
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C15 H7 O6 Zn), C3 H7 N O, 2(C2 H8 N)'
_chemical_formula_sum            'C37 H37 N3 O13 Zn2'
_chemical_formula_weight         862.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   13.6363(11)
_cell_length_b                   16.8584(15)
_cell_length_c                   8.2260(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1590(10)
_cell_angle_gamma                90.00
_cell_volume                     1866.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    145(13)
_cell_measurement_reflns_used    1566
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_T_max  0.7028
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      145(13)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6590
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3293
_reflns_number_gt                2605
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0351P)²+0.7059P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3293
_refine_ls_number_parameters     313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Zn1 Zn 0.36334(3) 1.02255(2) 0.37069(5) 0.02218(15) Uani 1 1 d . . .
N1 N 0.9573(5) 1.0002(4) 0.0303(7) 0.0321(15) Uani 0.50 1 d P . .
N2 N 0.6627(5) 0.8939(4) 0.2050(8) 0.032(2) Uani 0.495(9) 1 d P A 1
H2A H 0.7140 0.9280 0.2258 0.039 Uiso 0.495(9) 1 calc PR A 1
H2B H 0.6226 0.9027 0.2801 0.039 Uiso 0.495(9) 1 calc PR A 1
N2' N 0.6448(6) 0.8728(4) 0.0638(10) 0.030(2) Uani 0.505(9) 1 d P A 2
H2'1 H 0.5805 0.8740 0.0764 0.036 Uiso 0.505(9) 1 calc PR A 2
H2'2 H 0.6473 0.8651 -0.0438 0.036 Uiso 0.505(9) 1 calc PR A 2
O1 O 0.41806(18) 0.97879(13) 0.5970(3) 0.0262(6) Uani 1 1 d . . .
O2 O 0.5435(2) 0.89583(17) 0.6773(4) 0.0528(9) Uani 1 1 d . . .
O3 O 0.4744(4) 0.6235(3) 0.8033(8) 0.035(2) Uani 0.488(8) 1 d P B 1
O3' O 0.4615(4) 0.5986(3) 0.6432(7) 0.032(2) Uani 0.512(8) 1 d P B 2
O4 O 0.32057(17) 0.57198(14) 0.7407(3) 0.0280(6) Uani 1 1 d . . .
O5 O -0.23371(19) 0.86646(18) 0.8111(4) 0.0435(8) Uani 1 1 d . . .
O6 O -0.24243(19) 0.93192(16) 0.5704(3) 0.0391(7) Uani 1 1 d . . .
O7 O 0.8434(4) 0.9649(3) 0.1894(7) 0.0429(15) Uani 0.50 1 d P . .
C1 C -0.1975(3) 0.8869(2) 0.6880(5) 0.0311(9) Uani 1 1 d . . .
C2 C 0.4510(3) 0.9115(2) 0.6408(5) 0.0319(9) Uani 1 1 d . . .
C3 C 0.3838(10) 0.6311(8) 0.7566(15) 0.027(3) Uani 0.488(8) 1 d P B 1
C3' C 0.3815(10) 0.6164(7) 0.6836(15) 0.024(3) Uani 0.512(8) 1 d P B 2
C4 C -0.0940(2) 0.8612(2) 0.6728(4) 0.0236(8) Uani 1 1 d . . .
C5 C -0.0423(3) 0.8984(2) 0.5607(5) 0.0264(8) Uani 1 1 d . . .
H5 H -0.0745 0.9351 0.4862 0.032 Uiso 1 1 calc R . .
C6 C 0.0565(3) 0.88097(19) 0.5601(4) 0.0239(8) Uani 1 1 d . . .
H6 H 0.0912 0.9079 0.4886 0.029 Uiso 1 1 calc R . .
C7 C 0.1054(2) 0.82269(19) 0.6669(4) 0.0196(7) Uani 1 1 d . . .
C8 C 0.0518(2) 0.7833(2) 0.7726(4) 0.0231(8) Uani 1 1 d . . .
H8 H 0.0819 0.7434 0.8409 0.028 Uiso 1 1 calc R . .
C9 C -0.0462(3) 0.8033(2) 0.7768(4) 0.0258(8) Uani 1 1 d . . .
H9 H -0.0806 0.7775 0.8504 0.031 Uiso 1 1 calc R . .
C10 C 0.2119(2) 0.80354(19) 0.6674(4) 0.0196(8) Uani 1 1 d . . .
C11 C 0.2795(3) 0.8630(2) 0.6486(4) 0.0237(8) Uani 1 1 d . . .
H11 H 0.2574 0.9149 0.6302 0.028 Uiso 1 1 calc R . .
C12 C 0.3798(3) 0.8459(2) 0.6569(4) 0.0253(8) Uani 1 1 d . . .
C13 C 0.4126(3) 0.7684(2) 0.6796(5) 0.0348(10) Uani 1 1 d . B .
H13 H 0.4798 0.7569 0.6853 0.042 Uiso 1 1 calc R . .
C14 C 0.3459(3) 0.7076(2) 0.6939(5) 0.0327(10) Uani 1 1 d . . .
C15 C 0.2462(2) 0.7257(2) 0.6894(4) 0.0235(8) Uani 1 1 d . B .
H15 H 0.2015 0.6852 0.7013 0.028 Uiso 1 1 calc R . .
C16 C 0.8687(6) 1.0030(5) 0.0761(10) 0.0341(19) Uani 0.50 1 d P . .
H16 H 0.8218 1.0367 0.0176 0.041 Uiso 0.50 1 calc PR . .
C17 C 1.0240(4) 0.9455(3) 0.1070(5) 0.0529(13) Uani 1 1 d . . .
H17A H 1.0817 0.9725 0.1626 0.079 Uiso 1 1 d R . .
H17B H 1.0431 0.9099 0.0264 0.079 Uiso 1 1 d R . .
H17C H 0.9937 0.9159 0.1856 0.079 Uiso 1 1 d R . .
C18 C 0.6066(10) 0.9113(10) 0.0389(14) 0.068(4) Uani 0.495(9) 1 d P A 1
H18D H 0.6463 0.8972 -0.0432 0.102 Uiso 0.495(9) 1 calc PR A 1
H18E H 0.5912 0.9668 0.0306 0.102 Uiso 0.495(9) 1 calc PR A 1
H18F H 0.5462 0.8810 0.0220 0.102 Uiso 0.495(9) 1 calc PR A 1
C19 C 0.7013(19) 0.8125(16) 0.226(2) 0.044(4) Uani 0.495(9) 1 d P A 1
H19A H 0.6516 0.7760 0.1754 0.065 Uiso 0.495(9) 1 calc PR A 1
H19B H 0.7181 0.8007 0.3410 0.065 Uiso 0.495(9) 1 calc PR A 1
H19C H 0.7595 0.8078 0.1744 0.065 Uiso 0.495(9) 1 calc PR A 1
C18' C 0.6916(7) 0.9499(5) 0.1158(11) 0.047(3) Uani 0.505(9) 1 d P A 2
H18A H 0.6891 0.9584 0.2305 0.070 Uiso 0.505(9) 1 calc PR A 2
H18B H 0.6563 0.9918 0.0523 0.070 Uiso 0.505(9) 1 calc PR A 2
H18C H 0.7595 0.9497 0.0982 0.070 Uiso 0.505(9) 1 calc PR A 2
C19' C 0.6942(17) 0.8058(15) 0.1590(19) 0.043(4) Uani 0.505(9) 1 d P A 2
H19D H 0.7601 0.7996 0.1340 0.065 Uiso 0.505(9) 1 calc PR A 2
H19E H 0.6570 0.7581 0.1306 0.065 Uiso 0.505(9) 1 calc PR A 2
H19F H 0.6976 0.8162 0.2746 0.065 Uiso 0.505(9) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O6 1.948(2) 3_576 ?
Zn1 O2 1.955(2) 3_676 ?
Zn1 O4 1.956(2) 4_575 ?
Zn1 O1 2.031(3) . ?
N1 C16 1.322(10) . ?
N1 N1 1.337(13) 3_775 ?
N1 C17 1.375(8) . ?
N1 C17 1.508(8) 3_775 ?
N2 C19 1.47(3) . ?
N2 C18 1.484(14) . ?
N2' C19' 1.47(2) . ?
N2' C18' 1.482(12) . ?
O1 C2 1.252(4) . ?
O2 C2 1.276(5) . ?
O2 Zn1 1.955(2) 3_676 ?
O3 C3 1.240(15) . ?
O3' C3' 1.227(13) . ?
O4 C3' 1.264(12) . ?
O4 C3 1.311(14) . ?
O4 Zn1 1.956(2) 4_576 ?
O5 C1 1.244(4) . ?
O6 C1 1.303(5) . ?
O6 Zn1 1.948(2) 3_576 ?
O7 C16 1.226(9) . ?
C1 C4 1.501(5) . ?
C2 C12 1.492(5) . ?
C3 C14 1.454(14) . ?
C3' C14 1.619(13) . ?
C4 C9 1.390(5) . ?
C4 C5 1.396(5) . ?
C5 C6 1.379(5) . ?
C6 C7 1.413(5) . ?
C7 C8 1.391(4) . ?
C7 C10 1.487(5) . ?
C8 C9 1.383(5) . ?
C10 C11 1.387(4) . ?
C10 C15 1.396(5) . ?
C11 C12 1.389(5) . ?
C12 C13 1.385(5) . ?
C13 C14 1.387(5) . ?
C14 C15 1.388(5) . ?
C17 N1 1.508(8) 3_775 ?

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
O6 Zn1 O2 112.07(12) 3_576 3_676 ?
O6 Zn1 O4 105.45(11) 3_576 4_575 ?
O2 Zn1 O4 127.57(12) 3_676 4_575 ?
O6 Zn1 O1 96.73(11) 3_576 . ?
O2 Zn1 O1 106.55(12) 3_676 . ?
O4 Zn1 O1 103.86(10) 4_575 . ?
C16 N1 N1 174.4(9) . 3_775 ?
C16 N1 C17 117.4(6) . . ?
N1 N1 C17 67.5(6) 3_775 . ?
C16 N1 C17 117.5(7) . 3_775 ?
N1 N1 C17 57.5(5) 3_775 3_775 ?
C17 N1 C17 125.0(5) . 3_775 ?
C19 N2 C18 114.4(11) . . ?
C19' N2' C18' 112.3(11) . . ?
C2 O1 Zn1 131.0(2) . . ?
C2 O2 Zn1 117.1(2) . 3_676 ?
C3' O4 C3 29.0(5) . . ?
C3' O4 Zn1 122.0(6) . 4_576 ?
C3 O4 Zn1 115.5(6) . 4_576 ?
C1 O6 Zn1 111.2(2) . 3_576 ?
O5 C1 O6 124.4(3) . . ?
O5 C1 C4 119.2(4) . . ?
O6 C1 C4 116.3(3) . . ?
O1 C2 O2 123.5(3) . . ?
O1 C2 C12 119.2(3) . . ?
O2 C2 C12 117.3(3) . . ?
O3 C3 O4 124.1(11) . . ?
O3 C3 C14 118.8(11) . . ?
O4 C3 C14 116.6(10) . . ?
O3' C3' O4 128.4(11) . . ?
O3' C3' C14 122.3(9) . . ?
O4 C3' C14 108.8(8) . . ?
C9 C4 C5 119.1(3) . . ?
C9 C4 C1 120.4(3) . . ?
C5 C4 C1 120.4(3) . . ?
C6 C5 C4 120.1(3) . . ?
C5 C6 C7 120.7(3) . . ?
C8 C7 C6 118.5(3) . . ?
C8 C7 C10 120.4(3) . . ?
C6 C7 C10 121.1(3) . . ?
C9 C8 C7 120.4(3) . . ?
C8 C9 C4 121.0(3) . . ?
C11 C10 C15 118.6(3) . . ?
C11 C10 C7 120.6(3) . . ?
C15 C10 C7 120.8(3) . . ?
C10 C11 C12 120.8(3) . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 C2 120.7(3) . . ?
C11 C12 C2 119.5(3) . . ?
C12 C13 C14 120.4(3) . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 C3 118.9(6) . . ?
C15 C14 C3 119.8(6) . . ?
C13 C14 C3' 119.3(5) . . ?
C15 C14 C3' 120.5(5) . . ?
C3 C14 C3' 23.5(5) . . ?
C14 C15 C10 121.1(3) . . ?
O7 C16 N1 125.3(8) . . ?
N1 C17 N1 55.0(5) . 3_775 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.082

data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C15 H7 Cd O6), C3 H7 N O, 2(C2 H8 N)'
_chemical_formula_sum            'C37 H37 Cd2 N3 O13'
_chemical_formula_weight         956.50

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'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 2(1)/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   13.9411(8)
_cell_length_b                   17.0817(12)
_cell_length_c                   7.6680(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.974(9)
_cell_angle_gamma                90.00
_cell_volume                     1825.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    121.40(10)
_cell_measurement_reflns_used    1114
_cell_measurement_theta_min      2.7917
_cell_measurement_theta_max      28.3269

