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


data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H36 N4 O12 Zn2'
_chemical_formula_sum            'C35 H36 N4 O12 Zn2'
_chemical_formula_weight         835.42

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   P21212
_symmetry_space_group_name_hall  'P 2 2ab'

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

_cell_length_a                   16.397(3)
_cell_length_b                   18.642(3)
_cell_length_c                   7.9656(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2434.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    4725
_cell_measurement_theta_min      2.480
_cell_measurement_theta_max      25.964

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7744
_exptl_absorpt_correction_T_max  0.8041
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12983
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4784
_reflns_number_gt                4442
_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)+(0.0862P)²+0.5067P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constra
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(17)
_refine_ls_number_reflns         4784
_refine_ls_number_parameters     234
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1338
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3398(3) 0.6997(3) 0.5914(6) 0.0578(12) Uani 1 1 d . . .
H1 H 0.3546 0.7374 0.6617 0.069 Uiso 1 1 calc R . .
C2 C 0.4011(3) 0.6629(3) 0.5061(6) 0.0558(12) Uani 1 1 d . . .
H2 H 0.4554 0.6764 0.5180 0.067 Uiso 1 1 calc R . .
C3 C 0.3805(3) 0.6066(2) 0.4048(5) 0.0406(9) Uani 1 1 d U . .
C4 C 0.2990(2) 0.5889(2) 0.3891(6) 0.0419(9) Uani 1 1 d . . .
H4 H 0.2829 0.5510 0.3211 0.050 Uiso 1 1 calc R . .
C5 C 0.2432(3) 0.6279(2) 0.4745(6) 0.0475(10) Uani 1 1 d . . .
H5 H 0.1886 0.6155 0.4617 0.057 Uiso 1 1 calc R . .
C6 C 0.1764(3) 0.8818(2) 0.4801(5) 0.0456(9) Uani 1 1 d . . .
H6 H 0.2103 0.8987 0.5650 0.055 Uiso 1 1 calc R . .
C7 C 0.1546(3) 0.9278(2) 0.3552(5) 0.0508(11) Uani 1 1 d . . .
H7 H 0.1730 0.9750 0.3566 0.061 Uiso 1 1 calc R . .
C8 C 0.1047(2) 0.9039(2) 0.2252(5) 0.0374(8) Uani 1 1 d . . .
C9 C 0.0826(2) 0.8322(2) 0.2257(5) 0.0386(9) Uani 1 1 d . . .
H9 H 0.0518 0.8132 0.1384 0.046 Uiso 1 1 calc R . .
C10 C 0.1067(2) 0.7899(2) 0.3562(5) 0.0412(9) Uani 1 1 d . . .
H10 H 0.0913 0.7419 0.3540 0.049 Uiso 1 1 calc R . .
C11 C 0.0182(3) 0.9335(2) -0.0034(5) 0.0388(8) Uani 1 1 d . . .
H11A H -0.0299 0.9190 0.0588 0.047 Uiso 1 1 calc R . .
H11B H 0.0348 0.8942 -0.0754 0.047 Uiso 1 1 calc R . .
C12 C 0.0000 1.0000 -0.1078(6) 0.0317(10) Uani 1 2 d S . .
C13 C 0.4237(2) 0.5152(2) 0.2165(5) 0.0378(8) Uani 1 1 d . . .
H13A H 0.3776 0.5268 0.1453 0.045 Uiso 1 1 calc R . .
H13B H 0.4100 0.4733 0.2828 0.045 Uiso 1 1 calc R . .
C14 C 0.2496(3) 0.7648(3) 0.9740(6) 0.0577(12) Uani 1 1 d U . .
C15 C 0.2985(3) 0.7949(3) 1.1129(7) 0.0664(15) Uani 1 1 d . . .
H15A H 0.2781 0.7766 1.2188 0.080 Uiso 1 1 calc R . .
H15B H 0.2927 0.8467 1.1140 0.080 Uiso 1 1 calc R . .
C16 C 0.3879(3) 0.7758(3) 1.0958(6) 0.0538(11) Uani 1 1 d . . .
H16A H 0.4065 0.7885 0.9841 0.065 Uiso 1 1 calc R . .
H16B H 0.3946 0.7245 1.1095 0.065 Uiso 1 1 calc R . .
C17 C -0.0601(3) 0.6855(3) 0.7751(6) 0.0511(11) Uani 1 1 d . . .
H17A H -0.0572 0.6352 0.8051 0.061 Uiso 1 1 calc R . .
H17B H -0.0868 0.6888 0.6667 0.061 Uiso 1 1 calc R . .
C18 C 0.0253(3) 0.7140(3) 0.7582(6) 0.0459(10) Uani 1 1 d . . .
Zn1 Zn 0.17237(2) 0.74542(2) 0.68840(5) 0.03729(15) Uani 1 1 d . . .
N1 N 0.2607(2) 0.68329(18) 0.5766(5) 0.0423(8) Uani 1 1 d . . .
N2 N 0.15094(19) 0.81232(17) 0.4871(4) 0.0365(7) Uani 1 1 d . . .
O1 O 0.2216(2) 0.7027(2) 0.9736(5) 0.0702(7) Uani 1 1 d U . .
O2 O 0.2356(2) 0.8057(2) 0.8487(5) 0.0702(7) Uani 1 1 d . . .
O3 O 0.0472(2) 0.77111(18) 0.8207(5) 0.0608(8) Uani 1 1 d . . .
O4 O 0.07548(18) 0.67795(17) 0.6719(4) 0.0551(8) Uani 1 1 d . . .
O5 O 0.08261(18) 0.95217(15) 0.1093(4) 0.0447(7) Uani 1 1 d . . .
O6 O 0.44237(16) 0.57472(16) 0.3246(4) 0.0465(7) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.339(6) . ?
C1 C2 1.394(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.367(6) . ?
C2 H2 0.9300 . ?
C3 O6 1.338(5) . ?
C3 C4 1.380(6) . ?
C4 C5 1.353(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.345(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.361(6) . ?
C6 N2 1.363(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.393(6) . ?
C7 H7 0.9300 . ?
C8 O5 1.339(5) . ?
C8 C9 1.385(5) . ?
C9 C10 1.363(5) . ?
C9 H9 0.9300 . ?
C10 N2 1.337(5) . ?
C10 H10 0.9300 . ?
C11 O5 1.429(5) . ?
C11 C12 1.522(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C11 1.522(5) 2_575 ?
C12 C13 1.547(5) 4_465 ?
C12 C13 1.547(5) 3 ?
C13 O6 1.437(5) . ?
C13 C12 1.547(5) 3_545 ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O1 1.245(6) . ?
C14 O2 1.277(6) . ?
C14 C15 1.477(7) . ?
C15 C16 1.515(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.517(6) 4_567 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.503(6) . ?
C17 C16 1.517(6) 4_467 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O3 1.229(6) . ?
C18 O4 1.266(5) . ?
Zn1 O2 1.993(4) . ?
Zn1 O4 2.030(3) . ?
Zn1 N1 2.057(3) . ?
Zn1 N2 2.062(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.9(4) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
O6 C3 C2 115.8(4) . . ?
O6 C3 C4 125.8(4) . . ?
C2 C3 C4 118.4(4) . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 124.9(4) . . ?
N1 C5 H5 117.5 . . ?
C4 C5 H5 117.5 . . ?
C7 C6 N2 123.2(4) . . ?
C7 C6 H6 118.4 . . ?
N2 C6 H6 118.4 . . ?
C6 C7 C8 119.8(4) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
O5 C8 C9 125.5(4) . . ?
O5 C8 C7 117.2(3) . . ?
C9 C8 C7 117.4(4) . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N2 C10 C9 124.8(4) . . ?
N2 C10 H10 117.6 . . ?
C9 C10 H10 117.6 . . ?
O5 C11 C12 106.8(3) . . ?
O5 C11 H11A 110.4 . . ?
C12 C11 H11A 110.4 . . ?
O5 C11 H11B 110.4 . . ?
C12 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 C11 113.8(4) . 2_575 ?
C11 C12 C13 108.3(2) . 4_465 ?
C11 C12 C13 107.3(2) 2_575 4_465 ?
C11 C12 C13 107.3(2) . 3 ?
C11 C12 C13 108.3(2) 2_575 3 ?
C13 C12 C13 111.9(4) 4_465 3 ?
O6 C13 C12 107.8(3) . 3_545 ?
O6 C13 H13A 110.2 . . ?
C12 C13 H13A 110.2 3_545 . ?
O6 C13 H13B 110.2 . . ?
C12 C13 H13B 110.2 3_545 . ?
H13A C13 H13B 108.5 . . ?
O1 C14 O2 119.2(4) . . ?
O1 C14 C15 123.6(5) . . ?
O2 C14 C15 117.2(5) . . ?
C14 C15 C16 111.7(4) . . ?
C14 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 C17 111.8(4) . 4_567 ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 4_567 . ?
C15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 4_567 . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C16 114.6(4) . 4_467 ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17A 108.6 4_467 . ?
C18 C17 H17B 108.6 . . ?
C16 C17 H17B 108.6 4_467 . ?
H17A C17 H17B 107.6 . . ?
O3 C18 O4 119.3(4) . . ?
O3 C18 C17 122.9(4) . . ?
O4 C18 C17 117.8(4) . . ?
O2 Zn1 O4 142.97(15) . . ?
O2 Zn1 N1 103.24(16) . . ?
O4 Zn1 N1 100.02(13) . . ?
O2 Zn1 N2 104.22(15) . . ?
O4 Zn1 N2 101.01(13) . . ?
N1 Zn1 N2 97.11(13) . . ?
C1 N1 C5 115.8(4) . . ?
C1 N1 Zn1 121.0(3) . . ?
C5 N1 Zn1 123.0(3) . . ?
C10 N2 C6 115.6(3) . . ?
C10 N2 Zn1 120.7(3) . . ?
C6 N2 Zn1 123.7(3) . . ?
C14 O2 Zn1 104.9(3) . . ?
C18 O4 Zn1 98.3(3) . . ?
C8 O5 C11 118.0(3) . . ?
C3 O6 C13 117.9(3) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.031 381 79 ' '
2 0.500 0.000 -0.068 381 79 ' '
_platon_squeeze_details          ?


