# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew Burrows' _publ_contact_author_email A.D.BURROWS@BATH.AC.UK _publ_section_title ; Subtle structural variation in copper metal-organic frameworks: syntheses, structures, magnetic properties and application as catalysts ; loop_ _publ_author_name 'Andrew Burrows' 'J. Paul Attfield' 'Christopher G Frost' 'Mary Mahon' 'Christopher Richardson' ; J.A.Rodgers ; 'Melanie Winsper' # Attachment 'B807063F.cif' data_compound1_h06adb2 _database_code_depnum_ccdc_archive 'CCDC 686379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 Cu3 N9 O24' _chemical_formula_weight 1256.67 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 33.0450(3) _cell_length_b 18.7400(4) _cell_length_c 10.8580(5) _cell_angle_alpha 90.000 _cell_angle_beta 92.485(1) _cell_angle_gamma 90.000 _cell_volume 6717.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 131943 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description Irregular _exptl_crystal_colour Turquoise _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2580 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47807 _diffrn_reflns_av_R_equivalents 0.1221 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6002 _reflns_number_gt 4082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Lattice solvent molecules treated isotropically at atomic level, restrained to be flat, and inter-atomic distances therein also restrained to ideal values. May me more fractional solvent present (residual electron density is in the larger cavities bounded internally by nitro groups), but data quality precluded modelling of residual electron density, or indeed likely disorder in free solvent. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6002 _refine_ls_number_parameters 324 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1887 _refine_ls_R_factor_gt 0.1425 _refine_ls_wR_factor_ref 0.3697 _refine_ls_wR_factor_gt 0.3457 _refine_ls_goodness_of_fit_ref 2.415 _refine_ls_restrained_S_all 2.416 _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 0.24119(4) 0.21559(6) 0.60210(10) 0.0420(5) Uani 1 1 d . . . Cu2 Cu 0.02230(5) 0.0000 0.60422(16) 0.0593(7) Uani 1 2 d S . . O1 O 0.2242(2) 0.3114(3) 0.6537(6) 0.0457(16) Uani 1 1 d . . . O2 O 0.2416(2) 0.3696(3) 0.4853(6) 0.0525(18) Uani 1 1 d . . . O3 O 0.1517(3) 0.5579(5) 0.9629(9) 0.087(3) Uani 1 1 d . . . O4 O 0.1857(2) 0.2020(4) 0.5290(7) 0.0532(18) Uani 1 1 d . . . O5 O 0.2011(2) 0.2626(4) 0.3591(6) 0.0541(18) Uani 1 1 d . . . O6 O 0.0551(2) 0.0739(4) 0.5272(7) 0.0566(19) Uani 1 1 d . . . O7 O 0.0162(2) 0.0753(6) 0.3521(7) 0.088(3) Uani 1 1 d . . . O8 O 0.0941(4) 0.3241(10) 0.0632(13) 0.152(6) Uani 1 1 d . . . O9 O 0.0379(5) 0.2689(17) 0.064(2) 0.276(16) Uani 1 1 d . . . O10 O 0.2346(2) 0.1717(4) 0.7774(6) 0.0559(19) Uani 1 1 d D . . O11 O 0.0506(3) 0.0000 0.7801(12) 0.094(5) Uani 1 2 d SDU . . O12 O 0.1044(9) 0.1809(12) 0.829(2) 0.261(12) Uiso 1 1 d D . . O13 O 0.1694(8) 0.0000 0.966(3) 0.182(10) Uiso 1 2 d SD . . N1 N 0.1607(5) 0.5000 0.9190(13) 0.066(4) Uani 1 2 d S . . N2 N 0.0711(5) 0.2805(12) 0.1089(17) 0.154(9) Uani 1 1 d . . . N3 N 0.2112(4) 0.1792(7) 0.9688(9) 0.083(3) Uani 1 1 d D . . N4 N 0.0560(8) 0.0231(10) 0.974(2) 0.077(8) Uani 0.50 1 d PDU . . N5 N 0.0774(6) 0.2606(10) 0.6945(15) 0.136(6) Uiso 1 1 d D . . N6 N 0.1773(10) 0.0000 0.766(3) 0.245(19) Uiso 1 2 d SD . . C1 C 0.2242(5) 0.5000 0.5933(13) 0.047(3) Uani 1 2 d S . . H1 H 0.2390 0.5000 0.5202 0.056 Uiso 1 2 calc SR . . C2 C 0.2137(3) 0.4362(5) 0.6452(9) 0.044(2) Uani 1 1 d . . . C3 C 0.1925(3) 0.4358(5) 0.7505(9) 0.045(2) Uani 1 1 d . . . H3 H 0.1848 0.3920 0.7869 0.055 Uiso 1 1 calc R . . C4 C 0.1824(4) 0.5000 0.8027(15) 0.054(4) Uani 1 2 d S . . C5 C 0.2278(3) 0.3652(5) 0.5904(9) 0.041(2) Uani 1 1 d . . . C6 C 0.13528(12) 0.2174(3) 0.3746(4) 0.055(3) Uani 1 1 d G . . C7 C 0.12214(17) 0.2548(3) 0.2697(5) 0.077(4) Uani 1 1 d G . . H7 H 0.1391 0.2898 0.2354 0.093 Uiso 1 1 calc R . . C8 C 0.08415(17) 0.2409(4) 0.2150(5) 0.091(5) Uani 1 1 d G . . C9 C 0.05930(14) 0.1896(4) 0.2652(5) 0.102(6) Uani 1 1 d G . . H9 H 0.0333 0.1801 0.2278 0.123 Uiso 1 1 calc R . . C10 C 0.07244(13) 0.1523(3) 0.3700(5) 0.066(3) Uani 1 1 d G . . C11 C 0.11043(12) 0.1662(2) 0.4247(4) 0.054(3) Uani 1 1 d G . . H11 H 0.1194 0.1407 0.4964 0.065 Uiso 1 1 calc R . . C12 C 0.17755(13) 0.2276(3) 0.4231(5) 0.049(3) Uani 1 1 d G . . C13 C 0.04608(18) 0.0966(4) 0.4203(6) 0.066(3) Uani 1 1 d G . . C14 C 0.2110(3) 0.1907(6) 0.8450(6) 0.062(3) Uani 1 1 d GD . . H14 H 0.1889 0.2174 0.8105 0.074 Uiso 1 1 calc R . . C15 C 0.1843(6) 0.2099(14) 1.0503(16) 0.146(9) Uani 1 1 d D . . H15A H 0.1908 0.1929 1.1342 0.218 Uiso 1 1 calc R . . H15B H 0.1565 0.1962 1.0257 0.218 Uiso 1 1 calc R . . H15C H 0.1869 0.2620 1.0477 0.218 Uiso 1 1 calc R . . C16 C 0.2446(7) 0.1385(9) 1.0256(12) 0.126(8) Uani 1 1 d D . . H16A H 0.2409 0.1344 1.1144 0.189 Uiso 1 1 calc R . . H16B H 0.2702 0.1630 1.0117 0.189 Uiso 1 1 calc R . . H16C H 0.2452 0.0907 0.9889 0.189 Uiso 1 1 calc R . . C17 C 0.0512(6) 0.0307(11) 0.8562(18) 0.057(6) Uani 0.50 1 d PDU . . H17 H 0.0470 0.0795 0.8351 0.069 Uiso 0.50 1 calc PR . . C18 C 0.056(2) 0.081(2) 1.061(3) 0.18(2) Uani 0.50 1 d PDU . . H18A H 0.0614 0.0621 1.1441 0.273 Uiso 0.50 1 calc PR . . H18B H 0.0301 0.1053 1.0558 0.273 Uiso 0.50 1 calc PR . . H18C H 0.0778 0.1148 1.0413 0.273 Uiso 0.50 1 calc PR . . C19 C 0.0570(11) -0.0433(19) 1.038(3) 0.090(11) Uani 0.50 1 d PDU . . H19A H 0.0616 -0.0345 1.1266 0.135 Uiso 0.50 1 calc PR . . H19B H 0.0790 -0.0729 1.0082 0.135 Uiso 0.50 1 calc PR . . H19C H 0.0311 -0.0681 1.0237 0.135 Uiso 0.50 1 calc PR . . C20 C 0.1128(6) 0.3091(10) 0.708(2) 0.134(7) Uiso 1 1 d D . . H20A H 0.1095 0.3485 0.6491 0.201 Uiso 1 1 calc R . . H20B H 0.1376 0.2826 0.6914 0.201 Uiso 1 1 calc R . . H20C H 0.1148 0.3281 0.7920 0.201 Uiso 1 1 calc R . . C21 C 0.0789(9) 0.2037(13) 0.776(2) 0.205(13) Uiso 1 1 d D . . H21 H 0.0536 0.1812 0.7880 0.246 Uiso 1 1 calc R . . C22 C 0.0468(10) 0.2804(19) 0.620(3) 0.32(3) Uiso 1 1 d D . . H22A H 0.0547 0.3223 0.5727 0.480 Uiso 1 1 calc R . . H22B H 0.0235 0.2923 0.6688 0.480 Uiso 1 1 calc R . . H22C H 0.0396 0.2413 0.5634 0.480 Uiso 1 1 calc R . . C23 C 0.1577(8) 0.0000 0.874(3) 0.168(14) Uiso 1 2 d SD . . H23 H 0.1290 0.0000 0.8646 0.201 Uiso 1 2 calc SR . . C24 C 0.1569(16) 0.0000 0.649(3) 0.26(3) Uiso 1 2 d SD . . H24A H 0.1768 0.0000 0.5849 0.392 Uiso 1 2 calc SR . . H24B H 0.1399 0.0427 0.6409 0.392 Uiso 0.50 1 calc PR . . H24C H 0.1399 -0.0427 0.6409 0.392 Uiso 0.50 1 calc PR . . C25 C 0.2203(11) 0.0000 0.768(4) 0.49(7) Uiso 1 2 d SD . . H25A H 0.2309 0.0000 0.8539 0.731 Uiso 1 2 calc SR . . H25B H 0.2298 0.0427 0.7262 0.731 Uiso 0.50 1 calc PR . . H25C H 0.2298 -0.0427 0.7262 0.731 Uiso 0.50 1 calc PR . . 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 0.0511(8) 0.0285(7) 0.0463(7) -0.0009(5) 0.0010(5) -0.0061(5) Cu2 0.0265(9) 0.1041(17) 0.0470(11) 0.000 -0.0019(7) 0.000 O1 0.063(4) 0.026(3) 0.049(4) 0.001(3) 0.008(3) -0.007(3) O2 0.078(5) 0.033(4) 0.046(4) 0.001(3) 0.007(4) 0.002(3) O3 0.117(8) 0.052(5) 0.096(6) 0.000(5) 0.057(6) 0.010(5) O4 0.044(4) 0.046(4) 0.069(5) -0.007(3) -0.002(3) -0.014(3) O5 0.052(4) 0.056(4) 0.055(4) 0.001(3) 0.003(3) 0.000(4) O6 0.044(4) 0.065(5) 0.060(5) -0.002(4) -0.007(3) -0.007(4) O7 0.035(4) 0.172(10) 0.057(5) 0.014(5) -0.008(4) -0.033(5) O8 0.086(8) 0.230(17) 0.137(11) 0.092(12) -0.018(8) 0.010(10) O9 0.082(10) 0.50(4) 0.24(2) 0.25(2) -0.066(12) -0.064(16) O10 0.071(5) 0.046(4) 0.051(4) 0.006(3) 0.018(4) -0.008(4) O11 0.031(6) 0.206(17) 0.045(7) 0.000 -0.005(6) 0.000 N1 0.072(9) 0.059(9) 0.068(9) 0.000 0.021(7) 0.000 N2 0.079(11) 0.24(2) 0.140(14) 0.102(14) -0.029(10) -0.059(12) N3 0.085(8) 0.109(9) 0.056(6) 0.014(6) 0.000(6) -0.006(7) N4 0.074(12) 0.10(2) 0.054(13) -0.004(12) -0.006(12) 0.020(12) C1 0.058(9) 0.032(7) 0.050(8) 0.000 0.002(7) 0.000 C2 0.051(6) 0.031(5) 0.050(6) -0.004(4) 0.000(5) -0.002(4) C3 0.045(6) 0.027(5) 0.064(6) 0.009(4) 0.000(5) -0.007(4) C4 0.042(8) 0.053(9) 0.069(10) 0.000 0.016(7) 0.000 C5 0.050(6) 0.033(5) 0.040(5) -0.006(4) 0.000(4) -0.002(4) C6 0.044(6) 0.058(7) 0.061(7) 0.005(5) -0.002(5) 0.011(5) C7 0.061(8) 0.088(9) 0.084(9) 0.014(8) 0.002(7) -0.010(7) C8 0.043(7) 0.137(14) 0.091(10) 0.043(10) -0.016(7) 0.005(8) C9 0.036(7) 0.171(16) 0.099(11) 0.039(11) -0.002(7) -0.017(8) C10 0.044(6) 0.099(10) 0.054(7) 0.005(6) -0.002(5) 0.001(6) C11 0.033(5) 0.066(7) 0.062(6) -0.007(5) 0.001(5) 0.007(5) C12 0.050(6) 0.045(6) 0.050(6) -0.004(5) -0.009(5) -0.008(5) C13 0.050(7) 0.089(9) 0.059(7) 0.000(6) 0.016(6) -0.007(6) C14 0.080(9) 0.055(7) 0.050(7) 0.012(5) 0.008(6) -0.008(6) C15 0.140(17) 0.23(3) 0.073(10) 0.003(12) 0.069(12) -0.010(16) C16 0.24(2) 0.085(11) 0.055(9) 0.012(8) -0.027(11) -0.032(13) C17 0.037(10) 0.078(14) 0.056(13) -0.014(11) -0.002(11) 0.004(9) C18 0.24(5) 0.16(4) 0.14(3) -0.11(3) -0.09(3) 0.09(4) C19 0.070(19) 0.13(3) 0.07(2) 0.02(2) 0.00(2) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.955(7) 7_556 ? Cu1 O1 1.970(6) . ? Cu1 O5 1.977(7) 7_556 ? Cu1 O4 1.981(7) . ? Cu1 O10 2.093(7) . ? Cu1 Cu1 2.651(2) 7_556 ? Cu2 O6 1.968(7) 6 ? Cu2 O6 1.968(7) . ? Cu2 O7 1.971(9) 5_556 ? Cu2 O7 1.971(9) 2_556 ? Cu2 O11 2.090(13) . ? Cu2 Cu2 2.647(3) 5_556 ? O1 C5 1.229(11) . ? O2 C5 1.250(11) . ? O2 Cu1 1.955(7) 7_556 ? O3 N1 1.227(10) . ? O4 C12 1.265(9) . ? O5 C12 1.252(8) . ? O5 Cu1 1.977(7) 7_556 ? O6 C13 1.260(9) . ? O7 C13 1.273(9) . ? O7 Cu2 1.971(9) 5_556 ? O8 N2 1.235(18) . ? O9 N2 1.20(2) . ? O10 C14 1.150(12) . ? O11 C17 1.006(17) . ? O11 C17 1.006(17) 6 ? O12 C21 1.09(2) . ? O13 C23 1.05(2) . ? N1 O3 1.227(10) 6_565 ? N1 C4 1.48(2) . ? N2 C8 1.421(16) . ? N3 C14 1.361(11) . ? N3 C15 1.40(2) . ? N3 C16 1.46(2) . ? N4 C17 1.29(2) . ? N4 C19 1.43(2) . ? N4 C18 1.44(2) . ? N5 C22 1.32(3) . ? N5 C21 1.387(17) . ? N5 C20 1.48(2) . ? N6 C23 1.361(19) . ? N6 C24 1.407(19) . ? N6 C25 1.421(19) . ? C1 C2 1.373(12) . ? C1 C2 1.373(12) 6_565 ? C2 C3 1.367(14) . ? C2 C5 1.537(13) . ? C3 C4 1.377(12) . ? C4 C3 1.377(12) 6_565 ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C6 C12 1.4836 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C10 C13 1.4786 . ? 