# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 847754' #TrackingRef 'cusalen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 Cu N2 Na2 O14.50 S2' _chemical_formula_weight 703.09 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8998(4) _cell_length_b 11.5756(7) _cell_length_c 16.6900(9) _cell_angle_alpha 103.382(4) _cell_angle_beta 94.177(4) _cell_angle_gamma 103.844(4) _cell_volume 1428.30(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3972 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.30 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4012 _exptl_absorpt_correction_T_max 0.8067 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12691 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.75 _reflns_number_total 6590 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+5.2853P] 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 6590 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2273 _refine_ls_wR_factor_gt 0.2168 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3295(18) -0.2929(10) -0.4605(7) 0.029(2) Uani 0.50 1 d P A 1 H1A H -0.4563 -0.3300 -0.4653 0.035 Uiso 0.50 1 calc PR A 1 C1' C -0.214(2) -0.2660(11) -0.4665(8) 0.034(2) Uani 0.50 1 d P A 2 H1'A H -0.0973 -0.2441 -0.4836 0.041 Uiso 0.50 1 calc PR A 2 C2 C -0.258(2) -0.3268(11) -0.5439(7) 0.030(2) Uani 0.50 1 d P A 1 H2A H -0.1325 -0.2849 -0.5381 0.036 Uiso 0.50 1 calc PR A 1 C2' C -0.3537(19) -0.3531(11) -0.5382(8) 0.029(2) Uani 0.50 1 d P A 2 H2'A H -0.4682 -0.3752 -0.5186 0.035 Uiso 0.50 1 calc PR A 2 C3 C -0.3657(11) -0.2850(6) -0.6090(4) 0.0459(16) Uani 1 1 d . . . H3A H -0.2968 -0.2740 -0.6538 0.055 Uiso 1 1 calc R A 1 H3B H -0.4721 -0.3502 -0.6326 0.055 Uiso 1 1 calc R A 1 C4 C -0.417(3) -0.1650(13) -0.5734(10) 0.050(4) Uani 0.50 1 d P A 1 H4A H -0.4304 -0.1235 -0.6168 0.060 Uiso 0.50 1 calc PR A 1 H4B H -0.5284 -0.1833 -0.5516 0.060 Uiso 0.50 1 calc PR A 1 C4' C -0.327(3) -0.1427(17) -0.5778(12) 0.054(5) Uiso 0.50 1 d P A 2 H4'A H -0.2010 -0.1056 -0.5709 0.065 Uiso 0.50 1 calc PR A 2 H4'B H -0.3834 -0.1108 -0.6181 0.065 Uiso 0.50 1 calc PR A 2 C5 C -0.274(3) -0.0836(13) -0.5049(10) 0.055(4) Uani 