# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Mike Zaworotko' 'Heba Abourahma' 'Michael W. Bradner' 'Jianjiang Lu' 'Gregory J. McManus' 'Brian Moulton' _publ_contact_author_name 'Prof Mike Zaworotko' _publ_contact_author_address ; Chemistry University of South Florida 4202 E. Fowler Avenue Tampa 33620 UNITED STATES OF AMERICA ; _publ_contact_author_email XTAL@USF.EDU _publ_section_title ; A new 65.8 topology and a distorted 65.8 CdSO4 topology: two new supramolecular isomers of [M2(bdc)2(L)2]n coordination polymers ; data_gm1311 _database_code_CSD 202849 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 N2 O8 Zn2' _chemical_formula_weight 717.28 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 Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 30.2394(11) _cell_length_b 30.2394(11) _cell_length_c 18.2791(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14475.4(13) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6949 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.21 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6552 _exptl_absorpt_coefficient_mu 1.545 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 1.000 _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 '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 28023 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3916 _reflns_number_gt 3438 _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^)+(0.0612P)^2^+88.2216P] 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 3916 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn 0.448692(11) 0.971386(11) 0.037124(16) 0.01019(11) Uani 1 1 d . . . O1 O 0.41721(8) 0.97808(8) -0.05774(10) 0.0171(4) Uani 1 1 d . . . O2 O 0.46760(8) 1.04388(8) 0.06274(12) 0.0178(4) Uani 1 1 d . . . O3 O 0.50641(8) 0.98335(8) 0.11238(11) 0.0176(4) Uani 1 1 d . . . O4 O 0.45569(8) 0.91389(8) -0.00832(11) 0.0175(4) Uani 1 1 d . . . N1 N 0.39116(9) 0.92912(9) 0.10974(12) 0.0130(5) Uani 1 1 d . . . C1 C 0.44584(11) 0.99731(10) -0.11245(14) 0.0126(5) Uani 1 1 d . . . C2 C 0.42098(10) 0.99755(10) -0.18393(14) 0.0120(5) Uani 1 1 d . . . C3 C 0.37423(11) 0.99602(11) -0.18431(14) 0.0145(5) Uani 1 1 d . . . H3 H 0.3566 0.9923 -0.1397 0.017 Uiso 1 1 calc R . . C4 C 0.44511(12) 1.0000 -0.2500 0.0123(7) Uani 1 2 d S . . H4 H 0.4765 1.0000 -0.2500 0.015 Uiso 1 2 calc SR . . C5 C 0.35335(13) 1.0000 -0.2500 0.0158(8) Uani 1 2 d S . . H5 H 0.3219 1.0000 -0.2500 0.019 Uiso 1 2 calc SR . . C6 C 0.50742(11) 1.08366(11) 0.04375(14) 0.0134(5) Uani 1 1 d . . . C7 C 0.51062(10) 1.13331(10) 0.06396(14) 0.0125(5) Uani 1 1 d . . . C8 C 0.46602(13) 1.13268(13) 0.0833 0.0123(7) Uani 1 2 d S . . H8 H 0.4346 1.1013 0.0833 0.015 Uiso 1 2 calc SR . . C9 C 0.55642(11) 1.17957(11) 0.06197(16) 0.0176(6) Uani 1 1 d . . . H9 H 0.5868 1.1806 0.0460 0.021 Uiso 1 1 calc R . . C10 C 0.55766(14) 1.22433(14) 0.0833 0.0215(9) Uani 1 2 d S . . H10 H 0.5891 1.2557 0.0833 0.026 Uiso 1 2 calc SR . . C11 C 0.25817(13) 0.79262(13) 0.06003(18) 0.0268(7) Uani 1 1 d . . . H11 H 0.2285 0.7613 0.0479 0.032 Uiso 1 1 calc R . . C12 C 0.32510(12) 0.87148(12) 0.22242(16) 0.0215(6) Uani 1 1 d . . . H12 H 0.3030 0.8519 0.2612 0.026 Uiso 1 1 calc R . . C13 C 0.36822(12) 0.91655(13) 0.23717(15) 0.0206(6) Uani 1 1 d . . . H13 H 0.3762 0.9291 0.2859 0.025 Uiso 1 1 calc R . . C14 C 0.40059(11) 0.94411(11) 0.17902(15) 0.0167(6) Uani 1 1 d . . . H14 H 0.4309 0.9752 0.1898 0.020 Uiso 1 1 calc R . . C15 C 0.29166(12) 0.82353(12) 0.00442(17) 0.0230(6) Uani 1 1 d . . . H15 H 0.2839 0.8128 -0.0451 0.028 Uiso 1 1 calc R . . C16 C 0.31318(11) 0.85382(11) 0.14990(15) 0.0176(6) Uani 1 1 d . . . C17 C 0.26843(12) 0.80770(12) 0.13105(18) 0.0241(7) Uani 1 1 d . . . H17 H 0.2454 0.7871 0.1683 0.029 Uiso 1 1 calc R . . C18 C 0.34702(10) 0.88413(10) 0.09348(15) 0.0139(5) Uani 1 1 d . . . C20 C 0.33499(11) 0.86853(11) 0.02005(15) 0.0176(6) Uani 1 1 d . . . H20 H 0.3568 0.8891 -0.0183 0.021 Uiso 1 1 calc R . . O2S O 0.2497(9) 0.6944(8) 0.2204(12) 0.098(6) Uiso 0.25 1 d P . . O3S O 0.3352(5) 0.7292(5) 0.0141(7) 0.048(3) Uiso 0.25 1 d P . . O1SA O 0.3319(5) 0.7365(5) 0.0845(7) 0.051(3) Uiso 0.25 1 d P . . O2SA O 0.2801(5) 0.6978(5) 0.1963(7) 0.048(3) Uiso 0.25 1 d P . . O3SA O 0.2908(7) 0.7032(7) 0.1278(10) 0.082(5) Uiso 0.25 1 d P . . O4SA O 0.3333 0.6667 -0.0136(15) 0.103(8) Uiso 0.33 3 d SP . . O5SA O 0.3177(11) 0.7144(11) 0.2255(15) 0.133(9) Uiso 0.25 1 d P . . 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 Zn1 0.01126(17) 0.01283(17) 0.00723(17) 0.00045(10) 0.00109(11) 0.00659(13) O1 0.0175(10) 0.0246(11) 0.0095(8) 0.0028(8) 0.0005(7) 0.0107(9) O2 0.0186(10) 0.0141(10) 0.0218(10) -0.0025(8) 0.0017(8) 0.0089(8) O3 0.0145(10) 0.0241(11) 0.0122(9) 0.0026(8) -0.0017(7) 0.0082(9) O4 0.0188(10) 0.0201(10) 0.0180(9) -0.0019(8) 0.0031(8) 0.0131(9) N1 0.0129(11) 0.0168(11) 0.0101(10) 0.0014(8) 0.0014(8) 0.0080(9) C1 0.0165(13) 0.0120(12) 0.0111(12) -0.0011(10) -0.0011(10) 0.0083(11) C2 0.0141(12) 0.0128(12) 0.0084(11) 0.0016(9) -0.0005(9) 0.0061(10) C3 0.0159(13) 0.0177(13) 0.0106(12) 0.0002(10) 0.0025(10) 0.0090(11) C4 0.0116(12) 0.0144(18) 0.0118(17) -0.0005(14) -0.0003(7) 0.0072(9) C5 0.0137(13) 0.022(2) 0.0147(18) 0.0004(15) 0.0002(7) 0.0109(10) C6 0.0177(13) 0.0177(13) 0.0087(11) -0.0025(10) -0.0042(10) 0.0117(11) C7 0.0158(13) 0.0151(13) 0.0083(11) 0.0006(9) -0.0002(9) 0.0090(11) C8 0.0141(13) 0.0141(13) 0.0087(16) 0.0008(7) -0.0008(7) 0.0071(15) C9 0.0133(13) 0.0196(14) 0.0216(14) 0.0021(11) 0.0028(11) 0.0096(12) C10 0.0149(14) 0.0149(14) 0.033(2) 0.0007(9) -0.0007(9) 0.0061(16) C11 0.0204(15) 0.0200(15) 0.0294(17) -0.0016(13) 0.0016(13) 0.0022(13) C12 0.0212(15) 0.0291(16) 0.0140(13) 0.0088(12) 0.0094(11) 0.0126(13) C13 0.0228(15) 0.0312(17) 0.0094(12) 0.0003(11) 0.0015(11) 0.0147(13) C14 0.0162(14) 0.0219(14) 0.0122(12) -0.0007(11) 0.0012(10) 0.0096(12) C15 0.0230(15) 0.0227(15) 0.0184(14) -0.0029(12) -0.0009(12) 0.0077(13) C16 0.0186(14) 0.0198(14) 0.0149(13) 0.0021(11) 0.0034(11) 0.0100(12) C17 0.0205(15) 0.0203(15) 0.0250(15) 0.0052(12) 0.0078(12) 0.0052(13) C18 0.0129(13) 0.0144(13) 0.0145(12) 0.0010(10) 0.0022(10) 0.0068(11) C20 0.0176(14) 0.0198(14) 0.0131(12) 0.0005(11) 0.0029(11) 0.0075(12) _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 Zn1 O2 2.024(2) . ? Zn1 O4 2.031(2) . ? Zn1 O1 2.036(2) . ? Zn1 N1 2.049(2) . ? Zn1 O3 2.107(2) . ? Zn1 Zn1 3.0159(6) 19_675 ? O1 C1 1.259(3) . ? O2 C6 1.253(3) . ? O3 C1 1.258(3) 19_675 ? O4 C6 1.260(3) 19_675 ? N1 C14 1.327(4) . ? N1 C18 1.380(4) . ? C1 O3 1.258(3) 19_675 ? C1 C2 1.509(4) . ? C2 C3 1.391(4) . ? C2 C4 1.394(3) . ? C3 C5 1.390(3) . ? C4 C2 1.394(3) 5_674 ? C5 C3 1.390(3) 5_674 ? C6 O4 1.260(3) 19_675 ? C6 C7 1.502(4) . ? C7 C8 1.385(3) . ? C7 C9 1.392(4) . ? C8 C7 1.385(3) 16_454 ? C9 C10 1.391(4) . ? C10 C9 1.391(4) 16_454 ? C11 C17 1.359(5) . ? C11 C15 1.409(4) . ? C12 C13 1.361(5) . ? C12 C16 1.407(4) . ? C13 C14 1.402(4) . ? C15 C20 1.366(4) . ? C16 C17 1.417(4) . ? C16 C18 1.419(4) . ? C18 C20 1.409(4) . ? O2S O2SA 0.98(2) . ? O2S O1SA 1.23(2) 27 ? O3S O1SA 1.317(18) . ? O1SA O2S 1.23(2) 26_455 ? O1SA O2SA 1.287(18) 26_455 ? O1SA O3SA 1.39(2) . ? O1SA O5SA 1.65(3) 26_455 ? O2SA O5SA 1.12(3) . ? O2SA O3SA 1.28(2) . ? O2SA O1SA 1.287(18) 27 ? O3SA O5SA 1.42(3) 27 ? O5SA O3SA 1.42(3) 26_455 ? O5SA O1SA 1.65(3) 27 ? 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 Zn1 O4 158.06(8) . . ? O2 Zn1 O1 88.99(9) . . ? O4 Zn1 O1 89.47(8) . . ? O2 Zn1 N1 102.57(9) . . ? O4 Zn1 N1 98.65(9) . . ? O1 Zn1 N1 108.68(9) . . ? O2 Zn1 O3 84.37(8) . . ? O4 Zn1 O3 88.97(8) . . ? O1 Zn1 O3 158.02(8) . . ? N1 Zn1 O3 93.23(8) . . ? O2 Zn1 Zn1 80.23(6) . 19_675 ? O4 Zn1 Zn1 77.84(6) . 19_675 ? O1 Zn1 Zn1 87.58(6) . 19_675 ? N1 Zn1 Zn1 163.44(7) . 19_675 ? O3 Zn1 Zn1 70.66(6) . 19_675 ? C1 O1 Zn1 118.35(18) . . ? C6 O2 Zn1 126.25(18) . . ? C1 O3 Zn1 137.76(18) 19_675 . ? C6 O4 Zn1 128.92(19) 19_675 . ? C14 N1 C18 118.6(2) . . ? C14 N1 Zn1 115.76(19) . . ? C18 N1 Zn1 125.20(18) . . ? O3 C1 O1 125.3(2) 19_675 . ? O3 C1 C2 117.2(2) 19_675 . ? O1 C1 C2 117.4(2) . . ? C3 C2 C4 119.6(3) . . ? C3 C2 C1 120.3(2) . . ? C4 C2 C1 120.1(3) . . ? C5 C3 C2 120.0(3) . . ? C2 C4 C2 120.4(4) 5_674 . ? C3 C5 C3 120.3(4) . 5_674 ? O2 C6 O4 126.6(3) . 19_675 ? O2 C6 C7 116.3(2) . . ? O4 C6 C7 117.1(2) 19_675 . ? C8 C7 C9 119.5(3) . . ? C8 C7 C6 118.3(3) . . ? C9 C7 C6 122.2(2) . . ? C7 C8 C7 120.8(4) 16_454 . ? C10 C9 C7 120.0(3) . . ? C9 C10 C9 120.0(4) 16_454 . ? C17 C11 C15 119.9(3) . . ? C13 C12 C16 120.1(3) . . ? C12 C13 C14 118.7(3) . . ? N1 C14 C13 123.6(3) . . ? C20 C15 C11 121.5(3) . . ? C12 C16 C17 122.7(3) . . ? C12 C16 C18 118.3(3) . . ? C17 C16 C18 119.0(3) . . ? C11 C17 C16 120.5(3) . . ? N1 C18 C20 119.7(2) . . ? N1 C18 C16 120.7(3) . . ? C20 C18 C16 119.6(3) . . ? C15 C20 C18 119.4(3) . . ? O2SA O2S O1SA 70.1(18) . 