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7322
_exptl_absorpt_correction_T_max  0.7820
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      121.40(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6619
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3224
_reflns_number_gt                1736
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1024P)²+20.8486P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3224
_refine_ls_number_parameters     273
_refine_ls_number_restraints     829
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0810
_refine_ls_wR_factor_ref         0.2618
_refine_ls_wR_factor_gt          0.2001
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.057
_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
N2 N 0.5452(15) 0.4579(13) 0.014(3) 0.090(6) Uani 0.50 1 d PDU . .
Cd1 Cd 0.12674(6) 0.52202(5) 0.35893(19) 0.0707(6) Uani 1 1 d U . .
N1 N 0.1354(15) 0.6208(11) 0.783(3) 0.143(5) Uani 1 1 d DU . .
H1A H 0.1802 0.5923 0.7296 0.171 Uiso 1 1 calc R . .
H1B H 0.0803 0.6106 0.7223 0.171 Uiso 1 1 calc R . .
O1 O 0.0862(6) 0.4716(5) 0.6247(16) 0.0699(17) Uani 1 1 d U . .
O2 O -0.0231(5) 0.3817(5) 0.6732(13) 0.049(2) Uani 1 1 d U . .
O3 O 0.0733(5) 0.1024(5) 0.7502(13) 0.054(2) Uani 1 1 d U . .
O4 O 0.2237(5) 0.0706(4) 0.7314(12) 0.0450(19) Uani 1 1 d U . .
O5 O 0.7596(5) 0.3820(5) 0.7113(12) 0.048(2) Uani 1 1 d U . .
O6 O 0.7262(5) 0.4436(5) 0.4667(13) 0.050(2) Uani 1 1 d U . .
O7 O 0.4052(18) 0.5026(17) -0.051(4) 0.116(6) Uani 0.50 1 d PDU . .
C1 C 0.0639(8) 0.4023(7) 0.6511(18) 0.043(2) Uani 1 1 d U . .
C2 C 0.1601(7) 0.1208(6) 0.7205(17) 0.038(2) Uani 1 1 d U . .
C3 C 0.1388(7) 0.3402(6) 0.6542(17) 0.038(2) Uani 1 1 d U . .
C4 C 0.1139(7) 0.2619(6) 0.6805(17) 0.038(2) Uani 1 1 d U . .
H4 H 0.0500 0.2484 0.6945 0.046 Uiso 1 1 calc R . .
C5 C 0.1846(7) 0.2039(6) 0.6858(17) 0.037(2) Uani 1 1 d U . .
C6 C 0.2795(7) 0.2252(6) 0.6627(16) 0.036(2) Uani 1 1 d U . .
H6 H 0.3266 0.1866 0.6636 0.043 Uiso 1 1 calc R . .
C7 C 0.3059(7) 0.3032(6) 0.6382(16) 0.034(2) Uani 1 1 d U . .
C8 C 0.2338(7) 0.3597(7) 0.6342(17) 0.040(2) Uani 1 1 d U . .
H8 H 0.2502 0.4118 0.6177 0.048 Uiso 1 1 calc R . .
C9 C 0.7014(8) 0.4004(6) 0.5871(18) 0.038(2) Uani 1 1 d U . .
C10 C 0.6011(7) 0.3707(6) 0.5932(16) 0.031(2) Uani 1 1 d U . .
C11 C 0.5295(8) 0.4054(6) 0.4913(17) 0.039(2) Uani 1 1 d U . .
H11 H 0.5462 0.4446 0.4138 0.047 Uiso 1 1 calc R . .
C12 C 0.4336(7) 0.3842(6) 0.5000(16) 0.033(2) Uani 1 1 d U . .
H12 H 0.3867 0.4085 0.4298 0.040 Uiso 1 1 calc R . .
C13 C 0.4093(7) 0.3248(6) 0.6181(16) 0.030(2) Uani 1 1 d U . .
C14 C 0.4809(7) 0.2873(6) 0.7166(17) 0.035(2) Uani 1 1 d U . .
H14 H 0.4651 0.2461 0.7895 0.042 Uiso 1 1 calc R . .
C15 C 0.5755(7) 0.3108(7) 0.7070(17) 0.039(2) Uani 1 1 d U . .
H15 H 0.6225 0.2866 0.7769 0.047 Uiso 1 1 calc R . .
C16 C 0.1577(18) 0.7014(12) 0.725(4) 0.139(8) Uani 1 1 d DU . .
H16A H 0.1056 0.7209 0.6524 0.208 Uiso 1 1 calc R . .
H16B H 0.2154 0.7008 0.6599 0.208 Uiso 1 1 calc R . .
H16C H 0.1667 0.7346 0.8251 0.208 Uiso 1 1 calc R . .
C17 C 0.1225(16) 0.5759(14) 0.947(3) 0.125(7) Uani 1 1 d DU . .
H17A H 0.1136 0.6117 1.0415 0.187 Uiso 1 1 calc R . .
H17B H 0.1785 0.5445 0.9714 0.187 Uiso 1 1 calc R . .
H17C H 0.0673 0.5427 0.9334 0.187 Uiso 1 1 calc R . .
C19 C 0.4518(16) 0.4444(15) -0.001(3) 0.102(7) Uani 0.50 1 d PDU . .
H19 H 0.4228 0.3966 0.0211 0.123 Uiso 0.50 1 d PR . .
C20 C 0.587(2) 0.5345(15) -0.026(5) 0.099(7) Uani 0.50 1 d PDU . .
H20A H 0.6118 0.5576 0.0807 0.148 Uiso 0.50 1 d PR . .
H20B H 0.5389 0.5681 -0.0778 0.148 Uiso 0.50 1 d PR . .
H20C H 0.6383 0.5278 -0.1049 0.148 Uiso 0.50 1 d PR . .
C21 C 0.6160(19) 0.3976(15) 0.071(4) 0.086(5) Uani 0.50 1 d PDU . .
H21A H 0.6632 0.4205 0.1490 0.129 Uiso 0.50 1 d PR . .
H21B H 0.6469 0.3767 -0.0291 0.129 Uiso 0.50 1 d PR . .
H21C H 0.5833 0.3562 0.1293 0.129 Uiso 0.50 1 d PR . .


_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
N2 O7 1.00(4) 3_665 ?
N2 C19 1.323(9) . ?
N2 C20 1.470(10) . ?
N2 C21 1.481(9) . ?
N2 C19 1.67(4) 3_665 ?
N2 C20 1.85(5) 3_665 ?
Cd1 O2 2.198(8) 3_566 ?
Cd1 O1 2.301(12) . ?
Cd1 O4 2.319(8) 4_565 ?
Cd1 O5 2.355(8) 3_666 ?
Cd1 O3 2.393(9) 4_565 ?
Cd1 O6 2.479(9) 3_666 ?
Cd1 C2 2.708(11) 4_565 ?
Cd1 C9 2.757(11) 3_666 ?
N1 C16 1.483(10) . ?
N1 C17 1.489(10) . ?
O1 C1 1.242(14) . ?
O2 C1 1.279(12) . ?
O2 Cd1 2.198(8) 3_566 ?
O3 C2 1.279(12) . ?
O3 Cd1 2.393(9) 4_566 ?
O4 C2 1.234(13) . ?
O4 Cd1 2.319(8) 4_566 ?
O5 C9 1.269(15) . ?
O5 Cd1 2.355(8) 3_666 ?
O6 C9 1.241(14) . ?
O6 Cd1 2.479(9) 3_666 ?
O7 C20 0.87(4) 3_665 ?
O7 N2 1.00(4) 3_665 ?
O7 C19 1.241(10) . ?
O7 C21 1.74(4) 3_665 ?
C1 C3 1.489(15) . ?
C2 C5 1.485(15) . ?
C2 Cd1 2.708(11) 4_566 ?
C3 C8 1.379(14) . ?
C3 C4 1.398(15) . ?
C4 C5 1.398(15) . ?
C5 C6 1.390(14) . ?
C6 C7 1.397(15) . ?
C7 C8 1.392(14) . ?
C7 C13 1.502(14) . ?
C9 C10 1.490(14) . ?
C9 Cd1 2.757(11) 3_666 ?
C10 C11 1.380(15) . ?
C10 C15 1.398(15) . ?
C11 C12 1.390(14) . ?
C12 C13 1.410(15) . ?
C13 C14 1.386(15) . ?
C14 C15 1.383(14) . ?
C19 C20 0.69(5) 3_665 ?
C19 N2 1.67(4) 3_665 ?
C20 C19 0.69(5) 3_665 ?
C20 O7 0.87(4) 3_665 ?
C20 N2 1.85(5) 3_665 ?
C21 O7 1.74(4) 3_665 ?

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
O7 N2 C19 144(2) 3_665 . ?
O7 N2 C20 35(2) 3_665 . ?
C19 N2 C20 122.2(13) . . ?
O7 N2 C21 87(2) 3_665 . ?
C19 N2 C21 123.3(14) . . ?
C20 N2 C21 114.5(13) . . ?
O7 N2 C19 47.6(17) 3_665 3_665 ?
C19 N2 C19 101.2(16) . 3_665 ?
C20 N2 C19 24.3(17) . 3_665 ?
C21 N2 C19 134.0(18) . 3_665 ?
O7 N2 C20 128(3) 3_665 3_665 ?
C19 N2 C20 16.1(13) . 3_665 ?
C20 N2 C20 110.5(16) . 3_665 ?
C21 N2 C20 133.5(18) . 3_665 ?
C19 N2 C20 87.7(18) 3_665 3_665 ?
O2 Cd1 O1 101.5(3) 3_566 . ?
O2 Cd1 O4 148.6(3) 3_566 4_565 ?
O1 Cd1 O4 106.4(3) . 4_565 ?
O2 Cd1 O5 84.2(3) 3_566 3_666 ?
O1 Cd1 O5 130.6(3) . 3_666 ?
O4 Cd1 O5 88.4(3) 4_565 3_666 ?
O2 Cd1 O3 115.5(3) 3_566 4_565 ?
O1 Cd1 O3 83.8(3) . 4_565 ?
O4 Cd1 O3 55.0(3) 4_565 4_565 ?
O5 Cd1 O3 138.0(3) 3_666 4_565 ?
O2 Cd1 O6 114.3(3) 3_566 3_666 ?
O1 Cd1 O6 80.5(3) . 3_666 ?
O4 Cd1 O6 84.6(3) 4_565 3_666 ?
O5 Cd1 O6 53.7(3) 3_666 3_666 ?
O3 Cd1 O6 129.8(3) 4_565 3_666 ?
O2 Cd1 C2 138.8(3) 3_566 4_565 ?
O1 Cd1 C2 93.5(3) . 4_565 ?
O4 Cd1 C2 27.0(3) 4_565 4_565 ?
O5 Cd1 C2 114.3(3) 3_666 4_565 ?
O3 Cd1 C2 28.2(3) 4_565 4_565 ?
O6 Cd1 C2 105.9(3) 3_666 4_565 ?
O2 Cd1 C9 102.8(3) 3_566 3_666 ?
O1 Cd1 C9 106.6(4) . 3_666 ?
O4 Cd1 C9 82.8(3) 4_565 3_666 ?
O5 Cd1 C9 27.3(3) 3_666 3_666 ?
O3 Cd1 C9 137.6(3) 4_565 3_666 ?
O6 Cd1 C9 26.8(3) 3_666 3_666 ?
C2 Cd1 C9 109.4(3) 4_565 3_666 ?
C16 N1 C17 140(2) . . ?
C1 O1 Cd1 124.9(10) . . ?
C1 O2 Cd1 113.6(7) . 3_566 ?
C2 O3 Cd1 89.7(7) . 4_566 ?
C2 O4 Cd1 94.3(7) . 4_566 ?
C9 O5 Cd1 94.2(7) . 3_666 ?
C9 O6 Cd1 89.2(7) . 3_666 ?
C20 O7 N2 103(4) 3_665 3_665 ?
C20 O7 C19 32(3) 3_665 . ?
N2 O7 C19 96(3) 3_665 . ?
C20 O7 C21 142(4) 3_665 3_665 ?
N2 O7 C21 58.3(19) 3_665 3_665 ?
C19 O7 C21 154(2) . 3_665 ?
O1 C1 O2 121.9(10) . . ?
O1 C1 C3 120.1(10) . . ?
O2 C1 C3 118.0(10) . . ?
O4 C2 O3 120.0(10) . . ?
O4 C2 C5 120.5(9) . . ?
O3 C2 C5 119.4(10) . . ?
O4 C2 Cd1 58.7(6) . 4_566 ?
O3 C2 Cd1 62.1(6) . 4_566 ?
C5 C2 Cd1 167.1(9) . 4_566 ?
C8 C3 C4 119.4(10) . . ?
C8 C3 C1 120.2(10) . . ?
C4 C3 C1 120.4(9) . . ?
C3 C4 C5 120.3(10) . . ?
C6 C5 C4 118.9(10) . . ?
C6 C5 C2 119.9(10) . . ?
C4 C5 C2 121.1(9) . . ?
C5 C6 C7 121.5(10) . . ?
C8 C7 C6 118.1(9) . . ?
C8 C7 C13 121.5(9) . . ?
C6 C7 C13 120.4(9) . . ?
C3 C8 C7 121.7(10) . . ?
O6 C9 O5 121.3(11) . . ?
O6 C9 C10 120.8(11) . . ?
O5 C9 C10 117.9(11) . . ?
O6 C9 Cd1 64.1(6) . 3_666 ?
O5 C9 Cd1 58.4(6) . 3_666 ?
C10 C9 Cd1 166.2(8) . 3_666 ?
C11 C10 C15 118.2(9) . . ?
C11 C10 C9 119.8(10) . . ?
C15 C10 C9 121.9(10) . . ?
C10 C11 C12 122.6(11) . . ?
C11 C12 C13 118.1(10) . . ?
C14 C13 C12 119.9(9) . . ?
C14 C13 C7 120.4(10) . . ?
C12 C13 C7 119.7(9) . . ?
C15 C14 C13 120.4(11) . . ?
C14 C15 C10 120.6(10) . . ?
C20 C19 O7 43(4) 3_665 . ?
C20 C19 N2 132(4) 3_665 . ?
O7 C19 N2 113.1(16) . . ?
C20 C19 N2 61(3) 3_665 3_665 ?
O7 C19 N2 36.5(15) . 3_665 ?
N2 C19 N2 78.8(16) . 3_665 ?
C19 C20 O7 105(6) 3_665 3_665 ?
C19 C20 N2 95(4) 3_665 . ?
O7 C20 N2 42(2) 3_665 . ?
C19 C20 N2 32(3) 3_665 3_665 ?
O7 C20 N2 97(3) 3_665 3_665 ?
N2 C20 N2 69.5(16) . 3_665 ?
N2 C21 O7 35.1(13) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.299
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.174

data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H18 N2 O6 Zn'
_chemical_formula_sum            'C27 H18 N2 O6 Zn'
_chemical_formula_weight         531.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   15.1064(14)
_cell_length_b                   13.6928(12)
_cell_length_c                   22.126(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4576.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    121.40(10)
_cell_measurement_reflns_used    2150
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      28.46

