O 0.68963(13) 0.20052(13) 0.11437(13) 0.0148(4) Uani 1 1 d . . .
O5 O 0.67000(18) 0.17000(18) 0.33000(18) 0.0537(13) Uani 1 3 d SDU . .
H5A H 0.6714 0.1189 0.3109 0.064 Uiso 0.33 1 d PRD . .
H5B H 0.6983 0.1708 0.3752 0.064 Uiso 0.33 1 d PRD . .
O6 O 0.5609(14) 0.0609(14) 0.4391(14) 0.091(11) Uani 0.25 3 d SP . .
H6A H 0.5115 0.0309 0.4624 0.110 Uiso 0.08 1 d PR . .
H6B H 0.5382 0.0852 0.4117 0.110 Uiso 0.08 1 d 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
Ce1 0.00533(7) 0.00533(7) 0.00533(7) -0.00025(5) -0.00025(5) 0.00025(5)
Zn1 0.00943(16) 0.01046(17) 0.00720(16) -0.00093(12) 0.00039(12) 0.00116(12)
C1 0.0094(13) 0.0238(16) 0.0115(14) -0.0026(12) 0.0002(10) 0.0025(12)
C2 0.0090(13) 0.0220(16) 0.0118(14) -0.0059(12) -0.0016(10) 0.0045(12)
C3 0.0116(15) 0.0314(18) 0.0138(15) -0.0082(13) -0.0039(11) 0.0079(13)
C4 0.0098(13) 0.0167(15) 0.0108(13) -0.0031(11) -0.0032(10) 0.0019(11)
C5 0.0097(13) 0.0124(14) 0.0142(14) -0.0020(11) -0.0047(11) -0.0016(11)
N1 0.0102(12) 0.0146(12) 0.0071(11) -0.0018(9) -0.0014(9) 0.0006(9)
N2 0.0089(11) 0.0107(11) 0.0086(11) -0.0014(9) -0.0016(9) 0.0005(9)
O1 0.0083(9) 0.0187(11) 0.0090(9) -0.0026(8) -0.0031(7) 0.0032(8)
O2 0.0134(11) 0.0495(17) 0.0123(11) -0.0138(11) -0.0011(9) 0.0085(11)
O3 0.0106(10) 0.0173(11) 0.0095(10) -0.0032(8) -0.0028(7) 0.0032(8)
O4 0.0131(11) 0.0165(11) 0.0149(11) -0.0073(8) -0.0056(8) 0.0046(8)
O5 0.0537(13) 0.0537(13) 0.0537(13) 0.0152(11) 0.0152(11) -0.0152(11)
O6 0.091(11) 0.091(11) 0.091(11) -0.048(14) -0.048(14) 0.048(14)

_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
Ce1 O5 2.543(5) . ?
Ce1 O4 2.549(2) 11_556 ?
Ce1 O4 2.549(2) . ?
Ce1 O4 2.549(2) 8_645 ?
Ce1 O1 2.5711(19) 4 ?
Ce1 O1 2.5711(19) 10_655 ?
Ce1 O1 2.5711(19) 5_655 ?
Ce1 O3 2.605(2) 8_645 ?
Ce1 O3 2.605(2) 11_556 ?
Ce1 O3 2.605(2) . ?
Ce1 C5 2.925(3) 11_556 ?
Ce1 C5 2.925(3) 8_645 ?
Zn1 O2 1.995(2) 15_566 ?
Zn1 N2 2.025(2) . ?
Zn1 N1 2.073(2) 19_656 ?
Zn1 O3 2.130(2) . ?
Zn1 O1 2.165(2) 19_656 ?
C1 O2 1.243(4) . ?
C1 O1 1.286(3) . ?
C1 C2 1.475(4) . ?
C2 N1 1.345(4) . ?
C2 C3 1.388(4) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 N2 1.359(4) . ?
C4 C5 1.470(4) . ?
C5 O4 1.255(3) . ?
C5 O3 1.278(3) . ?
N1 N2 1.352(3) . ?
N1 Zn1 2.072(2) 22_565 ?
O1 Zn1 2.165(2) 22_565 ?
O1 Ce1 2.5711(19) 4_455 ?
O2 Zn1 1.995(2) 15_565 ?
O5 H5A 0.8926 . ?
O5 H5B 0.8720 . ?
O6 H6A 1.0194 . ?
O6 H6B 0.7048 . ?

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
O5 Ce1 O4 89.28(5) . 11_556 ?
O5 Ce1 O4 89.28(5) . . ?
O4 Ce1 O4 119.985(2) 11_556 . ?
O5 Ce1 O4 89.28(5) . 8_645 ?
O4 Ce1 O4 119.985(2) 11_556 8_645 ?
O4 Ce1 O4 119.984(2) . 8_645 ?
O5 Ce1 O1 136.40(5) . 4 ?
O4 Ce1 O1 134.25(7) 11_556 4 ?
O4 Ce1 O1 72.22(7) . 4 ?
O4 Ce1 O1 68.59(7) 8_645 4 ?
O5 Ce1 O1 136.40(5) . 10_655 ?
O4 Ce1 O1 72.22(7) 11_556 10_655 ?
O4 Ce1 O1 68.59(7) . 10_655 ?
O4 Ce1 O1 134.25(7) 8_645 10_655 ?
O1 Ce1 O1 73.34(7) 4 10_655 ?
O5 Ce1 O1 136.40(5) . 5_655 ?
O4 Ce1 O1 68.59(7) 11_556 5_655 ?
O4 Ce1 O1 134.25(7) . 5_655 ?
O4 Ce1 O1 72.22(7) 8_645 5_655 ?
O1 Ce1 O1 73.34(7) 4 5_655 ?
O1 Ce1 O1 73.34(7) 10_655 5_655 ?
O5 Ce1 O3 68.65(5) . 8_645 ?
O4 Ce1 O3 154.79(7) 11_556 8_645 ?
O4 Ce1 O3 73.43(7) . 8_645 ?
O4 Ce1 O3 50.71(6) 8_645 8_645 ?
O1 Ce1 O3 68.31(7) 4 8_645 ?
O1 Ce1 O3 132.31(6) 10_655 8_645 ?
O1 Ce1 O3 119.18(6) 5_655 8_645 ?
O5 Ce1 O3 68.65(5) . 11_556 ?
O4 Ce1 O3 50.71(6) 11_556 11_556 ?
O4 Ce1 O3 154.79(7) . 11_556 ?
O4 Ce1 O3 73.43(7) 8_645 11_556 ?
O1 Ce1 O3 132.31(6) 4 11_556 ?
O1 Ce1 O3 119.18(6) 10_655 11_556 ?
O1 Ce1 O3 68.31(7) 5_655 11_556 ?
O3 Ce1 O3 107.53(5) 8_645 11_556 ?
O5 Ce1 O3 68.65(5) . . ?
O4 Ce1 O3 73.43(7) 11_556 . ?
O4 Ce1 O3 50.71(6) . . ?
O4 Ce1 O3 154.79(7) 8_645 . ?
O1 Ce1 O3 119.18(6) 4 . ?
O1 Ce1 O3 68.31(7) 10_655 . ?
O1 Ce1 O3 132.31(6) 5_655 . ?
O3 Ce1 O3 107.53(5) 8_645 . ?
O3 Ce1 O3 107.52(5) 11_556 . ?
O5 Ce1 C5 81.47(6) . 11_556 ?
O4 Ce1 C5 25.32(7) 11_556 11_556 ?
O4 Ce1 C5 143.14(7) . 11_556 ?
O4 Ce1 C5 95.64(7) 8_645 11_556 ?
O1 Ce1 C5 135.62(7) 4 11_556 ?
O1 Ce1 C5 94.14(7) 10_655 11_556 ?
O1 Ce1 C5 62.29(8) 5_655 11_556 ?
O3 Ce1 C5 133.23(7) 8_645 11_556 ?
O3 Ce1 C5 25.89(7) 11_556 11_556 ?
O3 Ce1 C5 93.02(7) . 11_556 ?
O5 Ce1 C5 81.47(6) . 8_645 ?
O4 Ce1 C5 143.14(7) 11_556 8_645 ?
O4 Ce1 C5 95.64(7) . 8_645 ?
O4 Ce1 C5 25.32(7) 8_645 8_645 ?
O1 Ce1 C5 62.29(8) 4 8_645 ?
O1 Ce1 C5 135.62(7) 10_655 8_645 ?
O1 Ce1 C5 94.15(7) 5_655 8_645 ?
O3 Ce1 C5 25.89(7) 8_645 8_645 ?
O3 Ce1 C5 93.02(7) 11_556 8_645 ?
O3 Ce1 C5 133.23(7) . 8_645 ?
C5 Ce1 C5 117.84(3) 11_556 8_645 ?
O2 Zn1 N2 141.84(11) 15_566 . ?
O2 Zn1 N1 103.02(11) 15_566 19_656 ?
N2 Zn1 N1 112.98(9) . 19_656 ?
O2 Zn1 O3 82.87(9) 15_566 . ?
N2 Zn1 O3 79.84(9) . . ?
N1 Zn1 O3 98.40(9) 19_656 . ?
O2 Zn1 O1 86.22(9) 15_566 19_656 ?
N2 Zn1 O1 111.84(9) . 19_656 ?
N1 Zn1 O1 79.44(8) 19_656 19_656 ?
O3 Zn1 O1 168.10(8) . 19_656 ?
O2 C1 O1 127.0(3) . . ?
O2 C1 C2 116.6(3) . . ?
O1 C1 C2 116.4(3) . . ?
N1 C2 C3 111.7(3) . . ?
N1 C2 C1 119.3(3) . . ?
C3 C2 C1 129.0(3) . . ?
C4 C3 C2 102.6(3) . . ?
C4 C3 H3 128.7 . . ?
C2 C3 H3 128.7 . . ?
N2 C4 C3 110.9(3) . . ?
N2 C4 C5 117.6(3) . . ?
C3 C4 C5 131.5(3) . . ?
O4 C5 O3 121.3(3) . . ?
O4 C5 C4 122.4(3) . . ?
O3 C5 C4 116.3(3) . . ?
C2 N1 N2 107.1(2) . . ?
C2 N1 Zn1 111.36(18) . 22_565 ?
N2 N1 Zn1 139.93(19) . 22_565 ?
N1 N2 C4 107.7(2) . . ?
N1 N2 Zn1 139.36(19) . . ?
C4 N2 Zn1 112.87(19) . . ?
C1 O1 Zn1 112.52(18) . 22_565 ?
C1 O1 Ce1 133.62(18) . 4_455 ?
Zn1 O1 Ce1 112.58(8) 22_565 4_455 ?
C1 O2 Zn1 140.7(2) . 15_565 ?
C5 O3 Zn1 113.20(18) . . ?
C5 O3 Ce1 91.20(16) . . ?
Zn1 O3 Ce1 153.16(10) . . ?
C5 O4 Ce1 94.35(17) . . ?
Ce1 O5 H5A 108.9 . . ?
Ce1 O5 H5B 100.1 . . ?
H5A O5 H5B 107.3 . . ?
H6A O6 H6B 95.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 171.7(3) . . . . ?
O1 C1 C2 N1 -8.4(4) . . . . ?
O2 C1 C2 C3 -8.9(5) . . . . ?
O1 C1 C2 C3 171.1(3) . . . . ?
N1 C2 C3 C4 -0.4(4) . . . . ?
C1 C2 C3 C4 -179.9(3) . . . . ?
C2 C3 C4 N2 -0.2(4) . . . . ?
C2 C3 C4 C5 -179.9(3) . . . . ?
N2 C4 C5 O4 174.9(3) . . . . ?
C3 C4 C5 O4 -5.5(5) . . . . ?
N2 C4 C5 O3 -5.4(4) . . . . ?
C3 C4 C5 O3 174.3(3) . . . . ?
C3 C2 N1 N2 0.8(4) . . . . ?
C1 C2 N1 N2 -179.7(3) . . . . ?
C3 C2 N1 Zn1 -167.8(2) . . . 22_565 ?
C1 C2 N1 Zn1 11.7(3) . . . 22_565 ?
C2 N1 N2 C4 -0.9(3) . . . . ?
Zn1 N1 N2 C4 162.5(2) 22_565 . . . ?
C2 N1 N2 Zn1 175.3(2) . . . . ?
Zn1 N1 N2 Zn1 -21.4(5) 22_565 . . . ?
C3 C4 N2 N1 0.7(3) . . . . ?
C5 C4 N2 N1 -179.6(3) . . . . ?
C3 C4 N2 Zn1 -176.6(2) . . . . ?
C5 C4 N2 Zn1 3.1(3) . . . . ?
O2 Zn1 N2 N1 119.1(3) 15_566 . . . ?
N1 Zn1 N2 N1 -81.6(3) 19_656 . . . ?
O3 Zn1 N2 N1 -176.5(3) . . . . ?
O1 Zn1 N2 N1 5.8(3) 19_656 . . . ?
O2 Zn1 N2 C4 -64.9(3) 15_566 . . . ?
N1 Zn1 N2 C4 94.4(2) 19_656 . . . ?
O3 Zn1 N2 C4 -0.52(19) . . . . ?
O1 Zn1 N2 C4 -178.19(19) 19_656 . . . ?
O2 C1 O1 Zn1 -179.7(3) . . . 22_565 ?
C2 C1 O1 Zn1 0.4(3) . . . 22_565 ?
O2 C1 O1 Ce1 14.6(5) . . . 4_455 ?
C2 C1 O1 Ce1 -165.4(2) . . . 4_455 ?
O1 C1 O2 Zn1 -17.2(6) . . . 15_565 ?
C2 C1 O2 Zn1 162.8(3) . . . 15_565 ?
O4 C5 O3 Zn1 -175.6(2) . . . . ?
C4 C5 O3 Zn1 4.7(3) . . . . ?
O4 C5 O3 Ce1 15.9(3) . . . . ?
C4 C5 O3 Ce1 -163.8(2) . . . . ?
O2 Zn1 O3 C5 143.4(2) 15_566 . . . ?
N2 Zn1 O3 C5 -2.4(2) . . . . ?
N1 Zn1 O3 C5 -114.4(2) 19_656 . . . ?
O1 Zn1 O3 C5 167.0(3) 19_656 . . . ?
O2 Zn1 O3 Ce1 -62.8(2) 15_566 . . . ?
N2 Zn1 O3 Ce1 151.4(2) . . . . ?
N1 Zn1 O3 Ce1 39.4(2) 19_656 . . . ?
O1 Zn1 O3 Ce1 -39.2(5) 19_656 . . . ?
O5 Ce1 O3 C5 -116.16(17) . . . . ?
O4 Ce1 O3 C5 147.97(18) 11_556 . . . ?
O4 Ce1 O3 C5 -8.56(16) . . . . ?
O4 Ce1 O3 C5 -85.7(2) 8_645 . . . ?
O1 Ce1 O3 C5 16.08(19) 4 . . . ?
O1 Ce1 O3 C5 70.95(17) 10_655 . . . ?
O1 Ce1 O3 C5 109.77(17) 5_655 . . . ?
O3 Ce1 O3 C5 -58.4(2) 8_645 . . . ?
O3 Ce1 O3 C5 -173.92(15) 11_556 . . . ?
C5 Ce1 O3 C5 164.2(2) 11_556 . . . ?
C5 Ce1 O3 C5 -62.04(13) 8_645 . . . ?
O5 Ce1 O3 Zn1 87.8(2) . . . . ?
O4 Ce1 O3 Zn1 -8.1(2) 11_556 . . . ?
O4 Ce1 O3 Zn1 -164.6(3) . . . . ?
O4 Ce1 O3 Zn1 118.2(2) 8_645 . . . ?
O1 Ce1 O3 Zn1 -140.0(2) 4 . . . ?
O1 Ce1 O3 Zn1 -85.1(2) 10_655 . . . ?
O1 Ce1 O3 Zn1 -46.3(3) 5_655 . . . ?
O3 Ce1 O3 Zn1 145.55(16) 8_645 . . . ?
O3 Ce1 O3 Zn1 30.0(3) 11_556 . . . ?
C5 Ce1 O3 Zn1 8.2(2) 11_556 . . . ?
C5 Ce1 O3 Zn1 141.9(2) 8_645 . . . ?
O3 C5 O4 Ce1 -16.3(3) . . . . ?
C4 C5 O4 Ce1 163.4(3) . . . . ?
O5 Ce1 O4 C5 71.34(18) . . . . ?
O4 Ce1 O4 C5 -17.4(2) 11_556 . . . ?
O4 Ce1 O4 C5 160.09(14) 8_645 . . . ?
O1 Ce1 O4 C5 -148.79(19) 4 . . . ?
O1 Ce1 O4 C5 -70.19(18) 10_655 . . . ?
O1 Ce1 O4 C5 -105.91(19) 5_655 . . . ?
O3 Ce1 O4 C5 139.24(19) 8_645 . . . ?
O3 Ce1 O4 C5 43.2(3) 11_556 . . . ?
O3 Ce1 O4 C5 8.74(17) . . . . ?
C5 Ce1 O4 C5 -3.36(19) 11_556 . . . ?
C5 Ce1 O4 C5 152.7(2) 8_645 . . . ?