27 ? O2S O1SA O2SA 45.5(12) 26_455 26_455 ? O2S O1SA O3S 120.5(16) 26_455 . ? O2SA O1SA O3S 132.7(14) 26_455 . ? O2S O1SA O3SA 115.0(16) 26_455 . ? O2SA O1SA O3SA 94.4(13) 26_455 . ? O3S O1SA O3SA 123.4(14) . . ? O2S O1SA O5SA 77.5(16) 26_455 26_455 ? O2SA O1SA O5SA 42.8(11) 26_455 26_455 ? O3S O1SA O5SA 94.9(14) . 26_455 ? O3SA O1SA O5SA 107.4(15) . 26_455 ? O2S O2SA O5SA 121(2) . . ? O2S O2SA O3SA 128(2) . . ? O5SA O2SA O3SA 106(2) . . ? O2S O2SA O1SA 64.4(16) . 27 ? O5SA O2SA O1SA 86.1(18) . 27 ? O3SA O2SA O1SA 143.9(16) . 27 ? O2SA O3SA O1SA 136.5(18) . . ? O2SA O3SA O5SA 99.6(19) . 27 ? O1SA O3SA O5SA 113.4(19) . 27 ? O2SA O5SA O3SA 135(3) . 26_455 ? O2SA O5SA O1SA 51.1(15) . 27 ? O3SA O5SA O1SA 163(2) 26_455 27 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O1 C1 85.8(2) . . . . ? O4 Zn1 O1 C1 -72.3(2) . . . . ? N1 Zn1 O1 C1 -171.3(2) . . . . ? O3 Zn1 O1 C1 13.6(4) . . . . ? Zn1 Zn1 O1 C1 5.5(2) 19_675 . . . ? O4 Zn1 O2 C6 -0.5(4) . . . . ? O1 Zn1 O2 C6 -86.6(2) . . . . ? N1 Zn1 O2 C6 164.5(2) . . . . ? O3 Zn1 O2 C6 72.4(2) . . . . ? Zn1 Zn1 O2 C6 1.1(2) 19_675 . . . ? O2 Zn1 O3 C1 -84.2(3) . . . 19_675 ? O4 Zn1 O3 C1 74.9(3) . . . 19_675 ? O1 Zn1 O3 C1 -11.1(4) . . . 19_675 ? N1 Zn1 O3 C1 173.5(3) . . . 19_675 ? Zn1 Zn1 O3 C1 -2.6(3) 19_675 . . 19_675 ? O2 Zn1 O4 C6 4.5(4) . . . 19_675 ? O1 Zn1 O4 C6 90.5(2) . . . 19_675 ? N1 Zn1 O4 C6 -160.7(2) . . . 19_675 ? O3 Zn1 O4 C6 -67.6(2) . . . 19_675 ? Zn1 Zn1 O4 C6 2.8(2) 19_675 . . 19_675 ? O2 Zn1 N1 C14 -48.6(2) . . . . ? O4 Zn1 N1 C14 125.8(2) . . . . ? O1 Zn1 N1 C14 -141.8(2) . . . . ? O3 Zn1 N1 C14 36.4(2) . . . . ? Zn1 Zn1 N1 C14 49.4(4) 19_675 . . . ? O2 Zn1 N1 C18 139.0(2) . . . . ? O4 Zn1 N1 C18 -46.6(2) . . . . ? O1 Zn1 N1 C18 45.8(2) . . . . ? O3 Zn1 N1 C18 -136.0(2) . . . . ? Zn1 Zn1 N1 C18 -123.0(2) 19_675 . . . ? Zn1 O1 C1 O3 -5.8(4) . . . 19_675 ? Zn1 O1 C1 C2 174.60(17) . . . . ? O3 C1 C2 C3 -155.0(3) 19_675 . . . ? O1 C1 C2 C3 24.6(4) . . . . ? O3 C1 C2 C4 24.1(4) 19_675 . . . ? O1 C1 C2 C4 -156.2(2) . . . . ? C4 C2 C3 C5 -3.8(4) . . . . ? C1 C2 C3 C5 175.3(2) . . . . ? C3 C2 C4 C2 1.91(18) . . . 5_674 ? C1 C2 C4 C2 -177.2(3) . . . 5_674 ? C2 C3 C5 C3 1.92(18) . . . 5_674 ? Zn1 O2 C6 O4 -3.8(4) . . . 19_675 ? Zn1 O2 C6 C7 174.67(17) . . . . ? O2 C6 C7 C8 -17.0(3) . . . . ? O4 C6 C7 C8 161.6(2) 19_675 . . . ? O2 C6 C7 C9 164.7(3) . . . . ? O4 C6 C7 C9 -16.7(4) 19_675 . . . ? C9 C7 C8 C7 -1.81(19) . . . 16_454 ? C6 C7 C8 C7 179.8(2) . . . 16_454 ? C8 C7 C9 C10 3.6(4) . . . . ? C6 C7 C9 C10 -178.1(2) . . . . ? C7 C9 C10 C9 -1.82(19) . . . 16_454 ? C16 C12 C13 C14 -1.2(5) . . . . ? C18 N1 C14 C13 0.4(4) . . . . ? Zn1 N1 C14 C13 -172.5(2) . . . . ? C12 C13 C14 N1 1.1(5) . . . . ? C17 C11 C15 C20 0.7(5) . . . . ? C13 C12 C16 C17 -178.9(3) . . . . ? C13 C12 C16 C18 -0.1(4) . . . . ? C15 C11 C17 C16 -1.3(5) . . . . ? C12 C16 C17 C11 179.0(3) . . . . ? C18 C16 C17 C11 0.2(5) . . . . ? C14 N1 C18 C20 177.2(3) . . . . ? Zn1 N1 C18 C20 -10.6(4) . . . . ? C14 N1 C18 C16 -1.8(4) . . . . ? Zn1 N1 C18 C16 170.4(2) . . . . ? C12 C16 C18 N1 1.7(4) . . . . ? C17 C16 C18 N1 -179.5(3) . . . . ? C12 C16 C18 C20 -177.3(3) . . . . ? C17 C16 C18 C20 1.5(4) . . . . ? C11 C15 C20 C18 1.0(5) . . . . ? N1 C18 C20 C15 178.9(3) . . . . ? C16 C18 C20 C15 -2.1(4) . . . . ? O1SA O2S O2SA O5SA -68(3) 27 . . . ? O1SA O2S O2SA O3SA 140(2) 27 . . . ? O2S O2SA O3SA O1SA 129(3) . . . . ? O5SA O2SA O3SA O1SA -27(3) . . . . ? O1SA O2SA O3SA O1SA -133(3) 27 . . . ? O2S O2SA O3SA O5SA -92(3) . . . 27 ? O5SA O2SA O3SA O5SA 112(3) . . . 27 ? O1SA O2SA O3SA O5SA 7(3) 27 . . 27 ? O2S O1SA O3SA O2SA -21(3) 26_455 . . . ? O2SA O1SA O3SA O2SA 21(3) 26_455 . . . ? O3S O1SA O3SA O2SA 171(2) . . . . ? O5SA O1SA O3SA O2SA 63(3) 26_455 . . . ? O2S O1SA O3SA O5SA -157(2) 26_455 . . 27 ? O2SA O1SA O3SA O5SA -114.7(19) 26_455 . . 27 ? O3S O1SA O3SA O5SA 35(3) . . . 27 ? O5SA O1SA O3SA O5SA -73(2) 26_455 . . 27 ? O2S O2SA O5SA O3SA -144(3) . . . 26_455 ? O3SA O2SA O5SA O3SA 14(4) . . . 26_455 ? O1SA O2SA O5SA O3SA 159(3) 27 . . 26_455 ? O2S O2SA O5SA O1SA 57(2) . . . 27 ? O3SA O2SA O5SA O1SA -145.4(18) . . . 27 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.210 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.114 data_ha380 _database_code_CSD 202850 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.25 H31 Cu4 N3 O17' _chemical_formula_weight 1238.97 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 10.6661(12) _cell_length_b 30.303(4) _cell_length_c 16.3650(19) _cell_angle_alpha 90.00 _cell_angle_beta 95.877(2) _cell_angle_gamma 90.00 _cell_volume 5261.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelpipe _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2494 _exptl_absorpt_coefficient_mu 1.670 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 29732 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.32 _reflns_number_total 12275 _reflns_number_gt 7699 _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^)+(0.0644P)^2^+3.9942P] 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 12275 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 -0.12211(6) 0.99148(2) 0.49706(4) 0.01688(16) Uani 1 1 d . . . Cu2 Cu 0.02919(6) 0.77936(2) 1.01839(4) 0.01728(16) Uani 1 1 d . . . Cu3 Cu 0.07329(6) 0.71464(2) 0.91576(4) 0.01784(16) Uani 1 1 d . . . Cu4 Cu 0.44865(6) 0.99034(2) 1.06866(4) 0.02000(16) Uani 1 1 d . . . O1A O 0.4190(3) 0.81367(12) 0.4499(2) 0.0256(9) Uani 1 1 d . . . O2A O 0.3697(3) 0.75300(12) 0.5189(2) 0.0258(9) Uani 1 1 d . . . O3A O 0.1364(3) 0.94359(12) 0.4970(2) 0.0242(9) Uani 1 1 d . . . O4A O -0.0708(3) 0.92937(12) 0.4934(3) 0.0263(9) Uani 1 1 d . . . C1A C 0.3456(5) 0.79063(17) 0.4882(4) 0.0222(12) Uani 1 1 d . . . C2A C 0.2167(5) 0.80870(18) 0.4963(4) 0.0246(13) Uani 1 1 d . . . C3A C 0.1214(6) 0.78044(19) 0.5132(5) 0.0371(17) Uani 1 1 d . . . H3A H 0.1391 0.7500 0.5222 0.045 Uiso 1 1 calc R . . C4A C 0.0004(6) 0.7960(2) 0.5172(5) 0.048(2) Uani 1 1 d . . . H4A H -0.0652 0.7759 0.5259 0.058 Uiso 1 1 calc R . . C5A C -0.0261(6) 0.83993(19) 0.5087(4) 0.0348(16) Uani 1 1 d . . . H5A H -0.1096 0.8503 0.5114 0.042 Uiso 1 1 calc R . . C6A C 0.0706(5) 0.86948(18) 0.4961(3) 0.0213(12) Uani 1 1 d . . . C7A C 0.1905(5) 0.85333(18) 0.4891(3) 0.0213(12) Uani 1 1 d . . . H7A H 0.2560 0.8733 0.4792 0.026 Uiso 1 1 calc R . . C8A C 0.0435(5) 0.91782(17) 0.4945(3) 0.0198(11) Uani 1 1 d . . . O1B O -0.0960(3) 0.98936(13) 0.6178(2) 0.0243(9) Uani 1 1 d . . . O2B O 0.1103(4) 1.00427(13) 0.6225(2) 0.0264(9) Uani 1 1 d . . . O3B O 0.2874(4) 0.98568(14) 0.9998(2) 0.0315(10) Uani 1 1 d . . . O4B O 0.3748(4) 1.00075(13) 0.8843(2) 0.0270(9) Uani 1 1 d . . . C1B C 0.0120(5) 0.99548(17) 0.6557(3) 0.0221(12) Uani 1 1 d . . . C2B C 0.0247(5) 0.99189(16) 0.7474(3) 0.0184(11) Uani 1 1 d . . . C3B C -0.0812(5) 0.98492(17) 0.7890(3) 0.0222(12) Uani 1 1 d . . . H3B H -0.1630 0.9857 0.7599 0.027 Uiso 1 1 calc R . . C4B C -0.0674(5) 0.97687(19) 0.8725(3) 0.0262(13) Uani 1 1 d . . . H4B H -0.1394 0.9712 0.9006 0.031 Uiso 1 1 calc R . . C5B C 0.0511(5) 0.97712(19) 0.9149(4) 0.0248(13) Uani 1 1 d . . . H5B H 0.0607 0.9705 0.9720 0.030 Uiso 1 1 calc R . . C6B C 0.1562(5) 0.98687(17) 0.8752(3) 0.0195(11) Uani 1 1 d . . . C7B C 0.1418(5) 0.99372(17) 0.7910(3) 0.0217(12) Uani 1 1 d . . . H7B H 0.2138 0.9998 0.7631 0.026 Uiso 1 1 calc R . . C8B C 0.2832(5) 0.99118(18) 0.9237(3) 0.0215(12) Uani 1 1 d . . . O1C O 0.5760(4) 0.94555(13) 0.9177(3) 0.0332(10) Uani 1 1 d . . . O2C O 0.4833(4) 0.92980(13) 1.0313(3) 0.0304(10) Uani 1 1 d . . . O3C O 0.2204(4) 0.75255(12) 0.8995(3) 0.0283(9) Uani 1 1 d . . . O4C O 0.1953(4) 0.80226(13) 0.9981(3) 0.0297(10) Uani 1 1 d . . . C1C C 0.5254(5) 0.91951(19) 0.9646(4) 0.0266(13) Uani 1 1 d . . . C2C C 0.5072(5) 0.87302(19) 0.9375(4) 0.0271(13) Uani 1 1 d . . . C3C C 0.5877(6) 0.8523(2) 0.8887(4) 0.0412(17) Uani 1 1 d . . . H3C H 0.6609 0.8673 0.8748 0.049 Uiso 1 1 calc R . . C4C C 0.5628(7) 0.8102(2) 0.8598(5) 0.052(2) Uani 1 1 d . . . H4C H 0.6210 0.7956 0.8288 0.063 Uiso 1 1 calc R . . C5C C 0.4539(6) 0.7893(2) 0.8759(4) 0.0387(17) Uani 1 1 d . . . H5C H 0.4348 0.7609 0.8535 0.046 Uiso 1 1 calc R . . C6C C 0.3729(5) 0.80902(18) 0.9238(4) 0.0249(13) Uani 1 1 d . . . C7C C 0.3999(5) 0.85006(18) 0.9561(4) 0.0228(12) Uani 1 1 d . . . H7C H 0.3451 0.8631 0.9916 0.027 Uiso 1 1 calc R . . C8C C 0.2539(5) 0.78623(18) 0.9419(4) 0.0223(12) Uani 1 1 d . . . O1D O -0.0400(4) 0.81111(12) 0.9198(2) 0.0278(9) Uani 1 1 d . . . O2D O -0.0331(4) 0.75165(12) 0.8382(2) 0.0271(9) Uani 1 1 d . . . O3D O -0.3862(4) 0.76126(12) 0.6001(2) 0.0259(9) Uani 1 1 d . . . O4D O -0.3312(3) 0.81228(12) 0.5117(2) 0.0242(9) Uani 1 1 d . . . C1D C -0.0606(5) 0.79106(18) 0.8523(4) 0.0218(12) Uani 1 1 d . . . C2D C -0.1251(5) 0.81661(17) 0.7807(3) 0.0183(11) Uani 1 1 d . . . C3D C -0.1125(6) 0.86228(19) 0.7782(4) 0.0312(15) Uani 1 1 d . . . H3D H -0.0672 0.8773 0.8229 0.037 Uiso 1 1 calc R . . C4D C -0.1652(6) 0.8858(2) 0.7115(4) 0.0367(16) Uani 1 1 d . . . H4D