# Electronic Supplementary Material (ESI) for CrystEngComm # 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_Complex2 # CCDC 943447 _audit_creation_method SHELXL-97 _chemical_name_systematic Complex2 _chemical_name_common complex2 _chemical_formula_moiety 'C26 H34 Cl Cs Cu N2 O7' _chemical_formula_sum 'C26 H34 Cl Cs Cu N2 O7' _chemical_compound_source synthesis _exptl_crystal_recrystallization_method methanol _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour blue _diffrn_ambient_temperature 296(2) _chemical_formula_weight 718.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_int_tables_number 1 _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 5.8930(7) _cell_length_b 8.8346(11) _cell_length_c 15.801(2) _cell_angle_alpha 99.553(6) _cell_angle_beta 99.826(7) _cell_angle_gamma 109.432(6) _cell_volume 742.11(16) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4701 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 26.36 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 2.079 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5299 _exptl_absorpt_correction_T_max 0.7060 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 6252 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3623 _reflns_number_gt 3295 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^ > 2\s(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. Restrains used DELU 0.010 0.010 C17 C16 C4 C5 C3 C24 C13 C26 SIMU 0.040 0.080 1.700 C17 C16 C4 C5 C3 C24 C13 C26 ; _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^)+(0.0895P)^2^+2.3182P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(4) _refine_ls_number_reflns 3623 _refine_ls_number_parameters 344 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.089 _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 Cs1 Cs 0.18946(7) 0.86398(5) 0.31711(4) 0.0474(3) Uani 1 1 d . . . Cu1 Cu 0.4533(3) 0.44147(16) 0.30305(10) 0.0410(5) Uani 1 1 d . . . Cl1 Cl -0.0161(6) 0.4432(4) 0.3030(2) 0.0436(7) Uani 1 1 d . . . O2 O 0.3205(17) 0.2043(10) 0.2558(5) 0.042(2) Uani 1 1 d . . . O3 O 0.177(3) 0.0100(12) 0.1276(8) 0.086(4) Uani 1 1 d . . . O5 O 0.610(2) 0.6807(11) 0.3500(5) 0.036(2) Uani 1 1 d . . . O6 O 0.783(3) 0.8727(12) 0.4724(7) 0.085(4) Uani 1 1 d . . . O1 O 0.840(3) 0.7324(18) 0.1223(8) 0.088(4) Uani 1 1 d . . . O4 O 0.677(3) 0.1380(15) 0.4688(7) 0.077(3) Uani 1 1 d . . . O7 O 0.749(3) 1.0211(13) 0.2779(9) 0.071(4) Uani 1 1 d . . . N2 N 0.538(2) 0.4262(12) 0.4264(6) 0.042(3) Uani 1 1 d . . . H1 H 0.6600 0.3845 0.4274 0.050 Uiso 1 1 calc R . . N1 N 0.453(2) 0.4535(12) 0.1774(6) 0.039(3) Uani 1 1 d . . . H101 H 0.6167 0.4919 0.1771 0.047 Uiso 1 1 calc R . . C22 C 0.683(3) 0.7244(15) 0.4328(9) 0.045(3) Uani 1 1 d . . . C21 C 0.665(4) 0.5918(16) 0.4862(9) 0.059(5) Uani 1 1 d . . . H100 H 0.5684 0.6056 0.5296 0.071 Uiso 1 1 calc R . . C8 C 0.350(4) 0.2820(16) 0.1180(9) 0.061(4) Uani 1 1 d . . . H3 H 0.2034 0.2716 0.0739 0.073 Uiso 1 1 calc R . . C9 C 0.272(3) 0.1559(17) 0.1704(11) 0.053(4) Uani 1 1 d . . . C7 C 0.359(4) 0.5740(19) 0.1435(10) 0.067(5) Uani 1 1 d . . . H5A H 0.4337 0.6794 0.1867 0.080 Uiso 1 1 calc R . . H5B H 0.1811 0.5357 0.1375 0.080 Uiso 1 1 calc R . . C6 C 0.411(3) 0.6003(16) 0.0554(8) 0.047(4) Uani 1 1 d . . . C1 C 0.643(3) 0.6775(19) 0.0471(10) 0.049(4) Uani 1 1 d . . . C19 C 0.474(3) 0.2739(18) 0.5474(9) 0.054(4) Uani 1 1 d . . . C18 C 0.407(5) 0.327(3) 0.6241(14) 0.094(7) Uani 1 1 d . . . H21 H 0.2949 0.3805 0.6234 0.113 Uiso 1 1 calc R . . C14 C 0.616(3) 0.1903(19) 0.5463(10) 0.059(4) Uani 1 1 d . . . C17 C 0.518(6) 0.296(3) 0.7048(12) 0.122(8) Uani 1 1 d U . . H23 H 0.4828 0.3315 0.7580 0.147 Uiso 1 1 calc R . . C16 C 0.668(5) 0.217(3) 0.7017(11) 0.103(7) Uani 1 1 d U . . H24 H 0.7254 0.1921 0.7543 0.124 Uiso 1 1 calc R . . C15 C 0.753(4) 0.164(2) 0.6304(11) 0.073(5) Uani 1 1 d . . . H25 H 0.8752 0.1194 0.6333 0.088 Uiso 1 1 calc R . . C4 C 0.257(4) 0.581(3) -0.0948(13) 0.098(6) Uani 1 1 d U . . H27 H 0.1258 0.5526 -0.1440 0.118 Uiso 1 1 calc R . . C23 C 0.941(4) 0.618(2) 0.5380(9) 0.061(5) Uani 1 1 d . . . H10A H 0.9351 0.5160 0.5539 0.073 Uiso 1 1 calc R . . H16 H 1.0464 0.6369 0.4969 0.073 Uiso 1 1 calc R . . C20 C 0.355(3) 0.3103(19) 0.4586(9) 0.049(4) Uani 1 1 d . . . H10B H 0.2737 0.2074 0.4135 0.059 Uiso 1 1 calc R . . H10C H 0.2292 0.3546 0.4692 0.059 Uiso 1 1 calc R . . C5 C 0.195(4) 0.553(2) -0.0152(12) 0.075(5) Uani 1 1 d U . . H105 H 0.0332 0.5099 -0.0092 0.090 Uiso 1 1 calc R . . C3 C 0.481(5) 0.643(3) -0.1068(13) 0.095(6) Uani 1 1 d U . . H106 H 0.5017 0.6492 -0.1634 0.114 Uiso 1 1 calc R . . C2 C 0.689(4) 0.700(3) -0.0363(13) 0.081(5) Uani 1 1 d . . . H107 H 0.8483 0.7504 -0.0432 0.097 Uiso 1 1 calc R . . C10 C 0.557(4) 0.256(2) 0.0665(11) 0.073(5) Uani 1 1 d . . . H12A H 0.6326 0.3559 0.0473 0.087 Uiso 1 1 calc R . . H15 H 0.6862 0.2433 0.1084 0.087 Uiso 1 1 calc R . . C24 C 1.067(6) 0.759(3) 0.6218(15) 0.123(10) Uani 1 1 d U . . H109 H 1.0787 0.8604 0.6025 0.147 Uiso 1 1 calc R . . C11 C 0.467(4) 0.116(3) -0.0101(12) 0.078(5) Uani 1 1 d . . . H111 H 0.3932 0.0156 0.0100 0.093 Uiso 1 1 calc R . . C12 C 0.677(4) 0.097(3) -0.0515(13) 0.094(7) Uani 1 1 d . . . H12B H 0.6093 0.0042 -0.1017 0.141 Uiso 1 1 calc R . . H12C H 0.7965 0.0804 -0.0086 0.141 Uiso 1 1 calc R . . H12D H 0.7554 0.1958 -0.0702 0.141 Uiso 1 1 calc R . . C13 C 0.260(6) 0.129(6) -0.0815(18) 0.21(2) Uani 1 1 d . . . H13A H 0.2035 0.0358 -0.1311 0.315 Uiso 1 1 calc R . . H13B H 0.3254 0.2292 -0.1009 0.315 Uiso 1 1 calc R . . H13C H 0.1231 0.1317 -0.0565 0.315 Uiso 1 1 calc R . . C26 C 0.937(6) 0.758(6) 0.689(2) 0.21(2) Uani 1 1 d U . . H26A H 0.7708 0.7470 0.6639 0.312 Uiso 1 1 calc R . . H26B H 1.0192 0.8594 0.7334 0.312 Uiso 1 1 calc R . . H26C H 0.9341 0.6664 0.7146 0.312 Uiso 1 1 calc R . . C25 C 1.332(5) 0.775(3) 0.6560(19) 0.142(14) Uani 1 1 d . . . H25A H 1.4146 0.7798 0.6086 0.213 Uiso 1 1 calc R . . H25B H 1.3331 0.6813 0.6791 0.213 Uiso 1 1 calc R . . H25C H 1.4170 0.8744 0.7021 0.213 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 Cs1 0.0575(5) 0.0284(4) 0.0537(6) 0.0122(3) 0.0107(4) 0.0129(3) Cu1 0.0729(13) 0.0219(7) 0.0239(8) 0.0089(6) 0.0069(8) 0.0131(8) Cl1 0.0443(19) 0.0387(16) 0.0503(19) 0.0153(13) 0.0128(15) 0.0155(15) O2 0.065(6) 0.032(4) 0.030(5) 0.012(4) 0.020(4) 0.012(4) O3 0.123(11) 0.028(5) 0.059(8) -0.020(5) 0.010(7) -0.011(6) O5 0.061(6) 0.025(5) 0.014(4) 0.002(3) -0.011(4) 0.018(5) O6 0.135(11) 0.033(5) 0.059(7) 0.000(5) -0.036(7) 0.030(6) O1 0.102(10) 0.102(10) 0.045(7) 0.015(7) -0.004(7) 0.029(8) O4 0.130(11) 0.071(7) 0.057(7) 0.031(5) 0.032(7) 0.061(8) O7 0.094(9) 0.013(4) 0.104(9) 0.006(5) 0.057(8) 0.006(5) N2 0.074(8) 0.037(6) 0.023(5) 0.011(4) 0.007(5) 0.030(6) N1 0.063(7) 0.029(5) 0.019(5) 0.009(4) 0.012(5) 0.005(5) C22 0.069(9) 0.028(7) 0.041(8) 0.014(5) 0.001(7) 0.025(7) C21 0.119(14) 0.018(6) 0.027(7) 0.001(5) 0.017(8) 0.012(8) C8 0.111(14) 0.032(7) 0.026(7) 0.002(5) 0.013(8) 0.013(8) C9 0.052(9) 0.031(7) 0.075(11) 0.011(7) 0.019(8) 0.010(7) C7 0.119(15) 0.041(8) 0.037(8) 0.009(6) 0.005(9) 0.034(9) C6 0.081(12) 0.033(6) 0.027(7) 0.015(5) 0.005(7) 0.021(7) C1 0.056(10) 0.046(8) 0.046(10) 0.012(7) 0.002(8) 0.022(8) C19 0.084(12) 0.049(8) 0.026(7) 0.010(6) 0.008(7) 0.021(8) C18 0.14(2) 0.082(14) 0.093(15) 0.061(11) 0.063(14) 0.053(14) C14 0.076(11) 0.050(8) 0.043(9) 0.008(7) 0.004(8) 0.020(8) C17 0.23(3) 0.125(18) 0.027(10) 0.004(10) 0.039(13) 0.089(16) C16 0.18(2) 0.107(16) 0.025(9) 0.024(9) 0.010(11) 0.064(14) C15 0.128(17) 0.065(10) 0.049(10) 0.028(8) 0.016(10) 0.059(11) C4 0.094(12) 0.114(15) 0.048(9) 0.008(9) -0.022(9) 0.015(12) C23 0.109(14) 0.055(9) 0.026(8) 0.010(7) 0.002(8) 0.047(10) C20 0.056(9) 0.055(9) 0.042(8) 0.020(7) 0.019(7) 0.020(8) C5 0.078(11) 0.055(9) 0.077(11) 0.044(9) -0.018(8) 0.009(9) C3 0.120(15) 0.104(16) 0.055(11) 0.008(10) 0.017(11) 0.040(13) C2 0.085(14) 0.088(13) 0.083(14) 0.058(11) 0.021(11) 0.029(11) C10 0.098(14) 0.056(10) 0.055(10) 0.011(7) 0.001(9) 0.026(10) C24 0.17(3) 0.073(14) 0.072(14) -0.015(11) 0.025(14) -0.010(15) C11 0.087(14) 0.086(13) 0.054(10) 0.008(9) 0.012(10) 0.032(11) C12 0.113(17) 0.076(13) 0.069(13) -0.018(10) 0.021(12) 0.022(12) C13 0.12(2) 0.34(6) 0.08(2) -0.05(3) -0.066(18) 0.08(3) C26 0.14(3) 0.25(4) 0.16(3) -0.09(3) 0.06(2) 0.03(3) C25 0.13(2) 0.095(17) 0.14(2) -0.036(16) -0.087(19) 0.045(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cs1 O1 3.181(12) 1_455 ? Cs1 O2 3.202(8) 1_565 ? Cs1 O4 3.310(14) 1_565 ? Cs1 O7 3.335(14) . ? Cs1 O7 3.344(15) 1_455 ? Cs1 O5 3.400(10) . ? Cs1 O5 3.427(11) 1_455 ? Cs1 O3 3.450(14) 1_565 ? Cs1 Cl1 3.460(3) . ? Cs1 O6 3.718(16) 1_455 ? Cs1 C9 3.714(16) 1_565 ? Cs1 C22 3.733(16) 1_455 ? Cu1 O2 1.937(8) . ? Cu1 O5 1.953(10) . ? Cu1 N2 1.966(10) . ? Cu1 N1 2.006(9) . ? O2 C9 1.296(18) . ? O2 Cs1 3.202(8) 1_545 ? O3 C9 1.238(17) . ? O3 Cs1 3.450(14) 1_545 ? O5 C22 1.254(16) . ? O5 Cs1 3.427(11) 1_655 ? O6 C22 1.243(16) . ? O6 Cs1 3.718(16) 1_655 ? O1 C1 1.401(18) . ? O1 Cs1 3.181(12) 1_655 ? O4 C14 1.384(19) . ? O4 Cs1 3.310(14) 1_545 ? O7 Cs1 3.344(15) 1_655 ? N2 C20 1.449(19) . ? N2 C21 1.471(16) . ? N2 H1 0.9100 . ? N1 C7 1.486(19) . ? N1 C8 1.505(15) . ? N1 H101 0.9100 . ? C22 C21 1.541(19) . ? C22 Cs1 3.733(16) 1_655 ? C21 C23 1.61(3) . ? C21 H100 0.9800 . ? C8 C9 1.49(2) . ? C8 C10 1.63(3) . ? C8 H3 0.9800 . ? C9 Cs1 3.714(16) 1_545 ? C7 C6 1.51(2) . ? C7 H5A 0.9700 . ? C7 H5B 0.9700 . ? C6 C1 1.35(2) . ? C6 C5 1.43(2) . ? C1 C2 1.42(2) . ? C19 C14 1.29(2) . ? C19 C18 1.40(3) . ? C19 C20 1.59(2) . ? C18 C17 1.44(3) . ? C18 H21 0.9300 . ? C14 C15 1.53(2) . ? C17 C16 1.30(3) . ? C17 H23 0.9300 . ? C16 C15 1.38(3) . ? C16 H24 0.9300 . ? C15 H25 0.9300 . ? C4 C3 1.31(3) . ? C4 C5 1.41(3) . ? C4 H27 0.9300 . ? C23 C24 1.53(2) . ? C23 H10A 0.9700 . ? C23 H16 0.9700 . ? C20 Cs1 3.907(15) 1_545 ? C20 H10B 0.9700 . ? C20 H10C 0.9700 . ? C5 H105 0.9300 . ? C3 C2 1.39(3) . ? C3 H106 0.9300 . ? C2 H107 0.9300 . ? C10 C11 1.46(2) . ? C10 H12A 0.9700 . ? C10 H15 0.9700 . ? C24 C26 1.40(4) . ? C24 C25 1.51(4) . ? C24 H109 0.9800 . ? C11 C12 1.54(3) . ? C11 C13 1.56(3) . ? C11 H111 0.9800 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 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 O1 Cs1 O2 80.6(3) 1_455 1_565 ? O1 Cs1 O4 151.9(3) 1_455 1_565 ? O2 Cs1 O4 73.4(3) 1_565 1_565 ? O1 Cs1 O7 101.7(4) 1_455 . ? O2 Cs1 O7 63.1(3) 1_565 . ? O4 Cs1 O7 57.0(3) 1_565 . ? O1 Cs1 O7 64.4(4) 1_455 1_455 ? O2 Cs1 O7 61.0(3) 1_565 1_455 ? O4 Cs1 O7 109.8(3) 1_565 1_455 ? O7 Cs1 O7 123.9(4) . 