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

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Miao Du'
'Zhi-Hui Zhang'

_publ_contact_author_name        'Miao Du'
_publ_contact_author_address     
;
Tianjin Normal University
Tianjin
300387
CHINA
;

_publ_contact_author_email       DUMIAO@PUBLIC.TPT.TJ.CN

_publ_requested_journal          CrystEngComm

_publ_section_title              
;
Flexible and versatile anionic modules in the
direction of 1-D, 2-D, and 3-D
coordination frameworks by metal-ligand synergistic interactions
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 680430'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Co2 N12 O16 S4'
_chemical_formula_weight         1134.84

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'
Co Co 0.3494 0.9721 '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                   11.7254(12)
_cell_length_b                   12.6702(13)
_cell_length_c                   16.507(3)
_cell_angle_alpha                96.307(2)
_cell_angle_beta                 96.961(2)
_cell_angle_gamma                113.7600(10)
_cell_volume                     2193.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    4206
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.16

_exptl_crystal_description       Prism
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.779488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11805
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.01
_reflns_number_total             7618
_reflns_number_gt                5687
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0603P)²+0.6951P] 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         7618
_refine_ls_number_parameters     631
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Co1 Co 0.14412(4) -0.00939(3) 0.12859(2) 0.03564(13) Uani 1 1 d . . .
Co2 Co 0.83121(4) 1.01599(3) 0.37603(3) 0.03668(13) Uani 1 1 d . . .
S1 S 0.26915(8) -0.26429(7) 0.29392(5) 0.0426(2) Uani 1 1 d . . .
S2 S 0.48225(8) 0.75031(7) 0.50973(6) 0.0486(2) Uani 1 1 d . . .
S3 S 0.52866(8) 0.27009(7) -0.01497(5) 0.0470(2) Uani 1 1 d . . .
S4 S 1.29260(8) 1.73384(7) 0.79462(5) 0.0464(2) Uani 1 1 d . . .
O1 O 0.14882(18) -0.44827(16) 0.17326(12) 0.0361(5) Uani 1 1 d . . .
O2 O 0.0913(2) -0.06818(19) 0.25448(15) 0.0500(6) Uani 1 1 d . . .
O3 O 0.24686(19) -0.08028(17) 0.20028(12) 0.0379(5) Uani 1 1 d . . .
O4 O 0.40770(19) 0.55246(17) 0.40398(13) 0.0409(5) Uani 1 1 d . . .
O5 O 0.8288(2) 0.94318(19) 0.49314(14) 0.0485(6) Uani 1 1 d . . .
O6 O 0.6580(2) 0.9558(2) 0.43969(15) 0.0562(6) Uani 1 1 d . . .
O7 O 0.59348(19) 0.46082(17) 0.09698(13) 0.0409(5) Uani 1 1 d . . .
O8 O 0.3988(3) 0.0673(3) 0.06812(18) 0.0842(9) Uani 1 1 d . . .
O9 O 0.2084(2) 0.05663(19) 0.02700(14) 0.0503(6) Uani 1 1 d . . .
O10 O 1.15547(18) 1.55420(16) 0.67438(12) 0.0376(5) Uani 1 1 d . . .
O11 O 1.2581(2) 1.91326(17) 0.70152(12) 0.0406(5) Uani 1 1 d . . .
O12 O 1.1351(2) 1.9505(2) 0.77817(16) 0.0610(7) Uani 1 1 d . . .
O13 O -0.0226(2) 0.0032(2) 0.10410(14) 0.0587(7) Uani 1 1 d . . .
H13A H -0.0574 0.0048 0.1462 0.088 Uiso 1 1 d R . .
H13B H -0.0712 -0.0336 0.0582 0.088 Uiso 1 1 d R . .
O14 O 1.0064(2) 1.0285(2) 0.37334(14) 0.0606(7) Uani 1 1 d . . .
H14A H 1.0515 1.0230 0.4157 0.091 Uiso 1 1 d R . .
H14B H 1.0251 1.0140 0.3265 0.091 Uiso 1 1 d R . .
N1 N -0.0672(2) -0.8153(2) -0.04774(15) 0.0378(6) Uani 1 1 d . . .
N2 N -0.0450(2) -0.4589(2) 0.14456(16) 0.0414(6) Uani 1 1 d . . .
N3 N 0.0260(2) -0.3626(2) 0.20868(16) 0.0406(6) Uani 1 1 d . . .
N4 N 0.5829(3) 0.5320(2) 0.39200(18) 0.0503(7) Uani 1 1 d . . .
N5 N 0.6154(3) 0.6378(2) 0.44631(18) 0.0494(7) Uani 1 1 d . . .
N6 N 0.2427(2) 0.1614(2) 0.20763(15) 0.0379(6) Uani 1 1 d . . .
N7 N 0.4123(3) 0.4614(2) 0.11888(18) 0.0523(8) Uani 1 1 d . . .
N8 N 0.3860(3) 0.3604(2) 0.06093(18) 0.0502(7) Uani 1 1 d . . .
N9 N 0.7373(2) 0.8411(2) 0.30113(15) 0.0366(6) Uani 1 1 d . . .
N10 N 0.9664(2) 1.5553(2) 0.65393(16) 0.0402(6) Uani 1 1 d . . .
N11 N 1.0456(2) 1.6495(2) 0.71730(16) 0.0417(6) Uani 1 1 d . . .
N12 N 0.9129(2) 1.1904(2) 0.45582(16) 0.0394(6) Uani 1 1 d . . .
C1 C 0.0003(3) -0.6097(2) 0.06539(18) 0.0342(7) Uani 1 1 d . . .
C2 C 0.0875(3) -0.6535(3) 0.0524(2) 0.0441(8) Uani 1 1 d . . .
H2 H 0.1704 -0.6154 0.0814 0.053 Uiso 1 1 calc R . .
C3 C 0.0502(3) -0.7554(3) -0.0046(2) 0.0476(8) Uani 1 1 d . . .
H3 H 0.1105 -0.7837 -0.0132 0.057 Uiso 1 1 calc R . .
C4 C -0.1499(3) -0.7697(3) -0.03490(19) 0.0416(7) Uani 1 1 d . . .
H4 H -0.2321 -0.8089 -0.0648 0.050 Uiso 1 1 calc R . .
C5 C -0.1212(3) -0.6695(3) 0.01933(18) 0.0379(7) Uani 1 1 d . . .
H5 H -0.1824 -0.6415 0.0254 0.045 Uiso 1 1 calc R . .
C6 C 0.0296(3) -0.5057(2) 0.12653(18) 0.0336(7) Uani 1 1 d . . .
C7 C 0.1373(3) -0.3606(2) 0.22290(18) 0.0340(7) Uani 1 1 d . . .
C8 C 0.2072(3) -0.1599(3) 0.32433(19) 0.0412(7) Uani 1 1 d . . .
H8A H 0.1293 -0.2000 0.3445 0.049 Uiso 1 1 calc R . .
H8B H 0.2674 -0.1013 0.3699 0.049 Uiso 1 1 calc R . .
C9 C 0.1805(3) -0.0984(2) 0.25534(18) 0.0341(7) Uani 1 1 d . . .
C10 C 0.3834(3) 0.3752(2) 0.31393(18) 0.0359(7) Uani 1 1 d . . .
C11 C 0.4413(3) 0.3071(3) 0.2827(2) 0.0438(8) Uani 1 1 d . . .
H11 H 0.5285 0.3323 0.2967 0.053 Uiso 1 1 calc R . .
C12 C 0.3688(3) 0.2026(3) 0.2312(2) 0.0436(8) Uani 1 1 d . . .
H12 H 0.4089 0.1577 0.2114 0.052 Uiso 1 1 calc R . .
C13 C 0.1880(3) 0.2279(3) 0.2383(2) 0.0447(8) Uani 1 1 d . . .
H13 H 0.1006 0.2008 0.2233 0.054 Uiso 1 1 calc R . .
C14 C 0.2536(3) 0.3338(3) 0.2908(2) 0.0436(8) Uani 1 1 d . . .
H14 H 0.2113 0.3768 0.3104 0.052 Uiso 1 1 calc R . .
C15 C 0.4627(3) 0.4861(2) 0.36915(19) 0.0373(7) Uani 1 1 d . . .
C16 C 0.5097(3) 0.6442(2) 0.45079(19) 0.0386(7) Uani 1 1 d . . .
C17 C 0.6454(3) 0.8479(2) 0.55155(18) 0.0381(7) Uani 1 1 d . . .
H17A H 0.6482 0.9005 0.5999 0.046 Uiso 1 1 calc R . .
H17B H 0.6898 0.8021 0.5696 0.046 Uiso 1 1 calc R . .
C18 C 0.7141(3) 0.9201(2) 0.49090(18) 0.0380(7) Uani 1 1 d . . .
C19 C 0.6060(3) 0.6270(2) 0.19384(18) 0.0359(7) Uani 1 1 d . . .
C20 C 0.7363(3) 0.6730(3) 0.2185(2) 0.0460(8) Uani 1 1 d . . .
H20 H 0.7819 0.6331 0.1994 0.055 Uiso 1 1 calc R . .
C21 C 0.7972(3) 0.7788(3) 0.2717(2) 0.0462(8) Uani 1 1 d . . .
H21 H 0.8846 0.8087 0.2881 0.055 Uiso 1 1 calc R . .
C22 C 0.6112(3) 0.7958(3) 0.27665(19) 0.0420(8) Uani 1 1 d . . .
H22 H 0.5679 0.8377 0.2963 0.050 Uiso 1 1 calc R . .
C23 C 0.5431(3) 0.6912(3) 0.2244(2) 0.0430(8) Uani 1 1 d . . .
H23 H 0.4556 0.6631 0.2093 0.052 Uiso 1 1 calc R . .
C24 C 0.5330(3) 0.5164(2) 0.13741(19) 0.0371(7) Uani 1 1 d . . .
C25 C 0.4951(3) 0.3651(3) 0.05062(18) 0.0371(7) Uani 1 1 d . . .
C26 C 0.3687(3) 0.1585(2) -0.04591(18) 0.0378(7) Uani 1 1 d . . .
H26A H 0.3126 0.1950 -0.0610 0.045 Uiso 1 1 calc R . .
H26B H 0.3643 0.1055 -0.0945 0.045 Uiso 1 1 calc R . .
C27 C 0.3232(3) 0.0889(3) 0.0218(2) 0.0443(8) Uani 1 1 d . . .
C28 C 0.9956(3) 1.3980(2) 0.56894(18) 0.0341(7) Uani 1 1 d . . .
C29 C 0.8731(3) 1.3455(3) 0.52284(19) 0.0379(7) Uani 1 1 d . . .
H29 H 0.8166 1.3792 0.5292 0.045 Uiso 1 1 calc R . .
C30 C 0.8372(3) 1.2439(3) 0.46822(19) 0.0386(7) Uani 1 1 d . . .
H30 H 0.7551 1.2098 0.4378 0.046 Uiso 1 1 calc R . .
C31 C 1.0310(3) 1.2435(3) 0.4989(2) 0.0500(9) Uani 1 1 d . . .
H31 H 1.0861 1.2089 0.4904 0.060 Uiso 1 1 calc R . .
C32 C 1.0764(3) 1.3463(3) 0.5551(2) 0.0451(8) Uani 1 1 d . . .
H32 H 1.1599 1.3802 0.5831 0.054 Uiso 1 1 calc R . .
C33 C 1.0339(3) 1.5026(2) 0.63087(18) 0.0340(7) Uani 1 1 d . . .
C34 C 1.1539(3) 1.6448(2) 0.72692(18) 0.0360(7) Uani 1 1 d . . .
C35 C 1.2458(3) 1.8460(3) 0.83144(19) 0.0424(8) Uani 1 1 d . . .
H35A H 1.1738 1.8114 0.8585 0.051 Uiso 1 1 calc R . .
H35B H 1.3147 1.9042 0.8729 0.051 Uiso 1 1 calc R . .
C36 C 1.2106(3) 1.9074(2) 0.76542(19) 0.0375(7) Uani 1 1 d . . .
O15 O 0.5007(2) 0.0363(3) 0.35367(17) 0.0749(8) Uani 1 1 d . . .
H15A H 0.5371 0.0092 0.3880 0.112 Uiso 1 1 d R . .
H15B H 0.5330 0.0535 0.3109 0.112 Uiso 1 1 d R . .
O16 O 0.4753(2) 0.9294(3) 0.15526(17) 0.0732(8) Uani 1 1 d . . .
H16A H 0.4648 0.9672 0.1177 0.110 Uiso 1 1 d R . .
H16B H 0.4330 0.9258 0.1940 0.110 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O13 2.021(2) . ?
Co1 O9 2.046(2) . ?
Co1 O3 2.102(2) . ?
Co1 N6 2.172(2) . ?
Co1 N1 2.230(2) 2_545 ?
Co1 O2 2.353(2) . ?
Co2 O14 2.003(2) . ?
Co2 O11 2.055(2) 2_786 ?
Co2 N9 2.180(2) . ?
Co2 N12 2.210(2) . ?
Co2 O5 2.230(2) . ?
Co2 O6 2.293(3) . ?
S1 C7 1.726(3) . ?
S1 C8 1.802(3) . ?
S2 C16 1.730(3) . ?
S2 C17 1.803(3) . ?
S3 C25 1.724(3) . ?
S3 C26 1.803(3) . ?
S4 C34 1.724(3) . ?
S4 C35 1.791(3) . ?
O1 C7 1.368(3) . ?
O1 C6 1.369(3) . ?
O2 C9 1.250(3) . ?
O3 C9 1.248(3) . ?
O4 C16 1.355(3) . ?
O4 C15 1.369(4) . ?
O5 C18 1.251(4) . ?
O6 C18 1.242(4) . ?
O7 C25 1.357(3) . ?
O7 C24 1.363(4) . ?
O8 C27 1.233(4) . ?
O9 C27 1.257(4) . ?
O10 C33 1.368(3) . ?
O10 C34 1.368(3) . ?
O11 C36 1.247(4) . ?
O11 Co2 2.055(2) 2_786 ?
O12 C36 1.238(4) . ?
O13 H13A 0.8508 . ?
O13 H13B 0.8490 . ?
O14 H14A 0.8500 . ?
O14 H14B 0.8499 . ?
N1 C3 1.335(4) . ?
N1 C4 1.339(4) . ?
N1 Co1 2.230(2) 2_545 ?
N2 C6 1.283(4) . ?
N2 N3 1.410(3) . ?
N3 C7 1.287(4) . ?
N4 C15 1.277(4) . ?
N4 N5 1.410(4) . ?
N5 C16 1.285(4) . ?
N6 C12 1.343(4) . ?
N6 C13 1.341(4) . ?
N7 C24 1.279(4) . ?
N7 N8 1.410(4) . ?
N8 C25 1.290(4) . ?
N9 C22 1.341(4) . ?
N9 C21 1.341(4) . ?
N10 C33 1.289(4) . ?
N10 N11 1.406(3) . ?
N11 C34 1.286(4) . ?
N12 C31 1.334(4) . ?
N12 C30 1.338(4) . ?
C1 C2 1.373(4) . ?
C1 C5 1.387(4) . ?
C1 C6 1.460(4) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.364(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C8 C9 1.519(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 C14 1.382(4) . ?
C10 C11 1.389(4) . ?
C10 C15 1.460(4) . ?
C11 C12 1.367(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.377(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C17 C18 1.514(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C19 C20 1.385(4) . ?
C19 C23 1.394(4) . ?
C19 C24 1.455(4) . ?
C20 C21 1.377(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.367(4) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C26 C27 1.514(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C28 C32 1.377(4) . ?
C28 C29 1.393(4) . ?
C28 C33 1.455(4) . ?
C29 C30 1.365(4) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.378(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C35 C36 1.517(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O15 H15A 0.8501 . ?
O15 H15B 0.8498 . ?
O16 H16A 0.8498 . ?
O16 H16B 0.8502 . ?