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
O5 H5A O2 0.89 2.52 3.395(3) 166.0 18_655
O5 H5B O3 0.87 2.47 2.903(3) 111.0 11_556
O5 H5B O2 0.87 2.52 3.395(3) 175.9 21_656
O6 H6A O6 1.02 2.50 3.45(8) 154.9 13_656

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.122


data_pr1
_database_code_depnum_ccdc_archive 'CCDC 869775'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 N6 O13.25 Pr Zn3'
_chemical_formula_weight         818.77

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.3504(2)
_cell_length_b                   16.3504(2)
_cell_length_c                   16.3504(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4371.04(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6652
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      30.49

_exptl_crystal_description       pyramidal
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3140
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4716
_exptl_absorpt_correction_T_max  0.6079
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23131
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.74
_diffrn_reflns_theta_max         30.49
_reflns_number_total             2225
_reflns_number_gt                1952
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0230P)^2^+7.9982P] 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         2225
_refine_ls_number_parameters     126
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.098
_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
Pr1 Pr 0.239358(8) 0.239358(8) 0.239358(8) 0.00524(7) Uani 1 3 d S . .
Zn1 Zn 0.012716(18) 0.181386(18) 0.296355(18) 0.00948(8) Uani 1 1 d . . .
C1 C 0.12518(16) 0.05344(16) 0.24476(17) 0.0139(5) Uani 1 1 d . . .
C2 C 0.04385(16) 0.01577(16) 0.25042(17) 0.0132(5) Uani 1 1 d . . .
C3 C 0.01797(17) -0.06120(18) 0.2261(2) 0.0192(6) Uani 1 1 d . . .
H3 H 0.0491 -0.1035 0.2012 0.023 Uiso 1 1 calc R . .
C4 C -0.06369(16) -0.06168(16) 0.24680(16) 0.0117(5) Uani 1 1 d . . .
C5 C -0.12736(16) -0.12438(16) 0.23781(15) 0.0110(5) Uani 1 1 d . . .
N1 N -0.01899(13) 0.05930(13) 0.28259(13) 0.0100(4) Uani 1 1 d . . .
N2 N -0.08570(13) 0.01104(13) 0.28105(13) 0.0092(4) Uani 1 1 d . . .
O1 O 0.13010(11) 0.12979(11) 0.26222(11) 0.0123(4) Uani 1 1 d . . .
O2 O 0.18231(13) 0.00716(13) 0.22485(16) 0.0255(5) Uani 1 1 d . . .
O3 O -0.19694(11) -0.10794(11) 0.26976(11) 0.0122(4) Uani 1 1 d . . .
O4 O -0.11465(12) -0.19072(11) 0.20131(12) 0.0144(4) Uani 1 1 d . . .
O5 O 0.32855(17) 0.32855(17) 0.32855(17) 0.0552(15) Uani 1 3 d SD . .
H5A H 0.375(5) 0.306(10) 0.329(7) 0.066 Uiso 0.33 1 d PD . .
H5B H 0.320(9) 0.342(8) 0.378(2) 0.066 Uiso 0.33 1 d PD . .
O6 O 0.4453(4) 0.4453(4) 0.4453(4) 0.114(14) Uani 0.25 3 d SPD . .
H6A H 0.4807(5) 0.4715(3) 0.4715(3) 0.136 Uiso 0.08 1 d PRD . .
H6B H 0.4666(4) 0.40915(7) 0.41759(3) 0.136 Uiso 0.08 1 d PRD . .

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
Pr1 0.00524(7) 0.00524(7) 0.00524(7) 0.00014(4) 0.00014(4) 0.00014(4)
Zn1 0.00999(14) 0.01084(15) 0.00761(14) -0.00087(10) 0.00027(10) 0.00124(11)
C1 0.0090(12) 0.0104(12) 0.0222(13) -0.0025(10) 0.0039(10) -0.0032(9)
C2 0.0090(12) 0.0088(11) 0.0219(14) -0.0041(10) 0.0049(10) -0.0015(9)
C3 0.0138(13) 0.0118(13) 0.0320(16) -0.0079(11) 0.0087(12) -0.0031(10)
C4 0.0113(12) 0.0085(11) 0.0154(12) -0.0028(9) 0.0033(9) -0.0030(9)
C5 0.0111(11) 0.0114(12) 0.0105(11) 0.0008(9) 0.0008(9) -0.0027(9)
N1 0.0082(10) 0.0080(10) 0.0137(10) -0.0003(8) 0.0028(8) -0.0016(8)
N2 0.0076(9) 0.0089(9) 0.0113(10) -0.0008(8) -0.0001(8) -0.0021(8)
O1 0.0093(8) 0.0089(8) 0.0188(9) -0.0027(7) 0.0024(7) -0.0031(7)
O2 0.0131(10) 0.0132(10) 0.0503(15) -0.0099(10) 0.0134(10) -0.0018(8)
O3 0.0078(8) 0.0107(9) 0.0181(9) -0.0016(7) 0.0042(7) -0.0032(7)
O4 0.0144(9) 0.0133(9) 0.0157(9) -0.0052(7) 0.0062(7) -0.0050(7)
O5 0.0552(15) 0.0552(15) 0.0552(15) -0.0233(14) -0.0233(14) -0.0233(14)
O6 0.114(14) 0.114(14) 0.114(14) 0.066(17) 0.066(17) 0.066(17)

_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
Pr1 O5 2.526(5) . ?
Pr1 O4 2.5309(18) 11 ?
Pr1 O4 2.5310(18) 3 ?
Pr1 O4 2.5310(18) 7 ?
Pr1 O1 2.5574(18) 5 ?
Pr1 O1 2.5575(18) . ?
Pr1 O1 2.5575(18) 9 ?
Pr1 O3 2.5956(18) 11 ?
Pr1 O3 2.5956(18) 7 ?
Pr1 O3 2.5956(18) 3 ?
Pr1 C5 2.908(3) 11 ?
Pr1 C5 2.908(3) 3 ?
Zn1 O2 1.998(2) 9 ?
Zn1 N2 2.024(2) 22_566 ?
Zn1 N1 2.075(2) . ?
Zn1 O3 2.1311(18) 22_566 ?
Zn1 O1 2.1695(19) . ?
C1 O2 1.245(3) . ?
C1 O1 1.283(3) . ?
C1 C2 1.469(4) . ?
C2 N1 1.356(3) . ?
C2 C3 1.386(4) . ?
C3 C4 1.377(4) . ?
C3 H3 0.9500 . ?
C4 N2 1.363(3) . ?
C4 C5 1.468(3) . ?
C5 O4 1.255(3) . ?
C5 O3 1.280(3) . ?
C5 Pr1 2.908(3) 3_545 ?
N1 N2 1.347(3) . ?
N2 Zn1 2.024(2) 19_556 ?
O2 Zn1 1.998(2) 5 ?
O3 Zn1 2.1311(18) 19_556 ?
O3 Pr1 2.5955(18) 3_545 ?
O4 Pr1 2.5309(18) 3_545 ?
O5 H5A 0.850(10) . ?
O5 H5B 0.850(10) . ?
O6 H6A 0.8379 . ?
O6 H6B 0.8218 . ?

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
O5 Pr1 O4 89.03(5) . 11 ?
O5 Pr1 O4 89.03(5) . 3 ?
O4 Pr1 O4 119.972(3) 11 3 ?
O5 Pr1 O4 89.03(5) . 7 ?
O4 Pr1 O4 119.970(3) 11 7 ?
O4 Pr1 O4 119.972(3) 3 7 ?
O5 Pr1 O1 136.33(4) . 5 ?
O4 Pr1 O1 68.74(6) 11 5 ?
O4 Pr1 O1 134.57(6) 3 5 ?
O4 Pr1 O1 72.40(6) 7 5 ?
O5 Pr1 O1 136.33(4) . . ?
O4 Pr1 O1 134.57(6) 11 . ?
O4 Pr1 O1 72.40(6) 3 . ?
O4 Pr1 O1 68.74(6) 7 . ?
O1 Pr1 O1 73.45(7) 5 . ?
O5 Pr1 O1 136.33(4) . 9 ?
O4 Pr1 O1 72.40(6) 11 9 ?
O4 Pr1 O1 68.74(6) 3 9 ?
O4 Pr1 O1 134.57(6) 7 9 ?
O1 Pr1 O1 73.45(7) 5 9 ?
O1 Pr1 O1 73.45(7) . 9 ?
O5 Pr1 O3 68.41(4) . 11 ?
O4 Pr1 O3 51.12(6) 11 11 ?
O4 Pr1 O3 154.60(6) 3 11 ?
O4 Pr1 O3 72.88(6) 7 11 ?
O1 Pr1 O3 68.42(6) 5 11 ?
O1 Pr1 O3 132.12(6) . 11 ?
O1 Pr1 O3 119.71(6) 9 11 ?
O5 Pr1 O3 68.41(4) . 7 ?
O4 Pr1 O3 154.60(6) 11 7 ?
O4 Pr1 O3 72.89(6) 3 7 ?
O4 Pr1 O3 51.11(6) 7 7 ?
O1 Pr1 O3 119.71(6) 5 7 ?
O1 Pr1 O3 68.42(6) . 7 ?
O1 Pr1 O3 132.13(6) 9 7 ?
O3 Pr1 O3 107.27(5) 11 7 ?
O5 Pr1 O3 68.41(4) . 3 ?
O4 Pr1 O3 72.89(6) 11 3 ?
O4 Pr1 O3 51.11(6) 3 3 ?
O4 Pr1 O3 154.60(6) 7 3 ?
O1 Pr1 O3 132.12(6) 5 3 ?
O1 Pr1 O3 119.71(6) . 3 ?
O1 Pr1 O3 68.42(6) 9 3 ?
O3 Pr1 O3 107.27(5) 11 3 ?
O3 Pr1 O3 107.27(5) 7 3 ?
O5 Pr1 C5 81.21(5) . 11 ?
O4 Pr1 C5 25.50(6) 11 11 ?
O4 Pr1 C5 143.19(6) 3 11 ?
O4 Pr1 C5 95.41(6) 7 11 ?
O1 Pr1 C5 62.39(7) 5 11 ?
O1 Pr1 C5 135.82(7) . 11 ?
O1 Pr1 C5 94.48(7) 9 11 ?
O3 Pr1 C5 26.12(6) 11 11 ?
O3 Pr1 C5 133.16(7) 7 11 ?
O3 Pr1 C5 92.58(6) 3 11 ?
O5 Pr1 C5 81.21(5) . 3 ?
O4 Pr1 C5 95.41(6) 11 3 ?
O4 Pr1 C5 25.50(6) 3 3 ?
O4 Pr1 C5 143.19(6) 7 3 ?
O1 Pr1 C5 135.82(7) 5 3 ?
O1 Pr1 C5 94.48(7) . 3 ?
O1 Pr1 C5 62.39(7) 9 3 ?
O3 Pr1 C5 133.16(7) 11 3 ?
O3 Pr1 C5 92.58(6) 7 3 ?
O3 Pr1 C5 26.12(6) 3 3 ?
C5 Pr1 C5 117.71(3) 11 3 ?
O2 Zn1 N2 141.33(10) 9 22_566 ?
O2 Zn1 N1 103.28(10) 9 . ?
N2 Zn1 N1 113.08(9) 22_566 . ?
O2 Zn1 O3 82.68(8) 9 22_566 ?
N2 Zn1 O3 79.90(8) 22_566 22_566 ?
N1 Zn1 O3 97.75(8) . 22_566 ?
O2 Zn1 O1 86.47(8) 9 . ?
N2 Zn1 O1 112.03(8) 22_566 . ?
N1 Zn1 O1 79.57(7) . . ?
O3 Zn1 O1 167.92(7) 22_566 . ?
O2 C1 O1 127.0(2) . . ?
O2 C1 C2 116.2(2) . . ?
O1 C1 C2 116.8(2) . . ?
N1 C2 C3 110.9(2) . . ?
N1 C2 C1 119.4(2) . . ?
C3 C2 C1 129.7(2) . . ?
C4 C3 C2 103.3(2) . . ?
C4 C3 H3 128.3 . . ?
C2 C3 H3 128.3 . . ?
N2 C4 C3 110.6(2) . . ?
N2 C4 C5 117.6(2) . . ?
C3 C4 C5 131.8(2) . . ?
O4 C5 O3 121.5(2) . . ?
O4 C5 C4 122.2(2) . . ?
O3 C5 C4 116.3(2) . . ?
O4 C5 Pr1 60.22(13) . 3_545 ?
O3 C5 Pr1 63.19(13) . 3_545 ?
C4 C5 Pr1 165.57(18) . 3_545 ?
N2 N1 C2 107.4(2) . . ?
N2 N1 Zn1 140.21(17) . . ?
C2 N1 Zn1 110.96(16) . . ?
N1 N2 C4 107.8(2) . . ?
N1 N2 Zn1 139.30(17) . 19_556 ?
C4 N2 Zn1 112.84(17) . 19_556 ?
C1 O1 Zn1 112.35(16) . . ?
C1 O1 Pr1 133.85(16) . . ?
Zn1 O1 Pr1 112.53(7) . . ?
C1 O2 Zn1 139.95(19) . 5 ?
C5 O3 Zn1 113.14(16) . 19_556 ?
C5 O3 Pr1 90.68(15) . 3_545 ?
Zn1 O3 Pr1 153.93(8) 19_556 3_545 ?
C5 O4 Pr1 94.28(15) . 3_545 ?
Pr1 O5 H5A 106(10) . . ?
Pr1 O5 H5B 127(10) . . ?
H5A O5 H5B 105.1(17) . . ?
H6A O6 H6B 110.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 170.9(3) . . . . ?
O1 C1 C2 N1 -7.9(4) . . . . ?
O2 C1 C2 C3 -10.1(5) . . . . ?
O1 C1 C2 C3 171.1(3) . . . . ?
N1 C2 C3 C4 -0.9(3) . . . . ?
C1 C2 C3 C4 180.0(3) . . . . ?
C2 C3 C4 N2 0.4(3) . . . . ?
C2 C3 C4 C5 179.9(3) . . . . ?
N2 C4 C5 O4 174.3(2) . . . . ?
C3 C4 C5 O4 -5.2(5) . . . . ?
N2 C4 C5 O3 -6.0(4) . . . . ?
C3 C4 C5 O3 174.5(3) . . . . ?
N2 C4 C5 Pr1 -90.2(8) . . . 3_545 ?
C3 C4 C5 Pr1 90.3(8) . . . 3_545 ?
C3 C2 N1 N2 1.1(3) . . . . ?
C1 C2 N1 N2 -179.7(2) . . . . ?
C3 C2 N1 Zn1 -168.0(2) . . . . ?
C1 C2 N1 Zn1 11.1(3) . . . . ?
O2 Zn1 N1 N2 -87.9(3) 9 . . . ?
N2 Zn1 N1 N2 78.6(3) 22_566 . . . ?
O3 Zn1 N1 N2 -3.7(3) 22_566 . . . ?
O1 Zn1 N1 N2 -171.8(3) . . . . ?
O2 Zn1 N1 C2 75.79(19) 9 . . . ?
N2 Zn1 N1 C2 -117.67(18) 22_566 . . . ?
O3 Zn1 N1 C2 160.05(18) 22_566 . . . ?
O1 Zn1 N1 C2 -8.02(18) . . . . ?
C2 N1 N2 C4 -0.8(3) . . . . ?
Zn1 N1 N2 C4 163.3(2) . . . . ?
C2 N1 N2 Zn1 175.2(2) . . . 19_556 ?
Zn1 N1 N2 Zn1 -20.7(4) . . . 19_556 ?
C3 C4 N2 N1 0.3(3) . . . . ?
C5 C4 N2 N1 -179.4(2) . . . . ?
C3 C4 N2 Zn1 -176.9(2) . . . 19_556 ?
C5 C4 N2 Zn1 3.5(3) . . . 19_556 ?
O2 C1 O1 Zn1 -178.4(3) . . . . ?
C2 C1 O1 Zn1 0.2(3) . . . . ?
O2 C1 O1 Pr1 15.9(5) . . . . ?
C2 C1 O1 Pr1 -165.54(18) . . . . ?
O2 Zn1 O1 C1 -99.92(19) 9 . . . ?
N2 Zn1 O1 C1 115.11(19) 22_566 . . . ?
N1 Zn1 O1 C1 4.28(18) . . . . ?
O3 Zn1 O1 C1 -73.9(4) 22_566 . . . ?
O2 Zn1 O1 Pr1 69.01(10) 9 . . . ?
N2 Zn1 O1 Pr1 -75.97(10) 22_566 . . . ?
N1 Zn1 O1 Pr1 173.21(10) . . . . ?
O3 Zn1 O1 Pr1 95.0(3) 22_566 . . . ?
O5 Pr1 O1 C1 -116.9(2) . . . . ?
O4 Pr1 O1 C1 59.1(3) 11 . . . ?
O4 Pr1 O1 C1 174.1(3) 3 . . . ?
O4 Pr1 O1 C1 -52.6(2) 7 . . . ?
O1 Pr1 O1 C1 24.5(2) 5 . . . ?
O1 Pr1 O1 C1 101.7(2) 9 . . . ?
O3 Pr1 O1 C1 -13.7(3) 11 . . . ?
O3 Pr1 O1 C1 -107.8(3) 7 . . . ?
O3 Pr1 O1 C1 154.0(2) 3 . . . ?
C5 Pr1 O1 C1 22.6(3) 11 . . . ?
C5 Pr1 O1 C1 161.2(2) 3 . . . ?
O5 Pr1 O1 Zn1 77.37(9) . . . . ?
O4 Pr1 O1 Zn1 -106.69(9) 11 . . . ?
O4 Pr1 O1 Zn1 8.35(8) 3 . . . ?
O4 Pr1 O1 Zn1 141.65(10) 7 . . . ?
O1 Pr1 O1 Zn1 -141.22(8) 5 . . . ?
O1 Pr1 O1 Zn1 -64.03(11) 9 . . . ?
O3 Pr1 O1 Zn1 -179.40(6) 11 . . . ?
O3 Pr1 O1 Zn1 86.43(8) 7 . . . ?
O3 Pr1 O1 Zn1 -11.72(11) 3 . . . ?
C5 Pr1 O1 Zn1 -143.14(9) 11 . . . ?
C5 Pr1 O1 Zn1 -4.58(9) 3 . . . ?
O1 C1 O2 Zn1 -19.4(6) . . . 5 ?
C2 C1 O2 Zn1 162.0(2) . . . 5 ?
O4 C5 O3 Zn1 -175.1(2) . . . 19_556 ?
C4 C5 O3 Zn1 5.2(3) . . . 19_556 ?
Pr1 C5 O3 Zn1 169.11(14) 3_545 . . 19_556 ?
O4 C5 O3 Pr1 15.8(3) . . . 3_545 ?
C4 C5 O3 Pr1 -163.9(2) . . . 3_545 ?
O3 C5 O4 Pr1 -16.2(3) . . . 3_545 ?
C4 C5 O4 Pr1 163.4(2) . . . 3_545 ?

