# Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Hegen Zheng'
_publ_contact_author_email       ZHENGHG@NJU.EDU.CN

_publ_section_title              
;
Syntheses, structures, photoluminescence and magnetic
properties of five Compounds with 1,3,5-benzenetricarboxylate acid and
imidazole ligands
;
loop_
_publ_author_name
'Hegen Zheng'
'Jiao Xu'
'Stuart Batten'
'Zi-Jian Guo'
'Yi-Zhi Li'
'Zhao-Rui Pan'
'Tianwei Wang'

# Attachment '1.cif'

data_yy
_database_code_depnum_ccdc_archive 'CCDC 742383'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H20 N4 O7 Zn'
_chemical_formula_weight         529.80

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

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

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

_cell_length_a                   7.8282(13)
_cell_length_b                   16.447(3)
_cell_length_c                   16.779(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.137(3)
_cell_angle_gamma                90.00
_cell_volume                     2151.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_T_max  0.885
_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  '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            11417
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4217
_reflns_number_gt                2775
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0285P)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         4217
_refine_ls_number_parameters     313
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.007
_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 0.1555(6) 0.8606(2) 1.0570(2) 0.0257(10) Uani 1 1 d . . .
C2 C 0.1910(6) 0.8201(3) 0.9879(2) 0.0306(11) Uani 1 1 d . . .
H2 H 0.2948 0.7929 0.9865 0.037 Uiso 1 1 calc R . .
C3 C 0.0726(6) 0.8195(2) 0.9203(2) 0.0266(10) Uani 1 1 d . . .
C4 C -0.0790(5) 0.8611(2) 0.9228(2) 0.0292(11) Uani 1 1 d . . .
H4 H -0.1576 0.8618 0.8778 0.035 Uiso 1 1 calc RD . .
C5 C -0.1168(6) 0.9023(2) 0.9914(2) 0.0250(10) Uani 1 1 d . . .
C6 C 0.0030(6) 0.9019(2) 1.0577(2) 0.0268(10) Uani 1 1 d . . .
H6 H -0.0204 0.9302 1.1035 0.032 Uiso 1 1 calc R . .
C7 C 0.1109(7) 0.7698(3) 0.8487(3) 0.0333(12) Uani 1 1 d . . .
C8 C -0.2824(6) 0.9444(3) 0.9933(3) 0.0322(11) Uani 1 1 d . . .
C9 C 0.2837(6) 0.8582(3) 1.1302(3) 0.0301(11) Uani 1 1 d . . .
C10 C 0.9298(6) 0.7226(3) 1.1809(3) 0.0328(11) Uani 1 1 d . . .
H10 H 0.9854 0.7310 1.2315 0.039 Uiso 1 1 calc R . .
C11 C 0.9952(6) 0.6819(3) 1.1214(3) 0.0390(12) Uani 1 1 d . . .
H11 H 1.1025 0.6573 1.1231 0.047 Uiso 1 1 calc R . .
C12 C 0.7411(6) 0.7258(2) 1.0812(3) 0.0311(11) Uani 1 1 d . . .
H12 H 0.6417 0.7367 1.0483 0.037 Uiso 1 1 calc R . .
C13 C 0.8860(6) 0.6475(3) 0.9785(3) 0.0392(12) Uani 1 1 d . . .
H13A H 1.0062 0.6391 0.9710 0.047 Uiso 1 1 calc R . .
H13B H 0.8408 0.6861 0.9382 0.047 Uiso 1 1 calc R . .
C14 C 0.7925(6) 0.5679(3) 0.9648(3) 0.0289(11) Uani 1 1 d . . .
C15 C 0.7704(6) 0.5124(3) 1.0245(3) 0.0371(12) Uani 1 1 d . . .
H15 H 0.8123 0.5242 1.0768 0.045 Uiso 1 1 calc R . .
C16 C 0.6881(6) 0.4402(3) 1.0081(3) 0.0391(13) Uani 1 1 d . . .
H16 H 0.6736 0.4035 1.0491 0.047 Uiso 1 1 calc R . .
C17 C 0.6265(6) 0.4223(3) 0.9304(3) 0.0348(12) Uani 1 1 d . . .
H17 H 0.5711 0.3731 0.9191 0.042 Uiso 1 1 calc R . .
C18 C 0.6465(6) 0.4767(3) 0.8693(3) 0.0291(11) Uani 1 1 d . . .
C19 C 0.7308(6) 0.5488(3) 0.8871(3) 0.0319(11) Uani 1 1 d . . .
H19 H 0.7467 0.5854 0.8462 0.038 Uiso 1 1 calc R . .
C20 C 0.5746(6) 0.4595(3) 0.7839(3) 0.0341(12) Uani 1 1 d . . .
H30A H 0.6498 0.4832 0.7473 0.041 Uiso 1 1 calc R . .
H30B H 0.5723 0.4012 0.7752 0.041 Uiso 1 1 calc R . .
C21 C 0.3602(6) 0.5704(3) 0.7609(2) 0.0341(12) Uani 1 1 d . . .
H58 H 0.4392 0.6126 0.7678 0.041 Uiso 1 1 calc R . .
C22 C 0.2533(6) 0.4502(3) 0.7529(3) 0.0385(12) Uani 1 1 d . . .
H59 H 0.2417 0.3939 0.7527 0.046 Uiso 1 1 calc R . .
C23 C 0.1265(6) 0.5045(3) 0.7401(3) 0.0348(12) Uani 1 1 d . . .
H60 H 0.0108 0.4919 0.7297 0.042 Uiso 1 1 calc R . .
N1 N 0.7677(4) 0.7503(2) 1.1557(2) 0.0261(8) Uani 1 1 d . . .
N2 N 0.8734(5) 0.6836(2) 1.0581(2) 0.0344(9) Uani 1 1 d . . .
N3 N 0.4011(5) 0.4922(2) 0.76625(19) 0.0291(9) Uani 1 1 d . . .
N4 N 0.1928(5) 0.5810(2) 0.7446(2) 0.0305(9) Uani 1 1 d . . .
O1 O 0.4178(4) 0.81661(19) 1.12195(16) 0.0389(8) Uani 1 1 d . . .
O2 O 0.2530(4) 0.89457(19) 1.19056(17) 0.0459(9) Uani 1 1 d . . .
O3 O 0.2532(4) 0.7368(2) 0.84704(18) 0.0509(10) Uani 1 1 d . . .
O4 O -0.0070(4) 0.76224(18) 0.79242(17) 0.0395(8) Uani 1 1 d . . .
O5 O -0.3957(4) 0.9406(2) 0.93691(19) 0.0507(10) Uani 1 1 d . . .
O6 O -0.3014(4) 0.98434(19) 1.05823(18) 0.0480(9) Uani 1 1 d D . .
H6A H -0.3997 1.0067 1.0544 0.072 Uiso 1 1 d RD . .
O7 O 0.56823(7) 0.75974(3) 0.89866(3) 0.207(3) Uani 1 1 d . . .
H7D H 0.4639 0.7515 0.8820 0.248 Uiso 1 1 d R . .
H7B H 0.6023 0.8039 0.8790 0.310 Uiso 1 1 d R . .
Zn1 Zn 0.58903(7) 0.81157(3) 1.21380(3) 0.02788(16) Uani 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
C1 C6 1.375(5) . ?
C1 C2 1.386(5) . ?
C1 C9 1.516(6) . ?
C2 C3 1.398(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.374(5) . ?
C3 C7 1.505(6) . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(5) . ?
C5 C8 1.473(6) . ?
C6 H6 0.9300 . ?
C7 O3 1.242(5) . ?
C7 O4 1.267(5) . ?
C8 O5 1.239(5) . ?
C8 O6 1.293(5) . ?
C9 O2 1.218(5) . ?
C9 O1 1.271(5) . ?
C10 C11 1.341(6) . ?
C10 N1 1.378(5) . ?
C10 H10 0.9300 . ?
C11 N2 1.363(5) . ?
C11 H11 0.9300 . ?
C12 N1 1.312(5) . ?
C12 N2 1.332(5) . ?
C12 H12 0.9300 . ?
C13 N2 1.474(5) . ?
C13 C14 1.508(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.378(6) . ?
C14 C19 1.384(5) . ?
C15 C16 1.366(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(6) . ?
C18 C20 1.518(6) . ?
C19 H19 0.9300 . ?
C20 N3 1.467(5) . ?
C20 H30A 0.9700 . ?
C20 H30B 0.9700 . ?
C21 N3 1.326(5) . ?
C21 N4 1.326(5) . ?
C21 H58 0.9300 . ?
C22 C23 1.339(6) . ?
C22 N3 1.349(5) . ?
C22 H59 0.9300 . ?
C23 N4 1.361(5) . ?
C23 H60 0.9300 . ?
N1 Zn1 2.041(3) . ?
N4 Zn1 1.993(3) 4_575 ?
O1 Zn1 1.952(3) . ?
O4 Zn1 1.989(3) 4_575 ?
O6 H6A 0.8501 . ?
O7 H7D 0.8501 . ?
O7 H7B 0.8500 . ?
Zn1 O4 1.989(3) 4_676 ?
Zn1 N4 1.993(4) 4_676 ?