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
O13 Co1 O9 94.78(10) . . ?
O13 Co1 O3 145.07(9) . . ?
O9 Co1 O3 119.22(9) . . ?
O13 Co1 N6 94.87(9) . . ?
O9 Co1 N6 92.06(9) . . ?
O3 Co1 N6 91.86(8) . . ?
O13 Co1 N1 92.28(9) . 2_545 ?
O9 Co1 N1 85.84(9) . 2_545 ?
O3 Co1 N1 83.10(8) . 2_545 ?
N6 Co1 N1 172.70(9) . 2_545 ?
O13 Co1 O2 88.82(9) . . ?
O9 Co1 O2 173.50(8) . . ?
O3 Co1 O2 58.20(8) . . ?
N6 Co1 O2 82.23(9) . . ?
N1 Co1 O2 99.44(8) 2_545 . ?
O14 Co2 O11 123.79(10) . 2_786 ?
O14 Co2 N9 94.49(9) . . ?
O11 Co2 N9 93.90(8) 2_786 . ?
O14 Co2 N12 89.55(9) . . ?
O11 Co2 N12 85.27(9) 2_786 . ?
N9 Co2 N12 175.60(10) . . ?
O14 Co2 O5 90.56(9) . . ?
O11 Co2 O5 144.49(9) 2_786 . ?
N9 Co2 O5 91.77(9) . . ?
N12 Co2 O5 86.44(9) . . ?
O14 Co2 O6 147.55(9) . . ?
O11 Co2 O6 88.56(8) 2_786 . ?
N9 Co2 O6 84.67(9) . . ?
N12 Co2 O6 90.98(9) . . ?
O5 Co2 O6 57.11(8) . . ?
C7 S1 C8 97.10(14) . . ?
C16 S2 C17 97.56(15) . . ?
C25 S3 C26 96.91(14) . . ?
C34 S4 C35 97.70(15) . . ?
C7 O1 C6 101.7(2) . . ?
C9 O2 Co1 84.36(17) . . ?
C9 O3 Co1 95.96(18) . . ?
C16 O4 C15 101.8(2) . . ?
C18 O5 Co2 92.19(19) . . ?
C18 O6 Co2 89.5(2) . . ?
C25 O7 C24 102.2(2) . . ?
C27 O9 Co1 120.0(2) . . ?
C33 O10 C34 102.0(2) . . ?
C36 O11 Co2 106.5(2) . 2_786 ?
Co1 O13 H13A 113.9 . . ?
Co1 O13 H13B 117.8 . . ?
H13A O13 H13B 117.0 . . ?
Co2 O14 H14A 121.2 . . ?
Co2 O14 H14B 118.0 . . ?
H14A O14 H14B 117.1 . . ?
C3 N1 C4 116.1(3) . . ?
C3 N1 Co1 126.8(2) . 2_545 ?
C4 N1 Co1 116.81(19) . 2_545 ?
C6 N2 N3 106.5(2) . . ?
C7 N3 N2 105.7(2) . . ?
C15 N4 N5 106.8(3) . . ?
C16 N5 N4 105.1(2) . . ?
C12 N6 C13 116.5(3) . . ?
C12 N6 Co1 117.8(2) . . ?
C13 N6 Co1 125.7(2) . . ?
C24 N7 N8 106.5(3) . . ?
C25 N8 N7 105.4(2) . . ?
C22 N9 C21 117.0(3) . . ?
C22 N9 Co2 118.0(2) . . ?
C21 N9 Co2 124.8(2) . . ?
C33 N10 N11 106.7(2) . . ?
C34 N11 N10 105.9(2) . . ?
C31 N12 C30 116.3(3) . . ?
C31 N12 Co2 124.8(2) . . ?
C30 N12 Co2 118.6(2) . . ?
C2 C1 C5 117.7(3) . . ?
C2 C1 C6 122.8(3) . . ?
C5 C1 C6 119.4(3) . . ?
C1 C2 C3 119.1(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
N1 C3 C2 123.7(3) . . ?
N1 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
N1 C4 C5 124.1(3) . . ?
N1 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C4 C5 C1 119.3(3) . . ?
C4 C5 H5 120.4 . . ?
C1 C5 H5 120.4 . . ?
N2 C6 O1 112.9(2) . . ?
N2 C6 C1 127.8(3) . . ?
O1 C6 C1 119.3(3) . . ?
N3 C7 O1 113.3(3) . . ?
N3 C7 S1 129.1(2) . . ?
O1 C7 S1 117.6(2) . . ?
C9 C8 S1 114.2(2) . . ?
C9 C8 H8A 108.7 . . ?
S1 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
S1 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O2 C9 O3 121.4(3) . . ?
O2 C9 C8 119.1(3) . . ?
O3 C9 C8 119.5(3) . . ?
C14 C10 C11 118.0(3) . . ?
C14 C10 C15 123.7(3) . . ?
C11 C10 C15 118.4(3) . . ?
C12 C11 C10 119.3(3) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N6 C12 C11 123.5(3) . . ?
N6 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
N6 C13 C14 123.8(3) . . ?
N6 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C13 C14 C10 118.8(3) . . ?
C13 C14 H14 120.6 . . ?
C10 C14 H14 120.6 . . ?
N4 C15 O4 112.5(3) . . ?
N4 C15 C10 127.7(3) . . ?
O4 C15 C10 119.7(3) . . ?
N5 C16 O4 113.7(3) . . ?
N5 C16 S2 128.7(2) . . ?
O4 C16 S2 117.5(2) . . ?
C18 C17 S2 113.9(2) . . ?
C18 C17 H17A 108.8 . . ?
S2 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
S2 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
O6 C18 O5 120.4(3) . . ?
O6 C18 C17 120.8(3) . . ?
O5 C18 C17 118.8(3) . . ?
C20 C19 C23 117.8(3) . . ?
C20 C19 C24 123.2(3) . . ?
C23 C19 C24 119.0(3) . . ?
C21 C20 C19 119.0(3) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
N9 C21 C20 123.5(3) . . ?
N9 C21 H21 118.2 . . ?
C20 C21 H21 118.2 . . ?
N9 C22 C23 123.4(3) . . ?
N9 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C22 C23 C19 119.3(3) . . ?
C22 C23 H23 120.3 . . ?
C19 C23 H23 120.3 . . ?
N7 C24 O7 112.8(3) . . ?
N7 C24 C19 127.1(3) . . ?
O7 C24 C19 120.1(3) . . ?
N8 C25 O7 113.1(3) . . ?
N8 C25 S3 128.6(2) . . ?
O7 C25 S3 118.2(2) . . ?
C27 C26 S3 112.6(2) . . ?
C27 C26 H26A 109.1 . . ?
S3 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
S3 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
O8 C27 O9 124.0(3) . . ?
O8 C27 C26 119.4(3) . . ?
O9 C27 C26 116.6(3) . . ?
C32 C28 C29 118.0(3) . . ?
C32 C28 C33 122.0(3) . . ?
C29 C28 C33 119.9(3) . . ?
C30 C29 C28 118.9(3) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N12 C30 C29 123.9(3) . . ?
N12 C30 H30 118.0 . . ?
C29 C30 H30 118.0 . . ?
N12 C31 C32 124.1(3) . . ?
N12 C31 H31 118.0 . . ?
C32 C31 H31 118.0 . . ?
C28 C32 C31 118.7(3) . . ?
C28 C32 H32 120.7 . . ?
C31 C32 H32 120.7 . . ?
N10 C33 O10 112.4(3) . . ?
N10 C33 C28 128.6(3) . . ?
O10 C33 C28 119.1(3) . . ?
N11 C34 O10 113.0(3) . . ?
N11 C34 S4 129.9(2) . . ?
O10 C34 S4 117.1(2) . . ?
C36 C35 S4 115.1(2) . . ?
C36 C35 H35A 108.5 . . ?
S4 C35 H35A 108.5 . . ?
C36 C35 H35B 108.5 . . ?
S4 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
O12 C36 O11 122.8(3) . . ?
O12 C36 C35 117.6(3) . . ?
O11 C36 C35 119.6(3) . . ?
H15A O15 H15B 117.0 . . ?
H16A O16 H16B 117.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O13 Co1 O2 C9 166.01(17) . . . . ?
O3 Co1 O2 C9 -1.84(16) . . . . ?
N6 Co1 O2 C9 -98.91(17) . . . . ?
N1 Co1 O2 C9 73.90(18) 2_545 . . . ?
O13 Co1 O3 C9 -19.7(2) . . . . ?
O9 Co1 O3 C9 174.92(16) . . . . ?
N6 Co1 O3 C9 81.52(18) . . . . ?
N1 Co1 O3 C9 -103.78(17) 2_545 . . . ?
O2 Co1 O3 C9 1.85(16) . . . . ?