1_455 ? O1 Cs1 O5 112.9(3) 1_455 . ? O2 Cs1 O5 121.6(2) 1_565 . ? O4 Cs1 O5 73.7(2) 1_565 . ? O7 Cs1 O5 58.5(3) . . ? O7 Cs1 O5 176.4(3) 1_455 . ? O1 Cs1 O5 76.5(3) 1_455 1_455 ? O2 Cs1 O5 119.1(2) 1_565 1_455 ? O4 Cs1 O5 125.6(3) 1_565 1_455 ? O7 Cs1 O5 176.7(3) . 1_455 ? O7 Cs1 O5 58.1(2) 1_455 1_455 ? O5 Cs1 O5 119.3(3) . 1_455 ? O1 Cs1 O3 45.3(3) 1_455 1_565 ? O2 Cs1 O3 39.3(2) 1_565 1_565 ? O4 Cs1 O3 106.5(3) 1_565 1_565 ? O7 Cs1 O3 66.8(4) . 1_565 ? O7 Cs1 O3 67.2(3) 1_455 1_565 ? O5 Cs1 O3 113.0(3) . 1_565 ? O5 Cs1 O3 113.0(3) 1_455 1_565 ? O1 Cs1 Cl1 80.4(3) 1_455 . ? O2 Cs1 Cl1 159.63(15) 1_565 . ? O4 Cs1 Cl1 123.5(2) 1_565 . ? O7 Cs1 Cl1 114.1(2) . . ? O7 Cs1 Cl1 116.1(2) 1_455 . ? O5 Cs1 Cl1 60.59(19) . . ? O5 Cs1 Cl1 62.89(16) 1_455 . ? O3 Cs1 Cl1 120.34(16) 1_565 . ? O1 Cs1 O6 107.1(3) 1_455 1_455 ? O2 Cs1 O6 107.3(2) 1_565 1_455 ? O4 Cs1 O6 90.9(3) 1_565 1_455 ? O7 Cs1 O6 147.7(3) . 1_455 ? O7 Cs1 O6 59.8(3) 1_455 1_455 ? O5 Cs1 O6 120.0(2) . 1_455 ? O5 Cs1 O6 35.2(2) 1_455 1_455 ? O3 Cs1 O6 127.0(3) 1_565 1_455 ? Cl1 Cs1 O6 85.24(17) . 1_455 ? O1 Cs1 C9 62.8(4) 1_455 1_565 ? O2 Cs1 C9 19.9(3) 1_565 1_565 ? O4 Cs1 C9 89.7(3) 1_565 1_565 ? O7 Cs1 C9 62.5(3) . 1_565 ? O7 Cs1 C9 63.3(3) 1_455 1_565 ? O5 Cs1 C9 118.1(3) . 1_565 ? O5 Cs1 C9 118.6(3) 1_455 1_565 ? O3 Cs1 C9 19.5(3) 1_565 1_565 ? Cl1 Cs1 C9 139.8(2) . 1_565 ? O6 Cs1 C9 119.4(3) 1_455 1_565 ? O1 Cs1 C22 96.1(3) 1_455 1_455 ? O2 Cs1 C22 121.9(2) 1_565 1_455 ? O4 Cs1 C22 106.5(3) 1_565 1_455 ? O7 Cs1 C22 162.2(3) . 1_455 ? O7 Cs1 C22 65.5(3) 1_455 1_455 ? O5 Cs1 C22 113.0(3) . 1_455 ? O5 Cs1 C22 19.6(2) 1_455 1_455 ? O3 Cs1 C22 129.0(3) 1_565 1_455 ? Cl1 Cs1 C22 67.48(19) . 1_455 ? O6 Cs1 C22 19.2(2) 1_455 1_455 ? C9 Cs1 C22 128.8(3) 1_565 1_455 ? O2 Cu1 O5 175.9(4) . . ? O2 Cu1 N2 94.0(4) . . ? O5 Cu1 N2 85.9(4) . . ? O2 Cu1 N1 84.9(4) . . ? O5 Cu1 N1 94.2(4) . . ? N2 Cu1 N1 165.2(5) . . ? C9 O2 Cu1 115.4(8) . . ? C9 O2 Cs1 103.0(7) . 1_545 ? Cu1 O2 Cs1 141.5(4) . 1_545 ? C9 O3 Cs1 92.4(10) . 1_545 ? C22 O5 Cu1 114.0(8) . . ? C22 O5 Cs1 100.1(8) . . ? Cu1 O5 Cs1 110.9(4) . . ? C22 O5 Cs1 94.1(9) . 1_655 ? Cu1 O5 Cs1 115.9(4) . 1_655 ? Cs1 O5 Cs1 119.3(3) . 1_655 ? C22 O6 Cs1 81.1(10) . 1_655 ? C1 O1 Cs1 166.2(11) . 1_655 ? C14 O4 Cs1 112.3(10) . 1_545 ? Cs1 O7 Cs1 123.9(4) . 1_655 ? C20 N2 C21 115.0(11) . . ? C20 N2 Cu1 118.8(9) . . ? C21 N2 Cu1 110.8(8) . . ? C20 N2 H1 103.3 . . ? C21 N2 H1 103.3 . . ? Cu1 N2 H1 103.3 . . ? C7 N1 C8 115.1(11) . . ? C7 N1 Cu1 117.4(9) . . ? C8 N1 Cu1 110.0(8) . . ? C7 N1 H101 104.2 . . ? C8 N1 H101 104.2 . . ? Cu1 N1 H101 104.2 . . ? O6 C22 O5 121.5(12) . . ? O6 C22 C21 119.0(12) . . ? O5 C22 C21 119.3(11) . . ? O6 C22 Cs1 79.7(10) . 1_655 ? O5 C22 Cs1 66.3(8) . 1_655 ? C21 C22 Cs1 122.4(10) . 1_655 ? O6 C22 Cs1 83.5(8) . . ? O5 C22 Cs1 61.0(7) . . ? C21 C22 Cs1 131.6(11) . . ? Cs1 C22 Cs1 102.5(3) 1_655 . ? N2 C21 C22 109.7(11) . . ? N2 C21 C23 111.9(12) . . ? C22 C21 C23 108.6(14) . . ? N2 C21 H100 108.9 . . ? C22 C21 H100 108.9 . . ? C23 C21 H100 108.9 . . ? C9 C8 N1 110.4(11) . . ? C9 C8 C10 112.1(13) . . ? N1 C8 C10 109.1(13) . . ? C9 C8 H3 108.4 . . ? N1 C8 H3 108.4 . . ? C10 C8 H3 108.4 . . ? O3 C9 O2 125.1(14) . . ? O3 C9 C8 115.9(14) . . ? O2 C9 C8 118.9(12) . . ? O3 C9 Cs1 68.2(9) . 1_545 ? O2 C9 Cs1 57.2(7) . 1_545 ? C8 C9 Cs1 170.6(11) . 1_545 ? N1 C7 C6 114.1(13) . . ? N1 C7 H5A 108.7 . . ? C6 C7 H5A 108.7 . . ? N1 C7 H5B 108.7 . . ? C6 C7 H5B 108.7 . . ? H5A C7 H5B 107.6 . . ? C1 C6 C5 122.9(14) . . ? C1 C6 C7 121.9(14) . . ? C5 C6 C7 114.9(16) . . ? C6 C1 O1 118.6(14) . . ? C6 C1 C2 121.3(15) . . ? O1 C1 C2 120.1(16) . . ? C14 C19 C18 121.9(16) . . ? C14 C19 C20 120.5(13) . . ? C18 C19 C20 117.5(15) . . ? C19 C18 C17 117(2) . . ? C19 C18 H21 121.3 . . ? C17 C18 H21 121.3 . . ? C19 C14 O4 120.5(14) . . ? C19 C14 C15 122.7(14) . . ? O4 C14 C15 116.3(14) . . ? C16 C17 C18 118.8(18) . . ? C16 C17 H23 120.6 . . ? C18 C17 H23 120.6 . . ? C17 C16 C15 128.4(19) . . ? C17 C16 H24 115.8 . . ? C15 C16 H24 115.8 . . ? C16 C15 C14 110.0(17) . . ? C16 C15 H25 125.0 . . ? C14 C15 H25 125.0 . . ? C3 C4 C5 126.6(19) . . ? C3 C4 H27 116.7 . . ? C5 C4 H27 116.7 . . ? C24 C23 C21 118.1(17) . . ? C24 C23 H10A 107.8 . . ? C21 C23 H10A 107.8 . . ? C24 C23 H16 107.8 . . ? C21 C23 H16 107.8 . . ? H10A C23 H16 107.1 . . ? N2 C20 C19 112.2(12) . . ? N2 C20 Cs1 108.9(8) . 1_545 ? C19 C20 Cs1 94.0(8) . 1_545 ? N2 C20 H10B 109.2 . . ? C19 C20 H10B 109.2 . . ? Cs1 C20 H10B 17.5 1_545 . ? N2 C20 H10C 109.2 . . ? C19 C20 H10C 109.2 . . ? Cs1 C20 H10C 122.6 1_545 . ? H10B C20 H10C 107.9 . . ? C4 C5 C6 111.8(18) . . ? C4 C5 H105 124.1 . . ? C6 C5 H105 124.1 . . ? C4 C3 C2 121(2) . . ? C4 C3 H106 119.5 . . ? C2 C3 H106 119.5 . . ? C3 C2 C1 116.0(19) . . ? C3 C2 H107 122.0 . . ? C1 C2 H107 122.0 . . ? C11 C10 C8 116.1(15) . . ? C11 C10 H12A 108.3 . . ? C8 C10 H12A 108.3 . . ? C11 C10 H15 108.3 . . ? C8 C10 H15 108.3 . . ? H12A C10 H15 107.4 . . ? C26 C24 C25 113(3) . . ? C26 C24 C23 117(2) . . ? C25 C24 C23 110(2) . . ? C26 C24 H109 105.4 . . ? C25 C24 H109 105.4 . . ? C23 C24 H109 105.4 . . ? C10 C11 C12 112.2(17) . . ? C10 C11 C13 111(2) . . ? C12 C11 C13 110.0(19) . . ? C10 C11 H111 107.8 . . ? C12 C11 H111 107.8 . . ? C13 C11 H111 107.8 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12B C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.224 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.135 _database_code_depnum_ccdc_archive 'CCDC 943447' ####################################################################### # # 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_Complex3 # CCDC 943448 _audit_creation_method SHELXL-97 _chemical_name_systematic Complex3 _chemical_name_common complex3 _chemical_formula_moiety 'C78 H102 Cs Cu3 N6 O18 N O3 H12 O6' _chemical_formula_sum 'C78 H102 Cs Cu3 N6 O18 N O3 H12 O6' _chemical_compound_source syn _exptl_crystal_recrystallization_method methanol _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour blue _diffrn_ambient_temperature 296(2) _chemical_formula_weight 1905.32 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_int_tables_number 20 _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.365(4) _cell_length_b 21.101(5) _cell_length_c 27.684(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10728(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.62 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3595.73 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 45718 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.24 _reflns_number_total 8374 _reflns_number_gt 4736 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. DFIX 1.54 0.02 C3A C4A C4A C5A C4A C6A DFIX 1.54 0.02 C4B C3B C4B C6B C5B C4B DFIX 1.54 0.02 C3 C4 C4 C6 C4 C5 ; _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^)+(0.1991P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.25(3) _refine_ls_number_reflns 8374 _refine_ls_number_parameters 463 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.2883 _refine_ls_wR_factor_gt 0.2668 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 C8A C 0.5863(4) -0.0595(3) 0.6800(2) 0.110(4) Uani 1 1 d G . . C13A C 0.5515(4) -0.1168(3) 0.6888(3) 0.150(7) Uani 1 1 d G . . H13A H 0.5047 -0.1172 0.7016 0.180 Uiso 1 1 calc R . . C12A C 0.5865(4) -0.1736(3) 0.6784(3) 0.106(5) Uani 1 1 d G . . H12A H 0.5632 -0.2119 0.6844 0.128 Uiso 1 1 calc R . . C11A C 0.6565(5) -0.1730(2) 0.6592(2) 0.082(3) Uani 1 1 d G . . H11A H 0.6799 -0.2110 0.6523 0.099 Uiso 1 1 calc R . . C10A C 0.6913(4) -0.1157(3) 0.6504(3) 0.096(4) Uani 1 1 d G . . H10A H 0.7381 -0.1154 0.6376 0.115 Uiso 1 1 calc R . . C9A C 0.6563(3) -0.0590(2) 0.66077(19) 0.080(3) Uani 1 1 d G . . C8 C 0.5968(4) 0.2243(2) 0.5586(3) 0.074(3) Uani 1 1 d G . . C13 C 0.6308(4) 0.2817(2) 0.5487(3) 0.072(3) Uani 1 1 d G . . H13 H 0.6409 0.3097 0.5738 0.086 Uiso 1 1 calc R . . C12 C 0.6494(6) 0.2974(6) 0.5024(5) 0.087(3) Uani 1 1 d . . . H12 H 0.6714 0.3362 0.4961 0.105 Uiso 1 1 calc R . . C11 C 0.6353(7) 0.2542(8) 0.4634(5) 0.106(5) Uani 1 1 d . . . H11 H 0.6482 0.2648 0.4319 0.127 Uiso 1 1 calc R . . C10 C 0.6015(8) 0.1958(5) 0.4735(4) 0.084(3) Uani 1 1 d . . . H10 H 0.5915 0.1671 0.4489 0.101 Uiso 1 1 calc R . . C9 C 0.5838(6) 0.1824(5) 0.5204(5) 0.080(3) Uani 1 1 d . . . C9B C 0.8835(6) 0.1477(4) 0.4704(3) 0.060(2) Uani 1 1 d . . . C10B C 0.8285(7) 0.1899(5) 0.4590(5) 0.085(3) Uani 1 1 d . . . H10B H 0.7904 0.1948 0.4808 0.103 Uiso 1 1 calc R . . C11B C 0.8271(12) 0.2255(8) 0.4166(7) 0.134(6) Uani 1 1 d . . . H11B H 0.7892 0.2536 0.4104 0.161 Uiso 1 1 calc R . . C12B C 0.8848(8) 0.2177(6) 0.3833(5) 0.096(4) Uani 1 1 d . . . H12B H 0.8851 0.2397 0.3542 0.116 Uiso 1 1 calc R . . C13B C 0.9421(10) 0.1756(7) 0.3951(6) 0.127(5) Uani 1 1 d . . . H13B H 0.9815 0.1716 0.3742 0.152 Uiso 1 1 calc R . . C8B C 0.9407(7) 0.1383(5) 0.4395(4) 0.080(3) Uani 1 1 d . . . Cu2 Cu 0.90590(9) 0.0000 0.5000 0.0679(5) Uani 1 2 d S . . Cu1 Cu 0.60768(7) 0.07316(5) 0.60274(4) 0.0644(4) Uani 1 1 d . . . Cs1 Cs 0.70692(17) 0.0000 0.5000 0.302(3) Uani 1 2 d S . . O1B O 0.8363(4) 0.0071(3) 0.4460(2) 0.0676(17) Uani 1 1 d . . . O1A O 0.5867(4) -0.0013(3) 0.5658(2) 0.085(2) Uani 1 1 d . . . N1A N 0.5254(6) 0.0363(5) 0.6445(3) 0.082(3) Uani 1 1 d . . . H1A H 0.4993 0.0701 0.6553 0.098 Uiso 1 1 calc R . . C2A C 0.4778(6) 0.0017(6) 0.6136(4) 0.088(3) Uani 1 1 d . . . H2A H 0.4568 -0.0337 0.6319 0.105 Uiso 1 1 calc R . . N1B N 0.9754(5) 0.0274(4) 0.4509(3) 0.073(2) Uani 1 1 d . . . H1B H 1.0151 0.0026 0.4561 0.087 Uiso 1 1 calc R . . O3B O 0.8814(4) 0.1175(3) 0.5146(3) 0.086(2) Uani 1 1 d . . . C7B C 1.0030(6) 0.0897(5) 0.4522(5) 0.085(3) Uani 1 1 d . . . H7B2 H 1.0424 0.0938 0.4291 0.102 Uiso 1 1 calc R . . H7B1 H 1.0221 0.0987 0.4841 0.102 Uiso 1 1 calc R . . O1 O 0.6969(3) 0.0963(3) 0.5714(2) 0.0587(16) Uani 1 1 d . . . C1B C 0.8609(5) 0.0058(5) 0.4027(4) 0.061(2) Uani 1 1 d . . . C2B C 0.9471(6) 0.0068(5) 0.3974(4) 0.080(3) Uani 1 1 d . . . H2B H 0.9636 0.0360 0.3722 0.097 Uiso 1 1 calc R . . C2 C 0.6936(6) 0.1770(5) 0.6367(4) 0.070(3) Uani 1 1 d . . . H2 H 0.6987 0.2232 0.6353 0.084 Uiso 1 1 calc R . . C7 C 0.5743(5) 0.2080(5) 0.6080(4) 0.066(2) Uani 1 1 d . . . H7A H 0.5255 0.1904 0.6069 0.079 Uiso 1 1 calc R . . H7B H 0.5721 0.2466 0.6270 0.079 Uiso 1 1 calc R . . N1 N 0.6250(5) 0.1599(4) 0.6344(3) 0.070(2) Uani 1 1 d . . . H1 H 0.6087 0.1569 0.6653 0.084 Uiso 1 1 calc R . . C1 C 0.7336(6) 0.1433(5) 0.5913(3) 0.058(2) Uani 1 1 d . . . O2 O 0.7905(5) 0.1625(4) 0.5789(3) 0.087(2) Uani 1 1 d . . . O2B O 0.8285(5) 0.0132(4) 0.3659(3) 0.092(2) Uani 1 1 d . . . C7A C 0.5549(9) 0.0046(7) 0.6882(5) 0.111(4) Uani 1 1 d . . . H7A2 H 0.5161 0.0009 0.7118 0.133 Uiso 1 1 calc R . . H7A1 H 0.5923 0.0314 0.7021 0.133 Uiso 1 1 calc R . . O3A O 0.6917(4) -0.0044(3) 0.6487(3) 0.0745(18) Uani 1 1 d . . . O2A O 0.4941(4) -0.0687(4) 0.5465(3) 0.081(2) Uani 1 1 d . . . C1A C 0.5200(5) -0.0250(5) 0.5707(3) 0.057(2) Uani 1 1 d . . . C3A C 0.4136(5) 0.0421(5) 0.5907(4) 0.077(3) Uani 1 1 d D . . H3A1 H 0.4344 0.0813 0.5788 0.093 Uiso 1 1 calc R . . H3A2 H 0.3955 0.0190 0.5629 0.093 Uiso 1 1 calc R . . C3 C 0.7322(8) 0.1498(6) 0.6811(4) 0.090(4) Uani 1 1 d D . . H3B H 0.7052 0.1115 0.6883 0.108 Uiso 1 1 calc R . . H3A H 0.7788 0.1355 0.6687 0.108 Uiso 1 1 calc R . . C4B C 1.008(2) -0.0829(14) 0.3393(13) 0.55(8) Uani 1 1 d D . . H4B H 0.9731 -0.0834 0.3123 0.659 Uiso 1 1 calc R . . C3B C 0.9641(8) -0.0660(8) 0.3844(5) 0.112(4) Uani 1 1 d D . . H3B2 H 0.9895 -0.0841 0.4118 0.134 Uiso 1 1 calc R . . H3B1 H 0.9177 -0.0876 0.3820 0.134 Uiso 1 1 calc R . . C5B C 1.0677(19) -0.0360(18) 0.326(2) 0.33(4) Uani 1 1 d D . . H5B1 H 1.0569 -0.0176 0.2948 0.497 Uiso 1 1 calc R . . H5B2 H 1.1135 -0.0578 0.3241 0.497 Uiso 1 1 calc R . . H5B3 H 1.0704 -0.0032 0.3496 0.497 Uiso 1 1 calc R . . O3 O 0.5455(4) 0.1265(3) 0.5277(2) 0.0733(19) Uani 1 1 d . . . C4 C 0.7501(17) 0.1766(11) 0.7296(9) 0.29(2) Uani 1 1 d D . . H4 H 0.7467 0.2221 0.7362 0.345 Uiso 1 1 calc R . . C6 C 0.685(3) 0.133(3) 0.736(3) 0.49(5) Uiso 1 1 d D . . H6B H 0.6781 0.1078 0.7073 0.734 Uiso 1 1 calc R . . H6A H 0.6419 0.1574 0.7419 0.734 Uiso 1 1 calc R . . H6C H 0.6933 0.1049 0.7630 0.734 Uiso 1 1 calc R . . C6A C 0.2886(11) 0.0937(10) 0.5918(9) 0.182(10) Uani 1 1 d D . . H6A3 H 0.3015 0.1375 0.5881 0.273 Uiso 1 1 calc R . . H6A1 H 0.2424 0.0906 0.6078 0.273 Uiso 1 1 calc R . . H6A2 H 0.2853 0.0742 0.5605 0.273 Uiso 1 1 calc R . . C4A C 0.3479(10) 0.0593(10) 0.6224(6) 0.150(7) Uani 1 1 d D . . H4A H 0.3693 0.0980 0.6358 0.180 Uiso 1 1 calc R . . C6B C 1.036(2) -0.1516(12) 0.3450(13) 0.30(2) Uani 1 1 d D . . H6B2 H 1.0330 -0.1732 0.3146 0.445 Uiso 1 1 calc R . . H6B1 H 1.0074 -0.1735 0.3686 0.445 Uiso 1 1 calc R . . H6B3 H 1.0861 -0.1506 0.3554 0.445 Uiso 1 1 calc R . . C5 C 0.8215(12) 0.1374(13) 0.7416(10) 0.200(11) Uani 1 1 d D . . H5B H 0.8093 0.0935 0.7454 0.300 Uiso 1 1 calc R . . H5C H 0.8425 0.1530 0.7710 0.300 Uiso 1 1 calc R . . H5A H 0.8558 0.1421 0.7157 0.300 Uiso 1 1 calc R . . C5A C 0.3427(17) 0.0240(16) 0.6707(10) 0.29(2) Uani 1 1 d D . . H5A2 H 0.3232 0.0519 0.6949 0.431 Uiso 1 1 calc R . . H5A1 H 0.3903 0.0101 0.6803 0.431 Uiso 1 1 calc R . . H5A3 H 0.3112 -0.0120 0.6671 0.431 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 C8A 0.102(10) 0.124(12) 0.105(10) -0.007(8) -0.006(8) -0.012(9) C13A 0.22(2) 0.125(14) 0.103(12) 0.025(11) -0.019(13) -0.014(14) C12A 0.136(13) 0.069(8) 0.114(10) 0.034(7) -0.043(9) -0.005(8) C11A 0.072(8) 0.086(8) 0.089(8) 0.032(6) -0.007(7) -0.006(6) C10A 0.119(10) 0.088(8) 0.081(8) 0.028(7) -0.029(8) 0.016(8) C9A 0.113(9) 0.069(8) 0.058(6) -0.002(5) 0.006(6) 0.018(7) C8 0.091(8) 0.067(6) 0.065(6) 0.017(5) 0.014(6) -0.002(6) C13 0.062(6) 0.076(7) 0.079(8) -0.010(6) 0.007(5) 0.007(5) C12 0.094(8) 0.092(8) 0.077(8) 0.008(7) 0.011(8) 0.004(6) C11 0.096(9) 0.162(14) 0.061(8) 0.027(8) -0.005(7) 0.040(9) C10 0.113(9) 0.057(6) 0.082(8) 0.005(5) -0.025(8) -0.014(7) C9 0.080(8) 0.074(7) 0.087(8) 0.011(6) 0.021(6) 0.013(6) C9B 0.071(7) 0.054(5) 0.053(5) -0.008(4) 0.031(5) 0.000(5) C10B 0.108(10) 0.067(7) 0.081(8) 0.000(6) 0.030(7) -0.004(7) C11B 0.161(17) 0.124(13) 0.118(14) 0.005(11) -0.052(14) 0.007(12) C12B 0.108(10) 0.076(8) 0.105(10) 0.017(7) -0.002(9) -0.001(8) C13B 0.164(15) 0.106(10) 0.110(11) 0.029(10) 0.034(11) -0.033(11) C8B 0.082(8) 0.065(7) 0.092(8) -0.003(6) -0.011(7) -0.005(6) Cu2 0.0638(10) 0.0768(10) 0.0630(10) -0.0054(8) 0.000 0.000 Cu1 0.0754(8) 0.0634(7) 0.0543(7) -0.0041(5) 0.0042(6) 0.0011(6) Cs1 0.179(2) 0.461(7) 0.266(4) -0.123(4) 0.000 0.000 O1B 0.074(4) 0.082(4) 0.046(4) -0.003(3) -0.008(3) -0.002(4) O1A 0.114(6) 0.075(4) 0.065(4) 0.000(4) 0.027(4) -0.002(5) N1A 0.101(7) 0.081(6) 0.064(6) 0.000(5) 0.020(5) 0.025(5) C2A 0.099(8) 0.070(6) 0.094(9) -0.010(7) 0.032(7) -0.026(7) N1B 0.072(5) 0.081(6) 0.065(5) -0.006(4) 0.013(4) 0.015(4) O3B 0.108(6) 0.054(4) 0.097(5) 0.018(4) 0.006(5) -0.011(4) C7B 0.059(6) 0.084(8) 0.111(10) -0.006(7) 0.010(6) -0.011(6) O1 0.062(4) 0.065(4) 0.049(4) -0.009(3) 0.007(3) -0.007(3) C1B 0.070(6) 0.066(6) 0.048(6) -0.016(5) 0.005(5) 0.009(5) C2B 0.091(7) 0.076(7) 0.074(7) -0.003(6) 0.003(6) 0.008(6) C2 0.064(7) 0.086(7) 0.062(7) 0.007(5) -0.020(5) 0.006(6) C7 0.063(6) 0.075(6) 0.058(6) -0.007(5) 0.006(5) 0.008(5) N1 0.096(7) 0.057(5) 0.058(5) 0.002(4) 0.015(5) 0.006(4) C1 0.051(6) 0.081(7) 0.043(5) -0.001(5) 0.001(5) -0.002(5) O2 0.085(6) 0.092(5) 0.082(5) -0.007(4) -0.005(5) -0.002(5) O2B 0.103(6) 0.113(6) 0.060(5) 0.007(4) -0.004(4) 0.010(5) C7A 0.137(11) 0.104(10) 0.091(9) 0.009(8) 0.034(9) 0.017(10) O3A 0.095(5) 0.064(4) 0.064(4) 0.016(3) -0.013(4) -0.002(4) O2A 0.069(4) 0.081(5) 0.092(5) 0.016(5) 0.015(4) -0.008(4) C1A 0.055(6) 0.056(5) 0.060(6) -0.006(5) 0.006(5) -0.019(4) C3A 0.061(6) 0.080(7) 0.091(8) -0.002(6) 0.007(6) 0.007(5) C3 0.110(9) 0.099(8) 0.061(7) 0.012(6) 0.007(7) 0.009(7) C4B 0.32(6) 0.38(9) 1.0(2) -0.28(12) -0.16(10) 0.23(7) C3B 0.103(10) 0.122(11) 0.111(10) 0.004(9) 0.029(8) 0.019(9) C5B 0.20(3) 0.20(3) 0.59(10) 0.07(5) 0.13(5) 0.02(2) O3 0.078(5) 0.082(5) 0.061(4) 0.004(3) -0.006(4) -0.004(4) C4 0.44(5) 0.131(19) 0.29(4) -0.03(2) -0.23(4) -0.04(3) C6A 0.153(17) 0.160(18) 0.23(2) -0.057(17) 0.055(18) 0.030(13) C4A 0.147(15) 0.177(18) 0.127(14) 0.030(13) 0.037(12) 0.051(14) C6B 0.47(6) 0.15(2) 0.27(3) -0.04(2) 0.12(4) 0.13(3) C5 0.17(2) 0.21(2) 0.22(2) -0.02(2) -0.092(19) 0.053(18) C5A 0.25(3) 0.30(3) 0.31(4) 0.14(3) 0.19(3) 0.11(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C8A C13A 1.3900 . ? C8A C9A 1.3900 . ? C8A C7A 1.488(16) . ? C13A C12A 1.3900 . ? C12A C11A 1.3900 . ? C11A C10A 1.3900 . ? C10A C9A 1.3900 . ? C9A O3A 1.364(9) . ? C8 C13 1.3900 . ? C8 C9 1.397(14) . ? C8 C7 1.472(12) . ? C13 C12 1.368(15) . ? C12 C11 1.44(2) . ? C11 C10 1.408(19) . ? C10 C9 1.370(16) . ? C9 O3 1.390(13) . ? C9B C8B 1.369(15) . ? C9B O3B 1.380(11) . ? C9B C10B 1.383(16) . ? C10B C11B 1.39(2) . ? C11B C12B 1.41(2) . ? C12B C13B 1.42(2) . ? C13B C8B 1.460(19) . ? C8B C7B 1.575(16) . ? Cu2 N1B 1.952(8) . ? Cu2 N1B 1.952(8) 4_556 ? Cu2 O1B 1.973(6) . ? Cu2 O1B 1.973(6) 4_556 ? Cu2 Cs1 3.654(4) . ? Cu1 O1A 1.914(8) . ? Cu1 O1 1.918(6) . ? Cu1 N1 2.053(8) . ? Cu1 N1A 2.054(10) . ? Cu1 Cs1 3.714(2) . ? Cs1 O1B 2.810(7) . ? Cs1 O1B 2.810(7) 4_556 ? Cs1 O1 2.840(6) 4_556 ? Cs1 O1 2.840(6) . ? Cs1 O1A 2.861(7) 4_556 ? Cs1 O1A 2.861(7) . ? Cs1 Cu1 3.714(2) 4_556 ? Cs1 C1B 3.907(10) . ? Cs1 C1B 3.907(10) 4_556 ? O1B C1B 1.282(11) . ? O1A C1A 1.331(11) . ? N1A C2A 1.425(15) . ? N1A C7A 1.486(16) . ? C2A C1A 1.526(14) . ? C2A C3A 1.587(16) . ? N1B C7B 1.408(14) . ? N1B C2B 1.629(15) . ? O1 C1 1.320(12) . ? C1B O2B 1.190(11) . ? C1B C2B 1.590(14) . ? C2B C3B 1.607(19) . ? C2 N1 1.313(13) . ? C2 C3 1.530(15) . ? C2 C1 1.621(15) . ? C7 N1 1.558(13) . ? C1 O2 1.173(11) . ? O2A C1A 1.236(11) . ? C3A C4A 1.536(14) . ? C3 C4 1.493(17) . ? C4B C3B 1.52(2) . ? C4B C5B 1.527(19) . ? C4B C6B 1.549(19) . ? C4 C6 1.53(2) . ? C4 C5 1.585(18) . ? C6A C4A 1.560(17) . ? C4A C5A 1.534(17) . ? 