# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Miao Du'
_publ_contact_author_email       DUMIAO@PUBLIC.TPT.TJ.CN

_publ_section_title              
;
Structural modulation of polythreading and
interpenetrating coordination networks with an elongated dipyridyl
building block and various anionic co-ligands
;
loop_
_publ_author_name
'Miao Du.'
'Liang-Fu Tang.'
'Xiu-Guang Wang.'
'Zhi-Hui Zhang.'
;
Xiao-Jun Zhao
;

# Attachment 'B810121C.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 692028'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Cd N18'
_chemical_formula_weight         961.39

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pcca

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

_cell_length_a                   23.155(8)
_cell_length_b                   24.935(8)
_cell_length_c                   8.302(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4793(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    2286
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      19.12

_exptl_crystal_description       Lamellar
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   Multi-SCAN
_exptl_absorpt_correction_T_min  0.8835
_exptl_absorpt_correction_T_max  0.9323
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'Apex II 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            25483
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4217
_reflns_number_gt                2568
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_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.

All atoms of the dca anion were refined using the pseudo-isotropic "ISOR"
restraint, as the free refinement gave unrealistic anisotropic displacement
parameters. The central nitrogen atom of dca is disordered over two sites
with the distance of 0.895 Å and therefore the "EADP" restraint was
applied to their thermal parameters.
;

_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)+(0.0567P)²+12.2581P] 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         4217
_refine_ls_number_parameters     302
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1728
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.057
_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 0.0000 0.26407(3) 0.2500 0.0536(2) Uani 1 2 d S . .
N1 N 0.0499(2) 0.1962(2) 0.1068(6) 0.0557(14) Uani 1 1 d . . .
N2 N 0.1680(2) -0.0149(2) -0.1850(5) 0.0418(12) Uani 1 1 d . . .
N3 N 0.20369(19) 0.02077(19) -0.2577(5) 0.0432(11) Uani 1 1 d . . .
N4 N 0.0500(2) 0.3272(2) 0.0922(6) 0.0570(14) Uani 1 1 d . . .
N5 N 0.2012(2) 0.4846(2) -0.3431(5) 0.0451(13) Uani 1 1 d . . .
N6 N 0.1682(2) 0.5247(2) -0.2790(5) 0.0485(13) Uani 1 1 d . . .
N7 N 0.0732(3) 0.2648(3) 0.4431(9) 0.081(2) Uani 1 1 d U A .
N8 N 0.1600(9) 0.2441(8) 0.581(2) 0.121(4) Uani 0.50 1 d PU A 1
N8' N 0.1655(10) 0.2235(8) 0.494(2) 0.121(4) Uani 0.50 1 d PU A 2
N9 N 0.2623(6) 0.2597(5) 0.4971(17) 0.189(5) Uani 1 1 d U A .
C1 C 0.0729(3) 0.1562(3) 0.1890(8) 0.0601(19) Uani 1 1 d . . .
H1 H 0.0683 0.1558 0.3003 0.072 Uiso 1 1 calc R . .
C2 C 0.1032(3) 0.1154(3) 0.1180(8) 0.0588(18) Uani 1 1 d . . .
H2 H 0.1186 0.0880 0.1808 0.071 Uiso 1 1 calc R . .
C3 C 0.1111(3) 0.1150(3) -0.0473(7) 0.0472(15) Uani 1 1 d . . .
C4 C 0.0888(3) 0.1576(3) -0.1328(8) 0.064(2) Uani 1 1 d . . .
H4 H 0.0939 0.1597 -0.2438 0.077 Uiso 1 1 calc R . .
C5 C 0.0591(3) 0.1967(3) -0.0524(8) 0.068(2) Uani 1 1 d . . .
H5 H 0.0444 0.2253 -0.1117 0.082 Uiso 1 1 calc R . .
C6 C 0.1430(2) 0.0701(2) -0.1233(7) 0.0429(14) Uani 1 1 d . . .
C7 C 0.1309(2) 0.0149(2) -0.1036(6) 0.0429(15) Uani 1 1 d . . .
C8 C 0.0817(3) -0.0116(3) -0.0174(8) 0.0606(19) Uani 1 1 d . . .
H8A H 0.0472 0.0091 -0.0331 0.091 Uiso 1 1 calc R . .
H8B H 0.0903 -0.0136 0.0956 0.091 Uiso 1 1 calc R . .
H8C H 0.0762 -0.0471 -0.0594 0.091 Uiso 1 1 calc R . .
C9 C 0.2500 0.0000 -0.3548(9) 0.045(2) Uani 1 2 d S . .
H9A H 0.2647 0.0283 -0.4235 0.054 Uiso 0.50 1 calc PR . .
H9B H 0.2353 -0.0283 -0.4235 0.054 Uiso 0.50 1 calc PR . .
C10 C 0.1900(3) 0.0720(2) -0.2226(6) 0.0431(14) Uani 1 1 d . . .
C11 C 0.2238(3) 0.1187(3) -0.2846(8) 0.066(2) Uani 1 1 d . . .
H11A H 0.2643 0.1117 -0.2722 0.099 Uiso 1 1 calc R . .
H11B H 0.2136 0.1503 -0.2251 0.099 Uiso 1 1 calc R . .
H11C H 0.2151 0.1240 -0.3966 0.099 Uiso 1 1 calc R . .
C12 C 0.0221(3) 0.3672(3) 0.0223(9) 0.0618(19) Uani 1 1 d . . .
H12 H -0.0177 0.3695 0.0366 0.074 Uiso 1 1 calc R . .
C13 C 0.0487(3) 0.4055(3) -0.0703(7) 0.0537(17) Uani 1 1 d . . .
H13 H 0.0272 0.4332 -0.1154 0.064 Uiso 1 1 calc R . .
C14 C 0.1077(3) 0.4029(2) -0.0963(7) 0.0442(15) Uani 1 1 d . . .
C15 C 0.1359(3) 0.3601(3) -0.0253(8) 0.0548(17) Uani 1 1 d . . .
H15 H 0.1753 0.3555 -0.0410 0.066 Uiso 1 1 calc R . .
C16 C 0.1060(3) 0.3243(3) 0.0681(8) 0.0576(18) Uani 1 1 d . . .
H16 H 0.1264 0.2966 0.1168 0.069 Uiso 1 1 calc R . .
C17 C 0.1386(2) 0.4434(3) -0.1897(7) 0.0435(15) Uani 1 1 d . . .
C18 C 0.1300(3) 0.4992(3) -0.1877(7) 0.0447(15) Uani 1 1 d . . .
C19 C 0.0856(3) 0.5329(3) -0.1023(8) 0.0597(18) Uani 1 1 d . . .
H19A H 0.0993 0.5691 -0.0937 0.090 Uiso 1 1 calc R . .
H19B H 0.0790 0.5187 0.0035 0.090 Uiso 1 1 calc R . .
H19C H 0.0501 0.5325 -0.1622 0.090 Uiso 1 1 calc R . .
C20 C 0.2500 0.5000 -0.4406(10) 0.052(2) Uani 1 2 d S . .
H20A H 0.2609 0.4702 -0.5093 0.063 Uiso 0.50 1 calc PR . .
H20B H 0.2391 0.5298 -0.5093 0.063 Uiso 0.50 1 calc PR . .
C21 C 0.1853(3) 0.4353(3) -0.2916(7) 0.0469(15) Uani 1 1 d . . .
C22 C 0.2131(3) 0.3856(3) -0.3492(9) 0.070(2) Uani 1 1 d . . .
H22A H 0.2141 0.3856 -0.4648 0.105 Uiso 1 1 calc R . .
H22B H 0.1915 0.3552 -0.3121 0.105 Uiso 1 1 calc R . .
H22C H 0.2518 0.3837 -0.3082 0.105 Uiso 1 1 calc R . .
C23 C 0.1134(5) 0.2537(4) 0.4775(12) 0.095(3) Uani 1 1 d . . .
C24 C 0.2157(7) 0.2495(5) 0.5129(18) 0.143(4) 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
Cd1 N7 2.332(8) 3 ?
Cd1 N7 2.332(8) . ?
Cd1 N4 2.352(5) 3 ?
Cd1 N4 2.352(5) . ?
Cd1 N1 2.369(5) . ?
Cd1 N1 2.369(5) 3 ?
N1 C1 1.321(8) . ?
N1 C5 1.339(8) . ?
N2 C7 1.320(7) . ?
N2 N3 1.356(6) . ?
N3 C10 1.348(7) . ?
N3 C9 1.438(6) . ?
N4 C16 1.315(8) . ?
N4 C12 1.323(8) . ?
N5 C21 1.351(7) . ?
N5 N6 1.367(6) . ?
N5 C20 1.442(6) . ?
N6 C18 1.327(7) . ?
N7 C23 1.014(11) . ?
N8 C23 1.40(2) . ?
N8 C24 1.42(2) . ?
N8' C24 1.34(2) . ?
N8' C23 1.43(2) . ?
N9 C24 1.117(16) . ?
C1 C2 1.370(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(8) . ?
C3 C6 1.481(8) . ?
C4 C5 1.368(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C10 1.368(8) . ?
C6 C7 1.414(8) . ?
C7 C8 1.497(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N3 1.438(6) 2 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.493(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.373(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(8) . ?
C14 C17 1.461(8) . ?
C15 C16 1.369(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C21 1.387(8) . ?
C17 C18 1.406(9) . ?
C18 C19 1.505(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N5 1.442(6) 2_565 ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.477(8) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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
N7 Cd1 N7 179.1(4) 3 . ?
N7 Cd1 N4 91.2(2) 3 3 ?
N7 Cd1 N4 88.2(2) . 3 ?
N7 Cd1 N4 88.2(2) 3 . ?
N7 Cd1 N4 91.2(2) . . ?
N4 Cd1 N4 96.0(3) 3 . ?
N7 Cd1 N1 90.9(2) 3 . ?
N7 Cd1 N1 89.8(2) . . ?
N4 Cd1 N1 175.91(19) 3 . ?
N4 Cd1 N1 87.60(18) . . ?
N7 Cd1 N1 89.8(2) 3 3 ?
N7 Cd1 N1 90.9(2) . 3 ?
N4 Cd1 N1 87.60(18) 3 3 ?
N4 Cd1 N1 175.91(19) . 3 ?
N1 Cd1 N1 88.9(3) . 3 ?
C1 N1 C5 116.9(6) . . ?
C1 N1 Cd1 118.5(4) . . ?
C5 N1 Cd1 124.5(4) . . ?
C7 N2 N3 104.8(5) . . ?
C10 N3 N2 112.5(4) . . ?
C10 N3 C9 129.6(4) . . ?
N2 N3 C9 117.9(4) . . ?
C16 N4 C12 117.2(6) . . ?
C16 N4 Cd1 122.3(4) . . ?
C12 N4 Cd1 120.6(4) . . ?
C21 N5 N6 112.9(5) . . ?
C21 N5 C20 129.3(5) . . ?
N6 N5 C20 117.5(4) . . ?
C18 N6 N5 104.2(5) . . ?
C23 N7 Cd1 149.3(9) . . ?
C23 N8 C24 115.9(16) . . ?
C24 N8' C23 119.2(16) . . ?
N1 C1 C2 123.0(6) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 120.1(6) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 117.0(6) . . ?
C4 C3 C6 123.3(5) . . ?
C2 C3 C6 119.6(5) . . ?
C5 C4 C3 119.1(6) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 123.8(6) . . ?
N1 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C10 C6 C7 105.2(5) . . ?
C10 C6 C3 128.8(5) . . ?
C7 C6 C3 126.0(5) . . ?
N2 C7 C6 111.1(5) . . ?
N2 C7 C8 119.5(6) . . ?
C6 C7 C8 129.3(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 N3 111.8(6) . 2 ?
N3 C9 H9A 109.3 . . ?
N3 C9 H9A 109.3 2 . ?
N3 C9 H9B 109.3 . . ?
N3 C9 H9B 109.3 2 . ?
H9A C9 H9B 107.9 . . ?
N3 C10 C6 106.5(5) . . ?
N3 C10 C11 122.8(5) . . ?
C6 C10 C11 130.7(5) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 C13 123.5(6) . . ?
N4 C12 H12 118.3 . . ?
C13 C12 H12 118.3 . . ?
C12 C13 C14 119.8(6) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 115.8(6) . . ?
C15 C14 C17 122.0(5) . . ?
C13 C14 C17 122.2(6) . . ?
C16 C15 C14 120.4(6) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
N4 C16 C15 123.3(6) . . ?
N4 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
C21 C17 C18 105.2(5) . . ?
C21 C17 C14 127.2(6) . . ?
C18 C17 C14 127.5(5) . . ?
N6 C18 C17 111.8(5) . . ?
N6 C18 C19 117.2(6) . . ?
C17 C18 C19 131.0(6) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 C20 N5 111.7(6) 2_565 . ?
N5 C20 H20A 109.3 2_565 . ?
N5 C20 H20A 109.3 . . ?
N5 C20 H20B 109.3 2_565 . ?
N5 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N5 C21 C17 105.9(5) . . ?
N5 C21 C22 122.8(6) . . ?
C17 C21 C22 131.2(6) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N7 C23 N8 158.1(15) . . ?
N7 C23 N8' 161.4(14) . . ?
N9 C24 N8' 159(2) . . ?
N9 C24 N8 162(2) . . ?

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
N7 Cd1 N1 C1 -137.4(5) 3 . . . ?
N7 Cd1 N1 C1 43.2(5) . . . . ?
N4 Cd1 N1 C1 134.4(5) . . . . ?
N1 Cd1 N1 C1 -47.6(5) 3 . . . ?
N7 Cd1 N1 C5 46.0(6) 3 . . . ?
N7 Cd1 N1 C5 -133.3(6) . . . . ?
N4 Cd1 N1 C5 -42.2(6) . . . . ?
N1 Cd1 N1 C5 135.8(7) 3 . . . ?
C7 N2 N3 C10 0.5(6) . . . . ?
C7 N2 N3 C9 179.1(5) . . . . ?
N7 Cd1 N4 C16 -138.1(6) 3 . . . ?
N7 Cd1 N4 C16 42.6(6) . . . . ?
N4 Cd1 N4 C16 131.0(6) 3 . . . ?
N1 Cd1 N4 C16 -47.1(5) . . . . ?
N7 Cd1 N4 C12 41.3(6) 3 . . . ?
N7 Cd1 N4 C12 -138.1(6) . . . . ?
N4 Cd1 N4 C12 -49.7(5) 3 . . . ?
N1 Cd1 N4 C12 132.2(6) . . . . ?
C21 N5 N6 C18 -1.3(6) . . . . ?
C20 N5 N6 C18 -175.7(5) . . . . ?
N4 Cd1 N7 C23 -171.3(17) 3 . . . ?
N4 Cd1 N7 C23 -75.3(17) . . . . ?
N1 Cd1 N7 C23 12.3(17) . . . . ?
N1 Cd1 N7 C23 101.1(17) 3 . . . ?
C5 N1 C1 C2 -2.3(11) . . . . ?
Cd1 N1 C1 C2 -179.1(6) . . . . ?
N1 C1 C2 C3 0.2(12) . . . . ?
C1 C2 C3 C4 1.8(11) . . . . ?
C1 C2 C3 C6 -178.7(6) . . . . ?
C2 C3 C4 C5 -1.8(11) . . . . ?
C6 C3 C4 C5 178.8(7) . . . . ?
C1 N1 C5 C4 2.3(11) . . . . ?
Cd1 N1 C5 C4 179.0(6) . . . . ?
C3 C4 C5 N1 -0.3(12) . . . . ?
C4 C3 C6 C10 53.9(10) . . . . ?
C2 C3 C6 C10 -125.4(7) . . . . ?
C4 C3 C6 C7 -127.6(7) . . . . ?
C2 C3 C6 C7 53.0(9) . . . . ?
N3 N2 C7 C6 -0.3(6) . . . . ?
N3 N2 C7 C8 175.4(5) . . . . ?
C10 C6 C7 N2 0.0(6) . . . . ?
C3 C6 C7 N2 -178.7(5) . . . . ?
C10 C6 C7 C8 -175.1(6) . . . . ?
C3 C6 C7 C8 6.2(10) . . . . ?
C10 N3 C9 N3 102.8(6) . . . 2 ?
N2 N3 C9 N3 -75.5(4) . . . 2 ?
N2 N3 C10 C6 -0.5(6) . . . . ?
C9 N3 C10 C6 -178.8(5) . . . . ?
N2 N3 C10 C11 178.4(5) . . . . ?
C9 N3 C10 C11 0.1(9) . . . . ?
C7 C6 C10 N3 0.2(6) . . . . ?
C3 C6 C10 N3 178.9(6) . . . . ?
C7 C6 C10 C11 -178.5(6) . . . . ?
C3 C6 C10 C11 0.2(11) . . . . ?
C16 N4 C12 C13 -1.1(11) . . . . ?
Cd1 N4 C12 C13 179.5(5) . . . . ?
N4 C12 C13 C14 1.1(11) . . . . ?
C12 C13 C14 C15 0.5(9) . . . . ?
C12 C13 C14 C17 -178.1(6) . . . . ?
C13 C14 C15 C16 -1.9(9) . . . . ?
C17 C14 C15 C16 176.7(6) . . . . ?
C12 N4 C16 C15 -0.4(10) . . . . ?
Cd1 N4 C16 C15 179.0(5) . . . . ?
C14 C15 C16 N4 1.9(11) . . . . ?
C15 C14 C17 C21 37.0(9) . . . . ?
C13 C14 C17 C21 -144.5(6) . . . . ?
C15 C14 C17 C18 -138.5(6) . . . . ?
C13 C14 C17 C18 40.0(9) . . . . ?
N5 N6 C18 C17 1.2(6) . . . . ?
N5 N6 C18 C19 -178.5(5) . . . . ?
C21 C17 C18 N6 -0.6(7) . . . . ?
C14 C17 C18 N6 175.6(5) . . . . ?
C21 C17 C18 C19 178.9(6) . . . . ?
C14 C17 C18 C19 -4.8(10) . . . . ?
C21 N5 C20 N5 -93.5(6) . . . 2_565 ?
N6 N5 C20 N5 79.8(4) . . . 2_565 ?
N6 N5 C21 C17 0.9(6) . . . . ?
C20 N5 C21 C17 174.4(5) . . . . ?
N6 N5 C21 C22 177.5(6) . . . . ?
C20 N5 C21 C22 -9.0(9) . . . . ?
C18 C17 C21 N5 -0.2(6) . . . . ?
C14 C17 C21 N5 -176.5(5) . . . . ?
C18 C17 C21 C22 -176.3(7) . . . . ?
C14 C17 C21 C22 7.4(11) . . . . ?
Cd1 N7 C23 N8 -164(3) . . . . ?
Cd1 N7 C23 N8' -31(5) . . . . ?
C24 N8 C23 N7 -151(3) . . . . ?
C24 N8 C23 N8' 52.4(18) . . . . ?
C24 N8' C23 N7 148(4) . . . . ?
C24 N8' C23 N8 -60(2) . . . . ?
C23 N8' C24 N9 -138(5) . . . . ?
C23 N8' C24 N8 57(2) . . . . ?
C23 N8 C24 N9 140(5) . . . . ?
C23 N8 C24 N8' -55.8(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.075

#===END

data_1.Mn
_database_code_depnum_ccdc_archive 'CCDC 692029'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H45 Mn N18 O0.50'
_chemical_formula_weight         912.94

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   24.958(4)
_cell_length_b                   24.637(4)
_cell_length_c                   8.1686(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5022.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3683
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      23.69

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8737
_exptl_absorpt_correction_T_max  0.9264
_exptl_absorpt_process_details   SADABS

_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  'Apex II 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            24392
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_sigmaI/netI    0.1229
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4427
_reflns_number_gt                2742
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

All atoms of the dca anion were refined using the pseudo-isotropic "ISOR"
restraint as well as similar Uij (SIMU) restraint, as the free refinement
gave unrealistic anisotropic displacement parameters.
;

_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)+(0.2000P)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     SHELXL
_refine_ls_extinction_coef       0.026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4427
_refine_ls_number_parameters     307
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.1278
_refine_ls_wR_factor_ref         0.3484
_refine_ls_wR_factor_gt          0.3078
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.272
_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
Mn1 Mn 0.0000 0.23060(5) 0.2500 0.0695(7) Uani 1 2 d S . .
N1 N 0.4501(2) -0.2022(2) 0.1308(8) 0.0693(16) Uani 1 1 d . . .
N2 N 0.33981(17) 0.01360(17) -0.1481(6) 0.0514(12) Uani 1 1 d . . .
N3 N 0.30747(18) -0.02368(18) -0.2217(6) 0.0521(12) Uani 1 1 d . . .
N4 N 0.21717(17) 0.00826(18) -0.2265(6) 0.0525(12) Uani 1 1 d . . .
N5 N 0.18551(18) -0.03281(18) -0.1713(7) 0.0563(13) Uani 1 1 d . . .
N6 N 0.05213(19) 0.1663(2) 0.1274(8) 0.0705(16) Uani 1 1 d . . .
N7 N 0.0527(3) 0.2292(3) 0.4732(14) 0.097(3) Uani 1 1 d . . .
N8 N 0.1053(5) 0.2010(5) 0.6936(15) 0.145(3) Uani 1 1 d U . .
N9 N 0.1849(5) 0.2431(4) 0.807(2) 0.172(6) Uani 1 1 d . . .
C1 C 0.4011(3) -0.1209(3) 0.1568(10) 0.076(2) Uani 1 1 d . . .
H1 H 0.3876 -0.0940 0.2251 0.091 Uiso 1 1 calc R . .
C2 C 0.4275(3) -0.1652(3) 0.2236(11) 0.083(2) Uani 1 1 d . . .
H2 H 0.4292 -0.1689 0.3368 0.100 Uiso 1 1 calc R . .
C3 C 0.4446(3) -0.1980(3) -0.0306(11) 0.085(2) Uani 1 1 d . . .
H3 H 0.4604 -0.2244 -0.0962 0.102 Uiso 1 1 calc R . .
C4 C 0.4172(3) -0.1572(3) -0.1045(11) 0.082(2) Uani 1 1 d . . .
H4 H 0.4136 -0.1566 -0.2178 0.099 Uiso 1 1 calc R . .
C5 C 0.3949(2) -0.1166(2) -0.0101(8) 0.0584(16) Uani 1 1 d . . .
C6 C 0.3649(2) -0.0710(2) -0.0833(8) 0.0554(15) Uani 1 1 d . . .
C7 C 0.3214(2) -0.0743(2) -0.1843(8) 0.0557(15) Uani 1 1 d . . .
C8 C 0.2912(3) -0.1219(3) -0.2468(11) 0.085(2) Uani 1 1 d . . .
H8A H 0.2539 -0.1177 -0.2212 0.128 Uiso 1 1 calc R . .
H8B H 0.3045 -0.1543 -0.1963 0.128 Uiso 1 1 calc R . .
H8C H 0.2955 -0.1243 -0.3633 0.128 Uiso 1 1 calc R . .
C9 C 0.3749(2) -0.0153(2) -0.0644(7) 0.0514(14) Uani 1 1 d . . .
C10 C 0.4199(2) 0.0111(3) 0.0221(9) 0.0668(17) Uani 1 1 d . . .
H10A H 0.4493 0.0164 -0.0519 0.100 Uiso 1 1 d R . .
H10B H 0.4313 -0.0113 0.1118 0.100 Uiso 1 1 d R . .
H10C H 0.4080 0.0456 0.0631 0.100 Uiso 1 1 d R . .
C11 C 0.2641(2) -0.0048(3) -0.3217(8) 0.0560(15) Uani 1 1 d . . .
H11A H 0.2550 -0.0327 -0.4010 0.067 Uiso 1 1 calc R . .
H11B H 0.2755 0.0271 -0.3815 0.067 Uiso 1 1 calc R . .
C12 C 0.1457(2) -0.0084(2) -0.0928(8) 0.0561(14) Uani 1 1 d . . .
C13 C 0.1026(3) -0.0420(3) -0.0198(10) 0.0731(19) Uani 1 1 d . . .
H13A H 0.0732 -0.0445 -0.0951 0.110 Uiso 1 1 calc R . .
H13B H 0.0906 -0.0256 0.0802 0.110 Uiso 1 1 calc R . .
H13C H 0.1161 -0.0777 0.0027 0.110 Uiso 1 1 calc R . .
C14 C 0.1520(2) 0.0483(2) -0.0961(8) 0.0548(14) Uani 1 1 d . . .
C15 C 0.1981(2) 0.0576(2) -0.1821(8) 0.0547(14) Uani 1 1 d . . .
C16 C 0.2258(3) 0.1074(3) -0.2347(10) 0.075(2) Uani 1 1 d . . .
H16A H 0.2634 0.1042 -0.2114 0.113 Uiso 1 1 calc R . .
H16B H 0.2113 0.1379 -0.1767 0.113 Uiso 1 1 calc R . .
H16C H 0.2207 0.1125 -0.3502 0.113 Uiso 1 1 calc R . .
C17 C 0.1174(2) 0.0888(2) -0.0185(8) 0.0559(15) Uani 1 1 d . . .
C18 C 0.0621(2) 0.0872(3) -0.0335(10) 0.0725(19) Uani 1 1 d . . .
H18 H 0.0458 0.0599 -0.0942 0.087 Uiso 1 1 calc R . .
C19 C 0.0319(2) 0.1258(2) 0.0411(11) 0.077(2) Uani 1 1 d . . .
H19 H -0.0051 0.1235 0.0309 0.093 Uiso 1 1 calc R . .
C20 C 0.1043(2) 0.1681(2) 0.1422(10) 0.0674(18) Uani 1 1 d . . .
H20 H 0.1193 0.1961 0.2035 0.081 Uiso 1 1 calc R . .
C21 C 0.1382(2) 0.1309(2) 0.0722(9) 0.0643(17) Uani 1 1 d . . .
H21 H 0.1751 0.1342 0.0860 0.077 Uiso 1 1 calc R . .
C22 C 0.0759(4) 0.2204(4) 0.5596(15) 0.091(3) Uani 1 1 d U . .
C23 C 0.1477(6) 0.2277(5) 0.7513(19) 0.126(3) Uani 1 1 d U . .
O1 O 0.2997(12) 0.2368(13) 0.684(6) 0.158(16) Uani 0.25 1 d PD . .
H1A H 0.2774 0.2594 0.6452 0.237 Uiso 0.25 1 d PRD . .
H1B H 0.3011 0.2242 0.7950 0.237 Uiso 0.25 1 d PRD . .


_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
Mn1 N6 2.281(5) 3 ?
Mn1 N6 2.281(5) . ?
Mn1 N7 2.249(12) 3 ?
Mn1 N7 2.249(12) . ?
Mn1 N1 2.290(5) 6_566 ?
Mn1 N1 2.290(5) 8_665 ?
N1 C2 1.311(10) . ?
N1 C3 1.329(11) . ?
N1 Mn1 2.290(5) 6_656 ?
N2 C9 1.321(7) . ?
N2 N3 1.363(7) . ?
N3 C7 1.330(7) . ?
N3 C11 1.433(7) . ?
N4 C15 1.354(7) . ?
N4 N5 1.361(7) . ?
N4 C11 1.443(7) . ?
N5 C12 1.326(7) . ?
N6 C20 1.310(8) . ?
N6 C19 1.323(9) . ?
N7 C22 0.938(12) . ?
N8 C23 1.333(17) . ?
N8 C22 1.402(15) . ?
N9 C23 1.100(16) . ?
C1 C5 1.377(11) . ?
C1 C2 1.386(9) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.358(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.477(8) . ?
C6 C7 1.365(8) . ?
C6 C9 1.402(8) . ?
C7 C8 1.484(9) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.477(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.408(8) . ?
C12 C13 1.482(9) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.368(8) . ?
C14 C17 1.464(8) . ?
C15 C16 1.472(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.376(9) . ?
C17 C18 1.387(9) . ?
C18 C19 1.357(9) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.371(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
O1 H1A 0.8482 . ?
O1 H1B 0.9567 . ?

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
N6 Mn1 N6 92.1(3) 3 . ?
N6 Mn1 N7 90.7(2) 3 3 ?
N6 Mn1 N7 88.1(2) . 3 ?
N6 Mn1 N7 88.1(2) 3 . ?
N6 Mn1 N7 90.7(2) . . ?
N7 Mn1 N7 178.3(4) 3 . ?
N6 Mn1 N1 90.3(2) 3 6_566 ?
N6 Mn1 N1 177.61(18) . 6_566 ?
N7 Mn1 N1 92.1(3) 3 6_566 ?
N7 Mn1 N1 89.1(2) . 6_566 ?
N6 Mn1 N1 177.61(18) 3 8_665 ?
N6 Mn1 N1 90.3(2) . 8_665 ?
N7 Mn1 N1 89.1(2) 3 8_665 ?
N7 Mn1 N1 92.1(3) . 8_665 ?
N1 Mn1 N1 87.3(3) 6_566 8_665 ?
C2 N1 C3 118.4(6) . . ?
C2 N1 Mn1 119.3(5) . 6_656 ?
C3 N1 Mn1 122.2(4) . 6_656 ?
C9 N2 N3 104.9(4) . . ?
C7 N3 N2 112.1(4) . . ?
C7 N3 C11 129.2(5) . . ?
N2 N3 C11 118.7(5) . . ?
C15 N4 N5 112.0(5) . . ?
C15 N4 C11 129.0(5) . . ?
N5 N4 C11 118.9(5) . . ?
C12 N5 N4 105.0(4) . . ?
C20 N6 C19 117.0(5) . . ?
C20 N6 Mn1 120.3(4) . . ?
C19 N6 Mn1 122.7(4) . . ?
C22 N7 Mn1 167.0(10) . . ?
C23 N8 C22 121.5(11) . . ?
C5 C1 C2 120.4(7) . . ?
C5 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
N1 C2 C1 121.5(8) . . ?
N1 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
N1 C3 C4 123.3(7) . . ?
N1 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C3 C4 C5 119.5(8) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C1 C5 C4 116.8(6) . . ?
C1 C5 C6 121.2(6) . . ?
C4 C5 C6 122.0(6) . . ?
C7 C6 C9 105.5(5) . . ?
C7 C6 C5 127.0(5) . . ?
C9 C6 C5 127.5(5) . . ?
N3 C7 C6 106.9(5) . . ?
N3 C7 C8 121.9(5) . . ?
C6 C7 C8 131.3(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 110.6(5) . . ?
N2 C9 C10 120.9(5) . . ?
C6 C9 C10 128.3(5) . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 108.9 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 N4 112.2(5) . . ?
N3 C11 H11A 109.2 . . ?
N4 C11 H11A 109.2 . . ?
N3 C11 H11B 109.2 . . ?
N4 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N5 C12 C14 110.9(5) . . ?
N5 C12 C13 119.1(5) . . ?
C14 C12 C13 130.0(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 105.6(5) . . ?
C15 C14 C17 127.2(5) . . ?
C12 C14 C17 127.1(5) . . ?
N4 C15 C14 106.4(5) . . ?
N4 C15 C16 120.4(5) . . ?
C14 C15 C16 133.1(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 116.4(5) . . ?
C21 C17 C14 121.7(5) . . ?
C18 C17 C14 122.0(5) . . ?
C19 C18 C17 119.5(6) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
N6 C19 C18 123.8(6) . . ?
N6 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
N6 C20 C21 123.6(6) . . ?
N6 C20 H20 118.2 . . ?
C21 C20 H20 118.2 . . ?
C20 C21 C17 119.7(6) . . ?
C20 C21 H21 120.1 . . ?
C17 C21 H21 120.1 . . ?
N7 C22 N8 171.5(14) . . ?
N9 C23 N8 170.3(14) . . ?
H1A O1 H1B 126.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N2 N3 C7 0.6(6) . . . . ?
C9 N2 N3 C11 179.3(5) . . . . ?
C15 N4 N5 C12 0.7(7) . . . . ?
C11 N4 N5 C12 -178.6(5) . . . . ?
N6 Mn1 N6 C20 -128.0(7) 3 . . . ?
N7 Mn1 N6 C20 141.3(6) 3 . . . ?
N7 Mn1 N6 C20 -39.9(6) . . . . ?
N1 Mn1 N6 C20 52.2(6) 8_665 . . . ?
N6 Mn1 N6 C19 51.1(6) 3 . . . ?
N7 Mn1 N6 C19 -39.5(6) 3 . . . ?
N7 Mn1 N6 C19 139.3(7) . . . . ?
N1 Mn1 N6 C19 -128.6(6) 8_665 . . . ?
N6 Mn1 N7 C22 62(5) 3 . . . ?
N6 Mn1 N7 C22 -30(5) . . . . ?
N1 Mn1 N7 C22 152(5) 6_566 . . . ?
N1 Mn1 N7 C22 -121(5) 8_665 . . . ?
C3 N1 C2 C1 -3.8(12) . . . . ?
Mn1 N1 C2 C1 173.9(6) 6_656 . . . ?
C5 C1 C2 N1 4.5(13) . . . . ?
C2 N1 C3 C4 0.6(13) . . . . ?
Mn1 N1 C3 C4 -177.0(6) 6_656 . . . ?
N1 C3 C4 C5 1.9(13) . . . . ?
C2 C1 C5 C4 -1.9(11) . . . . ?
C2 C1 C5 C6 177.3(7) . . . . ?
C3 C4 C5 C1 -1.2(11) . . . . ?
C3 C4 C5 C6 179.7(7) . . . . ?
C1 C5 C6 C7 -123.1(7) . . . . ?
C4 C5 C6 C7 56.0(10) . . . . ?
C1 C5 C6 C9 57.1(10) . . . . ?
C4 C5 C6 C9 -123.8(8) . . . . ?
N2 N3 C7 C6 -0.6(7) . . . . ?
C11 N3 C7 C6 -179.0(5) . . . . ?
N2 N3 C7 C8 178.5(6) . . . . ?
C11 N3 C7 C8 0.0(10) . . . . ?
C9 C6 C7 N3 0.3(7) . . . . ?
C5 C6 C7 N3 -179.6(6) . . . . ?
C9 C6 C7 C8 -178.7(7) . . . . ?
C5 C6 C7 C8 1.5(12) . . . . ?
N3 N2 C9 C6 -0.5(6) . . . . ?
N3 N2 C9 C10 174.9(5) . . . . ?
C7 C6 C9 N2 0.1(7) . . . . ?
C5 C6 C9 N2 180.0(6) . . . . ?
C7 C6 C9 C10 -174.8(6) . . . . ?
C5 C6 C9 C10 5.0(11) . . . . ?
C7 N3 C11 N4 94.7(7) . . . . ?
N2 N3 C11 N4 -83.7(6) . . . . ?
C15 N4 C11 N3 103.2(7) . . . . ?
N5 N4 C11 N3 -77.6(7) . . . . ?
N4 N5 C12 C14 -0.5(7) . . . . ?
N4 N5 C12 C13 178.5(6) . . . . ?
N5 C12 C14 C15 0.2(7) . . . . ?
C13 C12 C14 C15 -178.7(7) . . . . ?
N5 C12 C14 C17 -177.8(6) . . . . ?
C13 C12 C14 C17 3.3(11) . . . . ?
N5 N4 C15 C14 -0.6(7) . . . . ?
C11 N4 C15 C14 178.6(6) . . . . ?
N5 N4 C15 C16 -178.0(6) . . . . ?
C11 N4 C15 C16 1.2(10) . . . . ?
C12 C14 C15 N4 0.3(7) . . . . ?
C17 C14 C15 N4 178.2(6) . . . . ?
C12 C14 C15 C16 177.2(7) . . . . ?
C17 C14 C15 C16 -4.9(12) . . . . ?
C15 C14 C17 C21 -44.4(10) . . . . ?
C12 C14 C17 C21 133.1(7) . . . . ?
C15 C14 C17 C18 134.9(7) . . . . ?
C12 C14 C17 C18 -47.5(10) . . . . ?
C21 C17 C18 C19 -0.6(11) . . . . ?
C14 C17 C18 C19 180.0(7) . . . . ?
C20 N6 C19 C18 -1.1(12) . . . . ?
Mn1 N6 C19 C18 179.7(6) . . . . ?
C17 C18 C19 N6 1.1(13) . . . . ?
C19 N6 C20 C21 0.7(11) . . . . ?
Mn1 N6 C20 C21 179.9(6) . . . . ?
N6 C20 C21 C17 -0.4(12) . . . . ?
C18 C17 C21 C20 0.3(10) . . . . ?
C14 C17 C21 C20 179.7(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.173

#===END

data_1.Ni
_database_code_depnum_ccdc_archive 'CCDC 692030'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H48 N18 Ni O2'
_chemical_formula_weight         943.73

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   24.893(2)
_cell_length_b                   24.682(2)
_cell_length_c                   8.1486(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5006.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1639
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      19.24

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8836
_exptl_absorpt_correction_T_max  0.9053
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            32086
_diffrn_reflns_av_R_equivalents  0.1471
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.84
_reflns_number_total             5962
_reflns_number_gt                2577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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)+(0.0879P)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         5962
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1932
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_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
Ni1 Ni 0.5000 0.23230(3) 1.2500 0.0418(2) Uani 1 2 d S . .
N1 N 0.45040(12) 0.17169(13) 1.1422(4) 0.0454(9) Uani 1 1 d . . .
N2 N 0.28410(12) 0.00941(13) 0.7989(4) 0.0376(8) Uani 1 1 d . . .
N3 N 0.31638(13) -0.03165(13) 0.8537(4) 0.0432(8) Uani 1 1 d . . .
N4 N 0.19383(13) -0.02373(13) 0.8043(4) 0.0390(8) Uani 1 1 d . . .
N5 N 0.16071(12) 0.01351(13) 0.8775(4) 0.0401(8) Uani 1 1 d . . .
N6 N 0.04817(13) -0.20558(13) 1.1476(4) 0.0441(9) Uani 1 1 d . . .
N7 N 0.54676(15) 0.23086(15) 1.0417(5) 0.0539(10) Uani 1 1 d . . .
N8 N 0.6021(2) 0.2028(2) 0.8085(7) 0.1101(19) Uani 1 1 d . . .
N9 N 0.6835(2) 0.2418(2) 0.7053(9) 0.118(2) Uani 1 1 d . . .
C1 C 0.39701(15) 0.17386(17) 1.1557(6) 0.0476(11) Uani 1 1 d . . .
H1 H 0.3819 0.2029 1.2118 0.057 Uiso 1 1 calc R . .
C2 C 0.36311(15) 0.13518(16) 1.0908(5) 0.0442(10) Uani 1 1 d . . .
H2 H 0.3262 0.1381 1.1067 0.053 Uiso 1 1 calc R . .
C3 C 0.38363(15) 0.09223(16) 1.0024(5) 0.0402(10) Uani 1 1 d . . .
C4 C 0.43960(16) 0.09080(17) 0.9887(6) 0.0506(12) Uani 1 1 d . . .
H4 H 0.4559 0.0627 0.9312 0.061 Uiso 1 1 calc R . .
C5 C 0.47058(17) 0.13005(17) 1.0588(6) 0.0553(13) Uani 1 1 d . . .
H5 H 0.5077 0.1276 1.0478 0.066 Uiso 1 1 calc R . .
C6 C 0.34888(15) 0.05089(16) 0.9295(5) 0.0395(10) Uani 1 1 d . . .
C7 C 0.30196(15) 0.05921(16) 0.8414(5) 0.0380(10) Uani 1 1 d . . .
C8 C 0.35612(16) -0.00639(17) 0.9310(5) 0.0421(10) Uani 1 1 d . . .
C9 C 0.27360(18) 0.10887(18) 0.7893(6) 0.0621(14) Uani 1 1 d . . .
H9A H 0.2733 0.1108 0.6716 0.093 Uiso 1 1 calc R . .
H9B H 0.2917 0.1400 0.8329 0.093 Uiso 1 1 calc R . .
H9C H 0.2373 0.1080 0.8294 0.093 Uiso 1 1 calc R . .
C10 C 0.39996(17) -0.0395(2) 1.0063(6) 0.0609(13) Uani 1 1 d . . .
H10A H 0.3868 -0.0752 1.0296 0.091 Uiso 1 1 calc R . .
H10B H 0.4117 -0.0226 1.1063 0.091 Uiso 1 1 calc R . .
H10C H 0.4296 -0.0418 0.9313 0.091 Uiso 1 1 calc R . .
C11 C 0.23743(14) -0.00501(17) 0.7035(5) 0.0413(10) Uani 1 1 d . . .
H11A H 0.2257 0.0263 0.6412 0.050 Uiso 1 1 calc R . .
H11B H 0.2471 -0.0332 0.6261 0.050 Uiso 1 1 calc R . .
C12 C 0.17981(16) -0.07522(16) 0.8409(5) 0.0433(10) Uani 1 1 d . . .
C13 C 0.13561(16) -0.07200(16) 0.9423(5) 0.0407(10) Uani 1 1 d . . .
C14 C 0.12542(15) -0.01617(16) 0.9613(5) 0.0384(10) Uani 1 1 d . . .
C15 C 0.21053(19) -0.12272(17) 0.7786(7) 0.0713(16) Uani 1 1 d . . .
H15A H 0.2053 -0.1260 0.6623 0.107 Uiso 1 1 calc R . .
H15B H 0.1980 -0.1550 0.8319 0.107 Uiso 1 1 calc R . .
H15C H 0.2480 -0.1178 0.8015 0.107 Uiso 1 1 calc R . .
C16 C 0.07993(16) 0.01107(18) 1.0473(5) 0.0523(12) Uani 1 1 d . . .
H16A H 0.0932 0.0418 1.1071 0.078 Uiso 1 1 calc R . .
H16B H 0.0634 -0.0140 1.1220 0.078 Uiso 1 1 calc R . .
H16C H 0.0539 0.0229 0.9680 0.078 Uiso 1 1 calc R . .
C17 C 0.06877(17) -0.16594(16) 1.2411(6) 0.0520(11) Uani 1 1 d . . .
H17 H 0.0639 -0.1681 1.3541 0.062 Uiso 1 1 calc R . .
C18 C 0.09683(17) -0.12194(17) 1.1796(6) 0.0518(12) Uani 1 1 d . . .
H18 H 0.1096 -0.0953 1.2503 0.062 Uiso 1 1 calc R . .
C19 C 0.10574(16) -0.11779(16) 1.0124(5) 0.0432(11) Uani 1 1 d . . .
C20 C 0.08529(18) -0.15913(17) 0.9154(5) 0.0548(12) Uani 1 1 d . . .
H20 H 0.0901 -0.1584 0.8022 0.066 Uiso 1 1 calc R . .
C21 C 0.05769(17) -0.20155(18) 0.9883(6) 0.0548(12) Uani 1 1 d . . .
H21 H 0.0450 -0.2291 0.9207 0.066 Uiso 1 1 calc R . .
C22 C 0.5751(2) 0.22031(19) 0.9364(7) 0.0607(13) Uani 1 1 d . . .
C23 C 0.6463(3) 0.2258(2) 0.7614(8) 0.0788(16) Uani 1 1 d . . .
O1 O 0.7953(3) 0.2393(4) 0.8344(13) 0.207(5) Uani 0.750(11) 1 d P A 1
O1' O 0.8185(10) 0.2094(13) 0.574(3) 0.25(2) Uani 0.250(11) 1 d P 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
Ni1 N7 2.059(5) . ?
Ni1 N7 2.059(5) 3_657 ?
Ni1 N6 2.118(3) 6_668 ?
Ni1 N6 2.118(3) 8_665 ?
Ni1 N1 2.129(3) . ?
Ni1 N1 2.129(3) 3_657 ?
N1 C5 1.330(5) . ?
N1 C1 1.335(5) . ?
N2 C7 1.352(5) . ?
N2 N3 1.368(4) . ?
N2 C11 1.442(5) . ?
N3 C8 1.328(5) . ?
N4 C12 1.351(5) . ?
N4 N5 1.371(4) . ?
N4 C11 1.438(5) . ?
N5 C14 1.332(5) . ?
N6 C21 1.323(5) . ?
N6 C17 1.342(5) . ?
N6 Ni1 2.118(3) 6_558 ?
N7 C22 1.140(6) . ?
N8 C23 1.294(7) . ?
N8 C22 1.314(7) . ?
N9 C23 1.107(7) . ?
C1 C2 1.380(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(5) . ?
C3 C6 1.464(5) . ?
C4 C5 1.364(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.386(5) . ?
C6 C8 1.425(6) . ?
C7 C9 1.477(5) . ?
C8 C10 1.495(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.378(5) . ?
C12 C15 1.489(6) . ?
C13 C14 1.410(5) . ?
C13 C19 1.469(5) . ?
C14 C16 1.492(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.385(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(5) . ?
C20 C21 1.386(6) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?

