# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ivan Huc' 'Gerald Linti' 'Victor Maurizot' _publ_contact_author_name 'Dr Ivan Huc' _publ_contact_author_address ; Institut Europeen de Chimie et Biologie 2 rue Robert Escarpit Pessac 33607 FRANCE ; _publ_contact_author_email I.HUC@IECB.U-BORDEAUX.FR _publ_contact_author_phone ' ' _publ_contact_author_fax '+33 (0)540 003009' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Solid state characterization of oligopyridine dicarboxamide helicates ; data_vm2 _database_code_depnum_ccdc_archive 'CCDC 228224' _publ_manuscript_creation 'RTF-File created by CIF6 (H.Schwenk 1996)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H33 Cu N7 O6' _chemical_formula_weight 675.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting moniclinic _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 20.896(4) _cell_length_b 14.040(3) _cell_length_c 24.185(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.42(3) _cell_angle_gamma 90.00 _cell_volume 6559(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22406 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.96 _reflns_number_total 5007 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5007 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 1.071 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.42887(2) 0.29728(3) 1.279078(16) 0.02371(16) Uani 1 1 d . . . N1 N 1.25348(19) 0.3388(2) 1.05660(13) 0.0328(7) Uani 1 1 d . . . N2 N 1.28598(15) 0.2884(2) 1.15284(12) 0.0290(7) Uani 1 1 d . . . N3 N 1.33264(15) 0.2375(2) 1.25078(12) 0.0315(7) Uani 1 1 d . . . N4 N 1.44682(15) 0.1892(2) 1.33123(12) 0.0304(7) Uani 1 1 d . . . N5 N 1.53547(14) 0.30812(18) 1.32419(11) 0.0217(6) Uani 1 1 d . . . N6 N 1.59227(14) 0.40466(18) 1.27862(11) 0.0207(6) Uani 1 1 d . . . N7 N 1.65707(17) 0.4958(2) 1.23404(13) 0.0310(7) Uani 1 1 d . . . O1 O 1.17619(14) 0.45242(19) 1.00684(11) 0.0423(7) Uani 1 1 d . . . O2 O 1.27356(14) 0.1134(2) 1.27416(13) 0.0515(8) Uani 1 1 d . . . O3 O 1.48073(13) -0.05385(17) 1.42977(11) 0.0380(6) Uani 1 1 d . . . O4 O 1.61448(12) 0.25572(18) 1.41706(10) 0.0354(6) Uani 1 1 d . . . O5 O 1.58221(14) 0.4107(2) 1.15692(10) 0.0418(7) Uani 1 1 d . . . C1 C 1.2621(2) 0.4078(3) 0.96891(18) 0.0470(10) Uani 1 1 d . . . H1B H 1.2735 0.4743 0.9641 0.070 Uiso 1 1 calc R . . H1C H 1.2316 0.3823 0.9301 0.070 Uiso 1 1 calc R . . H1D H 1.3048 0.3701 0.9844 0.070 Uiso 1 1 calc R . . C2 C 1.2260(2) 0.4029(3) 1.01223(15) 0.0329(8) Uani 1 1 d . . . C3 C 1.23347(18) 0.3216(2) 1.10473(15) 0.0273(8) Uani 1 1 d . . . C4 C 1.16710(19) 0.3342(3) 1.10285(16) 0.0338(8) Uani 1 1 d . . . H4A H 1.1307 0.3559 1.0676 0.041 Uiso 1 1 calc R . . C5 C 1.1557(2) 0.3140(3) 1.15437(18) 0.0387(9) Uani 1 1 d . . . H5A H 1.1108 0.3224 1.1549 0.046 Uiso 1 1 calc R . . C6 C 1.2089(2) 0.2819(3) 1.20485(17) 0.0382(9) Uani 1 1 d . . . H6A H 1.2019 0.2691 1.2407 0.046 Uiso 1 1 calc R . . C7 C 1.27312(18) 0.2690(2) 1.20154(15) 0.0297(8) Uani 1 1 d . . . C8 C 1.32572(19) 0.1610(3) 1.28070(16) 0.0351(9) Uani 1 1 d . . . C9 C 1.39394(19) 0.1310(3) 1.32758(16) 0.0335(9) Uani 1 1 d . . . C10 C 1.4049(2) 0.0509(3) 1.36177(16) 0.0365(9) Uani 1 1 d . . . H10A H 1.3675 0.0106 1.3596 0.044 Uiso 1 1 calc R . . C11 C 1.47306(19) 0.0297(2) 1.40031(15) 0.0337(9) Uani 1 1 d . . . C12 C 1.52622(19) 0.0921(2) 1.40641(15) 0.0318(8) Uani 1 1 d . . . H12A H 1.5720 0.0805 1.4341 0.038 Uiso 1 1 calc R . . C13 C 1.50993(18) 0.1727(2) 1.37034(15) 0.0290(8) Uani 1 1 d . . . C14 C 1.5499(2) -0.0918(3) 1.45864(17) 0.0384(9) Uani 1 1 d . . . H14A H 1.5724 -0.0659 1.4996 0.046 Uiso 1 1 calc R . . H14B H 1.5787 -0.0755 1.4356 0.046 Uiso 1 1 calc R . . C15 C 1.5411(2) -0.1976(3) 1.46040(16) 0.0349(9) Uani 1 1 d . . . C16 C 1.5470(2) -0.2441(3) 1.51222(18) 0.0463(10) Uani 1 1 d . . . H16A H 1.5590 -0.2093 1.5484 0.056 Uiso 1 1 calc R . . C17 C 1.5354(3) -0.3420(3) 1.5120(2) 0.0580(13) Uani 1 1 d . . . H17A H 1.5398 -0.3737 1.5479 0.070 Uiso 1 1 calc R . . C18 C 1.5176(3) -0.3922(3) 1.4598(2) 0.0555(12) Uani 1 1 d . . . H18A H 1.5089 -0.4586 1.4593 0.067 Uiso 1 1 calc R . . C19 C 1.5125(2) -0.3463(3) 1.40807(19) 0.0491(11) Uani 1 1 d . . . H19A H 1.5008 -0.3813 1.3719 0.059 Uiso 1 1 calc R . . C20 C 1.5242(2) -0.2499(3) 1.40840(17) 0.0395(9) Uani 1 1 d . . . H20A H 1.5206 -0.2189 1.3724 0.047 Uiso 1 1 calc R . . C21 C 1.56001(17) 0.2511(2) 1.37273(14) 0.0264(8) Uani 1 1 d . . . C22 C 1.57457(16) 0.3907(2) 1.32648(13) 0.0200(7) Uani 1 1 d . . . C23 C 1.59419(18) 0.4522(2) 1.37436(14) 0.0281(8) Uani 1 1 d . . . H23A H 1.5782 0.4433 1.4059 0.034 Uiso 1 1 calc R . . C24 C 1.6372(2) 0.5267(2) 1.37573(16) 0.0337(9) Uani 1 1 d . . . H24A H 1.6524 0.5689 1.4089 0.040 Uiso 1 1 calc R . . C25 C 1.6583(2) 0.5401(2) 1.32909(15) 0.0323(8) Uani 1 1 d . . . H25A H 1.6892 0.5903 1.3301 0.039 Uiso 1 1 calc R . . C26 C 1.63365(17) 0.4790(2) 1.28046(13) 0.0223(7) Uani 1 1 d . . . C27 C 1.6306(2) 0.4662(3) 1.17679(15) 0.0359(9) Uani 1 1 d . . . C28 C 1.6651(3) 0.5091(4) 1.13804(19) 0.0628(14) Uani 1 1 d . . . H28A H 1.6322 0.5103 1.0963 0.094 Uiso 1 1 calc R . . H28B H 1.7055 0.4707 1.1412 0.094 Uiso 1 1 calc R . . H28C H 1.6799 0.5743 1.1514 0.094 Uiso 1 1 calc R . . O8 O 1.8053(5) 0.3853(8) 1.1389(4) 0.107(3) Uani 0.50 1 d P A 1 C50 C 1.7292(11) 0.258(2) 1.088(2) 0.105(12) Uani 0.25 1 d P A 1 C50A C 1.752(2) 0.242(2) 1.041(2) 0.132(14) Uani 0.25 1 d P . 