_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 973268'

data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H48 Cu2 N4 O16'
_chemical_formula_sum            'C37 H48 Cu2 N4 O16'
_chemical_formula_weight         931.87

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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           'Tetragonal '
_symmetry_space_group_name_H-M   P42/n
_symmetry_space_group_name_hall  '-P 4bc'

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

_cell_length_a                   15.4019(10)
_cell_length_b                   15.4019(10)
_cell_length_c                   8.4768(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2010.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2176
_cell_measurement_theta_min      2.638
_cell_measurement_theta_max      23.275

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10740
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1758
_reflns_number_gt                1320
_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)+(0.0551P)²+12.7631P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constra
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1758
_refine_ls_number_parameters     129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1689
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 1.0000 0.0000 0.0393(3) Uani 1 2 d S . .
O1 O 0.7150(3) 0.8481(3) 0.5421(5) 0.0508(11) Uani 1 1 d . . .
O2 O 0.4163(3) 0.9071(3) 0.0304(6) 0.0614(13) Uani 1 1 d . . .
O3 O 0.4936(3) 0.8488(3) -0.1592(6) 0.065 Uani 1 1 d . . .
N1 N 0.5667(3) 0.9574(3) 0.1891(5) 0.0413(11) Uani 1 1 d . . .
C1 C 0.5277(4) 0.9249(4) 0.3174(7) 0.0450(14) Uani 1 1 d . . .
H1 H 0.4674 0.9268 0.3222 0.054 Uiso 1 1 calc R . .
C2 C 0.5722(4) 0.8889(4) 0.4431(7) 0.0445(14) Uani 1 1 d . . .
H2 H 0.5426 0.8670 0.5301 0.053 Uiso 1 1 calc R . .
C3 C 0.6623(4) 0.8862(4) 0.4359(6) 0.0402(13) Uani 1 1 d . . .
C4 C 0.7030(4) 0.9238(4) 0.3072(7) 0.0507(16) Uani 1 1 d . . .
H4 H 0.7633 0.9254 0.3014 0.061 Uiso 1 1 calc R . .
C5 C 0.6538(4) 0.9582(4) 0.1889(7) 0.0478(15) Uani 1 1 d . . .
H5 H 0.6821 0.9837 0.1038 0.057 Uiso 1 1 calc R . .
C6 C 0.6770(4) 0.7889(4) 0.6506(7) 0.0437(14) Uani 1 1 d . . .
H6A H 0.6465 0.7433 0.5943 0.052 Uiso 1 1 calc R . .
H6B H 0.6358 0.8188 0.7178 0.052 Uiso 1 1 calc R . .
C7 C 0.7500 0.7500 0.7500 0.036(2) Uani 1 4 d S . .
C8 C 0.4347(5) 0.8447(5) -0.0690(11) 0.067(2) Uani 1 1 d . . .
C9 C 0.3727(6) 0.7673(5) -0.0633(14) 0.098(3) Uani 1 1 d . . .
H9A H 0.3847 0.7300 -0.1529 0.118 Uiso 1 1 calc R . .
H9B H 0.3847 0.7341 0.0315 0.118 Uiso 1 1 calc R . .
C10 C 0.2802(5) 0.7898(5) -0.0649(12) 0.083(3) Uani 1 1 d . . .
H10A H 0.2682 0.8245 -0.1579 0.099 Uiso 1 1 calc R . .
H10B H 0.2673 0.8251 0.0269 0.099 Uiso 1 1 calc R . .
O1W O 0.315(2) -0.0001(16) 0.206(3) 0.454(17) Uani 1 1 d . . .
H1WA H 0.3649 -0.0151 0.2402 0.545 Uiso 1 1 d R . .
H1WB H 0.2896 0.0303 0.2762 0.681 Uiso 1 1 d 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
Cu1 O2 1.943(4) 5_675 ?
Cu1 O2 1.943(4) . ?
Cu1 N1 2.014(4) . ?
Cu1 N1 2.014(4) 5_675 ?
O1 C3 1.346(7) . ?
O1 C6 1.421(7) . ?
O2 C8 1.310(10) . ?
O3 C8 1.188(9) . ?
N1 C1 1.339(7) . ?
N1 C5 1.341(7) . ?
C1 C2 1.384(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.391(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(8) . ?
C4 C5 1.364(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.527(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C6 1.527(6) 6_577 ?
C7 C6 1.527(6) 8_757 ?
C7 C6 1.527(6) 3_665 ?
C8 C9 1.529(9) . ?
C9 C10 1.467(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C10 1.539(13) 3_565 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.000(1) 5_675 . ?
O2 Cu1 N1 90.41(18) 5_675 . ?
O2 Cu1 N1 89.59(18) . . ?
O2 Cu1 N1 89.59(18) 5_675 5_675 ?
O2 Cu1 N1 90.41(18) . 5_675 ?
N1 Cu1 N1 180.0(2) . 5_675 ?
C3 O1 C6 117.7(4) . . ?
C8 O2 Cu1 108.1(4) . . ?
C1 N1 C5 117.0(5) . . ?
C1 N1 Cu1 122.6(4) . . ?
C5 N1 Cu1 120.4(4) . . ?
N1 C1 C2 123.6(5) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.2(5) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
O1 C3 C4 115.9(5) . . ?
O1 C3 C2 125.8(5) . . ?
C4 C3 C2 118.3(5) . . ?
C3 C4 C5 119.3(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 123.5(5) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
O1 C6 C7 107.8(4) . . ?
O1 C6 H6A 110.1 . . ?
C7 C6 H6A 110.1 . . ?
O1 C6 H6B 110.1 . . ?
C7 C6 H6B 110.1 . . ?
H6A C6 H6B 108.5 . . ?
C6 C7 C6 107.7(2) 6_577 . ?
C6 C7 C6 113.0(4) 6_577 8_757 ?
C6 C7 C6 107.7(2) . 8_757 ?
C6 C7 C6 107.7(2) 6_577 3_665 ?
C6 C7 C6 113.0(4) . 3_665 ?
C6 C7 C6 107.7(2) 8_757 3_665 ?
O3 C8 O2 122.8(6) . . ?
O3 C8 C9 122.6(9) . . ?
O2 C8 C9 114.6(8) . . ?
C10 C9 C8 115.0(7) . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C10 113.5(10) . 3_565 ?
C9 C10 H10A 108.9 . . ?
C10 C10 H10A 108.9 3_565 . ?
C9 C10 H10B 108.9 . . ?
C10 C10 H10B 108.9 3_565 . ?
H10A C10 H10B 107.7 . . ?
H1WA O1W H1WB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu1 O2 C8 79(100) 5_675 . . . ?
N1 Cu1 O2 C8 -100.0(4) . . . . ?
N1 Cu1 O2 C8 80.0(4) 5_675 . . . ?
O2 Cu1 N1 C1 143.4(5) 5_675 . . . ?
O2 Cu1 N1 C1 -36.6(5) . . . . ?
N1 Cu1 N1 C1 -66(100) 5_675 . . . ?
O2 Cu1 N1 C5 -38.5(5) 5_675 . . . ?
O2 Cu1 N1 C5 141.5(5) . . . . ?
N1 Cu1 N1 C5 112(100) 5_675 . . . ?
C5 N1 C1 C2 -3.5(9) . . . . ?
Cu1 N1 C1 C2 174.6(5) . . . . ?
N1 C1 C2 C3 0.0(9) . . . . ?
C6 O1 C3 C4 -162.9(5) . . . . ?
C6 O1 C3 C2 15.4(9) . . . . ?
C1 C2 C3 O1 -174.9(6) . . . . ?
C1 C2 C3 C4 3.3(9) . . . . ?
O1 C3 C4 C5 175.3(6) . . . . ?
C2 C3 C4 C5 -3.0(9) . . . . ?
C1 N1 C5 C4 3.8(9) . . . . ?
Cu1 N1 C5 C4 -174.4(5) . . . . ?
C3 C4 C5 N1 -0.6(10) . . . . ?
C3 O1 C6 C7 176.2(4) . . . . ?
O1 C6 C7 C6 66.0(2) . . . 6_577 ?
O1 C6 C7 C6 -171.8(4) . . . 8_757 ?
O1 C6 C7 C6 -52.9(3) . . . 3_665 ?
Cu1 O2 C8 O3 -0.1(8) . . . . ?
Cu1 O2 C8 C9 -178.3(5) . . . . ?
O3 C8 C9 C10 -130.4(9) . . . . ?
O2 C8 C9 C10 47.8(12) . . . . ?
C8 C9 C10 C10 178.0(6) . . . 3_565 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.957
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.116
_database_code_depnum_ccdc_archive 'CCDC 973269'

data_101202c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H34 N6 O14 Zn2'
_chemical_formula_sum            'C33 H34 N6 O14 Zn2'
_chemical_formula_weight         869.40

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   'I b a m'
_symmetry_space_group_name_Hall  '-I 2 2c '