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
N7 Ni1 N7 178.0(2) . 3_657 ?
N7 Ni1 N6 91.00(14) . 6_668 ?
N7 Ni1 N6 90.44(14) 3_657 6_668 ?
N7 Ni1 N6 90.44(14) . 8_665 ?
N7 Ni1 N6 91.00(14) 3_657 8_665 ?
N6 Ni1 N6 87.24(17) 6_668 8_665 ?
N7 Ni1 N1 88.59(14) . . ?
N7 Ni1 N1 90.01(14) 3_657 . ?
N6 Ni1 N1 178.21(13) 6_668 . ?
N6 Ni1 N1 91.02(12) 8_665 . ?
N7 Ni1 N1 90.01(14) . 3_657 ?
N7 Ni1 N1 88.59(14) 3_657 3_657 ?
N6 Ni1 N1 91.02(12) 6_668 3_657 ?
N6 Ni1 N1 178.21(13) 8_665 3_657 ?
N1 Ni1 N1 90.73(17) . 3_657 ?
C5 N1 C1 116.7(3) . . ?
C5 N1 Ni1 122.3(3) . . ?
C1 N1 Ni1 121.0(3) . . ?
C7 N2 N3 113.4(3) . . ?
C7 N2 C11 128.8(3) . . ?
N3 N2 C11 117.8(3) . . ?
C8 N3 N2 104.2(3) . . ?
C12 N4 N5 112.3(3) . . ?
C12 N4 C11 128.6(4) . . ?
N5 N4 C11 119.2(3) . . ?
C14 N5 N4 104.5(3) . . ?
C21 N6 C17 115.7(4) . . ?
C21 N6 Ni1 122.8(3) . 6_558 ?
C17 N6 Ni1 121.3(3) . 6_558 ?
C22 N7 Ni1 166.8(4) . . ?
C23 N8 C22 121.8(6) . . ?
N1 C1 C2 123.3(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 120.4(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 115.4(4) . . ?
C2 C3 C6 121.9(4) . . ?
C4 C3 C6 122.6(4) . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
N1 C5 C4 123.3(4) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C7 C6 C8 105.0(3) . . ?
C7 C6 C3 127.2(4) . . ?
C8 C6 C3 127.8(4) . . ?
N2 C7 C6 106.0(3) . . ?
N2 C7 C9 121.6(4) . . ?
C6 C7 C9 132.4(4) . . ?
N3 C8 C6 111.5(4) . . ?
N3 C8 C10 118.8(4) . . ?
C6 C8 C10 129.6(4) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N2 112.3(3) . . ?
N4 C11 H11A 109.1 . . ?
N2 C11 H11A 109.1 . . ?
N4 C11 H11B 109.1 . . ?
N2 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 C13 106.5(4) . . ?
N4 C12 C15 122.2(4) . . ?
C13 C12 C15 131.3(4) . . ?
C12 C13 C14 105.4(3) . . ?
C12 C13 C19 126.4(4) . . ?
C14 C13 C19 128.2(4) . . ?
N5 C14 C13 111.3(4) . . ?
N5 C14 C16 119.6(4) . . ?
C13 C14 C16 129.0(4) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 C18 123.9(4) . . ?
N6 C17 H17 118.0 . . ?
C18 C17 H17 118.0 . . ?
C19 C18 C17 119.7(4) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 116.6(4) . . ?
C18 C19 C13 121.4(4) . . ?
C20 C19 C13 122.0(4) . . ?
C21 C20 C19 119.5(4) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
N6 C21 C20 124.5(4) . . ?
N6 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
N7 C22 N8 171.3(6) . . ?
N9 C23 N8 171.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.84
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.066

#===END

data_1.Cu
_database_code_depnum_ccdc_archive 'CCDC 692031'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44.34 H44 Cu N16.34 O2.50'
_chemical_formula_weight         909.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pcca

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

_cell_length_a                   23.791(4)
_cell_length_b                   24.236(4)
_cell_length_c                   8.1907(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4722.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3278
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      21.30

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1893.3
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_process_details   SADABS

_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  'Apex II 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            24221
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4175
_reflns_number_gt                3035
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

All atoms of the dca and nitrate anions were refined using the
pseudo-isotropic "ISOR" restraint as well as similar Uij (SIMU) restraint,
as the free refinement gave unrealistic anisotropic displacement parameters.
Standard geometry constraints were applied for both types of anions in order
to improve the refinement stability. The soft "SADI" constraint and "FLAT"
constraint were also imposed on both anions. In addition, the "EADP" and
"EXYZ" constraints were applied for O1 and N7 atoms to properly treat the
substitutional disorder.
;

_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)+(0.1409P)²+4.5790P] 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         4175
_refine_ls_number_parameters     327
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.2488
_refine_ls_wR_factor_gt          0.2236
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.182
_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
Cu1 Cu 0.0000 0.26090(3) 1.2500 0.0559(4) Uani 1 2 d S . .
N1 N 0.04738(16) 0.20103(16) 1.1427(5) 0.0505(10) Uani 1 1 d . A .
N2 N 0.17001(14) -0.01702(14) 0.8771(4) 0.0405(8) Uani 1 1 d . A .
N3 N 0.20368(14) 0.02024(15) 0.8011(4) 0.0395(8) Uani 1 1 d . A .
N4 N 0.04526(15) 0.31936(15) 1.1315(5) 0.0507(10) Uani 1 1 d . A .
N5 N 0.20195(15) 0.48467(16) 0.7280(4) 0.0408(9) Uani 1 1 d . A .
N6 N 0.16893(15) 0.52526(16) 0.7864(4) 0.0443(9) Uani 1 1 d . A .
C1 C 0.0875(2) 0.1578(2) 0.9089(6) 0.0546(13) Uani 1 1 d . A .
H1 H 0.0927 0.1579 0.7964 0.066 Uiso 1 1 calc R . .
C2 C 0.0565(2) 0.1993(2) 0.9816(6) 0.0548(13) Uani 1 1 d . . .
H2 H 0.0415 0.2271 0.9163 0.066 Uiso 1 1 calc R A .
C3 C 0.0705(2) 0.1612(2) 1.2337(6) 0.0536(12) Uani 1 1 d . . .
H3 H 0.0653 0.1624 1.3462 0.064 Uiso 1 1 calc R A .
C4 C 0.1011(2) 0.1192(2) 1.1703(6) 0.0525(12) Uani 1 1 d . A .
H4 H 0.1159 0.0922 1.2388 0.063 Uiso 1 1 calc R . .
C5 C 0.11051(18) 0.11644(18) 1.0022(6) 0.0449(10) Uani 1 1 d . . .
C6 C 0.14269(17) 0.07027(18) 0.9328(5) 0.0409(10) Uani 1 1 d . A .
C7 C 0.13289(17) 0.01335(19) 0.9564(5) 0.0408(10) Uani 1 1 d . . .
C8 C 0.18939(17) 0.07347(18) 0.8315(5) 0.0433(10) Uani 1 1 d . . .
C9 C 0.08537(18) -0.0144(2) 1.0447(6) 0.0527(12) Uani 1 1 d . A .
H9A H 0.0568 -0.0247 0.9677 0.079 Uiso 1 1 calc R . .
H9B H 0.0698 0.0105 1.1237 0.079 Uiso 1 1 calc R . .
H9C H 0.0991 -0.0468 1.0991 0.079 Uiso 1 1 calc R . .
C10 C 0.2500 0.0000 0.7024(7) 0.0422(14) Uani 1 2 d S . .
H10A H 0.2366 -0.0296 0.6327 0.051 Uiso 0.50 1 calc PR A .
H10B H 0.2634 0.0296 0.6327 0.051 Uiso 0.50 1 calc PR . .
C11 C 0.2196(2) 0.1212(2) 0.7641(7) 0.0669(16) Uani 1 1 d . A .
H11A H 0.2591 0.1171 0.7839 0.100 Uiso 1 1 calc R . .
H11B H 0.2063 0.1544 0.8157 0.100 Uiso 1 1 calc R . .
H11C H 0.2129 0.1235 0.6487 0.100 Uiso 1 1 calc R . .
C12 C 0.04877(18) 0.3987(2) 0.9611(6) 0.0537(12) Uani 1 1 d . A .
H12 H 0.0291 0.4255 0.9032 0.064 Uiso 1 1 calc R . .
C13 C 0.0199(2) 0.3588(2) 1.0464(7) 0.0599(14) Uani 1 1 d . . .
H13 H -0.0192 0.3594 1.0442 0.072 Uiso 1 1 calc R A .
C14 C 0.10130(19) 0.3191(2) 1.1319(6) 0.0521(12) Uani 1 1 d . . .
H14 H 0.1199 0.2918 1.1908 0.062 Uiso 1 1 calc R A .
C15 C 0.13267(18) 0.35751(19) 1.0486(6) 0.0493(11) Uani 1 1 d . A .
H15 H 0.1717 0.3554 1.0512 0.059 Uiso 1 1 calc R . .
C16 C 0.10706(17) 0.39916(18) 0.9612(5) 0.0413(10) Uani 1 1 d . . .
C17 C 0.13953(17) 0.44170(18) 0.8747(5) 0.0398(10) Uani 1 1 d . A .
C18 C 0.18643(17) 0.43372(19) 0.7765(5) 0.0405(10) Uani 1 1 d . . .
C19 C 0.13008(17) 0.49912(19) 0.8753(5) 0.0406(10) Uani 1 1 d . . .
C20 C 0.08518(19) 0.5316(2) 0.9562(6) 0.0546(12) Uani 1 1 d . A .
H20A H 0.0972 0.5692 0.9678 0.082 Uiso 1 1 calc R . .
H20B H 0.0776 0.5162 1.0620 0.082 Uiso 1 1 calc R . .
H20C H 0.0517 0.5303 0.8910 0.082 Uiso 1 1 calc R . .
C21 C 0.2149(2) 0.3827(2) 0.7250(7) 0.0607(14) Uani 1 1 d . A .
H21A H 0.2190 0.3826 0.6084 0.091 Uiso 1 1 calc R . .
H21B H 0.1930 0.3514 0.7580 0.091 Uiso 1 1 calc R . .
H21C H 0.2514 0.3808 0.7751 0.091 Uiso 1 1 calc R . .
C22 C 0.2500 0.5000 0.6295(7) 0.0465(15) Uani 1 2 d S . .
H22A H 0.2602 0.4692 0.5598 0.056 Uiso 0.50 1 calc PR A .
H22B H 0.2398 0.5308 0.5598 0.056 Uiso 0.50 1 calc PR . .
N7 N 0.0620(3) 0.2581(3) 1.4887(9) 0.1118(17) Uani 0.584(8) 1 d PDU A 1
C23 C 0.1089(5) 0.2520(5) 1.5153(15) 0.124(2) Uani 0.584(8) 1 d PDU A 1
N8 N 0.1586(4) 0.2291(7) 1.593(2) 0.144(3) Uani 0.584(8) 1 d PDU A 1
C24 C 0.2116(7) 0.2522(6) 1.5313(18) 0.152(4) Uani 0.584(8) 1 d PDU A 1
N9 N 0.2597(6) 0.2552(6) 1.530(2) 0.165(5) Uani 0.584(8) 1 d PDU A 1
O1 O 0.0620(3) 0.2581(3) 1.4887(9) 0.1118(17) Uani 0.416(8) 1 d PDU A 2
N10 N 0.1012(4) 0.2754(5) 1.5641(12) 0.118(2) Uani 0.416(8) 1 d PDU A 2
O2 O 0.1321(7) 0.2536(6) 1.661(2) 0.137(3) Uani 0.416(8) 1 d PDU A 2
O3 O 0.1120(6) 0.3244(5) 1.5377(19) 0.133(4) Uani 0.416(8) 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
Cu1 N4 2.027(4) . ?
Cu1 N4 2.027(4) 3_557 ?
Cu1 N1 2.037(4) 3_557 ?
Cu1 N1 2.037(4) . ?
Cu1 N7 2.450(7) 3_557 ?
Cu1 N7 2.450(7) . ?
N1 C3 1.337(6) . ?
N1 C2 1.338(6) . ?
N2 C7 1.321(5) . ?
N2 N3 1.358(5) . ?
N3 C8 1.357(6) . ?
N3 C10 1.452(5) . ?
N4 C13 1.328(6) . ?
N4 C14 1.333(6) . ?
N5 N6 1.347(5) . ?
N5 C18 1.349(6) . ?
N5 C22 1.448(5) . ?
N6 C19 1.337(5) . ?
C1 C5 1.375(7) . ?
C1 C2 1.381(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.356(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.470(6) . ?
C6 C8 1.389(6) . ?
C6 C7 1.412(6) . ?
C7 C9 1.501(6) . ?
C8 C11 1.470(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N3 1.452(5) 2 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.377(7) . ?
C12 C16 1.387(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.375(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.470(6) . ?
C17 C18 1.389(6) . ?
C17 C19 1.410(6) . ?
C18 C21 1.472(7) . ?
C19 C20 1.482(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N5 1.448(5) 2_565 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N7 C23 1.145(8) . ?
C23 N8 1.451(7) . ?
N8 C24 1.468(8) . ?
C24 N9 1.145(11) . ?
N10 O2 1.204(8) . ?
N10 O3 1.234(8) . ?

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
N4 Cu1 N4 91.3(2) . 3_557 ?
N4 Cu1 N1 176.91(17) . 3_557 ?
N4 Cu1 N1 89.85(15) 3_557 3_557 ?
N4 Cu1 N1 89.85(15) . . ?
N4 Cu1 N1 176.91(17) 3_557 . ?
N1 Cu1 N1 89.1(2) 3_557 . ?
N4 Cu1 N7 87.57(19) . 3_557 ?
N4 Cu1 N7 94.7(2) 3_557 3_557 ?
N1 Cu1 N7 89.48(19) 3_557 3_557 ?
N1 Cu1 N7 88.2(2) . 3_557 ?
N4 Cu1 N7 94.7(2) . . ?
N4 Cu1 N7 87.57(19) 3_557 . ?
N1 Cu1 N7 88.2(2) 3_557 . ?
N1 Cu1 N7 89.48(19) . . ?
N7 Cu1 N7 176.8(3) 3_557 . ?
C3 N1 C2 117.4(4) . . ?
C3 N1 Cu1 120.1(3) . . ?
C2 N1 Cu1 122.5(3) . . ?
C7 N2 N3 104.4(3) . . ?
C8 N3 N2 113.6(3) . . ?
C8 N3 C10 127.8(3) . . ?
N2 N3 C10 118.6(3) . . ?
C13 N4 C14 117.4(4) . . ?
C13 N4 Cu1 120.9(3) . . ?
C14 N4 Cu1 121.8(3) . . ?
N6 N5 C18 113.9(3) . . ?
N6 N5 C22 118.1(3) . . ?
C18 N5 C22 128.0(3) . . ?
C19 N6 N5 104.5(4) . . ?
C5 C1 C2 120.3(5) . . ?
C5 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
N1 C2 C1 122.3(5) . . ?
N1 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
N1 C3 C4 123.3(4) . . ?
N1 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C3 C4 C5 120.0(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C1 C5 C4 116.7(4) . . ?
C1 C5 C6 123.2(4) . . ?
C4 C5 C6 120.1(4) . . ?
C8 C6 C7 105.6(4) . . ?
C8 C6 C5 127.2(4) . . ?
C7 C6 C5 127.2(4) . . ?
N2 C7 C6 111.5(4) . . ?
N2 C7 C9 119.4(4) . . ?
C6 C7 C9 128.9(4) . . ?
N3 C8 C6 104.9(4) . . ?
N3 C8 C11 123.9(4) . . ?
C6 C8 C11 131.2(4) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 N3 112.3(5) 2 . ?
N3 C10 H10A 109.1 2 . ?
N3 C10 H10A 109.1 . . ?
N3 C10 H10B 109.1 2 . ?
N3 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C16 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C16 C12 H12 119.9 . . ?
N4 C13 C12 123.1(4) . . ?
N4 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
N4 C14 C15 122.5(4) . . ?
N4 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C16 120.9(4) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C12 115.9(4) . . ?
C15 C16 C17 122.1(4) . . ?
C12 C16 C17 122.0(4) . . ?
C18 C17 C19 105.5(4) . . ?
C18 C17 C16 127.1(4) . . ?
C19 C17 C16 127.3(4) . . ?
N5 C18 C17 105.2(4) . . ?
N5 C18 C21 124.0(4) . . ?
C17 C18 C21 130.8(4) . . ?
N6 C19 C17 110.8(4) . . ?
N6 C19 C20 119.4(4) . . ?
C17 C19 C20 129.8(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 N5 112.3(5) 2_565 . ?
N5 C22 H22A 109.2 2_565 . ?
N5 C22 H22A 109.2 . . ?
N5 C22 H22B 109.2 2_565 . ?
N5 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C23 N7 Cu1 137.9(7) . . ?
N7 C23 N8 157.6(16) . . ?
C23 N8 C24 113.9(14) . . ?
N9 C24 N8 152.1(19) . . ?
O2 N10 O3 114.2(10) . . ?

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
N4 Cu1 N1 C3 129.8(4) . . . . ?
N1 Cu1 N1 C3 -53.1(3) 3_557 . . . ?
N7 Cu1 N1 C3 -142.6(4) 3_557 . . . ?
N7 Cu1 N1 C3 35.1(4) . . . . ?
N4 Cu1 N1 C2 -50.6(4) . . . . ?
N1 Cu1 N1 C2 126.5(5) 3_557 . . . ?
N7 Cu1 N1 C2 37.0(4) 3_557 . . . ?
N7 Cu1 N1 C2 -145.2(4) . . . . ?
C7 N2 N3 C8 0.7(4) . . . . ?
C7 N2 N3 C10 179.6(4) . . . . ?
N4 Cu1 N4 C13 -54.0(4) 3_557 . . . ?
N1 Cu1 N4 C13 128.9(4) . . . . ?
N7 Cu1 N4 C13 40.6(4) 3_557 . . . ?
N7 Cu1 N4 C13 -141.7(4) . . . . ?
N4 Cu1 N4 C14 127.9(5) 3_557 . . . ?
N1 Cu1 N4 C14 -49.3(4) . . . . ?
N7 Cu1 N4 C14 -137.5(4) 3_557 . . . ?
N7 Cu1 N4 C14 40.2(4) . . . . ?
C18 N5 N6 C19 -0.6(4) . . . . ?
C22 N5 N6 C19 -178.0(3) . . . . ?
C3 N1 C2 C1 1.4(8) . . . . ?
Cu1 N1 C2 C1 -178.3(4) . . . . ?
C5 C1 C2 N1 -0.5(8) . . . . ?
C2 N1 C3 C4 -1.6(8) . . . . ?
Cu1 N1 C3 C4 178.0(4) . . . . ?
N1 C3 C4 C5 0.9(8) . . . . ?
C2 C1 C5 C4 -0.3(7) . . . . ?
C2 C1 C5 C6 178.4(5) . . . . ?
C3 C4 C5 C1 0.1(7) . . . . ?
C3 C4 C5 C6 -178.7(5) . . . . ?
C1 C5 C6 C8 54.6(7) . . . . ?
C4 C5 C6 C8 -126.6(5) . . . . ?
C1 C5 C6 C7 -126.0(5) . . . . ?
C4 C5 C6 C7 52.7(7) . . . . ?
N3 N2 C7 C6 -0.4(4) . . . . ?
N3 N2 C7 C9 175.0(4) . . . . ?
C8 C6 C7 N2 -0.1(5) . . . . ?
C5 C6 C7 N2 -179.5(4) . . . . ?
C8 C6 C7 C9 -174.9(4) . . . . ?
C5 C6 C7 C9 5.7(7) . . . . ?
N2 N3 C8 C6 -0.7(5) . . . . ?
C10 N3 C8 C6 -179.5(4) . . . . ?
N2 N3 C8 C11 179.7(4) . . . . ?
C10 N3 C8 C11 0.9(7) . . . . ?
C7 C6 C8 N3 0.5(5) . . . . ?
C5 C6 C8 N3 179.9(4) . . . . ?
C7 C6 C8 C11 -180.0(5) . . . . ?
C5 C6 C8 C11 -0.5(8) . . . . ?
C8 N3 C10 N3 104.0(4) . . . 2 ?
N2 N3 C10 N3 -74.8(3) . . . 2 ?
C14 N4 C13 C12 -0.4(8) . . . . ?
Cu1 N4 C13 C12 -178.6(4) . . . . ?
C16 C12 C13 N4 0.0(8) . . . . ?
C13 N4 C14 C15 0.0(7) . . . . ?
Cu1 N4 C14 C15 178.2(4) . . . . ?
N4 C14 C15 C16 0.8(8) . . . . ?
C14 C15 C16 C12 -1.2(7) . . . . ?
C14 C15 C16 C17 178.3(4) . . . . ?
C13 C12 C16 C15 0.8(7) . . . . ?
C13 C12 C16 C17 -178.7(5) . . . . ?
C15 C16 C17 C18 45.1(7) . . . . ?
C12 C16 C17 C18 -135.5(5) . . . . ?
C15 C16 C17 C19 -134.1(5) . . . . ?
C12 C16 C17 C19 45.4(7) . . . . ?
N6 N5 C18 C17 -0.1(5) . . . . ?
C22 N5 C18 C17 177.0(4) . . . . ?
N6 N5 C18 C21 178.2(4) . . . . ?
C22 N5 C18 C21 -4.7(7) . . . . ?
C19 C17 C18 N5 0.7(4) . . . . ?
C16 C17 C18 N5 -178.7(4) . . . . ?
C19 C17 C18 C21 -177.4(5) . . . . ?
C16 C17 C18 C21 3.3(8) . . . . ?
N5 N6 C19 C17 1.0(4) . . . . ?
N5 N6 C19 C20 -178.6(4) . . . . ?
C18 C17 C19 N6 -1.1(5) . . . . ?
C16 C17 C19 N6 178.3(4) . . . . ?
C18 C17 C19 C20 178.5(4) . . . . ?
C16 C17 C19 C20 -2.2(7) . . . . ?
N6 N5 C22 N5 82.7(3) . . . 2_565 ?
C18 N5 C22 N5 -94.2(4) . . . 2_565 ?
N4 Cu1 N7 C23 -53.5(12) . . . . ?
N4 Cu1 N7 C23 -144.7(12) 3_557 . . . ?
N1 Cu1 N7 C23 125.4(12) 3_557 . . . ?
N1 Cu1 N7 C23 36.3(12) . . . . ?
Cu1 N7 C23 N8 -130.0(17) . . . . ?
N7 C23 N8 C24 179.4(5) . . . . ?
C23 N8 C24 N9 179.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.095

#===END

data_1.Zn
_database_code_depnum_ccdc_archive 'CCDC 692032'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H57 N15 O5 Zn'
_chemical_formula_weight         989.46

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   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                   14.4057(10)
_cell_length_b                   25.3367(15)
_cell_length_c                   17.6104(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.3070(10)
_cell_angle_gamma                90.00
_cell_volume                     6302.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5773
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.38

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8694
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            16897
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5527
_reflns_number_gt                4430
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the disordered dca anion and
glycol molecule in order to improve the refinement stability. The O4, O6, and
O6' atoms of the lattice water molecules as well as the central N8 atom of
dca were refined using the pseudo-isotropic "ISOR" restraint, as the free
refinement gave unrealistic anisotropic displacement parameters.
;

_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)+(0.2854P)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         5527
_refine_ls_number_parameters     378
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.3161
_refine_ls_wR_factor_gt          0.2876
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.030
_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 0.5000 0.49485(2) 0.7500 0.0371(3) Uani 1 2 d S . .
N1 N 0.6091(2) 0.55552(13) 0.76575(18) 0.0402(7) Uani 1 1 d . . .
N2 N 0.9307(2) 0.73153(13) 0.7797(2) 0.0469(8) Uani 1 1 d . . .
N3 N 0.9336(3) 0.73163(15) 0.8577(2) 0.0544(9) Uani 1 1 d . . .
N4 N 0.3910(2) 0.43372(13) 0.73338(17) 0.0403(7) Uani 1 1 d . . .
N5 N 0.0609(3) 0.25909(14) 0.64003(19) 0.0480(8) Uani 1 1 d . . .
N6 N 0.0670(2) 0.25881(12) 0.71805(19) 0.0416(8) Uani 1 1 d . . .
C1 C 0.6048(3) 0.59591(15) 0.7162(2) 0.0460(9) Uani 1 1 d . . .
H1 H 0.5546 0.5972 0.6740 0.055 Uiso 1 1 calc R . .
C2 C 0.6711(3) 0.63538(15) 0.7249(2) 0.0451(9) Uani 1 1 d . . .
H2 H 0.6645 0.6629 0.6893 0.054 Uiso 1 1 calc R . .
C3 C 0.7484(3) 0.63464(15) 0.7868(2) 0.0434(9) Uani 1 1 d . . .
C4 C 0.7509(3) 0.59181(18) 0.8370(2) 0.0557(11) Uani 1 1 d . . .
H4 H 0.8007 0.5887 0.8793 0.067 Uiso 1 1 calc R . .
C5 C 0.6819(3) 0.55477(17) 0.8249(2) 0.0510(10) Uani 1 1 d . . .
H5 H 0.6857 0.5272 0.8602 0.061 Uiso 1 1 calc R . .
C6 C 0.8217(3) 0.67530(16) 0.7979(2) 0.0462(9) Uani 1 1 d . . .
C7 C 0.8687(3) 0.69736(17) 0.8697(2) 0.0504(10) Uani 1 1 d . . .
C8 C 0.8508(5) 0.6893(3) 0.9482(3) 0.0806(17) Uani 1 1 d . . .
H8A H 0.8702 0.6544 0.9655 0.121 Uiso 1 1 calc R . .
H8B H 0.7845 0.6935 0.9476 0.121 Uiso 1 1 calc R . .
H8C H 0.8860 0.7147 0.9827 0.121 Uiso 1 1 calc R . .
C9 C 0.8637(3) 0.69873(16) 0.7414(2) 0.0445(9) Uani 1 1 d . . .
C10 C 0.8457(4) 0.6923(2) 0.6566(3) 0.0703(14) Uani 1 1 d . . .
H10A H 0.8002 0.7181 0.6331 0.105 Uiso 1 1 calc R . .
H10B H 0.8214 0.6576 0.6433 0.105 Uiso 1 1 calc R . .
H10C H 0.9036 0.6971 0.6383 0.105 Uiso 1 1 calc R . .
C11 C 1.0000 0.7629(2) 0.7500 0.0521(14) Uani 1 2 d S . .
H11A H 1.0328 0.7855 0.7911 0.062 Uiso 0.50 1 calc PR . .
H11B H 0.9672 0.7855 0.7089 0.062 Uiso 0.50 1 calc PR . .
C12 C 0.3878(3) 0.39592(15) 0.6797(2) 0.0442(9) Uani 1 1 d . . .
H12 H 0.4338 0.3962 0.6493 0.053 Uiso 1 1 calc R . .
C13 C 0.3214(3) 0.35722(16) 0.6670(2) 0.0467(9) Uani 1 1 d . . .
H13 H 0.3233 0.3321 0.6288 0.056 Uiso 1 1 calc R . .
C14 C 0.2524(3) 0.39494(18) 0.7659(2) 0.0558(11) Uani 1 1 d . . .
H14 H 0.2064 0.3963 0.7962 0.067 Uiso 1 1 calc R . .
C15 C 0.3223(3) 0.43223(17) 0.7753(2) 0.0506(10) Uani 1 1 d . . .
H15 H 0.3224 0.4581 0.8128 0.061 Uiso 1 1 calc R . .
C16 C 0.2496(3) 0.35451(15) 0.7109(2) 0.0418(9) Uani 1 1 d . . .
C17 C 0.1764(3) 0.31457(16) 0.6989(2) 0.0427(9) Uani 1 1 d . . .
C18 C 0.1275(3) 0.29229(17) 0.6273(2) 0.0483(10) Uani 1 1 d . . .
C19 C 0.1411(4) 0.3017(3) 0.5480(3) 0.0785(17) Uani 1 1 d . . .
H19A H 0.1970 0.2836 0.5401 0.118 Uiso 1 1 calc R . .
H19B H 0.1482 0.3389 0.5402 0.118 Uiso 1 1 calc R . .
H19C H 0.0872 0.2888 0.5119 0.118 Uiso 1 1 calc R . .
C20 C 0.1347(3) 0.29132(16) 0.7556(2) 0.0425(9) Uani 1 1 d . . .
C21 C 0.1587(4) 0.2953(2) 0.8420(2) 0.0637(13) Uani 1 1 d . . .
H21A H 0.1108 0.3154 0.8600 0.096 Uiso 1 1 calc R . .
H21B H 0.2189 0.3124 0.8574 0.096 Uiso 1 1 calc R . .
H21C H 0.1617 0.2605 0.8640 0.096 Uiso 1 1 calc R . .
C22 C 0.0000 0.2268(2) 0.7500 0.0442(12) Uani 1 2 d S . .
H22A H 0.0345 0.2042 0.7904 0.053 Uiso 0.50 1 calc PR . .
H22B H -0.0345 0.2042 0.7096 0.053 Uiso 0.50 1 calc PR . .
C26 C 0.9118(7) 0.1408(4) 0.5219(4) 0.142(4) Uani 1 1 d D . .
H26A H 0.8437 0.1367 0.5068 0.170 Uiso 1 1 calc R . .
H26B H 0.9365 0.1077 0.5450 0.170 Uiso 1 1 calc R . .
C25 C 0.9494(8) 0.1479(4) 0.4500(5) 0.165(5) Uani 1 1 d D . .
H25A H 0.9690 0.1134 0.4351 0.198 Uiso 1 1 calc R . .
H25B H 0.8970 0.1590 0.4098 0.198 Uiso 1 1 calc R . .
O1 O 1.0246(5) 0.1828(2) 0.4481(3) 0.1211(18) Uani 1 1 d D . .
H1A H 1.0100 0.2030 0.4113 0.182 Uiso 1 1 calc R . .
O2 O 0.9277(5) 0.1769(3) 0.5767(4) 0.153(3) Uani 1 1 d D . .
H2A H 0.9790 0.1911 0.5768 0.230 Uiso 1 1 calc R . .
N7 N 0.4994(16) 0.5013(9) 0.8734(6) 0.034(3) Uani 0.50 1 d PD . .
C23 C 0.5241(11) 0.4955(4) 0.9388(5) 0.048(3) Uani 0.50 1 d PD . .
N8 N 0.5629(10) 0.4933(6) 1.0116(6) 0.132(6) Uani 0.50 1 d PDU . .
N9 N 0.4939(18) 0.5119(9) 1.1242(8) 0.042(5) Uani 0.50 1 d PD . .
C24 C 0.5246(11) 0.5004(5) 1.0711(7) 0.051(3) Uani 0.50 1 d PD . .
O3 O 0.7897(14) 0.5454(6) 0.5422(10) 0.070(5) Uani 0.20 1 d P . .
O4 O 0.0000 0.3992(19) 0.7500 0.142(14) Uani 0.20 2 d SPU . .
O5 O 0.757(3) 0.4640(12) 0.5440(16) 0.071(10) Uani 0.10 1 d P . .
O6 O 0.993(2) 0.4504(13) 0.8586(19) 0.016(7) Uani 0.05 1 d PU A 1
O6' O 0.939(4) 0.429(2) 0.912(3) 0.058(13) Uani 0.05 1 d PU B 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 N1 2.177(3) 2_656 ?
Zn1 N1 2.177(3) . ?
Zn1 N7 2.180(11) . ?
Zn1 N7 2.180(11) 2_656 ?
Zn1 N4 2.184(3) . ?
Zn1 N4 2.184(3) 2_656 ?
Zn1 N9 2.207(13) 6_565 ?
Zn1 N9 2.207(13) 5_667 ?
N1 C5 1.325(5) . ?
N1 C1 1.339(5) . ?
N2 C9 1.350(5) . ?
N2 N3 1.366(5) . ?
N2 C11 1.451(5) . ?
N3 C7 1.323(6) . ?
N4 C12 1.340(5) . ?
N4 C15 1.345(5) . ?
N5 C18 1.327(5) . ?
N5 N6 1.359(5) . ?
N6 C20 1.347(5) . ?
N6 C22 1.456(4) . ?
C1 C2 1.370(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.398(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.396(6) . ?
C3 C6 1.461(6) . ?
C4 C5 1.354(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C9 1.394(6) . ?
C6 C7 1.426(6) . ?
C7 C8 1.469(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.473(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.451(5) 2_756 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.358(5) . ?
C12 H12 0.9300 . ?
C13 C16 1.409(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.367(6) . ?
C14 C16 1.405(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.447(6) . ?
C17 C20 1.393(5) . ?
C17 C18 1.434(6) . ?
C18 C19 1.467(6) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.495(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N6 1.456(4) 2_556 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C26 O2 1.316(6) . ?
C26 C25 1.484(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 O1 1.403(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
O1 H1A 0.8200 . ?
O2 H2A 0.8200 . ?
N7 N9 0.35(4) 5_667 ?
N7 C24 1.10(2) 5_667 ?
N7 C23 1.147(8) . ?
C23 C24 0.697(13) 5_667 ?
C23 N9 1.11(2) 5_667 ?
C23 N8 1.295(8) . ?
C23 N8 1.69(2) 5_667 ?
N8 C24 1.289(8) . ?
N8 C23 1.69(2) 5_667 ?
N8 C24 1.737(18) 5_667 ?
N8 N8 1.81(3) 5_667 ?
N9 N7 0.35(4) 5_667 ?
N9 C23 1.11(2) 5_667 ?
N9 C24 1.147(8) . ?
N9 Zn1 2.207(13) 5_667 ?
C24 C23 0.697(13) 5_667 ?
C24 N7 1.10(2) 5_667 ?
C24 N8 1.737(18) 5_667 ?

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 Zn1 N1 90.17(17) 2_656 . ?
N1 Zn1 N7 86.0(4) 2_656 . ?
N1 Zn1 N7 88.0(7) . . ?
N1 Zn1 N7 88.0(7) 2_656 2_656 ?
N1 Zn1 N7 86.0(4) . 2_656 ?
N7 Zn1 N7 171.4(12) . 2_656 ?
N1 Zn1 N4 90.08(13) 2_656 . ?
N1 Zn1 N4 179.52(10) . . ?
N7 Zn1 N4 92.5(7) . . ?
N7 Zn1 N4 93.6(4) 2_656 . ?
N1 Zn1 N4 179.52(10) 2_656 2_656 ?
N1 Zn1 N4 90.08(13) . 2_656 ?
N7 Zn1 N4 93.6(4) . 2_656 ?
N7 Zn1 N4 92.5(7) 2_656 2_656 ?
N4 Zn1 N4 89.67(17) . 2_656 ?
N1 Zn1 N9 92.4(8) 2_656 6_565 ?
N1 Zn1 N9 93.9(4) . 6_565 ?
N7 Zn1 N9 177.5(12) . 6_565 ?
N7 Zn1 N9 9.1(10) 2_656 6_565 ?
N4 Zn1 N9 85.7(4) . 6_565 ?
N4 Zn1 N9 88.0(8) 2_656 6_565 ?
N1 Zn1 N9 93.9(4) 2_656 5_667 ?
N1 Zn1 N9 92.4(8) . 5_667 ?
N7 Zn1 N9 9.1(10) . 5_667 ?
N7 Zn1 N9 177.5(12) 2_656 5_667 ?
N4 Zn1 N9 88.0(8) . 5_667 ?
N4 Zn1 N9 85.7(4) 2_656 5_667 ?
N9 Zn1 N9 171.1(11) 6_565 5_667 ?
C5 N1 C1 116.9(3) . . ?
C5 N1 Zn1 122.0(3) . . ?
C1 N1 Zn1 121.1(2) . . ?
C9 N2 N3 112.4(3) . . ?
C9 N2 C11 129.2(3) . . ?
N3 N2 C11 118.3(3) . . ?
C7 N3 N2 106.0(3) . . ?
C12 N4 C15 116.1(3) . . ?
C12 N4 Zn1 121.7(2) . . ?
C15 N4 Zn1 122.2(3) . . ?
C18 N5 N6 105.6(3) . . ?
C20 N6 N5 113.0(3) . . ?
C20 N6 C22 128.5(3) . . ?
N5 N6 C22 118.5(3) . . ?
N1 C1 C2 122.8(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 114.9(4) . . ?
C4 C3 C6 122.4(4) . . ?
C2 C3 C6 122.6(4) . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
N1 C5 C4 123.8(4) . . ?
N1 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C9 C6 C7 105.6(4) . . ?
C9 C6 C3 127.5(4) . . ?
C7 C6 C3 126.8(4) . . ?
N3 C7 C6 110.1(4) . . ?
N3 C7 C8 120.1(4) . . ?
C6 C7 C8 129.8(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 105.9(3) . . ?
N2 C9 C10 122.8(4) . . ?
C6 C9 C10 131.4(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N2 113.6(5) . 2_756 ?
N2 C11 H11A 108.9 . . ?
N2 C11 H11A 108.9 2_756 . ?
N2 C11 H11B 108.9 . . ?
N2 C11 H11B 108.9 2_756 . ?
H11A C11 H11B 107.7 . . ?
N4 C12 C13 123.9(3) . . ?
N4 C12 H12 118.1 . . ?
C13 C12 H12 118.1 . . ?
C12 C13 C16 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C16 C13 H13 119.5 . . ?
C15 C14 C16 120.6(4) . . ?
C15 C14 H14 119.7 . . ?
C16 C14 H14 119.7 . . ?
N4 C15 C14 123.8(4) . . ?
N4 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
C14 C16 C13 114.7(4) . . ?
C14 C16 C17 122.1(4) . . ?
C13 C16 C17 123.2(3) . . ?
C20 C17 C18 104.9(3) . . ?
C20 C17 C16 126.6(4) . . ?
C18 C17 C16 128.4(3) . . ?
N5 C18 C17 110.3(3) . . ?
N5 C18 C19 120.0(4) . . ?
C17 C18 C19 129.6(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C17 106.2(3) . . ?
N6 C20 C21 122.7(4) . . ?
C17 C20 C21 130.9(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 N6 112.2(4) . 2_556 ?
N6 C22 H22A 109.2 . . ?
N6 C22 H22A 109.2 2_556 . ?
N6 C22 H22B 109.2 . . ?
N6 C22 H22B 109.2 2_556 . ?
H22A C22 H22B 107.9 . . ?
O2 C26 C25 120.1(7) . . ?
O2 C26 H26A 107.3 . . ?
C25 C26 H26A 107.3 . . ?
O2 C26 H26B 107.3 . . ?
C25 C26 H26B 107.3 . . ?
H26A C26 H26B 106.9 . . ?
O1 C25 C26 120.6(7) . . ?
O1 C25 H25A 107.2 . . ?
C26 C25 H25A 107.2 . . ?
O1 C25 H25B 107.2 . . ?
C26 C25 H25B 107.2 . . ?
H25A C25 H25B 106.8 . . ?
C25 O1 H1A 109.5 . . ?
C26 O2 H2A 109.5 . . ?
N9 N7 C24 89(5) 5_667 5_667 ?
N9 N7 C23 74(4) 5_667 . ?
N9 N7 Zn1 90(4) 5_667 . ?
C24 N7 Zn1 161(2) 5_667 . ?
C23 N7 Zn1 158.5(15) . . ?
C24 C23 N9 75.3(17) 5_667 5_667 ?
C24 C23 N7 68.2(19) 5_667 . ?
N7 C23 N8 171(2) . . ?
N9 C23 N8 120(2) 5_667 5_667 ?
N7 C23 N8 112.6(15) . 5_667 ?
N8 C23 N8 73.4(11) . 5_667 ?
C23 N8 C23 106.6(11) . 5_667 ?
C24 N8 C24 108.3(12) . 5_667 ?
C23 N8 C24 85.9(9) 5_667 5_667 ?
C24 N8 N8 65.7(10) . 5_667 ?
C23 N8 N8 63.3(9) . 5_667 ?
N7 N9 C23 88(5) 5_667 5_667 ?
N7 N9 C24 73(4) 5_667 . ?
N7 N9 Zn1 81(4) 5_667 5_667 ?
C23 N9 Zn1 162(2) 5_667 5_667 ?
C24 N9 Zn1 148.5(15) . 5_667 ?
C23 C24 N7 75.7(17) 5_667 5_667 ?
C23 C24 N9 68.7(19) 5_667 . ?
C23 C24 N8 113(2) 5_667 . ?
N7 C24 N8 167.6(17) 5_667 . ?
N9 C24 N8 173.0(19) . . ?
N7 C24 N8 116.5(17) 5_667 5_667 ?
N9 C24 N8 109.1(16) . 5_667 ?
N8 C24 N8 71.7(12) . 5_667 ?

