# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Li, Dan' _publ_contact_author_email dli@stu.edu.cn _publ_author_name 'Dan Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 826227' #TrackingRef '- Compounds 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H51 Cu6 N15' _chemical_formula_weight 1507.53 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.4693(15) _cell_length_b 14.3685(9) _cell_length_c 21.7069(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.1680(10) _cell_angle_gamma 90.00 _cell_volume 6619.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 1.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.754 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17070 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5812 _reflns_number_gt 3567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0467P)^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 5812 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 -0.20977(2) 0.65862(4) -0.05644(3) 0.06049(19) Uani 1 1 d . . . Cu2 Cu 0.00382(2) 0.59971(4) 0.08836(3) 0.05772(18) Uani 1 1 d . . . Cu3 Cu 0.21354(3) 0.66032(4) 0.23924(3) 0.0667(2) Uani 1 1 d . . . C1 C -0.07896(18) 0.6233(3) 0.04109(19) 0.0429(10) Uani 1 1 d . . . C2 C 0.13667(18) 0.6487(3) 0.1742(2) 0.0472(11) Uani 1 1 d . . . C3 C 0.24638(19) 0.7228(3) 0.3185(2) 0.0620(13) Uani 1 1 d . . . C4 C 0.3095(2) -0.1911(4) 0.0951(3) 0.109(2) Uani 1 1 d . . . H4A H 0.3008 -0.2566 0.0935 0.163 Uiso 1 1 calc R . . H4B H 0.3440 -0.1772 0.1339 0.163 Uiso 1 1 calc R . . H4C H 0.3204 -0.1734 0.0575 0.163 Uiso 1 1 calc R . . C5 C 0.2524(2) -0.1382(4) 0.0959(3) 0.0755(15) Uani 1 1 d . . . C6 C 0.1975(2) -0.1837(3) 0.0926(3) 0.0829(16) Uani 1 1 d . . . H6 H 0.1968 -0.2484 0.0915 0.099 Uiso 1 1 calc R . . C7 C 0.1436(2) -0.1367(3) 0.0911(2) 0.0693(14) Uani 1 1 d . . . H7 H 0.1074 -0.1702 0.0884 0.083 Uiso 1 1 calc R . . C8 C 0.14231(19) -0.0409(3) 0.09336(18) 0.0486(10) Uani 1 1 d . . . C9 C 0.1979(2) 0.0046(3) 0.0978(2) 0.0678(14) Uani 1 1 d . . . H9 H 0.1991 0.0693 0.1001 0.081 Uiso 1 1 calc R . . C10 C 0.2508(2) -0.0425(4) 0.0989(3) 0.0810(16) Uani 1 1 d . . . H10 H 0.2871 -0.0090 0.1019 0.097 Uiso 1 1 calc R . . C11 C 0.08442(18) 0.0117(3) 0.08968(18) 0.0453(10) Uani 1 1 d . . . C12 C 0.02819(19) -0.0325(3) 0.08603(18) 0.0488(10) Uani 1 1 d . . . H12 H 0.0267 -0.0972 0.0868 0.059 Uiso 1 1 calc R . . C13 C -0.02558(18) 0.0182(3) 0.08130(17) 0.0445(10) Uani 1 1 d . . . C14 C 0.02753(19) 0.1554(3) 0.08481(19) 0.0471(10) Uani 1 1 d . . . C15 C 0.08227(18) 0.1087(3) 0.08898(18) 0.0485(10) Uani 1 1 d . . . H15 H 0.1183 0.1424 0.0913 0.058 Uiso 1 1 calc R . . C16 C -0.08725(19) -0.0255(3) 0.07594(18) 0.0454(10) Uani 1 1 d . . . C17 C -0.0975(2) -0.1202(3) 0.0750(2) 0.0561(12) Uani 1 1 d . . . H17 H -0.0644 -0.1611 0.0785 0.067 Uiso 1 1 calc R . . C18 C -0.1560(2) -0.1542(3) 0.0689(2) 0.0576(12) Uani 1 1 d . . . H18 H -0.1611 -0.2184 0.0694 0.069 Uiso 1 1 calc R . . C19 C -0.1963(2) -0.0091(3) 0.0634(2) 0.0633(13) Uani 1 1 d . . . H19 H -0.2302 0.0304 0.0591 0.076 Uiso 1 1 calc R . . C20 C -0.1387(2) 0.0298(3) 0.0706(2) 0.0576(12) Uani 1 1 d . . . H20 H -0.1344 0.0942 0.0720 0.069 Uiso 1 1 calc R . . C21 C 0.02358(19) 0.2592(3) 0.0842(2) 0.0476(10) Uani 1 1 d . . . C22 C -0.03186(19) 0.3041(3) 0.0510(2) 0.0562(11) Uani 1 1 d . . . H22 H -0.0673 0.2697 0.0282 0.067 Uiso 1 1 calc R . . C23 C -0.03491(19) 0.3994(3) 0.0514(2) 0.0595(12) Uani 1 1 d . . . H23 H -0.0725 0.4280 0.0274 0.071 Uiso 1 1 calc R . . C24 C 0.06693(19) 0.4093(3) 0.1169(2) 0.0538(11) Uani 1 1 d . . . H24 H 0.1014 0.4451 0.1403 0.065 Uiso 1 1 calc R . . C25 C 0.07404(19) 0.3149(3) 0.1176(2) 0.0518(11) Uani 1 1 d . . . H25 H 0.1127 0.2881 0.1406 0.062 Uiso 1 1 calc R . . C26 C 0.3428(2) 0.6163(3) 0.2379(2) 0.0667(13) Uani 1 1 d . . . H26 H 0.3469 0.6808 0.2404 0.080 Uiso 1 1 calc R . . C27 C 0.3956(2) 0.5645(3) 0.2430(2) 0.0621(12) Uani 1 1 d . . . H27 H 0.4339 0.5938 0.2482 0.075 Uiso 1 1 calc R . . C28 C 0.39155(19) 0.4687(3) 0.24047(19) 0.0495(11) Uani 1 1 d . . . C29 C 0.3335(2) 0.4311(3) 0.2334(2) 0.0663(13) Uani 1 1 d . . . H29 H 0.3285 0.3669 0.2328 0.080 Uiso 1 1 calc R . . C30 C 0.2827(2) 0.4887(4) 0.2272(2) 0.0745(15) Uani 1 1 d . . . H30 H 0.2437 0.4613 0.2209 0.089 Uiso 1 1 calc R . . C31 C 0.44749(19) 0.4110(3) 0.24570(19) 0.0499(11) Uani 1 1 d . . . C32 C 0.4465(2) 0.3142(3) 0.2465(2) 0.0550(11) Uani 1 1 d . . . H32 H 0.4095 0.2835 0.2446 0.066 Uiso 1 1 calc R . . C33 C 0.5000 0.2627(4) 0.2500 0.0546(16) Uani 1 2 d S . . C34 C 0.5000 0.1599(4) 0.2500 0.0527(16) Uani 1 2 d S . . C35 C 0.5515(2) 0.1102(3) 0.2876(2) 0.0667(13) Uani 1 1 d . . . H35 H 0.5871 0.1418 0.3135 0.080 Uiso 1 1 calc R . . C36 C 0.5509(2) 0.0142(3) 0.2875(2) 0.0753(15) Uani 1 1 d . . . H36 H 0.5863 -0.0176 0.3136 0.090 Uiso 1 1 calc R . . C37 C 0.5000 -0.0360(5) 0.2500 0.0679(19) Uani 1 2 d S . . C38 C 0.5000 -0.1408(5) 0.2500 0.094(3) Uani 1 2 d S . . H38A H 0.4607 -0.1631 0.2205 0.142 Uiso 0.50 1 calc PR . . H38B H 0.5053 -0.1631 0.2932 0.142 Uiso 0.50 1 calc PR . . H38C H 0.5340 -0.1631 0.2363 0.142 Uiso 0.50 1 calc PR . . N1 N -0.1288(2) 0.6329(3) 0.0073(2) 0.0762(12) Uani 1 1 d . . . N2 N 0.0870(2) 0.6389(2) 0.1389(2) 0.0707(11) Uani 1 1 d . . . N3 N 0.26547(17) 0.7609(3) 0.3678(2) 0.0790(12) Uani 1 1 d . . . N4 N -0.20621(16) -0.1005(2) 0.06209(17) 0.0544(9) Uani 1 1 d . . . N5 N -0.02605(16) 0.1110(2) 0.08083(15) 0.0491(9) Uani 1 1 d . . . N6 N 0.01337(15) 0.4531(2) 0.08457(16) 0.0530(9) Uani 1 1 d . . . N7 N 0.28636(17) 0.5800(3) 0.22966(18) 0.0645(11) Uani 1 1 d . . . N8 N 0.5000 0.4587(3) 0.2500 0.0481(12) 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 0.0389(3) 0.0630(4) 0.0706(4) 0.0023(3) 0.0058(3) -0.0018(3) Cu2 0.0436(3) 0.0577(4) 0.0623(4) -0.0005(3) 0.0044(3) 0.0037(3) Cu3 0.0466(3) 0.0657(4) 0.0778(4) -0.0092(3) 0.0069(3) 0.0003(3) C1 0.022(2) 0.049(3) 0.044(3) 0.0044(19) -0.0074(19) 0.0097(18) C2 0.028(2) 0.053(3) 0.050(3) -0.014(2) -0.002(2) -0.005(2) C3 0.040(3) 0.056(3) 0.073(3) -0.022(3) -0.006(2) 0.013(2) C4 0.061(4) 0.098(5) 0.171(6) 0.005(4) 0.042(4) 0.016(3) C5 0.053(3) 0.076(4) 0.097(4) 0.007(3) 0.023(3) 0.012(3) C6 0.072(4) 0.058(3) 0.128(5) 0.002(3) 0.045(4) 0.012(3) C7 0.057(3) 0.051(3) 0.109(4) 0.004(3) 0.040(3) -0.001(2) C8 0.047(3) 0.051(3) 0.046(3) 0.002(2) 0.013(2) 0.001(2) C9 0.045(3) 0.052(3) 0.102(4) -0.009(3) 0.019(3) -0.004(2) C10 0.046(3) 0.076(4) 0.118(5) -0.005(3) 0.021(3) -0.003(3) C11 0.043(2) 0.053(3) 0.038(2) -0.0021(19) 0.011(2) -0.003(2) C12 0.049(3) 0.049(3) 0.049(3) -0.002(2) 0.018(2) -0.006(2) C13 0.045(2) 0.047(3) 0.040(2) 0.0018(19) 0.012(2) -0.002(2) C14 0.046(3) 0.046(3) 0.050(3) -0.002(2) 0.017(2) -0.006(2) C15 0.038(2) 0.047(3) 0.058(3) -0.004(2) 0.013(2) -0.007(2) C16 0.046(2) 0.048(3) 0.043(2) -0.001(2) 0.015(2) -0.003(2) C17 0.045(3) 0.046(3) 0.079(3) 0.000(2) 0.023(2) -0.003(2) C18 0.051(3) 0.048(3) 0.074(3) -0.001(2) 0.020(2) -0.005(2) C19 0.049(3) 0.058(3) 0.086(4) 0.016(3) 0.026(3) 0.010(2) C20 0.050(3) 0.046(3) 0.081(3) 0.005(2) 0.027(3) -0.003(2) C21 0.044(3) 0.042(3) 0.061(3) 0.000(2) 0.023(2) -0.006(2) C22 0.039(3) 0.052(3) 0.071(3) -0.005(2) 0.009(2) -0.010(2) C23 0.041(3) 0.052(3) 0.076(3) -0.001(2) 0.006(2) 0.003(2) C24 0.035(2) 0.049(3) 0.072(3) -0.002(2) 0.011(2) -0.004(2) C25 0.038(2) 0.047(3) 0.069(3) 0.006(2) 0.016(2) 0.003(2) C26 0.060(3) 0.055(3) 0.083(4) -0.011(3) 0.021(3) 0.000(3) C27 0.049(3) 0.057(3) 0.080(3) -0.006(3) 0.020(3) -0.004(2) C28 0.045(3) 0.056(3) 0.045(2) -0.010(2) 0.012(2) -0.005(2) C29 0.054(3) 0.057(3) 0.085(4) -0.017(3) 0.019(3) -0.005(2) C30 0.047(3) 0.072(4) 0.102(4) -0.031(3) 0.022(3) -0.012(3) C31 0.053(3) 0.051(3) 0.048(3) -0.001(2) 0.021(2) 0.003(2) C32 0.051(3) 0.059(3) 0.057(3) -0.003(2) 0.021(2) -0.005(2) C33 0.063(4) 0.060(4) 0.046(4) 0.000 0.026(3) 0.000 C34 0.063(4) 0.043(4) 0.058(4) 0.000 0.028(4) 0.000 C35 0.074(4) 0.057(3) 0.069(3) 0.008(3) 0.024(3) 0.001(3) C36 0.081(4) 0.060(4) 0.086(4) 0.015(3) 0.028(3) 0.013(3) C37 0.091(6) 0.058(5) 0.068(5) 0.000 0.044(5) 0.000 C38 0.127(7) 0.072(6) 0.096(6) 0.000 0.053(6) 0.000 N1 0.092(3) 0.062(3) 0.083(3) 0.003(2) 0.040(3) -0.005(2) N2 0.077(3) 0.052(3) 0.087(3) -0.002(2) 0.031(3) 0.004(2) N3 0.046(2) 0.072(3) 0.109(4) -0.012(3) 0.013(2) 0.020(2) N4 0.045(2) 0.050(2) 0.067(3) 0.0065(19) 0.0155(19) -0.0052(18) N5 0.051(2) 0.049(2) 0.051(2) -0.0025(17) 0.0206(18) -0.0111(18) N6 0.038(2) 0.049(2) 0.067(2) 0.0003(19) 0.0113(19) 0.0017(17) N7 0.049(2) 0.065(3) 0.074(3) -0.024(2) 0.013(2) -0.001(2) N8 0.043(3) 0.053(3) 0.047(3) 0.000 0.014(2) 0.000 _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 N1 1.926(5) . ? Cu1 N3 1.936(4) 8_465 ? Cu1 N4 2.031(3) 7_455 ? Cu2 C1 1.837(4) . ? Cu2 N2 1.916(4) . ? Cu2 N6 2.122(3) . ? Cu3 C2 1.845(4) . ? Cu3 C3 1.865(5) . ? Cu3 N7 2.068(4) . ? C1 N1 1.128(5) . ? C2 N2 1.135(5) . ? C3 N3 1.153(5) . ? C4 C5 1.497(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.378(6) . ? C5 C6 1.378(6) . ? C6 C7 1.377(6) . ? C6 H6 0.9300 . ? C7 C8 1.379(6) . ? C7 H7 0.9300 . ? C8 C9 1.384(5) . ? C8 C11 1.484(5) . ? C9 C10 1.362(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C15 1.394(5) . ? C11 C12 1.393(5) . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 N5 1.333(5) . ? C13 C16 1.491(5) . ? C14 N5 1.340(5) . ? C14 C15 1.378(5) . ? C14 C21 1.493(5) . ? C15 H15 0.9300 . ? C16 C20 1.376(5) . ? C16 C17 1.380(5) . ? C17 C18 1.368(5) . ? C17 H17 0.9300 . ? C18 N4 1.335(5) . ? C18 H18 0.9300 . ? C19 N4 1.330(5) . ? C19 C20 1.370(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.378(5) . ? C21 C25 1.384(5) . ? C22 C23 1.371(5) . ? C22 H22 0.9300 . ? C23 N6 1.333(5) . ? C23 H23 0.9300 . ? C24 N6 1.335(5) . ? C24 C25 1.365(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 N7 1.329(5) . ? C26 C27 1.374(6) . ? C26 H26 0.9300 . ? C27 C28 1.379(5) . ? C27 H27 0.9300 . ? C28 C29 1.372(5) . ? C28 C31 1.479(5) . ? C29 C30 1.380(6) . ? C29 H29 0.9300 . ? C30 N7 1.315(5) . ? C30 H30 0.9300 . ? C31 N8 1.341(4) . ? C31 C32 1.391(6) . ? C32 C33 1.393(5) . ? C32 H32 0.9300 . ? C33 C32 1.393(5) 2_655 ? C33 C34 1.477(8) . ? C34 C35 1.376(5) 2_655 ? C34 C35 1.376(5) . ? C35 C36 1.380(6) . ? C35 H35 0.9300 . ? C36 C37 1.371(5) . ? C36 H36 0.9300 . ? C37 C36 1.371(5) 2_655 ? C37 C38 1.507(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N3 Cu1 1.936(4) 8_566 ? N4 Cu1 2.031(3) 7_455 ? N8 C31 1.341(4) 2_655 ? 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 N1 Cu1 N3 131.70(15) . 8_465 ? N1 Cu1 N4 127.18(15) . 7_455 ? N3 Cu1 N4 101.09(15) 8_465 7_455 ? C1 Cu2 N2 152.22(17) . . ? C1 Cu2 N6 104.96(16) . . ? N2 Cu2 N6 102.82(14) . . ? C2 Cu3 C3 137.50(17) . . ? C2 Cu3 N7 116.45(16) . . ? C3 Cu3 N7 105.96(16) . . ? N1 C1 Cu2 173.3(4) . . ? N2 C2 Cu3 173.1(4) . . ? N3 C3 Cu3 178.5(5) . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 116.1(5) . . ? C10 C5 C4 122.9(5) . . ? C6 C5 C4 121.0(5) . . ? C5 C6 C7 122.2(5) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 121.2(4) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 116.4(4) . . ? C7 C8 C11 122.4(4) . . ? C9 C8 C11 121.2(4) . . ? C10 C9 C8 122.0(4) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C5 122.0(5) . . ? C9 C10 H10 119.0 . . ? C5 C10 H10 119.0 . . ? C15 C11 C12 115.4(4) . . ? C15 C11 C8 122.4(4) . . ? C12 C11 C8 122.2(4) . . ? C13 C12 C11 121.1(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? N5 C13 C12 122.1(4) . . ? N5 C13 C16 114.6(4) . . ? C12 C13 C16 123.3(4) . . ? N5 C14 C15 122.5(4) . . ? N5 C14 C21 115.1(4) . . ? C15 C14 C21 122.4(4) . . ? C14 C15 C11 120.9(4) . . ? C14 C15 H15 119.5 . . ? C11 C15 H15 119.5 . . ? C20 C16 C17 115.9(4) . . ? C20 C16 C13 119.8(4) . . ? C17 C16 C13 124.2(4) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? N4 C18 C17 123.7(4) . . ? N4 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N4 C19 C20 123.4(4) . . ? N4 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C16 120.7(4) . . ? C19 C20 H20 119.7 . . ? C16 C20 H20 119.7 . . ? C22 C21 C25 116.6(4) . . ? C22 C21 C14 120.9(4) . . ? C25 C21 C14 122.5(4) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? N6 C23 C22 123.2(4) . . ? N6 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? N6 C24 C25 123.8(4) . . ? N6 C24 H24 118.1 . . ? C25 C24 H24 118.1 . . ? C24 C25 C21 119.8(4) . . ? C24 C25 H25 120.1 . . ? C21 C25 H25 120.1 . . ? N7 C26 C27 124.0(4) . . ? N7 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 116.5(4) . . ? C29 C28 C31 122.7(4) . . ? C27 C28 C31 120.9(4) . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? N7 C30 C29 123.7(4) . . ? N7 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? N8 C31 C32 121.8(4) . . ? N8 C31 C28 115.2(4) . . ? C32 C31 C28 123.0(4) . . ? C31 C32 C33 121.0(4) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C32 115.7(6) . 2_655 ? C32 C33 C34 122.1(3) . . ? C32 C33 C34 122.1(3) 2_655 . ? C35 C34 C35 117.5(6) 2_655 . ? C35 C34 C33 121.2(3) 2_655 . ? C35 C34 C33 121.2(3) . . ? C36 C35 C34 120.8(5) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 122.2(5) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C36 C37 C36 116.6(7) . 2_655 ? C36 C37 C38 121.7(3) . . ? C36 C37 C38 121.7(3) 2_655 . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C1 N1 Cu1 173.2(4) . . ? C2 N2 Cu2 168.7(4) . . ? C3 N3 Cu1 171.1(4) . 8_566 ? C19 N4 C18 116.0(4) . . ? C19 N4 Cu1 123.6(3) . 7_455 ? C18 N4 Cu1 120.3(3) . 7_455 ? C13 N5 C14 118.1(4) . . ? C23 N6 C24 116.4(4) . . ? C23 N6 Cu2 121.4(3) . . ? C24 N6 Cu2 122.2(3) . . ? C30 N7 C26 116.2(4) . . ? C30 N7 Cu3 121.3(3) . . ? C26 N7 Cu3 121.3(3) . . ? C31 N8 C31 118.6(5) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu2 C1 N1 126(3) . . . . ? N6 Cu2 C1 N1 -53(4) . . . . ? C3 Cu3 C2 N2 -55(3) . . . . ? N7 Cu3 C2 N2 121(3) . . . . ? C2 Cu3 C3 N3 41(18) . . . . ? N7 Cu3 C3 N3 -135(18) . . . . ? C10 C5 C6 C7 1.5(8) . . . . ? C4 C5 C6 C7 -177.8(5) . . . . ? C5 C6 C7 C8 -0.7(8) . . . . ? C6 C7 C8 C9 -0.5(7) . . . . ? C6 C7 C8 C11 178.1(4) . . . . ? C7 C8 C9 C10 0.9(7) . . . . ? C11 C8 C9 C10 -177.7(4) . . . . ? C8 C9 C10 C5 -0.2(8) . . . . ? C6 C5 C10 C9 -1.0(8) . . . . ? C4 C5 C10 C9 178.2(5) . . . . ? C7 C8 C11 C15 -177.0(4) . . . . ? C9 C8 C11 C15 1.5(6) . . . . ? C7 C8 C11 C12 2.4(6) . . . . ? C9 C8 C11 C12 -179.1(4) . . . . ? C15 C11 C12 C13 0.7(5) . . . . ? C8 C11 C12 C13 -178.7(4) . . . . ? C11 C12 C13 N5 -0.8(6) . . . . ? C11 C12 C13 C16 178.8(3) . . . . ? N5 C14 C15 C11 -0.5(6) . . . . ? C21 C14 C15 C11 179.8(4) . . . . ? C12 C11 C15 C14 -0.1(5) . . . . ? C8 C11 C15 C14 179.3(4) . . . . ? N5 C13 C16 C20 0.4(5) . . . . ? C12 C13 C16 C20 -179.2(4) . . . . ? N5 C13 C16 C17 179.5(4) . . . . ? C12 C13 C16 C17 -0.2(6) . . . . ? C20 C16 C17 C18 0.1(6) . . . . ? C13 C16 C17 C18 -178.9(4) . . . . ? C16 C17 C18 N4 1.6(7) . . . . ? N4 C19 C20 C16 1.2(7) . . . . ? C17 C16 C20 C19 -1.4(6) . . . . ? C13 C16 C20 C19 177.7(4) . . . . ? N5 C14 C21 C22 -30.6(6) . . . . ? C15 C14 C21 C22 149.1(4) . . . . ? N5 C14 C21 C25 147.7(4) . . . . ? C15 C14 C21 C25 -32.6(6) . . . . ? C25 C21 C22 C23 0.9(6) . . . . ? C14 C21 C22 C23 179.3(4) . . . . ? C21 C22 C23 N6 -2.1(7) . . . . ? N6 C24 C25 C21 -0.9(6) . . . . ? C22 C21 C25 C24 0.5(6) . . . . ? C14 C21 C25 C24 -177.9(4) . . . . ? N7 C26 C27 C28 -0.9(7) . . . . ? C26 C27 C28 C29 -0.6(6) . . . . ? C26 C27 C28 C31 179.9(4) . . . . ? C27 C28 C29 C30 2.0(7) . . . . ? C31 C28 C29 C30 -178.5(4) . . . . ? C28 C29 C30 N7 -2.2(8) . . . . ? C29 C28 C31 N8 177.7(4) . . . . ? C27 C28 C31 N8 -2.8(5) . . . . ? C29 C28 C31 C32 -2.6(6) . . . . ? C27 C28 C31 C32 176.9(4) . . . . ? N8 C31 C32 C33 -1.8(6) . . . . ? C28 C31 C32 C33 178.5(3) . . . . ? C31 C32 C33 C32 0.9(3) . . . 2_655 ? C31 C32 C33 C34 -179.1(3) . . . . ? C32 C33 C34 C35 37.5(3) . . . 2_655 ? C32 C33 C34 C35 -142.5(3) 2_655 . . 2_655 ? C32 C33 C34 C35 -142.5(3) . . . . ? C32 C33 C34 C35 37.5(3) 2_655 . . . ? C35 C34 C35 C36 -0.2(3) 2_655 . . . ? C33 C34 C35 C36 179.8(3) . . . . ? C34 C35 C36 C37 0.5(6) . . . . ? C35 C36 C37 C36 -0.2(3) . . . 2_655 ? C35 C36 C37 C38 179.8(3) . . . . ? Cu2 C1 N1 Cu1 -69(6) . . . . ? N3 Cu1 N1 C1 -5(4) 8_465 . . . ? N4 Cu1 N1 C1 173(3) 7_455 . . . ? Cu3 C2 N2 Cu2 -46(5) . . . . ? C1 Cu2 N2 C2 147.0(19) . . . . ? N6 Cu2 N2 C2 -34(2) . . . . ? Cu3 C3 N3 Cu1 -85(19) . . . 8_566 ? C20 C19 N4 C18 0.5(6) . . . . ? C20 C19 N4 Cu1 176.5(3) . . . 7_455 ? C17 C18 N4 C19 -1.8(6) . . . . ? C17 C18 N4 Cu1 -178.0(3) . . . 7_455 ? C12 C13 N5 C14 0.3(6) . . . . ? C16 C13 N5 C14 -179.4(3) . . . . ? C15 C14 N5 C13 0.3(6) . . . . ? C21 C14 N5 C13 -179.9(3) . . . . ? C22 C23 N6 C24 1.8(6) . . . . ? C22 C23 N6 Cu2 -175.9(3) . . . . ? C25 C24 N6 C23 -0.3(6) . . . . ? C25 C24 N6 Cu2 177.4(3) . . . . ? C1 Cu2 N6 C23 1.3(4) . . . . ? N2 Cu2 N6 C23 -178.0(3) . . . . ? C1 Cu2 N6 C24 -176.2(3) . . . . ? N2 Cu2 N6 C24 4.5(3) . . . . ? C29 C30 N7 C26 0.8(7) . . . . ? C29 C30 N7 Cu3 -167.1(4) . . . . ? C27 C26 N7 C30 0.8(7) . . . . ? C27 C26 N7 Cu3 168.7(4) . . . . ? C2 Cu3 N7 C30 -59.9(4) . . . . ? C3 Cu3 N7 C30 117.2(4) . . . . ? C2 Cu3 N7 C26 132.8(4) . . . . ? C3 Cu3 N7 C26 -50.1(4) . . . . ? C32 C31 N8 C31 0.9(3) . . . 2_655 ? C28 C31 N8 C31 -179.4(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.434 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.066 #================================================ data_2 _database_code_depnum_ccdc_archive 'CCDC 826228' #TrackingRef '- Compounds 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H57 Cu6 N15' _chemical_formula_weight 1549.59 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' 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 C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.7172(10) _cell_length_b 14.5191(7) _cell_length_c 21.7987(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.7880(10) _cell_angle_gamma 90.00 _cell_volume 6806.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.784 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17510 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5983 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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. Both the pedant ethyl groups of the two assymmetric ligands in the unict cell are disordered over two postions, therefore they are refined as occupying on two postions and the DFIX, DELU, etc. are used for restraining the diordered ethyl groups. Addtional, the pendant phenyl group is also disordered, and the DFIX. DELU restrains are used in the refinements. ; _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^)+(0.0623P)^2^+1.8471P] 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 5983 _refine_ls_number_parameters 460 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.008 _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 0.201473(18) 0.33351(3) 1.05769(2) 0.05959(16) Uani 1 1 d . . . Cu2 Cu -0.005854(18) 0.40232(3) 0.90954(2) 0.05599(16) Uani 1 1 d . . . Cu3 Cu -0.215331(19) 0.34995(3) 0.75888(2) 0.06162(17) Uani 1 1 d . . . N1 N 0.22847(14) 0.2583(2) 1.13485(18) 0.0761(10) Uani 1 1 d . . . N2 N 0.07629(14) 0.3691(2) 0.95944(15) 0.0628(8) Uani 1 1 d . . . N3 N -0.13543(15) 0.3666(2) 0.82208(16) 0.0688(9) Uani 1 1 d . . . N4 N -0.28835(12) 0.4282(2) 0.76918(14) 0.0565(8) Uani 1 1 d . . . N5 N -0.5000 0.5480(3) 0.7500 0.0456(9) Uani 1 2 d S . . N6 N 0.28273(12) 0.3961(2) 1.05662(14) 0.0568(8) Uani 1 1 d . . . N7 N 0.45813(12) 0.61395(19) 1.07235(13) 0.0474(7) Uani 1 1 d . . . N8 N 0.50817(11) 0.9517(2) 1.08012(13) 0.0528(7) Uani 1 1 d . . . C1 C 0.24927(15) 0.2184(3) 1.18275(18) 0.0580(10) Uani 1 1 d . . . C2 C 0.12533(14) 0.3576(2) 0.99464(16) 0.0477(8) Uani 1 1 d . . . C3 C -0.08644(14) 0.3740(2) 0.85781(16) 0.0433(8) Uani 1 1 d . . . C4 C -0.34574(15) 0.3930(2) 0.75405(18) 0.0584(10) Uani 1 1 d . . . H4 H -0.3507 0.3301 0.7462 0.070 Uiso 1 1 calc R . . C5 C -0.39761(15) 0.4447(2) 0.74941(17) 0.0547(9) Uani 1 1 d . . . H5 H -0.4363 0.4163 0.7391 0.066 Uiso 1 1 calc R . . C6 C -0.39252(14) 0.5383(2) 0.76004(15) 0.0455(8) Uani 1 1 d . . . C7 C -0.33311(15) 0.5753(3) 0.77521(17) 0.0589(10) Uani 1 1 d . . . H7 H -0.3269 0.6383 0.7821 0.071 Uiso 1 1 calc R . . C8 C -0.28341(16) 0.5181(3) 0.77997(19) 0.0650(11) Uani 1 1 d . . . H8 H -0.2440 0.5442 0.7915 0.078 Uiso 1 1 calc R . . C9 C -0.44804(14) 0.5955(2) 0.75454(15) 0.0464(8) Uani 1 1 d . . . C10 C -0.44670(16) 0.6909(2) 0.75360(16) 0.0529(9) Uani 1 1 d . . . H10 H -0.4102 0.7216 0.7554 0.064 Uiso 1 1 calc R . . C11 C -0.5000 0.7409(3) 0.7500 0.0485(11) Uani 1 2 d S . . C12 C -0.5000 0.8425(4) 0.7500 0.0606(14) Uani 1 2 d S . . C13 C -0.5500(2) 0.8925(3) 0.7099(2) 0.0787(13) Uani 1 1 d . . . H13 H -0.5818 0.8523 0.6838 0.094 Uiso 1 1 d R . . C14 C -0.5636(4) 0.9809(8) 0.6997(6) 0.056(3) Uani 0.50 1 d P . . H14A H -0.6017 1.0035 0.6696 0.067 Uiso 0.50 1 d PR . . C15 C -0.5153(4) 1.0375(6) 0.7384(5) 0.050(3) Uani 0.50 1 d P . . C16 C -0.5245(4) 1.1401(6) 0.7326(4) 0.064(2) Uani 0.50 1 d P . . H16A H -0.5596 1.1567 0.7456 0.077 Uiso 0.50 1 d PR . . H16B H -0.5338 1.1574 0.6879 0.077 Uiso 0.50 1 d PR . . C17 C -0.4697(4) 1.1988(6) 0.7709(5) 0.081(3) Uani 0.50 1 d P . . H17A H -0.4788 1.2633 0.7646 0.122 Uiso 0.50 1 d PR . . H17B H -0.4605 1.1837 0.8158 0.122 Uiso 0.50 1 d PR . . H17C H -0.4344 1.1844 0.7575 0.122 Uiso 0.50 1 d PR . . C14' C -0.4646(5) 0.9944(9) 0.7804(6) 0.055(3) Uani 