# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'George Newkome'
'Charles N. Moorefield'
'Matthew Panzer'
'Pingshan Wang.'

_publ_contact_author_name        'Prof George Newkome'
_publ_contact_author_address     
;
Polymer Science
University of Akron
170 University Cr.
Akron
OH
44325-4717
UNITED STATES OF AMERICA
;

_publ_contact_author_email       NEWKOME@UAKRON.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Terpyridine copperII-polycarboxylic acid
architectures: formation of dimeric, helical, and cyclic nanostructures
and their included-water molecule motifs
;

data_mp
_database_code_depnum_ccdc_archive 'CCDC 269332'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H26 Cu2 N6 O10'
_chemical_formula_sum            'C44 H26 Cu2 N6 O10'
_chemical_formula_weight         925.79

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.198(4)
_cell_length_b                   12.339(7)
_cell_length_c                   12.865(8)
_cell_angle_alpha                89.136(9)
_cell_angle_beta                 84.562(10)
_cell_angle_gamma                82.987(10)
_cell_volume                     1129.0(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3893
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      28.14

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             470
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
Platon Squeeze was used to remove dissordered solvent waters.
Total (Positive) Electron Count in Voids/Cell = 88
Total (Fo-Fc)map Electron Count in Unit Cell = 88
N: Number of moved primary input atoms: .................................. 44
W: Number of unusual anisotropic displacement parameters ................. 1
N: Total Potential Solvent Accessible Void Vol .................. 257.2 Ang3
N: Electron Count / Cell = 88 - To be included in D(calc), F000 & Mol.Wght.
;