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
C6 C1 C2 119.0(4) . . ?
C6 C1 C9 121.2(4) . . ?
C2 C1 C9 119.9(4) . . ?
C1 C2 C3 120.9(4) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 118.9(4) . . ?
C4 C3 C7 121.9(4) . . ?
C2 C3 C7 119.1(4) . . ?
C3 C4 C5 121.1(4) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 118.9(4) . . ?
C6 C5 C8 121.2(4) . . ?
C4 C5 C8 120.0(4) . . ?
C1 C6 C5 121.3(4) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
O3 C7 O4 122.4(4) . . ?
O3 C7 C3 119.9(4) . . ?
O4 C7 C3 117.7(4) . . ?
O5 C8 O6 122.8(4) . . ?
O5 C8 C5 122.1(4) . . ?
O6 C8 C5 115.1(4) . . ?
O2 C9 O1 125.6(4) . . ?
O2 C9 C1 119.7(4) . . ?
O1 C9 C1 114.7(4) . . ?
C11 C10 N1 109.9(4) . . ?
C11 C10 H10 125.1 . . ?
N1 C10 H10 125.1 . . ?
C10 C11 N2 106.4(4) . . ?
C10 C11 H11 126.8 . . ?
N2 C11 H11 126.8 . . ?
N1 C12 N2 112.1(4) . . ?
N1 C12 H12 124.0 . . ?
N2 C12 H12 124.0 . . ?
N2 C13 C14 114.6(4) . . ?
N2 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
N2 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C15 C14 C19 118.5(4) . . ?
C15 C14 C13 123.8(4) . . ?
C19 C14 C13 117.7(4) . . ?
C16 C15 C14 121.2(4) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 119.6(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.6(4) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C18 C17 118.7(4) . . ?
C19 C18 C20 119.7(4) . . ?
C17 C18 C20 121.5(4) . . ?
C18 C19 C14 121.4(4) . . ?
C18 C19 H19 119.3 . . ?
C14 C19 H19 119.3 . . ?
N3 C20 C18 112.3(4) . . ?
N3 C20 H30A 109.1 . . ?
C18 C20 H30A 109.1 . . ?
N3 C20 H30B 109.1 . . ?
C18 C20 H30B 109.1 . . ?
H30A C20 H30B 107.9 . . ?
N3 C21 N4 111.7(4) . . ?
N3 C21 H58 124.1 . . ?
N4 C21 H58 124.1 . . ?
C23 C22 N3 107.3(4) . . ?
C23 C22 H59 126.3 . . ?
N3 C22 H59 126.3 . . ?
C22 C23 N4 109.5(4) . . ?
C22 C23 H60 125.2 . . ?
N4 C23 H60 125.2 . . ?
C12 N1 C10 104.7(4) . . ?
C12 N1 Zn1 123.4(3) . . ?
C10 N1 Zn1 131.9(3) . . ?
C12 N2 C11 107.0(4) . . ?
C12 N2 C13 126.2(4) . . ?
C11 N2 C13 126.8(4) . . ?
C21 N3 C22 106.7(4) . . ?
C21 N3 C20 125.7(4) . . ?
C22 N3 C20 127.6(4) . . ?
C21 N4 C23 104.7(4) . . ?
C21 N4 Zn1 122.9(3) . 4_575 ?
C23 N4 Zn1 131.3(3) . 4_575 ?
C9 O1 Zn1 116.9(3) . . ?
C7 O4 Zn1 105.1(3) . 4_575 ?
C8 O6 H6A 109.1 . . ?
H7D O7 H7B 109.5 . . ?
O1 Zn1 O4 106.01(13) . 4_676 ?
O1 Zn1 N4 113.73(14) . 4_676 ?
O4 Zn1 N4 122.56(13) 4_676 4_676 ?
O1 Zn1 N1 95.47(13) . . ?
O4 Zn1 N1 109.33(13) 4_676 . ?
N4 Zn1 N1 106.33(15) 4_676 . ?

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
O7 H7D O3 0.85 1.72 2.568(3) 178.8 .
O6 H6A O5 0.85 1.84 2.681(5) 170.8 3_477
O7 H7B O5 0.85 2.45 3.050(3) 128.4 1_655

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.079

# Attachment '2.cif'

data_80927bm
_database_code_depnum_ccdc_archive 'CCDC 742384'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H21 N6 O10 Zn2'
_chemical_formula_weight         684.21

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                   10.666(2)
_cell_length_b                   16.748(3)
_cell_length_c                   14.201(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.299(4)
_cell_angle_gamma                90.00
_cell_volume                     2525.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'block '
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  '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            13481
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.99
_reflns_number_total             4933
_reflns_number_gt                3419
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0807P)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         4933
_refine_ls_number_parameters     370
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1613
_refine_ls_wR_factor_gt          0.1541
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.9659(5) 0.2299(3) 0.6563(4) 0.0237(12) Uani 1 1 d . . .
C2 C 1.0779(5) 0.1896(3) 0.6796(4) 0.0266(13) Uani 1 1 d . . .
H2 H 1.0768 0.1343 0.6856 0.032 Uiso 1 1 calc R . .
C3 C 1.1899(5) 0.2294(3) 0.6941(4) 0.0235(12) Uani 1 1 d . . .
C4 C 1.1921(5) 0.3103(3) 0.6881(4) 0.0283(13) Uani 1 1 d . . .
H4 H 1.2683 0.3373 0.6991 0.034 Uiso 1 1 calc R . .
C5 C 1.0804(5) 0.3538(3) 0.6653(4) 0.0260(13) Uani 1 1 d . . .
C6 C 0.9683(5) 0.3126(3) 0.6492(4) 0.0258(13) Uani 1 1 d . . .
H6 H 0.8938 0.3404 0.6336 0.031 Uiso 1 1 calc R . .
C7 C 0.8437(6) 0.1865(3) 0.6415(4) 0.0293(13) Uani 1 1 d . . .
C8 C 1.0830(6) 0.4433(3) 0.6655(4) 0.0321(14) Uani 1 1 d . . .
C9 C 0.9611(5) 0.6552(3) 0.6018(4) 0.0284(13) Uani 1 1 d . . .
H9 H 0.9208 0.6062 0.6057 0.034 Uiso 1 1 calc R . .
C10 C 0.9938(5) 0.7830(3) 0.5792(4) 0.0316(14) Uani 1 1 d . . .
H10 H 0.9821 0.8369 0.5652 0.038 Uiso 1 1 calc RD . .
C11 C 1.1031(6) 0.7476(3) 0.6061(4) 0.0342(14) Uani 1 1 d . . .
H11 H 1.1809 0.7730 0.6143 0.041 Uiso 1 1 calc R . .
C12 C 0.7150(5) 0.8087(3) 0.5723(4) 0.0260(13) Uani 1 1 d . . .
H12 H 0.7640 0.8515 0.5955 0.031 Uiso 1 1 calc R . .
C13 C 0.7698(5) 0.7361(3) 0.5553(4) 0.0238(12) Uani 1 1 d . . .
C14 C 0.6965(5) 0.6720(3) 0.5194(4) 0.0263(13) Uani 1 1 d . . .
H14 H 0.7332 0.6228 0.5092 0.032 Uiso 1 1 calc R . .
C15 C 0.5689(5) 0.6830(3) 0.4995(4) 0.0250(12) Uani 1 1 d . . .
C16 C 0.5119(5) 0.7537(3) 0.5178(4) 0.0261(13) Uani 1 1 d . . .
H16 H 0.4252 0.7596 0.5060 0.031 Uiso 1 1 calc R . .
C17 C 0.5863(5) 0.8166(3) 0.5543(4) 0.0238(12) Uani 1 1 d . . .
C18 C 0.5379(5) 0.5600(3) 0.4039(4) 0.0256(12) Uani 1 1 d . . .
H18 H 0.6222 0.5532 0.3938 0.031 Uiso 1 1 calc R . .
C19 C 0.3394(6) 0.5437(3) 0.3998(4) 0.0323(14) Uani 1 1 d . . .
H19 H 0.2590 0.5230 0.3855 0.039 Uiso 1 1 calc R . .
C20 C 0.3676(5) 0.6085(3) 0.4544(4) 0.0311(14) Uani 1 1 d . . .
H20 H 0.3114 0.6398 0.4847 0.037 Uiso 1 1 calc R . .
C21 C 0.4119(6) 0.9165(3) 0.5382(4) 0.0329(14) Uani 1 1 d . . .
H21 H 0.3606 0.8937 0.4889 0.039 Uiso 1 1 calc R . .
C22 C 0.3889(6) 0.9829(3) 0.5859(4) 0.0354(15) Uani 1 1 d . . .
H22 H 0.3175 1.0146 0.5743 0.043 Uiso 1 1 calc R . .
C23 C 0.5666(6) 0.9396(3) 0.6466(4) 0.0301(13) Uani 1 1 d . . .
H23 H 0.6420 0.9342 0.6846 0.036 Uiso 1 1 calc R . .
C24 C 1.3112(6) 0.1868(4) 0.7188(4) 0.0376(16) Uani 1 1 d . . .
N1 N 1.0825(4) 0.6664(3) 0.6202(3) 0.0290(11) Uani 1 1 d . . .
N2 N 0.9014(4) 0.7254(3) 0.5760(3) 0.0245(10) Uani 1 1 d . . .
N3 N 0.4948(4) 0.6192(3) 0.4564(3) 0.0237(10) Uani 1 1 d . . .
N4 N 0.4475(4) 0.5132(3) 0.3689(3) 0.0279(11) Uani 1 1 d . . .
N5 N 0.5266(4) 0.8887(3) 0.5766(3) 0.0262(11) Uani 1 1 d . . .
N6 N 0.4854(4) 0.9980(3) 0.6544(3) 0.0306(11) Uani 1 1 d . . .
O1 O 0.8421(4) 0.1129(2) 0.6710(3) 0.0318(10) Uani 1 1 d . . .
O2 O 0.7507(4) 0.2202(3) 0.6028(4) 0.0511(13) Uani 1 1 d . . .
O3 O 1.3044(4) 0.1141(2) 0.7446(3) 0.0430(11) Uani 1 1 d . . .
O4 O 1.4116(5) 0.2219(3) 0.7146(4) 0.0708(17) Uani 1 1 d . . .
O5 O 0.9830(4) 0.4816(3) 0.6549(4) 0.0606(15) Uani 1 1 d . . .
O6 O 1.1924(4) 0.4760(2) 0.6779(3) 0.0381(11) Uani 1 1 d . . .
O7 O 1.3699(3) 0.6228(2) 0.6875(3) 0.0305(9) Uani 1 1 d . . .
O8 O 0.3708(4) 0.8002(2) 0.7375(3) 0.0762(17) Uani 1 1 d . . .
H8A H 0.4150 0.7859 0.7876 0.114 Uiso 1 1 d R . .
H8C H 0.3772 0.7655 0.6946 0.114 Uiso 1 1 d R . .
O9 O 0.9013(4) 0.9769(2) 0.5658(3) 0.138(4) Uani 1 1 d R . .
H9A H 0.9413 1.0089 0.6041 0.207 Uiso 1 1 d RD . .
H9C H 0.8947 0.9971 0.5106 0.207 Uiso 1 1 d R . .
O10 O 0.1538(7) 0.9368(3) 0.6855(5) 0.138 Uani 1 1 d . . .
H10A H 0.0944 0.9277 0.6427 0.207 Uiso 1 1 d R . .
H10C H 0.1335 0.9754 0.7197 0.207 Uiso 1 1 d R . .
Zn1 Zn 1.19736(6) 0.59110(4) 0.69710(5) 0.0283(2) Uani 1 1 d . . .
Zn2 Zn 1.52572(6) 0.56977(4) 0.73184(5) 0.0252(2) 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
C1 C2 1.385(7) . ?
C1 C6 1.389(7) . ?
C1 C7 1.491(8) . ?
C2 C3 1.366(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.358(7) . ?
C3 C24 1.490(8) . ?
C4 C5 1.409(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(7) . ?
C5 C8 1.498(7) . ?
C6 H6 0.9300 . ?
C7 O2 1.226(7) . ?
C7 O1 1.302(6) . ?
C8 O5 1.243(7) . ?
C8 O6 1.286(7) . ?
C9 N1 1.311(7) . ?
C9 N2 1.370(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.332(8) . ?
C10 N2 1.377(7) . ?
C10 H10 0.9300 . ?
C11 N1 1.395(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(7) . ?
C12 C17 1.379(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.396(7) . ?
C13 N2 1.419(7) . ?
C14 C15 1.377(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.366(7) . ?
C15 N3 1.433(7) . ?
C16 C17 1.391(7) . ?
C16 H16 0.9300 . ?
C17 N5 1.414(6) . ?
C18 N4 1.305(7) . ?
C18 N3 1.347(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.352(8) . ?
C19 N4 1.369(7) . ?
C19 H19 0.9300 . ?
C20 N3 1.366(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.337(8) . ?
C21 N5 1.374(7) . ?
C21 H21 0.9300 . ?
C22 N6 1.373(7) . ?
C22 H22 0.9300 . ?
C23 N6 1.317(7) . ?
C23 N5 1.349(7) . ?
C23 H23 0.9300 . ?
C24 O4 1.229(8) . ?
C24 O3 1.275(7) . ?
N1 Zn1 2.009(5) . ?
N4 Zn2 2.033(4) 3_766 ?
N6 Zn2 2.026(5) 2_756 ?
O1 Zn1 1.992(4) 2_746 ?
O3 Zn2 1.958(4) 2_846 ?
O6 Zn1 1.946(4) . ?
O7 Zn1 1.932(4) . ?
O7 Zn2 1.938(4) . ?
O8 H8A 0.8507 . ?
O8 H8C 0.8494 . ?
O9 H9A 0.8501 . ?
O9 H9C 0.8500 . ?
O10 H10A 0.8501 . ?
O10 H10C 0.8500 . ?
Zn1 O1 1.992(4) 2_756 ?
Zn2 O3 1.958(4) 2_856 ?
Zn2 N6 2.026(5) 2_746 ?
Zn2 N4 2.033(4) 3_766 ?