O14 Co2 O5 C18 -171.93(18) . . . . ?
O11 Co2 O5 C18 21.8(2) 2_786 . . . ?
N9 Co2 O5 C18 -77.42(18) . . . . ?
N12 Co2 O5 C18 98.56(18) . . . . ?
O6 Co2 O5 C18 5.08(16) . . . . ?
O14 Co2 O6 C18 0.5(3) . . . . ?
O11 Co2 O6 C18 -175.47(18) 2_786 . . . ?
N9 Co2 O6 C18 90.47(18) . . . . ?
N12 Co2 O6 C18 -90.23(18) . . . . ?
O5 Co2 O6 C18 -5.11(17) . . . . ?
O13 Co1 O9 C27 166.0(2) . . . . ?
O3 Co1 O9 C27 -22.4(3) . . . . ?
N6 Co1 O9 C27 70.9(2) . . . . ?
N1 Co1 O9 C27 -102.1(2) 2_545 . . . ?
C6 N2 N3 C7 0.2(3) . . . . ?
C15 N4 N5 C16 0.3(4) . . . . ?
O13 Co1 N6 C12 -170.4(2) . . . . ?
O9 Co1 N6 C12 -75.4(2) . . . . ?
O3 Co1 N6 C12 43.9(2) . . . . ?
O2 Co1 N6 C12 101.5(2) . . . . ?
O13 Co1 N6 C13 12.8(3) . . . . ?
O9 Co1 N6 C13 107.7(3) . . . . ?
O3 Co1 N6 C13 -132.9(2) . . . . ?
O2 Co1 N6 C13 -75.4(3) . . . . ?
C24 N7 N8 C25 0.1(4) . . . . ?
O14 Co2 N9 C22 -172.8(2) . . . . ?
O11 Co2 N9 C22 -48.5(2) 2_786 . . . ?
O5 Co2 N9 C22 96.5(2) . . . . ?
O6 Co2 N9 C22 39.7(2) . . . . ?
O14 Co2 N9 C21 1.3(3) . . . . ?
O11 Co2 N9 C21 125.7(2) 2_786 . . . ?
O5 Co2 N9 C21 -89.4(3) . . . . ?
O6 Co2 N9 C21 -146.1(3) . . . . ?
C33 N10 N11 C34 -0.2(3) . . . . ?
O14 Co2 N12 C31 -18.2(3) . . . . ?
O11 Co2 N12 C31 -142.2(3) 2_786 . . . ?
O5 Co2 N12 C31 72.4(3) . . . . ?
O6 Co2 N12 C31 129.3(3) . . . . ?
O14 Co2 N12 C30 167.7(2) . . . . ?
O11 Co2 N12 C30 43.7(2) 2_786 . . . ?
O5 Co2 N12 C30 -101.7(2) . . . . ?
O6 Co2 N12 C30 -44.7(2) . . . . ?
C5 C1 C2 C3 -1.0(5) . . . . ?
C6 C1 C2 C3 177.4(3) . . . . ?
C4 N1 C3 C2 1.7(5) . . . . ?
Co1 N1 C3 C2 -171.8(2) 2_545 . . . ?
C1 C2 C3 N1 -0.7(5) . . . . ?
C3 N1 C4 C5 -1.1(5) . . . . ?
Co1 N1 C4 C5 173.1(2) 2_545 . . . ?
N1 C4 C5 C1 -0.5(5) . . . . ?
C2 C1 C5 C4 1.6(4) . . . . ?
C6 C1 C5 C4 -176.9(3) . . . . ?
N3 N2 C6 O1 -0.4(3) . . . . ?
N3 N2 C6 C1 178.4(3) . . . . ?
C7 O1 C6 N2 0.5(3) . . . . ?
C7 O1 C6 C1 -178.5(2) . . . . ?
C2 C1 C6 N2 -178.6(3) . . . . ?
C5 C1 C6 N2 -0.2(5) . . . . ?
C2 C1 C6 O1 0.1(4) . . . . ?
C5 C1 C6 O1 178.5(3) . . . . ?
N2 N3 C7 O1 0.1(3) . . . . ?
N2 N3 C7 S1 179.9(2) . . . . ?
C6 O1 C7 N3 -0.4(3) . . . . ?
C6 O1 C7 S1 179.9(2) . . . . ?
C8 S1 C7 N3 -9.7(3) . . . . ?
C8 S1 C7 O1 170.1(2) . . . . ?
C7 S1 C8 C9 -64.5(2) . . . . ?
Co1 O2 C9 O3 3.1(3) . . . . ?
Co1 O2 C9 C8 -176.1(2) . . . . ?
Co1 O3 C9 O2 -3.5(3) . . . . ?
Co1 O3 C9 C8 175.7(2) . . . . ?
S1 C8 C9 O2 148.1(2) . . . . ?
S1 C8 C9 O3 -31.1(4) . . . . ?
C14 C10 C11 C12 -0.3(5) . . . . ?
C15 C10 C11 C12 179.7(3) . . . . ?
C13 N6 C12 C11 -0.9(5) . . . . ?
Co1 N6 C12 C11 -178.1(3) . . . . ?
C10 C11 C12 N6 0.8(5) . . . . ?
C12 N6 C13 C14 0.6(5) . . . . ?
Co1 N6 C13 C14 177.5(2) . . . . ?
N6 C13 C14 C10 -0.1(5) . . . . ?
C11 C10 C14 C13 0.0(5) . . . . ?
C15 C10 C14 C13 -180.0(3) . . . . ?
N5 N4 C15 O4 -0.2(4) . . . . ?
N5 N4 C15 C10 -179.0(3) . . . . ?
C16 O4 C15 N4 0.0(3) . . . . ?
C16 O4 C15 C10 178.9(3) . . . . ?
C14 C10 C15 N4 -178.2(3) . . . . ?
C11 C10 C15 N4 1.8(5) . . . . ?
C14 C10 C15 O4 3.1(5) . . . . ?
C11 C10 C15 O4 -176.9(3) . . . . ?
N4 N5 C16 O4 -0.3(4) . . . . ?
N4 N5 C16 S2 177.7(2) . . . . ?
C15 O4 C16 N5 0.2(3) . . . . ?
C15 O4 C16 S2 -178.0(2) . . . . ?
C17 S2 C16 N5 4.8(3) . . . . ?
C17 S2 C16 O4 -177.2(2) . . . . ?
C16 S2 C17 C18 76.7(2) . . . . ?
Co2 O6 C18 O5 8.9(3) . . . . ?
Co2 O6 C18 C17 -171.0(2) . . . . ?
Co2 O5 C18 O6 -9.2(3) . . . . ?
Co2 O5 C18 C17 170.8(2) . . . . ?
S2 C17 C18 O6 35.2(4) . . . . ?
S2 C17 C18 O5 -144.8(2) . . . . ?
C23 C19 C20 C21 0.2(5) . . . . ?
C24 C19 C20 C21 179.5(3) . . . . ?
C22 N9 C21 C20 0.2(5) . . . . ?
Co2 N9 C21 C20 -174.0(2) . . . . ?
C19 C20 C21 N9 -0.4(5) . . . . ?
C21 N9 C22 C23 0.1(5) . . . . ?
Co2 N9 C22 C23 174.7(3) . . . . ?
N9 C22 C23 C19 -0.3(5) . . . . ?
C20 C19 C23 C22 0.1(5) . . . . ?
C24 C19 C23 C22 -179.3(3) . . . . ?
N8 N7 C24 O7 -0.4(4) . . . . ?
N8 N7 C24 C19 178.9(3) . . . . ?
C25 O7 C24 N7 0.5(3) . . . . ?
C25 O7 C24 C19 -178.9(3) . . . . ?
C20 C19 C24 N7 171.5(3) . . . . ?
C23 C19 C24 N7 -9.2(5) . . . . ?
C20 C19 C24 O7 -9.3(4) . . . . ?
C23 C19 C24 O7 170.1(3) . . . . ?
N7 N8 C25 O7 0.2(4) . . . . ?
N7 N8 C25 S3 -177.6(2) . . . . ?
C24 O7 C25 N8 -0.4(3) . . . . ?
C24 O7 C25 S3 177.7(2) . . . . ?
C26 S3 C25 N8 -9.3(3) . . . . ?
C26 S3 C25 O7 173.0(2) . . . . ?
C25 S3 C26 C27 -73.5(2) . . . . ?
Co1 O9 C27 O8 11.7(4) . . . . ?
Co1 O9 C27 C26 -168.14(19) . . . . ?
S3 C26 C27 O8 -35.5(4) . . . . ?
S3 C26 C27 O9 144.3(2) . . . . ?
C32 C28 C29 C30 2.1(4) . . . . ?
C33 C28 C29 C30 -176.5(3) . . . . ?
C31 N12 C30 C29 -1.8(5) . . . . ?
Co2 N12 C30 C29 172.8(2) . . . . ?
C28 C29 C30 N12 0.0(5) . . . . ?
C30 N12 C31 C32 1.4(5) . . . . ?
Co2 N12 C31 C32 -172.8(3) . . . . ?
C29 C28 C32 C31 -2.4(5) . . . . ?
C33 C28 C32 C31 176.2(3) . . . . ?
N12 C31 C32 C28 0.6(5) . . . . ?
N11 N10 C33 O10 0.1(3) . . . . ?
N11 N10 C33 C28 178.0(3) . . . . ?
C34 O10 C33 N10 0.1(3) . . . . ?
C34 O10 C33 C28 -178.1(2) . . . . ?
C32 C28 C33 N10 -175.1(3) . . . . ?
C29 C28 C33 N10 3.5(5) . . . . ?
C32 C28 C33 O10 2.7(4) . . . . ?
C29 C28 C33 O10 -178.7(3) . . . . ?
N10 N11 C34 O10 0.2(3) . . . . ?
N10 N11 C34 S4 -179.7(2) . . . . ?
C33 O10 C34 N11 -0.2(3) . . . . ?
C33 O10 C34 S4 179.8(2) . . . . ?
C35 S4 C34 N11 -10.0(3) . . . . ?
C35 S4 C34 O10 170.0(2) . . . . ?
C34 S4 C35 C36 -60.0(3) . . . . ?
Co2 O11 C36 O12 -7.3(4) 2_786 . . . ?
Co2 O11 C36 C35 173.1(2) 2_786 . . . ?
S4 C35 C36 O12 153.2(3) . . . . ?
S4 C35 C36 O11 -27.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.060