_diffrn_ambient_temperature      100(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            9412
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         28.34
_reflns_number_total             5058
_reflns_number_gt                4000
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1592P)^2^+1.0312P] where P=(Fo^2^+2Fc^2^)/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         5058
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0773
_refine_ls_wR_factor_ref         0.2712
_refine_ls_wR_factor_gt          0.2252
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_restrained_S_all      1.201
_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
Cu1 Cu 0.56803(9) 0.68714(4) 0.87471(4) 0.0216(2) Uani 1 1 d . . .
O1 O 0.8343(6) 0.7618(3) 0.8416(3) 0.0339(9) Uani 1 1 d . . .
O2 O 0.5131(5) 0.6477(3) 0.7392(3) 0.0236(7) Uani 1 1 d . . .
O3 O 0.5772(7) 0.7923(3) 0.6417(3) 0.0362(10) Uani 1 1 d . . .
O4 O 0.9278(6) 0.3837(3) 0.2695(3) 0.0334(9) Uani 1 1 d . . .
O5 O 0.8153(6) 0.2699(3) 0.3889(3) 0.0340(9) Uani 1 1 d . . .
N1 N 0.7076(6) 0.5361(4) 0.9006(3) 0.0240(9) Uani 1 1 d . . .
N2 N 0.5676(6) 0.6908(3) 1.0256(3) 0.0221(8) Uani 1 1 d . . .
N3 N 0.4030(7) 0.8278(4) 0.9068(3) 0.0281(10) Uani 1 1 d . . .
C1 C 0.7749(8) 0.4619(4) 0.8291(4) 0.0253(10) Uani 1 1 d . . .
H1A H 0.7539 0.4765 0.7582 0.030 Uiso 1 1 calc R . .
C2 C 0.8760(8) 0.3629(4) 0.8549(4) 0.0288(11) Uani 1 1 d . . .
H2 H 0.9269 0.3117 0.8023 0.035 Uiso 1 1 calc R . .
C3 C 0.9003(7) 0.3413(4) 0.9578(4) 0.0273(11) Uani 1 1 d . . .
H3 H 0.9659 0.2736 0.9772 0.033 Uiso 1 1 calc R . .
C4 C 0.8287(7) 0.4184(4) 1.0340(4) 0.0258(10) Uani 1 1 d . . .
H4 H 0.8448 0.4046 1.1057 0.031 Uiso 1 1 calc R . .
C5 C 0.7335(8) 0.5156(4) 1.0021(4) 0.0244(10) Uani 1 1 d . . .
C6 C 0.6536(7) 0.6047(4) 1.0745(4) 0.0212(9) Uani 1 1 d . . .
C7 C 0.6644(9) 0.6046(5) 1.1811(4) 0.0320(12) Uani 1 1 d . . .
H7 H 0.7270 0.5444 1.2162 0.038 Uiso 1 1 calc R . .
C8 C 0.5771(8) 0.6989(5) 1.2351(4) 0.0314(12) Uani 1 1 d . . .
H8 H 0.5816 0.7025 1.3086 0.038 Uiso 1 1 calc R . .
C9 C 0.4864(8) 0.7852(5) 1.1849(4) 0.0286(11) Uani 1 1 d . . .
H9 H 0.4264 0.8475 1.2226 0.034 Uiso 1 1 calc R . .
C10 C 0.4842(7) 0.7794(4) 1.0772(4) 0.0232(10) Uani 1 1 d . . .
C11 C 0.3880(8) 0.8583(4) 1.0095(4) 0.0277(11) Uani 1 1 d . . .
C12 C 0.2923(9) 0.9582(5) 1.0445(5) 0.0339(13) Uani 1 1 d . . .
H12 H 0.2837 0.9778 1.1161 0.041 Uiso 1 1 calc R . .
C13 C 0.2105(10) 1.0280(5) 0.9719(6) 0.0397(15) Uani 1 1 d . . .
H13 H 0.1482 1.0976 0.9932 0.048 Uiso 1 1 calc R . .
C14 C 0.2188(10) 0.9973(5) 0.8696(5) 0.0385(14) Uani 1 1 d . . .
H14 H 0.1610 1.0448 0.8201 0.046 Uiso 1 1 calc R . .
C15 C 0.3124(9) 0.8959(5) 0.8387(5) 0.0338(12) Uani 1 1 d . . .
H15 H 0.3132 0.8737 0.7683 0.041 Uiso 1 1 calc R . .
C16 C 0.5848(8) 0.6213(4) 0.5586(4) 0.0242(10) Uani 1 1 d . . .
C17 C 0.7526(8) 0.6249(4) 0.5017(4) 0.0273(11) Uani 1 1 d . . .
H17 H 0.8240 0.6830 0.5120 0.033 Uiso 1 1 calc R . .
C18 C 0.8228(7) 0.5432(4) 0.4270(4) 0.0249(10) Uani 1 1 d . . .
H18 H 0.9404 0.5469 0.3875 0.030 Uiso 1 1 calc R . .
C19 C 0.7203(9) 0.4585(4) 0.4117(4) 0.0275(11) Uani 1 1 d . . .
C20 C 0.4661(7) 0.5417(4) 0.5379(3) 0.0211(10) Uani 1 1 d . . .
C26 C 0.5511(9) 0.6961(4) 0.6523(4) 0.0295(11) Uani 1 1 d . . .
C27 C 0.8252(8) 0.3627(4) 0.3504(4) 0.0276(11) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0297(4) 0.0182(3) 0.0166(3) -0.0054(2) 0.0022(2) -0.0049(2)
O1 0.044(2) 0.030(2) 0.028(2) -0.0142(16) 0.0058(17) -0.0119(18)
O2 0.0299(19) 0.0188(16) 0.0214(17) -0.0014(13) -0.0019(14) -0.0003(14)
O3 0.049(3) 0.0206(18) 0.037(2) -0.0032(16) 0.0062(19) -0.0049(17)
O4 0.038(2) 0.039(2) 0.0230(19) -0.0086(16) 0.0077(16) -0.0107(18)
O5 0.040(2) 0.029(2) 0.029(2) 0.0016(15) 0.0083(17) 0.0011(17)
N1 0.027(2) 0.024(2) 0.022(2) -0.0047(16) 0.0003(16) -0.0101(17)
N2 0.021(2) 0.0188(19) 0.027(2) -0.0056(16) -0.0030(16) -0.0010(16)
N3 0.041(3) 0.022(2) 0.022(2) -0.0032(16) 0.0032(18) -0.0097(19)
C1 0.030(3) 0.024(2) 0.023(2) -0.0021(19) 0.000(2) -0.008(2)
C2 0.026(3) 0.026(2) 0.033(3) -0.007(2) 0.011(2) -0.010(2)
C3 0.023(3) 0.020(2) 0.038(3) 0.000(2) 0.005(2) -0.0046(19)
C4 0.016(2) 0.029(3) 0.033(3) 0.002(2) 0.0029(19) -0.0098(19)
C5 0.030(3) 0.022(2) 0.022(2) -0.0009(18) 0.0051(19) -0.012(2)