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
C2 C1 C6 118.8(5) . . ?
C2 C1 C7 121.3(5) . . ?
C6 C1 C7 119.9(5) . . ?
C3 C2 C1 121.4(5) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 C24 118.2(5) . . ?
C2 C3 C24 122.0(5) . . ?
C3 C4 C5 120.8(5) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.7(5) . . ?
C6 C5 C8 121.1(5) . . ?
C4 C5 C8 120.1(5) . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O2 C7 O1 123.1(5) . . ?
O2 C7 C1 119.9(5) . . ?
O1 C7 C1 117.0(5) . . ?
O5 C8 O6 123.6(5) . . ?
O5 C8 C5 120.1(5) . . ?
O6 C8 C5 116.3(5) . . ?
N1 C9 N2 110.9(5) . . ?
N1 C9 H9 124.6 . . ?
N2 C9 H9 124.6 . . ?
C11 C10 N2 107.6(5) . . ?
C11 C10 H10 126.2 . . ?
N2 C10 H10 126.2 . . ?
C10 C11 N1 109.3(5) . . ?
C10 C11 H11 125.4 . . ?
N1 C11 H11 125.4 . . ?
C13 C12 C17 118.9(5) . . ?
C13 C12 H12 120.5 . . ?
C17 C12 H12 120.5 . . ?
C12 C13 C14 120.6(5) . . ?
C12 C13 N2 120.2(5) . . ?
C14 C13 N2 119.2(5) . . ?
C15 C14 C13 118.8(5) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C16 C15 C14 121.7(5) . . ?
C16 C15 N3 119.4(5) . . ?
C14 C15 N3 118.9(5) . . ?
C15 C16 C17 118.6(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C12 C17 C16 121.3(5) . . ?
C12 C17 N5 120.1(5) . . ?
C16 C17 N5 118.5(5) . . ?
N4 C18 N3 112.0(5) . . ?
N4 C18 H18 124.0 . . ?
N3 C18 H18 124.0 . . ?
C20 C19 N4 109.5(5) . . ?
C20 C19 H19 125.2 . . ?
N4 C19 H19 125.2 . . ?
C19 C20 N3 106.5(5) . . ?
C19 C20 H20 126.7 . . ?
N3 C20 H20 126.7 . . ?
C22 C21 N5 106.2(5) . . ?
C22 C21 H21 126.9 . . ?
N5 C21 H21 126.9 . . ?
C21 C22 N6 110.5(5) . . ?
C21 C22 H22 124.7 . . ?
N6 C22 H22 124.7 . . ?
N6 C23 N5 111.4(5) . . ?
N6 C23 H23 124.3 . . ?
N5 C23 H23 124.3 . . ?
O4 C24 O3 122.9(6) . . ?
O4 C24 C3 120.1(6) . . ?
O3 C24 C3 117.0(6) . . ?
C9 N1 C11 106.1(5) . . ?
C9 N1 Zn1 124.1(4) . . ?
C11 N1 Zn1 126.4(4) . . ?
C9 N2 C10 106.2(5) . . ?
C9 N2 C13 126.1(5) . . ?
C10 N2 C13 127.6(5) . . ?
C18 N3 C20 106.4(5) . . ?
C18 N3 C15 125.7(5) . . ?
C20 N3 C15 127.8(5) . . ?
C18 N4 C19 105.6(5) . . ?
C18 N4 Zn2 122.1(4) . 3_766 ?
C19 N4 Zn2 131.1(4) . 3_766 ?
C23 N5 C21 106.7(5) . . ?
C23 N5 C17 125.9(5) . . ?
C21 N5 C17 127.1(5) . . ?
C23 N6 C22 105.1(5) . . ?
C23 N6 Zn2 126.5(4) . 2_756 ?
C22 N6 Zn2 125.3(4) . 2_756 ?
C7 O1 Zn1 119.1(3) . 2_746 ?
C24 O3 Zn2 109.6(4) . 2_846 ?
C8 O6 Zn1 117.0(4) . . ?
Zn1 O7 Zn2 130.2(2) . . ?
H8A O8 H8C 109.5 . . ?
H9A O9 H9C 109.5 . . ?
H10A O10 H10C 109.5 . . ?
O7 Zn1 O6 106.01(17) . . ?
O7 Zn1 O1 107.54(17) . 2_756 ?
O6 Zn1 O1 107.94(17) . 2_756 ?
O7 Zn1 N1 109.04(18) . . ?
O6 Zn1 N1 122.53(19) . . ?
O1 Zn1 N1 103.02(17) 2_756 . ?
O7 Zn2 O3 129.36(18) . 2_856 ?
O7 Zn2 N6 114.79(18) . 2_746 ?
O3 Zn2 N6 102.15(19) 2_856 2_746 ?
O7 Zn2 N4 104.87(18) . 3_766 ?
O3 Zn2 N4 101.04(19) 2_856 3_766 ?
N6 Zn2 N4 100.21(18) 2_746 3_766 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.615
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.134

# Attachment '3.cif'

data_81007am
_database_code_depnum_ccdc_archive 'CCDC 742385'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H46 N8 O18 Zn3'
_chemical_formula_weight         1291.10