0.50 1 d P . . H14B H -0.4336 1.0346 0.8076 0.066 Uiso 0.50 1 d PR . . C18 C 0.33419(16) 0.3463(3) 1.06706(19) 0.0610(10) Uani 1 1 d . . . H18 H 0.3311 0.2827 1.0701 0.073 Uiso 1 1 calc R . . C19 C 0.39154(16) 0.3830(3) 1.07364(18) 0.0583(10) Uani 1 1 d . . . H19 H 0.4258 0.3445 1.0810 0.070 Uiso 1 1 calc R . . C20 C 0.39850(14) 0.4768(2) 1.06932(15) 0.0472(8) Uani 1 1 d . . . C21 C 0.34548(16) 0.5290(3) 1.0590(2) 0.0721(12) Uani 1 1 d . . . H21 H 0.3473 0.5928 1.0562 0.087 Uiso 1 1 calc R . . C22 C 0.28963(17) 0.4861(3) 1.0528(2) 0.0765(13) Uani 1 1 d . . . H22 H 0.2546 0.5230 1.0456 0.092 Uiso 1 1 calc R . . C23 C 0.45934(14) 0.5219(2) 1.07581(15) 0.0456(8) Uani 1 1 d . . . C24 C 0.51281(13) 0.4710(2) 1.08416(14) 0.0485(8) Uani 1 1 d . . . H24 H 0.5116 0.4073 1.0877 0.058 Uiso 1 1 calc R . . C25 C 0.56862(14) 0.5142(2) 1.08735(15) 0.0467(8) Uani 1 1 d . . . C26 C 0.56643(15) 0.6089(2) 1.08339(16) 0.0495(8) Uani 1 1 d . . . H26 H 0.6021 0.6415 1.0850 0.059 Uiso 1 1 calc R . . C27 C 0.51167(14) 0.6565(2) 1.07695(16) 0.0487(8) Uani 1 1 d . . . C28 C 0.51065(14) 0.7589(2) 1.07659(16) 0.0478(8) Uani 1 1 d . . . C29 C 0.45876(15) 0.8083(2) 1.04080(17) 0.0569(9) Uani 1 1 d . . . H29 H 0.4235 0.7777 1.0151 0.068 Uiso 1 1 calc R . . C30 C 0.45972(15) 0.9027(2) 1.04353(17) 0.0581(9) Uani 1 1 d . . . H30 H 0.4246 0.9344 1.0185 0.070 Uiso 1 1 calc R . . C31 C 0.55823(15) 0.9036(2) 1.11388(17) 0.0547(9) Uani 1 1 d . . . H31 H 0.5929 0.9359 1.1392 0.066 Uiso 1 1 calc R . . C32 C 0.56135(15) 0.8096(2) 1.11326(17) 0.0543(9) Uani 1 1 d . . . H32 H 0.5976 0.7797 1.1375 0.065 Uiso 1 1 calc R . . C33 C 0.62694(15) 0.4621(2) 1.09707(16) 0.0497(8) Uani 1 1 d . A . C34 C 0.62855(17) 0.3675(3) 1.0962(2) 0.0668(11) Uani 1 1 d . . . H34 H 0.5917 0.3349 1.0887 0.080 Uiso 1 1 calc R . . C35 C 0.68308(19) 0.3197(3) 1.1061(2) 0.0811(13) Uani 1 1 d . A . H35 H 0.6824 0.2556 1.1048 0.097 Uiso 1 1 calc R . . C36 C 0.73865(19) 0.3658(3) 1.1180(2) 0.0832(13) Uani 1 1 d . . . C37 C 0.73700(18) 0.4604(3) 1.1177(2) 0.0890(15) Uani 1 1 d . A . H37 H 0.7738 0.4930 1.1248 0.107 Uiso 1 1 calc R . . C38 C 0.68276(16) 0.5080(3) 1.1075(2) 0.0742(12) Uani 1 1 d . . . H38 H 0.6833 0.5721 1.1074 0.089 Uiso 1 1 calc R A . C39 C 0.8003(2) 0.3146(4) 1.1310(3) 0.1179(19) Uani 0.60 1 d PU A 1 H39A H 0.7961 0.2525 1.1441 0.141 Uiso 0.60 1 d PR A 1 H39B H 0.8318 0.3447 1.1655 0.141 Uiso 0.60 1 d PR A 1 C40 C 0.8195(5) 0.3153(7) 1.0737(5) 0.118(3) Uani 0.60 1 d PU A 1 H40A H 0.8583 0.2836 1.0818 0.177 Uiso 0.60 1 d PR A 1 H40B H 0.7879 0.2848 1.0396 0.177 Uiso 0.60 1 d PR A 1 H40C H 0.8238 0.3777 1.0611 0.177 Uiso 0.60 1 d PR A 1 C39' C 0.8003(2) 0.3146(4) 1.1310(3) 0.1179(19) Uani 0.40 1 d P A 2 H39C H 0.8091 0.2862 1.1754 0.141 Uiso 0.40 1 d PR A 2 H39D H 0.8327 0.3621 1.1400 0.141 Uiso 0.40 1 d PR A 2 C40' C 0.8107(7) 0.2563(11) 1.0988(8) 0.118(3) Uani 0.40 1 d PU A 2 H40D H 0.8525 0.2344 1.1179 0.177 Uiso 0.40 1 d PR A 2 H40E H 0.7822 0.2059 1.0934 0.177 Uiso 0.40 1 d PR A 2 H40F H 0.8062 0.2833 1.0573 0.177 Uiso 0.40 1 d PR A 2 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 0.0377(2) 0.0655(3) 0.0669(3) 0.0036(2) 0.0047(2) -0.0004(2) Cu2 0.0415(3) 0.0562(3) 0.0606(3) -0.0005(2) 0.0031(2) 0.00321(18) Cu3 0.0416(3) 0.0633(3) 0.0705(3) -0.0064(2) 0.0048(2) 0.0024(2) N1 0.0479(18) 0.072(2) 0.098(3) 0.008(2) 0.0086(18) -0.0213(16) N2 0.0563(19) 0.060(2) 0.068(2) 0.0024(16) 0.0155(17) 0.0061(15) N3 0.071(2) 0.061(2) 0.079(2) -0.0079(18) 0.0299(19) 0.0024(17) N4 0.0403(16) 0.061(2) 0.0634(19) -0.0164(16) 0.0096(14) 0.0012(14) N5 0.039(2) 0.043(2) 0.054(2) 0.000 0.0135(18) 0.000 N6 0.0395(16) 0.064(2) 0.0643(19) 0.0116(16) 0.0128(14) -0.0008(14) N7 0.0456(16) 0.0429(17) 0.0543(17) -0.0010(13) 0.0169(13) -0.0011(12) N8 0.0430(16) 0.0478(18) 0.0614(18) -0.0018(14) 0.0083(14) 0.0013(12) C1 0.0403(19) 0.053(2) 0.064(2) 0.0166(19) -0.0059(17) -0.0119(16) C2 0.0352(17) 0.051(2) 0.051(2) 0.0064(16) 0.0057(15) 0.0005(15) C3 0.0255(15) 0.046(2) 0.0490(19) -0.0072(15) -0.0006(14) -0.0021(13) C4 0.047(2) 0.046(2) 0.075(3) -0.0076(19) 0.0100(18) -0.0020(16) C5 0.0403(19) 0.051(2) 0.071(2) -0.0026(18) 0.0153(17) -0.0045(16) C6 0.0410(18) 0.048(2) 0.0466(19) -0.0036(15) 0.0132(15) -0.0030(14) C7 0.045(2) 0.052(2) 0.081(3) -0.0216(19) 0.0209(18) -0.0105(16) C8 0.042(2) 0.068(3) 0.083(3) -0.024(2) 0.0172(18) -0.0109(18) C9 0.0442(18) 0.047(2) 0.050(2) -0.0022(16) 0.0173(15) 0.0001(15) C10 0.053(2) 0.047(2) 0.063(2) -0.0011(17) 0.0235(17) -0.0074(16) C11 0.058(3) 0.040(3) 0.051(3) 0.000 0.024(2) 0.000 C12 0.083(4) 0.048(3) 0.064(3) 0.000 0.042(3) 0.000 C13 0.110(4) 0.052(3) 0.091(3) 0.015(2) 0.055(3) 0.016(2) C14 0.043(7) 0.052(6) 0.064(8) 0.006(5) 0.006(6) -0.003(6) C15 0.038(10) 0.061(6) 0.047(9) -0.009(5) 0.008(7) -0.008(4) C16 0.074(6) 0.052(5) 0.063(6) 0.009(5) 0.017(4) -0.004(4) C17 0.089(6) 0.055(6) 0.095(7) -0.013(6) 0.024(5) -0.015(5) C14' 0.035(8) 0.066(8) 0.060(10) -0.012(7) 0.007(7) -0.002(7) C18 0.053(2) 0.051(2) 0.081(3) -0.0047(19) 0.024(2) -0.0089(17) C19 0.045(2) 0.052(2) 0.079(3) -0.0025(19) 0.0211(18) -0.0014(16) C20 0.0428(18) 0.051(2) 0.048(2) 0.0032(16) 0.0152(15) -0.0015(15) C21 0.051(2) 0.054(2) 0.114(3) 0.025(2) 0.031(2) 0.0052(18) C22 0.045(2) 0.065(3) 0.119(4) 0.036(3) 0.027(2) 0.0114(19) C23 0.0431(18) 0.049(2) 0.0448(19) -0.0016(15) 0.0141(15) -0.0013(15) C24 0.0448(19) 0.045(2) 0.054(2) -0.0027(15) 0.0130(16) -0.0018(14) C25 0.0450(18) 0.050(2) 0.0453(19) -0.0019(16) 0.0142(15) 0.0006(15) C26 0.0431(19) 0.045(2) 0.061(2) -0.0044(17) 0.0169(16) -0.0062(15) C27 0.045(2) 0.049(2) 0.051(2) -0.0016(16) 0.0150(16) -0.0008(15) C28 0.0463(19) 0.046(2) 0.053(2) -0.0005(16) 0.0193(16) -0.0018(15) C29 0.0446(19) 0.052(2) 0.066(2) -0.0053(18) 0.0058(17) -0.0024(16) C30 0.045(2) 0.054(2) 0.065(2) -0.0012(18) 0.0034(17) 0.0060(16) C31 0.0419(19) 0.053(2) 0.062(2) -0.0002(18) 0.0061(16) -0.0036(16) C32 0.0428(19) 0.047(2) 0.069(2) 0.0063(18) 0.0116(17) 0.0038(15) C33 0.0431(18) 0.050(2) 0.054(2) -0.0040(16) 0.0128(15) 0.0010(15) C34 0.052(2) 0.057(3) 0.094(3) 0.005(2) 0.028(2) 0.0047(18) C35 0.067(3) 0.059(3) 0.120(4) 0.014(3) 0.033(3) 0.014(2) C36 0.053(2) 0.084(3) 0.103(4) 0.010(3) 0.012(2) 0.018(2) C37 0.039(2) 0.086(4) 0.133(4) -0.016(3) 0.016(2) -0.003(2) C38 0.045(2) 0.060(3) 0.109(3) -0.014(2) 0.013(2) -0.0030(18) C39 0.072(3) 0.115(4) 0.162(5) 0.010(4) 0.031(3) 0.036(3) C40 0.100(4) 0.119(6) 0.146(6) 0.007(5) 0.056(4) 0.019(5) C39' 0.072(3) 0.115(4) 0.162(5) 0.010(4) 0.031(3) 0.036(3) C40' 0.100(4) 0.119(6) 0.146(6) 0.007(5) 0.056(4) 0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C2 1.863(3) . ? Cu1 N1 1.933(4) . ? Cu1 N6 2.064(3) . ? Cu2 C3 1.861(3) . ? Cu2 N2 1.895(3) . ? Cu2 N8 2.133(3) 7_567 ? Cu3 C1 1.877(4) 8_455 ? Cu3 N3 1.908(3) . ? Cu3 N4 2.082(3) . ? N1 C1 1.154(5) . ? N2 C2 1.143(4) . ? N3 C3 1.139(4) . ? N4 C8 1.325(5) . ? N4 C4 1.339(4) . ? N5 C9 1.343(4) . ? N5 C9 1.343(4) 2_456 ? N6 C22 1.322(5) . ? N6 C18 1.330(4) . ? N7 C23 1.338(4) . ? N7 C27 1.339(4) . ? N8 C31 1.336(4) . ? N8 C30 1.338(4) . ? N8 Cu2 2.133(3) 7_567 ? C1 Cu3 1.877(4) 8_556 ? C4 C5 1.372(5) . ? C4 H4 0.9300 . ? C5 C6 1.377(4) . ? C5 H5 0.9300 . ? C6 C7 1.390(4) . ? C6 C9 1.482(4) . ? C7 C8 1.379(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.387(5) . ? C10 C11 1.392(4) . ? C10 H10 0.9300 . ? C11 C10 1.392(4) 2_456 ? C11 C12 1.474(7) . ? C12 C13 1.393(5) . ? C12 C13 1.393(5) 2_456 ? C13 C14 1.322(13) . ? C13 C14' 1.516(14) 2_456 ? C13 H13 0.9599 . ? C14 C14' 0.677(9) 2_456 ? C14 C15 1.413(11) . ? C14 H14A 0.9599 . ? C15 C15 0.717(15) 2_456 ? C15 C14' 0.805(11) 2_456 ? C15 C14' 1.371(13) . ? C15 C16 1.504(12) . ? C16 C17 0.862(10) 2_456 ? C16 C16 1.127(16) 2_456 ? C16 C17 1.518(9) . ? C16 H16A 0.9599 . ? C16 H16B 0.9600 . ? C17 C16 0.862(10) 2_456 ? C17 C17 1.385(17) 2_456 ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9599 . ? C14' C14 0.677(9) 2_456 ? C14' C15 0.805(11) 2_456 ? C14' C13 1.516(14) 2_456 ? C14' H14B 0.9600 . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.378(5) . ? C19 H19 0.9300 . ? C20 C21 1.379(5) . ? C20 C23 1.494(4) . ? C21 C22 1.381(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.383(4) . ? C24 C25 1.396(4) . ? C24 H24 0.9300 . ? C25 C26 1.378(5) . ? C25 C33 1.480(4) . ? C26 C27 1.390(4) . ? C26 H26 0.9300 . ? C27 C28 1.486(5) . ? C28 C32 1.384(4) . ? C28 C29 1.386(4) . ? C29 C30 1.371(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.367(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.374(5) . ? C33 C38 1.385(5) . ? C34 C35 1.375(5) . ? C34 H34 0.9300 . ? C35 C36 1.378(6) . ? C35 H35 0.9300 . ? C36 C37 1.375(6) . ? C36 C39 1.528(6) . ? C37 C38 1.367(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.450(10) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 1.0102 . ? C39 H39D 0.9808 . ? C40 H40A 0.9600 . ? C40 H40B 0.9601 . ? C40 H40C 0.9600 . ? C40 H40F 0.6046 . ? C40' H39A 1.1399 . ? C40' H40B 1.2943 . ? C40' H40D 0.9599 . ? C40' H40E 0.9600 . ? C40' H40F 0.9602 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Cu1 N1 135.01(14) . . ? C2 Cu1 N6 122.01(13) . . ? N1 Cu1 N6 102.97(12) . . ? C3 Cu2 N2 152.41(15) . . ? C3 Cu2 N8 103.35(12) . 7_567 ? N2 Cu2 N8 104.20(12) . 7_567 ? C1 Cu3 N3 137.93(14) 8_455 . ? C1 Cu3 N4 104.73(12) 8_455 . ? N3 Cu3 N4 117.31(12) . . ? C1 N1 Cu1 173.8(3) . . ? C2 N2 Cu2 171.5(3) . . ? C3 N3 Cu3 176.4(3) . . ? C8 N4 C4 116.1(3) . . ? C8 N4 Cu3 122.1(2) . . ? C4 N4 Cu3 120.8(2) . . ? C9 N5 C9 118.3(4) . 2_456 ? C22 N6 C18 115.6(3) . . ? C22 N6 Cu1 124.1(2) . . ? C18 N6 Cu1 119.9(3) . . ? C23 N7 C27 117.1(3) . . ? C31 N8 C30 116.2(3) . . ? C31 N8 Cu2 120.5(2) . 7_567 ? C30 N8 Cu2 123.3(2) . 7_567 ? N1 C1 Cu3 177.6(4) . 8_556 ? N2 C2 Cu1 174.2(3) . . ? N3 C3 Cu2 171.4(3) . . ? N4 C4 C5 123.7(3) . . ? N4 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 116.4(3) . . ? C5 C6 C9 121.1(3) . . ? C7 C6 C9 122.5(3) . . ? C8 C7 C6 119.6(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? N4 C8 C7 124.1(3) . . ? N4 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? N5 C9 C10 122.3(3) . . ? N5 C9 C6 115.1(3) . . ? C10 C9 C6 122.6(3) . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C10 117.2(5) 2_456 . ? C10 C11 C12 121.4(2) 2_456 . ? C10 C11 C12 121.4(2) . . ? C13 C12 C13 117.2(6) . 2_456 ? C13 C12 C11 121.4(3) . . ? C13 C12 C11 121.4(3) 2_456 . ? C14 C13 C12 135.3(6) . . ? C12 C13 C14' 108.9(6) . 2_456 ? C14 C13 H13 113.5 . . ? C12 C13 H13 111.2 . . ? C14' C13 H13 139.9 2_456 . ? C14' C14 C13 93(2) 2_456 . ? C13 C14 C15 111.7(8) . . ? C13 C14 C15 99.9(6) . 