C6 0.020(2) 0.022(2) 0.022(2) -0.0013(18) 0.0018(18) -0.0064(18)
C7 0.038(3) 0.039(3) 0.023(3) -0.003(2) -0.004(2) -0.017(3)
C8 0.031(3) 0.046(3) 0.019(2) -0.007(2) 0.003(2) -0.016(2)
C9 0.023(3) 0.035(3) 0.027(3) -0.013(2) 0.003(2) -0.007(2)
C10 0.022(2) 0.021(2) 0.026(2) -0.0084(19) 0.0038(19) -0.0060(19)
C11 0.036(3) 0.025(2) 0.024(2) -0.007(2) 0.003(2) -0.013(2)
C12 0.035(3) 0.027(3) 0.041(3) -0.015(2) 0.005(2) -0.012(2)
C13 0.046(4) 0.017(2) 0.056(4) -0.012(2) 0.006(3) -0.007(2)
C14 0.042(3) 0.028(3) 0.044(4) 0.004(2) 0.004(3) -0.003(2)
C15 0.036(3) 0.031(3) 0.034(3) 0.000(2) 0.006(2) -0.007(2)
C16 0.034(3) 0.020(2) 0.018(2) 0.0001(17) -0.0038(19) 0.000(2)
C17 0.039(3) 0.022(2) 0.022(2) -0.0024(19) -0.004(2) -0.008(2)
C18 0.022(2) 0.032(3) 0.020(2) -0.0005(19) 0.0001(18) -0.002(2)
C19 0.044(3) 0.026(2) 0.013(2) -0.0031(18) 0.001(2) -0.008(2)
C20 0.027(3) 0.023(2) 0.013(2) 0.0001(18) -0.0001(18) -0.0028(19)
C26 0.039(3) 0.025(3) 0.024(3) -0.008(2) 0.002(2) -0.007(2)
C27 0.033(3) 0.031(3) 0.018(2) -0.0068(19) 0.001(2) -0.005(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 O2 1.906(4) . ?
Cu1 N2 1.942(5) . ?
Cu1 N3 2.005(5) . ?
Cu1 N1 2.044(5) . ?
Cu1 O1 2.229(4) . ?
O2 C26 1.282(7) . ?
O3 C26 1.228(6) . ?
O4 C27 1.260(7) . ?
O5 C27 1.248(7) . ?
N1 C1 1.324(7) . ?
N1 C5 1.351(7) . ?
N2 C10 1.334(6) . ?
N2 C6 1.342(7) . ?
N3 C15 1.360(8) . ?
N3 C11 1.370(7) . ?
C1 C2 1.396(8) . ?
C1 H1A 0.9500 . ?
C2 C3 1.369(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.477(7) . ?
C6 C7 1.381(7) . ?
C7 C8 1.413(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.366(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.453(8) . ?
C11 C12 1.396(8) . ?
C12 C13 1.384(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.357(8) . ?
C16 C20 1.422(7) . ?
C16 C26 1.512(7) . ?
C17 C18 1.416(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.434(8) 2_666 ?
C19 C27 1.513(7) . ?
C20 C19 1.434(8) 2_666 ?
C20 C20 1.436(9) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N2 160.68(17) . . ?
O2 Cu1 N3 104.79(17) . . ?
N2 Cu1 N3 79.50(18) . . ?
O2 Cu1 N1 92.55(16) . . ?
N2 Cu1 N1 79.90(17) . . ?
N3 Cu1 N1 158.28(19) . . ?
O2 Cu1 O1 102.83(15) . . ?
N2 Cu1 O1 95.32(16) . . ?
N3 Cu1 O1 95.94(18) . . ?
N1 Cu1 O1 92.77(17) . . ?
C26 O2 Cu1 127.7(3) . . ?
C1 N1 C5 119.7(5) . . ?
C1 N1 Cu1 126.6(4) . . ?
C5 N1 Cu1 113.8(3) . . ?
C10 N2 C6 122.1(5) . . ?
C10 N2 Cu1 119.1(4) . . ?
C6 N2 Cu1 118.9(3) . . ?
C15 N3 C11 117.9(5) . . ?
C15 N3 Cu1 127.7(4) . . ?
C11 N3 Cu1 114.4(4) . . ?
N1 C1 C2 121.9(5) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 118.6(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.1(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 117.9(5) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N1 C5 C4 121.8(5) . . ?
N1 C5 C6 114.8(5) . . ?
C4 C5 C6 123.4(5) . . ?
N2 C6 C7 121.4(5) . . ?
N2 C6 C5 112.7(4) . . ?
C7 C6 C5 125.9(5) . . ?
C6 C7 C8 116.2(6) . . ?
C6 C7 H7 121.9 . . ?
C8 C7 H7 121.9 . . ?
C9 C8 C7 122.0(5) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C10 118.2(5) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
N2 C10 C9 120.2(5) . . ?
N2 C10 C11 112.4(5) . . ?
C9 C10 C11 127.3(5) . . ?
N3 C11 C12 122.3(5) . . ?
N3 C11 C10 114.3(5) . . ?
C12 C11 C10 123.4(5) . . ?
C13 C12 C11 118.1(5) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C14 C13 C12 120.3(5) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.5(6) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N3 C15 C14 121.7(6) . . ?
N3 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C20 120.8(5) . . ?
C17 C16 C26 114.6(5) . . ?
C20 C16 C26 124.0(5) . . ?
C16 C17 C18 121.0(5) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.8(5) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 120.6(5) . 2_666 ?
C18 C19 C27 115.6(5) . . ?
C20 C19 C27 123.4(4) 2_666 . ?
C16 C20 C19 122.9(4) . 2_666 ?
C16 C20 C20 118.9(6) . 2_666 ?
C19 C20 C20 118.2(5) 2_666 2_666 ?
O3 C26 O2 125.9(5) . . ?
O3 C26 C16 119.5(5) . . ?
O2 C26 C16 114.3(4) . . ?
O5 C27 O4 125.3(5) . . ?
O5 C27 C19 117.0(4) . . ?
O4 C27 C19 117.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.897
_diffrn_reflns_theta_full        26.30
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.782
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.167