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

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

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

_cell_length_a                   9.1215(14)
_cell_length_b                   20.539(3)
_cell_length_c                   13.621(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.457(3)
_cell_angle_gamma                90.00
_cell_volume                     2509.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  '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            13404
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1354
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4934
_reflns_number_gt                2761
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0115P)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         4934
_refine_ls_number_parameters     364
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1031
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.011
_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
C1 C 0.1066(6) 0.3048(3) 0.6252(5) 0.0342(16) Uani 1 1 d . . .
H16 H 0.1112 0.2888 0.5620 0.041 Uiso 1 1 calc R . .
C2 C 0.0487(7) 0.3182(3) 0.7676(4) 0.0406(17) Uani 1 1 d . . .
H17 H 0.0035 0.3127 0.8230 0.049 Uiso 1 1 calc R . .
C3 C 0.1515(7) 0.3637(3) 0.7603(5) 0.0476(19) Uani 1 1 d . . .
H34 H 0.1895 0.3947 0.8079 0.057 Uiso 1 1 calc R . .
C4 C 0.2855(7) 0.3960(3) 0.6253(5) 0.0437(18) Uani 1 1 d . . .
C5 C 0.3327(7) 0.4537(3) 0.6665(5) 0.0464(19) Uani 1 1 d . . .
H10 H 0.3089 0.4664 0.7273 0.056 Uiso 1 1 calc R . .
C6 C 0.4166(7) 0.4938(3) 0.6172(5) 0.0476(19) Uani 1 1 d . . .
H13 H 0.4473 0.5337 0.6461 0.057 Uiso 1 1 calc R . .
C7 C 0.4573(6) 0.4784(3) 0.5289(5) 0.0422(19) Uani 1 1 d . . .
C8 C 0.4132(8) 0.4174(3) 0.4883(6) 0.067 Uani 1 1 d . . .
H44 H 0.4420 0.4034 0.4297 0.081 Uiso 1 1 calc R . .
C9 C 0.3232(8) 0.3774(4) 0.5387(6) 0.067 Uani 1 1 d . . .
H12 H 0.2899 0.3374 0.5111 0.081 Uiso 1 1 calc R . .
C10 C 0.1800(6) 0.0141(3) 0.3343(4) 0.0261(14) Uani 1 1 d . . .
H8 H 0.1920 -0.0308 0.3306 0.031 Uiso 1 1 calc R . .
C11 C 0.1174(7) 0.1075(3) 0.3771(5) 0.0400(17) Uani 1 1 d . . .
H9 H 0.0767 0.1404 0.4106 0.048 Uiso 1 1 calc R . .
C12 C 0.1906(7) 0.1177(3) 0.3027(5) 0.0398(17) Uani 1 1 d . . .
H33 H 0.2096 0.1575 0.2750 0.048 Uiso 1 1 calc R . .
C13 C 0.3129(6) 0.0417(3) 0.1969(4) 0.0265(14) Uani 1 1 d . . .
C14 C 0.3023(6) 0.0810(3) 0.1156(4) 0.0289(15) Uani 1 1 d . . .
H2 H 0.2454 0.1188 0.1118 0.035 Uiso 1 1 calc R . .
C15 C 0.3755(6) 0.0651(3) 0.0390(4) 0.0305(15) Uani 1 1 d . . .
H3 H 0.3675 0.0925 -0.0161 0.037 Uiso 1 1 calc R . .
C16 C 0.4620(6) 0.0085(3) 0.0427(4) 0.0271(14) Uani 1 1 d . . .
C17 C 0.4725(7) -0.0288(3) 0.1269(5) 0.0452(19) Uani 1 1 d . . .
H5 H 0.5314 -0.0661 0.1325 0.054 Uiso 1 1 calc R . .
C18 C 0.3990(7) -0.0133(3) 0.2039(4) 0.0433(18) Uani 1 1 d . . .
H6 H 0.4079 -0.0399 0.2599 0.052 Uiso 1 1 calc R . .
C19 C 0.1031(6) 0.1063(3) 0.6643(4) 0.0244(14) Uani 1 1 d . . .
C20 C 0.2330(6) 0.1446(3) 0.7235(4) 0.0212(13) Uani 1 1 d U . .
C21 C 0.2186(6) 0.1755(3) 0.8105(4) 0.0243(14) Uani 1 1 d . . .
H23 H 0.1305 0.1712 0.8352 0.029 Uiso 1 1 calc R . .
C22 C 0.3347(6) 0.2132(3) 0.8626(4) 0.0245(14) Uani 1 1 d . . .
C23 C 0.4660(6) 0.2176(3) 0.8249(4) 0.0272(14) Uani 1 1 d . . .
H21 H 0.5439 0.2428 0.8587 0.033 Uiso 1 1 calc R . .
C24 C 0.4840(6) 0.1857(3) 0.7391(4) 0.0248(14) Uani 1 1 d . . .
C25 C 0.3659(6) 0.1485(2) 0.6887(4) 0.0247(14) Uani 1 1 d U . .
H19 H 0.3767 0.1260 0.6312 0.030 Uiso 1 1 calc R . .
C26 C 0.3142(7) 0.2438(3) 0.9591(4) 0.0322(16) Uani 1 1 d . . .
C27 C 0.6270(7) 0.1888(3) 0.7006(5) 0.0355(17) Uani 1 1 d . . .
N1 N 0.0190(5) 0.2812(2) 0.6841(4) 0.0305(12) Uani 1 1 d . . .
N2 N 0.1886(5) 0.3551(2) 0.6692(4) 0.0348(13) Uani 1 1 d . . .
N3 N 0.1094(5) 0.0424(2) 0.3982(3) 0.0299(13) Uani 1 1 d . . .
N4 N 0.2329(5) 0.0565(2) 0.2752(3) 0.0270(12) Uani 1 1 d . . .
O1 O 0.1324(4) 0.06192(18) 0.6109(3) 0.0351(11) Uani 1 1 d . . .
O2 O -0.0277(4) 0.12327(16) 0.6744(3) 0.0281(10) Uani 1 1 d . . .
O3 O 0.6440(4) 0.1543(2) 0.6280(3) 0.0437(12) Uani 1 1 d . . .
O4 O 0.7283(4) 0.22589(19) 0.7415(3) 0.0440(12) Uani 1 1 d . . .
O5 O 0.2195(5) 0.22297(19) 1.0043(3) 0.0447(12) Uani 1 1 d . . .
O6 O 0.4050(4) 0.28990(19) 0.9945(3) 0.0382(11) Uani 1 1 d . . .
O7 O -0.1746(4) 0.07102(17) 0.4617(3) 0.0394(11) Uani 1 1 d . . .
H7B H -0.2107 0.0800 0.5133 0.059 Uiso 1 1 d R . .
H7C H -0.1383 0.1053 0.4406 0.059 Uiso 1 1 d R . .
O8 O 0.5281(5) 0.0652(3) 0.4786(4) 0.097(2) Uani 1 1 d . . .
H8A H 0.5630 0.0831 0.4315 0.145 Uiso 1 1 d R . .
H8B H 0.5448 0.0895 0.5300 0.145 Uiso 1 1 d R . .
O9 O 0.3807(14) 0.2363(6) 0.4661(10) 0.431(9) Uani 1 1 d . . .
H9B H 0.3548 0.2345 0.4030 0.646 Uiso 1 1 d RD . .
H9C H 0.4731 0.2276 0.4822 0.646 Uiso 1 1 d R . .
Zn1 Zn -0.13108(7) 0.20856(3) 0.63974(5) 0.0296(2) Uani 1 1 d . . .
Zn2 Zn 0.0000 0.0000 0.5000 0.0267(3) Uani 1 2 d S . .


_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 1.322(6) . ?
C1 N2 1.350(6) . ?
C1 H16 0.9300 . ?
C2 C3 1.340(8) . ?
C2 N1 1.354(7) . ?
C2 H17 0.9300 . ?
C3 N2 1.357(7) . ?
C3 H34 0.9300 . ?
C4 C9 1.343(8) . ?
C4 C5 1.349(8) . ?
C4 N2 1.427(7) . ?
C5 C6 1.378(8) . ?
C5 H10 0.9300 . ?
C6 C7 1.359(8) . ?
C6 H13 0.9300 . ?
C7 C8 1.398(8) . ?
C7 C7 1.496(12) 3_666 ?
C8 C9 1.424(9) . ?
C8 H44 0.9300 . ?
C9 H12 0.9300 . ?
C10 N3 1.309(6) . ?
C10 N4 1.335(6) . ?
C10 H8 0.9300 . ?
C11 C12 1.326(7) . ?
C11 N3 1.373(6) . ?
C11 H9 0.9300 . ?
C12 N4 1.387(6) . ?
C12 H33 0.9300 . ?
C13 C14 1.359(7) . ?
C13 C18 1.369(7) . ?
C13 N4 1.430(6) . ?
C14 C15 1.376(7) . ?
C14 H2 0.9300 . ?
C15 C16 1.401(7) . ?
C15 H3 0.9300 . ?
C16 C17 1.368(7) . ?
C16 C16 1.499(10) 3_655 ?
C17 C18 1.381(7) . ?
C17 H5 0.9300 . ?
C18 H6 0.9300 . ?
C19 O1 1.225(6) . ?
C19 O2 1.274(6) . ?
C19 C20 1.526(7) . ?
C20 C21 1.371(7) . ?
C20 C25 1.382(7) . ?
C21 C22 1.397(6) . ?
C21 H23 0.9300 . ?
C22 C23 1.389(7) . ?
C22 C26 1.499(7) . ?
C23 C24 1.375(7) . ?
C23 H21 0.9300 . ?
C24 C25 1.396(6) . ?
C24 C27 1.493(7) . ?
C25 H19 0.9300 . ?
C26 O5 1.225(6) . ?
C26 O6 1.293(6) . ?
C27 O4 1.248(6) . ?
C27 O3 1.249(7) . ?
C27 Zn1 2.526(6) 1_655 ?
N1 Zn1 2.042(5) . ?
N3 Zn2 2.044(5) . ?
O1 Zn2 2.167(4) . ?
O2 Zn1 2.005(3) . ?
O3 Zn1 2.315(4) 1_655 ?
O4 Zn1 2.083(4) 1_655 ?
O6 Zn1 2.063(4) 4_666 ?
O7 Zn2 2.153(3) . ?
O7 H7B 0.8499 . ?
O7 H7C 0.8500 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8501 . ?
O9 H9B 0.8500 . ?
O9 H9C 0.8501 . ?
Zn1 O6 2.063(4) 4_565 ?
Zn1 O4 2.083(4) 1_455 ?
Zn1 O3 2.315(4) 1_455 ?
Zn1 C27 2.526(6) 1_455 ?
Zn2 N3 2.044(5) 3_556 ?
Zn2 O7 2.153(3) 3_556 ?
Zn2 O1 2.167(4) 3_556 ?