2_456 ? C14' C14 H14A 143.0 2_456 . ? C13 C14 H14A 123.9 . . ? C15 C14 H14A 124.4 . . ? C15 C14 H14A 136.2 2_456 . ? C15 C15 C14' 128.4(13) 2_456 2_456 ? C14' C15 C14' 101.6(19) 2_456 . ? C15 C15 C14 144.3(6) 2_456 . ? C14' C15 C14 117.2(9) . . ? C15 C15 C16 97.8(4) 2_456 . ? C14' C15 C16 133.5(14) 2_456 . ? C14' C15 C16 125.0(8) . . ? C14 C15 C16 117.8(8) . . ? C15 C15 C16 58.3(4) 2_456 2_456 ? C14' C15 C16 171.1(15) 2_456 2_456 ? C14' C15 C16 85.5(7) . 2_456 ? C14 C15 C16 157.2(9) . 2_456 ? C14' C15 C14 104.8(13) 2_456 2_456 ? C14 C15 C14 120.6(10) . 2_456 ? C16 C15 C14 121.6(6) . 2_456 ? C16 C15 C14 82.1(5) 2_456 2_456 ? C17 C16 C16 98.6(9) 2_456 2_456 ? C17 C16 C15 179.1(14) 2_456 . ? C16 C16 C15 82.1(4) 2_456 . ? C17 C16 C17 64.4(11) 2_456 . ? C15 C16 C17 116.3(6) . . ? C17 C16 C15 156.8(12) 2_456 2_456 ? C16 C16 C15 58.3(4) 2_456 2_456 ? C17 C16 C15 92.4(5) . 2_456 ? C17 C16 H16A 70.0 2_456 . ? C16 C16 H16A 122.3 2_456 . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 108.0 . . ? C15 C16 H16A 119.2 2_456 . ? C17 C16 H16B 71.1 2_456 . ? C16 C16 H16B 122.1 2_456 . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 106.6 . . ? C15 C16 H16B 120.6 2_456 . ? H16A C16 H16B 107.5 . . ? C16 C17 C17 81.4(9) 2_456 2_456 ? C16 C17 C16 47.3(9) 2_456 . ? C16 C17 H17A 158.8 2_456 . ? C17 C17 H17A 77.4 2_456 . ? C16 C17 H17A 111.6 . . ? C16 C17 H17B 80.8 2_456 . ? C17 C17 H17B 120.9 2_456 . ? C16 C17 H17B 107.7 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 83.0 2_456 . ? C17 C17 H17C 123.5 2_456 . ? C16 C17 H17C 109.1 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C14' C15 145(3) 2_456 2_456 ? C14 C14' C15 168(3) 2_456 . ? C14 C14' C13 60.6(18) 2_456 2_456 ? C15 C14' C13 153.3(16) 2_456 2_456 ? C15 C14' C13 129.7(11) . 2_456 ? C14 C14' C14' 162(2) 2_456 2_456 ? C15 C14' C14' 51.2(13) 2_456 2_456 ? C13 C14' C14' 102.4(4) 2_456 2_456 ? C14 C14' H14B 54.9 2_456 . ? C15 C14' H14B 91.3 2_456 . ? C15 C14' H14B 115.2 . . ? C13 C14' H14B 115.1 2_456 . ? C14' C14' H14B 142.5 2_456 . ? N6 C18 C19 124.0(4) . . ? N6 C18 H18 118.0 . . ? C19 C18 H18 118.0 . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 116.2(3) . . ? C19 C20 C23 123.3(3) . . ? C21 C20 C23 120.5(3) . . ? C20 C21 C22 119.7(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? N6 C22 C21 124.3(4) . . ? N6 C22 H22 117.8 . . ? C21 C22 H22 117.8 . . ? N7 C23 C24 122.8(3) . . ? N7 C23 C20 115.5(3) . . ? C24 C23 C20 121.7(3) . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 115.5(3) . . ? C26 C25 C33 122.1(3) . . ? C24 C25 C33 122.3(3) . . ? C25 C26 C27 121.0(3) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? N7 C27 C26 122.7(3) . . ? N7 C27 C28 116.7(3) . . ? C26 C27 C28 120.6(3) . . ? C32 C28 C29 116.6(3) . . ? C32 C28 C27 121.4(3) . . ? C29 C28 C27 122.0(3) . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N8 C30 C29 123.8(3) . . ? N8 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? N8 C31 C32 123.7(3) . . ? N8 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C31 C32 C28 120.1(3) . . ? C31 C32 H32 120.0 . . ? C28 C32 H32 120.0 . . ? C34 C33 C38 117.1(3) . . ? C34 C33 C25 122.4(3) . . ? C38 C33 C25 120.5(3) . . ? C33 C34 C35 122.0(4) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 117.6(4) . . ? C37 C36 C39 120.6(4) . . ? C35 C36 C39 121.9(5) . . ? C38 C37 C36 121.9(4) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C33 120.9(4) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? C40 C39 C36 110.4(6) . . ? C40 C39 H39A 110.4 . . ? C36 C39 H39A 109.9 . . ? C40 C39 H39B 108.4 . . ? C36 C39 H39B 109.4 . . ? H39A C39 H39B 108.4 . . ? C40 C39 H39C 143.7 . . ? C36 C39 H39C 105.3 . . ? H39A C39 H39C 48.7 . . ? H39B C39 H39C 64.5 . . ? C40 C39 H39D 75.7 . . ? C36 C39 H39D 106.2 . . ? H39A C39 H39D 137.8 . . ? H39C C39 H39D 101.0 . . ? C39 C40 H40A 110.5 . . ? C39 C40 H40B 107.9 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.9 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? H40A C40 H39D 98.6 . . ? H40B C40 H39D 143.5 . . ? H40C C40 H39D 81.1 . . ? C39 C40 H40D 71.3 . . ? H40B C40 H40D 102.8 . . ? H40C C40 H40D 144.9 . . ? H39D C40 H40D 80.9 . . ? C39 C40 H40F 105.9 . . ? H40A C40 H40F 89.5 . . ? H40C C40 H40F 129.3 . . ? H39D C40 H40F 143.7 . . ? H40D C40 H40F 80.3 . . ? H39A C40' H40A 139.0 . . ? H39A C40' H40B 138.2 . . ? H40A C40' H40B 74.0 . . ? H39A C40' H40D 97.5 . . ? H40A C40' H40D 55.4 . . ? H40B C40' H40D 124.1 . . ? H39A C40' H40E 72.3 . . ? H40A C40' H40E 141.3 . . ? H40B C40' H40E 94.8 . . ? H40D C40' H40E 109.5 . . ? H39A C40' H40F 149.8 . . ? H40A C40' H40F 57.2 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.386 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.077 #================================================ data_3 _database_code_depnum_ccdc_archive 'CCDC 826229' #TrackingRef '- Compounds 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H63 Cu6 N15' _chemical_formula_weight 1591.68 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 23.568(3) _cell_length_b 14.2616(16) _cell_length_c 24.342(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.922(2) _cell_angle_gamma 90.00 _cell_volume 7161.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 1.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36875 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12592 _reflns_number_gt 6997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0996P)^2^+1.1282P] 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 12592 _refine_ls_number_parameters 902 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.45673(4) 0.55526(5) 0.22711(4) 0.0605(2) Uani 1 1 d . . . Cu2 Cu 0.40091(4) 0.52790(5) 0.39781(4) 0.0615(2) Uani 1 1 d . . . Cu3 Cu 0.37406(4) 0.72728(5) 0.54838(4) 0.0587(2) Uani 1 1 d . . . Cu4 Cu 0.08657(4) -0.03398(5) 0.59334(4) 0.0630(2) Uani 1 1 d . . . Cu5 Cu 0.02250(4) -0.05460(5) 0.75869(4) 0.0589(2) Uani 1 1 d . . . Cu6 Cu 0.10768(4) -0.27550(5) 0.93653(4) 0.0634(2) Uani 1 1 d . . . C1 C 0.4224(3) 0.5357(3) 0.3329(3) 0.0487(14) Uani 1 1 d . . . C2 C 0.3825(3) 0.6533(4) 0.4895(3) 0.0461(14) Uani 1 1 d . . . C3 C 0.4292(3) 0.8709(4) 0.6545(3) 0.0574(16) Uani 1 1 d . . . C4 C 0.0661(3) -0.0441(3) 0.6590(3) 0.0484(14) Uani 1 1 d . . . C5 C 0.0494(3) -0.1347(4) 0.8280(3) 0.0528(15) Uani 1 1 d . . . C6 C 0.0996(3) -0.3437(4) 0.9980(3) 0.0516(15) Uani 1 1 d . . . C7 C 0.2678(3) 0.5883(4) 0.5251(3) 0.0665(17) Uani 1 1 d . . . H7 H 0.2859 0.5563 0.5040 0.080 Uiso 1 1 calc R . . C8 C 0.2181(3) 0.5464(4) 0.5299(3) 0.0655(18) Uani 1 1 d . . . H8 H 0.2040 0.4870 0.5132 0.079 Uiso 1 1 calc R . . C9 C 0.1890(3) 0.5921(4) 0.5594(3) 0.0489(13) Uani 1 1 d . . . C10 C 0.2129(3) 0.6798(4) 0.5840(3) 0.0529(14) Uani 1 1 d . . . H10 H 0.1950 0.7140 0.6044 0.063 Uiso 1 1 calc R . . C11 C 0.2641(3) 0.7160(4) 0.5779(3) 0.0556(15) Uani 1 1 d . . . H11 H 0.2800 0.7746 0.5951 0.067 Uiso 1 1 calc R . . C12 C 0.1354(3) 0.5477(4) 0.5669(3) 0.0494(13) Uani 1 1 d . . . C13 C 0.0893(2) 0.6020(4) 0.5714(2) 0.0514(14) Uani 1 1 d . . . H13 H 0.0904 0.6669 0.5689 0.062 Uiso 1 1 calc R . . C14 C 0.0413(2) 0.5591(4) 0.5797(2) 0.0458(13) Uani 1 1 d . . . C15 C 0.0418(2) 0.4619(3) 0.5810(2) 0.0475(13) Uani 1 1 d . . . H15 H 0.0098 0.4298 0.5853 0.057 Uiso 1 1 calc R . . C16 C 0.0896(2) 0.4122(3) 0.5759(2) 0.0458(13) Uani 1 1 d . . . C17 C -0.0078(3) 0.6123(4) 0.5892(3) 0.0495(13) Uani 1 1 d . . . C18 C -0.0010(3) 0.7074(4) 0.6025(3) 0.0672(17) Uani 1 1 d . . . H18 H 0.0330 0.7403 0.6023 0.081 Uiso 1 1 calc R . . C19 C -0.0441(3) 0.7536(4) 0.6161(3) 0.078(2) Uani 1 1 d . . . H19 H -0.0387 0.8175 0.6249 0.094 Uiso 1 1 calc R . . C20 C -0.0957(3) 0.7068(5) 0.6170(3) 0.0743(19) Uani 1 1 d . . . C21 C -0.1022(3) 0.6136(4) 0.6024(3) 0.0710(18) Uani 1 1 d . . . H21 H -0.1365 0.5808 0.6020 0.085 Uiso 1 1 calc R . . C22 C -0.0607(3) 0.5671(4) 0.5885(3) 0.0608(16) Uani 1 1 d . . . H22 H -0.0676 0.5038 0.5782 0.073 Uiso 1 1 calc R . . C23 C -0.1226(6) 0.7356(7) 0.7031(6) 0.168(5) Uani 1 1 d . . . H23A H -0.1539 0.7627 0.7129 0.253 Uiso 1 1 calc R . . H23B H -0.0808 0.7628 0.7295 0.253 Uiso 1 1 calc R . . H23C H -0.1205 0.6691 0.7101 0.253 Uiso 1 1 calc R . . C24 C -0.1418(5) 0.7540(6) 0.6368(5) 0.120(3) Uani 1 1 d . . . H24 H -0.1826 0.7194 0.6135 0.144 Uiso 1 1 calc R . . C25 C -0.1590(4) 0.8496(6) 0.6145(5) 0.137(4) Uani 1 1 d . . . H25A H -0.1868 0.8752 0.6292 0.205 Uiso 1 1 calc R . . H25B H -0.1811 0.8500 0.5694 0.205 Uiso 1 1 calc R . . H25C H -0.1203 0.8868 0.6299 0.205 Uiso 1 1 calc R . . C26 C 0.0910(2) 0.3082(3) 0.5794(2) 0.0463(13) Uani 1 1 d . . . C27 C 0.0658(3) 0.2604(4) 0.6124(3) 0.0659(17) Uani 1 1 d . . . H27 H 0.0482 0.2938 0.6334 0.079 Uiso 1 1 calc R . . C28 C 0.0665(3) 0.1646(4) 0.6142(3) 0.0685(18) Uani 1 1 d . . . H28 H 0.0485 0.1352 0.6363 0.082 Uiso 1 1 calc R . . C29 C 0.1161(3) 0.1577(4) 0.5551(3) 0.0635(16) Uani 1 1 d . . . H29 H 0.1334 0.1228 0.5344 0.076 Uiso 1 1 calc R . . C30 C 0.1178(3) 0.2534(4) 0.5514(3) 0.0619(16) Uani 1 1 d . . . H30 H 0.1371 0.2813 0.5300 0.074 Uiso 1 1 calc R . . C31 C -0.0603(3) 0.1142(4) 0.7390(3) 0.0570(15) Uani 1 1 d . . . H31 H -0.0312 0.1421 0.7285 0.068 Uiso 1 1 calc R . . C32 C -0.1074(2) 0.1698(4) 0.7401(3) 0.0550(15) Uani 1 1 d . . . H32 H -0.1085 0.2336 0.7319 0.066 Uiso 1 1 calc R . . C33 C -0.1533(2) 0.1310(3) 0.7534(2) 0.0464(13) Uani 1 1 d . . . C34 C -0.1485(3) 0.0357(4) 0.7644(3) 0.0518(14) Uani 1 1 d . . . H34 H -0.1789 0.0051 0.7719 0.062 Uiso 1 1 calc R . . C35 C -0.0988(3) -0.0138(4) 0.7640(3) 0.0553(15) Uani 1 1 d . . . H35 H -0.0962 -0.0776 0.7728 0.066 Uiso 1 1 calc R . . C36 C -0.2048(3) 0.1870(4) 0.7569(2) 0.0484(13) Uani 1 1 d . . . C37 C -0.2000(3) 0.2837(4) 0.7652(3) 0.0576(15) Uani 1 1 d . . . H37 H -0.1638 0.3154 0.7689 0.069 Uiso 1 1 calc R . . C38 C -0.2492(3) 0.3324(4) 0.7678(3) 0.0588(15) Uani 1 1 d . . . C39 C -0.3018(3) 0.2814(4) 0.7621(3) 0.0608(16) Uani 1 1 d . . . H39 H -0.3362 0.3121 0.7628 0.073 Uiso 1 1 calc R . . C40 C -0.3033(2) 0.1854(4) 0.7554(3) 0.0497(13) Uani 1 1 d . . . C41 C -0.2480(3) 0.4368(4) 0.7775(3) 0.0658(17) Uani 1 1 d . . . C42 C -0.2336(3) 0.4969(5) 0.7427(4) 0.085(2) Uani 1 1 d . . . H42 H -0.2192 0.4739 0.7158 0.101 Uiso 1 1 calc R . . C43 C -0.2407(3) 0.5953(5) 0.7474(3) 0.080(2) Uani 1 1 d . . . H43 H -0.2322 0.6365 0.7227 0.096 Uiso 1 1 calc R . . C44 C -0.2598(3) 0.6291(4) 0.7879(3) 0.0709(18) Uani 1 1 d . . . C45 C -0.2714(3) 0.5679(5) 0.8260(3) 0.084(2) Uani 1 1 d . . . H45 H -0.2825 0.5912 0.8552 0.101 Uiso 1 1 calc R . . C46 C -0.2663(4) 0.4714(4) 0.8199(4) 0.090(2) Uani 1 1 d . . . H46 H -0.2751 0.4301 0.8444 0.108 Uiso 1 1 calc R . . C47 C -0.2444(4) 0.8014(5) 0.7651(4) 0.115(3) Uani 1 1 d . . . H47A H -0.2560 0.8649 0.7684 0.173 Uiso 1 1 calc R . . H47B H -0.2592 0.7867 0.7218 0.173 Uiso 1 1 calc R . . H47C