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

_cell_length_a                   32.119(3)
_cell_length_b                   12.8479(10)
_cell_length_c                   20.8244(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8593.5(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    5890
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3568
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_T_max  0.7980
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22451
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4343
_reflns_number_gt                3330
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0918P)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         4343
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1509
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.32929(14) 0.7454(4) 0.5000 0.0328(10) Uani 1 2 d S . .
C3 C 0.25348(12) 0.8510(3) 0.60914(18) 0.0480(10) Uani 1 1 d . . .
C4 C 0.25078(12) 0.9537(3) 0.62166(18) 0.0451(9) Uani 1 1 d . . .
H4 H 0.2700 0.9989 0.6033 0.054 Uiso 1 1 calc R . .
C5 C 0.22065(11) 0.9925(3) 0.66038(17) 0.0395(8) Uani 1 1 d . . .
H5 H 0.2198 1.0640 0.6674 0.047 Uiso 1 1 calc R A .
C6 C 0.19469(11) 0.8317(3) 0.67664(17) 0.0410(8) Uani 1 1 d . . .
H6 H 0.1749 0.7880 0.6949 0.049 Uiso 1 1 calc R A .
C7 C 0.22471(12) 0.7893(3) 0.63889(18) 0.0497(10) Uani 1 1 d . . .
H7 H 0.2257 0.7175 0.6332 0.060 Uiso 1 1 calc R . .
C8 C 0.3706(3) 0.8012(5) 0.4806(3) 0.0390(17) Uani 0.50 1 d P . .
H8A H 0.3652 0.8739 0.4738 0.047 Uiso 0.50 1 d PR . .
H8B H 0.3809 0.7725 0.4411 0.047 Uiso 0.50 1 d PR . .
C9 C 0.43905(15) 0.8125(4) 0.5000 0.0468(13) Uani 1 2 d S . .
C10 C 0.45889(12) 0.8295(3) 0.5516(2) 0.0537(11) Uani 1 1 d . . .
H10 H 0.4447 0.8277 0.5905 0.064 Uiso 1 1 calc R . .
C11 C 0.50058(12) 0.8504(3) 0.5513(2) 0.0486(9) Uani 1 1 d . . .
H11 H 0.5136 0.8635 0.5904 0.058 Uiso 1 1 calc R . .
C12 C 0.62249(11) 0.9428(3) 0.61655(17) 0.0391(8) Uani 1 1 d . . .
C13 C 0.61776(12) 0.9944(3) 0.67963(17) 0.0393(8) Uani 1 1 d . . .
H13 H 0.6170 1.0698 0.6725 0.047 Uiso 1 1 calc R . .
C14 C 0.65382(12) 0.9708(3) 0.71760(18) 0.0498(10) Uani 1 1 d . . .
H14A H 0.6786 0.9896 0.6937 0.060 Uiso 1 1 calc R . .
H14B H 0.6548 0.8965 0.7256 0.060 Uiso 1 1 calc R . .
C15 C 0.58172(13) 0.9663(3) 0.71538(18) 0.0483(10) Uani 1 1 d . . .
H15A H 0.5820 0.8922 0.7243 0.058 Uiso 1 1 calc R . .
H15B H 0.5568 0.9823 0.6909 0.058 Uiso 1 1 calc R . .
C16 C 0.3358(2) 0.6361(5) 0.4751(3) 0.0365(15) Uani 0.50 1 d P . .
H16A H 0.3528 0.6363 0.4372 0.044 Uiso 0.50 1 d PR . .
H16B H 0.3096 0.6040 0.4652 0.044 Uiso 0.50 1 d PR . .
C17 C 0.36729(16) 0.4808(4) 0.5000 0.0430(12) Uani 1 2 d S . .
C18 C 0.37544(13) 0.4298(3) 0.44597(19) 0.0488(10) Uani 1 1 d . . .
H18 H 0.3724 0.4636 0.4068 0.059 Uiso 1 1 calc R . .
C19 C 0.38840(12) 0.3272(3) 0.44718(18) 0.0467(9) Uani 1 1 d . . .
H19 H 0.3940 0.2939 0.4085 0.056 Uiso 1 1 calc R . .
N1 N 0.39295(13) 0.2761(3) 0.5000 0.0407(10) Uani 1 2 d S . .
N2 N 0.19260(8) 0.9334(2) 0.68850(14) 0.0371(7) Uani 1 1 d . . .
N3 N 0.52288(12) 0.8531(3) 0.5000 0.0362(9) Uani 1 2 d S . .
N4 N 0.09214(10) 1.1822(3) 0.74313(17) 0.0503(8) Uani 1 1 d . . .
O2 O 0.40059(14) 0.7902(4) 0.5267(2) 0.0386(11) Uani 0.50 1 d P . .
O3 O 0.35520(15) 0.5782(4) 0.5214(2) 0.0406(12) Uani 0.50 1 d P . .
O4 O 0.59326(8) 0.94444(19) 0.58011(12) 0.0453(6) Uani 1 1 d . . .
O5 O 0.65630(8) 0.9079(2) 0.59847(13) 0.0498(7) Uani 1 1 d . . .
O6 O 0.11346(9) 1.1157(2) 0.71415(15) 0.0547(7) Uani 1 1 d . . .
O7 O 0.07479(9) 1.2534(2) 0.71236(14) 0.0549(7) Uani 1 1 d . . .
O8 O 0.08855(8) 1.1797(2) 0.80269(15) 0.0553(7) Uani 1 1 d . . .
Zn1 Zn 0.586034(16) 0.87332(4) 0.5000 0.03353(18) Uani 1 2 d S . .
Zn2 Zn 0.150549(18) 1.0000 0.7500 0.03909(19) Uani 1 2 d S . .
C2A C 0.3110(3) 0.8053(8) 0.5597(4) 0.0394(18) Uani 0.50 1 d P A 1
H2AA H 0.3317 0.8041 0.5937 0.047 Uiso 0.50 1 calc PR A 1
H2AB H 0.3068 0.8774 0.5476 0.047 Uiso 0.50 1 calc PR A 1
O1A O 0.27416(16) 0.7674(4) 0.5841(2) 0.0403(11) Uani 0.50 1 d P A 1
C2B C 0.2968(3) 0.7522(8) 0.5525(5) 0.044(2) Uani 0.50 1 d P . 2
H2BA H 0.2709 0.7229 0.5368 0.053 Uiso 0.50 1 calc PR . 2
H2BB H 0.3059 0.7107 0.5888 0.053 Uiso 0.50 1 calc PR . 2
O1B O 0.28954(16) 0.8535(4) 0.5732(3) 0.0425(12) Uani 0.50 1 d P . 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
C1 C16 1.511(8) . ?
C1 C16 1.511(8) 10_556 ?
C1 C2B 1.514(10) . ?
C1 C2B 1.514(10) 10_556 ?
C1 C8 1.562(9) 10_556 ?
C1 C8 1.562(9) . ?
C1 C2A 1.576(9) . ?
C1 C2A 1.576(9) 10_556 ?
C3 C4 1.348(5) . ?
C3 C7 1.366(6) . ?
C3 O1A 1.366(6) . ?
C3 O1B 1.380(7) . ?
C4 C5 1.355(5) . ?
C4 H4 0.9300 . ?
C5 N2 1.316(5) . ?
C5 H5 0.9300 . ?
C6 N2 1.332(5) . ?
C6 C7 1.358(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C8 0.808(12) 10_556 ?
C8 O2 0.985(8) 10_556 ?
C8 O2 1.367(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C9 C10 1.269(5) 10_556 ?
C9 C10 1.269(5) . ?
C9 O2 1.385(6) . ?
C9 O2 1.385(6) 10_556 ?
C10 C11 1.366(5) . ?
C10 H10 0.9300 . ?
C11 N3 1.287(5) . ?
C11 H11 0.9300 . ?
C12 O4 1.208(4) . ?
C12 O5 1.234(4) . ?
C12 C13 1.479(5) . ?
C13 C15 1.423(5) . ?
C13 C14 1.435(5) . ?
C13 H13 0.9800 . ?
C14 C14 1.543(8) 8_466 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C15 1.682(7) 8_466 ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O3 0.974(7) 10_556 ?
C16 C16 1.036(14) 10_556 ?
C16 O3 1.368(8) . ?
C16 C2B 2.031(11) 10_556 ?
C16 H16A 0.9599 . ?
C16 H16B 0.9600 . ?
C17 C18 1.328(5) . ?
C17 C18 1.328(5) 10_556 ?
C17 O3 1.383(6) . ?
C17 O3 1.383(6) 10_556 ?
C18 C19 1.382(5) . ?
C18 H18 0.9300 . ?
C19 N1 1.289(4) . ?
C19 H19 0.9300 . ?
N1 C19 1.289(4) 10_556 ?
N1 Zn1 2.035(4) 9_666 ?
N2 Zn2 2.048(3) . ?
N3 C11 1.287(5) 10_556 ?
N3 Zn1 2.045(4) . ?
N4 O8 1.246(4) . ?
N4 O7 1.248(4) . ?
N4 O6 1.250(4) . ?
O2 C8 0.985(8) 10_556 ?
O2 O2 1.113(9) 10_556 ?
O3 O3 0.891(9) 10_556 ?
O3 C16 0.974(7) 10_556 ?
O4 Zn1 1.916(2) . ?
O6 Zn2 2.046(3) . ?
Zn1 O4 1.916(2) 10_556 ?
Zn1 N1 2.035(4) 9_666 ?
Zn2 O6 2.046(3) 8_466 ?
Zn2 N2 2.048(3) 8_466 ?
C2A O1A 1.378(10) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2B O1B 1.389(10) . ?
C2B C16 2.031(11) 10_556 ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?

