data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H132 Cu6 I6 N42 O12' _chemical_formula_weight 3929.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 27.31030(10) _cell_length_b 27.31030(10) _cell_length_c 27.31030(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20369.46(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7109 _cell_measurement_theta_min 3.2337 _cell_measurement_theta_max 62.4981 _exptl_crystal_description Octahedral _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7800 _exptl_absorpt_coefficient_mu 8.288 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2880 _exptl_absorpt_correction_T_max 0.4912 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _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 15630 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 62.59 _reflns_number_total 5376 _reflns_number_gt 4224 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The ClO~4~^-^ anions and water solvents are severely disordered and removed by using SQUEEZ program from PLUTON ; _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^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5376 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 I1 I 0.222999(11) 0.522240(10) 0.160048(10) 0.05457(11) Uani 1 1 d . . . Cu1 Cu 0.653881(16) 0.851166(16) 0.590018(15) 0.02480(12) Uani 1 1 d . . . N1 N 0.68647(9) 0.80871(9) 0.53348(9) 0.0277(6) Uani 1 1 d . . . N2 N 0.71717(10) 0.83093(9) 0.62343(10) 0.0278(6) Uani 1 1 d . . . N3 N 0.78120(10) 0.78073(10) 0.62268(10) 0.0325(6) Uani 1 1 d . . . H3A H 0.8011 0.7573 0.6132 0.039 Uiso 1 1 calc R . . N4 N 0.59678(10) 0.80465(10) 0.57471(10) 0.0305(6) Uani 1 1 d . . . N5 N 0.56416(11) 0.75352(11) 0.52036(11) 0.0391(7) Uani 1 1 d . . . H5B H 0.5614 0.7351 0.4940 0.047 Uiso 1 1 calc R . . N6 N 0.66455(9) 0.90579(9) 0.53603(9) 0.0260(6) Uani 1 1 d . . . N7 N 0.69529(9) 0.92073(9) 0.46203(9) 0.0261(6) Uani 1 1 d . . . C1 C 0.71552(12) 0.76978(12) 0.55799(12) 0.0308(7) Uani 1 1 d . . . H1A H 0.7408 0.7567 0.5355 0.037 Uiso 1 1 calc R . . H1B H 0.6940 0.7425 0.5684 0.037 Uiso 1 1 calc R . . C2 C 0.73888(12) 0.79339(11) 0.60133(12) 0.0286(7) Uani 1 1 d . . . C3 C 0.74741(12) 0.84295(11) 0.66260(12) 0.0283(7) Uani 1 1 d . . . C4 C 0.74300(13) 0.87876(12) 0.69864(13) 0.0338(8) Uani 1 1 d . . . H4A H 0.7159 0.9005 0.6991 0.041 Uiso 1 1 calc R . . C5 C 0.77924(14) 0.88159(14) 0.73358(14) 0.0408(9) Uani 1 1 d . . . H5A H 0.7770 0.9057 0.7586 0.049 Uiso 1 1 calc R . . C6 C 0.81913(15) 0.84983(15) 0.73302(15) 0.0485(10) Uani 1 1 d . . . H6A