0.50 1 d P A 1 H5A H -0.2947 -0.0028 -0.4861 0.066 Uiso 0.50 1 calc PR A 1 H5B H -0.1601 -0.0739 -0.5242 0.066 Uiso 0.50 1 calc PR A 1 C5' C -0.396(3) -0.1106(15) -0.4948(10) 0.051(4) Uani 0.50 1 d P A 2 H5'A H -0.5195 -0.1540 -0.4997 0.061 Uiso 0.50 1 calc PR A 2 H5'B H -0.3848 -0.0228 -0.4768 0.061 Uiso 0.50 1 calc PR A 2 C6 C -0.2830(13) -0.1511(6) -0.4317(4) 0.056(2) Uani 1 1 d . . . H6A H -0.1699 -0.1219 -0.3969 0.067 Uiso 1 1 calc R A 1 H6B H -0.3699 -0.1276 -0.3978 0.067 Uiso 1 1 calc R A 1 C7 C -0.3175(9) -0.5308(6) -0.6363(4) 0.0376(13) Uani 1 1 d . A . H7A H -0.352(11) -0.491(8) -0.674(5) 0.06(2) Uiso 1 1 d . . . C8 C -0.2016(9) -0.3037(6) -0.3275(4) 0.0400(14) Uani 1 1 d . A . H8A H -0.201(19) -0.210(13) -0.293(9) 0.14(5) Uiso 1 1 d . . . C9 C -0.3003(7) -0.6553(5) -0.6610(3) 0.0286(11) Uani 1 1 d . . . C10 C -0.3559(7) -0.7209(5) -0.7444(3) 0.0292(11) Uani 1 1 d . . . H10A H -0.392(10) -0.683(7) -0.784(5) 0.044(19) Uiso 1 1 d . . . C11 C -0.3466(7) -0.8399(5) -0.7723(3) 0.0276(11) Uani 1 1 d . . . C12 C -0.2802(8) -0.8975(5) -0.7168(4) 0.0332(12) Uani 1 1 d . . . H12A H -0.2743 -0.9785 -0.7355 0.040 Uiso 1 1 calc R . . C13 C -0.2237(9) -0.8355(6) -0.6351(4) 0.0377(14) Uani 1 1 d . . . H13A H -0.1813 -0.8756 -0.5991 0.045 Uiso 1 1 calc R . . C14 C -0.2286(7) -0.7119(5) -0.6043(3) 0.0307(11) Uani 1 1 d . A . C15 C -0.1518(7) -0.3654(5) -0.2675(3) 0.0302(11) Uani 1 1 d . . . C16 C -0.1423(8) -0.3055(5) -0.1843(4) 0.0318(11) Uani 1 1 d . . . H16A H -0.146(11) -0.217(8) -0.165(5) 0.06(2) Uiso 1 1 d . . . C17 C -0.0916(8) -0.3542(5) -0.1214(4) 0.0328(12) Uani 1 1 d . . . C18 C -0.0495(9) -0.4674(6) -0.1425(4) 0.0406(14) Uani 1 1 d . . . H18A H -0.0157 -0.5018 -0.1009 0.049 Uiso 1 1 calc R . . C19 C -0.0581(11) -0.5273(6) -0.2240(4) 0.0477(17) Uani 1 1 d . . . H19A H -0.0277 -0.6017 -0.2367 0.057 Uiso 1 1 calc R . . C20 C -0.1113(8) -0.4806(5) -0.2896(3) 0.0339(12) Uani 1 1 d . A . N1 N -0.2239(8) -0.3469(5) -0.4063(3) 0.0424(13) Uani 1 1 d . . . N2 N -0.2843(8) -0.4630(5) -0.5625(3) 0.0378(12) Uani 1 1 d . . . O1 O -0.1202(7) -0.5451(4) -0.3668(3) 0.0414(10) Uani 1 1 d . . . O2 O -0.1680(6) -0.6575(4) -0.5264(2) 0.0406(10) Uani 1 1 d . . . O3 O -0.1109(6) -0.1570(4) -0.0151(3) 0.0380(9) Uani 1 1 d . . . O4 O -0.2381(7) -0.3521(5) 0.0113(3) 0.0564(14) Uani 1 1 d . . . O5 O 0.0787(7) -0.2708(5) 0.0277(3) 0.0546(13) Uani 1 1 d . . . O6 O -0.4910(7) -0.8458(4) -0.9183(3) 0.0480(12) Uani 1 1 d . . . O7 O -0.5436(6) -1.0344(4) -0.8780(3) 0.0437(11) Uani 1 1 d . . . O8 O -0.2600(6) -0.9501(5) -0.9109(3) 0.0475(12) Uani 1 1 d . . . O9 O 0.1272(10) 0.7944(6) 0.3821(5) 0.083(2) Uani 1 1 d . . . O10 O 0.5374(8) 0.4937(6) 0.1577(4) 0.0704(16) Uani 1 1 d . . . O11 O -0.4054(9) -1.2524(6) -0.8210(4) 0.0698(16) Uani 1 1 d . . . O12 O 0.0580(6) 0.0151(5) 0.1705(3) 0.0469(11) Uani 1 1 d . . . O13 O -0.6601(7) -1.3922(6) -1.0075(4) 0.0673(16) Uani 1 1 d . . . O14 O 0.3254(15) 0.8446(12) 0.2436(8) 0.074(4) Uani 0.50 1 d P . . O15 O -0.066(3) 0.871(2) 0.2684(15) 0.093(7) Uani 0.50 1 d P B 1 O15' O -0.070(4) 0.804(3) 0.230(3) 0.157(16) Uani 0.50 1 d P C 2 S1 S -0.08907(18) -0.27848(13) -0.01717(8) 0.0309(3) Uani 1 1 d . . . S2 S -0.41467(17) -0.92149(12) -0.87747(8) 0.0270(3) Uani 1 1 d . . . Na1 Na -0.4268(4) -1.2083(2) -0.95649(16) 0.0453(6) Uani 1 1 d . . . Na2 Na 0.1894(3) -0.0244(2) 0.04789(14) 0.0369(5) Uani 1 1 d . . . Cu1 Cu -0.19231(9) -0.50379(6) -0.46486(4) 0.0286(2) Uani 1 1 d . A . 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 C1 0.037(6) 0.027(5) 0.024(5) 0.004(4) 0.005(5) 0.011(5) C1' 0.044(7) 0.026(6) 0.034(6) 0.008(5) 0.004(5) 0.013(5) C2 0.038(7) 0.022(6) 0.026(6) -0.001(4) 0.004(5) 0.009(5) C2' 0.030(6) 0.025(6) 0.030(6) -0.005(5) 0.003(5) 0.013(5) C3 0.076(5) 0.037(3) 0.031(3) 0.005(3) 0.003(3) 0.029(3) C4 0.065(11) 0.030(7) 0.051(9) 0.001(6) -0.027(8) 0.023(7) C5 0.082(12) 0.028(7) 0.048(9) -0.001(6) -0.019(9) 0.022(8) C5' 0.080(12) 0.036(8) 0.046(8) 0.014(6) 0.009(8) 0.032(8) C6 0.100(6) 0.033(3) 0.037(4) -0.003(3) -0.009(4) 0.038(4) C7 0.058(4) 0.032(3) 0.023(3) 0.004(2) -0.003(3) 0.018(3) C8 0.059(4) 0.032(3) 0.030(3) -0.001(2) 0.001(3) 0.024(3) C9 0.034(3) 0.029(3) 0.022(2) 0.001(2) 0.001(2) 0.012(2) C10 0.036(3) 0.031(3) 0.020(2) 0.001(2) 0.000(2) 0.014(2) C11 0.028(2) 0.032(3) 