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
C16 C1 C16 40.1(5) . 10_556 ?
C16 C1 C2B 113.4(6) . . ?
C16 C1 C2B 84.4(5) 10_556 . ?
C16 C1 C2B 84.4(5) . 10_556 ?
C16 C1 C2B 113.4(6) 10_556 10_556 ?
C2B C1 C2B 92.5(8) . 10_556 ?
C16 C1 C8 113.4(5) . 10_556 ?
C16 C1 C8 102.7(4) 10_556 10_556 ?
C2B C1 C8 111.8(5) . 10_556 ?
C2B C1 C8 138.2(6) 10_556 10_556 ?
C16 C1 C8 102.7(4) . . ?
C16 C1 C8 113.4(5) 10_556 . ?
C2B C1 C8 138.2(6) . . ?
C2B C1 C8 111.8(5) 10_556 . ?
C8 C1 C8 30.0(5) 10_556 . ?
C16 C1 C2A 140.9(5) . . ?
C16 C1 C2A 103.6(4) 10_556 . ?
C2B C1 C2A 31.3(4) . . ?
C2B C1 C2A 106.6(5) 10_556 . ?
C8 C1 C2A 83.5(5) 10_556 . ?
C8 C1 C2A 107.2(5) . . ?
C16 C1 C2A 103.6(4) . 10_556 ?
C16 C1 C2A 140.9(5) 10_556 10_556 ?
C2B C1 C2A 106.6(5) . 10_556 ?
C2B C1 C2A 31.3(4) 10_556 10_556 ?
C8 C1 C2A 107.2(5) 10_556 10_556 ?
C8 C1 C2A 83.5(5) . 10_556 ?
C2A C1 C2A 104.3(6) . 10_556 ?
C4 C3 C7 115.9(3) . . ?
C4 C3 O1A 151.0(4) . . ?
C7 C3 O1A 92.6(4) . . ?
C4 C3 O1B 97.8(4) . . ?
C7 C3 O1B 145.9(4) . . ?
O1A C3 O1B 53.3(3) . . ?
C3 C4 C5 121.4(4) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
N2 C5 C4 122.8(3) . . ?
N2 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
N2 C6 C7 122.5(3) . . ?
N2 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C6 C7 C3 120.7(4) . . ?
C6 C7 H7 119.7 . . ?
C3 C7 H7 119.7 . . ?
C8 C8 O2 98.9(4) 10_556 10_556 ?
C8 C8 O2 45.4(3) 10_556 . ?
O2 C8 O2 53.5(5) 10_556 . ?
C8 C8 C1 75.0(2) 10_556 . ?
O2 C8 C1 143.6(7) 10_556 . ?
O2 C8 C1 111.7(4) . . ?
C8 C8 H8A 98.4 10_556 . ?
O2 C8 H8A 107.1 10_556 . ?
O2 C8 H8A 109.4 . . ?
C1 C8 H8A 109.3 . . ?
C8 C8 H8B 149.0 10_556 . ?
O2 C8 H8B 58.5 10_556 . ?
O2 C8 H8B 108.7 . . ?
C1 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C10 115.8(5) 10_556 . ?
C10 C9 O2 145.5(4) 10_556 . ?
C10 C9 O2 98.2(3) . . ?
C10 C9 O2 98.2(3) 10_556 10_556 ?
C10 C9 O2 145.5(4) . 10_556 ?
O2 C9 O2 47.4(4) . 10_556 ?
C9 C10 C11 121.5(4) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
N3 C11 C10 123.7(4) . . ?
N3 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
O4 C12 O5 119.9(3) . . ?
O4 C12 C13 118.1(3) . . ?
O5 C12 C13 121.6(3) . . ?
C15 C13 C14 108.3(3) . . ?
C15 C13 C12 115.7(3) . . ?
C14 C13 C12 108.2(3) . . ?
C15 C13 H13 108.1 . . ?
C14 C13 H13 108.1 . . ?
C12 C13 H13 108.1 . . ?
C13 C14 C14 112.3(3) . 8_466 ?
C13 C14 H14A 109.1 . . ?
C14 C14 H14A 109.1 8_466 . ?
C13 C14 H14B 109.1 . . ?
C14 C14 H14B 109.1 8_466 . ?
H14A C14 H14B 107.9 . . ?
C13 C15 C15 108.5(3) . 8_466 ?
C13 C15 H15A 110.0 . . ?
C15 C15 H15A 110.0 8_466 . ?
C13 C15 H15B 110.0 . . ?
C15 C15 H15B 110.0 8_466 . ?
H15A C15 H15B 108.4 . . ?
O3 C16 C16 85.7(5) 10_556 10_556 ?
O3 C16 O3 40.5(5) 10_556 . ?
C16 C16 O3 45.2(3) 10_556 . ?
O3 C16 C1 140.6(8) 10_556 . ?
C16 C16 C1 70.0(3) 10_556 . ?
O3 C16 C1 109.1(5) . . ?
O3 C16 C2B 167.8(7) 10_556 10_556 ?
C16 C16 C2B 106.5(3) 10_556 10_556 ?
O3 C16 C2B 151.7(6) . 10_556 ?
C1 C16 C2B 47.9(4) . 10_556 ?
O3 C16 H16A 72.5 10_556 . ?
C16 C16 H16A 145.3 10_556 . ?
O3 C16 H16A 108.7 . . ?
C1 C16 H16A 111.0 . . ?
C2B C16 H16A 96.6 10_556 . ?
O3 C16 H16B 104.5 10_556 . ?
C16 C16 H16B 102.4 10_556 . ?
O3 C16 H16B 108.5 . . ?
C1 C16 H16B 110.6 . . ?
C2B C16 H16B 73.4 10_556 . ?
H16A C16 H16B 108.9 . . ?
C18 C17 C18 115.8(4) . 10_556 ?
C18 C17 O3 140.8(3) . . ?
C18 C17 O3 103.2(3) 10_556 . ?
C18 C17 O3 103.2(3) . 10_556 ?
C18 C17 O3 140.8(3) 10_556 10_556 ?
O3 C17 O3 37.6(4) . 10_556 ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
N1 C19 C18 122.4(4) . . ?
N1 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C19 N1 C19 117.1(4) . 10_556 ?
C19 N1 Zn1 121.2(2) . 9_666 ?
C19 N1 Zn1 121.2(2) 10_556 9_666 ?
C5 N2 C6 116.7(3) . . ?
C5 N2 Zn2 119.3(2) . . ?
C6 N2 Zn2 124.0(2) . . ?
C11 N3 C11 112.3(5) . 10_556 ?
C11 N3 Zn1 123.7(2) . . ?
C11 N3 Zn1 123.7(2) 10_556 . ?
O8 N4 O7 119.2(3) . . ?
O8 N4 O6 120.9(3) . . ?
O7 N4 O6 119.8(3) . . ?
C8 O2 O2 81.1(4) 10_556 10_556 ?
C8 O2 C8 35.7(6) 10_556 . ?
O2 O2 C8 45.4(3) 10_556 . ?
C8 O2 C9 141.3(6) 10_556 . ?
O2 O2 C9 66.3(2) 10_556 . ?
C8 O2 C9 108.9(4) . . ?
O3 O3 C16 94.3(5) 10_556 10_556 ?
O3 O3 C16 45.2(3) 10_556 . ?
C16 O3 C16 49.1(7) 10_556 . ?
O3 O3 C17 71.21(19) 10_556 . ?
C16 O3 C17 153.5(7) 10_556 . ?
C16 O3 C17 113.1(4) . . ?
C12 O4 Zn1 129.3(2) . . ?
N4 O6 Zn2 129.7(3) . . ?
O4 Zn1 O4 121.06(16) . 10_556 ?
O4 Zn1 N1 114.19(8) . 9_666 ?
O4 Zn1 N1 114.19(8) 10_556 9_666 ?
O4 Zn1 N3 100.41(10) . . ?
O4 Zn1 N3 100.41(10) 10_556 . ?
N1 Zn1 N3 102.08(16) 9_666 . ?
O6 Zn2 O6 108.79(17) . 8_466 ?
O6 Zn2 N2 107.96(12) . 8_466 ?
O6 Zn2 N2 117.34(12) 8_466 8_466 ?
O6 Zn2 N2 117.34(12) . . ?
O6 Zn2 N2 107.96(12) 8_466 . ?
N2 Zn2 N2 97.51(16) 8_466 . ?
O1A C2A C1 116.0(9) . . ?
O1A C2A H2AA 108.3 . . ?
C1 C2A H2AA 108.3 . . ?
O1A C2A H2AB 108.3 . . ?
C1 C2A H2AB 108.3 . . ?
H2AA C2A H2AB 107.4 . . ?
C3 O1A C2A 106.3(6) . . ?
O1B C2B C1 113.2(8) . . ?
O1B C2B C16 151.5(9) . 10_556 ?
C1 C2B C16 47.8(4) . 10_556 ?
O1B C2B H2BA 108.9 . . ?
C1 C2B H2BA 108.9 . . ?
C16 C2B H2BA 98.4 10_556 . ?
O1B C2B H2BB 108.9 . . ?
C1 C2B H2BB 108.9 . . ?
C16 C2B H2BB 68.4 10_556 . ?
H2BA C2B H2BB 107.8 . . ?
C3 O1B C2B 106.7(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C3 C4 C5 -1.4(6) . . . . ?
O1A C3 C4 C5 -170.3(7) . . . . ?
O1B C3 C4 C5 -175.9(4) . . . . ?
C3 C4 C5 N2 0.7(6) . . . . ?
N2 C6 C7 C3 -2.5(6) . . . . ?
C4 C3 C7 C6 2.3(6) . . . . ?
O1A C3 C7 C6 176.9(4) . . . . ?
O1B C3 C7 C6 172.6(6) . . . . ?
C16 C1 C8 C8 -115.1(3) . . . 10_556 ?
C16 C1 C8 C8 -74.3(3) 10_556 . . 10_556 ?
C2B C1 C8 C8 34.6(6) . . . 10_556 ?
C2B C1 C8 C8 155.9(5) 10_556 . . 10_556 ?
C2A C1 C8 C8 39.4(3) . . . 10_556 ?
C2A C1 C8 C8 142.4(3) 10_556 . . 10_556 ?
C16 C1 C8 O2 -30.5(11) . . . 10_556 ?
C16 C1 C8 O2 10.4(12) 10_556 . . 10_556 ?
C2B C1 C8 O2 119.3(11) . . . 10_556 ?