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 C13A C8A C9A 120.0 . . ? C13A C8A C7A 125.8(7) . . ? C9A C8A C7A 114.2(7) . . ? C12A C13A C8A 120.0 . . ? C11A C12A C13A 120.0 . . ? C12A C11A C10A 120.0 . . ? C11A C10A C9A 120.0 . . ? O3A C9A C10A 117.1(4) . . ? O3A C9A C8A 122.8(4) . . ? C10A C9A C8A 120.0 . . ? C13 C8 C9 118.7(6) . . ? C13 C8 C7 120.8(5) . . ? C9 C8 C7 120.5(7) . . ? C12 C13 C8 120.4(7) . . ? C13 C12 C11 120.4(11) . . ? C10 C11 C12 119.1(11) . . ? C9 C10 C11 118.2(11) . . ? C10 C9 O3 115.6(11) . . ? C10 C9 C8 123.1(10) . . ? O3 C9 C8 121.0(9) . . ? C8B C9B O3B 120.5(9) . . ? C8B C9B C10B 120.8(9) . . ? O3B C9B C10B 118.6(9) . . ? C9B C10B C11B 123.5(14) . . ? C10B C11B C12B 118.2(16) . . ? C13B C12B C11B 118.6(13) . . ? C12B C13B C8B 121.4(14) . . ? C9B C8B C13B 117.5(12) . . ? C9B C8B C7B 120.8(10) . . ? C13B C8B C7B 121.7(12) . . ? N1B Cu2 N1B 98.4(5) . 4_556 ? N1B Cu2 O1B 82.8(3) . . ? N1B Cu2 O1B 166.8(3) 4_556 . ? N1B Cu2 O1B 166.8(3) . 4_556 ? N1B Cu2 O1B 82.8(3) 4_556 4_556 ? O1B Cu2 O1B 99.2(4) . 4_556 ? N1B Cu2 Cs1 130.8(3) . . ? N1B Cu2 Cs1 130.8(3) 4_556 . ? O1B Cu2 Cs1 49.6(2) . . ? O1B Cu2 Cs1 49.6(2) 4_556 . ? O1A Cu1 O1 97.9(3) . . ? O1A Cu1 N1 172.1(3) . . ? O1 Cu1 N1 80.4(3) . . ? O1A Cu1 N1A 81.0(3) . . ? O1 Cu1 N1A 168.3(3) . . ? N1 Cu1 N1A 102.2(4) . . ? O1A Cu1 Cs1 49.3(2) . . ? O1 Cu1 Cs1 48.66(18) . . ? N1 Cu1 Cs1 128.4(3) . . ? N1A Cu1 Cs1 129.4(3) . . ? O1B Cs1 O1B 64.6(3) . 4_556 ? O1B Cs1 O1 73.90(19) . 4_556 ? O1B Cs1 O1 112.7(2) 4_556 4_556 ? O1B Cs1 O1 112.7(2) . . ? O1B Cs1 O1 73.90(19) 4_556 . ? O1 Cs1 O1 172.6(3) 4_556 . ? O1B Cs1 O1A 108.2(2) . 4_556 ? O1B Cs1 O1A 172.2(2) 4_556 4_556 ? O1 Cs1 O1A 60.93(19) 4_556 4_556 ? O1 Cs1 O1A 112.7(2) . 4_556 ? O1B Cs1 O1A 172.2(2) . . ? O1B Cs1 O1A 108.2(2) 4_556 . ? O1 Cs1 O1A 112.7(2) 4_556 . ? O1 Cs1 O1A 60.93(19) . . ? O1A Cs1 O1A 79.0(3) 4_556 . ? O1B Cs1 Cu2 32.30(13) . . ? O1B Cs1 Cu2 32.30(13) 4_556 . ? O1 Cs1 Cu2 93.71(14) 4_556 . ? O1 Cs1 Cu2 93.71(14) . . ? O1A Cs1 Cu2 140.48(16) 4_556 . ? O1A Cs1 Cu2 140.48(16) . . ? O1B Cs1 Cu1 91.70(13) . 4_556 ? O1B Cs1 Cu1 143.12(14) 4_556 4_556 ? O1 Cs1 Cu1 30.47(12) 4_556 4_556 ? O1 Cs1 Cu1 142.98(16) . 4_556 ? O1A Cs1 Cu1 30.47(15) 4_556 4_556 ? O1A Cs1 Cu1 96.02(18) . 4_556 ? Cu2 Cs1 Cu1 119.39(5) . 4_556 ? O1B Cs1 Cu1 143.12(14) . . ? O1B Cs1 Cu1 91.70(13) 4_556 . ? O1 Cs1 Cu1 142.98(16) 4_556 . ? O1 Cs1 Cu1 30.47(12) . . ? O1A Cs1 Cu1 96.02(18) 4_556 . ? O1A Cs1 Cu1 30.47(15) . . ? Cu2 Cs1 Cu1 119.39(5) . . ? Cu1 Cs1 Cu1 121.23(9) 4_556 . ? O1B Cs1 C1B 11.49(19) . . ? O1B Cs1 C1B 75.9(2) 4_556 . ? O1 Cs1 C1B 65.76(19) 4_556 . ? O1 Cs1 C1B 120.3(2) . . ? O1A Cs1 C1B 96.9(2) 4_556 . ? O1A Cs1 C1B 175.7(2) . . ? Cu2 Cs1 C1B 43.63(16) . . ? Cu1 Cs1 C1B 80.81(15) 4_556 . ? Cu1 Cs1 C1B 150.47(15) . . ? O1B Cs1 C1B 75.9(2) . 4_556 ? O1B Cs1 C1B 11.49(19) 4_556 4_556 ? O1 Cs1 C1B 120.27(19) 4_556 4_556 ? O1 Cs1 C1B 65.76(19) . 4_556 ? O1A Cs1 C1B 175.7(2) 4_556 4_556 ? O1A Cs1 C1B 96.9(2) . 4_556 ? Cu2 Cs1 C1B 43.63(16) . 4_556 ? Cu1 Cs1 C1B 150.47(15) 4_556 4_556 ? Cu1 Cs1 C1B 80.81(15) . 4_556 ? C1B Cs1 C1B 87.3(3) . 4_556 ? C1B O1B Cu2 118.5(6) . . ? C1B O1B Cs1 142.6(6) . . ? Cu2 O1B Cs1 98.1(3) . . ? C1A O1A Cu1 116.0(6) . . ? C1A O1A Cs1 141.2(6) . . ? Cu1 O1A Cs1 100.2(3) . . ? C2A N1A C7A 118.7(11) . . ? C2A N1A Cu1 108.0(6) . . ? C7A N1A Cu1 111.2(8) . . ? N1A C2A C1A 110.1(8) . . ? N1A C2A C3A 114.8(10) . . ? C1A C2A C3A 105.3(9) . . ? C7B N1B C2B 112.8(9) . . ? C7B N1B Cu2 119.6(7) . . ? C2B N1B Cu2 110.2(6) . . ? N1B C7B C8B 109.9(9) . . ? C1 O1 Cu1 116.0(6) . . ? C1 O1 Cs1 142.7(6) . . ? Cu1 O1 Cs1 100.9(2) . . ? O2B C1B O1B 128.4(9) . . ? O2B C1B C2B 114.6(10) . . ? O1B C1B C2B 116.0(9) . . ? O2B C1B Cs1 103.4(6) . . ? C2B C1B Cs1 141.7(7) . . ? C1B C2B C3B 101.6(9) . . ? C1B C2B N1B 103.7(8) . . ? C3B C2B N1B 113.5(10) . . ? N1 C2 C3 112.4(10) . . ? N1 C2 C1 106.0(9) . . ? C3 C2 C1 104.3(8) . . ? C8 C7 N1 114.8(7) . . ? C2 N1 C7 114.7(8) . . ? C2 N1 Cu1 114.6(7) . . ? C7 N1 Cu1 106.8(6) . . ? O2 C1 O1 126.3(9) . . ? O2 C1 C2 118.7(9) . . ? O1 C1 C2 115.1(9) . . ? N1A C7A C8A 115.2(11) . . ? O2A C1A O1A 125.4(9) . . ? O2A C1A C2A 120.1(9) . . ? O1A C1A C2A 114.2(9) . . ? C4A C3A C2A 118.9(10) . . ? C4 C3 C2 133.0(13) . . ? C3B C4B C5B 115(3) . . ? C3B C4B C6B 108(2) . . ? C5B C4B C6B 113(3) . . ? C4B C3B C2B 120.6(15) . . ? C3 C4 C6 73(3) . . ? C3 C4 C5 100.0(17) . . ? C6 C4 C5 108(3) . . ? C5A C4A C3A 115.6(14) . . ? C5A C4A C6A 131.0(18) . . ? C3A C4A C6A 110.4(12) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.496 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.123 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.001 0.000 0.219 1717 738 ' ' 2 0.499 0.500 0.081 1717 738 ' ' _platon_squeeze_details ; During the refinement of the structure, electron density peaks were located and were believed to be one disordered nitrate anion and several disordered water molecules We could locate the disordered nitrate counterion and at least six water molecule in a high R factor structure. All the attempts made to model the solvent molecules were not successful and they were removed using the SQUEEZE routine from Platon (Spek, 2003). ; _database_code_depnum_ccdc_archive 'CCDC 943448' ####################################################################### # # 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_Complex5 #CCDC 943449 _audit_creation_method SHELXL-97 _chemical_name_systematic Complex5 _chemical_name_common Complex5 _chemical_formula_moiety 'C78 H102 Cu3 K N6 O18, Br, 5(O) ' _chemical_formula_sum 'C78 H102 Br Cu3 K N6 O23' _chemical_compound_source synthesis _exptl_crystal_recrystallization_method 'Methanol Acetonitrile mixture' _chemical_melting_point ? _exptl_crystal_description diamond _exptl_crystal_colour blue _diffrn_ambient_temperature 296(2) _chemical_formula_weight 1801.29 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' K K 0.2009 0.2494 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_int_tables_number 20 _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.675(5) _cell_length_b 21.173(5) _cell_length_c 26.561(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9940(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6924 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.64 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3748 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6272 _exptl_absorpt_correction_T_max 0.8036 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 39404 _diffrn_reflns_av_R_equivalents 0.2025 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.43 _reflns_number_total 10757 _reflns_number_gt 6697 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^ > 2\s(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. Restrictions used DELU 0.010 0.010 C24 C26 C25 SIMU 0.040 0.080 1.700 C24 C26 C25 ; _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^)+(0.0680P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(14) _refine_ls_number_reflns 10757 _refine_ls_number_parameters 511 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cu2 Cu 0.91455(4) 0.07475(3) 0.397568(16) 0.03721(16) Uani 1 1 d . . . Cu1 Cu 0.60823(6) 0.0000 0.5000 0.0452(2) Uani 1 2 d S . . K1 K 0.81243(11) 0.0000 0.5000 0.0494(4) Uani 1 2 d S . . C28 C 0.6823(5) 0.1883(3) 0.5517(2) 0.0616(18) Uani 1 1 d . . . H1 H 0.7203 0.1984 0.5289 0.074 Uiso 1 1 calc R . . C27 C 0.6269(4) 0.1446(3) 0.5389(2) 0.0498(15) Uani 1 1 d . . . C31 C 0.5694(5) 0.1589(4) 0.6195(2) 0.067(2) Uani 1 1 d . . . H4 H 0.5321 0.1490 0.6429 0.080 Uiso 1 1 calc R . . C29 C 0.6806(6) 0.2167(4) 0.5989(3) 0.080(2) Uani 1 1 d . . . H2 H 0.7182 0.2452 0.6081 0.095 Uiso 1 1 calc R . . C30 C 0.6238(7) 0.2026(4) 0.6315(3) 0.081(3) Uani 1 1 d . . . H3 H 0.6218 0.2230 0.6625 0.097 Uiso 1 1 calc R . . C32 C 0.5695(4) 0.1290(3) 0.5725(2) 0.0535(16) Uani 1 1 d . . . C33 C 0.5087(4) 0.0850(4) 0.5583(2) 0.0604(17) Uani 1 1 d . . . H8A H 0.4890 0.0973 0.5257 0.072 Uiso 1 1 calc R . . H8B H 0.4679 0.0887 0.5825 0.072 Uiso 1 1 calc R . . C5 C 0.9824(6) -0.1104(4) 0.3141(2) 0.074(2) Uani 1 1 d . . . H11 H 1.0326 -0.1107 0.3034 0.089 Uiso 1 1 calc R . . C2 C 0.8311(6) -0.1104(4) 0.3461(2) 0.071(2) Uani 1 1 d . . . H9 H 0.7809 -0.1109 0.3567 0.085 Uiso 1 1 calc R . . C3 C 0.8710(7) -0.1664(4) 0.3374(3) 0.082(3) Uani 1 1 d . . . H10 H 0.8467 -0.2049 0.3422 0.098 Uiso 1 1 calc R . . C6 C 0.9447(5) -0.0529(3) 0.32216(16) 0.0545(18) Uani 1 1 d . . . C1 C 0.8700(5) -0.0533(3) 0.33815(17) 0.0537(18) Uani 1 1 d . . . C4 C 0.9449(9) -0.1661(5) 0.3221(3) 0.094(4) Uani 1 1 d . . . H14 H 0.9700 -0.2041 0.3171 0.113 Uiso 1 1 calc R . . O7 O 0.6252(3) 0.1150(2) 0.49331(13) 