0.021(2) 0.000(2) 0.004(2) 0.010(2) C12 0.042(3) 0.026(3) 0.030(3) 0.000(2) -0.001(2) 0.014(2) C13 0.053(4) 0.036(3) 0.027(3) 0.002(2) -0.004(2) 0.026(3) C14 0.035(3) 0.030(3) 0.025(3) 0.000(2) -0.002(2) 0.014(2) C15 0.033(3) 0.032(3) 0.024(2) 0.001(2) 0.003(2) 0.011(2) C16 0.036(3) 0.027(3) 0.030(3) 0.001(2) 0.004(2) 0.010(2) C17 0.034(3) 0.033(3) 0.027(3) 0.001(2) 0.001(2) 0.007(2) C18 0.056(4) 0.042(3) 0.027(3) 0.009(3) 0.001(3) 0.020(3) C19 0.076(5) 0.039(3) 0.033(3) 0.002(3) 0.002(3) 0.032(3) C20 0.044(3) 0.033(3) 0.023(3) 0.000(2) 0.005(2) 0.015(2) N1 0.072(4) 0.031(3) 0.026(2) 0.002(2) -0.003(2) 0.024(3) N2 0.057(3) 0.032(3) 0.029(2) 0.006(2) 0.003(2) 0.022(2) O1 0.066(3) 0.035(2) 0.027(2) 0.0014(17) 0.0034(19) 0.028(2) O2 0.059(3) 0.039(2) 0.0232(19) -0.0038(17) -0.0083(18) 0.027(2) O3 0.047(2) 0.034(2) 0.032(2) -0.0024(17) 0.0048(18) 0.0181(18) O4 0.064(3) 0.051(3) 0.048(3) 0.008(2) 0.028(3) 0.002(2) O5 0.053(3) 0.075(4) 0.036(2) -0.001(2) -0.007(2) 0.035(3) O6 0.071(3) 0.047(3) 0.026(2) 0.0016(19) -0.008(2) 0.027(2) O7 0.046(3) 0.042(2) 0.032(2) 0.0031(19) -0.0016(19) 0.000(2) O8 0.036(2) 0.076(3) 0.028(2) -0.006(2) 0.0057(18) 0.026(2) O9 0.092(5) 0.062(4) 0.092(5) 0.014(4) 0.000(4) 0.027(4) O10 0.069(4) 0.069(4) 0.075(4) 0.027(3) 0.003(3) 0.016(3) O11 0.089(4) 0.077(4) 0.054(3) 0.024(3) 0.013(3) 0.034(3) O12 0.046(3) 0.051(3) 0.046(3) 0.013(2) 0.010(2) 0.015(2) O13 0.041(3) 0.064(4) 0.102(5) 0.028(3) 0.010(3) 0.016(3) O14 0.069(7) 0.102(9) 0.102(9) 0.082(8) 0.069(7) 0.050(7) O15 0.065(9) 0.108(16) 0.131(17) 0.094(15) 0.010(10) 0.009(12) O15' 0.083(14) 0.13(2) 0.30(5) 0.14(3) 0.03(2) 0.026(19) S1 0.0328(7) 0.0343(7) 0.0247(6) 0.0026(5) 0.0053(5) 0.0116(6) S2 0.0283(6) 0.0307(7) 0.0199(6) -0.0001(5) 0.0013(5) 0.0109(5) Na1 0.0559(16) 0.0445(14) 0.0385(14) 0.0094(11) 0.0070(12) 0.0202(12) Na2 0.0296(11) 0.0487(14) 0.0315(12) 0.0072(10) 0.0034(9) 0.0119(10) Cu1 0.0340(4) 0.0293(4) 0.0216(3) -0.0006(3) 0.0009(3) 0.0145(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.518(12) . ? C1 C6 1.543(13) . ? C1 C2 1.543(17) . ? C1' N1 1.518(12) . ? C1' C2' 1.542(18) . ? C1' C6 1.560(13) . ? C2 N2 1.495(12) . ? C2 