H -0.1532 0.9168 0.7089 0.044 Uiso 1 1 calc R . . C5D C -0.2369(6) 0.86377(19) 0.6471(4) 0.0290(14) Uani 1 1 d . . . H5D H -0.2746 0.8799 0.6013 0.035 Uiso 1 1 calc R . . C6D C -0.2522(5) 0.81891(17) 0.6506(3) 0.0188(11) Uani 1 1 d . . . C7D C -0.1950(5) 0.79522(18) 0.7170(3) 0.0201(12) Uani 1 1 d . . . H7D H -0.2040 0.7641 0.7185 0.024 Uiso 1 1 calc R . . C8D C -0.3295(5) 0.79560(18) 0.5822(3) 0.0203(12) Uani 1 1 d . . . N1PA N 0.1149(4) 0.66579(15) 0.8276(3) 0.0236(11) Uani 1 1 d . . . C1PA C 0.0882(7) 0.6726(2) 0.7479(4) 0.048(2) Uani 1 1 d . . . H1PA H 0.0568 0.7008 0.7306 0.058 Uiso 1 1 calc R . . C2PA C 0.1031(8) 0.6415(3) 0.6889(5) 0.065(3) Uani 1 1 d . . . H2PA H 0.0834 0.6480 0.6322 0.078 Uiso 1 1 calc R . . C3PA C 0.1478(7) 0.6003(3) 0.7144(5) 0.053(2) Uani 1 1 d . . . H3PA H 0.1579 0.5777 0.6755 0.064 Uiso 1 1 calc R . . C4PA C 0.1770(6) 0.5927(2) 0.7962(5) 0.0432(18) Uani 1 1 d . . . H4PA H 0.2089 0.5649 0.8154 0.052 Uiso 1 1 calc R . . C5PA C 0.1590(6) 0.6265(2) 0.8503(4) 0.0339(15) Uani 1 1 d . . . H5PA H 0.1796 0.6211 0.9073 0.041 Uiso 1 1 calc R . . N1PB N -0.0068(5) 0.82574(15) 1.1126(3) 0.0256(11) Uani 1 1 d . . . C1PB C 0.0011(7) 0.8689(2) 1.1012(5) 0.0418(17) Uani 1 1 d . . . H1PB H 0.0150 0.8793 1.0482 0.050 Uiso 1 1 calc R . . C2PB C -0.0097(8) 0.8992(2) 1.1621(5) 0.054(2) Uani 1 1 d . . . H2PB H -0.0028 0.9298 1.1509 0.064 Uiso 1 1 calc R . . C3PB C -0.0299(7) 0.8858(3) 1.2373(5) 0.056(2) Uani 1 1 d . . . H3PB H -0.0372 0.9064 1.2802 0.067 Uiso 1 1 calc R . . C4PB C -0.0402(9) 0.8402(3) 1.2512(5) 0.065(2) Uani 1 1 d . . . H4PB H -0.0549 0.8291 1.3037 0.078 Uiso 1 1 calc R . . C5PB C -0.0284(8) 0.8123(2) 1.1866(5) 0.052(2) Uani 1 1 d . . . H5PB H -0.0363 0.7815 1.1955 0.063 Uiso 1 1 calc R . . N1PC N 0.3874(5) 0.96962(17) 1.1826(3) 0.0272(11) Uani 1 1 d . . . C1PC C 0.3400(6) 0.9315(3) 1.1936(5) 0.0474(19) Uani 1 1 d . . . H1PC H 0.3209 0.9137 1.1462 0.057 Uiso 1 1 calc R . . C2PC C 0.3146(7) 0.9144(3) 1.2666(6) 0.061(3) Uani 1 1 d . . . H2PC H 0.2846 0.8850 1.2695 0.073 Uiso 1 1 calc R . . C3PC C 0.3325(8) 0.9400(4) 1.3368(6) 0.082(4) Uani 1 1 d . . . H3PC H 0.3089 0.9298 1.3879 0.098 Uiso 1 1 calc R . . C4PC C 0.3873(11) 0.9821(5) 1.3293(6) 0.124(6) Uani 1 1 d . . . H4PC H 0.4045 1.0002 1.3765 0.149 Uiso 1 1 calc R . . C5PC C 0.4178(9) 0.9979(4) 1.2491(6) 0.087(3) Uani 1 1 d . . . H5PC H 0.4561 1.0259 1.2427 0.104 Uiso 1 1 calc R . . O1WC O -0.3235(4) 0.98312(15) 0.4760(3) 0.0395(11) Uani 1 1 d . . . C1G C 0.4735(7) 1.0893(2) 1.4970(5) 0.051(2) Uiso 1 1 d . . . C2G C 0.6071(9) 1.0618(3) 1.3745(6) 0.072(3) Uiso 1 1 d . . . C3G C 0.5924(9) 1.1477(3) 1.3244(6) 0.072(3) Uiso 1 1 d . . . C11G C 0.6943(12) 1.0787(4) 1.3385(8) 0.031(3) Uiso 0.50 1 d P . . C12G C 0.5776(16) 1.1081(6) 1.3487(11) 0.064(5) Uiso 0.50 1 d P . . C13G C 0.5149(17) 1.0575(6) 1.4469(12) 0.070(5) Uiso 0.50 1 d P . . C14G C 0.7969(19) 1.1334(7) 1.2771(13) 0.078(6) Uiso 0.50 1 d P . . C15G C 0.6917(12) 1.1182(4) 1.3151(8) 0.030(3) Uiso 0.50 1 d P . . C21G C 0.721(3) 1.1448(10) 1.3016(18) 0.043(7) Uiso 0.25 1 d P . . C22G C 0.527(3) 1.0936(11) 1.424(2) 0.054(8) Uiso 0.25 1 d P . . C23G C 0.794(4) 1.1858(14) 1.294(3) 0.085(12) Uiso 0.25 1 d P . . 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 0.0145(3) 0.0180(3) 0.0170(4) 0.0004(3) -0.0035(2) 0.0010(3) Cu2 0.0167(3) 0.0173(3) 0.0170(4) -0.0024(3) -0.0019(3) -0.0021(3) Cu3 0.0180(3) 0.0174(3) 0.0174(4) -0.0024(3) -0.0020(3) -0.0015(3) Cu4 0.0185(3) 0.0259(4) 0.0148(4) 0.0038(3) -0.0025(3) -0.0058(3) O1A 0.016(2) 0.027(2) 0.034(3) 0.0055(18) 0.0025(17) 0.0062(16) O2A 0.020(2) 0.024(2) 0.033(3) 0.0019(17) 0.0008(18) 0.0041(16) O3A 0.020(2) 0.018(2) 0.035(3) 0.0009(16) 0.0032(17) 0.0018(16) O4A 0.015(2) 0.021(2) 0.042(3) -0.0007(17) -0.0003(17) 0.0031(16) C1A 0.016(3) 0.018(3) 0.031(3) -0.004(2) -0.003(2) 0.002(2) C2A 0.018(3) 0.019(3) 0.036(4) -0.004(2) -0.003(2) 0.004(2) C3A 0.025(3) 0.015(3) 0.072(5) -0.003(3) 0.010(3) 0.003(3) C4A 0.025(4) 0.023(3) 0.100(7) -0.005(4) 0.021(4) -0.003(3) C5A 0.020(3) 0.023(3) 0.062(5) -0.006(3) 0.005(3) 0.004(3) C6A 0.019(3) 0.021(3) 0.023(3) -0.002(2) -0.001(2) 0.003(2) C7A 0.015(3) 0.024(3) 0.024(3) 0.002(2) -0.001(2) 0.003(2) C8A 0.024(3) 0.020(3) 0.015(3) -0.001(2) 0.000(2) 0.004(2) O1B 0.025(2) 0.032(2) 0.013(2) -0.0002(16) -0.0082(16) -0.0040(18) O2B 0.024(2) 0.040(2) 0.014(2) -0.0012(17) -0.0045(16) -0.0032(18) O3B 0.021(2) 0.054(3) 0.018(2) 0.0053(19) -0.0046(17) -0.0049(19) O4B 0.022(2) 0.037(2) 0.021(2) 0.0031(17) -0.0037(17) -0.0098(18) C1B 0.030(3) 0.016(3) 0.020(3) -0.001(2) -0.001(2) 0.007(2) C2B 0.025(3) 0.014(3) 0.015(3) -0.003(2) -0.005(2) 0.000(2) C3B 0.025(3) 0.022(3) 0.018(3) -0.007(2) -0.005(2) 0.000(2) C4B 0.026(3) 0.033(3) 0.020(3) -0.003(2) 0.006(2) -0.002(3) C5B 0.022(3) 0.033(3) 0.017(3) 0.000(2) -0.005(2) 0.001(2) C6B 0.020(3) 0.017(3) 0.021(3) 0.000(2) -0.002(2) 0.000(2) C7B 0.028(3) 0.016(3) 0.021(3) -0.003(2) 0.000(2) -0.002(2) C8B 0.020(3) 0.022(3) 0.020(3) -0.002(2) -0.005(2) -0.005(2) O1C 0.036(3) 0.025(2) 0.039(3) 0.0058(19) 0.009(2) -0.0074(19) O2C 0.040(3) 0.026(2) 0.024(2) 0.0021(17) 0.0001(19) -0.0061(19) O3C 0.024(2) 0.028(2) 0.033(3) -0.0050(18) 0.0030(18) -0.0070(18) O4C 0.023(2) 0.032(2) 0.035(3) -0.0099(19) 0.0028(19) -0.0142(18) C1C 0.018(3) 0.029(3) 0.031(4) 0.004(3) -0.003(3) -0.004(2) C2C 0.025(3) 0.027(3) 0.029(4) 0.003(2) 0.003(3) -0.005(2) C3C 0.030(4) 0.041(4) 0.056(5) -0.007(3) 0.019(3) -0.014(3) C4C 0.048(5) 0.042(4) 0.073(6) -0.019(4) 0.034(4) -0.010(4) C5C 0.037(4) 0.034(4) 0.047(5) -0.012(3) 0.018(3) -0.010(3) C6C 0.020(3) 0.025(3) 0.030(3) -0.001(2) 0.003(2) -0.007(2) C7C 0.017(3) 0.024(3) 0.027(3) 0.003(2) 0.002(2) -0.004(2) C8C 0.017(3) 0.027(3) 0.023(3) 0.002(2) 0.001(2) 0.001(2) O1D 0.036(2) 0.022(2) 0.023(2) -0.0011(17) -0.0092(18) -0.0015(18) O2D 0.033(2) 0.021(2) 0.025(2) -0.0034(16) -0.0071(18) 0.0032(17) O3D 0.032(2) 0.021(2) 0.023(2) 0.0034(16) -0.0043(18) -0.0067(17) O4D 0.024(2) 0.027(2) 0.021(2) 0.0030(16) -0.0060(17) -0.0065(17) C1D 0.015(3) 0.026(3) 0.023(3) 0.008(2) -0.001(2) -0.006(2) C2D 0.018(3) 0.023(3) 0.014(3) -0.002(2) -0.002(2) -0.001(2) C3D 0.042(4) 0.023(3) 0.026(4) 0.000(2) -0.010(3) -0.009(3) C4D 0.052(4) 0.017(3) 0.038(4) 0.001(3) -0.009(3) -0.003(3) C5D 0.037(4) 0.025(3) 0.023(3) 0.004(2) -0.007(3) 0.000(3) C6D 0.015(3) 0.020(3) 0.021(3) -0.003(2) 0.000(2) 0.001(2) C7D 0.017(3) 0.018(3) 0.025(3) 0.003(2) 0.000(2) 0.000(2) C8D 0.018(3) 0.022(3) 0.021(3) -0.001(2) -0.001(2) 0.002(2) N1PA 0.025(3) 0.022(3) 0.024(3) -0.005(2) 0.001(2) 0.000(2) C1PA 0.069(5) 0.042(4) 0.031(4) -0.008(3) -0.005(4) 0.022(4) C2PA 0.079(6) 0.084(6) 0.030(5) -0.020(4) -0.012(4) 0.035(5) C3PA 0.045(5) 0.055(5) 0.059(6) -0.032(4) 0.002(4) -0.003(4) C4PA 0.052(5) 0.028(4) 0.049(5) -0.013(3) 0.002(4) 0.003(3) C5PA 0.034(4) 0.033(4) 0.036(4) -0.002(3) 0.009(3) 0.002(3) N1PB 0.030(3) 0.019(3) 0.028(3) -0.006(2) 0.005(2) 0.001(2) C1PB 0.052(4) 0.029(4) 0.044(5) -0.003(3) 0.003(3) 0.004(3) C2PB 0.079(6) 0.024(4) 0.058(6) -0.018(3) 0.006(5) 0.002(4) C3PB 0.064(5) 0.052(5) 0.053(6) -0.030(4) 0.009(4) 0.001(4) C4PB 0.100(7) 0.061(6) 0.036(5) -0.007(4) 0.024(5) -0.005(5) C5PB 0.087(6) 0.033(4) 0.040(5) -0.003(3) 0.023(4) 0.010(4) N1PC 0.028(3) 0.039(3) 0.015(3) 0.001(2) 0.004(2) -0.002(2) C1PC 0.040(4) 0.059(5) 0.042(5) 0.012(4) 0.003(3) -0.008(4) C2PC 0.046(5) 0.087(7) 0.050(6) 0.042(5) 0.005(4) -0.014(4) C3PC 0.053(6) 0.133(10) 0.062(7) 0.064(7) 0.022(5) 0.007(6) C4PC 0.082(8) 0.257(18) 0.032(6) -0.001(8) -0.007(5) 0.069(10) C5PC 0.063(6) 0.148(10) 0.052(7) 0.023(6) 0.009(5) 0.008(6) O1WC 0.017(2) 0.050(3) 0.050(3) 0.008(2) -0.002(2) -0.001(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 O4A 1.962(4) . ? Cu1 O1B 1.967(4) . ? Cu1 O3A 1.977(4) 3_576 ? Cu1 O2B 1.978(4) 3_576 ? Cu1 O1WC 2.156(4) . ? Cu1 Cu1 2.6476(13) 3_576 ? Cu2 O1D 1.957(4) . ? Cu2 O4C 1.962(4) . ? Cu2 O2A 1.965(4) 4_576 ? Cu2 O3D 1.968(4) 4_676 ? Cu2 N1PB 2.150(5) . ? Cu2 Cu3 2.6553(9) . ? Cu3 O4D 1.960(4) 4_676 ? Cu3 O2D 1.966(4) . ? Cu3 O3C 1.985(4) . ? Cu3 O1A 1.985(4) 4_576 ? Cu3 N1PA 2.145(5) . ? Cu4 O3B 1.962(4) . ? Cu4 O1C 1.976(4) 3_677 ? Cu4 O4B 1.979(4) 3_677 ? Cu4 O2C 1.980(4) . ? Cu4 N1PC 2.133(5) . ? Cu4 Cu4 2.6640(13) 3_677 ? O1A C1A 1.264(7) . ? O1A Cu3 1.985(4) 4_675 ? O2A C1A 1.262(6) . ? O2A Cu2 1.965(4) 4_675 ? O3A C8A 1.259(6) . ? O3A Cu1 1.977(4) 3_576 ? O4A C8A 1.267(6) . ? C1A C2A 1.498(7) . ? C2A C3A 1.379(8) . ? C2A C7A 1.383(7) . ? C3A C4A 1.382(8) . ? C4A C5A 1.365(8) . ? C5A C6A 1.397(8) . ? C6A C7A 1.386(7) . ? C6A C8A 1.493(7) . ? O1B C1B 1.266(6) . ? O2B C1B 1.258(7) . ? O2B Cu1 1.978(4) 3_576 ? O3B C8B 1.252(6) . ? O4B C8B 1.258(7) . ? O4B Cu4 1.979(4) 3_677 ? C1B C2B 1.497(7) . ? C2B C7B 1.374(7) . ? C2B C3B 1.394(8) . ? C3B C4B 1.380(8) . ? C4B C5B 1.379(8) . ? C5B C6B 1.385(8) . ? C6B C7B 1.386(7) . ? C6B C8B 1.503(7) . ? O1C C1C 1.259(7) . ? O1C Cu4 1.976(4) 3_677 ? O2C C1C 1.262(7) . ? O3C C8C 1.265(6) . ? O4C C8C 1.260(7) . ? C1C C2C 1.484(8) . ? C2C C3C 1.382(9) . ? C2C C7C 1.399(7) . ? C3C C4C 1.377(9) . ? C4C C5C 1.371(9) . ? C5C C6C 1.363(8) . ? C6C C7C 1.370(8) . ? C6C C8C 1.501(7) . ? O1D C1D 1.260(7) . ? O2D C1D 1.257(6) . ? O3D C8D 1.253(6) . ? O3D Cu2 1.968(4) 4_575 ? O4D C8D 1.258(6) . ? O4D Cu3 1.960(4) 4_575 ? C1D C2D 1.509(7) . ? C2D C7D 1.380(7) . ? C2D C3D 1.392(7) . ? C3D C4D 1.374(8) . ? C4D C5D 1.405(8) . ? C5D C6D 1.371(7) . ? C6D C7D 1.390(7) . ? C6D C8D 1.497(7) . ? N1PA C5PA 1.320(7) . ? N1PA C1PA 1.322(8) . ? C1PA C2PA 1.371(9) . ? C2PA C3PA 1.386(10) . ? C3PA C4PA 1.362(10) . ? C4PA C5PA 1.380(9) . ? N1PB C5PB 1.320(8) . ? N1PB C1PB 1.324(8) . ? C1PB C2PB 1.369(9) . ? C2PB C3PB 1.334(11) . ? C3PB C4PB 1.407(11) . ? C4PB C5PB 1.369(10) . ? N1PC C1PC 1.280(8) . ? N1PC C5PC 1.398(12) . ? C1PC C2PC 1.356(10) . ? C2PC C3PC 1.384(14) . ? C3PC C4PC 1.413(16) . ? C4PC C5PC 1.465(14) . ? C1G C13G 1.37(2) . ? C1G C22G 1.39(3) . ? C2G C11G 1.260(14) . ? C2G C12G 1.490(19) . ? C2G C22G 1.56(3) . ? C2G C13G 1.62(2) . ? C3G C12G 1.279(18) . ? C3G C15G 1.406(15) . ? C3G C21G 1.46(3) . ? C11G C15G 1.256(17) . ? C11G C12G 1.55(2) . ? C12G C15G 1.42(2) . ? C12G C22G 1.46(4) . ? C13G C22G 1.17(3) . ? C14G C21G 1.00(3) . ? C14G C15G 1.41(2) . ? C14G C23G 1.61(4) . ? C15G C21G 0.90(3) . ? C21G C23G 1.48(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 O4A Cu1 O1B 89.33(17) . . ? O4A Cu1 O3A 168.32(15) . 3_576 ? O1B Cu1 O3A 89.26(16) . 3_576 ? O4A Cu1 O2B 89.20(17) . 3_576 ? O1B Cu1 O2B 168.15(16) . 3_576 ? O3A Cu1 O2B 89.80(16) 3_576 3_576 ? O4A Cu1 O1WC 99.13(16) . . ? O1B Cu1 O1WC 101.11(17) . . ? O3A Cu1 O1WC 92.52(16) 3_576 . ? O2B Cu1 O1WC 90.73(17) 3_576 . ? O4A Cu1 Cu1 84.96(11) . 3_576 ? O1B Cu1 Cu1 86.13(11) . 3_576 ? O3A Cu1 Cu1 83.38(11) 3_576 3_576 ? O2B Cu1 Cu1 82.02(11) 3_576 3_576 ? O1WC Cu1 Cu1 171.66(13) . 3_576 ? O1D Cu2 O4C 87.56(17) . . ? O1D Cu2 O2A 89.72(17) . 4_576 ? O4C Cu2 O2A 167.03(17) . 4_576 ? O1D Cu2 O3D 167.43(16) . 4_676 ? O4C Cu2 O3D 88.69(17) . 4_676 ? O2A Cu2 O3D 91.26(16) 4_576 4_676 ? O1D Cu2 N1PB 100.94(18) . . ? O4C Cu2 N1PB 96.94(18) . . ? O2A Cu2 N1PB 96.02(17) 4_576 . ? O3D Cu2 N1PB 91.42(17) 4_676 . ? O1D Cu2 Cu3 85.30(12) . . ? O4C Cu2 Cu3 86.13(12) . . ? O2A Cu2 Cu3 81.01(12) 4_576 . ? O3D Cu2 Cu3 82.48(11) 4_676 . ? N1PB Cu2 Cu3 173.12(13) . . ? O4D Cu3 O2D 166.76(16) 4_676 . ? O4D Cu3 O3C 89.72(17) 4_676 . ? O2D Cu3 O3C 89.74(17) . . ? O4D Cu3 O1A 88.42(16) 4_676 4_576 ? O2D Cu3 O1A 89.30(17) . 4_576 ? O3C Cu3 O1A 167.71(16) . 4_576 ? O4D Cu3 N1PA 97.21(17) 4_676 . ? O2D Cu3 N1PA 96.01(17) . . ? O3C Cu3 N1PA 95.07(17) . . ? O1A Cu3 N1PA 97.21(17) 4_576 . ? O4D Cu3 Cu2 84.93(11) 4_676 . ? O2D Cu3 Cu2 81.90(11) . . ? O3C Cu3 Cu2 81.41(12) . . ? O1A Cu3 Cu2 86.32(11) 4_576 . ? N1PA Cu3 Cu2 175.90(13) . . ? O3B Cu4 O1C 90.97(18) . 3_677 ? O3B Cu4 O4B 167.52(17) . 3_677 ? O1C Cu4 O4B 87.37(17) 3_677 3_677 ? O3B Cu4 O2C 86.33(18) . . ? O1C Cu4 O2C 167.62(17) 3_677 . ? O4B Cu4 O2C 92.65(17) 3_677 . ? O3B Cu4 N1PC 98.78(18) . . ? O1C Cu4 N1PC 97.74(19) 3_677 . ? O4B Cu4 N1PC 93.70(17) 3_677 . ? O2C Cu4 N1PC 94.62(18) . . ? O3B Cu4 Cu4 86.72(12) . 3_677 ? O1C Cu4 Cu4 87.14(13) 3_677 3_677 ? O4B Cu4 Cu4 80.85(12) 3_677 3_677 ? O2C Cu4 Cu4 80.64(12) . 3_677 ? N1PC Cu4 Cu4 172.54(14) . 3_677 ? C1A O1A Cu3 118.3(3) . 4_675 ? C1A O2A Cu2 126.2(4) . 4_675 ? C8A O3A Cu1 123.7(3) . 3_576 ? C8A O4A Cu1 122.3(3) . . ? O2A C1A O1A 125.9(5) . . ? O2A C1A C2A 116.5(5) . . ? O1A C1A C2A 117.6(5) . . ? C3A C2A C7A 118.5(5) . . ? C3A C2A C1A 119.5(5) . . ? C7A C2A C1A 121.9(5) . . ? C2A C3A C4A 120.6(6) . . ? C5A C4A C3A 120.9(6) . . ? C4A C5A C6A 119.4(6) . . ? C7A C6A C5A 119.2(5) . . ? C7A C6A C8A 121.6(5) . . ? C5A C6A C8A 119.1(5) . . ? C2A C7A C6A 121.2(5) . . ? O3A C8A O4A 125.6(5) . . ? O3A C8A C6A 117.3(5) . . ? O4A C8A C6A 117.1(5) . . ? C1B O1B Cu1 121.1(4) . . ? C1B O2B Cu1 125.6(4) . 3_576 ? C8B O3B Cu4 120.2(4) . . ? C8B O4B Cu4 126.2(4) . 3_677 ? O2B C1B O1B 125.2(5) . . ? O2B C1B C2B 117.0(5) . . ? O1B C1B C2B 117.8(5) . . ? C7B C2B C3B 119.4(5) . . ? C7B C2B C1B 120.1(5) . . ? C3B C2B C1B 120.4(5) . . ? C4B C3B C2B 120.0(5) . . ? C5B C4B C3B 119.8(5) . . ? C4B C5B C6B 120.6(5) . . ? C5B C6B C7B 119.1(5) . . ? C5B C6B C8B 120.0(5) . . ? C7B C6B C8B 120.9(5) . . ? C2B C7B C6B 120.8(5) . . ? O3B C8B O4B 126.1(5) . . ? O3B C8B C6B 116.9(5) . . ? O4B C8B C6B 117.0(5) . . ? C1C O1C Cu4 118.5(4) . 3_677 ? C1C O2C Cu4 126.2(4) . . ? C8C O3C Cu3 125.2(4) . . ? C8C O4C Cu2 120.7(4) . . ? O1C C1C O2C 125.8(6) . . ? O1C C1C C2C 117.7(6) . . ? O2C C1C C2C 116.5(5) . . ? C3C C2C C7C 118.1(5) . . ? C3C C2C C1C 122.2(5) . . ? C7C C2C C1C 119.5(5) . . ? C4C C3C C2C 120.6(6) . . ? C5C C4C C3C 119.9(6) . . ? C6C C5C C4C 120.5(6) . . ? C5C C6C C7C 119.9(5) . . ? C5C C6C C8C 120.7(5) . . ? C7C C6C C8C 119.3(5) . . ? C6C C7C C2C 120.7(5) . . ? O4C C8C O3C 125.3(5) . . ? O4C C8C C6C 117.3(5) . . ? O3C C8C C6C 117.4(5) . . ? C1D O1D Cu2 120.2(4) . . ? C1D O2D Cu3 123.6(4) . . ? C8D O3D Cu2 124.0(4) . 4_575 ? C8D O4D Cu3 121.7(3) . 4_575 ? O2D C1D O1D 126.6(5) . . ? O2D C1D C2D 116.2(5) . . ? O1D C1D C2D 117.2(5) . . ? C7D C2D C3D 119.4(5) . . ? C7D C2D C1D 120.9(5) . . ? C3D C2D C1D 119.7(5) . . ? C4D C3D C2D 120.4(5) . . ? C3D C4D C5D 119.8(6) . . ? C6D C5D C4D 119.8(5) . . ? C5D C6D C7D 120.0(5) . . ? C5D C6D C8D 119.7(5) . . ? C7D C6D C8D 120.3(5) . . ? C2D C7D C6D 120.6(5) . . ? O3D C8D O4D 125.9(5) . . ? O3D C8D C6D 117.3(5) . . ? O4D C8D C6D 116.8(5) . . ? C5PA N1PA C1PA 117.1(5) . . ? C5PA N1PA Cu3 121.7(4) . . ? C1PA N1PA Cu3 121.1(4) . . ? N1PA C1PA C2PA 123.9(7) . . ? C1PA C2PA C3PA 117.9(7) . . ? C4PA C3PA C2PA 119.0(7) . . ? C3PA C4PA C5PA 118.2(7) . . ? N1PA C5PA C4PA 123.8(7) . . ? C5PB N1PB C1PB 117.0(6) . . ? C5PB N1PB Cu2 121.1(4) . . ? C1PB N1PB Cu2 121.7(4) . . ? N1PB C1PB C2PB 123.3(7) . . ? C3PB C2PB C1PB 120.1(7) . . ? C2PB C3PB C4PB 118.1(7) . . ? C5PB C4PB C3PB 117.8(8) . . ? N1PB C5PB C4PB 123.8(7) . . ? C1PC N1PC C5PC 120.6(7) . . ? C1PC N1PC Cu4 123.3(5) . . ? C5PC N1PC Cu4 115.6(5) . . ? N1PC C1PC C2PC 125.9(8) . . ? C1PC C2PC C3PC 119.6(8) . . ? C2PC C3PC C4PC 117.2(8) . . ? C3PC C4PC C5PC 120.4(11) . . ? N1PC C5PC C4PC 116.1(11) . . ? C13G C1G C22G 50.2(14) . . ? C11G C2G C12G 68.2(10) . . ? C11G C2G C22G 117.2(15) . . ? C12G C2G C22G 57.0(14) . . ? C11G C2G C13G 155.0(12) . . ? C12G C2G C13G 98.9(11) . . ? C22G C2G C13G 43.0(13) . . ? C12G C3G C15G 63.6(10) . . ? C12G C3G C21G 99.9(16) . . ? C15G C3G C21G 36.5(12) . . ? C15G C11G C2G 122.4(12) . . ? C15G C11G C12G 59.5(10) . . ? C2G C11G C12G 63.0(9) . . ? C3G C12G C15G 62.6(10) . . ? C3G C12G C22G 128(2) . . ? C15G C12G C22G 143(2) . . ? C3G C12G C2G 160.5(16) . . ? C15G C12G C2G 98.5(12) . . ? C22G C12G C2G 64.0(15) . . ? C3G C12G C11G 112.3(14) . . ? C15G C12G C11G 49.8(9) . . ? C22G C12G C11G 106.6(18) . . ? C2G C12G C11G 48.8(8) . . ? C22G C13G C1G 65.9(19) . . ? C22G C13G C2G 65.9(19) . . ? C1G C13G C2G 129.8(14) . . ? C21G C14G C15G 39.2(19) . . ? C21G C14G C23G 64(3) . . ? C15G C14G C23G 102(2) . . ? C21G C15G C11G 159(3) . . ? C21G C15G C3G 75(2) . . ? C11G C15G C3G 124.5(12) . . ? C21G C15G C14G 45(2) . . ? C11G C15G C14G 116.7(14) . . ? C3G C15G C14G 118.8(13) . . ? C21G C15G C12G 128(3) . . ? C11G C15G C12G 70.7(11) . . ? C3G C15G C12G 53.9(9) . . ? C14G C15G C12G 172.3(15) . . ? C15G C21G C14G 96(3) . . ? C15G C21G C3G 69(2) . . ? C14G C21G C3G 161(3) . . ? C15G C21G C23G 166(4) . . ? C14G C21G C23G 79(3) . . ? C3G C21G C23G 119(3) . . ? C13G C22G C1G 64(2) . . ? C13G C22G C12G 128(3) . . ? C1G C22G C12G 168(3) . . ? C13G C22G C2G 71(2) . . ? C1G C22G C2G 133(2) . . ? C12G C22G C2G 59.0(15) . . ? C21G C23G C14G 37.5(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1D Cu2 Cu3 O4D 170.53(16) . . . 4_676 ? O4C Cu2 Cu3 O4D 82.66(17) . . . 4_676 ? O2A Cu2 Cu3 O4D -99.01(16) 4_576 . . 4_676 ? O3D Cu2 Cu3 O4D -6.53(16) 4_676 . . 4_676 ? N1PB Cu2 Cu3 O4D -34.2(11) . . . 4_676 ? O1D Cu2 Cu3 O2D -10.92(17) . . . . ? O4C Cu2 Cu3 O2D -98.78(18) . . . . ? O2A Cu2 Cu3 O2D 79.54(17) 4_576 . . . ? O3D Cu2 Cu3 O2D 172.03(17) 4_676 . . . ? N1PB Cu2 Cu3 O2D 144.4(11) . . . . ? O1D Cu2 Cu3 O3C 80.04(17) . . . . ? O4C Cu2 Cu3 O3C -7.82(17) . . . . ? O2A Cu2 Cu3 O3C 170.50(16) 4_576 . . . ? O3D Cu2 Cu3 O3C -97.01(17) 4_676 . . . ? N1PB Cu2 Cu3 O3C -124.7(11) . . . . ? O1D Cu2 Cu3 O1A -100.74(16) . . . 4_576 ? O4C Cu2 Cu3 O1A 171.40(17) . . . 4_576 ? O2A Cu2 Cu3 O1A -10.27(16) 4_576 . . 4_576 ? O3D Cu2 Cu3 O1A 82.21(16) 4_676 . . 4_576 ? N1PB Cu2 Cu3 O1A 54.6(11) . . . 