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 167.2(3) 7_556 . ? O2 Cu1 O5 88.5(3) 7_556 7_556 ? O1 Cu1 O5 92.0(3) . 7_556 ? O2 Cu1 O4 89.1(3) 7_556 . ? O1 Cu1 O4 87.8(3) . . ? O5 Cu1 O4 168.0(3) 7_556 . ? O2 Cu1 O10 99.5(3) 7_556 . ? O1 Cu1 O10 93.3(3) . . ? O5 Cu1 O10 91.4(3) 7_556 . ? O4 Cu1 O10 100.6(3) . . ? O2 Cu1 Cu1 85.0(2) 7_556 7_556 ? O1 Cu1 Cu1 82.53(18) . 7_556 ? O5 Cu1 Cu1 80.4(2) 7_556 7_556 ? O4 Cu1 Cu1 87.7(2) . 7_556 ? O10 Cu1 Cu1 170.6(2) . 7_556 ? O6 Cu2 O6 89.4(4) 6 . ? O6 Cu2 O7 88.4(4) 6 5_556 ? O6 Cu2 O7 168.3(3) . 5_556 ? O6 Cu2 O7 168.3(3) 6 2_556 ? O6 Cu2 O7 88.4(4) . 2_556 ? O7 Cu2 O7 91.4(6) 5_556 2_556 ? O6 Cu2 O11 98.9(3) 6 . ? O6 Cu2 O11 98.9(3) . . ? O7 Cu2 O11 92.7(3) 5_556 . ? O7 Cu2 O11 92.7(3) 2_556 . ? O6 Cu2 Cu2 86.2(2) 6 5_556 ? O6 Cu2 Cu2 86.2(2) . 5_556 ? O7 Cu2 Cu2 82.2(2) 5_556 5_556 ? O7 Cu2 Cu2 82.2(2) 2_556 5_556 ? O11 Cu2 Cu2 172.8(4) . 5_556 ? C5 O1 Cu1 123.6(6) . . ? C5 O2 Cu1 120.9(6) . 7_556 ? C12 O4 Cu1 118.2(5) . . ? C12 O5 Cu1 127.4(5) . 7_556 ? C13 O6 Cu2 121.1(5) . . ? C13 O7 Cu2 125.2(6) . 5_556 ? C14 O10 Cu1 124.0(7) . . ? C17 O11 C17 70(2) . 6 ? C17 O11 Cu2 137.9(13) . . ? C17 O11 Cu2 137.9(13) 6 . ? O3 N1 O3 124.4(14) 6_565 . ? O3 N1 C4 117.8(7) 6_565 . ? O3 N1 C4 117.8(7) . . ? O9 N2 O8 121.7(16) . . ? O9 N2 C8 118.2(15) . . ? O8 N2 C8 120.1(13) . . ? C14 N3 C15 125.5(14) . . ? C14 N3 C16 118.2(12) . . ? C15 N3 C16 115.9(13) . . ? C17 N4 C19 125.6(15) . . ? C17 N4 C18 124.4(19) . . ? C19 N4 C18 110(3) . . ? C22 N5 C21 128(2) . . ? C22 N5 C20 117.9(19) . . ? C21 N5 C20 113.8(17) . . ? C23 N6 C24 123.2(16) . . ? C23 N6 C25 119.8(15) . . ? C24 N6 C25 117(2) . . ? C2 C1 C2 121.2(13) . 6_565 ? C3 C2 C1 119.7(9) . . ? C3 C2 C5 119.6(8) . . ? C1 C2 C5 120.6(9) . . ? C2 C3 C4 118.8(9) . . ? C3 C4 C3 121.8(13) . 6_565 ? C3 C4 N1 119.1(7) . . ? C3 C4 N1 119.1(7) 6_565 . ? O1 C5 O2 127.8(9) . . ? O1 C5 C2 117.1(8) . . ? O2 C5 C2 115.1(8) . . ? C7 C6 C11 120.0 . . ? C7 C6 C12 118.8 . . ? C11 C6 C12 120.8 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 N2 119.0(7) . . ? C9 C8 N2 121.0(7) . . ? C10 C9 C8 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 C13 120.7 . . ? C9 C10 C13 119.3 . . ? C10 C11 C6 120.0 . . ? O5 C12 O4 126.2(6) . . ? O5 C12 C6 117.9(4) . . ? O4 C12 C6 115.8(4) . . ? O6 C13 O7 125.2(6) . . ? O6 C13 C10 117.3(4) . . ? O7 C13 C10 117.5(5) . . ? O10 C14 N3 127.3(10) . . ? O11 C17 N4 138(2) . . ? O12 C21 N5 130(2) . . ? O13 C23 N6 130(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.424 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.209 #===END data_compound2_h06adb1 _database_code_depnum_ccdc_archive 'CCDC 686380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 Cu3 N11 O26' _chemical_formula_weight 1401.72 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3900(2) _cell_length_b 14.7670(2) _cell_length_c 18.4650(3) _cell_angle_alpha 113.079(1) _cell_angle_beta 101.608(1) _cell_angle_gamma 100.368(1) _cell_volume 3151.52(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 75832 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Turquoise _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44207 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.88 _diffrn_reflns_theta_max 27.45 _reflns_number_total 14170 _reflns_number_gt 10222 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0899P)^2^+8.9145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14170 _refine_ls_number_parameters 764 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1902 _refine_ls_wR_factor_gt 0.1666 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.073 _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 -0.07912(4) 0.51841(4) 0.53195(3) 0.02173(14) Uani 1 1 d . . . Cu2 Cu 0.07345(4) 0.47168(4) 0.03942(3) 0.02047(13) Uani 1 1 d . . . Cu3 Cu 0.50019(4) 0.90203(4) 0.47115(3) 0.02015(13) Uani 1 1 d . . . O1 O -0.1482(2) 0.5196(2) 0.42794(18) 0.0267(7) Uani 1 1 d . . . O2 O -0.0149(3) 0.4867(3) 0.3744(2) 0.0336(8) Uani 1 1 d . . . O3 O -0.0150(3) 0.4783(3) 0.11236(19) 0.0311(7) Uani 1 1 d . . . O4 O -0.1409(3) 0.5232(3) 0.04478(19) 0.0302(7) Uani 1 1 d . . . O5 O -0.4543(4) 0.5540(5) 0.1418(3) 0.0789(18) Uani 1 1 d . . . O6 O -0.4327(4) 0.5992(5) 0.2723(3) 0.0793(17) Uani 1 1 d . . . O7 O 0.1418(3) 0.6185(2) 0.10725(19) 0.0300(7) Uani 1 1 d . . . O8 O 0.0195(3) 0.6661(2) 0.03896(19) 0.0320(7) Uani 1 1 d . . . O9 O 0.3972(3) 0.8718(2) 0.36768(19) 0.0304(7) Uani 1 1 d . . . O10 O 0.3993(2) 1.0371(2) 0.41533(19) 0.0284(7) Uani 1 1 d . . . O11 O 0.0728(5) 1.0321(4) 0.1207(3) 0.0789(18) Uani 1 1 d . . . O12 O 0.1814(5) 1.1438(3) 0.2379(3) 0.0813(18) Uani 1 1 d . . . O13 O 0.3825(2) 0.8881(2) 0.5162(2) 0.0306(7) Uani 1 1 d . . . O14 O 0.3848(2) 1.0540(2) 0.5702(2) 0.0283(7) Uani 1 1 d . . . O15 O -0.0072(2) 0.6658(2) 0.5776(2) 0.0284(7) Uani 1 1 d . . . O16 O 0.1243(3) 0.6321(2) 0.5224(2) 0.0340(8) Uani 1 1 d . . . O17 O 0.0384(4) 1.0349(4) 0.7531(3) 0.0667(14) Uani 1 1 d . . . O18 O 0.1529(4) 1.1508(3) 0.7467(3) 0.0638(13) Uani 1 1 d . . . O19 O -0.2050(3) 0.5291(3) 0.5880(2) 0.0342(8) Uani 1 1 d . . . O20 O 0.1968(3) 0.4192(3) 0.0914(2) 0.0339(8) Uani 1 1 d . . . O21 O 0.5349(3) 0.7600(2) 0.4516(2) 0.0311(7) Uani 1 1 d . . . O22 O 0.0762(9) 0.9968(9) 0.4401(7) 0.082(3) Uiso 0.55 1 d PD A 1 O23 O 0.4971(6) 0.3652(7) 0.1954(6) 0.125(3) Uani 1 1 d . . . O24 O 0.7889(11) 0.2384(13) 0.0526(11) 0.154(6) Uiso 0.58 1 d PD B 1 O25 O 0.5473(16) 0.0298(13) -0.1577(12) 0.165(7) Uiso 0.50 1 d PD C 2 O26 O 0.7321(9) 0.2647(9) 0.2791(7) 0.179(4) Uiso 1 1 d D . . O22A O 0.1557(9) 0.9855(9) 0.4262(7) 0.063(3) Uiso 0.45 1 d PD D 2 O24A O 0.817(3) 0.212(3) 0.2177(19) 0.233(14) Uiso 0.42 1 d PDU E 2 O25A O 0.624(3) 0.163(5) -0.067(2) 0.42(3) Uiso 0.50 1 d PDU F 1 N1 N -0.4042(4) 0.5661(5) 0.2103(3) 0.0597(16) Uani 1 1 d . . . N2 N 0.1404(4) 1.0558(4) 0.1851(3) 0.0529(13) Uani 1 1 d . . . N3 N 0.1081(4) 1.0612(4) 0.7271(3) 0.0447(11) Uani 1 1 d . . . N4 N -0.2805(3) 0.4778(3) 0.6706(3) 0.0351(9) Uani 1 1 d . . . N5 N 0.2783(5) 0.3242(5) 0.0062(3) 0.0668(17) Uani 1 1 d . . . N6 N 0.6705(4) 0.7073(3) 0.5007(3) 0.0392(10) Uani 1 1 d . . . N7 N 0.0539(9) 0.8224(9) 0.3883(7) 0.042(3) Uiso 0.55 1 d PD A 1 N8 N 0.4645(9) 0.1935(9) 0.1120(6) 0.111(3) Uani 1 1 d . . . N9 N 0.5918(6) 0.2367(5) 0.3262(4) 0.0742(17) Uiso 1 1 d D . . N10 N 0.5702(12) 0.2047(11) -0.1259(10) 0.061(4) Uiso 0.50 1 d PD C 2 N11 N 0.9242(7) 0.2390(6) 0.1485(5) 0.088(2) Uiso 1 1 d D . . N7A N 0.0319(11) 0.8412(11) 0.3969(8) 0.044(4) Uiso 0.45 1 d PD D 2 N10A N 0.5604(14) 0.2266(14) -0.1340(11) 0.073(5) Uiso 0.50 1 d PDU F 1 C1 C -0.1038(3) 0.5041(3) 0.3722(3) 0.0237(9) Uani 1 1 d . . . C2 C -0.1593(3) 0.5105(3) 0.2958(3) 0.0246(9) Uani 1 1 d . . . C3 C -0.1110(4) 0.4982(3) 0.2344(3) 0.0250(9) Uani 1 1 d . . . H3 H -0.0450 0.4823 0.2397 0.030 Uiso 1 1 calc R . . C4 C -0.1581(4) 0.5088(4) 0.1649(3) 0.0267(9) Uani 1 1 d . . . C5 C -0.2554(4) 0.5301(4) 0.1559(3) 0.0350(11) Uani 1 1 d . . . H5 H -0.2892 0.5363 0.1083 0.042 Uiso 1 1 calc R . . C6 C -0.3018(4) 0.5421(5) 0.2184(3) 0.0403(12) Uani 1 1 d . . . C7 C -0.2568(4) 0.5325(4) 0.2878(3) 0.0339(11) Uani 1 1 d . . . H7 H -0.2913 0.5406 0.3293 0.041 Uiso 1 1 calc R . . C8 C -0.0998(3) 0.5017(3) 0.1015(2) 0.0245(9) Uani 1 1 d . . . C10 C 0.1023(3) 0.6843(3) 0.0947(3) 0.0250(9) Uani 1 1 d . . . C11 C 0.1575(3) 0.7948(3) 0.1542(3) 0.0259(9) Uani 1 1 d . . . C12 C 0.2385(3) 0.8193(3) 0.2240(3) 0.0247(9) Uani 1 1 d . . . H12 H 0.2623 0.7661 0.2319 0.030 Uiso 1 1 calc R . . C13 C 0.2858(3) 0.9206(3) 0.2829(3) 0.0247(9) Uani 1 1 d . . . C14 C 0.2527(4) 0.9992(4) 0.2707(3) 0.0300(10) Uani 1 1 d . . . H14 H 0.2834 1.0689 0.3106 0.036 Uiso 1 1 calc R . . C15 C 0.1742(4) 0.9727(4) 0.1990(3) 0.0340(11) Uani 1 1 d . . . C16 C 0.1242(4) 0.8723(4) 0.1409(3) 0.0311(10) Uani 1 1 d . . . H16 H 0.0684 0.8565 0.0931 0.037 Uiso 1 1 calc R . . C17 C 0.3675(3) 0.9452(3) 0.3617(3) 0.0253(9) Uani 1 1 d . . . C19 C 0.3502(3) 0.9621(3) 0.5562(3) 0.0257(9) Uani 1 1 