data_mp1
_database_code_depnum_ccdc_archive 'CCDC 269333'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H28 Cu2 N8 O8'
_chemical_formula_weight         923.82

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           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   8.728(3)
_cell_length_b                   18.451(7)
_cell_length_c                   49.722(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8007(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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            14828
_diffrn_reflns_av_R_equivalents  0.2119
_diffrn_reflns_av_sigmaI/netI    0.1003
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1986
_reflns_number_gt                1761
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0198P)^2^+121.5375P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1986
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1533
_refine_ls_wR_factor_gt          0.1474
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_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 1.1250 0.1250 0.056161(16) 0.0134(2) Uani 1 2 d S . .
N1 N 1.1250 0.1250 0.01675(12) 0.0169(11) Uani 1 2 d S . .
N3 N 0.8750 0.3750 0.13228(12) 0.0229(12) Uani 1 2 d S . .
O2 O 0.9739(4) 0.25243(15) 0.04899(7) 0.0173(7) Uani 1 1 d . . .
O1 O 1.0625(3) 0.20038(15) 0.08646(7) 0.0163(7) Uani 1 1 d . . .
N2 N 0.9161(4) 0.07990(18) 0.04873(8) 0.0144(8) Uani 1 1 d . . .
C1 C 0.9936(5) 0.2517(2) 0.07386(9) 0.0127(9) Uani 1 1 d . . .
C2 C 0.8750 0.3750 0.07594(14) 0.0176(13) Uani 1 2 d S . .
H2 H 0.8750 0.3750 0.0568 0.021 Uiso 1 2 calc SR . .
C3 C 0.8801(5) 0.0743(2) 0.02221(9) 0.0144(9) Uani 1 1 d . . .
C4 C 1.1250 0.1250 -0.03867(14) 0.0189(14) Uani 1 2 d S . .
H4 H 1.1250 0.1250 -0.0578 0.023 Uiso 1 2 calc SR . .
C5 C 0.9972(5) 0.0987(2) -0.02440(10) 0.0162(9) Uani 1 1 d . . .
H5 H 0.9100 0.0806 -0.0337 0.019 Uiso 1 1 calc R . .
C6 C 1.0014(5) 0.0997(2) 0.00355(10) 0.0147(9) Uani 1 1 d . . .
C7 C 0.9328(5) 0.3155(2) 0.09011(10) 0.0148(9) Uani 1 1 d . . .
C8 C 0.8146(5) 0.0577(2) 0.06703(10) 0.0191(10) Uani 1 1 d . . .
H8 H 0.8410 0.0607 0.0855 0.023 Uiso 1 1 calc R . .
C9 C 0.9312(5) 0.3186(2) 0.11798(10) 0.0158(9) Uani 1 1 d . . .
H9 H 0.9721 0.2786 0.1276 0.019 Uiso 1 1 calc R . .
C10 C 0.6333(6) 0.0256(2) 0.03303(11) 0.0218(10) Uani 1 1 d . . .
H10 H 0.5359 0.0075 0.0278 0.026 Uiso 1 1 calc R . .
C11 C 0.7380(5) 0.0474(2) 0.01374(10) 0.0160(9) Uani 1 1 d . . .
H11 H 0.7140 0.0441 -0.0049 0.019 Uiso 1 1 calc R . .
C12 C 0.6712(5) 0.0304(2) 0.05994(10) 0.0208(10) Uani 1 1 d . . .
H12 H 0.6008 0.0154 0.0734 0.025 Uiso 1 1 calc R . .
O3 O 0.3435(5) 0.1250 0.1250 0.0230(10) Uani 1 2 d S . .
O4 O 0.6250 0.1981(5) 0.1250 0.032(2) Uani 0.50 2 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0169(4) 0.0088(4) 0.0146(4) 0.000 0.000 -0.0010(3)