4_576 ? O1D Cu2 Cu3 N1PA 48.8(18) . . . . ? O4C Cu2 Cu3 N1PA -39.1(18) . . . . ? O2A Cu2 Cu3 N1PA 139.2(18) 4_576 . . . ? O3D Cu2 Cu3 N1PA -128.3(18) 4_676 . . . ? N1PB Cu2 Cu3 N1PA -156(2) . . . . ? O1B Cu1 O4A C8A -86.3(4) . . . . ? O3A Cu1 O4A C8A -3.2(11) 3_576 . . . ? O2B Cu1 O4A C8A 81.9(4) 3_576 . . . ? O1WC Cu1 O4A C8A 172.6(4) . . . . ? Cu1 Cu1 O4A C8A -0.1(4) 3_576 . . . ? Cu2 O2A C1A O1A 1.9(8) 4_675 . . . ? Cu2 O2A C1A C2A 180.0(4) 4_675 . . . ? Cu3 O1A C1A O2A 12.0(8) 4_675 . . . ? Cu3 O1A C1A C2A -166.0(4) 4_675 . . . ? O2A C1A C2A C3A -18.8(8) . . . . ? O1A C1A C2A C3A 159.5(6) . . . . ? O2A C1A C2A C7A 159.7(5) . . . . ? O1A C1A C2A C7A -22.1(8) . . . . ? C7A C2A C3A C4A 4.5(10) . . . . ? C1A C2A C3A C4A -177.0(7) . . . . ? C2A C3A C4A C5A -3.5(12) . . . . ? C3A C4A C5A C6A -0.2(12) . . . . ? C4A C5A C6A C7A 2.7(10) . . . . ? C4A C5A C6A C8A -174.5(6) . . . . ? C3A C2A C7A C6A -2.0(9) . . . . ? C1A C2A C7A C6A 179.6(5) . . . . ? C5A C6A C7A C2A -1.6(9) . . . . ? C8A C6A C7A C2A 175.5(5) . . . . ? Cu1 O3A C8A O4A 1.9(8) 3_576 . . . ? Cu1 O3A C8A C6A -175.8(4) 3_576 . . . ? Cu1 O4A C8A O3A -1.0(8) . . . . ? Cu1 O4A C8A C6A 176.7(4) . . . . ? C7A C6A C8A O3A -8.8(8) . . . . ? C5A C6A C8A O3A 168.3(5) . . . . ? C7A C6A C8A O4A 173.3(5) . . . . ? C5A C6A C8A O4A -9.6(8) . . . . ? O4A Cu1 O1B C1B 84.6(4) . . . . ? O3A Cu1 O1B C1B -83.8(4) 3_576 . . . ? O2B Cu1 O1B C1B 1.7(10) 3_576 . . . ? O1WC Cu1 O1B C1B -176.3(4) . . . . ? Cu1 Cu1 O1B C1B -0.4(4) 3_576 . . . ? O1C Cu4 O3B C8B 88.7(4) 3_677 . . . ? O4B Cu4 O3B C8B 6.5(11) 3_677 . . . ? O2C Cu4 O3B C8B -79.2(4) . . . . ? N1PC Cu4 O3B C8B -173.3(4) . . . . ? Cu4 Cu4 O3B C8B 1.7(4) 3_677 . . . ? Cu1 O2B C1B O1B -2.4(8) 3_576 . . . ? Cu1 O2B C1B C2B 177.4(3) 3_576 . . . ? Cu1 O1B C1B O2B 1.7(7) . . . . ? Cu1 O1B C1B C2B -178.1(3) . . . . ? O2B C1B C2B C7B -6.5(7) . . . . ? O1B C1B C2B C7B 173.3(5) . . . . ? O2B C1B C2B C3B 176.1(5) . . . . ? O1B C1B C2B C3B -4.1(7) . . . . ? C7B C2B C3B C4B -4.5(8) . . . . ? C1B C2B C3B C4B 172.9(5) . . . . ? C2B C3B C4B C5B 2.0(8) . . . . ? C3B C4B C5B C6B 2.2(9) . . . . ? C4B C5B C6B C7B -4.0(8) . . . . ? C4B C5B C6B C8B 174.3(5) . . . . ? C3B C2B C7B C6B 2.7(8) . . . . ? C1B C2B C7B C6B -174.7(5) . . . . ? C5B C6B C7B C2B 1.4(8) . . . . ? C8B C6B C7B C2B -176.8(5) . . . . ? Cu4 O3B C8B O4B -1.6(8) . . . . ? Cu4 O3B C8B C6B 179.7(3) . . . . ? Cu4 O4B C8B O3B 0.1(8) 3_677 . . . ? Cu4 O4B C8B C6B 178.8(3) 3_677 . . . ? C5B C6B C8B O3B -0.2(8) . . . . ? C7B C6B C8B O3B 178.0(5) . . . . ? C5B C6B C8B O4B -178.9(5) . . . . ? C7B C6B C8B O4B -0.7(8) . . . . ? O3B Cu4 O2C C1C 82.2(5) . . . . ? O1C Cu4 O2C C1C 4.5(11) 3_677 . . . ? O4B Cu4 O2C C1C -85.3(5) 3_677 . . . ? N1PC Cu4 O2C C1C -179.2(5) . . . . ? Cu4 Cu4 O2C C1C -5.0(4) 3_677 . . . ? O4D Cu3 O3C C8C -76.2(4) 4_676 . . . ? O2D Cu3 O3C C8C 90.6(5) . . . . ? O1A Cu3 O3C C8C 5.1(11) 4_576 . . . ? N1PA Cu3 O3C C8C -173.4(4) . . . . ? Cu2 Cu3 O3C C8C 8.8(4) . . . . ? O1D Cu2 O4C C8C -75.4(4) . . . . ? O2A Cu2 O4C C8C 2.6(11) 4_576 . . . ? O3D Cu2 O4C C8C 92.6(4) 4_676 . . . ? N1PB Cu2 O4C C8C -176.2(4) . . . . ? Cu3 Cu2 O4C C8C 10.0(4) . . . . ? Cu4 O1C C1C O2C -16.7(8) 3_677 . . . ? Cu4 O1C C1C C2C 159.9(4) 3_677 . . . ? Cu4 O2C C1C O1C 15.0(9) . . . . ? Cu4 O2C C1C C2C -161.6(4) . . . . ? O1C C1C C2C C3C 30.5(9) . . . . ? O2C C1C C2C C3C -152.6(6) . . . . ? O1C C1C C2C C7C -144.3(6) . . . . ? O2C C1C C2C C7C 32.6(8) . . . . ? C7C C2C C3C C4C -0.4(10) . . . . ? C1C C2C C3C C4C -175.3(7) . . . . ? C2C C3C C4C C5C 3.4(12) . . . . ? C3C C4C C5C C6C -3.4(12) . . . . ? C4C C5C C6C C7C 0.2(11) . . . . ? C4C C5C C6C C8C -179.7(6) . . . . ? C5C C6C C7C C2C 2.9(9) . . . . ? C8C C6C C7C C2C -177.2(5) . . . . ? C3C C2C C7C C6C -2.8(9) . . . . ? C1C C2C C7C C6C 172.3(5) . . . . ? Cu2 O4C C8C O3C -6.9(8) . . . . ? Cu2 O4C C8C C6C 173.0(4) . . . . ? Cu3 O3C C8C O4C -4.0(8) . . . . ? Cu3 O3C C8C C6C 176.1(4) . . . . ? C5C C6C C8C O4C 167.3(6) . . . . ? C7C C6C C8C O4C -12.6(8) . . . . ? C5C C6C C8C O3C -12.9(9) . . . . ? C7C C6C C8C O3C 167.2(5) . . . . ? O4C Cu2 O1D C1D 98.2(4) . . . . ? O2A Cu2 O1D C1D -69.2(4) 4_576 . . . ? O3D Cu2 O1D C1D 25.4(10) 4_676 . . . ? N1PB Cu2 O1D C1D -165.2(4) . . . . ? Cu3 Cu2 O1D C1D 11.8(4) . . . . ? O4D Cu3 O2D C1D 20.3(10) 4_676 . . . ? O3C Cu3 O2D C1D -67.4(4) . . . . ? O1A Cu3 O2D C1D 100.4(4) 4_576 . . . ? N1PA Cu3 O2D C1D -162.4(4) . . . . ? Cu2 Cu3 O2D C1D 14.0(4) . . . . ? Cu3 O2D C1D O1D -9.9(8) . . . . ? Cu3 O2D C1D C2D 170.3(3) . . . . ? Cu2 O1D C1D O2D -5.3(8) . . . . ? Cu2 O1D C1D C2D 174.5(3) . . . . ? O2D C1D C2D C7D 25.7(8) . . . . ? O1D C1D C2D C7D -154.1(5) . . . . ? O2D C1D C2D C3D -153.2(5) . . . . ? O1D C1D C2D C3D 26.9(8) . . . . ? C7D C2D C3D C4D -2.4(9) . . . . ? C1D C2D C3D C4D 176.6(6) . . . . ? C2D C3D C4D C5D 2.8(10) . . . . ? C3D C4D C5D C6D -1.1(10) . . . . ? C4D C5D C6D C7D -1.2(9) . . . . ? C4D C5D C6D C8D 179.5(6) . . . . ? C3D C2D C7D C6D 0.1(8) . . . . ? C1D C2D C7D C6D -178.8(5) . . . . ? C5D C6D C7D C2D 1.6(8) . . . . ? C8D C6D C7D C2D -179.1(5) . . . . ? Cu2 O3D C8D O4D 9.6(8) 4_575 . . . ? Cu2 O3D C8D C6D -170.1(3) 4_575 . . . ? Cu3 O4D C8D O3D -0.4(8) 4_575 . . . ? Cu3 O4D C8D C6D 179.4(3) 4_575 . . . ? C5D C6D C8D O3D -149.9(5) . . . . ? C7D C6D C8D O3D 30.7(8) . . . . ? C5D C6D C8D O4D 30.3(8) . . . . ? C7D C6D C8D O4D -149.0(5) . . . . ? O4D Cu3 N1PA C5PA 16.8(5) 4_676 . . . ? O2D Cu3 N1PA C5PA -162.6(5) . . . . ? O3C Cu3 N1PA C5PA 107.1(5) . . . . ? O1A Cu3 N1PA C5PA -72.5(5) 4_576 . . . ? Cu2 Cu3 N1PA C5PA 138.1(16) . . . . ? O4D Cu3 N1PA C1PA -168.5(5) 4_676 . . . ? O2D Cu3 N1PA C1PA 12.1(5) . . . . ? O3C Cu3 N1PA C1PA -78.2(5) . . . . ? O1A Cu3 N1PA C1PA 102.2(5) 4_576 . . . ? Cu2 Cu3 N1PA C1PA -47(2) . . . . ? C5PA N1PA C1PA C2PA 0.4(11) . . . . ? Cu3 N1PA C1PA C2PA -174.6(7) . . . . ? N1PA C1PA C2PA C3PA 0.6(13) . . . . ? C1PA C2PA C3PA C4PA -1.2(12) . . . . ? C2PA C3PA C4PA C5PA 0.9(11) . . . . ? C1PA N1PA C5PA C4PA -0.7(10) . . . . ? Cu3 N1PA C5PA C4PA 174.2(5) . . . . ? C3PA C4PA C5PA N1PA 0.1(11) . . . . ? O1D Cu2 N1PB C5PB 149.4(6) . . . . ? O4C Cu2 N1PB C5PB -121.8(6) . . . . ? O2A Cu2 N1PB C5PB 58.5(6) 4_576 . . . ? O3D Cu2 N1PB C5PB -32.9(6) 4_676 . . . ? Cu3 Cu2 N1PB C5PB -5.5(15) . . . . ? O1D Cu2 N1PB C1PB -35.9(5) . . . . ? O4C Cu2 N1PB C1PB 53.0(5) . . . . ? O2A Cu2 N1PB C1PB -126.7(5) 4_576 . . . ? O3D Cu2 N1PB C1PB 141.8(5) 4_676 . . . ? Cu3 Cu2 N1PB C1PB 169.2(9) . . . . ? C5PB N1PB C1PB C2PB 1.2(11) . . . . ? Cu2 N1PB C1PB C2PB -173.8(6) . . . . ? N1PB C1PB C2PB C3PB -0.4(13) . . . . ? C1PB C2PB C3PB C4PB -0.3(13) . . . . ? C2PB C3PB C4PB C5PB 0.2(13) . . . . ? C1PB N1PB C5PB C4PB -1.4(12) . . . . ? Cu2 N1PB C5PB C4PB 173.7(7) . . . . ? C3PB C4PB C5PB N1PB 0.7(14) . . . . ? O3B Cu4 N1PC C1PC 60.7(5) . . . . ? O1C Cu4 N1PC C1PC 152.9(5) 3_677 . . . ? O4B Cu4 N1PC C1PC -119.2(5) 3_677 . . . ? O2C Cu4 N1PC C1PC -26.3(5) . . . . ? Cu4 Cu4 N1PC C1PC -76.5(13) 3_677 . . . ? O3B Cu4 N1PC C5PC -127.7(5) . . . . ? O1C Cu4 N1PC C5PC -35.5(6) 3_677 . . . ? O4B Cu4 N1PC C5PC 52.3(5) 3_677 . . . ? O2C Cu4 N1PC C5PC 145.3(5) . . . . ? Cu4 Cu4 N1PC C5PC 95.0(12) 3_677 . . . ? C5PC N1PC C1PC C2PC -0.2(12) . . . . ? Cu4 N1PC C1PC C2PC 170.9(6) . . . . ? N1PC C1PC C2PC C3PC 4.3(13) . . . . ? C1PC C2PC C3PC C4PC -5.3(14) . . . . ? C2PC C3PC C4PC C5PC 2.7(15) . . . . ? C1PC N1PC C5PC C4PC -2.5(11) . . . . ? Cu4 N1PC C5PC C4PC -174.2(6) . . . . ? C3PC C4PC C5PC N1PC 1.1(14) . . . . ? C12G C2G C11G C15G 3.5(14) . . . . ? C22G C2G C11G C15G -27(2) . . . . ? C13G C2G C11G C15G -59(3) . . . . ? C22G C2G C11G C12G -30.0(17) . . . . ? C13G C2G C11G C12G -63(3) . . . . ? C21G C3G C12G C15G -4.3(15) . . . . ? C15G C3G C12G C22G 137(3) . . . . ? C21G C3G C12G C22G 133(3) . . . . ? C15G C3G C12G C2G 15(5) . . . . ? C21G C3G C12G C2G 11(5) . . . . ? C15G C3G C12G C11G 2.0(11) . . . . ? C21G C3G C12G C11G -2.3(19) . . . . ? C11G C2G C12G C3G -16(5) . . . . ? C22G C2G C12G C3G 132(5) . . . . ? C13G C2G C12G C3G 142(5) . . . . ? C11G C2G C12G C15G -2.6(11) . . . . ? C22G C2G C12G C15G 145(2) . . . . ? C13G C2G C12G C15G 155.1(12) . . . . ? C11G C2G C12G C22G -148.0(18) . . . . ? C13G C2G C12G C22G 9.7(18) . . . . ? C22G C2G C12G C11G 148.0(18) . . . . ? C13G C2G C12G C11G 157.7(12) . . . . ? C15G C11G C12G C3G -2.3(13) . . . . ? C2G C11G C12G C3G 174.3(17) . . . . ? C2G C11G C12G C15G 176.6(14) . . . . ? C15G C11G C12G C22G -147(2) . . . . ? C2G C11G C12G C22G 29.9(17) . . . . ? C15G C11G C12G C2G -176.6(14) . . . . ? C22G C1G C13G C2G 17(2) . . . . ? C11G C2G C13G C22G 44(4) . . . . ? C12G C2G C13G C22G -12(2) . . . . ? C11G C2G C13G C1G 28(4) . . . . ? C12G C2G C13G C1G -29(2) . . . . ? C22G C2G C13G C1G -17(2) . . . . ? C2G C11G C15G C21G 152(7) . . . . ? C12G C11G C15G C21G 155(7) . . . . ? C2G C11G C15G C3G -1(2) . . . . ? C12G C11G C15G C3G 2.3(13) . . . . ? C2G C11G C15G C14G 178.7(14) . . . . ? C12G C11G C15G C14G -177.8(17) . . . . ? C2G C11G C15G C12G -3.6(15) . . . . ? C12G C3G C15G C21G -173(3) . . . . ? C12G C3G C15G C11G -2.7(15) . . . . ? C21G C3G C15G C11G 170(3) . . . . ? C12G C3G C15G C14G 177.4(18) . . . . ? C21G C3G C15G C14G -10(2) . . . . ? C21G C3G C15G C12G 