H -0.1982 0.7945 0.7885 0.173 Uiso 1 1 calc R . . C48 C -0.2763(4) 0.7346(5) 0.7914(4) 0.096(2) Uani 1 1 d . . . H48 H -0.2608 0.7507 0.8355 0.116 Uiso 1 1 calc R . . C49 C -0.3517(4) 0.7448(6) 0.7553(4) 0.144(4) Uani 1 1 d . . . H49A H -0.3633 0.8083 0.7584 0.215 Uiso 1 1 calc R . . H49B H -0.3704 0.7034 0.7734 0.215 Uiso 1 1 calc R . . H49C H -0.3678 0.7289 0.7119 0.215 Uiso 1 1 calc R . . C50 C -0.3581(2) 0.1291(4) 0.7510(2) 0.0476(13) Uani 1 1 d . . . C51 C -0.4040(3) 0.1655(4) 0.7650(3) 0.0713(19) Uani 1 1 d . . . H51 H -0.4006 0.2274 0.7782 0.086 Uiso 1 1 calc R . . C52 C -0.4543(3) 0.1115(4) 0.7595(3) 0.0713(19) Uani 1 1 d . . . H52 H -0.4832 0.1377 0.7710 0.086 Uiso 1 1 calc R . . C53 C -0.4201(3) -0.0116(4) 0.7251(3) 0.0538(14) Uani 1 1 d . . . H53 H -0.4256 -0.0730 0.7105 0.065 Uiso 1 1 calc R . . C54 C -0.3674(3) 0.0365(3) 0.7310(3) 0.0507(14) Uani 1 1 d . . . H54 H -0.3378 0.0074 0.7217 0.061 Uiso 1 1 calc R . . C55 C 0.2205(3) -0.2844(4) 0.9106(3) 0.0580(15) Uani 1 1 d . . . H55 H 0.2050 -0.2253 0.8939 0.070 Uiso 1 1 calc R . . C56 C 0.2726(3) -0.3195(4) 0.9063(3) 0.0523(14) Uani 1 1 d . . . H56 H 0.2915 -0.2842 0.8873 0.063 Uiso 1 1 calc R . . C57 C 0.2968(3) -0.4074(4) 0.9303(3) 0.0531(14) Uani 1 1 d . . . C58 C 0.2673(3) -0.4548(4) 0.9588(3) 0.0717(19) Uani 1 1 d . . . H58 H 0.2822 -0.5137 0.9761 0.086 Uiso 1 1 calc R . . C59 C 0.2155(3) -0.4150(4) 0.9618(3) 0.0697(18) Uani 1 1 d . . . H59 H 0.1965 -0.4481 0.9817 0.084 Uiso 1 1 calc R . . C60 C 0.3527(3) -0.4489(4) 0.9271(3) 0.0548(14) Uani 1 1 d . . . C61 C 0.3998(3) -0.3916(4) 0.9265(2) 0.0516(14) Uani 1 1 d . . . H61 H 0.3969 -0.3268 0.9288 0.062 Uiso 1 1 calc R . . C62 C 0.4513(3) -0.4313(4) 0.9225(2) 0.0492(13) Uani 1 1 d . . . C63 C 0.4535(3) -0.5292(4) 0.9216(2) 0.0531(14) Uani 1 1 d . . . H63 H 0.4879 -0.5592 0.9202 0.064 Uiso 1 1 calc R . . C64 C 0.4049(3) -0.5813(4) 0.9227(2) 0.0512(14) Uani 1 1 d . . . C65 C 0.5011(3) -0.3724(4) 0.9185(2) 0.0519(14) Uani 1 1 d . . . C66 C 0.4958(3) -0.2765(4) 0.9138(3) 0.077(2) Uani 1 1 d . . . H66 H 0.4601 -0.2475 0.9132 0.093 Uiso 1 1 calc R . . C67 C 0.5424(3) -0.2222(5) 0.9099(3) 0.086(2) Uani 1 1 d . . . H67 H 0.5375 -0.1574 0.9074 0.104 Uiso 1 1 calc R . . C68 C 0.5956(3) -0.2609(5) 0.9098(3) 0.079(2) Uani 1 1 d . B . C69 C 0.6014(3) -0.3574(5) 0.9140(3) 0.079(2) Uani 1 1 d . . . H69 H 0.6365 -0.3862 0.9134 0.095 Uiso 1 1 calc R . . C70 C 0.5553(3) -0.4116(4) 0.9192(3) 0.0673(17) Uani 1 1 d . . . H70 H 0.5609 -0.4763 0.9233 0.081 Uiso 1 1 calc R . . C74 C 0.4051(3) -0.6866(4) 0.9205(3) 0.0511(13) Uani 1 1 d . . . C75 C 0.3552(3) -0.7388(4) 0.9194(3) 0.0734(19) Uani 1 1 d . . . H75 H 0.3211 -0.7085 0.9211 0.088 Uiso 1 1 calc R . . C76 C 0.3554(3) -0.8346(4) 0.9158(3) 0.079(2) Uani 1 1 d . . . H76 H 0.3216 -0.8677 0.9162 0.094 Uiso 1 1 calc R . . C77 C 0.4498(3) -0.8327(4) 0.9130(3) 0.077(2) Uani 1 1 d . . . H77 H 0.4832 -0.8640 0.9108 0.092 Uiso 1 1 calc R . . C78 C 0.4527(3) -0.7360(4) 0.9176(3) 0.0699(18) Uani 1 1 d . . . H78 H 0.4877 -0.7045 0.9187 0.084 Uiso 1 1 calc R . . N1 N 0.4349(3) 0.5413(3) 0.2939(3) 0.0808(17) Uani 1 1 d . . . N2 N 0.3873(3) 0.6072(4) 0.4549(3) 0.0825(17) Uani 1 1 d . . . N3 N 0.4097(3) 0.8209(4) 0.6123(3) 0.0798(16) Uani 1 1 d . . . N4 N 0.0504(3) -0.0439(3) 0.6959(3) 0.0847(17) Uani 1 1 d . . . N5 N 0.0711(3) -0.1852(4) 0.8698(3) 0.0824(17) Uani 1 1 d . . . N6 N 0.0960(3) -0.3883(4) 1.0336(3) 0.0883(18) Uani 1 1 d . . . N7 N 0.2916(2) 0.6722(3) 0.5490(2) 0.0554(12) Uani 1 1 d . . . N8 N 0.1368(2) 0.4542(3) 0.5685(2) 0.0509(11) Uani 1 1 d . . . N9 N 0.0913(2) 0.1110(3) 0.5864(2) 0.0541(12) Uani 1 1 d . . . N10 N -0.0538(2) 0.0230(3) 0.7520(2) 0.0499(11) Uani 1 1 d . . . N11 N -0.25544(19) 0.1380(3) 0.75250(18) 0.0471(11) Uani 1 1 d . . . N12 N -0.4644(2) 0.0233(3) 0.7387(2) 0.0526(12) Uani 1 1 d . . . N13 N 0.1912(2) -0.3302(3) 0.9373(2) 0.0581(12) Uani 1 1 d . . . N14 N 0.3544(2) -0.5425(3) 0.9252(2) 0.0537(12) Uani 1 1 d . . . N15 N 0.4022(2) -0.8828(3) 0.9117(2) 0.0606(13) Uani 1 1 d . . . C72 C 0.6474(4) -0.2029(6) 0.9050(4) 0.114(3) Uani 1 1 d D . . H72 H 0.6538 -0.2297 0.8713 0.137 Uiso 1 1 calc R A 1 C71 C 0.6298(18) -0.0993(16) 0.890(2) 0.28(3) Uani 0.50 1 d PD B 1 H71A H 0.6645 -0.0674 0.8875 0.420 Uiso 0.50 1 calc PR B 1 H71B H 0.6229 -0.0714 0.9218 0.420 Uiso 0.50 1 calc PR B 1 H71C H 0.5909 -0.0942 0.8499 0.420 Uiso 0.50 1 calc PR B 1 C71' C 0.6247(14) -0.1097(12) 0.8751(13) 0.106(9) Uani 0.50 1 d PD B 2 H71D H 0.5879 -0.1176 0.8342 0.160 Uiso 0.50 1 calc PR B 2 H71E H 0.6590 -0.0791 0.8714 0.160 Uiso 0.50 1 calc PR B 2 H71F H 0.6126 -0.0721 0.9006 0.160 Uiso 0.50 1 calc PR B 2 C73 C 0.7104(4) -0.2047(7) 0.9633(5) 0.163(4) Uani 1 1 d . B . H73A H 0.7412 -0.1671 0.9579 0.244 Uiso 1 1 calc R . . H73B H 0.7259 -0.2681 0.9725 0.244 Uiso 1 1 calc R . . H73C H 0.7052 -0.1801 0.9973 0.244 Uiso 1 1 calc R . . 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 0.0723(5) 0.0575(5) 0.0690(5) 0.0088(4) 0.0478(4) 0.0109(4) Cu2 0.0797(5) 0.0515(4) 0.0733(5) -0.0086(4) 0.0529(5) -0.0033(4) Cu3 0.0684(5) 0.0540(4) 0.0727(5) -0.0138(4) 0.0492(4) -0.0117(3) Cu4 0.0878(6) 0.0479(4) 0.0765(5) -0.0067(4) 0.0582(5) 0.0003(4) Cu5 0.0713(5) 0.0543(4) 0.0693(5) 0.0065(4) 0.0486(4) 0.0075(3) Cu6 0.0762(5) 0.0552(5) 0.0778(6) 0.0185(4) 0.0523(5) 0.0121(4) C1 0.072(4) 0.046(3) 0.053(4) 0.002(3) 0.050(3) 0.003(3) C2 0.061(4) 0.044(3) 0.056(4) -0.021(3) 0.047(3) -0.006(2) C3 0.083(4) 0.049(3) 0.061(4) -0.029(3) 0.052(4) -0.033(3) C4 0.077(4) 0.044(3) 0.060(4) 0.005(3) 0.061(3) 0.001(3) C5 0.075(4) 0.040(3) 0.061(4) 0.028(3) 0.047(3) 0.026(3) C6 0.069(4) 0.043(3) 0.064(4) 0.024(3) 0.048(3) 0.002(3) C7 0.074(4) 0.056(4) 0.096(5) -0.024(3) 0.062(4) -0.012(3) C8 0.066(4) 0.049(3) 0.101(5) -0.028(3) 0.057(4) -0.022(3) C9 0.052(3) 0.043(3) 0.059(4) 0.001(3) 0.032(3) -0.006(2) C10 0.063(4) 0.048(3) 0.068(4) -0.012(3) 0.048(3) -0.008(3) C11 0.072(4) 0.043(3) 0.073(4) -0.011(3) 0.051(4) -0.013(3) C12 0.059(4) 0.046(3) 0.051(3) -0.001(3) 0.033(3) -0.005(3) C13 0.051(3) 0.043(3) 0.059(4) -0.001(3) 0.025(3) -0.005(3) C14 0.050(3) 0.044(3) 0.045(3) 0.002(2) 0.024(3) -0.002(2) C15 0.046(3) 0.047(3) 0.056(3) -0.001(3) 0.029(3) -0.005(2) C16 0.049(3) 0.042(3) 0.048(3) 0.002(2) 0.024(3) -0.005(2) C17 0.051(3) 0.046(3) 0.053(3) 0.005(3) 0.027(3) 0.006(3) C18 0.061(4) 0.058(4) 0.081(5) -0.008(3) 0.034(4) -0.002(3) C19 0.080(5) 0.060(4) 0.097(5) -0.020(4) 0.045(4) 0.004(4) C20 0.068(4) 0.080(5) 0.077(5) -0.004(4) 0.036(4) 0.012(4) C21 0.072(4) 0.066(4) 0.091(5) -0.009(4) 0.052(4) 0.003(3) C22 0.060(4) 0.055(4) 0.075(4) 0.002(3) 0.039(3) 0.000(3) C23 0.241(14) 0.156(10) 0.193(12) -0.001(9) 0.171(12) 0.045(9) C24 0.131(8) 0.115(7) 0.138(8) -0.011(6) 0.083(7) 0.041(6) C25 0.115(7) 0.129(8) 0.159(9) -0.013(7) 0.061(7) 0.051(6) C26 0.048(3) 0.043(3) 0.052(3) 0.000(3) 0.028(3) -0.002(2) C27 0.080(4) 0.046(3) 0.101(5) -0.009(3) 0.067(4) -0.005(3) C28 0.083(4) 0.049(4) 0.110(5) -0.004(3) 0.076(4) -0.002(3) C29 0.087(5) 0.055(4) 0.077(4) 0.003(3) 0.062(4) 0.011(3) C30 0.075(4) 0.055(4) 0.078(4) 0.013(3) 0.055(4) 0.007(3) C31 0.060(4) 0.055(4) 0.065(4) 0.017(3) 0.037(3) 0.006(3) C32 0.050(3) 0.044(3) 0.076(4) 0.013(3) 0.035(3) 0.004(3) C33 0.047(3) 0.041(3) 0.052(3) 0.004(2) 0.024(3) 0.003(2) C34 0.062(4) 0.046(3) 0.065(4) -0.001(3) 0.044(3) -0.005(3) C35 0.074(4) 0.039(3) 0.073(4) 0.007(3) 0.052(4) 0.005(3) C36 0.050(3) 0.041(3) 0.052(3) 0.005(3) 0.024(3) 0.003(2) C37 0.047(3) 0.048(3) 0.081(4) 0.003(3) 0.033(3) -0.002(3) C38 0.051(4) 0.045(3) 0.077(4) 0.002(3) 0.029(3) 0.000(3) C39 0.048(3) 0.043(3) 0.088(5) -0.004(3) 0.030(3) 0.001(3) C40 0.041(3) 0.047(3) 0.060(4) -0.004(3) 0.023(3) 0.001(2) C41 0.048(3) 0.047(4) 0.102(5) -0.011(4) 0.036(4) -0.003(3) C42 0.084(5) 0.053(4) 0.124(6) 0.010(4) 0.056(5) -0.001(3) C43 0.094(5) 0.046(4) 0.106(6) -0.003(4) 0.052(5) 0.004(3) C44 0.068(4) 0.048(4) 0.081(5) 0.005(3) 0.024(4) 0.004(3) C45 0.092(5) 0.060(4) 0.097(6) -0.009(4) 0.044(5) 0.006(4) C46 0.107(6) 0.048(4) 0.124(6) -0.003(4) 0.063(5) 0.003(4) C47 0.129(7) 0.057(5) 0.162(9) 0.012(5) 0.073(7) -0.008(4) C48 0.118(7) 0.072(5) 0.082(5) -0.001(4) 0.035(5) 0.022(5) C49 0.107(7) 0.132(8) 0.144(9) -0.008(6) 0.023(6) 0.053(6) C50 0.047(3) 0.042(3) 0.054(3) 0.000(3) 0.025(3) 0.000(2) C51 0.066(4) 0.059(4) 0.106(5) -0.035(4) 0.055(4) -0.015(3) C52 0.067(4) 0.065(4) 0.103(5) -0.032(4) 0.058(4) -0.013(3) C53 0.064(4) 0.041(3) 0.066(4) -0.001(3) 0.039(3) -0.001(3) C54 0.052(3) 0.042(3) 0.067(4) 0.002(3) 0.035(3) 0.005(2) C55 0.074(4) 0.051(3) 0.065(4) 0.010(3) 0.047(4) 0.011(3) C56 0.058(4) 0.050(3) 0.058(4) 0.001(3) 0.035(3) 0.002(3) C57 0.055(3) 0.051(3) 0.060(4) -0.002(3) 0.033(3) 0.003(3) C58 0.068(4) 0.052(4) 0.107(5) 0.015(3) 0.052(4) 0.017(3) C59 0.072(4) 0.065(4) 0.092(5) 0.025(4) 0.055(4) 0.015(3) C60 0.059(4) 0.057(4) 0.054(4) -0.004(3) 0.031(3) 0.005(3) C61 0.056(3) 0.046(3) 0.056(4) -0.002(3) 0.029(3) 0.007(3) C62 0.053(3) 0.053(3) 0.044(3) -0.001(3) 0.026(3) 0.005(3) C63 0.055(4) 0.060(4) 0.050(3) -0.001(3) 0.030(3) 0.006(3) C64 0.057(4) 0.053(3) 0.048(3) -0.002(3) 0.029(3) 0.008(3) C65 0.049(3) 0.057(4) 0.048(3) 0.001(3) 0.021(3) 0.005(3) C66 0.066(4) 0.061(4) 0.106(6) 0.019(4) 0.042(4) 0.008(3) C67 0.080(5) 0.070(5) 0.112(6) 0.026(4) 0.049(5) 0.008(4) C68 0.066(5) 0.090(5) 0.081(5) 0.023(4) 0.037(4) 0.000(4) C69 0.075(5) 0.091(6) 0.093(5) 0.013(4) 0.057(4) 0.009(4) C70 0.073(4) 0.062(4) 0.076(5) -0.005(3) 0.043(4) 0.000(3) C74 0.060(4) 0.044(3) 0.052(3) -0.001(3) 0.029(3) 0.008(3) C75 0.091(5) 0.055(4) 0.113(6) -0.004(4) 0.079(5) 0.004(3) C76 0.111(6) 0.051(4) 0.120(6) -0.003(4) 0.092(5) -0.004(4) C77 0.068(4) 0.055(4) 0.119(6) -0.005(4) 0.054(4) 0.009(3) C78 0.057(4) 0.051(4) 0.110(6) -0.006(4) 0.047(4) 0.002(3) N1 0.073(4) 0.057(3) 0.107(5) 0.009(3) 0.039(4) 0.014(3) N2 0.085(4) 0.072(4) 0.105(5) 0.022(3) 0.057(4) -0.006(3) N3 0.082(4) 0.078(4) 0.109(5) 0.007(4) 0.070(4) -0.012(3) N4 0.087(4) 0.051(3) 0.108(5) 0.011(3) 0.041(4) 0.013(3) N5 0.086(4) 0.076(4) 0.120(5) -0.014(4) 0.078(4) 0.004(3) N6 0.094(4) 0.070(4) 0.111(5) -0.012(4) 0.058(4) 0.008(3) N7 0.060(3) 0.051(3) 0.069(3) -0.006(2) 0.042(3) -0.008(2) N8 0.054(3) 0.048(3) 0.061(3) -0.002(2) 0.036(3) -0.007(2) N9 0.062(3) 0.048(3) 0.062(3) -0.002(2) 0.037(3) -0.001(2) N10 0.059(3) 0.049(3) 0.052(3) 0.006(2) 0.034(2) 0.009(2) N11 0.046(3) 0.041(2) 0.058(3) -0.001(2) 0.029(2) -0.0028(19) N12 0.057(3) 0.054(3) 0.058(3) -0.007(2) 0.037(3) -0.008(2) N13 0.065(3) 0.054(3) 0.068(3) 0.008(2) 0.042(3) 0.011(2) N14 0.059(3) 0.048(3) 0.059(3) 0.001(2) 0.033(3) 0.009(2) N15 0.075(3) 0.050(3) 0.073(3) 0.000(2) 0.048(3) 0.002(3) C72 0.085(6) 0.142(8) 0.116(7) 0.033(6) 