d . . . C20 C 0.2608(3) 0.9362(3) 0.5888(3) 0.0264(9) Uani 1 1 d . . . C21 C 0.2134(4) 0.8333(4) 0.5660(3) 0.0272(9) Uani 1 1 d . . . H21 H 0.2394 0.7821 0.5317 0.033 Uiso 1 1 calc R . . C22 C 0.1284(3) 0.8045(4) 0.5925(3) 0.0276(9) Uani 1 1 d . . . C23 C 0.0925(4) 0.8790(4) 0.6453(3) 0.0315(10) Uani 1 1 d . . . H23 H 0.0353 0.8608 0.6649 0.038 Uiso 1 1 calc R . . C24 C 0.1433(4) 0.9805(4) 0.6682(3) 0.0328(10) Uani 1 1 d . . . C25 C 0.2253(4) 1.0112(4) 0.6409(3) 0.0306(10) Uani 1 1 d . . . H25 H 0.2568 1.0820 0.6574 0.037 Uiso 1 1 calc R . . C26 C 0.0776(3) 0.6913(3) 0.5618(3) 0.0262(9) Uani 1 1 d . . . C28 C -0.2312(4) 0.4651(4) 0.6134(3) 0.0333(11) Uani 1 1 d . . . H28 H -0.2147 0.4019 0.5901 0.040 Uiso 1 1 calc R . . C29 C -0.3084(5) 0.3982(5) 0.6973(4) 0.0469(14) Uani 1 1 d . . . H29A H -0.2988 0.3342 0.6594 0.070 Uiso 1 1 calc R . . H29B H -0.3829 0.3868 0.6972 0.070 Uiso 1 1 calc R . . H29C H -0.2623 0.4202 0.7532 0.070 Uiso 1 1 calc R . . C30 C -0.3072(7) 0.5720(6) 0.7110(4) 0.067(2) Uani 1 1 d . . . H30A H -0.3431 0.5666 0.7510 0.100 Uiso 1 1 calc R . . H30B H -0.3545 0.5837 0.6696 0.100 Uiso 1 1 calc R . . H30C H -0.2419 0.6297 0.7396 0.100 Uiso 1 1 calc R . . C31 C 0.2755(5) 0.4053(5) 0.0694(4) 0.0454(13) Uani 1 1 d D . . H31 H 0.3407 0.4580 0.1010 0.054 Uiso 1 1 calc R . . C32 C 0.1801(9) 0.2442(10) -0.0462(8) 0.157(7) Uani 1 1 d . . . H32A H 0.1948 0.1893 -0.0902 0.235 Uiso 1 1 calc R . . H32B H 0.1304 0.2730 -0.0707 0.235 Uiso 1 1 calc R . . H32C H 0.1484 0.2161 -0.0133 0.235 Uiso 1 1 calc R . . C33 C 0.3732(8) 0.3174(9) -0.0185(6) 0.094(3) Uani 1 1 d D . . H33A H 0.3584 0.2512 -0.0665 0.140 Uiso 1 1 calc R . . H33B H 0.4300 0.3229 0.0271 0.140 Uiso 1 1 calc R . . H33C H 0.3957 0.3734 -0.0329 0.140 Uiso 1 1 calc R . . C34 C 0.6309(4) 0.7737(4) 0.4821(3) 0.0320(10) Uani 1 1 d . . . H34 H 0.6793 0.8363 0.4929 0.038 Uiso 1 1 calc R . . C35 C 0.6039(6) 0.6090(5) 0.4837(5) 0.0621(18) Uani 1 1 d . . . H35A H 0.6477 0.5708 0.5017 0.093 Uiso 1 1 calc R . . H35B H 0.5676 0.5701 0.4243 0.093 Uiso 1 1 calc R . . H35C H 0.5508 0.6190 0.5135 0.093 Uiso 1 1 calc R . . C36 C 0.7849(5) 0.7325(5) 0.5409(4) 0.0523(15) Uani 1 1 d . . . H36A H 0.8000 0.6745 0.5498 0.078 Uiso 1 1 calc R . . H36B H 0.8061 0.7935 0.5941 0.078 Uiso 1 1 calc R . . H36C H 0.8251 0.7461 0.5056 0.078 Uiso 1 1 calc R . . C37 C 0.1076(12) 0.9197(10) 0.4102(7) 0.055(3) Uiso 0.55 1 d PD A 1 H37 H 0.1758 0.9307 0.4022 0.066 Uiso 0.55 1 calc PR A 1 C38 C -0.0568(17) 0.7897(17) 0.3913(13) 0.071(7) Uiso 0.55 1 d PD A 1 H38A H -0.0790 0.7151 0.3721 0.107 Uiso 0.55 1 calc PR A 1 H38B H -0.1052 0.8082 0.3557 0.107 Uiso 0.55 1 calc PR A 1 H38C H -0.0589 0.8243 0.4482 0.107 Uiso 0.55 1 calc PR A 1 C39 C 0.1010(11) 0.7434(10) 0.3530(8) 0.056(3) Uiso 0.55 1 d PD A 1 H39A H 0.0539 0.6769 0.3410 0.084 Uiso 0.55 1 calc PR A 1 H39B H 0.1697 0.7565 0.3920 0.084 Uiso 0.55 1 calc PR A 1 H39C H 0.1121 0.7422 0.3018 0.084 Uiso 0.55 1 calc PR A 1 C40 C 0.5297(13) 0.2936(13) 0.1492(9) 0.136(5) Uani 1 1 d . . . C41 C 0.3595(15) 0.165(2) 0.1197(16) 0.287(16) Uani 1 1 d . . . H41A H 0.3286 0.0906 0.0891 0.430 Uiso 1 1 calc R . . H41B H 0.3141 0.1991 0.0972 0.430 Uiso 1 1 calc R . . H41C H 0.3645 0.1872 0.1781 0.430 Uiso 1 1 calc R . . C42 C 0.4971(17) 0.1105(16) 0.0584(11) 0.199(8) Uani 1 1 d . . . H42A H 0.4426 0.0453 0.0388 0.298 Uiso 1 1 calc R . . H42B H 0.5647 0.1080 0.0889 0.298 Uiso 1 1 calc R . . H42C H 0.5063 0.1220 0.0110 0.298 Uiso 1 1 calc R . . C43 C 0.8274(18) 0.2414(14) 0.1160(14) 0.122(7) Uiso 0.58 1 d PD B 1 H43 H 0.7823 0.2463 0.1502 0.146 Uiso 0.58 1 calc PR B 1 C44 C 1.0003(11) 0.2470(15) 0.1025(13) 0.104(5) Uiso 0.58 1 d PD B 1 H44A H 1.0685 0.2429 0.1306 0.156 Uiso 0.58 1 calc PR B 1 H44B H 1.0108 0.3129 0.0998 0.156 Uiso 0.58 1 calc PR B 1 H44C H 0.9725 0.1906 0.0465 0.156 Uiso 0.58 1 calc PR B 1 C45 C 0.9620(17) 0.2510(14) 0.2268(12) 0.100(5) Uiso 0.58 1 d PD B 1 H45A H 1.0344 0.2442 0.2361 0.150 Uiso 0.58 1 calc PR B 1 H45B H 0.9158 0.1982 0.2345 0.150 Uiso 0.58 1 calc PR B 1 H45C H 0.9630 0.3192 0.2661 0.150 Uiso 0.58 1 calc PR B 1 C46 C 0.5877(16) 0.1234(12) -0.1178(13) 0.085(5) Uiso 0.50 1 d PD C 2 H46 H 0.6447 0.1413 -0.0701 0.103 Uiso 0.50 1 calc PR C 2 C47 C 0.4860(17) 0.1835(16) -0.1997(12) 0.081(6) Uiso 0.50 1 d PD C 2 H47D H 0.4809 0.2484 -0.2007 0.122 Uiso 0.50 1 calc PR C 2 H47E H 0.4179 0.1469 -0.1988 0.122 Uiso 0.50 1 calc PR C 2 H47F H 0.5028 0.1410 -0.2491 0.122 Uiso 0.50 1 calc PR C 2 C48 C 0.6258(18) 0.2962(18) -0.0715(14) 0.088(7) Uiso 0.50 1 d PD C 2 H48A H 0.6036 0.3465 -0.0884 0.131 Uiso 0.50 1 calc PR C 2 H48B H 0.7013 0.3036 -0.0668 0.131 Uiso 0.50 1 calc PR C 2 H48C H 0.6147 0.3081 -0.0181 0.131 Uiso 0.50 1 calc PR C 2 C49 C 0.6541(9) 0.2062(11) 0.2799(7) 0.113(5) Uiso 0.65 1 d PD G 3 H49 H 0.6379 0.1348 0.2450 0.135 Uiso 0.65 1 calc PR G 3 C50 C 0.6125(11) 0.3493(10) 0.3785(9) 0.100(5) Uiso 0.65 1 d PD G 3 H50A H 0.5621 0.3597 0.4107 0.151 Uiso 0.65 1 calc PR G 3 H50B H 0.6038 0.3840 0.3430 0.151 Uiso 0.65 1 calc PR G 3 H50C H 0.6854 0.3778 0.4161 0.151 Uiso 0.65 1 calc PR G 3 C51 C 0.4994(15) 0.1715(12) 0.3290(13) 0.134(7) Uiso 0.65 1 d PD G 3 H51A H 0.4693 0.2135 0.3698 0.201 Uiso 0.65 1 calc PR G 3 H51B H 0.5203 0.1198 0.3445 0.201 Uiso 0.65 1 calc PR G 3 H51C H 0.4459 0.1372 0.2745 0.201 Uiso 0.65 1 calc PR G 3 C37A C 0.0764(12) 0.9387(14) 0.4324(10) 0.054(4) Uiso 0.45 1 d PD D 2 H37A H 0.0428 0.9792 0.4681 0.065 Uiso 0.45 1 calc PR D 2 C38A C -0.0567(16) 0.7954(16) 0.4109(13) 0.050(5) Uiso 0.45 1 d PD D 2 H38D H -0.0759 0.7207 0.3783 0.074 Uiso 0.45 1 calc PR D 2 H38E H -0.1161 0.8207 0.3947 0.074 Uiso 0.45 1 calc PR D 2 H38F H -0.0409 0.8124 0.4697 0.074 Uiso 0.45 1 calc PR D 2 C39A C 0.0763(18) 0.7708(18) 0.3423(14) 0.081(6) Uiso 0.45 1 d PD D 2 H39D H 0.0318 0.7002 0.3215 0.121 Uiso 0.45 1 calc PR D 2 H39E H 0.1486 0.7778 0.3725 0.121 Uiso 0.45 1 calc PR D 2 H39F H 0.0785 0.7867 0.2957 0.121 Uiso 0.45 1 calc PR D 2 C43A C 0.898(4) 0.248(3) 0.217(2) 0.29(4) Uiso 0.42 1 d PDU E 2 H43A H 0.9521 0.2869 0.2689 0.354 Uiso 0.42 1 calc PR E 2 C44A C 0.868(3) 0.184(3) 0.074(2) 0.171(15) Uiso 0.42 1 d PD B 2 H44D H 0.8988 0.2067 0.0383 0.257 Uiso 0.42 1 calc PR B 2 H44E H 0.7955 0.1901 0.0679 0.257 Uiso 0.42 1 calc PR B 2 H44F H 0.8660 0.1119 0.0590 0.257 Uiso 0.42 1 calc PR B 2 C45A C 1.048(3) 0.294(3) 0.173(3) 0.175(15) Uiso 0.42 1 d PD B 2 H45D H 1.0784 0.3247 0.2335 0.262 Uiso 0.42 1 calc PR B 2 H45E H 1.0574 0.3485 0.1552 0.262 Uiso 0.42 1 calc PR B 2 H45F H 1.0835 0.2439 0.1469 0.262 Uiso 0.42 1 calc PR B 2 C46A C 0.556(2) 0.1370(17) -0.1332(19) 0.183(14) Uiso 0.50 1 d PDU F 1 H46A H 0.5126 0.0703 -0.1729 0.219 Uiso 0.50 1 calc PR F 1 C47A C 0.6211(15) 0.3228(15) -0.0782(12) 0.071(5) Uiso 0.50 1 d PDU F 1 H47A H 0.5985 0.3729 -0.0950 0.106 Uiso 0.50 1 calc PR F 1 H47B H 0.6960 0.3287 -0.0757 0.106 Uiso 0.50 1 calc PR F 1 H47C H 0.6128 0.3361 -0.0238 0.106 Uiso 0.50 1 calc PR F 1 C48A C 0.487(2) 0.213(2) -0.2077(15) 0.116(10) Uiso 0.50 1 d PDU F 1 H48D H 0.4479 0.1403 -0.2411 0.174 Uiso 0.50 1 calc PR F 1 H48E H 0.5256 0.2376 -0.2394 0.174 Uiso 0.50 1 calc PR F 1 H48F H 0.4364 0.2528 -0.1933 0.174 Uiso 0.50 1 calc PR F 1 C49A C 0.6776(11) 0.2958(11) 0.3249(11) 0.128(12) Uiso 0.35 1 d PD G 1 H49A H 0.6987 0.3670 0.3617 0.154 Uiso 0.35 1 calc PR G 1 C50A C 0.531(3) 0.262(3) 0.381(2) 0.130(12) Uiso 0.35 1 d PD G 1 H50D H 0.4727 0.2018 0.3665 0.195 Uiso 0.35 1 calc PR G 1 H50E H 0.5011 0.3168 0.3763 0.195 Uiso 0.35 1 calc PR G 1 H50F H 0.5759 0.2870 0.4373 0.195 Uiso 0.35 1 calc PR G 1 C51A C 0.5683(19) 0.1177(16) 0.2747(19) 0.114(10) Uiso 0.35 1 d PD G 1 H51D H 0.5036 0.0819 0.2806 0.171 Uiso 0.35 1 calc PR G 1 H51E H 0.6283 0.0957 0.2949 0.171 Uiso 0.35 1 calc PR G 1 H51F H 0.5582 0.1011 0.2164 0.171 Uiso 0.35 1 calc PR G 1 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 0.0219(3) 0.0288(3) 0.0237(3) 0.0174(2) 0.0118(2) 0.0098(2) Cu2 0.0200(3) 0.0255(3) 0.0121(2) 0.0067(2) 0.00164(19) 0.0054(2) Cu3 0.0173(2) 0.0158(2) 0.0208(3) 0.0055(2) 0.00088(19) 0.00145(18) O1 0.0292(16) 0.0374(17) 0.0218(15) 0.0176(14) 0.0116(13) 0.0135(14) O2 0.0332(18) 0.055(2) 0.0306(17) 0.0284(17) 0.0167(15) 0.0237(16) O3 0.0310(17) 0.048(2) 0.0220(15) 0.0191(15) 0.0112(13) 0.0166(15) O4 0.0304(17) 0.0454(19) 0.0222(15) 0.0193(15) 0.0105(13) 0.0148(15) O5 0.044(3) 0.166(6) 0.065(3) 0.074(4) 0.025(2) 0.054(3) O6 0.064(3) 0.156(6) 0.064(3) 0.068(4) 0.041(3) 0.070(4) O7 0.0305(17) 0.0246(16) 0.0222(15) 0.0038(13) -0.0027(13) 0.0057(13) O8 0.0286(17) 0.0281(16) 0.0233(16) 0.0052(14) -0.0056(13) 0.0012(13) O9 0.0305(17) 0.0223(15) 0.0268(16) 0.0062(13) -0.0037(13) 0.0060(13) O10 0.0293(17) 0.0218(15) 0.0214(15) 0.0026(13) -0.0014(13) 0.0041(13) O11 0.101(4) 0.048(3) 0.056(3) 0.017(2) -0.032(3) 0.027(3) O12 0.107(4) 0.028(2) 0.070(3) 0.010(2) -0.028(3) 0.017(2) O13 0.0260(16) 0.0248(16) 0.0392(19) 0.0133(15) 0.0122(14) 0.0028(13) O14 0.0289(17) 0.0240(15) 0.0306(17) 0.0119(14) 0.0092(14) 0.0045(13) O15 0.0245(16) 0.0314(17) 0.0305(17) 0.0157(14) 0.0098(13) 0.0047(13) O16 0.0369(19) 0.0300(17) 0.048(2) 0.0222(16) 