0.0592(12) Uani 1 1 d . . . N3 N 0.5333(3) 0.0176(3) 0.55584(17) 0.0546(13) Uani 1 1 d . . . H1A H 0.4915 -0.0065 0.5502 0.066 Uiso 1 1 calc R . . C34 C 0.5687(4) -0.0040(3) 0.60376(19) 0.0545(15) Uani 1 1 d . . . H15 H 0.5506 0.0230 0.6312 0.065 Uiso 1 1 calc R . . O1 O 0.8354(3) 0.0034(3) 0.34593(13) 0.0620(12) Uani 1 1 d . . . C7 C 0.9839(4) 0.0085(3) 0.31185(15) 0.0529(17) Uani 1 1 d . . . H16A H 0.9510 0.0347 0.2914 0.063 Uiso 1 1 calc R . . H16B H 1.0293 0.0002 0.2925 0.063 Uiso 1 1 calc R . . N1 N 1.0053(3) 0.0446(2) 0.35853(12) 0.0399(11) Uani 1 1 d . . . H2A H 1.0322 0.0792 0.3488 0.048 Uiso 1 1 calc R . . C9 C 1.0027(4) -0.0233(3) 0.43306(15) 0.0421(13) Uani 1 1 d . . . C8 C 1.0534(3) 0.0071(3) 0.39290(15) 0.0420(12) Uani 1 1 d . . . H17 H 1.0774 -0.0267 0.3734 0.050 Uiso 1 1 calc R . . C10 C 1.1163(4) 0.0471(3) 0.41736(19) 0.0521(15) Uani 1 1 d . . . H19A H 1.0929 0.0817 0.4354 0.063 Uiso 1 1 calc R . . H19B H 1.1426 0.0211 0.4419 0.063 Uiso 1 1 calc R . . O2 O 0.9370(2) -0.00011(19) 0.43872(9) 0.0399(8) Uani 1 1 d . . . O3 O 1.0296(3) -0.0673(2) 0.45769(12) 0.0536(11) Uani 1 1 d . . . O8 O 0.6821(2) 0.0055(2) 0.55518(11) 0.0464(9) Uani 1 1 d . . . O9 O 0.6914(3) 0.0041(3) 0.63849(13) 0.0666(13) Uani 1 1 d . . . C35 C 0.6546(4) 0.0030(3) 0.59961(19) 0.0523(14) Uani 1 1 d . . . C21 C 0.8163(4) 0.1735(3) 0.36596(16) 0.0435(13) Uani 1 1 d . . . H21 H 0.8107 0.2193 0.3703 0.052 Uiso 1 1 calc R . . C22 C 0.7823(4) 0.1405(3) 0.41252(16) 0.0446(14) Uani 1 1 d . . . O5 O 0.8195(2) 0.09547(17) 0.43154(10) 0.0423(9) Uani 1 1 d . . . O6 O 0.7204(3) 0.1591(2) 0.42715(14) 0.0598(12) Uani 1 1 d . . . N2 N 0.8985(3) 0.1586(2) 0.36290(11) 0.0412(11) Uani 1 1 d . . . H3A H 0.9110 0.1540 0.3299 0.049 Uiso 1 1 calc R . . C19 C 0.9247(4) 0.2262(3) 0.43829(16) 0.0434(13) Uani 1 1 d . . . C20 C 0.9460(4) 0.2095(3) 0.38454(15) 0.0437(13) Uani 1 1 d . . . H23A H 0.9412 0.2470 0.3637 0.052 Uiso 1 1 calc R . . H23B H 0.9985 0.1964 0.3837 0.052 Uiso 1 1 calc R . . C14 C 0.9439(4) 0.1851(3) 0.47800(17) 0.0453(14) Uani 1 1 d . . . C18 C 0.8887(4) 0.2814(3) 0.4496(2) 0.0534(16) Uani 1 1 d . . . H26 H 0.8769 0.3093 0.4237 0.064 Uiso 1 1 calc R . . O4 O 0.9794(3) 0.1311(2) 0.46557(11) 0.0482(11) Uani 1 1 d . . . C15 C 0.9226(5) 0.2007(3) 0.52682(16) 0.0550(17) Uani 1 1 d . . . H27 H 0.9336 0.1733 0.5532 0.066 Uiso 1 1 calc R . . C17 C 0.8692(5) 0.2971(3) 0.4987(3) 0.0658(18) Uani 1 1 d . . . H29 H 0.8453 0.3353 0.5054 0.079 Uiso 1 1 calc R . . C16 C 0.8848(5) 0.2575(4) 0.5362(2) 0.073(2) Uani 1 1 d . . . H28 H 0.8703 0.2676 0.5689 0.088 Uiso 1 1 calc R . . C11 C 1.1743(6) 0.0741(5) 0.3810(3) 0.084(2) Uani 1 1 d . . . H30 H 1.1483 0.1085 0.3633 0.101 Uiso 1 1 calc R . . C13 C 1.2369(7) 0.1068(6) 0.4135(4) 0.111(4) Uani 1 1 d . . . H31A H 1.2232 0.1047 0.4484 0.167 Uiso 1 1 calc R . . H31B H 1.2417 0.1502 0.4035 0.167 Uiso 1 1 calc R . . H31C H 1.2843 0.0855 0.4084 0.167 Uiso 1 1 calc R . . C12 C 1.2039(8) 0.0319(8) 0.3410(4) 0.142(6) Uani 1 1 d . . . H32A H 1.2217 -0.0067 0.3558 0.213 Uiso 1 1 calc R . . H32B H 1.2449 0.0524 0.3238 0.213 Uiso 1 1 calc R . . H32C H 1.1642 0.0226 0.3174 0.213 Uiso 1 1 calc R . . C36 C 0.5514(5) -0.0728(4) 0.6168(2) 0.073(2) Uani 1 1 d . . . H33A H 0.5620 -0.0991 0.5878 0.088 Uiso 1 1 calc R . . H33B H 0.5845 -0.0862 0.6439 0.088 Uiso 1 1 calc R . . C37 C 0.4692(8) -0.0829(6) 0.6329(4) 0.113(4) Uani 1 1 d . . . H34 H 0.4355 -0.0777 0.6038 0.135 Uiso 1 1 calc R . . C39 C 0.4709(14) -0.1592(7) 0.6508(6) 0.181(9) Uani 1 1 d . . . H35A H 0.4925 -0.1843 0.6244 0.271 Uiso 1 1 calc R . . H35B H 0.4203 -0.1732 0.6575 0.271 Uiso 1 1 calc R . . H35C H 0.5011 -0.1634 0.6807 0.271 Uiso 1 1 calc R . . C23 C 0.7733(5) 0.1536(4) 0.31774(19) 0.064(2) Uani 1 1 d . . . H36A H 0.8042 0.1230 0.3001 0.077 Uiso 1 1 calc R . . H36B H 0.7274 0.1321 0.3281 0.077 Uiso 1 1 calc R . . C38 C 0.4418(11) -0.0486(11) 0.6736(7) 0.211(10) Uani 1 1 d . . . H39A H 0.4748 -0.0543 0.7019 0.317 Uiso 1 1 calc R . . H39B H 0.3920 -0.0633 0.6821 0.317 Uiso 1 1 calc R . . H39C H 0.4397 -0.0047 0.6649 0.317 Uiso 1 1 calc R . . Br1 Br 0.0000 0.16128(6) 0.2500 0.1037(6) Uani 1 2 d S . . O11 O 0.2928(10) 0.0751(6) 0.5645(5) 0.224(7) Uani 1 1 d . . . O12 O 0.1622(10) 0.1394(17) 0.5592(6) 0.319(15) Uani 1 1 d . . . O10 O 0.3812(6) 0.0000 0.5000 0.127(4) Uani 1 2 d S . . C24 C 0.7545(18) 0.1972(10) 0.2858(7) 0.278(14) Uani 1 1 d U . . H24 H 0.8009 0.2076 0.2674 0.333 Uiso 1 1 calc R . . C26 C 0.7176(16) 0.2574(8) 0.2961(6) 0.198(10) Uani 1 1 d U . . H26A H 0.7150 0.2817 0.2656 0.297 Uiso 1 1 calc R . . H26B H 0.7462 0.2802 0.3209 0.297 Uiso 1 1 calc R . . H26C H 0.6674 0.2499 0.3085 0.297 Uiso 1 1 calc R . . C25 C 0.698(2) 0.1633(10) 0.2446(8) 0.347(19) Uani 1 1 d U . . H25A H 0.6847 0.1931 0.2190 0.521 Uiso 1 1 calc R . . H25B H 0.6532 0.1488 0.2613 0.521 Uiso 1 1 calc R . . H25C H 0.7237 0.1280 0.2296 0.521 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 Cu2 0.0470(4) 0.0366(3) 0.0281(2) 0.0051(2) 0.0046(2) 0.0018(3) Cu1 0.0383(6) 0.0484(6) 0.0490(4) 0.0030(4) 0.000 0.000 K1 0.0421(10) 0.0654(12) 0.0406(6) 0.0192(7) 0.000 0.000 C28 0.065(5) 0.042(4) 0.077(4) 0.006(3) 0.007(3) -0.006(3) C27 0.054(4) 0.037(3) 0.058(3) 0.005(2) 0.003(3) 0.004(3) C31 0.069(6) 0.057(4) 0.074(3) -0.001(3) 0.015(3) 0.011(4) C29 0.106(8) 0.048(4) 0.084(4) -0.002(3) -0.016(5) -0.014(4) C30 0.119(9) 0.057(5) 0.065(4) -0.008(3) 0.000(4) 0.015(5) C32 0.055(5) 0.038(3) 0.067(3) 0.009(2) 0.011(3) 0.010(3) C33 0.046(4) 0.057(4) 0.078(3) 0.009(3) 0.011(3) 0.012(4) C5 0.111(8) 0.054(5) 0.056(3) -0.014(3) 0.003(4) 0.007(5) C2 0.103(7) 0.053(5) 0.057(3) 0.001(3) -0.020(3) -0.021(4) C3 0.129(10) 0.049(5) 0.068(4) 0.003(3) -0.023(5) -0.016(5) C6 0.080(5) 0.058(4) 0.0255(19) -0.0017(19) -0.002(2) -0.001(3) C1 0.081(6) 0.044(3) 0.036(2) -0.0025(19) -0.017(3) 0.006(3) C4 0.158(12) 0.059(6) 0.064(4) -0.012(3) -0.012(5) 0.017(6) O7 0.065(3) 0.059(3) 0.0540(19) -0.0002(17) 0.0026(19) -0.006(2) N3 0.039(3) 0.052(3) 0.073(3) 0.009(2) 0.004(2) -0.003(3) C34 0.060(4) 0.053(3) 0.050(2) 0.006(3) 0.013(3) 0.005(3) O1 0.069(3) 0.055(3) 0.062(2) -0.0030(19) -0.0069(19) -0.005(3) C7 0.080(5) 0.052(4) 0.0262(19) 0.0007(19) 0.012(2) 0.006(3) N1 0.050(3) 0.038(3) 0.0320(16) 0.0050(15) 0.0051(17) -0.001(2) C9 0.056(4) 0.042(3) 0.0290(19) 0.0017(17) 0.007(2) 0.001(3) C8 0.050(3) 0.040(3) 0.0356(19) 0.005(2) 0.013(2) 0.005(3) C10 0.042(4) 0.061(4) 0.054(3) 0.006(2) 0.006(2) 0.004(3) O2 0.046(2) 0.043(2) 0.0314(13) 0.0069(13) 0.0065(13) 0.003(2) O3 0.064(3) 0.051(3) 0.0460(16) 0.0177(16) 0.0099(17) 0.009(2) O8 0.042(2) 0.051(2) 0.0456(16) 0.0030(16) 0.0078(15) 0.004(2) O9 0.069(3) 0.086(4) 0.0456(18) -0.0019(19) 0.0021(19) 0.004(3) C35 0.052(4) 0.055(4) 0.051(3) 0.007(3) 0.010(3) 0.009(3) C21 0.049(4) 0.042(3) 0.039(2) 0.0083(19) -0.006(2) 0.001(3) C22 0.055(4) 0.041(3) 0.038(2) 0.0022(18) 0.001(2) -0.001(3) O5 0.049(3) 0.038(2) 0.0390(15) 0.0070(13) 0.0065(15) 0.0038(18) O6 0.059(3) 0.058(3) 0.062(2) 0.0136(18) 0.015(2) 0.013(3) N2 0.064(4) 0.034(2) 0.0257(14) 0.0049(13) 0.0031(17) -0.001(2) C19 0.048(4) 0.036(3) 0.045(2) 0.0019(18) -0.001(2) -0.004(3) C20 0.055(4) 0.038(3) 0.038(2) 0.0038(18) 0.001(2) -0.003(3) C14 0.050(4) 0.046(3) 0.040(2) -0.007(2) -0.001(2) -0.004(3) C18 0.062(5) 0.035(3) 0.063(3) 0.000(2) -0.002(3) -0.001(3) O4 0.060(3) 0.050(3) 0.0349(15) -0.0014(14) -0.0033(15) 0.014(2) C15 0.067(5) 0.064(4) 0.035(2) -0.004(2) -0.001(2) -0.004(4) C17 0.077(5) 0.039(4) 0.081(4) -0.013(3) 0.013(4) 0.005(3) C16 0.088(6) 0.082(6) 0.050(3) -0.022(3) 0.009(3) 0.003(5) C11 0.074(6) 0.082(6) 0.097(5) 0.010(4) 0.015(4) -0.017(6) C13 0.062(7) 0.106(9) 0.165(9) 0.026(6) -0.010(6) -0.038(6) C12 0.094(10) 0.196(16) 0.137(8) -0.033(8) 0.064(8) -0.038(9) C36 0.088(6) 0.054(4) 0.078(4) 0.014(3) 0.024(4) -0.005(4) C37 0.115(10) 0.091(8) 0.133(7) 0.029(6) 0.028(7) -0.032(7) C39 0.26(2) 0.108(11) 0.177(10) -0.002(8) 0.081(13) -0.101(14) C23 0.076(6) 0.076(5) 0.041(2) 0.005(3) -0.022(3) -0.009(4) C38 0.154(16) 0.22(2) 0.259(17) 0.004(15) 0.155(16) -0.004(14) Br1 0.1658(16) 0.0657(8) 0.0797(6) 0.000 0.0760(8) 0.000 O11 0.245(16) 0.126(9) 0.301(14) -0.008(10) 0.153(13) -0.059(11) O12 0.129(13) 0.57(5) 0.253(14) 0.00(2) -0.015(11) -0.13(2) O10 0.064(7) 0.160(12) 0.158(7) -0.031(8) 0.000 0.000 C24 0.45(3) 0.187(16) 0.196(12) -0.090(11) -0.243(19) 0.159(18) C26 0.32(3) 0.094(9) 0.177(11) 0.010(7) -0.108(15) 0.060(13) C25 0.59(4) 0.210(18) 0.236(16) -0.097(15) -0.33(2) 0.15(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu2 O5 1.956(4) . ? Cu2 O2 1.966(4) . ? Cu2 N1 2.014(5) . ? Cu2 N2 2.019(4) . ? Cu1 O8 1.966(4) . ? Cu1 O8 1.966(4) 4_556 ? Cu1 N3 2.023(5) 4_556 ? Cu1 N3 2.023(5) . ? K1 O5 2.722(3) 4_556 ? K1 O5 2.722(3) . ? K1 O8 2.733(4) 4_556 ? K1 O8 2.733(4) . ? K1 O2 2.737(4) 4_556 ? K1 O2 2.737(4) . ? K1 Cu2 3.6283(12) 4_556 ? C28 C29 1.389(11) . ? C28 C27 1.389(10) . ? C28 H1 0.9300 . ? C27 O7 1.364(7) . ? C27 C32 1.391(9) . ? C31 C30 1.372(14) . ? C31 C32 1.401(9) . ? C31 H4 0.9300 . ? C29 C30 1.360(14) . ? C29 H2 0.9300 . ? C30 H3 0.9300 . ? C32 C33 1.471(11) . ? C33 N3 1.493(9) . ? C33 H8A 0.9700 . ? C33 H8B 0.9700 . ? C5 C4 1.370(14) . ? C5 C6 1.405(10) . ? C5 H11 0.9300 . ? C2 C3 1.399(13) . ? C2 C1 1.408(10) . ? C2 H9 0.9300 . ? C3 C4 1.367(16) . ? C3 H10 0.9300 . ? C6 