1 C51 C 1.779(2) 0.2953(14) 1.0955(19) 0.245(17) Uani 0.50 1 d P A 1 C52 C 1.8693(11) 0.5182(14) 1.1974(8) 0.131(7) Uani 0.50 1 d P A 1 H52A H 1.9176 0.5394 1.2153 0.196 Uiso 0.50 1 calc PR A 1 H52B H 1.8494 0.5172 1.2282 0.196 Uiso 0.50 1 calc PR A 1 H52C H 1.8427 0.5620 1.1654 0.196 Uiso 0.50 1 calc PR A 1 C53 C 1.8668(12) 0.4304(18) 1.1749(12) 0.199(14) Uani 0.50 1 d P A 1 H53A H 1.8896 0.3877 1.2094 0.239 Uiso 0.50 1 calc PR A 1 H53B H 1.8968 0.4315 1.1516 0.239 Uiso 0.50 1 calc PR A 1 O9 O 1.9631(4) 0.3354(6) 1.2315(3) 0.080(2) Uani 0.50 1 d P . 2 C54 C 1.9329(11) 0.4961(10) 1.2134(8) 0.115(6) Uani 0.50 1 d P B 2 H54A H 1.8950 0.5409 1.1936 0.172 Uiso 0.50 1 calc PR B 2 H54B H 1.9656 0.4970 1.1932 0.172 Uiso 0.50 1 calc PR B 2 H54C H 1.9568 0.5149 1.2553 0.172 Uiso 0.50 1 calc PR B 2 C55 C 1.9042(8) 0.3982(11) 1.2106(7) 0.095(4) Uani 0.50 1 d P B 2 H55A H 1.8772 0.3932 1.2364 0.114 Uiso 0.50 1 calc PR B 2 H55B H 1.8735 0.3820 1.1691 0.114 Uiso 0.50 1 calc PR B 2 C56 C 1.9464(6) 0.2379(8) 1.2300(5) 0.066(3) Uani 0.50 1 d P C 2 H56A H 1.9179 0.2281 1.2542 0.079 Uiso 0.50 1 calc PR C 2 H56B H 1.9178 0.2200 1.1883 0.079 Uiso 0.50 1 calc PR C 2 C57 C 2.0000 0.1811(8) 1.2500 0.102(3) Uani 1 2 d S . 2 H7 H 1.684(2) 0.537(3) 1.2417(17) 0.035(11) Uiso 1 1 d . . . H1 H 1.287(2) 0.315(3) 1.0607(16) 0.022(11) Uiso 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 0.0151(3) 0.0212(2) 0.0309(2) 0.00734(16) 0.00439(17) -0.00197(16) N1 0.022(2) 0.0356(18) 0.0357(17) 0.0036(13) 0.0054(14) 0.0113(15) N2 0.0183(17) 0.0258(15) 0.0362(16) 0.0033(12) 0.0030(12) 0.0007(12) N3 0.0167(17) 0.0322(17) 0.0375(16) 0.0141(13) 0.0013(12) -0.0027(12) N4 0.0158(17) 0.0313(16) 0.0362(16) 0.0096(12) 0.0011(12) -0.0076(12) N5 0.0180(16) 0.0163(13) 0.0291(14) 0.0035(10) 0.0072(11) -0.0031(11) N6 0.0165(16) 0.0173(13) 0.0267(13) 0.0011(10) 0.0064(11) 0.0004(11) N7 0.0265(19) 0.0370(18) 0.0323(16) -0.0030(13) 0.0144(13) -0.0173(15) O1 0.0335(17) 0.0396(15) 0.0429(14) 0.0067(12) 0.0023(12) 0.0122(13) O2 0.0225(17) 0.0498(17) 0.0641(18) 0.0278(14) -0.0037(12) -0.0170(13) O3 0.0253(15) 0.0261(13) 0.0515(15) 0.0194(11) 0.0022(11) -0.0055(11) O4 0.0194(15) 0.0382(14) 0.0383(13) 0.0123(11) -0.0006(11) -0.0083(11) O5 0.0415(18) 0.0520(17) 0.0312(13) -0.0073(12) 0.0130(12) -0.0198(14) C1 0.045(3) 0.049(3) 0.045(2) 0.0079(19) 0.015(2) 0.008(2) C2 0.025(2) 0.0284(19) 0.0351(19) -0.0013(15) -0.0003(15) 0.0012(17) C3 0.021(2) 0.0212(17) 0.0331(18) -0.0013(13) 0.0029(14) 0.0017(14) C4 0.020(2) 0.0313(19) 0.041(2) 0.0043(16) 0.0019(15) 0.0056(15) C5 0.018(2) 0.040(2) 0.055(2) 0.0113(18) 0.0111(17) 0.0051(16) C6 0.023(2) 0.045(2) 0.044(2) 0.0166(17) 0.0091(17) 0.0008(17) C7 0.016(2) 0.0251(18) 0.0399(19) 0.0070(14) 0.0009(15) -0.0031(14) C8 0.021(2) 0.034(2) 0.043(2) 0.0130(16) 0.0044(16) -0.0064(17) C9 0.020(2) 0.0295(19) 0.042(2) 0.0105(15) 0.0020(15) -0.0078(15) C10 0.024(2) 0.031(2) 0.047(2) 0.0138(16) 0.0048(16) -0.0098(16) C11 0.028(2) 0.0251(19) 0.0406(19) 0.0102(15) 0.0050(16) -0.0057(15) C12 0.021(2) 0.0277(19) 0.0373(19) 0.0127(15) -0.0001(15) -0.0030(15) C13 0.018(2) 0.0266(18) 0.0364(18) 0.0077(14) 0.0034(15) -0.0055(14) C14 0.026(2) 0.032(2) 0.046(2) 0.0137(16) 0.0010(17) -0.0029(16) C15 0.026(2) 0.034(2) 0.041(2) 0.0130(16) 0.0080(16) 0.0006(16) C16 0.058(3) 0.036(2) 0.041(2) 0.0092(17) 0.014(2) 0.001(2) C17 0.086(4) 0.037(2) 0.058(3) 0.021(2) 0.035(3) 0.003(2) C18 0.081(4) 0.030(2) 0.067(3) 0.008(2) 0.040(3) 0.001(2) C19 0.063(3) 0.035(2) 0.053(2) 0.0001(19) 0.026(2) 0.003(2) C20 0.037(3) 0.038(2) 0.041(2) 0.0108(17) 0.0129(17) 0.0031(18) C21 0.017(2) 0.0237(18) 0.0370(19) 0.0043(14) 0.0084(16) -0.0038(14) C22 0.0086(17) 0.0188(16) 0.0315(17) 0.0051(13) 0.0065(13) -0.0002(12) C23 0.030(2) 0.0275(18) 0.0292(17) -0.0041(14) 0.0138(15) -0.0049(15) C24 0.037(2) 0.029(2) 0.0360(19) -0.0095(15) 0.0138(16) -0.0089(16) C25 0.037(2) 0.0234(18) 0.0374(19) -0.0046(14) 0.0150(17) -0.0131(16) C26 0.0170(19) 0.0211(17) 0.0300(16) 0.0004(13) 0.0102(14) -0.0037(13) C27 0.034(2) 0.046(2) 0.0306(18) -0.0003(16) 0.0155(16) -0.0054(19) C28 0.054(3) 0.100(4) 0.043(2) -0.004(2) 0.029(2) -0.029(3) O8 0.092(8) 0.109(8) 0.106(7) -0.004(6) 0.024(6) 0.022(6) C50 0.000(12) 0.073(18) 0.21(3) -0.01(2) -0.002(14) -0.003(10) C50A 0.10(3) 0.037(15) 0.21(4) 0.03(2) 0.01(3) 0.001(15) C51 0.31(4) 0.055(12) 0.44(5) 0.01(2) 0.23(4) 0.079(18) C52 0.148(19) 0.122(15) 0.116(12) -0.053(11) 0.043(12) 0.001(13) C53 0.118(19) 0.14(2) 0.23(3) -0.008(19) -0.050(18) 0.055(15) O9 0.076(6) 0.081(5) 0.083(5) -0.016(4) 0.031(4) -0.005(4) C54 0.180(19) 0.067(9) 0.146(14) -0.004(9) 0.117(15) -0.009(11) C55 0.073(11) 0.106(11) 0.117(11) -0.002(9) 0.048(9) 0.008(9) C56 0.067(8) 0.061(7) 0.066(6) -0.004(5) 0.019(5) -0.010(5) C57 0.128(10) 0.094(7) 0.061(5) 0.000 0.011(5) 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 N4 1.916(3) . ? Cu1 N6 1.986(3) 2_857 ? Cu1 N3 2.041(3) . ? Cu1 N5 2.079(3) . ? Cu1 O5 2.293(3) 2_857 ? N1 C2 1.349(5) . ? N1 C3 1.400(5) . ? N2 C7 1.333(5) . ? N2 C3 1.342(4) . ? N3 C8 1.333(5) . ? N3 C7 1.425(4) . ? N4 C13 1.318(5) . ? N4 C9 1.350(4) . ? N5 C21 1.350(4) . ? N5 C22 1.407(4) . ? N6 C26 1.345(4) . ? N6 C22 1.357(4) . ? N6 Cu1 1.986(3) 2_857 ? N7 C27 1.346(5) . ? N7 C26 1.405(4) . ? O1 C2 1.216(4) . ? O2 C8 1.237(4) . ? O3 C11 1.350(4) . ? O3 