0.0256(17) 0.0128(14) O17 0.068(3) 0.054(3) 0.076(3) 0.014(2) 0.049(3) 0.016(2) O18 0.093(4) 0.034(2) 0.067(3) 0.014(2) 0.047(3) 0.020(2) O19 0.0349(18) 0.046(2) 0.043(2) 0.0308(18) 0.0248(16) 0.0204(16) O20 0.0319(18) 0.049(2) 0.0249(16) 0.0187(16) 0.0054(14) 0.0182(16) O21 0.0285(17) 0.0218(15) 0.0359(18) 0.0097(14) 0.0021(14) 0.0069(13) O23 0.100(6) 0.120(6) 0.148(7) 0.043(6) 0.052(5) 0.041(5) N1 0.037(3) 0.122(5) 0.050(3) 0.056(3) 0.023(2) 0.041(3) N2 0.064(3) 0.036(3) 0.046(3) 0.017(2) -0.009(2) 0.015(2) N3 0.048(3) 0.043(3) 0.044(3) 0.014(2) 0.022(2) 0.017(2) N4 0.038(2) 0.043(2) 0.028(2) 0.0185(19) 0.0167(18) 0.0087(19) N5 0.066(4) 0.093(4) 0.039(3) 0.017(3) 0.012(3) 0.050(3) N6 0.042(2) 0.036(2) 0.044(3) 0.019(2) 0.010(2) 0.0207(19) N8 0.128(8) 0.138(9) 0.094(6) 0.062(6) 0.046(6) 0.061(7) C1 0.028(2) 0.026(2) 0.021(2) 0.0141(18) 0.0080(17) 0.0073(17) C2 0.026(2) 0.031(2) 0.020(2) 0.0145(18) 0.0079(17) 0.0065(18) C3 0.025(2) 0.028(2) 0.023(2) 0.0113(18) 0.0066(17) 0.0075(17) C4 0.028(2) 0.032(2) 0.019(2) 0.0104(19) 0.0082(17) 0.0073(18) C5 0.030(2) 0.056(3) 0.025(2) 0.022(2) 0.0089(19) 0.015(2) C6 0.028(3) 0.070(4) 0.034(3) 0.030(3) 0.012(2) 0.020(2) C7 0.028(2) 0.051(3) 0.028(2) 0.021(2) 0.011(2) 0.012(2) C8 0.024(2) 0.030(2) 0.0144(19) 0.0057(17) 0.0046(16) 0.0060(17) C10 0.026(2) 0.028(2) 0.0161(19) 0.0074(18) 0.0043(17) 0.0044(18) C11 0.023(2) 0.027(2) 0.020(2) 0.0070(18) 0.0032(17) 0.0018(17) C12 0.023(2) 0.024(2) 0.022(2) 0.0079(18) 0.0041(17) 0.0048(17) C13 0.021(2) 0.027(2) 0.020(2) 0.0072(18) 0.0010(16) 0.0037(17) C14 0.028(2) 0.025(2) 0.025(2) 0.0056(19) 0.0009(18) 0.0005(18) C15 0.040(3) 0.029(2) 0.032(2) 0.016(2) 0.003(2) 0.011(2) C16 0.030(2) 0.032(2) 0.023(2) 0.011(2) -0.0007(18) 0.0056(19) C17 0.019(2) 0.026(2) 0.022(2) 0.0072(18) 0.0014(16) -0.0010(17) C19 0.021(2) 0.027(2) 0.026(2) 0.0131(19) 0.0013(17) 0.0028(17) C20 0.024(2) 0.029(2) 0.026(2) 0.0140(19) 0.0033(18) 0.0048(17) C21 0.025(2) 0.029(2) 0.028(2) 0.0153(19) 0.0070(18) 0.0066(18) C22 0.023(2) 0.030(2) 0.029(2) 0.016(2) 0.0053(18) 0.0035(18) C23 0.031(2) 0.037(3) 0.033(2) 0.019(2) 0.015(2) 0.010(2) C24 0.033(3) 0.035(3) 0.029(2) 0.012(2) 0.010(2) 0.012(2) C25 0.034(2) 0.029(2) 0.028(2) 0.013(2) 0.009(2) 0.0070(19) C26 0.024(2) 0.031(2) 0.030(2) 0.020(2) 0.0070(18) 0.0071(18) C28 0.036(3) 0.040(3) 0.034(3) 0.020(2) 0.022(2) 0.014(2) C29 0.047(3) 0.059(4) 0.042(3) 0.032(3) 0.020(3) 0.004(3) C30 0.101(6) 0.078(5) 0.057(4) 0.041(4) 0.055(4) 0.050(4) C31 0.048(3) 0.060(4) 0.044(3) 0.031(3) 0.018(3) 0.028(3) C32 0.094(8) 0.127(9) 0.118(9) -0.060(8) -0.019(7) 0.057(7) C33 0.107(7) 0.147(9) 0.075(6) 0.062(6) 0.057(5) 0.085(7) C34 0.037(3) 0.028(2) 0.031(2) 0.010(2) 0.010(2) 0.015(2) C35 0.069(4) 0.043(3) 0.081(5) 0.035(4) 0.014(4) 0.022(3) C36 0.045(3) 0.065(4) 0.058(4) 0.030(3) 0.016(3) 0.036(3) C40 0.168(14) 0.130(12) 0.109(10) 0.066(9) 0.029(10) 0.024(11) C41 0.113(14) 0.52(5) 0.28(3) 0.25(3) 0.049(16) 0.04(2) C42 0.26(2) 0.22(2) 0.154(15) 0.076(14) 0.088(15) 0.140(18) _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 O16 1.958(3) 2_566 ? Cu1 O2 1.960(3) 2_566 ? Cu1 O15 1.963(3) . ? Cu1 O1 1.965(3) . ? Cu1 O19 2.145(3) . ? Cu1 Cu1 2.6637(10) 2_566 ? Cu2 O7 1.950(3) . ? Cu2 O3 1.952(3) . ? Cu2 O8 1.959(3) 2_565 ? Cu2 O4 1.968(3) 2_565 ? Cu2 O20 2.158(3) . ? Cu2 Cu2 2.6613(10) 2_565 ? Cu3 O13 1.940(3) . ? Cu3 O9 1.950(3) . ? Cu3 O14 1.970(3) 2_676 ? Cu3 O10 1.991(3) 2_676 ? Cu3 O21 2.137(3) . ? Cu3 Cu3 2.6640(10) 2_676 ? O1 C1 1.255(5) . ? O2 C1 1.258(5) . ? O2 Cu1 1.960(3) 2_566 ? O3 C8 1.247(5) . ? O4 C8 1.260(5) . ? O4 Cu2 1.968(3) 2_565 ? O5 N1 1.234(6) . ? O6 N1 1.224(7) . ? O7 C10 1.260(5) . ? O8 C10 1.256(5) . ? O8 Cu2 1.959(3) 2_565 ? O9 C17 1.256(5) . ? O10 C17 1.254(5) . ? O10 Cu3 1.991(3) 2_676 ? O11 N2 1.217(6) . ? O12 N2 1.215(6) . ? O13 C19 1.261(6) . ? O14 C19 1.255(5) . ? O14 Cu3 1.970(3) 2_676 ? O15 C26 1.256(5) . ? O16 C26 1.252(6) . ? O16 Cu1 1.958(3) 2_566 ? O17 N3 1.204(6) . ? O18 N3 1.222(6) . ? O19 C28 1.238(6) . ? O20 C31 1.225(6) . ? O21 C34 1.239(6) . ? O22 C37 1.245(18) . ? O23 C40 1.281(17) . ? O24 C43 1.16(2) . ? O25 C46 1.232(3) . ? O26 C49A 1.234(3) . ? O26 C49 1.236(3) . ? O22A C37A 1.21(2) . ? O24A C43A 1.12(3) . ? O25A C46A 1.231(3) . ? N1 C6 1.470(7) . ? N2 C15 1.476(6) . ? N3 C24 1.488(6) . ? N4 C28 1.325(6) . ? N4 C30 1.446(8) . ? N4 C29 1.461(7) . ? N5 C31 1.318(8) . ? N5 C33 1.440(9) . ? N5 C32 1.448(12) . ? N6 C34 1.318(6) . ? N6 C35 1.437(8) . ? N6 C36 1.469(7) . ? N7 C37 1.341(17) . ? N7 C39 1.421(19) . ? N7 C38 1.49(2) . ? N8 C40 1.385(16) . ? N8 C41 1.444(19) . ? N8 C42 1.446(18) . ? N9 C49A 1.322(3) . ? N9 C49 1.323(3) . ? N9 C50A 1.40(3) . ? N9 C51 1.448(16) . ? N9 C50 1.497(13) . ? N9 C51A 1.57(2) . ? N10 C48 1.29(3) . ? N10 C46 1.322(3) . ? N10 C47 1.47(3) . ? N11 C44A 1.26(4) . ? N11 C43 1.33(2) . ? N11 C43A 1.35(3) . ? N11 C45 1.360(19) . ? N11 C44 1.469(19) . ? N11 C45A 1.59(4) . ? N7A C37A 1.29(2) . ? N7A C38A 1.38(3) . ? N7A C39A 1.45(3) . ? N10A C46A 1.321(3) . ? N10A C47A 1.36(3) . ? N10A C48A 1.43(3) . ? C1 C2 1.503(6) . ? C2 C3 1.384(6) . ? C2 C7 1.394(6) . ? C3 C4 1.391(6) . ? C4 C5 1.388(7) . ? C4 C8 1.515(6) . ? C5 C6 1.384(7) . ? C6 C7 1.374(7) . ? C10 C11 1.500(6) . ? C11 C12 1.378(6) . ? C11 C16 1.388(7) . ? C12 C13 1.388(6) . ? C13 C14 1.395(7) . ? C13 C17 1.499(6) . ? C14 C15 1.377(7) . ? C15 C16 1.381(7) . ? C19 C20 1.499(6) . ? C20 C25 1.384(7) . ? C20 C21 1.390(6) . ? C21 C22 1.389(6) . ? C22 C23 1.389(7) . ? C22 C26 1.508(6) . ? C23 C24 1.382(7) . ? C24 C25 1.374(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O16 Cu1 O2 88.39(15) 2_566 2_566 ? O16 Cu1 O15 167.59(13) 2_566 . ? O2 Cu1 O15 89.57(15) 2_566 . ? O16 Cu1 O1 90.13(14) 2_566 . ? O2 Cu1 O1 167.73(13) 2_566 . ? O15 Cu1 O1 89.27(13) . . ? O16 Cu1 O19 93.76(13) 2_566 . ? O2 Cu1 O19 92.11(13) 2_566 . ? O15 Cu1 O19 98.54(13) . . ? O1 Cu1 O19 100.14(13) . . ? O16 Cu1 Cu1 79.61(9) 2_566 2_566 ? O2 Cu1 Cu1 82.12(9) 2_566 2_566 ? O15 Cu1 Cu1 87.99(9) . 2_566 ? O1 Cu1 Cu1 85.64(9) . 2_566 ? O19 Cu1 Cu1 171.28(9) . 2_566 ? O7 Cu2 O3 88.22(14) . . ? O7 Cu2 O8 167.72(13) . 2_565 ? O3 Cu2 O8 89.44(15) . 2_565 ? O7 Cu2 O4 89.68(14) . 2_565 ? O3 Cu2 O4 167.76(13) . 2_565 ? O8 Cu2 O4 90.06(14) 2_565 2_565 ? O7 Cu2 O20 97.00(13) . . ? O3 Cu2 O20 100.69(13) . . ? O8 Cu2 O20 95.29(14) 2_565 . ? O4 Cu2 O20 91.54(13) 2_565 . ? O7 Cu2 Cu2 85.45(10) . 2_565 ? O3 Cu2 Cu2 84.88(10) . 2_565 ? O8 Cu2 Cu2 82.33(10) 2_565 2_565 ? O4 Cu2 Cu2 82.93(9) 2_565 2_565 ? O20 Cu2 Cu2 173.96(9) . 2_565 ? O13 Cu3 O9 88.24(15) . . ? O13 Cu3 O14 167.39(13) . 2_676 ? O9 Cu3 O14 89.08(14) . 2_676 ? O13 Cu3 O10 89.17(14) . 2_676 ? O9 Cu3 O10 167.61(13) . 2_676 ? O14 Cu3 O10 90.83(14) 2_676 2_676 ? O13 Cu3 O21 99.99(13) . . ? O9 Cu3 O21 104.62(13) . . ? O14 Cu3 O21 92.61(13) 2_676 . ? O10 Cu3 O21 87.76(13) 2_676 . ? O13 Cu3 Cu3 83.33(10) . 2_676 ? O9 Cu3 Cu3 89.52(9) . 2_676 ? O14 Cu3 Cu3 84.33(9) 2_676 2_676 ? O10 Cu3 Cu3 78.15(9) 2_676 2_676 ? O21 Cu3 Cu3 165.51(9) . 2_676 ? C1 O1 Cu1 120.6(3) . . ? C1 O2 Cu1 125.0(3) . 2_566 ? C8 O3 Cu2 121.9(3) . . ? C8 O4 Cu2 123.1(3) . 2_565 ? C10 O7 Cu2 121.3(3) . . ? C10 O8 Cu2 124.6(3) . 2_565 ? C17 O9 Cu3 117.3(3) . . ? C17 O10 Cu3 128.7(3) . 2_676 ? C19 O13 Cu3 124.2(3) . . ? C19 O14 Cu3 121.6(3) . 2_676 ? C26 O15 Cu1 117.7(3) . . ? C26 O16 Cu1 128.0(3) . 2_566 ? C28 O19 Cu1 117.8(3) . . ? C31 O20 Cu2 127.4(3) . . ? C34 O21 Cu3 111.5(3) . . ? C49A O26 C49 57.8(12) . . ? O6 N1 O5 124.3(5) . . ? O6 N1 C6 118.0(5) . . ? O5 N1 C6 117.6(5) . . ? O12 N2 O11 123.6(5) . . ? O12 N2 C15 118.6(5) . . ? O11 N2 C15 117.8(5) . . ? O17 N3 O18 123.8(5) . . ? O17 N3 C24 118.6(5) . . ? O18 N3 C24 117.6(5) . . ? C28 N4 C30 121.7(5) . . ? C28 N4 C29 121.6(5) . . ? C30 N4 C29 116.8(4) . . ? C31 N5 C33 122.4(7) . . ? C31 N5 C32 118.9(7) . . ? C33 N5 C32 118.3(7) . . ? C34 N6 C35 121.6(5) . . ? C34 N6 C36 120.7(5) . . ? C35 N6 C36 117.7(5) . . ? C37 N7 C39 118.3(12) . . ? C37 N7 C38 124.5(14) . . ? C39 N7 C38 117.0(12) . . ? C40 N8 C41 123.6(17) . . ? C40 N8 C42 120.5(15) . . ? C41 N8 C42 115.8(18) . . ? C49A N9 C49 53.6(11) . . ? C49A N9 C50A 128.6(17) . . ? C49 N9 C50A 172.8(16) . . ? C49A N9 C51 178.7(13) . . ? C49 N9 C51 126.4(11) . . ? C50A N9 C51 51.3(15) . . ? C49A N9 C50 65.4(5) . . ? C49 N9 C50 118.9(10) . . ? C50A N9 C50 64.4(15) . . ? C51 N9 C50 114.7(9) . . ? C49A N9 C51A 116.8(10) . . ? C49 N9 C51A 63.5(7) . . ? C50A N9 C51A 113.1(14) . . ? C51 N9 C51A 63.1(10) . . ? C50 N9 C51A 177.2(11) . . ? C48 N10 C46 120.7(19) . . ? C48 N10 C47 123.4(17) . . ? C46 N10 C47 115.9(17) . . ? C44A N11 C43 55.0(18) . . ? C44A N11 C43A 128(3) . . ? C43 N11 C43A 89(2) . . ? C44A N11 C45 150(2) . . ? C43 N11 C45 124.4(15) . . ? C43A N11 C45 35(2) . . ? C44A N11 C44 77.2(18) . . ? C43 N11 C44 115.7(14) . . ? C43A N11 C44 153(2) . . ? C45 N11 C44 118.5(13) . . ? C44A N11 C45A 122(2) . . ? C43 N11 C45A 143.9(18) . . ? C43A N11 C45A 109(2) . . ? C45 N11 C45A 76.7(18) . . ? C44 N11 C45A 45.2(15) . . ? C37A N7A C38A 123.5(16) . . ? C37A N7A C39A 121.4(16) . . ? C38A N7A C39A 115.1(15) . . ? C46A N10A C47A 