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
N1 Zn1 N1 C5 130.3(3) 2_656 . . . ?
N7 Zn1 N1 C5 44.3(5) . . . . ?
N7 Zn1 N1 C5 -141.7(8) 2_656 . . . ?
N4 Zn1 N1 C5 -49.3(3) 2_656 . . . ?
N9 Zn1 N1 C5 -137.3(8) 6_565 . . . ?
N9 Zn1 N1 C5 36.4(5) 5_667 . . . ?
N1 Zn1 N1 C1 -48.8(3) 2_656 . . . ?
N7 Zn1 N1 C1 -134.8(5) . . . . ?
N7 Zn1 N1 C1 39.2(8) 2_656 . . . ?
N4 Zn1 N1 C1 131.6(3) 2_656 . . . ?
N9 Zn1 N1 C1 43.6(8) 6_565 . . . ?
N9 Zn1 N1 C1 -142.7(5) 5_667 . . . ?
C9 N2 N3 C7 1.4(5) . . . . ?
C11 N2 N3 C7 -175.4(4) . . . . ?
N1 Zn1 N4 C12 125.2(3) 2_656 . . . ?
N7 Zn1 N4 C12 -148.8(5) . . . . ?
N7 Zn1 N4 C12 37.2(8) 2_656 . . . ?
N4 Zn1 N4 C12 -55.3(3) 2_656 . . . ?
N9 Zn1 N4 C12 32.8(8) 6_565 . . . ?
N9 Zn1 N4 C12 -140.9(5) 5_667 . . . ?
N1 Zn1 N4 C15 -53.7(3) 2_656 . . . ?
N7 Zn1 N4 C15 32.3(5) . . . . ?
N7 Zn1 N4 C15 -141.6(8) 2_656 . . . ?
N4 Zn1 N4 C15 125.9(3) 2_656 . . . ?
N9 Zn1 N4 C15 -146.1(8) 6_565 . . . ?
N9 Zn1 N4 C15 40.2(5) 5_667 . . . ?
C18 N5 N6 C22 178.1(4) . . . . ?
Zn1 N1 C1 C2 178.7(3) . . . . ?
N1 C1 C2 C3 0.9(6) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C3 C6 178.9(4) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C6 C3 C4 C5 -179.8(4) . . . . ?
C1 N1 C5 C4 -0.6(6) . . . . ?
Zn1 N1 C5 C4 -179.7(3) . . . . ?
C3 C4 C5 N1 1.0(7) . . . . ?
C4 C3 C6 C9 137.8(5) . . . . ?
C2 C3 C6 C9 -41.6(6) . . . . ?
C4 C3 C6 C7 -38.8(6) . . . . ?
C2 C3 C6 C7 141.8(4) . . . . ?
N2 N3 C7 C6 -1.0(5) . . . . ?
N2 N3 C7 C8 -177.7(5) . . . . ?
C9 C6 C7 N3 0.3(5) . . . . ?
C3 C6 C7 N3 177.5(4) . . . . ?
C9 C6 C7 C8 176.6(5) . . . . ?
C3 C6 C7 C8 -6.3(8) . . . . ?
N3 N2 C9 C6 -1.2(5) . . . . ?
C11 N2 C9 C6 175.2(4) . . . . ?
N3 N2 C9 C10 179.0(4) . . . . ?
C11 N2 C9 C10 -4.6(7) . . . . ?
C7 C6 C9 N2 0.5(5) . . . . ?
C3 C6 C9 N2 -176.6(4) . . . . ?
C7 C6 C9 C10 -179.7(5) . . . . ?
C3 C6 C9 C10 3.2(8) . . . . ?
C9 N2 C11 N2 -65.5(4) . . . 2_756 ?
N3 N2 C11 N2 110.8(4) . . . 2_756 ?
C15 N4 C12 C13 -0.9(6) . . . . ?
Zn1 N4 C12 C13 -179.8(3) . . . . ?
N4 C12 C13 C16 0.1(6) . . . . ?
C12 N4 C15 C14 0.3(6) . . . . ?
Zn1 N4 C15 C14 179.3(3) . . . . ?
C16 C14 C15 N4 1.0(7) . . . . ?
C15 C14 C16 C13 -1.6(6) . . . . ?
C15 C14 C16 C17 -179.6(4) . . . . ?
C12 C13 C16 C14 1.1(6) . . . . ?
C12 C13 C16 C17 179.1(4) . . . . ?
C14 C16 C17 C20 -36.8(6) . . . . ?
C13 C16 C17 C20 145.5(4) . . . . ?
C14 C16 C17 C18 139.7(4) . . . . ?
C13 C16 C17 C18 -38.1(6) . . . . ?
N6 N5 C18 C17 -1.0(5) . . . . ?
N6 N5 C18 C19 179.5(5) . . . . ?
C20 C17 C18 N5 1.0(5) . . . . ?
C16 C17 C18 N5 -176.0(4) . . . . ?
C20 C17 C18 C19 -179.6(5) . . . . ?
C16 C17 C18 C19 3.4(8) . . . . ?
N5 N6 C20 C17 -0.1(5) . . . . ?
C22 N6 C20 C17 -177.2(4) . . . . ?
N5 N6 C20 C21 -176.2(4) . . . . ?
C22 N6 C20 C21 6.7(7) . . . . ?
C18 C17 C20 N6 -0.5(4) . . . . ?
C16 C17 C20 N6 176.6(4) . . . . ?
C18 C17 C20 C21 175.1(5) . . . . ?
C16 C17 C20 C21 -7.8(8) . . . . ?
C20 N6 C22 N6 66.0(4) . . . 2_556 ?
N5 N6 C22 N6 -110.9(3) . . . 2_556 ?
O2 C26 C25 O1 19.9(16) . . . . ?
N1 Zn1 N7 N9 151(9) 2_656 . . 5_667 ?
N1 Zn1 N7 N9 -119(9) . . . 5_667 ?
N4 Zn1 N7 N9 61(9) . . . 5_667 ?
N4 Zn1 N7 N9 -29(9) 2_656 . . 5_667 ?
N1 Zn1 N7 C24 65(5) 2_656 . . 5_667 ?
N1 Zn1 N7 C24 155(5) . . . 5_667 ?
N4 Zn1 N7 C24 -25(5) . . . 5_667 ?
N4 Zn1 N7 C24 -115(5) 2_656 . . 5_667 ?
N9 Zn1 N7 C24 -86(11) 5_667 . . 5_667 ?
N1 Zn1 N7 C23 -168(6) 2_656 . . . ?
N1 Zn1 N7 C23 -78(6) . . . . ?
N4 Zn1 N7 C23 102(6) . . . . ?
N4 Zn1 N7 C23 12(6) 2_656 . . . ?
N9 Zn1 N7 C23 41(5) 5_667 . . . ?
N9 N7 C23 C24 -111(9) 5_667 . . 5_667 ?
Zn1 N7 C23 C24 -154(6) . . . 5_667 ?
C24 N7 C23 N9 111(9) 5_667 . . 5_667 ?
Zn1 N7 C23 N9 -43(5) . . . 5_667 ?
N9 N7 C23 N8 -118(8) 5_667 . . 5_667 ?
Zn1 N7 C23 N8 -161(5) . . . 5_667 ?
N9 C23 N8 C24 -146(6) 5_667 . . . ?
N8 C23 N8 C24 -1.5(14) 5_667 . . . ?
C24 C23 N8 C23 -2(2) 5_667 . . 5_667 ?
N9 C23 N8 C23 -144(7) 5_667 . . 5_667 ?
N9 C23 N8 C24 -142(8) 5_667 . . 5_667 ?
C24 C23 N8 N8 -2(2) 5_667 . . 5_667 ?
N9 C23 N8 N8 -144(7) 5_667 . . 5_667 ?
N7 N9 C24 C23 110(9) 5_667 . . 5_667 ?
Zn1 N9 C24 C23 148(4) 5_667 . . 5_667 ?
C23 N9 C24 N7 -110(9) 5_667 . . 5_667 ?
Zn1 N9 C24 N7 38(5) 5_667 . . 5_667 ?
N7 N9 C24 N8 118(8) 5_667 . . 5_667 ?
C23 N9 C24 N8 7.4(16) 5_667 . . 5_667 ?
Zn1 N9 C24 N8 155(3) 5_667 . . 5_667 ?
C23 N8 C24 C23 4(3) . . . 5_667 ?
C24 N8 C24 C23 2(2) 5_667 . . 5_667 ?
N8 N8 C24 C23 2(2) 5_667 . . 5_667 ?
C23 N8 C24 N7 134(8) . . . 5_667 ?
C23 N8 C24 N7 131(10) 5_667 . . 5_667 ?
C24 N8 C24 N7 133(9) 5_667 . . 5_667 ?
N8 N8 C24 N7 133(9) 5_667 . . 5_667 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.135

#===END

data_1.Ag
_database_code_depnum_ccdc_archive 'CCDC 692033'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H44 Ag3 N21'
_chemical_formula_weight         1238.65

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'
Ag Ag -0.8971 1.1015 '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           Triclinic
_symmetry_space_group_name_H-M   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2047(9)
_cell_length_b                   11.3457(9)
_cell_length_c                   11.5102(10)
_cell_angle_alpha                89.2990(10)
_cell_angle_beta                 77.7050(10)
_cell_angle_gamma                82.6040(10)
_cell_volume                     1291.09(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    2279
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.13

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_T_max  0.7895
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'Apex II 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            7066
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5834
_reflns_number_gt                4659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

One dca anion (N19, C47, N20, C48, and N21) was refined using the
pseudo-isotropic "ISOR" restraint, as the free refinement gave unrealistic
anisotropic displacement parameters.
;

_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)+(0.0929P)²+2.3930P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_number_reflns         5834
_refine_ls_number_parameters     658
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1643
_refine_ls_wR_factor_gt          0.1500
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
Ag1 Ag 0.77842(9) 0.63518(8) 0.20104(7) 0.0605(3) Uani 1 1 d . . .
Ag2 Ag 1.34678(11) 1.37948(11) -0.11460(9) 0.0805(4) Uani 1 1 d . . .
Ag3 Ag 0.27444(12) -0.16639(11) 0.46750(10) 0.0891(5) Uani 1 1 d . . .
N1 N 0.3723(14) 0.0073(11) 0.3932(11) 0.078(4) Uani 1 1 d . . .
N2 N 0.7499(9) 0.4164(8) 0.2084(8) 0.047(2) Uani 1 1 d . . .
N3 N 0.7528(9) 0.3641(8) 0.0999(7) 0.047(2) Uani 1 1 d . . .
N4 N 0.7418(10) 0.5153(9) -0.0470(8) 0.044(2) Uani 1 1 d . . .
N5 N 0.7013(11) 0.6160(9) 0.0240(9) 0.052(3) Uani 1 1 d . . .
N6 N 0.3673(12) 0.7626(11) -0.3854(10) 0.066(3) Uani 1 1 d . . .
N7 N 1.2241(13) 1.2312(10) -0.0147(11) 0.074(3) Uani 1 1 d . . .
N8 N 0.8229(8) 0.8991(7) 0.2968(8) 0.044(2) Uani 1 1 d . . .
N9 N 0.8221(9) 0.8462(8) 0.1924(8) 0.050(2) Uani 1 1 d . . .
N10 N 0.8395(9) 0.7469(8) 0.4432(8) 0.043(2) Uani 1 1 d . . .
N11 N 0.8677(10) 0.6470(9) 0.3739(8) 0.046(2) Uani 1 1 d . . .
N12 N 1.2277(12) 0.4767(10) 0.7562(9) 0.062(3) Uani 1 1 d . . .
N13 N 0.1663(12) -0.1854(11) 0.3304(10) 0.061(3) Uani 1 1 d . . .
N14 N 0.1805(11) -0.2661(10) 0.1297(9) 0.055(3) Uani 1 1 d . . .
N15 N 0.0524(11) -0.4248(10) 0.0850(9) 0.063(3) Uani 1 1 d . . .
N16 N 1.4152(11) 1.4409(11) 0.0369(11) 0.064(3) Uani 1 1 d . . .
N17 N 1.3902(11) 1.5180(11) 0.2392(10) 0.062(3) Uani 1 1 d . . .
N18 N 1.5034(11) 1.6785(10) 0.3019(9) 0.064(3) Uani 1 1 d . . .
N19 N 1.4625(19) 1.2342(17) -0.2737(17) 0.120(5) Uani 1 1 d U . .
N20 N 1.669(2) 1.114(2) -0.337(2) 0.141(7) Uani 1 1 d U . .
N21 N 1.889(3) 1.120(2) -0.274(3) 0.185(10) Uani 1 1 d U . .
C1 C 0.5501(16) 0.1304(13) 0.4004(14) 0.079(4) Uani 1 1 d . . .
H1 H 0.6132 0.1520 0.4410 0.095 Uiso 1 1 calc R . .
C2 C 0.4582(18) 0.0486(15) 0.4479(16) 0.093(5) Uani 1 1 d . . .
H2 H 0.4590 0.0220 0.5245 0.111 Uiso 1 1 calc R . .
C3 C 0.371(2) 0.0458(18) 0.2883(15) 0.106(6) Uani 1 1 d . . .
H3 H 0.3132 0.0162 0.2467 0.128 Uiso 1 1 calc R . .
C4 C 0.4510(19) 0.1295(16) 0.2330(15) 0.091(5) Uani 1 1 d . . .
H4 H 0.4441 0.1537 0.1568 0.109 Uiso 1 1 calc R . .
C5 C 0.5392(11) 0.1770(10) 0.2869(10) 0.047(3) Uani 1 1 d . . .
C6 C 0.6275(12) 0.2608(10) 0.2328(10) 0.049(3) Uani 1 1 d . . .
C7 C 0.6817(10) 0.2693(9) 0.1123(9) 0.042(2) Uani 1 1 d . . .
C8 C 0.6738(17) 0.1943(13) 0.0108(11) 0.072(4) Uani 1 1 d . . .
H8A H 0.5905 0.2188 -0.0141 0.108 Uiso 1 1 calc R . .
H8B H 0.6770 0.1127 0.0344 0.108 Uiso 1 1 calc R . .
H8C H 0.7486 0.2026 -0.0539 0.108 Uiso 1 1 calc R . .
C9 C 0.6735(11) 0.3539(9) 0.2884(10) 0.041(2) Uani 1 1 d . . .
C10 C 0.6432(15) 0.3918(12) 0.4139(11) 0.061(3) Uani 1 1 d . . .
H10A H 0.6839 0.4622 0.4216 0.091 Uiso 1 1 calc R . .
H10B H 0.6788 0.3296 0.4603 0.091 Uiso 1 1 calc R . .
H10C H 0.5470 0.4083 0.4419 0.091 Uiso 1 1 calc R . .
C11 C 0.8312(12) 0.4196(10) -0.0060(10) 0.050(3) Uani 1 1 d . . .
H11A H 0.9072 0.4514 0.0148 0.060 Uiso 1 1 calc R . .
H11B H 0.8661 0.3604 -0.0688 0.060 Uiso 1 1 calc R . .
C12 C 0.6859(12) 0.5218(12) -0.1450(10) 0.049(3) Uani 1 1 d . . .
C13 C 0.7118(16) 0.4244(13) -0.2318(12) 0.070(4) Uani 1 1 d . . .
H13A H 0.7658 0.4480 -0.3051 0.105 Uiso 1 1 calc R . .
H13B H 0.6274 0.4051 -0.2456 0.105 Uiso 1 1 calc R . .
H13C H 0.7592 0.3561 -0.2019 0.105 Uiso 1 1 calc R . .
C14 C 0.6048(11) 0.6323(10) -0.1354(10) 0.047(3) Uani 1 1 d . . .
C15 C 0.6197(11) 0.6861(10) -0.0304(9) 0.044(2) Uani 1 1 d . . .
C16 C 0.5558(15) 0.8022(11) 0.0204(12) 0.061(3) Uani 1 1 d . . .
H16A H 0.4618 0.7984 0.0538 0.091 Uiso 1 1 calc R . .
H16B H 0.5639 0.8607 -0.0408 0.091 Uiso 1 1 calc R . .
H16C H 0.5996 0.8237 0.0816 0.091 Uiso 1 1 calc R . .
C17 C 0.5223(12) 0.6779(10) -0.2201(10) 0.046(3) Uani 1 1 d . . .
C18 C 0.3951(14) 0.7371(12) -0.1819(12) 0.063(3) Uani 1 1 d . . .
H18 H 0.3581 0.7487 -0.1011 0.076 Uiso 1 1 calc R . .
C19 C 0.3204(14) 0.7805(12) -0.2682(11) 0.063(3) Uani 1 1 d . . .
H19 H 0.2352 0.8232 -0.2422 0.076 Uiso 1 1 calc R . .
C20 C 0.4934(15) 0.7048(13) -0.4197(11) 0.064(4) Uani 1 1 d . . .
H20 H 0.5294 0.6931 -0.5007 0.077 Uiso 1 1 calc R . .
C21 C 0.5715(14) 0.6622(12) -0.3411(11) 0.058(3) Uani 1 1 d . . .
H21 H 0.6579 0.6225 -0.3694 0.069 Uiso 1 1 calc R . .
C22 C 1.0312(14) 1.1943(10) 0.1325(11) 0.060(3) Uani 1 1 d . . .
H22 H 0.9605 1.2257 0.1935 0.072 Uiso 1 1 calc R . .
C23 C 1.1199(15) 1.2643(12) 0.0736(13) 0.071(4) Uani 1 1 d . . .
H23 H 1.1065 1.3438 0.0975 0.086 Uiso 1 1 calc R . .
C24 C 1.2441(18) 1.1131(13) -0.0409(15) 0.080(5) Uani 1 1 d . . .
H24 H 1.3200 1.0832 -0.0977 0.097 Uiso 1 1 calc R . .
C25 C 1.1553(16) 1.0333(12) 0.0142(14) 0.076(4) Uani 1 1 d . . .
H25 H 1.1700 0.9534 -0.0079 0.091 Uiso 1 1 calc R . .
C26 C 1.0462(11) 1.0775(9) 0.1016(9) 0.045(3) Uani 1 1 d . . .
C27 C 0.9503(10) 0.9962(9) 0.1628(10) 0.039(2) Uani 1 1 d . . .
C28 C 0.9023(13) 0.9055(12) 0.1091(11) 0.049(3) Uani 1 1 d . . .
C29 C 0.9168(16) 0.8727(12) -0.0185(11) 0.066(3) Uani 1 1 d . . .
H29A H 0.9558 0.7911 -0.0317 0.099 Uiso 1 1 calc R . .
H29B H 0.9744 0.9227 -0.0675 0.099 Uiso 1 1 calc R . .
H29C H 0.8294 0.8832 -0.0385 0.099 Uiso 1 1 calc R . .
C30 C 0.9011(11) 0.9876(9) 0.2829(10) 0.045(2) Uani 1 1 d . . .
C31 C 0.9296(15) 1.0537(13) 0.3844(12) 0.073(4) Uani 1 1 d . . .
H31A H 0.9747 0.9992 0.4321 0.109 Uiso 1 1 calc R . .
H31B H 0.8460 1.0910 0.4321 0.109 Uiso 1 1 calc R . .
H31C H 0.9863 1.1132 0.3541 0.109 Uiso 1 1 calc R . .
C32 C 0.7601(11) 0.8474(10) 0.4041(10) 0.050(3) Uani 1 1 d . . .
H32A H 0.6758 0.8228 0.3933 0.060 Uiso 1 1 calc R . .
H32B H 0.7379 0.9079 0.4665 0.060 Uiso 1 1 calc R . .
C33 C 0.9538(11) 0.5754(9) 0.4220(10) 0.046(3) Uani 1 1 d . . .
C34 C 1.0071(16) 0.4532(12) 0.3689(13) 0.069(4) Uani 1 1 d . . .
H34A H 0.9496 0.4315 0.3188 0.103 Uiso 1 1 calc R . .
H34B H 1.0085 0.3967 0.4315 0.103 Uiso 1 1 calc R . .
H34C H 1.0971 0.4537 0.3225 0.103 Uiso 1 1 calc R . .
C35 C 0.9781(11) 0.6273(11) 0.5243(9) 0.047(3) Uani 1 1 d . . .
C36 C 0.9026(14) 0.7367(11) 0.5343(11) 0.054(3) Uani 1 1 d . . .
C37 C 0.8892(19) 0.8346(13) 0.6247(13) 0.085(5) Uani 1 1 d . . .
H37A H 0.9125 0.9062 0.5848 0.128 Uiso 1 1 calc R . .
H37B H 0.9488 0.8121 0.6777 0.128 Uiso 1 1 calc R . .
H37C H 0.7976 0.8479 0.6694 0.128 Uiso 1 1 calc R . .
C38 C 1.0650(12) 0.5750(11) 0.6052(10) 0.050(3) Uani 1 1 d . . .
C39 C 1.1943(11) 0.5141(13) 0.5598(10) 0.057(3) Uani 1 1 d . . .
H39 H 1.2294 0.5057 0.4784 0.068 Uiso 1 1 calc R . .
C40 C 1.2651(13) 0.4685(14) 0.6396(12) 0.071(4) Uani 1 1 d . . .
H40 H 1.3498 0.4266 0.6090 0.085 Uiso 1 1 calc R . .
C41 C 1.1112(16) 0.5372(14) 0.7948(11) 0.070(4) Uani 1 1 d . . .
H41 H 1.0829 0.5467 0.8769 0.083 Uiso 1 1 calc R . .
C42 C 1.0243(14) 0.5890(12) 0.7272(10) 0.056(3) Uani 1 1 d . . .
H42 H 0.9415 0.6317 0.7620 0.067 Uiso 1 1 calc R . .
C43 C 0.1709(11) -0.2272(10) 0.2429(12) 0.048(3) Uani 1 1 d . . .
C44 C 0.1101(13) -0.3523(12) 0.1111(10) 0.051(3) Uani 1 1 d . . .
C45 C 1.4087(11) 1.4804(11) 0.1325(12) 0.047(3) Uani 1 1 d . . .
C46 C 1.4536(13) 1.6030(12) 0.2687(10) 0.052(3) Uani 1 1 d . . .
C47 C 1.561(2) 1.1806(17) -0.2951(17) 0.093(5) Uani 1 1 d U . .
C48 C 1.775(3) 1.127(2) -0.312(2) 0.126(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
Ag1 N5 2.357(11) . ?
Ag1 N11 2.370(10) . ?
Ag1 N9 2.488(9) . ?
Ag1 N2 2.535(9) . ?
Ag2 N16 2.165(12) . ?
Ag2 N12 2.300(10) 1_564 ?
Ag2 N7 2.367(11) . ?
Ag2 N19 2.473(19) . ?
Ag3 N13 2.137(12) . ?
Ag3 N6 2.206(10) 1_546 ?
Ag3 N1 2.391(11) . ?
N1 C3 1.281(19) . ?
N1 C2 1.32(2) . ?
N2 C9 1.334(14) . ?
N2 N3 1.382(13) . ?
N3 C7 1.363(14) . ?
N3 C11 1.489(14) . ?
N4 C12 1.366(15) . ?
N4 N5 1.379(14) . ?
N4 C11 1.467(14) . ?
N5 C15 1.326(14) . ?
N6 C19 1.340(16) . ?
N6 C20 1.347(18) . ?
N6 Ag3 2.206(10) 1_564 ?
N7 C23 1.324(18) . ?
N7 C24 1.357(18) . ?
N8 C30 1.348(14) . ?
N8 N9 1.353(13) . ?
N8 C32 1.422(13) . ?
N9 C28 1.354(16) . ?
N10 C36 1.339(17) . ?
N10 N11 1.358(13) . ?
N10 C32 1.437(14) . ?
N11 C33 1.323(14) . ?
N12 C41 1.286(17) . ?
N12 C40 1.316(16) . ?
N12 Ag2 2.300(10) 1_546 ?
N13 C43 1.108(17) . ?
N14 C44 1.331(19) . ?
N14 C43 1.361(17) . ?
N15 C44 1.148(17) . ?
N16 C45 1.179(17) . ?
N17 C45 1.272(18) . ?
N17 C46 1.314(19) . ?
N18 C46 1.157(17) . ?
N19 C47 1.09(2) . ?
N20 C48 1.20(3) . ?
N20 C47 1.26(2) . ?
N21 C48 1.32(3) . ?
C1 C5 1.425(18) . ?
C1 C2 1.43(2) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.39(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.36(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.438(16) . ?
C6 C7 1.386(15) . ?
C6 C9 1.421(16) . ?
C7 C8 1.476(17) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.469(17) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.402(16) . ?
C12 C13 1.459(19) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.405(16) . ?
C14 C17 1.467(15) . ?
C15 C16 1.462(16) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.367(18) . ?
C17 C21 1.382(17) . ?
C18 C19 1.423(18) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.373(19) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.350(18) . ?
C22 C26 1.357(16) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.41(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.376(18) . ?
C25 H25 0.9300 . ?
C26 C27 1.493(15) . ?
C27 C30 1.373(15) . ?
C27 C28 1.398(17) . ?
C28 C29 1.491(18) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.495(16) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C35 1.405(16) . ?
C33 C34 1.509(17) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.367(17) . ?
C35 C38 1.486(16) . ?
C36 C37 1.504(17) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C42 1.381(16) . ?
C38 C39 1.405(17) . ?
C39 C40 1.344(17) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.374(19) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?

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
N5 Ag1 N11 176.6(4) . . ?
N5 Ag1 N9 101.4(3) . . ?
N11 Ag1 N9 79.8(3) . . ?
N5 Ag1 N2 80.1(3) . . ?
N11 Ag1 N2 98.5(3) . . ?
N9 Ag1 N2 176.4(3) . . ?
N16 Ag2 N12 132.2(5) . 1_564 ?
N16 Ag2 N7 97.0(5) . . ?
N12 Ag2 N7 109.5(5) 1_564 . ?
N16 Ag2 N19 130.0(6) . . ?
N12 Ag2 N19 90.0(5) 1_564 . ?
N7 Ag2 N19 90.1(5) . . ?
N13 Ag3 N6 152.0(4) . 1_546 ?
N13 Ag3 N1 97.4(4) . . ?
N6 Ag3 N1 109.0(4) 1_546 . ?
C3 N1 C2 116.4(13) . . ?
C3 N1 Ag3 122.5(11) . . ?
C2 N1 Ag3 119.0(9) . . ?
C9 N2 N3 105.0(9) . . ?
C9 N2 Ag1 131.5(7) . . ?
N3 N2 Ag1 115.1(6) . . ?
C7 N3 N2 111.8(8) . . ?
C7 N3 C11 132.5(9) . . ?
N2 N3 C11 115.7(9) . . ?
C12 N4 N5 112.0(9) . . ?
C12 N4 C11 130.7(10) . . ?
N5 N4 C11 117.3(9) . . ?
C15 N5 N4 105.4(10) . . ?
C15 N5 Ag1 133.5(8) . . ?
N4 N5 Ag1 121.1(7) . . ?
C19 N6 C20 116.7(11) . . ?
C19 N6 Ag3 128.3(9) . 1_564 ?
C20 N6 Ag3 114.7(8) . 1_564 ?
C23 N7 C24 114.3(13) . . ?
C23 N7 Ag2 118.4(9) . . ?
C24 N7 Ag2 127.2(10) . . ?
C30 N8 N9 112.5(9) . . ?
C30 N8 C32 128.5(10) . . ?
N9 N8 C32 118.4(9) . . ?
N8 N9 C28 104.8(10) . . ?
N8 N9 Ag1 116.6(6) . . ?
C28 N9 Ag1 131.3(8) . . ?
C36 N10 N11 111.9(9) . . ?
C36 N10 C32 130.4(10) . . ?
N11 N10 C32 117.5(9) . . ?
C33 N11 N10 104.8(9) . . ?
C33 N11 Ag1 133.9(8) . . ?
N10 N11 Ag1 121.2(7) . . ?
C41 N12 C40 114.5(11) . . ?
C41 N12 Ag2 120.9(8) . 1_546 ?
C40 N12 Ag2 124.4(9) . 1_546 ?
C43 N13 Ag3 145.0(11) . . ?
C44 N14 C43 119.1(11) . . ?
C45 N16 Ag2 158.7(10) . . ?
C45 N17 C46 122.2(11) . . ?
C47 N19 Ag2 135.0(18) . . ?
C48 N20 C47 123(2) . . ?
C5 C1 C2 115.8(14) . . ?
C5 C1 H1 122.1 . . ?
C2 C1 H1 122.1 . . ?
N1 C2 C1 125.9(14) . . ?
N1 C2 H2 117.0 . . ?
C1 C2 H2 117.0 . . ?
N1 C3 C4 123.8(15) . . ?
N1 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C5 C4 C3 122.1(14) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C1 115.7(12) . . ?
C4 C5 C6 124.6(11) . . ?
C1 C5 C6 119.4(11) . . ?
C7 C6 C9 105.5(10) . . ?
C7 C6 C5 126.1(11) . . ?
C9 C6 C5 128.4(11) . . ?
N3 C7 C6 106.6(10) . . ?
N3 C7 C8 122.8(10) . . ?
C6 C7 C8 130.6(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 111.1(10) . . ?
N2 C9 C10 118.8(10) . . ?
C6 C9 C10 130.0(11) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N3 108.8(8) . . ?
N4 C11 H11A 109.9 . . ?
N3 C11 H11A 109.9 . . ?
N4 C11 H11B 109.9 . . ?
N3 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N4 C12 C14 105.4(10) . . ?
N4 C12 C13 121.8(12) . . ?
C14 C12 C13 132.8(12) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 106.0(10) . . ?
C12 C14 C17 125.1(11) . . ?
C15 C14 C17 128.9(10) . . ?
N5 C15 C14 111.3(10) . . ?
N5 C15 C16 120.9(10) . . ?
C14 C15 C16 127.9(10) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C21 118.1(11) . . ?
C18 C17 C14 121.2(11) . . ?
C21 C17 C14 120.7(11) . . ?
C17 C18 C19 118.7(12) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N6 C19 C18 123.0(12) . . ?
N6 C19 H19 118.5 . . ?
C18 C19 H19 118.5 . . ?
N6 C20 C21 123.2(12) . . ?
N6 C20 H20 118.4 . . ?
C21 C20 H20 118.4 . . ?
C20 C21 C17 120.3(12) . . ?
C20 C21 H21 119.8 . . ?
C17 C21 H21 119.8 . . ?
C23 C22 C26 119.3(12) . . ?
C23 C22 H22 120.4 . . ?
C26 C22 H22 120.4 . . ?
N7 C23 C22 126.4(13) . . ?
N7 C23 H23 116.8 . . ?
C22 C23 H23 116.8 . . ?
N7 C24 C25 123.1(14) . . ?
N7 C24 H24 118.4 . . ?
C25 C24 H24 118.4 . . ?
C26 C25 C24 118.0(13) . . ?
C26 C25 H25 121.0 . . ?
C24 C25 H25 121.0 . . ?
C22 C26 C25 118.6(12) . . ?
C22 C26 C27 121.6(10) . . ?
C25 C26 C27 119.8(10) . . ?
C30 C27 C28 106.0(10) . . ?
C30 C27 C26 127.4(10) . . ?
C28 C27 C26 126.3(10) . . ?
N9 C28 C27 110.2(10) . . ?
N9 C28 C29 118.3(12) . . ?
C27 C28 C29 131.3(12) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N8 C30 C27 106.5(10) . . ?
N8 C30 C31 123.5(10) . . ?
C27 C30 C31 129.9(11) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 N10 115.2(8) . . ?
N8 C32 H32A 108.5 . . ?
N10 C32 H32A 108.5 . . ?
N8 C32 H32B 108.5 . . ?
N10 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
N11 C33 C35 111.2(9) . . ?
N11 C33 C34 120.0(11) . . ?
C35 C33 C34 128.7(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C33 104.8(10) . . ?
C36 C35 C38 127.3(11) . . ?
C33 C35 C38 128.0(11) . . ?
N10 C36 C35 107.3(10) . . ?
N10 C36 C37 122.9(11) . . ?
C35 C36 C37 129.8(13) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C38 C39 117.6(11) . . ?
C42 C38 C35 121.4(11) . . ?
C39 C38 C35 121.0(10) . . ?
C40 C39 C38 116.8(11) . . ?
C40 C39 H39 121.6 . . ?
C38 C39 H39 121.6 . . ?
N12 C40 C39 127.1(13) . . ?
N12 C40 H40 116.4 . . ?
C39 C40 H40 116.4 . . ?
N12 C41 C42 126.6(12) . . ?
N12 C41 H41 116.7 . . ?
C42 C41 H41 116.7 . . ?
C41 C42 C38 117.2(12) . . ?
C41 C42 H42 121.4 . . ?
C38 C42 H42 121.4 . . ?
N13 C43 N14 173.2(14) . . ?
N15 C44 N14 174.2(13) . . ?
N16 C45 N17 173.9(14) . . ?
N18 C46 N17 175.4(13) . . ?
N19 C47 N20 170(3) . . ?
N20 C48 N21 168(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.900
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.111

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 692034'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 Cd N14 S2'
_chemical_formula_weight         945.45

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'
S S 0.1246 0.1234 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   16.546(4)
_cell_length_b                   24.142(5)
_cell_length_c                   25.043(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10004(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3751
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      20.22

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3888
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8534
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'Apex II 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            52218
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.03
_reflns_number_total             8834
_reflns_number_gt                4298
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the two disordered thiocyanate
anions in order to improve the refinement stability, which were also refined
using the pseudo-isotropic "ISOR" restraint, as the free refinement gave
unrealistic anisotropic displacement parameters.
;

_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)+(0.1158P)²+32.0150P] 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         8834
_refine_ls_number_parameters     593
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.2453
_refine_ls_wR_factor_gt          0.1776
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      1.003
_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
Cd1 Cd 0.38012(3) 0.49901(2) 0.770289(19) 0.0439(2) Uani 1 1 d . . .
N1 N 0.3070(4) 0.0498(2) 0.3346(3) 0.0491(16) Uani 1 1 d . . .
N2 N 0.1237(3) 0.2051(2) 0.5029(3) 0.0451(15) Uani 1 1 d . . .
N3 N 0.1601(4) 0.1729(3) 0.5401(2) 0.0475(15) Uani 1 1 d . . .
N4 N 0.1187(3) 0.2978(2) 0.5355(3) 0.0436(15) Uani 1 1 d . . .
N5 N 0.1463(4) 0.3319(3) 0.4965(3) 0.0520(16) Uani 1 1 d . . .
N6 N 0.3109(4) 0.4505(3) 0.7007(3) 0.0559(17) Uani 1 1 d . . .
N7 N 0.4466(4) 0.5512(3) 0.8359(3) 0.0531(17) Uani 1 1 d . . .
N8 N 0.6322(3) 0.7156(2) 0.9944(3) 0.0430(15) Uani 1 1 d . . .
N9 N 0.6053(4) 0.6822(3) 1.0349(3) 0.0493(16) Uani 1 1 d . . .
N10 N 0.6339(3) 0.8084(3) 1.0276(3) 0.0470(16) Uani 1 1 d . . .
N11 N 0.5930(4) 0.8396(3) 0.9906(3) 0.0493(16) Uani 1 1 d . . .
N12 N 0.4527(4) 0.9541(3) 1.2039(3) 0.0568(17) Uani 1 1 d . . .
N13 N 0.2773(4) 0.5643(3) 0.7701(3) 0.066(2) Uani 1 1 d D . .
N14 N 0.4799(4) 0.4316(3) 0.7742(3) 0.066(2) Uani 1 1 d D . .
C1 C 0.2672(5) 0.1359(3) 0.3731(3) 0.055(2) Uani 1 1 d . . .
H1 H 0.2672 0.1743 0.3707 0.066 Uiso 1 1 calc R . .
C2 C 0.3060(5) 0.1044(3) 0.3344(3) 0.057(2) Uani 1 1 d . . .
H2 H 0.3326 0.1228 0.3069 0.069 Uiso 1 1 calc R . .
C3 C 0.2685(5) 0.0251(3) 0.3743(3) 0.057(2) Uani 1 1 d . . .
H3 H 0.2679 -0.0135 0.3750 0.068 Uiso 1 1 calc R . .
C4 C 0.2293(5) 0.0529(3) 0.4146(3) 0.055(2) Uani 1 1 d . . .
H4 H 0.2030 0.0335 0.4415 0.066 Uiso 1 1 calc R . .
C5 C 0.2293(4) 0.1103(3) 0.4145(3) 0.0433(18) Uani 1 1 d . . .
C6 C 0.1907(4) 0.1427(3) 0.4571(3) 0.0427(18) Uani 1 1 d . . .
C7 C 0.2000(4) 0.1342(3) 0.5132(3) 0.0458(18) Uani 1 1 d . . .
C8 C 0.2448(5) 0.0901(3) 0.5431(4) 0.062(2) Uani 1 1 d . . .
H8A H 0.2578 0.1033 0.5782 0.093 Uiso 1 1 calc R . .
H8B H 0.2937 0.0812 0.5244 0.093 Uiso 1 1 calc R . .
H8C H 0.2117 0.0576 0.5458 0.093 Uiso 1 1 calc R . .
C9 C 0.1412(4) 0.1882(3) 0.4525(3) 0.0476(19) Uani 1 1 d . . .
C10 C 0.1064(6) 0.2166(4) 0.4055(4) 0.073(3) Uani 1 1 d . . .
H10A H 0.0486 0.2175 0.4087 0.110 Uiso 1 1 calc R . .
H10B H 0.1212 0.1968 0.3737 0.110 Uiso 1 1 calc R . .
H10C H 0.1269 0.2537 0.4037 0.110 Uiso 1 1 calc R . .
C11 C 0.0721(4) 0.2493(3) 0.5203(3) 0.052(2) Uani 1 1 d . . .
H11A H 0.0403 0.2370 0.5506 0.062 Uiso 1 1 calc R . .
H11B H 0.0352 0.2591 0.4918 0.062 Uiso 1 1 calc R . .
C12 C 0.1432(5) 0.3135(3) 0.5846(3) 0.0473(18) Uani 1 1 d . . .
C13 C 0.1210(6) 0.2828(4) 0.6333(4) 0.081(3) Uani 1 1 d . . .
H13A H 0.0633 0.2809 0.6361 0.122 Uiso 1 1 calc R . .
H13B H 0.1426 0.3015 0.6640 0.122 Uiso 1 1 calc R . .
H13C H 0.1429 0.2460 0.6315 0.122 Uiso 1 1 calc R . .
C14 C 0.1890(4) 0.3607(3) 0.5779(3) 0.0461(18) Uani 1 1 d . . .
C15 C 0.1886(4) 0.3701(3) 0.5221(3) 0.0477(19) Uani 1 1 d . . .
C16 C 0.2258(5) 0.4169(3) 0.4917(4) 0.065(2) Uani 1 1 d . . .
H16A H 0.1962 0.4228 0.4592 0.098 Uiso 1 1 calc R . .
H16B H 0.2809 0.4081 0.4833 0.098 Uiso 1 1 calc R . .
H16C H 0.2241 0.4500 0.5130 0.098 Uiso 1 1 calc R . .
C17 C 0.2304(5) 0.3928(3) 0.6197(3) 0.0483(19) Uani 1 1 d . . .
C18 C 0.3132(5) 0.4002(3) 0.6186(3) 0.058(2) Uani 1 1 d . . .
H18 H 0.3436 0.3859 0.5906 0.069 Uiso 1 1 calc R . .
C19 C 0.3503(5) 0.4288(4) 0.6590(4) 0.066(2) Uani 1 1 d . . .
H19 H 0.4061 0.4334 0.6574 0.079 Uiso 1 1 calc R . .
C20 C 0.2316(5) 0.4432(4) 0.7020(4) 0.066(2) Uani 1 1 d . . .
H20 H 0.2027 0.4580 0.7305 0.079 Uiso 1 1 calc R . .
C21 C 0.1897(5) 0.4146(4) 0.6629(4) 0.064(2) Uani 1 1 d . . .
H21 H 0.1341 0.4100 0.6658 0.077 Uiso 1 1 calc R . .
C22 C 0.4762(5) 0.6385(3) 0.8748(4) 0.067(3) Uani 1 1 d . . .
H22 H 0.4689 0.6767 0.8736 0.080 Uiso 1 1 calc R . .
C23 C 0.4394(6) 0.6053(4) 0.8371(4) 0.070(3) Uani 1 1 d . . .
H23 H 0.4078 0.6222 0.8110 0.084 Uiso 1 1 calc R . .
C24 C 0.4938(5) 0.5285(3) 0.8735(3) 0.057(2) Uani 1 1 d . . .
H24 H 0.5017 0.4904 0.8729 0.069 Uiso 1 1 calc R . .
C25 C 0.5312(5) 0.5589(3) 0.9131(3) 0.059(2) Uani 1 1 d . . .
H25 H 0.5617 0.5410 0.9391 0.071 Uiso 1 1 calc R . .
C26 C 0.5234(4) 0.6156(3) 0.9140(3) 0.0491(19) Uani 1 1 d . . .
C27 C 0.5634(4) 0.6506(3) 0.9544(3) 0.0471(19) Uani 1 1 d . . .
C28 C 0.5646(4) 0.6423(3) 1.0108(3) 0.0485(19) Uani 1 1 d . . .
C29 C 0.5285(5) 0.5971(3) 1.0442(3) 0.065(2) Uani 1 1 d . . .
H29A H 0.5615 0.5645 1.0417 0.097 Uiso 1 1 calc R . .
H29B H 0.4750 0.5890 1.0315 0.097 Uiso 1 1 calc R . .
H29C H 0.5257 0.6090 1.0807 0.097 Uiso 1 1 calc R . .
C30 C 0.6070(4) 0.6987(3) 0.9457(3) 0.0449(18) Uani 1 1 d . . .
C31 C 0.6306(5) 0.7267(3) 0.8957(3) 0.064(2) Uani 1 1 d . . .
H31A H 0.6101 0.7639 0.8957 0.097 Uiso 1 1 calc R . .
H31B H 0.6086 0.7069 0.8658 0.097 Uiso 1 1 calc R . .
H31C H 0.6885 0.7275 0.8930 0.097 Uiso 1 1 calc R . .
C32 C 0.6820(4) 0.7626(3) 1.0079(3) 0.053(2) Uani 1 1 d . . .
H32A H 0.7117 0.7744 0.9765 0.063 Uiso 1 1 calc R . .
H32B H 0.7208 0.7518 1.0350 0.063 Uiso 1 1 calc R . .
C33 C 0.6205(4) 0.8249(3) 1.0787(3) 0.051(2) Uani 1 1 d . . .
C34 C 0.6574(7) 0.7977(4) 1.1251(4) 0.091(3) Uani 1 1 d . . .
H34A H 0.6376 0.7604 1.1279 0.136 Uiso 1 1 calc R . .
H34B H 0.6438 0.8178 1.1570 0.136 Uiso 1 1 calc R . .
H34C H 0.7151 0.7970 1.1209 0.136 Uiso 1 1 calc R . .
C35 C 0.5680(4) 0.8687(3) 1.0755(3) 0.0460(18) Uani 1 1 d . . .
C36 C 0.5528(4) 0.8759(3) 1.0204(3) 0.0470(19) Uani 1 1 d . . .
C37 C 0.5043(5) 0.9200(3) 0.9928(4) 0.067(3) Uani 1 1 d . . .
H37A H 0.5238 0.9246 0.9570 0.101 Uiso 1 1 d R . .
H37B H 0.5098 0.9543 1.0119 0.101 Uiso 1 1 d R . .
H37C H 0.4484 0.9094 0.9919 0.101 Uiso 1 1 d R . .
C38 C 0.5294(5) 0.8991(3) 1.1195(3) 0.051(2) Uani 1 1 d . . .
C39 C 0.5728(5) 0.9238(4) 1.1600(4) 0.070(3) Uani 1 1 d . . .
H39 H 0.6289 0.9223 1.1600 0.084 Uiso 1 1 calc R . .
C40 C 0.5322(5) 0.9510(4) 1.2011(4) 0.068(3) Uani 1 1 d . . .
H40 H 0.5626 0.9677 1.2278 0.082 Uiso 1 1 calc R . .
C41 C 0.4105(5) 0.9304(4) 1.1639(4) 0.071(3) Uani 1 1 d . . .
H41 H 0.3544 0.9326 1.1645 0.085 Uiso 1 1 calc R . .
C42 C 0.4475(5) 0.9030(4) 1.1221(3) 0.065(2) Uani 1 1 d . . .
H42 H 0.4160 0.8870 1.0955 0.078 Uiso 1 1 calc R . .
S1 S 0.1860(7) 0.6376(4) 0.7139(5) 0.162(4) Uani 0.50 1 d PDU A 1
C43 C 0.2435(15) 0.5972(9) 0.7486(10) 0.076(9) Uani 0.50 1 d PDU A 1
S1' S 0.1699(4) 0.6069(3) 0.6973(3) 0.096(2) Uani 0.50 1 d PDU A 2
C43' C 0.2324(10) 0.5815(8) 0.7409(7) 0.044(5) Uani 0.50 1 d PDU A 2
S2 S 0.5830(4) 0.3927(3) 0.6978(3) 0.103(2) Uani 0.50 1 d PDU A 3
C44 C 0.5227(11) 0.4176(9) 0.7427(7) 0.056(6) Uani 0.50 1 d PDU A 3
S2' S 0.5723(8) 0.3593(5) 0.7184(5) 0.208(6) Uani 0.50 1 d PDU A 4
C44' C 0.5134(14) 0.3997(9) 0.7519(9) 0.073(8) Uani 0.50 1 d PDU A 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N13 2.320(6) . ?
Cd1 N14 2.321(6) . ?
Cd1 N1 2.333(6) 8_566 ?
Cd1 N12 2.343(6) 8_575 ?
Cd1 N7 2.345(6) . ?
Cd1 N6 2.391(6) . ?
N1 C2 1.320(9) . ?
N1 C3 1.323(9) . ?
N1 Cd1 2.333(6) 8_565 ?
N2 N3 1.354(8) . ?
N2 C9 1.357(10) . ?
N2 C11 1.435(8) . ?
N3 C7 1.327(9) . ?
N4 C12 1.349(9) . ?
N4 N5 1.357(9) . ?
N4 C11 1.450(9) . ?
N5 C15 1.322(9) . ?
N6 C20 1.325(10) . ?
N6 C19 1.338(10) . ?
N7 C23 1.313(9) . ?
N7 C24 1.339(10) . ?
N8 C30 1.351(9) . ?
N8 N9 1.369(8) . ?
N8 C32 1.443(9) . ?
N9 C28 1.321(9) . ?
N10 C33 1.359(10) . ?
N10 N11 1.373(9) . ?
N10 C32 1.447(9) . ?
N11 C36 1.330(9) . ?
N12 C40 1.320(10) . ?
N12 C41 1.347(10) . ?
N12 Cd1 2.343(6) 8_576 ?
N13 C43 1.110(8) . ?
N13 C43' 1.120(8) . ?
N14 C44' 1.100(8) . ?
N14 C44 1.113(8) . ?
C1 C5 1.360(10) . ?
C1 C2 1.388(11) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.375(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.468(10) . ?
C6 C9 1.376(10) . ?
C6 C7 1.429(11) . ?
C7 C8 1.497(11) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.478(11) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.379(10) . ?
C12 C13 1.474(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.414(11) . ?
C14 C17 1.472(10) . ?
C15 C16 1.496(11) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.378(11) . ?
C17 C18 1.383(10) . ?
C18 C19 1.370(11) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.386(11) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C26 1.372(11) . ?
C22 C23 1.380(11) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.380(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.375(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.474(10) . ?
C27 C30 1.385(10) . ?
C27 C28 1.428(11) . ?
C28 C29 1.498(11) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.476(11) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C35 1.371(10) . ?
C33 C34 1.470(12) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.412(11) . ?
C35 C38 1.470(10) . ?
C36 C37 1.502(11) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C42 1.361(10) . ?
C38 C39 1.378(11) . ?
C39 C40 1.392(11) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.382(11) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
S1 C43 1.616(8) . ?
S1' C43' 1.624(8) . ?
S2 C44 1.618(8) . ?
S2' C44' 1.614(8) . ?