C3 1.564(14) . ? C2' N2 1.488(12) . ? C2' C3 1.574(14) . ? C3 C4 1.541(15) . ? C3 C4' 1.56(2) . ? C4 C5 1.51(2) . ? C4' C5' 1.53(2) . ? C5 C6 1.593(18) . ? C5' C6 1.556(17) . ? C7 N2 1.269(8) . ? C7 C9 1.447(8) . ? C8 N1 1.277(8) . ? C8 C15 1.440(8) . ? C9 C10 1.403(7) . ? C9 C14 1.426(7) . ? C10 C11 1.369(8) . ? C11 C12 1.400(7) . ? C11 S2 1.765(5) . ? C12 C13 1.371(8) . ? C13 C14 1.414(8) . ? C14 O2 1.305(7) . ? C15 C16 1.388(8) . ? C15 C20 1.418(8) . ? C16 C17 1.379(8) . ? C17 C18 1.401(9) . ? C17 S1 1.754(6) . ? C18 C19 1.366(9) . ? C19 C20 1.408(8) . ? C20 O1 1.319(7) . ? N1 Cu1 1.935(5) . ? N2 Cu1 1.938(5) . ? O1 Cu1 1.894(4) . ? O2 Cu1 1.899(4) . ? O3 S1 1.450(4) . ? O3 Na2 2.490(5) 2 ? O3 Na2 2.497(5) . ? O3 Na1 2.730(5) 1_566 ? O4 S1 1.458(5) . ? O4 Na1 2.485(6) 1_566 ? O5 S1 1.447(5) . ? O5 Na2 2.708(6) . ? O6 S2 1.437(4) . ? O6 Na1 2.405(5) 2_433 ? O6 Na2 2.779(6) 1_444 ? O7 S2 1.450(5) . ? O7 Na2 2.407(5) 1_444 ? O7 Na1 2.543(6) . ? O8 S2 1.456(4) . ? O8 Na2 2.363(5) 2_544 ? O8 Na1 2.857(6) . ? O11 Na1 2.433(6) . ? O12 Na2 2.361(5) . ? O13 Na1 2.389(7) . ? S1 Na2 3.122(3) . ? S1 Na1 3.140(3) 1_566 ? S2 Na2 3.117(3) 1_444 ? S2 Na1 3.251(3) . ? Na1 O6 2.405(5) 2_433 ? Na1 O4 2.485(6) 1_544 ? Na1 O3 2.730(5) 1_544 ? Na1 S1 3.140(3) 1_544 ? Na1 Na2 3.606(4) 2_544 ? Na1 Na2 4.096(4) 1_444 ? Na2 O8 2.363(5) 2_544 ? Na2 O7 2.407(5) 1_666 ? Na2 O3 2.490(5) 2 ? Na2 O6 2.779(6) 1_666 ? Na2 S2 3.117(3) 1_666 ? Na2 Na2 3.515(5) 2 ? Na2 Na1 3.606(4) 2_544 ? Na2 Na1 4.096(4) 1_666 ? 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 C1 C6 112.2(8) . . ? N1 C1 C2 101.1(9) . . ? C6 C1 C2 107.1(9) . . ? N1 C1' C2' 99.6(9) . . ? N1 C1' C6 111.3(9) . . ? C2' C1' C6 107.3(10) . . ? N2 C2 C1 104.6(9) . . ? N2 C2 C3 113.8(9) . . ? C1 C2 C3 107.2(10) . . ? N2 C2' C1' 103.4(9) . . ? N2 C2' C3 113.6(9) . . ? C1' C2' C3 108.0(10) . . ? C4 C3 C4' 26.7(8) . . ? C4 C3 C2 114.3(8) . . ? C4' C3 C2 106.3(10) . . ? C4 C3 C2' 108.7(9) . . ? C4' C3 C2' 114.6(9) . . ? C2 C3 C2' 28.3(5) . . ? C5 C4 C3 108.4(12) . . ? C5' C4' C3 109.0(13) . . ? C4 C5 C6 105.8(14) . . ? C4' C5' C6 106.1(14) . . ? C1 C6 C5' 105.8(9) . . ? C1 