data_cm43 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H80 Cu4 N8 O24' _chemical_formula_weight 1551.48 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 Tetragonal _symmetry_space_group_name_H-M P4nc 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' '-y+1/2, -x+1/2, z+1/2' 'y, -x, z' '-y, x, z' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.5453(11) _cell_length_b 17.5453(11) _cell_length_c 14.7194(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4531.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.65 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7805 _exptl_absorpt_correction_T_max 0.8161 _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 'STOE-IPDS I' _diffrn_measurement_method 'oscillation, phi incr.= 1.3' _diffrn_detector_area_resol_mean 6.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24502 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.89 _reflns_number_total 4350 _reflns_number_gt 2399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _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^)+(0.0546P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4350 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3260(3) -0.0357(4) -0.6651(4) 0.0367(15) Uani 1 1 d . . . C2 C 1.3319(3) 0.0382(3) -0.7135(3) 0.0319(12) Uani 1 1 d . . . C3 C 1.3812(4) 0.0463(4) -0.7851(4) 0.0357(15) Uani 1 1 d . . . H3A H 1.4086 0.0044 -0.8058 0.043 Uiso 1 1 calc R . . C4 C 1.3908(3) 0.1171(4) -0.8273(3) 0.0353(13) Uani 1 1 d . . . C5 C 1.4475(5) 0.1259(4) -0.9008(4) 0.0394(17) Uani 1 1 d . . . C6 C 1.3495(3) 0.1791(3) -0.7967(3) 0.0354(13) Uani 1 1 d . . . H6 H 1.3549 0.2262 -0.8249 0.043 Uiso 1 1 calc R . . C7 C 1.2994(3) 0.1710(3) -0.7232(3) 0.0350(14) Uani 1 1 d . . . C8 C 1.2903(3) 0.1017(3) -0.6836(3) 0.0357(13) Uani 1 1 d . . . H8 H 1.2559 0.0962 -0.6359 0.043 Uiso 1 1 calc R . . C9 C 1.2582(3) 0.2408(4) -0.6885(3) 0.0410(13) Uani 1 1 d . . . C10 C 1.4808(5) -0.2265(5) -0.6683(6) 0.086(3) Uani 1 1 d . . . H10A H 1.4729 -0.1993 -0.7241 0.129 Uiso 1 1 calc R . . H10B H 1.4537 -0.2740 -0.6704 0.129 Uiso 1 1 calc R . . H10C H 1.5342 -0.2362 -0.6603 0.129 Uiso 1 1 calc R . . C11 C 1.4897(4) -0.1074(4) -0.5915(7) 0.082(2) Uani 1 1 d . . . H11A H 1.4808 -0.0832 -0.6489 0.122 Uiso 1 1 calc R . . H11B H 1.5434 -0.1152 -0.5833 0.122 Uiso 1 1 calc R . . H11C H 1.4705 -0.0757 -0.5435 0.122 Uiso 1 1 calc R . . C12 C 1.4624(6) -0.2171(10) -0.5038(7) 0.151(6) Uani 1 1 d . . . H12A H 1.4767 -0.2695 -0.5163 0.181 Uiso 1 1 calc R . . H12B H 1.5054 -0.1933 -0.4735 0.181 Uiso 1 1 calc R . . C13 C 1.4051(6) -0.2181(9) -0.4465(7) 0.160(6) Uani 1 1 d . . . H13A H 1.4095 -0.1734 -0.4082 0.192 Uiso 1 1 calc R . . H13B H 1.4117 -0.2622 -0.4074 