data_e:\xray\wendy\091119~1\work1\1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H28 Cu4 O24' _chemical_formula_weight 1110.75 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' '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, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2473(5) _cell_length_b 25.914 _cell_length_c 25.9141(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8224.6(4) _cell_formula_units_Z 4 _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 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8826 _exptl_absorpt_correction_T_max 0.9290 _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 35483 _diffrn_reflns_av_R_equivalents 0.1352 _diffrn_reflns_av_sigmaI/netI 0.2020 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.42 _reflns_number_total 8349 _reflns_number_gt 3456 _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^)+(0.0362P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8349 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_restrained_S_all 0.735 _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 1.07411(4) 0.49399(2) 0.036737(18) 0.03338(16) Uani 1 1 d . . . Cu2 Cu 1.00464(6) 0.29705(3) 0.2500 0.0348(2) Uani 1 2 d S . . Cu3 Cu 0.85425(5) 0.22377(3) 0.2500 0.0295(2) Uani 1 2 d S . . O1 O 0.8370(2) 0.45629(12) -0.00007(10) 0.0436(8) Uani 1 1 d . . . O2 O 0.9629(2) 0.44782(12) 0.06270(10) 0.0462(9) Uani 1 1 d . . . O3 O 0.9170(3) 0.32680(14) 0.19778(11) 0.0626(10) Uani 1 1 d . . . O4 O 0.7833(2) 0.26546(13) 0.19596(10) 0.0413(9) Uani 1 1 d . . . O5 O 0.5849(3) 0.31328(13) 0.02930(10) 0.0556(9) Uani 1 1 d . . . O6 O 0.3256(2) 0.27763(14) -0.06031(11) 0.0587(10) Uani 1 1 d . . . O7 O 0.1246(2) 0.43912(12) -0.00899(10) 0.0414(8) Uani 1 1 d . . . O8 O -0.0019(2) 0.44841(12) -0.07070(10) 0.0443(8) Uani 1 1 d . . . O9 O -0.0529(2) 0.30736(12) -0.19693(9) 0.0396(8) Uani 1 1 d . . . O10 O 0.0721(3) 0.24487(15) -0.19809(12) 0.0664(11) Uani 1 1 d . . . O11 O 1.1908(2) 0.47439(16) 0.09775(10) 0.0715(12) Uani 1 1 d . . . O12 O 1.1292(4) 0.3555(2) 0.2500 0.109(2) Uani 1 2 d S . . O13 O 0.7373(4) 0.1622(2) 0.2500 0.109(2) Uani 1 2 d S . . C1 C 0.8725(4) 0.43678(18) 0.04064(16) 0.0367(12) Uani 1 1 d . . . C2 C 0.8086(4) 0.3936(2) 0.06434(15) 0.0438(13) Uani 1 1 d . . . C3 C 0.8416(4) 0.3716(2) 0.11101(16) 0.0497(14) Uani 1 1 d . . . H3 H 0.9023 0.3856 0.1290 0.060 Uiso 1 1 calc R . . C4 C 0.7875(4) 0.33023(19) 0.13089(15) 0.0377(12) Uani 1 1 d . . . C5 C 0.6994(3) 0.3093(2) 0.10532(16) 0.0480(14) Uani 1 1 d . . . H5 H 0.6619 0.2803 0.1191 0.058 Uiso 1 1 calc R . . C6 C 0.6662(3) 0.33146(19) 0.05876(15) 0.0405(13) Uani 1 1 d . . . C7 C 0.7212(4) 0.3729(2) 0.03974(16) 0.0468(13) Uani 1 1 d . . . H7 H 