C2B C1 C8 O2 -119.4(11) 10_556 . . 10_556 ?
C8 C1 C8 O2 84.7(11) 10_556 . . 10_556 ?
C2A C1 C8 O2 124.1(11) . . . 10_556 ?
C2A C1 C8 O2 -133.0(11) 10_556 . . 10_556 ?
C16 C1 C8 O2 -87.9(5) . . . . ?
C16 C1 C8 O2 -47.0(6) 10_556 . . . ?
C2B C1 C8 O2 61.9(9) . . . . ?
C2B C1 C8 O2 -176.8(5) 10_556 . . . ?
C8 C1 C8 O2 27.3(5) 10_556 . . . ?
C2A C1 C8 O2 66.7(6) . . . . ?
C2A C1 C8 O2 169.6(6) 10_556 . . . ?
C10 C9 C10 C11 -8.9(9) 10_556 . . . ?
O2 C9 C10 C11 176.5(4) . . . . ?
O2 C9 C10 C11 -179.3(7) 10_556 . . . ?
C9 C10 C11 N3 -1.0(7) . . . . ?
O4 C12 C13 C15 50.7(5) . . . . ?
O5 C12 C13 C15 -136.4(4) . . . . ?
O4 C12 C13 C14 172.4(4) . . . . ?
O5 C12 C13 C14 -14.7(5) . . . . ?
C15 C13 C14 C14 -58.9(5) . . . 8_466 ?
C12 C13 C14 C14 174.9(4) . . . 8_466 ?
C14 C13 C15 C15 59.0(5) . . . 8_466 ?
C12 C13 C15 C15 -179.4(3) . . . 8_466 ?
C16 C1 C16 O3 -55.3(11) 10_556 . . 10_556 ?
C2B C1 C16 O3 -102.4(11) . . . 10_556 ?
C2B C1 C16 O3 167.3(11) 10_556 . . 10_556 ?
C8 C1 C16 O3 26.6(12) 10_556 . . 10_556 ?
C8 C1 C16 O3 56.1(11) . . . 10_556 ?
C2A C1 C16 O3 -83.2(14) . . . 10_556 ?
C2A C1 C16 O3 142.5(11) 10_556 . . 10_556 ?
C2B C1 C16 C16 -47.1(4) . . . 10_556 ?
C2B C1 C16 C16 -137.5(5) 10_556 . . 10_556 ?
C8 C1 C16 C16 81.8(3) 10_556 . . 10_556 ?
C8 C1 C16 C16 111.4(3) . . . 10_556 ?
C2A C1 C16 C16 -28.0(7) . . . 10_556 ?
C2A C1 C16 C16 -162.3(5) 10_556 . . 10_556 ?
C16 C1 C16 O3 -23.1(5) 10_556 . . . ?
C2B C1 C16 O3 -70.3(7) . . . . ?
C2B C1 C16 O3 -160.6(6) 10_556 . . . ?
C8 C1 C16 O3 58.7(6) 10_556 . . . ?
C8 C1 C16 O3 88.3(5) . . . . ?
C2A C1 C16 O3 -51.1(10) . . . . ?
C2A C1 C16 O3 174.6(6) 10_556 . . . ?
C16 C1 C16 C2B 137.5(5) 10_556 . . 10_556 ?
C2B C1 C16 C2B 90.3(8) . . . 10_556 ?
C8 C1 C16 C2B -140.7(5) 10_556 . . 10_556 ?
C8 C1 C16 C2B -111.1(5) . . . 10_556 ?
C2A C1 C16 C2B 109.5(10) . . . 10_556 ?
C2A C1 C16 C2B -24.8(5) 10_556 . . 10_556 ?
C18 C17 C18 C19 5.0(8) 10_556 . . . ?
O3 C17 C18 C19 178.2(6) . . . . ?
O3 C17 C18 C19 -179.5(4) 10_556 . . . ?
C17 C18 C19 N1 0.5(7) . . . . ?
C18 C19 N1 C19 -5.9(8) . . . 10_556 ?
C18 C19 N1 Zn1 -177.9(3) . . . 9_666 ?
C4 C5 N2 C6 -0.7(5) . . . . ?
C4 C5 N2 Zn2 176.6(3) . . . . ?
C7 C6 N2 C5 1.7(5) . . . . ?
C7 C6 N2 Zn2 -175.5(3) . . . . ?
C10 C11 N3 C11 10.4(7) . . . 10_556 ?
C10 C11 N3 Zn1 -175.1(3) . . . . ?
O2 C8 O2 C8 180.000(2) 10_556 . . 10_556 ?
C1 C8 O2 C8 -38.4(7) . . . 10_556 ?
C8 C8 O2 O2 180.000(3) 10_556 . . 10_556 ?
C1 C8 O2 O2 141.6(7) . . . 10_556 ?
C8 C8 O2 C9 -159.3(7) 10_556 . . . ?
O2 C8 O2 C9 20.7(7) 10_556 . . . ?
C1 C8 O2 C9 162.2(5) . . . . ?
C10 C9 O2 C8 -29.6(16) 10_556 . . 10_556 ?
C10 C9 O2 C8 141.7(10) . . . 10_556 ?
O2 C9 O2 C8 -35.2(11) 10_556 . . 10_556 ?
C10 C9 O2 O2 5.5(8) 10_556 . . 10_556 ?
C10 C9 O2 O2 176.8(5) . . . 10_556 ?
C10 C9 O2 C8 -10.4(11) 10_556 . . . ?
C10 C9 O2 C8 160.9(5) . . . . ?
O2 C9 O2 C8 -15.9(5) 10_556 . . . ?
C16 C16 O3 O3 180.000(4) 10_556 . . 10_556 ?
C1 C16 O3 O3 -148.7(7) . . . 10_556 ?
C2B C16 O3 O3 180(100) 10_556 . . 10_556 ?
O3 C16 O3 C16 180.000(3) 10_556 . . 10_556 ?
C1 C16 O3 C16 31.3(7) . . . 10_556 ?
C2B C16 O3 C16 -0.1(16) 10_556 . . 10_556 ?
O3 C16 O3 C17 -23.4(7) 10_556 . . . ?
C16 C16 O3 C17 156.6(7) 10_556 . . . ?
C1 C16 O3 C17 -172.1(4) . . . . ?
C2B C16 O3 C17 156.5(12) 10_556 . . . ?
C18 C17 O3 O3 3.8(6) . . . 10_556 ?
C18 C17 O3 O3 177.5(4) 10_556 . . 10_556 ?
C18 C17 O3 C16 63.4(17) . . . 10_556 ?
C18 C17 O3 C16 -122.9(14) 10_556 . . 10_556 ?
O3 C17 O3 C16 59.6(14) 10_556 . . 10_556 ?
C18 C17 O3 C16 21.2(10) . . . . ?
C18 C17 O3 C16 -165.1(5) 10_556 . . . ?
O3 C17 O3 C16 17.3(5) 10_556 . . . ?
O5 C12 O4 Zn1 14.9(5) . . . . ?
C13 C12 O4 Zn1 -172.1(2) . . . . ?
O8 N4 O6 Zn2 -5.9(6) . . . . ?
O7 N4 O6 Zn2 172.7(3) . . . . ?
C12 O4 Zn1 O4 -101.7(3) . . . 10_556 ?
C12 O4 Zn1 N1 40.9(4) . . . 9_666 ?
C12 O4 Zn1 N3 149.3(3) . . . . ?
C11 N3 Zn1 O4 -24.7(4) . . . . ?
C11 N3 Zn1 O4 149.2(3) 10_556 . . . ?
C11 N3 Zn1 O4 -149.2(3) . . . 10_556 ?
C11 N3 Zn1 O4 24.7(4) 10_556 . . 10_556 ?
C11 N3 Zn1 N1 93.0(4) . . . 9_666 ?
C11 N3 Zn1 N1 -93.0(4) 10_556 . . 9_666 ?
N4 O6 Zn2 O6 73.7(3) . . . 8_466 ?
N4 O6 Zn2 N2 -54.7(4) . . . 8_466 ?
N4 O6 Zn2 N2 -163.4(3) . . . . ?
C5 N2 Zn2 O6 58.3(3) . . . . ?
C6 N2 Zn2 O6 -124.6(3) . . . . ?
C5 N2 Zn2 O6 -178.4(3) . . . 8_466 ?
C6 N2 Zn2 O6 -1.3(3) . . . 8_466 ?
C5 N2 Zn2 N2 -56.5(2) . . . 8_466 ?
C6 N2 Zn2 N2 120.7(3) . . . 8_466 ?
C16 C1 C2A O1A -41.8(11) . . . . ?
C16 C1 C2A O1A -59.9(7) 10_556 . . . ?
C2B C1 C2A O1A -6.2(7) . . . . ?
C2B C1 C2A O1A 60.0(9) 10_556 . . . ?
C8 C1 C2A O1A -161.4(6) 10_556 . . . ?
C8 C1 C2A O1A 179.9(6) . . . . ?
C2A C1 C2A O1A 92.4(8) 10_556 . . . ?
C4 C3 O1A C2A 1.0(11) . . . . ?
C7 C3 O1A C2A -169.0(5) . . . . ?
O1B C3 O1A C2A 8.0(5) . . . . ?
C1 C2A O1A C3 -149.4(5) . . . . ?
C16 C1 C2B O1B -177.2(6) . . . . ?
C16 C1 C2B O1B 154.5(7) 10_556 . . . ?
C2B C1 C2B O1B -92.2(9) 10_556 . . . ?
C8 C1 C2B O1B 53.0(8) 10_556 . . . ?
C8 C1 C2B O1B 35.2(10) . . . . ?
C2A C1 C2B O1B 26.4(7) . . . . ?
C2A C1 C2B O1B -63.9(10) 10_556 . . . ?
C16 C1 C2B C16 28.3(4) . . . 10_556 ?
C2B C1 C2B C16 113.3(5) 10_556 . . 10_556 ?
C8 C1 C2B C16 -101.5(5) 10_556 . . 10_556 ?
C8 C1 C2B C16 -119.3(7) . . . 10_556 ?
C2A C1 C2B C16 -128.1(9) . . . 10_556 ?
C2A C1 C2B C16 141.6(6) 10_556 . . 10_556 ?
C4 C3 O1B C2B -177.3(5) . . . . ?
C7 C3 O1B C2B 11.5(9) . . . . ?
O1A C3 O1B C2B 6.1(5) . . . . ?
C1 C2B O1B C3 166.5(5) . . . . ?
C16 C2B O1B C3 -151.6(13) 10_556 . . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.004 651 50 ' '
2 0.295 0.187 0.500 25 4 ' '
3 0.705 0.187 0.000 25 4 ' '
4 0.500 0.500 0.235 651 50 ' '
5 0.197 0.252 0.000 16 3 ' '
6 0.795 0.313 0.500 25 4 ' '
7 0.219 0.429 0.000 9 1 ' '
8 0.205 0.687 0.500 25 4 ' '
9 0.795 0.687 0.000 25 4 ' '
10 0.295 0.813 0.000 25 4 ' '
11 0.697 0.752 0.500 16 3 ' '
12 0.719 0.929 0.500 9 1 ' '