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2176
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6345
_exptl_absorpt_correction_T_max  0.7021
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      121.40(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15962
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4034
_reflns_number_gt                2891
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0292P)²+8.0928P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4034
_refine_ls_number_parameters     354
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.0968
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.77774(3) 0.01919(3) 0.94345(2) 0.02337(15) Uani 1 1 d U . .
N1 N 0.7529(2) -0.0564(2) 0.86621(15) 0.0302(8) Uani 1 1 d . . .
N2 N 0.8000(2) -0.4134(2) 0.50780(15) 0.0304(8) Uani 1 1 d . . .
O1 O 1.16613(19) 0.4453(2) 1.01948(13) 0.0370(7) Uani 1 1 d . . .
O2 O 1.1048(2) 0.3365(2) 1.08148(13) 0.0427(8) Uani 1 1 d . . .
O3 O 0.8759(2) 0.1151(2) 0.98697(19) 0.0623(10) Uani 1 1 d U . .
O4 O 0.8326(2) 0.1392(2) 0.89466(18) 0.0546(10) Uani 1 1 d U . .
O5 O 1.0211(4) 0.2779(5) 0.6567(3) 0.0315(18) Uani 0.637(18) 1 d P A 2
H5 H 1.0198 0.2510 0.6236 0.047 Uiso 0.637(18) 1 calc PR A 2
O6 O 1.0439(5) 0.4138(9) 0.6009(4) 0.039(2) Uani 0.637(18) 1 d P A 2
O5' O 1.0058(16) 0.4389(12) 0.6037(9) 0.071(6) Uani 0.363(18) 1 d P A 1
H5' H 0.9813 0.4125 0.5749 0.107 Uiso 0.363(18) 1 calc PR A 1
O6' O 0.967(2) 0.3019(16) 0.6512(6) 0.109(10) Uani 0.363(18) 1 d P A 1
C1 C 1.1107(3) 0.3785(3) 1.03203(18) 0.0297(10) Uani 1 1 d . . .
C2 C 0.8791(3) 0.1623(3) 0.9390(3) 0.0464(14) Uani 1 1 d . . .
C3 C 1.0314(6) 0.3747(11) 0.6490(7) 0.030(3) Uani 0.637(18) 1 d P A 2
C3' C 0.991(2) 0.388(2) 0.6529(12) 0.061(7) Uani 0.363(18) 1 d P A 1
C4 C 1.0513(3) 0.3521(3) 0.98041(17) 0.0256(9) Uani 1 1 d . . .
C5 C 0.9932(3) 0.2732(3) 0.9849(2) 0.0319(10) Uani 1 1 d . . .
H5A H 0.9885 0.2386 1.0210 0.038 Uiso 1 1 calc R . .
C6 C 0.9423(3) 0.2468(3) 0.9349(2) 0.0330(11) Uani 1 1 d . . .
C7 C 0.9488(3) 0.2982(3) 0.88157(19) 0.0303(10) Uani 1 1 d . . .
H7 H 0.9141 0.2802 0.8487 0.036 Uiso 1 1 calc R . .
C8 C 1.0067(3) 0.3769(3) 0.87611(18) 0.0254(9) Uani 1 1 d . . .
C9 C 1.0570(3) 0.4024(3) 0.92645(17) 0.0240(9) Uani 1 1 d . . .
H9 H 1.0956 0.4551 0.9236 0.029 Uiso 1 1 calc R . .
C10 C 1.0162(3) 0.4310(3) 0.81799(18) 0.0265(9) Uani 1 1 d . . .
C11 C 1.0108(3) 0.3819(3) 0.76329(19) 0.0344(11) Uani 1 1 d . A .
H11 H 0.9991 0.3153 0.7630 0.041 Uiso 1 1 calc R . .
C12 C 1.0229(3) 0.4313(3) 0.70873(19) 0.0372(11) Uani 1 1 d . . .
C13 C 1.0419(3) 0.5305(3) 0.70909(19) 0.0361(11) Uani 1 1 d . A .
H13 H 1.0516 0.5636 0.6730 0.043 Uiso 1 1 calc R . .
C14 C 1.0464(3) 0.5793(3) 0.7634(2) 0.0411(12) Uani 1 1 d . . .
H14 H 1.0583 0.6460 0.7638 0.049 Uiso 1 1 calc R A .
C15 C 1.0335(3) 0.5307(3) 0.81746(19) 0.0354(11) Uani 1 1 d . A .
H15 H 1.0365 0.5649 0.8537 0.043 Uiso 1 1 calc R . .
C16 C 0.7191(3) -0.0088(3) 0.81848(19) 0.0339(10) Uani 1 1 d . . .
H16 H 0.6990 0.0547 0.8240 0.041 Uiso 1 1 calc R . .
C17 C 0.7129(3) -0.0495(3) 0.7619(2) 0.0414(12) Uani 1 1 d . . .
H17 H 0.6894 -0.0134 0.7301 0.050 Uiso 1 1 calc R . .
C18 C 0.7413(3) -0.1434(3) 0.7523(2) 0.0382(11) Uani 1 1 d . . .
C19 C 0.7716(4) -0.1945(3) 0.8019(2) 0.0481(14) Uani 1 1 d . . .
H19 H 0.7888 -0.2594 0.7977 0.058 Uiso 1 1 calc R . .
C20 C 0.7765(3) -0.1491(3) 0.8581(2) 0.0428(13) Uani 1 1 d . . .
H20 H 0.7970 -0.1848 0.8911 0.051 Uiso 1 1 calc R . .
C21 C 0.7401(3) -0.1881(4) 0.6915(2) 0.0432(12) Uani 1 1 d . . .
H21 H 0.6991 -0.1650 0.6636 0.052 Uiso 1 1 calc R . .
C22 C 0.7933(3) -0.2578(3) 0.6748(2) 0.0410(12) Uani 1 1 d . . .
H22 H 0.8345 -0.2786 0.7033 0.049 Uiso 1 1 calc R . .
C23 C 0.7954(3) -0.3072(3) 0.61570(19) 0.0336(11) Uani 1 1 d . . .
C24 C 0.7308(4) -0.2965(4) 0.5721(2) 0.0502(14) Uani 1 1 d . . .
H24 H 0.6846 -0.2525 0.5778 0.060 Uiso 1 1 calc R . .
C25 C 0.7349(3) -0.3511(3) 0.5203(2) 0.0480(14) Uani 1 1 d . . .
H25 H 0.6896 -0.3443 0.4922 0.058 Uiso 1 1 calc R . .
C26 C 0.8642(3) -0.4215(4) 0.5488(2) 0.0440(13) Uani 1 1 d . . .
H26 H 0.9116 -0.4629 0.5406 0.053 Uiso 1 1 calc RD . .
C27 C 0.8633(3) -0.3711(4) 0.6027(2) 0.0466(13) Uani 1 1 d . . .
H27 H 0.9087 -0.3803 0.6305 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.937(3) 4_457 ?
Zn1 N1 2.033(3) . ?
Zn1 N2 2.058(3) 7_556 ?
Zn1 O4 2.133(3) . ?
Zn1 O3 2.203(3) . ?
N1 C20 1.331(5) . ?
N1 C16 1.342(5) . ?
N2 C25 1.331(5) . ?
N2 C26 1.332(5) . ?
N2 Zn1 2.058(3) 7 ?
O1 C1 1.270(5) . ?
O1 Zn1 1.937(3) 4_557 ?
O2 C1 1.240(5) . ?
O3 C2 1.243(6) . ?
O4 C2 1.247(6) . ?
O5 C3 1.346(15) . ?
O6 C3 1.206(17) . ?
O5' C3' 1.31(3) . ?
O6' C3' 1.24(3) . ?
C1 C4 1.497(6) . ?
C2 C6 1.503(6) . ?
C3 C12 1.537(15) . ?
C3' C12 1.45(3) . ?
C4 C9 1.381(5) . ?
C4 C5 1.396(5) . ?
C5 C6 1.396(6) . ?
C6 C7 1.378(6) . ?
C7 C8 1.392(5) . ?
C8 C9 1.393(5) . ?
C8 C10 1.491(6) . ?
C10 C11 1.387(6) . ?
C10 C15 1.390(6) . ?
C11 C12 1.396(6) . ?
C12 C13 1.388(6) . ?
C13 C14 1.377(6) . ?
C14 C15 1.382(6) . ?
C16 C17 1.373(6) . ?
C17 C18 1.373(6) . ?
C18 C19 1.378(6) . ?
C18 C21 1.479(6) . ?
C19 C20 1.393(6) . ?
C21 C22 1.301(6) . ?
C22 C23 1.473(6) . ?
C23 C27 1.378(6) . ?
C23 C24 1.381(6) . ?
C24 C25 1.370(6) . ?
C26 C27 1.380(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 N1 108.86(14) 4_457 . ?
O1 Zn1 N2 91.51(13) 4_457 7_556 ?
N1 Zn1 N2 104.66(14) . 7_556 ?
O1 Zn1 O4 111.05(13) 4_457 . ?
N1 Zn1 O4 92.21(14) . . ?
N2 Zn1 O4 145.90(15) 7_556 . ?
O1 Zn1 O3 104.56(14) 4_457 . ?
N1 Zn1 O3 142.68(14) . . ?
N2 Zn1 O3 90.41(14) 7_556 . ?
O4 Zn1 O3 60.02(14) . . ?
C20 N1 C16 117.4(4) . . ?
C20 N1 Zn1 123.3(3) . . ?
C16 N1 Zn1 119.0(3) . . ?
C25 N2 C26 116.7(4) . . ?
C25 N2 Zn1 118.3(3) . 7 ?
C26 N2 Zn1 122.1(3) . 7 ?
C1 O1 Zn1 131.5(3) . 4_557 ?
C2 O3 Zn1 87.8(3) . . ?
C2 O4 Zn1 90.9(3) . . ?
O2 C1 O1 125.1(4) . . ?
O2 C1 C4 121.2(4) . . ?
O1 C1 C4 113.7(4) . . ?
O3 C2 O4 121.2(5) . . ?
O3 C2 C6 118.4(5) . . ?
O4 C2 C6 120.3(5) . . ?
O6 C3 O5 124.4(13) . . ?
O6 C3 C12 123.3(12) . . ?
O5 C3 C12 112.3(11) . . ?
O6' C3' O5' 122(2) . . ?
O6' C3' C12 121(2) . . ?
O5' C3' C12 116(2) . . ?
C9 C4 C5 119.2(4) . . ?
C9 C4 C1 120.1(4) . . ?
C5 C4 C1 120.6(4) . . ?
C4 C5 C6 119.4(4) . . ?
C7 C6 C5 120.5(4) . . ?
C7 C6 C2 119.4(4) . . ?
C5 C6 C2 120.1(4) . . ?
C6 C7 C8 121.0(4) . . ?
C7 C8 C9 117.9(4) . . ?
C7 C8 C10 121.3(4) . . ?
C9 C8 C10 120.8(3) . . ?
C4 C9 C8 122.1(4) . . ?
C11 C10 C15 118.7(4) . . ?
C11 C10 C8 120.4(4) . . ?
C15 C10 C8 120.9(4) . . ?
C10 C11 C12 120.8(4) . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 C3' 118.2(12) . . ?
C11 C12 C3' 119.7(12) . . ?
C13 C12 C3 118.7(7) . . ?
C11 C12 C3 120.7(7) . . ?
C3' C12 C3 24.6(12) . . ?
C14 C13 C12 119.3(4) . . ?
C13 C14 C15 121.0(4) . . ?
C14 C15 C10 120.4(4) . . ?
N1 C16 C17 123.2(4) . . ?
C18 C17 C16 119.9(5) . . ?
C17 C18 C19 117.2(4) . . ?
C17 C18 C21 121.6(4) . . ?
C19 C18 C21 121.2(4) . . ?
C18 C19 C20 120.1(4) . . ?
N1 C20 C19 122.1(4) . . ?
C22 C21 C18 123.6(5) . . ?
C21 C22 C23 127.0(5) . . ?
C27 C23 C24 116.6(4) . . ?
C27 C23 C22 119.5(4) . . ?
C24 C23 C22 123.9(4) . . ?
C25 C24 C23 119.6(4) . . ?
N2 C25 C24 123.9(5) . . ?
N2 C26 C27 122.7(4) . . ?
C23 C27 C26 120.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.081

data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H42 N4 O13 Zn2'
_chemical_formula_sum            'C54 H42 N4 O13 Zn2'
_chemical_formula_weight         1085.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbcm '
_symmetry_space_group_name_Hall  '-P 2c 2b'

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

_cell_length_a                   7.3348(5)
_cell_length_b                   18.9816(16)
_cell_length_c                   33.871(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4715.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    125(6)
_cell_measurement_reflns_used    2886
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      28.40