H 0.8435 0.8528 0.7577 0.058 Uiso 1 1 calc R . . C7 C 0.82436(14) 0.81403(15) 0.69753(15) 0.0452(9) Uani 1 1 d . . . H7A H 0.8516 0.7924 0.6972 0.054 Uiso 1 1 calc R . . C8 C 0.78777(12) 0.81133(12) 0.66239(13) 0.0325(7) Uani 1 1 d . . . C9 C 0.64698(12) 0.78852(13) 0.50200(12) 0.0328(7) Uani 1 1 d . . . H9A H 0.6397 0.8115 0.4749 0.039 Uiso 1 1 calc R . . H9B H 0.6574 0.7569 0.4877 0.039 Uiso 1 1 calc R . . C10 C 0.60285(12) 0.78137(12) 0.53271(12) 0.0313(7) Uani 1 1 d . . . C11 C 0.55029(13) 0.79112(13) 0.59123(13) 0.0368(8) Uani 1 1 d . . . C12 C 0.52377(14) 0.80422(16) 0.63228(14) 0.0465(9) Uani 1 1 d . . . H12A H 0.5372 0.8252 0.6565 0.056 Uiso 1 1 calc R . . C13 C 0.47711(16) 0.78568(19) 0.63680(17) 0.0604(12) Uani 1 1 d . . . H13A H 0.4582 0.7947 0.6646 0.072 Uiso 1 1 calc R . . C14 C 0.45672(17) 0.7544(2) 0.60238(18) 0.0672(14) Uani 1 1 d . . . H14A H 0.4244 0.7425 0.6071 0.081 Uiso 1 1 calc R . . C15 C 0.48237(16) 0.74038(18) 0.56172(18) 0.0578(11) Uani 1 1 d . . . H15A H 0.4687 0.7189 0.5380 0.069 Uiso 1 1 calc R . . C16 C 0.52976(13) 0.75927(15) 0.55670(14) 0.0425(9) Uani 1 1 d . . . C17 C 0.71835(12) 0.84203(12) 0.50477(12) 0.0300(7) Uani 1 1 d . . . H17A H 0.7501 0.8466 0.5217 0.036 Uiso 1 1 calc R . . H17B H 0.7247 0.8281 0.4719 0.036 Uiso 1 1 calc R . . C18 C 0.69246(11) 0.88942(12) 0.50027(11) 0.0254(7) Uani 1 1 d . . . C19 C 0.64780(11) 0.95116(11) 0.52086(11) 0.0258(7) Uani 1 1 d . . . C20 C 0.61645(12) 0.98450(12) 0.54359(12) 0.0291(7) Uani 1 1 d . . . H20A H 0.6029 0.9781 0.5749 0.035 Uiso 1 1 calc R . . C21 C 0.60599(13) 1.02725(12) 0.51865(13) 0.0356(8) Uani 1 1 d . . . H21A H 0.5848 1.0506 0.5333 0.043 Uiso 1 1 calc R . . C22 C 0.62583(14) 1.03697(13) 0.47242(13) 0.0380(8) Uani 1 1 d . . . H22A H 0.6182 1.0671 0.4568 0.046 Uiso 1 1 calc R . . C23 C 0.65610(13) 1.00411(13) 0.44884(12) 0.0356(8) Uani 1 1 d . . . H23A H 0.6692 1.0104 0.4172 0.043 Uiso 1 1 calc R . . C24 C 0.66623(11) 0.96111(11) 0.47428(11) 0.0269(7) Uani 1 1 d . . . C25 C 0.71628(11) 0.91072(12) 0.41414(11) 0.0287(7) Uani 1 1 d . . . H25A H 0.7455 0.8897 0.4183 0.034 Uiso 1 1 calc R . . H25B H 0.7272 0.9420 0.3994 0.034 Uiso 1 1 calc R . . C26 C 0.68013(11) 0.88516(11) 0.37842(10) 0.0211(6) Uani 1 1 d . . . O1 O 0.63909(8) 0.87438(8) 0.39475(8) 0.0281(5) Uani 1 1 d . . . O2 O 0.69629(8) 0.87808(9) 0.33649(8) 0.0337(5) 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 I1 0.06602(19) 0.05205(17) 0.04563(16) 0.00464(12) 0.01857(13) 0.00241(13) Cu1 0.0251(2) 0.0266(2) 0.0228(2) 0.00047(18) 0.00254(18) 0.00295(18) N1 