131(2) . . ? C46A N10A C48A 110(2) . . ? C47A N10A C48A 118.9(19) . . ? O1 C1 O2 126.7(4) . . ? O1 C1 C2 117.6(4) . . ? O2 C1 C2 115.7(4) . . ? C3 C2 C7 119.9(4) . . ? C3 C2 C1 119.4(4) . . ? C7 C2 C1 120.7(4) . . ? C2 C3 C4 120.6(4) . . ? C5 C4 C3 120.1(4) . . ? C5 C4 C8 120.5(4) . . ? C3 C4 C8 119.3(4) . . ? C6 C5 C4 118.0(4) . . ? C7 C6 C5 123.1(5) . . ? C7 C6 N1 118.2(4) . . ? C5 C6 N1 118.6(4) . . ? C6 C7 C2 118.3(4) . . ? O3 C8 O4 127.2(4) . . ? O3 C8 C4 116.5(4) . . ? O4 C8 C4 116.3(4) . . ? O8 C10 O7 126.3(4) . . ? O8 C10 C11 117.0(4) . . ? O7 C10 C11 116.6(4) . . ? C12 C11 C16 120.0(4) . . ? C12 C11 C10 119.9(4) . . ? C16 C11 C10 120.1(4) . . ? C11 C12 C13 121.0(4) . . ? C12 C13 C14 119.8(4) . . ? C12 C13 C17 120.3(4) . . ? C14 C13 C17 119.8(4) . . ? C15 C14 C13 117.9(4) . . ? C14 C15 C16 123.1(4) . . ? C14 C15 N2 118.1(4) . . ? C16 C15 N2 118.8(4) . . ? C15 C16 C11 118.2(4) . . ? O10 C17 O9 126.3(4) . . ? O10 C17 C13 116.8(4) . . ? O9 C17 C13 116.9(4) . . ? O14 C19 O13 126.4(4) . . ? O14 C19 C20 117.4(4) . . ? O13 C19 C20 116.2(4) . . ? C25 C20 C21 119.6(4) . . ? C25 C20 C19 122.2(4) . . ? C21 C20 C19 118.2(4) . . ? C22 C21 C20 120.9(4) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 C26 122.1(4) . . ? C21 C22 C26 117.8(4) . . ? C24 C23 C22 117.4(4) . . ? C25 C24 C23 123.8(4) . . ? C25 C24 N3 118.3(4) . . ? C23 C24 N3 117.9(4) . . ? C24 C25 C20 118.2(4) . . ? O16 C26 O15 126.7(4) . . ? O16 C26 C22 116.1(4) . . ? O15 C26 C22 117.3(4) . . ? O19 C28 N4 125.1(5) . . ? O20 C31 N5 126.2(6) . . ? O21 C34 N6 124.5(5) . . ? O22 C37 N7 126.0(15) . . ? O23 C40 N8 118.6(14) . . ? O24 C43 N11 131(2) . . ? O25 C46 N10 135(2) . . ? O26 C49 N9 124.2(12) . . ? O22A C37A N7A 128.3(19) . . ? O24A C43A N11 124(4) . . ? O25A C46A N10A 101(3) . . ? O26 C49A N9 124.4(12) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.492 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.117 #===END data_compound3_NZbath4 _database_code_depnum_ccdc_archive 'CCDC 686381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H198 Cu6 N12 O111' _chemical_formula_weight 2290.75 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' 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 Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-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' '-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' _cell_length_a 35.0028(5) _cell_length_b 35.0028(5) _cell_length_c 10.2067(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10829.8(4) _cell_formula_units_Z 3 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 2.89 _cell_measurement_theta_min 26.45 _cell_measurement_theta_max 98324 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5220 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.755 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 108(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52569 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.43 _reflns_number_total 4940 _reflns_number_gt 3405 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Data resolution is poor, as is characteristic of this genre of materials. It was surprising then, that credible locations for the hydrogens on the ligand waters appeared in the penultimate electron density map, enabling refinement at a distance of 0.9 \%A from the relevant parent oxygens (O7 and O8). Of these, the hydrogens attached to O8 are the most credible, as these are involved in h-bonding to ordered atoms. Residual electron density maximum and minimum are higher than desirable - however, these are located at chemically insignificant distance from the copper atom. The lattice solvent was modelled using the SQUEEZE procedure in PLATON, which yielded an estimate of the solvent content (based on the approximate number of electrons contained in the voids) as being in the region of 9.5 disordered solvent waters per asymmetric unit. F(000) and related parameters, as presented, are derived on the basis of inclusion of this solvent in the unit cell. Platon suggests potential missed symmetry in this structure. Indeed, a credible solution can be found in R-3m. The rationale for presenting the structure in space group R-3 was twofold: (a) The weighting scheme became worse in R-3m (b) The Hirshfeld Rigid-Bond test results were substantially worse for R-3m. These results were as follows: R-3: Sqrt(Sum(DelIJ**2)/Nrb) = 0.0166 (Nrb = 20) R-3m: Sqrt(Sum(DelIJ**2)/Nrb) = 0.0243 (Nrb = 16) ; _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^)+(0.1759P)^2^+46.7003P] 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 4940 _refine_ls_number_parameters 224 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.1037 _refine_ls_wR_factor_ref 0.3148 _refine_ls_wR_factor_gt 0.2971 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.106 _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 0.53113(3) 0.06227(3) 0.34867(7) 0.0683(4) Uani 1 1 d . A . O1 O 0.58571(14) 0.0607(2) 0.3490(4) 0.0752(13) Uani 1 1 d . . . O2 O 0.54972(13) -0.0124(2) 0.3421(5) 0.096(2) Uani 1 1 d . . . C7 C 0.58310(18) 0.0235(3) 0.3439(5) 0.0666(19) Uani 1 1 d . . . C1 C 0.62677(16) 0.0248(2) 0.3373(4) 0.0505(13) Uani 1 1 d . . . C2 C 0.66669(16) 0.06456(18) 0.3333(4) 0.0467(12) Uani 1 1 d . . . H2 H 0.6667 0.0917 0.3333 0.056 Uiso 1 1 calc R . . C3 C 0.70674(16) 0.06455(19) 0.3293(4) 0.0490(13) Uani 1 1 d . . . C8 C 0.75029(18) 0.1067(3) 0.3225(5) 0.0668(19) Uani 1 1 d . . . O3 O 0.74765(14) 0.14170(18) 0.3177(4) 0.0756(14) Uani 1 1 d . . . O4 O 0.78367(13) 0.1045(2) 0.3248(5) 0.0939(19) Uani 1 1 d . . . C4 C 0.7065(2) 0.0256(2) 0.3314(5) 0.0621(17) Uani 1 1 d . . . H4 H 0.7335 0.0253 0.3313 0.074 Uiso 1 1 calc R . . C5 C 0.6662(2) -0.0141(2) 0.3337(5) 0.0666(17) Uani 1 1 d . . . N1 N 0.6665(4) -0.0571(3) 0.3331(5) 0.095(2) Uani 1 1 d . . . O5 O 0.7028(4) -0.0545(3) 0.3315(7) 0.150(4) Uani 1 1 d . . . O6 O 0.6308(4) -0.0906(3) 0.3359(7) 0.154(4) Uani 1 1 d . . . C6 C 0.6271(2) -0.0146(2) 0.3353(5) 0.0621(17) Uani 1 1 d . . . H6 H 0.6001 -0.0419 0.3352 0.074 Uiso 1 1 calc R . . O7 O 0.5706(6) 0.1380(3) 0.3658(15) 0.226(6) Uani 1 1 d D . . O8 O 0.52748(11) 0.05478(12) 0.5401(4) 0.0490(9) Uani 1 1 d D . . O9 O 0.53073(16) 0.06153(19) 0.1504(5) 0.0824(14) Uani 1 1 d D . . C9A C 0.5613(6) 0.0802(5) 0.0841(14) 0.063(4) Uiso 0.40 1 d PD A 1 H9A H 0.5898 0.0948 0.1227 0.076 Uiso 0.40 1 calc PR A 1 N2A N 0.5576(4) 0.0817(4) -0.0404(11) 0.059(3) Uiso 0.40 1 d PD A 1 C10A C 0.5986(6) 0.1051(7) -0.1207(19) 0.091(6) Uiso 0.40 1 d PD A 1 H10A H 0.6244 0.1166 -0.0632 0.136 Uiso 0.40 1 calc PR A 1 H10B H 0.5987 0.1295 -0.1679 0.136 Uiso 0.40 1 calc PR A 1 H10C H 0.5995 0.0844 -0.1837 0.136 Uiso 0.40 1 calc PR A 1 C9 C 0.5200(5) 0.0797(5) 0.0855(15) 0.098(4) Uiso 0.60 1 d PD A 2 H9 H 0.5068 0.0949 0.1247 0.118 Uiso 0.60 1 calc PR A 2 N2 N 0.5243(4) 0.0814(4) -0.0406(12) 0.093(3) Uiso 0.60 1 d PD A 2 C10 C 0.5085(7) 0.1064(7) -0.120(2) 0.143(7) Uiso 0.60 1 d PD A 2 H10D H 0.4984 0.1218 -0.0619 0.215 Uiso 0.60 1 calc PR A 2 H10E H 0.4840 0.0858 -0.1762 0.215 Uiso 0.60 1 calc PR A 2 H10F H 0.5326 0.1279 -0.1752 0.215 Uiso 0.60 1 calc PR A 2 C11 C 0.5346(6) 0.0515(6) -0.1135(18) 0.113(6) Uiso 0.60 1 d PD A 2 H11A H 0.5547 0.0457 -0.0618 0.170 Uiso 0.60 1 calc PR A 2 H11B H 0.5486 0.0652 -0.1970 0.170 Uiso 0.60 1 calc PR A 2 H11C H 0.5073 0.0237 -0.1304 0.170 Uiso 0.60 1 calc PR A 2 C11A C 0.5175(6) 0.0541(6) -0.1182(19) 0.076(5) Uiso 0.40 1 d PD A 1 H11D H 0.5192 0.0293 -0.1564 0.114 Uiso 0.40 1 calc PR A 1 H11E H 0.5152 0.0719 -0.1885 0.114 Uiso 0.40 1 calc PR A 1 H11F H 0.4915 0.0428 -0.0614 0.114 Uiso 0.40 1 calc PR A 1 H8A H 0.5416(16) 0.0409(18) 0.570(6) 0.08(2) Uiso 1 1 d D . . H8B H 0.4991(8) 0.0414(19) 0.566(6) 0.09(2) Uiso 1 1 d D . . H7A H 0.598(2) 0.158(3) 0.343(15) 0.22(7) Uiso 1 1 d D . . H7B H 0.558(3) 0.150(3) 0.416(8) 0.10(3) Uiso 1 1 d 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 0.0624(5) 0.1000(7) 0.0549(5) 0.0273(4) 0.0137(3) 0.0499(5) O1 0.044(2) 0.116(4) 0.058(3) 0.010(3) 0.0115(18) 0.035(3) O2 0.036(2) 0.133(4) 0.068(3) -0.045(3) 0.0037(19) 0.005(3) C7 0.034(3) 0.120(6) 0.033(3) -0.009(3) 0.000(2) 0.028(4) C1 0.041(3) 0.070(3) 0.026(2) -0.006(2) 0.0028(18) 0.017(2) C2 0.045(3) 0.061(3) 0.026(2) -0.003(2) -0.0020(18) 0.020(2) C3 0.040(3) 0.071(4) 0.026(2) 0.007(2) 0.0007(18) 0.020(2) C8 0.034(3) 0.098(5) 0.033(3) 0.009(3) 0.001(2) 0.007(3) O3 0.046(2) 0.087(3) 0.058(3) -0.002(2) 0.0104(18) 0.007(2) O4 0.037(2) 0.151(5) 0.070(3) 0.046(3) 0.0025(19) 0.029(3) C4 0.058(3) 0.111(5) 0.026(2) 0.013(3) 0.005(2) 0.049(4) C5 0.089(5) 0.082(4) 0.029(3) 0.001(3) 0.005(3) 0.043(4) N1 0.157(8) 0.111(6) 0.030(3) 0.009(3) 0.016(4) 0.076(6) O5 0.256(11) 0.192(8) 0.089(5) 0.036(5) 0.042(6) 0.178(9) O6 0.270(12) 0.094(5) 0.088(5) 0.013(4) 0.047(6) 0.083(7) C6 0.061(4) 0.068(4) 0.025(2) -0.009(2) 0.007(2) 0.008(3) O7 0.278(16) 0.111(7) 0.248(14) 0.108(8) 0.096(12) 0.065(9) O8 0.044(2) 0.057(2) 0.051(2) 0.0067(16) 0.0027(15) 0.0285(18) O9 0.079(3) 0.109(4) 0.073(3) 0.004(3) -0.002(2) 0.057(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 O3 1.937(4) 17 ? Cu1 O1 1.939(5) . ? Cu1 O8 1.967(4) . ? Cu1 O9 2.024(5) . ? Cu1 O7 2.303(11) . ? O1 C7 1.259(9) . ? O2 C7 1.216(8) . ? C7 C1 1.508(8) . ? C1 C6 1.385(9) . ? C1 C2 1.395(7) . ? C2 C3 1.403(7) . ? C3 C4 1.361(9) . ? C3 C8 1.502(8) . ? C8 O4 1.209(8) . ? C8 O3 1.275(9) . ? O3 Cu1 1.937(4) 18_545 ? C4 C5 1.399(9) . ? C5 C6 1.361(9) . ? C5 N1 1.508(10) . ? N1 O6 1.214(12) . ? N1 O5 1.230(11) . ? O9 C9 1.107(16) . ? O9 C9A 1.154(16) . ? C9A N2A 1.281(16) . ? N2A C11A 1.476(14) . ? N2A C10A 1.491(15) . ? C9 N2 1.294(15) . ? N2 C11 1.468(14) . ? N2 C10 1.489(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O1 177.2(3) 17 . ? O3 Cu1 O8 89.84(16) 17 . ? O1 Cu1 O8 89.63(16) . . ? O3 Cu1 O9 90.05(19) 17 . ? O1 Cu1 O9 90.12(19) . . ? O8 Cu1 O9 172.7(2) . . ? O3 Cu1 O7 92.8(5) 17 . ? O1 Cu1 O7 90.1(5) . . ? O8 Cu1 O7 92.3(4) . . ? O9 Cu1 O7 95.0(4) . . ? C7 O1 Cu1 117.8(4) . . ? O2 C7 O1 127.3(6) . . ? O2 C7 C1 117.8(8) . . ? O1 C7 C1 115.0(6) . . ? C6 C1 C2 119.3(5) . . ? C6 C1 C7 119.0(5) . . ? C2 C1 C7 121.7(6) . . ? C1 C2 C3 120.2(5) . . ? C4 C3 C2 119.7(5) . . ? C4 C3 C8 118.7(6) . . ? C2 C3 C8 121.7(6) . . ? O4 C8 O3 126.8(6) . . ? O4 C8 C3 118.4(8) . . ? O3 C8 C3 114.8(6) . . ? C8 O3 Cu1 117.8(4) . 