N1 0.019(3) 0.012(2) 0.020(3) 0.000 0.000 0.002(2)
N3 0.033(3) 0.015(3) 0.020(3) 0.000 0.000 0.002(2)
O2 0.0243(16) 0.0129(15) 0.0146(17) -0.0011(13) 0.0015(13) 0.0015(12)
O1 0.0221(16) 0.0084(14) 0.0184(18) 0.0005(12) 0.0019(13) 0.0032(12)
N2 0.0147(18) 0.0100(16) 0.019(2) 0.0031(15) -0.0002(15) -0.0011(13)
C1 0.012(2) 0.0079(19) 0.018(2) 0.0011(17) 0.0022(17) -0.0020(15)
C2 0.020(3) 0.017(3) 0.016(3) 0.000 0.000 -0.003(3)
C3 0.020(2) 0.0085(18) 0.015(2) -0.0015(16) 0.0027(18) 0.0015(17)
C4 0.032(4) 0.008(3) 0.017(4) 0.000 0.000 0.001(3)
C5 0.024(2) 0.0083(19) 0.016(2) -0.0014(17) -0.0027(19) 0.0007(17)
C6 0.021(2) 0.0058(17) 0.017(2) -0.0006(16) -0.0007(19) 0.0016(16)
C7 0.017(2) 0.0059(19) 0.021(3) -0.0016(17) 0.0025(19) 0.0005(16)
C8 0.027(2) 0.0094(19) 0.021(3) -0.0004(18) 0.000(2) 0.0009(17)
C9 0.020(2) 0.010(2) 0.017(3) 0.0018(17) 0.0003(19) 0.0037(16)
C10 0.020(2) 0.017(2) 0.029(3) -0.003(2) -0.001(2) -0.0024(18)
C11 0.019(2) 0.015(2) 0.014(2) -0.0021(18) -0.0023(18) 0.0026(17)
C12 0.024(2) 0.018(2) 0.021(3) -0.0003(19) 0.006(2) -0.0028(18)
O3 0.027(2) 0.020(2) 0.022(3) 0.001(2) 0.000 0.000
O4 0.030(5) 0.032(5) 0.034(7) 0.000 -0.011(5) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.960(6) . ?
Cu1 N2 2.038(4) . ?
Cu1 N2 2.038(4) 14_645 ?
Cu1 O1 2.122(3) 14_645 ?
Cu1 O1 2.122(3) . ?
N1 C6 1.346(5) . ?
N1 C6 1.346(5) 14_645 ?
N3 C9 1.352(5) . ?
N3 C9 1.352(5) 2_655 ?
O2 C1 1.249(5) . ?
O1 C1 1.285(5) . ?
N2 C8 1.334(6) . ?
N2 C3 1.360(6) . ?
C1 C7 1.524(6) . ?
C2 C7 1.398(6) 2_655 ?
C2 C7 1.398(6) . ?
C3 C11 1.402(6) . ?
C3 C6 1.483(6) . ?
C4 C5 1.408(6) 14_645 ?
C4 C5 1.408(6) . ?
C5 C6 1.390(7) . ?
C7 C9 1.387(7) . ?
C8 C12 1.395(7) . ?
C10 C12 1.381(7) . ?
C10 C11 1.384(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N2 79.55(11) . . ?
N1 Cu1 N2 79.55(11) . 14_645 ?
N2 Cu1 N2 159.1(2) . 14_645 ?
N1 Cu1 O1 135.24(8) . 14_645 ?
N2 Cu1 O1 95.22(13) . 14_645 ?
N2 Cu1 O1 99.59(14) 14_645 14_645 ?
N1 Cu1 O1 135.24(8) . . ?
N2 Cu1 O1 99.59(14) . . ?
N2 Cu1 O1 95.22(13) 14_645 . ?
O1 Cu1 O1 89.51(17) 14_645 . ?
C6 N1 C6 121.7(6) . 14_645 ?
C6 N1 Cu1 119.2(3) . . ?
C6 N1 Cu1 119.2(3) 14_645 . ?
C9 N3 C9 116.5(6) . 2_655 ?
C1 O1 Cu1 104.9(3) . . ?
C8 N2 C3 119.0(4) . . ?
C8 N2 Cu1 126.5(3) . . ?
C3 N2 Cu1 114.4(3) . . ?
O2 C1 O1 123.8(4) . . ?
O2 C1 C7 118.0(4) . . ?
O1 C1 C7 118.3(4) . . ?
C7 C2 C7 119.5(6) 2_655 . ?
N2 C3 C11 121.5(4) . . ?
N2 C3 C6 114.7(4) . . ?
C11 C3 C6 123.8(4) . . ?
C5 C4 C5 119.5(6) 14_645 . ?
C6 C5 C4 118.5(4) . . ?
N1 C6 C5 120.9(4) . . ?
N1 C6 C3 112.1(4) . . ?
C5 C6 C3 127.0(4) . . ?
C9 C7 C2 117.9(4) . . ?
C9 C7 C1 124.4(4) . . ?
C2 C7 C1 117.7(5) . . ?
N2 C8 C12 122.3(5) . . ?
N3 C9 C7 124.1(4) . . ?
C12 C10 C11 119.7(4) . . ?
C10 C11 C3 118.6(4) . . ?
C10 C12 C8 118.9(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.121