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 N2 111.0(6) . . ?
N1 C1 H16 124.5 . . ?
N2 C1 H16 124.5 . . ?
C3 C2 N1 111.4(6) . . ?
C3 C2 H17 124.3 . . ?
N1 C2 H17 124.3 . . ?
C2 C3 N2 105.7(6) . . ?
C2 C3 H34 127.2 . . ?
N2 C3 H34 127.2 . . ?
C9 C4 C5 120.1(7) . . ?
C9 C4 N2 118.5(7) . . ?
C5 C4 N2 121.3(6) . . ?
C4 C5 C6 119.1(7) . . ?
C4 C5 H10 120.5 . . ?
C6 C5 H10 120.5 . . ?
C7 C6 C5 123.9(6) . . ?
C7 C6 H13 118.0 . . ?
C5 C6 H13 118.0 . . ?
C6 C7 C8 116.9(6) . . ?
C6 C7 C7 125.5(8) . 3_666 ?
C8 C7 C7 117.6(8) . 3_666 ?
C7 C8 C9 118.5(7) . . ?
C7 C8 H44 120.8 . . ?
C9 C8 H44 120.8 . . ?
C4 C9 C8 121.4(7) . . ?
C4 C9 H12 119.3 . . ?
C8 C9 H12 119.3 . . ?
N3 C10 N4 112.7(5) . . ?
N3 C10 H8 123.6 . . ?
N4 C10 H8 123.6 . . ?
C12 C11 N3 111.5(5) . . ?
C12 C11 H9 124.2 . . ?
N3 C11 H9 124.2 . . ?
C11 C12 N4 105.5(5) . . ?
C11 C12 H33 127.3 . . ?
N4 C12 H33 127.3 . . ?
C14 C13 C18 120.1(6) . . ?
C14 C13 N4 120.7(5) . . ?
C18 C13 N4 119.2(5) . . ?
C13 C14 C15 120.3(6) . . ?
C13 C14 H2 119.9 . . ?
C15 C14 H2 119.9 . . ?
C14 C15 C16 121.1(5) . . ?
C14 C15 H3 119.4 . . ?
C16 C15 H3 119.4 . . ?
C17 C16 C15 116.6(5) . . ?
C17 C16 C16 123.2(7) . 3_655 ?
C15 C16 C16 120.1(6) . 3_655 ?
C16 C17 C18 122.5(6) . . ?
C16 C17 H5 118.7 . . ?
C18 C17 H5 118.7 . . ?
C13 C18 C17 119.3(6) . . ?
C13 C18 H6 120.4 . . ?
C17 C18 H6 120.4 . . ?
O1 C19 O2 125.3(5) . . ?
O1 C19 C20 117.8(5) . . ?
O2 C19 C20 116.9(5) . . ?
C21 C20 C25 119.8(5) . . ?
C21 C20 C19 120.6(5) . . ?
C25 C20 C19 119.6(5) . . ?
C20 C21 C22 120.9(5) . . ?
C20 C21 H23 119.6 . . ?
C22 C21 H23 119.6 . . ?
C23 C22 C21 118.2(5) . . ?
C23 C22 C26 123.4(5) . . ?
C21 C22 C26 118.3(5) . . ?
C24 C23 C22 121.8(5) . . ?
C24 C23 H21 119.1 . . ?
C22 C23 H21 119.1 . . ?
C23 C24 C25 118.5(5) . . ?
C23 C24 C27 121.7(5) . . ?
C25 C24 C27 119.7(5) . . ?
C20 C25 C24 120.6(5) . . ?
C20 C25 H19 119.7 . . ?
C24 C25 H19 119.7 . . ?
O5 C26 O6 122.0(6) . . ?
O5 C26 C22 120.4(6) . . ?
O6 C26 C22 117.5(6) . . ?
O4 C27 O3 120.8(6) . . ?
O4 C27 C24 119.4(6) . . ?
O3 C27 C24 119.7(6) . . ?
O4 C27 Zn1 55.2(3) . 1_655 ?
O3 C27 Zn1 65.8(3) . 1_655 ?
C24 C27 Zn1 173.1(5) . 1_655 ?
C1 N1 C2 104.7(5) . . ?
C1 N1 Zn1 122.4(4) . . ?
C2 N1 Zn1 132.8(4) . . ?
C1 N2 C3 107.2(5) . . ?
C1 N2 C4 126.9(6) . . ?
C3 N2 C4 125.6(6) . . ?
C10 N3 C11 104.0(5) . . ?
C10 N3 Zn2 128.4(4) . . ?
C11 N3 Zn2 127.5(4) . . ?
C10 N4 C12 106.2(5) . . ?
C10 N4 C13 126.9(5) . . ?
C12 N4 C13 126.8(5) . . ?
C19 O1 Zn2 134.1(4) . . ?
C19 O2 Zn1 128.6(4) . . ?
C27 O3 Zn1 84.7(4) . 1_655 ?
C27 O4 Zn1 95.3(4) . 1_655 ?
C26 O6 Zn1 99.6(4) . 4_666 ?
Zn2 O7 H7B 109.1 . . ?
Zn2 O7 H7C 109.1 . . ?
H7B O7 H7C 109.5 . . ?
H8A O8 H8B 109.5 . . ?
H9B O9 H9C 109.5 . . ?
O2 Zn1 N1 107.91(16) . . ?
O2 Zn1 O6 95.12(16) . 4_565 ?
N1 Zn1 O6 93.27(18) . 4_565 ?
O2 Zn1 O4 108.21(16) . 1_455 ?
N1 Zn1 O4 98.00(18) . 1_455 ?
O6 Zn1 O4 149.31(16) 4_565 1_455 ?
O2 Zn1 O3 88.20(15) . 1_455 ?
N1 Zn1 O3 155.66(17) . 1_455 ?
O6 Zn1 O3 103.57(15) 4_565 1_455 ?
O4 Zn1 O3 58.90(14) 1_455 1_455 ?
O2 Zn1 C27 100.60(17) . 1_455 ?
N1 Zn1 C27 126.8(2) . 1_455 ?
O6 Zn1 C27 128.14(19) 4_565 1_455 ?
O4 Zn1 C27 29.46(17) 1_455 1_455 ?
O3 Zn1 C27 29.49(16) 1_455 1_455 ?
N3 Zn2 N3 180.0 3_556 . ?
N3 Zn2 O7 88.72(16) 3_556 3_556 ?
N3 Zn2 O7 91.28(16) . 3_556 ?
N3 Zn2 O7 91.28(16) 3_556 . ?
N3 Zn2 O7 88.72(16) . . ?
O7 Zn2 O7 180.0 3_556 . ?
N3 Zn2 O1 93.21(16) 3_556 . ?
N3 Zn2 O1 86.79(16) . . ?
O7 Zn2 O1 86.24(14) 3_556 . ?
O7 Zn2 O1 93.76(14) . . ?
N3 Zn2 O1 86.79(16) 3_556 3_556 ?
N3 Zn2 O1 93.21(16) . 3_556 ?
O7 Zn2 O1 93.76(14) 3_556 3_556 ?
O7 Zn2 O1 86.24(14) . 3_556 ?
O1 Zn2 O1 180.00(16) . 3_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.095