C14 1.447(5) . ? O4 C21 1.232(4) . ? O5 C27 1.221(5) . ? O5 Cu1 2.293(3) 2_857 ? C1 C2 1.509(6) . ? C3 C4 1.382(5) . ? C4 C5 1.385(5) . ? C5 C6 1.377(5) . ? C6 C7 1.386(5) . ? C8 C9 1.504(5) . ? C9 C10 1.362(5) . ? C10 C11 1.405(5) . ? C11 C12 1.378(5) . ? C12 C13 1.390(5) . ? C13 C21 1.505(5) . ? C14 C15 1.500(5) . ? C15 C16 1.377(5) . ? C15 C20 1.381(5) . ? C16 C17 1.395(6) . ? C17 C18 1.367(6) . ? C18 C19 1.375(6) . ? C19 C20 1.374(6) . ? C22 C23 1.376(4) . ? C23 C24 1.370(5) . ? C24 C25 1.372(5) . ? C25 C26 1.386(5) . ? C27 C28 1.508(5) . ? O8 C53 1.40(2) . ? O8 C51 1.60(3) . ? C50 C51 1.11(4) . ? C50 C50A 1.40(6) . ? C50A C51 1.43(5) . ? C50A C50A 1.98(10) 7_857 ? C52 C53 1.34(3) . ? O9 C56 1.410(13) . ? O9 C55 1.440(16) . ? O9 O9 1.458(16) 2_957 ? C54 C55 1.49(2) . ? C56 C57 1.309(12) . ? C57 C56 1.309(12) 2_957 ? 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 N4 Cu1 N6 176.95(11) . 2_857 ? N4 Cu1 N3 79.38(12) . . ? N6 Cu1 N3 98.62(11) 2_857 . ? N4 Cu1 N5 79.10(11) . . ? N6 Cu1 N5 102.70(11) 2_857 . ? N3 Cu1 N5 158.04(11) . . ? N4 Cu1 O5 98.64(11) . 2_857 ? N6 Cu1 O5 83.95(10) 2_857 2_857 ? N3 Cu1 O5 99.89(12) . 2_857 ? N5 Cu1 O5 87.63(10) . 2_857 ? C2 N1 C3 127.2(4) . . ? C7 N2 C3 117.6(3) . . ? C8 N3 C7 117.6(3) . . ? C8 N3 Cu1 116.5(2) . . ? C7 N3 Cu1 125.9(2) . . ? C13 N4 C9 120.7(3) . . ? C13 N4 Cu1 120.2(2) . . ? C9 N4 Cu1 119.1(2) . . ? C21 N5 C22 115.6(3) . . ? C21 N5 Cu1 112.9(2) . . ? C22 N5 Cu1 124.8(2) . . ? C26 N6 C22 117.7(3) . . ? C26 N6 Cu1 125.5(2) . 2_857 ? C22 N6 Cu1 115.4(2) . 2_857 ? C27 N7 C26 129.7(3) . . ? C11 O3 C14 118.1(3) . . ? C27 O5 Cu1 117.3(2) . 2_857 ? O1 C2 N1 123.6(4) . . ? O1 C2 C1 122.3(3) . . ? N1 C2 C1 114.1(4) . . ? N2 C3 C4 123.5(3) . . ? N2 C3 N1 112.1(3) . . ? C4 C3 N1 124.4(3) . . ? C3 C4 C5 117.4(3) . . ? C6 C5 C4 120.4(4) . . ? C5 C6 C7 117.7(4) . . ? N2 C7 C6 123.4(3) . . ? N2 C7 N3 113.3(3) . . ? C6 C7 N3 123.2(3) . . ? O2 C8 N3 129.7(3) . . ? O2 C8 C9 118.7(3) . . ? N3 C8 C9 111.5(3) . . ? N4 C9 C10 121.1(3) . . ? N4 C9 C8 113.3(3) . . ? C10 C9 C8 125.5(3) . . ? C9 C10 C11 118.1(3) . . ? O3 C11 C12 124.6(3) . . ? O3 C11 C10 114.9(3) . . ? C12 C11 C10 120.6(3) . . ? C11 C12 C13 117.1(3) . . ? N4 C13 C12 122.2(3) . . ? N4 C13 C21 112.9(3) . . ? C12 C13 C21 124.8(3) . . ? O3 C14 C15 105.5(3) . . ? C16 C15 C20 118.7(4) . . ? C16 C15 C14 121.8(4) . . ? C20 C15 C14 119.5(3) . . ? C15 C16 C17 120.6(4) . . ? C18 C17 C16 119.8(4) . . ? C17 C18 C19 119.9(4) . . ? C20 C19 C18 120.3(4) . . ? C19 C20 C15 120.8(3) . . ? O4 C21 N5 130.1(3) . . ? O4 C21 C13 118.1(3) . . ? N5 C21 C13 111.9(3) . . ? N6 C22 C23 122.4(3) . . ? N6 C22 N5 115.4(3) . . ? C23 C22 N5 122.2(3) . . ? C24 C23 C22 118.8(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 118.7(3) . . ? N6 C26 C25 122.3(3) . . ? N6 C26 N7 121.2(3) . . ? C25 C26 N7 116.4(3) . . ? O5 C27 N7 123.7(3) . . ? O5 C27 C28 122.0(3) . . ? N7 C27 C28 114.2(4) . . ? C53 O8 C51 140.7(18) . . ? C51 C50 C50A 68(3) . . ? C50 C50A C51 46(2) . . ? C50 C50A C50A 153(4) . 7_857 ? C51 C50A C50A 136(3) . 7_857 ? C50 C51 C50A 66(3) . . ? C50 C51 O8 123(4) . . ? C50A C51 O8 159(3) . . ? C52 C53 O8 124(2) . . ? C56 O9 C55 114.5(10) . . ? C56 O9 O9 102.1(6) . 2_957 ? C55 O9 O9 141.1(7) . 2_957 ? O9 C55 C54 105.8(14) . . ? C57 C56 O9 114.4(10) . . ? C56 C57 C56 104.9(13) 2_957 . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.96 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.830 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.107 data_vm273o _database_code_depnum_ccdc_archive 'CCDC 228225' _publ_manuscript_creation 'RTF-File created by CIF6 (H.Schwenk 1996)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H47 N15 O11 Cu3 x C2H6OS x 1/8NaO2C2H6 x 5/8 CH4O x 1/4 C2H6O' _chemical_formula_sum 'C69.13 H57.38 Cu3 N15 Na0.13 O13 S' _chemical_formula_weight 1531.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 32.177(6) _cell_length_b 15.395(3) _cell_length_c 29.607(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14666(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6284 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83122 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.00 _reflns_number_total 11402 _reflns_number_gt 6612 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11402 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2067 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 1.336 _refine_ls_shift/su_mean 0.029 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 0.128131(16) 0.56486(4) 0.302505(18) 0.03612(14) Uani 1 1 d . . . Cu2 Cu 0.201323(16) 0.69885(4) 0.243519(19) 0.03802(15) Uani 1 1 d . . . Cu3 Cu 0.085859(18) 0.35069(4) 0.32019(2) 0.04511(16) Uani 1 1 d . . . S1 S 0.08860(6) 0.43949(12) 0.62331(6) 0.0795(5) Uani 1 1 d . . . O1 O -0.08877(14) 0.4231(3) 0.17198(16) 0.0901(15) Uani 1 1 d . . . O2 O -0.00539(14) 0.2619(3) 0.40586(15) 0.0995(16) Uani 1 1 d . . . O3 O 0.1246(2) 0.2502(5) 0.51190(16) 0.146(3) Uani 1 1 d . C . O4 O 0.20230(15) 0.3808(3) 0.37640(19) 0.1114(18) Uani 1 1 d . . . O5 O 0.15564(13) 0.5374(2) 0.14716(13) 0.0711(12) Uani 1 1 d . . . O6 O 0.12159(12) 0.8481(3) 0.07778(12) 0.0669(11) Uani 1 1 d . . . O7 O 0.19129(11) 0.9596(2) 0.22373(12) 0.0580(10) Uani 1 1 d . . . O8 O 0.01174(10) 0.8065(2) 0.39741(12) 0.0574(10) Uani 1 1 d . . . O9 O 0.00590(9) 0.5754(2) 