0.0280(14) 0.0275(14) 0.0276(14) 0.0002(11) 0.0007(11) 0.0017(11) N2 0.0287(14) 0.0252(13) 0.0294(14) 0.0005(11) -0.0018(11) 0.0034(11) N3 0.0288(14) 0.0295(14) 0.0392(16) -0.0004(12) -0.0013(12) 0.0083(12) N4 0.0271(14) 0.0332(15) 0.0311(15) 0.0008(12) 0.0011(11) 0.0000(11) N5 0.0391(17) 0.0397(16) 0.0385(16) -0.0041(13) -0.0057(14) -0.0089(14) N6 0.0258(13) 0.0284(14) 0.0239(13) 0.0004(11) 0.0017(11) 0.0019(11) N7 0.0255(13) 0.0307(14) 0.0222(13) 0.0006(11) 0.0018(11) -0.0023(11) C1 0.0360(18) 0.0279(17) 0.0287(17) -0.0016(13) -0.0006(14) 0.0050(14) C2 0.0298(17) 0.0250(16) 0.0309(17) 0.0042(13) 0.0030(14) 0.0028(13) C3 0.0272(16) 0.0266(16) 0.0313(17) 0.0052(14) -0.0011(13) 0.0001(13) C4 0.0332(18) 0.0277(17) 0.0406(19) -0.0015(15) -0.0019(15) -0.0010(14) C5 0.044(2) 0.0363(19) 0.042(2) -0.0017(16) -0.0084(17) -0.0085(17) C6 0.045(2) 0.049(2) 0.052(2) 0.003(2) -0.0170(19) -0.0094(19) C7 0.0345(19) 0.045(2) 0.056(2) 0.0054(19) -0.0095(18) 0.0054(16) C8 0.0312(18) 0.0278(17) 0.0384(19) 0.0055(15) -0.0033(15) 0.0010(14) C9 0.0331(18) 0.0360(18) 0.0291(17) -0.0057(14) -0.0020(14) -0.0003(14) C10 0.0301(17) 0.0335(18) 0.0301(18) 0.0023(14) -0.0037(14) -0.0011(14) C11 0.0306(18) 0.0401(19) 0.040(2) 0.0037(16) 0.0001(15) -0.0090(15) C12 0.040(2) 0.059(2) 0.041(2) -0.0014(18) 0.0058(17) -0.0131(19) C13 0.040(2) 0.084(3) 0.057(3) -0.005(2) 0.012(2) -0.016(2) C14 0.041(2) 0.092(4) 0.069(3) 0.002(3) 0.008(2) -0.030(2) C15 0.046(2) 0.067(3) 0.060(3) 0.002(2) -0.006(2) -0.025(2) C16 0.035(2) 0.047(2) 0.046(2) 0.0049(18) -0.0036(17) -0.0084(17) C17 0.0273(16) 0.0321(17) 0.0307(17) 0.0012(14) 0.0052(14) 0.0030(14) C18 0.0224(15) 0.0322(17) 0.0216(15) 0.0000(13) -0.0012(13) -0.0020(13) C19 0.0257(16) 0.0275(16) 0.0243(15) -0.0003(13) -0.0039(13) -0.0039(13) C20 0.0308(17) 0.0301(17) 0.0265(16) -0.0063(13) 0.0020(13) 0.0000(14) C21 0.042(2) 0.0280(17) 0.0367(19) -0.0041(15) -0.0035(16) 0.0054(15) C22 0.049(2) 0.0266(17) 0.039(2) 0.0031(15) -0.0054(16) 0.0014(15) C23 0.044(2) 0.0331(18) 0.0296(17) 0.0038(15) 0.0008(15) -0.0032(16) C24 0.0288(16) 0.0277(16) 0.0242(16) -0.0045(13) -0.0010(13) -0.0027(13) C25 0.0241(16) 0.0357(18) 0.0262(16) 0.0009(14) 0.0030(13) -0.0045(13) C26 0.0267(16) 0.0204(15) 0.0163(15) 0.0005(12) 0.0027(12) 0.0010(12) O1 0.0249(12) 0.0333(12) 0.0261(11) -0.0041(9) 0.0045(9) -0.0035(9) O2 0.0306(12) 0.0437(13) 0.0268(12) -0.0014(10) 0.0059(10) -0.0024(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.952(2) 23_765 ? Cu1 N2 2.031(3) . ? Cu1 N4 2.054(3) . ? Cu1 N6 2.118(3) . ? Cu1 N1 