# 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        'Ji-Qing Xu'
_publ_contact_author_email       XJQ@MAIL.JLU.EDU.CN

_publ_section_title              
;
A Series of Metal?organic Complexes Constructed from
In Situ Generated Organic Amines
;
loop_
_publ_author_name
'Ji-Qing Xu.'
'Xiao-Bing Cui.'
'Qin Hou.'
'Jing Lu.'
'Tie-Gang Wang.'
;
Qing-Feng Yang
;
'Xiao-Yang Yu.'
'Jie-Hui Yu.'
'Xiao Zhang.'

# Attachment 'cif.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 675375'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H20 N8 Zn2'
_chemical_formula_sum            'C28 H20 N8 Zn2'
_chemical_formula_weight         599.26

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'
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                   16.106(3)
_cell_length_b                   16.126(3)
_cell_length_c                   19.511(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.37(3)
_cell_angle_gamma                90.00
_cell_volume                     5036.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2432
_exptl_absorpt_coefficient_mu    1.940
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24425
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.47
_reflns_number_total             5744
_reflns_number_gt                2734
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0669P)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         5744
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1158
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 1.09397(4) 0.7500 0.0182(2) Uani 1 2 d S . .
Zn2 Zn 0.75150(2) 0.84265(4) 0.750036(18) 0.01786(19) Uani 1 1 d . . .
Zn3 Zn 1.0000 0.59126(4) 0.7500 0.0181(2) Uani 1 2 d S . .
C1 C 1.1445(2) 1.1987(2) 0.7265(2) 0.0246(8) Uani 1 1 d . . .
H1 H 1.1760 1.1732 0.7634 0.030 Uiso 1 1 calc R . .
C2 C 1.0437(2) 1.22478(19) 0.64706(19) 0.0212(8) Uani 1 1 d . . .
C3 C 1.1054(2) 1.28528(19) 0.64542(19) 0.0220(8) Uani 1 1 d . . .
C4 C 1.0963(3) 1.3513(2) 0.5989(2) 0.0323(10) Uani 1 1 d . . .
H4 H 1.1380 1.3909 0.5970 0.039 Uiso 1 1 calc R . .
C5 C 1.0225(3) 1.3549(2) 0.5561(2) 0.0343(10) Uani 1 1 d . . .
H5 H 1.0137 1.3988 0.5252 0.041 Uiso 1 1 calc R . .
C6 C 0.9601(3) 1.2945(2) 0.5576(2) 0.0352(10) Uani 1 1 d . . .
H6 H 0.9113 1.2989 0.5276 0.042 Uiso 1 1 calc R . .
C7 C 0.9701(2) 1.2286(2) 0.6030(2) 0.0314(9) Uani 1 1 d . . .
H7 H 0.9289 1.1884 0.6040 0.038 Uiso 1 1 calc R . .
C8 C 0.8523(2) 0.9880(2) 0.7255(2) 0.0270(9) Uani 1 1 d . . .
H8 H 0.8304 1.0143 0.7620 0.032 Uiso 1 1 calc R . .
C9 C 0.8703(2) 0.89990(19) 0.64660(19) 0.0215(8) Uani 1 1 d . . .
C10 C 0.9305(2) 0.96260(19) 0.64607(18) 0.0212(8) Uani 1 1 d . . .
C11 C 0.9906(2) 0.9601(2) 0.5998(2) 0.0300(9) Uani 1 1 d . . .
H11 H 1.0295 1.0025 0.5983 0.036 Uiso 1 1 calc R . .
C12 C 0.9902(3) 0.8924(3) 0.5565(2) 0.0371(11) Uani 1 1 d . . .
H12 H 1.0309 0.8882 0.5263 0.045 Uiso 1 1 calc R . .
C13 C 0.9299(3) 0.8298(2) 0.5570(2) 0.0343(10) Uani 1 1 d . . .
H13 H 0.9307 0.7857 0.5264 0.041 Uiso 1 1 calc R . .
C14 C 0.8698(2) 0.8322(2) 0.6014(2) 0.0273(9) Uani 1 1 d . . .
H14 H 0.8300 0.7904 0.6015 0.033 Uiso 1 1 calc R . .
C15 C 0.8987(2) 0.7375(2) 0.7747(2) 0.0258(9) Uani 1 1 d . . .
H15 H 0.9199 0.7639 0.7379 0.031 Uiso 1 1 calc R . .
C16 C 0.8210(2) 0.7101(2) 0.85443(19) 0.0234(8) Uani 1 1 d . . .
C17 C 0.7616(2) 0.7073(2) 0.9010(2) 0.0294(9) Uani 1 1 d . . .
H17 H 0.7220 0.7490 0.9027 0.035 Uiso 1 1 calc R . .
C18 C 0.7642(3) 0.6398(3) 0.9446(2) 0.0363(10) Uani 1 1 d . . .
H18 H 0.7250 0.6356 0.9760 0.044 Uiso 1 1 calc R . .
C19 C 0.8244(3) 0.5774(2) 0.9427(2) 0.0351(10) Uani 1 1 d . . .
H19 H 0.8241 0.5326 0.9728 0.042 Uiso 1 1 calc R . .
C20 C 0.8840(3) 0.5808(2) 0.8974(2) 0.0302(9) Uani 1 1 d . . .
H20 H 0.9240 0.5393 0.8964 0.036 Uiso 1 1 calc R . .
C21 C 0.8823(2) 0.64803(19) 0.85344(19) 0.0222(8) Uani 1 1 d . . .
C22 C 0.8922(2) 0.4463(2) 0.7264(2) 0.0248(8) Uani 1 1 d . . .
H22 H 0.9232 0.4201 0.7632 0.030 Uiso 1 1 calc R . .
C23 C 0.8555(2) 0.53457(19) 0.64583(19) 0.0212(8) Uani 1 1 d . . .
C24 C 0.8475(3) 0.6014(2) 0.5996(2) 0.0301(9) Uani 1 1 d . . .
H24 H 0.8894 0.6410 0.5987 0.036 Uiso 1 1 calc R . .
C25 C 0.7749(3) 0.6056(2) 0.5558(2) 0.0364(11) Uani 1 1 d . . .
H25 H 0.7676 0.6493 0.5246 0.044 Uiso 1 1 calc R . .
C26 C 0.7113(3) 0.5463(2) 0.5562(2) 0.0347(10) Uani 1 1 d . . .
H26 H 0.6629 0.5518 0.5258 0.042 Uiso 1 1 calc R . .
C27 C 0.7195(2) 0.4799(2) 0.6011(2) 0.0268(8) Uani 1 1 d . . .
H27 H 0.6779 0.4400 0.6011 0.032 Uiso 1 1 calc R . .
C28 C 0.7926(2) 0.47489(19) 0.64617(18) 0.0212(8) Uani 1 1 d . . .
N1 N 1.0704(3) 1.1694(2) 0.6989(2) 0.0228(10) Uani 1 1 d . . .
N2 N 1.1695(3) 1.2674(2) 0.6968(2) 0.0223(10) Uani 1 1 d . . .
N3 N 0.8204(3) 0.9170(2) 0.6987(2) 0.0238(10) Uani 1 1 d . . .
N4 N 0.9167(2) 1.0190(2) 0.6974(2) 0.0249(10) Uani 1 1 d . . .
N5 N 0.8176(2) 0.4178(2) 0.6990(2) 0.0227(10) Uani 1 1 d . . .
N6 N 0.9189(2) 0.5145(2) 0.6974(2) 0.0253(10) Uani 1 1 d . . .
N7 N 0.9314(2) 0.6679(2) 0.8015(2) 0.0211(9) Uani 1 1 d . . .
N8 N 0.8337(2) 0.7675(2) 0.8033(2) 0.0218(10) 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
Zn1 N4 2.002(4) . ?
Zn1 N4 2.002(4) 2_756 ?
Zn1 N1 2.003(3) . ?
Zn1 N1 2.003(3) 2_756 ?
Zn2 N3 1.980(4) . ?
Zn2 N5 1.986(3) 4_656 ?
Zn2 N2 1.998(4) 3_445 ?
Zn2 N8 1.999(4) . ?
Zn3 N6 1.999(4) . ?
Zn3 N6 1.999(4) 2_756 ?
Zn3 N7 2.000(3) 2_756 ?
Zn3 N7 2.000(3) . ?
C1 N2 1.332(5) . ?
C1 N1 1.340(5) . ?
C1 H1 0.9300 . ?
C2 N1 1.382(5) . ?
C2 C7 1.387(5) . ?
C2 C3 1.395(4) . ?
C3 N2 1.387(5) . ?
C3 C4 1.396(5) . ?
C4 C5 1.376(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.380(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N4 1.325(5) . ?
C8 N3 1.338(5) . ?
C8 H8 0.9300 . ?
C9 N3 1.392(5) . ?
C9 C10 1.402(4) . ?
C9 C14 1.403(5) . ?
C10 N4 1.389(5) . ?
C10 C11 1.395(5) . ?
C11 C12 1.380(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.402(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 N7 1.322(5) . ?
C15 N8 1.332(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(5) . ?
C16 N8 1.392(5) . ?
C16 C21 1.407(4) . ?
C17 C18 1.379(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.401(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(5) . ?
C20 H20 0.9300 . ?
C21 N7 1.391(5) . ?
C22 N6 1.329(5) . ?
C22 N5 1.341(5) . ?
C22 H22 0.9300 . ?
C23 N6 1.390(5) . ?
C23 C28 1.399(4) . ?
C23 C24 1.402(5) . ?
C24 C25 1.372(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.402(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.381(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.391(5) . ?
C27 H27 0.9300 . ?
C28 N5 1.407(5) . ?
N2 Zn2 1.998(4) 3 ?
N5 Zn2 1.986(3) 4_646 ?