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 680431'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H16 N6 O8 S2 Zn'
_chemical_formula_weight         573.86

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'
Zn Zn 0.2839 1.4301 '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                   8.345(5)
_cell_length_b                   11.673(7)
_cell_length_c                   12.642(7)
_cell_angle_alpha                113.281(7)
_cell_angle_beta                 95.691(8)
_cell_angle_gamma                98.615(8)
_cell_volume                     1101.4(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1866
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Rhombic
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.743912
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5978
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3818
_reflns_number_gt                2933
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0438P)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         3818
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.24206(4) 0.15598(3) 0.48379(3) 0.03510(12) Uani 1 1 d . . .
S1 S -0.02458(11) 0.52460(8) 0.76847(7) 0.0484(2) Uani 1 1 d . . .
S2 S 0.59417(9) 0.28583(7) 0.23944(6) 0.0421(2) Uani 1 1 d . . .
O1 O 0.0372(3) 0.1974(2) 0.55683(17) 0.0527(6) Uani 1 1 d . . .
O2 O 0.1199(3) 0.3837(3) 0.5558(2) 0.0860(9) Uani 1 1 d . . .
O3 O 0.1957(2) 0.59363(18) 0.96020(15) 0.0404(5) Uani 1 1 d . . .
O4 O 0.5505(3) 0.1158(2) 0.44972(18) 0.0566(6) Uani 1 1 d . . .
O5 O 0.4029(2) 0.24271(17) 0.41508(15) 0.0341(4) Uani 1 1 d . . .
O6 O 0.3555(2) 0.15358(17) 0.05818(15) 0.0354(5) Uani 1 1 d . . .
O7 O 0.2235(3) -0.0181(2) 0.4783(2) 0.0746(8) Uani 1 1 d . . .
H7A H 0.3118 -0.0378 0.4985 0.112 Uiso 1 1 d R . .
H7B H 0.1351 -0.0737 0.4596 0.112 Uiso 1 1 d R . .
N1 N 0.6008(3) 0.7474(2) 1.34146(18) 0.0343(6) Uani 1 1 d . . .
N2 N 0.2339(3) 0.4134(2) 0.9653(2) 0.0507(7) Uani 1 1 d . . .
N3 N 0.1205(3) 0.3842(2) 0.8630(2) 0.0480(7) Uani 1 1 d . . .
N4 N -0.0810(3) -0.0771(2) -0.30704(19) 0.0394(6) Uani 1 1 d . . .
N5 N 0.3036(3) -0.0400(2) 0.05289(19) 0.0402(6) Uani 1 1 d . . .
N6 N 0.4316(3) 0.0366(2) 0.14828(19) 0.0400(6) Uani 1 1 d . . .
C1 C 0.3861(3) 0.6109(3) 1.1289(2) 0.0328(7) Uani 1 1 d . . .
C2 C 0.4337(4) 0.7418(3) 1.1731(2) 0.0424(8) Uani 1 1 d . . .
H2 H 0.3945 0.7864 1.1328 0.051 Uiso 1 1 calc R . .
C3 C 0.5409(4) 0.8051(3) 1.2784(2) 0.0409(7) Uani 1 1 d . . .
H3 H 0.5734 0.8932 1.3072 0.049 Uiso 1 1 calc R . .
C4 C 0.5509(4) 0.6204(3) 1.2975(2) 0.0420(8) Uani 1 1 d . . .
H4 H 0.5891 0.5778 1.3401 0.050 Uiso 1 1 calc R . .
C5 C 0.4463(4) 0.5500(3) 1.1927(2) 0.0409(7) Uani 1 1 d . . .
H5 H 0.4165 0.4618 1.1651 0.049 Uiso 1 1 calc R . .
C6 C 0.2728(3) 0.5341(3) 1.0178(2) 0.0353(7) Uani 1 1 d . . .
C7 C 0.1025(4) 0.4925(3) 0.8652(2) 0.0369(7) Uani 1 1 d . . .
C8 C -0.0964(3) 0.3631(3) 0.6602(2) 0.0334(7) Uani 1 1 d . . .
H8A H -0.1263 0.3083 0.6993 0.040 Uiso 1 1 calc R . .
H8B H -0.1946 0.3589 0.6097 0.040 Uiso 1 1 calc R . .
C9 C 0.0310(4) 0.3136(4) 0.5858(2) 0.0449(8) Uani 1 1 d . . .
C10 C 0.1431(3) -0.0029(3) -0.1012(2) 0.0324(7) Uani 1 1 d . . .
C11 C 0.0455(3) -0.1248(3) -0.1554(2) 0.0386(7) Uani 1 1 d . . .
H11 H 0.0532 -0.1835 -0.1235 0.046 Uiso 1 1 calc R . .
C12 C -0.0624(4) -0.1573(3) -0.2567(2) 0.0402(7) Uani 1 1 d . . .
H12 H -0.1262 -0.2395 -0.2925 0.048 Uiso 1 1 calc R . .
C13 C 0.0106(4) 0.0399(3) -0.2520(2) 0.0486(8) Uani 1 1 d . . .
H13 H -0.0013 0.0976 -0.2846 0.058 Uiso 1 1 calc R . .
C14 C 0.1224(4) 0.0816(3) -0.1496(2) 0.0453(8) Uani 1 1 d . . .
H14 H 0.1823 0.1650 -0.1143 0.054 Uiso 1 1 calc R . .
C15 C 0.2640(3) 0.0315(3) 0.0037(2) 0.0320(6) Uani 1 1 d . . .
C16 C 0.4557(3) 0.1478(3) 0.1470(2) 0.0336(7) Uani 1 1 d . . .
C17 C 0.6613(3) 0.2326(3) 0.3486(2) 0.0399(7) Uani 1 1 d . . .
H17A H 0.7120 0.1604 0.3120 0.048 Uiso 1 1 calc R . .
H17B H 0.7455 0.3003 0.4077 0.048 Uiso 1 1 calc R . .
C18 C 0.5287(3) 0.1939(3) 0.4089(2) 0.0344(7) Uani 1 1 d . . .
O8 O 0.3076(3) 0.4793(2) 0.4318(2) 0.0646(7) Uani 1 1 d . . .
H8' H 0.2359 0.4596 0.4684 0.097 Uiso 1 1 d R . .
H8" H 0.3834 0.4369 0.4186 0.097 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O7 1.987(2) . ?
Zn1 O5 2.0251(19) . ?
Zn1 O1 2.053(2) . ?
Zn1 N1 2.210(2) 2_667 ?
Zn1 N4 2.248(2) 2 ?
S1 C7 1.727(3) . ?
S1 C8 1.802(3) . ?
S2 C16 1.727(3) . ?
S2 C17 1.798(3) . ?
O1 C9 1.268(4) . ?
O2 C9 1.218(4) . ?
O3 C7 1.364(3) . ?
O3 C6 1.367(3) . ?
O4 C18 1.238(3) . ?
O5 C18 1.262(3) . ?
O6 C16 1.363(3) . ?
O6 C15 1.372(3) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8501 . ?
N1 C3 1.336(4) . ?
N1 C4 1.340(4) . ?
N1 Zn1 2.210(2) 2_667 ?
N2 C6 1.270(4) . ?
N2 N3 1.413(3) . ?
N3 C7 1.285(4) . ?
N4 C13 1.328(4) . ?
N4 C12 1.342(4) . ?
N4 Zn1 2.248(2) 2 ?
N5 C15 1.282(4) . ?
N5 N6 1.415(3) . ?
N6 C16 1.290(3) . ?
C1 C5 1.374(4) . ?
C1 C2 1.380(4) . ?
C1 C6 1.468(4) . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.375(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C8 C9 1.517(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 C14 1.373(4) . ?
C10 C11 1.389(4) . ?
C10 C15 1.459(4) . ?
C11 C12 1.370(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.382(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C17 C18 1.517(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
O8 H8' 0.8500 . ?
O8 H8" 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Zn1 O5 127.45(9) . . ?
O7 Zn1 O1 97.51(10) . . ?
O5 Zn1 O1 134.58(9) . . ?
O7 Zn1 N1 94.90(9) . 2_667 ?
O5 Zn1 N1 91.53(9) . 2_667 ?
O1 Zn1 N1 90.53(9) . 2_667 ?
O7 Zn1 N4 90.76(9) . 2 ?
O5 Zn1 N4 85.56(9) . 2 ?
O1 Zn1 N4 88.04(9) . 2 ?
N1 Zn1 N4 174.30(9) 2_667 2 ?
C7 S1 C8 97.59(14) . . ?
C16 S2 C17 97.67(14) . . ?
C9 O1 Zn1 111.1(2) . . ?
C7 O3 C6 101.7(2) . . ?
C18 O5 Zn1 108.04(18) . . ?
C16 O6 C15 102.0(2) . . ?
Zn1 O7 H7A 116.9 . . ?
Zn1 O7 H7B 126.1 . . ?
H7A O7 H7B 117.0 . . ?
C3 N1 C4 116.4(2) . . ?
C3 N1 Zn1 125.71(19) . 2_667 ?
C4 N1 Zn1 117.73(18) . 2_667 ?
C6 N2 N3 106.7(2) . . ?
C7 N3 N2 105.3(2) . . ?
C13 N4 C12 116.2(3) . . ?
C13 N4 Zn1 125.6(2) . 2 ?
C12 N4 Zn1 117.89(19) . 2 ?
C15 N5 N6 106.6(2) . . ?
C16 N6 N5 105.4(2) . . ?
C5 C1 C2 118.3(3) . . ?
C5 C1 C6 118.6(3) . . ?
C2 C1 C6 123.1(3) . . ?
C1 C2 C3 118.6(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
N1 C3 C2 123.9(3) . . ?
N1 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
N1 C4 C5 123.4(3) . . ?
N1 C4 H4 118.3 . . ?
C5 C4 H4 118.3 . . ?
C1 C5 C4 119.5(3) . . ?
C1 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
N2 C6 O3 113.0(2) . . ?
N2 C6 C1 127.5(3) . . ?
O3 C6 C1 119.5(3) . . ?
N3 C7 O3 113.2(3) . . ?
N3 C7 S1 129.1(2) . . ?
O3 C7 S1 117.7(2) . . ?
C9 C8 S1 112.8(2) . . ?
C9 C8 H8A 109.0 . . ?
S1 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
S1 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
O2 C9 O1 123.1(3) . . ?
O2 C9 C8 120.4(3) . . ?
O1 C9 C8 116.5(3) . . ?
C14 C10 C11 118.1(3) . . ?
C14 C10 C15 122.1(3) . . ?
C11 C10 C15 119.9(3) . . ?
C12 C11 C10 119.1(3) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N4 C12 C11 123.6(3) . . ?
N4 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
N4 C13 C14 124.4(3) . . ?
N4 C13 H13 117.8 . . ?
C14 C13 H13 117.8 . . ?
C10 C14 C13 118.6(3) . . ?
C10 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
N5 C15 O6 112.6(2) . . ?
N5 C15 C10 128.4(3) . . ?
O6 C15 C10 119.0(2) . . ?
N6 C16 O6 113.3(2) . . ?
N6 C16 S2 129.7(2) . . ?
O6 C16 S2 117.0(2) . . ?
C18 C17 S2 115.9(2) . . ?
C18 C17 H17A 108.3 . . ?
S2 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
S2 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
O4 C18 O5 123.6(3) . . ?
O4 C18 C17 117.8(3) . . ?
O5 C18 C17 118.6(3) . . ?
H8' O8 H8" 117.1 . . ?