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
O5 H5A O2 0.850(10) 2.54(3) 3.381(3) 173(17) 24_656
O5 H5B O2 0.850(10) 2.65(10) 3.381(3) 145(14) 20_566
O6 H6A O6 0.84 2.27 3.10(2) 168.4 13_666

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.118


data_sm1
_database_code_depnum_ccdc_archive 'CCDC 869776'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 N6 O13.25 Sm Zn3'
_chemical_formula_weight         828.21

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.30280(10)
_cell_length_b                   16.30280(10)
_cell_length_c                   16.30280(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4332.98(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3452
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.98

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3164
_exptl_absorpt_coefficient_mu    6.038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6437
_exptl_absorpt_correction_T_max  0.6437
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21914
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.75
_diffrn_reflns_theta_max         30.50
_reflns_number_total             2207
_reflns_number_gt                1716
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0205P)^2^+11.0328P] 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         2207
_refine_ls_number_parameters     124
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0664
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.237160(10) 0.237160(10) 0.237160(10) 0.00546(8) Uani 1 3 d S . .
Zn1 Zn 0.29594(2) 0.01171(2) 0.18027(2) 0.00978(11) Uani 1 1 d . . .
C1 C 0.2439(2) 0.1246(2) 0.0522(2) 0.0139(7) Uani 1 1 d . . .
C2 C 0.2500(2) 0.0436(2) 0.0144(2) 0.0146(8) Uani 1 1 d . . .
C3 C 0.2260(2) 0.0174(2) -0.0634(2) 0.0177(8) Uani 1 1 d . . .
H3 H 0.2011 0.0485 -0.1059 0.021 Uiso 1 1 calc R . .
C4 C 0.2471(2) -0.0643(2) -0.0637(2) 0.0122(7) Uani 1 1 d . . .
C5 C 0.2394(2) -0.1279(2) -0.1269(2) 0.0103(7) Uani 1 1 d . . .
N1 N 0.28227(18) -0.01946(17) 0.05791(18) 0.0100(6) Uani 1 1 d . . .
N2 N 0.28128(17) -0.08591(17) 0.00931(18) 0.0095(6) Uani 1 1 d . . .
O1 O 0.25994(15) 0.12970(15) 0.12908(14) 0.0117(5) Uani 1 1 d . . .
O2 O 0.22435(19) 0.18198(17) 0.00544(16) 0.0241(7) Uani 1 1 d . . .
O3 O 0.27239(15) -0.19724(15) -0.11093(15) 0.0127(5) Uani 1 1 d . . .
O4 O 0.20301(15) -0.11546(15) -0.19354(15) 0.0134(5) Uani 1 1 d . . .
O5 O 0.32517(18) 0.32517(18) 0.32517(18) 0.0461(17) Uani 1 3 d SD . .
H5A H 0.292(6) 0.316(9) 0.364(3) 0.055 Uiso 0.33 1 d PD . .
H5B H 0.3552(4) 0.3552(4) 0.3552(4) 0.055 Uiso 1 3 d SD . .
O6 O 0.4493(11) 0.4493(11) 0.4493(11) 0.15(2) Uani 0.25 3 d SPD . .
H6A H 0.4998(14) 0.4498(4) 0.4627(5) 0.179 Uiso 0.08 1 d PRD . .
H6B H 0.4260(10) 0.4344(3) 0.49499(17) 0.179 Uiso 0.08 1 d PRD . .

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
Sm1 0.00546(8) 0.00546(8) 0.00546(8) 0.00023(6) 0.00023(6) 0.00023(6)
Zn1 0.0083(2) 0.0103(2) 0.0107(2) 0.00108(16) -0.00079(16) 0.00042(15)
C1 0.0209(19) 0.0090(17) 0.0118(17) -0.0034(14) -0.0018(15) 0.0022(14)
C2 0.022(2) 0.0104(17) 0.0118(17) -0.0004(14) -0.0048(15) 0.0052(14)
C3 0.027(2) 0.0134(18) 0.0131(18) -0.0008(15) -0.0077(16) 0.0076(16)
C4 0.0170(19) 0.0114(17) 0.0083(16) -0.0009(14) -0.0025(14) 0.0028(14)
C5 0.0110(16) 0.0102(16) 0.0096(16) -0.0015(13) 0.0008(14) -0.0002(13)
N1 0.0115(15) 0.0071(14) 0.0114(15) -0.0011(11) -0.0013(12) 0.0013(11)
N2 0.0104(14) 0.0068(14) 0.0114(14) -0.0017(11) 0.0010(11) 0.0027(11)
O1 0.0178(13) 0.0087(12) 0.0087(12) -0.0032(9) -0.0024(10) 0.0021(10)
O2 0.045(2) 0.0136(14) 0.0141(14) -0.0002(11) -0.0096(13) 0.0138(13)
O3 0.0173(13) 0.0102(12) 0.0108(12) -0.0018(10) -0.0028(10) 0.0025(10)
O4 0.0152(13) 0.0130(13) 0.0119(13) -0.0035(10) -0.0060(10) 0.0060(10)
O5 0.0461(17) 0.0461(17) 0.0461(17) -0.0196(15) -0.0196(15) -0.0196(15)
O6 0.15(2) 0.15(2) 0.15(2) 0.10(3) 0.10(3) 0.10(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
Sm1 O4 2.483(2) 2 ?
Sm1 O4 2.483(2) 6 ?
Sm1 O4 2.483(2) 10 ?
Sm1 O5 2.485(5) . ?
Sm1 O1 2.512(2) 9 ?
Sm1 O1 2.512(2) 5 ?
Sm1 O1 2.512(2) . ?
Sm1 O3 2.565(2) 6 ?
Sm1 O3 2.565(2) 10 ?
Sm1 O3 2.565(2) 2 ?
Sm1 C5 2.869(3) 6 ?
Sm1 C5 2.869(3) 10 ?
Sm1 H5A 2.60(3) . ?
Zn1 O2 1.994(3) 9 ?
Zn1 N2 2.026(3) 24_656 ?
Zn1 N1 2.071(3) . ?
Zn1 O3 2.146(2) 24_656 ?
Zn1 O1 2.177(2) . ?
C1 O2 1.248(4) . ?
C1 O1 1.282(4) . ?
C1 C2 1.462(5) . ?
C2 N1 1.355(5) . ?
C2 C3 1.395(5) . ?
C3 C4 1.376(5) . ?
C3 H3 0.9500 . ?
C4 N2 1.360(4) . ?
C4 C5 1.468(5) . ?
C5 O4 1.255(4) . ?
C5 O3 1.278(4) . ?
C5 Sm1 2.869(3) 2_554 ?
N1 N2 1.342(4) . ?
N2 Zn1 2.026(3) 18_655 ?
O2 Zn1 1.994(3) 5 ?
O3 Zn1 2.146(2) 18_655 ?
O3 Sm1 2.565(2) 2_554 ?
O4 Sm1 2.483(2) 2_554 ?
O5 H5A 0.851(10) . ?
O5 H5B 0.848(10) . ?
O6 H6A 0.8503 . ?
O6 H6B 0.8706 . ?

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 Sm1 O4 119.922(6) 2 6 ?
O4 Sm1 O4 119.922(6) 2 10 ?
O4 Sm1 O4 119.921(6) 6 10 ?
O4 Sm1 O5 88.39(6) 2 . ?
O4 Sm1 O5 88.39(6) 6 . ?
O4 Sm1 O5 88.39(6) 10 . ?
O4 Sm1 O1 69.28(8) 2 9 ?
O4 Sm1 O1 135.31(8) 6 9 ?
O4 Sm1 O1 72.77(8) 10 9 ?
O5 Sm1 O1 136.24(6) . 9 ?
O4 Sm1 O1 135.31(8) 2 5 ?
O4 Sm1 O1 72.77(8) 6 5 ?
O4 Sm1 O1 69.28(8) 10 5 ?
O5 Sm1 O1 136.24(6) . 5 ?
O1 Sm1 O1 73.60(9) 9 5 ?
O4 Sm1 O1 72.77(8) 2 . ?
O4 Sm1 O1 69.28(8) 6 . ?
O4 Sm1 O1 135.31(8) 10 . ?
O5 Sm1 O1 136.23(6) . . ?
O1 Sm1 O1 73.60(9) 9 . ?
O1 Sm1 O1 73.60(9) 5 . ?
O4 Sm1 O3 71.80(8) 2 6 ?
O4 Sm1 O3 51.82(8) 6 6 ?
O4 Sm1 O3 153.99(8) 10 6 ?
O5 Sm1 O3 67.92(6) . 6 ?
O1 Sm1 O3 131.92(8) 9 6 ?
O1 Sm1 O3 120.61(8) 5 6 ?
O1 Sm1 O3 68.72(8) . 6 ?
O4 Sm1 O3 153.99(8) 2 10 ?
O4 Sm1 O3 71.80(8) 6 10 ?
O4 Sm1 O3 51.81(8) 10 10 ?
O5 Sm1 O3 67.92(6) . 10 ?
O1 Sm1 O3 120.61(8) 9 10 ?
O1 Sm1 O3 68.72(8) 5 10 ?
O1 Sm1 O3 131.92(8) . 10 ?
O3 Sm1 O3 106.75(6) 6 10 ?
O4 Sm1 O3 51.82(8) 2 2 ?
O4 Sm1 O3 153.99(8) 6 2 ?
O4 Sm1 O3 71.80(8) 10 2 ?
O5 Sm1 O3 67.92(6) . 2 ?
O1 Sm1 O3 68.72(8) 9 2 ?
O1 Sm1 O3 131.92(8) 5 2 ?
O1 Sm1 O3 120.61(8) . 2 ?
O3 Sm1 O3 106.74(6) 6 2 ?
O3 Sm1 O3 106.74(6) 10 2 ?
O4 Sm1 C5 94.89(9) 2 6 ?
O4 Sm1 C5 25.85(9) 6 6 ?
O4 Sm1 C5 143.20(9) 10 6 ?
O5 Sm1 C5 80.52(7) . 6 ?
O1 Sm1 C5 136.38(9) 9 6 ?
O1 Sm1 C5 95.13(9) 5 6 ?
O1 Sm1 C5 62.83(9) . 6 ?
O3 Sm1 C5 26.45(9) 6 6 ?
O3 Sm1 C5 91.71(9) 10 6 ?
O3 Sm1 C5 132.83(9) 2 6 ?
O4 Sm1 C5 143.20(9) 2 10 ?
O4 Sm1 C5 94.89(9) 6 10 ?
O4 Sm1 C5 25.85(9) 10 10 ?
O5 Sm1 C5 80.52(7) . 10 ?
O1 Sm1 C5 95.13(9) 9 10 ?
O1 Sm1 C5 62.83(9) 5 10 ?
O1 Sm1 C5 136.38(9) . 10 ?
O3 Sm1 C5 132.83(9) 6 10 ?
O3 Sm1 C5 26.45(9) 10 10 ?
O3 Sm1 C5 91.71(9) 2 10 ?
C5 Sm1 C5 117.34(4) 6 10 ?
O4 Sm1 H5A 84(4) 2 . ?
O4 Sm1 H5A 106.7(12) 6 . ?
O4 Sm1 H5A 75(3) 10 . ?
O5 Sm1 H5A 19.1(3) . . ?
O1 Sm1 H5A 117.9(10) 9 . ?
O1 Sm1 H5A 136(4) 5 . ?
O1 Sm1 H5A 149(3) . . ?
O3 Sm1 H5A 84(2) 6 . ?
O3 Sm1 H5A 70(4) 10 . ?
O3 Sm1 H5A 51(2) 2 . ?
C5 Sm1 H5A 99.5(6) 6 . ?
C5 Sm1 H5A 74(4) 10 . ?
O2 Zn1 N2 140.63(13) 9 24_656 ?
O2 Zn1 N1 103.55(12) 9 . ?
N2 Zn1 N1 113.31(11) 24_656 . ?
O2 Zn1 O3 82.59(11) 9 24_656 ?
N2 Zn1 O3 79.72(10) 24_656 24_656 ?
N1 Zn1 O3 97.09(10) . 24_656 ?
O2 Zn1 O1 86.12(11) 9 . ?
N2 Zn1 O1 113.07(11) 24_656 . ?
N1 Zn1 O1 79.55(10) . . ?
O3 Zn1 O1 167.13(9) 24_656 . ?
O2 C1 O1 127.0(3) . . ?
O2 C1 C2 115.9(3) . . ?
O1 C1 C2 117.1(3) . . ?
N1 C2 C3 110.7(3) . . ?
N1 C2 C1 119.5(3) . . ?
C3 C2 C1 129.9(3) . . ?
C4 C3 C2 103.2(3) . . ?
C4 C3 H3 128.4 . . ?
C2 C3 H3 128.4 . . ?
N2 C4 C3 110.5(3) . . ?
N2 C4 C5 117.8(3) . . ?
C3 C4 C5 131.7(3) . . ?
O4 C5 O3 121.2(3) . . ?
O4 C5 C4 122.3(3) . . ?
O3 C5 C4 116.5(3) . . ?
O4 C5 Sm1 59.63(17) . 2_554 ?
O3 C5 Sm1 63.41(18) . 2_554 ?
C4 C5 Sm1 165.9(2) . 2_554 ?
N2 N1 C2 107.4(3) . . ?
N2 N1 Zn1 140.2(2) . . ?
C2 N1 Zn1 111.1(2) . . ?
N1 N2 C4 108.2(3) . . ?
N1 N2 Zn1 138.8(2) . 18_655 ?
C4 N2 Zn1 112.9(2) . 18_655 ?
C1 O1 Zn1 111.9(2) . . ?
C1 O1 Sm1 134.4(2) . . ?
Zn1 O1 Sm1 112.77(10) . . ?
C1 O2 Zn1 139.3(3) . 5 ?
C5 O3 Zn1 112.7(2) . 18_655 ?
C5 O3 Sm1 90.1(2) . 2_554 ?
Zn1 O3 Sm1 155.24(12) 18_655 2_554 ?
C5 O4 Sm1 94.5(2) . 2_554 ?
Sm1 O5 H5A 88(2) . . ?
Sm1 O5 H5B 180.0(10) . . ?
H5A O5 H5B 92(2) . . ?
H6A O6 H6B 101.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 170.4(3) . . . . ?
O1 C1 C2 N1 -8.7(5) . . . . ?
O2 C1 C2 C3 -10.6(6) . . . . ?
O1 C1 C2 C3 170.3(4) . . . . ?
N1 C2 C3 C4 -0.9(4) . . . . ?
C1 C2 C3 C4 -179.9(4) . . . . ?
C2 C3 C4 N2 0.2(4) . . . . ?
C2 C3 C4 C5 -179.3(4) . . . . ?
N2 C4 C5 O4 174.4(3) . . . . ?
C3 C4 C5 O4 -6.2(6) . . . . ?
N2 C4 C5 O3 -6.1(5) . . . . ?
C3 C4 C5 O3 173.4(4) . . . . ?
N2 C4 C5 Sm1 -92.2(10) . . . 2_554 ?
C3 C4 C5 Sm1 87.3(11) . . . 2_554 ?
C3 C2 N1 N2 1.2(4) . . . . ?
C1 C2 N1 N2 -179.6(3) . . . . ?
C3 C2 N1 Zn1 -168.3(3) . . . . ?
C1 C2 N1 Zn1 10.9(4) . . . . ?
O2 Zn1 N1 N2 -88.2(4) 9 . . . ?
N2 Zn1 N1 N2 77.7(4) 24_656 . . . ?
O3 Zn1 N1 N2 -4.1(4) 24_656 . . . ?
O1 Zn1 N1 N2 -171.6(4) . . . . ?
O2 Zn1 N1 C2 76.1(3) 9 . . . ?
N2 Zn1 N1 C2 -118.1(3) 24_656 . . . ?
O3 Zn1 N1 C2 160.1(2) 24_656 . . . ?
O1 Zn1 N1 C2 -7.3(2) . . . . ?
C2 N1 N2 C4 -1.1(4) . . . . ?
Zn1 N1 N2 C4 163.5(3) . . . . ?
C2 N1 N2 Zn1 175.3(3) . . . 18_655 ?
Zn1 N1 N2 Zn1 -20.1(6) . . . 18_655 ?
C3 C4 N2 N1 0.6(4) . . . . ?
C5 C4 N2 N1 -179.9(3) . . . . ?
C3 C4 N2 Zn1 -176.9(3) . . . 18_655 ?
C5 C4 N2 Zn1 2.7(4) . . . 18_655 ?
O2 C1 O1 Zn1 -177.4(3) . . . . ?
C2 C1 O1 Zn1 1.6(4) . . . . ?
O2 C1 O1 Sm1 14.8(6) . . . . ?
C2 C1 O1 Sm1 -166.1(2) . . . . ?
O2 Zn1 O1 C1 -101.4(3) 9 . . . ?
N2 Zn1 O1 C1 114.1(2) 24_656 . . . ?
N1 Zn1 O1 C1 3.1(2) . . . . ?
O3 Zn1 O1 C1 -72.8(5) 24_656 . . . ?
O2 Zn1 O1 Sm1 69.08(12) 9 . . . ?
N2 Zn1 O1 Sm1 -75.34(13) 24_656 . . . ?
N1 Zn1 O1 Sm1 173.64(13) . . . . ?
O3 Zn1 O1 Sm1 97.8(4) 24_656 . . . ?
O4 Sm1 O1 C1 175.9(3) 2 . . . ?
O4 Sm1 O1 C1 -51.6(3) 6 . . . ?
O4 Sm1 O1 C1 60.5(3) 10 . . . ?
O5 Sm1 O1 C1 -115.6(3) . . . . ?
O1 Sm1 O1 C1 103.0(3) 9 . . . ?
O1 Sm1 O1 C1 25.7(3) 5 . . . ?
O3 Sm1 O1 C1 -107.4(3) 6 . . . ?
O3 Sm1 O1 C1 -13.7(4) 10 . . . ?
O3 Sm1 O1 C1 155.2(3) 2 . . . ?
C5 Sm1 O1 C1 -79.1(3) 6 . . . ?
C5 Sm1 O1 C1 23.0(4) 10 . . . ?
O4 Sm1 O1 Zn1 8.22(10) 2 . . . ?
O4 Sm1 O1 Zn1 140.73(13) 6 . . . ?
O4 Sm1 O1 Zn1 -107.19(12) 10 . . . ?
O5 Sm1 O1 Zn1 76.73(12) . . . . ?
O1 Sm1 O1 Zn1 -64.63(14) 9 . . . ?
O1 Sm1 O1 Zn1 -141.91(10) 5 . . . ?
O3 Sm1 O1 Zn1 84.92(11) 6 . . . ?
O3 Sm1 O1 Zn1 178.69(9) 10 . . . ?
O3 Sm1 O1 Zn1 -12.48(14) 2 . . . ?
C5 Sm1 O1 Zn1 113.27(14) 6 . . . ?
C5 Sm1 O1 Zn1 -144.62(12) 10 . . . ?
O1 C1 O2 Zn1 -19.1(7) . . . 5 ?
C2 C1 O2 Zn1 161.8(3) . . . 5 ?
O4 C5 O3 Zn1 -174.4(3) . . . 18_655 ?
C4 C5 O3 Zn1 6.0(4) . . . 18_655 ?
Sm1 C5 O3 Zn1 170.28(19) 2_554 . . 18_655 ?
O4 C5 O3 Sm1 15.3(3) . . . 2_554 ?
C4 C5 O3 Sm1 -164.3(3) . . . 2_554 ?
O3 C5 O4 Sm1 -15.8(3) . . . 2_554 ?
C4 C5 O4 Sm1 163.7(3) . . . 2_554 ?