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 Zn1 N4 105.7(2) . 2_756 ?
N4 Zn1 N1 119.68(16) . . ?
N4 Zn1 N1 103.75(17) 2_756 . ?
N4 Zn1 N1 103.75(16) . 2_756 ?
N4 Zn1 N1 119.68(16) 2_756 2_756 ?
N1 Zn1 N1 105.2(2) . 2_756 ?
N3 Zn2 N5 105.09(19) . 4_656 ?
N3 Zn2 N2 118.71(16) . 3_445 ?
N5 Zn2 N2 104.83(17) 4_656 3_445 ?
N3 Zn2 N8 104.74(17) . . ?
N5 Zn2 N8 119.02(16) 4_656 . ?
N2 Zn2 N8 105.3(2) 3_445 . ?
N6 Zn3 N6 103.4(2) . 2_756 ?
N6 Zn3 N7 119.42(16) . 2_756 ?
N6 Zn3 N7 105.93(16) 2_756 2_756 ?
N6 Zn3 N7 105.93(16) . . ?
N6 Zn3 N7 119.42(16) 2_756 . ?
N7 Zn3 N7 103.7(2) 2_756 . ?
N2 C1 N1 114.7(4) . . ?
N2 C1 H1 122.7 . . ?
N1 C1 H1 122.7 . . ?
N1 C2 C7 131.1(3) . . ?
N1 C2 C3 107.7(3) . . ?
C7 C2 C3 121.1(3) . . ?
N2 C3 C2 108.2(3) . . ?
N2 C3 C4 130.1(3) . . ?
C2 C3 C4 121.7(4) . . ?
C5 C4 C3 116.6(3) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
C4 C5 C6 122.0(4) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C5 121.1(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C2 117.5(3) . . ?
C6 C7 H7 121.2 . . ?
C2 C7 H7 121.2 . . ?
N4 C8 N3 116.4(4) . . ?
N4 C8 H8 121.8 . . ?
N3 C8 H8 121.8 . . ?
N3 C9 C10 108.6(3) . . ?
N3 C9 C14 130.5(3) . . ?
C10 C9 C14 120.8(3) . . ?
N4 C10 C11 131.5(3) . . ?
N4 C10 C9 107.5(3) . . ?
C11 C10 C9 121.0(3) . . ?
C12 C11 C10 117.6(3) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C11 C12 C13 121.4(4) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 121.6(4) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C9 117.6(3) . . ?
C13 C14 H14 121.2 . . ?
C9 C14 H14 121.2 . . ?
N7 C15 N8 116.1(4) . . ?
N7 C15 H15 122.0 . . ?
N8 C15 H15 122.0 . . ?
C17 C16 N8 131.0(3) . . ?
C17 C16 C21 121.3(3) . . ?
N8 C16 C21 107.7(3) . . ?
C18 C17 C16 116.9(3) . . ?
C18 C17 H17 121.5 . . ?
C16 C17 H17 121.5 . . ?
C17 C18 C19 121.7(4) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C20 C19 C18 121.4(4) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 117.6(3) . . ?
C19 C20 H20 121.2 . . ?
C21 C20 H20 121.2 . . ?
C20 C21 N7 131.3(3) . . ?
C20 C21 C16 121.1(3) . . ?
N7 C21 C16 107.6(3) . . ?
N6 C22 N5 115.6(4) . . ?
N6 C22 H22 122.2 . . ?
N5 C22 H22 122.2 . . ?
N6 C23 C28 108.1(3) . . ?
N6 C23 C24 130.8(3) . . ?
C28 C23 C24 121.1(3) . . ?
C25 C24 C23 116.7(3) . . ?
C25 C24 H24 121.6 . . ?
C23 C24 H24 121.6 . . ?
C24 C25 C26 122.4(4) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C25 120.9(4) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C28 117.5(3) . . ?
C26 C27 H27 121.3 . . ?
C28 C27 H27 121.3 . . ?
C27 C28 C23 121.3(3) . . ?
C27 C28 N5 130.9(3) . . ?
C23 C28 N5 107.7(3) . . ?
C1 N1 C2 104.9(3) . . ?
C1 N1 Zn1 122.9(3) . . ?
C2 N1 Zn1 127.5(3) . . ?
C1 N2 C3 104.5(4) . . ?
C1 N2 Zn2 119.6(3) . 3 ?
C3 N2 Zn2 130.2(3) . 3 ?
C8 N3 C9 103.2(3) . . ?
C8 N3 Zn2 122.2(3) . . ?
C9 N3 Zn2 130.6(3) . . ?
C8 N4 C10 104.3(3) . . ?
C8 N4 Zn1 121.7(3) . . ?
C10 N4 Zn1 127.8(3) . . ?
C22 N5 C28 103.8(3) . . ?
C22 N5 Zn2 122.5(3) . 4_646 ?
C28 N5 Zn2 129.4(3) . 4_646 ?
C22 N6 C23 104.8(3) . . ?
C22 N6 Zn3 121.2(3) . . ?
C23 N6 Zn3 127.8(3) . . ?
C15 N7 C21 104.5(3) . . ?
C15 N7 Zn3 122.9(3) . . ?
C21 N7 Zn3 127.9(2) . . ?
C15 N8 C16 104.1(3) . . ?
C15 N8 Zn2 120.6(3) . . ?
C16 N8 Zn2 129.4(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
N1 C2 C3 N2 -0.7(4) . . . . ?
C7 C2 C3 N2 177.3(3) . . . . ?
N1 C2 C3 C4 -179.0(3) . . . . ?
C7 C2 C3 C4 -1.0(5) . . . . ?
N2 C3 C4 C5 -176.2(4) . . . . ?
C2 C3 C4 C5 1.7(5) . . . . ?
C3 C4 C5 C6 -1.4(6) . . . . ?
C4 C5 C6 C7 0.5(6) . . . . ?
C5 C6 C7 C2 0.3(6) . . . . ?
N1 C2 C7 C6 177.5(4) . . . . ?
C3 C2 C7 C6 0.0(5) . . . . ?
N3 C9 C10 N4 -0.9(4) . . . . ?
C14 C9 C10 N4 -178.2(4) . . . . ?
N3 C9 C10 C11 178.4(4) . . . . ?
C14 C9 C10 C11 1.1(5) . . . . ?
N4 C10 C11 C12 176.9(4) . . . . ?
C9 C10 C11 C12 -2.2(6) . . . . ?
C10 C11 C12 C13 2.3(6) . . . . ?
C11 C12 C13 C14 -1.3(7) . . . . ?
C12 C13 C14 C9 0.2(6) . . . . ?
N3 C9 C14 C13 -176.7(4) . . . . ?
C10 C9 C14 C13 -0.1(6) . . . . ?
N8 C16 C17 C18 178.2(4) . . . . ?
C21 C16 C17 C18 -1.8(6) . . . . ?
C16 C17 C18 C19 0.8(6) . . . . ?
C17 C18 C19 C20 0.2(7) . . . . ?
C18 C19 C20 C21 -0.2(6) . . . . ?
C19 C20 C21 N7 -177.9(4) . . . . ?
C19 C20 C21 C16 -0.9(6) . . . . ?
C17 C16 C21 C20 2.0(5) . . . . ?
N8 C16 C21 C20 -178.0(4) . . . . ?
C17 C16 C21 N7 179.6(4) . . . . ?
N8 C16 C21 N7 -0.4(4) . . . . ?
N6 C23 C24 C25 -177.6(4) . . . . ?
C28 C23 C24 C25 0.7(5) . . . . ?
C23 C24 C25 C26 -0.2(6) . . . . ?
C24 C25 C26 C27 -0.6(6) . . . . ?
C25 C26 C27 C28 0.9(6) . . . . ?
C26 C27 C28 C23 -0.4(5) . . . . ?
C26 C27 C28 N5 177.0(4) . . . . ?
N6 C23 C28 C27 178.3(3) . . . . ?
C24 C23 C28 C27 -0.4(5) . . . . ?
N6 C23 C28 N5 0.3(4) . . . . ?
C24 C23 C28 N5 -178.3(3) . . . . ?
N2 C1 N1 C2 -1.1(5) . . . . ?
N2 C1 N1 Zn1 -158.4(3) . . . . ?
C7 C2 N1 C1 -176.7(4) . . . . ?
C3 C2 N1 C1 1.1(4) . . . . ?
C7 C2 N1 Zn1 -20.9(6) . . . . ?
C3 C2 N1 Zn1 156.9(3) . . . . ?
N4 Zn1 N1 C1 -156.0(3) . . . . ?
N4 Zn1 N1 C1 -38.6(3) 2_756 . . . ?
N1 Zn1 N1 C1 87.9(3) 2_756 . . . ?
N4 Zn1 N1 C2 52.1(4) . . . . ?
N4 Zn1 N1 C2 169.5(3) 2_756 . . . ?
N1 Zn1 N1 C2 -63.9(3) 2_756 . . . ?
N1 C1 N2 C3 0.7(5) . . . . ?
N1 C1 N2 Zn2 156.7(3) . . . 3 ?
C2 C3 N2 C1 0.0(4) . . . . ?
C4 C3 N2 C1 178.1(4) . . . . ?
C2 C3 N2 Zn2 -152.3(3) . . . 3 ?
C4 C3 N2 Zn2 25.8(6) . . . 3 ?
N4 C8 N3 C9 -0.1(5) . . . . ?
N4 C8 N3 Zn2 159.5(3) . . . . ?
C10 C9 N3 C8 0.6(4) . . . . ?
C14 C9 N3 C8 177.6(4) . . . . ?
C10 C9 N3 Zn2 -156.6(3) . . . . ?
C14 C9 N3 Zn2 20.4(7) . . . . ?
N5 Zn2 N3 C8 37.8(3) 4_656 . . . ?
N2 Zn2 N3 C8 154.6(3) 3_445 . . . ?
N8 Zn2 N3 C8 -88.4(4) . . . . ?
N5 Zn2 N3 C9 -168.7(5) 4_656 . . . ?
N2 Zn2 N3 C9 -52.0(5) 3_445 . . . ?
N8 Zn2 N3 C9 65.1(4) . . . . ?
N3 C8 N4 C10 -0.4(5) . . . . ?
N3 C8 N4 Zn1 -154.9(3) . . . . ?
C11 C10 N4 C8 -178.4(4) . . . . ?
C9 C10 N4 C8 0.8(4) . . . . ?
C11 C10 N4 Zn1 -26.1(6) . . . . ?
C9 C10 N4 Zn1 153.1(3) . . . . ?
N4 Zn1 N4 C8 85.0(3) 2_756 . . . ?
N1 Zn1 N4 C8 -158.6(3) . . . . ?
N1 Zn1 N4 C8 -41.8(4) 2_756 . . . ?
N4 Zn1 N4 C10 -63.1(3) 2_756 . . . ?
N1 Zn1 N4 C10 53.3(4) . . . . ?
N1 Zn1 N4 C10 170.1(4) 2_756 . . . ?
N6 C22 N5 C28 -0.5(5) . . . . ?
N6 C22 N5 Zn2 -159.3(3) . . . 4_646 ?
C27 C28 N5 C22 -177.6(4) . . . . ?
C23 C28 N5 C22 0.1(4) . . . . ?
C27 C28 N5 Zn2 -20.9(6) . . . 4_646 ?
C23 C28 N5 Zn2 156.8(3) . . . 4_646 ?
N5 C22 N6 C23 0.7(5) . . . . ?
N5 C22 N6 Zn3 154.9(3) . . . . ?
C28 C23 N6 C22 -0.6(4) . . . . ?
C24 C23 N6 C22 177.9(4) . . . . ?
C28 C23 N6 Zn3 -152.6(3) . . . . ?
C24 C23 N6 Zn3 25.9(6) . . . . ?
N6 Zn3 N6 C22 41.1(3) 2_756 . . . ?
N7 Zn3 N6 C22 158.3(3) 2_756 . . . ?
N7 Zn3 N6 C22 -85.3(3) . . . . ?
N6 Zn3 N6 C23 -171.0(4) 2_756 . . . ?
N7 Zn3 N6 C23 -53.8(4) 2_756 . . . ?
N7 Zn3 N6 C23 62.6(4) . . . . ?
N8 C15 N7 C21 0.9(5) . . . . ?
N8 C15 N7 Zn3 158.2(3) . . . . ?
C20 C21 N7 C15 177.1(4) . . . . ?
C16 C21 N7 C15 -0.3(4) . . . . ?
C20 C21 N7 Zn3 21.3(7) . . . . ?
C16 C21 N7 Zn3 -156.1(3) . . . . ?
N6 Zn3 N7 C15 -87.5(4) . . . . ?
N6 Zn3 N7 C15 156.5(3) 2_756 . . . ?
N7 Zn3 N7 C15 39.0(3) 2_756 . . . ?
N6 Zn3 N7 C21 64.3(4) . . . . ?
N6 Zn3 N7 C21 -51.7(4) 2_756 . . . ?
N7 Zn3 N7 C21 -169.2(5) 2_756 . . . ?
N7 C15 N8 C16 -1.1(5) . . . . ?
N7 C15 N8 Zn2 -156.3(3) . . . . ?
C17 C16 N8 C15 -179.2(4) . . . . ?
C21 C16 N8 C15 0.8(4) . . . . ?
C17 C16 N8 Zn2 -27.0(6) . . . . ?
C21 C16 N8 Zn2 153.0(3) . . . . ?
N3 Zn2 N8 C15 -40.6(4) . . . . ?
N5 Zn2 N8 C15 -157.6(3) 4_656 . . . ?
N2 Zn2 N8 C15 85.4(3) 3_445 . . . ?
N3 Zn2 N8 C16 171.2(3) . . . . ?
N5 Zn2 N8 C16 54.2(4) 4_656 . . . ?
N2 Zn2 N8 C16 -62.9(4) 3_445 . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.108

data_2
_database_code_depnum_ccdc_archive 'CCDC 675376'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H20.67 Cd N8 O4.33 S'
_chemical_formula_sum            'C28 H20.67 Cd N8 O4.33 S'
_chemical_formula_weight         682.93

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.118(2)
_cell_length_b                   12.765(3)
_cell_length_c                   13.366(3)
_cell_angle_alpha                66.445(4)
_cell_angle_beta                 72.416(4)
_cell_angle_gamma                80.184(4)
_cell_volume                     1357.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      25.10