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.123
_database_code_depnum_ccdc_archive 'CCDC 973270'

data_cao

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H32 N4 Ni O12'
_chemical_formula_sum            'C29 H32 N4 Ni O12'
_chemical_formula_weight         687.30

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'
Ni Ni 0.3393 1.1124 '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'

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                   17.334(2)
_cell_length_b                   9.2474(10)
_cell_length_c                   20.562(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.815(4)
_cell_angle_gamma                90.00
_cell_volume                     3119.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7553
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2738
_reflns_number_gt                2482
_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)+(0.0743P)²+2.0244P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constra
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2738
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2500 1.2500 0.5000 0.02027(17) Uani 1 2 d S . .
O3 O 0.22124(10) 1.38359(17) 0.41292(8) 0.0288(4) Uani 1 1 d . . .
O1 O 0.36015(10) 1.20160(19) 0.48606(9) 0.0306(4) Uani 1 1 d . . .
O2 O 0.37654(11) 0.9835(2) 0.53489(10) 0.0420(5) Uani 1 1 d . . .
N1 N 0.19493(12) 1.0780(2) 0.43412(10) 0.0273(4) Uani 1 1 d . . .
O5 O 0.02954(11) 0.35744(19) 0.18614(9) 0.0404(5) Uani 1 1 d . . .
C8 C 0.06726(14) 0.4602(2) 0.23894(13) 0.0311(5) Uani 1 1 d . . .
H8A H 0.1053 0.5200 0.2252 0.037 Uiso 1 1 calc R . .
H8B H 0.0969 0.4105 0.2812 0.037 Uiso 1 1 calc R . .
C13 C 0.39741(14) 1.0831(3) 0.50311(12) 0.0285(5) Uani 1 1 d . . .
C7 C 0.0000 0.5538(3) 0.2500 0.0268(7) Uani 1 2 d S . .
C5 C 0.12471(15) 0.8510(2) 0.34555(12) 0.0300(5) Uani 1 1 d . . .
C10 C 0.16171(19) 0.2568(3) 0.19616(17) 0.0427(7) Uani 1 1 d . . .
H10 H 0.1901 0.3272 0.2269 0.051 Uiso 1 1 calc R . .
O4 O 0.09228(13) 0.74585(16) 0.29870(10) 0.0370(5) Uani 1 1 d . . .
C6 C 0.03667(15) 0.6473(2) 0.31360(12) 0.0290(5) Uani 1 1 d . . .
H6A H -0.0059 0.7000 0.3245 0.035 Uiso 1 1 calc R . .
H6B H 0.0651 0.5872 0.3527 0.035 Uiso 1 1 calc R . .
C9 C 0.07754(17) 0.2579(2) 0.17089(15) 0.0334(6) Uani 1 1 d . . .
C1 C 0.15996(16) 0.9654(3) 0.45384(12) 0.0352(6) Uani 1 1 d . . .
H1 H 0.1594 0.9645 0.4989 0.042 Uiso 1 1 calc R . .
N2 N 0.16648(16) 0.0432(3) 0.13199(14) 0.0517(6) Uani 1 1 d . . .
C2 C 0.12443(16) 0.8497(3) 0.41246(13) 0.0350(6) Uani 1 1 d . . .
H2 H 0.1012 0.7736 0.4292 0.042 Uiso 1 1 calc R . .
C14 C 0.47314(16) 1.0617(3) 0.48242(15) 0.0410(7) Uani 1 1 d . . .
H14A H 0.4564 1.0459 0.4332 0.049 Uiso 1 1 calc R . .
H14B H 0.5050 1.1501 0.4922 0.049 Uiso 1 1 calc R . .
C11 C 0.20242(18) 0.1491(3) 0.17466(17) 0.0495(7) Uani 1 1 d . . .
H11 H 0.2591 0.1504 0.1911 0.059 Uiso 1 1 calc R . .
C4 C 0.16095(19) 0.9658(3) 0.32368(13) 0.0445(7) Uani 1 1 d . . .
H4 H 0.1623 0.9691 0.2788 0.053 Uiso 1 1 calc R . .
C15 C 0.0855(2) 0.0453(4) 0.10896(18) 0.0575(9) Uani 1 1 d . . .
H15 H 0.0587 -0.0283 0.0794 0.069 Uiso 1 1 calc R . .
C3 C 0.19482(18) 1.0742(3) 0.36886(14) 0.0409(6) Uani 1 1 d . . .
H3 H 0.2194 1.1504 0.3534 0.049 Uiso 1 1 calc R . .
C12 C 0.03878(18) 0.1492(3) 0.12606(17) 0.0515(8) Uani 1 1 d . . .
H12 H -0.0178 0.1465 0.1079 0.062 Uiso 1 1 calc R . .
O6 O 0.3484(18) 0.252(3) 0.3406(19) 0.86(3) Uani 1 1 d . . .
H6F H 0.3498 0.3396 0.3541 1.031 Uiso 1 1 d R . .
H6D H 0.3406 0.1966 0.3708 1.289 Uiso 1 1 d 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
Ni1 O1 2.0690(16) . ?
Ni1 O1 2.0690(16) 7_576 ?
Ni1 O3 2.0988(15) . ?
Ni1 O3 2.0988(15) 7_576 ?
Ni1 N1 2.1075(19) 7_576 ?
Ni1 N1 2.1075(19) . ?
O1 C13 1.263(3) . ?
O2 C13 1.249(3) . ?
N1 C1 1.332(3) . ?
N1 C3 1.342(3) . ?
O5 C9 1.344(3) . ?
O5 C8 1.432(3) . ?
C8 C7 1.527(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 C14 1.518(3) . ?
C7 C6 1.525(3) . ?
C7 C6 1.525(3) 2 ?
C7 C8 1.527(3) 2 ?
C5 O4 1.357(3) . ?
C5 C2 1.378(3) . ?
C5 C4 1.380(4) . ?
C10 C11 1.374(4) . ?
C10 C9 1.382(4) . ?
C10 H10 0.9300 . ?
O4 C6 1.430(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C12 1.383(4) . ?
C1 C2 1.382(3) . ?
C1 H1 0.9300 . ?
N2 C11 1.328(4) . ?
N2 C15 1.330(4) . ?
C2 H2 0.9300 . ?
C14 C14 1.503(5) 5_676 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11 0.9300 . ?
C4 C3 1.365(4) . ?
C4 H4 0.9300 . ?
C15 C12 1.373(4) . ?
C15 H15 0.9300 . ?
C3 H3 0.9300 . ?
C12 H12 0.9300 . ?
O6 H6F 0.8500 . ?
O6 H6D 0.8500 . ?