# Attachment '4.cif'

data_yy2
_database_code_depnum_ccdc_archive 'CCDC 742386'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H44 N8 Ni3 O17'
_chemical_formula_weight         1253.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.0505(11)
_cell_length_b                   20.457(2)
_cell_length_c                   13.5723(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.210(2)
_cell_angle_gamma                90.00
_cell_volume                     2464.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13167
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4843
_reflns_number_gt                3476
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0612P)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         4843
_refine_ls_number_parameters     368
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1418
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0937(5) 0.3920(2) 0.1621(3) 0.0166(10) Uani 1 1 d . . .
C2 C 0.2262(5) 0.3555(2) 0.2195(3) 0.0163(10) Uani 1 1 d . . .
C3 C 0.3593(5) 0.3513(2) 0.1834(3) 0.0180(10) Uani 1 1 d . . .
H3 H 0.3676 0.3735 0.1249 0.022 Uiso 1 1 calc R . .
C4 C 0.4803(5) 0.3147(2) 0.2331(3) 0.0192(11) Uani 1 1 d . . .
C5 C 0.6238(6) 0.3104(2) 0.1936(4) 0.0214(11) Uani 1 1 d . . .
C6 C 0.4661(5) 0.2814(2) 0.3208(3) 0.0196(11) Uani 1 1 d . . .
H6 H 0.5449 0.2555 0.3537 0.023 Uiso 1 1 calc R . .
C7 C 0.3355(5) 0.2868(2) 0.3589(3) 0.0170(10) Uani 1 1 d . . .
C8 C 0.3243(6) 0.2538(2) 0.4561(3) 0.0192(11) Uani 1 1 d . . .
C9 C 0.2156(5) 0.3239(2) 0.3081(3) 0.0181(10) Uani 1 1 d . . .
H9 H 0.1279 0.3276 0.3339 0.022 Uiso 1 1 calc R . .
C10 C 0.1072(6) 0.1986(2) 0.1182(4) 0.0279(12) Uani 1 1 d . . .
H10 H 0.1137 0.2135 0.0544 0.033 Uiso 1 1 calc R . .
C11 C 0.0432(6) 0.1874(2) 0.2602(4) 0.0271(12) Uani 1 1 d . . .
H11 H -0.0038 0.1936 0.3146 0.032 Uiso 1 1 calc R . .
C12 C 0.1473(7) 0.1426(3) 0.2555(4) 0.0360(14) Uani 1 1 d . . .
H12 H 0.1844 0.1119 0.3048 0.043 Uiso 1 1 calc R . .
C13 C 0.2879(6) 0.1082(3) 0.1216(4) 0.0293(13) Uani 1 1 d . . .
C14 C 0.3349(7) 0.0495(3) 0.1645(4) 0.0376(14) Uani 1 1 d . . .
H14 H 0.3107 0.0375 0.2255 0.045 Uiso 1 1 calc R . .
C15 C 0.4184(7) 0.0082(3) 0.1166(4) 0.0396(15) Uani 1 1 d . . .
H15 H 0.4501 -0.0314 0.1471 0.048 Uiso 1 1 calc R . .
C16 C 0.4571(6) 0.0227(3) 0.0260(5) 0.0390(14) Uani 1 1 d U . .
C17 C 0.4103(8) 0.0829(3) -0.0150(5) 0.0534(17) Uani 1 1 d U . .
H17 H 0.4339 0.0950 -0.0762 0.064 Uiso 1 1 calc R . .
C18 C 0.3293(7) 0.1254(3) 0.0333(5) 0.050 Uani 1 1 d U . .
H18 H 0.3026 0.1663 0.0054 0.060 Uiso 1 1 calc R . .
C19 C 0.1221(6) 0.3925(3) -0.1196(4) 0.0272(12) Uani 1 1 d U . .
H19 H 0.0821 0.3596 -0.0855 0.033 Uiso 1 1 calc R . .
C20 C 0.1956(6) 0.3826(2) -0.1951(4) 0.0302(13) Uani 1 1 d . . .
H20 H 0.2142 0.3427 -0.2233 0.036 Uiso 1 1 calc R . .
C21 C 0.1846(6) 0.4874(2) -0.1636(3) 0.0198(11) Uani 1 1 d . . .
H21 H 0.1960 0.5324 -0.1674 0.024 Uiso 1 1 calc R . .
C22 C 0.3164(6) 0.4592(2) -0.3010(4) 0.0218(11) Uani 1 1 d . . .
C23 C 0.4035(6) 0.5137(3) -0.2949(4) 0.0328(13) Uani 1 1 d U . .
H23 H 0.4148 0.5401 -0.2382 0.039 Uiso 1 1 calc R . .
C24 C 0.4749(6) 0.5300(3) -0.3717(4) 0.0325(13) Uani 1 1 d U . .
H24 H 0.5334 0.5677 -0.3664 0.039 Uiso 1 1 calc R . .
C25 C 0.4618(6) 0.4910(2) -0.4583(3) 0.0237(12) Uani 1 1 d . . .
C26 C 0.3760(6) 0.4347(2) -0.4606(4) 0.0249(12) Uani 1 1 d . . .
H26 H 0.3675 0.4068 -0.5156 0.030 Uiso 1 1 calc R . .
C27 C 0.3023(6) 0.4187(2) -0.3834(3) 0.0223(11) Uani 1 1 d . . .
H27 H 0.2440 0.3810 -0.3871 0.027 Uiso 1 1 calc R . .
N1 N 0.0149(4) 0.22316(18) 0.1733(3) 0.0215(9) Uani 1 1 d . . .
N2 N 0.1899(5) 0.14971(19) 0.1654(3) 0.0258(10) Uani 1 1 d . . .
N3 N 0.1144(5) 0.45768(19) -0.1000(3) 0.0217(10) Uani 1 1 d . . .
N4 N 0.2379(5) 0.44383(19) -0.2225(3) 0.0220(9) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.5000 0.0000 0.0153(2) Uani 1 2 d S . .
Ni2 Ni -0.14740(7) 0.29009(3) 0.12741(4) 0.01871(19) Uani 1 1 d . . .
O1 O 0.1226(4) 0.43813(16) 0.1084(2) 0.0239(8) Uani 1 1 d . . .
O2 O -0.0364(4) 0.37480(14) 0.1725(2) 0.0193(7) Uani 1 1 d . . .
O3 O 0.6382(4) 0.34211(16) 0.1168(2) 0.0264(8) Uani 1 1 d . . .
O4 O 0.7291(4) 0.27481(16) 0.2373(2) 0.0245(8) Uani 1 1 d . . .
O5 O 0.4089(4) 0.20576(15) 0.4859(2) 0.0222(8) Uani 1 1 d . . .
O6 O 0.2352(4) 0.27528(16) 0.5080(2) 0.0264(8) Uani 1 1 d . . .
O7 O 0.1691(4) 0.56849(16) 0.0441(2) 0.0266(8) Uani 1 1 d D . .
H7 H 0.1385 0.6048 0.0241 0.040 Uiso 1 1 calc R . .
H7A H 0.2558 0.5597 0.0402 0.040 Uiso 1 1 d RD . .
O8 O 0.5337(5) 0.4347(2) 0.9732(3) 0.0660(14) Uani 1 1 d . . .
H8A H 0.5355 0.3936 0.9822 0.099 Uiso 1 1 d R . .
H8B H 0.4601 0.4510 0.9953 0.099 Uiso 1 1 d R . .
O9 O 0.8855(5) 0.2339(2) 0.4529(3) 0.248(11) Uani 0.50 1 d PR . .
H9A H 0.8584 0.2504 0.3946 0.298 Uiso 0.50 1 d PR . .
H9B H 0.9661 0.2524 0.4827 0.372 Uiso 0.50 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.251(5) . ?
C1 O2 1.263(5) . ?
C1 C2 1.497(6) . ?
C2 C9 1.384(6) . ?
C2 C3 1.389(6) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C6 1.399(6) . ?
C4 C5 1.501(6) . ?
C5 O4 1.253(6) . ?
C5 O3 1.257(5) . ?
C5 Ni2 2.448(5) 1_655 ?
C6 C7 1.384(6) . ?
C6 H6 0.9300 . ?
C7 C9 1.393(6) . ?
C7 C8 1.502(6) . ?
C8 O6 1.249(5) . ?
C8 O5 1.264(5) . ?
C8 Ni2 2.459(5) 4_666 ?
C9 H9 0.9300 . ?
C10 N1 1.324(6) . ?
C10 N2 1.336(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.325(7) . ?
C11 N1 1.369(6) . ?
C11 H11 0.9300 . ?
C12 N2 1.361(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(7) . ?
C13 C18 1.370(7) . ?
C13 N2 1.437(6) . ?
C14 C15 1.377(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(8) . ?
C16 C16 1.475(11) 3_655 ?
C17 C18 1.382(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.341(6) . ?
C19 N3 1.364(6) . ?
C19 H19 0.9300 . ?
C20 N4 1.381(6) . ?
C20 H20 0.9300 . ?
C21 N3 1.315(6) . ?
C21 N4 1.347(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.359(7) . ?
C22 C27 1.377(6) . ?
C22 N4 1.425(5) . ?
C23 C24 1.370(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.406(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(7) . ?
C25 C25 1.485(9) 3_664 ?
C26 C27 1.386(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
N1 Ni2 2.016(4) . ?
N3 Ni1 2.052(4) . ?
Ni1 N3 2.052(4) 3_565 ?
Ni1 O7 2.075(3) 3_565 ?
Ni1 O7 2.075(3) . ?
Ni1 O1 2.088(3) . ?
Ni1 O1 2.088(3) 3_565 ?
Ni2 O2 2.037(3) . ?
Ni2 O4 2.054(3) 1_455 ?
Ni2 O5 2.082(3) 4_565 ?
Ni2 O3 2.193(3) 1_455 ?
Ni2 O6 2.208(3) 4_565 ?
Ni2 C5 2.448(5) 1_455 ?
Ni2 C8 2.459(5) 4_565 ?
O3 Ni2 2.193(3) 1_655 ?
O4 Ni2 2.054(3) 1_655 ?
O5 Ni2 2.082(3) 4_666 ?
O6 Ni2 2.208(3) 4_666 ?
O7 H7 0.8200 . ?
O7 H7A 0.8169 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8499 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8499 . ?