0.192 Uiso 1 1 calc R . . C14 C 1.2775(7) -0.1674(5) -0.4260(5) 0.113(4) Uani 1 1 d . . . H14A H 1.2272 -0.1686 -0.4519 0.170 Uiso 1 1 calc R . . H14B H 1.2969 -0.1163 -0.4282 0.170 Uiso 1 1 calc R . . H14C H 1.2753 -0.1843 -0.3640 0.170 Uiso 1 1 calc R . . C15 C 1.2969(6) -0.2985(5) -0.4784(5) 0.095(3) Uani 1 1 d . . . H15A H 1.2480 -0.2981 -0.5074 0.142 Uiso 1 1 calc R . . H15B H 1.2914 -0.3149 -0.4165 0.142 Uiso 1 1 calc R . . H15C H 1.3302 -0.3329 -0.5100 0.142 Uiso 1 1 calc R . . Cu1 Cu 1.33650(3) -0.17425(3) -0.60656(6) 0.03918(18) Uani 1 1 d . . . N1 N 1.4515(3) -0.1791(3) -0.5895(4) 0.0502(14) Uani 1 1 d . . . N2 N 1.3300(4) -0.2201(4) -0.4802(4) 0.0660(17) Uani 1 1 d . . . O1 O 1.3440(2) -0.0962(2) -0.7049(3) 0.0457(10) Uani 1 1 d . . . O2 O 1.3032(3) -0.0365(2) -0.5830(2) 0.0476(11) Uani 1 1 d . . . O3 O 1.4324(3) 0.1816(3) -0.9570(3) 0.0660(15) Uani 1 1 d . . . H3 H 1.4657 0.1839 -0.9959 0.099 Uiso 1 1 calc R . . O4 O 1.5033(3) 0.0875(3) -0.9076(3) 0.0773(15) Uani 1 1 d . . . O5 O 1.2819(3) 0.3052(3) -0.7077(3) 0.0507(12) Uani 1 1 d . . . O6 O 1.2290(2) -0.2007(2) -0.6378(2) 0.0488(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 C1 0.044(4) 0.041(4) 0.025(3) -0.009(3) -0.004(3) -0.007(3) C2 0.036(3) 0.035(3) 0.024(3) -0.007(2) 0.000(3) -0.002(3) C3 0.043(4) 0.032(4) 0.033(3) -0.009(3) 0.001(3) 0.007(3) C4 0.036(4) 0.043(4) 0.027(3) 0.001(3) 0.001(2) 0.000(3) C5 0.049(5) 0.035(4) 0.035(3) 0.001(3) 0.008(3) 0.006(3) C6 0.036(3) 0.035(3) 0.035(3) 0.002(2) 0.000(2) 0.004(3) C7 0.037(3) 0.046(3) 0.023(3) -0.001(3) 0.001(2) 0.004(3) C8 0.040(3) 0.049(4) 0.018(3) 0.000(2) 0.001(2) 0.001(3) C9 0.041(4) 0.053(4) 0.029(3) 0.003(3) -0.003(3) 0.015(3) C10 0.056(5) 0.077(6) 0.126(7) -0.030(5) 0.014(5) 0.001(4) C11 0.062(4) 0.071(5) 0.111(6) -0.022(6) 0.009(6) -0.028(4) C12 0.052(7) 0.303(18) 0.097(8) 0.092(10) -0.001(6) 0.023(8) C13 0.092(9) 0.313(18) 0.074(7) 0.071(9) -0.030(6) -0.037(10) C14 0.190(11) 0.103(8) 0.046(5) -0.012(5) 0.046(6) -0.034(7) C15 0.147(10) 0.069(6) 0.068(5) 0.017(5) 0.016(6) -0.029(6) Cu1 0.0458(4) 0.0414(4) 0.0303(2) -0.0043(5) 0.0071(5) -0.0136(3) N1 0.043(3) 0.064(3) 0.044(3) 0.002(3) 0.011(3) -0.011(2) N2 0.071(4) 0.089(5) 0.038(3) 0.010(3) -0.001(3) -0.031(4) O1 0.065(3) 0.039(2) 0.034(2) -0.0063(19) 0.008(2) -0.006(2) O2 0.070(3) 0.043(2) 0.030(2) -0.0032(19) 0.004(2) -0.006(2) O3 0.064(3) 0.086(4) 0.048(3) 0.020(3) 0.022(2) 0.013(3) O4 0.074(4) 0.074(4) 0.084(3) 0.027(3) 0.041(3) 0.022(3) O5 0.061(3) 0.041(3) 0.050(2) 0.009(2) 0.017(2) 0.007(2) O6 0.055(3) 0.045(2) 0.046(3) -0.0107(19) 0.0042(19) -0.013(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 C1 O1 1.252(7) . ? C1 O2 1.272(6) . ? C1 C2 1.484(8) . ? C2 C3 1.371(8) . ? C2 