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
O5 H5A O3 0.851(10) 2.24(9) 2.822(4) 126(9) 2
O5 H5A O2 0.851(10) 2.551(17) 3.369(3) 161(3) 15_566
O5 H5B O6 0.848(10) 2.66(3) 3.51(3) 180.0(13) .
O6 H6A O6 0.85 2.33 2.86(6) 120.5 13_666

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.175


data_euzn1
_database_code_depnum_ccdc_archive 'CCDC 869777'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 Eu N6 O13.25 Zn3'
_chemical_formula_weight         829.82

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.29390(10)
_cell_length_b                   16.29390(10)
_cell_length_c                   16.29390(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4325.89(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7499
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      28.96

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3172
_exptl_absorpt_coefficient_mu    6.233
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_T_max  0.7061
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            54490
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         30.51
_reflns_number_total             2205
_reflns_number_gt                1681
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0177P)^2^+14.0526P] 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         2205
_refine_ls_number_parameters     128
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0549
_refine_ls_wR_factor_gt          0.0492
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.763338(9) 0.263338(9) 0.236662(9) 0.00514(7) Uani 1 3 d S . .
Zn1 Zn 0.70432(2) 0.48860(2) 0.18020(2) 0.00895(9) Uani 1 1 d . . .
C1 C 0.7560(2) 0.3754(2) 0.05212(19) 0.0120(6) Uani 1 1 d . . .
C2 C 0.7500(2) 0.4573(2) 0.0142(2) 0.0131(7) Uani 1 1 d . . .
C3 C 0.7732(2) 0.4826(2) -0.0636(2) 0.0173(7) Uani 1 1 d . . .
H3 H 0.7974 0.4511 -0.1063 0.021 Uiso 1 1 calc R . .
C4 C 0.7527(2) 0.5647(2) -0.0640(2) 0.0121(6) Uani 1 1 d . . .
C5 C 0.7602(2) 0.62820(19) -0.12717(19) 0.0098(6) Uani 1 1 d . . .
N1 N 0.71789(16) 0.51951(16) 0.05772(16) 0.0099(6) Uani 1 1 d . . .
N2 N 0.71924(16) 0.58630(16) 0.00908(16) 0.0089(5) Uani 1 1 d . . .
O1 O 0.74052(14) 0.37073(13) 0.12861(13) 0.0108(4) Uani 1 1 d . . .
O2 O 0.77570(18) 0.31801(15) 0.00523(15) 0.0224(6) Uani 1 1 d . . .
O3 O 0.72693(14) 0.69741(13) -0.11129(13) 0.0116(5) Uani 1 1 d . . .
O4 O 0.79638(14) 0.61569(14) -0.19413(14) 0.0125(5) Uani 1 1 d . . .
O5 O 0.67547(19) 0.17547(19) 0.32453(19) 0.0433(15) Uani 1 3 d SD . .
H5A H 0.6245(16) 0.182(10) 0.334(8) 0.052 Uiso 0.33 1 d PD . .
H5B H 0.698(8) 0.175(11) 0.372(4) 0.052 Uiso 0.33 1 d PD . .
O6 O 0.5620(18) 0.0620(18) 0.4380(18) 0.112(16) Uani 0.25 3 d SPD . .
H6A H 0.5319(18) 0.0319(18) 0.4681(18) 0.134 Uiso 0.25 3 d SPD . .
H6B H 0.530(15) 0.08(5) 0.40(4) 0.134 Uiso 0.08 1 d PD . .

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
Eu1 0.00514(7) 0.00514(7) 0.00514(7) -0.00031(6) -0.00031(6) 0.00031(6)
Zn1 0.00704(17) 0.00983(18) 0.00997(18) -0.00114(14) 0.00083(14) 0.00029(14)
C1 0.0160(17) 0.0099(15) 0.0100(15) 0.0009(12) 0.0015(13) 0.0037(12)
C2 0.0204(18) 0.0077(14) 0.0113(15) 0.0013(12) 0.0027(13) 0.0052(13)
C3 0.030(2) 0.0118(16) 0.0101(15) 0.0015(13) 0.0093(14) 0.0069(15)
C4 0.0148(17) 0.0088(15) 0.0127(15) 0.0028(12) 0.0020(13) 0.0017(12)
C5 0.0091(14) 0.0113(15) 0.0091(14) 0.0029(12) -0.0013(12) -0.0002(12)
N1 0.0131(14) 0.0075(12) 0.0090(12) 0.0013(10) 0.0001(10) 0.0026(10)
N2 0.0105(13) 0.0065(12) 0.0097(12) 0.0020(10) 0.0005(10) 0.0014(10)
O1 0.0168(11) 0.0079(10) 0.0078(10) 0.0029(8) 0.0031(9) 0.0011(9)
O2 0.0434(17) 0.0124(12) 0.0114(12) 0.0025(10) 0.0089(11) 0.0117(12)
O3 0.0176(12) 0.0084(11) 0.0087(10) 0.0027(8) 0.0022(9) 0.0027(9)
O4 0.0134(11) 0.0137(11) 0.0104(11) 0.0045(9) 0.0033(9) 0.0043(9)
O5 0.0433(15) 0.0433(15) 0.0433(15) 0.0184(15) 0.0184(15) -0.0184(15)
O6 0.112(16) 0.112(16) 0.112(16) -0.063(19) -0.063(19) 0.063(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
Eu1 O4 2.471(2) 12_654 ?
Eu1 O4 2.471(2) 2_665 ?
Eu1 O4 2.471(2) 7_564 ?
Eu1 O5 2.480(5) . ?
Eu1 O1 2.510(2) . ?
Eu1 O1 2.510(2) 8_645 ?
Eu1 O1 2.510(2) 11_556 ?
Eu1 O3 2.564(2) 2_665 ?
Eu1 O3 2.564(2) 12_654 ?
Eu1 O3 2.564(2) 7_564 ?
Eu1 C5 2.862(3) 7_564 ?
Eu1 C5 2.862(3) 12_654 ?
Zn1 O2 1.990(2) 11_556 ?
Zn1 N2 2.026(3) 22_565 ?
Zn1 N1 2.070(3) . ?
Zn1 O3 2.142(2) 22_565 ?
Zn1 O1 2.178(2) . ?
C1 O2 1.249(4) . ?
C1 O1 1.274(4) . ?
C1 C2 1.473(4) . ?
C2 N1 1.344(4) . ?
C2 C3 1.386(5) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 N2 1.355(4) . ?
C4 C5 1.465(4) . ?
C5 O4 1.257(4) . ?
C5 O3 1.277(4) . ?
C5 Eu1 2.862(3) 2_664 ?
N1 N2 1.346(4) . ?
N2 Zn1 2.026(3) 19_656 ?
O2 Zn1 1.990(2) 8_645 ?
O3 Zn1 2.142(2) 19_656 ?
O3 Eu1 2.564(2) 2_664 ?
O4 Eu1 2.471(2) 2_664 ?
O5 H5A 0.851(10) . ?
O5 H5B 0.851(10) . ?
O6 H6A 0.850(10) . ?
O6 H6B 0.850(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Eu1 O4 119.909(6) 12_654 2_665 ?
O4 Eu1 O4 119.908(6) 12_654 7_564 ?
O4 Eu1 O4 119.910(6) 2_665 7_564 ?
O4 Eu1 O5 88.26(6) 12_654 . ?
O4 Eu1 O5 88.26(6) 2_665 . ?
O4 Eu1 O5 88.26(6) 7_564 . ?
O4 Eu1 O1 135.45(8) 12_654 . ?
O4 Eu1 O1 72.88(7) 2_665 . ?
O4 Eu1 O1 69.35(7) 7_564 . ?
O5 Eu1 O1 136.22(5) . . ?
O4 Eu1 O1 69.35(7) 12_654 8_645 ?
O4 Eu1 O1 135.46(8) 2_665 8_645 ?
O4 Eu1 O1 72.88(7) 7_564 8_645 ?
O5 Eu1 O1 136.22(5) . 8_645 ?
O1 Eu1 O1 73.63(8) . 8_645 ?
O4 Eu1 O1 72.88(7) 12_654 11_556 ?
O4 Eu1 O1 69.35(7) 2_665 11_556 ?
O4 Eu1 O1 135.45(8) 7_564 11_556 ?
O5 Eu1 O1 136.22(5) . 11_556 ?
O1 Eu1 O1 73.63(8) . 11_556 ?
O1 Eu1 O1 73.63(8) 8_645 11_556 ?
O4 Eu1 O3 71.57(7) 12_654 2_665 ?
O4 Eu1 O3 51.99(7) 2_665 2_665 ?
O4 Eu1 O3 153.84(8) 7_564 2_665 ?
O5 Eu1 O3 67.78(5) . 2_665 ?
O1 Eu1 O3 120.87(7) . 2_665 ?
O1 Eu1 O3 131.86(7) 8_645 2_665 ?
O1 Eu1 O3 68.82(7) 11_556 2_665 ?
O4 Eu1 O3 51.99(7) 12_654 12_654 ?
O4 Eu1 O3 153.83(8) 2_665 12_654 ?
O4 Eu1 O3 71.57(7) 7_564 12_654 ?
O5 Eu1 O3 67.78(5) . 12_654 ?
O1 Eu1 O3 131.86(7) . 12_654 ?
O1 Eu1 O3 68.82(7) 8_645 12_654 ?
O1 Eu1 O3 120.87(7) 11_556 12_654 ?
O3 Eu1 O3 106.59(6) 2_665 12_654 ?
O4 Eu1 O3 153.84(8) 12_654 7_564 ?
O4 Eu1 O3 71.57(7) 2_665 7_564 ?
O4 Eu1 O3 51.99(7) 7_564 7_564 ?
O5 Eu1 O3 67.78(5) . 7_564 ?
O1 Eu1 O3 68.82(7) . 7_564 ?
O1 Eu1 O3 120.87(7) 8_645 7_564 ?
O1 Eu1 O3 131.86(7) 11_556 7_564 ?
O3 Eu1 O3 106.59(6) 2_665 7_564 ?
O3 Eu1 O3 106.59(6) 12_654 7_564 ?
O4 Eu1 C5 143.19(8) 12_654 7_564 ?
O4 Eu1 C5 94.77(8) 2_665 7_564 ?
O4 Eu1 C5 25.96(8) 7_564 7_564 ?
O5 Eu1 C5 80.31(6) . 7_564 ?
O1 Eu1 C5 62.96(8) . 7_564 ?
O1 Eu1 C5 95.36(8) 8_645 7_564 ?
O1 Eu1 C5 136.53(8) 11_556 7_564 ?
O3 Eu1 C5 132.69(8) 2_665 7_564 ?
O3 Eu1 C5 91.49(8) 12_654 7_564 ?
O3 Eu1 C5 26.51(8) 7_564 7_564 ?
O4 Eu1 C5 25.96(8) 12_654 12_654 ?
O4 Eu1 C5 143.19(8) 2_665 12_654 ?
O4 Eu1 C5 94.77(8) 7_564 12_654 ?
O5 Eu1 C5 80.31(6) . 12_654 ?
O1 Eu1 C5 136.53(8) . 12_654 ?
O1 Eu1 C5 62.95(8) 8_645 12_654 ?
O1 Eu1 C5 95.36(8) 11_556 12_654 ?
O3 Eu1 C5 91.49(8) 2_665 12_654 ?
O3 Eu1 C5 26.51(8) 12_654 12_654 ?
O3 Eu1 C5 132.69(8) 7_564 12_654 ?
C5 Eu1 C5 117.23(4) 7_564 12_654 ?
O2 Zn1 N2 140.31(11) 11_556 22_565 ?
O2 Zn1 N1 103.67(11) 11_556 . ?
N2 Zn1 N1 113.55(11) 22_565 . ?
O2 Zn1 O3 82.73(9) 11_556 22_565 ?
N2 Zn1 O3 79.69(10) 22_565 22_565 ?
N1 Zn1 O3 96.96(10) . 22_565 ?
O2 Zn1 O1 86.09(10) 11_556 . ?
N2 Zn1 O1 113.25(10) 22_565 . ?
N1 Zn1 O1 79.26(9) . . ?
O3 Zn1 O1 167.00(9) 22_565 . ?
O2 C1 O1 127.2(3) . . ?
O2 C1 C2 116.0(3) . . ?
O1 C1 C2 116.8(3) . . ?
N1 C2 C3 111.4(3) . . ?
N1 C2 C1 119.2(3) . . ?
C3 C2 C1 129.4(3) . . ?
C4 C3 C2 103.1(3) . . ?
C4 C3 H3 128.5 . . ?
C2 C3 H3 128.5 . . ?
N2 C4 C3 110.2(3) . . ?
N2 C4 C5 117.9(3) . . ?
C3 C4 C5 131.9(3) . . ?
O4 C5 O3 121.2(3) . . ?
O4 C5 C4 122.3(3) . . ?
O3 C5 C4 116.5(3) . . ?
O4 C5 Eu1 59.35(16) . 2_664 ?
O3 C5 Eu1 63.59(16) . 2_664 ?
C4 C5 Eu1 165.9(2) . 2_664 ?
C2 N1 N2 107.0(3) . . ?
C2 N1 Zn1 111.5(2) . . ?
N2 N1 Zn1 140.0(2) . . ?
N1 N2 C4 108.3(3) . . ?
N1 N2 Zn1 138.7(2) . 19_656 ?
C4 N2 Zn1 112.9(2) . 19_656 ?
C1 O1 Zn1 112.25(19) . . ?
C1 O1 Eu1 134.3(2) . . ?
Zn1 O1 Eu1 112.59(9) . . ?
C1 O2 Zn1 139.4(2) . 8_645 ?
C5 O3 Zn1 112.71(19) . 19_656 ?
C5 O3 Eu1 89.90(18) . 2_664 ?
Zn1 O3 Eu1 155.61(11) 19_656 2_664 ?
C5 O4 Eu1 94.69(19) . 2_664 ?
Eu1 O5 H5A 127(10) . . ?
Eu1 O5 H5B 106(10) . . ?
H5A O5 H5B 105.1(17) . . ?
H6A O6 H6B 105.3(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 170.5(3) . . . . ?
O1 C1 C2 N1 -9.4(5) . . . . ?
O2 C1 C2 C3 -9.3(6) . . . . ?
O1 C1 C2 C3 170.7(4) . . . . ?
N1 C2 C3 C4 0.0(4) . . . . ?
C1 C2 C3 C4 179.8(3) . . . . ?
C2 C3 C4 N2 -0.2(4) . . . . ?
C2 C3 C4 C5 -179.5(4) . . . . ?
N2 C4 C5 O4 174.0(3) . . . . ?
C3 C4 C5 O4 -6.7(6) . . . . ?
N2 C4 C5 O3 -6.7(5) . . . . ?
C3 C4 C5 O3 172.6(4) . . . . ?
N2 C4 C5 Eu1 -93.4(10) . . . 2_664 ?
C3 C4 C5 Eu1 85.9(10) . . . 2_664 ?
C3 C2 N1 N2 0.2(4) . . . . ?
C1 C2 N1 N2 -179.6(3) . . . . ?
C3 C2 N1 Zn1 -168.8(2) . . . . ?
C1 C2 N1 Zn1 11.3(4) . . . . ?
O2 Zn1 N1 C2 75.9(2) 11_556 . . . ?
N2 Zn1 N1 C2 -118.2(2) 22_565 . . . ?
O3 Zn1 N1 C2 160.0(2) 22_565 . . . ?
O1 Zn1 N1 C2 -7.4(2) . . . . ?
O2 Zn1 N1 N2 -87.7(3) 11_556 . . . ?
N2 Zn1 N1 N2 78.2(3) 22_565 . . . ?
O3 Zn1 N1 N2 -3.6(3) 22_565 . . . ?
O1 Zn1 N1 N2 -171.0(3) . . . . ?
C2 N1 N2 C4 -0.4(3) . . . . ?
Zn1 N1 N2 C4 163.7(3) . . . . ?
C2 N1 N2 Zn1 174.7(3) . . . 19_656 ?
Zn1 N1 N2 Zn1 -21.2(5) . . . 19_656 ?
C3 C4 N2 N1 0.4(4) . . . . ?
C5 C4 N2 N1 179.8(3) . . . . ?
C3 C4 N2 Zn1 -176.1(2) . . . 19_656 ?
C5 C4 N2 Zn1 3.3(4) . . . 19_656 ?
O2 C1 O1 Zn1 -177.7(3) . . . . ?
C2 C1 O1 Zn1 2.3(4) . . . . ?
O2 C1 O1 Eu1 13.9(6) . . . . ?
C2 C1 O1 Eu1 -166.1(2) . . . . ?
O2 Zn1 O1 C1 -102.0(2) 11_556 . . . ?
N2 Zn1 O1 C1 113.9(2) 22_565 . . . ?
N1 Zn1 O1 C1 2.7(2) . . . . ?
O3 Zn1 O1 C1 -71.4(5) 22_565 . . . ?
O2 Zn1 O1 Eu1 69.02(11) 11_556 . . . ?
N2 Zn1 O1 Eu1 -75.09(12) 22_565 . . . ?
N1 Zn1 O1 Eu1 173.74(12) . . . . ?
O3 Zn1 O1 Eu1 99.6(4) 22_565 . . . ?
O4 Eu1 O1 C1 61.0(3) 12_654 . . . ?
O4 Eu1 O1 C1 176.6(3) 2_665 . . . ?
O4 Eu1 O1 C1 -51.1(3) 7_564 . . . ?
O5 Eu1 O1 C1 -115.0(3) . . . . ?
O1 Eu1 O1 C1 26.4(3) 8_645 . . . ?
O1 Eu1 O1 C1 103.7(3) 11_556 . . . ?
O3 Eu1 O1 C1 155.8(3) 2_665 . . . ?
O3 Eu1 O1 C1 -13.4(3) 12_654 . . . ?
O3 Eu1 O1 C1 -107.1(3) 7_564 . . . ?
C5 Eu1 O1 C1 -78.7(3) 7_564 . . . ?
C5 Eu1 O1 C1 23.4(3) 12_654 . . . ?
O4 Eu1 O1 Zn1 -107.32(11) 12_654 . . . ?
O4 Eu1 O1 Zn1 8.20(9) 2_665 . . . ?
O4 Eu1 O1 Zn1 140.55(12) 7_564 . . . ?
O5 Eu1 O1 Zn1 76.65(11) . . . . ?
O1 Eu1 O1 Zn1 -141.99(10) 8_645 . . . ?
O1 Eu1 O1 Zn1 -64.70(13) 11_556 . . . ?
O3 Eu1 O1 Zn1 -12.60(13) 2_665 . . . ?
O3 Eu1 O1 Zn1 178.25(8) 12_654 . . . ?
O3 Eu1 O1 Zn1 84.59(10) 7_564 . . . ?
C5 Eu1 O1 Zn1 112.98(13) 7_564 . . . ?
C5 Eu1 O1 Zn1 -145.01(11) 12_654 . . . ?
O1 C1 O2 Zn1 -18.4(6) . . . 8_645 ?
C2 C1 O2 Zn1 161.6(3) . . . 8_645 ?
O4 C5 O3 Zn1 -174.4(2) . . . 19_656 ?
C4 C5 O3 Zn1 6.3(4) . . . 19_656 ?
Eu1 C5 O3 Zn1 170.60(17) 2_664 . . 19_656 ?
O4 C5 O3 Eu1 15.0(3) . . . 2_664 ?
C4 C5 O3 Eu1 -164.3(3) . . . 2_664 ?
O3 C5 O4 Eu1 -15.6(3) . . . 2_664 ?
C4 C5 O4 Eu1 163.6(3) . . . 2_664 ?