C1 1.387(11) . ? C6 C7 1.497(9) . ? C1 O1 1.364(8) . ? C4 H14 0.9300 . ? N3 C34 1.490(8) . ? N3 H1A 0.9100 . ? C34 C36 1.530(10) . ? C34 C35 1.530(10) . ? C34 H15 0.9800 . ? C7 N1 1.505(7) . ? C7 H16A 0.9700 . ? C7 H16B 0.9700 . ? N1 C8 1.479(7) . ? N1 H2A 0.9100 . ? C9 O3 1.233(7) . ? C9 O2 1.271(7) . ? C9 C8 1.535(7) . ? C8 C10 1.540(9) . ? C8 H17 0.9800 . ? C10 C11 1.520(10) . ? C10 H19A 0.9700 . ? C10 H19B 0.9700 . ? O8 C35 1.277(6) . ? O9 C35 1.221(7) . ? C21 N2 1.488(8) . ? C21 C22 1.543(7) . ? C21 C23 1.548(7) . ? C21 H21 0.9800 . ? C22 O6 1.226(8) . ? C22 O5 1.264(7) . ? N2 C20 1.483(8) . ? N2 H3A 0.9100 . ? C19 C18 1.364(9) . ? C19 C14 1.408(8) . ? C19 C20 1.518(7) . ? C20 H23A 0.9700 . ? C20 H23B 0.9700 . ? C14 O4 1.345(7) . ? C14 C15 1.389(7) . ? C18 C17 1.391(9) . ? C18 H26 0.9300 . ? C15 C16 1.399(11) . ? C15 H27 0.9300 . ? C17 C16 1.330(11) . ? C17 H29 0.9300 . ? C16 H28 0.9300 . ? C11 C12 1.485(16) . ? C11 C13 1.564(14) . ? C11 H30 0.9800 . ? C13 H31A 0.9600 . ? C13 H31B 0.9600 . ? C13 H31C 0.9600 . ? C12 H32A 0.9600 . ? C12 H32B 0.9600 . ? C12 H32C 0.9600 . ? C36 C37 1.529(16) . ? C36 H33A 0.9700 . ? C36 H33B 0.9700 . ? C37 C38 1.39(2) . ? C37 C39 1.684(19) . ? C37 H34 0.9800 . ? C39 H35A 0.9600 . ? C39 H35B 0.9600 . ? C39 H35C 0.9600 . ? C23 C24 1.296(19) . ? C23 H36A 0.9700 . ? C23 H36B 0.9700 . ? C38 H39A 0.9600 . ? C38 H39B 0.9600 . ? C38 H39C 0.9600 . ? C24 C26 1.46(2) . ? C24 C25 1.65(3) . ? C24 H24 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 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 O5 Cu2 O2 95.59(14) . . ? O5 Cu2 N1 172.92(18) . . ? O2 Cu2 N1 82.53(15) . . ? O5 Cu2 N2 83.82(17) . . ? O2 Cu2 N2 172.11(16) . . ? N1 Cu2 N2 98.98(18) . . ? O8 Cu1 O8 96.8(2) . 4_556 ? O8 Cu1 N3 172.8(2) . 4_556 ? O8 Cu1 N3 82.97(19) 4_556 4_556 ? O8 Cu1 N3 82.97(19) . . ? O8 Cu1 N3 172.8(2) 4_556 . ? N3 Cu1 N3 98.2(3) 4_556 . ? O5 K1 O5 174.7(2) 4_556 . ? O5 K1 O8 111.44(13) 4_556 4_556 ? O5 K1 O8 73.28(12) . 4_556 ? O5 K1 O8 73.28(12) 4_556 . ? O5 K1 O8 111.44(13) . . ? O8 K1 O8 65.09(16) 4_556 . ? O5 K1 O2 64.30(12) 4_556 4_556 ? O5 K1 O2 111.07(13) . 4_556 ? O8 K1 O2 175.32(11) 4_556 4_556 ? O8 K1 O2 111.03(10) . 4_556 ? O5 K1 O2 111.07(13) 4_556 . ? O5 K1 O2 64.30(12) . . ? O8 K1 O2 111.03(10) 4_556 . ? O8 K1 O2 175.32(11) . . ? O2 K1 O2 72.97(14) 4_556 . ? O5 K1 Cu2 32.02(9) 4_556 4_556 ? O5 K1 Cu2 143.32(11) . 4_556 ? O8 K1 Cu2 143.41(9) 4_556 4_556 ? O8 K1 Cu2 92.05(8) . 4_556 ? O2 K1 Cu2 32.28(8) 4_556 4_556 ? O2 K1 Cu2 92.61(8) . 4_556 ? C29 C28 C27 119.6(7) . . ? C29 C28 H1 120.2 . . ? C27 C28 H1 120.2 . . ? O7 C27 C28 122.6(6) . . ? O7 C27 C32 116.4(6) . . ? C28 C27 C32 121.0(6) . . ? C30 C31 C32 120.8(7) . . ? C30 C31 H4 119.6 . . ? C32 C31 H4 119.6 . . ? C30 C29 C28 119.7(9) . . ? C30 C29 H2 120.1 . . ? C28 C29 H2 120.1 . . ? C29 C30 C31 121.1(7) . . ? C29 C30 H3 119.4 . . ? C31 C30 H3 119.4 . . ? C27 C32 C31 117.7(7) . . ? C27 C32 C33 121.2(5) . . ? C31 C32 C33 121.0(7) . . ? C32 C33 N3 113.9(6) . . ? C32 C33 H8A 108.8 . . ? N3 C33 H8A 108.8 . . ? C32 C33 H8B 108.8 . . ? N3 C33 H8B 108.8 . . ? H8A C33 H8B 107.7 . . ? C4 C5 C6 119.5(10) . . ? C4 C5 H11 120.2 . . ? C6 C5 H11 120.2 . . ? C3 C2 C1 117.2(9) . . ? C3 C2 H9 121.4 . . ? C1 C2 H9 121.4 . . ? C4 C3 C2 121.7(9) . . ? C4 C3 H10 119.1 . . ? C2 C3 H10 119.1 . . ? C1 C6 C5 119.5(7) . . ? C1 C6 C7 120.1(6) . . ? C5 C6 C7 120.3(7) . . ? O1 C1 C6 117.9(6) . . ? O1 C1 C2 121.0(8) . . ? C6 C1 C2 121.2(7) . . ? C3 C4 C5 120.9(10) . . ? C3 C4 H14 119.5 . . ? C5 C4 H14 119.5 . . ? C34 N3 C33 112.2(5) . . ? C34 N3 Cu1 107.1(4) . . ? C33 N3 Cu1 113.5(4) . . ? C34 N3 H1A 107.9 . . ? C33 N3 H1A 107.9 . . ? Cu1 N3 H1A 107.9 . . ? N3 C34 C36 113.7(6) . . ? N3 C34 C35 109.0(4) . . ? C36 C34 C35 107.9(6) . . ? N3 C34 H15 108.7 . . ? C36 C34 H15 108.7 . . ? C35 C34 H15 108.7 . . ? C6 C7 N1 114.0(4) . . ? C6 C7 H16A 108.8 . . ? N1 C7 H16A 108.8 . . ? C6 C7 H16B 108.8 . . ? N1 C7 H16B 108.8 . . ? H16A C7 H16B 107.7 . . ? C8 N1 C7 112.4(4) . . ? C8 N1 Cu2 108.1(3) . . ? C7 N1 Cu2 112.6(4) . . ? C8 N1 H2A 107.9 . . ? C7 N1 H2A 107.9 . . ? Cu2 N1 H2A 107.9 . . ? O3 C9 O2 125.6(5) . . ? O3 C9 C8 117.4(6) . . ? O2 C9 C8 117.0(5) . . ? N1 C8 C9 108.5(5) . . ? N1 C8 C10 112.3(5) . . ? C9 C8 C10 111.0(4) . . ? N1 C8 H17 108.3 . . ? C9 C8 H17 108.3 . . ? C10 C8 H17 108.3 . . ? C11 C10 C8 115.2(5) . . ? C11 C10 H19A 108.5 . . ? C8 C10 H19A 108.5 . . ? C11 C10 H19B 108.5 . . ? C8 C10 H19B 108.5 . . ? H19A C10 H19B 107.5 . . ? C9 O2 Cu2 115.5(3) . . ? C9 O2 K1 143.7(3) . . ? Cu2 O2 K1 99.67(15) . . ? C35 O8 Cu1 115.7(4) . . ? C35 O8 K1 144.5(4) . . ? Cu1 O8 K1 99.06(12) . . ? O9 C35 O8 125.4(6) . . ? O9 C35 C34 118.0(5) . . ? O8 C35 C34 116.6(5) . . ? N2 C21 C22 109.1(4) . . ? N2 C21 C23 112.1(5) . . ? C22 C21 C23 110.3(5) . . ? N2 C21 H21 108.4 . . ? C22 C21 H21 108.4 . . ? C23 C21 H21 108.4 . . ? O6 C22 O5 125.5(5) . . ? O6 C22 C21 117.1(5) . . ? O5 C22 C21 117.3(6) . . ? C22 O5 Cu2 115.6(3) . . ? C22 O5 K1 143.4(4) . . ? Cu2 O5 K1 100.44(15) . . ? C20 N2 C21 112.1(4) . . ? C20 N2 Cu2 112.5(3) . . ? C21 N2 Cu2 107.4(3) . . ? C20 N2 H3A 108.2 . . ? C21 N2 H3A 108.2 . . ? Cu2 N2 H3A 108.2 . . ? C18 C19 C14 118.4(5) . . ? C18 C19 C20 121.4(5) . . ? C14 C19 C20 120.1(5) . . ? N2 C20 C19 113.1(5) . . ? N2 C20 H23A 109.0 . . ? C19 C20 H23A 109.0 . . ? N2 C20 H23B 109.0 . . ? C19 C20 H23B 109.0 . . ? H23A C20 H23B 107.8 . . ? O4 C14 C15 123.8(5) . . ? O4 C14 C19 116.9(4) . . ? C15 C14 C19 119.2(6) . . ? C19 C18 C17 121.8(5) . . ? C19 C18 H26 119.1 . . ? C17 C18 H26 119.1 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H27 120.0 . . ? C16 C15 H27 120.0 . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H29 120.0 . . ? C18 C17 H29 120.0 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H28 119.7 . . ? C15 C16 H28 119.7 . . ? C12 C11 C10 117.7(9) . . ? C12 C11 C13 114.3(10) . . ? C10 C11 C13 107.1(7) . . ? C12 C11 H30 105.6 . . ? C10 C11 H30 105.6 . . ? C13 C11 H30 105.6 . . ? C11 C13 H31A 109.5 . . ? C11 C13 H31B 109.5 . . ? H31A C13 H31B 109.5 . . ? C11 C13 H31C 109.5 . . ? H31A C13 H31C 109.5 . . ? H31B C13 H31C 109.5 . . ? C11 C12 H32A 109.5 . . ? C11 C12 H32B 109.5 . . ? H32A C12 H32B 109.5 . . ? C11 C12 H32C 109.5 . . ? H32A C12 H32C 109.5 . . ? H32B C12 H32C 109.5 . . ? C37 C36 C34 112.7(8) . . ? C37 C36 H33A 109.0 . . ? C34 C36 H33A 109.0 . . ? C37 C36 H33B 109.0 . . ? C34 C36 H33B 109.0 . . ? H33A C36 H33B 107.8 . . ? C38 C37 C36 118.3(13) . . ? C38 C37 C39 106.7(11) . . ? C36 C37 C39 101.2(12) . . ? C38 C37 H34 110.0 . . ? C36 C37 H34 110.0 . . ? C39 C37 H34 110.0 . . ? C37 C39 H35A 109.5 . . ? C37 C39 H35B 109.5 . . ? H35A C39 H35B 109.5 . . ? C37 C39 H35C 109.5 . . ? H35A C39 H35C 109.5 . . ? H35B C39 H35C 109.5 . . ? C24 C23 C21 118.2(10) . . ? C24 C23 H36A 107.8 . . ? C21 C23 H36A 107.8 . . ? C24 C23 H36B 107.8 . . ? C21 C23 H36B 107.8 . . ? H36A C23 H36B 107.1 . . ? C37 C38 H39A 109.5 . . ? C37 C38 H39B 109.5 . . ? H39A C38 H39B 109.5 . . ? C37 C38 H39C 109.5 . . ? H39A C38 H39C 109.5 . . ? H39B C38 H39C 109.5 . . ? C23 C24 C26 128.0(17) . . ? C23 C24 C25 106.2(18) . . ? C26 C24 C25 103.7(16) . . ? C23 C24 H24 105.8 . . ? C26 C24 H24 105.8 . . ? C25 C24 H24 105.8 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.258 _refine_diff_density_min -2.075 _refine_diff_density_rms 0.205 _database_code_depnum_ccdc_archive 'CCDC 943449' ####################################################################### # # 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_Complex6 #CCDC 943450 _audit_creation_method SHELXL-97 _chemical_name_systematic Complex6 _chemical_name_common Complex6 _chemical_formula_moiety ' C78 H96 Cu3 K N6 O18, 2(C O), I, 7(O)' _chemical_formula_sum 'C80 H96 Cu3 I K N6 O27' _chemical_compound_source syn _exptl_crystal_recrystallization_method methanol _chemical_melting_point ? _exptl_crystal_description diamond _exptl_crystal_colour blue _diffrn_ambient_temperature 296(2) _chemical_formula_weight 1930.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_int_tables_number 20 _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'C 2c 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.5555(12) _cell_length_b 20.9943(13) _cell_length_c 27.1327(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10569.