data_mp2
_database_code_depnum_ccdc_archive 'CCDC 269334'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H28 Cu2 N8 O8, 6(H2O)'
_chemical_formula_sum            'C44 H28 Cu2 N8 O14'
_chemical_formula_weight         1019.82

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '

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

_cell_length_a                   9.263(3)
_cell_length_b                   10.844(3)
_cell_length_c                   12.754(4)
_cell_angle_alpha                113.383(5)
_cell_angle_beta                 93.110(5)
_cell_angle_gamma                111.129(5)
_cell_volume                     1067.3(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3489
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.11

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             518
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7176
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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            8969
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         28.34
_reflns_number_total             4853
_reflns_number_gt                3948
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constrC44
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4853
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1645
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Cu Cu 0.83543(5) 0.27777(5) 0.15538(3) 0.01094(16) Uani 1 1 d . . .
O1 O 0.8880(3) 0.5043(3) 0.2756(2) 0.0157(5) Uani 1 1 d . . .
O2 O 0.6499(3) 0.5077(3) 0.2369(2) 0.0167(6) Uani 1 1 d . . .
O3 O 1.0680(3) 0.7374(3) 0.7172(2) 0.0158(5) Uani 1 1 d . . .
O4 O 1.1009(3) 0.9730(3) 0.8187(2) 0.0207(6) Uani 1 1 d . . .
O5 O 0.6460(4) 0.0740(4) 0.4807(3) 0.0339(8) Uani 1 1 d . . .
O6 O 0.4283(4) 0.4894(4) 0.3950(3) 0.0367(8) Uani 1 1 d . . .
O7 O 0.2224(4) 0.6248(4) 0.3944(3) 0.0360(8) Uani 1 1 d . . .
N1 N 0.6086(3) 0.1934(3) 0.1654(3) 0.0123(6) Uani 1 1 d . . .
N2 N 0.7303(3) 0.2483(3) 0.0067(3) 0.0115(6) Uani 1 1 d . . .
N3 N 1.0236(3) 0.3239(3) 0.0818(3) 0.0114(6) Uani 1 1 d . . .
N4 N 0.8265(4) 0.9287(3) 0.5238(3) 0.0149(6) Uani 1 1 d . . .
C1 C 0.5594(4) 0.1749(4) 0.2558(3) 0.0167(8) Uani 1 1 d . . .
H1 H 0.6359 0.1968 0.3207 0.020 Uiso 1 1 calc R . .
C2 C 0.3999(5) 0.1247(4) 0.2592(3) 0.0190(8) Uani 1 1 d . . .
H2 H 0.3677 0.1138 0.3257 0.023 Uiso 1 1 calc R . .
C3 C 0.2884(4) 0.0907(4) 0.1634(3) 0.0169(8) Uani 1 1 d . . .
H3 H 0.1783 0.0547 0.1628 0.020 Uiso 1 1 calc R . .
C4 C 0.3391(4) 0.1099(4) 0.0686(3) 0.0148(7) Uani 1 1 d . . .
H4 H 0.2645 0.0857 0.0017 0.018 Uiso 1 1 calc R . .
C5 C 0.5002(4) 0.1647(4) 0.0730(3) 0.0127(7) Uani 1 1 d . . .
C6 C 0.5719(4) 0.1971(4) -0.0191(3) 0.0123(7) Uani 1 1 d . . .
C7 C 0.4925(5) 0.1763(4) -0.1234(3) 0.0173(8) Uani 1 1 d . . .
H7 H 0.3798 0.1389 -0.1431 0.021 Uiso 1 1 calc R . .
C8 C 0.5838(5) 0.2123(4) -0.1990(3) 0.0176(8) Uani 1 1 d . . .
H8 H 0.5326 0.2020 -0.2705 0.021 Uiso 1 1 calc R . .
C9 C 0.7472(5) 0.2625(4) -0.1721(3) 0.0164(8) Uani 1 1 d . . .
H9 H 0.8088 0.2851 -0.2245 0.020 Uiso 1 1 calc R . .
C10 C 0.8183(4) 0.2788(4) -0.0668(3) 0.0124(7) Uani 1 1 d . . .
C11 C 0.9905(4) 0.3250(4) -0.0217(3) 0.0140(7) Uani 1 1 d . . .
C12 C 1.1064(4) 0.3620(4) -0.0807(3) 0.0160(8) Uani 1 1 d . . .
H12 H 1.0797 0.3613 -0.1540 0.019 Uiso 1 1 calc R . .