_exptl_crystal_description       club-shaped
_exptl_crystal_colour            light-blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             687
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7143
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4748
_reflns_number_gt                4315
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0491P)²+0.9716P] 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         4748
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1117
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_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
C1 C 1.0438(6) 0.7564(4) 0.7471(4) 0.0354(11) Uani 1 1 d . . .
C2 C 0.9707(7) 0.6585(5) 0.8247(4) 0.0482(14) Uani 1 1 d . . .
H2 H 0.8656 0.6607 0.8588 0.058 Uiso 1 1 calc R . .
C3 C 1.0604(8) 0.5574(5) 0.8496(5) 0.0612(17) Uani 1 1 d . . .
H3 H 1.0149 0.4900 0.9016 0.073 Uiso 1 1 calc R . .
C4 C 1.2186(8) 0.5548(5) 0.7977(5) 0.0635(18) Uani 1 1 d . . .
H4 H 1.2757 0.4852 0.8167 0.076 Uiso 1 1 calc R . .
C5 C 1.2925(7) 0.6508(5) 0.7201(5) 0.0561(16) Uani 1 1 d . . .
H5 H 1.3976 0.6480 0.6861 0.067 Uiso 1 1 calc R . .
C6 C 1.2024(6) 0.7530(5) 0.6947(4) 0.0392(12) Uani 1 1 d . . .
C7 C 1.1046(5) 0.9284(4) 0.6323(4) 0.0315(11) Uani 1 1 d . . .
C8 C 1.0815(5) 1.0510(4) 0.5746(3) 0.0315(11) Uani 1 1 d . . .
C9 C 0.9612(6) 1.2164(4) 0.5267(4) 0.0348(11) Uani 1 1 d . . .
C10 C 0.8533(7) 1.3097(5) 0.5113(4) 0.0489(14) Uani 1 1 d . . .
H10 H 0.7485 1.2999 0.5443 0.059 Uiso 1 1 calc R . .
C11 C 0.9073(8) 1.4150(5) 0.4463(5) 0.0571(16) Uani 1 1 d . . .
H11 H 0.8379 1.4784 0.4357 0.068 Uiso 1 1 calc R . .
C12 C 1.0633(8) 1.4311(5) 0.3950(5) 0.0629(17) Uani 1 1 d . . .
H12 H 1.0949 1.5049 0.3505 0.075 Uiso 1 1 calc R . .
C13 C 1.1717(7) 1.3415(5) 0.4081(5) 0.0576(16) Uani 1 1 d . . .
H13 H 1.2762 1.3525 0.3746 0.069 Uiso 1 1 calc R . .
C14 C 1.1171(6) 1.2334(4) 0.4740(4) 0.0364(11) Uani 1 1 d . . .
C15 C 0.8965(5) 1.1246(4) 0.8760(4) 0.0305(10) Uani 1 1 d . . .
C16 C 0.9997(6) 1.2032(4) 0.7930(4) 0.0397(12) Uani 1 1 d . . .
H16 H 1.0196 1.2134 0.7174 0.048 Uiso 1 1 calc R . .
C17 C 1.0717(6) 1.2656(4) 0.8258(4) 0.0434(13) Uani 1 1 d . . .
H17 H 1.1416 1.3187 0.7716 0.052 Uiso 1 1 calc R . .
C18 C 1.0413(6) 1.2505(4) 0.9406(5) 0.0437(13) Uani 1 1 d . . .
H18 H 1.0926 1.2935 0.9602 0.052 Uiso 1 1 calc R . .
C19 C 0.9384(6) 1.1742(4) 1.0243(4) 0.0381(12) Uani 1 1 d . . .
H19 H 0.9180 1.1649 1.0998 0.046 Uiso 1 1 calc R . .
C20 C 0.8663(5) 1.1113(4) 0.9899(4) 0.0303(10) Uani 1 1 d . . .
C21 C 0.7368(5) 0.9916(4) 0.9755(4) 0.0280(10) Uani 1 1 d . . .
C22 C 0.6428(5) 0.8996(4) 1.0007(4) 0.0303(10) Uani 1 1 d . . .
C23 C 0.4940(5) 0.7529(4) 1.0866(4) 0.0357(11) Uani 1 1 d . . .
C24 C 0.3984(6) 0.6649(5) 1.1598(5) 0.0497(14) Uani 1 1 d . . .
H24 H 0.3680 0.6485 1.2372 0.060 Uiso 1 1 calc R . .
C25 C 0.3506(7) 0.6033(5) 1.1131(5) 0.0582(16) Uani 1 1 d . . .
H25 H 0.2877 0.5427 1.1598 0.070 Uiso 1 1 calc R . .
C26 C 0.3946(7) 0.6297(5) 0.9961(5) 0.0570(16) Uani 1 1 d . . .
H26 H 0.3592 0.5865 0.9671 0.068 Uiso 1 1 calc R . .
C27 C 0.4873(6) 0.7166(5) 0.9234(5) 0.0475(14) Uani 1 1 d . . .
H27 H 0.5155 0.7335 0.8459 0.057 Uiso 1 1 calc R . .
C28 C 0.5380(5) 0.7785(4) 0.9695(4) 0.0341(11) Uani 1 1 d . . .
Cd1 Cd 0.76697(4) 0.98467(3) 0.74042(3) 0.03143(14) Uani 1 1 d . . .
N1 N 0.9866(4) 0.8685(3) 0.7060(3) 0.0324(9) Uani 1 1 d . . .
N2 N 1.2368(5) 0.8632(4) 0.6221(3) 0.0374(10) Uani 1 1 d . . .
H2A H 1.3256 0.8860 0.5786 0.045 Uiso 1 1 calc R . .
N3 N 1.1906(5) 1.1258(4) 0.5064(3) 0.0404(10) Uani 1 1 d . . .
H3A H 1.2879 1.1096 0.4866 0.049 Uiso 1 1 calc R . .
N4 N 0.9415(4) 1.1010(3) 0.5887(3) 0.0321(9) Uani 1 1 d . . .
N5 N 0.8110(4) 1.0494(3) 0.8692(3) 0.0302(9) Uani 1 1 d . . .
N6 N 0.7646(4) 1.0269(3) 1.0502(3) 0.0333(9) Uani 1 1 d . . .
H6 H 0.7257 1.0012 1.1222 0.040 Uiso 1 1 calc R . .
N7 N 0.5618(4) 0.8318(3) 1.1038(3) 0.0350(9) Uani 1 1 d . . .
H7 H 0.5539 0.8367 1.1676 0.042 Uiso 1 1 calc R . .
N8 N 0.6334(5) 0.8705(3) 0.9172(3) 0.0342(9) Uani 1 1 d . . .
O1 O 0.5920(4) 0.9603(4) 0.6596(3) 0.0539(10) Uani 1 1 d . . .
O2 O 0.4843(4) 1.1268(4) 0.5349(3) 0.0543(11) Uani 1 1 d . . .
O3 O 0.3295(4) 1.0308(3) 0.7214(3) 0.0481(10) Uani 1 1 d . . .
O4 O 0.5467(4) 1.1304(3) 0.6975(3) 0.0492(9) Uani 1 1 d . . .
S1 S 0.48438(14) 1.06224(12) 0.65344(10) 0.0382(3) Uani 1 1 d . . .
O1W O 0.4288(16) 0.3824(11) 0.5714(15) 0.103(6) Uani 0.33 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
C1 N1 1.383(6) . ?
C1 C2 1.383(7) . ?
C1 C6 1.405(7) . ?
C2 C3 1.380(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.401(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(7) . ?
C5 H5 0.9300 . ?
C6 N2 1.376(6) . ?
C7 N1 1.322(6) . ?
C7 N2 1.347(6) . ?
C7 C8 1.453(7) . ?
C8 N4 1.321(6) . ?
C8 N3 1.346(6) . ?
C9 N4 1.383(6) . ?
C9 C14 1.394(7) . ?
C9 C10 1.399(7) . ?
C10 C11 1.356(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.369(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(7) . ?
C13 H13 0.9300 . ?
C14 N3 1.382(6) . ?
C15 N5 1.381(6) . ?
C15 C16 1.387(7) . ?
C15 C20 1.407(6) . ?
C16 C17 1.375(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.412(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.374(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.395(6) . ?
C19 H19 0.9300 . ?
C20 N6 1.366(6) . ?
C21 N5 1.330(6) . ?
C21 N6 1.348(6) . ?
C21 C22 1.443(6) . ?
C22 N8 1.337(6) . ?
C22 N7 1.358(6) . ?
C23 C24 1.385(7) . ?
C23 N7 1.390(6) . ?
C23 C28 1.405(7) . ?
C24 C25 1.369(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.402(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.360(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(7) . ?
C27 H27 0.9300 . ?
C28 N8 1.397(6) . ?
Cd1 O1 2.299(4) . ?
Cd1 N4 2.302(4) . ?
Cd1 N8 2.302(4) . ?
Cd1 N1 2.323(4) . ?
Cd1 N5 2.340(4) . ?
Cd1 O4 2.528(4) . ?
N2 H2A 0.8600 . ?
N3 H3A 0.8600 . ?
N6 H6 0.8600 . ?
N7 H7 0.8600 . ?
O1 S1 1.480(4) . ?
O2 S1 1.465(3) . ?
O3 S1 1.451(4) . ?
O4 S1 1.485(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 130.7(5) . . ?
N1 C1 C6 107.9(4) . . ?
C2 C1 C6 121.4(5) . . ?
C3 C2 C1 117.2(6) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C2 C3 C4 121.1(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 122.4(6) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C4 C5 C6 116.7(6) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
N2 C6 C5 132.3(5) . . ?
N2 C6 C1 106.5(4) . . ?
C5 C6 C1 121.2(5) . . ?
N1 C7 N2 112.5(4) . . ?
N1 C7 C8 119.6(4) . . ?
N2 C7 C8 127.9(4) . . ?
N4 C8 N3 112.7(4) . . ?
N4 C8 C7 120.2(4) . . ?
N3 C8 C7 127.1(4) . . ?
N4 C9 C14 109.5(4) . . ?
N4 C9 C10 130.5(5) . . ?
C14 C9 C10 120.0(5) . . ?
C11 C10 C9 117.4(6) . . ?
C11 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
C10 C11 C12 122.1(6) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C13 C12 C11 121.9(6) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 116.3(6) . . ?
C12 C13 H13 121.8 . . ?
C14 C13 H13 121.8 . . ?
N3 C14 C13 132.4(5) . . ?
N3 C14 C9 105.3(4) . . ?
C13 C14 C9 122.3(5) . . ?
N5 C15 C16 131.2(4) . . ?
N5 C15 C20 108.6(4) . . ?
C16 C15 C20 120.2(4) . . ?
C17 C16 C15 118.1(5) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C16 C17 C18 121.0(5) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 122.1(5) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C18 C19 C20 116.3(5) . . ?
C18 C19 H19 121.8 . . ?
C20 C19 H19 121.8 . . ?
N6 C20 C19 131.4(4) . . ?
N6 C20 C15 106.3(4) . . ?
C19 C20 C15 122.3(5) . . ?
N5 C21 N6 112.9(4) . . ?
N5 C21 C22 120.2(4) . . ?
N6 C21 C22 126.9(4) . . ?
N8 C22 N7 112.7(4) . . ?
N8 C22 C21 119.8(4) . . ?
N7 C22 C21 127.5(4) . . ?
C24 C23 N7 132.5(5) . . ?
C24 C23 C28 121.3(5) . . ?
N7 C23 C28 106.2(4) . . ?
C25 C24 C23 117.0(5) . . ?
C25 C24 H24 121.5 . . ?
C23 C24 H24 121.5 . . ?
C24 C25 C26 121.2(6) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C27 C26 C25 122.2(6) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C28 117.2(5) . . ?
C26 C27 H27 121.4 . . ?
C28 C27 H27 121.4 . . ?
C27 C28 N8 130.1(5) . . ?
C27 C28 C23 121.0(5) . . ?
N8 C28 C23 108.8(4) . . ?
O1 Cd1 N4 103.43(14) . . ?
O1 Cd1 N8 91.09(14) . . ?
N4 Cd1 N8 165.48(13) . . ?
O1 Cd1 N1 108.28(13) . . ?
N4 Cd1 N1 73.67(13) . . ?
N8 Cd1 N1 101.74(13) . . ?
O1 Cd1 N5 147.41(13) . . ?
N4 Cd1 N5 93.90(13) . . ?
N8 Cd1 N5 73.45(13) . . ?
N1 Cd1 N5 102.96(13) . . ?
O1 Cd1 O4 58.39(12) . . ?
N4 Cd1 O4 91.64(13) . . ?
N8 Cd1 O4 96.31(13) . . ?
N1 Cd1 O4 157.93(12) . . ?
N5 Cd1 O4 94.23(12) . . ?
C7 N1 C1 106.3(4) . . ?
C7 N1 Cd1 112.2(3) . . ?
C1 N1 Cd1 140.8(3) . . ?
C7 N2 C6 106.8(4) . . ?
C7 N2 H2A 126.6 . . ?
C6 N2 H2A 126.6 . . ?
C8 N3 C14 107.2(4) . . ?
C8 N3 H3A 126.4 . . ?
C14 N3 H3A 126.4 . . ?
C8 N4 C9 105.3(4) . . ?
C8 N4 Cd1 112.2(3) . . ?
C9 N4 Cd1 139.1(3) . . ?
C21 N5 C15 105.2(4) . . ?
C21 N5 Cd1 112.7(3) . . ?
C15 N5 Cd1 142.0(3) . . ?
C21 N6 C20 106.9(4) . . ?
C21 N6 H6 126.6 . . ?
C20 N6 H6 126.6 . . ?
C22 N7 C23 106.9(4) . . ?
C22 N7 H7 126.6 . . ?
C23 N7 H7 126.6 . . ?
C22 N8 C28 105.4(4) . . ?
C22 N8 Cd1 113.9(3) . . ?
C28 N8 Cd1 140.7(3) . . ?
S1 O1 Cd1 102.9(2) . . ?
S1 O4 Cd1 93.00(18) . . ?
O3 S1 O2 110.3(2) . . ?
O3 S1 O1 111.7(2) . . ?
O2 S1 O1 108.4(2) . . ?
O3 S1 O4 110.0(2) . . ?
O2 S1 O4 110.6(2) . . ?
O1 S1 O4 105.7(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
N1 C1 C2 C3 -179.5(5) . . . . ?
C6 C1 C2 C3 0.7(7) . . . . ?
C1 C2 C3 C4 -0.1(8) . . . . ?
C2 C3 C4 C5 -0.3(10) . . . . ?
C3 C4 C5 C6 0.2(9) . . . . ?
C4 C5 C6 N2 -179.6(5) . . . . ?
C4 C5 C6 C1 0.3(8) . . . . ?
N1 C1 C6 N2 -0.7(5) . . . . ?
C2 C1 C6 N2 179.1(4) . . . . ?
N1 C1 C6 C5 179.4(4) . . . . ?
C2 C1 C6 C5 -0.8(7) . . . . ?
N1 C7 C8 N4 -5.4(6) . . . . ?
N2 C7 C8 N4 175.5(4) . . . . ?
N1 C7 C8 N3 172.9(4) . . . . ?
N2 C7 C8 N3 -6.2(8) . . . . ?
N4 C9 C10 C11 179.0(5) . . . . ?
C14 C9 C10 C11 -1.5(7) . . . . ?
C9 C10 C11 C12 0.9(9) . . . . ?
C10 C11 C12 C13 -0.6(10) . . . . ?
C11 C12 C13 C14 1.0(9) . . . . ?
C12 C13 C14 N3 -179.0(5) . . . . ?
C12 C13 C14 C9 -1.6(8) . . . . ?
N4 C9 C14 N3 -0.4(5) . . . . ?
C10 C9 C14 N3 180.0(4) . . . . ?
N4 C9 C14 C13 -178.4(5) . . . . ?
C10 C9 C14 C13 2.0(7) . . . . ?
N5 C15 C16 C17 -178.4(5) . . . . ?
C20 C15 C16 C17 0.8(7) . . . . ?
C15 C16 C17 C18 -0.2(8) . . . . ?
C16 C17 C18 C19 -0.5(8) . . . . ?
C17 C18 C19 C20 0.6(7) . . . . ?
C18 C19 C20 N6 177.1(5) . . . . ?
C18 C19 C20 C15 0.0(7) . . . . ?
N5 C15 C20 N6 0.9(5) . . . . ?
C16 C15 C20 N6 -178.5(4) . . . . ?
N5 C15 C20 C19 178.6(4) . . . . ?
C16 C15 C20 C19 -0.8(7) . . . . ?
N5 C21 C22 N8 1.7(7) . . . . ?
N6 C21 C22 N8 -176.2(4) . . . . ?
N5 C21 C22 N7 179.1(4) . . . . ?
N6 C21 C22 N7 1.3(8) . . . . ?
N7 C23 C24 C25 179.3(5) . . . . ?
C28 C23 C24 C25 0.9(8) . . . . ?
C23 C24 C25 C26 -1.1(9) . . . . ?
C24 C25 C26 C27 0.6(10) . . . . ?
C25 C26 C27 C28 0.2(9) . . . . ?
C26 C27 C28 N8 179.6(5) . . . . ?
C26 C27 C28 C23 -0.5(8) . . . . ?
C24 C23 C28 C27 -0.1(7) . . . . ?
N7 C23 C28 C27 -178.9(5) . . . . ?
C24 C23 C28 N8 179.8(4) . . . . ?
N7 C23 C28 N8 1.0(5) . . . . ?
N2 C7 N1 C1 -0.2(5) . . . . ?
C8 C7 N1 C1 -179.4(4) . . . . ?
N2 C7 N1 Cd1 172.5(3) . . . . ?
C8 C7 N1 Cd1 -6.7(5) . . . . ?
C2 C1 N1 C7 -179.2(5) . . . . ?
C6 C1 N1 C7 0.6(5) . . . . ?
C2 C1 N1 Cd1 11.4(9) . . . . ?
C6 C1 N1 Cd1 -168.8(4) . . . . ?
O1 Cd1 N1 C7 109.2(3) . . . . ?
N4 Cd1 N1 C7 10.1(3) . . . . ?
N8 Cd1 N1 C7 -155.7(3) . . . . ?
N5 Cd1 N1 C7 -80.2(3) . . . . ?
O4 Cd1 N1 C7 60.0(5) . . . . ?
O1 Cd1 N1 C1 -81.8(5) . . . . ?
N4 Cd1 N1 C1 179.1(5) . . . . ?
N8 Cd1 N1 C1 13.3(5) . . . . ?
N5 Cd1 N1 C1 88.7(5) . . . . ?
O4 Cd1 N1 C1 -131.0(5) . . . . ?
N1 C7 N2 C6 -0.2(5) . . . . ?
C8 C7 N2 C6 178.9(4) . . . . ?
C5 C6 N2 C7 -179.5(5) . . . . ?
C1 C6 N2 C7 0.5(5) . . . . ?
N4 C8 N3 C14 0.7(5) . . . . ?
C7 C8 N3 C14 -177.7(4) . . . . ?
C13 C14 N3 C8 177.6(6) . . . . ?
C9 C14 N3 C8 -0.1(5) . . . . ?
N3 C8 N4 C9 -0.9(5) . . . . ?
C7 C8 N4 C9 177.6(4) . . . . ?
N3 C8 N4 Cd1 -164.2(3) . . . . ?
C7 C8 N4 Cd1 14.4(5) . . . . ?
C14 C9 N4 C8 0.8(5) . . . . ?
C10 C9 N4 C8 -179.6(5) . . . . ?
C14 C9 N4 Cd1 156.7(4) . . . . ?
C10 C9 N4 Cd1 -23.7(8) . . . . ?
O1 Cd1 N4 C8 -118.1(3) . . . . ?
N8 Cd1 N4 C8 60.7(7) . . . . ?
N1 Cd1 N4 C8 -12.7(3) . . . . ?
N5 Cd1 N4 C8 89.7(3) . . . . ?
O4 Cd1 N4 C8 -176.0(3) . . . . ?
O1 Cd1 N4 C9 87.0(5) . . . . ?
N8 Cd1 N4 C9 -94.1(7) . . . . ?
N1 Cd1 N4 C9 -167.5(5) . . . . ?
N5 Cd1 N4 C9 -65.2(5) . . . . ?
O4 Cd1 N4 C9 29.2(5) . . . . ?
N6 C21 N5 C15 2.1(5) . . . . ?
C22 C21 N5 C15 -176.1(4) . . . . ?
N6 C21 N5 Cd1 178.6(3) . . . . ?
C22 C21 N5 Cd1 0.4(5) . . . . ?
C16 C15 N5 C21 177.6(5) . . . . ?
C20 C15 N5 C21 -1.8(5) . . . . ?
C16 C15 N5 Cd1 2.8(8) . . . . ?
C20 C15 N5 Cd1 -176.6(3) . . . . ?
O1 Cd1 N5 C21 63.3(4) . . . . ?
N4 Cd1 N5 C21 -174.1(3) . . . . ?
N8 Cd1 N5 C21 -1.4(3) . . . . ?
N1 Cd1 N5 C21 -100.0(3) . . . . ?
O4 Cd1 N5 C21 94.0(3) . . . . ?
O1 Cd1 N5 C15 -122.1(5) . . . . ?
N4 Cd1 N5 C15 0.5(5) . . . . ?
N8 Cd1 N5 C15 173.2(5) . . . . ?
N1 Cd1 N5 C15 74.6(5) . . . . ?
O4 Cd1 N5 C15 -91.5(5) . . . . ?
N5 C21 N6 C20 -1.5(5) . . . . ?
C22 C21 N6 C20 176.5(4) . . . . ?
C19 C20 N6 C21 -177.1(5) . . . . ?
C15 C20 N6 C21 0.3(5) . . . . ?
N8 C22 N7 C23 -0.2(5) . . . . ?
C21 C22 N7 C23 -177.8(4) . . . . ?
C24 C23 N7 C22 -179.1(5) . . . . ?
C28 C23 N7 C22 -0.5(5) . . . . ?
N7 C22 N8 C28 0.9(5) . . . . ?
C21 C22 N8 C28 178.6(4) . . . . ?
N7 C22 N8 Cd1 179.3(3) . . . . ?
C21 C22 N8 Cd1 -2.9(5) . . . . ?
C27 C28 N8 C22 178.7(5) . . . . ?
C23 C28 N8 C22 -1.2(5) . . . . ?
C27 C28 N8 Cd1 0.9(9) . . . . ?
C23 C28 N8 Cd1 -179.0(3) . . . . ?
O1 Cd1 N8 C22 -148.7(3) . . . . ?
N4 Cd1 N8 C22 32.4(7) . . . . ?
N1 Cd1 N8 C22 102.4(3) . . . . ?
N5 Cd1 N8 C22 2.2(3) . . . . ?
O4 Cd1 N8 C22 -90.4(3) . . . . ?
O1 Cd1 N8 C28 29.0(5) . . . . ?
N4 Cd1 N8 C28 -149.9(5) . . . . ?
N1 Cd1 N8 C28 -79.9(5) . . . . ?
N5 Cd1 N8 C28 179.9(5) . . . . ?
O4 Cd1 N8 C28 87.3(5) . . . . ?
N4 Cd1 O1 S1 -85.1(2) . . . . ?
N8 Cd1 O1 S1 95.2(2) . . . . ?
N1 Cd1 O1 S1 -162.04(19) . . . . ?
N5 Cd1 O1 S1 35.2(4) . . . . ?
O4 Cd1 O1 S1 -1.53(17) . . . . ?
O1 Cd1 O4 S1 1.49(16) . . . . ?
N4 Cd1 O4 S1 106.28(18) . . . . ?
N8 Cd1 O4 S1 -85.90(18) . . . . ?
N1 Cd1 O4 S1 59.0(4) . . . . ?
N5 Cd1 O4 S1 -159.69(17) . . . . ?
Cd1 O1 S1 O3 -117.4(2) . . . . ?
Cd1 O1 S1 O2 120.9(2) . . . . ?
Cd1 O1 S1 O4 2.3(3) . . . . ?
Cd1 O4 S1 O3 118.67(19) . . . . ?
Cd1 O4 S1 O2 -119.18(19) . . . . ?
Cd1 O4 S1 O1 -2.0(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O2 0.86 1.96 2.749(5) 151.9 2_776
N3 H3A O2 0.86 2.15 2.820(5) 134.5 1_655
N6 H6 O3 0.86 1.88 2.726(5) 166.6 2_677
N7 H7 O4 0.86 1.94 2.746(5) 156.6 2_677