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
N13 Cd1 N14 177.1(2) . . ?
N13 Cd1 N1 88.0(2) . 8_566 ?
N14 Cd1 N1 89.2(2) . 8_566 ?
N13 Cd1 N12 92.6(2) . 8_575 ?
N14 Cd1 N12 90.3(2) . 8_575 ?
N1 Cd1 N12 178.3(2) 8_566 8_575 ?
N13 Cd1 N7 88.9(2) . . ?
N14 Cd1 N7 90.8(2) . . ?
N1 Cd1 N7 91.8(2) 8_566 . ?
N12 Cd1 N7 89.9(2) 8_575 . ?
N13 Cd1 N6 88.8(2) . . ?
N14 Cd1 N6 91.6(2) . . ?
N1 Cd1 N6 90.4(2) 8_566 . ?
N12 Cd1 N6 88.0(2) 8_575 . ?
N7 Cd1 N6 176.8(2) . . ?
C2 N1 C3 116.6(7) . . ?
C2 N1 Cd1 120.6(5) . 8_565 ?
C3 N1 Cd1 122.8(5) . 8_565 ?
N3 N2 C9 111.8(6) . . ?
N3 N2 C11 118.9(6) . . ?
C9 N2 C11 129.2(7) . . ?
C7 N3 N2 106.1(6) . . ?
C12 N4 N5 112.4(6) . . ?
C12 N4 C11 128.7(7) . . ?
N5 N4 C11 118.8(6) . . ?
C15 N5 N4 104.7(6) . . ?
C20 N6 C19 116.8(7) . . ?
C20 N6 Cd1 121.4(5) . . ?
C19 N6 Cd1 121.8(5) . . ?
C23 N7 C24 116.4(7) . . ?
C23 N7 Cd1 120.4(6) . . ?
C24 N7 Cd1 123.1(5) . . ?
C30 N8 N9 113.0(6) . . ?
C30 N8 C32 128.6(7) . . ?
N9 N8 C32 118.4(6) . . ?
C28 N9 N8 104.9(6) . . ?
C33 N10 N11 113.2(6) . . ?
C33 N10 C32 129.4(7) . . ?
N11 N10 C32 117.4(6) . . ?
C36 N11 N10 103.3(6) . . ?
C40 N12 C41 116.9(7) . . ?
C40 N12 Cd1 125.2(5) . 8_576 ?
C41 N12 Cd1 117.8(5) . 8_576 ?
C43 N13 Cd1 149.0(17) . . ?
C43' N13 Cd1 137.6(13) . . ?
C44' N14 Cd1 145.8(16) . . ?
C44 N14 Cd1 129.5(14) . . ?
C5 C1 C2 119.9(7) . . ?
C5 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
N1 C2 C1 123.4(8) . . ?
N1 C2 H2 118.3 . . ?
C1 C2 H2 118.3 . . ?
N1 C3 C4 123.9(7) . . ?
N1 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
C3 C4 C5 119.2(7) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C1 C5 C4 117.0(7) . . ?
C1 C5 C6 120.8(7) . . ?
C4 C5 C6 122.2(7) . . ?
C9 C6 C7 105.1(7) . . ?
C9 C6 C5 128.7(7) . . ?
C7 C6 C5 126.1(7) . . ?
N3 C7 C6 110.1(7) . . ?
N3 C7 C8 119.5(7) . . ?
C6 C7 C8 130.4(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 106.8(7) . . ?
N2 C9 C10 121.3(7) . . ?
C6 C9 C10 131.8(7) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N4 111.3(6) . . ?
N2 C11 H11A 109.4 . . ?
N4 C11 H11A 109.4 . . ?
N2 C11 H11B 109.4 . . ?
N4 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N4 C12 C14 106.7(7) . . ?
N4 C12 C13 122.5(7) . . ?
C14 C12 C13 130.8(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 104.5(7) . . ?
C12 C14 C17 127.2(7) . . ?
C15 C14 C17 128.3(7) . . ?
N5 C15 C14 111.7(7) . . ?
N5 C15 C16 119.8(8) . . ?
C14 C15 C16 128.5(7) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 116.7(7) . . ?
C21 C17 C14 122.2(7) . . ?
C18 C17 C14 121.0(7) . . ?
C19 C18 C17 119.7(8) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
N6 C19 C18 123.7(8) . . ?
N6 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
N6 C20 C21 123.0(8) . . ?
N6 C20 H20 118.5 . . ?
C21 C20 H20 118.5 . . ?
C17 C21 C20 120.1(8) . . ?
C17 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C26 C22 C23 120.5(8) . . ?
C26 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
N7 C23 C22 123.5(8) . . ?
N7 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N7 C24 C25 123.3(8) . . ?
N7 C24 H24 118.3 . . ?
C25 C24 H24 118.3 . . ?
C26 C25 C24 119.9(8) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C22 C26 C25 116.3(7) . . ?
C22 C26 C27 121.0(7) . . ?
C25 C26 C27 122.7(7) . . ?
C30 C27 C28 105.4(7) . . ?
C30 C27 C26 127.4(7) . . ?
C28 C27 C26 127.2(7) . . ?
N9 C28 C27 110.9(7) . . ?
N9 C28 C29 118.7(8) . . ?
C27 C28 C29 130.5(7) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N8 C30 C27 105.8(7) . . ?
N8 C30 C31 123.1(7) . . ?
C27 C30 C31 130.9(7) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 N10 111.5(6) . . ?
N8 C32 H32A 109.3 . . ?
N10 C32 H32A 109.3 . . ?
N8 C32 H32B 109.3 . . ?
N10 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
N10 C33 C35 106.0(7) . . ?
N10 C33 C34 123.1(7) . . ?
C35 C33 C34 130.9(8) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 C36 105.3(7) . . ?
C33 C35 C38 128.0(7) . . ?
C36 C35 C38 126.5(7) . . ?
N11 C36 C35 112.3(7) . . ?
N11 C36 C37 118.5(7) . . ?
C35 C36 C37 129.1(7) . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.7 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C38 C39 116.9(7) . . ?
C42 C38 C35 120.2(7) . . ?
C39 C38 C35 122.8(7) . . ?
C38 C39 C40 119.8(8) . . ?
C38 C39 H39 120.1 . . ?
C40 C39 H39 120.1 . . ?
N12 C40 C39 123.2(8) . . ?
N12 C40 H40 118.4 . . ?
C39 C40 H40 118.4 . . ?
N12 C41 C42 122.4(8) . . ?
N12 C41 H41 118.8 . . ?
C42 C41 H41 118.8 . . ?
C38 C42 C41 120.7(8) . . ?
C38 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
N13 C43 S1 171(3) . . ?
N13 C43' S1' 178.1(19) . . ?
N14 C44 S2 176(2) . . ?
N14 C44' S2' 172(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N2 N3 C7 -1.3(8) . . . . ?
C11 N2 N3 C7 176.8(6) . . . . ?
C12 N4 N5 C15 -0.5(8) . . . . ?
C11 N4 N5 C15 -177.4(6) . . . . ?
N13 Cd1 N6 C20 -42.8(7) . . . . ?
N14 Cd1 N6 C20 134.3(7) . . . . ?
N1 Cd1 N6 C20 45.2(7) 8_566 . . . ?
N12 Cd1 N6 C20 -135.4(7) 8_575 . . . ?
N13 Cd1 N6 C19 138.1(7) . . . . ?
N14 Cd1 N6 C19 -44.8(7) . . . . ?
N1 Cd1 N6 C19 -134.0(7) 8_566 . . . ?
N12 Cd1 N6 C19 45.4(7) 8_575 . . . ?
N13 Cd1 N7 C23 -31.6(7) . . . . ?
N14 Cd1 N7 C23 151.3(7) . . . . ?
N1 Cd1 N7 C23 -119.5(7) 8_566 . . . ?
N12 Cd1 N7 C23 61.0(7) 8_575 . . . ?
N13 Cd1 N7 C24 148.9(6) . . . . ?
N14 Cd1 N7 C24 -28.2(6) . . . . ?
N1 Cd1 N7 C24 61.0(6) 8_566 . . . ?
N12 Cd1 N7 C24 -118.5(6) 8_575 . . . ?
C30 N8 N9 C28 2.3(8) . . . . ?
C32 N8 N9 C28 -177.7(6) . . . . ?
C33 N10 N11 C36 -0.6(8) . . . . ?
C32 N10 N11 C36 177.5(6) . . . . ?
N1 Cd1 N13 C43 -155(3) 8_566 . . . ?
N12 Cd1 N13 C43 24(3) 8_575 . . . ?
N7 Cd1 N13 C43 114(3) . . . . ?
N6 Cd1 N13 C43 -64(3) . . . . ?
N1 Cd1 N13 C43' -118.3(18) 8_566 . . . ?
N12 Cd1 N13 C43' 60.0(18) 8_575 . . . ?
N7 Cd1 N13 C43' 149.9(18) . . . . ?
N6 Cd1 N13 C43' -27.9(18) . . . . ?
N1 Cd1 N14 C44 151.2(17) 8_566 . . . ?
N12 Cd1 N14 C44 -27.2(17) 8_575 . . . ?
N7 Cd1 N14 C44 -117.1(17) . . . . ?
N6 Cd1 N14 C44 60.8(17) . . . . ?
C3 N1 C2 C1 0.0(12) . . . . ?
Cd1 N1 C2 C1 -176.5(6) 8_565 . . . ?
C5 C1 C2 N1 1.5(13) . . . . ?
C2 N1 C3 C4 -0.7(12) . . . . ?
Cd1 N1 C3 C4 175.7(6) 8_565 . . . ?
N1 C3 C4 C5 -0.1(13) . . . . ?
C2 C1 C5 C4 -2.3(12) . . . . ?
C2 C1 C5 C6 177.6(7) . . . . ?
C3 C4 C5 C1 1.6(12) . . . . ?
C3 C4 C5 C6 -178.2(7) . . . . ?
C1 C5 C6 C9 45.4(11) . . . . ?
C4 C5 C6 C9 -134.8(9) . . . . ?
C1 C5 C6 C7 -132.0(8) . . . . ?
C4 C5 C6 C7 47.8(11) . . . . ?
N2 N3 C7 C6 1.6(8) . . . . ?
N2 N3 C7 C8 -177.8(6) . . . . ?
C9 C6 C7 N3 -1.4(8) . . . . ?
C5 C6 C7 N3 176.6(6) . . . . ?
C9 C6 C7 C8 177.9(7) . . . . ?
C5 C6 C7 C8 -4.2(13) . . . . ?
N3 N2 C9 C6 0.4(8) . . . . ?
C11 N2 C9 C6 -177.4(6) . . . . ?
N3 N2 C9 C10 178.5(7) . . . . ?
C11 N2 C9 C10 0.7(12) . . . . ?
C7 C6 C9 N2 0.5(8) . . . . ?
C5 C6 C9 N2 -177.3(7) . . . . ?
C7 C6 C9 C10 -177.3(9) . . . . ?
C5 C6 C9 C10 4.9(14) . . . . ?
N3 N2 C11 N4 81.0(8) . . . . ?
C9 N2 C11 N4 -101.3(9) . . . . ?
C12 N4 C11 N2 -96.4(9) . . . . ?
N5 N4 C11 N2 80.0(8) . . . . ?
N5 N4 C12 C14 0.4(9) . . . . ?
C11 N4 C12 C14 176.9(6) . . . . ?
N5 N4 C12 C13 -179.8(8) . . . . ?
C11 N4 C12 C13 -3.2(12) . . . . ?
N4 C12 C14 C15 -0.1(8) . . . . ?
C13 C12 C14 C15 -179.9(9) . . . . ?
N4 C12 C14 C17 -178.8(7) . . . . ?
C13 C12 C14 C17 1.4(14) . . . . ?
N4 N5 C15 C14 0.4(8) . . . . ?
N4 N5 C15 C16 -177.3(7) . . . . ?
C12 C14 C15 N5 -0.2(9) . . . . ?
C17 C14 C15 N5 178.5(7) . . . . ?
C12 C14 C15 C16 177.2(8) . . . . ?
C17 C14 C15 C16 -4.1(13) . . . . ?
C12 C14 C17 C21 -56.6(12) . . . . ?
C15 C14 C17 C21 125.0(9) . . . . ?
C12 C14 C17 C18 120.2(9) . . . . ?
C15 C14 C17 C18 -58.2(12) . . . . ?
C21 C17 C18 C19 -1.0(13) . . . . ?
C14 C17 C18 C19 -177.9(8) . . . . ?
C20 N6 C19 C18 0.1(13) . . . . ?
Cd1 N6 C19 C18 179.3(7) . . . . ?
C17 C18 C19 N6 0.3(14) . . . . ?
C19 N6 C20 C21 0.2(13) . . . . ?
Cd1 N6 C20 C21 -178.9(7) . . . . ?
C18 C17 C21 C20 1.3(13) . . . . ?
C14 C17 C21 C20 178.2(8) . . . . ?
N6 C20 C21 C17 -1.0(15) . . . . ?
C24 N7 C23 C22 -1.1(14) . . . . ?
Cd1 N7 C23 C22 179.4(7) . . . . ?
C26 C22 C23 N7 0.0(15) . . . . ?
C23 N7 C24 C25 2.4(13) . . . . ?
Cd1 N7 C24 C25 -178.1(6) . . . . ?
N7 C24 C25 C26 -2.5(13) . . . . ?
C23 C22 C26 C25 0.0(13) . . . . ?
C23 C22 C26 C27 179.6(8) . . . . ?
C24 C25 C26 C22 1.2(13) . . . . ?
C24 C25 C26 C27 -178.5(8) . . . . ?
C22 C26 C27 C30 -46.7(12) . . . . ?
C25 C26 C27 C30 133.0(9) . . . . ?
C22 C26 C27 C28 132.6(9) . . . . ?
C25 C26 C27 C28 -47.7(12) . . . . ?
N8 N9 C28 C27 -1.6(8) . . . . ?
N8 N9 C28 C29 178.4(6) . . . . ?
C30 C27 C28 N9 0.4(8) . . . . ?
C26 C27 C28 N9 -179.1(7) . . . . ?
C30 C27 C28 C29 -179.5(8) . . . . ?
C26 C27 C28 C29 1.0(13) . . . . ?
N9 N8 C30 C27 -2.1(8) . . . . ?
C32 N8 C30 C27 177.9(6) . . . . ?
N9 N8 C30 C31 -177.7(7) . . . . ?
C32 N8 C30 C31 2.3(12) . . . . ?
C28 C27 C30 N8 1.0(8) . . . . ?
C26 C27 C30 N8 -179.6(7) . . . . ?
C28 C27 C30 C31 176.1(8) . . . . ?
C26 C27 C30 C31 -4.4(14) . . . . ?
C30 N8 C32 N10 101.0(9) . . . . ?
N9 N8 C32 N10 -79.0(8) . . . . ?
C33 N10 C32 N8 100.0(9) . . . . ?
N11 N10 C32 N8 -77.6(8) . . . . ?
N11 N10 C33 C35 0.3(9) . . . . ?
C32 N10 C33 C35 -177.4(7) . . . . ?
N11 N10 C33 C34 179.7(8) . . . . ?
C32 N10 C33 C34 2.0(13) . . . . ?
N10 C33 C35 C36 0.1(8) . . . . ?
C34 C33 C35 C36 -179.3(10) . . . . ?
N10 C33 C35 C38 175.0(7) . . . . ?
C34 C33 C35 C38 -4.4(15) . . . . ?
N10 N11 C36 C35 0.6(8) . . . . ?
N10 N11 C36 C37 176.2(6) . . . . ?
C33 C35 C36 N11 -0.4(9) . . . . ?
C38 C35 C36 N11 -175.4(7) . . . . ?
C33 C35 C36 C37 -175.4(8) . . . . ?
C38 C35 C36 C37 9.5(13) . . . . ?
C33 C35 C38 C42 -123.1(10) . . . . ?
C36 C35 C38 C42 50.8(12) . . . . ?
C33 C35 C38 C39 55.9(12) . . . . ?
C36 C35 C38 C39 -130.2(9) . . . . ?
C42 C38 C39 C40 0.2(14) . . . . ?
C35 C38 C39 C40 -178.8(8) . . . . ?
C41 N12 C40 C39 -1.3(14) . . . . ?
Cd1 N12 C40 C39 -178.3(7) 8_576 . . . ?
C38 C39 C40 N12 0.7(15) . . . . ?
C40 N12 C41 C42 1.2(14) . . . . ?
Cd1 N12 C41 C42 178.4(7) 8_576 . . . ?
C39 C38 C42 C41 -0.3(14) . . . . ?
C35 C38 C42 C41 178.7(8) . . . . ?
N12 C41 C42 C38 -0.4(15) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.129

#===END

data_2.Co
_database_code_depnum_ccdc_archive 'CCDC 692035'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 Co N14 S2'
_chemical_formula_weight         891.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   24.758(2)
_cell_length_b                   24.387(2)
_cell_length_c                   8.2917(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5006.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2094
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      19.39

_exptl_crystal_description       PRISM
_exptl_crystal_colour            PINK
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1860
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8687
_exptl_absorpt_correction_T_max  0.8932
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            25637
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4405
_reflns_number_gt                2383
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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)+(0.1436P)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         4405
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2366
_refine_ls_wR_factor_gt          0.2150
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
Co1 Co 0.5000 0.73208(3) -0.2500 0.0531(3) Uani 1 2 d S . .
S1 S 0.63097(14) 0.72016(15) -0.6717(4) 0.231(2) Uani 1 1 d . . .
N1 N 0.54965(14) 0.67027(15) -0.1334(5) 0.0588(10) Uani 1 1 d . . .
N2 N 0.71570(14) 0.50924(15) 0.2237(4) 0.0503(9) Uani 1 1 d . . .
N3 N 0.68401(15) 0.46753(15) 0.1699(5) 0.0580(10) Uani 1 1 d . . .
N4 N 0.80709(15) 0.47659(15) 0.2184(4) 0.0506(9) Uani 1 1 d . . .
N5 N 0.83899(14) 0.51448(14) 0.1452(4) 0.0512(9) Uani 1 1 d . . .
N6 N 0.95233(15) 0.29629(15) -0.1361(5) 0.0568(10) Uani 1 1 d . . .
N7 N 0.55161(18) 0.73187(16) -0.4465(6) 0.0661(11) Uani 1 1 d . . .
C1 C 0.61620(17) 0.59077(18) 0.0140(6) 0.0541(12) Uani 1 1 d . . .
C2 C 0.55992(18) 0.59028(19) 0.0308(7) 0.0670(14) Uani 1 1 d . . .
H2 H 0.5433 0.5632 0.0923 0.080 Uiso 1 1 calc R . .
C3 C 0.52919(18) 0.6299(2) -0.0437(7) 0.0700(15) Uani 1 1 d . . .
H3 H 0.4919 0.6284 -0.0308 0.084 Uiso 1 1 calc R . .
C4 C 0.60326(18) 0.67109(19) -0.1447(6) 0.0643(13) Uani 1 1 d . . .
H4 H 0.6190 0.6995 -0.2028 0.077 Uiso 1 1 calc R . .
C5 C 0.63677(19) 0.63281(19) -0.0764(6) 0.0615(13) Uani 1 1 d . . .
H5 H 0.6739 0.6354 -0.0918 0.074 Uiso 1 1 calc R . .
C6 C 0.65071(18) 0.54964(18) 0.0913(5) 0.0534(12) Uani 1 1 d . . .
C7 C 0.69748(18) 0.55918(18) 0.1780(6) 0.0522(11) Uani 1 1 d . . .
C8 C 0.7252(2) 0.6103(2) 0.2295(7) 0.0760(16) Uani 1 1 d . . .
H8A H 0.7290 0.6104 0.3447 0.114 Uiso 1 1 calc R . .
H8B H 0.7042 0.6415 0.1966 0.114 Uiso 1 1 calc R . .
H8C H 0.7603 0.6121 0.1804 0.114 Uiso 1 1 calc R . .
C9 C 0.64423(18) 0.49205(19) 0.0909(6) 0.0560(12) Uani 1 1 d . . .
C10 C 0.6011(2) 0.4584(2) 0.0149(7) 0.0748(15) Uani 1 1 d . . .
H10A H 0.6148 0.4223 -0.0069 0.112 Uiso 1 1 calc R . .
H10B H 0.5899 0.4752 -0.0842 0.112 Uiso 1 1 calc R . .
H10C H 0.5708 0.4558 0.0868 0.112 Uiso 1 1 calc R . .
C11 C 0.76270(17) 0.4958(2) 0.3193(6) 0.0567(12) Uani 1 1 d . . .
H11A H 0.7533 0.4675 0.3967 0.068 Uiso 1 1 calc R . .
H11B H 0.7742 0.5280 0.3788 0.068 Uiso 1 1 calc R . .
C12 C 0.87461(18) 0.48535(18) 0.0613(5) 0.0509(11) Uani 1 1 d . . .
C13 C 0.91892(17) 0.5134(2) -0.0275(6) 0.0629(13) Uani 1 1 d . . .
H13A H 0.9058 0.5474 -0.0708 0.094 Uiso 1 1 calc R . .
H13B H 0.9312 0.4903 -0.1139 0.094 Uiso 1 1 calc R . .
H13C H 0.9483 0.5205 0.0449 0.094 Uiso 1 1 calc R . .
C14 C 0.86545(18) 0.42837(18) 0.0806(5) 0.0549(12) Uani 1 1 d . . .
C15 C 0.82191(18) 0.42486(18) 0.1835(6) 0.0537(11) Uani 1 1 d . . .
C16 C 0.7931(2) 0.3758(2) 0.2478(7) 0.0856(18) Uani 1 1 d . . .
H16A H 0.8006 0.3721 0.3609 0.128 Uiso 1 1 calc R . .
H16B H 0.8052 0.3437 0.1919 0.128 Uiso 1 1 calc R . .
H16C H 0.7549 0.3802 0.2322 0.128 Uiso 1 1 calc R . .
C17 C 0.89555(18) 0.38299(18) 0.0074(6) 0.0554(12) Uani 1 1 d . . .
C18 C 0.90252(19) 0.37976(18) -0.1566(6) 0.0613(13) Uani 1 1 d . . .
H18 H 0.8883 0.4069 -0.2231 0.074 Uiso 1 1 calc R . .
C19 C 0.9304(2) 0.33661(19) -0.2226(6) 0.0642(14) Uani 1 1 d . . .
H19 H 0.9341 0.3354 -0.3341 0.077 Uiso 1 1 calc R . .
C20 C 0.9450(2) 0.2991(2) 0.0225(7) 0.0683(14) Uani 1 1 d . . .
H20 H 0.9590 0.2710 0.0858 0.082 Uiso 1 1 calc R . .
C21 C 0.9179(2) 0.3411(2) 0.0987(6) 0.0699(15) Uani 1 1 d . . .
H21 H 0.9146 0.3413 0.2105 0.084 Uiso 1 1 calc R . .
C22 C 0.5849(3) 0.7277(2) -0.5363(7) 0.0773(17) Uani 1 1 d . . .


_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
Co1 N7 2.070(5) . ?
Co1 N7 2.070(5) 3_654 ?
Co1 N1 2.172(4) 3_654 ?
Co1 N1 2.172(4) . ?
Co1 N6 2.176(4) 8_765 ?
Co1 N6 2.176(4) 6_565 ?
S1 C22 1.611(7) . ?
N1 C4 1.331(6) . ?
N1 C3 1.334(6) . ?
N2 C7 1.353(5) . ?
N2 N3 1.360(5) . ?
N2 C11 1.446(5) . ?
N3 C9 1.325(5) . ?
N4 C15 1.345(5) . ?
N4 N5 1.359(5) . ?
N4 C11 1.458(5) . ?
N5 C12 1.329(5) . ?
N6 C20 1.329(6) . ?
N6 C19 1.333(6) . ?
N6 Co1 2.176(4) 6_655 ?
N7 C22 1.116(6) . ?
C1 C5 1.369(6) . ?
C1 C2 1.400(6) . ?
C1 C6 1.465(6) . ?
C2 C3 1.376(6) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.371(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.383(6) . ?
C6 C9 1.414(6) . ?
C7 C8 1.486(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.487(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.417(6) . ?
C12 C13 1.488(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.378(6) . ?
C14 C17 1.465(6) . ?
C15 C16 1.490(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.373(7) . ?
C17 C21 1.387(6) . ?
C18 C19 1.372(6) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.378(7) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?

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
N7 Co1 N7 179.7(2) . 3_654 ?
N7 Co1 N1 89.84(15) . 3_654 ?
N7 Co1 N1 89.97(15) 3_654 3_654 ?
N7 Co1 N1 89.97(15) . . ?
N7 Co1 N1 89.84(16) 3_654 . ?
N1 Co1 N1 92.1(2) 3_654 . ?
N7 Co1 N6 90.48(16) . 8_765 ?
N7 Co1 N6 89.72(16) 3_654 8_765 ?
N1 Co1 N6 177.91(14) 3_654 8_765 ?
N1 Co1 N6 89.96(14) . 8_765 ?
N7 Co1 N6 89.72(16) . 6_565 ?
N7 Co1 N6 90.48(16) 3_654 6_565 ?
N1 Co1 N6 89.96(14) 3_654 6_565 ?
N1 Co1 N6 177.91(14) . 6_565 ?
N6 Co1 N6 87.98(19) 8_765 6_565 ?
C4 N1 C3 115.4(4) . . ?
C4 N1 Co1 121.5(3) . . ?
C3 N1 Co1 123.1(3) . . ?
C7 N2 N3 112.9(4) . . ?
C7 N2 C11 128.8(4) . . ?
N3 N2 C11 118.3(4) . . ?
C9 N3 N2 104.7(4) . . ?
C15 N4 N5 112.5(3) . . ?
C15 N4 C11 129.1(4) . . ?
N5 N4 C11 118.4(4) . . ?
C12 N5 N4 104.8(3) . . ?
C20 N6 C19 116.0(4) . . ?
C20 N6 Co1 122.7(3) . 6_655 ?
C19 N6 Co1 121.3(3) . 6_655 ?
C22 N7 Co1 169.0(4) . . ?
C5 C1 C2 115.5(4) . . ?
C5 C1 C6 122.4(4) . . ?
C2 C1 C6 122.1(4) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
N1 C3 C2 124.0(4) . . ?
N1 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
N1 C4 C5 124.3(5) . . ?
N1 C4 H4 117.8 . . ?
C5 C4 H4 117.8 . . ?
C1 C5 C4 120.7(4) . . ?
C1 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C7 C6 C9 105.3(4) . . ?
C7 C6 C1 126.9(4) . . ?
C9 C6 C1 127.8(4) . . ?
N2 C7 C6 105.9(4) . . ?
N2 C7 C8 121.4(4) . . ?
C6 C7 C8 132.6(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 111.3(4) . . ?
N3 C9 C10 119.6(4) . . ?
C6 C9 C10 129.2(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N4 111.4(4) . . ?
N2 C11 H11A 109.3 . . ?
N4 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
N4 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N5 C12 C14 111.0(4) . . ?
N5 C12 C13 120.2(4) . . ?
C14 C12 C13 128.6(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 104.8(4) . . ?
C15 C14 C17 127.4(4) . . ?
C12 C14 C17 127.8(4) . . ?
N4 C15 C14 106.8(4) . . ?
N4 C15 C16 123.0(4) . . ?
C14 C15 C16 130.2(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C21 116.6(4) . . ?
C18 C17 C14 121.1(4) . . ?
C21 C17 C14 122.2(5) . . ?
C19 C18 C17 120.1(4) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
N6 C19 C18 123.8(5) . . ?
N6 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
N6 C20 C21 124.0(5) . . ?
N6 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C20 C21 C17 119.4(5) . . ?
C20 C21 H21 120.3 . . ?
C17 C21 H21 120.3 . . ?
N7 C22 S1 177.2(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
N7 Co1 N1 C4 38.1(4) . . . . ?
N7 Co1 N1 C4 -142.1(4) 3_654 . . . ?
N1 Co1 N1 C4 128.0(4) 3_654 . . . ?
N6 Co1 N1 C4 -52.4(4) 8_765 . . . ?
N7 Co1 N1 C3 -143.3(4) . . . . ?
N7 Co1 N1 C3 36.5(4) 3_654 . . . ?
N1 Co1 N1 C3 -53.4(4) 3_654 . . . ?
N6 Co1 N1 C3 126.3(4) 8_765 . . . ?
C7 N2 N3 C9 -1.2(5) . . . . ?
C11 N2 N3 C9 178.6(4) . . . . ?
C15 N4 N5 C12 0.4(5) . . . . ?
C11 N4 N5 C12 -179.1(4) . . . . ?
N1 Co1 N7 C22 -109(3) 3_654 . . . ?
N1 Co1 N7 C22 -17(3) . . . . ?
N6 Co1 N7 C22 73(3) 8_765 . . . ?
N6 Co1 N7 C22 161(3) 6_565 . . . ?
C5 C1 C2 C3 1.1(7) . . . . ?
C6 C1 C2 C3 179.8(5) . . . . ?
C4 N1 C3 C2 -1.5(8) . . . . ?
Co1 N1 C3 C2 179.8(4) . . . . ?
C1 C2 C3 N1 -0.3(8) . . . . ?
C3 N1 C4 C5 2.5(8) . . . . ?
Co1 N1 C4 C5 -178.8(4) . . . . ?
C2 C1 C5 C4 -0.2(7) . . . . ?
C6 C1 C5 C4 -178.9(5) . . . . ?
N1 C4 C5 C1 -1.7(8) . . . . ?
C5 C1 C6 C7 45.4(7) . . . . ?
C2 C1 C6 C7 -133.2(5) . . . . ?
C5 C1 C6 C9 -133.2(5) . . . . ?
C2 C1 C6 C9 48.1(7) . . . . ?
N3 N2 C7 C6 0.9(5) . . . . ?
C11 N2 C7 C6 -178.8(4) . . . . ?
N3 N2 C7 C8 177.7(4) . . . . ?
C11 N2 C7 C8 -2.0(7) . . . . ?
C9 C6 C7 N2 -0.3(5) . . . . ?
C1 C6 C7 N2 -179.1(4) . . . . ?
C9 C6 C7 C8 -176.5(5) . . . . ?
C1 C6 C7 C8 4.6(9) . . . . ?
N2 N3 C9 C6 1.0(5) . . . . ?
N2 N3 C9 C10 -179.8(4) . . . . ?
C7 C6 C9 N3 -0.5(5) . . . . ?
C1 C6 C9 N3 178.4(4) . . . . ?
C7 C6 C9 C10 -179.6(5) . . . . ?
C1 C6 C9 C10 -0.7(9) . . . . ?
C7 N2 C11 N4 -102.0(5) . . . . ?
N3 N2 C11 N4 78.3(5) . . . . ?
C15 N4 C11 N2 -96.7(5) . . . . ?
N5 N4 C11 N2 82.6(5) . . . . ?
N4 N5 C12 C14 0.1(5) . . . . ?
N4 N5 C12 C13 -176.0(4) . . . . ?
N5 C12 C14 C15 -0.5(5) . . . . ?
C13 C12 C14 C15 175.2(4) . . . . ?
N5 C12 C14 C17 179.5(4) . . . . ?
C13 C12 C14 C17 -4.8(8) . . . . ?
N5 N4 C15 C14 -0.7(5) . . . . ?
C11 N4 C15 C14 178.7(4) . . . . ?
N5 N4 C15 C16 -179.5(4) . . . . ?
C11 N4 C15 C16 -0.2(8) . . . . ?
C12 C14 C15 N4 0.7(5) . . . . ?
C17 C14 C15 N4 -179.3(4) . . . . ?
C12 C14 C15 C16 179.4(5) . . . . ?
C17 C14 C15 C16 -0.6(9) . . . . ?
C15 C14 C17 C18 125.4(5) . . . . ?
C12 C14 C17 C18 -54.5(7) . . . . ?
C15 C14 C17 C21 -53.9(7) . . . . ?
C12 C14 C17 C21 126.1(5) . . . . ?
C21 C17 C18 C19 0.0(7) . . . . ?
C14 C17 C18 C19 -179.3(5) . . . . ?
C20 N6 C19 C18 1.3(7) . . . . ?
Co1 N6 C19 C18 -176.2(4) 6_655 . . . ?
C17 C18 C19 N6 -0.5(8) . . . . ?
C19 N6 C20 C21 -1.7(8) . . . . ?
Co1 N6 C20 C21 175.8(4) 6_655 . . . ?
N6 C20 C21 C17 1.3(8) . . . . ?
C18 C17 C21 C20 -0.4(7) . . . . ?
C14 C17 C21 C20 179.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.093

#===END

data_2.Cu
_database_code_depnum_ccdc_archive 'CCDC 692036'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H48 Cu N14 O2 S2'
_chemical_formula_weight         932.62

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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                   24.263(5)
_cell_length_b                   16.387(4)
_cell_length_c                   24.450(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9721(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4046
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      20.87

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3896
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            50726
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         25.03
_reflns_number_total             8591
_reflns_number_gt                5062
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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)+(0.0998P)²+11.8122P] 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         8591
_refine_ls_number_parameters     593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.2082
_refine_ls_wR_factor_gt          0.1674
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Cu1 Cu 0.73192(2) 0.37975(3) 0.49910(2) 0.03297(19) Uani 1 1 d . . .
S1 S 0.79629(9) 0.16069(14) 0.62106(11) 0.1205(9) Uani 1 1 d . . .
S2 S 0.80363(11) 0.58703(15) 0.38174(13) 0.1439(12) Uani 1 1 d . . .
N1 N 0.29271(14) 0.4351(2) 0.95636(14) 0.0327(8) Uani 1 1 d . . .
N2 N 0.51363(15) 0.5651(2) 0.83968(15) 0.0349(9) Uani 1 1 d . . .
N3 N 0.47639(15) 0.6088(2) 0.80908(15) 0.0343(9) Uani 1 1 d . . .
N4 N 0.51027(15) 0.6057(2) 0.71711(14) 0.0338(9) Uani 1 1 d . . .
N5 N 0.46824(15) 0.5815(2) 0.68365(15) 0.0368(9) Uani 1 1 d . . .
N6 N 0.67328(14) 0.4321(2) 0.54765(14) 0.0335(9) Uani 1 1 d . . .
N7 N 0.67225(14) 0.3257(2) 0.45334(14) 0.0323(8) Uani 1 1 d . . .
N8 N 0.49965(14) 0.1503(2) 0.29396(14) 0.0317(8) Uani 1 1 d . . .
N9 N 0.46005(15) 0.1838(2) 0.32648(15) 0.0353(9) Uani 1 1 d . . .
N10 N 0.46582(15) 0.1416(2) 0.20193(14) 0.0333(9) Uani 1 1 d . . .
N11 N 0.50576(15) 0.1718(2) 0.16778(15) 0.0349(9) Uani 1 1 d . . .
N12 N 0.29258(14) 0.3246(2) 0.04720(14) 0.0338(9) Uani 1 1 d . . .
N13 N 0.72909(18) 0.2584(3) 0.55792(18) 0.0526(11) Uani 1 1 d . . .
N14 N 0.72718(18) 0.4970(3) 0.43824(18) 0.0491(11) Uani 1 1 d . . .
C1 C 0.33898(19) 0.5541(3) 0.9236(2) 0.0427(12) Uani 1 1 d . . .
H1 H 0.3404 0.6107 0.9216 0.051 Uiso 1 1 calc R . .
C2 C 0.29595(19) 0.5163(3) 0.95086(19) 0.0400(11) Uani 1 1 d . . .
H2 H 0.2683 0.5484 0.9659 0.048 Uiso 1 1 calc R . .
C3 C 0.33201(19) 0.3900(3) 0.9330(2) 0.0395(11) Uani 1 1 d . . .
H3 H 0.3301 0.3335 0.9361 0.047 Uiso 1 1 calc R . .
C4 C 0.37489(19) 0.4235(3) 0.9049(2) 0.0433(12) Uani 1 1 d . . .
H4 H 0.4013 0.3897 0.8891 0.052 Uiso 1 1 calc R . .
C5 C 0.37962(18) 0.5078(3) 0.89945(17) 0.0342(10) Uani 1 1 d . . .
C6 C 0.42617(18) 0.5434(3) 0.86874(18) 0.0342(10) Uani 1 1 d . . .
C7 C 0.48319(18) 0.5252(3) 0.87611(17) 0.0331(10) Uani 1 1 d . . .
C8 C 0.5108(2) 0.4757(3) 0.9189(2) 0.0471(13) Uani 1 1 d . . .
H8A H 0.5492 0.4704 0.9103 0.071 Uiso 1 1 calc R . .
H8B H 0.4942 0.4226 0.9203 0.071 Uiso 1 1 calc R . .
H8C H 0.5068 0.5021 0.9537 0.071 Uiso 1 1 calc R . .
C9 C 0.42379(18) 0.5973(3) 0.82558(18) 0.0362(11) Uani 1 1 d . . .
C10 C 0.3763(2) 0.6367(4) 0.7988(2) 0.0663(17) Uani 1 1 d . . .
H10A H 0.3783 0.6946 0.8043 0.099 Uiso 1 1 calc R . .
H10B H 0.3428 0.6162 0.8145 0.099 Uiso 1 1 calc R . .
H10C H 0.3770 0.6249 0.7604 0.099 Uiso 1 1 calc R . .
C11 C 0.4968(2) 0.6559(3) 0.76384(18) 0.0380(11) Uani 1 1 d . . .
H11A H 0.5294 0.6855 0.7753 0.046 Uiso 1 1 calc R . .
H11B H 0.4691 0.6956 0.7533 0.046 Uiso 1 1 calc R . .
C12 C 0.56037(18) 0.5806(3) 0.69964(17) 0.0329(10) Uani 1 1 d . . .
C13 C 0.61165(19) 0.6023(3) 0.7287(2) 0.0477(13) Uani 1 1 d . . .
H13A H 0.6141 0.6606 0.7320 0.072 Uiso 1 1 calc R . .
H13B H 0.6428 0.5823 0.7085 0.072 Uiso 1 1 calc R . .
H13C H 0.6114 0.5782 0.7644 0.072 Uiso 1 1 calc R . .
C14 C 0.55083(17) 0.5382(3) 0.65154(17) 0.0327(10) Uani 1 1 d . . .
C15 C 0.49281(18) 0.5419(3) 0.64291(18) 0.0347(10) Uani 1 1 d . . .
C16 C 0.4591(2) 0.5066(3) 0.5980(2) 0.0470(13) Uani 1 1 d . . .
H16A H 0.4217 0.4999 0.6103 0.071 Uiso 1 1 calc R . .
H16B H 0.4739 0.4546 0.5877 0.071 Uiso 1 1 calc R . .
H16C H 0.4597 0.5427 0.5671 0.071 Uiso 1 1 calc R . .
C17 C 0.59236(18) 0.5004(3) 0.61558(18) 0.0347(10) Uani 1 1 d . . .
C18 C 0.63447(18) 0.4516(3) 0.63615(18) 0.0399(11) Uani 1 1 d . . .
H18 H 0.6364 0.4409 0.6735 0.048 Uiso 1 1 calc R . .
C19 C 0.67324(19) 0.4192(3) 0.60140(19) 0.0400(11) Uani 1 1 d . . .
H19 H 0.7008 0.3866 0.6162 0.048 Uiso 1 1 calc R . .
C20 C 0.63306(18) 0.4792(3) 0.52764(18) 0.0381(11) Uani 1 1 d . . .
H20 H 0.6325 0.4894 0.4902 0.046 Uiso 1 1 calc R . .
C21 C 0.59253(19) 0.5132(3) 0.55952(18) 0.0390(11) Uani 1 1 d . . .
H21 H 0.5652 0.5450 0.5435 0.047 Uiso 1 1 calc R . .
C22 C 0.59055(18) 0.2465(3) 0.44557(18) 0.0387(11) Uani 1 1 d . . .
H22 H 0.5633 0.2162 0.4630 0.046 Uiso 1 1 calc R . .
C23 C 0.63172(18) 0.2814(3) 0.47574(18) 0.0379(11) Uani 1 1 d . . .
H23 H 0.6316 0.2741 0.5135 0.045 Uiso 1 1 calc R . .
C24 C 0.67169(18) 0.3348(3) 0.39876(18) 0.0374(11) Uani 1 1 d . . .
H24 H 0.6995 0.3651 0.3823 0.045 Uiso 1 1 calc R . .
C25 C 0.63150(18) 0.3010(3) 0.36632(18) 0.0352(11) Uani 1 1 d . . .
H25 H 0.6328 0.3087 0.3287 0.042 Uiso 1 1 calc R . .
C26 C 0.58912(17) 0.2558(3) 0.38889(17) 0.0309(10) Uani 1 1 d . . .
C27 C 0.54530(17) 0.2189(3) 0.35563(17) 0.0319(10) Uani 1 1 d . . .
C28 C 0.55174(17) 0.1709(3) 0.30940(17) 0.0307(10) Uani 1 1 d . . .
C29 C 0.6006(2) 0.1406(3) 0.2804(2) 0.0480(13) Uani 1 1 d . . .
H29A H 0.6036 0.0827 0.2855 0.072 Uiso 1 1 calc R . .
H29B H 0.6329 0.1669 0.2946 0.072 Uiso 1 1 calc R . .
H29C H 0.5971 0.1524 0.2421 0.072 Uiso 1 1 calc R . .
C30 C 0.48824(18) 0.2245(3) 0.36470(18) 0.0326(10) Uani 1 1 d . . .
C31 C 0.4576(2) 0.2673(3) 0.40909(19) 0.0439(12) Uani 1 1 d . . .
H31A H 0.4219 0.2832 0.3959 0.066 Uiso 1 1 calc R . .
H31B H 0.4778 0.3150 0.4201 0.066 Uiso 1 1 calc R . .
H31C H 0.4534 0.2313 0.4398 0.066 Uiso 1 1 calc R . .
C32 C 0.48249(19) 0.0969(3) 0.24971(17) 0.0364(11) Uani 1 1 d . . .
H32A H 0.5127 0.0609 0.2402 0.044 Uiso 1 1 calc R . .
H32B H 0.4520 0.0633 0.2621 0.044 Uiso 1 1 calc R . .
C33 C 0.47815(18) 0.2134(3) 0.12977(17) 0.0338(10) Uani 1 1 d . . .
C34 C 0.5078(2) 0.2509(3) 0.0834(2) 0.0502(13) Uani 1 1 d . . .
H34A H 0.5466 0.2525 0.0913 0.075 Uiso 1 1 d R . .
H34B H 0.4945 0.3054 0.0778 0.075 Uiso 1 1 d R . .
H34C H 0.5017 0.2192 0.0509 0.075 Uiso 1 1 d R . .
C35 C 0.42054(18) 0.2100(3) 0.13949(17) 0.0327(10) Uani 1 1 d . . .
C36 C 0.41422(17) 0.1631(3) 0.18611(18) 0.0351(10) Uani 1 1 d . . .
C37 C 0.3644(2) 0.1371(4) 0.2168(2) 0.0616(16) Uani 1 1 d . . .
H37A H 0.3585 0.0798 0.2113 0.092 Uiso 1 1 calc R . .
H37B H 0.3330 0.1670 0.2038 0.092 Uiso 1 1 calc R . .
H37C H 0.3696 0.1478 0.2551 0.092 Uiso 1 1 calc R . .
C38 C 0.37632(18) 0.2487(3) 0.10721(18) 0.0351(10) Uani 1 1 d . . .
C39 C 0.37680(19) 0.3321(3) 0.09717(19) 0.0388(11) Uani 1 1 d . . .
H39 H 0.4055 0.3642 0.1104 0.047 Uiso 1 1 calc R . .
C40 C 0.33500(18) 0.3670(3) 0.06779(19) 0.0390(11) Uani 1 1 d . . .
H40 H 0.3361 0.4230 0.0618 0.047 Uiso 1 1 calc R . .
C41 C 0.2918(2) 0.2442(3) 0.0571(2) 0.0429(12) Uani 1 1 d . . .
H41 H 0.2626 0.2135 0.0434 0.051 Uiso 1 1 calc R . .
C42 C 0.3323(2) 0.2049(3) 0.0867(2) 0.0439(12) Uani 1 1 d . . .
H42 H 0.3299 0.1490 0.0927 0.053 Uiso 1 1 calc R . .
C43 C 0.7563(2) 0.2176(3) 0.5840(2) 0.0477(13) Uani 1 1 d . . .
C44 C 0.7576(2) 0.5346(3) 0.4144(2) 0.0532(14) Uani 1 1 d . . .
O1 O 0.2549(5) 0.8292(7) 0.8007(4) 0.116(4) Uani 0.50 1 d P . .
O2 O 0.2370(4) 0.0030(6) 0.8004(3) 0.085(3) Uani 0.50 1 d P . .
O3 O 0.2580(4) 0.7520(8) 0.2056(5) 0.126(4) Uani 0.50 1 d P . .
O4 O 0.2470(5) 0.9195(7) 0.2011(3) 0.100(3) Uani 0.50 1 d P . .


_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 N7 2.032(3) . ?
Cu1 N6 2.042(4) . ?
Cu1 N1 2.046(3) 6_657 ?
Cu1 N12 2.065(3) 6_656 ?
Cu1 N14 2.433(5) . ?
Cu1 N13 2.455(5) . ?
S1 C43 1.622(6) . ?
S2 C44 1.619(6) . ?
N1 C3 1.335(6) . ?
N1 C2 1.339(6) . ?
N1 Cu1 2.046(3) 6_557 ?
N2 C7 1.329(5) . ?
N2 N3 1.374(5) . ?
N3 C9 1.351(6) . ?
N3 C11 1.437(5) . ?
N4 C12 1.353(5) . ?
N4 N5 1.366(5) . ?
N4 C11 1.446(5) . ?
N5 C15 1.330(6) . ?
N6 C19 1.331(6) . ?
N6 C20 1.337(5) . ?
N7 C23 1.340(5) . ?
N7 C24 1.343(5) . ?
N8 C28 1.361(5) . ?
N8 N9 1.363(5) . ?
N8 C32 1.453(5) . ?
N9 C30 1.336(5) . ?
N10 C36 1.357(5) . ?
N10 N11 1.371(5) . ?
N10 C32 1.437(5) . ?
N11 C33 1.333(5) . ?
N12 C41 1.339(6) . ?
N12 C40 1.340(6) . ?
N12 Cu1 2.065(3) 6_556 ?
N13 C43 1.136(6) . ?
N14 C44 1.125(6) . ?
C1 C5 1.377(6) . ?
C1 C2 1.385(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.363(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.476(6) . ?
C6 C9 1.378(6) . ?
C6 C7 1.426(6) . ?
C7 C8 1.483(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.473(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.385(6) . ?
C12 C13 1.476(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.425(6) . ?
C14 C17 1.474(6) . ?
C15 C16 1.486(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.387(6) . ?
C17 C18 1.392(6) . ?
C18 C19 1.374(6) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.374(6) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.367(6) . ?
C22 C26 1.395(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.374(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.469(6) . ?
C27 C28 1.386(6) . ?
C27 C30 1.405(6) . ?
C28 C29 1.467(6) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.491(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C35 1.419(6) . ?
C33 C34 1.478(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.383(6) . ?
C35 C38 1.475(6) . ?
C36 C37 1.484(6) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C42 1.383(6) . ?
C38 C39 1.388(6) . ?
C39 C40 1.368(6) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.379(6) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?