0.6977 0.3878 0.0082 0.056 Uiso 1 1 calc R . . C8 C 0.8321(4) 0.3042(3) 0.17974(15) 0.0484(15) Uani 1 1 d . . . C9 C 0.5309(3) 0.2680(2) 0.04503(15) 0.0470(13) Uani 1 1 d . . . H9A H 0.4858 0.2750 0.0760 0.056 Uiso 1 1 calc R . . H9B H 0.5847 0.2409 0.0537 0.056 Uiso 1 1 calc R . . C10 C 0.4577(4) 0.2500 0.0000 0.0292(16) Uani 1 2 d S . . C11 C 0.3860(3) 0.29527(19) -0.01653(15) 0.0434(13) Uani 1 1 d . . . H11A H 0.3359 0.3053 0.0117 0.052 Uiso 1 1 calc R . . H11B H 0.4315 0.3254 -0.0258 0.052 Uiso 1 1 calc R . . C12 C 0.2421(4) 0.3064(2) -0.07741(16) 0.0435(13) Uani 1 1 d . . . C13 C 0.1866(3) 0.2864(2) -0.11941(16) 0.0511(14) Uani 1 1 d . . . H13 H 0.2112 0.2554 -0.1351 0.061 Uiso 1 1 calc R . . C14 C 0.0948(3) 0.3116(2) -0.13875(15) 0.0400(12) Uani 1 1 d . . . C15 C 0.0600(3) 0.35810(19) -0.11755(15) 0.0417(12) Uani 1 1 d . . . H15 H -0.0018 0.3756 -0.1311 0.050 Uiso 1 1 calc R . . C16 C 0.1185(3) 0.37861(19) -0.07543(15) 0.0380(12) Uani 1 1 d . . . C17 C 0.2086(3) 0.3530(2) -0.05558(16) 0.0445(13) Uani 1 1 d . . . H17 H 0.2475 0.3672 -0.0272 0.053 Uiso 1 1 calc R . . C18 C 0.0343(4) 0.2860(2) -0.18098(15) 0.0400(14) Uani 1 1 d . . . C19 C 0.0780(4) 0.42677(18) -0.05025(16) 0.0323(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 0.0292(3) 0.0296(4) 0.0414(3) -0.0024(3) -0.0087(2) -0.0020(3) Cu2 0.0341(4) 0.0387(6) 0.0316(4) 0.000 0.000 -0.0099(4) Cu3 0.0267(4) 0.0370(6) 0.0249(4) 0.000 0.000 -0.0048(4) O1 0.048(2) 0.040(2) 0.0422(17) 0.0129(16) -0.0094(15) -0.0081(18) O2 0.0383(18) 0.045(2) 0.0555(18) 0.0065(17) -0.0106(15) -0.0147(18) O3 0.058(2) 0.071(3) 0.058(2) 0.0210(19) -0.0234(18) -0.017(2) O4 0.044(2) 0.049(3) 0.0305(16) 0.0134(15) -0.0009(14) -0.0046(19) O5 0.056(2) 0.053(3) 0.0579(19) 0.0311(18) -0.0260(17) -0.028(2) O6 0.050(2) 0.053(3) 0.073(2) -0.0273(19) -0.0339(17) 0.024(2) O7 0.0362(18) 0.035(2) 0.0525(18) -0.0106(16) -0.0156(15) 0.0064(17) O8 0.0419(18) 0.040(2) 0.0510(17) -0.0138(16) -0.0111(16) 0.0091(19) O9 0.0325(18) 0.050(2) 0.0363(16) -0.0059(15) -0.0123(14) 0.0014(18) O10 0.064(2) 0.058(3) 0.077(2) -0.033(2) -0.0329(19) 0.033(2) O11 0.058(2) 0.116(4) 0.0401(17) -0.0061(19) -0.0177(16) -0.009(2) O12 0.060(4) 0.058(5) 0.209(6) 0.000 0.000 -0.043(3) O13 0.035(3) 0.045(4) 0.247(7) 0.000 0.000 -0.013(3) C1 0.044(3) 0.029(3) 0.037(3) -0.005(2) 0.015(2) -0.007(3) C2 0.041(3) 0.053(4) 0.037(3) 0.013(2) -0.009(2) -0.004(3) C3 0.040(3) 0.064(4) 0.045(3) 0.000(3) -0.014(2) -0.011(3) C4 0.038(3) 0.036(4) 0.039(3) 0.008(2) 0.002(2) -0.010(3) C5 0.040(3) 0.053(4) 0.052(3) 0.020(3) -0.008(2) -0.019(3) C6 0.037(3) 0.044(4) 0.041(3) 0.012(2) -0.012(2) -0.023(3) C7 0.044(3) 0.054(4) 0.043(3) 0.013(3) -0.006(2) -0.017(3) C8 0.048(3) 0.076(5) 