173(2) . . . . ? C23G C14G C15G C21G 11(3) . . . . ? C21G C14G C15G C11G -166(3) . . . . ? C23G C14G C15G C11G -155(2) . . . . ? C21G C14G C15G C3G 13(3) . . . . ? C23G C14G C15G C3G 25(2) . . . . ? C21G C14G C15G C12G 29(12) . . . . ? C23G C14G C15G C12G 41(12) . . . . ? C3G C12G C15G C21G 9(3) . . . . ? C22G C12G C15G C21G -109(4) . . . . ? C2G C12G C15G C21G -166(3) . . . . ? C11G C12G C15G C21G -169(3) . . . . ? C3G C12G C15G C11G 177.6(13) . . . . ? C22G C12G C15G C11G 60(3) . . . . ? C2G C12G C15G C11G 2.6(11) . . . . ? C22G C12G C15G C3G -117(3) . . . . ? C2G C12G C15G C3G -175.0(15) . . . . ? C11G C12G C15G C3G -177.6(13) . . . . ? C3G C12G C15G C14G -17(12) . . . . ? C22G C12G C15G C14G -135(11) . . . . ? C2G C12G C15G C14G 168(11) . . . . ? C11G C12G C15G C14G 165(12) . . . . ? C11G C15G C21G C14G 35(8) . . . . ? C3G C15G C21G C14G -168(3) . . . . ? C12G C15G C21G C14G -175(2) . . . . ? C11G C15G C21G C3G -157(7) . . . . ? C14G C15G C21G C3G 168(3) . . . . ? C12G C15G C21G C3G -7(3) . . . . ? C11G C15G C21G C23G -30(21) . . . . ? C3G C15G C21G C23G 127(16) . . . . ? C14G C15G C21G C23G -65(15) . . . . ? C12G C15G C21G C23G 120(15) . . . . ? C23G C14G C21G C15G -168(3) . . . . ? C15G C14G C21G C3G -36(8) . . . . ? C23G C14G C21G C3G 156(10) . . . . ? C15G C14G C21G C23G 168(3) . . . . ? C12G C3G C21G C15G 6(2) . . . . ? C12G C3G C21G C14G 45(10) . . . . ? C15G C3G C21G C14G 39(9) . . . . ? C12G C3G C21G C23G -161(3) . . . . ? C15G C3G C21G C23G -168(4) . . . . ? C2G C13G C22G C1G -165.9(16) . . . . ? C1G C13G C22G C12G -179(4) . . . . ? C2G C13G C22G C12G 16(3) . . . . ? C1G C13G C22G C2G 165.9(16) . . . . ? C13G C1G C22G C12G 175(14) . . . . ? C13G C1G C22G C2G -18(2) . . . . ? C3G C12G C22G C13G -179(3) . . . . ? C15G C12G C22G C13G -86(5) . . . . ? C2G C12G C22G C13G -17(3) . . . . ? C11G C12G C22G C13G -42(4) . . . . ? C3G C12G C22G C1G 7(14) . . . . ? C15G C12G C22G C1G 100(13) . . . . ? C2G C12G C22G C1G 169(13) . . . . ? C11G C12G C22G C1G 144(12) . . . . ? C3G C12G C22G C2G -162(2) . . . . ? C15G C12G C22G C2G -68(3) . . . . ? C11G C12G C22G C2G -24.6(13) . . . . ? C11G C2G C22G C13G -160.5(17) . . . . ? C12G C2G C22G C13G 166(3) . . . . ? C11G C2G C22G C1G -143(3) . . . . ? C12G C2G C22G C1G -177(4) . . . . ? C13G C2G C22G C1G 17(2) . . . . ? C11G C2G C22G C12G 33.6(18) . . . . ? C13G C2G C22G C12G -166(3) . . . . ? C15G C21G C23G C14G 67(16) . . . . ? C3G C21G C23G C14G -171(4) . . . . ? C15G C14G C23G C21G -8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.139 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.132 data_mbco35 _database_code_CSD 202851 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H11 Co N O6.48' _chemical_formula_weight 391.80 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 30.3087(15) _cell_length_b 30.3087(15) _cell_length_c 18.3364(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14587.4(15) _cell_formula_units_Z 36 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red/purpl _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.75 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7157 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type none _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 '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 30199 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3985 _reflns_number_gt 2650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0523P)^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 3985 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 Co1 Co 0.306224(16) 0.188734(16) 0.13346(2) 0.01866(13) Uani 1 1 d . . . N1 N 0.26346(10) 0.20331(10) 0.05834(14) 0.0198(6) Uani 1 1 d . . . O1 O 0.34929(9) 0.18989(9) 0.27857(12) 0.0275(5) Uani 1 1 d . . . O2 O 0.37697(8) 0.24265(8) 0.10374(13) 0.0256(5) Uani 1 1 d . . . O3 O 0.31067(9) 0.22775(9) 0.22492(12) 0.0266(5) Uani 1 1 d . . . O4 O 0.41948(8) 0.20932(8) 0.15963(12) 0.0263(5) Uani 1 1 d . . . C1 C 0.20185(13) 0.19841(13) 0.14589(19) 0.0270(8) Uani 1 1 d . . . H1 H 0.2217 0.1964 0.1845 0.032 Uiso 1 1 calc R . . C2 C 0.41711(12) 0.24335(12) 0.12336(17) 0.0212(7) Uani 1 1 d . . . C3 C 0.33064(11) 0.24327(11) 0.35078(17) 0.0192(7) Uani 1 1 d . . . C4 C 0.46595(14) 0.3333 0.0833 0.0188(9) Uani 1 2 d S . . H4 H 0.4346 0.3333 0.0833 0.023 Uiso 1 2 calc SR . . C5 C 0.21832(12) 0.20259(12) 0.07315(18) 0.0220(7) Uani 1 1 d . . . C6 C 0.32914(12) 0.28872(12) 0.35164(18) 0.0228(7) Uani 1 1 d . . . H6 H 0.3252 0.3026 0.3073 0.027 Uiso 1 1 calc R . . C7 C 0.3333 0.22219(14) 0.4167 0.0186(9) Uani 1 2 d S . . H7 H 0.3333 0.1909 0.4167 0.022 Uiso 1 2 calc SR . . C8 C 0.33006(12) 0.21838(12) 0.27989(17) 0.0217(7) Uani 1 1 d . . . C9 C 0.3333 0.31333(14) 0.4167 0.0255(11) Uani 1 2 d S . . H9 H 0.3333 0.3447 0.4167 0.031 Uiso 1 2 calc SR . . C10 C 0.46644(12) 0.28973(11) 0.10287(17) 0.0190(7) Uani 1 1 d . . . C11 C 0.18877(13) 0.20658(13) 0.0163(2) 0.0274(8) Uani 1 1 d . . . C12 C 0.20724(14) 0.21294(14) -0.0552(2) 0.0355(9) Uani 1 1 d . . . H12 H 0.1884 0.2162 -0.0942 0.043 Uiso 1 1 calc R . . C13 C 0.25190(15) 0.21451(14) -0.06880(19) 0.0341(9) Uani 1 1 d . . . H13 H 0.2649 0.2192 -0.1170 0.041 Uiso 1 1 calc R . . C14 C 0.27854(13) 0.20909(12) -0.01014(18) 0.0261(8) Uani 1 1 d . . . H14 H 0.3095 0.2096 -0.0205 0.031 Uiso 1 1 calc R . . C15 C 0.14286(13) 0.20543(14) 0.0345(2) 0.0370(9) Uani 1 1 d . . . H15 H 0.1228 0.2082 -0.0031 0.044 Uiso 1 1 calc R . . C16 C 0.15686(14) 0.19724(14) 0.1604(2) 0.0353(9) Uani 1 1 d . . . H16 H 0.1457 0.1942 0.2095 0.042 Uiso 1 1 calc R . . C17 C 0.55694(16) 0.3333 0.0833 0.0305(12) Uani 1 2 d S . . H17 H 0.5883 0.3333 0.0833 0.037 Uiso 1 2 calc SR . . C18 C 0.51247(12) 0.29007(12) 0.10508(19) 0.0250(8) Uani 1 1 d . . . H18 H 0.5135 0.2608 0.1214 0.030 Uiso 1 1 calc R . . C19 C 0.12713(14) 0.20042(15) 0.1047(2) 0.0393(10) Uani 1 1 d . . . H19 H 0.0959 0.1991 0.1160 0.047 Uiso 1 1 calc R . . O101 O 0.2861(8) 0.5838(6) 0.2002(10) 0.119(5) Uiso 0.38 1 d P . . O102 O 0.3342(5) 0.6087(6) 0.0090(8) 0.118(4) Uiso 0.38 1 d P . . O103 O 0.3333 0.6667 -0.0205(17) 0.122(10) Uiso 0.30 3 d SP . . O104 O 0.3370(7) 0.5993(7) 0.0814(11) 0.154(6) Uiso 0.38 1 d P . . O105 O 0.2539(13) 0.5889(13) 0.149(2) 0.188(11) Uiso 0.25 1 d P . . O106 O 0.2927(9) 0.5872(7) 0.1258(12) 0.106(6) Uiso 0.25 1 d P . . O107 O 0.2983(9) 0.6474(11) 0.0232(15) 0.169(11) Uiso 0.25 1 d P . . O108 O 0.2858(9) 0.6216(9) 0.0983(13) 0.128(7) Uiso 0.25 1 d P . . O109 O 0.2545(11) 0.5584(11) 0.2181(16) 0.156(10) Uiso 0.25 1 d P . . 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 Co1 0.0212(2) 0.0196(2) 0.0144(2) 0.00222(18) -0.00084(19) 0.00965(19) N1 0.0262(14) 0.0213(14) 0.0151(14) -0.0006(11) -0.0021(12) 0.0142(12) O1 0.0374(14) 0.0309(13) 0.0202(12) -0.0063(11) -0.0033(11) 0.0216(11) O2 0.0230(12) 0.0224(12) 0.0281(13) 0.0051(10) 0.0021(11) 0.0089(10) O3 0.0354(13) 0.0307(13) 0.0140(11) -0.0019(10) -0.0033(10) 0.0169(11) O4 0.0300(13) 0.0191(11) 0.0254(13) 0.0070(10) 0.0026(11) 0.0089(10) C1 0.0281(18) 0.035(2) 0.0210(19) 0.0036(16) -0.0017(15) 0.0179(16) C2 0.0288(18) 0.0181(16) 0.0139(16) -0.0047(13) 0.0025(14) 0.0096(14) C3 0.0192(16) 0.0201(16) 0.0179(16) -0.0019(13) -0.0019(14) 0.0095(13) C4 0.0217(16) 0.024(2) 0.011(2) -0.0036(19) -0.0018(9) 0.0120(12) C5 0.0223(17) 0.0195(16) 0.0228(18) 0.0003(14) -0.0019(14) 0.0096(14) C6 0.0266(17) 0.0269(17) 0.0160(16) 0.0034(14) -0.0007(14) 0.0142(15) C7 0.021(2) 0.0182(16) 0.017(2) -0.0004(9) -0.0007(19) 0.0105(11) C8 0.0227(17) 0.0204(16) 0.0152(16) 0.0019(14) 0.0019(14) 0.0057(14) C9 0.034(3) 0.0196(16) 0.028(3) 0.0006(11) 0.001(2) 0.0169(14) C10 0.0237(17) 0.0169(15) 0.0130(16) -0.0006(13) 0.0008(13) 0.0077(13) C11 0.0315(19) 0.0267(18) 0.026(2) 0.0020(15) -0.0048(16) 0.0160(16) C12 0.048(2) 0.045(2) 0.0212(19) -0.0007(18) -0.0125(18) 0.029(2) C13 0.051(2) 0.046(2) 0.0130(17) 0.0032(17) 0.0014(17) 0.030(2) C14 0.037(2) 0.0278(18) 0.0194(17) -0.0019(15) 0.0007(16) 0.0202(16) C15 0.032(2) 0.044(2) 0.039(2) 0.0051(19) -0.0099(18) 0.0220(18) C16 0.033(2) 0.046(2) 0.029(2) 0.0066(18) 0.0081(17) 0.0214(19) C17 0.0231(18) 0.029(3) 0.041(3) -0.004(2) -0.0020(12) 0.0143(13) C18 0.0290(18) 0.0197(16) 0.0273(19) -0.0009(15) -0.0025(16) 0.0128(15) C19 0.027(2) 0.052(2) 0.046(3) 0.006(2) 0.0019(19) 0.0252(19) _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 Co1 O2 2.015(2) . ? Co1 O3 2.017(2) . ? Co1 O4 2.021(2) 25 ? Co1 N1 2.085(3) . ? Co1 O1 2.132(2) 25 ? Co1 Co1 2.8584(8) 25 ? N1 C14 1.318(4) . ? N1 C5 1.384(4) . ? O1 C8 1.261(4) . ? O1 Co1 2.132(2) 25 ? O2 C2 1.259(4) . ? O3 C8 1.269(4) . ? O4 C2 1.259(4) . ? O4 Co1 2.021(2) 25 ? C1 C16 1.372(5) . ? C1 C5 1.408(5) . ? C2 C10 1.500(4) . ? C3 C7 1.388(4) . ? C3 C6 1.401(4) . ? C3 C8 1.499(4) . ? C4 C10 1.377(4) . ? C4 C10 1.377(4) 17_554 ? C5 C11 1.418(5) . ? C6 C9 1.378(4) . ? C7 C3 1.388(4) 12 ? C9 C6 1.378(4) 12 ? C10 C18 1.391(4) . ? C11 C12 1.401(5) . ? C11 C15 1.414(5) . ? C12 C13 1.354(5) . ? C13 C14 1.403(5) . ? C15 C19 1.354(5) . ? C16 C19 1.397(5) . ? C17 C18 1.388(4) 17_554 ? C17 C18 1.388(4) . ? O101 O109 0.94(3) . ? O101 O104 1.27(2) 26_455 ? O101 O105 1.36(3) 27 ? O101 O106 1.38(2) . ? O101 O108 1.39(2) 27 ? O101 O105 1.42(3) . ? O102 O107 1.14(3) 2_665 ? O102 O104 1.37(2) . ? O103 O107 1.22(3) . ? O103 O107 1.22(3) 3_565 ? O103 O107 1.22(3) 2_665 ? O104 O109 1.18(3) 27 ? O104 O101 1.27(2) 27 ? O104 O106 1.45(2) . ? O104 O108 1.75(3) 2_665 ? O104 O107 1.75(3) 2_665 ? O105 O106 1.27(3) . ? O105 O108 1.34(4) . ? O105 O101 1.36(3) 26_455 ? O105 O109 1.58(4) . ? O105 O106 1.60(3) 26_455 ? O106 O108 1.27(3) . ? O106 O105 1.60(3) 27 ? O107 O102 1.14(3) 3_565 ? O107 O108 1.53(3) . ? O107 O107 1.60(4) 3_565 ? O107 O107 1.60(4) 2_665 ? O107 O104 1.75(3) 3_565 ? O108 O101 1.39(2) 26_455 ? O108 O104 1.75(3) 3_565 ? O109 O104 1.18(3) 26_455 ? 