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
O7 Zn1 O1 C9 170.86(19) . . . . ?
O5 Zn1 O1 C9 -16.8(2) . . . . ?
N1 Zn1 O1 C9 75.8(2) 2_667 . . . ?
N4 Zn1 O1 C9 -98.6(2) 2 . . . ?
O7 Zn1 O5 C18 -25.6(2) . . . . ?
O1 Zn1 O5 C18 163.98(16) . . . . ?
N1 Zn1 O5 C18 71.72(18) 2_667 . . . ?
N4 Zn1 O5 C18 -113.18(18) 2 . . . ?
C6 N2 N3 C7 -0.3(3) . . . . ?
C15 N5 N6 C16 0.3(3) . . . . ?
C5 C1 C2 C3 0.7(4) . . . . ?
C6 C1 C2 C3 -180.0(3) . . . . ?
C4 N1 C3 C2 -0.2(4) . . . . ?
Zn1 N1 C3 C2 -175.3(2) 2_667 . . . ?
C1 C2 C3 N1 -0.7(5) . . . . ?
C3 N1 C4 C5 1.0(4) . . . . ?
Zn1 N1 C4 C5 176.6(2) 2_667 . . . ?
C2 C1 C5 C4 0.1(4) . . . . ?
C6 C1 C5 C4 -179.2(3) . . . . ?
N1 C4 C5 C1 -1.0(5) . . . . ?
N3 N2 C6 O3 -0.2(3) . . . . ?
N3 N2 C6 C1 179.5(3) . . . . ?
C7 O3 C6 N2 0.5(3) . . . . ?
C7 O3 C6 C1 -179.1(2) . . . . ?
C5 C1 C6 N2 -7.6(5) . . . . ?
C2 C1 C6 N2 173.1(3) . . . . ?
C5 C1 C6 O3 172.0(2) . . . . ?
C2 C1 C6 O3 -7.3(4) . . . . ?
N2 N3 C7 O3 0.6(3) . . . . ?
N2 N3 C7 S1 -177.4(2) . . . . ?
C6 O3 C7 N3 -0.7(3) . . . . ?
C6 O3 C7 S1 177.59(19) . . . . ?
C8 S1 C7 N3 -7.1(3) . . . . ?
C8 S1 C7 O3 174.9(2) . . . . ?
C7 S1 C8 C9 -75.7(2) . . . . ?
Zn1 O1 C9 O2 11.4(4) . . . . ?
Zn1 O1 C9 C8 -169.40(18) . . . . ?
S1 C8 C9 O2 -37.9(4) . . . . ?
S1 C8 C9 O1 142.9(2) . . . . ?
C14 C10 C11 C12 2.4(4) . . . . ?
C15 C10 C11 C12 -177.2(2) . . . . ?
C13 N4 C12 C11 -1.0(4) . . . . ?
Zn1 N4 C12 C11 172.9(2) 2 . . . ?
C10 C11 C12 N4 -0.6(4) . . . . ?
C12 N4 C13 C14 1.0(5) . . . . ?
Zn1 N4 C13 C14 -172.4(2) 2 . . . ?
C11 C10 C14 C13 -2.5(4) . . . . ?
C15 C10 C14 C13 177.1(3) . . . . ?
N4 C13 C14 C10 0.8(5) . . . . ?
N6 N5 C15 O6 -0.1(3) . . . . ?
N6 N5 C15 C10 177.3(2) . . . . ?
C16 O6 C15 N5 -0.2(3) . . . . ?
C16 O6 C15 C10 -177.8(2) . . . . ?
C14 C10 C15 N5 -174.7(3) . . . . ?
C11 C10 C15 N5 4.8(4) . . . . ?
C14 C10 C15 O6 2.5(4) . . . . ?
C11 C10 C15 O6 -177.9(2) . . . . ?
N5 N6 C16 O6 -0.4(3) . . . . ?
N5 N6 C16 S2 179.9(2) . . . . ?
C15 O6 C16 N6 0.4(3) . . . . ?
C15 O6 C16 S2 -179.94(18) . . . . ?
C17 S2 C16 N6 -10.1(3) . . . . ?
C17 S2 C16 O6 170.23(19) . . . . ?
C16 S2 C17 C18 -60.2(2) . . . . ?
Zn1 O5 C18 O4 -6.4(3) . . . . ?
Zn1 O5 C18 C17 173.75(18) . . . . ?
S2 C17 C18 O4 153.9(2) . . . . ?
S2 C17 C18 O5 -26.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.059

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 680432'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 N6 O7 Pb S2'
_chemical_formula_weight         697.67

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'
Pb Pb -3.3944 10.1111 '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                   24.2121(19)
_cell_length_b                   11.5806(6)
_cell_length_c                   7.8686(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6520(10)
_cell_angle_gamma                90.00
_cell_volume                     2175.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2903
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      25.54