_exptl_crystal_description       flake
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2232
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7710
_exptl_absorpt_correction_T_max  0.8394
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      125(6)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17813
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4239
_reflns_number_gt                3144
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+19.9522P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4239
_refine_ls_number_parameters     382
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1173
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.079
_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
Zn1 Zn 0.85175(10) 0.88354(4) 0.7500 0.0282(2) Uani 1 2 d S . .
Zn2 Zn 0.13488(10) 0.7500 1.0000 0.0273(2) Uani 1 2 d SU . .
N1 N 1.0913(7) 0.8152(3) 0.7500 0.0258(13) Uani 1 2 d S . .
N3 N -0.0490(5) 0.6694(2) 1.00414(12) 0.0278(9) Uani 1 1 d . A .
O1 O 0.7794(5) 0.83413(19) 0.79806(11) 0.0427(9) Uani 1 1 d . . .
O2 O 0.5280(6) 0.8869(2) 0.82043(15) 0.0745(15) Uani 1 1 d . . .
O3 O 0.2494(11) 0.7765(4) 0.9458(2) 0.031(3) Uani 0.537(17) 1 d P A 1
O4 O 0.3561(13) 0.6738(6) 0.9660(3) 0.039(2) Uani 0.537(17) 1 d PU A 1
O3' O 0.3261(18) 0.7090(9) 0.9684(4) 0.049(4) Uani 0.463(17) 1 d P A 2
O4' O 0.1555(18) 0.7608(5) 0.9229(4) 0.058(5) Uani 0.463(17) 1 d P A 2
O5 O 0.7699(7) 0.4132(2) 0.91937(13) 0.0762(15) Uani 1 1 d . . .
H5A H 0.7452 0.3717 0.9235 0.114 Uiso 1 1 calc R . .
O6 O 0.9848(8) 0.3663(3) 0.88182(17) 0.0824(16) Uani 1 1 d . . .
O7 O 0.6084(7) 0.9486(3) 0.7500 0.0574(17) Uani 1 2 d S . .
H7B H 0.5786 0.9253 0.7701 0.069 Uiso 0.50 1 d PR . .
H7C H 0.5786 0.9253 0.7299 0.069 Uiso 0.50 1 d PR . .
C1 C 0.6452(8) 0.8401(3) 0.82136(18) 0.0456(15) Uani 1 1 d . . .
C2 C 0.3337(11) 0.7283(4) 0.9380(3) 0.068(2) Uani 1 1 d . A .
C3 C 0.9045(12) 0.4171(5) 0.8952(2) 0.071(2) Uani 1 1 d . . .
C4 C 0.6342(8) 0.7823(3) 0.85215(16) 0.0445(15) Uani 1 1 d . . .
C5 C 0.4920(9) 0.7815(3) 0.87947(17) 0.0542(18) Uani 1 1 d . A .
H5 H 0.4038 0.8167 0.8790 0.065 Uiso 1 1 calc R . .
C6 C 0.4829(9) 0.7276(3) 0.90750(18) 0.0571(19) Uani 1 1 d . . .
C7 C 0.6108(8) 0.6743(3) 0.90750(17) 0.0521(17) Uani 1 1 d . A .
H7A H 0.6022 0.6385 0.9261 0.062 Uiso 1 1 calc R . .
C8 C 0.7527(8) 0.6733(3) 0.88011(16) 0.0466(15) Uani 1 1 d . . .
C9 C 0.7614(8) 0.7288(3) 0.85324(16) 0.0443(15) Uani 1 1 d . A .
H9 H 0.8572 0.7298 0.8352 0.053 Uiso 1 1 calc R . .
C10 C 0.8879(8) 0.6150(3) 0.87894(16) 0.0506(16) Uani 1 1 d . A .
C11 C 0.8356(9) 0.5462(3) 0.88716(16) 0.0528(17) Uani 1 1 d . . .
H11 H 0.7154 0.5368 0.8941 0.063 Uiso 1 1 calc R A .
C12 C 0.9597(9) 0.4911(4) 0.88522(17) 0.0582(18) Uani 1 1 d . A .
C13 C 1.1402(9) 0.5042(4) 0.87446(18) 0.0618(18) Uani 1 1 d . . .
H13 H 1.2232 0.4673 0.8723 0.074 Uiso 1 1 calc R A .
C14 C 1.1935(9) 0.5729(4) 0.86707(19) 0.0639(19) Uani 1 1 d . A .
H14 H 1.3143 0.5823 0.8606 0.077 Uiso 1 1 calc R . .
C15 C 1.0685(9) 0.6279(4) 0.86920(17) 0.0570(18) Uani 1 1 d . . .
H15 H 1.1065 0.6737 0.8640 0.068 Uiso 1 1 calc R A .
C16 C 1.1589(7) 0.7889(3) 0.71663(17) 0.0412(13) Uani 1 1 d . . .
H16 H 1.1196 0.8076 0.6927 0.049 Uiso 1 1 calc R . .
C17 C 1.2844(7) 0.7352(3) 0.7161(2) 0.060(2) Uani 1 1 d . . .
H17 H 1.3269 0.7186 0.6920 0.073 Uiso 1 1 calc R . .
C18 C 1.3482(11) 0.7058(4) 0.7500 0.059(3) Uani 1 2 d S . .
C19 C 1.4797(13) 0.6447(5) 0.7500 0.083(4) Uani 1 2 d S . .
H19A H 1.4542 0.6160 0.7731 0.100 Uiso 0.50 1 calc PR . .
H19B H 1.4542 0.6160 0.7269 0.100 Uiso 0.50 1 calc PR . .
C20 C 1.6618(11) 0.6601(4) 0.7500 0.066(3) Uani 1 2 d S . .
H20A H 1.6970 0.6783 0.7752 0.079 Uiso 0.50 1 d PR . .
H20B H 1.6883 0.6956 0.7308 0.079 Uiso 0.50 1 d PR . .
C21 C 1.7826(12) 0.5947(5) 0.7421(9) 0.038(8) Uani 0.50 1 d P . .
C22 C 1.9325(13) 0.5898(5) 0.7657(3) 0.037(3) Uani 0.50 1 d P . .
H22 H 1.9496 0.6251 0.7838 0.045 Uiso 0.50 1 d PR . .
C23 C 2.0341(13) 0.5283(5) 0.7664(3) 0.035(3) Uani 0.50 1 d P . .
H23 H 2.1383 0.5291 0.7823 0.042 Uiso 0.50 1 d PR . .
N2 N 1.9956(8) 0.4737(3) 0.7500 0.0425(17) Uani 1 2 d S . .
C24 C 1.8512(13) 0.4782(5) 0.7192(3) 0.030(2) Uani 0.50 1 d P . .
H24 H 1.8450 0.4441 0.7001 0.037 Uiso 0.50 1 d PR . .
C25 C 1.7451(14) 0.5382(5) 0.7173(3) 0.037(3) Uani 0.50 1 d P . .
H25 H 1.6546 0.5406 0.6982 0.044 Uiso 0.50 1 d PR . .
C26 C -0.0387(7) 0.6110(2) 0.98197(14) 0.0288(11) Uani 1 1 d . . .
H26 H 0.0527 0.6077 0.9630 0.035 Uiso 1 1 calc R A .
C27 C -0.1577(7) 0.5558(2) 0.98621(14) 0.0304(11) Uani 1 1 d . A .
H27 H -0.1443 0.5159 0.9705 0.036 Uiso 1 1 calc R . .
C28 C -0.2982(6) 0.5589(3) 1.01368(14) 0.0297(11) Uani 1 1 d . . .
C29 C -0.3078(7) 0.6190(3) 1.03640(16) 0.0411(14) Uani 1 1 d . A .
H29 H -0.3983 0.6237 1.0554 0.049 Uiso 1 1 calc R . .
C30 C -0.1833(7) 0.6720(3) 1.03081(16) 0.0417(14) Uani 1 1 d . . .
H30 H -0.1929 0.7121 1.0465 0.050 Uiso 1 1 calc R A .
C31 C -0.4335(7) 0.4999(3) 1.01737(14) 0.0348(12) Uani 1 1 d . . .
H31A H -0.5007 0.5049 1.0419 0.042 Uiso 1 1 calc R . .
H31B H -0.3693 0.4552 1.0182 0.042 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.952(4) 6_557 ?
Zn1 O1 1.952(4) . ?
Zn1 N2 2.044(6) 7_865 ?
Zn1 O7 2.170(5) . ?
Zn1 N1 2.184(5) . ?
Zn2 O3' 1.927(14) . ?
Zn2 O3' 1.927(14) 3_567 ?
Zn2 N3 2.044(4) . ?
Zn2 N3 2.044(4) 3_567 ?
Zn2 O3 2.082(7) 3_567 ?
Zn2 O3 2.082(7) . ?
Zn2 O4 2.460(11) 3_567 ?
Zn2 O4 2.460(10) . ?
Zn2 C2 2.589(7) 3_567 ?
Zn2 C2 2.589(7) . ?
N1 C16 1.331(6) 6_557 ?
N1 C16 1.331(6) . ?
N3 C30 1.337(6) . ?
N3 C26 1.342(6) . ?
O1 C1 1.267(6) . ?
O2 C1 1.236(7) . ?
O3 C2 1.135(9) . ?
O4 C2 1.411(15) . ?
O3' C2 1.094(14) . ?
O4' C2 1.534(16) . ?
O5 C3 1.284(9) . ?
O6 C3 1.218(9) . ?
C1 C4 1.516(8) . ?
C2 C6 1.506(9) . ?
C3 C12 1.501(9) . ?
C4 C9 1.380(8) . ?
C4 C5 1.394(7) . ?
C5 C6 1.397(8) . ?
C6 C7 1.379(9) . ?
C7 C8 1.395(8) . ?
C8 C9 1.393(8) . ?
C8 C10 1.486(9) . ?
C10 C15 1.387(8) . ?
C10 C11 1.390(8) . ?
C11 C12 1.387(9) . ?
C12 C13 1.395(9) . ?
C13 C14 1.384(9) . ?
C14 C15 1.391(9) . ?
C16 C17 1.373(8) . ?
C17 C18 1.359(8) . ?
C18 C17 1.359(8) 6_557 ?
C18 C19 1.509(11) . ?
C19 C20 1.367(12) . ?
C20 C21 1.548(12) 6_557 ?
C20 C21 1.548(12) . ?
C21 C21 0.54(6) 6_557 ?
C21 C22 1.135(13) 6_557 ?
C21 C22 1.36(2) . ?
C21 C25 1.39(2) . ?
C21 C25 1.77(3) 6_557 ?
C22 C22 1.06(2) 6_557 ?
C22 C21 1.135(13) 6_557 ?
C22 C23 1.384(12) . ?
C22 C23 1.759(13) 6_557 ?
C22 C25 1.783(14) 6_557 ?
C23 C23 1.11(2) 6_557 ?
C23 N2 1.210(10) . ?
C23 C24 1.716(13) 6_557 ?
C23 C22 1.759(13) 6_557 ?
N2 C23 1.210(10) 6_557 ?
N2 C24 1.489(10) . ?
N2 C24 1.489(10) 6_557 ?
N2 Zn1 2.044(6) 7_855 ?
C24 C25 1.380(13) . ?
C24 C23 1.716(13) 6_557 ?
C25 C21 1.77(3) 6_557 ?
C25 C22 1.783(14) 6_557 ?
C26 C27 1.371(7) . ?
C27 C28 1.390(7) . ?
C28 C29 1.379(7) . ?
C28 C31 1.501(7) . ?
C29 C30 1.371(7) . ?
C31 C31 1.529(9) 5_467 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 113.0(2) 6_557 . ?
O1 Zn1 N2 123.43(11) 6_557 7_865 ?
O1 Zn1 N2 123.43(11) . 7_865 ?
O1 Zn1 O7 92.84(13) 6_557 . ?
O1 Zn1 O7 92.84(13) . . ?
N2 Zn1 O7 88.5(2) 7_865 . ?
O1 Zn1 N1 86.17(13) 6_557 . ?
O1 Zn1 N1 86.17(13) . . ?
N2 Zn1 N1 93.3(2) 7_865 . ?
O7 Zn1 N1 178.20(19) . . ?
O3' Zn2 O3' 86.6(7) . 3_567 ?
O3' Zn2 N3 102.5(4) . . ?
O3' Zn2 N3 138.1(5) 3_567 . ?
O3' Zn2 N3 138.1(5) . 3_567 ?
O3' Zn2 N3 102.5(4) 3_567 3_567 ?
N3 Zn2 N3 97.4(2) . 3_567 ?
O3' Zn2 O3 95.7(6) . 3_567 ?
O3' Zn2 O3 46.7(6) 3_567 3_567 ?
N3 Zn2 O3 91.4(2) . 3_567 ?
N3 Zn2 O3 120.5(3) 3_567 3_567 ?
O3' Zn2 O3 46.7(6) . . ?
O3' Zn2 O3 95.7(6) 3_567 . ?
N3 Zn2 O3 120.5(3) . . ?
N3 Zn2 O3 91.4(2) 3_567 . ?
O3 Zn2 O3 132.4(5) 3_567 . ?
O3' Zn2 O4 91.0(3) . 3_567 ?
O3' Zn2 O4 12.3(5) 3_567 3_567 ?
N3 Zn2 O4 147.4(3) . 3_567 ?
N3 Zn2 O4 91.6(3) 3_567 3_567 ?
O3 Zn2 O4 57.5(3) 3_567 3_567 ?
O3 Zn2 O4 90.3(4) . 3_567 ?
O3' Zn2 O4 12.3(5) . . ?
O3' Zn2 O4 91.0(3) 3_567 . ?
N3 Zn2 O4 91.6(3) . . ?
N3 Zn2 O4 147.4(3) 3_567 . ?
O3 Zn2 O4 90.3(4) 3_567 . ?
O3 Zn2 O4 57.5(3) . . ?
O4 Zn2 O4 97.5(5) 3_567 . ?
O3' Zn2 C2 96.0(5) . 3_567 ?
O3' Zn2 C2 22.5(5) 3_567 3_567 ?
N3 Zn2 C2 115.8(2) . 3_567 ?
N3 Zn2 C2 107.94(17) 3_567 3_567 ?
O3 Zn2 C2 25.3(3) 3_567 3_567 ?
O3 Zn2 C2 116.7(4) . 3_567 ?
O4 Zn2 C2 32.3(3) 3_567 3_567 ?
O4 Zn2 C2 95.9(3) . 3_567 ?
O3' Zn2 C2 22.5(5) . . ?
O3' Zn2 C2 96.0(5) 3_567 . ?
N3 Zn2 C2 107.94(17) . . ?
N3 Zn2 C2 115.8(2) 3_567 . ?
O3 Zn2 C2 116.7(4) 3_567 . ?
O3 Zn2 C2 25.3(2) . . ?
O4 Zn2 C2 95.9(3) 3_567 . ?
O4 Zn2 C2 32.3(3) . . ?
C2 Zn2 C2 111.4(4) 3_567 . ?
C16 N1 C16 116.2(6) 6_557 . ?
C16 N1 Zn1 121.5(3) 6_557 . ?
C16 N1 Zn1 121.5(3) . . ?
C30 N3 C26 116.7(4) . . ?
C30 N3 Zn2 120.3(3) . . ?
C26 N3 Zn2 122.9(3) . . ?
C1 O1 Zn1 133.5(4) . . ?
C2 O3 Zn2 103.2(6) . . ?
C2 O4 Zn2 78.9(6) . . ?
C2 O3' Zn2 115.1(14) . . ?
O2 C1 O1 126.1(6) . . ?
O2 C1 C4 120.0(5) . . ?
O1 C1 C4 113.9(5) . . ?
O3' C2 O3 91.4(11) . . ?
O3' C2 O4 29.6(7) . . ?
O3 C2 O4 120.0(9) . . ?
O3' C2 C6 132.9(12) . . ?
O3 C2 C6 124.1(8) . . ?
O4 C2 C6 111.7(8) . . ?
O3' C2 O4' 113.9(11) . . ?
O3 C2 O4' 44.6(6) . . ?
O4 C2 O4' 128.2(7) . . ?
C6 C2 O4' 113.2(8) . . ?
O3' C2 Zn2 42.4(10) . . ?
O3 C2 Zn2 51.5(5) . . ?
O4 C2 Zn2 68.8(6) . . ?
C6 C2 Zn2 165.4(5) . . ?
O4' C2 Zn2 74.1(5) . . ?
O6 C3 O5 124.3(7) . . ?
O6 C3 C12 121.8(8) . . ?
O5 C3 C12 114.0(8) . . ?
C9 C4 C5 118.7(6) . . ?
C9 C4 C1 121.0(5) . . ?
C5 C4 C1 120.3(6) . . ?
C4 C5 C6 119.6(6) . . ?
C7 C6 C5 120.3(6) . . ?
C7 C6 C2 120.0(7) . . ?
C5 C6 C2 119.7(7) . . ?
C6 C7 C8 121.2(6) . . ?
C9 C8 C7 117.3(6) . . ?
C9 C8 C10 121.0(5) . . ?
C7 C8 C10 121.7(6) . . ?
C4 C9 C8 122.9(5) . . ?
C15 C10 C11 118.4(7) . . ?
C15 C10 C8 120.9(6) . . ?
C11 C10 C8 120.7(6) . . ?
C12 C11 C10 121.2(6) . . ?
C11 C12 C13 120.1(6) . . ?
C11 C12 C3 121.1(7) . . ?
C13 C12 C3 118.8(7) . . ?
C14 C13 C12 118.9(7) . . ?
C13 C14 C15 120.8(6) . . ?
C10 C15 C14 120.7(6) . . ?
N1 C16 C17 122.6(6) . . ?
C18 C17 C16 121.6(6) . . ?
C17 C18 C17 115.2(8) . 6_557 ?
C17 C18 C19 122.4(4) . . ?
C17 C18 C19 122.4(4) 6_557 . ?
C20 C19 C18 117.4(8) . . ?
C19 C20 C21 112.8(7) . 6_557 ?
C19 C20 C21 112.8(7) . . ?
C21 C20 C21 20(2) 6_557 . ?
C21 C21 C22 103.4(16) 6_557 6_557 ?
C21 C21 C22 54.0(11) 6_557 . ?
C22 C21 C22 49.3(11) 6_557 . ?
C21 C21 C25 127.1(11) 6_557 . ?
C22 C21 C25 89.3(14) 6_557 . ?
C22 C21 C25 117.4(9) . . ?
C21 C21 C20 80.0(11) 6_557 . ?
C22 C21 C20 131.4(10) 6_557 . ?
C22 C21 C20 114.5(15) . . ?
C25 C21 C20 127.7(12) . . ?
C21 C21 C25 38.8(8) 6_557 6_557 ?
C22 C21 C25 106.3(14) 6_557 6_557 ?
C22 C21 C25 68.0(13) . 6_557 ?
C25 C21 C25 88.3(10) . 6_557 ?
C20 C21 C25 105.2(14) . 6_557 ?
C22 C22 C21 76.6(16) 6_557 6_557 ?
C22 C22 C21 54.0(12) 6_557 . ?
C21 C22 C21 23(3) 6_557 . ?
C22 C22 C23 91.0(6) 6_557 . ?
C21 C22 C23 126.6(11) 6_557 . ?
C21 C22 C23 120.2(10) . . ?
C22 C22 C23 51.9(4) 6_557 6_557 ?
C21 C22 C23 108.8(14) 6_557 6_557 ?
C21 C22 C23 91.4(11) . 6_557 ?
C23 C22 C23 39.1(7) . 6_557 ?
C22 C22 C25 108.8(5) 6_557 6_557 ?
C21 C22 C25 51.2(11) 6_557 6_557 ?
C21 C22 C25 66.8(10) . 6_557 ?
C23 C22 C25 87.0(7) . 6_557 ?
C23 C22 C25 99.3(6) 6_557 6_557 ?
C23 C23 N2 62.7(5) 6_557 . ?
C23 C23 C22 89.0(6) 6_557 . ?
N2 C23 C22 126.1(9) . . ?
C23 C23 C24 106.5(5) 6_557 6_557 ?
N2 C23 C24 58.2(5) . 6_557 ?
C22 C23 C24 92.9(7) . 6_557 ?
C23 C23 C22 51.9(4) 6_557 6_557 ?
N2 C23 C22 100.7(7) . 6_557 ?
C22 C23 C22 37.2(8) . 6_557 ?
C24 C23 C22 102.2(7) 6_557 6_557 ?
C23 N2 C23 54.6(10) . 6_557 ?
C23 N2 C24 115.9(7) . . ?
C23 N2 C24 78.2(6) 6_557 . ?
C23 N2 C24 78.2(6) . 6_557 ?
C23 N2 C24 115.9(7) 6_557 6_557 ?
C24 N2 C24 88.9(8) . 6_557 ?
C23 N2 Zn1 126.2(6) . 7_855 ?
C23 N2 Zn1 126.2(6) 6_557 7_855 ?
C24 N2 Zn1 116.0(5) . 7_855 ?
C24 N2 Zn1 116.0(5) 6_557 7_855 ?
C25 C24 N2 118.8(9) . . ?
C25 C24 C23 89.8(7) . 6_557 ?
N2 C24 C23 43.7(4) . 6_557 ?
C24 C25 C21 119.8(11) . . ?
C24 C25 C21 112.2(9) . 6_557 ?
C21 C25 C21 14.1(16) . 6_557 ?
C24 C25 C22 90.2(7) . 6_557 ?
C21 C25 C22 39.5(6) . 6_557 ?
C21 C25 C22 45.2(6) 6_557 6_557 ?
N3 C26 C27 122.5(5) . . ?
C26 C27 C28 120.7(4) . . ?
C29 C28 C27 116.5(5) . . ?
C29 C28 C31 122.5(5) . . ?
C27 C28 C31 121.0(5) . . ?
C30 C29 C28 119.8(5) . . ?
N3 C30 C29 123.8(5) . . ?
C28 C31 C31 110.8(5) . 5_467 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.089