0.27054(11) 0.0497(9) Uani 1 1 d . . . O10 O 0.11016(14) 0.2231(3) 0.29844(14) 0.0737(13) Uani 1 1 d . . . O11 O 0.17287(10) 0.7334(2) 0.39633(11) 0.0496(9) Uani 1 1 d . . . O12 O 0.0872(4) 0.4262(7) 0.5651(3) 0.228(5) Uani 1 1 d . . . O13 O 0.1242(3) 0.9812(8) 0.4093(4) 0.050(4) Uani 0.25 1 d PD A 1 H13A H 0.1022 0.9757 0.3943 0.075 Uiso 0.25 1 calc PR A 1 O14 O 0.2220(7) 0.733(3) 0.5279(13) 0.091(12) Uani 0.13 1 d P . . O15 O 0.2067(7) 1.1492(14) 0.3408(8) 0.102(11) Uani 0.13 1 d PD B 1 N1 N -0.03930(14) 0.4462(3) 0.22455(16) 0.0661(14) Uani 1 1 d . . . H1 H -0.0205 0.4846 0.2326 0.079 Uiso 1 1 calc R . . N2 N -0.00960(12) 0.3723(3) 0.28226(15) 0.0528(12) Uani 1 1 d . . . N3 N 0.02851(13) 0.3116(3) 0.34084(14) 0.0534(12) Uani 1 1 d . . . N4 N 0.09613(14) 0.3306(3) 0.38319(15) 0.0542(12) Uani 1 1 d . . . N5 N 0.14639(13) 0.3931(3) 0.32685(14) 0.0522(12) Uani 1 1 d . . . N6 N 0.16614(11) 0.4863(2) 0.27091(14) 0.0429(11) Uani 1 1 d . . . N7 N 0.17964(12) 0.5901(3) 0.21519(14) 0.0478(11) Uani 1 1 d . . . N8 N 0.17568(12) 0.7441(3) 0.18975(13) 0.0430(11) Uani 1 1 d . . . N9 N 0.21004(11) 0.8251(2) 0.25273(13) 0.0399(10) Uani 1 1 d . . . N10 N 0.23114(10) 0.6504(2) 0.29653(13) 0.0354(9) Uani 1 1 d . . . N11 N 0.16935(11) 0.6375(2) 0.33610(13) 0.0391(10) Uani 1 1 d . . . N12 N 0.09168(10) 0.6418(2) 0.33396(12) 0.0355(10) Uani 1 1 d . . . N13 N 0.07317(11) 0.5202(2) 0.28061(12) 0.0386(10) Uani 1 1 d . . . N14 N 0.07955(12) 0.3787(3) 0.25384(13) 0.0424(10) Uani 1 1 d . . . N18 N 0.09053(15) 0.2356(3) 0.22475(16) 0.0624(14) Uani 1 1 d . . . H18B H 0.0860 0.2032 0.2008 0.075 Uiso 1 1 calc R . . C1 C -0.0482(2) 0.5524(5) 0.1677(2) 0.087(2) Uani 1 1 d . . . H1A H -0.0730 0.5839 0.1576 0.130 Uiso 1 1 calc R . . H1B H -0.0300 0.5413 0.1418 0.130 Uiso 1 1 calc R . . H1C H -0.0333 0.5872 0.1902 0.130 Uiso 1 1 calc R . . C2 C -0.06090(18) 0.4681(5) 0.1883(2) 0.0707(19) Uani 1 1 d . . . C3 C -0.04098(15) 0.3729(4) 0.25234(19) 0.0568(15) Uani 1 1 d . . . C4 C -0.07130(17) 0.3084(4) 0.2511(2) 0.0685(18) Uani 1 1 d . . . H4A H -0.0932 0.3088 0.2296 0.082 Uiso 1 1 calc R . . C5 C -0.06753(18) 0.2444(4) 0.2828(2) 0.079(2) Uani 1 1 d . . . H5A H -0.0878 0.1995 0.2832 0.095 Uiso 1 1 calc R . . C6 C -0.03648(17) 0.2413(4) 0.3137(2) 0.0717(19) Uani 1 1 d . . . H6A H -0.0348 0.1956 0.3352 0.086 Uiso 1 1 calc R . . C7 C -0.00724(16) 0.3076(3) 0.31277(19) 0.0549(15) Uani 1 1 d . . . C8 C 0.0266(2) 0.2881(4) 0.3850(2) 0.0680(18) Uani 1 1 d . . . C9 C 0.0668(2) 0.2959(4) 0.4087(2) 0.0667(18) Uani 1 1 d . . . C10 C 0.0763(2) 0.2683(5) 0.4530(2) 0.092(2) Uani 1 1 d . . . H10A H 0.0555 0.2435 0.4717 0.110 Uiso 1 1 calc R . . C11 C 0.1178(2) 0.2784(6) 0.4691(2) 0.093(3) Uani 1 1 d . . . C12 C 0.1475(3) 0.3137(5) 0.4429(2) 0.090(2) Uani 1 1 d . . . H12A H 0.1754 0.3202 0.4529 0.108 Uiso 1 1 calc R . . C13 C 0.1347(2) 0.3401(4) 0.3999(2) 0.0683(18) Uani 1 1 d . . . C14 C 0.1643(2) 0.3738(4) 0.3665(2) 0.0709(19) Uani 1 1 d . . . C15 C 0.17231(15) 0.4094(3) 0.2906(2) 0.0540(15) Uani 1 1 d . . . C16 C 0.2012(2) 0.3504(4) 0.2731(3) 0.089(2) Uani 1 1 d . . . H16A H 0.2053 0.2959 0.2874 0.107 Uiso 1 1 calc R . . C17 C 0.2230(2) 0.3711(4) 0.2359(3) 0.118(3) Uani 1 1 d . . . H17A H 0.2430 0.3316 0.2243 0.141 Uiso 1 1 calc R . . C18 C 0.21653(19) 0.4489(4) 0.2150(3) 0.091(2) Uani 1 1 d . . . H18A H 0.2318 0.4638 0.1886 0.109 Uiso 1 1 calc R . . C19 C 0.18747(16) 0.5059(3) 0.23266(19) 0.0541(15) Uani 1 1 d . . . C20 C 0.16507(16) 0.5961(3) 0.17249(18) 0.0505(14) Uani 1 1 d . . . C21 C 0.16016(15) 0.6893(3) 0.15916(16) 0.0448(13) Uani 1 1 d . . . C22 C 0.14131(17) 0.7184(3) 0.12049(18) 0.0562(15) Uani 1 1 d . . . H22A H 0.1303 0.6790 0.0989 0.067 Uiso 1 1 calc R . . C23 C 0.13880(17) 0.8092(4) 0.11399(18) 0.0591(16) Uani 1 1 d . . . C24 C 0.15472(16) 0.8643(4) 0.14651(18) 0.0538(15) Uani 1 1 d . . . H24A H 0.1526 0.9254 0.1428 0.065 Uiso 1 1 calc R . . C25 C 0.17370(15) 0.8305(3) 0.18425(16) 0.0452(13) Uani 1 1 d . . . C26 C 0.19219(14) 0.8795(3) 0.22215(17) 0.0444(13) Uani 1 1 d . . . C27 C 0.1037(2) 0.7930(4) 0.04258(18) 0.0682(18) Uani 1 1 d . . . H27A H 0.0795 0.7605 0.0544 0.082 Uiso 1 1 calc R . . H27B H 0.1246 0.7509 0.0314 0.082 Uiso 1 1 calc R . . C28 C 0.09074(18) 0.8534(4) 0.00566(18) 0.0623(17) Uani 1 1 d . . . C29 C 0.0499(2) 0.8703(5) -0.0002(2) 0.084(2) Uani 1 1 d . . . H29A H 0.0297 0.8427 0.0183 0.101 Uiso 1 1 calc R . . C30 C 0.0373(2) 0.9296(6) -0.0344(2) 0.098(3) Uani 1 1 d . . . H30A H 0.0088 0.9426 -0.0389 0.118 Uiso 1 1 calc R . . C31 C 0.0673(3) 0.9677(5) -0.0607(2) 0.097(3) Uani 1 1 d . . . H31A H 0.0591 1.0076 -0.0835 0.117 Uiso 1 1 calc R . . C32 C 0.1085(3) 0.9498(4) -0.0550(2) 0.084(2) Uani 1 1 d . . . H32A H 0.1288 0.9763 -0.0737 0.101 Uiso 1 1 calc R . . C33 C 0.1198(2) 0.8925(4) -0.0217(2) 0.077(2) Uani 1 1 d . . . H33A H 0.1484 0.8796 -0.0173 0.093 Uiso 1 1 calc R . . C34 C 0.27346(13) 0.6400(3) 0.29239(17) 0.0394(12) Uani 1 1 d . . . C35 C 0.29665(14) 0.6031(3) 0.32616(17) 0.0451(13) Uani 1 1 d . . . H35A H 0.3258 0.5956 0.3225 0.054 Uiso 1 1 calc R . . C36 C 0.27726(15) 0.5768(4) 0.36576(18) 0.0537(15) Uani 1 1 d . . . H36A H 0.2927 0.5502 0.3894 0.064 Uiso 1 1 calc R . . C37 C 0.23484(15) 0.5902(3) 0.37005(17) 0.0470(14) Uani 1 1 d . . . H37A H 0.2210 0.5746 0.3972 0.056 Uiso 1 1 calc R . . C38 C 0.21299(13) 0.6259(3) 0.33530(14) 0.0344(11) Uani 