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
N7 Cu1 N6 90.37(14) . . ?
N7 Cu1 N1 178.76(14) . 6_657 ?
N6 Cu1 N1 90.38(14) . 6_657 ?
N7 Cu1 N12 90.87(14) . 6_656 ?
N6 Cu1 N12 177.65(14) . 6_656 ?
N1 Cu1 N12 88.41(14) 6_657 6_656 ?
N7 Cu1 N14 88.47(14) . . ?
N6 Cu1 N14 89.49(15) . . ?
N1 Cu1 N14 90.55(14) 6_657 . ?
N12 Cu1 N14 92.53(15) 6_656 . ?
N7 Cu1 N13 87.13(15) . . ?
N6 Cu1 N13 88.85(15) . . ?
N1 Cu1 N13 93.87(15) 6_657 . ?
N12 Cu1 N13 89.22(15) 6_656 . ?
N14 Cu1 N13 175.29(15) . . ?
C3 N1 C2 117.7(4) . . ?
C3 N1 Cu1 119.8(3) . 6_557 ?
C2 N1 Cu1 122.4(3) . 6_557 ?
C7 N2 N3 104.8(4) . . ?
C9 N3 N2 112.7(3) . . ?
C9 N3 C11 129.0(4) . . ?
N2 N3 C11 118.2(4) . . ?
C12 N4 N5 113.2(3) . . ?
C12 N4 C11 128.8(4) . . ?
N5 N4 C11 118.0(4) . . ?
C15 N5 N4 104.8(3) . . ?
C19 N6 C20 116.9(4) . . ?
C19 N6 Cu1 120.5(3) . . ?
C20 N6 Cu1 122.6(3) . . ?
C23 N7 C24 117.3(4) . . ?
C23 N7 Cu1 122.3(3) . . ?
C24 N7 Cu1 120.4(3) . . ?
C28 N8 N9 113.1(3) . . ?
C28 N8 C32 128.4(4) . . ?
N9 N8 C32 118.4(3) . . ?
C30 N9 N8 104.4(3) . . ?
C36 N10 N11 112.6(3) . . ?
C36 N10 C32 128.6(4) . . ?
N11 N10 C32 118.7(3) . . ?
C33 N11 N10 104.7(3) . . ?
C41 N12 C40 116.9(4) . . ?
C41 N12 Cu1 121.3(3) . 6_556 ?
C40 N12 Cu1 121.8(3) . 6_556 ?
C43 N13 Cu1 142.2(4) . . ?
C44 N14 Cu1 135.9(4) . . ?
C5 C1 C2 120.0(4) . . ?
C5 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
N1 C2 C1 122.5(4) . . ?
N1 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
N1 C3 C4 122.5(4) . . ?
N1 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C1 C5 C4 116.5(4) . . ?
C1 C5 C6 123.3(4) . . ?
C4 C5 C6 120.2(4) . . ?
C9 C6 C7 105.7(4) . . ?
C9 C6 C5 127.6(4) . . ?
C7 C6 C5 126.5(4) . . ?
N2 C7 C6 110.6(4) . . ?
N2 C7 C8 119.4(4) . . ?
C6 C7 C8 129.9(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 106.1(4) . . ?
N3 C9 C10 123.0(4) . . ?
C6 C9 C10 130.8(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 N4 112.3(3) . . ?
N3 C11 H11A 109.1 . . ?
N4 C11 H11A 109.1 . . ?
N3 C11 H11B 109.1 . . ?
N4 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 C14 105.7(4) . . ?
N4 C12 C13 122.2(4) . . ?
C14 C12 C13 132.1(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 105.6(4) . . ?
C12 C14 C17 127.1(4) . . ?
C15 C14 C17 127.2(4) . . ?
N5 C15 C14 110.6(4) . . ?
N5 C15 C16 119.7(4) . . ?
C14 C15 C16 129.6(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 116.2(4) . . ?
C21 C17 C14 121.9(4) . . ?
C18 C17 C14 121.9(4) . . ?
C19 C18 C17 120.1(4) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
N6 C19 C18 123.3(4) . . ?
N6 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
N6 C20 C21 123.3(4) . . ?
N6 C20 H20 118.3 . . ?
C21 C20 H20 118.3 . . ?
C20 C21 C17 120.1(4) . . ?
C20 C21 H21 120.0 . . ?
C17 C21 H21 120.0 . . ?
C23 C22 C26 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C26 C22 H22 119.7 . . ?
N7 C23 C22 122.9(4) . . ?
N7 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
N7 C24 C25 122.5(4) . . ?
N7 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C24 C25 C26 120.9(4) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C22 115.9(4) . . ?
C25 C26 C27 122.6(4) . . ?
C22 C26 C27 121.6(4) . . ?
C28 C27 C30 106.1(4) . . ?
C28 C27 C26 127.1(4) . . ?
C30 C27 C26 126.8(4) . . ?
N8 C28 C27 105.2(4) . . ?
N8 C28 C29 122.1(4) . . ?
C27 C28 C29 132.6(4) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N9 C30 C27 111.2(4) . . ?
N9 C30 C31 119.3(4) . . ?
C27 C30 C31 129.6(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N10 C32 N8 112.2(3) . . ?
N10 C32 H32A 109.2 . . ?
N8 C32 H32A 109.2 . . ?
N10 C32 H32B 109.2 . . ?
N8 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
N11 C33 C35 111.0(4) . . ?
N11 C33 C34 120.2(4) . . ?
C35 C33 C34 128.7(4) . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.6 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C33 105.6(4) . . ?
C36 C35 C38 126.8(4) . . ?
C33 C35 C38 127.6(4) . . ?
N10 C36 C35 106.1(4) . . ?
N10 C36 C37 122.2(4) . . ?
C35 C36 C37 131.8(4) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C38 C39 117.0(4) . . ?
C42 C38 C35 122.3(4) . . ?
C39 C38 C35 120.8(4) . . ?
C40 C39 C38 119.9(4) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
N12 C40 C39 123.4(4) . . ?
N12 C40 H40 118.3 . . ?
C39 C40 H40 118.3 . . ?
N12 C41 C42 123.0(4) . . ?
N12 C41 H41 118.5 . . ?
C42 C41 H41 118.5 . . ?
C41 C42 C38 119.9(4) . . ?
C41 C42 H42 120.1 . . ?
C38 C42 H42 120.1 . . ?
N13 C43 S1 178.7(5) . . ?
N14 C44 S2 177.5(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 N2 N3 C9 0.2(5) . . . . ?
C7 N2 N3 C11 -177.0(4) . . . . ?
C12 N4 N5 C15 -1.8(5) . . . . ?
C11 N4 N5 C15 175.8(4) . . . . ?
N7 Cu1 N6 C19 123.1(4) . . . . ?
N1 Cu1 N6 C19 -57.9(4) 6_657 . . . ?
N14 Cu1 N6 C19 -148.4(4) . . . . ?
N13 Cu1 N6 C19 36.0(4) . . . . ?
N7 Cu1 N6 C20 -55.8(4) . . . . ?
N1 Cu1 N6 C20 123.2(4) 6_657 . . . ?
N14 Cu1 N6 C20 32.6(4) . . . . ?
N13 Cu1 N6 C20 -142.9(4) . . . . ?
N6 Cu1 N7 C23 -51.6(4) . . . . ?
N12 Cu1 N7 C23 126.4(4) 6_656 . . . ?
N14 Cu1 N7 C23 -141.1(4) . . . . ?
N13 Cu1 N7 C23 37.2(4) . . . . ?
N6 Cu1 N7 C24 127.2(4) . . . . ?
N12 Cu1 N7 C24 -54.8(4) 6_656 . . . ?
N14 Cu1 N7 C24 37.7(4) . . . . ?
N13 Cu1 N7 C24 -144.0(4) . . . . ?
C28 N8 N9 C30 -2.1(5) . . . . ?
C32 N8 N9 C30 176.1(3) . . . . ?
C36 N10 N11 C33 0.2(5) . . . . ?
C32 N10 N11 C33 -176.6(4) . . . . ?
N7 Cu1 N13 C43 145.7(7) . . . . ?
N6 Cu1 N13 C43 -123.8(7) . . . . ?
N1 Cu1 N13 C43 -33.5(7) 6_657 . . . ?
N12 Cu1 N13 C43 54.8(7) 6_656 . . . ?
N7 Cu1 N14 C44 -129.3(6) . . . . ?
N6 Cu1 N14 C44 140.3(6) . . . . ?
N1 Cu1 N14 C44 49.9(6) 6_657 . . . ?
N12 Cu1 N14 C44 -38.5(6) 6_656 . . . ?
C3 N1 C2 C1 -2.0(7) . . . . ?
Cu1 N1 C2 C1 175.9(4) 6_557 . . . ?
C5 C1 C2 N1 2.0(8) . . . . ?
C2 N1 C3 C4 0.8(7) . . . . ?
Cu1 N1 C3 C4 -177.1(4) 6_557 . . . ?
N1 C3 C4 C5 0.3(8) . . . . ?
C2 C1 C5 C4 -0.8(7) . . . . ?
C2 C1 C5 C6 178.7(4) . . . . ?
C3 C4 C5 C1 -0.3(7) . . . . ?
C3 C4 C5 C6 -179.9(4) . . . . ?
C1 C5 C6 C9 -53.9(7) . . . . ?
C4 C5 C6 C9 125.6(5) . . . . ?
C1 C5 C6 C7 129.6(5) . . . . ?
C4 C5 C6 C7 -50.8(7) . . . . ?
N3 N2 C7 C6 0.0(5) . . . . ?
N3 N2 C7 C8 -175.8(4) . . . . ?
C9 C6 C7 N2 -0.3(5) . . . . ?
C5 C6 C7 N2 176.8(4) . . . . ?
C9 C6 C7 C8 175.0(5) . . . . ?
C5 C6 C7 C8 -7.9(8) . . . . ?
N2 N3 C9 C6 -0.4(5) . . . . ?
C11 N3 C9 C6 176.5(4) . . . . ?
N2 N3 C9 C10 -179.3(5) . . . . ?
C11 N3 C9 C10 -2.4(8) . . . . ?
C7 C6 C9 N3 0.4(5) . . . . ?
C5 C6 C9 N3 -176.6(4) . . . . ?
C7 C6 C9 C10 179.1(5) . . . . ?
C5 C6 C9 C10 2.1(9) . . . . ?
C9 N3 C11 N4 -100.6(5) . . . . ?
N2 N3 C11 N4 76.2(5) . . . . ?
C12 N4 C11 N3 -102.1(5) . . . . ?
N5 N4 C11 N3 80.8(5) . . . . ?
N5 N4 C12 C14 0.7(5) . . . . ?
C11 N4 C12 C14 -176.5(4) . . . . ?
N5 N4 C12 C13 177.9(4) . . . . ?
C11 N4 C12 C13 0.7(7) . . . . ?
N4 C12 C14 C15 0.6(5) . . . . ?
C13 C12 C14 C15 -176.2(5) . . . . ?
N4 C12 C14 C17 178.2(4) . . . . ?
C13 C12 C14 C17 1.4(8) . . . . ?
N4 N5 C15 C14 2.1(5) . . . . ?
N4 N5 C15 C16 -179.9(4) . . . . ?
C12 C14 C15 N5 -1.8(5) . . . . ?
C17 C14 C15 N5 -179.3(4) . . . . ?
C12 C14 C15 C16 -179.5(5) . . . . ?
C17 C14 C15 C16 2.9(8) . . . . ?
C12 C14 C17 C21 -131.0(5) . . . . ?
C15 C14 C17 C21 46.1(7) . . . . ?
C12 C14 C17 C18 47.3(7) . . . . ?
C15 C14 C17 C18 -135.7(5) . . . . ?
C21 C17 C18 C19 0.0(7) . . . . ?
C14 C17 C18 C19 -178.3(4) . . . . ?
C20 N6 C19 C18 0.0(7) . . . . ?
Cu1 N6 C19 C18 -179.0(4) . . . . ?
C17 C18 C19 N6 0.3(8) . . . . ?
C19 N6 C20 C21 -0.6(7) . . . . ?
Cu1 N6 C20 C21 178.4(4) . . . . ?
N6 C20 C21 C17 0.9(7) . . . . ?
C18 C17 C21 C20 -0.6(7) . . . . ?
C14 C17 C21 C20 177.8(4) . . . . ?
C24 N7 C23 C22 -0.5(7) . . . . ?
Cu1 N7 C23 C22 178.3(4) . . . . ?
C26 C22 C23 N7 0.0(7) . . . . ?
C23 N7 C24 C25 0.3(7) . . . . ?
Cu1 N7 C24 C25 -178.5(3) . . . . ?
N7 C24 C25 C26 0.2(7) . . . . ?
C24 C25 C26 C22 -0.7(7) . . . . ?
C24 C25 C26 C27 179.8(4) . . . . ?
C23 C22 C26 C25 0.5(7) . . . . ?
C23 C22 C26 C27 -179.9(4) . . . . ?
C25 C26 C27 C28 50.2(7) . . . . ?
C22 C26 C27 C28 -129.2(5) . . . . ?
C25 C26 C27 C30 -130.5(5) . . . . ?
C22 C26 C27 C30 50.0(7) . . . . ?
N9 N8 C28 C27 1.6(5) . . . . ?
C32 N8 C28 C27 -176.3(4) . . . . ?
N9 N8 C28 C29 179.2(4) . . . . ?
C32 N8 C28 C29 1.3(7) . . . . ?
C30 C27 C28 N8 -0.5(5) . . . . ?
C26 C27 C28 N8 178.9(4) . . . . ?
C30 C27 C28 C29 -177.8(5) . . . . ?
C26 C27 C28 C29 1.6(8) . . . . ?
N8 N9 C30 C27 1.7(5) . . . . ?
N8 N9 C30 C31 -178.0(4) . . . . ?
C28 C27 C30 N9 -0.8(5) . . . . ?
C26 C27 C30 N9 179.8(4) . . . . ?
C28 C27 C30 C31 178.9(4) . . . . ?
C26 C27 C30 C31 -0.5(8) . . . . ?
C36 N10 C32 N8 -96.7(5) . . . . ?
N11 N10 C32 N8 79.5(5) . . . . ?
C28 N8 C32 N10 -99.9(5) . . . . ?
N9 N8 C32 N10 82.3(5) . . . . ?
N10 N11 C33 C35 0.0(5) . . . . ?
N10 N11 C33 C34 -176.2(4) . . . . ?
N11 C33 C35 C36 -0.2(5) . . . . ?
C34 C33 C35 C36 175.6(5) . . . . ?
N11 C33 C35 C38 179.3(4) . . . . ?
C34 C33 C35 C38 -4.8(8) . . . . ?
N11 N10 C36 C35 -0.3(5) . . . . ?
C32 N10 C36 C35 176.0(4) . . . . ?
N11 N10 C36 C37 179.8(4) . . . . ?
C32 N10 C36 C37 -3.8(7) . . . . ?
C33 C35 C36 N10 0.3(5) . . . . ?
C38 C35 C36 N10 -179.2(4) . . . . ?
C33 C35 C36 C37 -179.8(5) . . . . ?
C38 C35 C36 C37 0.6(8) . . . . ?
C36 C35 C38 C42 -54.4(7) . . . . ?
C33 C35 C38 C42 126.2(5) . . . . ?
C36 C35 C38 C39 124.2(5) . . . . ?
C33 C35 C38 C39 -55.2(7) . . . . ?
C42 C38 C39 C40 -0.4(7) . . . . ?
C35 C38 C39 C40 -179.1(4) . . . . ?
C41 N12 C40 C39 0.8(7) . . . . ?
Cu1 N12 C40 C39 -177.9(4) 6_556 . . . ?
C38 C39 C40 N12 -0.4(7) . . . . ?
C40 N12 C41 C42 -0.4(7) . . . . ?
Cu1 N12 C41 C42 178.3(4) 6_556 . . . ?
N12 C41 C42 C38 -0.4(8) . . . . ?
C39 C38 C42 C41 0.8(7) . . . . ?
C35 C38 C42 C41 179.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.101

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 692037'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H44 Cd N16.17 O2.74'
_chemical_formula_weight         931.62

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           Orthorhombic
_symmetry_space_group_name_H-M   Pcca

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

_cell_length_a                   23.637(7)
_cell_length_b                   25.067(7)
_cell_length_c                   8.195(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4856(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3079
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      21.42

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1916.6
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8491
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'Apex II 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            24505
_diffrn_reflns_av_R_equivalents  0.1290
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4290
_reflns_number_gt                2976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the nitrate and azide anions
in order to improve the refinement stability, which were also refined using
the pseudo-isotropic "ISOR" restraint, as the free refinement gave unrealistic
anisotropic displacement parameters. In addition, the soft "SADI" constraint
was imposed on the oxygen atoms of nitrate. The distance between the central
nitrogen atoms of azide and nitrate is 0.497 Å and therefore the "EADP"
restraint was applied to their thermal parameters.
;

_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)+(0.1484P)²+2.5489P] 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     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4290
_refine_ls_number_parameters     313
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2425
_refine_ls_wR_factor_gt          0.2146
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.078
_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 0.0000 0.23354(2) 0.2500 0.0726(4) Uani 1 2 d S . .
N1 N 0.0539(2) 0.30110(18) 0.3764(6) 0.0662(14) Uani 1 1 d . A .
N2 N 0.20417(17) 0.47936(17) 0.7275(5) 0.0438(10) Uani 1 1 d . . .
N3 N 0.16923(16) 0.51541(15) 0.6523(5) 0.0470(10) Uani 1 1 d . . .
N4 N -0.0479(2) 0.17058(17) 0.0921(6) 0.0665(14) Uani 1 1 d . A .
N5 N -0.1697(2) -0.02599(19) -0.2751(5) 0.0522(11) Uani 1 1 d . A .
N6 N -0.20175(19) 0.01429(17) -0.3378(5) 0.0517(11) Uani 1 1 d . A .
C1 C 0.1129(2) 0.3848(2) 0.5181(7) 0.0510(12) Uani 1 1 d . . .
C2 C 0.0922(3) 0.3427(2) 0.6107(7) 0.0652(15) Uani 1 1 d . A .
H2 H 0.0984 0.3415 0.7228 0.078 Uiso 1 1 calc R . .
C3 C 0.0626(3) 0.3029(3) 0.5348(8) 0.0728(18) Uani 1 1 d . . .
H3 H 0.0479 0.2756 0.5988 0.087 Uiso 1 1 calc R A .
C4 C 0.0740(3) 0.3415(2) 0.2876(7) 0.0661(16) Uani 1 1 d . . .
H4 H 0.0682 0.3412 0.1754 0.079 Uiso 1 1 calc R A .
C5 C 0.1024(2) 0.3828(2) 0.3547(7) 0.0598(14) Uani 1 1 d . A .
H5 H 0.1151 0.4103 0.2881 0.072 Uiso 1 1 calc R . .
C6 C 0.1438(2) 0.43074(19) 0.5920(6) 0.0461(12) Uani 1 1 d . . .
C7 C 0.13265(19) 0.4849(2) 0.5709(6) 0.0452(11) Uani 1 1 d . . .
C8 C 0.0845(2) 0.5115(2) 0.4820(7) 0.0621(15) Uani 1 1 d . . .
H8A H 0.0971 0.5450 0.4383 0.093 Uiso 1 1 calc R . .
H8B H 0.0538 0.5175 0.5565 0.093 Uiso 1 1 calc R . .
H8C H 0.0720 0.4889 0.3947 0.093 Uiso 1 1 calc R . .
C9 C 0.1904(2) 0.4282(2) 0.6951(7) 0.0488(12) Uani 1 1 d . . .
C10 C 0.2224(3) 0.3818(3) 0.7608(8) 0.0728(18) Uani 1 1 d . . .
H10A H 0.2622 0.3890 0.7553 0.109 Uiso 1 1 calc R . .
H10B H 0.2138 0.3506 0.6973 0.109 Uiso 1 1 calc R . .
H10C H 0.2117 0.3758 0.8723 0.109 Uiso 1 1 calc R . .
C11 C 0.2500 0.5000 0.8267(9) 0.0468(16) Uani 1 2 d S . .
H11A H 0.2643 0.4718 0.8963 0.056 Uiso 0.50 1 calc PR . .
H11B H 0.2357 0.5282 0.8963 0.056 Uiso 0.50 1 calc PR . .
C12 C -0.0218(3) 0.1311(2) 0.0187(9) 0.0742(19) Uani 1 1 d . . .
H12 H 0.0173 0.1290 0.0288 0.089 Uiso 1 1 calc R A .
C13 C -0.0491(2) 0.0921(2) -0.0733(7) 0.0641(15) Uani 1 1 d . A .
H13 H -0.0286 0.0647 -0.1214 0.077 Uiso 1 1 calc R . .
C14 C -0.1073(2) 0.0948(2) -0.0922(6) 0.0483(12) Uani 1 1 d . . .
C15 C -0.1341(2) 0.1370(2) -0.0173(7) 0.0599(14) Uani 1 1 d . A .
H15 H -0.1729 0.1413 -0.0301 0.072 Uiso 1 1 calc R . .
C16 C -0.1043(3) 0.1725(2) 0.0759(8) 0.0667(16) Uani 1 1 d . . .
H16 H -0.1240 0.1992 0.1304 0.080 Uiso 1 1 calc R A .
C17 C -0.1390(2) 0.0545(2) -0.1859(6) 0.0468(12) Uani 1 1 d . A .
C18 C -0.1311(2) -0.0010(2) -0.1847(6) 0.0478(12) Uani 1 1 d . . .
C19 C -0.0872(2) -0.0347(2) -0.1009(7) 0.0625(15) Uani 1 1 d . A .
H19A H -0.1002 -0.0709 -0.0950 0.094 Uiso 1 1 calc R . .
H19B H -0.0809 -0.0213 0.0073 0.094 Uiso 1 1 calc R . .
H19C H -0.0525 -0.0333 -0.1616 0.094 Uiso 1 1 calc R . .
C20 C -0.1855(2) 0.0633(2) -0.2855(6) 0.0501(13) Uani 1 1 d . . .
C21 C -0.2119(3) 0.1135(2) -0.3464(8) 0.0706(17) Uani 1 1 d . A .
H21A H -0.2143 0.1124 -0.4633 0.106 Uiso 1 1 calc R . .
H21B H -0.1891 0.1434 -0.3139 0.106 Uiso 1 1 calc R . .
H21C H -0.2491 0.1171 -0.3012 0.106 Uiso 1 1 calc R . .
C22 C -0.2500 0.0000 -0.4378(9) 0.059(2) Uani 1 2 d S . .
H22A H -0.2401 -0.0299 -0.5074 0.071 Uiso 0.50 1 calc PR A .
H22B H -0.2599 0.0299 -0.5074 0.071 Uiso 0.50 1 calc PR . .
N7 N 0.0675(7) 0.2305(8) 0.0735(19) 0.122(6) Uani 0.543(17) 1 d PDU A 1
N8 N 0.0915(7) 0.2298(8) -0.052(2) 0.122(5) Uani 0.543(17) 1 d PDU A 1
N9 N 0.1266(8) 0.2333(7) -0.1539(18) 0.117(6) Uani 0.543(17) 1 d PDU A 1
N8' N 0.1006(7) 0.2395(8) -0.006(3) 0.122(5) Uani 0.457(17) 1 d PDU A 2
O1 O 0.0560(5) 0.2618(5) -0.0219(19) 0.109(6) Uani 0.457(17) 1 d PDU A 2
O2 O 0.1031(7) 0.1964(6) 0.059(2) 0.147(8) Uani 0.457(17) 1 d PDU A 2
O3 O 0.1404(8) 0.2568(9) -0.083(4) 0.204(12) Uani 0.457(17) 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
Cd1 N7 2.156(11) 4 ?
Cd1 N7 2.156(11) . ?
Cd1 N4 2.334(4) . ?
Cd1 N4 2.334(4) 4 ?
Cd1 N1 2.359(4) . ?
Cd1 N1 2.359(4) 4 ?
N1 C3 1.315(8) . ?
N1 C4 1.334(7) . ?
N2 C9 1.349(7) . ?
N2 N3 1.371(6) . ?
N2 C11 1.450(6) . ?
N3 C7 1.333(6) . ?
N4 C12 1.312(8) . ?
N4 C16 1.339(7) . ?
N5 C18 1.332(7) . ?
N5 N6 1.363(6) . ?
N6 C20 1.357(7) . ?
N6 C22 1.450(6) . ?
C1 C5 1.363(8) . ?
C1 C2 1.389(7) . ?
C1 C6 1.492(7) . ?
C2 C3 1.367(8) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.351(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C9 1.390(7) . ?
C6 C7 1.394(7) . ?
C7 C8 1.506(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.488(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.450(6) 2_565 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.392(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(7) . ?
C14 C17 1.473(7) . ?
C15 C16 1.368(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C20 1.388(8) . ?
C17 C18 1.404(7) . ?
C18 C19 1.502(7) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.490(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N6 1.450(6) 2_455 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N7 N8 1.174(7) . ?
N8 N9 1.1811(11) . ?
N8' O1 1.200(10) . ?
N8' O2 1.206(10) . ?
N8' O3 1.213(10) . ?

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
N7 Cd1 N7 176.0(10) 4 . ?
N7 Cd1 N4 89.4(6) 4 . ?
N7 Cd1 N4 87.9(4) . . ?
N7 Cd1 N4 87.9(4) 4 4 ?
N7 Cd1 N4 89.4(6) . 4 ?
N4 Cd1 N4 94.9(2) . 4 ?
N7 Cd1 N1 97.5(6) 4 . ?
N7 Cd1 N1 85.4(4) . . ?
N4 Cd1 N1 172.32(18) . . ?
N4 Cd1 N1 88.84(17) 4 . ?
N7 Cd1 N1 85.4(4) 4 4 ?
N7 Cd1 N1 97.5(6) . 4 ?
N4 Cd1 N1 88.84(17) . 4 ?
N4 Cd1 N1 172.32(18) 4 4 ?
N1 Cd1 N1 88.2(2) . 4 ?
C3 N1 C4 117.1(5) . . ?
C3 N1 Cd1 122.9(4) . . ?
C4 N1 Cd1 119.8(4) . . ?
C9 N2 N3 113.2(4) . . ?
C9 N2 C11 129.0(4) . . ?
N3 N2 C11 117.8(3) . . ?
C7 N3 N2 103.7(4) . . ?
C12 N4 C16 116.7(5) . . ?
C12 N4 Cd1 122.4(4) . . ?
C16 N4 Cd1 120.9(4) . . ?
C18 N5 N6 104.0(4) . . ?
C20 N6 N5 113.3(4) . . ?
C20 N6 C22 128.7(4) . . ?
N5 N6 C22 117.9(3) . . ?
C5 C1 C2 116.4(5) . . ?
C5 C1 C6 121.1(5) . . ?
C2 C1 C6 122.5(5) . . ?
C3 C2 C1 119.0(6) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
N1 C3 C2 123.7(6) . . ?
N1 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
N1 C4 C5 122.4(5) . . ?
N1 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C1 121.3(5) . . ?
C4 C5 H5 119.4 . . ?
C1 C5 H5 119.4 . . ?
C9 C6 C7 105.7(4) . . ?
C9 C6 C1 126.8(5) . . ?
C7 C6 C1 127.5(4) . . ?
N3 C7 C6 112.0(4) . . ?
N3 C7 C8 118.6(5) . . ?
C6 C7 C8 129.3(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 105.5(4) . . ?
N2 C9 C10 123.4(5) . . ?
C6 C9 C10 131.1(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N2 111.8(5) . 2_565 ?
N2 C11 H11A 109.3 . . ?
N2 C11 H11A 109.3 2_565 . ?
N2 C11 H11B 109.3 . . ?
N2 C11 H11B 109.3 2_565 . ?
H11A C11 H11B 107.9 . . ?
N4 C12 C13 124.0(5) . . ?
N4 C12 H12 118.0 . . ?
C13 C12 H12 118.0 . . ?
C14 C13 C12 119.1(5) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C15 C14 C13 116.4(5) . . ?
C15 C14 C17 121.7(5) . . ?
C13 C14 C17 122.0(5) . . ?
C16 C15 C14 120.7(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
N4 C16 C15 123.0(6) . . ?
N4 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C20 C17 C18 105.5(4) . . ?
C20 C17 C14 126.9(5) . . ?
C18 C17 C14 127.5(5) . . ?
N5 C18 C17 111.8(5) . . ?
N5 C18 C19 117.6(5) . . ?
C17 C18 C19 130.7(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C17 105.4(5) . . ?
N6 C20 C21 122.8(5) . . ?
C17 C20 C21 131.5(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 N6 111.1(6) . 2_455 ?
N6 C22 H22A 109.4 . . ?
N6 C22 H22A 109.4 2_455 . ?
N6 C22 H22B 109.4 . . ?
N6 C22 H22B 109.4 2_455 . ?
H22A C22 H22B 108.0 . . ?
N8 N7 Cd1 161.0(18) . . ?
N7 N8 N9 163(2) . . ?
O1 N8' O2 120.5(13) . . ?
O1 N8' O3 117.4(12) . . ?
O2 N8' O3 120.8(13) . . ?

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
N7 Cd1 N1 C3 42.3(7) 4 . . . ?
N7 Cd1 N1 C3 -134.9(8) . . . . ?
N4 Cd1 N1 C3 -45.4(5) 4 . . . ?
N1 Cd1 N1 C3 127.5(6) 4 . . . ?
N7 Cd1 N1 C4 -133.4(6) 4 . . . ?
N7 Cd1 N1 C4 49.3(8) . . . . ?
N4 Cd1 N1 C4 138.8(5) 4 . . . ?
N1 Cd1 N1 C4 -48.3(4) 4 . . . ?
C9 N2 N3 C7 0.1(5) . . . . ?
C11 N2 N3 C7 179.4(4) . . . . ?
N7 Cd1 N4 C12 -138.8(7) 4 . . . ?
N7 Cd1 N4 C12 38.2(8) . . . . ?
N4 Cd1 N4 C12 -50.9(5) 4 . . . ?
N1 Cd1 N4 C12 135.8(5) 4 . . . ?
N7 Cd1 N4 C16 39.4(6) 4 . . . ?
N7 Cd1 N4 C16 -143.5(8) . . . . ?
N4 Cd1 N4 C16 127.3(6) 4 . . . ?
N1 Cd1 N4 C16 -46.0(5) 4 . . . ?
C18 N5 N6 C20 -2.0(6) . . . . ?
C18 N5 N6 C22 -177.3(4) . . . . ?
C5 C1 C2 C3 -0.7(9) . . . . ?
C6 C1 C2 C3 177.8(6) . . . . ?
C4 N1 C3 C2 -1.9(10) . . . . ?
Cd1 N1 C3 C2 -177.8(5) . . . . ?
C1 C2 C3 N1 2.2(11) . . . . ?
C3 N1 C4 C5 0.3(10) . . . . ?
Cd1 N1 C4 C5 176.3(5) . . . . ?
N1 C4 C5 C1 1.1(11) . . . . ?
C2 C1 C5 C4 -0.8(9) . . . . ?
C6 C1 C5 C4 -179.3(6) . . . . ?
C5 C1 C6 C9 -128.9(6) . . . . ?
C2 C1 C6 C9 52.7(8) . . . . ?
C5 C1 C6 C7 50.2(8) . . . . ?
C2 C1 C6 C7 -128.2(6) . . . . ?
N2 N3 C7 C6 -0.4(5) . . . . ?
N2 N3 C7 C8 175.6(4) . . . . ?
C9 C6 C7 N3 0.5(6) . . . . ?
C1 C6 C7 N3 -178.8(5) . . . . ?
C9 C6 C7 C8 -174.9(5) . . . . ?
C1 C6 C7 C8 5.8(9) . . . . ?
N3 N2 C9 C6 0.3(6) . . . . ?
C11 N2 C9 C6 -179.0(5) . . . . ?
N3 N2 C9 C10 179.3(5) . . . . ?
C11 N2 C9 C10 0.0(9) . . . . ?
C7 C6 C9 N2 -0.5(6) . . . . ?
C1 C6 C9 N2 178.8(5) . . . . ?
C7 C6 C9 C10 -179.4(6) . . . . ?
C1 C6 C9 C10 -0.1(10) . . . . ?
C9 N2 C11 N2 104.1(5) . . . 2_565 ?
N3 N2 C11 N2 -75.2(3) . . . 2_565 ?
C16 N4 C12 C13 0.2(10) . . . . ?
Cd1 N4 C12 C13 178.5(5) . . . . ?
N4 C12 C13 C14 1.0(10) . . . . ?
C12 C13 C14 C15 0.3(9) . . . . ?
C12 C13 C14 C17 -179.1(6) . . . . ?
C13 C14 C15 C16 -2.6(8) . . . . ?
C17 C14 C15 C16 176.7(5) . . . . ?
C12 N4 C16 C15 -2.7(10) . . . . ?
Cd1 N4 C16 C15 179.0(5) . . . . ?
C14 C15 C16 N4 4.0(10) . . . . ?
C15 C14 C17 C20 37.6(8) . . . . ?
C13 C14 C17 C20 -143.1(6) . . . . ?
C15 C14 C17 C18 -137.7(6) . . . . ?
C13 C14 C17 C18 41.6(8) . . . . ?
N6 N5 C18 C17 1.5(6) . . . . ?
N6 N5 C18 C19 -178.2(4) . . . . ?
C20 C17 C18 N5 -0.6(6) . . . . ?
C14 C17 C18 N5 175.5(5) . . . . ?
C20 C17 C18 C19 179.1(5) . . . . ?
C14 C17 C18 C19 -4.8(9) . . . . ?
N5 N6 C20 C17 1.7(6) . . . . ?
C22 N6 C20 C17 176.4(5) . . . . ?
N5 N6 C20 C21 175.8(5) . . . . ?
C22 N6 C20 C21 -9.5(9) . . . . ?
C18 C17 C20 N6 -0.6(6) . . . . ?
C14 C17 C20 N6 -176.8(5) . . . . ?
C18 C17 C20 C21 -174.1(6) . . . . ?
C14 C17 C20 C21 9.8(10) . . . . ?
C20 N6 C22 N6 -93.4(5) . . . 2_455 ?
N5 N6 C22 N6 81.1(4) . . . 2_455 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.117

#===END

data_3.Cu
_database_code_depnum_ccdc_archive 'CCDC 692038'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H46 Cu N14 O7'
_chemical_formula_weight         922.47

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pcca

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

_cell_length_a                   23.955(16)
_cell_length_b                   24.334(16)
_cell_length_c                   8.163(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4758(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3824
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      22.23

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1924
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8941
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_process_details   SADABS

_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  'Apex II 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            24062
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4188
_reflns_number_gt                2799
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the disordered nitrate anion
in order to improve the refinement stability, which was also refined using
the pseudo-isotropic "ISOR" restraint, as the free refinement gave
unrealistic anisotropic displacement parameters. In addition, the "FLAT"
constraint was imposed on nitrate.
;

_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)+(0.1576P)²+6.4657P] 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     SHELXL
_refine_ls_extinction_coef       0.0054(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4188
_refine_ls_number_parameters     328
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2679
_refine_ls_wR_factor_gt          0.2333
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.072
_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 0.26129(4) 0.2500 0.0567(4) Uani 1 2 d S . .
N1 N 0.45495(17) 0.31973(18) 0.3666(6) 0.0553(12) Uani 1 1 d . . .
N2 N 0.29779(17) 0.48458(17) 0.7686(5) 0.0418(10) Uani 1 1 d . . .
N3 N 0.33100(17) 0.52565(18) 0.7100(5) 0.0453(10) Uani 1 1 d . . .
N4 N 0.45216(18) 0.20161(17) 0.3529(6) 0.0529(12) Uani 1 1 d . . .
N5 N 0.32977(16) -0.01681(16) 0.6158(5) 0.0432(10) Uani 1 1 d . . .
N6 N 0.29586(16) 0.02033(17) 0.6903(5) 0.0424(10) Uani 1 1 d . . .
C1 C 0.39271(19) 0.39969(19) 0.5355(6) 0.0425(12) Uani 1 1 d . . .
C2 C 0.3678(2) 0.3592(2) 0.4450(7) 0.0518(14) Uani 1 1 d . . .
H2 H 0.3290 0.3579 0.4382 0.062 Uiso 1 1 calc R . .
C3 C 0.3995(2) 0.3196(2) 0.3625(7) 0.0538(14) Uani 1 1 d . . .
H3 H 0.3812 0.2924 0.3031 0.065 Uiso 1 1 calc R A .
C4 C 0.4794(2) 0.3587(2) 0.4550(9) 0.0655(18) Uani 1 1 d . . .
H4 H 0.5182 0.3590 0.4597 0.079 Uiso 1 1 calc R A .
C5 C 0.4510(2) 0.3984(2) 0.5398(8) 0.0550(14) Uani 1 1 d . . .
H5 H 0.4705 0.4245 0.6002 0.066 Uiso 1 1 calc R . .
C6 C 0.3603(2) 0.4420(2) 0.6227(6) 0.0439(12) Uani 1 1 d . . .
C7 C 0.3136(2) 0.4340(2) 0.7185(6) 0.0427(12) Uani 1 1 d . . .
C8 C 0.2849(2) 0.3835(2) 0.7716(8) 0.0611(16) Uani 1 1 d . . .
H8A H 0.2845 0.3819 0.8891 0.092 Uiso 1 1 calc R . .
H8B H 0.3043 0.3521 0.7292 0.092 Uiso 1 1 calc R . .
H8C H 0.2473 0.3837 0.7311 0.092 Uiso 1 1 calc R . .
C9 C 0.36995(19) 0.4993(2) 0.6227(6) 0.0439(12) Uani 1 1 d . . .
C10 C 0.4148(2) 0.5319(2) 0.5417(8) 0.0551(14) Uani 1 1 d . . .
H10A H 0.4011 0.5681 0.5172 0.083 Uiso 1 1 calc R . .
H10B H 0.4258 0.5140 0.4420 0.083 Uiso 1 1 calc R . .
H10C H 0.4464 0.5347 0.6136 0.083 Uiso 1 1 calc R . .
C11 C 0.2500 0.5000 0.8678(8) 0.0464(17) Uani 1 2 d S . .
H11A H 0.2398 0.4694 0.9378 0.056 Uiso 0.50 1 calc PR . .
H11B H 0.2602 0.5306 0.9378 0.056 Uiso 0.50 1 calc PR . .
C12 C 0.3894(2) 0.1162(2) 0.4916(7) 0.0473(12) Uani 1 1 d . . .
C13 C 0.3989(2) 0.1200(2) 0.3229(7) 0.0549(14) Uani 1 1 d . . .
H13 H 0.3842 0.0934 0.2532 0.066 Uiso 1 1 calc R . .
C14 C 0.4297(2) 0.1622(2) 0.2594(7) 0.0550(14) Uani 1 1 d . . .
H14 H 0.4353 0.1636 0.1468 0.066 Uiso 1 1 calc R A .
C15 C 0.4429(2) 0.1992(2) 0.5159(8) 0.0613(16) Uani 1 1 d . . .
H15 H 0.4578 0.2266 0.5822 0.074 Uiso 1 1 calc R A .
C16 C 0.4120(2) 0.1577(2) 0.5881(7) 0.0586(15) Uani 1 1 d . . .
H16 H 0.4065 0.1575 0.7009 0.070 Uiso 1 1 calc R . .
C17 C 0.3567(2) 0.0703(2) 0.5595(6) 0.0444(12) Uani 1 1 d . . .
C18 C 0.36677(19) 0.0139(2) 0.5345(6) 0.0432(12) Uani 1 1 d . . .
C19 C 0.4143(2) -0.0137(2) 0.4490(7) 0.0553(14) Uani 1 1 d . . .
H19A H 0.4369 0.0135 0.3953 0.083 Uiso 1 1 calc R . .
H19B H 0.4001 -0.0390 0.3693 0.083 Uiso 1 1 calc R . .
H19C H 0.4366 -0.0332 0.5276 0.083 Uiso 1 1 calc R . .
C20 C 0.3105(2) 0.0733(2) 0.6612(6) 0.0453(12) Uani 1 1 d . . .
C21 C 0.2803(3) 0.1208(3) 0.7300(9) 0.0709(19) Uani 1 1 d . . .
H21A H 0.2919 0.1265 0.8413 0.106 Uiso 1 1 calc R . .
H21B H 0.2409 0.1137 0.7269 0.106 Uiso 1 1 calc R . .
H21C H 0.2886 0.1530 0.6664 0.106 Uiso 1 1 calc R . .
C22 C 0.2500 0.0000 0.7902(9) 0.0455(17) Uani 1 2 d S . .
H22A H 0.2634 -0.0294 0.8601 0.055 Uiso 0.50 1 calc PR . .
H22B H 0.2366 0.0294 0.8601 0.055 Uiso 0.50 1 calc PR . .
O4 O 0.7645(10) 0.2509(8) 0.615(3) 0.217(10) Uani 0.50 1 d PU . .
H4A H 0.7880 0.2469 0.6990 0.325 Uiso 0.50 1 d PR . .
H4B H 0.7922 0.2524 0.5184 0.325 Uiso 0.50 1 d PR . .
N7 N 0.6007(3) 0.2670(3) 0.5709(8) 0.132(3) Uani 1 1 d DU . .
O1 O 0.5584(3) 0.2516(3) 0.5125(12) 0.091(3) Uani 0.75 1 d PDU A 1
O2 O 0.6345(5) 0.2419(6) 0.6488(18) 0.199(6) Uani 0.75 1 d PDU A 1
O3 O 0.6122(6) 0.3173(4) 0.548(2) 0.236(7) Uani 0.75 1 d PDU A 1
O1' O 0.6406(8) 0.2353(10) 0.537(3) 0.131(10) Uani 0.25 1 d PDU A 2
O2' O 0.6004(10) 0.2895(11) 0.7007(18) 0.133(10) Uani 0.25 1 d PDU A 2
O3' O 0.5653(7) 0.2715(8) 0.466(2) 0.066(6) Uani 0.25 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
Cu1 N1 2.023(4) 3_655 ?
Cu1 N1 2.023(4) . ?
Cu1 N4 2.032(4) . ?
Cu1 N4 2.032(4) 3_655 ?
Cu1 O3' 2.371(10) 3_655 ?
Cu1 O3' 2.371(10) . ?
N1 C4 1.327(8) . ?
N1 C3 1.330(6) . ?
N2 C7 1.352(6) . ?
N2 N3 1.364(6) . ?
N2 C11 1.452(5) . ?
N3 C9 1.338(6) . ?
N4 C14 1.338(7) . ?
N4 C15 1.350(8) . ?
N5 C18 1.335(6) . ?
N5 N6 1.359(6) . ?
N6 C20 1.357(6) . ?
N6 C22 1.455(6) . ?
C1 C2 1.370(7) . ?
C1 C5 1.396(7) . ?
C1 C6 1.473(7) . ?
C2 C3 1.398(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.370(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.378(7) . ?
C6 C9 1.415(7) . ?
C7 C8 1.472(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.490(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.452(5) 2_565 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C16 1.391(7) . ?
C12 C13 1.399(8) . ?
C12 C17 1.472(7) . ?
C13 C14 1.368(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.384(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C20 1.385(7) . ?
C17 C18 1.410(7) . ?
C18 C19 1.495(7) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.474(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N6 1.455(6) 2 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O4 H4A 0.8954 . ?
O4 H4B 1.0288 . ?
N7 O1 1.181(7) . ?
N7 O2' 1.193(8) . ?
N7 O2 1.196(8) . ?
N7 O3' 1.211(9) . ?
N7 O1' 1.258(9) . ?
N7 O3 1.269(8) . ?

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 Cu1 N1 90.7(2) 3_655 . ?
N1 Cu1 N4 176.2(2) 3_655 . ?
N1 Cu1 N4 90.40(18) . . ?
N1 Cu1 N4 90.40(18) 3_655 3_655 ?
N1 Cu1 N4 176.2(2) . 3_655 ?
N4 Cu1 N4 88.8(2) . 3_655 ?
N1 Cu1 O3' 85.8(5) 3_655 3_655 ?
N1 Cu1 O3' 85.7(5) . 3_655 ?
N4 Cu1 O3' 90.6(5) . 3_655 ?
N4 Cu1 O3' 98.0(5) 3_655 3_655 ?
N1 Cu1 O3' 85.7(5) 3_655 . ?
N1 Cu1 O3' 85.8(5) . . ?
N4 Cu1 O3' 98.0(5) . . ?
N4 Cu1 O3' 90.6(5) 3_655 . ?
O3' Cu1 O3' 167.9(10) 3_655 . ?
C4 N1 C3 117.2(5) . . ?
C4 N1 Cu1 121.5(4) . . ?
C3 N1 Cu1 121.3(4) . . ?
C7 N2 N3 113.5(4) . . ?
C7 N2 C11 128.7(4) . . ?
N3 N2 C11 117.8(3) . . ?
C9 N3 N2 104.1(4) . . ?
C14 N4 C15 117.7(5) . . ?
C14 N4 Cu1 120.2(4) . . ?
C15 N4 Cu1 122.1(4) . . ?
C18 N5 N6 104.3(4) . . ?
C20 N6 N5 113.5(4) . . ?
C20 N6 C22 128.1(4) . . ?
N5 N6 C22 118.4(3) . . ?
C2 C1 C5 115.6(4) . . ?
C2 C1 C6 122.3(4) . . ?
C5 C1 C6 122.1(5) . . ?
C1 C2 C3 121.3(5) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
N1 C3 C2 121.9(5) . . ?
N1 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
N1 C4 C5 124.0(5) . . ?
N1 C4 H4 118.0 . . ?
C5 C4 H4 118.0 . . ?
C4 C5 C1 120.1(5) . . ?
C4 C5 H5 120.0 . . ?
C1 C5 H5 120.0 . . ?
C7 C6 C9 105.9(4) . . ?
C7 C6 C1 127.1(5) . . ?
C9 C6 C1 127.0(4) . . ?
N2 C7 C6 105.6(4) . . ?
N2 C7 C8 122.7(5) . . ?
C6 C7 C8 131.6(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 110.9(4) . . ?
N3 C9 C10 119.0(5) . . ?
C6 C9 C10 130.1(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N2 112.2(5) 2_565 . ?
N2 C11 H11A 109.2 2_565 . ?
N2 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 2_565 . ?
N2 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C16 C12 C13 116.6(5) . . ?
C16 C12 C17 123.0(5) . . ?
C13 C12 C17 120.4(5) . . ?
C14 C13 C12 120.6(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
N4 C14 C13 122.7(5) . . ?
N4 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
N4 C15 C16 122.6(5) . . ?
N4 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C12 119.8(5) . . ?
C15 C16 H16 120.1 . . ?
C12 C16 H16 120.1 . . ?
C20 C17 C18 105.9(4) . . ?
C20 C17 C12 127.7(5) . . ?
C18 C17 C12 126.4(5) . . ?
N5 C18 C17 111.1(4) . . ?
N5 C18 C19 119.2(4) . . ?
C17 C18 C19 129.4(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C17 105.2(4) . . ?
N6 C20 C21 123.4(5) . . ?
C17 C20 C21 131.4(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 N6 111.8(6) 2 . ?
N6 C22 H22A 109.3 2 . ?
N6 C22 H22A 109.3 . . ?
N6 C22 H22B 109.3 2 . ?
N6 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
H4A O4 H4B 100.7 . . ?
O1 N7 O2' 119.9(12) . . ?
O1 N7 O2 129.3(9) . . ?
O2' N7 O2 76.5(12) . . ?
O2' N7 O3' 125.4(10) . . ?
O2 N7 O3' 153.8(12) . . ?
O1 N7 O1' 111.6(12) . . ?
O2' N7 O1' 119.0(10) . . ?
O2 N7 O1' 45.0(11) . . ?
O3' N7 O1' 115.6(9) . . ?
O1 N7 O3 115.6(8) . . ?
O2' N7 O3 71.8(13) . . ?
O2 N7 O3 115.0(8) . . ?
O3' N7 O3 87.7(11) . . ?
O1' N7 O3 113.2(15) . . ?
N7 O3' Cu1 168.2(14) . . ?