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.100

data_3
_database_code_depnum_ccdc_archive 'CCDC 675377'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H48 Cl2 Co2 N20'
_chemical_formula_sum            'C70 H48 Cl2 Co2 N20'
_chemical_formula_weight         1358.04

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'
Cl Cl 0.1484 0.1585 '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           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                   12.899(3)
_cell_length_b                   19.526(4)
_cell_length_c                   25.889(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.64(3)
_cell_angle_gamma                90.00
_cell_volume                     6499(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18946
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_sigmaI/netI    0.1127
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5735
_reflns_number_gt                2471
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1174P)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       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5735
_refine_ls_number_parameters     425
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1804
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.2330
_refine_ls_wR_factor_gt          0.1614
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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
N3 N 0.6309(4) 0.1732(3) 0.22820(18) 0.0552(14) Uani 1 1 d . . .
Co1 Co 0.43754(6) 0.16005(4) 0.34878(3) 0.0528(3) Uani 1 1 d . . .
Cl1 Cl 0.14355(14) 0.38456(9) 0.46498(7) 0.0719(6) Uani 1 1 d . . .
C1 C 0.5538(4) 0.1726(3) 0.2604(2) 0.0491(15) Uani 1 1 d . . .
C2 C 0.6868(5) 0.1661(3) 0.3137(2) 0.0517(16) Uani 1 1 d . . .
C3 C 0.7598(5) 0.1606(3) 0.3560(3) 0.0647(18) Uani 1 1 d . . .
H3 H 0.7392 0.1594 0.3896 0.078 Uiso 1 1 calc R . .
C4 C 0.8617(6) 0.1571(4) 0.3472(3) 0.076(2) Uani 1 1 d . . .
H4 H 0.9112 0.1521 0.3751 0.092 Uiso 1 1 calc R . .
C5 C 0.7185(4) 0.1687(3) 0.2627(2) 0.0490(15) Uani 1 1 d . . .
C6 C 0.8223(5) 0.1661(4) 0.2538(3) 0.072(2) Uani 1 1 d . . .
H6 H 0.8436 0.1678 0.2204 0.087 Uiso 1 1 calc R . .
C7 C 0.8944(5) 0.1610(4) 0.2969(3) 0.080(2) Uani 1 1 d . . .
H7 H 0.9651 0.1600 0.2922 0.096 Uiso 1 1 calc R . .
C8 C 0.2777(5) 0.2298(3) 0.4041(2) 0.0541(17) Uani 1 1 d . . .
C9 C 0.3421(5) 0.2845(3) 0.3871(2) 0.0560(16) Uani 1 1 d . . .
C10 C 0.4662(5) 0.3326(3) 0.3495(2) 0.0594(18) Uani 1 1 d . . .
C11 C 0.4046(5) 0.3857(4) 0.3670(3) 0.0651(18) Uani 1 1 d . . .
C12 C 0.5531(6) 0.3471(4) 0.3227(3) 0.078(2) Uani 1 1 d . . .
H12 H 0.5964 0.3130 0.3117 0.094 Uiso 1 1 calc R . .
C13 C 0.5702(7) 0.4154(5) 0.3137(3) 0.101(3) Uani 1 1 d . . .
H13 H 0.6280 0.4275 0.2964 0.122 Uiso 1 1 calc R . .
C14 C 0.5056(7) 0.4676(5) 0.3290(3) 0.099(3) Uani 1 1 d . . .
H14 H 0.5196 0.5127 0.3204 0.119 Uiso 1 1 calc R . .
C15 C 0.4216(6) 0.4533(4) 0.3565(3) 0.085(2) Uani 1 1 d . . .
H15 H 0.3786 0.4877 0.3674 0.102 Uiso 1 1 calc R . .
C16 C 0.2239(5) 0.1273(3) 0.4120(2) 0.0545(16) Uani 1 1 d . . .
C17 C 0.1611(5) 0.1683(3) 0.4402(2) 0.0542(16) Uani 1 1 d . . .
C18 C 0.0830(5) 0.1436(4) 0.4688(3) 0.076(2) Uani 1 1 d . . .
H18 H 0.0430 0.1720 0.4881 0.091 Uiso 1 1 calc R . .
C19 C 0.0687(6) 0.0737(4) 0.4665(3) 0.092(3) Uani 1 1 d . . .
H19 H 0.0165 0.0544 0.4846 0.111 Uiso 1 1 calc R . .
C20 C 0.1302(6) 0.0302(4) 0.4379(3) 0.086(2) Uani 1 1 d . . .
H20 H 0.1184 -0.0168 0.4378 0.103 Uiso 1 1 calc R . .
C21 C 0.2071(5) 0.0570(3) 0.4103(3) 0.0667(19) Uani 1 1 d . . .
H21 H 0.2471 0.0287 0.3909 0.080 Uiso 1 1 calc R . .
C22 C 0.5374(5) 0.0627(3) 0.4234(2) 0.0549(16) Uani 1 1 d . . .
C23 C 0.4908(5) 0.0195(3) 0.3816(2) 0.0560(16) Uani 1 1 d . . .
C24 C 0.4364(5) -0.0681(4) 0.3338(3) 0.0640(18) Uani 1 1 d . . .
C25 C 0.4031(5) -0.0053(4) 0.3103(2) 0.0574(17) Uani 1 1 d . . .
C26 C 0.3446(5) -0.0060(4) 0.2631(3) 0.072(2) Uani 1 1 d . . .
H26 H 0.3227 0.0346 0.2470 0.086 Uiso 1 1 calc R . .
C27 C 0.3199(6) -0.0681(5) 0.2407(3) 0.090(2) Uani 1 1 d . . .
H27 H 0.2810 -0.0693 0.2089 0.107 Uiso 1 1 calc R . .
C28 C 0.3518(7) -0.1296(5) 0.2646(3) 0.094(3) Uani 1 1 d . . .
H28 H 0.3328 -0.1707 0.2485 0.113 Uiso 1 1 calc R . .
C29 C 0.4106(6) -0.1309(4) 0.3115(3) 0.082(2) Uani 1 1 d . . .
H29 H 0.4319 -0.1719 0.3273 0.099 Uiso 1 1 calc R . .
C30 C 0.6202(5) 0.1034(3) 0.4941(3) 0.0581(17) Uani 1 1 d . . .
C31 C 0.6765(5) 0.1157(4) 0.5412(3) 0.0688(19) Uani 1 1 d . . .
H31 H 0.7075 0.0804 0.5610 0.083 Uiso 1 1 calc R . .
C32 C 0.6840(6) 0.1825(4) 0.5572(3) 0.072(2) Uani 1 1 d . . .
H32 H 0.7194 0.1925 0.5890 0.087 Uiso 1 1 calc R . .
C33 C 0.6404(6) 0.2358(4) 0.5274(3) 0.074(2) Uani 1 1 d . . .
H33 H 0.6476 0.2805 0.5396 0.089 Uiso 1 1 calc R . .
C34 C 0.5867(5) 0.2239(3) 0.4799(3) 0.0640(19) Uani 1 1 d . . .
H34 H 0.5592 0.2597 0.4594 0.077 Uiso 1 1 calc R . .
C35 C 0.5756(5) 0.1563(3) 0.4641(2) 0.0513(15) Uani 1 1 d . . .
N1 N 0.5794(4) 0.1687(3) 0.31097(17) 0.0517(13) Uani 1 1 d . . .
N2 N 0.2968(4) 0.1666(3) 0.38948(17) 0.0499(13) Uani 1 1 d . . .
N4 N 0.5957(4) 0.0437(3) 0.46668(19) 0.0587(14) Uani 1 1 d . . .
H4A H 0.6140 0.0028 0.4755 0.070 Uiso 1 1 calc R . .
N5 N 0.4377(4) 0.0486(3) 0.34250(19) 0.0545(13) Uani 1 1 d . . .
N6 N 0.4261(4) 0.2693(3) 0.36324(19) 0.0556(14) Uani 1 1 d . . .
N7 N 0.5242(4) 0.1296(3) 0.41957(18) 0.0535(13) Uani 1 1 d . . .
N8 N 0.1980(4) 0.2347(3) 0.43500(19) 0.0612(15) Uani 1 1 d . . .
H8 H 0.1749 0.2713 0.4486 0.073 Uiso 1 1 calc R . .
N9 N 0.3252(4) 0.3527(3) 0.3915(2) 0.0636(15) Uani 1 1 d . . .
H9 H 0.2756 0.3720 0.4064 0.076 Uiso 1 1 calc R . .
N10 N 0.4926(4) -0.0498(3) 0.3792(2) 0.0664(15) Uani 1 1 d . . .
H10 H 0.5229 -0.0771 0.4017 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
N3 C1 1.348(7) . ?
N3 C5 1.385(7) . ?
N3 Co1 2.129(5) 2_655 ?
Co1 N3 2.129(5) 2_655 ?
Co1 N1 2.150(5) . ?
Co1 N7 2.151(5) . ?
Co1 N6 2.174(5) . ?
Co1 N2 2.175(4) . ?
Co1 N5 2.183(5) . ?
C1 N1 1.327(7) . ?
C1 C1 1.447(11) 2_655 ?
C2 N1 1.383(7) . ?
C2 C3 1.390(8) . ?
C2 C5 1.412(7) . ?
C3 C4 1.354(9) . ?
C3 H3 0.9300 . ?
C4 C7 1.401(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(8) . ?
C6 C7 1.397(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N2 1.321(7) . ?
C8 N8 1.357(7) . ?
C8 C9 1.442(8) . ?
C9 N6 1.324(7) . ?
C9 N9 1.357(7) . ?
C10 N6 1.395(7) . ?
C10 C12 1.395(9) . ?
C10 C11 1.404(9) . ?
C11 C15 1.370(9) . ?
C11 N9 1.405(8) . ?
C12 C13 1.375(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.372(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 N2 1.379(7) . ?
C16 C17 1.388(8) . ?
C16 C21 1.390(9) . ?
C17 C18 1.385(8) . ?
C17 N8 1.390(8) . ?
C18 C19 1.377(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.411(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.372(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 N7 1.322(7) . ?
C22 N4 1.349(7) . ?
C22 C23 1.462(8) . ?
C23 N5 1.306(7) . ?
C23 N10 1.355(8) . ?
C24 N10 1.376(8) . ?
C24 C29 1.385(9) . ?
C24 C25 1.419(9) . ?
C25 C26 1.383(9) . ?
C25 N5 1.393(8) . ?
C26 C27 1.370(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.398(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.377(11) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 N4 1.387(8) . ?
C30 C35 1.389(8) . ?
C30 C31 1.390(9) . ?
C31 C32 1.369(9) . ?
C31 H31 0.9300 . ?
C32 C33 1.388(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.380(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.387(8) . ?
C34 H34 0.9300 . ?
C35 N7 1.383(7) . ?
N4 H4A 0.8600 . ?
N8 H8 0.8600 . ?
N9 H9 0.8600 . ?
N10 H10 0.8600 . ?