1 1 d . . . C39 C 0.15359(13) 0.6913(3) 0.36767(15) 0.0378(12) Uani 1 1 d . . . C40 C 0.10695(13) 0.6968(3) 0.36381(14) 0.0361(12) Uani 1 1 d . . . C41 C 0.08213(13) 0.7536(3) 0.38760(15) 0.0412(12) Uani 1 1 d . . . H41A H 0.0934 0.7918 0.4096 0.049 Uiso 1 1 calc R . . C42 C 0.03959(14) 0.7524(3) 0.37790(16) 0.0457(13) Uani 1 1 d . . . C43 C 0.02369(14) 0.6941(3) 0.34633(16) 0.0443(13) Uani 1 1 d . . . H43A H -0.0052 0.6918 0.3400 0.053 Uiso 1 1 calc R . . C44 C 0.05098(13) 0.6403(3) 0.32487(15) 0.0360(12) Uani 1 1 d . . . C45 C 0.04055(15) 0.5748(3) 0.28868(16) 0.0434(13) Uani 1 1 d . . . C46 C 0.07033(14) 0.4621(3) 0.24388(16) 0.0405(12) Uani 1 1 d . . . C47 C 0.06218(16) 0.4898(4) 0.20077(17) 0.0492(14) Uani 1 1 d . . . H47A H 0.0561 0.5492 0.1951 0.059 Uiso 1 1 calc R . . C48 C 0.06285(17) 0.4315(4) 0.16588(18) 0.0590(16) Uani 1 1 d . . . H48A H 0.0572 0.4501 0.1359 0.071 Uiso 1 1 calc R . . C49 C 0.07154(16) 0.3480(4) 0.17449(17) 0.0544(15) Uani 1 1 d . . . H49A H 0.0719 0.3067 0.1507 0.065 Uiso 1 1 calc R . . C50 C 0.08012(16) 0.3221(3) 0.21894(19) 0.0509(14) Uani 1 1 d . . . C51 C 0.02648(16) 0.8658(4) 0.43156(18) 0.0620(16) Uani 1 1 d . . . H51A H 0.0506 0.8992 0.4202 0.074 Uiso 1 1 calc R . . H51B H 0.0350 0.8336 0.4590 0.074 Uiso 1 1 calc R . . C52 C -0.00913(16) 0.9255(4) 0.44200(16) 0.0571(16) Uani 1 1 d . . . C53 C -0.0030(2) 1.0157(4) 0.44102(18) 0.0691(18) Uani 1 1 d . . . H53A H 0.0236 1.0386 0.4338 0.083 Uiso 1 1 calc R . . C54 C -0.0354(2) 1.0713(4) 0.45059(19) 0.0725(19) Uani 1 1 d . . . H54A H -0.0316 1.1323 0.4486 0.087 Uiso 1 1 calc R . . C55 C -0.0733(2) 1.0381(5) 0.4630(2) 0.084(2) Uani 1 1 d . . . H55A H -0.0955 1.0763 0.4703 0.100 Uiso 1 1 calc R . . C56 C -0.07932(19) 0.9501(5) 0.4648(2) 0.080(2) Uani 1 1 d . . . H56A H -0.1057 0.9281 0.4737 0.095 Uiso 1 1 calc R . . C57 C -0.04774(18) 0.8921(4) 0.45393(18) 0.0660(18) Uani 1 1 d . . . H57A H -0.0524 0.8312 0.4546 0.079 Uiso 1 1 calc R . . C58 C 0.1695(4) 0.2531(16) 0.5282(3) 0.282(11) Uani 1 1 d . . . C59 C 0.17553(19) 0.2715(5) 0.5760(2) 0.069(4) Uani 0.482(5) 1 d PG C 1 C60 C 0.1668(2) 0.1977(5) 0.6014(3) 0.080(5) Uani 0.482(5) 1 d PG C 1 H60A H 0.1583 0.1458 0.5867 0.096 Uiso 0.50 1 calc PR C 1 C61 C 0.1704(3) 0.2000(7) 0.6481(3) 0.274(11) Uani 0.482(5) 1 d PG C 1 H61A H 0.1644 0.1496 0.6655 0.328 Uiso 0.50 1 calc PR C 1 C62 C 0.1827(3) 0.2761(8) 0.6696(2) 0.109(6) Uani 0.482(5) 1 d PG C 1 H62A H 0.1852 0.2777 0.7015 0.130 Uiso 0.50 1 calc PR C 1 C63 C 0.1915(3) 0.3499(6) 0.6442(3) 0.069(4) Uani 0.482(5) 1 d PG C 1 H63A H 0.2000 0.4019 0.6589 0.082 Uiso 0.50 1 calc PR C 1 C64 C 0.1879(3) 0.3476(5) 0.5975(3) 0.118(7) Uani 0.482(5) 1 d PG C 1 H64A H 0.1939 0.3980 0.5801 0.141 Uiso 0.50 1 calc PR C 1 C65 C 0.1060(2) 0.1926(4) 0.2595(2) 0.0668(18) Uani 1 1 d . . . C66 C 0.1194(3) 0.0988(4) 0.2495(3) 0.121(3) Uani 1 1 d . . . H66A H 0.1410 0.0812 0.2710 0.182 Uiso 1 1 calc R . . H66B H 0.1305 0.0953 0.2187 0.182 Uiso 1 1 calc R . . H66C H 0.0954 0.0600 0.2524 0.182 Uiso 1 1 calc R . . C67 C 0.07834(16) 0.3569(3) 0.64301(18) 0.0505(14) Uani 1 1 d . . . H67A H 0.0751 0.3636 0.6757 0.076 Uiso 1 1 calc R . . H67B H 0.1007 0.3153 0.6368 0.076 Uiso 1 1 calc R . . H67C H 0.0523 0.3356 0.6300 0.076 Uiso 1 1 calc R . . C68 C 0.0450(2) 0.5059(5) 0.6284(3) 0.094(2) Uani 1 1 d . . . H68A H 0.0206 0.4756 0.6164 0.141 Uiso 1 1 calc R . . H68B H 0.0494 0.5598 0.6115 0.141 Uiso 1 1 calc R . . H68C H 0.0403 0.5197 0.6604 0.141 Uiso 1 1 calc R . . C641 C 0.1826(5) 0.1420(11) 0.5157(7) 1.72(3) Uani 0.518(5) 1 d PG C 2 C642 C 0.1925(6) 0.0750(13) 0.5452(6) 0.45(3) Uani 0.518(5) 1 d PG C 2 H64B H 0.1770 0.0676 0.5723 0.543 Uiso 0.50 1 calc PR C 2 C643 C 0.2250(7) 0.0187(12) 0.5352(8) 1.05(7) Uani 0.518(5) 1 d PG C 2 H64C H 0.2317 -0.0271 0.5554 1.261 Uiso 0.50 1 calc PR C 2 C644 C 0.2476(6) 0.0295(13) 0.4956(9) 0.47(4) Uani 0.518(5) 1 d PG C 2 H64D H 0.2699 -0.0090 0.4888 0.564 Uiso 0.50 1 calc PR C 2 C645 C 0.2378(6) 0.0965(14) 0.4661(7) 0.182(11) Uani 0.518(5) 1 d PG C 2 H64E H 0.2533 0.1039 0.4390 0.218 Uiso 0.50 1 calc PR C 2 C646 C 0.2053(5) 0.1528(12) 0.4761(7) 0.79(5) Uani 0.518(5) 1 d PG C 2 H64F H 0.1986 0.1986 0.4559 0.951 Uiso 0.50 1 calc PR C 2 C69 C 0.1303(5) 1.0660(12) 0.4191(6) 0.052(6) Uani 0.25 1 d PD A 1 H69A H 0.1056 1.0897 0.4348 0.062 Uiso 0.25 1 calc PR A 1 H69B H 0.1345 1.0994 0.3909 0.062 Uiso 0.25 1 calc PR A 1 C70 C 0.1662(6) 1.073(2) 0.4474(7) 0.108(12) Uani 0.25 1 d PD A 1 H70D H 0.1704 1.1345 0.4556 0.162 Uiso 0.25 1 calc PR A 1 H70E H 0.1907 1.0520 0.4311 0.162 Uiso 0.25 1 calc PR A 1 H70F H 0.1621 1.0389 0.4748 0.162 Uiso 0.25 1 calc PR A 1 C71 C 0.2500 0.7500 0.5470(10) 0.19(4) Uani 0.25 2 d SPD . . C72 C 0.2500 0.7500 0.5972(11) 0.21(4) Uani 0.25 2 d SPD . . H72A H 0.2249 0.7792 0.6083 0.322 Uiso 0.13 1 calc PR . . H72B H 0.2746 0.7808 0.6083 0.322 Uiso 0.13 1 calc PR . . H72C H 0.2505 0.6900 0.6083 0.322 Uiso 0.13 1 calc PR . . C73 C 0.2169(10) 1.141(2) 0.3883(10) 0.12(2) Uani 0.13 1 d PD . . H73A H 0.2225 1.1989 0.4008 0.181 Uiso 0.13 1 calc PR B 1 H73B H 0.2416 1.1045 0.3917 0.181 Uiso 0.13 1 calc PR B 1 H73C H 0.1935 1.1148 0.4044 0.181 Uiso 0.13 1 calc PR B 1 C74 C 0.1776(4) 0.8979(12) 0.4906(7) 0.432(17) Uani 0.50 1 d PD . . H74A H 0.1961 0.9264 0.4689 0.647 Uiso 0.50 1 calc PR . . H74B H 0.1938 0.8586 0.5098 0.647 Uiso 0.50 1 calc PR . . H74C H 0.1641 0.9419 0.5094 0.647 Uiso 0.50 1 calc PR . . Na1 Na 0.2500 0.7500 0.4479(5) 0.068(4) Uani 0.25 2 d SP . . O16 O 0.1460(2) 0.8482(5) 0.4662(2) 0.056(2) Uani 0.50 1 d PD . . 