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6665 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.60 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3972 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6630 _exptl_absorpt_correction_T_max 0.7890 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 54624 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.32 _reflns_number_total 9577 _reflns_number_gt 5647 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^ > 2\s(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. Restrains used DFIX 1.500 0.020 C34 C40 DFIX 1.500 0.020 C33 C34 DELU 0.010 0.010 C34 C40 C33 C28 C30 C29 C37 C38 C39 DFIX 1.500 0.020 C39 C37 DFIX 1.400 0.020 O21 C01 ; _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^)+(0.2000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(4) _refine_ls_number_reflns 9577 _refine_ls_number_parameters 537 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.3224 _refine_ls_wR_factor_gt 0.3032 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.006 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 C34 C 0.732(3) 0.3226(9) 0.7114(12) 0.31(3) Uani 1 1 d DU . . H34 H 0.6893 0.3188 0.6908 0.376 Uiso 1 1 calc R . . C40 C 0.698(3) 0.3563(15) 0.7543(13) 0.29(3) Uani 1 1 d DU . . H40A H 0.6782 0.3254 0.7765 0.442 Uiso 1 1 calc R . . H40B H 0.6605 0.3837 0.7425 0.442 Uiso 1 1 calc R . . H40C H 0.7338 0.3812 0.7712 0.442 Uiso 1 1 calc R . . C33 C 0.7405(16) 0.2538(11) 0.7238(8) 0.167(12) Uani 1 1 d DU . . H33A H 0.7100 0.2435 0.7513 0.251 Uiso 1 1 calc R . . H33B H 0.7897 0.2450 0.7321 0.251 Uiso 1 1 calc R . . H33C H 0.7267 0.2284 0.6958 0.251 Uiso 1 1 calc R . . O20 O 0.278(5) 0.565(3) 0.591(2) 0.80(10) Uani 1 1 d . . . O21 O 0.151(2) 0.664(2) 0.5583(17) 0.42(3) Uani 1 1 d D . . C01 C 0.100(2) 0.713(3) 0.566(2) 0.69(13) Uani 1 1 d D . . Cu1 Cu 0.89673(9) 0.42977(7) 0.60310(5) 0.0627(5) Uani 1 1 d . . . Cu2 Cu 0.60590(12) 0.5000 0.5000 0.0704(6) Uani 1 2 d S . . K1 K 0.8020(2) 0.5000 0.5000 0.0608(9) Uani 1 2 d S . . C2 C 0.8540(11) 0.5621(9) 0.6597(5) 0.085(5) Uani 1 1 d . . . C5 C 0.9237(15) 0.6740(10) 0.6785(10) 0.135(9) Uani 1 1 d . . . H5 H 0.9474 0.7118 0.6862 0.162 Uiso 1 1 calc R . . C1 C 0.8198(13) 0.6227(9) 0.6496(6) 0.107(7) Uani 1 1 d . . . H1 H 0.7730 0.6242 0.6374 0.129 Uiso 1 1 calc R . . C3 C 0.926(2) 0.5641(8) 0.6750(7) 0.151(12) Uani 1 1 d . . . C6 C 0.8552(17) 0.6751(9) 0.6580(6) 0.122(9) Uani 1 1 d . . . H6 H 0.8342 0.7140 0.6500 0.146 Uiso 1 1 calc R . . C4 C 0.9543(12) 0.6193(8) 0.6869(7) 0.105(6) Uani 1 1 d . . . H4 H 0.9991 0.6192 0.7023 0.126 Uiso 1 1 calc R . . C12 C 0.9110(6) 0.2753(6) 0.5631(4) 0.055(3) Uani 1 1 d . . . C7 C 0.9231(9) 0.3181(8) 0.5247(5) 0.080(4) Uani 1 1 d . . . C8 C 0.9084(7) 0.3019(7) 0.4741(4) 0.068(4) Uani 1 1 d . . . H8 H 0.9238 0.3270 0.4479 0.082 Uiso 1 1 calc R . . C9 C 0.8668(10) 0.2422(8) 0.4667(8) 0.099(5) Uani 1 1 d . . . H9 H 0.8508 0.2312 0.4354 0.119 Uiso 1 1 calc R . . C11 C 0.8730(10) 0.2198(8) 0.5527(6) 0.094(5) Uani 1 1 d . . . H11 H 0.8613 0.1927 0.5786 0.113 Uiso 1 1 calc R . . C10 C 0.8520(8) 0.2030(8) 0.5062(5) 0.079(4) Uani 1 1 d . . . H10 H 0.8275 0.1649 0.5012 0.095 Uiso 1 1 calc R . . O1 O 0.9563(5) 0.3737(4) 0.5343(3) 0.066(2) Uani 1 1 d . . . C13 C 0.9268(9) 0.2962(7) 0.6142(4) 0.074(4) Uani 1 1 d . . . H13A H 0.9244 0.2588 0.6351 0.089 Uiso 1 1 calc R . . H13B H 0.9764 0.3108 0.6147 0.089 Uiso 1 1 calc R . . N1 N 0.8835(7) 0.3450(5) 0.6371(4) 0.079(4) Uani 1 1 d . . . H1A H 0.8980 0.3492 0.6690 0.095 Uiso 1 1 calc R . . C14 C 0.8015(11) 0.3301(7) 0.6369(5) 0.097(6) Uani 1 1 d . . . H14 H 0.7946 0.2839 0.6353 0.117 Uiso 1 1 calc R . . C15 C 0.7714(9) 0.3608(8) 0.5892(5) 0.074(4) Uani 1 1 d . . . O3 O 0.8086(4) 0.4049(4) 0.5697(3) 0.0523(19) Uani 1 1 d . . . O2 O 0.7134(5) 0.3413(5) 0.5800(4) 0.079(3) Uani 1 1 d . . . O4 O 0.8161(6) 0.5051(5) 0.6514(3) 0.079(3) Uani 1 1 d . . . C16 C 0.9555(10) 0.4998(7) 0.6868(5) 0.085(4) Uani 1 1 d . . . H16A H 0.9191 0.4756 0.7043 0.101 Uiso 1 1 calc R . . H16B H 0.9963 0.5050 0.7088 0.101 Uiso 1 1 calc R . . N2 N 0.9796(7) 0.4617(5) 0.6427(4) 0.075(3) Uani 1 1 d . . . H2 H 1.0051 0.4275 0.6537 0.090 Uiso 1 1 calc R . . C18 C 0.6766(8) 0.6960(8) 0.5446(7) 0.082(4) Uani 1 1 d . . . H18 H 0.7176 0.7016 0.5253 0.098 Uiso 1 1 calc R . . C17 C 0.6265(8) 0.6484(7) 0.5269(7) 0.082(5) Uani 1 1 d . . . C19 C 0.6733(18) 0.2706(11) 0.4197(15) 0.198(17) Uani 1 1 d . . . H19 H 0.7050 0.2367 0.4155 0.238 Uiso 1 1 calc R . . C20 C 0.5678(8) 0.3617(6) 0.4372(7) 0.083(5) Uani 1 1 d . . . C21 C 0.5632(11) 0.3277(8) 0.3914(8) 0.116(7) Uani 1 1 d . . . H21 H 0.5271 0.3329 0.3680 0.139 Uiso 1 1 calc R . . C22 C 0.6243(9) 0.2831(9) 0.3869(13) 0.138(11) Uani 1 1 d . . . H22 H 0.6281 0.2614 0.3572 0.166 Uiso 1 1 calc R . . O5 O 0.6768(4) 0.4914(5) 0.4459(3) 0.070(2) Uani 1 1 d . . . N3 N 0.5363(6) 0.4771(6) 0.4464(5) 0.081(3) Uani 1 1 d . . . H3 H 0.4963 0.5015 0.4508 0.097 Uiso 1 1 calc R . . C24 C 0.6482(6) 0.4904(5) 0.4021(5) 0.055(3) Uani 1 1 d . . . C23 C 0.5685(10) 0.4950(11) 0.3963(8) 0.117(7) Uani 1 1 d . . . H23 H 0.5516 0.4657 0.3707 0.141 Uiso 1 1 calc R . . O6 O 0.6804(7) 0.4878(6) 0.3649(5) 0.102(4) Uani 1 1 d . . . O7 O 0.6279(5) 0.6152(5) 0.4878(4) 0.077(3) Uani 1 1 d . . . O8 O 0.9181(5) 0.5046(4) 0.5621(3) 0.063(2) Uani 1 1 d . . . C25 C 1.0286(8) 0.5005(7) 0.6074(6) 0.085(5) Uani 1 1 d . . . H25 H 1.0502 0.5355 0.6262 0.102 Uiso 1 1 calc R . . C26 C 0.9784(7) 0.5295(6) 0.5679(5) 0.060(3) Uani 1 1 d . . . I1 I 0.5000 0.16521(8) 0.2500 0.1063(7) Uani 1 2 d S . . C27 C 0.5451(9) 0.5670(8) 0.3837(6) 0.085(4) Uani 1 1 d . . . H27A H 0.5639 0.5949 0.4091 0.102 Uiso 1 1 calc R . . H27B H 0.5674 0.5793 0.3528 0.102 Uiso 1 1 calc R . . C28 C 0.466(3) 0.5773(14) 0.380(3) 0.40(4) Uani 1 1 d U . . H28 H 0.4363 0.5684 0.4088 0.475 Uiso 1 1 calc R . . O9 O 1.0053(6) 0.5706(5) 0.5419(4) 0.082(3) Uani 1 1 d . . . C30 C 0.447(3) 0.5454(16) 0.336(2) 0.36(4) Uani 1 1 d U . . H30A H 0.4536 0.5003 0.3401 0.542 Uiso 1 1 calc R . . H30B H 0.4783 0.5597 0.3095 0.542 Uiso 1 1 calc R . . H30C H 0.3982 0.5543 0.3273 0.542 Uiso 1 1 calc R . . C29 C 0.457(4) 0.6447(16) 0.3548(16) 0.39(4) Uani 1 1 d U . . H29A H 0.4623 0.6773 0.3794 0.592 Uiso 1 1 calc R . . H29B H 0.4099 0.6479 0.3402 0.592 Uiso 1 1 calc R . . H29C H 0.4930 0.6500 0.3299 0.592 Uiso 1 1 calc R . . C31 C 0.7702(17) 0.3538(9) 0.6815(6) 0.144(11) Uani 1 1 d . . . H31A H 0.8099 0.3708 0.7007 0.173 Uiso 1 1 calc R . . H31B H 0.7410 0.3901 0.6719 0.173 Uiso 1 1 calc R . . C35 C 1.0877(9) 0.4603(8) 0.5877(11) 0.134(10) Uani 1 1 d . . . H35A H 1.0653 0.4253 0.5701 0.161 Uiso 1 1 calc R . . H35B H 1.1131 0.4857 0.5633 0.161 Uiso 1 1 calc R . . C36 C 0.5121(9) 0.4069(7) 0.4481(8) 0.105(6) Uani 1 1 d . . . H36A H 0.4932 0.3979 0.4807 0.126 Uiso 1 1 calc R . . H36B H 0.4731 0.4010 0.4248 0.126 Uiso 1 1 calc R . . C37 C 1.1428(15) 0.4324(13) 0.6205(15) 0.24(2) Uani 1 1 d DU . . H37 H 1.1175 0.3985 0.6383 0.287 Uiso 1 1 calc R . . C38 C 1.2009(18) 0.4025(12) 0.5990(16) 0.220(17) Uani 1 1 d U . . C39 C 1.1693(13) 0.4779(14) 0.6607(11) 0.178(12) Uani 1 1 d DU . . H39A H 1.1307 0.5057 0.6703 0.268 Uiso 1 1 calc R . . H39B H 1.2088 0.5027 0.6483 0.268 Uiso 1 1 calc R . . H39C H 1.1850 0.4537 0.6888 0.268 Uiso 1 1 calc R . . O16 O 0.3852(12) 0.5000 0.5000 0.232(18) Uani 1 2 d S . . O18 O 0.8469(14) 0.1098(11) 0.7325(6) 0.216(12) Uani 1 1 d . . . O19 O 0.901(3) 0.1218(14) 0.6638(12) 0.32(2) 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 C34 0.56(7) 0.082(12) 0.30(4) -0.043(15) 0.36(5) -0.06(2) C40 0.45(6) 0.19(2) 0.24(3) -0.14(3) 0.27(4) -0.15(3) C33 0.21(3) 0.174(16) 0.118(17) 0.065(15) 0.106(18) 0.02(2) O20 1.4(2) 0.53(8) 0.46(8) 0.32(7) -0.55(12) -0.74(12) O21 0.31(4) 0.51(6) 0.43(6) 0.18(5) -0.08(4) -0.37(5) C01 0.29(6) 1.3(3) 0.47(10) -0.63(15) 0.30(7) -0.54(12) Cu1 0.0846(11) 0.0555(8) 0.0480(7) 0.0014(6) -0.0188(7) 0.0051(8) Cu2 0.0498(11) 0.0664(13) 0.0949(16) 0.0096(12) 0.000 0.000 K1 0.055(2) 0.075(2) 0.0525(19) 0.0088(18) 0.000 0.000 C2 0.111(13) 0.103(14) 0.043(7) -0.005(7) -0.006(7) 0.013(11) C5 0.17(2) 0.072(13) 0.16(2) 0.007(13) -0.064(19) -0.007(13) C1 0.169(19) 0.088(13) 0.065(9) 0.020(9) 0.035(11) 0.059(13) C3 0.33(4) 0.055(10) 0.068(10) -0.002(8) -0.034(17) -0.016(16) C6 0.25(3) 0.058(11) 0.057(9) -0.010(7) 0.020(12) 0.017(14) C4 0.147(17) 0.072(11) 0.095(12) -0.032(9) -0.017(12) 0.002(11) C12 0.060(8) 0.049(6) 0.056(6) 0.003(5) -0.019(5) -0.012(5) C7 0.100(11) 0.086(11) 0.054(7) -0.010(7) -0.020(7) -0.004(8) C8 0.059(8) 0.093(10) 0.053(6) 0.008(6) 0.008(6) 0.016(7) C9 0.117(14) 0.067(10) 0.113(14) -0.015(9) -0.030(11) 0.002(9) C11 0.139(15) 0.079(10) 0.064(8) 0.013(7) -0.002(9) 0.024(10) C10 0.079(9) 0.100(11) 0.060(8) -0.013(8) 0.000(7) 0.018(8) O1 0.082(6) 0.064(5) 0.052(5) -0.017(4) 0.005(4) -0.002(5) C13 0.106(11) 0.064(8) 0.051(7) -0.012(6) -0.035(7) 0.007(7) N1 0.099(10) 0.060(7) 0.077(7) 0.000(6) -0.042(7) 0.024(7) C14 0.176(18) 0.059(8) 0.057(7) 0.022(6) -0.012(9) 0.068(11) C15 0.071(10) 0.080(10) 0.069(8) -0.009(7) -0.015(7) 0.032(8) O3 0.048(5) 0.056(5) 0.053(4) 0.015(4) 0.000(3) 0.007(4) O2 0.063(6) 0.081(6) 0.094(6) 0.030(5) -0.016(5) -0.005(5) O4 0.105(8) 0.074(6) 0.058(5) 0.001(5) -0.017(5) 0.002(6) C16 0.122(12) 0.078(9) 0.054(7) -0.001(7) -0.033(8) 0.027(9) N2 0.116(10) 0.048(6) 0.062(6) 0.007(5) -0.039(6) -0.008(6) C18 0.065(9) 0.068(10) 0.113(12) 0.024(9) 0.004(9) -0.009(8) C17 0.055(9) 0.063(9) 0.128(14) 0.023(9) -0.031(9) 0.013(7) C19 0.20(3) 0.069(13) 0.33(4) -0.056(19) -0.14(3) -0.028(16) C20 0.047(8) 0.048(8) 0.156(16) -0.002(9) 0.009(9) -0.013(7) C21 0.128(15) 0.069(10) 0.150(17) 0.010(12) -0.070(14) -0.036(11) C22 0.057(10) 0.075(12) 0.28(3) -0.064(16) 0.018(15) -0.015(9) O5 0.062(5) 0.104(7) 0.043(4) 0.012(4) -0.012(4) -0.025(5) N3 0.067(7) 0.082(8) 0.093(8) 0.021(7) -0.004(6) -0.009(6) C24 0.057(7) 0.042(6) 0.066(7) 0.007(6) -0.003(6) 0.002(5) C23 0.100(12) 0.137(16) 0.114(13) 0.057(13) -0.015(11) 0.042(12) O6 0.102(8) 0.114(9) 0.089(8) 0.001(7) -0.006(7) -0.012(7) O7 0.084(7) 0.058(5) 0.090(7) -0.008(5) -0.006(5) 0.005(5) O8 0.070(5) 0.046(4) 0.074(5) 0.019(4) -0.015(4) -0.005(4) C25 0.106(11) 0.058(7) 0.091(10) 0.004(8) -0.056(9) 0.003(8) C26 0.056(8) 0.056(7) 0.069(7) 0.017(6) -0.030(6) 0.005(6) I1 0.1552(16) 