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
O5 H5A O2 0.851(10) 2.62(9) 3.369(3) 147(15) 18_655
O5 H5B O2 0.851(10) 2.52(2) 3.369(3) 175(18) 15_566
O6 H6A O6 0.850(10) 2.65(10) 3.50(10) 180.0(16) 13_656

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.140


data_35pa-3
_database_code_depnum_ccdc_archive 'CCDC 869778'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 Gd N6 O13.25 Zn3'
_chemical_formula_weight         835.11

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.29440(10)
_cell_length_b                   16.29440(10)
_cell_length_c                   16.29440(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4326.29(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4238
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      30.17

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3180
_exptl_absorpt_coefficient_mu    6.399
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6285
_exptl_absorpt_correction_T_max  0.6285
_exptl_absorpt_process_details   Sadabs

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10474
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         27.86
_reflns_number_total             1725
_reflns_number_gt                1507
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0166P)^2^+5.6355P] 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         1725
_refine_ls_number_parameters     124
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0461
_refine_ls_wR_factor_gt          0.0443
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.264239(8) 0.764239(8) 0.735761(8) 0.00769(7) Uani 1 3 d S . .
Zn1 Zn 0.20425(2) 0.98905(2) 0.67969(2) 0.01277(9) Uani 1 1 d . . .
C1 C 0.25696(18) 0.87534(18) 0.55152(18) 0.0158(6) Uani 1 1 d . . .
C2 C 0.25063(19) 0.95712(19) 0.51355(18) 0.0170(6) Uani 1 1 d . . .
C3 C 0.2740(2) 0.98275(19) 0.43618(19) 0.0225(7) Uani 1 1 d . . .
H3 H 0.2982 0.9520 0.3946 0.027 Uiso 1 1 calc R . .
C4 C 0.25302(17) 1.06467(18) 0.43535(17) 0.0146(6) Uani 1 1 d . . .
C5 C 0.25988(17) 1.12811(17) 0.37252(17) 0.0127(6) Uani 1 1 d . . .
N1 N 0.21825(14) 1.01959(14) 0.55731(14) 0.0124(5) Uani 1 1 d . . .
N2 N 0.21881(14) 1.08629(14) 0.50848(14) 0.0115(5) Uani 1 1 d . . .
O1 O 0.24118(12) 0.87079(12) 0.62825(12) 0.0148(4) Uani 1 1 d . . .
O2 O 0.27642(16) 0.81822(13) 0.50485(13) 0.0277(6) Uani 1 1 d . . .
O3 O 0.22642(12) 1.19699(12) 0.38774(12) 0.0164(4) Uani 1 1 d . . .
O4 O 0.29595(12) 1.11575(12) 0.30519(12) 0.0169(4) Uani 1 1 d . . .
O5 O 0.17652(17) 0.67652(17) 0.82348(17) 0.0466(13) Uani 1 3 d SD . .
H5A H 0.202(8) 0.681(6) 0.869(5) 0.056 Uiso 0.33 1 d PD . .
H5B H 0.171(7) 0.6252(18) 0.816(7) 0.056 Uiso 0.33 1 d PD . .
O6 O 0.5520(18) -0.0520(18) 1.0520(18) 0.165(19) Uani 0.25 3 d SP . .
H6A H 0.5609 -0.0378 1.0888 0.198 Uiso 0.08 1 d PR . .
H6B H 0.5219 -0.0124 1.0124 0.198 Uiso 0.08 1 d 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
Gd1 0.00769(7) 0.00769(7) 0.00769(7) -0.00027(5) -0.00027(5) 0.00027(5)
Zn1 0.00952(17) 0.01492(18) 0.01389(17) -0.00177(13) 0.00125(13) 0.00076(13)
C1 0.0196(15) 0.0121(14) 0.0157(15) 0.0039(12) 0.0034(12) 0.0032(12)
C2 0.0241(16) 0.0127(14) 0.0142(15) 0.0002(12) 0.0030(12) 0.0057(12)
C3 0.0360(19) 0.0186(16) 0.0128(15) 0.0024(12) 0.0110(14) 0.0101(14)
C4 0.0176(15) 0.0134(14) 0.0127(14) 0.0021(11) 0.0021(11) 0.0030(11)
C5 0.0118(13) 0.0138(14) 0.0126(14) 0.0025(11) -0.0040(11) -0.0001(11)
N1 0.0174(13) 0.0095(12) 0.0104(12) 0.0034(9) 0.0021(10) 0.0026(9)
N2 0.0130(12) 0.0101(11) 0.0116(11) 0.0023(9) 0.0008(9) 0.0021(9)
O1 0.0213(11) 0.0111(10) 0.0120(10) 0.0025(8) 0.0021(8) 0.0015(8)
O2 0.0538(17) 0.0129(11) 0.0163(11) 0.0006(9) 0.0072(11) 0.0140(11)
O3 0.0241(12) 0.0122(10) 0.0129(10) 0.0011(8) 0.0017(9) 0.0049(9)
O4 0.0174(10) 0.0201(11) 0.0132(10) 0.0055(8) 0.0048(8) 0.0063(9)
O5 0.0466(13) 0.0466(13) 0.0466(13) 0.0144(14) 0.0144(14) -0.0144(14)
O6 0.165(19) 0.165(19) 0.165(19) -0.09(2) 0.09(2) -0.09(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
Gd1 O4 2.4627(19) 7_564 ?
Gd1 O4 2.4628(19) 2_575 ?
Gd1 O4 2.4628(19) 12_665 ?
Gd1 O5 2.476(5) . ?
Gd1 O1 2.4948(19) 11_466 ?
Gd1 O1 2.4948(19) . ?
Gd1 O1 2.4949(19) 8_656 ?
Gd1 O3 2.5603(19) 7_564 ?
Gd1 O3 2.5603(19) 2_575 ?
Gd1 O3 2.5603(19) 12_665 ?
Gd1 C5 2.863(3) 2_575 ?
Gd1 C5 2.863(3) 7_564 ?
Zn1 O2 1.993(2) 11_466 ?
Zn1 N2 2.025(2) 22_476 ?
Zn1 N1 2.068(2) . ?
Zn1 O3 2.150(2) 22_476 ?
Zn1 O1 2.1858(19) . ?
C1 O2 1.243(3) . ?
C1 O1 1.279(3) . ?
C1 C2 1.473(4) . ?
C2 N1 1.350(4) . ?
C2 C3 1.382(4) . ?
C3 C4 1.378(4) . ?
C3 H3 0.9300 . ?
C4 N2 1.362(4) . ?
C4 C5 1.459(4) . ?
C5 O4 1.261(3) . ?
C5 O3 1.272(3) . ?
C5 Gd1 2.863(3) 2_574 ?
N1 N2 1.347(3) . ?
N2 Zn1 2.025(2) 19_567 ?
O2 Zn1 1.993(2) 8_656 ?
O3 Zn1 2.150(2) 19_567 ?
O3 Gd1 2.5603(19) 2_574 ?
O4 Gd1 2.4628(19) 2_574 ?
O5 H5A 0.85(2) . ?
O5 H5B 0.85(2) . ?
O6 H6A 0.6594 . ?
O6 H6B 1.0364 . ?