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
N1 Cu1 N1 C4 -55.1(4) 3_655 . . . ?
O3' Cu1 N1 C4 -140.9(7) 3_655 . . . ?
O3' Cu1 N1 C4 30.5(7) . . . . ?
N1 Cu1 N1 C3 127.2(6) 3_655 . . . ?
N4 Cu1 N1 C3 -49.2(5) . . . . ?
O3' Cu1 N1 C3 41.4(7) 3_655 . . . ?
O3' Cu1 N1 C3 -147.2(7) . . . . ?
C7 N2 N3 C9 -1.4(5) . . . . ?
C11 N2 N3 C9 -178.9(4) . . . . ?
N1 Cu1 N4 C14 129.9(4) . . . . ?
N4 Cu1 N4 C14 -53.8(4) 3_655 . . . ?
O3' Cu1 N4 C14 44.2(7) 3_655 . . . ?
O3' Cu1 N4 C14 -144.2(6) . . . . ?
N1 Cu1 N4 C15 -51.7(5) . . . . ?
N4 Cu1 N4 C15 124.6(5) 3_655 . . . ?
O3' Cu1 N4 C15 -137.4(7) 3_655 . . . ?
O3' Cu1 N4 C15 34.2(7) . . . . ?
C18 N5 N6 C20 -1.0(5) . . . . ?
C18 N5 N6 C22 179.8(4) . . . . ?
C5 C1 C2 C3 -0.3(8) . . . . ?
C6 C1 C2 C3 179.7(5) . . . . ?
C4 N1 C3 C2 1.1(9) . . . . ?
Cu1 N1 C3 C2 178.8(4) . . . . ?
C1 C2 C3 N1 -0.7(9) . . . . ?
C3 N1 C4 C5 -0.5(10) . . . . ?
Cu1 N1 C4 C5 -178.3(5) . . . . ?
N1 C4 C5 C1 -0.4(10) . . . . ?
C2 C1 C5 C4 0.8(9) . . . . ?
C6 C1 C5 C4 -179.1(5) . . . . ?
C2 C1 C6 C7 45.6(8) . . . . ?
C5 C1 C6 C7 -134.4(6) . . . . ?
C2 C1 C6 C9 -133.0(6) . . . . ?
C5 C1 C6 C9 47.0(8) . . . . ?
N3 N2 C7 C6 0.6(6) . . . . ?
C11 N2 C7 C6 177.8(4) . . . . ?
N3 N2 C7 C8 177.8(5) . . . . ?
C11 N2 C7 C8 -5.0(8) . . . . ?
C9 C6 C7 N2 0.4(5) . . . . ?
C1 C6 C7 N2 -178.4(5) . . . . ?
C9 C6 C7 C8 -176.4(6) . . . . ?
C1 C6 C7 C8 4.7(9) . . . . ?
N2 N3 C9 C6 1.6(5) . . . . ?
N2 N3 C9 C10 -178.9(4) . . . . ?
C7 C6 C9 N3 -1.3(6) . . . . ?
C1 C6 C9 N3 177.5(5) . . . . ?
C7 C6 C9 C10 179.3(5) . . . . ?
C1 C6 C9 C10 -1.9(9) . . . . ?
C7 N2 C11 N2 -94.1(5) . . . 2_565 ?
N3 N2 C11 N2 82.9(3) . . . 2_565 ?
C16 C12 C13 C14 0.8(8) . . . . ?
C17 C12 C13 C14 -179.3(5) . . . . ?
C15 N4 C14 C13 -0.9(9) . . . . ?
Cu1 N4 C14 C13 177.5(5) . . . . ?
C12 C13 C14 N4 0.1(9) . . . . ?
C14 N4 C15 C16 0.8(9) . . . . ?
Cu1 N4 C15 C16 -177.6(5) . . . . ?
N4 C15 C16 C12 0.1(9) . . . . ?
C13 C12 C16 C15 -0.9(8) . . . . ?
C17 C12 C16 C15 179.2(5) . . . . ?
C16 C12 C17 C20 53.2(8) . . . . ?
C13 C12 C17 C20 -126.7(6) . . . . ?
C16 C12 C17 C18 -126.2(6) . . . . ?
C13 C12 C17 C18 53.9(8) . . . . ?
N6 N5 C18 C17 0.8(5) . . . . ?
N6 N5 C18 C19 174.5(4) . . . . ?
C20 C17 C18 N5 -0.4(6) . . . . ?
C12 C17 C18 N5 179.0(5) . . . . ?
C20 C17 C18 C19 -173.3(5) . . . . ?
C12 C17 C18 C19 6.1(9) . . . . ?
N5 N6 C20 C17 0.7(6) . . . . ?
C22 N6 C20 C17 179.9(5) . . . . ?
N5 N6 C20 C21 -179.4(5) . . . . ?
C22 N6 C20 C21 -0.2(9) . . . . ?
C18 C17 C20 N6 -0.2(6) . . . . ?
C12 C17 C20 N6 -179.6(5) . . . . ?
C18 C17 C20 C21 180.0(6) . . . . ?
C12 C17 C20 C21 0.5(10) . . . . ?
C20 N6 C22 N6 105.2(5) . . . 2 ?
N5 N6 C22 N6 -75.7(4) . . . 2 ?
O1 N7 O3' Cu1 -55(7) . . . . ?
O2' N7 O3' Cu1 -145(7) . . . . ?
O2 N7 O3' Cu1 -2(9) . . . . ?
O1' N7 O3' Cu1 34(7) . . . . ?
O3 N7 O3' Cu1 149(7) . . . . ?
N1 Cu1 O3' N7 -118(7) 3_655 . . . ?
N1 Cu1 O3' N7 151(7) . . . . ?
N4 Cu1 O3' N7 61(7) . . . . ?
N4 Cu1 O3' N7 -28(7) 3_655 . . . ?
O3' Cu1 O3' N7 -164(7) 3_655 . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.105

#===END

data_4
_database_code_depnum_ccdc_archive 'CCDC 692039'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H44 Cd Cl2 N12'
_chemical_formula_weight         900.20

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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/c

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                   12.6199(10)
_cell_length_b                   7.8969(6)
_cell_length_c                   25.1700(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.632(3)
_cell_angle_gamma                90.00
_cell_volume                     2403.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4926
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      25.66

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             924
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8663
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_process_details   SADABS

_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  'Apex II 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            12720
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4245
_reflns_number_gt                3477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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)+(0.1223P)²+0.5042P] 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         4245
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1896
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_restrained_S_all      1.304
_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 1.0000 0.0000 1.0000 0.0358(2) Uani 1 2 d S . .
Cl1 Cl 1.09248(10) 0.22202(17) 0.95030(6) 0.0557(4) Uani 1 1 d . . .
N1 N 0.8341(3) 0.1649(5) 0.97512(15) 0.0411(9) Uani 1 1 d . . .
N2 N 0.3617(4) 0.5318(5) 0.9071(2) 0.0456(10) Uani 1 1 d . . .
N3 N 0.4188(4) 0.6776(6) 0.90608(19) 0.0531(11) Uani 1 1 d . . .
N4 N 0.1953(4) 0.5338(5) 0.83142(18) 0.0446(10) Uani 1 1 d . . .
N5 N 0.1831(4) 0.3795(6) 0.80595(18) 0.0557(12) Uani 1 1 d . . .
C1 C 0.6369(4) 0.3543(6) 0.94487(19) 0.0420(11) Uani 1 1 d . . .
C2 C 0.6518(4) 0.2171(6) 0.9820(2) 0.0480(11) Uani 1 1 d . . .
H2 H 0.5958 0.1868 0.9974 0.058 Uiso 1 1 calc R . .
C3 C 0.7493(4) 0.1284(6) 0.99535(19) 0.0453(11) Uani 1 1 d . . .
H3 H 0.7571 0.0379 1.0198 0.054 Uiso 1 1 calc R . .
C4 C 0.8209(4) 0.2961(7) 0.9408(2) 0.0504(12) Uani 1 1 d . . .
H4 H 0.8794 0.3255 0.9271 0.060 Uiso 1 1 calc R . .
C5 C 0.7251(4) 0.3915(7) 0.9244(2) 0.0535(13) Uani 1 1 d . . .
H5 H 0.7199 0.4806 0.8996 0.064 Uiso 1 1 calc R . .
C6 C 0.5340(4) 0.4521(7) 0.9289(2) 0.0445(11) Uani 1 1 d . . .
C7 C 0.4280(4) 0.3951(7) 0.9204(2) 0.0444(11) Uani 1 1 d . . .
C8 C 0.3816(5) 0.2199(7) 0.9209(3) 0.0674(16) Uani 1 1 d . . .
H8A H 0.3115 0.2120 0.8932 0.101 Uiso 1 1 calc R . .
H8B H 0.3721 0.1972 0.9567 0.101 Uiso 1 1 calc R . .
H8C H 0.4318 0.1385 0.9132 0.101 Uiso 1 1 calc R . .
C9 C 0.5241(4) 0.6288(7) 0.9195(2) 0.0503(12) Uani 1 1 d . . .
C10 C 0.6101(5) 0.7603(8) 0.9224(3) 0.0771(19) Uani 1 1 d . . .
H10A H 0.5788 0.8706 0.9235 0.116 Uiso 1 1 calc R . .
H10B H 0.6366 0.7518 0.8904 0.116 Uiso 1 1 calc R . .
H10C H 0.6705 0.7435 0.9553 0.116 Uiso 1 1 calc R . .
C11 C 0.2414(4) 0.5397(7) 0.8908(2) 0.0477(12) Uani 1 1 d . . .
H11A H 0.2129 0.4454 0.9073 0.057 Uiso 1 1 calc R . .
H11B H 0.2184 0.6436 0.9048 0.057 Uiso 1 1 calc R . .
C12 C 0.1721(4) 0.6636(6) 0.7941(2) 0.0456(11) Uani 1 1 d . . .
C13 C 0.1751(6) 0.8423(7) 0.8132(2) 0.0710(18) Uani 1 1 d . . .
H13A H 0.2503 0.8813 0.8247 0.107 Uiso 1 1 calc R . .
H13B H 0.1443 0.8489 0.8439 0.107 Uiso 1 1 calc R . .
H13C H 0.1327 0.9119 0.7834 0.107 Uiso 1 1 calc R . .
C14 C 0.1424(4) 0.5897(7) 0.7417(2) 0.0455(11) Uani 1 1 d . . .
C15 C 0.1500(5) 0.4122(7) 0.7521(2) 0.0515(13) Uani 1 1 d . . .
C16 C 0.1274(7) 0.2668(7) 0.7123(3) 0.084(2) Uani 1 1 d . . .
H16A H 0.0505 0.2665 0.6917 0.127 Uiso 1 1 calc R . .
H16B H 0.1454 0.1625 0.7324 0.127 Uiso 1 1 calc R . .
H16C H 0.1717 0.2782 0.6872 0.127 Uiso 1 1 calc R . .
C17 C 0.1142(4) 0.6735(6) 0.68801(19) 0.0429(11) Uani 1 1 d . . .
C18 C 0.0467(4) 0.6004(6) 0.6401(2) 0.0486(12) Uani 1 1 d . . .
H18 H 0.0166 0.4937 0.6417 0.058 Uiso 1 1 calc R . .
C21 C 0.1603(5) 0.8255(7) 0.6804(2) 0.0619(15) Uani 1 1 d . . .
H21 H 0.2115 0.8761 0.7103 0.074 Uiso 1 1 calc R . .
C19 C 0.0237(5) 0.6842(7) 0.5899(2) 0.0537(13) Uani 1 1 d . . .
H19 H -0.0202 0.6299 0.5585 0.064 Uiso 1 1 calc R . .
N6 N 0.0612(4) 0.8389(5) 0.58412(16) 0.0502(10) Uani 1 1 d . . .
C20 C 0.1324(5) 0.9062(8) 0.6289(2) 0.0669(16) Uani 1 1 d . . .
H20 H 0.1644 1.0104 0.6258 0.080 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 N1 2.392(4) 3_757 ?
Cd1 N1 2.392(4) . ?
Cd1 N6 2.400(4) 4_666 ?
Cd1 N6 2.400(4) 2_646 ?
Cd1 Cl1 2.6148(12) . ?
Cd1 Cl1 2.6148(12) 3_757 ?
N1 C4 1.328(6) . ?
N1 C3 1.341(6) . ?
N2 C7 1.349(6) . ?
N2 N3 1.363(6) . ?
N2 C11 1.456(7) . ?
N3 C9 1.331(7) . ?
N4 N5 1.364(6) . ?
N4 C12 1.365(6) . ?
N4 C11 1.441(7) . ?
N5 C15 1.323(7) . ?
C1 C5 1.385(7) . ?
C1 C2 1.408(7) . ?
C1 C6 1.464(7) . ?
C2 C3 1.372(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.384(7) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.370(7) . ?
C6 C9 1.415(7) . ?
C7 C8 1.503(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.489(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.392(7) . ?
C12 C13 1.488(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.424(8) . ?
C14 C17 1.454(7) . ?
C15 C16 1.497(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.371(7) . ?
C17 C18 1.388(7) . ?
C18 C19 1.382(7) . ?
C18 H18 0.9300 . ?
C21 C20 1.395(7) . ?
C21 H21 0.9300 . ?
C19 N6 1.333(7) . ?
C19 H19 0.9300 . ?
N6 C20 1.335(7) . ?
N6 Cd1 2.400(4) 2_666 ?
C20 H20 0.9300 . ?

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 Cd1 N1 180.000(2) 3_757 . ?
N1 Cd1 N6 91.19(14) 3_757 4_666 ?
N1 Cd1 N6 88.81(14) . 4_666 ?
N1 Cd1 N6 88.81(14) 3_757 2_646 ?
N1 Cd1 N6 91.19(14) . 2_646 ?
N6 Cd1 N6 180.000(1) 4_666 2_646 ?
N1 Cd1 Cl1 90.75(10) 3_757 . ?
N1 Cd1 Cl1 89.25(10) . . ?
N6 Cd1 Cl1 89.52(11) 4_666 . ?
N6 Cd1 Cl1 90.48(11) 2_646 . ?
N1 Cd1 Cl1 89.25(10) 3_757 3_757 ?
N1 Cd1 Cl1 90.75(10) . 3_757 ?
N6 Cd1 Cl1 90.48(11) 4_666 3_757 ?
N6 Cd1 Cl1 89.52(11) 2_646 3_757 ?
Cl1 Cd1 Cl1 180.0 . 3_757 ?
C4 N1 C3 116.7(4) . . ?
C4 N1 Cd1 122.2(3) . . ?
C3 N1 Cd1 121.2(3) . . ?
C7 N2 N3 112.8(4) . . ?
C7 N2 C11 128.9(5) . . ?
N3 N2 C11 118.2(4) . . ?
C9 N3 N2 104.2(4) . . ?
N5 N4 C12 111.9(4) . . ?
N5 N4 C11 118.3(4) . . ?
C12 N4 C11 129.3(5) . . ?
C15 N5 N4 105.5(4) . . ?
C5 C1 C2 116.2(4) . . ?
C5 C1 C6 122.0(5) . . ?
C2 C1 C6 121.8(4) . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
N1 C3 C2 123.7(5) . . ?
N1 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
N1 C4 C5 123.7(5) . . ?
N1 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C4 C5 C1 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C1 C5 H5 120.0 . . ?
C7 C6 C9 105.2(4) . . ?
C7 C6 C1 128.3(5) . . ?
C9 C6 C1 126.5(5) . . ?
N2 C7 C6 106.6(5) . . ?
N2 C7 C8 121.6(5) . . ?
C6 C7 C8 131.8(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 111.3(5) . . ?
N3 C9 C10 118.1(5) . . ?
C6 C9 C10 130.6(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N2 111.7(4) . . ?
N4 C11 H11A 109.3 . . ?
N2 C11 H11A 109.3 . . ?
N4 C11 H11B 109.3 . . ?
N2 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 C14 106.5(4) . . ?
N4 C12 C13 120.6(5) . . ?
C14 C12 C13 132.8(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 104.6(4) . . ?
C12 C14 C17 128.1(5) . . ?
C15 C14 C17 127.2(4) . . ?
N5 C15 C14 111.4(5) . . ?
N5 C15 C16 118.7(5) . . ?
C14 C15 C16 129.9(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 114.9(4) . . ?
C21 C17 C14 121.9(5) . . ?
C18 C17 C14 123.0(5) . . ?
C19 C18 C17 120.8(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C17 C21 C20 121.7(5) . . ?
C17 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
N6 C19 C18 123.4(5) . . ?
N6 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
C19 N6 C20 116.6(5) . . ?
C19 N6 Cd1 123.1(3) . 2_666 ?
C20 N6 Cd1 120.2(4) . 2_666 ?
N6 C20 C21 122.2(5) . . ?
N6 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.124

#===END

data_5a
_database_code_depnum_ccdc_archive 'CCDC 692040'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H49.50 Cd2 N7.50 O13.50'
_chemical_formula_weight         1100.19

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   P21/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                   16.893(14)
_cell_length_b                   16.155(13)
_cell_length_c                   20.514(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.628(8)
_cell_angle_gamma                90.00
_cell_volume                     5240(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8715
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      23.18

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2232
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_process_details   sadabs

_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  'Apex II 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            24155
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.03
_reflns_number_total             9016
_reflns_number_gt                5878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the lattice DMF and methanol
molecules in order to improve the refinement stability. In addition, the soft
"SADI" constraint was imposed on the carbon atoms of this DMF. Some carbon
atoms of pypz and DMF ligands (C13, C15, C42, and C43) were refined using the
pseudo-isotropic "ISOR" restraint, as the free refinement gave unrealistic
anisotropic displacement parameters. Rigid bond (DELU) restraint was also
used to treat these atoms.
;

_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)+(0.0608P)²+278.9506P] 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         9016
_refine_ls_number_parameters     630
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.1195
_refine_ls_wR_factor_ref         0.3318
_refine_ls_wR_factor_gt          0.3122
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.078
_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 0.25336(8) -0.08208(8) 0.25552(8) 0.0397(4) Uani 1 1 d . . .
Cd2 Cd 0.17751(8) -0.01491(9) 0.06599(9) 0.0465(5) Uani 1 1 d . . .
O1 O 0.0867(10) -0.2088(10) 0.1677(9) 0.070(5) Uani 1 1 d . . .
O2 O 0.1544(10) -0.1637(10) 0.2754(9) 0.077(5) Uani 1 1 d . . .
O3 O -0.1548(10) -0.4764(11) 0.2841(9) 0.080(5) Uani 1 1 d . . .
O4 O -0.0922(7) -0.4368(8) 0.3931(7) 0.041(3) Uani 1 1 d . . .
O5 O 0.2995(10) 0.0491(10) 0.1228(10) 0.072(5) Uani 1 1 d . . .
O6 O 0.3476(9) -0.0022(10) 0.2307(9) 0.070(5) Uani 1 1 d . . .
O7 O 0.6769(11) 0.2764(13) 0.3297(11) 0.100(7) Uani 1 1 d . . .
O8 O 0.6527(9) 0.3119(9) 0.2168(11) 0.078(6) Uani 1 1 d . . .
O9 O 0.0524(8) -0.0905(9) 0.0103(8) 0.061(4) Uani 1 1 d . . .
O10 O 0.1991(7) -0.1244(8) 0.1419(7) 0.045(3) Uani 1 1 d . . .
H10' H 0.1459 -0.1527 0.1338 0.054 Uiso 1 1 calc R . .
H10" H 0.2379 -0.1634 0.1331 0.054 Uiso 1 1 calc R . .
O11 O 0.2453(12) -0.1017(11) 0.0059(11) 0.086(6) Uani 1 1 d . . .
N1 N 0.2789(9) -0.0218(10) 0.3624(9) 0.046(4) Uani 1 1 d . . .
N2 N 0.2597(15) 0.2130(12) 0.6073(15) 0.078(7) Uani 1 1 d . . .
N3 N 0.3389(14) 0.1860(12) 0.6461(13) 0.079(7) Uani 1 1 d . . .
N4 N 0.1184(19) 0.1614(16) 0.6506(17) 0.118(11) Uani 1 1 d . . .
N5 N 0.1802(15) 0.2154(14) 0.6819(16) 0.088(9) Uani 1 1 d . . .
N6 N 0.1633(11) 0.0611(12) 0.9654(10) 0.060(5) Uani 1 1 d . . .
N7 N 0.2856(15) -0.2131(16) -0.0364(12) 0.084(7) Uani 1 1 d . . .
N8 N 0.783(2) 0.0652(19) 0.3350(17) 0.074(13) Uani 0.50 1 d PD . .
C1 C 0.2185(12) -0.0156(14) 0.3860(12) 0.054(6) Uani 1 1 d . . .
H1 H 0.1694 -0.0460 0.3647 0.065 Uiso 1 1 calc R . .
C2 C 0.2232(15) 0.0347(17) 0.4421(13) 0.069(7) Uani 1 1 d . . .
H2 H 0.1772 0.0359 0.4571 0.082 Uiso 1 1 calc R . .
C3 C 0.2907(13) 0.0817(13) 0.4757(12) 0.056(6) Uani 1 1 d . . .
C4 C 0.3552(15) 0.0723(17) 0.4507(12) 0.066(7) Uani 1 1 d . . .
H4 H 0.4057 0.1000 0.4732 0.079 Uiso 1 1 calc R . .
C5 C 0.3494(12) 0.0255(15) 0.3957(12) 0.060(6) Uani 1 1 d . . .
H5 H 0.3943 0.0247 0.3794 0.071 Uiso 1 1 calc R . .
C6 C 0.2949(13) 0.1326(13) 0.5338(14) 0.062(7) Uani 1 1 d . . .
C7 C 0.2318(15) 0.1840(15) 0.5405(16) 0.066(7) Uani 1 1 d . . .
C8 C 0.1473(18) 0.207(2) 0.4886(15) 0.098(11) Uani 1 1 d . . .
H8A H 0.1041 0.1746 0.4966 0.147 Uiso 1 1 calc R . .
H8B H 0.1469 0.1970 0.4424 0.147 Uiso 1 1 calc R . .
H8C H 0.1368 0.2648 0.4935 0.147 Uiso 1 1 calc R . .
C9 C 0.3572(15) 0.1387(14) 0.6014(13) 0.060(6) Uani 1 1 d U . .
C10 C 0.4461(15) 0.0936(19) 0.6264(18) 0.103(11) Uani 1 1 d . . .
H10A H 0.4769 0.1077 0.6741 0.154 Uiso 1 1 calc R . .
H10B H 0.4776 0.1110 0.5979 0.154 Uiso 1 1 calc R . .
H10C H 0.4377 0.0348 0.6224 0.154 Uiso 1 1 calc R . .
C11 C 0.212(2) 0.2666(16) 0.637(2) 0.108(13) Uani 1 1 d . . .
H11A H 0.1647 0.2915 0.6002 0.130 Uiso 1 1 calc R . .
H11B H 0.2475 0.3105 0.6640 0.130 Uiso 1 1 calc R . .
C12 C 0.2063(15) 0.2130(14) 0.752(2) 0.085(10) Uani 1 1 d . . .
C13 C 0.2675(19) 0.2711(18) 0.8032(19) 0.107(12) Uani 1 1 d . . .
H13A H 0.3201 0.2714 0.7952 0.161 Uiso 1 1 calc R . .
H13B H 0.2769 0.2529 0.8499 0.161 Uiso 1 1 calc R . .
H13C H 0.2442 0.3260 0.7969 0.161 Uiso 1 1 calc R . .
C14 C 0.1580(15) 0.1507(15) 0.7707(17) 0.073(8) Uani 1 1 d . . .
C15 C 0.1044(18) 0.1216(19) 0.7005(14) 0.080(9) Uani 1 1 d . . .
C16 C 0.032(2) 0.057(2) 0.6893(18) 0.139(18) Uani 1 1 d . . .
H16A H -0.0133 0.0812 0.7007 0.209 Uiso 1 1 calc R . .
H16B H 0.0536 0.0095 0.7189 0.209 Uiso 1 1 calc R . .
H16C H 0.0111 0.0390 0.6415 0.209 Uiso 1 1 calc R . .
C17 C 0.1605(14) 0.1234(16) 0.8351(19) 0.081(9) Uani 1 1 d . . .
C18 C 0.2348(17) 0.1203(18) 0.8956(17) 0.082(9) Uani 1 1 d . . .
H18 H 0.2848 0.1420 0.8934 0.098 Uiso 1 1 calc R . .
C19 C 0.2355(16) 0.0863(17) 0.958(2) 0.110(13) Uani 1 1 d . . .
H19 H 0.2865 0.0809 0.9948 0.132 Uiso 1 1 calc R . .
C20 C 0.0940(14) 0.0742(18) 0.9114(15) 0.074(7) Uani 1 1 d . . .
H20 H 0.0434 0.0668 0.9191 0.089 Uiso 1 1 calc R . .
C21 C 0.0866(17) 0.0980(16) 0.8439(14) 0.076(8) Uani 1 1 d . . .
H21 H 0.0351 0.0968 0.8071 0.091 Uiso 1 1 calc R . .
C22 C 0.1013(11) -0.2076(11) 0.2313(11) 0.041(5) Uani 1 1 d . . .
C23 C 0.0501(12) -0.2668(11) 0.2588(12) 0.046(5) Uani 1 1 d . . .
C24 C -0.0081(13) -0.3204(13) 0.2135(11) 0.053(5) Uani 1 1 d . . .
H24 H -0.0138 -0.3214 0.1667 0.064 Uiso 1 1 calc R . .
C25 C -0.0574(13) -0.3719(14) 0.2368(13) 0.058(6) Uani 1 1 d . . .
H25 H -0.0981 -0.4048 0.2050 0.070 Uiso 1 1 calc R . .
C26 C -0.0475(11) -0.3757(12) 0.3068(11) 0.043(5) Uani 1 1 d . . .
C27 C 0.012(2) -0.326(2) 0.3513(19) 0.149(19) Uani 1 1 d . . .
H27 H 0.0228 -0.3300 0.3988 0.179 Uiso 1 1 calc R . .
C28 C 0.0562(18) -0.2696(18) 0.3285(14) 0.089(10) Uani 1 1 d . . .
H28 H 0.0913 -0.2321 0.3600 0.107 Uiso 1 1 calc R . .
C29 C -0.0999(11) -0.4363(11) 0.3304(14) 0.050(6) Uani 1 1 d . . .
C30 C 0.3499(13) 0.0441(12) 0.1847(16) 0.058(7) Uani 1 1 d . . .
C31 C 0.4294(13) 0.1003(13) 0.2045(16) 0.069(8) Uani 1 1 d . . .
C32 C 0.4809(15) 0.1103(15) 0.2710(15) 0.075(8) Uani 1 1 d . . .
H32 H 0.4690 0.0801 0.3050 0.090 Uiso 1 1 calc R . .
C33 C 0.5502(16) 0.1621(17) 0.2925(16) 0.088(10) Uani 1 1 d . . .
H33 H 0.5842 0.1679 0.3390 0.106 Uiso 1 1 calc R . .
C34 C 0.5661(12) 0.2077(12) 0.2360(15) 0.060(7) Uani 1 1 d . . .
C35 C 0.6399(14) 0.2699(13) 0.2614(13) 0.055(6) Uani 1 1 d . . .
C36 C 0.5166(12) 0.1988(15) 0.1713(13) 0.057(6) Uani 1 1 d . . .
H36 H 0.5270 0.2298 0.1370 0.069 Uiso 1 1 calc R . .
C37 C 0.4490(13) 0.1448(14) 0.1524(13) 0.059(6) Uani 1 1 d . . .
H37 H 0.4164 0.1374 0.1056 0.071 Uiso 1 1 calc R . .
C38 C 0.260(2) -0.168(2) 0.004(2) 0.122(15) Uani 1 1 d . . .
H38 H 0.2513 -0.1987 0.0391 0.146 Uiso 1 1 calc R . .
C39 C 0.299(3) -0.173(3) -0.0889(19) 0.19(2) Uani 1 1 d . . .
H39A H 0.2935 -0.1142 -0.0832 0.279 Uiso 1 1 calc R . .
H39B H 0.2576 -0.1901 -0.1324 0.279 Uiso 1 1 calc R . .
H39C H 0.3545 -0.1850 -0.0886 0.279 Uiso 1 1 calc R . .
C40 C 0.293(4) -0.297(3) -0.040(3) 0.23(3) Uani 1 1 d . . .
H40A H 0.3470 -0.3109 -0.0420 0.345 Uiso 1 1 calc R . .
H40B H 0.2491 -0.3175 -0.0812 0.345 Uiso 1 1 calc R . .
H40C H 0.2865 -0.3223 0.0003 0.345 Uiso 1 1 calc R . .
O12 O 0.846(4) 0.101(4) 0.442(3) 0.15(2) Uani 0.50 1 d P . .
C41 C 0.837(3) 0.121(3) 0.3873(18) 0.19(6) Uani 0.50 1 d PD . .
H41 H 0.8614 0.1678 0.3766 0.230 Uiso 0.50 1 calc PR . .
C42 C 0.744(4) -0.005(3) 0.356(3) 0.12(2) Uani 0.50 1 d PDU . .
H42A H 0.7008 0.0140 0.3720 0.177 Uiso 0.50 1 calc PR . .
H42B H 0.7864 -0.0346 0.3921 0.177 Uiso 0.50 1 calc PR . .
H42C H 0.7199 -0.0409 0.3163 0.177 Uiso 0.50 1 calc PR . .
C43 C 0.763(3) 0.084(3) 0.2619(16) 0.14(3) Uani 0.50 1 d PD . .
H43A H 0.8144 0.0922 0.2529 0.207 Uiso 0.50 1 calc PR . .
H43B H 0.7289 0.1327 0.2500 0.207 Uiso 0.50 1 calc PR . .
H43C H 0.7323 0.0381 0.2344 0.207 Uiso 0.50 1 calc PR . .
O13 O 0.0567(19) 0.7390(17) 0.012(2) 0.198(16) Uani 1 1 d . . .
O14 O 0.489(2) 0.151(6) 0.912(2) 0.18(3) Uani 0.50 1 d PD . .
O15 O 0.463(3) 0.223(4) 0.970(2) 0.15(2) Uani 0.50 1 d P . .
C44 C 0.490(5) 0.118(4) 0.846(4) 0.19(6) Uani 0.50 1 d PD . .


_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 O6 2.243(14) . ?
Cd1 O8 2.268(14) 2_645 ?
Cd1 O2 2.276(16) . ?
Cd1 O10 2.288(13) . ?
Cd1 N1 2.297(17) . ?
Cd1 O3 2.322(14) 2 ?
Cd2 O5 2.231(15) . ?
Cd2 O4 2.286(11) 2 ?
Cd2 O10 2.300(13) . ?
Cd2 N6 2.340(19) 1_554 ?
Cd2 O9 2.358(14) . ?
Cd2 O11 2.406(17) . ?
O1 C22 1.24(2) . ?
O2 C22 1.25(2) . ?
O3 C29 1.25(2) . ?
O3 Cd1 2.322(14) 2_545 ?
O4 C29 1.25(3) . ?
O4 Cd2 2.286(11) 2_545 ?
O5 C30 1.26(3) . ?
O6 C30 1.22(3) . ?
O7 C35 1.32(3) . ?
O8 C35 1.22(3) . ?
O8 Cd1 2.268(14) 2_655 ?
O10 H10' 0.9700 . ?
O10 H10" 0.9700 . ?
O11 C38 1.11(3) . ?
N1 C1 1.28(2) . ?
N1 C5 1.38(3) . ?
N2 N3 1.36(3) . ?
N2 C7 1.37(3) . ?
N2 C11 1.46(3) . ?
N3 C9 1.31(3) . ?
N4 C15 1.30(4) . ?
N4 N5 1.34(3) . ?
N5 C12 1.35(4) . ?
N5 C11 1.47(4) . ?
N6 C20 1.31(3) . ?
N6 C19 1.35(3) . ?
N6 Cd2 2.340(19) 1_556 ?
N7 C38 1.28(3) . ?
N7 C39 1.34(3) . ?
N7 C40 1.37(4) . ?
N8 C42 1.443(10) . ?
N8 C43 1.446(10) . ?
N8 C41 1.447(10) . ?
C1 C2 1.39(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.34(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.37(3) . ?
C3 C6 1.43(3) . ?
C4 C5 1.33(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.40(3) . ?
C6 C9 1.42(3) . ?
C7 C8 1.50(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.58(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.43(3) . ?
C12 C13 1.51(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C17 1.38(4) . ?
C14 C15 1.48(4) . ?
C15 C16 1.57(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.38(4) . ?
C17 C18 1.42(4) . ?
C18 C19 1.39(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.40(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.53(2) . ?
C23 C24 1.39(3) . ?
C23 C28 1.40(3) . ?
C24 C25 1.38(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.39(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.36(3) . ?
C26 C29 1.51(3) . ?
C27 C28 1.36(3) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C30 C31 1.55(3) . ?
C31 C32 1.35(4) . ?
C31 C37 1.42(3) . ?
C32 C33 1.38(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.48(4) . ?
C33 H33 0.9300 . ?
C34 C36 1.30(3) . ?
C34 C35 1.54(3) . ?
C36 C37 1.38(3) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
O12 C41 1.13(6) . ?
C41 H41 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
O14 C44 1.449(10) . ?

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 Cd1 O8 90.1(6) . 2_645 ?
O6 Cd1 O2 177.4(6) . . ?
O8 Cd1 O2 90.6(6) 2_645 . ?
O6 Cd1 O10 90.1(6) . . ?
O8 Cd1 O10 91.3(6) 2_645 . ?
O2 Cd1 O10 87.3(5) . . ?
O6 Cd1 N1 93.6(6) . . ?
O8 Cd1 N1 101.7(6) 2_645 . ?
O2 Cd1 N1 88.7(6) . . ?
O10 Cd1 N1 166.5(5) . . ?
O6 Cd1 O3 88.7(6) . 2 ?
O8 Cd1 O3 174.5(7) 2_645 2 ?
O2 Cd1 O3 90.4(7) . 2 ?
O10 Cd1 O3 83.3(5) . 2 ?
N1 Cd1 O3 83.8(6) . 2 ?
O5 Cd2 O4 97.9(6) . 2 ?
O5 Cd2 O10 96.1(6) . . ?
O4 Cd2 O10 98.4(5) 2 . ?
O5 Cd2 N6 90.4(7) . 1_554 ?
O4 Cd2 N6 98.8(6) 2 1_554 ?
O10 Cd2 N6 160.6(6) . 1_554 ?
O5 Cd2 O9 176.2(6) . . ?
O4 Cd2 O9 83.7(5) 2 . ?
O10 Cd2 O9 80.3(5) . . ?
N6 Cd2 O9 92.8(6) 1_554 . ?
O5 Cd2 O11 91.1(7) . . ?
O4 Cd2 O11 170.1(6) 2 . ?
O10 Cd2 O11 84.7(6) . . ?
N6 Cd2 O11 76.9(7) 1_554 . ?
O9 Cd2 O11 87.6(6) . . ?
C22 O2 Cd1 125.9(15) . . ?
C29 O3 Cd1 153.6(16) . 2_545 ?
C29 O4 Cd2 122.2(11) . 2_545 ?
C30 O5 Cd2 132.1(15) . . ?
C30 O6 Cd1 138.6(14) . . ?
C35 O8 Cd1 121.8(16) . 2_655 ?
Cd1 O10 Cd2 111.8(5) . . ?
Cd1 O10 H10' 109.3 . . ?
Cd2 O10 H10' 109.3 . . ?
Cd1 O10 H10" 109.3 . . ?
Cd2 O10 H10" 109.3 . . ?
H10' O10 H10" 107.9 . . ?
C38 O11 Cd2 138(3) . . ?
C1 N1 C5 115.8(18) . . ?
C1 N1 Cd1 119.2(14) . . ?
C5 N1 Cd1 123.2(13) . . ?
N3 N2 C7 113(2) . . ?
N3 N2 C11 121(3) . . ?
C7 N2 C11 125(3) . . ?
C9 N3 N2 102(2) . . ?
C15 N4 N5 106(3) . . ?
N4 N5 C12 113(3) . . ?
N4 N5 C11 117(3) . . ?
C12 N5 C11 129(2) . . ?
C20 N6 C19 115(3) . . ?
C20 N6 Cd2 127.8(16) . 1_556 ?
C19 N6 Cd2 116(2) . 1_556 ?
C38 N7 C39 115(4) . . ?
C38 N7 C40 131(4) . . ?
C39 N7 C40 113(4) . . ?
C42 N8 C43 120.1(6) . . ?
C42 N8 C41 120.0(6) . . ?
C43 N8 C41 119.8(6) . . ?
N1 C1 C2 123(2) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 123(2) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C2 C3 C4 113(2) . . ?
C2 C3 C6 123(2) . . ?
C4 C3 C6 124(2) . . ?
C5 C4 C3 123(2) . . ?
C5 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
C4 C5 N1 121.9(19) . . ?
C4 C5 H5 119.1 . . ?
N1 C5 H5 119.1 . . ?
C7 C6 C3 128(2) . . ?
C7 C6 C9 101(2) . . ?
C3 C6 C9 131(2) . . ?
N2 C7 C6 107(2) . . ?
N2 C7 C8 122(2) . . ?
C6 C7 C8 130(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 117(2) . . ?
N3 C9 C10 118(2) . . ?
C6 C9 C10 125(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N5 108(2) . . ?
N2 C11 H11A 110.1 . . ?
N5 C11 H11A 110.1 . . ?
N2 C11 H11B 110.1 . . ?
N5 C11 H11B 110.1 . . ?
H11A C11 H11B 108.5 . . ?
N5 C12 C14 108(3) . . ?
N5 C12 C13 127(3) . . ?
C14 C12 C13 125(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C12 131(3) . . ?
C17 C14 C15 129(2) . . ?
C12 C14 C15 100(3) . . ?
N4 C15 C14 113(3) . . ?
N4 C15 C16 124(3) . . ?
C14 C15 C16 122(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 C21 120(3) . . ?
C14 C17 C18 125(2) . . ?
C21 C17 C18 116(3) . . ?
C19 C18 C17 122(3) . . ?
C19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
N6 C19 C18 121(3) . . ?
N6 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
N6 C20 C21 128(2) . . ?
N6 C20 H20 115.8 . . ?
C21 C20 H20 115.8 . . ?
C17 C21 C20 116(3) . . ?
C17 C21 H21 122.0 . . ?
C20 C21 H21 122.0 . . ?
O1 C22 O2 126.8(18) . . ?
O1 C22 C23 116.8(18) . . ?
O2 C22 C23 116.4(19) . . ?
C24 C23 C28 116.4(19) . . ?
C24 C23 C22 120(2) . . ?
C28 C23 C22 123.5(18) . . ?
C25 C24 C23 121(2) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 121.3(19) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 117(2) . . ?
C27 C26 C29 123(2) . . ?
C25 C26 C29 119.4(19) . . ?
C28 C27 C26 122(3) . . ?
C28 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C27 C28 C23 121(3) . . ?
C27 C28 H28 119.3 . . ?
C23 C28 H28 119.3 . . ?
O4 C29 O3 124.1(18) . . ?
O4 C29 C26 118.4(18) . . ?
O3 C29 C26 117(2) . . ?
O6 C30 O5 128.8(19) . . ?
O6 C30 C31 115(2) . . ?
O5 C30 C31 116(2) . . ?
C32 C31 C37 117.7(19) . . ?
C32 C31 C30 122(2) . . ?
C37 C31 C30 121(2) . . ?
C31 C32 C33 125(3) . . ?
C31 C32 H32 117.6 . . ?
C33 C32 H32 117.6 . . ?
C32 C33 C34 115(2) . . ?
C32 C33 H33 122.5 . . ?
C34 C33 H33 122.5 . . ?
C36 C34 C33 121.0(19) . . ?
C36 C34 C35 125(2) . . ?
C33 C34 C35 114(2) . . ?
O8 C35 O7 127.6(19) . . ?
O8 C35 C34 116(2) . . ?
O7 C35 C34 116(2) . . ?
C34 C36 C37 122(2) . . ?
C34 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
C36 C37 C31 120(2) . . ?
C36 C37 H37 120.1 . . ?
C31 C37 H37 120.1 . . ?
O11 C38 N7 135(5) . . ?
O11 C38 H38 112.6 . . ?
N7 C38 H38 112.6 . . ?
N7 C39 H39A 109.5 . . ?
N7 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N7 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N7 C40 H40A 109.5 . . ?
N7 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N7 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O12 C41 N8 113(4) . . ?
O12 C41 H41 123.3 . . ?
N8 C41 H41 123.3 . . ?
N8 C42 H42A 109.5 . . ?
N8 C42 H42B 109.5 . . ?
N8 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N8 C43 H43A 109.5 . . ?
N8 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N8 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 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
O8 Cd1 O2 C22 -90.5(18) 2_645 . . . ?
O10 Cd1 O2 C22 0.8(17) . . . . ?
N1 Cd1 O2 C22 167.8(18) . . . . ?
O3 Cd1 O2 C22 84.0(18) 2 . . . ?
O4 Cd2 O5 C30 79(2) 2 . . . ?
O10 Cd2 O5 C30 -20(2) . . . . ?
N6 Cd2 O5 C30 178(2) 1_554 . . . ?
O11 Cd2 O5 C30 -105(2) . . . . ?
O8 Cd1 O6 C30 133(2) 2_645 . . . ?
O10 Cd1 O6 C30 41(2) . . . . ?
N1 Cd1 O6 C30 -126(2) . . . . ?
O3 Cd1 O6 C30 -42(2) 2 . . . ?
O6 Cd1 O10 Cd2 -46.4(6) . . . . ?
O8 Cd1 O10 Cd2 -136.4(6) 2_645 . . . ?
O2 Cd1 O10 Cd2 133.0(6) . . . . ?
N1 Cd1 O10 Cd2 60(2) . . . . ?
O3 Cd1 O10 Cd2 42.3(6) 2 . . . ?
O5 Cd2 O10 Cd1 43.1(7) . . . . ?
O4 Cd2 O10 Cd1 -55.9(6) 2 . . . ?
N6 Cd2 O10 Cd1 151.9(14) 1_554 . . . ?
O9 Cd2 O10 Cd1 -137.9(6) . . . . ?
O11 Cd2 O10 Cd1 133.6(6) . . . . ?
O5 Cd2 O11 C38 115(4) . . . . ?
O10 Cd2 O11 C38 19(4) . . . . ?
N6 Cd2 O11 C38 -155(4) 1_554 . . . ?
O9 Cd2 O11 C38 -62(4) . . . . ?
O6 Cd1 N1 C1 147.6(16) . . . . ?
O8 Cd1 N1 C1 -121.6(16) 2_645 . . . ?
O2 Cd1 N1 C1 -31.2(16) . . . . ?
O10 Cd1 N1 C1 42(3) . . . . ?
O3 Cd1 N1 C1 59.4(16) 2 . . . ?
O6 Cd1 N1 C5 -16.6(17) . . . . ?
O8 Cd1 N1 C5 74.2(17) 2_645 . . . ?
O2 Cd1 N1 C5 164.6(17) . . . . ?
O10 Cd1 N1 C5 -122(2) . . . . ?
O3 Cd1 N1 C5 -104.9(17) 2 . . . ?
C7 N2 N3 C9 -1(3) . . . . ?
C11 N2 N3 C9 178(2) . . . . ?
C15 N4 N5 C12 -1(3) . . . . ?
C15 N4 N5 C11 177(2) . . . . ?
C5 N1 C1 C2 -1(3) . . . . ?
Cd1 N1 C1 C2 -166.0(17) . . . . ?
N1 C1 C2 C3 1(4) . . . . ?
C1 C2 C3 C4 -2(3) . . . . ?
C1 C2 C3 C6 -179(2) . . . . ?
C2 C3 C4 C5 4(4) . . . . ?
C6 C3 C4 C5 -179(2) . . . . ?
C3 C4 C5 N1 -4(4) . . . . ?
C1 N1 C5 C4 2(3) . . . . ?
Cd1 N1 C5 C4 167.1(19) . . . . ?
C2 C3 C6 C7 -44(4) . . . . ?
C4 C3 C6 C7 139(2) . . . . ?
C2 C3 C6 C9 128(3) . . . . ?
C4 C3 C6 C9 -48(4) . . . . ?
N3 N2 C7 C6 1(3) . . . . ?
C11 N2 C7 C6 -178(2) . . . . ?
N3 N2 C7 C8 -179(2) . . . . ?
C11 N2 C7 C8 2(4) . . . . ?
C3 C6 C7 N2 173(2) . . . . ?
C9 C6 C7 N2 -1(2) . . . . ?
C3 C6 C7 C8 -7(4) . . . . ?
C9 C6 C7 C8 179(3) . . . . ?
N2 N3 C9 C6 1(3) . . . . ?
N2 N3 C9 C10 -180(2) . . . . ?
C7 C6 C9 N3 0(3) . . . . ?
C3 C6 C9 N3 -173(2) . . . . ?
C7 C6 C9 C10 -179(2) . . . . ?
C3 C6 C9 C10 7(4) . . . . ?
N3 N2 C11 N5 -75(3) . . . . ?
C7 N2 C11 N5 104(3) . . . . ?
N4 N5 C11 N2 -71(4) . . . . ?
C12 N5 C11 N2 107(3) . . . . ?
N4 N5 C12 C14 1(3) . . . . ?
C11 N5 C12 C14 -178(2) . . . . ?
N4 N5 C12 C13 -173(2) . . . . ?
C11 N5 C12 C13 9(4) . . . . ?
N5 C12 C14 C17 179(2) . . . . ?
C13 C12 C14 C17 -7(4) . . . . ?
N5 C12 C14 C15 0(3) . . . . ?
C13 C12 C14 C15 174(2) . . . . ?
N5 N4 C15 C14 1(3) . . . . ?
N5 N4 C15 C16 175(3) . . . . ?
C17 C14 C15 N4 180(3) . . . . ?
C12 C14 C15 N4 -1(3) . . . . ?
C17 C14 C15 C16 6(5) . . . . ?
C12 C14 C15 C16 -175(3) . . . . ?
C12 C14 C17 C21 146(2) . . . . ?
C15 C14 C17 C21 -35(4) . . . . ?
C12 C14 C17 C18 -33(4) . . . . ?
C15 C14 C17 C18 146(3) . . . . ?
C14 C17 C18 C19 -175(3) . . . . ?
C21 C17 C18 C19 6(4) . . . . ?
C20 N6 C19 C18 -3(4) . . . . ?
Cd2 N6 C19 C18 170(2) 1_556 . . . ?
C17 C18 C19 N6 -6(5) . . . . ?
C19 N6 C20 C21 12(4) . . . . ?
Cd2 N6 C20 C21 -160(2) 1_556 . . . ?
C14 C17 C21 C20 -178(2) . . . . ?
C18 C17 C21 C20 1(3) . . . . ?
N6 C20 C21 C17 -11(4) . . . . ?
Cd1 O2 C22 O1 -8(3) . . . . ?
Cd1 O2 C22 C23 171.2(12) . . . . ?
O1 C22 C23 C24 2(3) . . . . ?
O2 C22 C23 C24 -177.4(19) . . . . ?
O1 C22 C23 C28 -177(2) . . . . ?
O2 C22 C23 C28 4(3) . . . . ?
C28 C23 C24 C25 1(3) . . . . ?
C22 C23 C24 C25 -177(2) . . . . ?
C23 C24 C25 C26 -4(3) . . . . ?
C24 C25 C26 C27 1(4) . . . . ?
C24 C25 C26 C29 -176.9(19) . . . . ?
C25 C26 C27 C28 5(5) . . . . ?
C29 C26 C27 C28 -178(3) . . . . ?
C26 C27 C28 C23 -8(6) . . . . ?
C24 C23 C28 C27 4(4) . . . . ?
C22 C23 C28 C27 -177(3) . . . . ?
Cd2 O4 C29 O3 1(3) 2_545 . . . ?
Cd2 O4 C29 C26 173.2(11) 2_545 . . . ?
Cd1 O3 C29 O4 -21(5) 2_545 . . . ?
Cd1 O3 C29 C26 167(3) 2_545 . . . ?
C27 C26 C29 O4 5(4) . . . . ?
C25 C26 C29 O4 -177.6(18) . . . . ?
C27 C26 C29 O3 177(3) . . . . ?
C25 C26 C29 O3 -5(3) . . . . ?
Cd1 O6 C30 O5 -19(4) . . . . ?
Cd1 O6 C30 C31 165.4(16) . . . . ?
Cd2 O5 C30 O6 5(4) . . . . ?
Cd2 O5 C30 C31 -179.8(14) . . . . ?
O6 C30 C31 C32 -14(3) . . . . ?
O5 C30 C31 C32 169(2) . . . . ?
O6 C30 C31 C37 167(2) . . . . ?
O5 C30 C31 C37 -9(3) . . . . ?
C37 C31 C32 C33 2(4) . . . . ?
C30 C31 C32 C33 -177(3) . . . . ?
C31 C32 C33 C34 -1(4) . . . . ?
C32 C33 C34 C36 1(4) . . . . ?
C32 C33 C34 C35 176(2) . . . . ?
Cd1 O8 C35 O7 -1(4) 2_655 . . . ?
Cd1 O8 C35 C34 172.0(13) 2_655 . . . ?
C36 C34 C35 O8 -1(3) . . . . ?
C33 C34 C35 O8 -176(2) . . . . ?
C36 C34 C35 O7 173(2) . . . . ?
C33 C34 C35 O7 -2(3) . . . . ?
C33 C34 C36 C37 -2(4) . . . . ?
C35 C34 C36 C37 -177(2) . . . . ?
C34 C36 C37 C31 3(4) . . . . ?
C32 C31 C37 C36 -3(3) . . . . ?
C30 C31 C37 C36 176(2) . . . . ?
Cd2 O11 C38 N7 168(3) . . . . ?
C39 N7 C38 O11 0(6) . . . . ?
C40 N7 C38 O11 -171(4) . . . . ?
C42 N8 C41 O12 2(8) . . . . ?
C43 N8 C41 O12 178(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         2.326
_refine_diff_density_min         -2.078
_refine_diff_density_rms         0.217