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
C1 N3 C5 101.8(5) . . ?
C1 N3 Co1 107.8(4) . 2_655 ?
C5 N3 Co1 148.4(4) . 2_655 ?
N3 Co1 N1 82.42(18) 2_655 . ?
N3 Co1 N7 168.00(19) 2_655 . ?
N1 Co1 N7 90.39(18) . . ?
N3 Co1 N6 90.8(2) 2_655 . ?
N1 Co1 N6 94.21(19) . . ?
N7 Co1 N6 99.3(2) . . ?
N3 Co1 N2 98.47(18) 2_655 . ?
N1 Co1 N2 171.94(19) . . ?
N7 Co1 N2 90.00(18) . . ?
N6 Co1 N2 77.79(18) . . ?
N3 Co1 N5 93.0(2) 2_655 . ?
N1 Co1 N5 92.20(18) . . ?
N7 Co1 N5 77.6(2) . . ?
N6 Co1 N5 172.90(18) . . ?
N2 Co1 N5 95.74(18) . . ?
N1 C1 N3 118.2(5) . . ?
N1 C1 C1 121.3(6) . 2_655 ?
N3 C1 C1 120.3(7) . 2_655 ?
N1 C2 C3 130.9(5) . . ?
N1 C2 C5 108.4(5) . . ?
C3 C2 C5 120.7(6) . . ?
C4 C3 C2 118.4(6) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C7 121.5(7) . . ?
C3 C4 H4 119.2 . . ?
C7 C4 H4 119.2 . . ?
C6 C5 N3 130.3(5) . . ?
C6 C5 C2 120.8(6) . . ?
N3 C5 C2 108.8(5) . . ?
C5 C6 C7 117.6(6) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
C6 C7 C4 120.9(6) . . ?
C6 C7 H7 119.5 . . ?
C4 C7 H7 119.5 . . ?
N2 C8 N8 113.7(5) . . ?
N2 C8 C9 118.7(5) . . ?
N8 C8 C9 127.6(6) . . ?
N6 C9 N9 113.7(5) . . ?
N6 C9 C8 119.4(6) . . ?
N9 C9 C8 127.0(6) . . ?
N6 C10 C12 129.5(6) . . ?
N6 C10 C11 110.0(6) . . ?
C12 C10 C11 120.5(6) . . ?
C15 C11 C10 123.0(7) . . ?
C15 C11 N9 131.8(7) . . ?
C10 C11 N9 105.0(6) . . ?
C13 C12 C10 115.4(7) . . ?
C13 C12 H12 122.3 . . ?
C10 C12 H12 122.3 . . ?
C12 C13 C14 123.5(8) . . ?
C12 C13 H13 118.2 . . ?
C14 C13 H13 118.2 . . ?
C15 C14 C13 121.0(8) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C11 C15 C14 116.4(8) . . ?
C11 C15 H15 121.8 . . ?
C14 C15 H15 121.8 . . ?
N2 C16 C17 110.4(6) . . ?
N2 C16 C21 130.2(6) . . ?
C17 C16 C21 119.4(6) . . ?
C18 C17 C16 124.1(6) . . ?
C18 C17 N8 130.3(6) . . ?
C16 C17 N8 105.5(5) . . ?
C19 C18 C17 115.0(6) . . ?
C19 C18 H18 122.5 . . ?
C17 C18 H18 122.5 . . ?
C18 C19 C20 122.7(7) . . ?
C18 C19 H19 118.6 . . ?
C20 C19 H19 118.6 . . ?
C21 C20 C19 120.3(7) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C16 118.5(6) . . ?
C20 C21 H21 120.8 . . ?
C16 C21 H21 120.8 . . ?
N7 C22 N4 113.2(6) . . ?
N7 C22 C23 118.2(6) . . ?
N4 C22 C23 128.7(6) . . ?
N5 C23 N10 114.1(6) . . ?
N5 C23 C22 118.8(6) . . ?
N10 C23 C22 127.0(6) . . ?
N10 C24 C29 132.7(7) . . ?
N10 C24 C25 105.2(6) . . ?
C29 C24 C25 122.0(7) . . ?
C26 C25 N5 131.3(7) . . ?
C26 C25 C24 119.7(7) . . ?
N5 C25 C24 109.0(6) . . ?
C27 C26 C25 118.3(8) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 121.5(8) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 121.8(8) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C24 116.7(8) . . ?
C28 C29 H29 121.7 . . ?
C24 C29 H29 121.7 . . ?
N4 C30 C35 105.7(6) . . ?
N4 C30 C31 132.6(6) . . ?
C35 C30 C31 121.7(6) . . ?
C32 C31 C30 116.7(7) . . ?
C32 C31 H31 121.6 . . ?
C30 C31 H31 121.6 . . ?
C31 C32 C33 122.0(7) . . ?
C31 C32 H32 119.0 . . ?
C33 C32 H32 119.0 . . ?
C34 C33 C32 121.4(7) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C35 117.1(6) . . ?
C33 C34 H34 121.5 . . ?
C35 C34 H34 121.5 . . ?
N7 C35 C34 129.4(6) . . ?
N7 C35 C30 109.6(6) . . ?
C34 C35 C30 121.0(6) . . ?
C1 N1 C2 102.7(5) . . ?
C1 N1 Co1 107.5(4) . . ?
C2 N1 Co1 149.3(4) . . ?
C8 N2 C16 104.4(5) . . ?
C8 N2 Co1 112.1(4) . . ?
C16 N2 Co1 142.8(4) . . ?
C22 N4 C30 106.5(5) . . ?
C22 N4 H4A 126.8 . . ?
C30 N4 H4A 126.8 . . ?
C23 N5 C25 104.9(5) . . ?
C23 N5 Co1 112.3(4) . . ?
C25 N5 Co1 142.8(5) . . ?
C9 N6 C10 104.8(5) . . ?
C9 N6 Co1 111.6(4) . . ?
C10 N6 Co1 142.5(4) . . ?
C22 N7 C35 105.0(5) . . ?
C22 N7 Co1 113.1(4) . . ?
C35 N7 Co1 141.9(4) . . ?
C8 N8 C17 105.9(5) . . ?
C8 N8 H8 127.0 . . ?
C17 N8 H8 127.0 . . ?
C9 N9 C11 106.5(5) . . ?
C9 N9 H9 126.7 . . ?
C11 N9 H9 126.7 . . ?
C23 N10 C24 106.7(6) . . ?
C23 N10 H10 126.6 . . ?
C24 N10 H10 126.6 . . ?