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 Gd1 O4 119.866(6) 7_564 2_575 ?
O4 Gd1 O4 119.867(6) 7_564 12_665 ?
O4 Gd1 O4 119.867(6) 2_575 12_665 ?
O4 Gd1 O5 87.90(5) 7_564 . ?
O4 Gd1 O5 87.90(5) 2_575 . ?
O4 Gd1 O5 87.90(5) 12_665 . ?
O4 Gd1 O1 135.96(7) 7_564 11_466 ?
O4 Gd1 O1 69.54(6) 2_575 11_466 ?
O4 Gd1 O1 73.14(6) 12_665 11_466 ?
O5 Gd1 O1 136.07(5) . 11_466 ?
O4 Gd1 O1 69.54(6) 7_564 . ?
O4 Gd1 O1 73.14(6) 2_575 . ?
O4 Gd1 O1 135.96(7) 12_665 . ?
O5 Gd1 O1 136.07(5) . . ?
O1 Gd1 O1 73.85(7) 11_466 . ?
O4 Gd1 O1 73.14(6) 7_564 8_656 ?
O4 Gd1 O1 135.96(7) 2_575 8_656 ?
O4 Gd1 O1 69.54(6) 12_665 8_656 ?
O5 Gd1 O1 136.07(5) . 8_656 ?
O1 Gd1 O1 73.85(7) 11_466 8_656 ?
O1 Gd1 O1 73.85(7) . 8_656 ?
O4 Gd1 O3 51.93(6) 7_564 7_564 ?
O4 Gd1 O3 71.40(6) 2_575 7_564 ?
O4 Gd1 O3 153.33(7) 12_665 7_564 ?
O5 Gd1 O3 67.56(5) . 7_564 ?
O1 Gd1 O3 131.96(6) 11_466 7_564 ?
O1 Gd1 O3 68.88(6) . 7_564 ?
O1 Gd1 O3 121.09(6) 8_656 7_564 ?
O4 Gd1 O3 153.33(7) 7_564 2_575 ?
O4 Gd1 O3 51.94(6) 2_575 2_575 ?
O4 Gd1 O3 71.40(6) 12_665 2_575 ?
O5 Gd1 O3 67.56(5) . 2_575 ?
O1 Gd1 O3 68.88(6) 11_466 2_575 ?
O1 Gd1 O3 121.09(6) . 2_575 ?
O1 Gd1 O3 131.95(6) 8_656 2_575 ?
O3 Gd1 O3 106.35(5) 7_564 2_575 ?
O4 Gd1 O3 71.40(6) 7_564 12_665 ?
O4 Gd1 O3 153.33(7) 2_575 12_665 ?
O4 Gd1 O3 51.94(6) 12_665 12_665 ?
O5 Gd1 O3 67.57(5) . 12_665 ?
O1 Gd1 O3 121.09(6) 11_466 12_665 ?
O1 Gd1 O3 131.95(6) . 12_665 ?
O1 Gd1 O3 68.88(6) 8_656 12_665 ?
O3 Gd1 O3 106.35(5) 7_564 12_665 ?
O3 Gd1 O3 106.35(5) 2_575 12_665 ?
O4 Gd1 C5 143.03(7) 7_564 2_575 ?
O4 Gd1 C5 26.02(7) 2_575 2_575 ?
O4 Gd1 C5 94.61(7) 12_665 2_575 ?
O5 Gd1 C5 79.93(6) . 2_575 ?
O1 Gd1 C5 63.14(7) 11_466 2_575 ?
O1 Gd1 C5 95.71(7) . 2_575 ?
O1 Gd1 C5 136.91(7) 8_656 2_575 ?
O3 Gd1 C5 91.31(7) 7_564 2_575 ?
O3 Gd1 C5 26.38(7) 2_575 2_575 ?
O3 Gd1 C5 132.28(7) 12_665 2_575 ?
O4 Gd1 C5 26.02(7) 7_564 7_564 ?
O4 Gd1 C5 94.62(7) 2_575 7_564 ?
O4 Gd1 C5 143.03(7) 12_665 7_564 ?
O5 Gd1 C5 79.93(6) . 7_564 ?
O1 Gd1 C5 136.91(7) 11_466 7_564 ?
O1 Gd1 C5 63.14(7) . 7_564 ?
O1 Gd1 C5 95.71(7) 8_656 7_564 ?
O3 Gd1 C5 26.38(7) 7_564 7_564 ?
O3 Gd1 C5 132.28(7) 2_575 7_564 ?
O3 Gd1 C5 91.31(7) 12_665 7_564 ?
C5 Gd1 C5 117.01(3) 2_575 7_564 ?
O2 Zn1 N2 140.40(10) 11_466 22_476 ?
O2 Zn1 N1 103.37(10) 11_466 . ?
N2 Zn1 N1 113.79(9) 22_476 . ?
O2 Zn1 O3 82.97(8) 11_466 22_476 ?
N2 Zn1 O3 79.50(8) 22_476 22_476 ?
N1 Zn1 O3 97.06(8) . 22_476 ?
O2 Zn1 O1 85.70(9) 11_466 . ?
N2 Zn1 O1 113.54(8) 22_476 . ?
N1 Zn1 O1 79.17(8) . . ?
O3 Zn1 O1 166.90(8) 22_476 . ?
O2 C1 O1 127.3(3) . . ?
O2 C1 C2 116.0(3) . . ?
O1 C1 C2 116.7(3) . . ?
N1 C2 C3 111.2(3) . . ?
N1 C2 C1 119.2(3) . . ?
C3 C2 C1 129.6(3) . . ?
C4 C3 C2 103.5(3) . . ?
C4 C3 H3 128.3 . . ?
C2 C3 H3 128.3 . . ?
N2 C4 C3 110.1(3) . . ?
N2 C4 C5 117.5(2) . . ?
C3 C4 C5 132.4(3) . . ?
O4 C5 O3 120.7(3) . . ?
O4 C5 C4 122.2(3) . . ?
O3 C5 C4 117.1(2) . . ?
O4 C5 Gd1 58.97(14) . 2_574 ?
O3 C5 Gd1 63.41(14) . 2_574 ?
C4 C5 Gd1 165.8(2) . 2_574 ?
N2 N1 C2 107.1(2) . . ?
N2 N1 Zn1 139.86(18) . . ?
C2 N1 Zn1 111.77(18) . . ?
N1 N2 C4 108.1(2) . . ?
N1 N2 Zn1 138.75(18) . 19_567 ?
C4 N2 Zn1 113.05(18) . 19_567 ?
C1 O1 Zn1 112.28(18) . . ?
C1 O1 Gd1 134.16(18) . . ?
Zn1 O1 Gd1 112.69(8) . . ?
C1 O2 Zn1 139.4(2) . 8_656 ?
C5 O3 Zn1 112.47(17) . 19_567 ?
C5 O3 Gd1 90.21(16) . 2_574 ?
Zn1 O3 Gd1 155.57(9) 19_567 2_574 ?
C5 O4 Gd1 95.01(16) . 2_574 ?
Gd1 O5 H5A 99(10) . . ?
Gd1 O5 H5B 123(9) . . ?
H5A O5 H5B 105(3) . . ?
H6A O6 H6B 116.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 170.3(3) . . . . ?
O1 C1 C2 N1 -9.1(4) . . . . ?
O2 C1 C2 C3 -10.1(5) . . . . ?
O1 C1 C2 C3 170.5(3) . . . . ?
N1 C2 C3 C4 -0.6(4) . . . . ?
C1 C2 C3 C4 179.8(3) . . . . ?
C2 C3 C4 N2 -0.1(4) . . . . ?
C2 C3 C4 C5 -179.2(3) . . . . ?
N2 C4 C5 O4 174.7(3) . . . . ?
C3 C4 C5 O4 -6.2(5) . . . . ?
N2 C4 C5 O3 -6.5(4) . . . . ?
C3 C4 C5 O3 172.6(3) . . . . ?
N2 C4 C5 Gd1 -94.9(8) . . . 2_574 ?
C3 C4 C5 Gd1 84.1(9) . . . 2_574 ?
C3 C2 N1 N2 1.1(3) . . . . ?
C1 C2 N1 N2 -179.3(3) . . . . ?
C3 C2 N1 Zn1 -168.7(2) . . . . ?
C1 C2 N1 Zn1 11.0(3) . . . . ?
O2 Zn1 N1 N2 -89.0(3) 11_466 . . . ?
N2 Zn1 N1 N2 77.0(3) 22_476 . . . ?
O3 Zn1 N1 N2 -4.6(3) 22_476 . . . ?
O1 Zn1 N1 N2 -171.8(3) . . . . ?
O2 Zn1 N1 C2 75.7(2) 11_466 . . . ?
N2 Zn1 N1 C2 -118.3(2) 22_476 . . . ?
O3 Zn1 N1 C2 160.1(2) 22_476 . . . ?
O1 Zn1 N1 C2 -7.2(2) . . . . ?
C2 N1 N2 C4 -1.1(3) . . . . ?
Zn1 N1 N2 C4 164.0(2) . . . . ?
C2 N1 N2 Zn1 175.2(2) . . . 19_567 ?
Zn1 N1 N2 Zn1 -19.6(5) . . . 19_567 ?
C3 C4 N2 N1 0.8(3) . . . . ?
C5 C4 N2 N1 180.0(2) . . . . ?
C3 C4 N2 Zn1 -176.6(2) . . . 19_567 ?
C5 C4 N2 Zn1 2.6(3) . . . 19_567 ?
O2 C1 O1 Zn1 -177.2(3) . . . . ?
C2 C1 O1 Zn1 2.1(3) . . . . ?
O2 C1 O1 Gd1 14.6(5) . . . . ?
C2 C1 O1 Gd1 -166.12(19) . . . . ?
O2 Zn1 O1 C1 -101.8(2) 11_466 . . . ?
N2 Zn1 O1 C1 114.1(2) 22_476 . . . ?
N1 Zn1 O1 C1 2.7(2) . . . . ?
O3 Zn1 O1 C1 -71.6(4) 22_476 . . . ?
O2 Zn1 O1 Gd1 69.06(10) 11_466 . . . ?
N2 Zn1 O1 Gd1 -75.04(11) 22_476 . . . ?
N1 Zn1 O1 Gd1 173.57(11) . . . . ?
O3 Zn1 O1 Gd1 99.3(3) 22_476 . . . ?
O4 Gd1 O1 C1 -51.6(3) 7_564 . . . ?
O4 Gd1 O1 C1 176.4(3) 2_575 . . . ?
O4 Gd1 O1 C1 60.7(3) 12_665 . . . ?
O5 Gd1 O1 C1 -115.3(2) . . . . ?
O1 Gd1 O1 C1 103.5(2) 11_466 . . . ?
O1 Gd1 O1 C1 26.0(3) 8_656 . . . ?
O3 Gd1 O1 C1 -107.5(3) 7_564 . . . ?
O3 Gd1 O1 C1 155.7(2) 2_575 . . . ?
O3 Gd1 O1 C1 -14.1(3) 12_665 . . . ?
C5 Gd1 O1 C1 163.3(3) 2_575 . . . ?
C5 Gd1 O1 C1 -79.2(3) 7_564 . . . ?
O4 Gd1 O1 Zn1 140.18(10) 7_564 . . . ?
O4 Gd1 O1 Zn1 8.23(8) 2_575 . . . ?
O4 Gd1 O1 Zn1 -107.57(10) 12_665 . . . ?
O5 Gd1 O1 Zn1 76.52(10) . . . . ?
O1 Gd1 O1 Zn1 -64.76(12) 11_466 . . . ?
O1 Gd1 O1 Zn1 -142.19(8) 8_656 . . . ?
O3 Gd1 O1 Zn1 84.32(9) 7_564 . . . ?
O3 Gd1 O1 Zn1 -12.54(12) 2_575 . . . ?
O3 Gd1 O1 Zn1 177.68(7) 12_665 . . . ?
C5 Gd1 O1 Zn1 -4.88(10) 2_575 . . . ?
C5 Gd1 O1 Zn1 112.57(11) 7_564 . . . ?
O1 C1 O2 Zn1 -18.7(6) . . . 8_656 ?
C2 C1 O2 Zn1 162.0(2) . . . 8_656 ?
O4 C5 O3 Zn1 -174.6(2) . . . 19_567 ?
C4 C5 O3 Zn1 6.6(3) . . . 19_567 ?
Gd1 C5 O3 Zn1 170.70(15) 2_574 . . 19_567 ?
O4 C5 O3 Gd1 14.7(3) . . . 2_574 ?
C4 C5 O3 Gd1 -164.1(2) . . . 2_574 ?
O3 C5 O4 Gd1 -15.3(3) . . . 2_574 ?
C4 C5 O4 Gd1 163.4(2) . . . 2_574 ?

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
O5 H5A O3 0.85(2) 2.32(10) 2.801(3) 116(9) 2_575
O5 H5A O2 0.85(2) 2.53(2) 3.375(3) 175(10) 15_576
O5 H5B O2 0.85(2) 2.61(7) 3.375(3) 151(11) 21_666
O6 H6B O6 1.04 1.91 2.94(10) 169.2 13_657

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.86
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.101


data_zdc
_database_code_depnum_ccdc_archive 'CCDC 869779'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5.50 N6 O13.25 Tb Zn3'
_chemical_formula_weight         836.78

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.2707(3)
_cell_length_b                   16.2707(3)
_cell_length_c                   16.2707(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4307.44(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    982
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      24.08

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3188
_exptl_absorpt_coefficient_mu    6.631
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_T_max  0.8259
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9257
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         30.47
_reflns_number_total             2193
_reflns_number_gt                1644
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0168P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2193
_refine_ls_number_parameters     120
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.764658(12) 0.264658(12) 0.235342(12) 0.00707(9) Uani 1 3 d S . .
Zn1 Zn 0.79566(3) -0.01091(3) 0.17936(3) 0.00845(12) Uani 1 1 d . . .
C1 C 1.1245(3) -0.0512(3) 0.2570(3) 0.0118(9) Uani 1 1 d . . .
C2 C 1.0424(3) -0.0135(3) 0.2509(3) 0.0128(9) Uani 1 1 d . . .
C3 C 1.0172(3) 0.0648(3) 0.2743(3) 0.0144(9) Uani 1 1 d . . .
H3 H 1.0486 0.1075 0.2990 0.017 Uiso 1 1 calc R . .
C4 C 0.9350(3) 0.0649(3) 0.2525(3) 0.0105(8) Uani 1 1 d . . .
C5 C 0.8711(3) 0.1285(3) 0.2593(3) 0.0111(8) Uani 1 1 d . . .
N1 N 0.9804(2) -0.0568(2) 0.2179(2) 0.0083(7) Uani 1 1 d . . .
N2 N 0.9134(2) -0.0080(2) 0.2185(2) 0.0068(7) Uani 1 1 d . . .
O1 O 1.12928(17) -0.12799(17) 0.24179(18) 0.0103(6) Uani 1 1 d . . .
O2 O 1.18204(19) -0.00438(19) 0.2768(2) 0.0209(8) Uani 1 1 d . . .
O3 O 0.80284(18) 0.11299(18) 0.22519(19) 0.0120(6) Uani 1 1 d . . .
O4 O 0.88373(18) 0.19586(18) 0.29560(19) 0.0124(7) Uani 1 1 d . . .
O5 O 0.6776(2) 0.1776(2) 0.3224(2) 0.0357(17) Uani 1 3 d SD . .
H5A H 0.666(6) 0.127(2) 0.312(4) 0.043 Uiso 0.33 1 d PRD . .
H5B H 0.623(3) 0.191(3) 0.344(6) 0.043 Uiso 0.33 1 d PRD . .
O6 O 0.5576(18) 0.0576(18) 0.4424(18) 0.084(14) Uani 0.25 3 d SP . .
H6A H 0.5274 0.0274 0.4726 0.101 Uiso 0.25 3 d SPR . .
H6B H 0.5918 0.0567 0.4008 0.101 Uiso 0.08 1 d 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
Tb1 0.00707(9) 0.00707(9) 0.00707(9) -0.00040(8) -0.00040(8) 0.00040(8)
Zn1 0.0064(2) 0.0098(2) 0.0092(2) -0.00150(18) -0.00045(19) -0.00009(18)
C1 0.010(2) 0.009(2) 0.016(2) -0.0009(17) -0.0029(17) 0.0016(16)
C2 0.010(2) 0.010(2) 0.018(2) -0.0027(17) -0.0048(17) -0.0017(16)
C3 0.010(2) 0.011(2) 0.022(3) -0.0042(18) -0.0072(18) 0.0025(17)
C4 0.011(2) 0.009(2) 0.012(2) -0.0004(16) -0.0021(16) 0.0007(16)
C5 0.013(2) 0.010(2) 0.010(2) 0.0020(16) 0.0002(17) 0.0000(17)
N1 0.0054(17) 0.0077(17) 0.0119(19) -0.0018(14) -0.0001(13) -0.0004(13)
N2 0.0054(16) 0.0062(16) 0.0089(18) 0.0012(13) -0.0011(13) 0.0001(13)
O1 0.0081(15) 0.0067(15) 0.0162(16) -0.0026(12) 0.0001(12) -0.0005(11)
O2 0.0093(16) 0.0126(17) 0.041(2) -0.0063(15) -0.0106(15) 0.0056(13)
O3 0.0097(15) 0.0097(15) 0.0168(17) -0.0027(12) -0.0050(12) 0.0036(12)
O4 0.0112(16) 0.0100(16) 0.0162(16) -0.0019(12) -0.0029(13) 0.0033(12)
O5 0.0357(17) 0.0357(17) 0.0357(17) 0.0126(16) 0.0126(16) -0.0126(16)
O6 0.084(14) 0.084(14) 0.084(14) -0.051(17) -0.051(17) 0.051(17)

_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
Tb1 O4 2.443(3) 8_645 ?
Tb1 O4 2.443(3) . ?
Tb1 O4 2.443(3) 11_556 ?
Tb1 O5 2.453(6) . ?
Tb1 O1 2.483(3) 6_565 ?
Tb1 O1 2.483(3) 9_654 ?
Tb1 O1 2.483(3) 3_755 ?
Tb1 O3 2.550(3) . ?
Tb1 O3 2.550(3) 11_556 ?
Tb1 O3 2.550(3) 8_645 ?
Tb1 C5 2.839(4) 8_645 ?
Tb1 C5 2.839(4) . ?
Zn1 O2 1.985(3) 14_556 ?
Zn1 N2 2.020(3) . ?
Zn1 N1 2.066(3) 17_665 ?
Zn1 O3 2.153(3) . ?
Zn1 O1 2.186(3) 17_665 ?
C1 O2 1.248(5) . ?
C1 O1 1.277(5) . ?
C1 C2 1.474(6) . ?
C2 N1 1.342(5) . ?
C2 C3 1.391(6) . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 N2 1.354(5) . ?
C4 C5 1.471(6) . ?
C5 O4 1.262(5) . ?
C5 O3 1.267(5) . ?
N1 N2 1.349(5) . ?
N1 Zn1 2.066(3) 21_656 ?
O1 Zn1 2.186(3) 21_656 ?
O1 Tb1 2.483(3) 3_745 ?
O2 Zn1 1.985(3) 14_656 ?
O5 H5A 0.8697 . ?
O5 H5B 0.9836 . ?
O6 H6A 0.8510 . ?
O6 H6B 0.8761 . ?