18_545 ? C3 C4 C5 119.6(5) . . ? C6 C5 C4 121.3(6) . . ? C6 C5 N1 119.7(7) . . ? C4 C5 N1 119.0(7) . . ? O6 N1 O5 126.7(10) . . ? O6 N1 C5 116.6(9) . . ? O5 N1 C5 116.6(9) . . ? C5 C6 C1 119.9(5) . . ? C9 O9 C9A 79.0(11) . . ? C9 O9 Cu1 126.4(9) . . ? C9A O9 Cu1 125.5(8) . . ? O9 C9A N2A 121.4(14) . . ? C9A N2A C11A 126.1(14) . . ? C9A N2A C10A 118.6(14) . . ? C11A N2A C10A 113.8(14) . . ? O9 C9 N2 123.7(15) . . ? C9 N2 C11 122.5(14) . . ? C9 N2 C10 120.0(14) . . ? C11 N2 C10 115.9(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.412 _refine_diff_density_min -1.602 _refine_diff_density_rms 0.103 #===END data_compound4_k08adb22 _database_code_depnum_ccdc_archive 'CCDC 686382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.50 H20.50 Cu N1.50 O6.50 S' _chemical_formula_weight 415.42 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3m1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' _cell_length_a 18.5590(3) _cell_length_b 18.5590(3) _cell_length_c 10.9800(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3275.23(10) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55186 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31244 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2116 _reflns_number_gt 1826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. The copper and ligand water oxygen sit on one of the crystallographic mirror planes present, while carbons 4, 5, 6 and 7 are located on the other crystallographically distinct mirror plane intrinsic to this space group. This necessarily results in 50:50 disorder of the sulphur atom, in addition to precluding of the hydrogen atoms for C6 and C7, which were omitted from the refinement. The lattice solvent was modelled using the SQUEEZE procedure in PLATON, which yielded an estimate of the solvent content (based on the approximate number of electrons contained in the voids) as being in the region of 9 disordered solvent DMFs per unit cell [1.5 molecules per each full copper centre]. F(000) and related parameters, as presented, are derived on the basis of inclusion of this solvent in the unit cell. ; _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^)+(0.1065P)^2^+1.8770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2116 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.476171(15) 0.523829(15) 0.59810(5) 0.0408(3) Uani 1 2 d S . . S1 S 0.0586(2) 0.2277(4) 0.0489(5) 0.202(3) Uani 0.50 1 d P . . O1 O 0.37154(15) 0.48137(16) 0.5098(2) 0.0547(6) Uani 1 1 d . . . O2 O 0.41101(16) 0.44020(18) 0.3438(2) 0.0583(7) Uani 1 1 d . . . O3 O 0.43926(17) 0.56074(17) 0.7601(5) 0.114(2) Uani 1 2 d S . . C1 C 0.3592(2) 0.4504(2) 0.4059(3) 0.0499(8) Uani 1 1 d . . . C2 C 0.2764(2) 0.4232(2) 0.3476(3) 0.0518(9) Uani 1 1 d . . . C3 C 0.2547(3) 0.3814(3) 0.2370(4) 0.0662(11) Uani 1 1 d . . . H3 H 0.2917 0.3668 0.1993 0.079 Uiso 1 1 calc R . . C4 C 0.1804(2) 0.3609(5) 0.1808(6) 0.0744(18) Uani 1 2 d S . . C5 C 0.22170(15) 0.4434(3) 0.4035(5) 0.0494(11) Uani 1 2 d S . . H5 H 0.2355 0.4710 0.4800 0.059 Uiso 1 2 calc SR . . C6 C 0.0821(4) 0.1643(7) 0.1671(12) 0.166(5) Uani 1 2 d S . . C7 C 0.1588(3) 0.3176(7) 0.0549(8) 0.111(3) Uani 1 2 d S . . 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 0.0476(3) 0.0476(3) 0.0419(4) -0.00214(10) 0.00214(10) 0.0348(3) S1 0.087(2) 0.287(7) 0.246(6) -0.208(6) -0.083(3) 0.104(3) O1 0.0486(14) 0.0698(16) 0.0580(15) -0.0095(12) -0.0039(11) 0.0388(13) O2 0.0543(15) 0.0764(18) 0.0607(14) -0.0131(13) -0.0087(12) 0.0450(14) O3 0.113(3) 0.113(3) 0.113(4) -0.0404(18) 0.0404(18) 0.055(3) C1 0.052(2) 0.055(2) 0.056(2) 0.0007(16) -0.0017(16) 0.0369(18) C2 0.048(2) 0.057(2) 0.059(2) -0.0055(16) -0.0018(16) 0.0330(17) C3 0.060(2) 0.085(3) 0.071(2) -0.023(2) -0.010(2) 0.049(2) C4 0.060(2) 0.102(5) 0.075(4) -0.036(4) -0.0181(18) 0.051(2) C5 0.0450(19) 0.047(3) 0.057(3) 0.001(2) 0.0004(11) 0.0235(13) C6 0.191(10) 0.117(9) 0.165(11) -0.048(8) -0.024(4) 0.059(4) C7 0.090(3) 0.172(9) 0.098(5) -0.075(6) -0.038(3) 0.086(4) _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 O1 1.950(2) . ? Cu1 O1 1.950(2) 12_665 ? Cu1 O2 1.959(2) 7_666 ? Cu1 O2 1.959(2) 6_556 ? Cu1 O3 2.139(4) . ? Cu1 Cu1 2.6435(10) 7_666 ? S1 C7 1.773(9) . ? S1 C6 1.943(13) . ? O1 C1 1.246(4) . ? O2 C1 1.267(4) . ? O2 Cu1 1.959(2) 7_666 ? C1 C2 1.501(5) . ? C2 C3 1.388(5) . ? C2 C5 1.388(4) . ? C3 C4 1.379(5) . ? C4 C3 1.379(5) 10 ? C4 C7 1.547(9) . ? C5 C2 1.388(4) 10 ? C6 S1 1.943(13) 10 ? C7 S1 1.773(9) 10 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 88.86(15) . 12_665 ? O1 Cu1 O2 168.03(10) . 7_666 ? O1 Cu1 O2 89.52(12) 12_665 7_666 ? O1 Cu1 O2 89.52(12) . 6_556 ? O1 Cu1 O2 168.03(10) 12_665 6_556 ? O2 Cu1 O2 89.62(17) 7_666 6_556 ? O1 Cu1 O3 97.43(14) . . ? O1 Cu1 O3 97.43(14) 12_665 . ? O2 Cu1 O3 94.54(15) 7_666 . ? O2 Cu1 O3 94.54(15) 6_556 . ? O1 Cu1 Cu1 83.79(7) . 7_666 ? O1 Cu1 Cu1 83.79(7) 12_665 7_666 ? O2 Cu1 Cu1 84.25(7) 7_666 7_666 ? O2 Cu1 Cu1 84.25(7) 6_556 7_666 ? O3 Cu1 Cu1 178.28(18) . 7_666 ? C7 S1 C6 95.6(5) . . ? C7 S1 S1 54.7(3) . 10 ? C6 S1 S1 58.1(3) . 10 ? C7 S1 S1 143.8(5) . 5 ? C6 S1 S1 120.0(4) . 5 ? S1 S1 S1 138.8(2) 10 5 ? C1 O1 Cu1 123.9(2) . . ? C1 O2 Cu1 122.4(2) . 7_666 ? O1 C1 O2 125.7(3) . . ? O1 C1 C2 117.8(3) . . ? O2 C1 C2 116.5(3) . . ? C3 C2 C5 119.4(3) . . ? C3 C2 C1 121.5(3) . . ? C5 C2 C1 119.0(3) . . ? C4 C3 C2 121.1(4) . . ? C3 C4 C3 119.0(5) 10 . ? C3 C4 C7 120.5(3) 10 . ? C3 C4 C7 120.5(3) . . ? C2 C5 C2 120.0(5) . 10 ? S1 C6 S1 63.7(5) 10 . ? C4 C7 S1 113.5(6) . 10 ? C4 C7 S1 113.5(6) . . ? S1 C7 S1 70.7(5) 10 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.609 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 25.1 13.0 2 0.010 0.406 -0.028 1880.5 353.5 _platon_squeeze_details ; ; #===END data_compound6_k06adb10 _database_code_depnum_ccdc_archive 'CCDC 686383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Cu4 N4 O24' _chemical_formula_weight 1323.14 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7640(1) _cell_length_b 32.5740(3) _cell_length_c 10.4820(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.025(1) _cell_angle_gamma 90.00 _cell_volume 5382.47(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 275102 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Blue/green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69596 _diffrn_reflns_av_R_equivalents 0.0951 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 29.00 _reflns_number_total 14249 _reflns_number_gt 8746 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0343P)^2^+6.8633P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14249 _refine_ls_number_parameters 734 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.20773(4) 0.100548(19) -0.05340(6) 0.01505(14) Uani 1 1 d . . . Cu2 Cu 0.21348(4) 0.159797(18) 0.11659(6) 0.01493(14) Uani 1 1 d . . . Cu3 Cu 0.70818(4) 0.099223(19) -0.37803(6) 0.01591(15) Uani 1 1 d . . . Cu4 Cu 0.71574(4) 0.157498(19) -0.55157(6) 0.01558(15) Uani 1 1 d . . . O1 O 0.1269(2) 0.07037(12) 0.0543(4) 0.0235(9) Uani 1 1 d . . . O2 O 0.1253(2) 0.12278(12) 0.1923(4) 0.0234(9) Uani 1 1 d . . . O3 O 0.2836(3) 0.13853(10) -0.1431(3) 0.0213(8) Uani 1 1 d . . . O4 O 0.3008(2) 0.18629(11) 0.0100(3) 0.0215(9) Uani 1 1 d . . . O5 O 0.3042(2) 0.07773(12) 0.0419(4) 0.0250(10) Uani 1 1 d . . . O6 O 0.3019(2) 0.12597(12) 0.1938(3) 0.0228(9) Uani 1 1 d . . . O7 O 0.1105(2) 0.13283(13) -0.1185(4) 0.0209(9) Uani 1 1 d . . . O8 O 0.1230(2) 0.18565(12) 0.0174(4) 0.0224(9) Uani 1 1 d . . . O9 O 0.2147(3) 0.05938(11) -0.2141(3) 0.0230(9) Uani 1 1 d . . . O10 O 0.2076(2) 0.19920(11) 0.2831(3) 0.0231(9) Uani 1 1 d . . . O11 O -0.0332(2) 0.13179(12) 0.2966(4) 0.0242(10) Uani 1 1 d . . . O12 O 0.4647(2) 0.13012(14) -0.1735(4) 0.0284(11) Uani 1 1 d . . . O13 O 0.6106(2) 0.13230(13) -0.3140(4) 0.0220(10) Uani 1 1 d . . . O14 O 0.6275(2) 0.18474(11) -0.4506(4) 