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 0.0356(3) 0.0316(3) 0.0411(3) -0.0026(2) 0.0023(2) 0.0018(2) Cu2 0.0371(3) 0.0281(3) 0.0489(3) -0.0024(3) 0.0002(2) 0.0037(2) Cu3 0.0539(3) 0.0372(3) 0.0442(3) 0.0039(3) 0.0072(3) -0.0021(3) S1 0.0928(11) 0.0667(11) 0.0792(11) 0.0109(9) -0.0014(9) -0.0038(9) O1 0.081(3) 0.091(3) 0.098(3) -0.038(3) -0.031(2) 0.008(3) O2 0.103(3) 0.101(4) 0.094(3) 0.028(3) 0.055(3) -0.002(3) O3 0.165(5) 0.218(7) 0.055(3) 0.018(4) -0.011(3) 0.058(5) O4 0.092(3) 0.092(3) 0.151(4) 0.036(3) -0.063(3) -0.020(3) O5 0.096(3) 0.049(2) 0.069(2) -0.020(2) 0.002(2) -0.012(2) O6 0.090(3) 0.061(2) 0.050(2) -0.0020(19) -0.026(2) -0.007(2) O7 0.075(2) 0.0321(19) 0.067(2) -0.0029(17) -0.0254(19) 0.0099(17) O8 0.0430(17) 0.069(2) 0.060(2) -0.0236(19) 0.0022(16) 0.0193(17) O9 0.0375(16) 0.056(2) 0.056(2) -0.0036(17) -0.0080(15) -0.0002(16) O10 0.100(3) 0.048(2) 0.073(3) 0.003(2) 0.006(2) 0.013(2) O11 0.0459(17) 0.053(2) 0.0502(19) -0.0149(17) -0.0004(15) 0.0002(16) O12 0.358(13) 0.205(9) 0.122(6) 0.000(6) -0.025(7) 0.044(9) O13 0.028(6) 0.072(10) 0.050(8) -0.002(7) -0.014(6) 0.009(6) O14 0.018(12) 0.12(3) 0.13(3) -0.04(2) -0.041(14) -0.016(16) O15 0.045(12) 0.020(11) 0.24(3) 0.074(16) -0.065(17) 0.042(10) N1 0.057(3) 0.070(3) 0.072(3) -0.004(3) -0.016(2) -0.006(2) N2 0.045(2) 0.052(3) 0.061(3) -0.007(2) 0.004(2) -0.008(2) N3 0.064(2) 0.040(2) 0.057(3) 0.003(2) 0.019(2) -0.002(2) N4 0.075(3) 0.034(2) 0.053(3) 0.002(2) 0.010(2) -0.002(2) N5 0.060(2) 0.041(2) 0.056(3) 0.007(2) -0.005(2) 0.007(2) N6 0.0387(19) 0.031(2) 0.059(2) -0.003(2) 0.0008(18) -0.0003(17) N7 0.054(2) 0.030(2) 0.059(3) -0.005(2) 0.013(2) -0.0006(19) N8 0.047(2) 0.031(2) 0.051(2) -0.0007(19) -0.0027(18) 0.0018(18) N9 0.0397(19) 0.029(2) 0.051(2) -0.0037(18) -0.0130(17) 0.0093(16) N10 0.0326(17) 0.0223(19) 0.051(2) -0.0055(17) 0.0021(16) 0.0047(15) N11 0.0322(17) 0.039(2) 0.046(2) -0.0069(19) 0.0046(16) 0.0091(17) N12 0.0325(18) 0.036(2) 0.037(2) -0.0013(18) 0.0044(15) -0.0022(17) N13 0.046(2) 0.034(2) 0.036(2) -0.0025(18) 0.0009(17) 0.0017(18) N14 0.045(2) 0.033(2) 0.050(2) -0.0073(19) 0.0084(18) -0.0058(18) N18 0.079(3) 0.041(3) 0.067(3) -0.011(2) -0.001(3) 0.001(2) C1 0.091(4) 0.106(6) 0.064(4) -0.008(4) -0.018(3) 0.018(4) C2 0.060(3) 0.077(4) 0.075(4) -0.025(4) -0.010(3) 0.001(3) C3 0.045(3) 0.053(3) 0.072(4) -0.020(3) 0.009(3) -0.006(3) C4 0.048(3) 0.065(4) 0.093(4) -0.032(3) 0.005(3) -0.008(3) C5 0.063(3) 0.046(4) 0.129(5) -0.020(4) 0.038(4) -0.021(3) C6 0.057(3) 0.045(3) 0.113(5) -0.011(3) 0.024(3) -0.014(3) C7 0.053(3) 0.042(3) 0.069(3) -0.004(3) 0.025(3) -0.002(3) C8 0.095(4) 0.043(3) 0.066(4) 0.013(3) 0.033(3) 0.007(3) C9 0.093(4) 0.050(4) 0.056(3) 0.002(3) 0.013(3) 0.003(3) C10 0.115(5) 0.106(6) 0.054(4) 0.026(4) 0.027(4) 0.012(5) C11 0.099(5) 0.127(7) 0.053(4) 0.000(4) -0.005(4) 0.016(5) C12 0.134(6) 0.080(5) 0.057(4) 0.006(4) -0.021(4) -0.026(4) C13 0.103(4) 0.041(3) 0.061(4) 0.004(3) -0.021(3) -0.002(3) C14 0.077(4) 0.044(3) 0.091(5) 0.010(3) -0.010(4) -0.012(3) C15 0.045(3) 0.036(3) 0.081(4) 0.004(3) -0.001(3) -0.004(2) C16 0.090(4) 0.027(3) 0.150(7) 0.010(4) 0.023(5) 0.019(3) C17 0.108(4) 0.044(4) 0.202(7) 0.026(4) 0.102(5) 0.022(4) C18 0.083(4) 0.042(4) 0.149(6) 0.002(4) 0.071(4) 0.009(3) C19 0.060(3) 0.028(3) 0.074(4) -0.006(3) 0.019(3) 0.000(2) C20 0.055(3) 0.043(3) 0.054(3) -0.011(3) 0.009(2) -0.006(3) C21 0.053(3) 0.033(3) 0.048(3) -0.009(2) 0.004(2) -0.002(2) C22 0.076(3) 0.043(3) 0.050(3) -0.008(3) -0.009(3) -0.009(3) C23 0.064(3) 0.069(4) 0.045(3) -0.006(3) -0.016(3) -0.007(3) C24 0.060(3) 0.044(3) 0.058(3) -0.004(3) -0.008(3) 0.001(3) C25 0.048(3) 0.043(3) 0.045(3) -0.001(2) -0.010(2) 0.004(2) C26 0.042(2) 0.033(3) 0.059(3) -0.004(2) -0.008(2) 0.002(2) C27 0.089(4) 0.069(4) 0.047(3) -0.011(3) -0.016(3) -0.006(3) C28 0.076(4) 0.070(4) 0.040(3) -0.009(3) -0.012(3) 0.006(3) C29 0.079(4) 0.111(6) 0.063(4) -0.006(4) -0.003(3) -0.007(4) C30 0.087(4) 0.128(7) 0.081(5) -0.002(5) -0.025(4) 0.022(5) C31 0.151(7) 0.081(5) 0.060(4) -0.003(4) -0.020(5) 0.014(5) C32 0.130(6) 0.064(4) 0.060(4) -0.009(3) 0.005(4) -0.001(4) C33 0.089(4) 0.081(5) 0.061(4) -0.012(4) 0.002(3) 0.005(4) C34 0.039(2) 0.024(2) 0.055(3) -0.004(2) 0.011(2) 0.004(2) C35 0.033(2) 0.045(3) 0.057(3) 0.005(3) 0.002(2) 0.006(2) C36 0.045(3) 0.060(3) 0.056(3) 0.009(3) -0.003(2) 0.009(3) C37 0.047(3) 0.051(3) 0.043(3) 0.007(2) 0.007(2) 0.002(2) C38 0.035(2) 0.034(3) 0.035(2) -0.006(2) 0.0048(19) -0.002(2) C39 0.038(2) 0.038(3) 0.038(2) 0.006(2) 0.004(2) 0.000(2) C40 0.039(2) 0.038(3) 0.032(2) 0.002(2) 0.0035(19) 0.008(2) C41 0.041(2) 0.044(3) 0.038(2) -0.007(2) 0.001(2) 0.005(2) C42 0.045(2) 0.049(3) 0.043(3) -0.001(2) 0.004(2) 0.014(2) C43 0.038(2) 0.051(3) 0.044(3) -0.002(2) 0.000(2) 0.010(2) C44 0.033(2) 0.038(3) 0.037(2) 0.001(2) 0.0005(19) 0.000(2) C45 0.047(3) 0.037(3) 0.045(3) 0.006(2) 0.006(2) -0.001(2) C46 0.042(2) 0.037(3) 0.042(3) 0.002(2) 0.002(2) -0.005(2) C47 0.058(3) 0.041(3) 0.049(3) -0.004(3) -0.003(2) 0.003(2) C48 0.070(3) 0.064(4) 0.042(3) 0.000(3) -0.011(3) 0.001(3) C49 0.064(3) 0.057(4) 0.043(3) -0.012(3) -0.003(2) -0.005(3) C50 0.054(3) 0.033(3) 