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 Co1 O3 90.99(10) . . ? O2 Co1 O4 162.29(9) . 25 ? O3 Co1 O4 91.87(9) . 25 ? O2 Co1 N1 99.88(10) . . ? O3 Co1 N1 106.94(10) . . ? O4 Co1 N1 95.99(10) 25 . ? O2 Co1 O1 83.81(9) . 25 ? O3 Co1 O1 162.66(9) . 25 ? O4 Co1 O1 88.33(9) 25 25 ? N1 Co1 O1 90.27(9) . 25 ? O2 Co1 Co1 82.37(7) . 25 ? O3 Co1 Co1 91.99(7) . 25 ? O4 Co1 Co1 80.07(7) 25 25 ? N1 Co1 Co1 160.84(8) . 25 ? O1 Co1 Co1 70.96(6) 25 25 ? C14 N1 C5 117.6(3) . . ? C14 N1 Co1 116.5(2) . . ? C5 N1 Co1 125.5(2) . . ? C8 O1 Co1 136.9(2) . 25 ? C2 O2 Co1 124.3(2) . . ? C8 O3 Co1 115.6(2) . . ? C2 O4 Co1 127.0(2) . 25 ? C16 C1 C5 119.3(3) . . ? O2 C2 O4 126.0(3) . . ? O2 C2 C10 116.5(3) . . ? O4 C2 C10 117.5(3) . . ? C7 C3 C6 118.7(3) . . ? C7 C3 C8 120.8(3) . . ? C6 C3 C8 120.5(3) . . ? C10 C4 C10 121.2(4) . 17_554 ? N1 C5 C1 119.4(3) . . ? N1 C5 C11 121.1(3) . . ? C1 C5 C11 119.5(3) . . ? C9 C6 C3 120.2(3) . . ? C3 C7 C3 121.4(4) . 12 ? O1 C8 O3 124.3(3) . . ? O1 C8 C3 117.9(3) . . ? O3 C8 C3 117.8(3) . . ? C6 C9 C6 120.6(4) 12 . ? C4 C10 C18 119.5(3) . . ? C4 C10 C2 118.7(3) . . ? C18 C10 C2 121.7(3) . . ? C12 C11 C15 123.0(3) . . ? C12 C11 C5 118.3(3) . . ? C15 C11 C5 118.7(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C14 118.6(3) . . ? N1 C14 C13 124.4(3) . . ? C19 C15 C11 120.9(3) . . ? C1 C16 C19 121.6(4) . . ? C18 C17 C18 120.2(4) 17_554 . ? C17 C18 C10 119.7(3) . . ? C15 C19 C16 120.0(3) . . ? O109 O101 O104 62(2) . 26_455 ? O109 O101 O105 136(3) . 27 ? O104 O101 O105 138(3) 26_455 27 ? O109 O101 O106 117(3) . . ? O104 O101 O106 142(2) 26_455 . ? O105 O101 O106 71.5(17) 27 . ? O109 O101 O108 132(3) . 27 ? O104 O101 O108 82.0(17) 26_455 27 ? O105 O101 O108 58.4(18) 27 27 ? O106 O101 O108 110.3(19) . 27 ? O109 O101 O105 81(3) . . ? O104 O101 O105 90.8(19) 26_455 . ? O105 O101 O105 125.3(19) 27 . ? O106 O101 O105 54.1(15) . . ? O108 O101 O105 133(2) 27 . ? O107 O102 O104 88.0(19) 2_665 . ? O107 O103 O107 82(3) . 3_565 ? O107 O103 O107 82(3) . 2_665 ? O107 O103 O107 82(3) 3_565 2_665 ? O109 O104 O101 44.9(16) 27 27 ? O109 O104 O102 134(2) 27 . ? O101 O104 O102 137.3(19) 27 . ? O109 O104 O106 107(2) 27 . ? O101 O104 O106 95.1(17) 27 . ? O102 O104 O106 116.7(19) . . ? O109 O104 O108 92(2) 27 2_665 ? O101 O104 O108 52.0(13) 27 2_665 ? O102 O104 O108 91.3(15) . 2_665 ? O106 O104 O108 103.8(14) . 2_665 ? O109 O104 O107 131(2) 27 2_665 ? O101 O104 O107 103.0(18) 27 2_665 ? O102 O104 O107 40.6(12) . 2_665 ? O106 O104 O107 111.8(17) . 2_665 ? O108 O104 O107 52.0(12) 2_665 2_665 ? O106 O105 O108 57.9(19) . . ? O106 O105 O101 118(3) . 26_455 ? O108 O105 O101 62(2) . 26_455 ? O106 O105 O101 61.0(17) . . ? O108 O105 O101 105(3) . . ? O101 O105 O101 128(3) 26_455 . ? O106 O105 O109 88(3) . . ? O108 O105 O109 140(3) . . ? O101 O105 O109 138(3) 26_455 . ? O101 O105 O109 35.9(15) . . ? O106 O105 O106 126(3) . 26_455 ? O108 O105 O106 101(2) . 26_455 ? O101 O105 O106 54.6(14) 26_455 26_455 ? O101 O105 O106 83(2) . 26_455 ? O109 O105 O106 84(2) . 26_455 ? O108 O106 O105 64(2) . . ? O108 O106 O101 112(2) . . ? O105 O106 O101 64.9(19) . . ? O108 O106 O104 95(2) . . ? O105 O106 O104 158(3) . . ? O101 O106 O104 131(2) . . ? O108 O106 O105 134(2) . 27 ? O105 O106 O105 118.4(18) . 27 ? O101 O106 O105 53.8(14) . 27 ? O104 O106 O105 77.9(19) . 27 ? O102 O107 O103 103(3) 3_565 . ? O102 O107 O108 114(3) 3_565 . ? O103 O107 O108 140(3) . . ? O102 O107 O107 91(3) 3_565 3_565 ? O103 O107 O107 49.2(13) . 3_565 ? O108 O107 O107 113.0(12) . 3_565 ? O102 O107 O107 148(3) 3_565 2_665 ? O103 O107 O107 49.2(13) . 2_665 ? O108 O107 O107 91(2) . 2_665 ? O107 O107 O107 60.000(11) 3_565 2_665 ? O102 O107 O104 51.4(15) 3_565 3_565 ? O103 O107 O104 141(3) . 3_565 ? O108 O107 O104 64.0(16) . 3_565 ? O107 O107 O104 98(2) 3_565 3_565 ? O107 O107 O104 138.0(12) 2_665 3_565 ? O106 O108 O105 58.3(19) . . ? O106 O108 O101 117(2) . 26_455 ? O105 O108 O101 59.7(18) . 26_455 ? O106 O108 O107 133(3) . . ? O105 O108 O107 153(3) . . ? O101 O108 O107 109(2) 26_455 . ? O106 O108 O104 163(2) . 3_565 ? O105 O108 O104 104(2) . 3_565 ? O101 O108 O104 46.0(12) 26_455 3_565 ? O107 O108 O104 64.0(16) . 3_565 ? O101 O109 O104 73(2) . 26_455 ? O101 O109 O105 63(2) . . ? O104 O109 O105 87(2) 26_455 . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.654 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.120 data_jl8132 _database_code_CSD 202852 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 Cu2 N2 O8' _chemical_formula_weight 713.62 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 30.337(2) _cell_length_b 30.337(2) _cell_length_c 18.380(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14649(2) _cell_formula_units_Z 18 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6516 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 18919 _diffrn_reflns_av_R_equivalents 0.1775 _diffrn_reflns_av_sigmaI/netI 0.1795 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2352 _reflns_number_gt 1145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0704P)^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 2352 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _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 0.51927(4) 0.97383(4) 0.03335(6) 0.0285(4) Uani 1 1 d . . . O1 O 0.4798(2) 0.9828(2) 0.1143(3) 0.0352(17) Uani 1 1 d . . . O2 O 0.5762(2) 1.0412(2) 0.0588(3) 0.0348(17) Uani 1 1 d . . . O3 O 0.4571(2) 0.9151(2) -0.0050(3) 0.0317(16) Uani 1 1 d . . . O4 O 0.5547(2) 0.9769(2) -0.0583(3) 0.0343(17) Uani 1 1 d . . . N1 N 0.5380(3) 0.9284(3) 0.1068(4) 0.032(2) Uani 1 1 d . . . C1 C 0.5355(3) 0.8825(4) 0.0914(6) 0.034(3) Uani 1 1 d . . . C2 C 0.5453(4) 0.9430(4) 0.1751(5) 0.039(3) Uani 1 1 d . . . H2 H 0.5477 0.9747 0.1863 0.01(2) Uiso 1 1 calc R . . C3 C 0.5300(4) 0.8659(4) 0.0200(6) 0.041(3) Uani 1 1 d . . . H3 H 0.5275 0.8857 -0.0181 0.06(4) Uiso 1 1 calc R . . C4 C 0.5393(4) 0.8525(4) 0.1477(6) 0.040(3) Uani 1 1 d . . . C5 C 0.5497(4) 0.9155(5) 0.2325(6) 0.050(3) Uani 1 1 d . . . H5 H 0.5552 0.9284 0.2808 0.05(3) Uiso 1 1 calc R . . C6 C 0.5281(4) 0.8208(4) 0.0045(7) 0.052(3) Uani 1 1 d . . . H6 H 0.5242 0.8095 -0.0445 0.07(4) Uiso 1 1 calc R . . C7 C 0.5368(4) 0.8061(4) 0.1280(7) 0.055(3) Uani 1 1 d . . . H7 H 0.5388 0.7852 0.1649 0.04(3) Uiso 1 1 calc R . . C8 C 0.5459(4) 0.8700(5) 0.2177(6) 0.052(3) Uani 1 1 d . . . H8 H 0.5479 0.8502 0.2562 0.08(4) Uiso 1 1 calc R . . C9 C 0.5318(4) 0.7911(4) 0.0591(7) 0.059(3) Uani 1 1 d . . . H9 H 0.5308 0.7602 0.0471 0.04(3) Uiso 1 1 calc R . . C10 C 0.4529(3) 1.0036(3) 0.1142(5) 0.028(2) Uani 1 1 d . . . C11 C 0.4276(3) 1.0033(3) 0.1851(5) 0.025(2) Uani 1 1 d . . . C12 C 0.4475(5) 1.0000 0.2500 0.030(3) Uani 1 2 d S . . H12 H 0.4788 1.0000 0.2500 0.03(4) Uiso 1 2 calc SR . . C13 C 0.3828(4) 1.0046(3) 0.1853(5) 0.029(2) Uani 1 1 d . . . H13 H 0.3690 1.0087 0.1410 0.01(2) Uiso 1 1 calc R . . C14 C 0.3584(4) 1.0000 0.2500 0.033(4) Uani 1 2 d S . . H14 H 0.3271 1.0000 0.2500 0.05(4) Uiso 1 2 calc SR . . C15 C 0.5773(3) 1.0819(4) 0.0405(5) 0.028(2) Uani 1 1 d . . . C16 C 0.6234(3) 1.1308(4) 0.0623(5) 0.027(2) Uani 1 1 d . . . C17 C 0.6247(4) 1.1773(4) 0.0597(5) 0.035(3) Uani 1 1 d . . . H17 H 0.5961 1.1787 0.0412 0.03(3) Uiso 1 1 calc R . . C18 C 0.6667 1.1306(4) 0.0833 0.028(3) Uani 1 2 d S . . H18 H 0.6667 1.0993 0.0833 0.01(3) Uiso 1 2 calc SR . . C19 C 0.6667 1.2215(5) 0.0833 0.042(4) Uani 1 2 d S . . H19 H 0.6667 1.2528 0.0833 0.03(4) Uiso 1 2 calc SR . . C1S C 0.3976(19) 0.6729(18) 0.282(3) 0.185(19) Uiso 0.50 1 d P . . C2S C 0.4195(14) 0.6872(18) 0.213(3) 0.131(15) Uiso 0.50 1 d P . . C3S C 0.4089(15) 0.7007(18) 0.129(3) 0.157(14) Uiso 0.50 1 d P . . C4S C 0.3830(18) 0.638(2) 0.126(3) 0.154(17) Uiso 0.50 1 d P . . C5S C 0.3657(13) 0.671(2) 0.325(2) 0.166(18) Uiso 0.50 1 d P . . 