0.049(6) -0.018(6) C71 0.09(2) 0.27(5) 0.32(5) 0.20(4) -0.02(2) -0.01(3) C71' 0.13(2) 0.102(17) 0.113(15) 0.042(12) 0.084(17) -0.036(14) C73 0.086(7) 0.180(10) 0.200(12) 0.029(9) 0.052(8) -0.044(7) _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 C3 1.883(5) 4_575 ? Cu1 N1 1.938(7) . ? Cu1 N12 2.069(4) 4_665 ? Cu2 C1 1.881(5) . ? Cu2 N2 1.935(6) . ? Cu2 N15 2.095(5) 4 ? Cu3 C2 1.867(5) . ? Cu3 N3 1.909(6) . ? Cu3 N7 2.103(4) . ? Cu4 C4 1.886(5) . ? Cu4 N6 1.925(7) 4 ? Cu4 N9 2.082(4) . ? Cu5 C5 1.875(5) . ? Cu5 N4 1.941(7) . ? Cu5 N10 2.051(4) . ? Cu6 C6 1.870(5) . ? Cu6 N5 1.920(7) . ? Cu6 N13 2.109(4) . ? C1 N1 1.126(7) . ? C2 N2 1.115(7) . ? C3 N3 1.148(7) . ? C3 Cu1 1.883(5) 4_576 ? C4 N4 1.124(7) . ? C5 N5 1.147(7) . ? C6 N6 1.110(7) . ? C7 N7 1.330(7) . ? C7 C8 1.370(7) . ? C7 H7 0.9300 . ? C8 C9 1.374(7) . ? C8 H8 0.9300 . ? C9 C10 1.384(7) . ? C9 C12 1.499(7) . ? C10 C11 1.384(7) . ? C10 H10 0.9300 . ? C11 N7 1.322(6) . ? C11 H11 0.9300 . ? C12 N8 1.334(6) . ? C12 C13 1.382(7) . ? C13 C14 1.384(7) . ? C13 H13 0.9300 . ? C14 C15 1.386(7) . ? C14 C17 1.491(7) . ? C15 C16 1.388(7) . ? C15 H15 0.9300 . ? C16 N8 1.349(6) . ? C16 C26 1.485(7) . ? C17 C18 1.385(7) . ? C17 C22 1.396(7) . ? C18 C19 1.380(8) . ? C18 H18 0.9300 . ? C19 C20 1.396(9) . ? C19 H19 0.9300 . ? C20 C21 1.365(8) . ? C20 C24 1.541(9) . ? C21 C22 1.353(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.474(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.450(11) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C30 1.375(7) . ? C26 C27 1.386(7) . ? C27 C28 1.367(7) . ? C27 H27 0.9300 . ? C28 N9 1.330(7) . ? C28 H28 0.9300 . ? C29 N9 1.342(6) . ? C29 C30 1.369(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 N10 1.330(6) . ? C31 C32 1.375(7) . ? C31 H31 0.9300 . ? C32 C33 1.385(7) . ? C32 H32 0.9300 . ? C33 C34 1.378(7) . ? C33 C36 1.488(7) . ? C34 C35 1.372(7) . ? C34 H34 0.9300 . ? C35 N10 1.334(6) . ? C35 H35 0.9300 . ? C36 N11 1.342(6) . ? C36 C37 1.392(7) . ? C37 C38 1.379(7) . ? C37 H37 0.9300 . ? C38 C39 1.385(7) . ? C38 C41 1.505(8) . ? C39 C40 1.377(7) . ? C39 H39 0.9300 . ? C40 N11 1.346(6) . ? C40 C50 1.482(7) . ? C41 C42 1.358(9) . ? C41 C46 1.387(9) . ? C42 C43 1.426(9) . ? C42 H42 0.9300 . ? C43 C44 1.352(8) . ? C43 H43 0.9300 . ? C44 C45 1.394(9) . ? C44 C48 1.568(8) . ? C45 C46 1.397(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.532(10) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.563(10) . ? C48 H48 0.9800 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.382(7) . ? C50 C54 1.387(7) . ? C51 C52 1.365(7) . ? C51 H51 0.9300 . ? C52 N12 1.333(7) . ? C52 H52 0.9300 . ? C53 N12 1.336(6) . ? C53 C54 1.365(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 N13 1.327(6) . ? C55 C56 1.375(7) . ? C55 H55 0.9300 . ? C56 C57 1.385(7) . ? C56 H56 0.9300 . ? C57 C58 1.375(8) . ? C57 C60 1.480(7) . ? C58 C59 1.381(8) . ? C58 H58 0.9300 . ? C59 N13 1.347(7) . ? C59 H59 0.9300 . ? C60 N14 1.337(6) . ? C60 C61 1.384(7) . ? C61 C62 1.385(7) . ? C61 H61 0.9300 . ? C62 C63 1.398(7) . ? C62 C65 1.484(7) . ? C63 C64 1.378(7) . ? C63 H63 0.9300 . ? C64 N14 1.340(6) . ? C64 C74 1.504(7) . ? C65 C66 1.373(7) . ? C65 C70 1.386(7) . ? C66 C67 1.385(8) . ? C66 H66 0.9300 . ? C67 C68 1.370(9) . ? C67 H67 0.9300 . ? C68 C69 1.382(9) . ? C68 C72 1.526(9) . ? C69 C70 1.388(8) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C74 C78 1.355(7) . ? C74 C75 1.380(8) . ? C75 C76 1.369(8) . ? C75 H75 0.9300 . ? C76 N15 1.344(7) . ? C76 H76 0.9300 . ? C77 N15 1.317(7) . ? C77 C78 1.381(8) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? N6 Cu4 1.925(7) 4_556 ? N12 Cu1 2.069(4) 4_466 ? N15 Cu2 2.095(5) 4_556 ? C72 C73 1.477(11) . ? C72 C71' 1.485(15) . ? C72 C71 1.531(18) . ? C72 H72 0.9800 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C71' H71D 0.9600 . ? C71' H71E 0.9600 . ? C71' H71F 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? 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 C3 Cu1 N1 137.3(2) 4_575 . ? C3 Cu1 N12 108.1(2) 4_575 4_665 ? N1 Cu1 N12 114.49(19) . 4_665 ? C1 Cu2 N2 140.7(2) . . ? C1 Cu2 N15 101.8(2) . 4 ? N2 Cu2 N15 117.1(2) . 4 ? C2 Cu3 N3 148.5(2) . . ? C2 Cu3 N7 103.7(2) . . ? N3 Cu3 N7 107.41(19) . . ? C4 Cu4 N6 140.1(2) . 4 ? C4 Cu4 N9 100.98(19) . . ? N6 Cu4 N9 118.7(2) 4 . ? C5 Cu5 N4 131.3(2) . . ? C5 Cu5 N10 107.5(2) . . ? N4 Cu5 N10 120.9(2) . . ? C6 Cu6 N5 148.0(2) . . ? C6 Cu6 N13 104.8(2) . . ? N5 Cu6 N13 106.89(19) . . ? N1 C1 Cu2 179.3(6) . . ? N2 C2 Cu3 178.3(5) . . ? N3 C3 Cu1 173.9(5) . 4_576 ? N4 C4 Cu4 174.1(5) . . ? N5 C5 Cu5 173.3(5) . . ? N6 C6 Cu6 176.3(6) . . ? N7 C7 C8 123.6(5) . . ? N7 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 120.1(5) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 116.9(5) . . ? C8 C9 C12 121.7(5) . . ? C10 C9 C12 121.4(5) . . ? C9 C10 C11 119.0(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? N7 C11 C10 124.0(5) . . ? N7 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? N8 C12 C13 124.5(5) . . ? N8 C12 C9 114.5(5) . . ? C13 C12 C9 121.0(5) . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 116.5(5) . . ? C13 C14 C17 123.2(5) . . ? C15 C14 C17 120.3(5) . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? N8 C16 C15 122.9(5) . . ? N8 C16 C26 117.1(4) . . ? C15 C16 C26 120.0(4) . . ? C18 C17 C22 117.2(5) . . ? C18 C17 C14 121.6(5) . . ? C22 C17 C14 121.2(5) . . ? C19 C18 C17 120.6(6) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 121.6(6) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 116.7(6) . . ? C21 C20 C24 120.0(7) . . ? C19 C20 C24 123.2(7) . . ? C22 C21 C20 122.6(6) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C17 121.3(6) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.4 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C23 117.5(8) . . ? C25 C24 C20 113.8(8) . . ? C23 C24 C20 112.0(8) . . ? C25 C24 H24 103.9 . . ? C23 C24 H24 103.9 . . ? C20 C24 H24 103.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C30 C26 C27 115.8(5) . . ? C30 C26 C16 122.8(5) . . ? C27 C26 C16 121.4(5) . . ? C28 C27 C26 120.6(5) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? N9 C28 C27 124.0(5) . . ? N9 C28 H28 118.0 . . ? C27 C28 H28 118.0 . . ? N9 C29 C30 124.5(5) . . ? N9 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C29 C30 C26 120.0(5) . . ? C29 C30 H30 120.0 . . ? C26 C30 H30 120.0 . . ? N10 C31 C32 124.0(5) . . ? N10 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C31 C32 C33 120.2(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 116.0(5) . . ? C34 C33 C36 120.7(5) . . ? C32 C33 C36 123.3(5) . . ? C35 C34 C33 119.8(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? N10 C35 C34 124.7(5) . . ? N10 C35 H35 117.6 . . ? C34 C35 H35 117.6 . . ? N11 C36 C37 122.3(5) . . ? N11 C36 C33 115.7(4) . . ? C37 C36 C33 122.0(5) . . ? C38 C37 C36 119.7(5) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 117.5(5) . . ? C37 C38 C41 123.5(5) . . ? C39 C38 C41 118.9(5) . . ? C40 C39 C38 120.3(5) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? N11 C40 C39 122.1(5) . . ? N11 C40 C50 116.6(4) . . ? C39 C40 C50 121.3(5) . . ? C42 C41 C46 120.0(6) . . ? C42 C41 C38 121.2(7) . . ? C46 C41 C38 118.6(6) . . ? C41 C42 C43 119.7(7) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.2(7) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.2(6) . . ? C43 C44 C48 124.1(6) . . ? C45 C44 C48 115.5(7) . . ? C44 C45 C46 119.4(7) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 120.3(7) . . ? C41 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C47 C48 C49 111.2(7) . . ? C47 C48 C44 112.9(6) . . ? C49 C48 C44 107.7(6) . . ? C47 C48 H48 108.3 . . ? C49 C48 H48 108.3 . . ? C44 C48 H48 108.3 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C54 115.8(5) . . ? C51 C50 C40 122.5(5) . . ? C54 C50 C40 121.7(5) . . ? C52 C51 C50 120.7(5) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? N12 C52 C51 123.8(5) . . ? N12 C52 H52 118.1 . . ? C51 C52 H52 118.1 . . ? N12 C53 C54 124.5(5) . . ? N12 C53 H53 117.7 . . ? C54 C53 H53 117.7 . . ? C53 C54 C50 119.8(5) . . ? C53 C54 H54 120.1 . . ? C50 C54 H54 120.1 . . ? N13 C55 C56 123.5(5) . . ? N13 C55 H55 118.2 . . ? C56 C55 H55 118.2 . . ? C55 C56 C57 120.0(5) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 116.8(5) . . ? C58 C57 C60 120.8(5) . . ? C56 C57 C60 122.4(5) . . ? C57 C58 C59 120.2(6) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? N13 C59 C58 122.8(5) . . ? N13 C59 H59 118.6 . . ? C58 C59 H59 118.6 . . ? N14 C60 C61 123.5(5) . . ? N14 C60 C57 116.2(5) . . ? C61 C60 C57 120.2(5) . . ? C60 C61 C62 119.6(5) . . ? C60 C61 H61 120.2 . . ? C62 C61 H61 120.2 . . ? C61 C62 C63 116.8(5) . . ? C61 C62 C65 121.4(5) . . ? C63 C62 C65 121.8(5) . . ? C64 C63 C62 120.0(5) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? N14 C64 C63 123.0(5) . . ? N14 C64 C74 115.6(5) . . ? C63 C64 C74 121.4(5) . . ? C66 C65 C70 116.7(6) . . ? C66 C65 C62 121.7(5) . . ? C70 C65 C62 121.6(5) . . ? C65 C66 C67 121.2(6) . . ? C65 C66 H66 119.4 . . ? C67 C66 H66 119.4 . . ? C68 C67 C66 122.2(7) . . ? C68 C67 H67 118.9 . . ? C66 C67 H67 118.9 . . ? C67 C68 C69 117.3(6) . . ? C67 C68 C72 123.3(7) . . ? C69 C68 C72 119.4(7) . . ? C68 C69 C70 120.5(6) . . ? C68 C69 H69 119.7 . . ? C70 C69 H69 119.7 . . ? C65 C70 C69 122.1(6) . . ? C65 C70 H70 119.0 . . ? C69 C70 H70 119.0 . . ? C78 C74 C75 116.0(5) . . ? C78 C74 C64 122.6(5) . . ? C75 C74 C64 121.4(5) . . ? C76 C75 C74 120.6(5) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? N15 C76 C75 122.9(6) . . ? N15 C76 H76 118.6 . . ? C75 C76 H76 118.6 . . ? N15 C77 C78 123.5(6) . . ? N15 C77 H77 118.3 . . ? C78 C77 H77 118.3 . . ? C74 C78 C77 120.9(6) . . ? C74 C78 H78 119.6 . . ? C77 C78 H78 119.6 . . ? C1 N1 Cu1 178.1(5) . . ? C2 N2 Cu2 176.7(6) . . ? C3 N3 Cu3 172.5(5) . . ? C4 N4 Cu5 175.3(5) . . ? C5 N5 Cu6 176.6(5) . . ? C6 N6 Cu4 178.0(6) . 4_556 ? C11 N7 C7 116.4(5) . . ? C11 N7 Cu3 121.4(4) . . ? C7 N7 Cu3 122.0(4) . . ? C12 N8 C16 115.9(4) . . ? C28 N9 C29 115.1(5) . . ? C28 N9 Cu4 118.4(4) . . ? C29 N9 Cu4 126.5(4) . . ? C31 N10 C35 115.1(4) . . ? C31 N10 Cu5 122.8(4) . . ? C35 N10 Cu5 122.0(4) . . ? C36 N11 C40 118.0(4) . . ? C52 N12 C53 115.4(5) . . ? C52 N12 Cu1 123.1(4) . 4_466 ? C53 N12 Cu1 121.5(4) . 4_466 ? C55 N13 C59 116.7(5) . . ? C55 N13 Cu6 121.2(4) . . ? C59 N13 Cu6 122.0(4) . . ? C60 N14 C64 117.0(5) . . ? C77 N15 C76 116.1(5) . . ? C77 N15 Cu2 119.1(4) . 4_556 ? C76 N15 Cu2 124.7(4) . 