data_120817a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H30 Cd2 N2 O14, 2(H2 O)'
_chemical_formula_sum            'C42 H34 Cd2 N2 O16'
_chemical_formula_weight         1047.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   10.2647(11)
_cell_length_b                   13.9260(14)
_cell_length_c                   29.090(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3770(10)
_cell_angle_gamma                90.00
_cell_volume                     4102.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1312
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      25.894

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_T_max  0.9464
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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            21094
_diffrn_reflns_av_R_equivalents  0.2020
_diffrn_reflns_av_sigmaI/netI    0.2362
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7247
_reflns_number_gt                2843
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0335P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7247
_refine_ls_number_parameters     578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1925
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1312
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_restrained_S_all      0.888
_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
Cd1 Cd 1.35057(7) 0.36169(6) 0.03895(3) 0.0375(3) Uani 1 1 d . . .
Cd2 Cd 1.05606(8) 0.15268(7) 0.04668(3) 0.0409(3) Uani 1 1 d . . .
N1 N 1.1125(11) 0.1643(7) 0.1260(4) 0.053(3) Uani 1 1 d . A .
N2 N 1.3167(10) 0.1514(7) 0.4582(4) 0.052(3) Uani 1 1 d . . .
O1 O 0.4857(9) 0.0550(7) -0.2990(4) 0.089(3) Uani 1 1 d . . .
H1 H 0.5025 0.0907 -0.3197 0.134 Uiso 1 1 calc R . .
O2 O 0.5587(11) 0.1806(9) -0.2514(4) 0.096(4) Uani 1 1 d . . .
O3 O 0.1925(7) 0.0939(6) -0.0023(3) 0.050(2) Uani 1 1 d . . .
O4 O 0.3165(7) 0.1949(6) 0.0456(3) 0.043(2) Uani 1 1 d . . .
O5 O 0.8845(7) 0.1488(6) -0.0158(3) 0.050(2) Uani 1 1 d . . .
O6 O 0.8107(7) 0.1566(6) 0.0519(3) 0.057(3) Uani 1 1 d . . .
O7 O 1.0111(7) -0.0090(5) 0.0664(3) 0.056(2) Uani 1 1 d . . .
H7A H 0.9350 -0.0215 0.0512 0.067 Uiso 1 1 d R . .
H7B H 1.0662 -0.0459 0.0564 0.067 Uiso 1 1 d R . .
O8 O 1.3289(8) 0.5242(6) 0.0236(3) 0.066(3) Uani 1 1 d . . .
H8A H 1.3588 0.5539 0.0021 0.079 Uiso 1 1 d R . .
H8B H 1.2688 0.5584 0.0323 0.079 Uiso 1 1 d R . .
O9 O 1.0657(7) 0.3262(5) 0.0338(3) 0.043(2) Uani 1 1 d . . .
O10 O 1.2107(7) 0.4002(5) 0.0891(3) 0.041(2) Uani 1 1 d . . .
O11 O 0.5777(7) 0.3720(5) 0.0471(3) 0.046(2) Uani 1 1 d . . .
O12 O 0.5238(7) 0.3632(6) 0.1178(3) 0.053(2) Uani 1 1 d . . .
O13 O 0.8093(10) 0.1820(9) 0.3131(4) 0.100(4) Uani 1 1 d . . .
H13 H 0.7700 0.1496 0.3300 0.149 Uiso 1 1 calc R . .
O14 O 0.8477(13) 0.2789(9) 0.3758(5) 0.112(4) Uani 1 1 d . . .
O15 O 0.3135(9) 0.5650(7) 0.1394(4) 0.096(4) Uani 1 1 d . . .
H15A H 0.2748 0.5218 0.1215 0.115 Uiso 1 1 d R . .
H15B H 0.3694 0.5376 0.1600 0.115 Uiso 1 1 d R . .
O16 O 0.1385(9) 0.6383(7) 0.0491(3) 0.091(3) Uani 1 1 d . . .
H16A H 0.0785 0.6517 0.0262 0.109 Uiso 1 1 d R . .
H16B H 0.1383 0.6812 0.0698 0.109 Uiso 1 1 d R . .
C1 C 0.5137(13) 0.1012(12) -0.2567(5) 0.058(4) Uani 1 1 d . . .
C2 C 0.3006(11) 0.1392(9) 0.0119(4) 0.037(3) Uani 1 1 d . . .
C3 C 0.7899(10) 0.1461(9) 0.0081(5) 0.039(3) Uani 1 1 d . . .
C4 C 0.4839(12) 0.0367(11) -0.2162(5) 0.054(4) Uani 1 1 d . . .
C5 C 0.4226(13) -0.0522(11) -0.2242(5) 0.063(4) Uani 1 1 d . . .
H5 H 0.4020 -0.0763 -0.2543 0.075 Uiso 1 1 calc R . .
C6 C 0.3925(12) -0.1050(10) -0.1863(5) 0.060(4) Uani 1 1 d . . .
H6 H 0.3574 -0.1665 -0.1906 0.072 Uiso 1 1 calc R . .
C7 C 0.4163(12) -0.0635(11) -0.1421(5) 0.059(4) Uani 1 1 d . . .
H7 H 0.3914 -0.0971 -0.1173 0.071 Uiso 1 1 calc R . .
C8 C 0.4740(12) 0.0238(11) -0.1336(5) 0.050(4) Uani 1 1 d . . .
C9 C 0.5118(12) 0.0756(10) -0.1710(5) 0.056(4) Uani 1 1 d . . .
H9 H 0.5545 0.1345 -0.1659 0.067 Uiso 1 1 calc R . .
C10 C 0.4990(11) 0.0671(8) -0.0857(4) 0.042(3) Uani 1 1 d . . .
C11 C 0.3971(11) 0.0780(8) -0.0593(4) 0.042(3) Uani 1 1 d . . .
H11 H 0.3129 0.0579 -0.0725 0.051 Uiso 1 1 calc R . .
C12 C 0.4137(10) 0.1168(8) -0.0149(4) 0.036(3) Uani 1 1 d . . .
C13 C 0.5448(10) 0.1425(8) 0.0065(4) 0.040(3) Uani 1 1 d . . .
H13A H 0.5591 0.1684 0.0364 0.048 Uiso 1 1 calc R . .
C14 C 0.6521(10) 0.1288(8) -0.0175(4) 0.038(3) Uani 1 1 d . . .
C15 C 0.6288(11) 0.0920(8) -0.0617(4) 0.041(3) Uani 1 1 d . . .
H15 H 0.7004 0.0827 -0.0771 0.049 Uiso 1 1 calc R . .
C16 C 0.6100(10) 0.3714(9) 0.0915(4) 0.037(3) Uani 1 1 d . . .
C17 C 0.8573(16) 0.2602(12) 0.3357(6) 0.066(4) Uani 1 1 d . . .
C18 C 1.0951(11) 0.3695(8) 0.0723(4) 0.036(3) Uani 1 1 d . . .
C19 C 0.9886(10) 0.3829(8) 0.1030(4) 0.037(3) Uani 1 1 d . . .
C20 C 0.8527(10) 0.3749(7) 0.0827(4) 0.035(3) Uani 1 1 d . . .
H20 H 0.8290 0.3684 0.0507 0.042 Uiso 1 1 calc R . .
C21 C 0.7542(10) 0.3770(8) 0.1115(4) 0.039(3) Uani 1 1 d . . .
C22 C 0.7961(11) 0.3846(8) 0.1604(4) 0.043(3) Uani 1 1 d . . .
H22 H 0.7325 0.3851 0.1798 0.051 Uiso 1 1 calc R . .
C23 C 0.9311(11) 0.3913(9) 0.1807(4) 0.043(3) Uani 1 1 d . . .
C24 C 1.0252(11) 0.3911(8) 0.1507(4) 0.040(3) Uani 1 1 d . . .
H24 H 1.1143 0.3965 0.1633 0.048 Uiso 1 1 calc R . .
C25 C 0.9694(12) 0.3891(9) 0.2332(5) 0.051(4) Uani 1 1 d . . .
C26 C 1.0836(12) 0.4344(9) 0.2556(5) 0.051(4) Uani 1 1 d . . .
H26 H 1.1362 0.4694 0.2385 0.061 Uiso 1 1 calc R . .
C27 C 1.1188(14) 0.4268(10) 0.3046(5) 0.062(4) Uani 1 1 d . . .
H27 H 1.1953 0.4572 0.3190 0.074 Uiso 1 1 calc R . .
C28 C 1.0455(14) 0.3770(10) 0.3314(5) 0.060(4) Uani 1 1 d . . .
H28 H 1.0692 0.3755 0.3637 0.073 Uiso 1 1 calc R . .
C29 C 0.9308(14) 0.3270(10) 0.3088(5) 0.054(4) Uani 1 1 d . . .
C30 C 0.8965(13) 0.3313(9) 0.2615(5) 0.056(4) Uani 1 1 d . . .
H30 H 0.8243 0.2960 0.2471 0.068 Uiso 1 1 calc R . .
C31 C 1.0211(14) 0.1480(9) 0.1531(5) 0.059(4) Uani 1 1 d . . .
H31 H 0.9350 0.1359 0.1387 0.071 Uiso 1 1 calc R . .
C32 C 1.0468(15) 0.1483(10) 0.2012(5) 0.067(4) Uani 1 1 d . A .
H32 H 0.9785 0.1380 0.2180 0.081 Uiso 1 1 calc R . .
C33 C 1.1703(18) 0.1634(11) 0.2239(5) 0.070(5) Uani 1 1 d . . .
C34 C 1.2687(15) 0.1804(10) 0.1988(5) 0.070(4) Uani 1 1 d . A .
H34 H 1.3542 0.1911 0.2141 0.084 Uiso 1 1 calc R . .
C35 C 1.2413(13) 0.1819(9) 0.1487(5) 0.055(4) Uani 1 1 d . . .
H35 H 1.3085 0.1945 0.1316 0.066 Uiso 1 1 calc R A .
C36 C 1.171(8) 0.156(3) 0.276(2) 0.061(15) Uani 0.62(13) 1 d P A 1
H36 H 1.0914 0.1428 0.2865 0.074 Uiso 0.62(13) 1 d PR A 1
C37 C 1.277(8) 0.167(3) 0.307(2) 0.068(18) Uani 0.62(13) 1 d P A 1
H37 H 1.3567 0.1813 0.2976 0.081 Uiso 0.62(13) 1 d PR A 1
C36' C 1.249(12) 0.173(6) 0.274(4) 0.07(3) Uani 0.38(13) 1 d P A 2
H36' H 1.3331 0.1992 0.2801 0.081 Uiso 0.38(13) 1 d PR A 2
C37' C 1.185(13) 0.142(6) 0.306(3) 0.06(3) Uani 0.38(13) 1 d P A 2
H37' H 1.1017 0.1148 0.3007 0.077 Uiso 0.38(13) 1 d PR A 2
C38 C 1.2700(18) 0.1552(11) 0.3591(6) 0.073(5) Uani 1 1 d . . .
C39 C 1.1679(16) 0.1395(10) 0.3840(5) 0.074(5) Uani 1 1 d . A .
H39 H 1.0822 0.1320 0.3681 0.089 Uiso 1 1 calc R . .
C40 C 1.1923(15) 0.1347(10) 0.4331(5) 0.070(4) Uani 1 1 d . . .
H40 H 1.1231 0.1200 0.4489 0.084 Uiso 1 1 calc R A .
C41 C 1.4127(16) 0.1677(10) 0.4314(5) 0.067(4) Uani 1 1 d . . .
H41 H 1.4984 0.1775 0.4469 0.081 Uiso 1 1 calc R A .
C42 C 1.3925(17) 0.1708(10) 0.3833(5) 0.074(5) Uani 1 1 d . A .
H42 H 1.4626 0.1835 0.3676 0.089 Uiso 1 1 calc R . .