0.066(3) -0.013(3) 0.004(3) -0.004(2) C51 0.055(3) 0.079(4) 0.051(3) -0.025(3) -0.006(2) 0.024(3) C52 0.064(3) 0.077(4) 0.031(3) -0.005(3) 0.002(2) 0.028(3) C53 0.079(4) 0.084(5) 0.044(3) -0.006(3) 0.001(3) 0.018(4) C54 0.096(4) 0.068(4) 0.053(3) -0.003(3) 0.009(3) 0.035(4) C55 0.082(4) 0.097(5) 0.072(4) -0.001(4) 0.012(3) 0.051(4) C56 0.063(3) 0.104(5) 0.071(4) 0.003(4) 0.017(3) 0.027(4) C57 0.077(4) 0.072(4) 0.049(3) 0.010(3) 0.012(3) 0.021(3) C58 0.171(10) 0.59(3) 0.084(6) 0.020(12) -0.070(7) 0.042(15) C59 0.053(6) 0.090(10) 0.065(8) 0.001(7) -0.014(6) 0.010(7) C60 0.055(7) 0.143(13) 0.043(6) 0.029(8) 0.001(5) -0.002(8) C61 0.019(6) 0.55(3) 0.251(16) 0.319(17) 0.002(8) 0.022(12) C62 0.031(6) 0.158(15) 0.137(13) -0.072(12) 0.007(7) 0.002(8) C63 0.081(8) 0.066(8) 0.059(7) 0.000(6) -0.033(6) -0.012(7) C64 0.088(10) 0.143(16) 0.123(13) 0.022(12) -0.039(10) 0.028(11) C65 0.087(4) 0.045(3) 0.069(4) -0.012(3) 0.019(3) 0.001(3) C66 0.218(9) 0.044(4) 0.102(6) 0.005(4) 0.044(6) 0.040(5) C67 0.060(3) 0.031(3) 0.061(3) 0.029(2) -0.014(2) -0.002(2) C68 0.111(5) 0.064(4) 0.108(5) 0.001(4) 0.018(5) 0.011(4) C641 1.18(4) 1.96(4) 2.00(6) 1.53(4) 0.57(5) -0.503 C642 0.22(2) 0.90(7) 0.24(3) -0.28(4) 0.05(2) -0.28(4) C643 1.40(13) 0.31(4) 1.45(16) -0.48(6) -1.00(12) 0.52(6) C644 0.82(11) 0.16(2) 0.43(5) -0.18(3) 0.23(6) -0.13(4) C645 0.150(18) 0.111(16) 0.28(3) -0.047(19) 0.01(2) -0.005(14) C646 0.29(2) 0.085(18) 2.00(16) 0.10(4) -0.61(5) 0.018(19) C69 0.034(9) 0.079(15) 0.041(10) -0.024(10) -0.025(8) 0.025(10) C70 0.041(11) 0.25(4) 0.037(12) -0.049(18) -0.003(10) 0.023(18) C71 0.25(9) 0.11(5) 0.21(8) 0.000 0.000 0.02(6) C72 0.04(2) 0.28(9) 0.33(10) 0.000 0.000 0.03(4) C73 0.026(16) 0.001(17) 0.33(7) -0.06(3) 0.09(3) 0.003(15) C74 0.41(3) 0.51(4) 0.37(3) 0.32(3) 0.28(2) 0.37(3) Na1 0.049(6) 0.072(9) 0.083(9) 0.000 0.000 -0.008(6) O16 0.059(4) 0.062(5) 0.045(4) -0.026(4) 0.011(3) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N12 1.910(4) . ? Cu1 N6 1.958(4) . ? Cu1 N11 2.000(4) . ? Cu1 N13 2.005(4) . ? Cu2 N8 1.923(4) . ? Cu2 N9 1.983(4) . ? Cu2 N10 1.985(4) . ? Cu2 N7 1.999(4) . ? Cu3 N4 1.920(4) . ? Cu3 N14 2.021(4) . ? Cu3 N3 2.035(4) . ? Cu3 N5 2.064(4) . ? Cu3 O10 2.210(4) . ? S1 C67 1.437(5) . ? S1 O12 1.735(8) . ? S1 C68 1.743(7) . ? O1 C2 1.232(7) . ? O2 C8 1.268(7) . ? O3 C11 1.358(8) . ? O3 C58 1.526(14) . ? O4 C14 1.261(8) . ? O5 C20 1.214(6) . ? O6 C23 1.347(6) . ? O6 C27 1.461(7) . ? O7 C26 1.235(6) . ? O8 C42 1.352(6) . ? O8 C51 1.442(6) . ? O9 C45 1.238(6) . ? O10 C65 1.252(7) . ? O11 C39 1.235(5) . ? O11 Na1 2.925(8) . ? O13 C69 1.352(19) . ? O14 C71 1.10(3) . ? O14 Na1 2.55(4) . ? O15 C73 1.45(3) . ? N1 C2 1.323(8) . ? N1 C3 1.397(8) . ? N2 C3 1.343(7) . ? N2 C7 1.347(7) . ? N3 C8 1.358(7) . ? N3 C7 1.420(7) . ? N4 C9 1.320(7) . ? N4 C13 1.345(8) . ? N5 C14 1.341(8) . ? N5 C15 1.382(7) . ? N6 C15 1.335(6) . ? N6 C19 1.358(6) . ? N7 C20 1.352(7) . ? N7 C19 1.418(6) . ? N8 C21 1.334(6) . ? N8 C25 1.343(6) . ? N9 C26 1.360(6) . ? N9 C34 1.396(6) 2_565 ? N10 C38 1.342(6) . ? N10 C34 1.377(5) . ? N11 C39 1.347(6) . ? N11 C38 1.416(5) . ? N12 C40 1.319(6) . ? N12 C44 1.337(5) . ? N13 C45 1.366(6) . ? N13 C46 1.411(6) . ? N14 C46 1.351(6) . ? N14 C50 1.351(6) . ? N18 C65 1.322(8) . ? N18 C50 1.384(7) . ? C1 C2 1.490(10) . ? C3 C4 1.393(8) . ? C4 C5 1.366(9) . ? C5 C6 1.355(9) . ? C6 C7 1.388(8) . ? C8 C9 1.476(9) . ? C9 C10 1.413(9) . ? C10 C11 1.424(10) . ? C11 C12 1.347(10) . ? C12 C13 1.396(9) . ? C13 C14 1.469(9) . ? C15 C16 1.399(8) . ? C16 C17 1.342(10) . ? C17 C18 1.365(9) . ? C18 C19 1.384(8) . ? C20 C21 1.496(7) . ? C21 C22 1.371(7) . ? C22 C23 1.412(8) . ? C23 C24 1.382(7) . ? C24 C25 1.375(7) . ? C25 C26 1.477(7) . ? C27 C28 1.494(8) . ? C28 C29 1.352(9) . ? C28 C33 1.376(9) . ? C29 C30 1.420(10) . ? C30 C31 1.371(11) . ? C31 C32 1.364(11) . ? C32 C33 1.373(9) . ? C34 C35 1.371(7) . ? C34 N9 1.396(6) 2_565 ? C35 C36 1.389(7) . ? C36 C37 1.386(7) . ? C37 C38 1.361(6) . ? C39 C40 1.508(6) . ? C40 C41 1.378(6) . ? C41 C42 1.398(6) . ? C42 C43 1.394(7) . ? C43 C44 1.364(6) . ? C44 C45 1.509(7) . ? C46 C47 1.371(7) . ? C47 C48 1.368(7) . ? C48 C49 1.340(8) . ? C49 C50 1.403(7) . ? C51 C52 1.501(7) . ? C52 C57 1.390(8) . ? C52 C53 1.404(9) . ? C53 C54 1.380(8) . ? C54 C55 1.372(9) . ? C55 C56 1.370(10) . ? C56 C57 1.390(8) . ? C58 C59 1.456(13) . ? C58 C641 1.80(3) . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C65 C66 1.536(9) . ? C641 C642 1.3900 . ? C641 C646 1.3900 . ? C642 C643 1.3900 . ? C643 C644 1.3900 . ? C644 C645 1.3900 . ? C645 C646 1.3900 . ? C69 C70 1.43(2) . ? C71 O14 1.10(3) 2_565 ? C71 C72 1.49(3) . ? C71 Na1 2.94(3) . ? C74 O16 1.462(10) . ? Na1 O14 2.55(4) 2_565 ? Na1 O11 2.925(8) 2_565 ? 