C13 C 1.2631(5) 0.4004(4) -0.0314(3) 0.0185(8) Uani 1 1 d . . .
H13 H 1.3453 0.4263 -0.0703 0.022 Uiso 1 1 calc R . .
C14 C 1.2964(4) 0.4000(4) 0.0740(3) 0.0157(8) Uani 1 1 d . . .
H14 H 1.4027 0.4259 0.1094 0.019 Uiso 1 1 calc R . .
C15 C 1.1744(4) 0.3614(4) 0.1295(3) 0.0148(7) Uani 1 1 d . . .
H15 H 1.1987 0.3618 0.2030 0.018 Uiso 1 1 calc R . .
C16 C 0.7836(4) 0.5572(4) 0.2997(3) 0.0140(7) Uani 1 1 d . . .
C17 C 0.8337(4) 0.6932(4) 0.4150(3) 0.0124(7) Uani 1 1 d . . .
C18 C 0.9240(4) 0.7099(4) 0.5132(3) 0.0127(7) Uani 1 1 d . . .
H18 H 0.9573 0.6354 0.5097 0.015 Uiso 1 1 calc R . .
C19 C 0.9654(4) 0.8371(4) 0.6170(3) 0.0117(7) Uani 1 1 d . . .
C20 C 1.0531(4) 0.8545(4) 0.7280(3) 0.0138(7) Uani 1 1 d . . .
C21 C 0.9157(4) 0.9437(4) 0.6172(3) 0.0127(7) Uani 1 1 d . . .
H21 H 0.9471 1.0322 0.6879 0.015 Uiso 1 1 calc R . .
C22 C 0.7851(4) 0.8040(4) 0.4260(3) 0.0147(7) Uani 1 1 d . . .
H22 H 0.7181 0.7898 0.3593 0.018 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.0089(2) 0.0150(3) 0.0093(2) 0.00614(18) 0.00003(16) 0.00492(18)
O1 0.0149(13) 0.0157(13) 0.0149(13) 0.0050(11) 0.0031(10) 0.0068(11)
O2 0.0141(13) 0.0205(14) 0.0147(13) 0.0072(11) -0.0020(10) 0.0079(11)
O3 0.0162(13) 0.0208(14) 0.0142(13) 0.0097(11) 0.0004(10) 0.0099(11)
O4 0.0199(14) 0.0237(15) 0.0117(13) 0.0025(11) -0.0029(11) 0.0089(12)
O5 0.0334(18) 0.0311(17) 0.0368(18) 0.0107(15) -0.0040(14) 0.0196(15)
O6 0.0336(19) 0.041(2) 0.045(2) 0.0226(17) 0.0189(16) 0.0204(16)
O7 0.0208(16) 0.0329(18) 0.0402(19) 0.0065(15) 0.0004(14) 0.0083(14)
N1 0.0106(14) 0.0126(15) 0.0109(14) 0.0042(12) 0.0003(11) 0.0034(12)
N2 0.0105(14) 0.0087(14) 0.0125(14) 0.0029(12) 0.0006(11) 0.0035(11)
N3 0.0088(14) 0.0145(15) 0.0126(14) 0.0070(12) 0.0015(11) 0.0056(12)
N4 0.0134(15) 0.0172(16) 0.0168(16) 0.0086(13) 0.0050(12) 0.0076(13)
C1 0.0146(18) 0.0214(19) 0.0168(18) 0.0100(16) 0.0034(14) 0.0087(15)
C2 0.021(2) 0.023(2) 0.0172(19) 0.0108(16) 0.0089(15) 0.0105(16)
C3 0.0127(18) 0.0176(19) 0.0205(19) 0.0074(16) 0.0068(14) 0.0072(15)
C4 0.0145(18) 0.0109(17) 0.0151(18) 0.0045(14) -0.0003(14) 0.0033(14)
C5 0.0122(17) 0.0105(16) 0.0142(17) 0.0034(14) 0.0019(13) 0.0058(14)
C6 0.0122(17) 0.0090(16) 0.0135(17) 0.0028(13) 0.0010(13) 0.0050(13)
C7 0.0143(18) 0.0198(19) 0.0145(18) 0.0069(15) -0.0013(14) 0.0051(15)
C8 0.0187(19) 0.023(2) 0.0132(18) 0.0102(15) -0.0020(14) 0.0092(16)
C9 0.0193(19) 0.0176(19) 0.0159(18) 0.0091(15) 0.0051(15) 0.0095(15)
C10 0.0125(17) 0.0124(17) 0.0107(16) 0.0046(14) 0.0011(13) 0.0045(14)
C11 0.0137(17) 0.0120(17) 0.0166(18) 0.0075(14) 0.0009(14) 0.0048(14)
C12 0.0180(19) 0.0206(19) 0.0127(17) 0.0097(15) 0.0034(14) 0.0090(15)
C13 0.0160(19) 0.0180(19) 0.022(2) 0.0106(16) 0.0067(15) 0.0059(15)
C14 0.0104(17) 0.0139(18) 0.0217(19) 0.0082(15) 0.0006(14) 0.0041(14)
C15 0.0139(18) 0.0163(18) 0.0151(18) 0.0078(15) -0.0022(14) 0.0069(15)
C16 0.0147(18) 0.0188(19) 0.0115(17) 0.0098(15) 0.0040(13) 0.0067(15)
C17 0.0095(16) 0.0128(17) 0.0139(17) 0.0069(14) 0.0024(13) 0.0025(14)
C18 0.0137(17) 0.0148(18) 0.0118(17) 0.0073(14) 0.0038(13) 0.0067(14)
C19 0.0082(16) 0.0152(17) 0.0107(16) 0.0060(14) 0.0008(13) 0.0037(13)
C20 0.0080(16) 0.0180(18) 0.0160(18) 0.0089(15) 0.0036(13) 0.0045(14)
C21 0.0127(17) 0.0118(17) 0.0119(17) 0.0045(14) 0.0024(13) 0.0042(14)
C22 0.0134(17) 0.0210(19) 0.0141(17) 0.0107(15) 0.0010(13) 0.0090(15)

