 
data_z 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C64 H80 Cu4 N64 O8' 
_chemical_formula_weight          2128.12 
 
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            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    22.834(2) 
_cell_length_b                    14.4584(12) 
_cell_length_c                    6.9109(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.391(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      2271.5(4) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(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     1.556 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1092 
_exptl_absorpt_coefficient_mu     1.013 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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             6361 
_diffrn_reflns_av_R_equivalents   0.0489 
_diffrn_reflns_av_sigmaI/netI     0.0780 
_diffrn_reflns_limit_h_min        -30 
_diffrn_reflns_limit_h_max        29 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          2.82 
_diffrn_reflns_theta_max          28.27 
_reflns_number_total              2815 
_reflns_number_gt                 2025 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1000P)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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2815 
_refine_ls_number_parameters      159 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0999 
_refine_ls_R_factor_gt            0.0695 
_refine_ls_wR_factor_ref          0.2070 
_refine_ls_wR_factor_gt           0.1879 
_refine_ls_goodness_of_fit_ref    1.221 
_refine_ls_restrained_S_all       1.221 
_refine_ls_shift/su_max           0.031 
_refine_ls_shift/su_mean          0.002 
 
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 
N7 N 0.05451(15) 0.1859(2) 0.1624(5) 0.0236(8) Uani 1 1 d . . . 
C1 C 0.0445(2) 0.2550(3) 0.0319(8) 0.0354(12) Uani 1 1 d . . . 
H1B H 0.0071 0.2650 -0.0373 0.043 Uiso 1 1 calc R . . 
C2 C 0.11112(18) 0.1955(3) 0.2203(6) 0.0238(9) Uani 1 1 d . . . 
H2A H 0.1329 0.1565 0.3113 0.029 Uiso 1 1 calc R . . 
C3 C 0.2033(2) 0.3935(3) 0.1031(8) 0.0298(10) Uani 1 1 d . . . 
H3A H 0.1727 0.4319 0.0459 0.036 Uiso 1 1 calc R . . 
C4 C 0.19186(17) 0.3034(3) 0.1586(6) 0.0222(9) Uani 1 1 d . . . 
C5 C 0.23559(18) 0.2470(3) 0.2418(6) 0.0243(9) Uani 1 1 d . . . 
H5A H 0.2271 0.1853 0.2773 0.029 Uiso 1 1 calc R . . 
C6 C 0.29261(18) 0.2817(3) 0.2735(6) 0.0235(9) Uani 1 1 d . . . 
H11A H 0.3230 0.2432 0.3321 0.028 Uiso 1 1 calc R . . 
C7 C 0.2611(2) 0.4265(3) 0.1333(8) 0.0296(11) Uani 1 1 d . . . 
H9B H 0.2699 0.4873 0.0932 0.035 Uiso 1 1 calc R . . 
C8 C 0.30577(18) 0.3712(3) 0.2213(6) 0.0211(9) Uani 1 1 d . . . 
C9 C 0.36614(18) 0.4058(3) 0.2668(6) 0.0195(8) Uani 1 1 d . . . 
Cu1 Cu 0.0000 0.08809(5) 0.2500 0.0205(3) Uani 1 2 d S . . 
O1 O 0.0798(6) 0.4246(7) 0.5239(19) 0.257(7) Uani 1 1 d . . . 
H1A H 0.0497 0.4409 0.5680 0.308 Uiso 1 1 d R . . 
H1C H 0.0952 0.4533 0.4341 0.308 Uiso 1 1 d R . . 
N1 N 0.40734(15) 0.3583(2) 0.3757(5) 0.0215(8) Uani 1 1 d . . . 
N2 N 0.45419(15) 0.4134(2) 0.3948(5) 0.0213(8) Uani 1 1 d . . . 
N3 N 0.44114(14) 0.4900(2) 0.2957(5) 0.0198(7) Uani 1 1 d . . . 
N4 N 0.38574(14) 0.4886(2) 0.2127(5) 0.0212(8) Uani 1 1 d . . . 
N5 N 0.13319(15) 0.2687(2) 0.1311(5) 0.0226(8) Uani 1 1 d . . . 
N6 N 0.09012(17) 0.3070(3) 0.0078(7) 0.0391(11) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
N7 C2 1.324(5) . ? 
N7 C1 1.351(6) . ? 
N7 Cu1 2.014(3) . ? 
C1 N6 1.308(6) . ? 
C1 H1B 0.9500 . ? 
C2 N5 1.346(5) . ? 
C2 H2A 0.9500 . ? 
C3 C4 1.391(6) . ? 
C3 C7 1.399(6) . ? 