C6 C1' 34.1(6) . . ? C5' C6 C1' 117.0(8) . . ? C1 C6 C5 114.9(8) . . ? C5' C6 C5 36.2(8) . . ? C1' C6 C5 103.8(9) . . ? N2 C7 C9 125.2(5) . . ? N1 C8 C15 125.4(5) . . ? C10 C9 C14 119.7(5) . . ? C10 C9 C7 117.8(5) . . ? C14 C9 C7 122.5(5) . . ? C11 C10 C9 121.3(5) . . ? C10 C11 C12 119.6(5) . . ? C10 C11 S2 121.1(4) . . ? C12 C11 S2 119.3(4) . . ? C13 C12 C11 120.5(5) . . ? C12 C13 C14 121.6(5) . . ? O2 C14 C13 118.2(5) . . ? O2 C14 C9 124.4(5) . . ? C13 C14 C9 117.4(5) . . ? C16 C15 C20 120.0(5) . . ? C16 C15 C8 116.6(5) . . ? C20 C15 C8 123.4(5) . . ? C17 C16 C15 121.7(5) . . ? C16 C17 C18 118.8(5) . . ? C16 C17 S1 120.3(5) . . ? C18 C17 S1 120.8(4) . . ? C19 C18 C17 120.1(5) . . ? C18 C19 C20 122.4(6) . . ? O1 C20 C19 118.9(5) . . ? O1 C20 C15 124.2(5) . . ? C19 C20 C15 117.0(5) . . ? C8 N1 C1 119.1(6) . . ? C8 N1 C1' 122.8(7) . . ? C1 N1 C1' 34.9(6) . . ? C8 N1 Cu1 125.8(4) . . ? C1 N1 Cu1 112.9(5) . . ? C1' N1 Cu1 108.1(5) . . ? C7 N2 C2' 121.4(6) . . ? C7 N2 C2 122.0(6) . . ? C2' N2 C2 29.8(6) . . ? C7 N2 Cu1 126.6(4) . . ? C2' N2 Cu1 110.6(5) . . ? C2 N2 Cu1 108.9(5) . . ? C20 O1 Cu1 126.8(4) . . ? C14 O2 Cu1 126.9(4) . . ? S1 O3 Na2 165.3(3) . 2 ? S1 O3 Na2 101.2(2) . . ? Na2 O3 Na2 89.64(16) 2 . ? S1 O3 Na1 92.2(2) . 1_566 ? Na2 O3 Na1 87.25(15) 2 1_566 ? Na2 O3 Na1 133.94(19) . 1_566 ? S1 O4 Na1 102.4(3) . 1_566 ? S1 O5 Na2 92.3(3) . . ? S2 O6 Na1 149.9(3) . 2_433 ? S2 O6 Na2 89.5(2) . 1_444 ? Na1 O6 Na2 87.84(17) 2_433 1_444 ? S2 O7 Na2 105.1(3) . 1_444 ? S2 O7 Na1 105.8(3) . . ? Na2 O7 Na1 111.65(19) 1_444 . ? S2 O8 Na2 129.7(3) . 2_544 ? S2 O8 Na1 92.0(3) . . ? Na2 O8 Na1 86.85(17) 2_544 . ? O5 S1 O3 111.2(3) . . ? O5 S1 O4 113.1(3) . . ? O3 S1 O4 111.0(3) . . ? O5 S1 C17 107.7(3) . . ? O3 S1 C17 107.6(3) . . ? O4 S1 C17 105.9(3) . . ? O5 S1 Na2 60.1(2) . . ? O3 S1 Na2 51.68(19) . . ? O4 S1 Na2 138.2(2) . . ? C17 S1 Na2 115.4(2) . . ? O5 S1 Na1 131.7(2) . 1_566 ? O3 S1 Na1 60.35(19) . 1_566 ? O4 S1 Na1 50.6(2) . 1_566 ? C17 S1 Na1 120.3(2) . 1_566 ? Na2 S1 Na1 100.43(8) . 1_566 ? O6 S2 O7 111.2(3) . . ? O6 S2 O8 114.1(3) . . ? O7 S2 O8 109.8(3) . . ? O6 S2 C11 107.7(3) . . ? O7 S2 C11 106.7(3) . . ? O8 S2 C11 106.9(3) . . ? O6 S2 Na2 63.1(2) . 