_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
Cu O3 1.906(3) 2_766 ?
Cu N2 1.934(3) . ?
Cu N1 2.001(3) . ?
Cu N3 2.022(3) . ?
Cu O1 2.166(3) . ?
O1 C16 1.285(4) . ?
O2 C16 1.239(4) . ?
O3 C20 1.280(4) . ?
O3 Cu 1.906(3) 2_766 ?
O4 C20 1.241(4) . ?
N1 C1 1.324(5) . ?
N1 C5 1.359(4) . ?
N2 C6 1.335(5) . ?
N2 C10 1.336(5) . ?
N3 C15 1.337(4) . ?
N3 C11 1.345(5) . ?
N4 C22 1.329(5) . ?
N4 C21 1.331(5) . ?
C1 C2 1.388(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.389(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.479(5) . ?
C6 C7 1.379(5) . ?
C7 C8 1.396(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.491(5) . ?
C11 C12 1.377(5) . ?
C12 C13 1.390(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.366(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.505(5) . ?
C17 C18 1.378(5) . ?
C17 C22 1.388(5) . ?
C18 C19 1.384(5) . ?
C18 H18 0.9500 . ?
C19 C21 1.390(5) . ?
C19 C20 1.501(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?

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
O3 Cu N2 167.34(11) 2_766 . ?
O3 Cu N1 98.67(12) 2_766 . ?
N2 Cu N1 80.30(12) . . ?
O3 Cu N3 98.91(11) 2_766 . ?
N2 Cu N3 79.91(12) . . ?
N1 Cu N3 158.72(12) . . ?
O3 Cu O1 87.82(10) 2_766 . ?
N2 Cu O1 104.84(11) . . ?
N1 Cu O1 95.98(11) . . ?
N3 Cu O1 96.57(11) . . ?
C16 O1 Cu 124.8(2) . . ?
C20 O3 Cu 123.0(2) . 2_766 ?
C1 N1 C5 119.3(3) . . ?
C1 N1 Cu 125.8(2) . . ?
C5 N1 Cu 114.7(2) . . ?
C6 N2 C10 122.4(3) . . ?
C6 N2 Cu 118.6(2) . . ?
C10 N2 Cu 119.0(2) . . ?
C15 N3 C11 118.8(3) . . ?
C15 N3 Cu 126.4(3) . . ?
C11 N3 Cu 114.6(2) . . ?
C22 N4 C21 116.7(3) . . ?
N1 C1 C2 122.3(4) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 118.5(4) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 113.6(3) . . ?
C4 C5 C6 124.8(3) . . ?
N2 C6 C7 120.5(3) . . ?
N2 C6 C5 112.7(3) . . ?
C7 C6 C5 126.9(3) . . ?
C6 C7 C8 117.5(3) . . ?
C6 C7 H7 121.3 . . ?
C8 C7 H7 121.3 . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 117.9(3) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N2 C10 C9 120.3(3) . . ?
N2 C10 C11 112.3(3) . . ?
C9 C10 C11 127.3(3) . . ?
N3 C11 C12 122.2(3) . . ?
N3 C11 C10 113.8(3) . . ?
C12 C11 C10 123.9(3) . . ?
C11 C12 C13 119.0(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 118.7(4) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 119.8(3) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N3 C15 C14 121.5(3) . . ?
N3 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
O2 C16 O1 126.1(3) . . ?
O2 C16 C17 118.7(3) . . ?
O1 C16 C17 115.2(3) . . ?
C18 C17 C22 118.1(3) . . ?
C18 C17 C16 121.5(3) . . ?
C22 C17 C16 120.4(3) . . ?
C17 C18 C19 118.8(3) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C18 C19 C21 118.4(3) . . ?
C18 C19 C20 120.5(3) . . ?
C21 C19 C20 121.0(3) . . ?
O4 C20 O3 126.4(3) . . ?
O4 C20 C19 120.3(3) . . ?
O3 C20 C19 113.3(3) . . ?
N4 C21 C19 123.6(3) . . ?
N4 C21 H21 118.2 . . ?
C19 C21 H21 118.2 . . ?
N4 C22 C17 124.2(3) . . ?
N4 C22 H22 117.9 . . ?
C17 C22 H22 117.9 . . ?

_diffrn_measured_fraction_theta_max 0.911
_diffrn_reflns_theta_full        26.30
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.141