0.022(2) 0.001(3) -0.003(2) 0.018(4) C9 0.039(3) 0.055(4) 0.047(3) 0.005(3) -0.007(2) -0.004(3) C10 0.025(3) 0.032(5) 0.030(3) 0.004(3) 0.000 0.000 C11 0.035(3) 0.047(4) 0.048(3) -0.013(2) -0.015(2) 0.006(3) C12 0.030(3) 0.046(4) 0.054(3) -0.007(3) -0.013(2) 0.006(3) C13 0.046(3) 0.052(4) 0.055(3) -0.019(3) -0.014(2) 0.017(3) C14 0.036(3) 0.043(4) 0.041(2) -0.008(2) -0.008(2) 0.010(3) C15 0.038(3) 0.038(4) 0.049(3) -0.006(2) -0.006(2) 0.018(3) C16 0.035(3) 0.043(4) 0.037(2) 0.001(2) -0.003(2) -0.004(3) C17 0.038(3) 0.045(4) 0.050(3) -0.014(3) -0.017(2) 0.004(3) C18 0.035(3) 0.056(4) 0.029(2) -0.006(2) -0.009(2) -0.013(3) C19 0.034(3) 0.021(3) 0.042(3) -0.008(2) -0.002(2) 0.000(3) _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 1.934(3) . ? Cu1 O1 1.936(3) 5_765 ? Cu1 O8 1.946(3) 5_665 ? Cu1 O7 1.951(3) 1_655 ? Cu1 O11 2.191(3) . ? Cu1 Cu1 2.6492(9) 5_765 ? Cu2 O3 1.891(3) . ? Cu2 O3 1.891(3) 6_556 ? Cu2 O10 1.916(3) 8_666 ? Cu2 O10 1.916(3) 3_655 ? Cu2 O12 2.149(5) . ? Cu2 Cu3 2.6454(11) . ? Cu3 O9 1.958(3) 8_666 ? Cu3 O9 1.958(3) 3_655 ? Cu3 O4 1.970(3) 6_556 ? Cu3 O4 1.970(3) . ? Cu3 O13 2.144(5) . ? O1 C1 1.248(5) . ? O1 Cu1 1.936(3) 5_765 ? O2 C1 1.279(5) . ? O3 C8 1.282(6) . ? O4 C8 1.242(6) . ? O5 C6 1.340(4) . ? O5 C9 1.407(5) . ? O6 C12 1.342(5) . ? O6 C11 1.429(4) . ? O7 C19 1.253(4) . ? O7 Cu1 1.951(3) 1_455 ? O8 C19 1.246(4) . ? O8 Cu1 1.946(3) 5_665 ? O9 C18 1.272(5) . ? O9 Cu3 1.958(3) 3_455 ? O10 C18 1.244(5) . ? O10 Cu2 1.916(3) 3_455 ? C1 C2 1.496(6) . ? C2 C7 1.357(5) . ? C2 C3 1.397(5) . ? C3 C4 1.361(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 C8 1.534(6) . ? C5 C6 1.397(5) . ? C5 H5 0.9500 . ? C6 C7 1.360(6) . ? C7 H7 0.9500 . ? C9 C10 1.544(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.527(5) . ? C10 C11 1.527(5) 3 ? C10 C9 1.544(5) 3 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.384(5) . ? C12 C17 1.395(6) . ? C13 C14 1.393(5) . ? C13 H13 0.9500 . ? C14 C15 1.390(6) . ? C14 C18 1.479(6) . ? C15 C16 1.410(5) . ? C15 H15 0.9500 . ? C16 C17 1.386(5) . ? C16 C19 1.493(6) . ? C17 H17 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 O2 Cu1 O1 168.14(11) . 5_765 ? O2 Cu1 O8 89.83(13) . 5_665 ? O1 Cu1 O8 88.13(13) 5_765 5_665 ? O2 Cu1 O7 89.04(13) . 1_655 ? O1 Cu1 O7 90.50(12) 5_765 1_655 ? O8 Cu1 O7 167.89(11) 5_665 1_655 ? O2 Cu1 O11 93.73(12) . . ? O1 Cu1 O11 98.13(12) 5_765 . ? O8 Cu1 O11 98.52(12) 5_665 . ? O7 Cu1 O11 93.59(12) 1_655 . ? O2 Cu1 Cu1 80.80(8) . 5_765 ? O1 Cu1 Cu1 87.39(8) 5_765 5_765 ? O8 Cu1 Cu1 85.60(9) 5_665 5_765 ? O7 Cu1 Cu1 82.31(8) 1_655 5_765 ? O11 Cu1 Cu1 173.18(11) . 5_765 ? O3 Cu2 O3 91.4(2) . 6_556 ? O3 Cu2 O10 167.94(15) . 8_666 ? O3 Cu2 O10 88.47(15) 6_556 8_666 ? O3 Cu2 O10 88.47(15) . 