_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
Cd1 O10 2.271(7) . ?
Cd1 O11 2.309(7) 1_655 ?
Cd1 O8 2.310(8) . ?
Cd1 N2 2.324(11) 4_565 ?
Cd1 O4 2.361(8) 1_655 ?
Cd2 N1 2.293(11) . ?
Cd2 O3 2.303(8) 1_655 ?
Cd2 O5 2.316(7) . ?
Cd2 O7 2.387(8) . ?
Cd2 O9 2.449(8) . ?
Cd2 O6 2.549(7) . ?
N1 C31 1.339(14) . ?
N1 C35 1.400(15) . ?
N2 C41 1.372(15) . ?
N2 C40 1.385(15) . ?
N2 Cd1 2.324(11) 4_566 ?
O1 C1 1.379(16) . ?
O2 C1 1.199(15) . ?
O3 C2 1.284(13) . ?
O3 Cd2 2.303(8) 1_455 ?
O4 C2 1.242(13) . ?
O4 Cd1 2.361(8) 1_455 ?
O5 C3 1.283(12) . ?
O6 C3 1.266(13) . ?
O9 C18 1.266(13) . ?
O10 C18 1.281(12) . ?
O11 C16 1.278(13) . ?
O11 Cd1 2.309(7) 1_455 ?
O12 C16 1.266(11) . ?
O13 C17 1.325(17) . ?
O14 C17 1.215(17) . ?
C1 C4 1.551(19) . ?
C2 C12 1.531(14) . ?
C3 C14 1.506(15) . ?
C4 C5 1.391(17) . ?
C4 C9 1.406(17) . ?
C5 C6 1.400(18) . ?
C6 C7 1.395(18) . ?
C7 C8 1.357(16) . ?
C8 C9 1.413(17) . ?
C8 C10 1.502(17) . ?
C10 C11 1.402(14) . ?
C10 C15 1.441(15) . ?
C11 C12 1.386(15) . ?
C12 C13 1.433(14) . ?
C13 C14 1.411(13) . ?
C14 C15 1.370(15) . ?
C16 C21 1.502(14) . ?
C17 C29 1.496(19) . ?
C18 C19 1.531(14) . ?
C19 C24 1.384(15) . ?
C19 C20 1.427(14) . ?
C20 C21 1.414(14) . ?
C21 C22 1.420(15) . ?
C22 C23 1.419(15) . ?
C23 C24 1.403(14) . ?
C23 C25 1.514(16) . ?
C25 C26 1.396(16) . ?
C25 C30 1.444(16) . ?
C26 C27 1.416(17) . ?
C27 C28 1.359(16) . ?
C28 C29 1.433(17) . ?
C29 C30 1.366(17) . ?
C31 C32 1.381(18) . ?
C32 C33 1.347(19) . ?
C33 C34 1.361(18) . ?
C33 C36 1.52(6) . ?
C33 C36' 1.55(10) . ?
C34 C35 1.437(18) . ?
C36 C37 1.31(15) . ?
C37 C38 1.53(6) . ?
C36' C37' 1.3(3) . ?
C37' C38 1.64(9) . ?
C38 C42 1.35(2) . ?
C38 C39 1.384(19) . ?
C39 C40 1.410(18) . ?
C41 C42 1.382(18) . ?

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
O10 Cd1 O11 130.7(3) . 1_655 ?
O10 Cd1 O8 80.9(3) . . ?
O11 Cd1 O8 91.3(3) 1_655 . ?
O10 Cd1 N2 131.4(3) . 4_565 ?
O11 Cd1 N2 95.2(3) 1_655 4_565 ?
O8 Cd1 N2 83.6(3) . 4_565 ?
O10 Cd1 O4 93.6(3) . 1_655 ?
O11 Cd1 O4 102.3(3) 1_655 1_655 ?
O8 Cd1 O4 165.5(3) . 1_655 ?
N2 Cd1 O4 90.4(3) 4_565 1_655 ?
N1 Cd2 O3 124.6(3) . 1_655 ?
N1 Cd2 O5 145.8(3) . . ?
O3 Cd2 O5 88.2(3) 1_655 . ?
N1 Cd2 O7 81.4(3) . . ?
O3 Cd2 O7 88.6(3) 1_655 . ?
O5 Cd2 O7 90.9(3) . . ?
N1 Cd2 O9 94.3(3) . . ?
O3 Cd2 O9 102.2(3) 1_655 . ?
O5 Cd2 O9 87.0(3) . . ?
O7 Cd2 O9 168.9(3) . . ?
N1 Cd2 O6 91.6(3) . . ?
O3 Cd2 O6 138.6(3) 1_655 . ?
O5 Cd2 O6 54.2(3) . . ?
O7 Cd2 O6 76.9(3) . . ?
O9 Cd2 O6 93.1(3) . . ?
C31 N1 C35 116.8(12) . . ?
C31 N1 Cd2 119.6(9) . . ?
C35 N1 Cd2 123.5(9) . . ?
C41 N2 C40 114.4(12) . . ?
C41 N2 Cd1 125.8(9) . 4_566 ?
C40 N2 Cd1 119.6(9) . 4_566 ?
C2 O3 Cd2 102.1(7) . 1_455 ?
C2 O4 Cd1 123.5(8) . 1_455 ?
C3 O5 Cd2 97.0(7) . . ?
C3 O6 Cd2 86.8(6) . . ?
C18 O9 Cd2 110.1(7) . . ?
C18 O10 Cd1 108.7(7) . . ?
C16 O11 Cd1 101.2(7) . 1_455 ?
O2 C1 O1 124.4(15) . . ?
O2 C1 C4 123.8(15) . . ?
O1 C1 C4 111.7(14) . . ?
O4 C2 O3 123.7(10) . . ?
O4 C2 C12 121.1(10) . . ?
O3 C2 C12 115.1(11) . . ?
O6 C3 O5 121.6(10) . . ?
O6 C3 C14 120.4(11) . . ?
O5 C3 C14 118.0(11) . . ?
C5 C4 C9 121.1(13) . . ?
C5 C4 C1 121.9(14) . . ?
C9 C4 C1 116.8(13) . . ?
C4 C5 C6 119.2(14) . . ?
C7 C6 C5 118.6(14) . . ?
C8 C7 C6 123.1(14) . . ?
C7 C8 C9 118.9(13) . . ?
C7 C8 C10 122.2(13) . . ?
C9 C8 C10 118.9(12) . . ?
C4 C9 C8 118.9(13) . . ?
C11 C10 C15 115.1(11) . . ?
C11 C10 C8 121.3(10) . . ?
C15 C10 C8 123.4(10) . . ?
C12 C11 C10 124.2(11) . . ?
C11 C12 C13 117.9(10) . . ?
C11 C12 C2 124.4(10) . . ?
C13 C12 C2 117.6(11) . . ?
C14 C13 C12 120.3(11) . . ?
C15 C14 C13 119.0(10) . . ?
C15 C14 C3 122.0(10) . . ?
C13 C14 C3 118.7(11) . . ?
C14 C15 C10 123.4(11) . . ?
O12 C16 O11 121.3(10) . . ?
O12 C16 C21 120.7(11) . . ?
O11 C16 C21 117.9(10) . . ?
O14 C17 O13 124.8(16) . . ?
O14 C17 C29 119.7(16) . . ?
O13 C17 C29 115.4(14) . . ?
O9 C18 O10 124.7(11) . . ?
O9 C18 C19 119.0(10) . . ?
O10 C18 C19 116.3(11) . . ?
C24 C19 C20 120.5(11) . . ?
C24 C19 C18 119.5(10) . . ?
C20 C19 C18 119.5(11) . . ?
C21 C20 C19 120.0(11) . . ?
C20 C21 C22 117.7(10) . . ?
C20 C21 C16 121.6(11) . . ?
C22 C21 C16 120.7(10) . . ?
C23 C22 C21 122.6(11) . . ?
C24 C23 C22 117.7(12) . . ?
C24 C23 C25 122.3(11) . . ?
C22 C23 C25 119.7(11) . . ?
C19 C24 C23 121.5(11) . . ?
C26 C25 C30 117.4(13) . . ?
C26 C25 C23 121.5(12) . . ?
C30 C25 C23 120.8(11) . . ?
C25 C26 C27 119.5(13) . . ?
C28 C27 C26 122.8(13) . . ?
C27 C28 C29 118.4(13) . . ?
C30 C29 C28 119.9(13) . . ?
C30 C29 C17 119.0(14) . . ?
C28 C29 C17 120.6(14) . . ?
C29 C30 C25 121.8(13) . . ?
N1 C31 C32 124.0(13) . . ?
C33 C32 C31 120.5(15) . . ?
C32 C33 C34 119.0(15) . . ?
C32 C33 C36 109(3) . . ?
C34 C33 C36 132(3) . . ?
C32 C33 C36' 141(5) . . ?
C34 C33 C36' 100(5) . . ?
C36 C33 C36' 32(3) . . ?
C33 C34 C35 120.5(14) . . ?
N1 C35 C34 119.2(13) . . ?
C37 C36 C33 123(8) . . ?
C36 C37 C38 120(8) . . ?
C37' C36' C33 114(10) . . ?
C36' C37' C38 113(10) . . ?
C42 C38 C39 118.2(16) . . ?
C42 C38 C37 108(4) . . ?
C39 C38 C37 134(4) . . ?
C42 C38 C37' 144(5) . . ?
C39 C38 C37' 98(5) . . ?
C37 C38 C37' 36(2) . . ?
C38 C39 C40 120.8(15) . . ?
N2 C40 C39 121.6(14) . . ?
N2 C41 C42 125.3(15) . . ?
C38 C42 C41 119.7(16) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.736
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.148

data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H32 Cd2 N2 O14, 2(H2 O)'
_chemical_formula_sum            'C42 H36 Cd2 N2 O16'
_chemical_formula_weight         1049.53

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.1479(12)
_cell_length_b                   13.8385(15)
_cell_length_c                   28.596(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1040(10)
_cell_angle_gamma                90.00
_cell_volume                     3953.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    121.20(14)
_cell_measurement_reflns_used    2309
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.43