1_444 ? O7 S2 Na2 48.2(2) . 1_444 ? O8 S2 Na2 129.7(2) . 1_444 ? C11 S2 Na2 122.16(19) . 1_444 ? O6 S2 Na1 125.7(2) . . ? O7 S2 Na1 48.8(2) . . ? O8 S2 Na1 61.4(2) . . ? C11 S2 Na1 125.74(19) . . ? Na2 S2 Na1 80.02(8) 1_444 . ? O13 Na1 O6 86.4(2) . 2_433 ? O13 Na1 O11 89.6(2) . . ? O6 Na1 O11 167.0(2) 2_433 . ? O13 Na1 O4 83.2(2) . 1_544 ? O6 Na1 O4 108.49(19) 2_433 1_544 ? O11 Na1 O4 83.3(2) . 1_544 ? O13 Na1 O7 110.4(2) . . ? O6 Na1 O7 87.40(17) 2_433 . ? O11 Na1 O7 82.4(2) . . ? O4 Na1 O7 160.1(2) 1_544 . ? O13 Na1 O3 126.0(2) . 1_544 ? O6 Na1 O3 78.79(18) 2_433 1_544 ? O11 Na1 O3 113.4(2) . 1_544 ? O4 Na1 O3 54.47(15) 1_544 1_544 ? O7 Na1 O3 120.17(17) . 1_544 ? O13 Na1 O8 157.4(2) . . ? O6 Na1 O8 79.41(17) 2_433 . ? O11 Na1 O8 100.3(2) . . ? O4 Na1 O8 117.94(18) 1_544 . ? O7 Na1 O8 51.85(14) . . ? O3 Na1 O8 68.39(14) 1_544 . ? O13 Na1 S1 105.10(17) . 1_544 ? O6 Na1 S1 94.09(15) 2_433 1_544 ? O11 Na1 S1 98.93(18) . 1_544 ? O4 Na1 S1 26.98(12) 1_544 1_544 ? O7 Na1 S1 144.44(15) . 1_544 ? O3 Na1 S1 27.48(9) 1_544 1_544 ? O8 Na1 S1 93.46(12) . 1_544 ? O13 Na1 S2 133.70(18) . . ? O6 Na1 S2 80.78(13) 2_433 . ? O11 Na1 S2 93.14(18) . . ? O4 Na1 S2 143.05(17) 1_544 . ? O7 Na1 S2 25.41(11) . . ? O3 Na1 S2 94.77(12) 1_544 . ? O8 Na1 S2 26.59(9) . . ? S1 Na1 S2 119.98(10) 1_544 . ? O13 Na1 Na2 134.67(19) . 2_544 ? O6 Na1 Na2 50.36(14) 2_433 2_544 ? O11 Na1 Na2 135.6(2) . 2_544 ? O4 Na1 Na2 97.01(14) 1_544 2_544 ? O7 Na1 Na2 83.76(13) . 2_544 ? O3 Na1 Na2 43.61(10) 1_544 2_544 ? O8 Na1 Na2 40.86(10) . 2_544 ? S1 Na1 Na2 70.46(7) 1_544 2_544 ? S2 Na1 Na2 60.69(7) . 2_544 ? O13 Na1 Na2 86.09(16) . 1_444 ? O6 Na1 Na2 62.86(14) 2_433 1_444 ? O11 Na1 Na2 104.52(18) . 1_444 ? O4 Na1 Na2 166.70(17) 1_544 1_444 ? O7 Na1 Na2 33.11(11) . 1_444 ? O3 Na1 Na2 128.58(12) 1_544 1_444 ? O8 Na1 Na2 71.81(11) . 1_444 ? S1 Na1 Na2 154.09(9) 1_544 1_444 ? S2 Na1 Na2 48.55(5) . 1_444 ? Na2 Na1 Na2 84.98(7) 2_544 1_444 ? O12 Na2 O8 165.55(19) . 2_544 ? O12 Na2 O7 92.69(18) . 1_666 ? O8 Na2 O7 101.46(17) 2_544 1_666 ? O12 Na2 O3 88.18(17) . 