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 C1 O2 125.5(4) . . ?
O1 C1 C2 116.3(4) . . ?
O2 C1 C2 118.2(4) . . ?
C9 C2 C3 119.3(4) . . ?
C9 C2 C1 120.1(4) . . ?
C3 C2 C1 120.6(4) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C6 118.8(4) . . ?
C3 C4 C5 120.9(4) . . ?
C6 C4 C5 120.3(4) . . ?
O4 C5 O3 120.0(4) . . ?
O4 C5 C4 119.8(4) . . ?
O3 C5 C4 120.2(4) . . ?
O4 C5 Ni2 57.0(2) . 1_655 ?
O3 C5 Ni2 63.3(3) . 1_655 ?
C4 C5 Ni2 173.5(3) . 1_655 ?
C7 C6 C4 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C4 C6 H6 119.8 . . ?
C6 C7 C9 119.9(4) . . ?
C6 C7 C8 120.1(4) . . ?
C9 C7 C8 120.0(4) . . ?
O6 C8 O5 120.7(4) . . ?
O6 C8 C7 119.9(4) . . ?
O5 C8 C7 119.4(4) . . ?
O6 C8 Ni2 63.6(2) . 4_666 ?
O5 C8 Ni2 57.8(2) . 4_666 ?
C7 C8 Ni2 169.0(3) . 4_666 ?
C2 C9 C7 120.3(4) . . ?
C2 C9 H9 119.8 . . ?
C7 C9 H9 119.8 . . ?
N1 C10 N2 111.7(5) . . ?
N1 C10 H10 124.2 . . ?
N2 C10 H10 124.2 . . ?
C12 C11 N1 110.2(5) . . ?
C12 C11 H11 124.9 . . ?
N1 C11 H11 124.9 . . ?
C11 C12 N2 107.3(5) . . ?
C11 C12 H12 126.4 . . ?
N2 C12 H12 126.4 . . ?
C14 C13 C18 118.9(5) . . ?
C14 C13 N2 120.6(5) . . ?
C18 C13 N2 120.4(5) . . ?
C13 C14 C15 119.5(6) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 123.3(5) . . ?
C16 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C15 C16 C17 116.1(5) . . ?
C15 C16 C16 122.8(7) . 3_655 ?
C17 C16 C16 121.1(7) . 3_655 ?
C18 C17 C16 121.3(6) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C13 C18 C17 120.9(6) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 N3 110.4(5) . . ?
C20 C19 H19 124.8 . . ?
N3 C19 H19 124.8 . . ?
C19 C20 N4 105.9(4) . . ?
C19 C20 H20 127.1 . . ?
N4 C20 H20 127.1 . . ?
N3 C21 N4 111.0(4) . . ?
N3 C21 H21 124.5 . . ?
N4 C21 H21 124.5 . . ?
C23 C22 C27 120.2(4) . . ?
C23 C22 N4 120.2(4) . . ?
C27 C22 N4 119.6(4) . . ?
C22 C23 C24 120.5(5) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 121.4(5) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C26 C25 C24 116.5(4) . . ?
C26 C25 C25 122.1(5) . 3_664 ?
C24 C25 C25 121.3(6) . 3_664 ?
C25 C26 C27 121.9(4) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C22 C27 C26 119.4(4) . . ?
C22 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C10 N1 C11 104.5(4) . . ?
C10 N1 Ni2 125.8(3) . . ?
C11 N1 Ni2 129.2(3) . . ?
C10 N2 C12 106.3(4) . . ?
C10 N2 C13 125.2(4) . . ?
C12 N2 C13 127.9(4) . . ?
C21 N3 C19 105.9(4) . . ?
C21 N3 Ni1 127.6(3) . . ?
C19 N3 Ni1 126.4(3) . . ?
C21 N4 C20 106.9(4) . . ?
C21 N4 C22 125.9(4) . . ?
C20 N4 C22 127.2(4) . . ?
N3 Ni1 N3 180.0 3_565 . ?
N3 Ni1 O7 92.12(15) 3_565 3_565 ?
N3 Ni1 O7 87.88(15) . 3_565 ?
N3 Ni1 O7 87.88(15) 3_565 . ?
N3 Ni1 O7 92.12(15) . . ?
O7 Ni1 O7 180.00(13) 3_565 . ?
N3 Ni1 O1 93.27(14) 3_565 . ?
N3 Ni1 O1 86.73(14) . . ?
O7 Ni1 O1 93.14(13) 3_565 . ?
O7 Ni1 O1 86.86(13) . . ?
N3 Ni1 O1 86.73(14) 3_565 3_565 ?
N3 Ni1 O1 93.27(14) . 3_565 ?
O7 Ni1 O1 86.86(13) 3_565 3_565 ?
O7 Ni1 O1 93.14(13) . 3_565 ?
O1 Ni1 O1 180.00(14) . 3_565 ?
N1 Ni2 O2 101.41(15) . . ?
N1 Ni2 O4 97.99(15) . 1_455 ?
O2 Ni2 O4 102.57(13) . 1_455 ?
N1 Ni2 O5 91.06(15) . 4_565 ?
O2 Ni2 O5 92.74(12) . 4_565 ?
O4 Ni2 O5 160.23(14) 1_455 4_565 ?
N1 Ni2 O3 158.77(14) . 1_455 ?
O2 Ni2 O3 89.17(13) . 1_455 ?
O4 Ni2 O3 61.47(12) 1_455 1_455 ?
O5 Ni2 O3 106.93(13) 4_565 1_455 ?
N1 Ni2 O6 91.89(15) . 4_565 ?
O2 Ni2 O6 151.04(13) . 4_565 ?
O4 Ni2 O6 100.87(13) 1_455 4_565 ?
O5 Ni2 O6 61.10(12) 4_565 4_565 ?
O3 Ni2 O6 87.26(13) 1_455 4_565 ?
N1 Ni2 C5 128.27(16) . 1_455 ?
O2 Ni2 C5 98.54(14) . 1_455 ?
O4 Ni2 C5 30.76(14) 1_455 1_455 ?
O5 Ni2 C5 135.05(15) 4_565 1_455 ?
O3 Ni2 C5 30.80(13) 1_455 1_455 ?
O6 Ni2 C5 92.96(14) 4_565 1_455 ?
N1 Ni2 C8 88.83(16) . 4_565 ?
O2 Ni2 C8 123.35(14) . 4_565 ?
O4 Ni2 C8 131.25(15) 1_455 4_565 ?
O5 Ni2 C8 30.91(13) 4_565 4_565 ?
O3 Ni2 C8 100.76(14) 1_455 4_565 ?
O6 Ni2 C8 30.43(13) 4_565 4_565 ?
C5 Ni2 C8 117.97(17) 1_455 4_565 ?
C1 O1 Ni1 136.5(3) . . ?
C1 O2 Ni2 128.3(3) . . ?
C5 O3 Ni2 85.9(3) . 1_655 ?
C5 O4 Ni2 92.3(3) . 1_655 ?
C8 O5 Ni2 91.3(3) . 4_666 ?
C8 O6 Ni2 86.0(3) . 4_666 ?
Ni1 O7 H7 109.5 . . ?
Ni1 O7 H7A 119.8 . . ?
H7 O7 H7A 116.4 . . ?
H8A O8 H8B 109.5 . . ?
H9A O9 H9B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.104

# Attachment '5.cif'

data_yy3
_database_code_depnum_ccdc_archive 'CCDC 742387'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H38 Cu3 N8 O15'
_chemical_formula_weight         1229.57