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 N12 Cu1 N6 179.16(16) . . ? N12 Cu1 N11 79.49(15) . . ? N6 Cu1 N11 99.73(15) . . ? N12 Cu1 N13 80.14(15) . . ? N6 Cu1 N13 100.63(15) . . ? N11 Cu1 N13 159.64(15) . . ? N8 Cu2 N9 79.61(16) . . ? N8 Cu2 N10 176.15(15) . . ? N9 Cu2 N10 101.04(15) . . ? N8 Cu2 N7 78.82(17) . . ? N9 Cu2 N7 158.20(16) . . ? N10 Cu2 N7 100.69(16) . . ? N4 Cu3 N14 174.93(18) . . ? N4 Cu3 N3 79.42(19) . . ? N14 Cu3 N3 105.31(16) . . ? N4 Cu3 N5 78.20(18) . . ? N14 Cu3 N5 96.91(16) . . ? N3 Cu3 N5 157.02(17) . . ? N4 Cu3 O10 94.51(17) . . ? N14 Cu3 O10 86.66(16) . . ? N3 Cu3 O10 98.36(17) . . ? N5 Cu3 O10 88.56(17) . . ? C67 S1 O12 107.0(4) . . ? C67 S1 C68 107.4(3) . . ? O12 S1 C68 97.7(5) . . ? C11 O3 C58 116.1(8) . . ? C23 O6 C27 118.1(4) . . ? C42 O8 C51 118.1(4) . . ? C65 O10 Cu3 124.3(4) . . ? C39 O11 Na1 146.2(3) . . ? C71 O14 Na1 100(2) . . ? C2 N1 C3 131.6(5) . . ? C3 N2 C7 119.3(5) . . ? C8 N3 C7 121.1(5) . . ? C8 N3 Cu3 114.1(4) . . ? C7 N3 Cu3 124.8(3) . . ? C9 N4 C13 119.5(5) . . ? C9 N4 Cu3 119.8(4) . . ? C13 N4 Cu3 120.0(4) . . ? C14 N5 C15 117.4(5) . . ? C14 N5 Cu3 114.8(4) . . ? C15 N5 Cu3 123.6(3) . . ? C15 N6 C19 119.1(4) . . ? C15 N6 Cu1 115.6(3) . . ? C19 N6 Cu1 125.2(3) . . ? C20 N7 C19 117.8(4) . . ? C20 N7 Cu2 117.1(3) . . ? C19 N7 Cu2 123.4(3) . . ? C21 N8 C25 121.7(4) . . ? C21 N8 Cu2 119.6(3) . . ? C25 N8 Cu2 118.7(3) . . ? C26 N9 C34 118.9(4) . 2_565 ? C26 N9 Cu2 116.9(3) . . ? C34 N9 Cu2 123.1(3) 2_565 . ? C38 N10 C34 118.3(4) . . ? C38 N10 Cu2 124.9(3) . . ? C34 N10 Cu2 116.8(3) . . ? C39 N11 C38 117.6(4) . . ? C39 N11 Cu1 116.0(3) . . ? C38 N11 Cu1 125.3(3) . . ? C40 N12 C44 120.7(4) . . ? C40 N12 Cu1 119.8(3) . . ? C44 N12 Cu1 119.5(3) . . ? C45 N13 C46 118.4(4) . . ? C45 N13 Cu1 114.2(3) . . ? C46 N13 Cu1 121.6(3) . . ? C46 N14 C50 116.7(4) . . ? C46 N14 Cu3 115.9(3) . . ? C50 N14 Cu3 127.2(3) . . ? C65 N18 C50 132.1(5) . . ? O1 C2 N1 123.8(7) . . ? O1 C2 C1 121.9(6) . . ? N1 C2 C1 114.2(5) . . ? N2 C3 C4 122.6(6) . . ? N2 C3 N1 111.4(5) . . ? C4 C3 N1 126.0(5) . . ? C5 C4 C3 115.8(6) . . ? C6 C5 C4 123.6(6) . . ? C5 C6 C7 117.4(6) . . ? N2 C7 C6 121.2(5) . . ? N2 C7 N3 114.0(4) . . ? C6 C7 N3 124.7(5) . . ? O2 C8 N3 126.2(6) . . ? O2 C8 C9 120.4(5) . . ? N3 C8 C9 113.4(5) . . ? N4 C9 C10 119.9(6) . . ? N4 C9 C8 112.8(5) . . ? C10 C9 C8 127.3(6) . . ? C9 C10 C11 118.7(6) . . ? C12 C11 O3 123.5(7) . . ? C12 C11 C10 121.1(6) . . ? O3 C11 C10 115.4(7) . . ? C11 C12 C13 115.6(7) . . ? N4 C13 C12 125.1(6) . . ? N4 C13 C14 112.9(5) . . ? C12 C13 C14 121.7(6) . . ? O4 C14 N5 127.0(6) . . ? O4 C14 C13 120.1(6) . . ? N5 C14 C13 112.9(5) . . ? N6 C15 N5 114.2(4) . . ? N6 C15 C16 120.8(5) . . ? N5 C15 C16 124.8(5) . . ? C17 C16 C15 119.8(6) . . ? C16 C17 C18 120.1(6) . . ? C17 C18 C19 119.1(6) . . ? N6 C19 C18 121.1(5) . . ? N6 C19 N7 114.7(4) . . ? C18 C19 N7 124.1(5) . . ? O5 C20 N7 127.8(5) . . ? O5 C20 C21 121.7(5) . . ? N7 C20 C21 110.5(4) . . ? N8 C21 C22 121.8(5) . . ? N8 C21 C20 112.8(4) . . ? C22 C21 C20 125.5(5) . . ? C21 C22 C23 117.5(5) . . ? O6 C23 C24 115.7(5) . . ? O6 C23 C22 124.9(5) . . ? C24 C23 C22 119.4(5) . . ? C25 C24 C23 119.9(5) . . ? N8 C25 C24 119.6(5) . . ? N8 C25 C26 113.3(4) . . ? C24 C25 C26 127.1(5) . . ? O7 C26 N9 126.8(5) . . ? O7 C26 C25 121.9(4) . . ? N9 C26 C25 111.2(4) . . ? O6 C27 C28 105.7(5) . . ? C29 C28 C33 120.1(6) . . ? C29 C28 C27 119.1(6) . . ? C33 C28 C27 120.8(6) . . ? C28 C29 C30 119.4(7) . . ? C31 C30 C29 118.7(7) . . ? C32 C31 C30 121.8(7) . . ? C31 C32 C33 118.5(7) . . ? C32 C33 C28 121.6(7) . . ? N10 C34 C35 121.4(4) . . ? N10 C34 N9 114.0(4) . 2_565 ? C35 C34 N9 124.5(4) . 2_565 ? C34 C35 C36 119.5(4) . . ? C35 C36 C37 118.4(5) . . ? C38 C37 C36 120.0(5) . . ? N10 C38 C37 122.3(4) . . ? N10 C38 N11 114.2(4) . . ? C37 C38 N11 123.4(4) . . ? O11 C39 N11 127.6(4) . . ? O11 C39 C40 121.5(4) . . ? N11 C39 C40 110.9(4) . . ? N12 C40 C41 122.3(4) . . ? N12 C40 C39 112.7(4) . . ? C41 C40 C39 125.0(4) . . ? C40 C41 C42 117.0(4) . . ? O8 C42 C43 116.1(4) . . ? O8 C42 C41 123.6(4) . . ? C43 C42 C41 120.3(4) . . ? C44 C43 C42 117.9(4) . . ? N12 C44 C43 121.7(4) . . ? N12 C44 C45 111.9(4) . . ? C43 C44 C45 126.4(4) . . ? O9 C45 N13 128.4(5) . . ? O9 C45 C44 120.2(4) . . ? N13 C45 C44 111.4(4) . . ? N14 C46 C47 122.7(4) . . ? N14 C46 N13 114.9(4) . . ? C47 C46 N13 122.2(4) . . ? C48 C47 C46 119.8(5) . . ? C49 C48 C47 119.2(5) . . ? C48 C49 C50 119.5(5) . . ? N14 C50 N18 121.9(5) . . ? N14 C50 C49 122.1(5) . . ? N18 C50 C49 116.0(5) . . ? O8 C51 C52 106.3(4) . . ? C57 C52 C53 119.8(5) . . ? C57 C52 C51 120.6(6) . . ? C53 C52 C51 119.6(5) . . ? C54 C53 C52 120.2(6) . . ? C55 C54 C53 119.8(6) . . ? C56 C55 C54 120.3(6) . . ? C55 C56 C57 121.5(6) . . ? C52 C57 C56 118.4(6) . . ? C59 C58 O3 116.1(10) . . ? C59 C58 C641 110.8(13) . . ? O3 C58 C641 97.4(13) . . ? C60 C59 C64 120.0 . . ? C60 C59 C58 109.8(10) . . ? C64 C59 C58 130.2(10) . . ? C61 C60 C59 120.0 . . ? C60 C61 C62 120.0 . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C63 C64 C59 120.0 . . ? O10 C65 N18 124.7(5) . . ? O10 C65 C66 120.0(6) . . ? N18 C65 C66 115.3(6) . . ? C642 C641 C646 120.0 . . ? C642 C641 C58 128.9(11) . . ? C646 C641 C58 100.6(10) . . ? C641 C642 C643 120.0 . . ? C642 C643 C644 120.0 . . ? C645 C644 C643 120.0 . . ? C646 C645 C644 120.0 . . ? C645 C646 C641 120.0 . . ? O13 C69 C70 108.7(19) . . ? O14 C71 O14 118(5) . 2_565 ? O14 C71 C72 121(2) . . ? O14 C71 C72 121(2) 2_565 . ? O14 C71 Na1 59(2) . . ? O14 C71 Na1 59(2) 2_565 . ? C72 C71 Na1 180.000(6) . . ? O14 Na1 O14 43.2(11) 2_565 . ? O14 Na1 O11 142.6(6) 2_565 . ? O14 Na1 O11 100.1(5) . . ? O14 Na1 O11 100.1(5) 2_565 2_565 ? O14 Na1 O11 142.6(6) . 2_565 ? O11 Na1 O11 117.1(5) . 2_565 ? O14 Na1 C71 21.6(5) 2_565 . ? O14 Na1 C71 21.6(5) . . ? O11 Na1 C71 121.5(2) . . ? O11 Na1 C71 121.5(2) 2_565 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.977 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.122