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 Tb1 O4 119.855(10) 8_645 . ?
O4 Tb1 O4 119.853(10) 8_645 11_556 ?
O4 Tb1 O4 119.853(10) . 11_556 ?
O4 Tb1 O5 87.80(7) 8_645 . ?
O4 Tb1 O5 87.80(7) . . ?
O4 Tb1 O5 87.80(7) 11_556 . ?
O4 Tb1 O1 73.20(10) 8_645 6_565 ?
O4 Tb1 O1 136.01(10) . 6_565 ?
O4 Tb1 O1 69.66(10) 11_556 6_565 ?
O5 Tb1 O1 136.12(7) . 6_565 ?
O4 Tb1 O1 136.02(10) 8_645 9_654 ?
O4 Tb1 O1 69.66(10) . 9_654 ?
O4 Tb1 O1 73.21(10) 11_556 9_654 ?
O5 Tb1 O1 136.12(7) . 9_654 ?
O1 Tb1 O1 73.79(11) 6_565 9_654 ?
O4 Tb1 O1 69.66(10) 8_645 3_755 ?
O4 Tb1 O1 73.20(10) . 3_755 ?
O4 Tb1 O1 136.02(10) 11_556 3_755 ?
O5 Tb1 O1 136.12(7) . 3_755 ?
O1 Tb1 O1 73.79(11) 6_565 3_755 ?
O1 Tb1 O1 73.79(11) 9_654 3_755 ?
O4 Tb1 O3 153.50(10) 8_645 . ?
O4 Tb1 O3 52.37(10) . . ?
O4 Tb1 O3 70.84(10) 11_556 . ?
O5 Tb1 O3 67.63(7) . . ?
O1 Tb1 O3 131.56(9) 6_565 . ?
O1 Tb1 O3 68.82(10) 9_654 . ?
O1 Tb1 O3 121.40(9) 3_755 . ?
O4 Tb1 O3 70.84(10) 8_645 11_556 ?
O4 Tb1 O3 153.50(10) . 11_556 ?
O4 Tb1 O3 52.37(10) 11_556 11_556 ?
O5 Tb1 O3 67.62(7) . 11_556 ?
O1 Tb1 O3 68.82(10) 6_565 11_556 ?
O1 Tb1 O3 121.40(9) 9_654 11_556 ?
O1 Tb1 O3 131.56(9) 3_755 11_556 ?
O3 Tb1 O3 106.42(8) . 11_556 ?
O4 Tb1 O3 52.37(10) 8_645 8_645 ?
O4 Tb1 O3 70.85(10) . 8_645 ?
O4 Tb1 O3 153.50(10) 11_556 8_645 ?
O5 Tb1 O3 67.63(7) . 8_645 ?
O1 Tb1 O3 121.40(9) 6_565 8_645 ?
O1 Tb1 O3 131.56(9) 9_654 8_645 ?
O1 Tb1 O3 68.82(10) 3_755 8_645 ?
O3 Tb1 O3 106.42(8) . 8_645 ?
O3 Tb1 O3 106.42(8) 11_556 8_645 ?
O4 Tb1 C5 26.30(11) 8_645 8_645 ?
O4 Tb1 C5 94.32(11) . 8_645 ?
O4 Tb1 C5 143.21(11) 11_556 8_645 ?
O5 Tb1 C5 79.78(9) . 8_645 ?
O1 Tb1 C5 95.98(11) 6_565 8_645 ?
O1 Tb1 C5 136.90(11) 9_654 8_645 ?
O1 Tb1 C5 63.21(11) 3_755 8_645 ?
O3 Tb1 C5 132.41(11) . 8_645 ?
O3 Tb1 C5 91.02(11) 11_556 8_645 ?
O3 Tb1 C5 26.51(10) 8_645 8_645 ?
O4 Tb1 C5 143.21(11) 8_645 . ?
O4 Tb1 C5 26.29(11) . . ?
O4 Tb1 C5 94.32(11) 11_556 . ?
O5 Tb1 C5 79.78(9) . . ?
O1 Tb1 C5 136.90(11) 6_565 . ?
O1 Tb1 C5 63.21(11) 9_654 . ?
O1 Tb1 C5 95.98(11) 3_755 . ?
O3 Tb1 C5 26.51(10) . . ?
O3 Tb1 C5 132.41(11) 11_556 . ?
O3 Tb1 C5 91.02(11) 8_645 . ?
C5 Tb1 C5 116.92(5) 8_645 . ?
O2 Zn1 N2 140.25(15) 14_556 . ?
O2 Zn1 N1 103.57(15) 14_556 17_665 ?
N2 Zn1 N1 113.60(14) . 17_665 ?
O2 Zn1 O3 82.87(13) 14_556 . ?
N2 Zn1 O3 79.46(13) . . ?
N1 Zn1 O3 96.62(12) 17_665 . ?
O2 Zn1 O1 85.70(13) 14_556 17_665 ?
N2 Zn1 O1 113.95(13) . 17_665 ?
N1 Zn1 O1 79.21(12) 17_665 17_665 ?
O3 Zn1 O1 166.56(11) . 17_665 ?
O2 C1 O1 127.0(4) . . ?
O2 C1 C2 116.3(4) . . ?
O1 C1 C2 116.7(4) . . ?
N1 C2 C3 111.7(4) . . ?
N1 C2 C1 119.3(4) . . ?
C3 C2 C1 129.0(4) . . ?
C4 C3 C2 102.4(4) . . ?
C4 C3 H3 128.8 . . ?
C2 C3 H3 128.8 . . ?
N2 C4 C3 110.8(4) . . ?
N2 C4 C5 117.6(4) . . ?
C3 C4 C5 131.6(4) . . ?
O4 C5 O3 121.4(4) . . ?
O4 C5 C4 122.1(4) . . ?
O3 C5 C4 116.5(4) . . ?
O4 C5 Tb1 59.1(2) . . ?
O3 C5 Tb1 63.9(2) . . ?
C4 C5 Tb1 165.9(3) . . ?
C2 N1 N2 107.1(3) . . ?
C2 N1 Zn1 111.7(3) . 21_656 ?
N2 N1 Zn1 139.8(3) . 21_656 ?
N1 N2 C4 108.0(3) . . ?
N1 N2 Zn1 138.6(3) . . ?
C4 N2 Zn1 113.3(3) . . ?
C1 O1 Zn1 112.0(3) . 21_656 ?
C1 O1 Tb1 134.6(3) . 3_745 ?
Zn1 O1 Tb1 112.65(12) 21_656 3_745 ?
C1 O2 Zn1 139.3(3) . 14_656 ?
C5 O3 Zn1 112.7(3) . . ?
C5 O3 Tb1 89.6(2) . . ?
Zn1 O3 Tb1 156.28(14) . . ?
C5 O4 Tb1 94.6(3) . . ?
Tb1 O5 H5A 124.4 . . ?
Tb1 O5 H5B 127.5 . . ?
H5A O5 H5B 94.4 . . ?
H6A O6 H6B 143.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 169.8(4) . . . . ?
O1 C1 C2 N1 -10.3(6) . . . . ?
O2 C1 C2 C3 -9.3(7) . . . . ?
O1 C1 C2 C3 170.5(4) . . . . ?
N1 C2 C3 C4 -0.1(5) . . . . ?
C1 C2 C3 C4 179.1(4) . . . . ?
C2 C3 C4 N2 -0.2(5) . . . . ?
C2 C3 C4 C5 -179.5(4) . . . . ?
N2 C4 C5 O4 174.5(4) . . . . ?
C3 C4 C5 O4 -6.2(8) . . . . ?
N2 C4 C5 O3 -6.9(6) . . . . ?
C3 C4 C5 O3 172.4(5) . . . . ?
N2 C4 C5 Tb1 -95.2(13) . . . . ?
C3 C4 C5 Tb1 84.1(13) . . . . ?
O4 Tb1 C5 O4 -33.9(3) 8_645 . . . ?
O4 Tb1 C5 O4 166.9(3) 11_556 . . . ?
O5 Tb1 C5 O4 -106.1(3) . . . . ?
O1 Tb1 C5 O4 102.4(3) 6_565 . . . ?
O1 Tb1 C5 O4 98.2(3) 9_654 . . . ?
O1 Tb1 C5 O4 29.8(3) 3_755 . . . ?
O3 Tb1 C5 O4 -165.7(4) . . . . ?
O3 Tb1 C5 O4 -152.6(2) 11_556 . . . ?
O3 Tb1 C5 O4 -39.0(3) 8_645 . . . ?
C5 Tb1 C5 O4 -33.2(4) 8_645 . . . ?
O4 Tb1 C5 O3 131.8(2) 8_645 . . . ?
O4 Tb1 C5 O3 165.7(4) . . . . ?
O4 Tb1 C5 O3 -27.3(3) 11_556 . . . ?
O5 Tb1 C5 O3 59.7(2) . . . . ?
O1 Tb1 C5 O3 -91.9(3) 6_565 . . . ?
O1 Tb1 C5 O3 -96.0(3) 9_654 . . . ?
O1 Tb1 C5 O3 -164.5(2) 3_755 . . . ?
O3 Tb1 C5 O3 13.2(3) 11_556 . . . ?
O3 Tb1 C5 O3 126.7(3) 8_645 . . . ?
C5 Tb1 C5 O3 132.58(18) 8_645 . . . ?
O4 Tb1 C5 C4 -132.9(12) 8_645 . . . ?
O4 Tb1 C5 C4 -99.0(13) . . . . ?
O4 Tb1 C5 C4 68.0(13) 11_556 . . . ?
O5 Tb1 C5 C4 154.9(13) . . . . ?
O1 Tb1 C5 C4 3.4(13) 6_565 . . . ?
O1 Tb1 C5 C4 -0.8(12) 9_654 . . . ?
O1 Tb1 C5 C4 -69.2(13) 3_755 . . . ?
O3 Tb1 C5 C4 95.3(13) . . . . ?
O3 Tb1 C5 C4 108.5(12) 11_556 . . . ?
O3 Tb1 C5 C4 -138.0(13) 8_645 . . . ?
C5 Tb1 C5 C4 -132.1(12) 8_645 . . . ?
C3 C2 N1 N2 0.3(5) . . . . ?
C1 C2 N1 N2 -179.0(4) . . . . ?
C3 C2 N1 Zn1 -168.8(3) . . . 21_656 ?
C1 C2 N1 Zn1 12.0(5) . . . 21_656 ?
C2 N1 N2 C4 -0.4(4) . . . . ?
Zn1 N1 N2 C4 163.8(3) 21_656 . . . ?
C2 N1 N2 Zn1 175.8(3) . . . . ?
Zn1 N1 N2 Zn1 -20.0(7) 21_656 . . . ?
C3 C4 N2 N1 0.3(5) . . . . ?
C5 C4 N2 N1 179.8(3) . . . . ?
C3 C4 N2 Zn1 -176.9(3) . . . . ?
C5 C4 N2 Zn1 2.5(5) . . . . ?
O2 Zn1 N2 N1 119.8(4) 14_556 . . . ?
N1 Zn1 N2 N1 -82.4(4) 17_665 . . . ?
O3 Zn1 N2 N1 -175.1(4) . . . . ?
O1 Zn1 N2 N1 5.9(4) 17_665 . . . ?
O2 Zn1 N2 C4 -64.2(4) 14_556 . . . ?
N1 Zn1 N2 C4 93.6(3) 17_665 . . . ?
O3 Zn1 N2 C4 0.9(3) . . . . ?
O1 Zn1 N2 C4 -178.1(3) 17_665 . . . ?
O2 C1 O1 Zn1 -177.3(4) . . . 21_656 ?
C2 C1 O1 Zn1 2.9(5) . . . 21_656 ?
O2 C1 O1 Tb1 13.8(7) . . . 3_745 ?
C2 C1 O1 Tb1 -166.0(3) . . . 3_745 ?
O1 C1 O2 Zn1 -18.0(8) . . . 14_656 ?
C2 C1 O2 Zn1 161.8(4) . . . 14_656 ?
O4 C5 O3 Zn1 -174.1(3) . . . . ?
C4 C5 O3 Zn1 7.3(5) . . . . ?
Tb1 C5 O3 Zn1 171.6(2) . . . . ?
O4 C5 O3 Tb1 14.3(4) . . . . ?
C4 C5 O3 Tb1 -164.3(3) . . . . ?
O2 Zn1 O3 C5 139.5(3) 14_556 . . . ?
N2 Zn1 O3 C5 -4.7(3) . . . . ?
N1 Zn1 O3 C5 -117.6(3) 17_665 . . . ?
O1 Zn1 O3 C5 171.4(4) 17_665 . . . ?
O2 Zn1 O3 Tb1 -61.9(4) 14_556 . . . ?
N2 Zn1 O3 Tb1 153.9(4) . . . . ?
N1 Zn1 O3 Tb1 41.1(4) 17_665 . . . ?
O1 Zn1 O3 Tb1 -29.9(8) 17_665 . . . ?
O4 Tb1 O3 C5 -90.0(3) 8_645 . . . ?
O4 Tb1 O3 C5 -7.9(2) . . . . ?
O4 Tb1 O3 C5 151.0(3) 11_556 . . . ?
O5 Tb1 O3 C5 -113.3(3) . . . . ?
O1 Tb1 O3 C5 114.1(3) 6_565 . . . ?
O1 Tb1 O3 C5 72.2(3) 9_654 . . . ?
O1 Tb1 O3 C5 18.2(3) 3_755 . . . ?
O3 Tb1 O3 C5 -169.9(2) 11_556 . . . ?
O3 Tb1 O3 C5 -56.7(3) 8_645 . . . ?
C5 Tb1 O3 C5 -62.8(2) 8_645 . . . ?
O4 Tb1 O3 Zn1 109.7(4) 8_645 . . . ?
O4 Tb1 O3 Zn1 -168.3(4) . . . . ?
O4 Tb1 O3 Zn1 -9.3(4) 11_556 . . . ?
O5 Tb1 O3 Zn1 86.4(4) . . . . ?
O1 Tb1 O3 Zn1 -46.2(4) 6_565 . . . ?
O1 Tb1 O3 Zn1 -88.2(4) 9_654 . . . ?
O1 Tb1 O3 Zn1 -142.2(3) 3_755 . . . ?
O3 Tb1 O3 Zn1 29.8(4) 11_556 . . . ?
O3 Tb1 O3 Zn1 143.0(3) 8_645 . . . ?
C5 Tb1 O3 Zn1 136.9(3) 8_645 . . . ?
C5 Tb1 O3 Zn1 -160.3(5) . . . . ?
O3 C5 O4 Tb1 -15.0(4) . . . . ?
C4 C5 O4 Tb1 163.5(4) . . . . ?
O4 Tb1 O4 C5 157.3(2) 8_645 . . . ?
O4 Tb1 O4 C5 -15.0(3) 11_556 . . . ?
O5 Tb1 O4 C5 71.1(3) . . . . ?
O1 Tb1 O4 C5 -106.1(3) 6_565 . . . ?
O1 Tb1 O4 C5 -70.4(3) 9_654 . . . ?
O1 Tb1 O4 C5 -148.9(3) 3_755 . . . ?
O3 Tb1 O4 C5 8.0(2) . . . . ?
O3 Tb1 O4 C5 49.7(4) 11_556 . . . ?
O3 Tb1 O4 C5 138.2(3) 8_645 . . . ?
C5 Tb1 O4 C5 150.7(3) 8_645 . . . ?

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
O5 H5A O2 0.87 2.59 3.373(4) 151.0 14_556
O5 H5B O2 0.98 2.54 3.373(4) 142.9 24_657
O6 H6A O6 0.85 2.40 3.25(10) 180.0 13_656

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.178


data_yzr-3
_database_code_depnum_ccdc_archive 'CCDC 869780'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H5 N6 O13 Y Zn3'
_chemical_formula_weight         762.27

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'
Y Y -2.7962 3.5667 '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           Cubic
_symmetry_space_group_name_H-M   Pa-3

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

_cell_length_a                   16.2486(17)
_cell_length_b                   16.2486(17)
_cell_length_c                   16.2486(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4289.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9221
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      32.84

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2960
_exptl_absorpt_coefficient_mu    6.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4075
_exptl_absorpt_correction_T_max  0.4075
_exptl_absorpt_process_details   Sadabs

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38823
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         33.18
_reflns_number_total             2737
_reflns_number_gt                2246
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0251P)^2^+4.5050P] 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         2737
_refine_ls_number_parameters     117
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0609
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.265903(10) 0.734097(10) 0.234097(10) 0.00836(6) Uani 1 3 d S . .
Zn1 Zn -0.010163(14) 0.678774(13) 0.204565(13) 0.01210(6) Uani 1 1 d . . .
C1 C -0.05038(11) 0.75820(13) -0.12429(11) 0.0150(3) Uani 1 1 d . . .
C2 C -0.01250(12) 0.75131(13) -0.04258(12) 0.0163(4) Uani 1 1 d . . .
C3 C 0.06567(12) 0.77449(14) -0.01691(12) 0.0204(4) Uani 1 1 d . . .
H3 H 0.1075 0.7988 -0.0476 0.024 Uiso 1 1 calc R . .
C4 C 0.06622(11) 0.75273(12) 0.06492(12) 0.0142(3) Uani 1 1 d . . .
C5 C 0.12977(11) 0.75861(11) 0.12875(11) 0.0122(3) Uani 1 1 d . . .
N1 N -0.05602(10) 0.71842(10) 0.02005(9) 0.0130(3) Uani 1 1 d . . .
N2 N -0.00714(9) 0.71855(10) 0.08672(9) 0.0120(3) Uani 1 1 d . . .
O1 O -0.12775(8) 0.74304(9) -0.12905(8) 0.0141(3) Uani 1 1 d . . .
O2 O -0.00339(9) 0.77728(12) -0.18158(9) 0.0260(4) Uani 1 1 d . . .
O3 O 0.11429(9) 0.72384(9) 0.19719(8) 0.0166(3) Uani 1 1 d . . .
O4 O 0.19728(8) 0.79431(9) 0.11661(9) 0.0160(3) Uani 1 1 d . . .
O5 O 0.17937(11) 0.82063(11) 0.32063(11) 0.0409(8) Uani 1 3 d SD . .
H5A H 0.2059(17) 0.823(3) 0.3649(12) 0.049 Uiso 0.33 1 d PRD . .
H5B H 0.179(3) 0.8682(11) 0.300(2) 0.049 Uiso 0.33 1 d PRD . .