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    8.004
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.562048
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5743
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1900
_reflns_number_gt                1792
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0064P)²+1.2242P] 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         1900
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_ref         0.0367
_refine_ls_wR_factor_gt          0.0361
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Pb1 Pb 0.0000 0.098769(12) 0.7500 0.03104(7) Uani 1 2 d S . .
S1 S 0.11824(4) 0.40321(7) 0.46012(13) 0.0450(2) Uani 1 1 d . . .
O1 O 0.03711(11) 0.11466(18) 0.4420(3) 0.0508(6) Uani 1 1 d . . .
O2 O 0.02619(10) 0.26849(17) 0.5947(3) 0.0449(6) Uani 1 1 d . . .
O3 O 0.21335(9) 0.37210(17) 0.6763(3) 0.0368(5) Uani 1 1 d . . .
N1 N 0.17610(11) 0.2073(2) 0.5706(4) 0.0421(6) Uani 1 1 d . . .
N2 N 0.22667(11) 0.1837(2) 0.6843(3) 0.0415(6) Uani 1 1 d . . .
N3 N 0.39812(11) 0.3461(2) 1.0829(3) 0.0402(6) Uani 1 1 d . . .
C1 C 0.04398(12) 0.2188(2) 0.4734(4) 0.0325(7) Uani 1 1 d . . .
C2 C 0.07527(13) 0.2888(3) 0.3557(4) 0.0399(7) Uani 1 1 d . . .
H2A H 0.0481 0.3219 0.2641 0.048 Uiso 1 1 calc R . .
H2B H 0.0988 0.2368 0.3029 0.048 Uiso 1 1 calc R . .
C3 C 0.17068(12) 0.3184(3) 0.5719(4) 0.0347(7) Uani 1 1 d . . .
C4 C 0.24635(12) 0.2816(2) 0.7424(4) 0.0334(7) Uani 1 1 d . . .
C5 C 0.29797(12) 0.3044(3) 0.8623(4) 0.0332(7) Uani 1 1 d . . .
C6 C 0.33006(13) 0.2142(2) 0.9406(4) 0.0369(7) Uani 1 1 d . . .
H6 H 0.3185 0.1380 0.9210 0.044 Uiso 1 1 calc R . .
C7 C 0.37920(13) 0.2393(3) 1.0477(4) 0.0390(8) Uani 1 1 d . . .
H7 H 0.4007 0.1782 1.0990 0.047 Uiso 1 1 calc R . .
C8 C 0.36599(15) 0.4322(3) 1.0104(5) 0.0484(9) Uani 1 1 d . . .
H8 H 0.3779 0.5076 1.0355 0.058 Uiso 1 1 calc R . .
C9 C 0.31587(14) 0.4156(3) 0.9000(5) 0.0431(8) Uani 1 1 d . . .
H9 H 0.2947 0.4782 0.8523 0.052 Uiso 1 1 calc R . .
O4 O 0.0000 0.5196(3) 0.2500 0.0697(11) Uani 1 2 d S . .
H4' H 0.0129 0.5596 0.1751 0.105 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.453(2) 2_556 ?
Pb1 O2 2.453(2) . ?
Pb1 N3 2.671(3) 7_557 ?
Pb1 N3 2.671(3) 8_455 ?
Pb1 O1 2.729(2) 2_556 ?
Pb1 O1 2.729(2) . ?
S1 C3 1.725(3) . ?
S1 C2 1.796(3) . ?
O1 C1 1.236(3) . ?
O2 C1 1.251(3) . ?
O3 C3 1.358(4) . ?
O3 C4 1.367(3) . ?
N1 C3 1.294(4) . ?
N1 N2 1.417(4) . ?
N2 C4 1.284(4) . ?
N3 C7 1.331(4) . ?
N3 C8 1.333(4) . ?
N3 Pb1 2.671(3) 7_557 ?
C1 C2 1.525(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C5 1.458(4) . ?
C5 C9 1.375(4) . ?
C5 C6 1.384(4) . ?
C6 C7 1.369(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.383(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
O4 H4' 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O2 73.50(10) 2_556 . ?
O2 Pb1 N3 81.82(8) 2_556 7_557 ?
O2 Pb1 N3 76.07(8) . 7_557 ?
O2 Pb1 N3 76.07(8) 2_556 8_455 ?
O2 Pb1 N3 81.82(8) . 8_455 ?
N3 Pb1 N3 152.35(11) 7_557 8_455 ?
O2 Pb1 O1 49.65(6) 2_556 2_556 ?
O2 Pb1 O1 122.65(6) . 2_556 ?
N3 Pb1 O1 87.76(8) 7_557 2_556 ?
N3 Pb1 O1 90.39(8) 8_455 2_556 ?
O2 Pb1 O1 122.65(6) 2_556 . ?
O2 Pb1 O1 49.65(6) . . ?
N3 Pb1 O1 90.39(8) 7_557 . ?
N3 Pb1 O1 87.76(8) 8_455 . ?
O1 Pb1 O1 172.27(9) 2_556 . ?
C3 S1 C2 97.68(14) . . ?
C1 O1 Pb1 86.62(19) . . ?
C1 O2 Pb1 99.32(17) . . ?
C3 O3 C4 102.5(2) . . ?
C3 N1 N2 105.4(2) . . ?
C4 N2 N1 106.5(2) . . ?
C7 N3 C8 116.8(3) . . ?
C7 N3 Pb1 125.5(2) . 7_557 ?
C8 N3 Pb1 117.2(2) . 7_557 ?
O1 C1 O2 123.3(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 119.2(3) . . ?
C1 C2 S1 115.1(2) . . ?
C1 C2 H2A 108.5 . . ?
S1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
S1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N1 C3 O3 113.1(3) . . ?
N1 C3 S1 129.0(2) . . ?
O3 C3 S1 117.9(2) . . ?
N2 C4 O3 112.6(2) . . ?
N2 C4 C5 128.1(3) . . ?
O3 C4 C5 119.4(2) . . ?
C9 C5 C6 118.5(3) . . ?
C9 C5 C4 120.9(3) . . ?
C6 C5 C4 120.5(3) . . ?
C7 C6 C5 118.6(3) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N3 C7 C6 124.0(3) . . ?
N3 C7 H7 118.0 . . ?
C6 C7 H7 118.0 . . ?
N3 C8 C9 123.5(3) . . ?
N3 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C5 C9 C8 118.6(3) . . ?
C5 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Pb1 O1 C1 15.0(2) 2_556 . . . ?
O2 Pb1 O1 C1 5.70(17) . . . . ?
N3 Pb1 O1 C1 -65.54(19) 7_557 . . . ?
N3 Pb1 O1 C1 86.86(19) 8_455 . . . ?
O2 Pb1 O2 C1 -177.5(2) 2_556 . . . ?
N3 Pb1 O2 C1 97.01(19) 7_557 . . . ?
N3 Pb1 O2 C1 -99.73(19) 8_455 . . . ?
O1 Pb1 O2 C1 175.08(17) 2_556 . . . ?
O1 Pb1 O2 C1 -5.70(17) . . . . ?
C3 N1 N2 C4 0.2(3) . . . . ?
Pb1 O1 C1 O2 -10.2(3) . . . . ?
Pb1 O1 C1 C2 170.5(2) . . . . ?
Pb1 O2 C1 O1 11.5(3) . . . . ?
Pb1 O2 C1 C2 -169.2(2) . . . . ?
O1 C1 C2 S1 -145.7(3) . . . . ?
O2 C1 C2 S1 35.0(4) . . . . ?
C3 S1 C2 C1 72.4(2) . . . . ?
N2 N1 C3 O3 0.2(3) . . . . ?
N2 N1 C3 S1 179.6(2) . . . . ?
C4 O3 C3 N1 -0.5(3) . . . . ?
C4 O3 C3 S1 -180.0(2) . . . . ?
C2 S1 C3 N1 2.2(3) . . . . ?
C2 S1 C3 O3 -178.4(2) . . . . ?
N1 N2 C4 O3 -0.5(3) . . . . ?
N1 N2 C4 C5 -179.2(3) . . . . ?
C3 O3 C4 N2 0.6(3) . . . . ?
C3 O3 C4 C5 179.5(3) . . . . ?
N2 C4 C5 C9 174.0(3) . . . . ?
O3 C4 C5 C9 -4.7(4) . . . . ?
N2 C4 C5 C6 -6.0(5) . . . . ?
O3 C4 C5 C6 175.3(3) . . . . ?
C9 C5 C6 C7 -2.2(5) . . . . ?
C4 C5 C6 C7 177.8(3) . . . . ?
C8 N3 C7 C6 1.3(5) . . . . ?
Pb1 N3 C7 C6 -170.1(2) 7_557 . . . ?
C5 C6 C7 N3 0.6(5) . . . . ?
C7 N3 C8 C9 -1.6(5) . . . . ?
Pb1 N3 C8 C9 170.5(3) 7_557 . . . ?
C6 C5 C9 C8 2.0(5) . . . . ?
C4 C5 C9 C8 -178.0(3) . . . . ?
N3 C8 C9 C5 0.0(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.070

#===END

data_4
_database_code_depnum_ccdc_archive 'CCDC 680433'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Cu N6 O9 S2'
_chemical_formula_weight         590.04

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   7.4910(7)
_cell_length_b                   14.3672(13)
_cell_length_c                   22.775(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2451.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6832
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.55