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
C5 N3 C1 N1 0.3(7) . . . . ?
Co1 N3 C1 N1 169.1(4) 2_655 . . . ?
C5 N3 C1 C1 -176.5(3) . . . 2_655 ?
Co1 N3 C1 C1 -7.7(4) 2_655 . . 2_655 ?
N1 C2 C3 C4 178.1(7) . . . . ?
C5 C2 C3 C4 -0.8(10) . . . . ?
C2 C3 C4 C7 2.0(11) . . . . ?
C1 N3 C5 C6 179.0(7) . . . . ?
Co1 N3 C5 C6 19.7(13) 2_655 . . . ?
C1 N3 C5 C2 -0.3(6) . . . . ?
Co1 N3 C5 C2 -159.6(6) 2_655 . . . ?
N1 C2 C5 C6 -179.2(6) . . . . ?
C3 C2 C5 C6 -0.1(10) . . . . ?
N1 C2 C5 N3 0.2(7) . . . . ?
C3 C2 C5 N3 179.2(6) . . . . ?
N3 C5 C6 C7 -179.3(7) . . . . ?
C2 C5 C6 C7 -0.1(10) . . . . ?
C5 C6 C7 C4 1.3(11) . . . . ?
C3 C4 C7 C6 -2.3(12) . . . . ?
N2 C8 C9 N6 -8.6(9) . . . . ?
N8 C8 C9 N6 170.1(6) . . . . ?
N2 C8 C9 N9 169.5(6) . . . . ?
N8 C8 C9 N9 -11.9(11) . . . . ?
N6 C10 C11 C15 -176.1(7) . . . . ?
C12 C10 C11 C15 3.9(11) . . . . ?
N6 C10 C11 N9 -0.4(8) . . . . ?
C12 C10 C11 N9 179.6(6) . . . . ?
N6 C10 C12 C13 177.9(7) . . . . ?
C11 C10 C12 C13 -2.1(11) . . . . ?
C10 C12 C13 C14 -1.1(13) . . . . ?
C12 C13 C14 C15 2.8(15) . . . . ?
C10 C11 C15 C14 -2.2(12) . . . . ?
N9 C11 C15 C14 -176.5(8) . . . . ?
C13 C14 C15 C11 -1.0(13) . . . . ?
N2 C16 C17 C18 -177.6(6) . . . . ?
C21 C16 C17 C18 1.9(11) . . . . ?
N2 C16 C17 N8 -0.5(7) . . . . ?
C21 C16 C17 N8 179.1(6) . . . . ?
C16 C17 C18 C19 -1.5(11) . . . . ?
N8 C17 C18 C19 -178.0(7) . . . . ?
C17 C18 C19 C20 0.9(13) . . . . ?
C18 C19 C20 C21 -0.8(13) . . . . ?
C19 C20 C21 C16 1.0(12) . . . . ?
N2 C16 C21 C20 177.9(7) . . . . ?
C17 C16 C21 C20 -1.6(10) . . . . ?
N7 C22 C23 N5 -0.4(8) . . . . ?
N4 C22 C23 N5 -179.2(6) . . . . ?
N7 C22 C23 N10 -177.6(5) . . . . ?
N4 C22 C23 N10 3.6(10) . . . . ?
N10 C24 C25 C26 179.5(6) . . . . ?
C29 C24 C25 C26 -1.2(10) . . . . ?
N10 C24 C25 N5 -1.4(7) . . . . ?
C29 C24 C25 N5 177.9(6) . . . . ?
N5 C25 C26 C27 -178.3(6) . . . . ?
C24 C25 C26 C27 0.5(10) . . . . ?
C25 C26 C27 C28 0.4(11) . . . . ?
C26 C27 C28 C29 -0.8(13) . . . . ?
C27 C28 C29 C24 0.2(12) . . . . ?
N10 C24 C29 C28 179.9(7) . . . . ?
C25 C24 C29 C28 0.8(11) . . . . ?
N4 C30 C31 C32 -179.1(6) . . . . ?
C35 C30 C31 C32 1.3(10) . . . . ?
C30 C31 C32 C33 -1.8(10) . . . . ?
C31 C32 C33 C34 0.2(11) . . . . ?
C32 C33 C34 C35 1.9(10) . . . . ?
C33 C34 C35 N7 178.4(6) . . . . ?
C33 C34 C35 C30 -2.4(9) . . . . ?
N4 C30 C35 N7 0.5(7) . . . . ?
C31 C30 C35 N7 -179.8(6) . . . . ?
N4 C30 C35 C34 -178.9(5) . . . . ?
C31 C30 C35 C34 0.8(9) . . . . ?
N3 C1 N1 C2 -0.2(7) . . . . ?
C1 C1 N1 C2 176.6(3) 2_655 . . . ?
N3 C1 N1 Co1 -175.1(4) . . . . ?
C1 C1 N1 Co1 1.7(4) 2_655 . . . ?
C3 C2 N1 C1 -178.9(7) . . . . ?
C5 C2 N1 C1 0.0(7) . . . . ?
C3 C2 N1 Co1 -8.5(13) . . . . ?
C5 C2 N1 Co1 170.5(6) . . . . ?
N3 Co1 N1 C1 -4.4(4) 2_655 . . . ?
N7 Co1 N1 C1 166.0(4) . . . . ?
N6 Co1 N1 C1 -94.6(4) . . . . ?
N2 Co1 N1 C1 -101.3(13) . . . . ?
N5 Co1 N1 C1 88.4(4) . . . . ?
N3 Co1 N1 C2 -174.6(8) 2_655 . . . ?
N7 Co1 N1 C2 -4.2(8) . . . . ?
N6 Co1 N1 C2 95.2(8) . . . . ?
N2 Co1 N1 C2 88.5(16) . . . . ?
N5 Co1 N1 C2 -81.8(8) . . . . ?
N8 C8 N2 C16 0.7(7) . . . . ?
C9 C8 N2 C16 179.5(6) . . . . ?
N8 C8 N2 Co1 -172.4(4) . . . . ?
C9 C8 N2 Co1 6.5(7) . . . . ?
C17 C16 N2 C8 -0.1(7) . . . . ?
C21 C16 N2 C8 -179.6(7) . . . . ?
C17 C16 N2 Co1 169.2(5) . . . . ?
C21 C16 N2 Co1 -10.3(12) . . . . ?
N3 Co1 N2 C8 -91.7(4) 2_655 . . . ?
N1 Co1 N2 C8 4.1(15) . . . . ?
N7 Co1 N2 C8 96.9(4) . . . . ?
N6 Co1 N2 C8 -2.7(4) . . . . ?
N5 Co1 N2 C8 174.4(4) . . . . ?
N3 Co1 N2 C16 99.6(7) 2_655 . . . ?
N1 Co1 N2 C16 -164.7(11) . . . . ?
N7 Co1 N2 C16 -71.9(7) . . . . ?
N6 Co1 N2 C16 -171.4(7) . . . . ?
N5 Co1 N2 C16 5.6(7) . . . . ?
N7 C22 N4 C30 1.7(7) . . . . ?
C23 C22 N4 C30 -179.4(6) . . . . ?
C35 C30 N4 C22 -1.3(6) . . . . ?
C31 C30 N4 C22 179.1(7) . . . . ?
N10 C23 N5 C25 -1.7(7) . . . . ?
C22 C23 N5 C25 -179.3(5) . . . . ?
N10 C23 N5 Co1 179.8(4) . . . . ?
C22 C23 N5 Co1 2.3(7) . . . . ?
C26 C25 N5 C23 -179.1(7) . . . . ?
C24 C25 N5 C23 1.9(6) . . . . ?
C26 C25 N5 Co1 -1.6(11) . . . . ?
C24 C25 N5 Co1 179.5(5) . . . . ?
N3 Co1 N5 C23 170.0(4) 2_655 . . . ?
N1 Co1 N5 C23 87.5(4) . . . . ?
N7 Co1 N5 C23 -2.4(4) . . . . ?
N6 Co1 N5 C23 -67.1(18) . . . . ?
N2 Co1 N5 C23 -91.1(4) . . . . ?
N3 Co1 N5 C25 -7.4(6) 2_655 . . . ?
N1 Co1 N5 C25 -89.9(6) . . . . ?
N7 Co1 N5 C25 -179.8(6) . . . . ?
N6 Co1 N5 C25 115.5(16) . . . . ?
N2 Co1 N5 C25 91.4(6) . . . . ?
N9 C9 N6 C10 -1.8(7) . . . . ?
C8 C9 N6 C10 176.5(6) . . . . ?
N9 C9 N6 Co1 -172.7(4) . . . . ?
C8 C9 N6 Co1 5.6(7) . . . . ?
C12 C10 N6 C9 -178.7(7) . . . . ?
C11 C10 N6 C9 1.3(7) . . . . ?
C12 C10 N6 Co1 -12.6(12) . . . . ?
C11 C10 N6 Co1 167.4(5) . . . . ?
N3 Co1 N6 C9 96.9(4) 2_655 . . . ?
N1 Co1 N6 C9 179.3(4) . . . . ?
N7 Co1 N6 C9 -89.6(4) . . . . ?
N2 Co1 N6 C9 -1.6(4) . . . . ?
N5 Co1 N6 C9 -26.1(19) . . . . ?
N3 Co1 N6 C10 -68.6(7) 2_655 . . . ?
N1 Co1 N6 C10 13.9(7) . . . . ?
N7 Co1 N6 C10 104.9(7) . . . . ?
N2 Co1 N6 C10 -167.1(7) . . . . ?
N5 Co1 N6 C10 168.4(14) . . . . ?
N4 C22 N7 C35 -1.4(7) . . . . ?
C23 C22 N7 C35 179.6(5) . . . . ?
N4 C22 N7 Co1 177.2(4) . . . . ?
C23 C22 N7 Co1 -1.8(7) . . . . ?
C34 C35 N7 C22 179.8(6) . . . . ?
C30 C35 N7 C22 0.5(7) . . . . ?
C34 C35 N7 Co1 1.9(11) . . . . ?
C30 C35 N7 Co1 -177.4(4) . . . . ?
N3 Co1 N7 C22 -37.0(11) 2_655 . . . ?
N1 Co1 N7 C22 -90.0(4) . . . . ?
N6 Co1 N7 C22 175.7(4) . . . . ?
N2 Co1 N7 C22 98.1(4) . . . . ?
N5 Co1 N7 C22 2.2(4) . . . . ?
N3 Co1 N7 C35 140.8(8) 2_655 . . . ?
N1 Co1 N7 C35 87.8(6) . . . . ?
N6 Co1 N7 C35 -6.5(6) . . . . ?
N2 Co1 N7 C35 -84.1(6) . . . . ?
N5 Co1 N7 C35 180.0(6) . . . . ?
N2 C8 N8 C17 -1.0(7) . . . . ?
C9 C8 N8 C17 -179.7(6) . . . . ?
C18 C17 N8 C8 177.8(7) . . . . ?
C16 C17 N8 C8 0.8(7) . . . . ?
N6 C9 N9 C11 1.5(8) . . . . ?
C8 C9 N9 C11 -176.6(6) . . . . ?
C15 C11 N9 C9 174.5(8) . . . . ?
C10 C11 N9 C9 -0.6(7) . . . . ?
N5 C23 N10 C24 0.9(7) . . . . ?
C22 C23 N10 C24 178.2(6) . . . . ?
C29 C24 N10 C23 -178.8(7) . . . . ?
C25 C24 N10 C23 0.4(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A Cl1 0.86 2.36 3.170(5) 157.4 3_545
N8 H8 Cl1 0.86 2.29 3.123(6) 161.6 .
N9 H9 Cl1 0.86 2.38 3.196(5) 157.8 .
N10 H10 Cl1 0.86 2.29 3.108(6) 158.7 3_545

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.099

data_4
_database_code_depnum_ccdc_archive 'CCDC 675378'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Co N4 O4'
_chemical_formula_sum            'C12 H10 Co N4 O4'
_chemical_formula_weight         333.17

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'
Co Co 0.3494 0.9721 '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                   12.5026(11)
_cell_length_b                   11.8042(11)
_cell_length_c                   9.3038(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.637(2)
_cell_angle_gamma                90.00
_cell_volume                     1353.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      28.27

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8416
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         28.27
_reflns_number_total             3103
_reflns_number_gt                2384
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0383P)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    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3103
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1130
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
O3 O 0.67762(19) 1.2282(2) -0.2019(3) 0.0304(6) Uani 1 1 d . . .
O2 O 0.85743(19) 1.3391(2) -0.0753(3) 0.0278(6) Uani 1 1 d . . .
C11 C 0.8169(3) 1.2691(3) 0.0003(4) 0.0234(8) Uani 1 1 d . . .
C1 C 0.6655(3) 0.9513(3) 0.4301(4) 0.0301(9) Uani 1 1 d . . .
C2 C 0.7551(4) 0.9409(4) 0.5408(5) 0.0434(11) Uani 1 1 d . . .
C3 C 0.7494(4) 0.8625(4) 0.6485(5) 0.0581(14) Uani 1 1 d . . .
C4 C 0.6582(5) 0.7960(5) 0.6470(6) 0.0676(16) Uani 1 1 d . . .
C5 C 0.5699(4) 0.8046(4) 0.5398(6) 0.0562(14) Uani 1 1 d . . .
C6 C 0.5748(3) 0.8831(3) 0.4314(5) 0.0376(10) Uani 1 1 d . . .
C7 C 0.5511(3) 0.9921(4) 0.2392(5) 0.0367(10) Uani 1 1 d . . .
C8 C 0.8502(4) 0.9379(4) 0.0443(5) 0.0579(15) Uani 1 1 d . . .
C9 C 0.9280(4) 0.8579(4) 0.0555(6) 0.0626(16) Uani 1 1 d . . .
C10 C 0.9361(4) 0.9455(4) 0.2570(5) 0.0451(12) Uani 1 1 d . . .
C12 C 0.7123(3) 1.2060(3) -0.0702(4) 0.0248(8) Uani 1 1 d . . .
Co1 Co 0.75812(4) 1.12584(4) 0.22314(5) 0.02430(17) Uani 1 1 d . . .
H1 H 0.818(3) 0.983(4) 0.537(4) 0.054(13) Uiso 1 1 d . . .
H2 H 0.812(3) 0.847(3) 0.723(5) 0.056(14) Uiso 1 1 d . . .
H3 H 0.659(4) 0.743(4) 0.718(5) 0.071(16) Uiso 1 1 d . . .
H4 H 0.512(3) 0.763(3) 0.536(4) 0.047(13) Uiso 1 1 d . . .
H5 H 0.446(3) 0.879(3) 0.281(4) 0.039(12) Uiso 1 1 d . . .
H6 H 0.517(3) 1.029(3) 0.157(4) 0.027(10) Uiso 1 1 d . . .
H7 H 0.798(3) 0.949(4) -0.033(5) 0.062(15) Uiso 1 1 d . . .
H8 H 0.941(3) 0.804(4) -0.014(5) 0.070(16) Uiso 1 1 d . . .
H9 H 1.029(4) 0.825(4) 0.234(5) 0.068(17) Uiso 1 1 d . . .
H10 H 0.964(3) 0.967(3) 0.349(4) 0.042(12) Uiso 1 1 d . . .
N1 N 0.6483(2) 1.0203(3) 0.3057(3) 0.0304(7) Uani 1 1 d . . .
N2 N 0.5034(3) 0.9131(3) 0.3081(4) 0.0406(9) Uani 1 1 d . . .
N3 N 0.8555(2) 0.9939(3) 0.1730(3) 0.0327(7) Uani 1 1 d . . .
N4 N 0.9817(3) 0.8639(3) 0.1920(5) 0.0496(11) Uani 1 1 d . . .
O1 O 0.85372(19) 1.2430(2) 0.1296(3) 0.0316(6) Uani 1 1 d . . .
O4 O 0.67053(18) 1.1392(2) 0.0082(3) 0.0286(6) 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
O3 C12 1.257(4) . ?
O3 Co1 2.169(2) 4_585 ?
O2 C11 1.247(4) . ?
O2 Co1 2.110(2) 4_585 ?
C11 O1 1.253(4) . ?
C11 C12 1.552(5) . ?
C1 C6 1.393(5) . ?
C1 C2 1.394(5) . ?
C1 N1 1.402(4) . ?
C2 C3 1.374(6) . ?
C2 H1 0.93(4) . ?
C3 C4 1.384(7) . ?
C3 H2 0.97(4) . ?
C4 C5 1.361(7) . ?
C4 H3 0.91(5) . ?
C5 C6 1.379(6) . ?
C5 H4 0.87(4) . ?
C6 N2 1.377(5) . ?
C7 N1 1.311(4) . ?
C7 N2 1.328(5) . ?
C7 H6 0.92(3) . ?
C8 C9 1.347(6) . ?
C8 N3 1.360(5) . ?
C8 H7 0.90(4) . ?
C9 N4 1.335(6) . ?
C9 H8 0.94(4) . ?
C10 N3 1.300(5) . ?
C10 N4 1.317(5) . ?
C10 H10 0.91(4) . ?
C12 O4 1.247(4) . ?
Co1 N3 2.077(3) . ?
Co1 N1 2.093(3) . ?
Co1 O1 2.108(2) . ?
Co1 O2 2.110(2) 4_586 ?
Co1 O4 2.119(2) . ?
Co1 O3 2.169(2) 4_586 ?
N2 H5 0.83(4) . ?
N4 H9 0.80(5) . ?