#===END

data_5b
_database_code_depnum_ccdc_archive 'CCDC 692041'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33.50 H41.50 Cd N7.50 O8'
_chemical_formula_weight         789.64

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           Orthorhombic
_symmetry_space_group_name_H-M   Pccn

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

_cell_length_a                   28.816(6)
_cell_length_b                   14.330(3)
_cell_length_c                   21.034(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8686(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5682
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      27.37

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8272
_exptl_absorpt_correction_T_max  0.8468
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            44960
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.01
_reflns_number_total             7645
_reflns_number_gt                6052
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the lattice DMF molecules in
order to improve the refinement stability, which were also refined using the
pseudo-isotropic "ISOR" restraint, as the free refinement gave unrealistic
anisotropic displacement parameters. In addition, the soft "SADI" constraint
was imposed on the carbon atoms of both molecules and the "FLAT" constraint
was used to treat one of them (C33, C34, C35, and N8).
;

_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)+(0.1093P)²+19.9782P] 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         7645
_refine_ls_number_parameters     541
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1880
_refine_ls_wR_factor_gt          0.1742
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.060
_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 0.063865(13) 0.39633(2) 0.410809(14) 0.03635(16) Uani 1 1 d . . .
O1 O 0.0770(2) 0.4036(3) 0.29452(19) 0.0722(13) Uani 1 1 d . A .
O2 O 0.05807(13) 0.2716(3) 0.33824(15) 0.0494(9) Uani 1 1 d . A .
O3 O 0.05863(14) 0.0669(3) 0.03265(17) 0.0527(10) Uani 1 1 d . . .
O4 O 0.05719(14) 0.2081(3) -0.00696(16) 0.0516(9) Uani 1 1 d . . .
O5 O -0.01587(14) 0.4223(3) 0.40084(18) 0.0551(9) Uani 1 1 d . . .
H5A H -0.0265 0.4705 0.4194 0.083 Uiso 1 1 d R . .
H5B H -0.0330 0.3740 0.4005 0.083 Uiso 1 1 d R . .
N1 N 0.06635(15) 0.5582(3) 0.40180(19) 0.0421(10) Uani 1 1 d . . .
N2 N 0.07329(16) 1.0056(3) 0.3989(2) 0.0439(10) Uani 1 1 d . A .
N3 N 0.07827(18) 0.9968(3) 0.3351(2) 0.0535(11) Uani 1 1 d . A .
N4 N 0.13202(16) 1.0982(3) 0.4495(2) 0.0475(10) Uani 1 1 d . A .
N5 N 0.14137(18) 1.0689(4) 0.5087(2) 0.0671(14) Uani 1 1 d . A .
N6 N 0.35365(17) 1.1137(3) 0.4234(2) 0.0521(11) Uani 1 1 d . . .
C1 C 0.06494(17) 0.7540(3) 0.3877(2) 0.0405(11) Uani 1 1 d . . .
C2 C 0.0800(6) 0.7099(8) 0.4452(5) 0.050(3) Uani 0.64(3) 1 d P A 1
H2 H 0.0906 0.7461 0.4789 0.060 Uiso 0.64(3) 1 calc PR A 1
C3 C 0.0790(6) 0.6149(7) 0.4507(5) 0.046(3) Uani 0.64(3) 1 d P A 1
H3 H 0.0874 0.5880 0.4893 0.056 Uiso 0.64(3) 1 calc PR A 1
C4 C 0.0504(4) 0.6002(9) 0.3508(7) 0.044(3) Uani 0.64(3) 1 d P A 1
H4 H 0.0384 0.5630 0.3185 0.052 Uiso 0.64(3) 1 calc PR A 1
C5 C 0.0502(5) 0.6941(6) 0.3418(5) 0.041(3) Uani 0.64(3) 1 d P A 1
H5 H 0.0396 0.7180 0.3033 0.049 Uiso 0.64(3) 1 calc PR A 1
C2' C 0.0524(14) 0.7104(14) 0.4388(11) 0.063(8) Uani 0.36(3) 1 d P A 2
H2' H 0.0426 0.7449 0.4738 0.076 Uiso 0.36(3) 1 calc PR A 2
C3' C 0.0531(13) 0.6153(16) 0.4428(12) 0.061(7) Uani 0.36(3) 1 d P A 2
H3' H 0.0425 0.5900 0.4808 0.073 Uiso 0.36(3) 1 calc PR A 2
C4' C 0.0764(18) 0.6015(16) 0.3463(12) 0.080(11) Uani 0.36(3) 1 d P A 2
H4' H 0.0814 0.5637 0.3111 0.096 Uiso 0.36(3) 1 calc PR A 2
C5' C 0.0800(17) 0.6949(14) 0.3374(10) 0.080(11) Uani 0.36(3) 1 d P A 2
H5' H 0.0919 0.7194 0.2999 0.096 Uiso 0.36(3) 1 calc PR A 2
C6 C 0.06680(17) 0.8553(3) 0.3796(2) 0.0408(11) Uani 1 1 d . A .
C7 C 0.06581(18) 0.9224(4) 0.4281(3) 0.0424(11) Uani 1 1 d . . .
C8 C 0.0569(3) 0.9137(4) 0.4964(3) 0.0675(19) Uani 1 1 d . A .
H8A H 0.0413 0.9687 0.5114 0.101 Uiso 1 1 calc R . .
H8B H 0.0859 0.9067 0.5186 0.101 Uiso 1 1 calc R . .
H8C H 0.0378 0.8601 0.5041 0.101 Uiso 1 1 calc R . .
C9 C 0.0735(2) 0.9066(4) 0.3236(3) 0.0519(14) Uani 1 1 d . . .
C10 C 0.0745(4) 0.8735(5) 0.2553(3) 0.098(3) Uani 1 1 d . A .
H10A H 0.0458 0.8430 0.2453 0.148 Uiso 1 1 calc R . .
H10B H 0.0997 0.8305 0.2496 0.148 Uiso 1 1 calc R . .
H10C H 0.0787 0.9261 0.2276 0.148 Uiso 1 1 calc R . .
C11 C 0.0843(2) 1.0951(3) 0.4281(3) 0.0450(12) Uani 1 1 d . . .
H11A H 0.0790 1.1447 0.3976 0.054 Uiso 1 1 calc R A .
H11B H 0.0638 1.1054 0.4641 0.054 Uiso 1 1 calc R . .
C12 C 0.1705(2) 1.1145(4) 0.4156(2) 0.0485(13) Uani 1 1 d . . .
C13 C 0.1693(2) 1.1517(6) 0.3498(3) 0.0771(19) Uani 1 1 d . A .
H13A H 0.1661 1.1010 0.3203 0.116 Uiso 1 1 calc R . .
H13B H 0.1976 1.1847 0.3412 0.116 Uiso 1 1 calc R . .
H13C H 0.1435 1.1935 0.3454 0.116 Uiso 1 1 calc R . .
C14 C 0.2075(2) 1.0983(4) 0.4564(3) 0.0558(14) Uani 1 1 d . A .
C15 C 0.1862(2) 1.0697(6) 0.5136(3) 0.0717(18) Uani 1 1 d . . .
C16 C 0.2107(3) 1.0367(11) 0.5737(4) 0.146(5) Uani 1 1 d . A .
H16A H 0.2435 1.0341 0.5661 0.219 Uiso 1 1 calc R . .
H16B H 0.1996 0.9757 0.5849 0.219 Uiso 1 1 calc R . .
H16C H 0.2044 1.0794 0.6077 0.219 Uiso 1 1 calc R . .
C17 C 0.2573(2) 1.1058(4) 0.4429(3) 0.0555(14) Uani 1 1 d . . .
C18 C 0.2871(2) 1.1493(5) 0.4858(3) 0.0643(15) Uani 1 1 d . A .
H18 H 0.2751 1.1767 0.5224 0.077 Uiso 1 1 calc R . .
C19 C 0.3347(2) 1.1520(4) 0.4740(3) 0.0586(14) Uani 1 1 d . . .
H19 H 0.3538 1.1822 0.5031 0.070 Uiso 1 1 calc R A .
C20 C 0.3254(2) 1.0748(5) 0.3816(3) 0.0711(17) Uani 1 1 d . . .
H20 H 0.3384 1.0491 0.3450 0.085 Uiso 1 1 calc R A .
C21 C 0.2776(2) 1.0699(5) 0.3889(3) 0.0737(18) Uani 1 1 d . A .
H21 H 0.2594 1.0426 0.3575 0.088 Uiso 1 1 calc R . .
C22 C 0.06760(18) 0.3197(4) 0.2907(2) 0.0449(12) Uani 1 1 d . . .
C23 C 0.06688(18) 0.2740(3) 0.2260(2) 0.0438(12) Uani 1 1 d . A .
C24 C 0.06383(18) 0.1796(3) 0.2190(2) 0.0462(12) Uani 1 1 d . . .
H24 H 0.0629 0.1415 0.2548 0.055 Uiso 1 1 calc R A .
C25 C 0.06209(19) 0.1395(4) 0.1585(2) 0.0471(12) Uani 1 1 d . A .
H25 H 0.0611 0.0749 0.1542 0.057 Uiso 1 1 calc R . .
C26 C 0.06179(17) 0.1947(3) 0.1053(2) 0.0407(11) Uani 1 1 d . . .
C27 C 0.0653(3) 0.2888(4) 0.1126(3) 0.082(3) Uani 1 1 d . A .
H27 H 0.0661 0.3270 0.0769 0.099 Uiso 1 1 calc R . .
C28 C 0.0678(3) 0.3282(4) 0.1726(3) 0.091(3) Uani 1 1 d . . .
H28 H 0.0702 0.3927 0.1766 0.109 Uiso 1 1 calc R A .
C29 C 0.05860(16) 0.1533(4) 0.0395(2) 0.0416(11) Uani 1 1 d U A .
C30 C 0.0534(3) 0.7773(5) 0.6300(4) 0.106(3) Uani 1 1 d DU B 1
H30 H 0.0219 0.7633 0.6282 0.127 Uiso 1 1 calc R B 1
C31 C 0.0301(3) 0.9273(7) 0.6742(6) 0.157(5) Uani 1 1 d DU B 1
H31A H 0.0390 0.9613 0.7116 0.235 Uiso 1 1 calc R B 1
H31B H 0.0020 0.8934 0.6825 0.235 Uiso 1 1 calc R B 1
H31C H 0.0252 0.9701 0.6398 0.235 Uiso 1 1 calc R B 1
C32 C 0.1121(3) 0.8892(7) 0.6633(6) 0.150(5) Uani 1 1 d DU B 1
H32A H 0.1316 0.8390 0.6493 0.225 Uiso 1 1 calc R B 1
H32B H 0.1188 0.9031 0.7070 0.225 Uiso 1 1 calc R B 1
H32C H 0.1179 0.9435 0.6378 0.225 Uiso 1 1 calc R B 1
C33 C 0.3403(6) 0.9542(14) 0.6088(9) 0.150(8) Uani 0.50 1 d PDU . .
H33A H 0.3426 1.0209 0.6052 0.225 Uiso 0.50 1 calc PR . .
H33B H 0.3315 0.9283 0.5685 0.225 Uiso 0.50 1 calc PR . .
H33C H 0.3698 0.9291 0.6214 0.225 Uiso 0.50 1 calc PR . .
C34 C 0.2819(9) 0.8416(16) 0.6527(13) 0.218(14) Uani 0.50 1 d PDU . .
H34A H 0.2871 0.8076 0.6914 0.327 Uiso 0.50 1 calc PR . .
H34B H 0.2938 0.8063 0.6175 0.327 Uiso 0.50 1 calc PR . .
H34C H 0.2493 0.8518 0.6471 0.327 Uiso 0.50 1 calc PR . .
C35 C 0.2948(11) 0.9957(18) 0.7064(12) 0.237(18) Uani 0.50 1 d PDU . .
H35 H 0.3115 1.0497 0.7153 0.284 Uiso 0.50 1 calc PR . .
N7 N 0.0661(2) 0.8634(5) 0.6575(3) 0.097(2) Uani 1 1 d DU . .
N8 N 0.3057(5) 0.9306(12) 0.6561(7) 0.158(7) Uani 0.50 1 d PDU . .
O6 O 0.0795(2) 0.7216(4) 0.6091(3) 0.0940(16) Uani 1 1 d U . .
O7 O 0.2637(11) 0.972(2) 0.7329(15) 0.274(13) Uani 0.50 1 d PU . .
O8 O 0.2651(13) 0.274(3) 0.7105(17) 0.169(14) Uani 0.25 1 d PU . 1
O8' O 0.3005(18) 0.250(4) 0.674(2) 0.22(2) Uani 0.25 1 d PU C 2
O9 O 0.1901(7) 0.7858(15) 0.4072(9) 0.168(7) Uani 0.50 1 d PU D 3
O9' O 0.1903(12) 0.730(2) 0.3420(16) 0.291(15) Uani 0.50 1 d PU E 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O4 2.296(3) 7_566 ?
Cd1 N1 2.328(4) . ?
Cd1 O5 2.337(4) . ?
Cd1 O2 2.356(3) . ?
Cd1 N6 2.396(5) 2_565 ?
Cd1 O1 2.477(4) . ?
Cd1 O3 2.621(4) 7_566 ?
Cd1 C22 2.757(5) . ?
O1 C22 1.234(6) . ?
O2 C22 1.245(6) . ?
O3 C29 1.247(7) . ?
O3 Cd1 2.621(4) 7_565 ?
O4 C29 1.255(6) . ?
O4 Cd1 2.296(3) 7_565 ?
O5 H5A 0.8509 . ?
O5 H5B 0.8501 . ?
N1 C3' 1.25(2) . ?
N1 C4 1.313(14) . ?
N1 C4' 1.35(3) . ?
N1 C3 1.361(12) . ?
N2 N3 1.355(6) . ?
N2 C7 1.358(7) . ?
N2 C11 1.456(6) . ?
N3 C9 1.322(7) . ?
N4 C12 1.339(7) . ?
N4 N5 1.341(7) . ?
N4 C11 1.448(7) . ?
N5 C15 1.295(8) . ?
N6 C19 1.317(7) . ?
N6 C20 1.321(8) . ?
N6 Cd1 2.396(5) 2_565 ?
C1 C2' 1.29(2) . ?
C1 C5 1.361(10) . ?
C1 C5' 1.42(2) . ?
C1 C2 1.431(13) . ?
C1 C6 1.463(7) . ?
C2 C3 1.367(15) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.360(15) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C2' C3' 1.37(3) . ?
C2' H2' 0.9300 . ?
C3' H3' 0.9300 . ?
C4' C5' 1.35(3) . ?
C4' H4' 0.9300 . ?
C5' H5' 0.9300 . ?
C6 C7 1.402(8) . ?
C6 C9 1.403(7) . ?
C7 C8 1.465(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.513(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.389(8) . ?
C12 C13 1.482(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.413(9) . ?
C14 C17 1.467(8) . ?
C15 C16 1.523(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.377(9) . ?
C17 C18 1.391(8) . ?
C18 C19 1.394(8) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.389(9) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.509(7) . ?
C23 C24 1.364(7) . ?
C23 C28 1.367(8) . ?
C24 C25 1.398(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.371(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.360(7) . ?
C26 C29 1.508(6) . ?
C27 C28 1.385(8) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C30 O6 1.182(9) . ?
C30 N7 1.411(8) . ?
C30 H30 0.9300 . ?
C31 N7 1.427(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 N7 1.382(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N8 1.450(10) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N8 1.449(10) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 O7 1.11(4) . ?
C35 N8 1.445(10) . ?
C35 H35 0.9300 . ?
O8 O8 1.11(6) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cd1 N1 135.52(14) 7_566 . ?
O4 Cd1 O5 95.11(14) 7_566 . ?
N1 Cd1 O5 82.20(14) . . ?
O4 Cd1 O2 89.29(13) 7_566 . ?
N1 Cd1 O2 134.83(13) . . ?
O5 Cd1 O2 89.60(13) . . ?
O4 Cd1 N6 87.76(15) 7_566 2_565 ?
N1 Cd1 N6 92.18(15) . 2_565 ?
O5 Cd1 N6 174.15(14) . 2_565 ?
O2 Cd1 N6 95.54(14) . 2_565 ?
O4 Cd1 O1 141.63(12) 7_566 . ?
N1 Cd1 O1 82.72(13) . . ?
O5 Cd1 O1 93.16(16) . . ?
O2 Cd1 O1 53.33(12) . . ?
N6 Cd1 O1 87.70(17) 2_565 . ?
O4 Cd1 O3 52.39(12) 7_566 7_566 ?
N1 Cd1 O3 83.15(13) . 7_566 ?
O5 Cd1 O3 89.95(13) . 7_566 ?
O2 Cd1 O3 141.45(12) . 7_566 ?
N6 Cd1 O3 87.77(14) 2_565 7_566 ?
O1 Cd1 O3 164.98(13) . 7_566 ?
O4 Cd1 C22 115.73(14) 7_566 . ?
N1 Cd1 C22 108.72(14) . . ?
O5 Cd1 C22 91.12(14) . . ?
O2 Cd1 C22 26.74(14) . . ?
N6 Cd1 C22 92.22(16) 2_565 . ?
O1 Cd1 C22 26.60(14) . . ?
O3 Cd1 C22 168.11(14) 7_566 . ?
C22 O1 Cd1 89.4(3) . . ?
C22 O2 Cd1 94.9(3) . . ?
C29 O3 Cd1 85.0(3) . 7_565 ?
C29 O4 Cd1 100.1(3) . 7_565 ?
Cd1 O5 H5A 116.3 . . ?
Cd1 O5 H5B 116.2 . . ?
H5A O5 H5B 117.1 . . ?
C3' N1 C4 99.0(13) . . ?
C3' N1 C4' 111.1(15) . . ?
C4 N1 C3 116.0(8) . . ?
C4' N1 C3 108.6(13) . . ?
C3' N1 Cd1 126.0(11) . . ?
C4 N1 Cd1 120.8(6) . . ?
C4' N1 Cd1 122.3(10) . . ?
C3 N1 Cd1 122.8(5) . . ?
N3 N2 C7 112.4(4) . . ?
N3 N2 C11 118.5(4) . . ?
C7 N2 C11 128.1(4) . . ?
C9 N3 N2 105.2(4) . . ?
C12 N4 N5 112.5(5) . . ?
C12 N4 C11 128.8(5) . . ?
N5 N4 C11 118.0(5) . . ?
C15 N5 N4 105.8(5) . . ?
C19 N6 C20 117.3(5) . . ?
C19 N6 Cd1 121.8(4) . 2_565 ?
C20 N6 Cd1 120.8(4) . 2_565 ?
C2' C1 C5 101.4(12) . . ?
C2' C1 C5' 114.5(13) . . ?
C5 C1 C2 114.6(7) . . ?
C5' C1 C2 105.8(12) . . ?
C2' C1 C6 125.9(10) . . ?
C5 C1 C6 123.7(6) . . ?
C5' C1 C6 119.5(9) . . ?
C2 C1 C6 121.7(6) . . ?
C3 C2 C1 120.3(9) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
N1 C3 C2 122.4(10) . . ?
N1 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
N1 C4 C5 124.7(10) . . ?
N1 C4 H4 117.6 . . ?
C5 C4 H4 117.6 . . ?
C4 C5 C1 121.6(9) . . ?
C4 C5 H5 119.2 . . ?
C1 C5 H5 119.2 . . ?
C1 C2' C3' 121.9(18) . . ?
C1 C2' H2' 119.0 . . ?
C3' C2' H2' 119.0 . . ?
N1 C3' C2' 128(2) . . ?
N1 C3' H3' 116.0 . . ?
C2' C3' H3' 116.0 . . ?
N1 C4' C5' 126(2) . . ?
N1 C4' H4' 117.0 . . ?
C5' C4' H4' 117.0 . . ?
C4' C5' C1 117.5(17) . . ?
C4' C5' H5' 121.3 . . ?
C1 C5' H5' 121.3 . . ?
C7 C6 C9 104.7(4) . . ?
C7 C6 C1 126.5(5) . . ?
C9 C6 C1 128.6(5) . . ?
N2 C7 C6 105.7(5) . . ?
N2 C7 C8 123.0(5) . . ?
C6 C7 C8 131.2(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 111.8(5) . . ?
N3 C9 C10 118.6(5) . . ?
C6 C9 C10 129.5(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N2 111.4(4) . . ?
N4 C11 H11A 109.4 . . ?
N2 C11 H11A 109.4 . . ?
N4 C11 H11B 109.4 . . ?
N2 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N4 C12 C14 106.1(5) . . ?
N4 C12 C13 122.7(5) . . ?
C14 C12 C13 130.9(6) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 103.9(5) . . ?
C12 C14 C17 128.3(6) . . ?
C15 C14 C17 127.7(6) . . ?
N5 C15 C14 111.6(6) . . ?
N5 C15 C16 121.8(6) . . ?
C14 C15 C16 126.5(6) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 116.1(6) . . ?
C21 C17 C14 123.2(6) . . ?
C18 C17 C14 120.7(6) . . ?
C17 C18 C19 120.2(6) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
N6 C19 C18 122.7(6) . . ?
N6 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
N6 C20 C21 123.9(6) . . ?
N6 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C17 C21 C20 119.6(6) . . ?
C17 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
O1 C22 O2 122.3(5) . . ?
O1 C22 C23 119.0(5) . . ?
O2 C22 C23 118.7(4) . . ?
O1 C22 Cd1 64.0(3) . . ?
O2 C22 Cd1 58.4(3) . . ?
C23 C22 Cd1 176.2(4) . . ?
C24 C23 C28 118.4(5) . . ?
C24 C23 C22 121.9(4) . . ?
C28 C23 C22 119.6(5) . . ?
C23 C24 C25 120.6(5) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 120.4(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 118.6(5) . . ?
C27 C26 C29 119.9(5) . . ?
C25 C26 C29 121.4(5) . . ?
C26 C27 C28 120.8(5) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 121.1(5) . . ?
C23 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
O3 C29 O4 122.2(4) . . ?
O3 C29 C26 119.8(4) . . ?
O4 C29 C26 118.0(4) . . ?
O6 C30 N7 125.2(7) . . ?
O6 C30 H30 117.4 . . ?
N7 C30 H30 117.4 . . ?
N7 C31 H31A 109.5 . . ?
N7 C31 H31B 109.5 . . ?
N7 C31 H31C 109.5 . . ?
N7 C32 H32A 109.5 . . ?
N7 C32 H32B 109.5 . . ?
N7 C32 H32C 109.5 . . ?
N8 C33 H33A 109.5 . . ?
N8 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N8 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N8 C34 H34A 109.5 . . ?
N8 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N8 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O7 C35 N8 110(2) . . ?
O7 C35 H35 124.9 . . ?
N8 C35 H35 124.9 . . ?
C32 N7 C30 121.4(5) . . ?
C32 N7 C31 120.2(5) . . ?
C30 N7 C31 118.2(4) . . ?
C35 N8 C34 120.1(6) . . ?
C35 N8 C33 120.1(6) . . ?
C34 N8 C33 119.8(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
O4 Cd1 O1 C22 16.1(5) 7_566 . . . ?
N1 Cd1 O1 C22 -167.9(4) . . . . ?
O5 Cd1 O1 C22 -86.2(4) . . . . ?
O2 Cd1 O1 C22 1.0(3) . . . . ?
N6 Cd1 O1 C22 99.6(4) 2_565 . . . ?
O3 Cd1 O1 C22 172.1(5) 7_566 . . . ?
O4 Cd1 O2 C22 -171.6(3) 7_566 . . . ?
N1 Cd1 O2 C22 14.7(4) . . . . ?
O5 Cd1 O2 C22 93.3(3) . . . . ?
N6 Cd1 O2 C22 -83.9(3) 2_565 . . . ?
O1 Cd1 O2 C22 -0.9(3) . . . . ?
O3 Cd1 O2 C22 -177.3(3) 7_566 . . . ?
O4 Cd1 N1 C3' -18(2) 7_566 . . . ?
O5 Cd1 N1 C3' 71(2) . . . . ?
O2 Cd1 N1 C3' 152(2) . . . . ?
N6 Cd1 N1 C3' -108(2) 2_565 . . . ?
O1 Cd1 N1 C3' 165(2) . . . . ?
O3 Cd1 N1 C3' -20(2) 7_566 . . . ?
C22 Cd1 N1 C3' 159(2) . . . . ?
O4 Cd1 N1 C4 -149.7(8) 7_566 . . . ?
O5 Cd1 N1 C4 -60.3(8) . . . . ?
O2 Cd1 N1 C4 21.3(8) . . . . ?
N6 Cd1 N1 C4 121.3(8) 2_565 . . . ?
O1 Cd1 N1 C4 33.9(8) . . . . ?
O3 Cd1 N1 C4 -151.2(8) 7_566 . . . ?
C22 Cd1 N1 C4 28.2(8) . . . . ?
O4 Cd1 N1 C4' 171(3) 7_566 . . . ?
O5 Cd1 N1 C4' -99(3) . . . . ?
O2 Cd1 N1 C4' -18(3) . . . . ?
N6 Cd1 N1 C4' 82(3) 2_565 . . . ?
O1 Cd1 N1 C4' -5(3) . . . . ?
O3 Cd1 N1 C4' 170(3) 7_566 . . . ?
C22 Cd1 N1 C4' -11(3) . . . . ?
O4 Cd1 N1 C3 22.5(10) 7_566 . . . ?
O5 Cd1 N1 C3 111.9(10) . . . . ?
O2 Cd1 N1 C3 -166.5(9) . . . . ?
N6 Cd1 N1 C3 -66.5(10) 2_565 . . . ?
O1 Cd1 N1 C3 -153.9(10) . . . . ?
O3 Cd1 N1 C3 21.0(9) 7_566 . . . ?
C22 Cd1 N1 C3 -159.6(9) . . . . ?
C7 N2 N3 C9 0.4(6) . . . . ?
C11 N2 N3 C9 170.0(5) . . . . ?
C12 N4 N5 C15 2.4(7) . . . . ?
C11 N4 N5 C15 173.7(5) . . . . ?
C2' C1 C2 C3 73(2) . . . . ?
C5 C1 C2 C3 0.2(14) . . . . ?
C5' C1 C2 C3 -37(2) . . . . ?
C6 C1 C2 C3 -178.2(9) . . . . ?
C3' N1 C3 C2 -72(2) . . . . ?
C4 N1 C3 C2 -6.9(15) . . . . ?
C4' N1 C3 C2 28(2) . . . . ?
Cd1 N1 C3 C2 -179.4(9) . . . . ?
C1 C2 C3 N1 3.6(18) . . . . ?
C3' N1 C4 C5 37.5(18) . . . . ?
C4' N1 C4 C5 -78(2) . . . . ?
C3 N1 C4 C5 6.8(14) . . . . ?
Cd1 N1 C4 C5 179.5(8) . . . . ?
N1 C4 C5 C1 -3.2(16) . . . . ?
C2' C1 C5 C4 -33.6(17) . . . . ?
C5' C1 C5 C4 82.7(18) . . . . ?
C2 C1 C5 C4 -0.5(13) . . . . ?
C6 C1 C5 C4 177.9(8) . . . . ?
C5 C1 C2' C3' 35(3) . . . . ?
C5' C1 C2' C3' -1(3) . . . . ?
C2 C1 C2' C3' -83(3) . . . . ?
C6 C1 C2' C3' -177.9(17) . . . . ?
C4 N1 C3' C2' -38(3) . . . . ?
C4' N1 C3' C2' -6(3) . . . . ?
C3 N1 C3' C2' 86(3) . . . . ?
Cd1 N1 C3' C2' -177(2) . . . . ?
C1 C2' C3' N1 2(4) . . . . ?
C3' N1 C4' C5' 11(4) . . . . ?
C4 N1 C4' C5' 84(4) . . . . ?
C3 N1 C4' C5' -25(4) . . . . ?
Cd1 N1 C4' C5' -178(2) . . . . ?
N1 C4' C5' C1 -10(5) . . . . ?
C2' C1 C5' C4' 5(3) . . . . ?
C5 C1 C5' C4' -70(3) . . . . ?
C2 C1 C5' C4' 40(3) . . . . ?
C6 C1 C5' C4' -178(2) . . . . ?
C2' C1 C6 C7 16(2) . . . . ?
C5 C1 C6 C7 156.4(9) . . . . ?
C5' C1 C6 C7 -161(2) . . . . ?
C2 C1 C6 C7 -25.3(11) . . . . ?
C2' C1 C6 C9 -170(2) . . . . ?
C5 C1 C6 C9 -29.2(11) . . . . ?
C5' C1 C6 C9 13(2) . . . . ?
C2 C1 C6 C9 149.1(10) . . . . ?
N3 N2 C7 C6 1.0(6) . . . . ?
C11 N2 C7 C6 -167.3(5) . . . . ?
N3 N2 C7 C8 -176.8(6) . . . . ?
C11 N2 C7 C8 14.9(9) . . . . ?
C9 C6 C7 N2 -1.9(6) . . . . ?
C1 C6 C7 N2 173.6(5) . . . . ?
C9 C6 C7 C8 175.6(6) . . . . ?
C1 C6 C7 C8 -8.9(10) . . . . ?
N2 N3 C9 C6 -1.7(7) . . . . ?
N2 N3 C9 C10 176.5(6) . . . . ?
C7 C6 C9 N3 2.3(7) . . . . ?
C1 C6 C9 N3 -173.1(5) . . . . ?
C7 C6 C9 C10 -175.7(7) . . . . ?
C1 C6 C9 C10 8.9(11) . . . . ?
C12 N4 C11 N2 80.5(6) . . . . ?
N5 N4 C11 N2 -89.2(6) . . . . ?
N3 N2 C11 N4 -92.5(6) . . . . ?
C7 N2 C11 N4 75.2(7) . . . . ?
N5 N4 C12 C14 -2.5(6) . . . . ?
C11 N4 C12 C14 -172.7(4) . . . . ?
N5 N4 C12 C13 -177.0(6) . . . . ?
C11 N4 C12 C13 12.8(8) . . . . ?
N4 C12 C14 C15 1.6(6) . . . . ?
C13 C12 C14 C15 175.5(7) . . . . ?
N4 C12 C14 C17 179.7(5) . . . . ?
C13 C12 C14 C17 -6.4(10) . . . . ?
N4 N5 C15 C14 -1.2(8) . . . . ?
N4 N5 C15 C16 -177.3(9) . . . . ?
C12 C14 C15 N5 -0.2(8) . . . . ?
C17 C14 C15 N5 -178.4(6) . . . . ?
C12 C14 C15 C16 175.6(9) . . . . ?
C17 C14 C15 C16 -2.5(13) . . . . ?
C12 C14 C17 C21 -45.5(9) . . . . ?
C15 C14 C17 C21 132.3(8) . . . . ?
C12 C14 C17 C18 135.6(6) . . . . ?
C15 C14 C17 C18 -46.7(9) . . . . ?
C21 C17 C18 C19 -2.2(9) . . . . ?
C14 C17 C18 C19 176.9(5) . . . . ?
C20 N6 C19 C18 2.8(9) . . . . ?
Cd1 N6 C19 C18 -172.6(5) 2_565 . . . ?
C17 C18 C19 N6 -0.8(10) . . . . ?
C19 N6 C20 C21 -1.9(10) . . . . ?
Cd1 N6 C20 C21 173.5(6) 2_565 . . . ?
C18 C17 C21 C20 3.0(10) . . . . ?
C14 C17 C21 C20 -176.0(6) . . . . ?
N6 C20 C21 C17 -1.1(12) . . . . ?
Cd1 O1 C22 O2 -1.7(6) . . . . ?
Cd1 O1 C22 C23 177.3(4) . . . . ?
Cd1 O2 C22 O1 1.8(6) . . . . ?
Cd1 O2 C22 C23 -177.2(4) . . . . ?
O4 Cd1 C22 O1 -169.0(4) 7_566 . . . ?
N1 Cd1 C22 O1 12.7(4) . . . . ?
O5 Cd1 C22 O1 94.8(4) . . . . ?
O2 Cd1 C22 O1 -178.3(6) . . . . ?
N6 Cd1 C22 O1 -80.4(4) 2_565 . . . ?
O3 Cd1 C22 O1 -170.1(6) 7_566 . . . ?
O4 Cd1 C22 O2 9.3(4) 7_566 . . . ?
N1 Cd1 C22 O2 -169.0(3) . . . . ?
O5 Cd1 C22 O2 -86.9(3) . . . . ?
N6 Cd1 C22 O2 97.9(3) 2_565 . . . ?
O1 Cd1 C22 O2 178.3(6) . . . . ?
O3 Cd1 C22 O2 8.2(9) 7_566 . . . ?
O1 C22 C23 C24 169.8(6) . . . . ?
O2 C22 C23 C24 -11.1(8) . . . . ?
O1 C22 C23 C28 -12.3(9) . . . . ?
O2 C22 C23 C28 166.8(6) . . . . ?
C28 C23 C24 C25 0.5(9) . . . . ?
C22 C23 C24 C25 178.4(5) . . . . ?
C23 C24 C25 C26 -2.3(8) . . . . ?
C24 C25 C26 C27 2.9(9) . . . . ?
C24 C25 C26 C29 -178.3(5) . . . . ?
C25 C26 C27 C28 -1.8(11) . . . . ?
C29 C26 C27 C28 179.4(7) . . . . ?
C24 C23 C28 C27 0.6(11) . . . . ?
C22 C23 C28 C27 -177.4(7) . . . . ?
C26 C27 C28 C23 0.0(13) . . . . ?
Cd1 O3 C29 O4 5.5(5) 7_565 . . . ?
Cd1 O3 C29 C26 -172.6(4) 7_565 . . . ?
Cd1 O4 C29 O3 -6.3(5) 7_565 . . . ?
Cd1 O4 C29 C26 171.8(4) 7_565 . . . ?
C27 C26 C29 O3 175.0(6) . . . . ?
C25 C26 C29 O3 -3.8(7) . . . . ?
C27 C26 C29 O4 -3.2(8) . . . . ?
C25 C26 C29 O4 178.1(5) . . . . ?
O6 C30 N7 C32 -1.3(16) . . . . ?
O6 C30 N7 C31 173.3(10) . . . . ?
O7 C35 N8 C34 -10(3) . . . . ?
O7 C35 N8 C33 170(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.102

#===END

data_5.Ni
_database_code_depnum_ccdc_archive 'CCDC 692042'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H44.50 N7 Ni O8.75'
_chemical_formula_weight         798.02

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   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                   11.414(4)
_cell_length_b                   16.924(5)
_cell_length_c                   23.486(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.533(4)
_cell_angle_gamma                90.00
_cell_volume                     4474(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2844
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      22.23

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1678
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8969
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_process_details   SADABS

_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  'APEX II 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            21875
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         25.01
_reflns_number_total             7856
_reflns_number_gt                3865
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

Standard geometry constraints were applied for the lattice DMF molecule in
order to improve the refinement stability. In addition, the soft "SADI"
constraint (for carbon atoms) and "FLAT" constraint were also imposed.
;