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 Ni1 O1 180.0 . 7_576 ?
O1 Ni1 O3 89.15(6) . . ?
O1 Ni1 O3 90.86(6) 7_576 . ?
O1 Ni1 O3 90.85(6) . 7_576 ?
O1 Ni1 O3 89.14(6) 7_576 7_576 ?
O3 Ni1 O3 180.00(7) . 7_576 ?
O1 Ni1 N1 90.31(7) . 7_576 ?
O1 Ni1 N1 89.69(7) 7_576 7_576 ?
O3 Ni1 N1 92.17(7) . 7_576 ?
O3 Ni1 N1 87.83(7) 7_576 7_576 ?
O1 Ni1 N1 89.69(7) . . ?
O1 Ni1 N1 90.31(7) 7_576 . ?
O3 Ni1 N1 87.83(7) . . ?
O3 Ni1 N1 92.17(7) 7_576 . ?
N1 Ni1 N1 180.0 7_576 . ?
C13 O1 Ni1 124.17(15) . . ?
C1 N1 C3 115.5(2) . . ?
C1 N1 Ni1 123.41(16) . . ?
C3 N1 Ni1 121.11(16) . . ?
C9 O5 C8 117.76(19) . . ?
O5 C8 C7 107.77(17) . . ?
O5 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
O5 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
O2 C13 O1 125.2(2) . . ?
O2 C13 C14 118.3(2) . . ?
O1 C13 C14 116.5(2) . . ?
C6 C7 C6 110.9(3) . 2 ?
C6 C7 C8 108.78(13) . . ?
C6 C7 C8 108.71(13) 2 . ?
C6 C7 C8 108.71(13) . 2 ?
C6 C7 C8 108.78(13) 2 2 ?
C8 C7 C8 110.9(3) . 2 ?
O4 C5 C2 124.6(2) . . ?
O4 C5 C4 116.6(2) . . ?
C2 C5 C4 118.7(2) . . ?
C11 C10 C9 118.3(3) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
C5 O4 C6 117.30(19) . . ?
O4 C6 C7 107.52(17) . . ?
O4 C6 H6A 110.2 . . ?
C7 C6 H6A 110.2 . . ?
O4 C6 H6B 110.2 . . ?
C7 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
O5 C9 C10 125.1(2) . . ?
O5 C9 C12 116.7(2) . . ?
C10 C9 C12 118.2(2) . . ?
N1 C1 C2 125.0(2) . . ?
N1 C1 H1 117.5 . . ?
C2 C1 H1 117.5 . . ?
C11 N2 C15 116.2(2) . . ?
C5 C2 C1 117.6(2) . . ?
C5 C2 H2 121.2 . . ?
C1 C2 H2 121.2 . . ?
C14 C14 C13 115.0(3) 5_676 . ?
C14 C14 H14A 108.5 5_676 . ?
C13 C14 H14A 108.5 . . ?
C14 C14 H14B 108.5 5_676 . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
N2 C11 C10 124.5(3) . . ?
N2 C11 H11 117.7 . . ?
C10 C11 H11 117.7 . . ?
C3 C4 C5 119.0(2) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N2 C15 C12 124.1(3) . . ?
N2 C15 H15 117.9 . . ?
C12 C15 H15 117.9 . . ?
N1 C3 C4 124.2(2) . . ?
N1 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
C15 C12 C9 118.7(3) . . ?
C15 C12 H12 120.7 . . ?
C9 C12 H12 120.7 . . ?
H6F O6 H6D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ni1 O1 C13 85(12) 7_576 . . . ?
O3 Ni1 O1 C13 -149.85(19) . . . . ?
O3 Ni1 O1 C13 30.15(19) 7_576 . . . ?
N1 Ni1 O1 C13 117.98(19) 7_576 . . . ?
N1 Ni1 O1 C13 -62.02(19) . . . . ?
O1 Ni1 N1 C1 119.2(2) . . . . ?
O1 Ni1 N1 C1 -60.8(2) 7_576 . . . ?
O3 Ni1 N1 C1 -151.7(2) . . . . ?
O3 Ni1 N1 C1 28.3(2) 7_576 . . . ?
N1 Ni1 N1 C1 -51(16) 7_576 . . . ?
O1 Ni1 N1 C3 -59.3(2) . . . . ?
O1 Ni1 N1 C3 120.7(2) 7_576 . . . ?
O3 Ni1 N1 C3 29.9(2) . . . . ?
O3 Ni1 N1 C3 -150.1(2) 7_576 . . . ?
N1 Ni1 N1 C3 131(16) 7_576 . . . ?
C9 O5 C8 C7 -176.2(2) . . . . ?
Ni1 O1 C13 O2 -5.4(3) . . . . ?
Ni1 O1 C13 C14 174.11(17) . . . . ?
O5 C8 C7 C6 170.82(18) . . . . ?
O5 C8 C7 C6 -68.3(2) . . . 2 ?
O5 C8 C7 C8 51.29(13) . . . 2 ?
C2 C5 O4 C6 16.7(4) . . . . ?
C4 C5 O4 C6 -164.0(2) . . . . ?
C5 O4 C6 C7 172.37(19) . . . . ?
C6 C7 C6 O4 -53.54(14) 2 . . . ?
C8 C7 C6 O4 66.0(2) . . . . ?
C8 C7 C6 O4 -173.10(18) 2 . . . ?
C8 O5 C9 C10 -8.2(4) . . . . ?
C8 O5 C9 C12 172.2(2) . . . . ?
C11 C10 C9 O5 -178.7(3) . . . . ?
C11 C10 C9 C12 0.9(4) . . . . ?
C3 N1 C1 C2 -0.4(4) . . . . ?
Ni1 N1 C1 C2 -178.9(2) . . . . ?
O4 C5 C2 C1 -179.9(2) . . . . ?
C4 C5 C2 C1 0.8(4) . . . . ?
N1 C1 C2 C5 -0.4(4) . . . . ?
O2 C13 C14 C14 -14.6(5) . . . 5_676 ?
O1 C13 C14 C14 165.8(3) . . . 5_676 ?
C15 N2 C11 C10 0.6(5) . . . . ?
C9 C10 C11 N2 -1.4(5) . . . . ?
O4 C5 C4 C3 -179.7(3) . . . . ?
C2 C5 C4 C3 -0.4(4) . . . . ?
C11 N2 C15 C12 0.7(5) . . . . ?
C1 N1 C3 C4 0.9(4) . . . . ?
Ni1 N1 C3 C4 179.4(2) . . . . ?
C5 C4 C3 N1 -0.5(5) . . . . ?
N2 C15 C12 C9 -1.1(5) . . . . ?
O5 C9 C12 C15 179.9(3) . . . . ?
C10 C9 C12 C15 0.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.086
_database_code_depnum_ccdc_archive 'CCDC 973271'

data_cao

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H60 Cd2 N4 O20'
_chemical_formula_sum            'C41 H60 Cd2 N4 O20'
_chemical_formula_weight         1153.73

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/c'
_symmetry_space_group_name_hall  ' -P 2yc '