C8 1.403(7) . ? C3 C4 1.399(9) . ? C3 H3A 0.9300 . ? C4 C6 1.382(7) . ? C4 C5 1.478(9) . ? C5 O4 1.192(8) . ? C5 O3 1.308(7) . ? C6 C7 1.401(7) . ? C6 H6 0.9300 . ? C7 C8 1.359(7) . ? C7 C9 1.510(7) . ? C8 H8 0.9300 . ? C9 O5 1.236(7) . ? C9 O6 1.272(7) 7_645 ? C9 Cu1 2.539(5) 7_645 ? C10 N1 1.518(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N1 1.424(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.314(13) . ? C12 N1 1.439(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.408(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N2 1.531(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N2 1.492(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? Cu1 O6 1.996(4) . ? Cu1 O1 1.997(4) . ? Cu1 N2 2.030(6) . ? Cu1 N1 2.035(5) . ? Cu1 C9 2.539(5) 6_665 ? O3 H3 0.8200 . ? O6 C9 1.272(7) 6_665 ? 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 121.0(6) . . ? O1 C1 C2 119.9(5) . . ? O2 C1 C2 119.2(6) . . ? C3 C2 C8 119.1(5) . . ? C3 C2 C1 120.3(5) . . ? C8 C2 C1 120.5(5) . . ? C2 C3 C4 120.6(5) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C6 C4 C3 119.4(5) . . ? C6 C4 C5 120.7(6) . . ? C3 C4 C5 119.9(5) . . ? O4 C5 O3 122.4(6) . . ? O4 C5 C4 123.7(6) . . ? O3 C5 C4 113.8(6) . . ? C4 C6 C7 120.1(5) . . ? C4 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 119.7(5) . . ? C8 C7 C9 121.6(5) . . ? C6 C7 C9 118.6(5) . . ? C7 C8 C2 121.0(5) . . ? C7 C8 H8 119.5 . . ? C2 C8 H8 119.5 . . ? O5 C9 O6 123.2(5) . 7_645 ? O5 C9 C7 120.2(5) . . ? O6 C9 C7 116.5(6) 7_645 . ? O5 C9 Cu1 72.4(3) . 7_645 ? O6 C9 Cu1 50.8(3) 7_645 7_645 ? C7 C9 Cu1 167.0(5) . 7_645 ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N1 117.9(9) . . ? C13 C12 H12A 107.8 . . ? N1 C12 H12A 107.8 . . ? C13 C12 H12B 107.8 . . ? N1 C12 H12B 107.8 . . ? H12A C12 H12B 107.2 . . ? C12 C13 N2 119.4(9) . . ? C12 C13 H13A 107.5 . . ? N2 C13 H13A 107.5 . . ? C12 C13 H13B 107.5 . . ? N2 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 Cu1 O1 93.12(17) . . ? O6 Cu1 N2 93.8(2) . . ? O1 Cu1 N2 160.0(2) . . ? O6 Cu1 N1 162.9(2) . . ? O1 Cu1 N1 93.06(19) . . ? N2 Cu1 N1 85.7(2) . . ? O6 Cu1 C9 29.61(19) . 6_665 ? O1 Cu1 C9 95.58(16) . 6_665 ? N2 Cu1 C9 99.7(2) . 6_665 ? N1 Cu1 C9 133.7(2) . 6_665 ? C11 N1 C12 111.4(8) . . ? C11 N1 C10 108.0(6) . . ? C12 N1 C10 111.8(8) . . ? C11 N1 Cu1 115.2(4) . . ? C12 N1 Cu1 105.1(5) . . ? C10 N1 Cu1 105.3(4) . . ? C13 N2 C15 112.4(9) . . ? C13 N2 C14 111.4(9) . . ? C15 N2 C14 108.2(7) . . ? C13 N2 Cu1 105.1(5) . . ? C15 N2 Cu1 113.8(5) . . ? C14 N2 Cu1 105.7(5) . . ? C1 O1 Cu1 103.0(4) . . ? C5 O3 H3 109.5 . . ? C9 O6 Cu1 99.6(4) 6_665 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.475 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.065