_exptl_crystal_description       Needle
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1204
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.744531
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13336
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4303
_reflns_number_gt                4009
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0628P)²+0.9345P] 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_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_number_reflns         4303
_refine_ls_number_parameters     336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.49767(5) 0.50238(3) 0.083187(14) 0.03460(13) Uani 1 1 d . . .
S1 S -0.04172(11) 0.44365(6) 0.25232(3) 0.0396(2) Uani 1 1 d . . .
S2 S 1.05623(13) 0.55606(7) -0.07864(4) 0.0468(2) Uani 1 1 d . . .
O1 O 0.2610(3) 0.50583(18) 0.11859(9) 0.0414(5) Uani 1 1 d . . .
O2 O 0.2949(4) 0.39875(19) 0.18749(13) 0.0541(7) Uani 1 1 d . . .
O3 O 0.0452(3) 0.53335(15) 0.34846(8) 0.0352(5) Uani 1 1 d . . .
O4 O 0.7170(4) 0.5993(2) -0.01632(14) 0.0695(9) Uani 1 1 d . . .
O5 O 0.7421(3) 0.48808(19) 0.05153(9) 0.0452(6) Uani 1 1 d . . .
O6 O 0.9654(3) 0.47082(16) -0.17754(9) 0.0389(5) Uani 1 1 d . . .
O7 O 0.3761(4) 0.6199(2) 0.02146(13) 0.0651(8) Uani 1 1 d . . .
H7A H 0.3331 0.6605 0.0447 0.098 Uiso 1 1 d R . .
H7B H 0.4617 0.6370 -0.0005 0.098 Uiso 1 1 d R . .
N1 N 0.1448(4) 0.6055(2) 0.26969(11) 0.0439(7) Uani 1 1 d . . .
N2 N 0.1887(4) 0.6587(2) 0.31973(12) 0.0433(7) Uani 1 1 d . . .
N3 N 0.0850(4) 0.59656(18) 0.52591(10) 0.0315(6) Uani 1 1 d . . .
N4 N 0.8507(5) 0.4022(2) -0.09931(12) 0.0479(8) Uani 1 1 d . . .
N5 N 0.8045(5) 0.3509(2) -0.14926(13) 0.0480(8) Uani 1 1 d . . .
N6 N 0.9086(4) 0.40785(19) -0.35574(11) 0.0344(6) Uani 1 1 d . . .
C1 C 0.2078(4) 0.4572(2) 0.16137(13) 0.0332(7) Uani 1 1 d . . .
C2 C 0.0152(4) 0.4774(2) 0.17833(12) 0.0357(7) Uani 1 1 d . . .
H2A H -0.0632 0.4450 0.1513 0.043 Uiso 1 1 calc R . .
H2B H -0.0066 0.5436 0.1739 0.043 Uiso 1 1 calc R . .
C3 C 0.0605(4) 0.5343(2) 0.28870(13) 0.0340(7) Uani 1 1 d . . .
C4 C 0.1263(4) 0.6147(2) 0.36401(14) 0.0344(7) Uani 1 1 d . . .
C5 C 0.1348(4) 0.6400(2) 0.42627(13) 0.0323(7) Uani 1 1 d . . .
C6 C 0.0743(4) 0.5777(2) 0.46837(12) 0.0323(7) Uani 1 1 d . . .
H6 H 0.0250 0.5215 0.4563 0.039 Uiso 1 1 calc R . .
C7 C 0.1537(4) 0.6775(2) 0.54302(13) 0.0354(7) Uani 1 1 d . . .
H7 H 0.1615 0.6902 0.5830 0.042 Uiso 1 1 calc R . .
C8 C 0.2132(5) 0.7430(3) 0.50397(16) 0.0423(8) Uani 1 1 d . . .
H8 H 0.2596 0.7991 0.5175 0.051 Uiso 1 1 calc R . .
C9 C 0.2042(5) 0.7251(2) 0.44400(15) 0.0415(8) Uani 1 1 d . . .
H9 H 0.2434 0.7687 0.4167 0.050 Uiso 1 1 calc R . .
C10 C 0.8002(5) 0.5380(3) 0.01015(14) 0.0414(8) Uani 1 1 d . . .
C11 C 0.9929(4) 0.5161(3) -0.00639(13) 0.0445(8) Uani 1 1 d . . .
H11A H 1.0105 0.4492 -0.0044 0.053 Uiso 1 1 calc R . .
H11B H 1.0715 0.5445 0.0223 0.053 Uiso 1 1 calc R . .
C12 C 0.9458(5) 0.4703(2) -0.11804(13) 0.0380(8) Uani 1 1 d . . .
C13 C 0.8728(4) 0.3933(2) -0.19347(13) 0.0354(7) Uani 1 1 d . . .
C14 C 0.8589(4) 0.3680(2) -0.25494(13) 0.0345(7) Uani 1 1 d . . .
C15 C 0.9238(4) 0.4269(2) -0.29820(12) 0.0331(7) Uani 1 1 d . . .
H15 H 0.9800 0.4818 -0.2869 0.040 Uiso 1 1 calc R . .
C16 C 0.8260(5) 0.3288(3) -0.37130(15) 0.0437(8) Uani 1 1 d . . .
H16 H 0.8128 0.3155 -0.4110 0.052 Uiso 1 1 calc R . .
C17 C 0.7600(6) 0.2667(3) -0.33066(17) 0.0528(11) Uani 1 1 d . . .
H17 H 0.7043 0.2123 -0.3429 0.063 Uiso 1 1 calc R . .
C18 C 0.7772(5) 0.2860(3) -0.27170(16) 0.0456(9) Uani 1 1 d . . .
H18 H 0.7346 0.2445 -0.2437 0.055 Uiso 1 1 calc R . .
O8 O 0.6429(4) 0.3464(2) 0.17148(15) 0.0742(10) Uani 1 1 d . . .
H8A H 0.5376 0.3568 0.1838 0.111 Uiso 1 1 d R . .
H8B H 0.6877 0.2934 0.1792 0.111 Uiso 1 1 d R . .
O9 O 0.7166(13) 0.7478(4) 0.9143(2) 0.102(3) Uani 0.579(7) 1 d P A 1
H9A H 0.6532 0.7354 0.8843 0.153 Uiso 0.579(7) 1 d PR A 1
H9B H 0.8288 0.7408 0.9109 0.153 Uiso 0.579(7) 1 d PR A 1
O9' O 0.7314(11) 0.7429(6) 0.8476(5) 0.091(4) Uani 0.421(7) 1 d P A 2
H9C H 0.7373 0.7616 0.8123 0.136 Uiso 0.421(7) 1 d PR A 2
H9D H 0.6574 0.6995 0.8551 0.136 Uiso 0.421(7) 1 d PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.948(2) . ?
Cu1 O5 1.979(2) . ?
Cu1 N6 2.023(3) 2_665 ?
Cu1 N3 2.026(2) 2_564 ?
Cu1 O7 2.378(3) . ?
S1 C3 1.723(3) . ?
S1 C2 1.805(3) . ?
S2 C12 1.734(4) . ?
S2 C11 1.806(3) . ?
O1 C1 1.264(4) . ?
O2 C1 1.218(4) . ?
O3 C4 1.364(4) . ?
O3 C3 1.366(3) . ?
O4 C10 1.236(5) . ?
O5 C10 1.261(4) . ?
O6 C13 1.362(4) . ?
O6 C12 1.363(4) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8500 . ?
N1 C3 1.277(4) . ?
N1 N2 1.411(4) . ?
N2 C4 1.279(4) . ?
N3 C7 1.331(4) . ?
N3 C6 1.340(4) . ?
N3 Cu1 2.026(2) 2_565 ?
N4 C12 1.283(5) . ?
N4 N5 1.398(4) . ?
N5 C13 1.283(4) . ?
N6 C16 1.340(4) . ?
N6 C15 1.344(4) . ?
N6 Cu1 2.023(3) 2_664 ?
C1 C2 1.522(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C5 1.465(4) . ?
C5 C6 1.387(4) . ?
C5 C9 1.388(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.369(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.525(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.450(4) . ?
C14 C18 1.381(5) . ?
C14 C15 1.387(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.378(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
O8 H8A 0.8505 . ?
O8 H8B 0.8500 . ?
O9 H9A 0.8505 . ?
O9 H9B 0.8500 . ?
O9' H9A 1.0261 . ?
O9' H9C 0.8499 . ?
O9' H9D 0.8512 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O5 174.61(11) . . ?
O1 Cu1 N6 90.86(10) . 2_665 ?
O5 Cu1 N6 89.75(10) . 2_665 ?
O1 Cu1 N3 90.36(10) . 2_564 ?
O5 Cu1 N3 88.58(10) . 2_564 ?
N6 Cu1 N3 174.96(12) 2_665 2_564 ?
O1 Cu1 O7 83.00(10) . . ?
O5 Cu1 O7 102.28(11) . . ?
N6 Cu1 O7 94.97(11) 2_665 . ?
N3 Cu1 O7 90.03(10) 2_564 . ?
C3 S1 C2 98.09(14) . . ?
C12 S2 C11 96.90(16) . . ?
C1 O1 Cu1 126.3(2) . . ?
C4 O3 C3 102.3(2) . . ?
C10 O5 Cu1 122.2(2) . . ?
C13 O6 C12 101.9(2) . . ?
Cu1 O7 H7A 105.3 . . ?
Cu1 O7 H7B 105.3 . . ?
H7A O7 H7B 117.0 . . ?
C3 N1 N2 106.0(2) . . ?
C4 N2 N1 106.5(3) . . ?
C7 N3 C6 119.1(3) . . ?
C7 N3 Cu1 122.9(2) . 2_565 ?
C6 N3 Cu1 118.0(2) . 2_565 ?
C12 N4 N5 105.6(3) . . ?
C13 N5 N4 106.9(3) . . ?
C16 N6 C15 118.0(3) . . ?
C16 N6 Cu1 121.2(2) . 2_664 ?
C15 N6 Cu1 120.7(2) . 2_664 ?
O2 C1 O1 126.1(3) . . ?
O2 C1 C2 121.0(3) . . ?
O1 C1 C2 112.9(3) . . ?
C1 C2 S1 114.2(2) . . ?
C1 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N1 C3 O3 112.8(3) . . ?
N1 C3 S1 131.4(2) . . ?
O3 C3 S1 115.7(2) . . ?
N2 C4 O3 112.5(3) . . ?
N2 C4 C5 128.6(3) . . ?
O3 C4 C5 118.9(3) . . ?
C6 C5 C9 119.3(3) . . ?
C6 C5 C4 119.6(3) . . ?
C9 C5 C4 121.1(3) . . ?
N3 C6 C5 121.7(3) . . ?
N3 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
N3 C7 C8 122.4(3) . . ?
N3 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C5 C9 C8 117.8(3) . . ?
C5 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
O4 C10 O5 126.6(3) . . ?
O4 C10 C11 120.3(3) . . ?
O5 C10 C11 113.2(3) . . ?
C10 C11 S2 114.1(3) . . ?
C10 C11 H11A 108.7 . . ?
S2 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
S2 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N4 C12 O6 113.2(3) . . ?
N4 C12 S2 129.4(3) . . ?
O6 C12 S2 117.3(2) . . ?
N5 C13 O6 112.4(3) . . ?
N5 C13 C14 127.6(3) . . ?
O6 C13 C14 119.9(3) . . ?
C18 C14 C15 118.7(3) . . ?
C18 C14 C13 120.8(3) . . ?
C15 C14 C13 120.5(3) . . ?
N6 C15 C14 122.6(3) . . ?
N6 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
N6 C16 C17 122.5(3) . . ?
N6 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C18 C17 C16 119.4(4) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C14 118.8(3) . . ?
C17 C18 H18 120.6 . . ?
C14 C18 H18 120.6 . . ?
H8A O8 H8B 117.0 . . ?
H9A O9 H9B 117.0 . . ?
H9A O9' H9C 146.5 . . ?
H9A O9' H9D 52.4 . . ?
H9C O9' H9D 117.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Cu1 O1 C1 -84.5(3) 2_665 . . . ?
N3 Cu1 O1 C1 90.6(3) 2_564 . . . ?
O7 Cu1 O1 C1 -179.4(3) . . . . ?
N6 Cu1 O5 C10 -92.3(3) 2_665 . . . ?
N3 Cu1 O5 C10 92.5(3) 2_564 . . . ?
O7 Cu1 O5 C10 2.7(3) . . . . ?
C3 N1 N2 C4 -0.1(4) . . . . ?
C12 N4 N5 C13 -1.1(4) . . . . ?
Cu1 O1 C1 O2 -1.0(5) . . . . ?
Cu1 O1 C1 C2 179.75(19) . . . . ?
O2 C1 C2 S1 21.8(4) . . . . ?
O1 C1 C2 S1 -158.9(2) . . . . ?
C3 S1 C2 C1 76.4(3) . . . . ?
N2 N1 C3 O3 -1.1(4) . . . . ?
N2 N1 C3 S1 176.3(3) . . . . ?
C4 O3 C3 N1 1.7(4) . . . . ?
C4 O3 C3 S1 -176.0(2) . . . . ?
C2 S1 C3 N1 2.3(4) . . . . ?
C2 S1 C3 O3 179.6(2) . . . . ?
N1 N2 C4 O3 1.3(4) . . . . ?
N1 N2 C4 C5 -179.7(3) . . . . ?
C3 O3 C4 N2 -1.8(4) . . . . ?
C3 O3 C4 C5 179.1(3) . . . . ?
N2 C4 C5 C6 -173.5(4) . . . . ?
O3 C4 C5 C6 5.4(5) . . . . ?
N2 C4 C5 C9 5.8(6) . . . . ?
O3 C4 C5 C9 -175.3(3) . . . . ?
C7 N3 C6 C5 0.7(5) . . . . ?
Cu1 N3 C6 C5 -177.3(2) 2_565 . . . ?
C9 C5 C6 N3 -1.6(5) . . . . ?
C4 C5 C6 N3 177.7(3) . . . . ?
C6 N3 C7 C8 0.4(5) . . . . ?
Cu1 N3 C7 C8 178.3(3) 2_565 . . . ?
N3 C7 C8 C9 -0.6(6) . . . . ?
C6 C5 C9 C8 1.4(5) . . . . ?
C4 C5 C9 C8 -177.9(3) . . . . ?
C7 C8 C9 C5 -0.3(6) . . . . ?
Cu1 O5 C10 O4 -1.2(5) . . . . ?
Cu1 O5 C10 C11 179.0(2) . . . . ?
O4 C10 C11 S2 -19.3(5) . . . . ?
O5 C10 C11 S2 160.5(2) . . . . ?
C12 S2 C11 C10 -75.6(3) . . . . ?
N5 N4 C12 O6 1.3(4) . . . . ?
N5 N4 C12 S2 -175.9(3) . . . . ?
C13 O6 C12 N4 -1.0(4) . . . . ?
C13 O6 C12 S2 176.5(2) . . . . ?
C11 S2 C12 N4 0.3(4) . . . . ?
C11 S2 C12 O6 -176.8(3) . . . . ?
N4 N5 C13 O6 0.5(4) . . . . ?
N4 N5 C13 C14 -178.7(3) . . . . ?
C12 O6 C13 N5 0.2(4) . . . . ?
C12 O6 C13 C14 179.5(3) . . . . ?
N5 C13 C14 C18 -5.7(6) . . . . ?
O6 C13 C14 C18 175.1(3) . . . . ?
N5 C13 C14 C15 172.7(4) . . . . ?
O6 C13 C14 C15 -6.5(5) . . . . ?
C16 N6 C15 C14 0.5(5) . . . . ?
Cu1 N6 C15 C14 179.0(2) 2_664 . . . ?
C18 C14 C15 N6 0.7(5) . . . . ?
C13 C14 C15 N6 -177.8(3) . . . . ?
C15 N6 C16 C17 -1.2(5) . . . . ?
Cu1 N6 C16 C17 -179.6(3) 2_664 . . . ?
N6 C16 C17 C18 0.6(6) . . . . ?
C16 C17 C18 C14 0.7(6) . . . . ?
C15 C14 C18 C17 -1.3(5) . . . . ?
C13 C14 C18 C17 177.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.063