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7086
_exptl_absorpt_correction_T_max  0.8103
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      121.20(14)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23483
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1319
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6942
_reflns_number_gt                4121
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1020P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6942
_refine_ls_number_parameters     560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0812
_refine_ls_wR_factor_ref         0.2431
_refine_ls_wR_factor_gt          0.1943
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
Cd1 Cd -0.34534(7) 0.14019(6) 0.46278(3) 0.0281(3) Uani 1 1 d . . .
Cd2 Cd -0.06081(7) 0.34878(6) 0.45410(3) 0.0299(3) Uani 1 1 d . . .
O1 O 0.5134(8) 0.4415(6) 0.8018(3) 0.048(2) Uani 1 1 d . . .
H1A H 0.4910 0.4061 0.8220 0.058 Uiso 1 1 calc R . .
O2 O 0.4237(8) 0.3222(6) 0.7530(3) 0.045(2) Uani 1 1 d . . .
O3 O 0.8062(7) 0.4087(6) 0.5040(2) 0.0344(18) Uani 1 1 d . . .
O4 O 0.6843(6) 0.3059(6) 0.4570(2) 0.0312(18) Uani 1 1 d . . .
O5 O 0.1143(7) 0.3522(5) 0.5164(3) 0.0341(18) Uani 1 1 d . . .
O6 O 0.1853(7) 0.3446(5) 0.4476(3) 0.0354(19) Uani 1 1 d . . .
O7 O -0.0134(7) 0.5077(5) 0.4341(2) 0.0383(19) Uani 1 1 d . . .
H7A H 0.0642 0.5209 0.4491 0.046 Uiso 1 1 d R . .
H7B H -0.0684 0.5454 0.4438 0.046 Uiso 1 1 d R . .
O8 O -0.3337(7) -0.0253(6) 0.4748(3) 0.041(2) Uani 1 1 d . . .
H8A H -0.3671 -0.0557 0.4956 0.049 Uiso 1 1 d R . .
H8B H -0.2748 -0.0603 0.4656 0.049 Uiso 1 1 d R . .
O9 O -0.0629(6) 0.1755(5) 0.4676(2) 0.0293(17) Uani 1 1 d . . .
O10 O -0.2059(6) 0.0984(5) 0.4135(2) 0.0299(17) Uani 1 1 d . . .
O11 O 0.4290(7) 0.1318(5) 0.4545(2) 0.0297(18) Uani 1 1 d . . .
O12 O 0.4789(7) 0.1413(5) 0.3833(3) 0.0319(18) Uani 1 1 d . . .
O13 O 0.1771(9) 0.3189(7) 0.1864(3) 0.052(2) Uani 1 1 d . . .
H13A H 0.2191 0.3514 0.1701 0.078 Uiso 1 1 calc R . .
O14 O 0.1513(9) 0.2216(7) 0.1231(3) 0.060(3) Uani 1 1 d . . .
O15 O 0.7019(8) 0.9389(6) 0.3586(3) 0.046(2) Uani 1 1 d . . .
H15A H 0.6428 0.9664 0.3385 0.056 Uiso 1 1 d R . .
H15B H 0.7396 0.9811 0.3778 0.056 Uiso 1 1 d R . .
O16 O 0.8598(8) 0.6382(6) 0.9510(3) 0.046(2) Uani 1 1 d . . .
H16A H 0.9214 0.6513 0.9742 0.056 Uiso 1 1 d R . .
H16B H 0.8597 0.6806 0.9297 0.056 Uiso 1 1 d R . .
N1 N -0.1283(9) 0.3304(7) 0.3749(3) 0.033(2) Uani 1 1 d . . .
N2 N -0.3095(9) 0.3471(6) 0.0443(3) 0.032(2) Uani 1 1 d . . .
C1 C 0.4772(11) 0.4012(10) 0.7587(4) 0.038(3) Uani 1 1 d . . .
C2 C 0.6986(11) 0.3641(8) 0.4899(4) 0.033(3) Uani 1 1 d . . .
C3 C 0.2079(10) 0.3552(8) 0.4914(4) 0.030(3) Uani 1 1 d . . .
C4 C 0.5131(10) 0.4607(8) 0.7192(4) 0.035(3) Uani 1 1 d . . .
C5 C 0.5751(11) 0.5517(9) 0.7277(4) 0.041(3) Uani 1 1 d . . .
H5 H 0.5928 0.5774 0.7582 0.049 Uiso 1 1 calc R . .
C6 C 0.6096(11) 0.6026(9) 0.6891(4) 0.042(3) Uani 1 1 d . . .
H6 H 0.6497 0.6631 0.6940 0.051 Uiso 1 1 calc R . .
C7 C 0.5845(11) 0.5637(9) 0.6435(4) 0.039(3) Uani 1 1 d . . .
H7 H 0.6085 0.5981 0.6184 0.047 Uiso 1 1 calc R . .
C8 C 0.5243(10) 0.4745(9) 0.6354(4) 0.032(3) Uani 1 1 d . . .
C9 C 0.4857(10) 0.4241(9) 0.6734(4) 0.036(3) Uani 1 1 d . . .
H9 H 0.4411 0.3654 0.6678 0.044 Uiso 1 1 calc R . .
C10 C 0.4991(10) 0.4330(8) 0.5869(4) 0.032(3) Uani 1 1 d . . .
C11 C 0.6054(10) 0.4215(8) 0.5614(4) 0.032(3) Uani 1 1 d . . .
H11 H 0.6914 0.4409 0.5750 0.038 Uiso 1 1 calc R . .
C12 C 0.5826(10) 0.3813(8) 0.5160(4) 0.030(3) Uani 1 1 d . . .
C13 C 0.4546(9) 0.3587(7) 0.4948(4) 0.027(2) Uani 1 1 d . . .
H13 H 0.4397 0.3335 0.4642 0.032 Uiso 1 1 calc R . .
C14 C 0.3474(10) 0.3722(8) 0.5177(4) 0.032(3) Uani 1 1 d . . .
C15 C 0.3726(11) 0.4051(8) 0.5637(4) 0.034(3) Uani 1 1 d . . .
H15 H 0.3015 0.4090 0.5802 0.041 Uiso 1 1 calc R . .
C16 C -0.0912(11) 0.1310(8) 0.4291(4) 0.033(3) Uani 1 1 d . . .
C17 C 0.3927(10) 0.1336(8) 0.4104(4) 0.028(2) Uani 1 1 d . . .
C18 C 0.1355(11) 0.2375(9) 0.1634(4) 0.041(3) Uani 1 1 d . . .
C19 C 0.0164(10) 0.1188(8) 0.3994(4) 0.031(3) Uani 1 1 d . . .
C20 C 0.1497(10) 0.1280(8) 0.4184(4) 0.031(3) Uani 1 1 d . . .
H20 H 0.1755 0.1346 0.4511 0.037 Uiso 1 1 calc R . .
C21 C 0.2484(10) 0.1275(8) 0.3892(4) 0.030(3) Uani 1 1 d . . .
C22 C 0.2074(10) 0.1200(8) 0.3409(4) 0.030(3) Uani 1 1 d . . .
H22 H 0.2715 0.1212 0.3213 0.036 Uiso 1 1 calc R . .
C23 C 0.0735(10) 0.1105(8) 0.3204(4) 0.032(3) Uani 1 1 d . . .
C24 C -0.0230(10) 0.1075(8) 0.3503(4) 0.030(3) Uani 1 1 d . . .
H24 H -0.1128 0.0981 0.3374 0.036 Uiso 1 1 calc R . .
C25 C 0.0338(10) 0.1093(9) 0.2678(4) 0.035(3) Uani 1 1 d . . .
C26 C -0.0696(10) 0.0511(9) 0.2451(4) 0.036(3) Uani 1 1 d . . .
H26 H -0.1173 0.0121 0.2627 0.044 Uiso 1 1 calc R . .
C27 C -0.1012(11) 0.0519(9) 0.1953(4) 0.042(3) Uani 1 1 d . . .
H27 H -0.1702 0.0132 0.1798 0.051 Uiso 1 1 calc R . .
C28 C -0.0295(11) 0.1106(9) 0.1689(4) 0.040(3) Uani 1 1 d . . .
H28 H -0.0484 0.1094 0.1359 0.047 Uiso 1 1 calc R . .
C29 C 0.0669(11) 0.1688(9) 0.1916(4) 0.036(3) Uani 1 1 d . . .
C30 C 0.1011(11) 0.1696(9) 0.2416(4) 0.039(3) Uani 1 1 d . . .
H30 H 0.1682 0.2104 0.2567 0.046 Uiso 1 1 calc R . .
C31 C -0.0408(11) 0.3460(8) 0.3463(4) 0.036(3) Uani 1 1 d . . .
H31 H 0.0453 0.3650 0.3599 0.044 Uiso 1 1 calc R . .
C32 C -0.0692(12) 0.3358(8) 0.2982(4) 0.040(3) Uani 1 1 d . . .
H32 H -0.0042 0.3484 0.2797 0.048 Uiso 1 1 calc R . .
C33 C -0.1986(12) 0.3059(9) 0.2769(4) 0.044(3) Uani 1 1 d . . .
C34 C -0.2921(12) 0.2935(9) 0.3062(4) 0.042(3) Uani 1 1 d . . .
H34 H -0.3799 0.2772 0.2934 0.050 Uiso 1 1 calc R . .
C35 C -0.2545(11) 0.3054(9) 0.3547(4) 0.038(3) Uani 1 1 d . . .
H35 H -0.3180 0.2960 0.3741 0.045 Uiso 1 1 calc R . .
C36 C -0.2354(13) 0.2894(10) 0.2228(4) 0.048(3) Uani 1 1 d . . .
H36A H -0.1681 0.2488 0.2125 0.057 Uiso 1 1 calc R . .
H36B H -0.3205 0.2559 0.2157 0.057 Uiso 1 1 calc R . .
C37 C -0.2445(14) 0.3799(10) 0.1969(4) 0.052(4) Uani 1 1 d . . .
H37A H -0.1619 0.4156 0.2066 0.063 Uiso 1 1 calc R . .
H37B H -0.3165 0.4180 0.2058 0.063 Uiso 1 1 calc R . .
C38 C -0.2693(13) 0.3694(9) 0.1428(4) 0.045(3) Uani 1 1 d . . .
C39 C -0.1657(13) 0.3740(9) 0.1186(4) 0.048(3) Uani 1 1 d . . .
H39 H -0.0790 0.3838 0.1349 0.057 Uiso 1 1 calc R . .
C40 C -0.1889(12) 0.3643(9) 0.0697(4) 0.043(3) Uani 1 1 d . . .
H40 H -0.1167 0.3701 0.0539 0.051 Uiso 1 1 calc R . .
C41 C -0.4107(12) 0.3362(9) 0.0685(4) 0.041(3) Uani 1 1 d . . .
H41 H -0.4947 0.3190 0.0520 0.049 Uiso 1 1 calc R . .
C42 C -0.3949(13) 0.3493(9) 0.1162(4) 0.043(3) Uani 1 1 d . . .
H42 H -0.4687 0.3449 0.1313 0.051 Uiso 1 1 calc R . .


_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
Cd1 O10 2.242(7) . ?
Cd1 O11 2.263(7) 1_455 ?
Cd1 N2 2.302(9) 4_566 ?
Cd1 O8 2.315(8) . ?
Cd1 O4 2.323(8) 1_455 ?
Cd1 O12 2.633(7) 1_455 ?
Cd2 N1 2.261(8) . ?
Cd2 O5 2.285(7) . ?
Cd2 O3 2.286(7) 1_455 ?
Cd2 O7 2.343(7) . ?
Cd2 O9 2.430(7) . ?
Cd2 O6 2.538(7) . ?
Cd2 C3 2.750(11) . ?
O1 C1 1.343(13) . ?
O2 C1 1.219(14) . ?
O3 C2 1.258(12) . ?
O3 Cd2 2.286(7) 1_655 ?
O4 C2 1.228(13) . ?
O4 Cd1 2.323(8) 1_655 ?
O5 C3 1.285(12) . ?
O6 C3 1.242(12) . ?
O9 C16 1.250(13) . ?
O10 C16 1.255(12) . ?
O11 C17 1.250(11) . ?
O11 Cd1 2.263(7) 1_655 ?
O12 C17 1.271(12) . ?
O12 Cd1 2.633(7) 1_655 ?
O13 C18 1.334(14) . ?
O14 C18 1.210(13) . ?
N1 C31 1.327(13) . ?
N1 C35 1.354(13) . ?
N2 C40 1.331(14) . ?
N2 C41 1.344(14) . ?
N2 Cd1 2.302(9) 4_565 ?
C1 C4 1.494(16) . ?
C2 C12 1.518(15) . ?
C3 C14 1.500(15) . ?
C4 C9 1.387(14) . ?
C4 C5 1.409(16) . ?
C5 C6 1.406(16) . ?
C6 C7 1.392(15) . ?
C7 C8 1.379(15) . ?
C8 C9 1.404(15) . ?
C8 C10 1.479(14) . ?
C10 C15 1.393(14) . ?
C10 C11 1.414(14) . ?
C11 C12 1.394(14) . ?
C12 C13 1.370(14) . ?
C13 C14 1.377(14) . ?
C14 C15 1.373(15) . ?
C16 C19 1.505(15) . ?
C17 C21 1.486(14) . ?
C18 C29 1.495(15) . ?
C19 C20 1.373(14) . ?
C19 C24 1.398(13) . ?
C20 C21 1.413(14) . ?
C21 C22 1.376(14) . ?
C22 C23 1.389(14) . ?
C23 C24 1.409(14) . ?
C23 C25 1.487(14) . ?
C25 C30 1.381(16) . ?
C25 C26 1.389(15) . ?
C26 C27 1.405(14) . ?
C27 C28 1.397(16) . ?
C28 C29 1.343(16) . ?
C29 C30 1.412(15) . ?
C31 C32 1.362(15) . ?
C32 C33 1.409(16) . ?
C33 C34 1.382(16) . ?
C33 C36 1.544(15) . ?
C34 C35 1.383(14) . ?
C36 C37 1.450(17) . ?
C37 C38 1.528(16) . ?
C38 C39 1.359(17) . ?
C38 C42 1.393(17) . ?
C39 C40 1.383(16) . ?
C41 C42 1.358(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Cd1 O11 131.3(2) . 1_455 ?
O10 Cd1 N2 130.7(3) . 4_566 ?
O11 Cd1 N2 95.0(3) 1_455 4_566 ?
O10 Cd1 O8 79.4(3) . . ?
O11 Cd1 O8 89.4(3) 1_455 . ?
N2 Cd1 O8 86.0(3) 4_566 . ?
O10 Cd1 O4 96.1(3) . 1_455 ?
O11 Cd1 O4 100.6(2) 1_455 1_455 ?
N2 Cd1 O4 89.8(3) 4_566 1_455 ?
O8 Cd1 O4 169.5(2) . 1_455 ?
O10 Cd1 O12 82.2(2) . 1_455 ?
O11 Cd1 O12 52.4(2) 1_455 1_455 ?
N2 Cd1 O12 146.8(3) 4_566 1_455 ?
O8 Cd1 O12 98.2(2) . 1_455 ?
O4 Cd1 O12 90.5(2) 1_455 1_455 ?
N1 Cd2 O5 147.1(3) . . ?
N1 Cd2 O3 123.9(3) . 1_455 ?
O5 Cd2 O3 88.2(3) . 1_455 ?
N1 Cd2 O7 84.3(3) . . ?
O5 Cd2 O7 90.3(2) . . ?
O3 Cd2 O7 88.9(3) 1_455 . ?
N1 Cd2 O9 92.2(3) . . ?
O5 Cd2 O9 85.7(2) . . ?
O3 Cd2 O9 103.7(2) 1_455 . ?
O7 Cd2 O9 166.6(2) . . ?
N1 Cd2 O6 93.1(3) . . ?
O5 Cd2 O6 54.3(2) . . ?
O3 Cd2 O6 138.6(2) 1_455 . ?
O7 Cd2 O6 75.9(3) . . ?
O9 Cd2 O6 91.4(2) . . ?
N1 Cd2 C3 119.8(3) . . ?
O5 Cd2 C3 27.7(3) . . ?
O3 Cd2 C3 113.6(3) 1_455 . ?
O7 Cd2 C3 80.3(3) . . ?
O9 Cd2 C3 90.4(3) . . ?
O6 Cd2 C3 26.8(3) . . ?
C2 O3 Cd2 101.3(7) . 1_655 ?
C2 O4 Cd1 126.3(7) . 1_655 ?
C3 O5 Cd2 96.8(6) . . ?
C3 O6 Cd2 86.2(6) . . ?
C16 O9 Cd2 110.7(7) . . ?
C16 O10 Cd1 109.4(6) . . ?
C17 O11 Cd1 102.6(6) . 1_655 ?
C17 O12 Cd1 84.6(6) . 1_655 ?
C31 N1 C35 117.6(9) . . ?
C31 N1 Cd2 118.8(7) . . ?
C35 N1 Cd2 123.6(7) . . ?
C40 N2 C41 116.8(10) . . ?
C40 N2 Cd1 120.4(7) . 4_565 ?
C41 N2 Cd1 122.1(8) . 4_565 ?
O2 C1 O1 122.6(11) . . ?
O2 C1 C4 123.8(10) . . ?
O1 C1 C4 113.6(11) . . ?
O4 C2 O3 123.1(10) . . ?
O4 C2 C12 118.8(10) . . ?
O3 C2 C12 118.0(10) . . ?
O6 C3 O5 122.2(10) . . ?
O6 C3 C14 121.0(9) . . ?
O5 C3 C14 116.8(10) . . ?
O6 C3 Cd2 67.0(6) . . ?
O5 C3 Cd2 55.6(5) . . ?
C14 C3 Cd2 169.7(7) . . ?
C9 C4 C5 119.9(11) . . ?
C9 C4 C1 118.6(11) . . ?
C5 C4 C1 121.5(10) . . ?
C6 C5 C4 118.5(11) . . ?
C7 C6 C5 120.8(12) . . ?
C8 C7 C6 120.5(11) . . ?
C7 C8 C9 119.3(10) . . ?
C7 C8 C10 120.3(10) . . ?
C9 C8 C10 120.5(11) . . ?
C4 C9 C8 120.9(11) . . ?
C15 C10 C11 116.5(10) . . ?
C15 C10 C8 123.2(9) . . ?
C11 C10 C8 120.3(9) . . ?
C12 C11 C10 120.6(9) . . ?
C13 C12 C11 119.5(9) . . ?
C13 C12 C2 120.3(10) . . ?
C11 C12 C2 120.2(10) . . ?
C12 C13 C14 121.8(10) . . ?
C15 C14 C13 118.0(10) . . ?
C15 C14 C3 122.2(9) . . ?
C13 C14 C3 119.7(10) . . ?
C14 C15 C10 123.4(10) . . ?
O9 C16 O10 123.1(10) . . ?
O9 C16 C19 118.3(10) . . ?
O10 C16 C19 118.5(10) . . ?
O11 C17 O12 120.3(9) . . ?
O11 C17 C21 120.3(9) . . ?
O12 C17 C21 119.4(9) . . ?
O14 C18 O13 122.6(11) . . ?
O14 C18 C29 123.3(12) . . ?
O13 C18 C29 114.0(10) . . ?
C20 C19 C24 119.8(9) . . ?
C20 C19 C16 121.8(10) . . ?
C24 C19 C16 118.1(9) . . ?
C19 C20 C21 121.1(10) . . ?
C22 C21 C20 118.3(10) . . ?
C22 C21 C17 121.1(9) . . ?
C20 C21 C17 120.6(9) . . ?
C21 C22 C23 122.1(10) . . ?
C22 C23 C24 118.7(9) . . ?
C22 C23 C25 119.9(9) . . ?
C24 C23 C25 121.3(9) . . ?
C19 C24 C23 120.0(9) . . ?
C30 C25 C26 120.1(10) . . ?
C30 C25 C23 118.0(10) . . ?
C26 C25 C23 121.9(10) . . ?
C25 C26 C27 119.3(10) . . ?
C28 C27 C26 120.3(11) . . ?
C29 C28 C27 119.5(11) . . ?
C28 C29 C30 121.5(11) . . ?
C28 C29 C18 119.4(10) . . ?
C30 C29 C18 119.1(11) . . ?
C25 C30 C29 119.2(11) . . ?
N1 C31 C32 124.1(11) . . ?
C31 C32 C33 118.8(11) . . ?
C34 C33 C32 117.5(11) . . ?
C34 C33 C36 121.2(11) . . ?
C32 C33 C36 121.3(11) . . ?
C33 C34 C35 119.7(11) . . ?
N1 C35 C34 122.1(11) . . ?
C37 C36 C33 111.5(11) . . ?
C36 C37 C38 114.7(11) . . ?
C39 C38 C42 116.5(11) . . ?
C39 C38 C37 120.4(12) . . ?
C42 C38 C37 123.0(12) . . ?
C38 C39 C40 120.1(12) . . ?
N2 C40 C39 123.2(11) . . ?
N2 C41 C42 122.4(12) . . ?
C41 C42 C38 120.8(11) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.173
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.204