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
C12 O3 Co1 112.1(2) . 4_585 ?
C11 O2 Co1 113.4(2) . 4_585 ?
O2 C11 O1 125.9(3) . . ?
O2 C11 C12 118.3(3) . . ?
O1 C11 C12 115.9(3) . . ?
C6 C1 C2 119.8(4) . . ?
C6 C1 N1 109.3(3) . . ?
C2 C1 N1 130.9(3) . . ?
C3 C2 C1 117.7(4) . . ?
C3 C2 H1 122(3) . . ?
C1 C2 H1 120(3) . . ?
C2 C3 C4 121.2(5) . . ?
C2 C3 H2 121(3) . . ?
C4 C3 H2 118(3) . . ?
C5 C4 C3 122.1(5) . . ?
C5 C4 H3 120(3) . . ?
C3 C4 H3 118(3) . . ?
C4 C5 C6 117.1(4) . . ?
C4 C5 H4 124(3) . . ?
C6 C5 H4 119(3) . . ?
N2 C6 C5 132.9(4) . . ?
N2 C6 C1 105.0(4) . . ?
C5 C6 C1 122.1(4) . . ?
N1 C7 N2 114.0(4) . . ?
N1 C7 H6 122(2) . . ?
N2 C7 H6 123(2) . . ?
C9 C8 N3 110.2(4) . . ?
C9 C8 H7 126(3) . . ?
N3 C8 H7 123(3) . . ?
N4 C9 C8 106.1(5) . . ?
N4 C9 H8 125(3) . . ?
C8 C9 H8 129(3) . . ?
N3 C10 N4 113.4(4) . . ?
N3 C10 H10 125(2) . . ?
N4 C10 H10 121(2) . . ?
O4 C12 O3 126.3(3) . . ?
O4 C12 C11 117.5(3) . . ?
O3 C12 C11 116.1(3) . . ?
N3 Co1 N1 94.65(12) . . ?
N3 Co1 O1 90.28(11) . . ?
N1 Co1 O1 173.65(11) . . ?
N3 Co1 O2 93.83(11) . 4_586 ?
N1 Co1 O2 96.61(11) . 4_586 ?
O1 Co1 O2 87.04(9) . 4_586 ?
N3 Co1 O4 94.21(11) . . ?
N1 Co1 O4 97.09(10) . . ?
O1 Co1 O4 78.52(9) . . ?
O2 Co1 O4 163.49(9) 4_586 . ?
N3 Co1 O3 171.42(11) . 4_586 ?
N1 Co1 O3 89.25(11) . 4_586 ?
O1 Co1 O3 86.40(10) . 4_586 ?
O2 Co1 O3 78.12(9) 4_586 4_586 ?
O4 Co1 O3 92.88(9) . 4_586 ?
C7 N1 C1 104.1(3) . . ?
C7 N1 Co1 126.2(3) . . ?
C1 N1 Co1 129.0(2) . . ?
C7 N2 C6 107.6(3) . . ?
C7 N2 H5 129(3) . . ?
C6 N2 H5 122(3) . . ?
C10 N3 C8 103.5(4) . . ?
C10 N3 Co1 128.3(3) . . ?
C8 N3 Co1 128.2(3) . . ?
C10 N4 C9 106.8(4) . . ?
C10 N4 H9 123(3) . . ?
C9 N4 H9 130(3) . . ?
C11 O1 Co1 114.5(2) . . ?
C12 O4 Co1 113.5(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
Co1 O2 C11 O1 -172.0(3) 4_585 . . . ?
Co1 O2 C11 C12 8.9(4) 4_585 . . . ?
C6 C1 C2 C3 -0.3(6) . . . . ?
N1 C1 C2 C3 -178.2(4) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
C4 C5 C6 N2 179.0(5) . . . . ?
C4 C5 C6 C1 0.0(7) . . . . ?
C2 C1 C6 N2 -179.1(4) . . . . ?
N1 C1 C6 N2 -0.7(4) . . . . ?
C2 C1 C6 C5 0.1(6) . . . . ?
N1 C1 C6 C5 178.5(4) . . . . ?
N3 C8 C9 N4 0.2(7) . . . . ?
Co1 O3 C12 O4 168.1(3) 4_585 . . . ?
Co1 O3 C12 C11 -11.6(4) 4_585 . . . ?
O2 C11 C12 O4 -177.5(3) . . . . ?
O1 C11 C12 O4 3.3(5) . . . . ?
O2 C11 C12 O3 2.2(5) . . . . ?
O1 C11 C12 O3 -177.0(3) . . . . ?
N2 C7 N1 C1 0.6(4) . . . . ?
N2 C7 N1 Co1 172.2(3) . . . . ?
C6 C1 N1 C7 0.1(4) . . . . ?
C2 C1 N1 C7 178.2(4) . . . . ?
C6 C1 N1 Co1 -171.1(2) . . . . ?
C2 C1 N1 Co1 7.0(6) . . . . ?
N3 Co1 N1 C7 -103.5(3) . . . . ?
O1 Co1 N1 C7 37.2(11) . . . . ?
O2 Co1 N1 C7 162.1(3) 4_586 . . . ?
O4 Co1 N1 C7 -8.7(3) . . . . ?
O3 Co1 N1 C7 84.1(3) 4_586 . . . ?
N3 Co1 N1 C1 65.9(3) . . . . ?
O1 Co1 N1 C1 -153.3(9) . . . . ?
O2 Co1 N1 C1 -28.5(3) 4_586 . . . ?
O4 Co1 N1 C1 160.8(3) . . . . ?
O3 Co1 N1 C1 -106.4(3) 4_586 . . . ?
N1 C7 N2 C6 -1.0(5) . . . . ?
C5 C6 N2 C7 -178.1(5) . . . . ?
C1 C6 N2 C7 1.0(4) . . . . ?
N4 C10 N3 C8 -0.1(6) . . . . ?
N4 C10 N3 Co1 -179.9(3) . . . . ?
C9 C8 N3 C10 0.0(6) . . . . ?
C9 C8 N3 Co1 179.8(3) . . . . ?
N1 Co1 N3 C10 -86.9(4) . . . . ?
O1 Co1 N3 C10 97.1(4) . . . . ?
O2 Co1 N3 C10 10.1(4) 4_586 . . . ?
O4 Co1 N3 C10 175.6(4) . . . . ?
O3 Co1 N3 C10 30.0(10) 4_586 . . . ?
N1 Co1 N3 C8 93.3(4) . . . . ?
O1 Co1 N3 C8 -82.7(4) . . . . ?
O2 Co1 N3 C8 -169.7(4) 4_586 . . . ?
O4 Co1 N3 C8 -4.2(4) . . . . ?
O3 Co1 N3 C8 -149.8(7) 4_586 . . . ?
N3 C10 N4 C9 0.2(6) . . . . ?
C8 C9 N4 C10 -0.2(6) . . . . ?
O2 C11 O1 Co1 177.5(3) . . . . ?
C12 C11 O1 Co1 -3.4(4) . . . . ?
N3 Co1 O1 C11 96.4(2) . . . . ?
N1 Co1 O1 C11 -44.5(11) . . . . ?
O2 Co1 O1 C11 -169.8(2) 4_586 . . . ?
O4 Co1 O1 C11 2.2(2) . . . . ?
O3 Co1 O1 C11 -91.5(2) 4_586 . . . ?
O3 C12 O4 Co1 179.0(3) . . . . ?
C11 C12 O4 Co1 -1.3(4) . . . . ?
N3 Co1 O4 C12 -89.7(2) . . . . ?
N1 Co1 O4 C12 175.1(2) . . . . ?
O1 Co1 O4 C12 -0.3(2) . . . . ?
O2 Co1 O4 C12 29.2(5) 4_586 . . . ?
O3 Co1 O4 C12 85.5(2) 4_586 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H5 O3 0.83(4) 2.03(4) 2.852(4) 169(4) 3_675
N4 H9 O1 0.80(5) 2.01(5) 2.807(4) 170(5) 2_745

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.088

data_5
_database_code_depnum_ccdc_archive 'CCDC 675379'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H14 N4 O4 Zn'
_chemical_formula_sum            'C22 H14 N4 O4 Zn'
_chemical_formula_weight         463.74

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)/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                   7.3340(14)
_cell_length_b                   21.958(4)
_cell_length_c                   11.623(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.677(4)
_cell_angle_gamma                90.00
_cell_volume                     1854.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11663
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         28.27
_reflns_number_total             4201
_reflns_number_gt                3460
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0516P)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    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4201
_refine_ls_number_parameters     336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_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
O1 O -0.5077(2) 0.15117(7) 0.42287(14) 0.0281(4) Uani 1 1 d . . .
O2 O -0.7342(2) 0.20936(8) 0.46427(16) 0.0353(4) Uani 1 1 d . . .
C22 C -0.5663(3) 0.19964(10) 0.46678(19) 0.0270(5) Uani 1 1 d . . .
C1 C 0.1703(3) 0.40751(12) 1.1651(2) 0.0286(5) Uani 1 1 d . . .
C2 C 0.1471(4) 0.35088(13) 1.2150(3) 0.0396(6) Uani 1 1 d . . .
C3 C 0.1151(4) 0.35026(16) 1.3288(3) 0.0477(7) Uani 1 1 d . . .
C4 C 0.1046(4) 0.40431(18) 1.3923(3) 0.0487(7) Uani 1 1 d . . .
C5 C 0.1276(4) 0.46030(15) 1.3442(2) 0.0406(6) Uani 1 1 d . . .
C6 C 0.1635(3) 0.46141(12) 1.2294(2) 0.0306(5) Uani 1 1 d . . .
C7 C 0.2229(3) 0.48275(10) 1.05350(19) 0.0249(5) Uani 1 1 d . . .
C8 C 0.2648(3) 0.51120(10) 0.9482(2) 0.0248(5) Uani 1 1 d . . .
C9 C 0.3148(3) 0.51509(11) 0.7698(2) 0.0269(5) Uani 1 1 d . . .
C10 C 0.3408(4) 0.50284(13) 0.6548(2) 0.0349(6) Uani 1 1 d . . .
C11 C 0.3804(4) 0.55183(14) 0.5884(2) 0.0397(6) Uani 1 1 d . . .
C12 C 0.3947(4) 0.61096(13) 0.6333(3) 0.0407(7) Uani 1 1 d . . .
C13 C 0.3707(4) 0.62375(12) 0.7461(3) 0.0393(6) Uani 1 1 d . . .
C14 C 0.3314(3) 0.57449(11) 0.8138(2) 0.0290(5) Uani 1 1 d . . .
C15 C -0.3500(3) 0.31898(11) 0.6737(2) 0.0304(5) Uani 1 1 d . . .
C16 C -0.4808(3) 0.28370(11) 0.6078(2) 0.0297(5) Uani 1 1 d . . .
C17 C -0.4279(3) 0.24299(10) 0.52687(19) 0.0253(5) Uani 1 1 d . . .
C18 C -0.2444(3) 0.24001(11) 0.5084(2) 0.0283(5) Uani 1 1 d . . .
C19 C -0.1152(3) 0.27677(11) 0.5718(2) 0.0287(5) Uani 1 1 d . . .
C20 C -0.1662(3) 0.31502(10) 0.6569(2) 0.0267(5) Uani 1 1 d . . .
C21 C -0.0205(3) 0.34838(11) 0.7361(2) 0.0287(5) Uani 1 1 d . . .
H1 H 0.143(4) 0.3118(16) 1.168(3) 0.060(10) Uiso 1 1 d . . .
H2 H 0.098(4) 0.3159(16) 1.361(3) 0.057(10) Uiso 1 1 d . . .
H3 H 0.078(4) 0.4018(15) 1.472(3) 0.059(9) Uiso 1 1 d . . .
H4 H 0.122(5) 0.4957(19) 1.386(3) 0.069(11) Uiso 1 1 d . . .
H5 H 0.173(4) 0.5457(16) 1.175(3) 0.052(9) Uiso 1 1 d . . .
H6 H 0.323(4) 0.5932(16) 0.982(3) 0.049(9) Uiso 1 1 d . . .
H7 H 0.380(4) 0.6651(16) 0.777(3) 0.055(9) Uiso 1 1 d . . .
H8 H 0.419(4) 0.6418(16) 0.590(3) 0.056(10) Uiso 1 1 d . . .
H9 H 0.395(4) 0.5467(14) 0.513(3) 0.040(8) Uiso 1 1 d . . .
H10 H 0.324(4) 0.4649(15) 0.624(3) 0.045(8) Uiso 1 1 d . . .
H11 H -0.384(4) 0.3433(13) 0.728(2) 0.040(8) Uiso 1 1 d . . .
H12 H -0.605(4) 0.2854(12) 0.623(2) 0.030(7) Uiso 1 1 d . . .
H13 H -0.207(3) 0.2143(12) 0.456(2) 0.029(7) Uiso 1 1 d . . .
H14 H 0.002(3) 0.2754(12) 0.557(2) 0.028(7) Uiso 1 1 d . . .
N1 N 0.2065(2) 0.42241(9) 1.05404(16) 0.0265(4) Uani 1 1 d . . .
N2 N 0.1985(3) 0.50819(10) 1.15598(17) 0.0296(4) Uani 1 1 d . . .
N3 N 0.2733(3) 0.47612(8) 0.85587(16) 0.0256(4) Uani 1 1 d . . .
N4 N 0.2970(3) 0.57028(9) 0.92803(18) 0.0291(4) Uani 1 1 d . . .
O3 O 0.1429(2) 0.34750(9) 0.71665(16) 0.0400(4) Uani 1 1 d . . .
O4 O -0.0649(2) 0.37420(8) 0.82602(16) 0.0342(4) Uani 1 1 d . . .
Zn1 Zn 0.22538(3) 0.384463(12) 0.88891(2) 0.02584(11) 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
O1 C22 1.279(3) . ?
O1 Zn1 2.0960(16) 4_465 ?
O2 C22 1.246(3) . ?
O2 Zn1 2.2427(18) 4_465 ?
C22 C17 1.495(3) . ?
C22 Zn1 2.489(2) 4_465 ?
C1 N1 1.391(3) . ?
C1 C2 1.392(4) . ?
C1 C6 1.405(4) . ?
C2 C3 1.374(4) . ?
C2 H1 1.01(3) . ?
C3 C4 1.405(5) . ?
C3 H2 0.86(4) . ?
C4 C5 1.370(5) . ?
C4 H3 0.97(3) . ?
C5 C6 1.394(4) . ?
C5 H4 0.92(4) . ?
C6 N2 1.381(3) . ?
C7 N1 1.330(3) . ?
C7 N2 1.349(3) . ?
C7 C8 1.443(3) . ?
C8 N3 1.329(3) . ?
C8 N4 1.345(3) . ?
C9 N3 1.381(3) . ?
C9 C10 1.400(3) . ?
C9 C14 1.401(3) . ?
C10 C11 1.377(4) . ?
C10 H10 0.91(3) . ?
C11 C12 1.398(4) . ?
C11 H9 0.90(3) . ?
C12 C13 1.375(4) . ?
C12 H8 0.88(4) . ?
C13 C14 1.391(4) . ?
C13 H7 0.97(3) . ?
C14 N4 1.387(3) . ?
C15 C16 1.383(3) . ?
C15 C20 1.390(3) . ?
C15 H11 0.89(3) . ?
C16 C17 1.389(3) . ?
C16 H12 0.95(3) . ?
C17 C18 1.392(3) . ?
C18 C19 1.380(3) . ?
C18 H13 0.90(3) . ?
C19 C20 1.386(3) . ?
C19 H14 0.90(3) . ?
C20 C21 1.505(3) . ?
C21 O3 1.249(3) . ?
C21 O4 1.269(3) . ?
C21 Zn1 2.486(2) . ?
N1 Zn1 2.1138(19) . ?
N2 H5 0.88(3) . ?
N3 Zn1 2.0875(19) . ?
N4 H6 0.80(4) . ?
O3 Zn1 2.1701(18) . ?
O4 Zn1 2.1683(18) . ?
Zn1 O1 2.0960(16) 4_666 ?
Zn1 O2 2.2427(18) 4_666 ?
Zn1 C22 2.489(2) 4_666 ?