#===END

data_5
_database_code_depnum_ccdc_archive 'CCDC 680434'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 Cd N6 O6 S2'
_chemical_formula_weight         584.86

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           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                   4.7162(4)
_cell_length_b                   26.4099(19)
_cell_length_c                   8.1806(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.4840(10)
_cell_angle_gamma                90.00
_cell_volume                     981.95(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    4039
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.81

_exptl_crystal_description       Lamellar
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.692642
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5298
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1733
_reflns_number_gt                1631
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0180P)²+0.9783P] 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         1733
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0459
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 1.0000 1.0000 0.02570(8) Uani 1 2 d S . .
S1 S -0.06344(14) 0.66572(2) 0.64178(9) 0.03979(17) Uani 1 1 d . . .
O1 O -0.0028(4) 0.76437(5) 0.6669(2) 0.0352(4) Uani 1 1 d . . .
O2 O 0.3022(4) 0.53426(6) 0.6986(2) 0.0362(4) Uani 1 1 d . . .
O3 O -0.1551(4) 0.56321(6) 0.5943(2) 0.0415(4) Uani 1 1 d . . .
N1 N 0.2582(4) 0.93838(7) 0.8000(2) 0.0307(4) Uani 1 1 d . . .
N2 N 0.3984(6) 0.77778(8) 0.8715(3) 0.0554(7) Uani 1 1 d . . .
N3 N 0.3536(5) 0.72484(7) 0.8534(3) 0.0500(6) Uani 1 1 d . . .
C1 C 0.1250(5) 0.85229(8) 0.7254(3) 0.0311(5) Uani 1 1 d . . .
C2 C 0.3010(5) 0.88868(8) 0.8255(3) 0.0327(5) Uani 1 1 d . . .
H2 H 0.4565 0.8780 0.9148 0.039 Uiso 1 1 calc R . .
C3 C 0.0389(6) 0.95262(8) 0.6682(3) 0.0347(5) Uani 1 1 d . . .
H3 H 0.0097 0.9871 0.6469 0.042 Uiso 1 1 calc R . .
C4 C -0.1465(6) 0.91927(9) 0.5621(3) 0.0407(6) Uani 1 1 d . . .
H4 H -0.2967 0.9311 0.4718 0.049 Uiso 1 1 calc R . .
C5 C -0.1061(6) 0.86772(9) 0.5917(3) 0.0377(6) Uani 1 1 d . . .
H5 H -0.2306 0.8442 0.5237 0.045 Uiso 1 1 calc R . .
C6 C 0.1873(5) 0.79844(8) 0.7614(3) 0.0339(5) Uani 1 1 d . . .
C7 C 0.1181(5) 0.71972(8) 0.7324(3) 0.0334(5) Uani 1 1 d . . .
C8 C 0.2127(5) 0.62017(8) 0.7401(3) 0.0312(5) Uani 1 1 d . . .
H8A H 0.3980 0.6285 0.7163 0.037 Uiso 1 1 calc R . .
H8B H 0.2422 0.6205 0.8621 0.037 Uiso 1 1 calc R . .
C9 C 0.1105(5) 0.56805(8) 0.6699(3) 0.0283(5) 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
Cd1 O2 2.2667(16) 4_576 ?
Cd1 O2 2.2667(16) 2_656 ?
Cd1 O3 2.3146(16) 4_676 ?
Cd1 O3 2.3146(16) 2_556 ?
Cd1 N1 2.3726(18) . ?
Cd1 N1 2.3726(18) 3_677 ?
S1 C7 1.726(2) . ?
S1 C8 1.798(2) . ?
O1 C7 1.356(3) . ?
O1 C6 1.357(3) . ?
O2 C9 1.247(3) . ?
O2 Cd1 2.2667(16) 2_646 ?
O3 C9 1.247(3) . ?
O3 Cd1 2.3146(15) 2_546 ?
N1 C3 1.333(3) . ?
N1 C2 1.336(3) . ?
N2 C6 1.273(3) . ?
N2 N3 1.416(3) . ?
N3 C7 1.283(3) . ?
C1 C5 1.383(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.466(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C8 C9 1.520(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O2 180.00(7) 4_576 2_656 ?
O2 Cd1 O3 81.96(7) 4_576 4_676 ?
O2 Cd1 O3 98.04(7) 2_656 4_676 ?
O2 Cd1 O3 98.04(7) 4_576 2_556 ?
O2 Cd1 O3 81.96(7) 2_656 2_556 ?
O3 Cd1 O3 180.000(1) 4_676 2_556 ?
O2 Cd1 N1 90.37(6) 4_576 . ?
O2 Cd1 N1 89.63(6) 2_656 . ?
O3 Cd1 N1 84.31(6) 4_676 . ?
O3 Cd1 N1 95.69(6) 2_556 . ?
O2 Cd1 N1 89.63(6) 4_576 3_677 ?
O2 Cd1 N1 90.37(6) 2_656 3_677 ?
O3 Cd1 N1 95.69(6) 4_676 3_677 ?
O3 Cd1 N1 84.31(6) 2_556 3_677 ?
N1 Cd1 N1 180.00(6) . 3_677 ?
C7 S1 C8 98.26(11) . . ?
C7 O1 C6 101.97(18) . . ?
C9 O2 Cd1 124.54(15) . 2_646 ?
C9 O3 Cd1 139.72(15) . 2_546 ?
C3 N1 C2 117.10(19) . . ?
C3 N1 Cd1 119.36(14) . . ?
C2 N1 Cd1 122.78(15) . . ?
C6 N2 N3 106.4(2) . . ?
C7 N3 N2 105.0(2) . . ?
C5 C1 C2 118.9(2) . . ?
C5 C1 C6 121.2(2) . . ?
C2 C1 C6 119.9(2) . . ?
N1 C2 C1 123.2(2) . . ?
N1 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
N1 C3 C4 123.7(2) . . ?
N1 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C3 C4 C5 119.0(2) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C1 C5 C4 118.0(2) . . ?
C1 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
N2 C6 O1 113.1(2) . . ?
N2 C6 C1 129.4(2) . . ?
O1 C6 C1 117.5(2) . . ?
N3 C7 O1 113.53(19) . . ?
N3 C7 S1 130.31(18) . . ?
O1 C7 S1 116.16(17) . . ?
C9 C8 S1 108.54(15) . . ?
C9 C8 H8A 110.0 . . ?
S1 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
S1 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O3 C9 O2 127.0(2) . . ?
O3 C9 C8 117.1(2) . . ?
O2 C9 C8 115.9(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
O2 Cd1 N1 C3 110.83(19) 4_576 . . . ?
O2 Cd1 N1 C3 -69.17(19) 2_656 . . . ?
O3 Cd1 N1 C3 -167.28(19) 4_676 . . . ?
O3 Cd1 N1 C3 12.72(19) 2_556 . . . ?
O2 Cd1 N1 C2 -58.93(19) 4_576 . . . ?
O2 Cd1 N1 C2 121.07(19) 2_656 . . . ?
O3 Cd1 N1 C2 22.95(19) 4_676 . . . ?
O3 Cd1 N1 C2 -157.05(19) 2_556 . . . ?
C6 N2 N3 C7 0.3(3) . . . . ?
C3 N1 C2 C1 -1.8(4) . . . . ?
Cd1 N1 C2 C1 168.14(19) . . . . ?
C5 C1 C2 N1 0.3(4) . . . . ?
C6 C1 C2 N1 179.8(2) . . . . ?
C2 N1 C3 C4 1.7(4) . . . . ?
Cd1 N1 C3 C4 -168.6(2) . . . . ?
N1 C3 C4 C5 -0.1(4) . . . . ?
C2 C1 C5 C4 1.3(4) . . . . ?
C6 C1 C5 C4 -178.1(3) . . . . ?
C3 C4 C5 C1 -1.4(4) . . . . ?
N3 N2 C6 O1 -0.1(3) . . . . ?
N3 N2 C6 C1 179.7(3) . . . . ?
C7 O1 C6 N2 -0.1(3) . . . . ?
C7 O1 C6 C1 -179.9(2) . . . . ?
C5 C1 C6 N2 175.4(3) . . . . ?
C2 C1 C6 N2 -4.0(5) . . . . ?
C5 C1 C6 O1 -4.9(4) . . . . ?
C2 C1 C6 O1 175.7(2) . . . . ?
N2 N3 C7 O1 -0.4(3) . . . . ?
N2 N3 C7 S1 179.3(2) . . . . ?
C6 O1 C7 N3 0.3(3) . . . . ?
C6 O1 C7 S1 -179.44(18) . . . . ?
C8 S1 C7 N3 -10.3(3) . . . . ?
C8 S1 C7 O1 169.45(19) . . . . ?
C7 S1 C8 C9 -176.32(17) . . . . ?
Cd1 O3 C9 O2 13.0(4) 2_546 . . . ?
Cd1 O3 C9 C8 -164.83(18) 2_546 . . . ?
Cd1 O2 C9 O3 73.6(3) 2_646 . . . ?
Cd1 O2 C9 C8 -108.5(2) 2_646 . . . ?
S1 C8 C9 O3 -16.2(3) . . . . ?
S1 C8 C9 O2 165.66(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.047

#===END