_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)+(0.1360P)²+1.3351P] 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     SHELXL
_refine_ls_extinction_coef       0.0049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7856
_refine_ls_number_parameters     512
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.2280
_refine_ls_wR_factor_gt          0.1972
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Ni1 Ni 1.17583(7) 0.25339(5) 0.32544(3) 0.0433(3) Uani 1 1 d . . .
O1 O 1.0401(4) 0.2863(3) 0.2646(2) 0.0530(11) Uani 1 1 d . . .
O2 O 1.0868(4) 0.4083(3) 0.2426(2) 0.0661(14) Uani 1 1 d . . .
O3 O 0.2644(5) 0.4000(3) -0.0930(3) 0.0829(18) Uani 1 1 d . . .
O4 O 0.3149(4) 0.2791(3) -0.1162(2) 0.0535(12) Uani 1 1 d . . .
O5 O 1.0876(4) 0.1473(3) 0.3289(2) 0.0613(13) Uani 1 1 d . . .
H5A H 1.0801 0.1334 0.2937 0.092 Uiso 1 1 d R . .
H5B H 1.1338 0.1112 0.3446 0.092 Uiso 1 1 d R . .
O6 O 1.2586(4) 0.3639(2) 0.3238(2) 0.0546(12) Uani 1 1 d . . .
H6A H 1.2868 0.3695 0.3593 0.082 Uiso 1 1 d R . .
H6B H 1.2116 0.3862 0.2967 0.082 Uiso 1 1 d R . .
N1 N 1.0879(4) 0.2956(3) 0.3905(2) 0.0472(13) Uani 1 1 d . . .
N2 N 0.7763(5) 0.4474(3) 0.5632(3) 0.0512(14) Uani 1 1 d . . .
N3 N 0.8628(5) 0.4253(3) 0.6064(2) 0.0563(15) Uani 1 1 d . . .
N4 N 0.5828(5) 0.4389(3) 0.5897(2) 0.0510(14) Uani 1 1 d . . .
N5 N 0.5041(5) 0.4077(3) 0.5457(3) 0.0565(15) Uani 1 1 d . . .
N6 N 0.2660(4) 0.2871(3) 0.7604(2) 0.0498(13) Uani 1 1 d . . .
C1 C 0.9691(5) 0.3542(4) 0.4764(3) 0.0493(16) Uani 1 1 d . . .
C2 C 0.9881(6) 0.3995(4) 0.4310(3) 0.0562(18) Uani 1 1 d . . .
H2 H 0.9612 0.4515 0.4283 0.067 Uiso 1 1 calc R . .
C3 C 1.0464(6) 0.3697(4) 0.3891(3) 0.0540(17) Uani 1 1 d . . .
H3 H 1.0576 0.4022 0.3585 0.065 Uiso 1 1 calc R . .
C4 C 1.0696(6) 0.2521(4) 0.4354(3) 0.0533(17) Uani 1 1 d . . .
H4 H 1.0980 0.2005 0.4375 0.064 Uiso 1 1 calc R . .
C5 C 1.0123(6) 0.2776(4) 0.4785(3) 0.0573(18) Uani 1 1 d . . .
H5 H 1.0024 0.2442 0.5088 0.069 Uiso 1 1 calc R . .
C6 C 0.9057(6) 0.3863(4) 0.5207(3) 0.0521(17) Uani 1 1 d . . .
C7 C 0.7982(6) 0.4252(4) 0.5106(3) 0.0520(17) Uani 1 1 d . . .
C8 C 0.7132(7) 0.4395(5) 0.4564(3) 0.074(2) Uani 1 1 d . . .
H8A H 0.6336 0.4299 0.4630 0.111 Uiso 1 1 calc R . .
H8B H 0.7310 0.4045 0.4268 0.111 Uiso 1 1 calc R . .
H8C H 0.7200 0.4932 0.4443 0.111 Uiso 1 1 calc R . .
C9 C 0.9414(6) 0.3866(4) 0.5806(3) 0.0563(18) Uani 1 1 d . . .
C10 C 1.0524(7) 0.3541(5) 0.6150(3) 0.084(3) Uani 1 1 d . . .
H10A H 1.1157 0.3915 0.6153 0.126 Uiso 1 1 calc R . .
H10B H 1.0729 0.3056 0.5979 0.126 Uiso 1 1 calc R . .
H10C H 1.0401 0.3443 0.6538 0.126 Uiso 1 1 calc R . .
C11 C 0.6742(6) 0.4898(4) 0.5755(3) 0.0524(16) Uani 1 1 d . . .
H11A H 0.6990 0.5255 0.6075 0.063 Uiso 1 1 calc R . .
H11B H 0.6419 0.5214 0.5421 0.063 Uiso 1 1 calc R . .
C12 C 0.5571(6) 0.4203(4) 0.6418(3) 0.0525(17) Uani 1 1 d . . .
C13 C 0.6336(7) 0.4445(5) 0.6959(3) 0.076(2) Uani 1 1 d . . .
H13A H 0.7140 0.4500 0.6893 0.114 Uiso 1 1 calc R . .
H13B H 0.6304 0.4050 0.7250 0.114 Uiso 1 1 calc R . .
H13C H 0.6062 0.4940 0.7086 0.114 Uiso 1 1 calc R . .
C14 C 0.4575(6) 0.3735(4) 0.6317(3) 0.0517(17) Uani 1 1 d . . .
C15 C 0.4287(6) 0.3667(4) 0.5710(3) 0.0535(17) Uani 1 1 d . . .
C16 C 0.3292(6) 0.3265(5) 0.5350(4) 0.077(2) Uani 1 1 d . . .
H16A H 0.3300 0.3384 0.4951 0.115 Uiso 1 1 calc R . .
H16B H 0.2557 0.3442 0.5454 0.115 Uiso 1 1 calc R . .
H16C H 0.3367 0.2705 0.5409 0.115 Uiso 1 1 calc R . .
C17 C 0.3929(6) 0.3423(4) 0.6750(3) 0.0539(17) Uani 1 1 d . . .
C18 C 0.3772(6) 0.3880(4) 0.7231(3) 0.064(2) Uani 1 1 d . . .
H18 H 0.4090 0.4386 0.7276 0.077 Uiso 1 1 calc R . .
C19 C 0.3152(6) 0.3582(4) 0.7636(3) 0.0598(19) Uani 1 1 d . . .
H19 H 0.3073 0.3898 0.7951 0.072 Uiso 1 1 calc R . .
C20 C 0.2797(6) 0.2443(4) 0.7145(3) 0.0596(19) Uani 1 1 d . . .
H20 H 0.2447 0.1946 0.7106 0.072 Uiso 1 1 calc R . .
C21 C 0.3424(6) 0.2688(4) 0.6725(3) 0.061(2) Uani 1 1 d . . .
H21 H 0.3505 0.2351 0.6421 0.074 Uiso 1 1 calc R . .
C22 C 1.0230(6) 0.3488(4) 0.2354(3) 0.0534(17) Uani 1 1 d . . .
C23 C 0.9217(6) 0.3467(4) 0.1874(3) 0.0564(18) Uani 1 1 d . . .
C24 C 0.8835(7) 0.4140(4) 0.1586(4) 0.082(3) Uani 1 1 d . . .
H24 H 0.9229 0.4614 0.1684 0.099 Uiso 1 1 calc R . .
C25 C 0.7884(8) 0.4124(4) 0.1157(4) 0.097(3) Uani 1 1 d . . .
H25 H 0.7622 0.4595 0.0976 0.116 Uiso 1 1 calc R . .
C26 C 0.7281(7) 0.3425(4) 0.0976(4) 0.078(3) Uani 1 1 d . . .
C27 C 0.7672(7) 0.2744(4) 0.1276(4) 0.077(3) Uani 1 1 d . . .
H27 H 0.7288 0.2267 0.1176 0.092 Uiso 1 1 calc R . .
C28 C 0.8625(7) 0.2766(4) 0.1721(3) 0.069(2) Uani 1 1 d . . .
H28 H 0.8873 0.2304 0.1920 0.082 Uiso 1 1 calc R . .
C29 C 0.6254(7) 0.3419(4) 0.0507(4) 0.076(2) Uani 1 1 d . . .
C30 C 0.5425(8) 0.4006(5) 0.0445(4) 0.107(4) Uani 1 1 d . . .
H30 H 0.5501 0.4415 0.0713 0.128 Uiso 1 1 calc R . .
C31 C 0.4495(8) 0.4012(5) 0.0005(4) 0.093(3) Uani 1 1 d . . .
H31 H 0.3950 0.4425 -0.0027 0.112 Uiso 1 1 calc R . .
C32 C 0.4353(6) 0.3415(4) -0.0392(3) 0.064(2) Uani 1 1 d . . .
C33 C 0.5156(7) 0.2814(5) -0.0330(4) 0.070(2) Uani 1 1 d . . .
H33 H 0.5055 0.2396 -0.0591 0.084 Uiso 1 1 calc R . .
C34 C 0.6108(7) 0.2812(4) 0.0108(4) 0.071(2) Uani 1 1 d . . .
H34 H 0.6657 0.2402 0.0137 0.085 Uiso 1 1 calc R . .
C35 C 0.3313(6) 0.3409(4) -0.0866(3) 0.0592(19) Uani 1 1 d . . .
O9 O 0.0346(7) 0.5611(3) 0.2635(3) 0.119(3) Uani 1 1 d . . .
H9A H 0.0611 0.5177 0.2532 0.178 Uiso 1 1 d R . .
H9B H 0.0830 0.5992 0.2613 0.178 Uiso 1 1 d R . .
O7 O 0.4872(6) 0.3706(5) 0.3068(4) 0.136(3) Uani 1 1 d D . .
N7 N 0.6627(6) 0.3106(4) 0.3075(4) 0.120(3) Uani 1 1 d D . .
C36 C 0.5425(7) 0.3092(5) 0.3177(4) 0.121(4) Uani 1 1 d D . .
H36 H 0.5088 0.2646 0.3316 0.146 Uiso 1 1 calc R . .
O8 O 0.186(2) 0.0121(13) 0.5848(12) 0.111(9) Uani 0.25 1 d P . .
H8' H 0.1818 -0.0335 0.5693 0.166 Uiso 0.25 1 d PR . .
H8" H 0.2179 0.0151 0.6201 0.166 Uiso 0.25 1 d PR . .
C38 C 0.7368(9) 0.2412(6) 0.3190(7) 0.224(9) Uani 1 1 d D . .
H38A H 0.7056 0.2076 0.3458 0.336 Uiso 1 1 calc R . .
H38B H 0.8162 0.2569 0.3352 0.336 Uiso 1 1 calc R . .
H38C H 0.7379 0.2130 0.2836 0.336 Uiso 1 1 calc R . .
C37 C 0.7102(10) 0.3806(6) 0.2845(8) 0.218(9) Uani 1 1 d D . .
H37A H 0.6506 0.4039 0.2558 0.327 Uiso 1 1 calc R . .
H37B H 0.7780 0.3665 0.2673 0.327 Uiso 1 1 calc R . .
H37C H 0.7337 0.4178 0.3151 0.327 Uiso 1 1 calc R . .
O10 O 0.1595(15) 0.1341(13) 0.5740(8) 0.180(8) Uani 0.50 1 d P . .
H10' H 0.1510 0.0853 0.5660 0.270 Uiso 0.50 1 d PR . .
H10" H 0.2174 0.1577 0.5628 0.270 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
Ni1 O4 1.994(4) 4_666 ?
Ni1 O1 2.005(4) . ?
Ni1 O5 2.066(5) . ?
Ni1 N1 2.089(5) . ?
Ni1 N6 2.093(5) 4_665 ?
Ni1 O6 2.098(4) . ?
O1 C22 1.258(8) . ?
O2 C22 1.237(8) . ?
O3 C35 1.252(8) . ?
O4 C35 1.254(8) . ?
O4 Ni1 1.994(4) 4_465 ?
O5 H5A 0.8518 . ?
O5 H5B 0.8498 . ?
O6 H6A 0.8487 . ?
O6 H6B 0.8500 . ?
N1 C4 1.330(8) . ?
N1 C3 1.338(8) . ?
N2 N3 1.346(7) . ?
N2 C7 1.353(8) . ?
N2 C11 1.438(8) . ?
N3 C9 1.335(8) . ?
N4 C12 1.341(8) . ?
N4 N5 1.360(7) . ?
N4 C11 1.433(8) . ?
N5 C15 1.321(8) . ?
N6 C19 1.326(8) . ?
N6 C20 1.328(9) . ?
N6 Ni1 2.093(5) 4_466 ?
C1 C2 1.360(9) . ?
C1 C5 1.385(9) . ?
C1 C6 1.468(9) . ?
C2 C3 1.372(9) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.363(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.377(9) . ?
C6 C9 1.397(9) . ?
C7 C8 1.489(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.490(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.374(9) . ?
C12 C13 1.476(10) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.413(9) . ?
C14 C17 1.450(9) . ?
C15 C16 1.468(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.369(9) . ?
C17 C18 1.405(10) . ?
C18 C19 1.371(9) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.374(10) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.476(9) . ?
C23 C24 1.359(9) . ?
C23 C28 1.383(9) . ?
C24 C25 1.353(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.400(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(10) . ?
C26 C29 1.469(10) . ?
C27 C28 1.378(9) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.363(11) . ?
C29 C34 1.382(10) . ?
C30 C31 1.353(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.367(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.360(10) . ?
C32 C35 1.487(9) . ?
C33 C34 1.366(9) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
O9 H9A 0.8447 . ?
O9 H9B 0.8560 . ?
O7 C36 1.221(12) . ?
N7 C36 1.432(11) . ?
N7 C37 1.444(14) . ?
N7 C38 1.446(13) . ?
C36 H36 0.9300 . ?
O8 H8' 0.8511 . ?
O8 H8" 0.8511 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
O10 H10' 0.8498 . ?
O10 H10" 0.8498 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O1 177.84(19) 4_666 . ?
O4 Ni1 O5 94.07(19) 4_666 . ?
O1 Ni1 O5 86.88(18) . . ?
O4 Ni1 N1 90.91(19) 4_666 . ?
O1 Ni1 N1 91.05(19) . . ?
O5 Ni1 N1 88.40(19) . . ?
O4 Ni1 N6 88.9(2) 4_666 4_665 ?
O1 Ni1 N6 89.17(19) . 4_665 ?
O5 Ni1 N6 92.7(2) . 4_665 ?
N1 Ni1 N6 178.9(2) . 4_665 ?
O4 Ni1 O6 87.05(18) 4_666 . ?
O1 Ni1 O6 92.09(18) . . ?
O5 Ni1 O6 177.08(17) . . ?
N1 Ni1 O6 88.88(19) . . ?
N6 Ni1 O6 90.1(2) 4_665 . ?
C22 O1 Ni1 130.8(4) . . ?
C35 O4 Ni1 129.8(4) . 4_465 ?
Ni1 O5 H5A 99.9 . . ?
Ni1 O5 H5B 111.7 . . ?
H5A O5 H5B 100.3 . . ?
Ni1 O6 H6A 100.5 . . ?
Ni1 O6 H6B 100.4 . . ?
H6A O6 H6B 141.0 . . ?
C4 N1 C3 116.0(6) . . ?
C4 N1 Ni1 123.2(4) . . ?
C3 N1 Ni1 120.9(5) . . ?
N3 N2 C7 112.7(5) . . ?
N3 N2 C11 120.3(6) . . ?
C7 N2 C11 126.9(6) . . ?
C9 N3 N2 105.0(6) . . ?
C12 N4 N5 112.7(5) . . ?
C12 N4 C11 129.1(6) . . ?
N5 N4 C11 118.1(5) . . ?
C15 N5 N4 105.0(6) . . ?
C19 N6 C20 115.8(6) . . ?
C19 N6 Ni1 120.7(5) . 4_466 ?
C20 N6 Ni1 123.5(4) . 4_466 ?
C2 C1 C5 117.0(6) . . ?
C2 C1 C6 120.6(6) . . ?
C5 C1 C6 122.4(6) . . ?
C1 C2 C3 120.9(6) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
N1 C3 C2 122.5(7) . . ?
N1 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
N1 C4 C5 124.8(6) . . ?
N1 C4 H4 117.6 . . ?
C5 C4 H4 117.6 . . ?
C4 C5 C1 118.8(7) . . ?
C4 C5 H5 120.6 . . ?
C1 C5 H5 120.6 . . ?
C7 C6 C9 105.9(6) . . ?
C7 C6 C1 125.8(7) . . ?
C9 C6 C1 128.2(6) . . ?
N2 C7 C6 105.7(6) . . ?
N2 C7 C8 122.9(6) . . ?
C6 C7 C8 131.4(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C6 110.6(6) . . ?
N3 C9 C10 120.7(7) . . ?
C6 C9 C10 128.6(7) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 N2 113.1(5) . . ?
N4 C11 H11A 109.0 . . ?
N2 C11 H11A 109.0 . . ?
N4 C11 H11B 109.0 . . ?
N2 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N4 C12 C14 106.2(6) . . ?
N4 C12 C13 122.2(6) . . ?
C14 C12 C13 131.5(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 C15 105.5(6) . . ?
C12 C14 C17 126.3(7) . . ?
C15 C14 C17 128.1(6) . . ?
N5 C15 C14 110.7(6) . . ?
N5 C15 C16 118.9(7) . . ?
C14 C15 C16 130.4(6) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 115.2(6) . . ?
C21 C17 C14 124.1(7) . . ?
C18 C17 C14 120.8(6) . . ?
C19 C18 C17 120.3(6) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
N6 C19 C18 123.9(7) . . ?
N6 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
N6 C20 C21 124.3(7) . . ?
N6 C20 H20 117.9 . . ?
C21 C20 H20 117.9 . . ?
C17 C21 C20 120.6(7) . . ?
C17 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
O2 C22 O1 125.1(6) . . ?
O2 C22 C23 119.6(6) . . ?
O1 C22 C23 115.2(6) . . ?
C24 C23 C28 119.1(6) . . ?
C24 C23 C22 120.4(6) . . ?
C28 C23 C22 120.5(6) . . ?
C25 C24 C23 120.4(7) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 122.4(7) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C25 116.6(7) . . ?
C27 C26 C29 121.7(7) . . ?
C25 C26 C29 121.6(7) . . ?
C28 C27 C26 120.7(7) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C23 120.7(7) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
C30 C29 C34 117.8(7) . . ?
C30 C29 C26 121.9(8) . . ?
C34 C29 C26 120.3(7) . . ?
C31 C30 C29 122.0(8) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 120.3(8) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 118.5(7) . . ?
C33 C32 C35 121.1(7) . . ?
C31 C32 C35 120.4(7) . . ?
C32 C33 C34 121.4(7) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C29 120.0(7) . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
O3 C35 O4 124.6(6) . . ?
O3 C35 C32 118.7(7) . . ?
O4 C35 C32 116.6(6) . . ?
H9A O9 H9B 112.0 . . ?
C36 N7 C37 120.4(7) . . ?
C36 N7 C38 120.2(4) . . ?
C37 N7 C38 119.4(4) . . ?
O7 C36 N7 115.3(7) . . ?
O7 C36 H36 122.3 . . ?
N7 C36 H36 122.3 . . ?
H8' O8 H8" 117.0 . . ?
N7 C38 H38A 109.5 . . ?
N7 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N7 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N7 C37 H37A 109.5 . . ?
N7 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N7 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
H10' O10 H10" 117.1 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.116

#===END

data_5.Zn
_database_code_depnum_ccdc_archive 'CCDC 692043'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H32 N6 O9 Zn2'
_chemical_formula_weight         835.43

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   P2(1)/n

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

_cell_length_a                   10.9672(12)
_cell_length_b                   10.8989(12)
_cell_length_c                   39.656(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2940(10)
_cell_angle_gamma                90.00
_cell_volume                     4732.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3703
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.18

_exptl_crystal_description       BLOCK
_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      NONE
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_T_max  0.8597
_exptl_absorpt_process_details   SADABS

_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  'Apex II 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            25133
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.03
_reflns_number_total             8319
_reflns_number_gt                5458
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_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.

The phenyl ring of one terephthalate (C30, C31, C32, C33, C34, and, C35)
and disordered lattice water were refined using the pseudo-isotropic
"ISOR" restraint, as the free refinement gave unrealistic anisotropic
displacement parameters. Rigid bond (DELU) restraint was also used to
treat this phenyl group.
;

_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)+(0.1152P)²+20.6279P] 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         8319
_refine_ls_number_parameters     518
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2426
_refine_ls_wR_factor_gt          0.2185
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.064
_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 0.58906(7) 0.26937(7) 0.140041(18) 0.0214(2) Uani 1 1 d . . .
Zn2 Zn 0.60978(7) 0.27393(7) 0.215182(18) 0.0223(2) Uani 1 1 d . . .
O1 O 0.4235(5) 0.2785(6) 0.20105(14) 0.0498(15) Uani 1 1 d . . .
O2 O 0.4047(5) 0.2699(5) 0.14492(14) 0.0450(14) Uani 1 1 d . . .
O3 O -0.2273(5) 0.2684(5) 0.15384(14) 0.0432(14) Uani 1 1 d . . .
O4 O -0.2073(5) 0.2714(5) 0.20966(14) 0.0433(14) Uani 1 1 d . . .
O5 O 0.5879(5) 0.4512(4) 0.15210(12) 0.0399(13) Uani 1 1 d . . .
O6 O 0.6116(5) 0.4576(4) 0.20847(13) 0.0402(13) Uani 1 1 d . . .
O7 O 0.6063(6) 1.0955(5) 0.20132(13) 0.0477(14) Uani 1 1 d . . .
O8 O 0.5901(5) 1.0855(5) 0.14565(13) 0.0471(14) Uani 1 1 d . . .
N1 N 0.5980(5) 0.2882(6) 0.08927(14) 0.0314(14) Uani 1 1 d . . .
N2 N 0.6689(8) 0.4225(9) -0.06503(17) 0.063(2) Uani 1 1 d . . .
N3 N 0.5961(9) 0.3252(10) -0.07340(19) 0.080(3) Uani 1 1 d . . .
N4 N 0.8159(7) 0.4548(8) -0.10758(17) 0.062(2) Uani 1 1 d . . .
N5 N 0.9265(8) 0.4742(9) -0.09201(19) 0.075(3) Uani 1 1 d . . .
N6 N 1.0789(6) 0.2578(6) -0.23578(15) 0.0353(15) Uani 1 1 d . . .
C1 C 0.6243(12) 0.2088(11) 0.0345(2) 0.079(4) Uani 1 1 d . . .
H1 H 0.6355 0.1401 0.0211 0.095 Uiso 1 1 calc R . .
C2 C 0.6147(11) 0.1961(9) 0.0692(2) 0.069(3) Uani 1 1 d . . .
H2 H 0.6205 0.1177 0.0784 0.082 Uiso 1 1 calc R . .
C3 C 0.5914(8) 0.3995(8) 0.0753(2) 0.047(2) Uani 1 1 d . . .
H3 H 0.5805 0.4666 0.0893 0.057 Uiso 1 1 calc R . .
C4 C 0.5999(8) 0.4205(9) 0.0409(2) 0.052(2) Uani 1 1 d . . .
H4 H 0.5938 0.4999 0.0324 0.063 Uiso 1 1 calc R . .
C5 C 0.6171(8) 0.3253(8) 0.01994(18) 0.043(2) Uani 1 1 d . . .
C6 C 0.6280(8) 0.3432(9) -0.01644(19) 0.049(2) Uani 1 1 d . . .
C7 C 0.6894(9) 0.4384(9) -0.0312(2) 0.055(2) Uani 1 1 d . . .
C8 C 0.5697(11) 0.2767(11) -0.0437(2) 0.072(3) Uani 1 1 d . . .
C9 C 0.7655(14) 0.5406(12) -0.0167(3) 0.112(5) Uani 1 1 d . . .
H9A H 0.8397 0.5459 -0.0283 0.169 Uiso 1 1 calc R . .
H9B H 0.7845 0.5256 0.0068 0.169 Uiso 1 1 calc R . .
H9C H 0.7213 0.6164 -0.0194 0.169 Uiso 1 1 calc R . .
C10 C 0.4845(18) 0.1706(17) -0.0432(3) 0.160(9) Uani 1 1 d . . .
H10A H 0.4711 0.1385 -0.0657 0.239 Uiso 1 1 calc R . .
H10B H 0.4081 0.1969 -0.0350 0.239 Uiso 1 1 calc R . .
H10C H 0.5193 0.1079 -0.0286 0.239 Uiso 1 1 calc R . .
C11 C 0.7067(11) 0.4992(11) -0.0922(2) 0.084(4) Uani 1 1 d . . .
H11A H 0.7220 0.5814 -0.0836 0.100 Uiso 1 1 calc R . .
H11B H 0.6405 0.5041 -0.1095 0.100 Uiso 1 1 calc R . .
C12 C 1.0060(9) 0.4348(11) -0.1139(2) 0.069(3) Uani 1 1 d . . .
C13 C 0.9436(8) 0.3843(10) -0.14280(19) 0.054(2) Uani 1 1 d . . .
C14 C 0.8206(8) 0.4002(9) -0.1385(2) 0.054(2) Uani 1 1 d . . .
C15 C 1.1406(10) 0.4398(15) -0.1055(3) 0.107(5) Uani 1 1 d . . .
H15A H 1.1568 0.4932 -0.0865 0.160 Uiso 1 1 calc R . .
H15B H 1.1812 0.4706 -0.1246 0.160 Uiso 1 1 calc R . .
H15C H 1.1702 0.3590 -0.1000 0.160 Uiso 1 1 calc R . .
C16 C 0.7106(9) 0.3736(12) -0.1607(3) 0.081(4) Uani 1 1 d . . .
H16A H 0.6579 0.3191 -0.1493 0.122 Uiso 1 1 calc R . .
H16B H 0.7345 0.3358 -0.1811 0.122 Uiso 1 1 calc R . .
H16C H 0.6680 0.4488 -0.1660 0.122 Uiso 1 1 calc R . .
C17 C 0.9963(7) 0.3350(9) -0.17360(19) 0.045(2) Uani 1 1 d . . .
C18 C 1.0806(8) 0.4028(9) -0.1903(2) 0.049(2) Uani 1 1 d . . .
H18 H 1.1121 0.4752 -0.1810 0.059 Uiso 1 1 calc R . .
C19 C 1.1177(8) 0.3620(7) -0.22134(19) 0.043(2) Uani 1 1 d . . .
H19 H 1.1727 0.4099 -0.2326 0.052 Uiso 1 1 calc R . .
C20 C 1.0016(10) 0.1917(10) -0.2191(2) 0.069(3) Uani 1 1 d . . .
H20 H 0.9755 0.1171 -0.2283 0.083 Uiso 1 1 calc R . .
C21 C 0.9577(10) 0.2271(9) -0.1889(2) 0.067(3) Uani 1 1 d . . .
H21 H 0.9012 0.1778 -0.1787 0.080 Uiso 1 1 calc R . .
C22 C 0.2252(6) 0.2724(7) 0.17553(19) 0.0347(17) Uani 1 1 d . . .
C23 C 0.1509(7) 0.2675(8) 0.1467(2) 0.043(2) Uani 1 1 d . . .
H23 H 0.1847 0.2649 0.1258 0.052 Uiso 1 1 calc R . .
C24 C 0.0245(7) 0.2663(8) 0.1487(2) 0.044(2) Uani 1 1 d . . .
H24 H -0.0254 0.2638 0.1289 0.052 Uiso 1 1 calc R . .
C25 C -0.0274(6) 0.2688(7) 0.17924(18) 0.0328(16) Uani 1 1 d . . .
C26 C 0.0487(7) 0.2731(10) 0.2082(2) 0.059(3) Uani 1 1 d . . .
H26 H 0.0153 0.2745 0.2292 0.071 Uiso 1 1 calc R . .
C27 C 0.1729(7) 0.2751(10) 0.2062(2) 0.061(3) Uani 1 1 d . . .
H27 H 0.2228 0.2784 0.2260 0.073 Uiso 1 1 calc R . .
C28 C 0.3618(7) 0.2727(7) 0.1735(2) 0.0339(17) Uani 1 1 d . . .
C29 C -0.1652(6) 0.2696(7) 0.18105(19) 0.0314(16) Uani 1 1 d . . .
C30 C 0.5995(6) 0.6447(6) 0.17853(17) 0.0298(14) Uani 1 1 d U . .
C31 C 0.6036(7) 0.7132(7) 0.20788(18) 0.0331(15) Uani 1 1 d U . .
H31 H 0.6062 0.6738 0.2287 0.040 Uiso 1 1 calc R . .
C32 C 0.6039(7) 0.8397(7) 0.20642(18) 0.0344(15) Uani 1 1 d U . .
H32 H 0.6070 0.8851 0.2263 0.041 Uiso 1 1 calc R . .
C33 C 0.5997(6) 0.8992(6) 0.17572(17) 0.0294(14) Uani 1 1 d U . .
C34 C 0.5951(7) 0.8302(7) 0.14634(18) 0.0358(16) Uani 1 1 d U . .
H34 H 0.5914 0.8693 0.1255 0.043 Uiso 1 1 calc R . .
C35 C 0.5959(7) 0.7039(6) 0.14784(18) 0.0334(15) Uani 1 1 d U . .
H35 H 0.5939 0.6584 0.1280 0.040 Uiso 1 1 calc R . .
C36 C 0.5994(7) 0.5069(6) 0.17985(19) 0.0330(17) Uani 1 1 d . . .
C37 C 0.5992(6) 1.0376(6) 0.17415(18) 0.0305(16) Uani 1 1 d . . .
O9 O 0.322(3) 0.019(3) 0.1021(9) 0.102(11) Uani 0.25 1 d PU . .
O10 O 0.871(4) 0.975(4) 0.1080(12) 0.146(16) Uani 0.25 1 d PU . .
O11 O 0.712(4) 0.027(4) 0.7949(10) 0.117(12) Uani 0.25 1 d PU . .
O12 O 0.011(4) 0.720(4) 0.9477(10) 0.115(12) Uani 0.25 1 d PU . .


_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 O8 2.017(5) 1_545 ?
Zn1 N1 2.032(6) . ?
Zn1 O5 2.038(5) . ?
Zn1 O2 2.043(5) . ?
Zn1 O3 2.057(5) 1_655 ?
Zn1 Zn2 2.9758(10) . ?
Zn2 O6 2.019(5) . ?
Zn2 O7 2.021(5) 1_545 ?
Zn2 N6 2.023(6) 4_566 ?
Zn2 O4 2.031(5) 1_655 ?
Zn2 O1 2.087(5) . ?
O1 C28 1.252(9) . ?
O2 C28 1.254(9) . ?
O3 C29 1.243(9) . ?
O3 Zn1 2.057(5) 1_455 ?
O4 C29 1.249(9) . ?
O4 Zn2 2.031(5) 1_455 ?
O5 C36 1.257(8) . ?
O6 C36 1.256(8) . ?
O7 C37 1.247(8) . ?
O7 Zn2 2.021(5) 1_565 ?
O8 C37 1.244(8) . ?
O8 Zn1 2.017(5) 1_565 ?
N1 C2 1.302(11) . ?
N1 C3 1.334(10) . ?
N2 N3 1.356(12) . ?
N2 C7 1.359(11) . ?
N2 C11 1.444(11) . ?
N3 C8 1.337(12) . ?
N4 N5 1.346(11) . ?
N4 C14 1.366(11) . ?
N4 C11 1.457(11) . ?
N5 C12 1.336(11) . ?
N6 C20 1.318(11) . ?
N6 C19 1.331(10) . ?
N6 Zn2 2.023(6) 4_665 ?
C1 C2 1.391(12) . ?
C1 C5 1.395(13) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.392(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.467(10) . ?
C6 C7 1.385(12) . ?
C6 C8 1.423(13) . ?
C7 C9 1.487(14) . ?
C8 C10 1.487(16) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.412(12) . ?
C12 C15 1.495(14) . ?
C13 C14 1.380(11) . ?
C13 C17 1.482(10) . ?
C14 C16 1.481(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C21 1.380(13) . ?
C17 C18 1.383(11) . ?
C18 C19 1.390(11) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.370(12) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.365(11) . ?
C22 C27 1.374(11) . ?
C22 C28 1.505(10) . ?
C23 C24 1.393(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.368(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.380(11) . ?
C25 C29 1.518(9) . ?
C26 C27 1.369(11) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C30 C35 1.376(10) . ?
C30 C31 1.381(10) . ?
C30 C36 1.504(10) . ?
C31 C32 1.380(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.378(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.386(9) . ?
C33 C37 1.510(10) . ?
C34 C35 1.377(10) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?

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
O8 Zn1 N1 102.1(2) 1_545 . ?
O8 Zn1 O5 160.1(2) 1_545 . ?
N1 Zn1 O5 97.8(2) . . ?
O8 Zn1 O2 89.5(2) 1_545 . ?
N1 Zn1 O2 101.4(2) . . ?
O5 Zn1 O2 87.5(2) . . ?
O8 Zn1 O3 88.1(2) 1_545 1_655 ?
N1 Zn1 O3 99.3(2) . 1_655 ?
O5 Zn1 O3 87.8(2) . 1_655 ?
O2 Zn1 O3 159.2(2) . 1_655 ?
O8 Zn1 Zn2 84.64(15) 1_545 . ?
N1 Zn1 Zn2 170.17(18) . . ?
O5 Zn1 Zn2 75.53(14) . . ?
O2 Zn1 Zn2 85.65(16) . . ?
O3 Zn1 Zn2 73.53(15) 1_655 . ?
O6 Zn2 O7 156.7(2) . 1_545 ?
O6 Zn2 N6 107.4(2) . 4_566 ?
O7 Zn2 N6 95.5(2) 1_545 4_566 ?
O6 Zn2 O4 89.0(2) . 1_655 ?
O7 Zn2 O4 87.8(2) 1_545 1_655 ?
N6 Zn2 O4 108.8(2) 4_566 1_655 ?
O6 Zn2 O1 87.6(2) . . ?
O7 Zn2 O1 87.0(2) 1_545 . ?
N6 Zn2 O1 92.7(2) 4_566 . ?
O4 Zn2 O1 158.3(2) 1_655 . ?
O6 Zn2 Zn1 83.41(15) . . ?
O7 Zn2 Zn1 73.28(15) 1_545 . ?
N6 Zn2 Zn1 162.26(19) 4_566 . ?
O4 Zn2 Zn1 84.88(15) 1_655 . ?
O1 Zn2 Zn1 73.40(16) . . ?
C28 O1 Zn2 134.8(5) . . ?
C28 O2 Zn1 120.7(5) . . ?
C29 O3 Zn1 135.3(5) . 1_455 ?
C29 O4 Zn2 121.1(5) . 1_455 ?
C36 O5 Zn1 132.3(5) . . ?
C36 O6 Zn2 122.8(5) . . ?
C37 O7 Zn2 136.1(5) . 1_565 ?
C37 O8 Zn1 121.1(5) . 1_565 ?
C2 N1 C3 117.0(7) . . ?
C2 N1 Zn1 123.1(6) . . ?
C3 N1 Zn1 119.9(5) . . ?
N3 N2 C7 113.8(8) . . ?
N3 N2 C11 117.4(9) . . ?
C7 N2 C11 128.7(10) . . ?
C8 N3 N2 104.4(8) . . ?
N5 N4 C14 113.6(7) . . ?
N5 N4 C11 119.8(8) . . ?
C14 N4 C11 126.4(9) . . ?
C12 N5 N4 104.8(8) . . ?
C20 N6 C19 116.7(7) . . ?
C20 N6 Zn2 122.5(6) . 4_665 ?
C19 N6 Zn2 119.5(5) . 4_665 ?
C2 C1 C5 119.6(9) . . ?
C2 C1 H1 120.2 . . ?
C5 C1 H1 120.2 . . ?
N1 C2 C1 123.3(9) . . ?
N1 C2 H2 118.3 . . ?
C1 C2 H2 118.3 . . ?
N1 C3 C4 123.5(8) . . ?
N1 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
C5 C4 C3 119.8(8) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C1 116.8(8) . . ?
C4 C5 C6 121.7(8) . . ?
C1 C5 C6 121.5(8) . . ?
C7 C6 C8 105.6(7) . . ?
C7 C6 C5 125.7(8) . . ?
C8 C6 C5 128.4(8) . . ?
N2 C7 C6 105.3(9) . . ?
N2 C7 C9 122.3(9) . . ?
C6 C7 C9 132.4(8) . . ?
N3 C8 C6 110.9(10) . . ?
N3 C8 C10 119.2(10) . . ?
C6 C8 C10 129.8(9) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 N4 113.5(8) . . ?
N2 C11 H11A 108.9 . . ?
N4 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
N4 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N5 C12 C13 110.4(9) . . ?
N5 C12 C15 121.0(9) . . ?
C13 C12 C15 128.4(8) . . ?
C14 C13 C12 106.4(8) . . ?
C14 C13 C17 125.3(8) . . ?
C12 C13 C17 128.0(8) . . ?
N4 C14 C13 104.7(8) . . ?
N4 C14 C16 123.2(8) . . ?
C13 C14 C16 132.1(8) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 116.2(7) . . ?
C21 C17 C13 123.2(8) . . ?
C18 C17 C13 120.3(8) . . ?
C17 C18 C19 119.4(8) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
N6 C19 C18 123.4(8) . . ?
N6 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
N6 C20 C21 123.6(9) . . ?
N6 C20 H20 118.2 . . ?
C21 C20 H20 118.2 . . ?
C20 C21 C17 120.7(8) . . ?
C20 C21 H21 119.7 . . ?
C17 C21 H21 119.7 . . ?
C23 C22 C27 118.8(7) . . ?
C23 C22 C28 120.3(7) . . ?
C27 C22 C28 120.9(7) . . ?
C22 C23 C24 120.1(7) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 121.0(7) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 118.3(7) . . ?
C24 C25 C29 120.5(7) . . ?
C26 C25 C29 121.1(7) . . ?
C27 C26 C25 120.6(7) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C22 121.1(8) . . ?
C26 C27 H27 119.4 . . ?
C22 C27 H27 119.4 . . ?
O1 C28 O2 125.3(7) . . ?
O1 C28 C22 116.4(7) . . ?
O2 C28 C22 118.3(7) . . ?
O3 C29 O4 125.2(7) . . ?
O3 C29 C25 117.2(6) . . ?
O4 C29 C25 117.7(7) . . ?
C35 C30 C31 119.4(7) . . ?
C35 C30 C36 119.9(6) . . ?
C31 C30 C36 120.7(6) . . ?
C30 C31 C32 120.3(7) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 120.5(7) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.0(7) . . ?
C32 C33 C37 120.5(6) . . ?
C34 C33 C37 120.5(6) . . ?
C35 C34 C33 120.4(7) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C30 C35 C34 120.4(7) . . ?
C30 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
O6 C36 O5 125.8(7) . . ?
O6 C36 C30 117.3(7) . . ?
O5 C36 C30 116.9(6) . . ?
O8 C37 O7 124.8(7) . . ?
O8 C37 C33 117.2(6) . . ?
O7 C37 C33 118.0(7) . . ?

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
O8 Zn1 Zn2 O6 179.0(2) 1_545 . . . ?
O5 Zn1 Zn2 O6 -2.6(2) . . . . ?
O2 Zn1 Zn2 O6 -91.1(2) . . . . ?
O3 Zn1 Zn2 O6 89.4(2) 1_655 . . . ?
O8 Zn1 Zn2 O7 0.3(2) 1_545 . . 1_545 ?
O5 Zn1 Zn2 O7 178.7(2) . . . 1_545 ?
O2 Zn1 Zn2 O7 90.2(2) . . . 1_545 ?
O3 Zn1 Zn2 O7 -89.3(2) 1_655 . . 1_545 ?
O8 Zn1 Zn2 N6 -52.1(6) 1_545 . . 4_566 ?
O5 Zn1 Zn2 N6 126.4(6) . . . 4_566 ?
O2 Zn1 Zn2 N6 37.9(6) . . . 4_566 ?
O3 Zn1 Zn2 N6 -141.6(6) 1_655 . . 4_566 ?
O8 Zn1 Zn2 O4 89.5(2) 1_545 . . 1_655 ?
O5 Zn1 Zn2 O4 -92.1(2) . . . 1_655 ?
O2 Zn1 Zn2 O4 179.4(2) . . . 1_655 ?
O3 Zn1 Zn2 O4 -0.1(2) 1_655 . . 1_655 ?
O8 Zn1 Zn2 O1 -91.6(3) 1_545 . . . ?
O5 Zn1 Zn2 O1 86.8(2) . . . . ?
O2 Zn1 Zn2 O1 -1.6(2) . . . . ?
O3 Zn1 Zn2 O1 178.9(3) 1_655 . . . ?
O6 Zn2 O1 C28 87.9(8) . . . . ?
O7 Zn2 O1 C28 -69.4(8) 1_545 . . . ?
N6 Zn2 O1 C28 -164.8(8) 4_566 . . . ?
O4 Zn2 O1 C28 6.8(12) 1_655 . . . ?
Zn1 Zn2 O1 C28 4.1(7) . . . . ?
O8 Zn1 O2 C28 85.3(6) 1_545 . . . ?
N1 Zn1 O2 C28 -172.5(6) . . . . ?
O5 Zn1 O2 C28 -75.1(6) . . . . ?
O3 Zn1 O2 C28 2.0(10) 1_655 . . . ?
Zn2 Zn1 O2 C28 0.6(6) . . . . ?
O8 Zn1 O5 C36 8.1(12) 1_545 . . . ?
N1 Zn1 O5 C36 -169.1(7) . . . . ?
O2 Zn1 O5 C36 89.7(7) . . . . ?
O3 Zn1 O5 C36 -70.0(7) 1_655 . . . ?
Zn2 Zn1 O5 C36 3.5(6) . . . . ?
O7 Zn2 O6 C36 6.2(10) 1_545 . . . ?
N6 Zn2 O6 C36 -162.4(6) 4_566 . . . ?
O4 Zn2 O6 C36 88.1(6) 1_655 . . . ?
O1 Zn2 O6 C36 -70.4(6) . . . . ?
Zn1 Zn2 O6 C36 3.2(6) . . . . ?
O8 Zn1 N1 C2 -6.9(8) 1_545 . . . ?
O5 Zn1 N1 C2 172.2(8) . . . . ?
O2 Zn1 N1 C2 -98.9(8) . . . . ?
O3 Zn1 N1 C2 83.1(8) 1_655 . . . ?
O8 Zn1 N1 C3 175.7(6) 1_545 . . . ?
O5 Zn1 N1 C3 -5.2(6) . . . . ?
O2 Zn1 N1 C3 83.7(6) . . . . ?
O3 Zn1 N1 C3 -94.3(6) 1_655 . . . ?
C7 N2 N3 C8 -0.4(12) . . . . ?
C11 N2 N3 C8 -176.1(9) . . . . ?
C14 N4 N5 C12 2.1(12) . . . . ?
C11 N4 N5 C12 -173.7(9) . . . . ?
C3 N1 C2 C1 -0.7(16) . . . . ?
Zn1 N1 C2 C1 -178.1(9) . . . . ?
C5 C1 C2 N1 0.5(19) . . . . ?
C2 N1 C3 C4 0.7(13) . . . . ?
Zn1 N1 C3 C4 178.3(7) . . . . ?
N1 C3 C4 C5 -0.7(14) . . . . ?
C3 C4 C5 C1 0.5(14) . . . . ?
C3 C4 C5 C6 -179.3(8) . . . . ?
C2 C1 C5 C4 -0.4(16) . . . . ?
C2 C1 C5 C6 179.4(10) . . . . ?
C4 C5 C6 C7 39.2(14) . . . . ?
C1 C5 C6 C7 -140.5(11) . . . . ?
C4 C5 C6 C8 -133.7(11) . . . . ?
C1 C5 C6 C8 46.5(15) . . . . ?
N3 N2 C7 C6 1.5(11) . . . . ?
C11 N2 C7 C6 176.6(9) . . . . ?
N3 N2 C7 C9 -179.2(11) . . . . ?
C11 N2 C7 C9 -4.1(16) . . . . ?
C8 C6 C7 N2 -1.9(11) . . . . ?
C5 C6 C7 N2 -176.2(8) . . . . ?
C8 C6 C7 C9 179.0(13) . . . . ?
C5 C6 C7 C9 4.7(19) . . . . ?
N2 N3 C8 C6 -0.9(13) . . . . ?
N2 N3 C8 C10 176.6(14) . . . . ?
C7 C6 C8 N3 1.8(13) . . . . ?
C5 C6 C8 N3 175.8(9) . . . . ?
C7 C6 C8 C10 -175.4(16) . . . . ?
C5 C6 C8 C10 -1(2) . . . . ?
N3 N2 C11 N4 -85.9(13) . . . . ?
C7 N2 C11 N4 99.1(12) . . . . ?
N5 N4 C11 N2 -78.4(14) . . . . ?
C14 N4 C11 N2 106.4(12) . . . . ?
N4 N5 C12 C13 -3.1(13) . . . . ?
N4 N5 C12 C15 -179.3(11) . . . . ?
N5 C12 C13 C14 3.1(13) . . . . ?
C15 C12 C13 C14 178.9(12) . . . . ?
N5 C12 C13 C17 177.4(10) . . . . ?
C15 C12 C13 C17 -7(2) . . . . ?
N5 N4 C14 C13 -0.2(12) . . . . ?
C11 N4 C14 C13 175.2(9) . . . . ?
N5 N4 C14 C16 -178.0(10) . . . . ?
C11 N4 C14 C16 -2.6(16) . . . . ?
C12 C13 C14 N4 -1.7(11) . . . . ?
C17 C13 C14 N4 -176.1(9) . . . . ?
C12 C13 C14 C16 175.8(11) . . . . ?
C17 C13 C14 C16 1.3(19) . . . . ?
C14 C13 C17 C21 -50.6(15) . . . . ?
C12 C13 C17 C21 136.1(12) . . . . ?
C14 C13 C17 C18 123.1(11) . . . . ?
C12 C13 C17 C18 -50.1(15) . . . . ?
C21 C17 C18 C19 2.0(13) . . . . ?
C13 C17 C18 C19 -172.2(8) . . . . ?
C20 N6 C19 C18 -0.3(13) . . . . ?
Zn2 N6 C19 C18 166.8(7) 4_665 . . . ?
C17 C18 C19 N6 -1.8(14) . . . . ?
C19 N6 C20 C21 2.3(16) . . . . ?
Zn2 N6 C20 C21 -164.4(9) 4_665 . . . ?
N6 C20 C21 C17 -2.1(18) . . . . ?
C18 C17 C21 C20 -0.2(16) . . . . ?
C13 C17 C21 C20 173.8(10) . . . . ?
C27 C22 C23 C24 0.5(13) . . . . ?
C28 C22 C23 C24 179.6(7) . . . . ?
C22 C23 C24 C25 -0.7(13) . . . . ?
C23 C24 C25 C26 0.3(13) . . . . ?
C23 C24 C25 C29 179.0(7) . . . . ?
C24 C25 C26 C27 0.2(14) . . . . ?
C29 C25 C26 C27 -178.5(9) . . . . ?
C25 C26 C27 C22 -0.3(16) . . . . ?
C23 C22 C27 C26 0.0(15) . . . . ?
C28 C22 C27 C26 -179.1(9) . . . . ?
Zn2 O1 C28 O2 -5.1(13) . . . . ?
Zn2 O1 C28 C22 176.4(5) . . . . ?
Zn1 O2 C28 O1 1.9(11) . . . . ?
Zn1 O2 C28 C22 -179.7(5) . . . . ?
C23 C22 C28 O1 179.4(8) . . . . ?
C27 C22 C28 O1 -1.6(12) . . . . ?
C23 C22 C28 O2 0.8(11) . . . . ?
C27 C22 C28 O2 179.9(8) . . . . ?
Zn1 O3 C29 O4 0.4(13) 1_455 . . . ?
Zn1 O3 C29 C25 -179.6(5) 1_455 . . . ?
Zn2 O4 C29 O3 -0.5(11) 1_455 . . . ?
Zn2 O4 C29 C25 179.6(5) 1_455 . . . ?
C24 C25 C29 O3 -0.2(11) . . . . ?
C26 C25 C29 O3 178.4(8) . . . . ?
C24 C25 C29 O4 179.7(7) . . . . ?
C26 C25 C29 O4 -1.6(12) . . . . ?
C35 C30 C31 C32 0.1(11) . . . . ?
C36 C30 C31 C32 179.9(7) . . . . ?
C30 C31 C32 C33 0.2(11) . . . . ?
C31 C32 C33 C34 0.1(11) . . . . ?
C31 C32 C33 C37 179.6(7) . . . . ?
C32 C33 C34 C35 -0.6(11) . . . . ?
C37 C33 C34 C35 179.9(7) . . . . ?
C31 C30 C35 C34 -0.7(11) . . . . ?
C36 C30 C35 C34 179.6(7) . . . . ?
C33 C34 C35 C30 0.9(11) . . . . ?
Zn2 O6 C36 O5 -1.9(11) . . . . ?
Zn2 O6 C36 C30 178.6(5) . . . . ?
Zn1 O5 C36 O6 -2.3(12) . . . . ?
Zn1 O5 C36 C30 177.1(5) . . . . ?
C35 C30 C36 O6 175.0(7) . . . . ?
C31 C30 C36 O6 -4.7(11) . . . . ?
C35 C30 C36 O5 -4.5(11) . . . . ?
C31 C30 C36 O5 175.7(7) . . . . ?
Zn1 O8 C37 O7 1.2(11) 1_565 . . . ?
Zn1 O8 C37 C33 -179.7(5) 1_565 . . . ?
Zn2 O7 C37 O8 -0.9(13) 1_565 . . . ?
Zn2 O7 C37 C33 -180.0(5) 1_565 . . . ?
C32 C33 C37 O8 -177.0(7) . . . . ?
C34 C33 C37 O8 2.4(10) . . . . ?
C32 C33 C37 O7 2.1(11) . . . . ?
C34 C33 C37 O7 -178.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.153

#===END