0.0209(9) Uani 1 1 d . . . O15 O 0.8046(2) 0.07517(11) -0.4663(4) 0.0218(9) Uani 1 1 d . . . O16 O 0.8018(2) 0.12194(12) -0.6249(3) 0.0247(9) Uani 1 1 d . . . O17 O 0.7845(3) 0.13770(11) -0.2914(3) 0.0236(8) Uani 1 1 d . . . O18 O 0.8041(2) 0.18364(12) -0.4478(4) 0.0232(10) Uani 1 1 d . . . O19 O 0.6264(2) 0.07010(12) -0.4876(4) 0.0254(10) Uani 1 1 d . . . O20 O 0.6250(2) 0.12259(12) -0.6258(4) 0.0212(9) Uani 1 1 d . . . O21 O 0.7132(3) 0.05849(11) -0.2165(4) 0.0247(9) Uani 1 1 d . . . O22 O 0.7137(2) 0.19642(11) -0.7211(3) 0.0233(9) Uani 1 1 d . . . O23 O 0.4690(2) 0.13449(12) 0.2673(4) 0.0213(9) Uani 1 1 d . . . O24 O 0.9632(2) 0.12879(13) -0.2570(4) 0.0220(10) Uani 1 1 d . . . N1 N 0.2236(3) 0.06139(16) -0.4307(5) 0.0336(13) Uani 1 1 d . . . N2 N 0.1542(3) 0.19603(15) 0.4850(5) 0.0290(12) Uani 1 1 d . . . N3 N 0.7187(4) 0.05640(16) -0.0011(5) 0.0383(13) Uani 1 1 d . . . N4 N 0.6581(3) 0.19557(16) -0.9214(5) 0.0294(13) Uani 1 1 d . . . C1 C 0.0988(3) 0.08889(18) 0.1509(6) 0.0208(13) Uani 1 1 d . . . C2 C 0.0291(4) 0.06819(17) 0.2248(7) 0.0275(14) Uani 1 1 d . . . C3 C 0.0281(4) 0.0253(2) 0.2278(8) 0.054(2) Uani 1 1 d . . . H3 H 0.0670 0.0102 0.1771 0.065 Uiso 1 1 calc R . . C4 C -0.0300(5) 0.0047(2) 0.3054(10) 0.089(4) Uani 1 1 d . . . H4 H -0.0281 -0.0244 0.3115 0.107 Uiso 1 1 calc R . . C5 C -0.0900(4) 0.0262(2) 0.3728(9) 0.063(3) Uani 1 1 d . . . H5 H -0.1283 0.0119 0.4268 0.076 Uiso 1 1 calc R . . C6 C -0.0954(4) 0.06865(19) 0.3632(6) 0.0280(15) Uani 1 1 d . . . C7 C -0.0335(3) 0.09009(18) 0.2919(6) 0.0208(13) Uani 1 1 d . . . C8 C -0.0642(4) 0.1511(2) 0.1828(7) 0.0402(18) Uani 1 1 d . . . H8A H -0.0431 0.1363 0.1079 0.060 Uiso 1 1 calc R . . H8B H -0.0443 0.1796 0.1798 0.060 Uiso 1 1 calc R . . H8C H -0.1264 0.1507 0.1828 0.060 Uiso 1 1 calc R . . C9 C 0.3177(3) 0.17075(17) -0.0951(6) 0.0184(13) Uani 1 1 d . . . C10 C 0.3821(3) 0.19115(16) -0.1813(5) 0.0176(12) Uani 1 1 d . . . C11 C 0.3708(3) 0.23115(19) -0.2198(5) 0.0274(14) Uani 1 1 d . . . H11 H 0.3249 0.2467 -0.1864 0.033 Uiso 1 1 calc R . . C12 C 0.4255(3) 0.2489(2) -0.3066(6) 0.0286(15) Uani 1 1 d . . . H12 H 0.4159 0.2761 -0.3364 0.034 Uiso 1 1 calc R . . C13 C 0.4944(3) 0.22664(18) -0.3496(6) 0.0274(14) Uani 1 1 d . . . H13 H 0.5319 0.2390 -0.4091 0.033 Uiso 1 1 calc R . . C14 C 0.5108(3) 0.18673(17) -0.3088(5) 0.0186(12) Uani 1 1 d . . . C15 C 0.4536(3) 0.16856(17) -0.2233(5) 0.0196(13) Uani 1 1 d . . . C16 C 0.4397(4) 0.0966(2) -0.2509(7) 0.0400(18) Uani 1 1 d . . . H16A H 0.3795 0.0993 -0.2726 0.060 Uiso 1 1 calc R . . H16B H 0.4489 0.0709 -0.2044 0.060 Uiso 1 1 calc R . . H16C H 0.4736 0.0965 -0.3293 0.060 Uiso 1 1 calc R . . C17 C 0.5900(3) 0.16603(18) -0.3598(6) 0.0204(13) Uani 1 1 d . . . C18 C 0.3299(3) 0.09425(18) 0.1421(5) 0.0180(12) Uani 1 1 d . . . C19 C 0.3987(3) 0.07163(17) 0.2127(6) 0.0201(13) Uani 1 1 d . . . C20 C 0.3930(3) 0.02955(18) 0.2199(6) 0.0253(13) Uani 1 1 d . . . H20 H 0.3496 0.0157 0.1740 0.030 Uiso 1 1 calc R . . C21 C 0.4495(3) 0.00699(19) 0.2933(6) 0.0289(14) Uani 1 1 d . . . H21 H 0.4447 -0.0220 0.2989 0.035 Uiso 1 1 calc R . . C22 C 0.5132(3) 0.02759(17) 0.3581(5) 0.0222(13) Uani 1 1 d . . . H22 H 0.5517 0.0123 0.4093 0.027 Uiso 1 1 calc R . . C23 C 0.5225(3) 0.06988(17) 0.3505(5) 0.0181(12) Uani 1 1 d . . . C24 C 0.4632(3) 0.09236(17) 0.2789(5) 0.0186(12) Uani 1 1 d . . . C25 C 0.4403(4) 0.15680(19) 0.3780(6) 0.0332(15) Uani 1 1 d . . . H25A H 0.3786 0.1601 0.3741 0.050 Uiso 1 1 calc R . . H25B H 0.4673 0.1839 0.3799 0.050 Uiso 1 1 calc R . . H25C H 0.4556 0.1416 0.4554 0.050 Uiso 1 1 calc R . . C26 C 0.1924(4) 0.07224(18) -0.3195(6) 0.0291(15) Uani 1 1 d . . . H26 H 0.1481 0.0920 -0.3205 0.035 Uiso 1 1 calc R . . C27 C 0.1937(5) 0.0783(2) -0.5500(6) 0.059(2) Uani 1 1 d . . . H27A H 0.1405 0.0931 -0.5356 0.088 Uiso 1 1 calc R . . H27B H 0.1841 0.0560 -0.6111 0.088 Uiso 1 1 calc R . . H27C H 0.2363 0.0972 -0.5842 0.088 Uiso 1 1 calc R . . C28 C 0.2927(5) 0.03205(19) -0.4399(6) 0.0428(16) Uani 1 1 d . . . H28A H 0.3085 0.0227 -0.3542 0.064 Uiso 1 1 calc R . . H28B H 0.3417 0.0452 -0.4805 0.064 Uiso 1 1 calc R . . H28C H 0.2746 0.0085 -0.4911 0.064 Uiso 1 1 calc R . . C29 C 0.1496(4) 0.19113(18) 0.3603(6) 0.0247(14) Uani 1 1 d . . . H29 H 0.0981 0.1806 0.3264 0.030 Uiso 1 1 calc R . . C30 C 0.0821(4) 0.1856(2) 0.5677(7) 0.0423(19) Uani 1 1 d . . . H30A H 0.0350 0.1755 0.5153 0.063 Uiso 1 1 calc R . . H30B H 0.0639 0.2101 0.6146 0.063 Uiso 1 1 calc R . . H30C H 0.0992 0.1642 0.6283 0.063 Uiso 1 1 calc R . . C31 C 0.2287(4) 0.2109(2) 0.5466(6) 0.0491(19) Uani 1 1 d . . . H31A H 0.2468 0.1912 0.6118 0.074 Uiso 1 1 calc R . . H31B H 0.2165 0.2374 0.5868 0.074 Uiso 1 1 calc R . . H31C H 0.2740 0.2143 0.4835 0.074 Uiso 1 1 calc R . . C32 C 0.8320(3) 0.09052(19) -0.5706(6) 0.0216(13) Uani 1 1 d . . . C33 C 0.8199(3) 0.16850(18) -0.3399(6) 0.0178(12) Uani 1 1 d . . . C34 C 0.8837(3) 0.19025(17) -0.2582(5) 0.0199(12) Uani 1 1 d . . . C35 C 0.8712(3) 0.23073(17) -0.2227(5) 0.0242(14) Uani 1 1 d . . . H35 H 0.8249 0.2458 -0.2573 0.029 Uiso 1 1 calc R . . C36 C 0.9257(3) 0.24929(19) -0.1374(6) 0.0289(15) Uani 1 1 d . . . H36 H 0.9165 0.2770 -0.1123 0.035 Uiso 1 1 calc R . . C37 C 0.9938(3) 0.22753(17) -0.0883(5) 0.0226(13) Uani 1 1 d . . . H37 H 1.0306 0.2403 -0.0286 0.027 Uiso 1 1 calc R . . C38 C 1.0089(3) 0.18688(16) -0.1258(5) 0.0166(12) Uani 1 1 d . . . C39 C 0.9526(3) 0.16782(17) -0.2091(5) 0.0178(12) Uani 1 1 d . . . C40 C 0.9366(4) 0.09602(18) -0.1729(7) 0.0330(15) Uani 1 1 d . . . H40A H 0.9854 0.0863 -0.1235 0.050 Uiso 1 1 calc R . . H40B H 0.9136 0.0733 -0.2236 0.050 Uiso 1 1 calc R . . H40C H 0.8929 0.1062 -0.1146 0.050 Uiso 1 1 calc R . . C41 C 0.5972(3) 0.08944(18) -0.5830(6) 0.0180(13) Uani 1 1 d . . . C42 C 0.6915(4) 0.07070(19) -0.1116(6) 0.0312(15) Uani 1 1 d . . . H42 H 0.6515 0.0925 -0.1091 0.037 Uiso 1 1 calc R . . C43 C 0.6884(7) 0.0734(3) 0.1215(7) 0.092(4) Uani 1 1 d . . . H43A H 0.7370 0.0830 0.1717 0.137 Uiso 1 1 calc R . . H43B H 0.6582 0.0520 0.1691 0.137 Uiso 1 1 calc R . . H43C H 0.6499 0.0964 0.1051 0.137 Uiso 1 1 calc R . . C44 C 0.7835(5) 0.02428(19) 0.0042(6) 0.0448(17) Uani 1 1 d . . . H44A H 0.7997 0.0165 -0.0827 0.067 Uiso 1 1 calc R . . H44B H 0.7608 0.0003 0.0490 0.067 Uiso 1 1 calc R . . H44C H 0.8334 0.0346 0.0498 0.067 Uiso 1 1 calc R . . C45 C 0.6549(4) 0.18995(17) -0.7961(6) 0.0244(14) Uani 1 1 d . . . H45 H 0.6031 0.1801 -0.7613 0.029 Uiso 1 1 calc R . . C46 C 0.5870(4) 0.1858(2) -1.0034(6) 0.0441(19) Uani 1 1 d . . . H46A H 0.5408 0.1743 -0.9521 0.066 Uiso 1 1 calc R . . H46B H 0.6047 0.1657 -1.0676 0.066 Uiso 1 1 calc R . . H46C H 0.5673 0.2108 -1.0461 0.066 Uiso 1 1 calc R . . C47 C 0.7353(4) 0.2103(2) -0.9821(6) 0.0454(19) Uani 1 1 d . . . H47A H 0.7268 0.2385 -1.0119 0.068 Uiso 1 1 calc R . . H47B H 0.7492 0.1926 -1.0549 0.068 Uiso 1 1 calc R . . H47C H 0.7821 0.2096 -0.9205 0.068 Uiso 1 1 calc R . . C76 C 0.0863(3) 0.16627(17) -0.0709(5) 0.0169(12) 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 0.0097(3) 0.0186(3) 0.0169(4) -0.0007(3) -0.0018(3) 0.0005(3) Cu2 0.0096(3) 0.0199(3) 0.0153(4) -0.0005(3) -0.0018(3) 0.0007(3) Cu3 0.0098(3) 0.0212(4) 0.0167(4) 0.0013(3) -0.0020(3) -0.0002(3) Cu4 0.0100(3) 0.0210(4) 0.0158(4) 0.0009(3) -0.0013(3) -0.0013(3) O1 0.023(2) 0.022(2) 0.025(2) -0.0023(19) 0.0079(19) -0.0013(17) O2 0.020(2) 0.026(2) 0.025(2) -0.0022(19) 0.0042(18) -0.0054(17) O3 0.0176(17) 0.026(2) 0.021(2) -0.0026(15) 0.000(2) -0.003(2) O4 0.015(2) 0.029(2) 0.020(2) -0.0038(17) 0.0021(17) -0.0019(16) O5 0.020(2) 0.030(2) 0.026(2) -0.0005(19) -0.0074(18) 0.0052(17) O6 0.016(2) 0.029(2) 0.023(2) -0.0010(17) -0.0050(16) 0.0035(17) O7 0.0165(18) 0.021(2) 0.026(3) -0.004(2) -0.0061(17) 0.0055(15) O8 0.0176(19) 0.027(2) 0.023(2) -0.0021(18) -0.0100(17) 0.0038(16) O9 0.031(2) 0.022(2) 0.016(2) -0.0022(16) -0.0016(18) 0.0027(18) O10 0.0222(19) 0.028(2) 0.019(2) -0.0051(17) 0.0041(18) -0.0036(18) O11 0.020(2) 0.020(2) 0.033(3) -0.003(2) 0.0040(18) 0.0002(16) O12 0.020(2) 0.027(3) 0.038(3) 0.007(2) 0.005(2) 0.0008(17) O13 0.0166(18) 0.030(3) 0.020(2) 0.003(2) 0.0031(17) 0.0066(17) O14 0.0215(19) 0.023(2) 0.018(2) -0.0006(19) 0.0095(17) 0.0010(16) O15 0.017(2) 0.024(2) 0.024(2) 0.0077(17) 0.0043(16) -0.0006(15) O16 0.012(2) 0.045(3) 0.016(2) 0.0047(19) 0.0041(16) -0.0009(18) O17 0.0167(17) 0.026(2) 0.028(2) 0.0064(16) -0.011(2) -0.008(2) O18 0.021(2) 0.026(2) 0.023(2) -0.0007(18) -0.0057(18) -0.0077(16) O19 0.026(2) 0.026(2) 0.025(2) 0.0022(18) -0.0120(18) -0.0059(17) O20 0.0139(18) 0.028(2) 0.022(2) 0.0044(19) -0.0084(17) -0.0038(16) O21 0.026(2) 0.028(2) 0.020(2) 0.0009(18) 0.002(2) -0.004(2) O22 0.0210(19) 0.027(2) 0.022(2) 0.0074(16) -0.0052(18) -0.0034(18) O23 0.022(2) 0.016(2) 0.027(2) 0.0017(19) -0.0050(18) -0.0011(16) O24 0.020(2) 0.017(2) 0.030(3) -0.0068(19) -0.0029(19) 0.0025(15) N1 0.043(3) 0.037(3) 0.020(3) 0.001(2) -0.003(3) 0.007(3) N2 0.032(3) 0.026(3) 0.029(3) 0.002(2) 0.006(3) -0.001(2) N3 0.065(4) 0.028(3) 0.022(3) 0.002(2) 0.006(3) 0.004(3) N4 0.039(3) 0.029(3) 0.021(3) -0.001(3) -0.006(3) -0.003(2) C1 0.012(3) 0.020(3) 0.030(4) 