2 ? O8 Na2 O3 80.65(17) 2_544 2 ? O7 Na2 O3 129.10(18) 1_666 2 ? O12 Na2 O3 84.15(17) . . ? O8 Na2 O3 86.76(17) 2_544 . ? O7 Na2 O3 140.38(18) 1_666 . ? O3 Na2 O3 90.36(16) 2 . ? O12 Na2 O5 91.84(18) . . ? O8 Na2 O5 91.99(19) 2_544 . ? O7 Na2 O5 86.28(16) 1_666 . ? O3 Na2 O5 144.59(17) 2 . ? O3 Na2 O5 54.49(15) . . ? O12 Na2 O6 104.63(18) . 1_666 ? O8 Na2 O6 81.75(17) 2_544 1_666 ? O7 Na2 O6 54.12(14) 1_666 1_666 ? O3 Na2 O6 76.48(15) 2 1_666 ? O3 Na2 O6 163.72(16) . 1_666 ? O5 Na2 O6 137.03(17) . 1_666 ? O12 Na2 S2 99.92(14) . 1_666 ? O8 Na2 S2 91.61(13) 2_544 1_666 ? O7 Na2 S2 26.68(11) 1_666 1_666 ? O3 Na2 S2 103.32(13) 2 1_666 ? O3 Na2 S2 165.78(14) . 1_666 ? O5 Na2 S2 111.52(13) . 1_666 ? O6 Na2 S2 27.45(9) 1_666 1_666 ? O12 Na2 S1 90.14(14) . . ? O8 Na2 S1 86.84(15) 2_544 . ? O7 Na2 S1 113.87(14) 1_666 . ? O3 Na2 S1 117.01(13) 2 . ? O3 Na2 S1 27.10(10) . . ? O5 Na2 S1 27.60(10) . . ? O6 Na2 S1 160.71(14) 1_666 . ? S2 Na2 S1 138.73(9) 1_666 . ? O12 Na2 Na2 84.56(15) . 2 ? O8 Na2 Na2 81.07(14) 2_544 2 ? O7 Na2 Na2 173.67(18) 1_666 2 ? O3 Na2 Na2 45.26(12) 2 2 ? O3 Na2 Na2 45.10(11) . 2 ? O5 Na2 Na2 99.48(14) . 2 ? O6 Na2 Na2 121.08(15) 1_666 2 ? S2 Na2 Na2 148.41(13) 1_666 2 ? S1 Na2 Na2 71.90(8) . 2 ? O12 Na2 Na1 125.00(16) . 2_544 ? O8 Na2 Na1 52.29(15) 2_544 2_544 ? O7 Na2 Na1 91.96(13) 1_666 2_544 ? O3 Na2 Na1 49.14(12) 2 2_544 ? O3 Na2 Na1 121.99(13) . 2_544 ? O5 Na2 Na1 143.15(14) . 2_544 ? O6 Na2 Na1 41.79(10) 1_666 2_544 ? S2 Na2 Na1 66.70(7) 1_666 2_544 ? S1 Na2 Na1 136.10(9) . 2_544 ? Na2 Na2 Na1 85.00(10) 2 2_544 ? O12 Na2 Na1 118.21(14) . 1_666 ? O8 Na2 Na1 75.87(13) 2_544 1_666 ? O7 Na2 Na1 35.24(12) 1_666 1_666 ? O3 Na2 Na1 144.14(14) 2 1_666 ? O3 Na2 Na1 114.65(13) . 1_666 ? O5 Na2 Na1 63.63(12) . 1_666 ? O6 Na2 Na1 73.66(11) 1_666 1_666 ? S2 Na2 Na1 51.43(6) 1_666 1_666 ? S1 Na2 Na1 88.53(8) . 1_666 ? Na2 Na2 Na1 150.50(12) 2 1_666 ? Na1 Na2 Na1 95.02(7) 2_544 1_666 ? O1 Cu1 O2 88.04(17) . . ? O1 Cu1 N1 94.35(19) . . ? O2 Cu1 N1 177.46(19) . . ? O1 Cu1 N2 175.5(2) . . ? O2 Cu1 N2 93.53(19) . . ? N1 Cu1 N2 84.0(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.500 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.140