3_655 ? O3 Cu2 O10 167.93(15) 6_556 3_655 ? O10 Cu2 O10 89.2(2) 8_666 3_655 ? O3 Cu2 O12 96.63(16) . . ? O3 Cu2 O12 96.63(16) 6_556 . ? O10 Cu2 O12 95.37(16) 8_666 . ? O10 Cu2 O12 95.37(16) 3_655 . ? O3 Cu2 Cu3 84.12(11) . . ? O3 Cu2 Cu3 84.11(11) 6_556 . ? O10 Cu2 Cu3 83.87(10) 8_666 . ? O10 Cu2 Cu3 83.87(10) 3_655 . ? O12 Cu2 Cu3 178.93(17) . . ? O9 Cu3 O9 89.22(16) 8_666 3_655 ? O9 Cu3 O4 89.01(11) 8_666 6_556 ? O9 Cu3 O4 168.79(14) 3_655 6_556 ? O9 Cu3 O4 168.79(14) 8_666 . ? O9 Cu3 O4 89.01(11) 3_655 . ? O4 Cu3 O4 90.58(17) 6_556 . ? O9 Cu3 O13 94.66(14) 8_666 . ? O9 Cu3 O13 94.66(14) 3_655 . ? O4 Cu3 O13 96.51(14) 6_556 . ? O4 Cu3 O13 96.51(14) . . ? O9 Cu3 Cu2 83.77(9) 8_666 . ? O9 Cu3 Cu2 83.77(9) 3_655 . ? O4 Cu3 Cu2 85.04(10) 6_556 . ? O4 Cu3 Cu2 85.04(10) . . ? O13 Cu3 Cu2 177.79(15) . . ? C1 O1 Cu1 119.2(3) . 5_765 ? C1 O2 Cu1 126.4(3) . . ? C8 O3 Cu2 122.4(3) . . ? C8 O4 Cu3 118.2(3) . . ? C6 O5 C9 118.5(3) . . ? C12 O6 C11 118.6(4) . . ? C19 O7 Cu1 124.1(3) . 1_455 ? C19 O8 Cu1 120.7(3) . 5_665 ? C18 O9 Cu3 122.5(3) . 3_455 ? C18 O10 Cu2 125.2(3) . 3_455 ? O1 C1 O2 126.1(4) . . ? O1 C1 C2 117.9(4) . . ? O2 C1 C2 115.9(4) . . ? C7 C2 C3 118.2(4) . . ? C7 C2 C1 121.0(4) . . ? C3 C2 C1 120.7(4) . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 C8 119.0(4) . . ? C5 C4 C8 120.1(5) . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? O5 C6 C7 116.0(4) . . ? O5 C6 C5 124.3(4) . . ? C7 C6 C5 119.6(4) . . ? C2 C7 C6 122.2(4) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? O4 C8 O3 129.5(4) . . ? O4 C8 C4 117.6(5) . . ? O3 C8 C4 112.9(5) . . ? O5 C9 C10 107.8(3) . . ? O5 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? O5 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? C11 C10 C11 109.8(5) . 3 ? C11 C10 C9 110.8(2) . 3 ? C11 C10 C9 108.3(2) 3 3 ? C11 C10 C9 108.3(2) . . ? C11 C10 C9 110.8(2) 3 . ? C9 C10 C9 109.0(5) 3 . ? O6 C11 C10 105.9(3) . . ? O6 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? O6 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? O6 C12 C13 115.2(5) . . ? O6 C12 C17 124.9(4) . . ? C13 C12 C17 119.9(4) . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.7(4) . . ? C15 C14 C18 121.8(4) . . ? C13 C14 C18 117.4(4) . . ? C14 C15 C16 118.5(4) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 120.8(4) . . ? C17 C16 C19 120.1(4) . . ? C15 C16 C19 119.0(4) . . ? C16 C17 C12 119.8(4) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? O10 C18 O9 124.7(4) . . ? O10 C18 C14 117.5(4) . . ? O9 C18 C14 117.8(5) . . ? O8 C19 O7 127.2(4) . . ? O8 C19 C16 116.8(4) . . ? O7 C19 C16 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.747 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.071