data_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H23 N3 O10 Zn'
_chemical_formula_weight         614.85

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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   19.507(2)
_cell_length_b                   12.5344(9)
_cell_length_c                   11.6931(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.375(10)
_cell_angle_gamma                90.00
_cell_volume                     2583.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    121.50(14)
_cell_measurement_reflns_used    556
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      28.34

_exptl_crystal_description       flake
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8373
_exptl_absorpt_correction_T_max  0.9319
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      121.50(14)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector_area_resol_mean 16.2563
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4592
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.1361
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2279
_reflns_number_gt                1305
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0747P)²+1.7079P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2279
_refine_ls_number_parameters     200
_refine_ls_number_restraints     743
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.2139
_refine_ls_wR_factor_gt          0.1690
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.0000 0.86125(9) 0.2500 0.0448(5) Uani 1 2 d SU . .
N1 N -0.0870(3) 0.9683(4) 0.1748(5) 0.0396(13) Uani 1 1 d U B .
N2 N 0.1484(4) 0.4014(6) 0.0821(7) 0.0577(17) Uani 0.50 1 d PDU A 2
O1 O -0.0136(5) 0.8142(9) 0.0512(10) 0.0505(16) Uani 0.582(15) 1 d PDU B 1
O2 O 0.0778(7) 0.7393(8) 0.2201(8) 0.046(2) Uani 0.582(15) 1 d PDU B 1
O3 O 0.1727(7) 0.3966(12) 0.2009(7) 0.074(3) Uani 0.79(3) 1 d PDU A 1
O4 O 0.1673(7) 0.3340(8) 0.0180(9) 0.077(3) Uani 0.79(3) 1 d PDU A 1
H4 H 0.1934 0.2868 0.0651 0.116 Uiso 0.396(13) 1 calc PRD A 1
O5 O 0.2701(5) 0.1988(8) 0.1476(10) 0.189(4) Uani 1 1 d DU . .
H5C H 0.3135 0.2145 0.2056 0.227 Uiso 1 1 d RD A .
H5D H 0.2758 0.1634 0.0903 0.227 Uiso 1 1 d RD . .
C1 C 0.0360(4) 0.7518(6) 0.0979(7) 0.0509(16) Uani 1 1 d DU . .
C2 C 0.1484(4) 0.4014(6) 0.0821(7) 0.0577(17) Uani 0.50 1 d PU A 1
C3 C 0.0510(4) 0.6647(5) 0.0224(6) 0.0429(16) Uani 1 1 d DU B .
C4 C 0.0950(4) 0.5772(5) 0.0849(7) 0.0462(16) Uani 1 1 d DU . .
H4A H 0.1195 0.5760 0.1728 0.055 Uiso 1 1 calc R B .
C5 C 0.1022(4) 0.4922(5) 0.0156(6) 0.0430(16) Uani 1 1 d DU A .
C6 C 0.0646(3) 0.4916(5) -0.1166(6) 0.0388(16) Uani 1 1 d DU . .
H6 H 0.0693 0.4329 -0.1615 0.047 Uiso 1 1 calc R B .
C7 C 0.0204(3) 0.5783(5) -0.1816(6) 0.0329(14) Uani 1 1 d DU . .
C8 C 0.0150(3) 0.6658(5) -0.1100(6) 0.0379(15) Uani 1 1 d DU . .
H8 H -0.0130 0.7254 -0.1516 0.045 Uiso 1 1 calc R B .
C9 C -0.1389(4) 0.9648(7) 0.0559(7) 0.0560(19) Uani 1 1 d U . .
H9 H -0.1361 0.9104 0.0040 0.067 Uiso 1 1 calc R B .
C10 C -0.1965(4) 1.0379(7) 0.0060(8) 0.059(2) Uani 1 1 d U B .
H10 H -0.2306 1.0324 -0.0788 0.071 Uiso 1 1 calc R . .
C11 C -0.2053(4) 1.1192(6) 0.0780(7) 0.0403(16) Uani 1 1 d U . .
C12 C -0.1517(4) 1.1206(6) 0.2041(7) 0.0473(18) Uani 1 1 d U B .
H12 H -0.1542 1.1729 0.2586 0.057 Uiso 1 1 calc R . .
C13 C -0.0953(4) 1.0453(6) 0.2482(7) 0.0479(18) Uani 1 1 d U . .
H13 H -0.0610 1.0476 0.3331 0.057 Uiso 1 1 calc R B .
C14 C -0.2641(4) 1.2033(6) 0.0253(7) 0.0434(17) Uani 1 1 d U . .
H14A H -0.2782 1.2283 0.0909 0.052 Uiso 1 1 calc R . .
H14B H -0.3090 1.1734 -0.0425 0.052 Uiso 1 1 calc R . .
O2' O 0.0057(9) 0.8422(10) 0.0355(12) 0.046(2) Uani 0.418(15) 1 d PDU B 2
O1' O 0.0437(9) 0.7445(13) 0.2072(12) 0.0505(16) Uani 0.418(15) 1 d PDU B 2
O4' O 0.135(3) 0.316(2) 0.020(4) 0.077(3) Uani 0.21(3) 1 d PDU A 2
H4' H 0.1627 0.2686 0.0641 0.116 Uiso 0.104(13) 1 calc PR A 2
O3' O 0.198(2) 0.403(5) 0.195(2) 0.074(3) Uani 0.21(3) 1 d PDU A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1' 1.867(16) 2 ?
Zn1 O1' 1.867(16) . ?
Zn1 N1 2.043(5) 2 ?
Zn1 N1 2.043(5) . ?
Zn1 O2 2.285(12) 2 ?
Zn1 O2 2.285(12) . ?
Zn1 O1 2.301(11) . ?
Zn1 O1 2.301(11) 2 ?
Zn1 C1 2.571(8) 2 ?
N1 C9 1.324(8) . ?
N1 C13 1.347(8) . ?
N2 O4' 1.259(15) . ?
N2 O3' 1.261(15) . ?
N2 C5 1.453(9) . ?
N2 O5 3.334(11) . ?
O1 C1 1.181(9) . ?
O2 C1 1.317(10) . ?
O4 H4 0.8200 . ?
O5 H5C 0.8501 . ?
O5 H5D 0.8501 . ?
C1 O1' 1.225(11) . ?
C1 O2' 1.341(11) . ?
C1 C3 1.509(10) . ?
C3 C4 1.391(7) . ?
C3 C8 1.399(7) . ?
C4 C5 1.382(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.399(7) . ?
C6 C7 1.393(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.411(7) . ?
C7 C7 1.449(12) 2_554 ?
C8 H8 0.9300 . ?
C9 C10 1.372(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(10) . ?
C11 C14 1.484(9) . ?
C12 C13 1.371(9) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C14 1.518(13) 7_475 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
O4' H4' 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1' Zn1 O1' 76.7(9) 2 . ?
O1' Zn1 N1 142.2(5) 2 2 ?
O1' Zn1 N1 103.9(5) . 2 ?
O1' Zn1 N1 103.9(5) 2 . ?
O1' Zn1 N1 142.2(5) . . ?
N1 Zn1 N1 97.9(3) 2 . ?
O1' Zn1 O2 12.7(5) 2 2 ?
O1' Zn1 O2 85.7(5) . 2 ?
N1 Zn1 O2 149.0(3) 2 2 ?
N1 Zn1 O2 91.2(3) . 2 ?
O1' Zn1 O2 85.7(5) 2 . ?
O1' Zn1 O2 12.7(5) . . ?
N1 Zn1 O2 91.2(3) 2 . ?
N1 Zn1 O2 149.0(3) . . ?
O2 Zn1 O2 96.0(6) 2 . ?
O1' Zn1 O1 101.6(5) 2 . ?
O1' Zn1 O1 52.9(5) . . ?
N1 Zn1 O1 108.6(3) 2 . ?
N1 Zn1 O1 91.0(3) . . ?
O2 Zn1 O1 100.7(4) 2 . ?
O2 Zn1 O1 58.0(3) . . ?
O1' Zn1 O1 52.9(5) 2 2 ?
O1' Zn1 O1 101.6(5) . 2 ?
N1 Zn1 O1 91.0(3) 2 2 ?
N1 Zn1 O1 108.6(3) . 2 ?
O2 Zn1 O1 58.0(3) 2 2 ?
O2 Zn1 O1 100.7(4) . 2 ?
O1 Zn1 O1 150.3(6) . 2 ?
O1' Zn1 C1 26.4(4) 2 2 ?
O1' Zn1 C1 93.3(4) . 2 ?
N1 Zn1 C1 118.4(2) 2 2 ?
N1 Zn1 C1 103.1(2) . 2 ?
O2 Zn1 C1 30.8(2) 2 2 ?
O2 Zn1 C1 98.3(3) . 2 ?
O1 Zn1 C1 127.9(4) . 2 ?
O1 Zn1 C1 27.3(2) 2 2 ?
C9 N1 C13 116.5(6) . . ?
C9 N1 Zn1 123.4(5) . . ?
C13 N1 Zn1 120.0(5) . . ?
O4' N2 O3' 120(4) . . ?
O4' N2 C5 115(2) . . ?
O3' N2 C5 124(3) . . ?
O4' N2 O5 56(2) . . ?
O3' N2 O5 68(3) . . ?
C5 N2 O5 159.5(5) . . ?
C1 O1 Zn1 89.2(7) . . ?
C1 O2 Zn1 86.7(6) . . ?
N2 O5 H5C 112.0 . . ?
N2 O5 H5D 122.5 . . ?
H5C O5 H5D 109.3 . . ?
O1 C1 O1' 104.0(11) . . ?
O1 C1 O2 125.8(9) . . ?
O1' C1 O2 28.0(6) . . ?
O1 C1 O2' 26.5(6) . . ?
O1' C1 O2' 117.4(11) . . ?
O2 C1 O2' 128.0(10) . . ?
O1 C1 C3 122.3(8) . . ?
O1' C1 C3 126.1(10) . . ?
O2 C1 C3 111.3(7) . . ?
O2' C1 C3 116.3(8) . . ?
C4 C3 C8 119.5(6) . . ?
C4 C3 C1 119.5(6) . . ?
C8 C3 C1 120.6(6) . . ?
C5 C4 C3 119.6(7) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 121.1(6) . . ?
C4 C5 N2 119.1(6) . . ?
C6 C5 N2 119.9(6) . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 118.0(6) . . ?
C6 C7 C7 121.4(4) . 2_554 ?
C8 C7 C7 120.7(4) . 2_554 ?
C3 C8 C7 121.3(6) . . ?
C3 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
N1 C9 C10 122.9(7) . . ?
N1 C9 H9 118.6 . . ?
C10 C9 H9 118.6 . . ?
C9 C10 C11 121.8(7) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C12 115.0(7) . . ?
C10 C11 C14 123.2(7) . . ?
C12 C11 C14 121.7(7) . . ?
C13 C12 C11 120.4(7) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
N1 C13 C12 123.4(7) . . ?
N1 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C11 C14 C14 111.3(6) . 7_475 ?
C11 C14 H14A 109.4 . . ?
C14 C14 H14A 109.4 7_475 . ?
C11 C14 H14B 109.4 . . ?
C14 C14 H14B 109.4 7_475 . ?
H14A C14 H14B 108.0 . . ?
C1 O1' Zn1 110.8(11) . . ?
N2 O4' H4' 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.096