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
C22 O1 Zn1 91.75(13) . 4_465 ?
C22 O2 Zn1 86.01(14) . 4_465 ?
O2 C22 O1 121.1(2) . . ?
O2 C22 C17 120.6(2) . . ?
O1 C22 C17 118.2(2) . . ?
O2 C22 Zn1 64.03(12) . 4_465 ?
O1 C22 Zn1 57.33(11) . 4_465 ?
C17 C22 Zn1 171.07(16) . 4_465 ?
N1 C1 C2 130.2(3) . . ?
N1 C1 C6 108.7(2) . . ?
C2 C1 C6 121.0(2) . . ?
C3 C2 C1 117.1(3) . . ?
C3 C2 H1 121(2) . . ?
C1 C2 H1 122(2) . . ?
C2 C3 C4 121.7(3) . . ?
C2 C3 H2 119(2) . . ?
C4 C3 H2 120(2) . . ?
C5 C4 C3 121.7(3) . . ?
C5 C4 H3 119(2) . . ?
C3 C4 H3 119(2) . . ?
C4 C5 C6 117.1(3) . . ?
C4 C5 H4 122(2) . . ?
C6 C5 H4 121(2) . . ?
N2 C6 C5 132.7(3) . . ?
N2 C6 C1 105.9(2) . . ?
C5 C6 C1 121.3(3) . . ?
N1 C7 N2 112.7(2) . . ?
N1 C7 C8 117.7(2) . . ?
N2 C7 C8 129.6(2) . . ?
N3 C8 N4 112.9(2) . . ?
N3 C8 C7 118.2(2) . . ?
N4 C8 C7 128.9(2) . . ?
N3 C9 C10 130.1(2) . . ?
N3 C9 C14 109.2(2) . . ?
C10 C9 C14 120.8(2) . . ?
C11 C10 C9 116.8(3) . . ?
C11 C10 H10 121.6(19) . . ?
C9 C10 H10 121.5(19) . . ?
C10 C11 C12 121.8(3) . . ?
C10 C11 H9 121(2) . . ?
C12 C11 H9 118(2) . . ?
C13 C12 C11 122.2(3) . . ?
C13 C12 H8 117(2) . . ?
C11 C12 H8 121(2) . . ?
C12 C13 C14 116.3(3) . . ?
C12 C13 H7 122(2) . . ?
C14 C13 H7 122(2) . . ?
N4 C14 C13 132.2(2) . . ?
N4 C14 C9 105.7(2) . . ?
C13 C14 C9 122.1(2) . . ?
C16 C15 C20 120.1(2) . . ?
C16 C15 H11 119.3(17) . . ?
C20 C15 H11 120.6(17) . . ?
C15 C16 C17 120.0(2) . . ?
C15 C16 H12 119.0(16) . . ?
C17 C16 H12 120.8(16) . . ?
C16 C17 C18 119.8(2) . . ?
C16 C17 C22 119.5(2) . . ?
C18 C17 C22 120.5(2) . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H13 118.8(16) . . ?
C17 C18 H13 121.3(16) . . ?
C18 C19 C20 120.2(2) . . ?
C18 C19 H14 119.0(16) . . ?
C20 C19 H14 120.8(16) . . ?
C19 C20 C15 119.8(2) . . ?
C19 C20 C21 119.6(2) . . ?
C15 C20 C21 120.4(2) . . ?
O3 C21 O4 120.9(2) . . ?
O3 C21 C20 120.1(2) . . ?
O4 C21 C20 118.8(2) . . ?
O3 C21 Zn1 60.80(12) . . ?
O4 C21 Zn1 60.70(12) . . ?
C20 C21 Zn1 168.72(16) . . ?
C7 N1 C1 105.50(19) . . ?
C7 N1 Zn1 111.80(15) . . ?
C1 N1 Zn1 142.51(17) . . ?
C7 N2 C6 107.2(2) . . ?
C7 N2 H5 132(2) . . ?
C6 N2 H5 119(2) . . ?
C8 N3 C9 105.35(19) . . ?
C8 N3 Zn1 112.51(15) . . ?
C9 N3 Zn1 142.13(16) . . ?
C8 N4 C14 106.9(2) . . ?
C8 N4 H6 120(2) . . ?
C14 N4 H6 130(2) . . ?
C21 O3 Zn1 89.05(15) . . ?
C21 O4 Zn1 88.61(14) . . ?
N3 Zn1 O1 102.63(7) . 4_666 ?
N3 Zn1 N1 79.63(7) . . ?
O1 Zn1 N1 98.57(7) 4_666 . ?
N3 Zn1 O4 102.71(7) . . ?
O1 Zn1 O4 151.03(6) 4_666 . ?
N1 Zn1 O4 99.59(7) . . ?
N3 Zn1 O3 102.94(7) . . ?
O1 Zn1 O3 99.92(6) 4_666 . ?
N1 Zn1 O3 160.24(7) . . ?
O4 Zn1 O3 60.66(7) . . ?
N3 Zn1 O2 160.18(6) . 4_666 ?
O1 Zn1 O2 60.80(6) 4_666 4_666 ?
N1 Zn1 O2 91.65(7) . 4_666 ?
O4 Zn1 O2 96.24(6) . 4_666 ?
O3 Zn1 O2 91.30(7) . 4_666 ?
N3 Zn1 C21 107.44(7) . . ?
O1 Zn1 C21 125.85(7) 4_666 . ?
N1 Zn1 C21 130.18(8) . . ?
O4 Zn1 C21 30.70(8) . . ?
O3 Zn1 C21 30.16(7) . . ?
O2 Zn1 C21 91.82(7) 4_666 . ?
N3 Zn1 C22 132.23(8) . 4_666 ?
O1 Zn1 C22 30.92(7) 4_666 4_666 ?
N1 Zn1 C22 94.23(7) . 4_666 ?
O4 Zn1 C22 124.94(7) . 4_666 ?
O3 Zn1 C22 98.04(7) . 4_666 ?
O2 Zn1 C22 29.96(7) 4_666 4_666 ?
C21 Zn1 C22 112.01(8) . 4_666 ?

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
Zn1 O2 C22 O1 5.5(2) 4_465 . . . ?
Zn1 O2 C22 C17 -171.31(19) 4_465 . . . ?
Zn1 O1 C22 O2 -5.9(2) 4_465 . . . ?
Zn1 O1 C22 C17 171.02(17) 4_465 . . . ?
N1 C1 C2 C3 179.0(2) . . . . ?
C6 C1 C2 C3 0.8(4) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C4 C5 C6 N2 -177.9(3) . . . . ?
C4 C5 C6 C1 1.8(4) . . . . ?
N1 C1 C6 N2 -0.8(2) . . . . ?
C2 C1 C6 N2 177.7(2) . . . . ?
N1 C1 C6 C5 179.4(2) . . . . ?
C2 C1 C6 C5 -2.1(4) . . . . ?
N1 C7 C8 N3 4.1(3) . . . . ?
N2 C7 C8 N3 -176.7(2) . . . . ?
N1 C7 C8 N4 -176.3(2) . . . . ?
N2 C7 C8 N4 2.9(4) . . . . ?
N3 C9 C10 C11 179.6(2) . . . . ?
C14 C9 C10 C11 -0.9(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C12 C13 C14 N4 -179.0(3) . . . . ?
C12 C13 C14 C9 -0.7(4) . . . . ?
N3 C9 C14 N4 -0.6(3) . . . . ?
C10 C9 C14 N4 179.8(2) . . . . ?
N3 C9 C14 C13 -179.3(2) . . . . ?
C10 C9 C14 C13 1.2(4) . . . . ?
C20 C15 C16 C17 1.8(4) . . . . ?
C15 C16 C17 C18 -3.2(4) . . . . ?
C15 C16 C17 C22 172.4(2) . . . . ?
O2 C22 C17 C16 18.8(3) . . . . ?
O1 C22 C17 C16 -158.1(2) . . . . ?
Zn1 C22 C17 C16 -100.2(11) 4_465 . . . ?
O2 C22 C17 C18 -165.6(2) . . . . ?
O1 C22 C17 C18 17.5(3) . . . . ?
Zn1 C22 C17 C18 75.3(12) 4_465 . . . ?
C16 C17 C18 C19 1.0(4) . . . . ?
C22 C17 C18 C19 -174.5(2) . . . . ?
C17 C18 C19 C20 2.4(4) . . . . ?
C18 C19 C20 C15 -3.8(4) . . . . ?
C18 C19 C20 C21 171.7(2) . . . . ?
C16 C15 C20 C19 1.6(4) . . . . ?
C16 C15 C20 C21 -173.8(2) . . . . ?
C19 C20 C21 O3 8.6(3) . . . . ?
C15 C20 C21 O3 -175.9(2) . . . . ?
C19 C20 C21 O4 -167.3(2) . . . . ?
C15 C20 C21 O4 8.1(3) . . . . ?
C19 C20 C21 Zn1 -82.9(10) . . . . ?
C15 C20 C21 Zn1 92.5(9) . . . . ?
N2 C7 N1 C1 -0.5(2) . . . . ?
C8 C7 N1 C1 178.84(18) . . . . ?
N2 C7 N1 Zn1 175.69(14) . . . . ?
C8 C7 N1 Zn1 -5.0(2) . . . . ?
C2 C1 N1 C7 -177.6(2) . . . . ?
C6 C1 N1 C7 0.8(2) . . . . ?
C2 C1 N1 Zn1 8.3(4) . . . . ?
C6 C1 N1 Zn1 -173.38(18) . . . . ?
N1 C7 N2 C6 0.0(3) . . . . ?
C8 C7 N2 C6 -179.2(2) . . . . ?
C5 C6 N2 C7 -179.8(3) . . . . ?
C1 C6 N2 C7 0.5(2) . . . . ?
N4 C8 N3 C9 0.3(3) . . . . ?
C7 C8 N3 C9 179.96(19) . . . . ?
N4 C8 N3 Zn1 179.46(15) . . . . ?
C7 C8 N3 Zn1 -0.9(2) . . . . ?
C10 C9 N3 C8 179.7(2) . . . . ?
C14 C9 N3 C8 0.2(2) . . . . ?
C10 C9 N3 Zn1 1.0(4) . . . . ?
C14 C9 N3 Zn1 -178.55(18) . . . . ?
N3 C8 N4 C14 -0.7(3) . . . . ?
C7 C8 N4 C14 179.7(2) . . . . ?
C13 C14 N4 C8 179.2(3) . . . . ?
C9 C14 N4 C8 0.7(2) . . . . ?
O4 C21 O3 Zn1 8.8(2) . . . . ?
C20 C21 O3 Zn1 -167.06(19) . . . . ?
O3 C21 O4 Zn1 -8.8(2) . . . . ?
C20 C21 O4 Zn1 167.10(18) . . . . ?
C8 N3 Zn1 O1 -97.90(15) . . . 4_666 ?
C9 N3 Zn1 O1 80.8(2) . . . 4_666 ?
C8 N3 Zn1 N1 -1.34(15) . . . . ?
C9 N3 Zn1 N1 177.4(3) . . . . ?
C8 N3 Zn1 O4 96.26(15) . . . . ?
C9 N3 Zn1 O4 -85.0(2) . . . . ?
C8 N3 Zn1 O3 158.65(15) . . . . ?
C9 N3 Zn1 O3 -22.6(3) . . . . ?
C8 N3 Zn1 O2 -66.4(3) . . . 4_666 ?
C9 N3 Zn1 O2 112.3(3) . . . 4_666 ?
C8 N3 Zn1 C21 127.71(15) . . . . ?
C9 N3 Zn1 C21 -53.6(3) . . . . ?
C8 N3 Zn1 C22 -87.63(17) . . . 4_666 ?
C9 N3 Zn1 C22 91.1(3) . . . 4_666 ?
C7 N1 Zn1 N3 3.44(15) . . . . ?
C1 N1 Zn1 N3 177.4(2) . . . . ?
C7 N1 Zn1 O1 104.81(15) . . . 4_666 ?
C1 N1 Zn1 O1 -81.3(2) . . . 4_666 ?
C7 N1 Zn1 O4 -97.86(15) . . . . ?
C1 N1 Zn1 O4 76.1(2) . . . . ?
C7 N1 Zn1 O3 -96.0(3) . . . . ?
C1 N1 Zn1 O3 77.9(3) . . . . ?
C7 N1 Zn1 O2 165.52(15) . . . 4_666 ?
C1 N1 Zn1 O2 -20.5(2) . . . 4_666 ?
C7 N1 Zn1 C21 -100.70(16) . . . . ?
C1 N1 Zn1 C21 73.2(3) . . . . ?
C7 N1 Zn1 C22 135.63(15) . . . 4_666 ?
C1 N1 Zn1 C22 -50.4(2) . . . 4_666 ?
C21 O4 Zn1 N3 102.82(14) . . . . ?
C21 O4 Zn1 O1 -47.6(2) . . . 4_666 ?
C21 O4 Zn1 N1 -175.75(14) . . . . ?
C21 O4 Zn1 O3 4.97(13) . . . . ?
C21 O4 Zn1 O2 -83.01(14) . . . 4_666 ?
C21 O4 Zn1 C22 -73.67(16) . . . 4_666 ?
C21 O3 Zn1 N3 -102.51(15) . . . . ?
C21 O3 Zn1 O1 151.95(14) . . . 4_666 ?
C21 O3 Zn1 N1 -7.2(3) . . . . ?
C21 O3 Zn1 O4 -5.05(13) . . . . ?
C21 O3 Zn1 O2 91.38(15) . . . 4_666 ?
C21 O3 Zn1 C22 120.69(15) . . . 4_666 ?
O3 C21 Zn1 N3 85.79(15) . . . . ?
O4 C21 Zn1 N3 -85.56(14) . . . . ?
C20 C21 Zn1 N3 -176.2(9) . . . . ?
O3 C21 Zn1 O1 -34.86(17) . . . 4_666 ?
O4 C21 Zn1 O1 153.79(12) . . . 4_666 ?
C20 C21 Zn1 O1 63.1(10) . . . 4_666 ?
O3 C21 Zn1 N1 176.84(14) . . . . ?
O4 C21 Zn1 N1 5.49(18) . . . . ?
C20 C21 Zn1 N1 -85.2(9) . . . . ?
O3 C21 Zn1 O4 171.4(2) . . . . ?
C20 C21 Zn1 O4 -90.7(9) . . . . ?
O4 C21 Zn1 O3 -171.4(2) . . . . ?
C20 C21 Zn1 O3 98.0(10) . . . . ?
O3 C21 Zn1 O2 -89.46(15) . . . 4_666 ?
O4 C21 Zn1 O2 99.19(14) . . . 4_666 ?
C20 C21 Zn1 O2 8.5(9) . . . 4_666 ?
O3 C21 Zn1 C22 -66.70(16) . . . 4_666 ?
O4 C21 Zn1 C22 121.95(14) . . . 4_666 ?
C20 C21 Zn1 C22 31.3(10) . . . 4_666 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H5 O4 0.88(3) 1.93(3) 2.780(3) 163(3) 3_567
N4 H6 O1 0.80(4) 2.07(3) 2.798(3) 151(3) 2_556
C15 H11 O1 0.89(3) 2.55(3) 3.324(3) 146(2) 4_566

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.097