C3 H3A 0.9500 . ? 
C4 C5 1.372(6) . ? 
C4 N5 1.426(5) . ? 
C5 C6 1.393(6) . ? 
C5 H5A 0.9500 . ? 
C6 C8 1.384(6) . ? 
C6 H11A 0.9500 . ? 
C7 C8 1.390(6) . ? 
C7 H9B 0.9500 . ? 
C8 C9 1.473(6) . ? 
C9 N1 1.338(5) . ? 
C9 N4 1.343(5) . ? 
Cu1 N3 1.999(3) 4_545 ? 
Cu1 N3 1.999(3) 3_445 ? 
Cu1 N7 2.014(3) 2 ? 
Cu1 N2 2.577(4) 8_455 ? 
Cu1 N2 2.577(4) 7_556 ? 
O1 H1A 0.8110 . ? 
O1 H1C 0.8501 . ? 
N1 N2 1.331(5) . ? 
N2 N3 1.321(5) . ? 
N2 Cu1 2.577(4) 7_556 ? 
N3 N4 1.339(4) . ? 
N3 Cu1 1.999(3) 3 ? 
N5 N6 1.357(5) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 N7 C1 102.9(4) . . ? 
C2 N7 Cu1 126.6(3) . . ? 
C1 N7 Cu1 130.5(3) . . ? 
N6 C1 N7 115.0(4) . . ? 
N6 C1 H1B 122.5 . . ? 
N7 C1 H1B 122.5 . . ? 
N7 C2 N5 109.9(4) . . ? 
N7 C2 H2A 125.0 . . ? 
N5 C2 H2A 125.0 . . ? 
C4 C3 C7 118.5(4) . . ? 
C4 C3 H3A 120.8 . . ? 
C7 C3 H3A 120.8 . . ? 
C5 C4 C3 121.5(4) . . ? 
C5 C4 N5 119.0(4) . . ? 
C3 C4 N5 119.4(4) . . ? 
C4 C5 C6 119.0(4) . . ? 
C4 C5 H5A 120.5 . . ? 
C6 C5 H5A 120.5 . . ? 
C8 C6 C5 121.2(4) . . ? 
C8 C6 H11A 119.4 . . ? 
C5 C6 H11A 119.4 . . ? 
C8 C7 C3 120.8(4) . . ? 
C8 C7 H9B 119.6 . . ? 
C3 C7 H9B 119.6 . . ? 
C6 C8 C7 118.9(4) . . ? 
C6 C8 C9 119.0(4) . . ? 
C7 C8 C9 122.1(4) . . ? 
N1 C9 N4 112.3(4) . . ? 
N1 C9 C8 122.7(4) . . ? 
N4 C9 C8 125.0(4) . . ? 
N3 Cu1 N3 89.65(19) 4_545 3_445 ? 
N3 Cu1 N7 90.40(14) 4_545 . ? 
N3 Cu1 N7 171.52(14) 3_445 . ? 
N3 Cu1 N7 171.52(14) 4_545 2 ? 
N3 Cu1 N7 90.39(14) 3_445 2 ? 
N7 Cu1 N7 90.8(2) . 2 ? 
N3 Cu1 N2 93.57(12) 4_545 8_455 ? 
N3 Cu1 N2 85.73(13) 3_445 8_455 ? 
N7 Cu1 N2 85.80(13) . 8_455 ? 
N7 Cu1 N2 94.89(13) 2 8_455 ? 
N3 Cu1 N2 85.73(13) 4_545 7_556 ? 
N3 Cu1 N2 93.57(12) 3_445 7_556 ? 
N7 Cu1 N2 94.89(13) . 7_556 ? 
N7 Cu1 N2 85.80(13) 2 7_556 ? 
N2 Cu1 N2 179.01(15) 8_455 7_556 ? 
H1A O1 H1C 123.8 . . ? 
N2 N1 C9 105.3(3) . . ? 
N3 N2 N1 108.1(3) . . ? 
N3 N2 Cu1 123.5(3) . 7_556 ? 
N1 N2 Cu1 109.9(3) . 7_556 ? 
N2 N3 N4 111.5(3) . . ? 
N2 N3 Cu1 123.6(3) . 3 ? 
N4 N3 Cu1 124.4(3) . 3 ? 
N3 N4 C9 102.8(3) . . ? 
C2 N5 N6 109.1(3) . . ? 
C2 N5 C4 127.1(4) . . ? 
N6 N5 C4 123.8(4) . . ? 
C1 N6 N5 103.0(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              28.27 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    1.231 
_refine_diff_density_min   -0.845 
_refine_diff_density_rms    0.129 