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
Y1 0.00836(6) 0.00836(6) 0.00836(6) 0.00042(5) -0.00042(5) -0.00042(5)
Zn1 0.01455(10) 0.01302(10) 0.00874(10) 0.00118(7) 0.00079(7) -0.00172(7)
C1 0.0123(8) 0.0223(9) 0.0104(8) 0.0038(7) -0.0019(6) -0.0027(7)
C2 0.0122(8) 0.0268(10) 0.0100(7) 0.0061(7) -0.0025(6) -0.0047(7)
C3 0.0125(8) 0.0356(12) 0.0131(8) 0.0100(8) -0.0015(7) -0.0083(8)
C4 0.0104(8) 0.0205(9) 0.0118(8) 0.0039(6) -0.0024(6) -0.0030(6)
C5 0.0116(8) 0.0126(8) 0.0125(8) -0.0002(6) -0.0023(6) 0.0015(6)
N1 0.0108(7) 0.0190(8) 0.0092(7) 0.0028(5) -0.0013(5) -0.0022(6)
N2 0.0101(6) 0.0162(7) 0.0098(6) 0.0023(5) -0.0015(5) -0.0016(5)
O1 0.0107(6) 0.0202(7) 0.0114(6) 0.0012(5) -0.0017(5) -0.0030(5)
O2 0.0146(7) 0.0502(11) 0.0132(6) 0.0122(7) -0.0015(5) -0.0070(7)
O3 0.0135(6) 0.0248(7) 0.0114(6) 0.0041(5) -0.0028(5) -0.0022(5)
O4 0.0122(6) 0.0181(7) 0.0177(7) 0.0048(5) -0.0047(5) -0.0036(5)
O5 0.0409(8) 0.0409(8) 0.0409(8) -0.0118(8) 0.0118(8) 0.0118(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
Y1 O4 2.4176(14) 11_655 ?
Y1 O4 2.4177(14) 6_564 ?
Y1 O4 2.4177(14) . ?
Y1 O5 2.435(3) . ?
Y1 O1 2.4571(13) 10_455 ?
Y1 O1 2.4571(14) 3_565 ?
Y1 O1 2.4571(14) 7_556 ?
Y1 O3 2.5409(14) 11_655 ?
Y1 O3 2.5409(14) . ?
Y1 O3 2.5409(14) 6_564 ?
Y1 C5 2.8251(18) 6_564 ?
Y1 C5 2.8251(18) . ?
Zn1 O2 1.9860(15) 16_576 ?
Zn1 N2 2.0215(15) . ?
Zn1 N1 2.0665(16) 20_565 ?
Zn1 O3 2.1540(14) . ?
Zn1 O1 2.1931(14) 20_565 ?
C1 O2 1.243(2) . ?
C1 O1 1.283(2) . ?
C1 C2 1.468(3) . ?
C2 N1 1.350(2) . ?
C2 C3 1.389(3) . ?
C3 C4 1.376(3) . ?
C3 H3 0.9300 . ?
C4 N2 1.362(2) . ?
C4 C5 1.467(3) . ?
C5 O4 1.256(2) . ?
C5 O3 1.273(2) . ?
N1 N2 1.343(2) . ?
N1 Zn1 2.0665(16) 22_665 ?
O1 Zn1 2.1931(14) 22_665 ?
O1 Y1 2.4571(13) 3_465 ?
O2 Zn1 1.9861(15) 16_575 ?
O5 H5A 0.8398 . ?
O5 H5B 0.8399 . ?

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 Y1 O4 119.811(6) 11_655 6_564 ?
O4 Y1 O4 119.806(6) 11_655 . ?
O4 Y1 O4 119.807(5) 6_564 . ?
O4 Y1 O5 87.48(4) 11_655 . ?
O4 Y1 O5 87.48(4) 6_564 . ?
O4 Y1 O5 87.48(4) . . ?
O4 Y1 O1 73.42(5) 11_655 10_455 ?
O4 Y1 O1 136.42(5) 6_564 10_455 ?
O4 Y1 O1 69.88(5) . 10_455 ?
O5 Y1 O1 136.04(3) . 10_455 ?
O4 Y1 O1 136.42(5) 11_655 3_565 ?
O4 Y1 O1 69.88(5) 6_564 3_565 ?
O4 Y1 O1 73.42(5) . 3_565 ?
O5 Y1 O1 136.04(3) . 3_565 ?
O1 Y1 O1 73.91(5) 10_455 3_565 ?
O4 Y1 O1 69.89(5) 11_655 7_556 ?
O4 Y1 O1 73.42(5) 6_564 7_556 ?
O4 Y1 O1 136.42(5) . 7_556 ?
O5 Y1 O1 136.04(3) . 7_556 ?
O1 Y1 O1 73.91(5) 10_455 7_556 ?
O1 Y1 O1 73.91(5) 3_565 7_556 ?
O4 Y1 O3 52.63(4) 11_655 11_655 ?
O4 Y1 O3 70.41(5) 6_564 11_655 ?
O4 Y1 O3 153.04(5) . 11_655 ?
O5 Y1 O3 67.32(3) . 11_655 ?
O1 Y1 O3 121.86(4) 10_455 11_655 ?
O1 Y1 O3 131.54(5) 3_565 11_655 ?
O1 Y1 O3 69.01(5) 7_556 11_655 ?
O4 Y1 O3 70.41(5) 11_655 . ?
O4 Y1 O3 153.04(5) 6_564 . ?
O4 Y1 O3 52.63(4) . . ?
O5 Y1 O3 67.32(3) . . ?
O1 Y1 O3 69.01(5) 10_455 . ?
O1 Y1 O3 121.86(4) 3_565 . ?
O1 Y1 O3 131.53(5) 7_556 . ?
O3 Y1 O3 106.08(4) 11_655 . ?
O4 Y1 O3 153.04(5) 11_655 6_564 ?
O4 Y1 O3 52.63(4) 6_564 6_564 ?
O4 Y1 O3 70.41(5) . 6_564 ?
O5 Y1 O3 67.32(3) . 6_564 ?
O1 Y1 O3 131.53(5) 10_455 6_564 ?
O1 Y1 O3 69.02(5) 3_565 6_564 ?
O1 Y1 O3 121.86(4) 7_556 6_564 ?
O3 Y1 O3 106.08(4) 11_655 6_564 ?
O3 Y1 O3 106.08(4) . 6_564 ?
O4 Y1 C5 142.98(5) 11_655 6_564 ?
O4 Y1 C5 26.28(5) 6_564 6_564 ?
O4 Y1 C5 94.24(5) . 6_564 ?
O5 Y1 C5 79.42(4) . 6_564 ?
O1 Y1 C5 137.28(5) 10_455 6_564 ?
O1 Y1 C5 63.48(5) 3_565 6_564 ?
O1 Y1 C5 96.22(5) 7_556 6_564 ?
O3 Y1 C5 90.48(5) 11_655 6_564 ?
O3 Y1 C5 132.23(5) . 6_564 ?
O3 Y1 C5 26.77(5) 6_564 6_564 ?
O4 Y1 C5 94.24(5) 11_655 . ?
O4 Y1 C5 142.98(5) 6_564 . ?
O4 Y1 C5 26.29(5) . . ?
O5 Y1 C5 79.42(4) . . ?
O1 Y1 C5 63.48(5) 10_455 . ?
O1 Y1 C5 96.22(5) 3_565 . ?
O1 Y1 C5 137.28(5) 7_556 . ?
O3 Y1 C5 132.23(5) 11_655 . ?
O3 Y1 C5 26.77(5) . . ?
O3 Y1 C5 90.48(5) 6_564 . ?
C5 Y1 C5 116.71(2) 6_564 . ?
O2 Zn1 N2 140.00(7) 16_576 . ?
O2 Zn1 N1 103.44(7) 16_576 20_565 ?
N2 Zn1 N1 113.95(6) . 20_565 ?
O2 Zn1 O3 82.97(6) 16_576 . ?
N2 Zn1 O3 79.38(6) . . ?
N1 Zn1 O3 96.38(6) 20_565 . ?
O2 Zn1 O1 85.36(6) 16_576 20_565 ?
N2 Zn1 O1 114.35(6) . 20_565 ?
N1 Zn1 O1 79.24(5) 20_565 20_565 ?
O3 Zn1 O1 166.23(5) . 20_565 ?
O2 C1 O1 127.18(18) . . ?
O2 C1 C2 116.03(17) . . ?
O1 C1 C2 116.79(16) . . ?
N1 C2 C3 111.10(16) . . ?
N1 C2 C1 119.51(16) . . ?
C3 C2 C1 129.39(17) . . ?
C4 C3 C2 103.09(16) . . ?
C4 C3 H3 128.5 . . ?
C2 C3 H3 128.5 . . ?
N2 C4 C3 110.52(16) . . ?
N2 C4 C5 117.31(16) . . ?
C3 C4 C5 132.15(17) . . ?
O4 C5 O3 120.99(17) . . ?
O4 C5 C4 122.26(17) . . ?
O3 C5 C4 116.73(16) . . ?
O4 C5 Y1 58.45(9) . . ?
O3 C5 Y1 64.07(10) . . ?
C4 C5 Y1 166.05(13) . . ?
N2 N1 C2 107.33(15) . . ?
N2 N1 Zn1 139.68(12) . 22_665 ?
C2 N1 Zn1 111.69(12) . 22_665 ?
N1 N2 C4 107.96(15) . . ?
N1 N2 Zn1 138.50(12) . . ?
C4 N2 Zn1 113.46(12) . . ?
C1 O1 Zn1 111.83(11) . 22_665 ?
C1 O1 Y1 134.57(12) . 3_465 ?
Zn1 O1 Y1 112.90(5) 22_665 3_465 ?
C1 O2 Zn1 138.86(14) . 16_575 ?
C5 O3 Zn1 112.65(12) . . ?
C5 O3 Y1 89.17(11) . . ?
Zn1 O3 Y1 156.83(7) . . ?
C5 O4 Y1 95.27(11) . . ?
Y1 O5 H5A 103.2 . . ?
Y1 O5 H5B 108.2 . . ?
H5A O5 H5B 107.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 -169.5(2) . . . . ?
O1 C1 C2 N1 9.7(3) . . . . ?
O2 C1 C2 C3 10.5(4) . . . . ?
O1 C1 C2 C3 -170.2(2) . . . . ?
N1 C2 C3 C4 0.4(3) . . . . ?
C1 C2 C3 C4 -179.6(2) . . . . ?
C2 C3 C4 N2 0.1(2) . . . . ?
C2 C3 C4 C5 178.9(2) . . . . ?
N2 C4 C5 O4 -174.84(17) . . . . ?
C3 C4 C5 O4 6.4(4) . . . . ?
N2 C4 C5 O3 6.9(3) . . . . ?
C3 C4 C5 O3 -171.9(2) . . . . ?
N2 C4 C5 Y1 96.6(5) . . . . ?
C3 C4 C5 Y1 -82.1(6) . . . . ?
O4 Y1 C5 O4 -167.28(13) 11_655 . . . ?
O4 Y1 C5 O4 34.87(12) 6_564 . . . ?
O5 Y1 C5 O4 106.09(11) . . . . ?
O1 Y1 C5 O4 -98.19(12) 10_455 . . . ?
O1 Y1 C5 O4 -29.66(12) 3_565 . . . ?
O1 Y1 C5 O4 -102.63(12) 7_556 . . . ?
O3 Y1 C5 O4 151.71(10) 11_655 . . . ?
O3 Y1 C5 O4 166.04(18) . . . . ?
O3 Y1 C5 O4 39.28(11) 6_564 . . . ?
C5 Y1 C5 O4 33.73(15) 6_564 . . . ?
O4 Y1 C5 O3 26.68(11) 11_655 . . . ?
O4 Y1 C5 O3 -131.16(11) 6_564 . . . ?
O4 Y1 C5 O3 -166.04(18) . . . . ?
O5 Y1 C5 O3 -59.95(10) . . . . ?
O1 Y1 C5 O3 95.78(11) 10_455 . . . ?
O1 Y1 C5 O3 164.31(11) 3_565 . . . ?
O1 Y1 C5 O3 91.34(12) 7_556 . . . ?
O3 Y1 C5 O3 -14.32(12) 11_655 . . . ?
O3 Y1 C5 O3 -126.75(13) 6_564 . . . ?
C5 Y1 C5 O3 -132.31(8) 6_564 . . . ?
O4 Y1 C5 C4 -70.0(5) 11_655 . . . ?
O4 Y1 C5 C4 132.1(5) 6_564 . . . ?
O4 Y1 C5 C4 97.2(6) . . . . ?
O5 Y1 C5 C4 -156.7(5) . . . . ?
O1 Y1 C5 C4 -0.9(5) 10_455 . . . ?
O1 Y1 C5 C4 67.6(5) 3_565 . . . ?
O1 Y1 C5 C4 -5.4(6) 7_556 . . . ?
O3 Y1 C5 C4 -111.0(5) 11_655 . . . ?
O3 Y1 C5 C4 -96.7(6) . . . . ?
O3 Y1 C5 C4 136.5(5) 6_564 . . . ?
C5 Y1 C5 C4 131.0(5) 6_564 . . . ?
C3 C2 N1 N2 -0.8(2) . . . . ?
C1 C2 N1 N2 179.28(18) . . . . ?
C3 C2 N1 Zn1 168.85(15) . . . 22_665 ?
C1 C2 N1 Zn1 -11.1(2) . . . 22_665 ?
C2 N1 N2 C4 0.8(2) . . . . ?
Zn1 N1 N2 C4 -164.24(16) 22_665 . . . ?
C2 N1 N2 Zn1 -175.57(16) . . . . ?
Zn1 N1 N2 Zn1 19.4(3) 22_665 . . . ?
C3 C4 N2 N1 -0.6(2) . . . . ?
C5 C4 N2 N1 -179.58(16) . . . . ?
C3 C4 N2 Zn1 176.84(15) . . . . ?
C5 C4 N2 Zn1 -2.2(2) . . . . ?
O2 Zn1 N2 N1 -119.67(19) 16_576 . . . ?
N1 Zn1 N2 N1 82.7(2) 20_565 . . . ?
O3 Zn1 N2 N1 175.0(2) . . . . ?
O1 Zn1 N2 N1 -6.0(2) 20_565 . . . ?
O2 Zn1 N2 C4 64.09(17) 16_576 . . . ?
N1 Zn1 N2 C4 -93.58(14) 20_565 . . . ?
O3 Zn1 N2 C4 -1.26(13) . . . . ?
O1 Zn1 N2 C4 177.75(12) 20_565 . . . ?
O2 C1 O1 Zn1 176.26(19) . . . 22_665 ?
C2 C1 O1 Zn1 -2.9(2) . . . 22_665 ?
O2 C1 O1 Y1 -14.3(3) . . . 3_465 ?
C2 C1 O1 Y1 166.57(13) . . . 3_465 ?
O1 C1 O2 Zn1 18.7(4) . . . 16_575 ?
C2 C1 O2 Zn1 -162.17(18) . . . 16_575 ?
O4 C5 O3 Zn1 174.13(14) . . . . ?
C4 C5 O3 Zn1 -7.5(2) . . . . ?
Y1 C5 O3 Zn1 -171.99(11) . . . . ?
O4 C5 O3 Y1 -13.88(18) . . . . ?
C4 C5 O3 Y1 164.45(15) . . . . ?
O2 Zn1 O3 C5 -138.94(14) 16_576 . . . ?
N2 Zn1 O3 C5 5.00(13) . . . . ?
N1 Zn1 O3 C5 118.24(13) 20_565 . . . ?
O1 Zn1 O3 C5 -171.20(19) 20_565 . . . ?
O2 Zn1 O3 Y1 61.79(18) 16_576 . . . ?
N2 Zn1 O3 Y1 -154.27(19) . . . . ?
N1 Zn1 O3 Y1 -41.03(19) 20_565 . . . ?
O1 Zn1 O3 Y1 29.5(4) 20_565 . . . ?
O4 Y1 O3 C5 -151.62(12) 11_655 . . . ?
O4 Y1 O3 C5 90.72(14) 6_564 . . . ?
O4 Y1 O3 C5 7.73(10) . . . . ?
O5 Y1 O3 C5 112.75(11) . . . . ?
O1 Y1 O3 C5 -72.45(11) 10_455 . . . ?
O1 Y1 O3 C5 -18.46(13) 3_565 . . . ?
O1 Y1 O3 C5 -115.03(11) 7_556 . . . ?
O3 Y1 O3 C5 169.01(9) 11_655 . . . ?
O3 Y1 O3 C5 56.49(13) 6_564 . . . ?
C5 Y1 O3 C5 63.15(9) 6_564 . . . ?
O4 Y1 O3 Zn1 9.31(17) 11_655 . . . ?
O4 Y1 O3 Zn1 -108.34(19) 6_564 . . . ?
O4 Y1 O3 Zn1 168.7(2) . . . . ?
O5 Y1 O3 Zn1 -86.32(18) . . . . ?
O1 Y1 O3 Zn1 88.48(18) 10_455 . . . ?
O1 Y1 O3 Zn1 142.48(17) 3_565 . . . ?
O1 Y1 O3 Zn1 45.9(2) 7_556 . . . ?
O3 Y1 O3 Zn1 -30.1(2) 11_655 . . . ?
O3 Y1 O3 Zn1 -142.58(14) 6_564 . . . ?
C5 Y1 O3 Zn1 -135.92(17) 6_564 . . . ?
C5 Y1 O3 Zn1 160.9(3) . . . . ?
O3 C5 O4 Y1 14.66(19) . . . . ?
C4 C5 O4 Y1 -163.57(16) . . . . ?
O4 Y1 O4 C5 14.65(15) 11_655 . . . ?
O4 Y1 O4 C5 -156.62(9) 6_564 . . . ?
O5 Y1 O4 C5 -70.98(11) . . . . ?
O1 Y1 O4 C5 70.59(11) 10_455 . . . ?
O1 Y1 O4 C5 149.12(12) 3_565 . . . ?
O1 Y1 O4 C5 106.20(12) 7_556 . . . ?
O3 Y1 O4 C5 -50.72(17) 11_655 . . . ?
O3 Y1 O4 C5 -7.86(10) . . . . ?
O3 Y1 O4 C5 -137.78(12) 6_564 . . . ?
C5 Y1 O4 C5 -150.17(14) 6_564 . . . ?

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
O5 H5A O2 0.84 2.53 3.3691(19) 173.9 24_566
O5 H5B O2 0.84 2.53 3.3691(19) 172.9 17_566

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        33.18
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.096