0.000(3) 0.003(3) 0.001(2) C2 0.023(3) 0.021(3) 0.038(4) -0.002(3) 0.005(3) 0.002(2) C3 0.049(4) 0.024(4) 0.089(6) -0.001(4) 0.050(4) 0.003(3) C4 0.081(6) 0.017(4) 0.169(10) -0.003(5) 0.096(6) 0.002(4) C5 0.043(4) 0.032(4) 0.114(7) 0.005(5) 0.054(5) 0.002(3) C6 0.021(3) 0.023(3) 0.040(4) -0.003(3) 0.009(3) 0.001(2) C7 0.018(3) 0.022(3) 0.023(3) -0.005(3) 0.001(2) 0.000(2) C8 0.037(4) 0.036(4) 0.048(5) 0.020(4) 0.013(3) 0.010(3) C9 0.009(2) 0.018(3) 0.028(4) 0.007(3) -0.002(2) 0.000(2) C10 0.018(3) 0.016(3) 0.019(3) -0.004(2) -0.003(2) -0.002(2) C11 0.019(3) 0.038(4) 0.025(4) -0.004(3) 0.003(3) 0.006(3) C12 0.027(3) 0.026(4) 0.033(4) 0.004(3) 0.006(3) 0.003(3) C13 0.025(3) 0.027(4) 0.030(4) 0.004(3) 0.004(3) 0.003(3) C14 0.015(2) 0.023(3) 0.018(3) -0.001(2) 0.001(2) -0.003(2) C15 0.021(3) 0.017(3) 0.020(3) -0.001(3) -0.002(2) 0.002(2) C16 0.029(3) 0.026(4) 0.065(5) -0.005(4) 0.011(3) -0.004(3) C17 0.015(3) 0.018(3) 0.028(4) -0.001(3) -0.004(2) -0.001(2) C18 0.011(2) 0.028(3) 0.014(3) 0.000(3) 0.000(2) -0.004(2) C19 0.015(3) 0.020(3) 0.025(3) 0.001(3) -0.002(2) 0.004(2) C20 0.015(3) 0.023(3) 0.038(4) -0.005(3) -0.010(2) -0.002(2) C21 0.030(3) 0.018(3) 0.038(4) 0.004(3) -0.013(3) -0.005(2) C22 0.016(2) 0.023(3) 0.027(3) 0.004(3) -0.008(2) 0.003(2) C23 0.013(2) 0.020(3) 0.021(3) 0.002(2) -0.003(2) -0.001(2) C24 0.011(2) 0.022(3) 0.022(3) 0.003(3) 0.002(2) 0.000(2) C25 0.028(3) 0.028(4) 0.044(4) -0.005(3) -0.013(3) 0.000(2) C26 0.037(4) 0.022(3) 0.028(4) -0.003(3) -0.004(3) 0.002(3) C27 0.083(6) 0.075(6) 0.018(4) -0.003(4) 0.003(4) 0.026(5) C28 0.043(3) 0.045(4) 0.040(4) -0.009(3) 0.005(4) 0.012(4) C29 0.028(3) 0.024(3) 0.022(4) -0.006(3) 0.002(3) 0.003(3) C30 0.052(4) 0.038(4) 0.036(5) 0.009(3) 0.016(3) 0.013(3) C31 0.055(5) 0.056(5) 0.036(4) -0.010(4) -0.008(4) 0.001(4) C32 0.012(3) 0.023(3) 0.029(4) -0.004(3) 0.002(2) -0.001(2) C33 0.013(2) 0.023(3) 0.017(3) 0.002(2) -0.004(2) 0.006(2) C34 0.015(3) 0.025(3) 0.020(3) 0.002(3) -0.007(2) 0.003(2) C35 0.013(3) 0.021(3) 0.039(4) -0.002(3) -0.004(2) 0.004(2) C36 0.032(3) 0.019(3) 0.035(4) -0.004(3) -0.002(3) 0.001(2) C37 0.019(3) 0.024(3) 0.025(3) -0.003(3) -0.006(2) -0.003(2) C38 0.015(2) 0.017(3) 0.018(3) 0.003(2) -0.001(2) 0.000(2) C39 0.013(2) 0.019(3) 0.021(3) 0.002(2) -0.004(2) -0.001(2) C40 0.027(3) 0.019(3) 0.054(5) -0.001(3) -0.009(3) 0.002(2) C41 0.013(2) 0.019(3) 0.021(3) -0.003(3) -0.002(2) 0.003(2) C42 0.037(4) 0.027(4) 0.029(4) 0.005(3) 0.004(3) 0.005(3) C43 0.152(10) 0.089(8) 0.033(5) -0.004(5) 0.018(6) 0.043(7) C44 0.052(4) 0.047(4) 0.036(4) 0.010(3) -0.007(4) 0.017(4) C45 0.020(3) 0.025(3) 0.028(4) 0.004(3) 0.001(3) -0.002(2) C46 0.048(4) 0.050(5) 0.034(4) -0.006(4) -0.022(3) 0.006(3) C47 0.047(4) 0.059(5) 0.030(4) 0.009(4) 0.003(3) -0.008(3) C76 0.011(2) 0.022(3) 0.017(3) 0.004(3) -0.003(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.961(4) . ? Cu1 O5 1.965(4) . ? Cu1 O1 1.967(4) . ? Cu1 O7 1.979(4) . ? Cu1 O9 2.155(3) . ? Cu2 O6 1.952(4) . ? Cu2 O8 1.956(3) . ? Cu2 O4 1.972(4) . ? Cu2 O2 2.005(4) . ? Cu2 O10 2.169(4) . ? Cu3 O15 1.944(4) . ? Cu3 O17 1.960(4) . ? Cu3 O19 1.970(4) . ? Cu3 O13 1.994(4) . ? Cu3 O21 2.153(4) . ? Cu4 O16 1.943(4) . ? Cu4 O14 1.961(4) . ? Cu4 O18 1.962(4) . ? Cu4 O20 1.986(3) . ? Cu4 O22 2.183(3) . ? O1 C1 1.259(7) . ? O2 C1 1.257(7) . ? O3 C9 1.282(6) . ? O4 C9 1.242(7) . ? O5 C18 1.247(6) . ? O6 C18 1.247(6) . ? O7 C76 1.258(6) . ? O8 C76 1.260(6) . ? O9 C26 1.233(7) . ? O10 C29 1.248(7) . ? O11 C7 1.359(7) . ? O11 C8 1.435(7) . ? O12 C15 1.368(7) . ? O12 C16 1.415(7) . ? O13 C17 1.242(7) . ? O14 C17 1.275(7) . ? O15 C32 1.278(7) . ? O16 C32 1.264(7) . ? O17 C33 1.256(6) . ? O18 C33 1.258(6) . ? O19 C41 1.268(6) . ? O20 C41 1.249(6) . ? O21 C42 1.218(7) . ? O22 C45 1.233(6) . ? O23 C24 1.381(6) . ? O23 C25 1.442(7) . ? O24 C39 1.377(6) . ? O24 C40 1.446(7) . ? N1 C26 1.314(7) . ? N1 C27 1.445(8) . ? N1 C28 1.452(8) . ? N2 C29 1.319(7) . ? N2 C31 1.424(8) . ? N2 C30 1.470(8) . ? N3 C42 1.320(7) . ? N3 C44 1.463(8) . ? N3 C43 1.479(9) . ? N4 C45 1.327(7) . ? N4 C46 1.449(7) . ? N4 C47 1.455(8) . ? C1 C2 1.504(8) . ? C2 C3 1.396(8) . ? C2 C7 1.407(8) . ? C3 C4 1.397(9) . ? C4 C5 1.372(9) . ? C5 C6 1.388(9) . ? C6 C7 1.414(8) . ? C6 C32 1.517(8) 1_456 ? C9 C10 1.512(7) . ? C10 C11 1.376(8) . ? C10 C15 1.416(7) . ? C11 C12 1.381(8) . ? C12 C13 1.382(8) . ? C13 C14 1.393(8) . ? C14 C15 1.402(7) . ? C14 C17 1.517(7) . ? C18 C19 1.506(7) . ? C19 C20 1.376(7) . ? C19 C24 1.404(7) . ? C20 C21 1.388(8) . ? C21 C22 1.385(7) . ? C22 C23 1.388(7) . ? C23 C24 1.405(7) . ? C23 C41 1.509(7) 1_556 ? C32 C6 1.517(8) 1_654 ? C33 C34 1.499(7) . ? C34 C35 1.384(7) . ? C34 C39 1.407(7) . ? C35 C36 1.380(8) . ? C36 C37 1.385(8) . ? C37 C38 1.402(7) . ? C38 C39 1.391(7) . ? C38 C76 1.508(7) 1_655 ? C41 C23 1.509(7) 1_554 ? C76 C38 1.508(7) 1_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 O3 Cu1 O5 90.60(17) . . ? O3 Cu1 O1 170.47(16) . . ? O5 Cu1 O1 91.20(16) . . ? O3 Cu1 O7 88.37(17) . . ? O5 Cu1 O7 167.14(16) . . ? O1 Cu1 O7 87.80(16) . . ? O3 Cu1 O9 89.23(14) . . ? O5 Cu1 O9 97.03(16) . . ? O1 Cu1 O9 99.83(16) . . ? O7 Cu1 O9 95.77(15) . . ? O6 Cu2 O8 169.76(16) . . ? O6 Cu2 O4 89.05(16) . . ? O8 Cu2 O4 91.12(15) . . ? O6 Cu2 O2 89.52(15) . . ? O8 Cu2 O2 87.91(16) . . ? O4 Cu2 O2 166.41(15) . . ? O6 Cu2 O10 91.79(15) . . ? O8 Cu2 O10 98.14(15) . . ? O4 Cu2 O10 103.14(15) . . ? O2 Cu2 O10 90.42(15) . . ? O15 Cu3 O17 89.92(17) . . ? O15 Cu3 O19 92.28(16) . . ? O17 Cu3 O19 168.39(15) . . ? O15 Cu3 O13 168.76(16) . . ? O17 Cu3 O13 88.39(18) . . ? O19 Cu3 O13 87.23(17) . . ? O15 Cu3 O21 95.61(16) . . ? O17 Cu3 O21 90.43(14) . . ? O19 Cu3 O21 100.69(16) . . ? O13 Cu3 O21 95.52(16) . . ? O16 Cu4 O14 168.30(16) . . ? O16 Cu4 O18 88.98(16) . . ? O14 Cu4 O18 90.47(15) . . ? O16 Cu4 O20 90.38(15) . . ? O14 Cu4 O20 87.68(15) . . ? O18 Cu4 O20 167.72(16) . . ? O16 Cu4 O22 91.96(15) . . ? O14 Cu4 O22 99.59(15) . . ? O18 Cu4 O22 102.09(15) . . ? O20 Cu4 O22 90.19(15) . . ? C1 O1 Cu1 116.8(4) . . ? C1 O2 Cu2 128.4(4) . . ? C9 O3 Cu1 125.7(4) . . ? C9 O4 Cu2 118.3(3) . . ? C18 O5 Cu1 121.0(4) . . ? C18 O6 Cu2 122.7(3) . . ? C76 O7 Cu1 123.9(3) . . ? C76 O8 Cu2 120.6(4) . . ? C26 O9 Cu1 118.3(4) . . ? C29 O10 Cu2 115.4(4) . . ? C7 O11 C8 114.0(5) . . ? C15 O12 C16 116.8(5) . . ? C17 O13 Cu3 123.3(4) . . ? C17 O14 Cu4 121.0(4) . . ? C32 O15 Cu3 121.0(3) . . ? C32 O16 Cu4 124.6(4) . . ? C33 O17 Cu3 126.6(3) . . ? C33 O18 Cu4 117.9(4) . . ? C41 O19 Cu3 117.2(4) . . ? C41 O20 Cu4 127.4(3) . . ? C42 O21 Cu3 119.9(4) . . ? C45 O22 Cu4 115.5(4) . . ? C24 O23 C25 114.1(4) . . ? C39 O24 C40 115.1(5) . . ? C26 N1 C27 122.9(6) . . ? C26 N1 C28 121.1(6) . . ? C27 N1 C28 116.0(5) . . ? C29 N2 C31 122.3(5) . . ? C29 N2 C30 121.0(5) . . ? C31 N2 C30 116.7(5) . . ? C42 N3 C44 120.8(6) . . ? C42 N3 C43 121.7(6) . . ? C44 N3 C43 117.4(6) . . ? C45 N4 C46 121.8(5) . . ? C45 N4 C47 120.7(5) . . ? C46 N4 C47 117.4(5) . . ? O2 C1 O1 125.6(5) . . ? O2 C1 C2 117.3(5) . . ? O1 C1 C2 117.1(5) . . ? C3 C2 C7 119.2(6) . . ? C3 C2 C1 117.9(5) . . ? C7 C2 C1 122.9(5) . . ? C4 C3 C2 120.1(6) . . ? C5 C4 C3 120.4(7) . . ? C4 C5 C6 120.9(7) . . ? C5 C6 C7 119.2(6) . . ? C5 C6 C32 118.7(5) . 1_456 ? C7 C6 C32 122.1(5) . 1_456 ? O11 C7 C2 121.5(5) . . ? O11 C7 C6 118.5(5) . . ? C2 C7 C6 119.9(5) . . ? O4 C9 O3 126.3(5) . . ? O4 C9 C10 119.7(5) . . ? O3 C9 C10 114.0(5) . . ? C11 C10 C15 120.2(5) . . ? C11 C10 C9 120.3(5) . . ? C15 C10 C9 119.4(5) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C11 119.0(6) . . ? C12 C13 C14 122.4(6) . . ? C13 C14 C15 118.1(5) . . ? C13 C14 C17 117.3(5) . . ? C15 C14 C17 124.6(5) . . ? O12 C15 C14 123.2(5) . . ? O12 C15 C10 117.3(5) . . ? C14 C15 C10 119.4(5) . . ? O13 C17 O14 126.2(5) . . ? O13 C17 C14 118.2(5) . . ? O14 C17 C14 115.6(5) . . ? O5 C18 O6 127.5(5) . . ? O5 C18 C19 115.9(5) . . ? O6 C18 C19 116.5(5) . . ? C20 C19 C24 120.0(5) . . ? C20 C19 C18 117.9(5) . . ? C24 C19 C18 122.0(5) . . ? C19 C20 C21 121.1(5) . . ? C22 C21 C20 118.7(5) . . ? C21 C22 C23 122.0(5) . . ? C22 C23 C24 118.5(5) . . ? C22 C23 C41 118.4(5) . 1_556 ? C24 C23 C41 123.1(5) . 1_556 ? O23 C24 C23 121.4(5) . . ? O23 C24 C19 118.8(5) . . ? C23 C24 C19 119.7(5) . . ? O9 C26 N1 126.7(6) . . ? O10 C29 N2 125.2(6) . . ? O16 C32 O15 125.1(5) . . ? O16 C32 C6 117.3(5) . 1_654 ? O15 C32 C6 117.6(5) . 1_654 ? O17 C33 O18 126.1(5) . . ? O17 C33 C34 116.4(5) . . ? O18 C33 C34 117.4(5) . . ? C35 C34 C39 120.4(5) . . ? C35 C34 C33 120.6(5) . . ? C39 C34 C33 118.8(5) . . ? C36 C35 C34 120.2(5) . . ? C35 C36 C37 119.9(6) . . ? C36 C37 C38 120.7(5) . . ? C39 C38 C37 119.3(5) . . ? C39 C38 C76 123.9(5) . 1_655 ? C37 C38 C76 116.8(5) . 1_655 ? O24 C39 C38 124.3(5) . . ? O24 C39 C34 116.1(5) . . ? C38 C39 C34 119.3(5) . . ? O20 C41 O19 125.9(5) . . ? O20 C41 C23 118.2(5) . 1_554 ? O19 C41 C23 115.9(5) . 1_554 ? O21 C42 N3 125.9(6) . . ? O22 C45 N4 125.4(5) . . ? O7 C76 O8 125.9(5) . . ? O7 C76 C38 118.7(5) . 1_455 ? O8 C76 C38 115.3(5) . 1_455 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.891 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.134