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

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

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

_cell_length_a                   8.9636(10)
_cell_length_b                   20.589(2)
_cell_length_c                   13.5194(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.469(2)
_cell_angle_gamma                90.00
_cell_volume                     2461.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1250
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6
_exptl_absorpt_correction_T_max  0.7
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13165
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.1526
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4826
_reflns_number_gt                2735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0000P)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         4826
_refine_ls_number_parameters     367
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_restrained_S_all      0.950
_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
O9 O 0.0000 0.5000 0.0000 0.482(7) Uani 1 2 d S . .
H9B H 0.0921 0.5108 0.0178 0.722 Uiso 0.50 1 d PR . .
H9C H -0.0082 0.4762 -0.0519 0.722 Uiso 0.50 1 d PR . .
O7 O 0.2538(7) 0.4312(2) -0.0322(4) 0.063(2) Uani 0.50 1 d P . .
H7A H 0.1863 0.4509 -0.0728 0.094 Uiso 0.50 1 d PR . .
H7C H 0.2221 0.4250 0.0229 0.094 Uiso 0.50 1 d PR . .
C1 C 0.5882(4) 0.39066(17) -0.1264(3) 0.0360(13) Uani 1 1 d . . .
H1 H 0.5437 0.3583 -0.0931 0.043 Uiso 1 1 calc R . .
C2 C 0.6684(4) 0.38074(17) -0.2001(3) 0.0354(13) Uani 1 1 d . . .
H2 H 0.6888 0.3409 -0.2273 0.043 Uiso 1 1 calc R . .
C3 C 0.6573(4) 0.48363(17) -0.1687(3) 0.0264(11) Uani 1 1 d . . .
H3 H 0.6707 0.5283 -0.1720 0.032 Uiso 1 1 calc R . .
C4 C 0.8022(4) 0.45606(17) -0.3040(3) 0.0264(11) Uani 1 1 d . . .
C5 C 0.8009(4) 0.41608(16) -0.3847(3) 0.0251(12) Uani 1 1 d . . .
H5 H 0.7468 0.3774 -0.3889 0.030 Uiso 1 1 calc R . .
C6 C 0.8804(4) 0.43340(17) -0.4600(3) 0.0288(12) Uani 1 1 d . . .
H6 H 0.8805 0.4050 -0.5136 0.035 Uiso 1 1 calc R . .
C7 C 0.9593(4) 0.49072(18) -0.4594(3) 0.0257(12) Uani 1 1 d . . .
C8 C 0.9607(4) 0.52926(18) -0.3760(3) 0.0414(13) Uani 1 1 d . . .
H8 H 1.0142 0.5681 -0.3719 0.050 Uiso 1 1 calc R . .
C9 C 0.8859(5) 0.51239(18) -0.2984(3) 0.0447(14) Uani 1 1 d . . .
H9 H 0.8920 0.5391 -0.2423 0.054 Uiso 1 1 calc R . .
C10 C 0.5397(4) 0.19157(17) 0.2613(3) 0.0376(14) Uani 1 1 d . . .
H10 H 0.4905 0.1996 0.3155 0.045 Uiso 1 1 calc R . .
C11 C 0.6494(4) 0.14700(19) 0.2609(3) 0.0433(15) Uani 1 1 d . . .
H11 H 0.6892 0.1193 0.3129 0.052 Uiso 1 1 calc R . .
C12 C 0.6032(4) 0.19716(17) 0.1182(3) 0.0329(13) Uani 1 1 d . . .
H12 H 0.6083 0.2094 0.0526 0.039 Uiso 1 1 calc R . .
C13 C 0.7883(4) 0.10842(18) 0.1252(3) 0.0387(14) Uani 1 1 d . . .
C14 C 0.8182(4) 0.04707(18) 0.1620(3) 0.0426(15) Uani 1 1 d . . .
H14 H 0.7818 0.0330 0.2189 0.051 Uiso 1 1 calc R . .
C15 C 0.9043(4) 0.00632(19) 0.1121(3) 0.0442(15) Uani 1 1 d . . .
H15 H 0.9266 -0.0349 0.1386 0.053 Uiso 1 1 calc R . .
C16 C 0.9584(4) 0.02265(18) 0.0267(4) 0.0404(15) Uani 1 1 d . . .
C17 C 0.9304(5) 0.08616(19) -0.0048(4) 0.057 Uani 1 1 d . . .
H17 H 0.9690 0.1010 -0.0605 0.069 Uiso 1 1 calc R . .
C18 C 0.8465(5) 0.1282(2) 0.0440(4) 0.0681(18) Uani 1 1 d . . .
H18 H 0.8300 0.1706 0.0208 0.082 Uiso 1 1 calc R . .
C19 C 0.7965(4) 0.26624(16) 0.4446(3) 0.0250(11) Uani 1 1 d . . .
C20 C 0.8249(4) 0.29541(16) 0.3469(3) 0.0212(11) Uani 1 1 d . . .
C21 C 0.7075(4) 0.33205(16) 0.2927(3) 0.0210(11) Uani 1 1 d . . .
C22 C 0.7343(4) 0.36196(16) 0.2044(3) 0.0213(11) Uani 1 1 d . . .
C23 C 0.8716(4) 0.35678(16) 0.1716(3) 0.0242(11) Uani 1 1 d . . .
H23 H 0.8871 0.3781 0.1135 0.029 Uiso 1 1 calc R . .
C24 C 0.9876(4) 0.31943(16) 0.2257(3) 0.0236(11) Uani 1 1 d . . .
C25 C 0.9619(4) 0.28873(17) 0.3122(3) 0.0240(11) Uani 1 1 d . . .
H25 H 1.0376 0.2631 0.3479 0.029 Uiso 1 1 calc R . .
C26 C 1.1349(4) 0.31264(17) 0.1893(3) 0.0265(12) Uani 1 1 d . . .
C27 C 0.6062(4) 0.40028(17) 0.1424(3) 0.0271(12) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.0000 0.0325(2) Uani 1 2 d S . .
Cu2 Cu 0.35548(5) 0.28735(2) 0.12343(4) 0.02746(14) Uani 1 1 d . . .
N1 N 0.5817(3) 0.45607(14) -0.1074(2) 0.0252(9) Uani 1 1 d . . .
N2 N 0.7150(3) 0.44082(14) -0.2279(2) 0.0279(10) Uani 1 1 d . . .
N3 N 0.5106(3) 0.22322(14) 0.1720(2) 0.0302(10) Uani 1 1 d . . .
N4 N 0.6902(3) 0.15088(15) 0.1679(3) 0.0358(11) Uani 1 1 d . . .
O1 O 0.6905(3) 0.28672(12) 0.4826(2) 0.0380(8) Uani 1 1 d . . .
O2 O 0.8895(3) 0.22281(11) 0.48450(19) 0.0288(8) Uani 1 1 d . . .
O3 O 1.2378(3) 0.27778(12) 0.23812(19) 0.0319(8) Uani 1 1 d . . .
O4 O 1.1554(3) 0.33869(12) 0.1094(2) 0.0318(8) Uani 1 1 d . . .
O5 O 0.6431(3) 0.44800(12) 0.0946(2) 0.0352(9) Uani 1 1 d . . .
O6 O 0.4730(3) 0.38180(11) 0.1445(2) 0.0359(9) Uani 1 1 d . . .
O8 O 0.8717(13) 0.2655(5) 0.9540(11) 0.285(8) Uani 0.50 1 d P . .
H8B H 0.9650 0.2631 0.9789 0.428 Uiso 0.50 1 d PR . .
H8C H 0.8346 0.3002 0.9738 0.428 Uiso 0.50 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O9 H9B 0.8500 . ?
O9 H9C 0.8499 . ?
O7 Cu1 2.598(5) . ?
O7 H7A 0.8500 . ?
O7 H7C 0.8501 . ?
C1 C2 1.336(6) . ?
C1 N1 1.374(4) . ?
C1 H1 0.9300 . ?
C2 N2 1.378(4) . ?
C2 H2 0.9300 . ?
C3 N1 1.285(5) . ?
C3 N2 1.349(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(5) . ?
C4 C9 1.376(5) . ?
C4 N2 1.426(5) . ?
C5 C6 1.382(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.375(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(5) . ?
C7 C7 1.466(7) 3_764 ?
C8 C9 1.379(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.346(5) . ?
C10 N3 1.359(5) . ?
C10 H10 0.9300 . ?
C11 N4 1.368(6) . ?
C11 H11 0.9300 . ?
C12 N3 1.306(5) . ?
C12 N4 1.339(4) . ?
C12 H12 0.9300 . ?
C13 C18 1.354(7) . ?
C13 C14 1.368(5) . ?
C13 N4 1.427(5) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.366(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(5) . ?
C16 C16 1.457(8) 3_755 ?
C17 C18 1.383(6) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O1 1.227(4) . ?
C19 O2 1.280(4) . ?
C19 C20 1.510(5) . ?
C20 C25 1.391(5) . ?
C20 C21 1.400(4) . ?
C21 C22 1.399(5) . ?
C22 C23 1.379(5) . ?
C22 C27 1.526(5) . ?
C23 C24 1.399(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.382(5) . ?
C24 C26 1.488(5) . ?
C25 H25 0.9300 . ?
C26 O4 1.247(4) . ?
C26 O3 1.265(4) . ?
C26 Cu2 2.357(4) 1_655 ?
C27 O5 1.250(4) . ?
C27 O6 1.258(4) . ?
Cu1 N1 1.953(3) . ?
Cu1 N1 1.953(3) 3_665 ?
Cu1 O5 1.972(2) . ?
Cu1 O5 1.972(2) 3_665 ?
Cu2 N3 1.951(3) . ?
Cu2 O2 1.963(3) 4_565 ?
Cu2 O3 2.024(3) 1_455 ?
Cu2 O4 2.063(2) 1_455 ?
Cu2 O6 2.208(2) . ?
Cu2 C26 2.357(4) 1_455 ?
O2 Cu2 1.963(3) 4_666 ?
O3 Cu2 2.024(3) 1_655 ?
O4 Cu2 2.063(2) 1_655 ?
O8 H8B 0.8501 . ?
O8 H8C 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
H9B O9 H9C 109.5 . . ?
Cu1 O7 H7A 110.1 . . ?
Cu1 O7 H7C 109.4 . . ?
H7A O7 H7C 109.4 . . ?
C2 C1 N1 109.5(3) . . ?
C2 C1 H1 125.3 . . ?
N1 C1 H1 125.3 . . ?
C1 C2 N2 106.9(3) . . ?
C1 C2 H2 126.5 . . ?
N2 C2 H2 126.5 . . ?
N1 C3 N2 112.8(3) . . ?
N1 C3 H3 123.6 . . ?
N2 C3 H3 123.6 . . ?
C5 C4 C9 119.0(4) . . ?
C5 C4 N2 120.7(3) . . ?
C9 C4 N2 120.3(4) . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C7 C6 C5 122.9(4) . . ?
C7 C6 H6 118.5 . . ?
C5 C6 H6 118.5 . . ?
C6 C7 C8 115.8(4) . . ?
C6 C7 C7 122.5(4) . 3_764 ?
C8 C7 C7 121.6(4) . 3_764 ?
C7 C8 C9 122.5(4) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C4 C9 C8 119.9(4) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 N3 110.9(4) . . ?
C11 C10 H10 124.5 . . ?
N3 C10 H10 124.5 . . ?
C10 C11 N4 105.7(4) . . ?
C10 C11 H11 127.2 . . ?
N4 C11 H11 127.2 . . ?
N3 C12 N4 112.6(4) . . ?
N3 C12 H12 123.7 . . ?
N4 C12 H12 123.7 . . ?
C18 C13 C14 119.6(4) . . ?
C18 C13 N4 119.2(4) . . ?
C14 C13 N4 121.0(4) . . ?
C13 C14 C15 118.2(4) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C16 C15 C14 124.4(4) . . ?
C16 C15 H15 117.8 . . ?
C14 C15 H15 117.8 . . ?
C15 C16 C17 114.9(4) . . ?
C15 C16 C16 122.9(5) . 3_755 ?
C17 C16 C16 122.3(6) . 3_755 ?
C18 C17 C16 122.0(5) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C13 C18 C17 120.7(4) . . ?
C13 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
O1 C19 O2 124.0(4) . . ?
O1 C19 C20 118.9(3) . . ?
O2 C19 C20 117.0(3) . . ?
C25 C20 C21 120.4(3) . . ?
C25 C20 C19 122.8(3) . . ?
C21 C20 C19 116.8(3) . . ?
C22 C21 C20 117.6(3) . . ?
C23 C22 C21 121.9(3) . . ?
C23 C22 C27 119.6(3) . . ?
C21 C22 C27 118.5(3) . . ?
C22 C23 C24 120.0(4) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 118.7(4) . . ?
C25 C24 C26 121.1(3) . . ?
C23 C24 C26 120.2(3) . . ?
C24 C25 C20 121.3(3) . . ?
C24 C25 H25 119.3 . . ?
C20 C25 H25 119.3 . . ?
O4 C26 O3 119.8(4) . . ?
O4 C26 C24 120.7(3) . . ?
O3 C26 C24 119.4(3) . . ?
O4 C26 Cu2 61.0(2) . 1_655 ?
O3 C26 Cu2 59.1(2) . 1_655 ?
C24 C26 Cu2 171.9(3) . 1_655 ?
O5 C27 O6 125.6(3) . . ?
O5 C27 C22 116.8(3) . . ?
O6 C27 C22 117.5(3) . . ?
N1 Cu1 N1 180.000(1) . 3_665 ?
N1 Cu1 O5 86.97(11) . . ?
N1 Cu1 O5 93.03(11) 3_665 . ?
N1 Cu1 O5 93.03(11) . 3_665 ?
N1 Cu1 O5 86.97(11) 3_665 3_665 ?
O5 Cu1 O5 180.0 . 3_665 ?
N1 Cu1 O7 92.02(15) . . ?
N1 Cu1 O7 87.98(15) 3_665 . ?
O5 Cu1 O7 104.89(13) . . ?
O5 Cu1 O7 75.11(14) 3_665 . ?
N3 Cu2 O2 92.04(12) . 4_565 ?
N3 Cu2 O3 96.25(12) . 1_455 ?
O2 Cu2 O3 154.90(10) 4_565 1_455 ?
N3 Cu2 O4 159.72(13) . 1_455 ?
O2 Cu2 O4 103.67(10) 4_565 1_455 ?
O3 Cu2 O4 64.24(10) 1_455 1_455 ?
N3 Cu2 O6 104.72(11) . . ?
O2 Cu2 O6 94.08(10) 4_565 . ?
O3 Cu2 O6 106.55(10) 1_455 . ?
O4 Cu2 O6 87.12(10) 1_455 . ?
N3 Cu2 C26 128.17(14) . 1_455 ?
O2 Cu2 C26 131.11(11) 4_565 1_455 ?
O3 Cu2 C26 32.45(10) 1_455 1_455 ?
O4 Cu2 C26 31.89(11) 1_455 1_455 ?
O6 Cu2 C26 99.73(11) . 1_455 ?
C3 N1 C1 105.6(3) . . ?
C3 N1 Cu1 125.2(3) . . ?
C1 N1 Cu1 128.7(3) . . ?
C3 N2 C2 105.2(3) . . ?
C3 N2 C4 126.4(3) . . ?
C2 N2 C4 128.4(3) . . ?
C12 N3 C10 104.5(3) . . ?
C12 N3 Cu2 125.0(3) . . ?
C10 N3 Cu2 130.2(3) . . ?
C12 N4 C11 106.3(3) . . ?
C12 N4 C13 125.4(4) . . ?
C11 N4 C13 127.7(3) . . ?
C19 O2 Cu2 106.5(2) . 4_666 ?
C26 O3 Cu2 88.4(2) . 1_655 ?
C26 O4 Cu2 87.1(2) . 1_655 ?
C27 O5 Cu1 124.2(2) . . ?
C27 O6 Cu2 134.3(2) . . ?
H8B O8 H8C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.088