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 0.0279(7) 0.0375(8) 0.0198(6) 0.0009(6) -0.0009(6) 0.0161(6) O1 0.042(4) 0.052(5) 0.017(4) 0.003(3) 0.006(3) 0.027(4) O2 0.030(4) 0.029(4) 0.039(4) -0.012(4) -0.014(3) 0.010(4) O3 0.024(4) 0.031(4) 0.034(4) 0.001(3) -0.006(3) 0.009(3) O4 0.041(4) 0.043(4) 0.023(4) 0.005(3) 0.001(3) 0.025(4) N1 0.030(5) 0.043(5) 0.026(5) 0.004(4) 0.002(4) 0.022(4) C1 0.028(6) 0.047(7) 0.032(6) 0.005(6) 0.005(5) 0.023(6) C2 0.044(7) 0.058(8) 0.028(6) -0.003(6) 0.004(6) 0.035(6) C3 0.046(7) 0.037(7) 0.037(7) 0.001(6) -0.003(6) 0.018(6) C4 0.046(7) 0.051(8) 0.028(7) 0.001(6) -0.001(5) 0.029(6) C5 0.063(8) 0.092(10) 0.015(6) 0.005(7) -0.004(6) 0.054(8) C6 0.072(9) 0.050(8) 0.045(8) -0.021(7) -0.020(7) 0.039(7) C7 0.059(8) 0.056(9) 0.057(9) 0.018(7) -0.003(7) 0.035(7) C8 0.069(9) 0.072(9) 0.032(7) 0.018(7) 0.005(6) 0.047(8) C9 0.085(10) 0.043(8) 0.056(9) -0.009(7) -0.013(8) 0.039(7) C10 0.028(6) 0.028(6) 0.022(6) -0.004(5) -0.004(5) 0.012(5) C11 0.029(6) 0.023(5) 0.020(5) -0.001(5) -0.005(5) 0.011(5) C12 0.031(6) 0.034(9) 0.027(9) -0.003(7) -0.001(3) 0.017(4) C13 0.038(6) 0.028(6) 0.019(6) 0.002(5) -0.004(5) 0.016(5) C14 0.021(6) 0.049(10) 0.038(9) -0.011(8) -0.006(4) 0.025(5) C15 0.024(6) 0.042(7) 0.012(5) -0.001(5) 0.009(5) 0.012(5) C16 0.023(6) 0.037(6) 0.014(5) 0.006(5) 0.004(4) 0.010(5) C17 0.026(6) 0.042(7) 0.033(7) 0.003(5) 0.001(5) 0.014(6) C18 0.030(9) 0.029(6) 0.024(8) 0.002(3) 0.005(7) 0.015(4) C19 0.040(10) 0.033(7) 0.057(12) 0.002(4) 0.004(9) 0.020(5) _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 1.962(6) . ? Cu1 O3 1.967(6) . ? Cu1 O4 1.974(6) . ? Cu1 O1 2.011(6) . ? Cu1 N1 2.197(8) . ? Cu1 Cu1 2.692(2) 19_675 ? O1 C10 1.258(10) . ? O2 C15 1.264(10) . ? O3 C15 1.270(10) 19_675 ? O4 C10 1.262(10) 19_675 ? N1 C2 1.312(12) . ? N1 C1 1.386(11) . ? C1 C3 1.385(13) . ? C1 C4 1.421(13) . ? C2 C5 1.391(13) . ? C3 C6 1.372(13) . ? C4 C8 1.369(14) . ? C4 C7 1.419(13) . ? C5 C8 1.354(14) . ? C6 C9 1.388(14) . ? C7 C9 1.328(14) . ? C10 O4 1.262(10) 19_675 ? C10 C11 1.511(12) . ? C11 C12 1.363(10) . ? C11 C13 1.379(12) . ? C12 C11 1.363(10) 5_675 ? C13 C14 1.371(10) . ? C14 C13 1.371(10) 5_675 ? C15 O3 1.270(10) 19_675 ? C15 C16 1.496(12) . ? C16 C18 1.373(11) . ? C16 C17 1.393(12) . ? C17 C19 1.378(11) . ? C18 C16 1.373(11) 18_654 ? C19 C17 1.378(11) 18_654 ? C1S C5S 1.22(5) . ? C1S C2S 1.40(6) . ? C1S C4S 1.81(7) 27 ? C1S C3S 1.92(6) 26_455 ? C2S C4S 1.03(5) 27 ? C2S C3S 1.66(6) . ? C2S C3S 1.76(5) 26_455 ? C3S C4S 1.49(5) 27 ? C3S C4S 1.66(5) . ? C3S C2S 1.76(5) 27 ? C3S C1S 1.92(6) 27 ? C4S C2S 1.03(5) 26_455 ? C4S C3S 1.49(5) 26_455 ? C4S C1S 1.81(7) 26_455 ? C5S C5S 1.60(6) 3_565 ? C5S C5S 1.60(5) 2_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 O2 Cu1 O3 167.1(3) . . ? O2 Cu1 O4 88.8(3) . . ? O3 Cu1 O4 89.4(2) . . ? O2 Cu1 O1 87.5(3) . . ? O3 Cu1 O1 91.2(3) . . ? O4 Cu1 O1 166.2(3) . . ? O2 Cu1 N1 97.9(3) . . ? O3 Cu1 N1 94.9(3) . . ? O4 Cu1 N1 104.4(3) . . ? O1 Cu1 N1 89.3(3) . . ? O2 Cu1 Cu1 84.8(2) . 19_675 ? O3 Cu1 Cu1 82.38(18) . 19_675 ? O4 Cu1 Cu1 88.28(19) . 19_675 ? O1 Cu1 Cu1 78.11(18) . 19_675 ? N1 Cu1 Cu1 167.0(2) . 19_675 ? C10 O1 Cu1 130.3(6) . . ? C15 O2 Cu1 122.3(6) . . ? C15 O3 Cu1 124.8(6) 19_675 . ? C10 O4 Cu1 119.6(6) 19_675 . ? C2 N1 C1 116.7(9) . . ? C2 N1 Cu1 115.5(7) . . ? C1 N1 Cu1 127.1(6) . . ? C3 C1 N1 119.7(10) . . ? C3 C1 C4 119.4(10) . . ? N1 C1 C4 120.9(9) . . ? N1 C2 C5 125.1(11) . . ? C6 C3 C1 119.8(11) . . ? C8 C4 C7 123.4(11) . . ? C8 C4 C1 118.6(10) . . ? C7 C4 C1 118.0(10) . . ? C8 C5 C2 118.3(11) . . ? C3 C6 C9 121.3(11) . . ? C9 C7 C4 121.5(12) . . ? C5 C8 C4 120.4(11) . . ? C7 C9 C6 120.0(11) . . ? O1 C10 O4 123.5(9) . 19_675 ? O1 C10 C11 116.8(8) . . ? O4 C10 C11 119.7(8) 19_675 . ? C12 C11 C13 118.7(10) . . ? C12 C11 C10 120.9(9) . . ? C13 C11 C10 120.4(8) . . ? C11 C12 C11 122.7(13) . 5_675 ? C14 C13 C11 119.2(10) . . ? C13 C14 C13 121.5(13) 5_675 . ? O2 C15 O3 125.7(8) . 19_675 ? O2 C15 C16 116.9(9) . . ? O3 C15 C16 117.5(9) 19_675 . ? C18 C16 C17 118.1(10) . . ? C18 C16 C15 119.5(9) . . ? C17 C16 C15 122.3(9) . . ? C19 C17 C16 121.2(10) . . ? C16 C18 C16 122.3(13) 18_654 . ? C17 C19 C17 118.7(14) . 18_654 ? C5S C1S C2S 147(6) . . ? C5S C1S C4S 114(5) . 27 ? C2S C1S C4S 35(2) . 27 ? C5S C1S C3S 112(5) . 26_455 ? C2S C1S C3S 62(3) . 26_455 ? C4S C1S C3S 80(3) 27 26_455 ? C4S C2S C1S 95(5) 27 . ? C4S C2S C3S 62(4) 27 . ? C1S C2S C3S 143(4) . . ? C4S C2S C3S 116(4) 27 26_455 ? C1S C2S C3S 74(3) . 26_455 ? C3S C2S C3S 90(3) . 26_455 ? C4S C3S C4S 109(3) 27 . ? C4S C3S C2S 38(2) 27 . ? C4S C3S C2S 78(3) . . ? C4S C3S C2S 79(3) 27 27 ? C4S C3S C2S 147(3) . 27 ? C2S C3S C2S 117(3) . 27 ? C4S C3S C1S 123(3) 27 27 ? C4S C3S C1S 116(4) . 27 ? C2S C3S C1S 161(4) . 27 ? C2S C3S C1S 45(2) 27 27 ? C2S C4S C3S 80(4) 26_455 26_455 ? C2S C4S C3S 155(5) 26_455 . ? C3S C4S C3S 100(4) 26_455 . ? C2S C4S C1S 51(4) 26_455 26_455 ? C3S C4S C1S 123(4) 26_455 26_455 ? C3S C4S C1S 114(4) . 26_455 ? C1S C5S C5S 129(5) . 3_565 ? C1S C5S C5S 134(5) . 2_665 ? C5S C5S C5S 60.000(11) 3_565 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 O1 C10 86.9(8) . . . . ? O3 Cu1 O1 C10 -80.2(8) . . . . ? O4 Cu1 O1 C10 12.4(15) . . . . ? N1 Cu1 O1 C10 -175.1(8) . . . . ? Cu1 Cu1 O1 C10 1.7(7) 19_675 . . . ? O3 Cu1 O2 C15 7.1(16) . . . . ? O4 Cu1 O2 C15 89.3(7) . . . . ? O1 Cu1 O2 C15 -77.4(7) . . . . ? N1 Cu1 O2 C15 -166.3(7) . . . . ? Cu1 Cu1 O2 C15 0.9(6) 19_675 . . . ? O2 Cu1 O3 C15 -8.6(16) . . . 19_675 ? O4 Cu1 O3 C15 -90.8(7) . . . 19_675 ? O1 Cu1 O3 C15 75.4(7) . . . 19_675 ? N1 Cu1 O3 C15 164.8(7) . . . 19_675 ? Cu1 Cu1 O3 C15 -2.4(7) 19_675 . . 19_675 ? O2 Cu1 O4 C10 -89.3(7) . . . 19_675 ? O3 Cu1 O4 C10 78.0(7) . . . 19_675 ? O1 Cu1 O4 C10 -14.8(15) . . . 19_675 ? N1 Cu1 O4 C10 172.9(7) . . . 19_675 ? Cu1 Cu1 O4 C10 -4.4(6) 19_675 . . 19_675 ? O2 Cu1 N1 C2 52.0(7) . . . . ? O3 Cu1 N1 C2 -126.5(7) . . . . ? O4 Cu1 N1 C2 142.8(7) . . . . ? O1 Cu1 N1 C2 -35.3(7) . . . . ? Cu1 Cu1 N1 C2 -49.4(14) 19_675 . . . ? O2 Cu1 N1 C1 -138.3(7) . . . . ? O3 Cu1 N1 C1 43.2(7) . . . . ? O4 Cu1 N1 C1 -47.5(8) . . . . ? O1 Cu1 N1 C1 134.3(7) . . . . ? Cu1 Cu1 N1 C1 120.3(10) 19_675 . . . ? C2 N1 C1 C3 -177.3(9) . . . . ? Cu1 N1 C1 C3 13.1(12) . . . . ? C2 N1 C1 C4 1.6(13) . . . . ? Cu1 N1 C1 C4 -167.9(7) . . . . ? C1 N1 C2 C5 -1.2(15) . . . . ? Cu1 N1 C2 C5 169.6(8) . . . . ? N1 C1 C3 C6 179.2(9) . . . . ? C4 C1 C3 C6 0.3(15) . . . . ? C3 C1 C4 C8 178.5(10) . . . . ? N1 C1 C4 C8 -0.4(15) . . . . ? C3 C1 C4 C7 -0.6(15) . . . . ? N1 C1 C4 C7 -179.6(9) . . . . ? N1 C2 C5 C8 -0.5(17) . . . . ? C1 C3 C6 C9 -0.3(16) . . . . ? C8 C4 C7 C9 -178.1(12) . . . . ? C1 C4 C7 C9 1.0(17) . . . . ? C2 C5 C8 C4 1.8(17) . . . . ? C7 C4 C8 C5 177.8(10) . . . . ? C1 C4 C8 C5 -1.3(17) . . . . ? C4 C7 C9 C6 -1.0(19) . . . . ? C3 C6 C9 C7 0.6(18) . . . . ? Cu1 O1 C10 O4 1.2(14) . . . 19_675 ? Cu1 O1 C10 C11 179.3(5) . . . . ? O1 C10 C11 C12 25.3(12) . . . . ? O4 C10 C11 C12 -156.5(7) 19_675 . . . ? O1 C10 C11 C13 -152.5(8) . . . . ? O4 C10 C11 C13 25.7(13) 19_675 . . . ? C13 C11 C12 C11 1.6(6) . . . 5_675 ? C10 C11 C12 C11 -176.2(9) . . . 5_675 ? C12 C11 C13 C14 -3.3(12) . . . . ? C10 C11 C13 C14 174.6(7) . . . . ? C11 C13 C14 C13 1.7(6) . . . 5_675 ? Cu1 O2 C15 O3 0.6(12) . . . 19_675 ? Cu1 O2 C15 C16 -179.0(6) . . . . ? O2 C15 C16 C18 16.5(12) . . . . ? O3 C15 C16 C18 -163.2(7) 19_675 . . . ? O2 C15 C16 C17 -165.8(8) . . . . ? O3 C15 C16 C17 14.5(13) 19_675 . . . ? C18 C16 C17 C19 -5.4(12) . . . . ? C15 C16 C17 C19 176.8(7) . . . . ? C17 C16 C18 C16 2.7(6) . . . 18_654 ? C15 C16 C18 C16 -179.6(9) . . . 18_654 ? C16 C17 C19 C17 2.8(6) . . . 18_654 ? C5S C1S C2S C4S 28(12) . . . 27 ? C3S C1S C2S C4S 116(4) 26_455 . . 27 ? C5S C1S C2S C3S -21(15) . . . . ? C4S C1S C2S C3S -49(6) 27 . . . ? C3S C1S C2S C3S 67(6) 26_455 . . . ? C5S C1S C2S C3S -88(10) . . . 26_455 ? C4S C1S C2S C3S -116(4) 27 . . 26_455 ? C1S C2S C3S C4S 58(7) . . . 27 ? C3S C2S C3S C4S 120(4) 26_455 . . 27 ? C4S C2S C3S C4S -145(6) 27 . . . ? C1S C2S C3S C4S -87(7) . . . . ? C3S C2S C3S C4S -25(3) 26_455 . . . ? C4S C2S C3S C2S 3(5) 27 . . 27 ? C1S C2S C3S C2S 61(7) . . . 27 ? C3S C2S C3S C2S 123.2(16) 26_455 . . 27 ? C4S C2S C3S C1S -6(10) 27 . . 27 ? C1S C2S C3S C1S 51(13) . . . 27 ? C3S C2S C3S C1S 113(9) 26_455 . . 27 ? C4S C3S C4S C2S 96(15) 27 . . 26_455 ? C2S C3S C4S C2S 118(15) . . . 26_455 ? C2S C3S C4S C2S -3(19) 27 . . 26_455 ? C1S C3S C4S C2S -48(17) 27 . . 26_455 ? C4S C3S C4S C3S 8(6) 27 . . 26_455 ? C2S C3S C4S C3S 30(3) . . . 26_455 ? C2S C3S C4S C3S -90(7) 27 . . 26_455 ? C1S C3S C4S C3S -136(3) 27 . . 26_455 ? C4S C3S C4S C1S 141(4) 27 . . 26_455 ? C2S C3S C4S C1S 163(4) . . . 26_455 ? C2S C3S C4S C1S 42(9) 27 . . 26_455 ? C1S C3S C4S C1S -3(5) 27 . . 26_455 ? C2S C1S C5S C5S 75(14) . . . 3_565 ? C4S C1S C5S C5S 92(8) 27 . . 3_565 ? C3S C1S C5S C5S 3(9) 26_455 . . 3_565 ? C2S C1S C5S C5S -9(16) . . . 2_665 ? C4S C1S C5S C5S 8(10) 27 . . 2_665 ? C3S C1S C5S C5S -81(9) 26_455 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.994 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.147