4_556 ? C73 C72 C71' 116.3(14) . . ? C73 C72 C68 112.8(7) . . ? C71' C72 C68 114.2(11) . . ? C73 C72 C71 106.2(17) . . ? C71' C72 C71 13(3) . . ? C68 C72 C71 114.1(16) . . ? C73 C72 H72 107.8 . . ? C71' C72 H72 96.1 . . ? C68 C72 H72 107.8 . . ? C71 C72 H72 107.8 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C72 C71' H71D 109.5 . . ? C72 C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? C72 C71' H71F 109.5 . . ? H71D C71' H71F 109.5 . . ? H71E C71' H71F 109.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.243 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.104 #======================================= data_4 _database_code_depnum_ccdc_archive 'CCDC 826230' #TrackingRef '- Compounds 1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H61 Cu6 N15 O2' _chemical_formula_weight 1729.74 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 32.9876(14) _cell_length_b 15.2044(6) _cell_length_c 15.3966(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7722.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4040 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 19.06 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_T_max 0.7630 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37252 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6811 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.0754P)^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 6811 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.548110(14) 0.44833(4) 0.11052(3) 0.0689(2) Uani 1 1 d . . . Cu2 Cu 0.587029(17) 0.30578(4) 0.38324(3) 0.0793(2) Uani 1 1 d . . . Cu3 Cu 0.697130(18) 0.24630(4) 0.59046(4) 0.0894(2) Uani 1 1 d . . . C1 C 0.51009(10) 0.4884(3) 0.0282(2) 0.0678(10) Uani 0.50 1 d P . 1 N1 N 0.51009(10) 0.4884(3) 0.0282(2) 0.0678(10) Uani 0.50 1 d P . 2 C2 C 0.55919(12) 0.3958(3) 0.2153(2) 0.0604(11) Uani 1 1 d . . . C3 C 0.63168(12) 0.2780(3) 0.4518(3) 0.0674(11) Uani 1 1 d . . . C4 C 0.70105(12) 0.2474(3) 0.7123(2) 0.0874(13) Uani 0.50 1 d P . 1 N4 N 0.70105(12) 0.2474(3) 0.7123(2) 0.0874(13) Uani 0.50 1 d P . 2 C5 C 0.63980(11) 0.4484(3) 0.0843(2) 0.0623(10) Uani 1 1 d . . . H5 H 0.6402 0.4285 0.1414 0.075 Uiso 1 1 calc R . . C6 C 0.67618(11) 0.4559(3) 0.0408(2) 0.0633(11) Uani 1 1 d . . . H6 H 0.7002 0.4410 0.0686 0.076 Uiso 1 1 calc R . . C7 C 0.67710(11) 0.4856(3) -0.0440(2) 0.0602(10) Uani 1 1 d . . . C8 C 0.64040(12) 0.5071(3) -0.0796(2) 0.0808(14) Uani 1 1 d . . . H8 H 0.6392 0.5277 -0.1365 0.097 Uiso 1 1 calc R . . C9 C 0.60530(12) 0.4987(3) -0.0323(3) 0.0795(13) Uani 1 1 d . . . H9 H 0.5810 0.5152 -0.0581 0.095 Uiso 1 1 calc R . . C10 C 0.71525(11) 0.4929(3) -0.0934(2) 0.0596(10) Uani 1 1 d . . . C11 C 0.71459(11) 0.4916(3) -0.1831(2) 0.0661(11) Uani 1 1 d . . . H11 H 0.6900 0.4850 -0.2118 0.079 Uiso 1 1 calc R . . C12 C 0.7500 0.5000 -0.2312(3) 0.0590(14) Uani 1 2 d S . . C13 C 0.7500 0.5000 -0.3274(3) 0.0609(14) Uani 1 2 d S . . C14 C 0.77923(13) 0.5435(3) -0.3743(3) 0.0879(15) Uani 1 1 d . . . H14 H 0.7997 0.5732 -0.3448 0.105 Uiso 1 1 calc R . . C15 C 0.77915(13) 0.5444(3) -0.4637(3) 0.0862(14) Uani 1 1 d . . . H15 H 0.7991 0.5756 -0.4931 0.103 Uiso 1 1 calc R . . C16 C 0.7500 0.5000 -0.5101(3) 0.0526(13) Uani 1 2 d S . . C17 C 0.7500 0.5000 -0.6069(3) 0.0556(14) Uani 1 2 d S . . C18 C 0.77377(13) 0.5582(3) -0.6535(2) 0.0759(13) Uani 1 1 d . . . H18 H 0.7898 0.5986 -0.6240 0.091 Uiso 1 1 calc R . . C19 C 0.77407(15) 0.5574(3) -0.7431(2) 0.0908(16) Uani 1 1 d . . . H19 H 0.7907 0.5962 -0.7733 0.109 Uiso 1 1 calc R . . C20 C 0.7500 0.5000 -0.7873(4) 0.095(2) Uani 1 2 d S . . H20 H 0.7500 0.5000 -0.8477 0.114 Uiso 1 2 calc SR . . C21 C 0.92951(18) -0.0708(4) -0.2543(3) 0.1007(17) Uani 1 1 d . . . H21 H 0.9327 -0.0930 -0.3102 0.121 Uiso 1 1 calc R . . C22 C 0.89763(17) -0.0993(4) -0.2035(3) 0.0998(16) Uani 1 1 d . . . H22 H 0.8796 -0.1412 -0.2244 0.120 Uiso 1 1 calc R . . C23 C 0.89302(15) -0.0648(3) -0.1217(3) 0.0836(14) Uani 1 1 d . . . H23 H 0.8711 -0.0832 -0.0883 0.100 Uiso 1 1 calc R . . C24 C 0.91946(14) -0.0041(3) -0.0868(3) 0.0753(12) Uani 1 1 d . . . C25 C 0.95159(15) 0.0230(4) -0.1403(3) 0.1005(17) Uani 1 1 d . . . H25 H 0.9702 0.0641 -0.1199 0.121 Uiso 1 1 calc R . . C26 C 0.95589(17) -0.0112(4) -0.2236(3) 0.1112(19) Uani 1 1 d . . . H26 H 0.9773 0.0075 -0.2584 0.133 Uiso 1 1 calc R . . C27 C 0.91497(13) 0.0302(3) 0.0023(3) 0.0714(12) Uani 1 1 d . . . C28 C 0.87759(15) 0.0454(4) 0.0390(3) 0.0962(16) Uani 1 1 d . . . H28 H 0.8545 0.0348 0.0061 0.115 Uiso 1 1 calc R . . C29 C 0.87325(15) 0.0757(4) 0.1231(3) 0.0931(16) Uani 1 1 d . . . H29 H 0.8473 0.0838 0.1452 0.112 Uiso 1 1 calc R . . C30 C 0.90575(12) 0.0944(3) 0.1751(3) 0.0653(11) Uani 1 1 d . . . C31 C 0.94289(14) 0.0812(4) 0.1369(3) 0.0895(15) Uani 1 1 d . . . H31 H 0.9661 0.0937 0.1689 0.107 Uiso 1 1 calc R . . C32 C 0.94728(14) 0.0507(4) 0.0538(3) 0.1001(17) Uani 1 1 d . . . H32 H 0.9733 0.0437 0.0316 0.120 Uiso 1 1 calc R . . C33 C 0.90196(12) 0.1299(3) 0.2640(2) 0.0614(10) Uani 1 1 d . . . C34 C 0.86501(12) 0.1476(3) 0.3036(3) 0.0671(11) Uani 1 1 d . . . H34 H 0.8411 0.1354 0.2740 0.080 Uiso 1 1 calc R . . C35 C 0.86315(12) 0.1833(3) 0.3870(3) 0.0633(11) Uani 1 1 d . . . C36 C 0.93239(12) 0.1864(3) 0.3952(3) 0.0634(11) Uani 1 1 d . . . C37 C 0.93613(12) 0.1502(3) 0.3139(3) 0.0672(11) Uani 1 1 d . . . H37 H 0.9618 0.1390 0.2916 0.081 Uiso 1 1 calc R . . C38 C 0.82408(12) 0.2010(3) 0.4322(3) 0.0659(11) Uani 1 1 d . . . C39 C 0.78720(13) 0.2041(3) 0.3911(3) 0.0743(12) Uani 1 1 d . . . H39 H 0.7858 0.1957 0.3314 0.089 Uiso 1 1 calc R . . C40 C 0.75236(13) 0.2195(3) 0.4372(3) 0.0760(12) Uani 1 1 d . . . H40 H 0.7281 0.2226 0.4065 0.091 Uiso 1 1 calc R . . C41 C 0.78678(15) 0.2275(4) 0.5617(3) 0.1058(19) Uani 1 1 d . . . H41 H 0.7873 0.2353 0.6216 0.127 Uiso 1 1 calc R . . C42 C 0.82285(14) 0.2141(4) 0.5206(3) 0.1001(17) Uani 1 1 d . . . H42 H 0.8468 0.2138 0.5525 0.120 Uiso 1 1 calc R . . C43 C 0.96886(12) 0.2131(3) 0.4471(3) 0.0675(11) Uani 1 1 d . . . C44 C 0.96632(13) 0.2276(3) 0.5355(3) 0.0837(14) Uani 1 1 d . . . H44 H 0.9417 0.2201 0.5642 0.100 Uiso 1 1 calc R . . C45 C 1.00013(14) 0.2530(3) 0.5809(3) 0.0840(14) Uani 1 1 d . . . H45 H 0.9975 0.2626 0.6403 0.101 Uiso 1 1 calc R . . C46 C 1.03877(13) 0.2500(3) 0.4600(3) 0.0815(13) Uani 1 1 d . . . H46 H 1.0638 0.2575 0.4331 0.098 Uiso 1 1 calc R . . C47 C 1.00626(13) 0.2243(3) 0.4097(3) 0.0772(13) Uani 1 1 d . . . H47 H 1.0097 0.2147 0.3505 0.093 Uiso 1 1 calc R . . N2 N 0.56977(11) 0.3613(3) 0.2783(3) 0.0903(12) Uani 1 1 d . . . N3 N 0.65670(12) 0.2646(3) 0.5026(3) 0.0901(12) Uani 1 1 d . . . N5 N 0.60428(9) 0.4682(2) 0.04864(19) 0.0628(9) Uani 1 1 d . . . N6 N 0.7500 0.5000 -0.0476(3) 0.0609(12) Uani 1 2 d S . . N7 N 0.75103(10) 0.2301(2) 0.5226(2) 0.0790(10) Uani 1 1 d . . . N8 N 0.89661(10) 0.2018(2) 0.4331(2) 0.0661(9) Uani 1 1 d . . . N9 N 1.03625(10) 0.2648(2) 0.5453(2) 0.0758(10) 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 0.0534(3) 0.0981(4) 0.0552(3) 0.0052(3) 0.0023(2) 0.0013(3) Cu2 0.0694(4) 0.1026(5) 0.0658(4) 0.0146(3) -0.0021(3) 0.0020(3) Cu3 0.0724(4) 0.1267(6) 0.0690(4) 0.0042(3) 0.0013(3) 0.0237(4) C1 0.049(2) 0.089(3) 0.065(3) 0.009(2) 0.0015(16) -0.001(2) N1 0.049(2) 0.089(3) 0.065(3) 0.009(2) 0.0015(16) -0.001(2) C2 0.053(2) 0.086(3) 0.042(2) 0.012(2) -0.0045(18) 0.003(2) C3 0.049(2) 0.096(3) 0.058(2) 0.006(2) -0.002(2) 0.004(2) C4 0.060(2) 0.126(3) 0.076(3) 0.014(3) 0.0005(17) 0.010(3) N4 0.060(2) 0.126(3) 0.076(3) 0.014(3) 0.0005(17) 0.010(3) C5 0.054(2) 0.087(3) 0.047(2) 0.004(2) -0.0022(18) 0.002(2) C6 0.046(2) 0.095(3) 0.049(2) -0.002(2) -0.0032(17) 0.004(2) C7 0.051(2) 0.087(3) 0.042(2) -0.003(2) 0.0009(17) -0.007(2) C8 0.049(2) 0.150(4) 0.044(2) 0.013(3) 0.0016(18) 0.005(3) C9 0.046(2) 0.133(4) 0.060(3) 0.013(3) -0.0013(19) 0.007(2) C10 0.043(2) 0.085(3) 0.051(2) -0.007(2) -0.0005(17) 0.005(2) C11 0.041(2) 0.110(3) 0.047(2) -0.003(2) -0.0048(16) -0.003(2) C12 0.047(3) 0.086(4) 0.044(3) 0.000 0.000 -0.004(3) C13 0.042(3) 0.089(4) 0.052(3) 0.000 0.000 -0.006(3) C14 0.064(3) 0.144(5) 0.056(3) -0.002(3) -0.006(2) -0.023(3) C15 0.067(3) 0.129(4) 0.062(3) 0.001(3) 0.005(2) -0.021(3) C16 0.042(3) 0.071(4) 0.045(3) 0.000 0.000 -0.006(3) C17 0.046(3) 0.074(4) 0.047(3) 0.000 0.000 0.003(3) C18 0.080(3) 0.100(3) 0.047(2) -0.001(2) -0.002(2) -0.019(3) C19 0.098(4) 0.126(4) 0.048(3) 0.008(3) 0.003(2) -0.040(3) C20 0.103(5) 0.137(6) 0.044(3) 0.000 0.000 -0.027(5) C21 0.102(4) 0.130(5) 0.070(3) -0.012(3) -0.018(3) 0.027(4) C22 0.097(4) 0.124(4) 0.079(4) -0.016(3) 0.000(3) -0.001(3) C23 0.075(3) 0.099(4) 0.077(3) 0.002(3) 0.002(2) -0.006(3) C24 0.073(3) 0.090(3) 0.062(3) 0.007(2) 0.003(2) -0.003(3) C25 0.086(4) 0.145(5) 0.070(3) 0.005(3) 0.004(3) -0.025(3) C26 0.090(4) 0.174(6) 0.070(4) 0.001(4) 0.017(3) 0.004(4) C27 0.062(3) 0.086(3) 0.066(3) 0.002(2) 0.002(2) -0.012(2) C28 0.066(3) 0.136(5) 0.086(3) -0.027(3) 0.001(3) -0.013(3) C29 0.061(3) 0.131(4) 0.087(3) -0.035(3) 0.012(2) -0.013(3) C30 0.057(3) 0.071(3) 0.068(3) 0.004(2) 0.001(2) -0.003(2) C31 0.063(3) 0.138(5) 0.068(3) -0.010(3) -0.002(2) -0.006(3) C32 0.061(3) 0.171(5) 0.068(3) -0.010(3) 0.002(2) 0.003(3) C33 0.060(2) 0.060(3) 0.065(3) 0.006(2) 0.002(2) -0.003(2) C34 0.058(3) 0.075(3) 0.068(3) 0.008(2) 0.000(2) 0.004(2) C35 0.055(2) 0.063(3) 0.072(3) 0.005(2) 0.003(2) 0.003(2) C36 0.060(3) 0.065(3) 0.066(3) 0.004(2) 0.000(2) -0.002(2) C37 0.054(2) 0.077(3) 0.071(3) -0.002(2) 0.001(2) -0.006(2) C38 0.053(2) 0.074(3) 0.070(3) 0.002(2) 0.001(2) 0.004(2) C39 0.062(3) 0.099(3) 0.062(3) 0.003(2) 0.002(2) 0.001(2) C40 0.054(3) 0.097(3) 0.077(3) 0.004(3) -0.004(2) 0.006(2) C41 0.068(3) 0.180(6) 0.070(3) -0.021(3) -0.009(3) 0.034(3) C42 0.061(3) 0.173(5) 0.066(3) -0.012(3) -0.011(2) 0.032(3) C43 0.057(2) 0.073(3) 0.072(3) -0.007(2) 0.001(2) 0.004(2) C44 0.059(3) 0.115(4) 0.078(3) -0.022(3) 0.013(2) 0.001(3) C45 0.061(3) 0.118(4) 0.073(3) -0.025(3) 0.005(2) -0.001(3) C46 0.058(3) 0.114(4) 0.072(3) -0.010(3) 0.006(2) -0.014(3) C47 0.063(3) 0.109(4) 0.060(3) -0.012(2) 0.006(2) -0.009(3) N2 0.070(3) 0.106(3) 0.094(3) -0.005(3) 0.008(2) -0.013(2) N3 0.080(3) 0.112(3) 0.079(3) -0.008(2) 0.013(2) 0.010(2) N5 0.0493(18) 0.094(3) 0.0447(18) 0.0057(17) 0.0000(14) 0.0017(17) N6 0.042(2) 0.090(4) 0.050(2) 0.000 0.000 0.006(2) N7 0.060(2) 0.112(3) 0.065(2) -0.001(2) -0.0017(18) 0.013(2) N8 0.051(2) 0.072(2) 0.076(2) -0.0004(18) 0.0024(17) 0.0027(17) N9 0.059(2) 0.100(3) 0.069(2) -0.022(2) 0.0073(18) -0.0026(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C2 1.836(4) . ? Cu1 C1 1.885(3) . ? Cu1 N5 2.105(3) . ? Cu2 C3 1.861(4) . ? Cu2 N2 1.911(4) . ? Cu2 N9 2.099(3) 6_556 ? Cu3 C4 1.881(4) . ? Cu3 N3 1.919(4) . ? Cu3 N7 2.077(3) . ? C1 C1 1.148(6) 5_665 ? C2 N2 1.157(5) . ? C3 N3 1.156(5) . ? C4 C4 1.163(8) 4_556 ? C5 N5 1.328(4) . ? C5 C6 1.379(5) . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.369(5) . ? C7 C10 1.475(5) . ? C8 C9 1.375(5) . ? C8 H8 0.9300 . ? C9 N5 1.329(5) . ? C9 H9 0.9300 . ? C10 N6 1.350(4) . ? C10 C11 1.381(5) . ? C11 C12 1.389(4) . ? C11 H11 0.9300 . ? C12 C11 1.389(4) 2_665 ? C12 C13 1.482(7) . ? C13 C14 1.374(5) 2_665 ? C13 C14 1.374(5) . ? C14 C15 1.376(5) . ? C14 H14 0.9300 . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 C15 1.375(5) 2_665 ? C16 C17 1.491(7) . ? C17 C18 1.383(4) 2_665 ? C17 C18 1.383(4) . ? C18 C19 1.378(5) . ? C18 H18 0.9300 . ? C19 C20 1.363(5) . ? C19 H19 0.9300 . ? C20 C19 1.363(5) 2_665 ? C20 H20 0.9300 . ? C21 C26 1.342(7) . ? C21 C22 1.380(7) . ? C21 H21 0.9300 . ? C22 C23 1.373(6) . ? C22 H22 0.9300 . ? C23 C24 1.379(6) . ? C23 H23 0.9300 . ? C24 C25 1.404(6) . ? C24 C27 1.475(6) . ? C25 C26 1.391(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.365(6) . ? C27 C28 1.376(6) . ? C28 C29 1.383(6) . ? C28 H28 0.9300 . ? C29 C30 1.368(6) . ? C29 H29 0.9300 . ? C30 C31 1.374(6) . ? C30 C33 1.477(5) . ? C31 C32 1.368(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.389(5) . ? C33 C37 1.398(5) . ? C34 C35 1.396(5) . ? C34 H34 0.9300 . ? C35 N8 1.341(5) . ? C35 C38 1.489(5) . ? C36 N8 1.337(5) . ? C36 C37 1.374(5) . ? C36 C43 1.500(6) . ? C37 H37 0.9300 . ? C38 C39 1.372(5) . ? C38 C42 1.376(6) . ? C39 C40 1.370(6) . ? C39 H39 0.9300 . ? C40 N7 1.325(5) . ? C40 H40 0.9300 . ? C41 N7 1.325(5) . ? C41 C42 1.363(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C47 1.372(6) . ? C43 C44 1.382(6) . ? C44 C45 1.372(6) . ? C44 H44 0.9300 . ? C45 N9 1.324(5) . ? C45 H45 0.9300 . ? C46 N9 1.334(5) . ? C46 C47 1.380(6) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? N6 C10 1.350(4) 2_665 ? N9 Cu2 2.099(3) 6_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Cu1 C1 149.76(16) . . ? C2 Cu1 N5 106.54(15) . . ? C1 Cu1 N5 103.57(14) . . ? C3 Cu2 N2 144.71(17) . . ? C3 Cu2 N9 105.47(16) . 6_556 ? N2 Cu2 N9 109.70(15) . 6_556 ? C4 Cu3 N3 138.51(16) . . ? C4 Cu3 N7 116.38(15) . . ? N3 Cu3 N7 104.92(15) . . ? C1 C1 Cu1 173.1(5) 5_665 . ? N2 C2 Cu1 173.6(4) . . ? N3 C3 Cu2 171.7(4) . . ? C4 C4 Cu3 174.9(4) 4_556 . ? N5 C5 C6 123.2(3) . . ? N5 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 115.9(3) . . ? C8 C7 C10 122.0(3) . . ? C6 C7 C10 122.1(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? N5 C9 C8 123.4(4) . . ? N5 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? N6 C10 C11 122.4(3) . . ? N6 C10 C7 117.5(3) . . ? C11 C10 C7 120.1(3) . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C11 115.6(5) 2_665 . ? C11 C12 C13 122.2(2) 2_665 . ? C11 C12 C13 122.2(2) . . ? C14 C13 C14 116.6(5) 2_665 . ? C14 C13 C12 121.7(3) 2_665 . ? C14 C13 C12 121.7(3) . . ? C13 C14 C15 121.9(4) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C15 117.4(5) . 2_665 ? C15 C16 C17 121.3(3) . . ? C15 C16 C17 121.3(3) 2_665 . ? C18 C17 C18 117.5(5) 2_665 . ? C18 C17 C16 121.2(2) 2_665 . ? C18 C17 C16 121.2(2) . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 120.1(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C19 120.0(6) . 2_665 ? C19 C20 H20 120.0 . . ? C19 C20 H20 120.0 2_665 . ? C26 C21 C22 120.4(5) . . ? C26 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.0(5) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 122.9(5) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C25 116.4(4) . . ? C23 C24 C27 122.4(4) . . ? C25 C24 C27 121.2(4) . . ? C26 C25 C24 120.6(5) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C21 C26 C25 120.7(5) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C32 C27 C28 115.0(4) . . ? C32 C27 C24 122.9(4) . . ? C28 C27 C24 122.1(4) . . ? C27 C28 C29 122.2(4) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C30 C29 C28 122.4(4) . . ? C30 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C29 C30 C31 114.7(4) . . ? C29 C30 C33 123.5(4) . . ? C31 C30 C33 121.7(4) . . ? C32 C31 C30 123.0(4) . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C27 C32 C31 122.5(4) . . ? C27 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C34 C33 C37 115.1(4) . . ? C34 C33 C30 123.5(4) . . ? C37 C33 C30 121.4(4) . . ? C33 C34 C35 121.2(4) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? N8 C35 C34 122.1(4) . . ? N8 C35 C38 115.3(4) . . ? C34 C35 C38 122.6(4) . . ? N8 C36 C37 123.1(4) . . ? N8 C36 C43 115.4(4) . . ? C37 C36 C43 121.4(4) . . ? C36 C37 C33 121.1(4) . . ? C36 C37 H37 119.4 . . ? C33 C37 H37 119.4 . . ? C39 C38 C42 115.1(4) . . ? C39 C38 C35 123.9(4) . . ? C42 C38 C35 120.9(4) . . ? C40 C39 C38 120.7(4) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? N7 C40 C39 124.2(4) . . ? N7 C40 H40 117.9 . . ? C39 C40 H40 117.9 . . ? N7 C41 C42 124.8(5) . . ? N7 C41 H41 117.6 . . ? C42 C41 H41 117.6 . . ? C41 C42 C38 120.4(4) . . ? C41 C42 H42 119.8 . . ? C38 C42 H42 119.8 . . ? C47 C43 C44 116.6(4) . . ? C47 C43 C36 122.1(4) . . ? C44 C43 C36 121.2(4) . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? N9 C45 C44 124.0(4) . . ? N9 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? N9 C46 C47 123.5(4) . . ? N9 C46 H46 118.2 . . ? C47 C46 H46 118.2 . . ? C43 C47 C46 119.9(4) . . ? C43 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C2 N2 Cu2 179.2(4) . . ? C3 N3 Cu3 177.4(4) . . ? C5 N5 C9 116.3(3) . . ? C5 N5 Cu1 123.8(3) . . ? C9 N5 Cu1 119.7(3) . . ? C10 N6 C10 117.1(4) . 2_665 ? C41 N7 C40 114.7(4) . . ? C41 N7 Cu3 122.4(3) . . ? C40 N7 Cu3 122.8(3) . . ? C36 N8 C35 117.4(4) . . ? C45 N9 C46 116.2(4) . . ? C45 N9 Cu2 122.8(3) . 6_656 ? C46 N9 Cu2 121.1(3) . 6_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Cu1 C1 C1 -153(4) . . . 5_665 ? N5 Cu1 C1 C1 22(5) . . . 5_665 ? C1 Cu1 C2 N2 161(4) . . . . ? N5 Cu1 C2 N2 -14(4) . . . . ? N2 Cu2 C3 N3 132(3) . . . . ? N9 Cu2 C3 N3 -43(3) 6_556 . . . ? N3 Cu3 C4 C4 -27(6) . . . 4_556 ? N7 Cu3 C4 C4 147(6) . . . 4_556 ? N5 C5 C6 C7 0.3(7) . . . . ? C5 C6 C7 C8 0.7(6) . . . . ? C5 C6 C7 C10 -178.8(4) . . . . ? C6 C7 C8 C9 -0.2(7) . . . . ? C10 C7 C8 C9 179.3(4) . . . . ? C7 C8 C9 N5 -1.4(8) . . . . ? C8 C7 C10 N6 157.8(4) . . . . ? C6 C7 C10 N6 -22.7(6) . . . . ? C8 C7 C10 C11 -22.8(7) . . . . ? C6 C7 C10 C11 156.7(4) . . . . ? N6 C10 C11 C12 -1.8(6) . . . . ? C7 C10 C11 C12 178.8(3) . . . . ? C10 C11 C12 C11 0.9(3) . . . 2_665 ? C10 C11 C12 C13 -179.1(3) . . . . ? C11 C12 C13 C14 151.8(3) 2_665 . . 2_665 ? C11 C12 C13 C14 -28.2(3) . . . 2_665 ? C11 C12 C13 C14 -28.2(3) 2_665 . . . ? C11 C12 C13 C14 151.8(3) . . . . ? C14 C13 C14 C15 0.7(4) 2_665 . . . ? C12 C13 C14 C15 -179.3(4) . . . . ? C13 C14 C15 C16 -1.3(7) . . . . ? C14 C15 C16 C15 0.6(3) . . . 2_665 ? C14 C15 C16 C17 -179.4(3) . . . . ? C15 C16 C17 C18 166.6(3) . . . 2_665 ? C15 C16 C17 C18 -13.4(3) 2_665 . . 2_665 ? C15 C16 C17 C18 -13.4(3) . . . . ? C15 C16 C17 C18 166.6(3) 2_665 . . . ? C18 C17 C18 C19 -0.7(4) 2_665 . . . ? C16 C17 C18 C19 179.3(4) . . . . ? C17 C18 C19 C20 1.5(7) . . . . ? C18 C19 C20 C19 -0.7(3) . . . 2_665 ? C26 C21 C22 C23 0.9(9) . . . . ? C21 C22 C23 C24 -1.5(8) . . . . ? C22 C23 C24 C25 1.2(7) . . . . ? C22 C23 C24 C27 -177.9(5) . . . . ? C23 C24 C25 C26 -0.4(8) . . . . ? C27 C24 C25 C26 178.8(5) . . . . ? C22 C21 C26 C25 -0.1(9) . . . . ? C24 C25 C26 C21 -0.2(9) . . . . ? C23 C24 C27 C32 145.2(5) . . . . ? C25 C24 C27 C32 -33.9(7) . . . . ? C23 C24 C27 C28 -36.0(7) . . . . ? C25 C24 C27 C28 145.0(5) . . . . ? C32 C27 C28 C29 -2.5(8) . . . . ? C24 C27 C28 C29 178.6(5) . . . . ? C27 C28 C29 C30 1.2(9) . . . . ? C28 C29 C30 C31 0.5(8) . . . . ? C28 C29 C30 C33 177.7(4) . . . . ? C29 C30 C31 C32 -0.9(8) . . . . ? C33 C30 C31 C32 -178.2(5) . . . . ? C28 C27 C32 C31 2.1(8) . . . . ? C24 C27 C32 C31 -179.0(5) . . . . ? C30 C31 C32 C27 -0.5(9) . . . . ? C29 C30 C33 C34 0.2(7) . . . . ? C31 C30 C33 C34 177.2(4) . . . . ? C29 C30 C33 C37 -178.2(4) . . . . ? C31 C30 C33 C37 -1.2(6) . . . . ? C37 C33 C34 C35 0.2(6) . . . . ? C30 C33 C34 C35 -178.3(4) . . . . ? C33 C34 C35 N8 -0.4(6) . . . . ? C33 C34 C35 C38 -178.4(4) . . . . ? N8 C36 C37 C33 2.3(6) . . . . ? C43 C36 C37 C33 -176.5(4) . . . . ? C34 C33 C37 C36 -1.1(6) . . . . ? C30 C33 C37 C36 177.4(4) . . . . ? N8 C35 C38 C39 165.9(4) . . . . ? C34 C35 C38 C39 -16.0(7) . . . . ? N8 C35 C38 C42 -15.3(6) . . . . ? C34 C35 C38 C42 162.9(5) . . . . ? C42 C38 C39 C40 0.1(7) . . . . ? C35 C38 C39 C40 179.0(4) . . . . ? C38 C39 C40 N7 -1.7(7) . . . . ? N7 C41 C42 C38 -0.8(10) . . . . ? C39 C38 C42 C41 1.0(8) . . . . ? C35 C38 C42 C41 -177.9(5) . . . . ? N8 C36 C43 C47 -161.8(4) . . . . ? C37 C36 C43 C47 17.1(6) . . . . ? N8 C36 C43 C44 18.2(6) . . . . ? C37 C36 C43 C44 -162.9(4) . . . . ? C47 C43 C44 C45 0.8(7) . . . . ? C36 C43 C44 C45 -179.2(4) . . . . ? C43 C44 C45 N9 -0.3(8) . . . . ? C44 C43 C47 C46 -0.8(7) . . . . ? C36 C43 C47 C46 179.2(4) . . . . ? N9 C46 C47 C43 0.3(8) . . . . ? Cu1 C2 N2 Cu2 125(27) . . . . ? C3 Cu2 N2 C2 -101(29) . . . . ? N9 Cu2 N2 C2 74(29) 6_556 . . . ? Cu2 C3 N3 Cu3 -21(13) . . . . ? C4 Cu3 N3 C3 33(10) . . . . ? N7 Cu3 N3 C3 -141(10) . . . . ? C6 C5 N5 C9 -1.8(6) . . . . ? C6 C5 N5 Cu1 175.2(3) . . . . ? C8 C9 N5 C5 2.4(7) . . . . ? C8 C9 N5 Cu1 -174.8(4) . . . . ? C2 Cu1 N5 C5 -2.6(4) . . . . ? C1 Cu1 N5 C5 -179.9(3) . . . . ? C2 Cu1 N5 C9 174.3(3) . . . . ? C1 Cu1 N5 C9 -3.0(4) . . . . ? C11 C10 N6 C10 0.9(3) . . . 2_665 ? C7 C10 N6 C10 -179.7(4) . . . 2_665 ? C42 C41 N7 C40 -0.7(9) . . . . ? C42 C41 N7 Cu3 177.7(5) . . . . ? C39 C40 N7 C41 2.0(7) . . . . ? C39 C40 N7 Cu3 -176.5(3) . . . . ? C4 Cu3 N7 C41 -5.1(5) . . . . ? N3 Cu3 N7 C41 170.9(4) . . . . ? C4 Cu3 N7 C40 173.2(4) . . . . ? N3 Cu3 N7 C40 -10.8(4) . . . . ? C37 C36 N8 C35 -2.4(6) . . . . ? C43 C36 N8 C35 176.5(4) . . . . ? C34 C35 N8 C36 1.5(6) . . . . ? C38 C35 N8 C36 179.6(3) . . . . ? C44 C45 N9 C46 -0.3(7) . . . . ? C44 C45 N9 Cu2 179.0(4) . . . 6_656 ? C47 C46 N9 C45 0.3(7) . . . . ? C47 C46 N9 Cu2 -179.0(4) . . . 6_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.070 # 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 0.376 0.250 0.250 134.7 21.9 2 0.876 0.250 0.750 134.7 22.2 3 0.193 0.250 0.750 19.0 6.2 4 0.693 0.250 0.250 19.0 6.2 5 0.124 0.750 0.250 134.8 21.6 6 0.624 0.750 0.750 134.7 21.5 7 0.307 0.750 0.750 19.0 6.3 8 0.807 0.750 0.250 19.0 6.4 _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT220_3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.10 Ratio RESPONSE: The disordered group propyl shows much larger ADPs than the very rigidly bonded carbon ; _vrf_PLAT242_3 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C71' RESPONSE: it is explained by the strong disorder of the group propyl and its rotation around bond C-C. ; # end Validation Reply Form #End of Crystallographic Information File