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

_cell_length_a                   11.4622(15)
_cell_length_b                   9.4091(12)
_cell_length_c                   22.611(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.698(2)
_cell_angle_gamma                90.00
_cell_volume                     2437.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1180
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12579
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4781
_reflns_number_gt                4061
_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)+(0.0769P)²+0.7749P] 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         4781
_refine_ls_number_parameters     305
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2892(4) 1.2146(5) 0.3033(2) 0.0512(11) Uani 1 1 d . . .
H1 H 0.2929 1.2864 0.3316 0.061 Uiso 1 1 calc R . .
C2 C 0.2098(4) 1.1087(5) 0.3100(2) 0.0504(11) Uani 1 1 d . . .
H2 H 0.1614 1.1078 0.3423 0.061 Uiso 1 1 calc R . .
C3 C 0.2025(3) 1.0018(4) 0.26767(19) 0.0379(9) Uani 1 1 d . . .
C4 C 0.2758(4) 1.0075(4) 0.2209(2) 0.0469(11) Uani 1 1 d . . .
H4 H 0.2731 0.9377 0.1917 0.056 Uiso 1 1 calc R . .
C5 C 0.3531(4) 1.1186(5) 0.2180(2) 0.0491(10) Uani 1 1 d . . .
H5 H 0.4021 1.1224 0.1860 0.059 Uiso 1 1 calc R . .
C6 C 0.1017(3) 0.7984(4) 0.23053(16) 0.0337(8) Uani 1 1 d . . .
H6A H 0.1701 0.7401 0.2245 0.040 Uiso 1 1 calc R . .
H6B H 0.0816 0.8472 0.1938 0.040 Uiso 1 1 calc R . .
C7 C 0.0000 0.7070(5) 0.2500 0.0302(10) Uani 1 2 d S . .
C8 C 0.0423(3) 0.6146(4) 0.30156(17) 0.0334(8) Uani 1 1 d . . .
H8A H 0.1063 0.5546 0.2896 0.040 Uiso 1 1 calc R . .
H8B H 0.0694 0.6736 0.3343 0.040 Uiso 1 1 calc R . .
C9 C -0.0368(3) 0.4289(4) 0.3603(2) 0.0435(10) Uani 1 1 d . . .
C10 C 0.0615(4) 0.4162(5) 0.3973(2) 0.0513(11) Uani 1 1 d . . .
H10 H 0.1223 0.4814 0.3956 0.062 Uiso 1 1 calc R . .
C11 C 0.0662(4) 0.3057(5) 0.4360(2) 0.0572(12) Uani 1 1 d . . .
H11 H 0.1328 0.2977 0.4603 0.069 Uiso 1 1 calc R . .
C12 C -0.1093(4) 0.2232(6) 0.4063(3) 0.0686(16) Uani 1 1 d . . .
H12 H -0.1685 0.1559 0.4086 0.082 Uiso 1 1 calc R . .
C13 C -0.1241(4) 0.3309(6) 0.3665(3) 0.0706(17) Uani 1 1 d . . .
H13 H -0.1927 0.3379 0.3437 0.085 Uiso 1 1 calc R . .
C14 C 0.2594(3) -0.0701(4) 0.46789(19) 0.0412(9) Uani 1 1 d . . .
C15 C 0.3898(3) -0.0663(4) 0.47977(18) 0.0391(9) Uani 1 1 d . . .
H15 H 0.4222 -0.1550 0.4645 0.047 Uiso 1 1 calc R . .
C16 C 0.4438(3) 0.0555(5) 0.4460(2) 0.0454(10) Uani 1 1 d . . .
H16A H 0.4240 0.0459 0.4042 0.055 Uiso 1 1 calc R . .
H16B H 0.4121 0.1449 0.4596 0.055 Uiso 1 1 calc R . .
C17 C 0.5751(3) 0.0565(5) 0.4549(2) 0.0469(10) Uani 1 1 d . . .
H17A H 0.6073 0.1369 0.4340 0.056 Uiso 1 1 calc R . .
H17B H 0.6073 -0.0296 0.4384 0.056 Uiso 1 1 calc R . .
C18 C 0.5611(4) 1.5258(6) 0.3772(2) 0.0569(12) Uani 1 1 d . . .
Cd1 Cd 0.5000 1.39987(4) 0.2500 0.03350(14) Uani 1 2 d S . .
Cd2 Cd 0.0000 0.0000 0.5000 0.03210(14) Uani 1 2 d S . .
N1 N 0.3620(3) 1.2211(4) 0.25842(15) 0.0430(8) Uani 1 1 d . . .
N2 N -0.0168(3) 0.2080(4) 0.44199(17) 0.0485(9) Uani 1 1 d . . .
O1 O 0.2215(3) -0.1508(4) 0.42797(17) 0.0695(10) Uani 1 1 d . . .
O2 O 0.1976(2) 0.0107(3) 0.49775(14) 0.0432(7) Uani 1 1 d . . .
O3 O 0.0054(3) 0.1170(4) 0.58827(16) 0.0652(10) Uani 1 1 d . . .
H3B H 0.0637 0.1729 0.5896 0.098 Uiso 1 1 d R . .
H3C H -0.0570 0.1647 0.5916 0.098 Uiso 1 1 d R . .
O4 O 0.3491(3) 1.5621(4) 0.25762(14) 0.0576(8) Uani 1 1 d . . .
H4A H 0.3765 1.6459 0.2557 0.086 Uiso 1 1 d R . .
H4B H 0.2998 1.5491 0.2293 0.086 Uiso 1 1 d R . .
O5 O -0.0543(2) 0.5290(3) 0.31884(15) 0.0516(8) Uani 1 1 d . . .
O6 O 0.1238(3) 0.8994(3) 0.27757(13) 0.0432(7) Uani 1 1 d . . .
O7 O 0.5260(3) 1.4185(4) 0.34968(14) 0.0573(8) Uani 1 1 d . . .
O8 O 0.6155(4) 1.6270(4) 0.35464(16) 0.0794(12) Uani 1 1 d . . .
O1W O 0.2104(3) 0.2414(5) 0.5801(2) 0.1032(17) Uani 1 1 d . . .
H1WB H 0.2714 0.1956 0.5712 0.155 Uiso 1 1 d R . .
H1WC H 0.2290 0.3085 0.6037 0.155 Uiso 1 1 d R . .
O2W O 0.6232(4) 0.2187(5) 0.66419(19) 0.0973(15) Uani 1 1 d . . .
H2WD H 0.5881 0.2664 0.6371 0.117 Uiso 1 1 d R . .
H2WC H 0.6861 0.1850 0.6510 0.146 Uiso 1 1 d R . .
C20 C 0.4080(4) 1.5036(6) 0.4547(2) 0.0547(12) Uani 1 1 d . . .
H20A H 0.3538 1.5609 0.4311 0.066 Uiso 1 1 calc R . .
H20B H 0.3962 1.4050 0.4436 0.066 Uiso 1 1 calc R . .
C21 C 0.6179(5) 1.4785(8) 0.4811(2) 0.0738(16) Uani 1 1 d . . .
H21A H 0.6946 1.5173 0.4740 0.089 Uiso 1 1 calc R . .
H21B H 0.6201 1.3778 0.4720 0.089 Uiso 1 1 calc R . .
C19 C 0.5331(4) 1.5472(7) 0.4412(2) 0.0656(13) Uani 1 1 d . . .
H19 H 0.5388 1.6495 0.4488 0.079 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
C1 N1 1.334(5) . ?
C1 C2 1.362(6) . ?
C2 C3 1.389(6) . ?
C3 O6 1.343(4) . ?
C3 C4 1.372(6) . ?
C4 C5 1.374(6) . ?
C5 N1 1.330(5) . ?
C6 O6 1.443(4) . ?
C6 C7 1.524(4) . ?
C7 C8 1.522(4) 2 ?
C7 C8 1.522(4) . ?
C7 C6 1.524(4) 2 ?
C8 O5 1.432(4) . ?
C9 O5 1.339(5) . ?
C9 C13 1.371(6) . ?
C9 C10 1.388(6) . ?
C10 C11 1.359(6) . ?
C11 N2 1.333(5) . ?
C12 N2 1.321(6) . ?
C12 C13 1.363(6) . ?
C14 O1 1.248(5) . ?
C14 O2 1.251(5) . ?
C14 C15 1.511(5) . ?
C15 C16 1.519(6) . ?
C15 C17 1.522(6) 3_656 ?
C16 C17 1.513(5) . ?
C17 C15 1.522(6) 3_656 ?
C18 O7 1.246(6) . ?
C18 O8 1.255(6) . ?
C18 C19 1.504(7) . ?
Cd1 O7 2.272(3) . ?
Cd1 O7 2.272(3) 2_655 ?
Cd1 O4 2.317(3) 2_655 ?
Cd1 O4 2.317(3) . ?
Cd1 N1 2.321(3) . ?
Cd1 N1 2.321(3) 2_655 ?
Cd2 O2 2.269(3) 3_556 ?
Cd2 O2 2.269(3) . ?
Cd2 O3 2.279(3) . ?
Cd2 O3 2.279(3) 3_556 ?
Cd2 N2 2.361(3) 3_556 ?
Cd2 N2 2.361(3) . ?
C20 C21 1.500(7) 3_686 ?
C20 C19 1.531(7) . ?
C21 C19 1.458(7) . ?
C21 C20 1.500(7) 3_686 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.6(4) . . ?
C1 C2 C3 118.7(4) . . ?
O6 C3 C4 125.9(4) . . ?
O6 C3 C2 115.6(4) . . ?
C4 C3 C2 118.6(4) . . ?
C3 C4 C5 118.4(4) . . ?
N1 C5 C4 123.8(4) . . ?
O6 C6 C7 106.1(3) . . ?
C8 C7 C8 110.3(4) 2 . ?
C8 C7 C6 109.3(2) 2 . ?
C8 C7 C6 108.34(19) . . ?
C8 C7 C6 108.34(19) 2 2 ?
C8 C7 C6 109.3(2) . 2 ?
C6 C7 C6 111.3(4) . 2 ?
O5 C8 C7 107.4(3) . . ?
O5 C9 C13 116.7(4) . . ?
O5 C9 C10 125.8(4) . . ?
C13 C9 C10 117.5(4) . . ?
C11 C10 C9 118.1(4) . . ?
N2 C11 C10 125.3(4) . . ?
N2 C12 C13 124.4(4) . . ?
C12 C13 C9 119.4(4) . . ?
O1 C14 O2 124.7(4) . . ?
O1 C14 C15 117.7(4) . . ?
O2 C14 C15 117.6(4) . . ?
C14 C15 C16 110.1(3) . . ?
C14 C15 C17 113.9(3) . 3_656 ?
C16 C15 C17 110.0(3) . 3_656 ?
C17 C16 C15 110.9(4) . . ?
C16 C17 C15 111.3(4) . 3_656 ?
O7 C18 O8 124.6(5) . . ?
O7 C18 C19 120.9(5) . . ?
O8 C18 C19 114.3(5) . . ?
O7 Cd1 O7 171.13(17) . 2_655 ?
O7 Cd1 O4 86.93(12) . 2_655 ?
O7 Cd1 O4 87.23(12) 2_655 2_655 ?
O7 Cd1 O4 87.23(12) . . ?
O7 Cd1 O4 86.93(12) 2_655 . ?
O4 Cd1 O4 97.57(19) 2_655 . ?
O7 Cd1 N1 92.55(12) . . ?
O7 Cd1 N1 93.88(12) 2_655 . ?
O4 Cd1 N1 174.70(13) 2_655 . ?
O4 Cd1 N1 87.67(13) . . ?
O7 Cd1 N1 93.88(12) . 2_655 ?
O7 Cd1 N1 92.55(12) 2_655 2_655 ?
O4 Cd1 N1 87.67(13) 2_655 2_655 ?
O4 Cd1 N1 174.70(13) . 2_655 ?
N1 Cd1 N1 87.10(17) . 2_655 ?
O2 Cd2 O2 180.00(16) 3_556 . ?
O2 Cd2 O3 90.18(11) 3_556 . ?
O2 Cd2 O3 89.82(11) . . ?
O2 Cd2 O3 89.82(11) 3_556 3_556 ?
O2 Cd2 O3 90.18(11) . 3_556 ?
O3 Cd2 O3 180.0 . 3_556 ?
O2 Cd2 N2 90.90(11) 3_556 3_556 ?
O2 Cd2 N2 89.10(11) . 3_556 ?
O3 Cd2 N2 85.08(14) . 3_556 ?
O3 Cd2 N2 94.92(14) 3_556 3_556 ?
O2 Cd2 N2 89.10(11) 3_556 . ?
O2 Cd2 N2 90.90(11) . . ?
O3 Cd2 N2 94.92(14) . . ?
O3 Cd2 N2 85.08(14) 3_556 . ?
N2 Cd2 N2 180.0 3_556 . ?
C5 N1 C1 116.9(3) . . ?
C5 N1 Cd1 120.5(3) . . ?
C1 N1 Cd1 122.6(3) . . ?
C12 N2 C11 115.2(4) . . ?
C12 N2 Cd2 118.7(3) . . ?
C11 N2 Cd2 125.6(3) . . ?
C14 O2 Cd2 124.5(3) . . ?
C9 O5 C8 119.0(3) . . ?
C3 O6 C6 117.0(3) . . ?
C18 O7 Cd1 126.1(3) . . ?
C21 C20 C19 112.1(4) 3_686 . ?
C19 C21 C20 113.7(5) . 3_686 ?
C21 C19 C18 112.2(5) . . ?
C21 C19 C20 111.6(5) . . ?
C18 C19 C20 112.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.114
_database_code_depnum_ccdc_archive 'CCDC 973272'