0.0902(11) 0.0736(9) 0.000 0.0623(10) 0.000 C27 0.080(10) 0.087(10) 0.088(10) -0.018(8) -0.029(8) -0.006(9) C28 0.33(6) 0.066(15) 0.79(10) -0.08(3) -0.31(7) 0.04(2) O9 0.084(6) 0.081(6) 0.080(6) 0.019(5) -0.018(5) -0.010(6) C30 0.37(6) 0.11(2) 0.61(9) 0.05(3) -0.31(7) 0.08(3) C29 0.74(12) 0.17(2) 0.27(4) -0.12(3) -0.13(6) 0.28(5) C31 0.30(3) 0.081(11) 0.049(9) -0.013(8) 0.042(13) -0.045(15) C35 0.074(11) 0.061(9) 0.27(3) -0.046(14) -0.065(15) 0.006(8) C36 0.070(10) 0.066(9) 0.179(18) 0.009(10) -0.062(12) -0.015(8) C37 0.139(17) 0.119(18) 0.46(6) -0.08(3) -0.19(3) 0.053(17) C38 0.20(2) 0.110(17) 0.35(4) -0.07(2) -0.18(3) 0.087(19) C39 0.096(15) 0.20(3) 0.24(3) -0.03(2) -0.076(19) 0.005(16) O16 0.077(13) 0.22(3) 0.39(6) -0.06(4) 0.000 0.000 O18 0.29(3) 0.22(2) 0.131(13) 0.084(13) 0.119(16) 0.15(2) O19 0.53(7) 0.17(2) 0.27(3) 0.04(2) 0.05(4) 0.10(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C34 C31 1.25(3) . ? C34 C33 1.491(18) . ? C34 C40 1.504(17) . ? C34 H34 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O21 C01 1.40(2) . ? Cu1 O3 1.942(8) . ? Cu1 O8 1.964(8) . ? Cu1 N2 1.992(11) . ? Cu1 N1 2.019(11) . ? Cu1 K1 3.618(2) . ? Cu2 O5 1.979(9) . ? Cu2 O5 1.979(9) 4_566 ? Cu2 N3 2.003(12) . ? Cu2 N3 2.003(12) 4_566 ? Cu2 K1 3.639(4) . ? K1 O8 2.737(9) . ? K1 O8 2.737(9) 4_566 ? K1 O3 2.752(7) . ? K1 O3 2.752(7) 4_566 ? K1 O5 2.754(8) 4_566 ? K1 O5 2.754(8) . ? K1 Cu1 3.618(2) 4_566 ? C2 C3 1.39(4) . ? C2 O4 1.41(2) . ? C2 C1 1.45(2) . ? C5 C4 1.30(3) . ? C5 C6 1.39(3) . ? C5 H5 0.9300 . ? C1 C6 1.30(3) . ? C1 H1 0.9300 . ? C3 C4 1.32(3) . ? C3 C16 1.49(3) . ? C6 H6 0.9300 . ? C4 H4 0.9300 . ? C12 C11 1.39(2) . ? C12 C7 1.393(19) . ? C12 C13 1.483(16) . ? C7 O1 1.345(18) . ? C7 C8 1.441(17) . ? C8 C9 1.48(2) . ? C8 H8 0.9300 . ? C9 C10 1.38(2) . ? C9 H9 0.9300 . ? C11 C10 1.37(2) . ? C11 H11 0.9300 . ? C10 H10 0.9300 . ? C13 N1 1.444(19) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? N1 C14 1.55(2) . ? N1 H1A 0.9100 . ? C14 C31 1.43(2) . ? C14 C15 1.550(18) . ? C14 H14 0.9800 . ? C15 O2 1.178(18) . ? C15 O3 1.271(19) . ? C16 N2 1.506(18) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? N2 C25 1.55(2) . ? N2 H2 0.9100 . ? C18 C19 1.20(3) 4_566 ? C18 C17 1.45(2) . ? C18 H18 0.9300 . ? C17 O7 1.27(2) . ? C17 C20 1.48(2) 4_566 ? C19 C18 1.20(3) 4_566 ? C19 C22 1.30(4) . ? C19 H19 0.9300 . ? C20 C21 1.44(3) . ? C20 C36 1.43(2) . ? C20 C17 1.48(2) 4_566 ? C21 C22 1.47(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? O5 C24 1.302(14) . ? N3 C23 1.53(2) . ? N3 C36 1.542(19) . ? N3 H3 0.9100 . ? C24 O6 1.174(16) . ? C24 C23 1.49(2) . ? C23 C27 1.61(3) . ? C23 H23 0.9800 . ? O8 C26 1.246(14) . ? C25 C35 1.48(2) . ? C25 C26 1.546(16) . ? C25 H25 0.9800 . ? C26 O9 1.220(15) . ? C27 C28 1.49(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C30 1.41(7) . ? C28 C29 1.57(6) . ? C28 H28 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C35 C37 1.48(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.38(5) . ? C37 C39 1.532(18) . ? C37 H37 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 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 C31 C34 C33 127(2) . . ? C31 C34 C40 119(2) . . ? C33 C34 C40 109(2) . . ? C31 C34 H34 97.5 . . ? C33 C34 H34 97.6 . . ? C40 C34 H34 97.6 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 Cu1 O8 96.9(3) . . ? O3 Cu1 N2 173.1(4) . . ? O8 Cu1 N2 83.2(4) . . ? O3 Cu1 N1 82.8(4) . . ? O8 Cu1 N1 171.0(5) . . ? N2 Cu1 N1 98.3(4) . . ? O3 Cu1 K1 48.6(2) . . ? O8 Cu1 K1 48.3(2) . . ? N2 Cu1 K1 130.9(3) . . ? N1 Cu1 K1 130.8(3) . . ? O5 Cu2 O5 96.7(4) . 4_566 ? O5 Cu2 N3 82.4(4) . . ? O5 Cu2 N3 171.4(5) 4_566 . ? O5 Cu2 N3 171.4(5) . 4_566 ? O5 Cu2 N3 82.4(4) 4_566 4_566 ? N3 Cu2 N3 99.7(8) . 4_566 ? O5 Cu2 K1 48.3(2) . . ? O5 Cu2 K1 48.3(2) 4_566 . ? N3 Cu2 K1 130.1(4) . . ? N3 Cu2 K1 130.1(4) 4_566 . ? O8 K1 O8 76.2(4) . 4_566 ? O8 K1 O3 64.4(2) . . ? O8 K1 O3 111.3(2) 4_566 . ? O8 K1 O3 111.3(2) . 4_566 ? O8 K1 O3 64.4(2) 4_566 4_566 ? O3 K1 O3 174.9(3) . 4_566 ? O8 K1 O5 109.5(3) . 4_566 ? O8 K1 O5 174.0(3) 4_566 4_566 ? O3 K1 O5 73.7(2) . 4_566 ? O3 K1 O5 110.9(3) 4_566 4_566 ? O8 K1 O5 174.0(3) . . ? O8 K1 O5 109.5(3) 4_566 . ? O3 K1 O5 110.9(3) . . ? O3 K1 O5 73.7(2) 4_566 . ? O5 K1 O5 65.0(4) 4_566 . ? O8 K1 Cu1 32.39(17) . . ? O8 K1 Cu1 94.6(2) 4_566 . ? O3 K1 Cu1 31.97(17) . . ? O3 K1 Cu1 143.61(19) 4_566 . ? O5 K1 Cu1 91.41(17) 4_566 . ? O5 K1 Cu1 142.67(19) . . ? O8 K1 Cu1 94.6(2) . 4_566 ? O8 K1 Cu1 32.39(17) 4_566 4_566 ? O3 K1 Cu1 143.61(19) . 4_566 ? O3 K1 Cu1 31.97(17) 4_566 4_566 ? O5 K1 Cu1 142.67(19) 4_566 4_566 ? O5 K1 Cu1 91.41(17) . 4_566 ? Cu1 K1 Cu1 121.86(12) . 4_566 ? O8 K1 Cu2 141.90(19) . . ? O8 K1 Cu2 141.90(19) 4_566 . ? O3 K1 Cu2 92.56(17) . . ? O3 K1 Cu2 92.56(17) 4_566 . ? O5 K1 Cu2 32.48(18) 4_566 . ? O5 K1 Cu2 32.48(18) . . ? Cu1 K1 Cu2 119.07(6) . . ? Cu1 K1 Cu2 119.07(6) 4_566 . ? C3 C2 O4 123.4(16) . . ? C3 C2 C1 117(2) . . ? O4 C2 C1 119.9(18) . . ? C4 C5 C6 119(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C6 C1 C2 119(2) . . ? C6 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C4 C3 C2 119(2) . . ? C4 C3 C16 126(3) . . ? C2 C3 C16 113.0(19) . . ? C1 C6 C5 121(2) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C5 C4 C3 124(2) . . ? C5 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C11 C12 C7 118.1(11) . . ? C11 C12 C13 122.6(12) . . ? C7 C12 C13 118.4(11) . . ? O1 C7 C12 119.3(10) . . ? O1 C7 C8 118.4(13) . . ? C12 C7 C8 121.9(13) . . ? C7 C8 C9 115.2(14) . . ? C7 C8 H8 122.4 . . ? C9 C8 H8 122.4 . . ? C10 C9 C8 120.2(15) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C10 C11 C12 123.2(15) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C9 C10 C11 120.5(17) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N1 C13 C12 120.1(11) . . ? N1 C13 H13A 107.3 . . ? C12 C13 H13A 107.3 . . ? N1 C13 H13B 107.3 . . ? C12 C13 H13B 107.3 . . ? H13A C13 H13B 106.9 . . ? C13 N1 C14 113.7(11) . . ? C13 N1 Cu1 111.1(10) . . ? C14 N1 Cu1 107.2(7) . . ? C13 N1 H1A 108.2 . . ? C14 N1 H1A 108.2 . . ? Cu1 N1 H1A 108.2 . . ? C31 C14 C15 114.6(15) . . ? C31 C14 N1 108.9(17) . . ? C15 C14 N1 105.8(13) . . ? C31 C14 H14 109.1 . . ? C15 C14 H14 109.1 . . ? N1 C14 H14 109.1 . . ? O2 C15 O3 131.4(13) . . ? O2 C15 C14 111.2(17) . . ? O3 C15 C14 117.1(15) . . ? C15 O3 Cu1 117.3(8) . . ? C15 O3 K1 142.3(8) . . ? Cu1 O3 K1 99.4(3) . . ? C3 C16 N2 114.9(12) . . ? C3 C16 H16A 108.6 . . ? N2 C16 H16A 108.6 . . ? C3 C16 H16B 108.5 . . ? N2 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C16 N2 C25 112.6(11) . . ? C16 N2 Cu1 112.2(10) . . ? C25 N2 Cu1 107.2(7) . . ? C16 N2 H2 108.2 . . ? C25 N2 H2 108.2 . . ? Cu1 N2 H2 108.2 . . ? C19 C18 C17 130(2) 4_566 . ? C19 C18 H18 115.1 4_566 . ? C17 C18 H18 115.1 . . ? O7 C17 C18 130.1(17) . . ? O7 C17 C20 119.1(14) . 4_566 ? C18 C17 C20 110.8(17) . 4_566 ? C18 C19 C22 118(3) 4_566 . ? C18 C19 H19 120.9 4_566 . ? C22 C19 H19 120.9 . . ? C21 C20 C36 117.7(17) . . ? C21 C20 C17 122.9(15) . 4_566 ? C36 C20 C17 119.4(16) . 4_566 ? C20 C21 C22 110.0(18) . . ? C20 C21 H21 125.0 . . ? C22 C21 H21 125.0 . . ? C19 C22 C21 128(3) . . ? C19 C22 H22 116.2 . . ? C21 C22 H22 116.2 . . ? C24 O5 Cu2 114.0(8) . . ? C24 O5 K1 146.3(8) . . ? Cu2 O5 K1 99.2(3) . . ? C23 N3 C36 112.0(16) . . ? C23 N3 Cu2 109.5(10) . . ? C36 N3 Cu2 113.3(9) . . ? C23 N3 H3 107.2 . . ? C36 N3 H3 107.2 . . ? Cu2 N3 H3 107.2 . . ? O6 C24 O5 125.3(12) . . ? O6 C24 C23 114.7(14) . . ? O5 C24 C23 120.0(14) . . ? C24 C23 N3 106.1(13) . . ? C24 C23 C27 110.5(16) . . ? N3 C23 C27 108.3(16) . . ? C24 C23 H23 110.6 . . ? N3 C23 H23 110.6 . . ? C27 C23 H23 110.6 . . ? C26 O8 Cu1 116.5(7) . . ? C26 O8 K1 143.1(7) . . ? Cu1 O8 K1 99.3(3) . . ? C35 C25 C26 114.8(16) . . ? C35 C25 N2 110.9(14) . . ? C26 C25 N2 106.3(11) . . ? C35 C25 H25 108.2 . . ? C26 C25 H25 108.2 . . ? N2 C25 H25 108.2 . . ? O9 C26 O8 126.3(11) . . ? O9 C26 C25 115.6(12) . . ? O8 C26 C25 117.6(12) . . ? C28 C27 C23 115(2) . . ? C28 C27 H27A 108.2 . . ? C23 C27 H27A 108.6 . . ? C28 C27 H27B 109.1 . . ? C23 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C27 C28 C30 103(5) . . ? C27 C28 C29 105(5) . . ? C30 C28 C29 92(5) . . ? C27 C28 H28 117.5 . . ? C30 C28 H28 116.0 . . ? C29 C28 H28 117.4 . . ? C28 C30 H30A 109.3 . . ? C28 C30 H30B 109.7 . . ? H30A C30 H30B 108.0 . . ? C28 C30 H30C 111.0 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C29 H29A 109.0 . . ? C28 C29 H29B 109.6 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.8 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C31 C14 126.2(18) . . ? C34 C31 H31A 105.7 . . ? C14 C31 H31A 105.7 . . ? C34 C31 H31B 105.8 . . ? C14 C31 H31B 105.8 . . ? H31A C31 H31B 106.2 . . ? C37 C35 C25 121(2) . . ? C37 C35 H35A 107.0 . . ? C25 C35 H35A 107.0 . . ? C37 C35 H35B 107.0 . . ? C25 C35 H35B 107.0 . . ? H35A C35 H35B 106.7 . . ? C20 C36 N3 114.6(13) . . ? C20 C36 H36A 108.6 . . ? N3 C36 H36A 108.6 . . ? C20 C36 H36B 108.6 . . ? N3 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C35 118(3) . . ? C38 C37 C39 110(2) . . ? C35 C37 C39 113.8(19) . . ? C38 C37 H37 104.7 . . ? C35 C37 H37 104.7 . . ? C39 C37 H37 104.7 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.715 _refine_diff_density_min -1.475 _refine_diff_density_rms 0.130 _database_code_depnum_ccdc_archive 'CCDC 943450'