2.126(3) . ? N1 C17 1.484(4) . ? N1 C9 1.485(4) . ? N1 C1 1.486(4) . ? N2 C2 1.329(4) . ? N2 C3 1.391(4) . ? N3 C2 1.340(4) . ? N3 C8 1.381(5) . ? N3 H3A 0.8800 . ? N4 C10 1.322(4) . ? N4 C11 1.397(5) . ? N5 C10 1.345(5) . ? N5 C16 1.376(5) . ? N5 H5B 0.8800 . ? N6 C18 1.317(4) . ? N6 C19 1.384(4) . ? N7 C18 1.352(4) . ? N7 C24 1.399(4) . ? N7 C25 1.454(4) . ? C1 C2 1.491(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.393(5) . ? C3 C8 1.401(5) . ? C4 C5 1.377(5) . ? C4 H4A 0.9500 . ? C5 C6 1.393(6) . ? C5 H5A 0.9500 . ? C6 C7 1.384(6) . ? C6 H6A 0.9500 . ? C7 C8 1.387(5) . ? C7 H7A 0.9500 . ? C9 C10 1.481(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.382(6) . ? C11 C16 1.400(5) . ? C12 C13 1.377(6) . ? C12 H12A 0.9500 . ? C13 C14 1.387(7) . ? C13 H13A 0.9500 . ? C14 C15 1.367(7) . ? C14 H14A 0.9500 . ? C15 C16 1.400(6) . ? C15 H15A 0.9500 . ? C17 C18 1.480(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C24 1.395(5) . ? C19 C20 1.396(5) . ? C20 C21 1.381(5) . ? C20 H20A 0.9500 . ? C21 C22 1.399(5) . ? C21 H21A 0.9500 . ? C22 C23 1.380(5) . ? C22 H22A 0.9500 . ? C23 C24 1.392(5) . ? C23 H23A 0.9500 . ? C25 C26 1.554(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O1 1.242(4) . ? C26 O2 1.242(4) . ? O1 Cu1 1.952(2) 20_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 101.19(10) 23_765 . ? O1 Cu1 N4 102.52(10) 23_765 . ? N2 Cu1 N4 124.68(11) . . ? O1 Cu1 N6 95.91(9) 23_765 . ? N2 Cu1 N6 112.80(10) . . ? N4 Cu1 N6 113.48(10) . . ? O1 Cu1 N1 175.47(10) 23_765 . ? N2 Cu1 N1 79.73(10) . . ? N4 Cu1 N1 80.37(10) . . ? N6 Cu1 N1 79.68(10) . . ? C17 N1 C9 110.4(3) . . ? C17 N1 C1 111.3(2) . . ? C9 N1 C1 112.5(3) . . ? C17 N1 Cu1 107.16(19) . . ? C9 N1 Cu1 108.60(19) . . ? C1 N1 Cu1 106.66(19) . . ? C2 N2 C3 105.5(3) . . ? C2 N2 Cu1 112.7(2) . . ? C3 N2 Cu1 141.9(2) . . ? C2 N3 C8 107.3(3) . . ? C2 N3 H3A 126.3 . . ? C8 N3 H3A 126.3 . . ? C10 N4 C11 105.5(3) . . ? C10 N4 Cu1 112.3(2) . . ? C11 N4 Cu1 142.0(2) . . ? C10 N5 C16 106.9(3) . . ? C10 N5 H5B 126.5 . . ? C16 N5 H5B 126.5 . . ? C18 N6 C19 105.9(3) . . ? C18 N6 Cu1 110.9(2) . . ? C19 N6 Cu1 142.5(2) . . ? C18 N7 C24 106.4(2) . . ? C18 N7 C25 126.8(3) . . ? C24 N7 C25 125.9(3) . . ? N1 C1 C2 106.1(3) . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? N2 C2 N3 112.7(3) . . ? N2 C2 C1 120.2(3) . . ? N3 C2 C1 127.1(3) . . ? N2 C3 C4 131.2(3) . . ? N2 C3 C8 108.6(3) . . ? C4 C3 C8 120.3(3) . . ? C5 C4 C3 117.9(3) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 121.9(4) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 116.6(4) . . ? C6 C7 H7A 121.7 . . ? C8 C7 H7A 121.7 . . ? N3 C8 C7 132.0(3) . . ? N3 C8 C3 105.9(3) . . ? C7 C8 C3 122.1(3) . . ? C10 C9 N1 108.2(3) . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9B 110.1 . . ? N1 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N4 C10 N5 113.0(3) . . ? N4 C10 C9 122.0(3) . . ? N5 C10 C9 124.9(3) . . ? C12 C11 N4 132.1(3) . . ? C12 C11 C16 119.8(3) . . ? N4 C11 C16 108.1(3) . . ? C13 C12 C11 117.6(4) . . ? C13 C12 H12A 121.2 . . ? C11 C12 H12A 121.2 . . ? C12 C13 C14 122.5(4) . . ? C12 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C15 C14 C13 121.1(4) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C14 C15 C16 116.7(4) . . ? C14 C15 H15A 121.6 . . ? C16 C15 H15A 121.6 . . ? N5 C16 C15 131.3(4) . . ? N5 C16 C11 106.5(3) . . ? C15 C16 C11 122.2(4) . . ? C18 C17 N1 107.4(2) . . ? C18 C17 H17A 110.2 . . ? N1 C17 H17A 110.2 . . ? C18 C17 H17B 110.2 . . ? N1 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? N6 C18 N7 113.0(3) . . ? N6 C18 C17 120.8(3) . . ? N7 C18 C17 126.2(3) . . ? N6 C19 C24 109.2(3) . . ? N6 C19 C20 130.8(3) . . ? C24 C19 C20 120.0(3) . . ? C21 C20 C19 117.3(3) . . ? C21 C20 H20A 121.3 . . ? C19 C20 H20A 121.3 . . ? C20 C21 C22 121.7(3) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C23 C22 C21 122.0(3) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C22 C23 C24 115.8(3) . . ? C22 C23 H23A 122.1 . . ? C24 C23 H23A 122.1 . . ? C23 C24 C19 123.2(3) . . ? C23 C24 N7 131.2(3) . . ? C19 C24 N7 105.6(3) . . ? N7 C25 C26 113.5(2) . . ? N7 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? N7 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O1 C26 O2 127.9(3) . . ? O1 C26 C25 117.0(2) . . ? O2 C26 C25 115.0(3) . . ? C26 O1 Cu1 119.64(19) . 20_575 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 N1 C17 14.6(14) 23_765 . . . ? N2 Cu1 N1 C17 -87.4(2) . . . . ? N4 Cu1 N1 C17 144.5(2) . . . . ? N6 Cu1 N1 C17 28.27(19) . . . . ? O1 Cu1 N1 C9 -104.6(12) 23_765 . . . ? N2 Cu1 N1 C9 153.4(2) . . . . ? N4 Cu1 N1 C9 25.3(2) . . . . ? N6 Cu1 N1 C9 -90.9(2) . . . . ? O1 Cu1 N1 C1 133.9(12) 23_765 . . . ? N2 Cu1 N1 C1 31.9(2) . . . . ? N4 Cu1 N1 C1 -96.2(2) . . . . ? N6 Cu1 N1 C1 147.6(2) . . . . ? O1 Cu1 N2 C2 167.5(2) 23_765 . . . ? N4 Cu1 N2 C2 53.6(3) . . . . ? N6 Cu1 N2 C2 -91.1(2) . . . . ? N1 Cu1 N2 C2 -17.0(2) . . . . ? O1 Cu1 N2 C3 -13.1(4) 23_765 . . . ? N4 Cu1 N2 C3 -127.0(3) . . . . ? N6 Cu1 N2 C3 88.3(3) . . . . ? N1 Cu1 N2 C3 162.4(4) . . . . ? O1 Cu1 N4 C10 161.5(2) 23_765 . . . ? N2 Cu1 N4 C10 -85.2(2) . . . . ? N6 Cu1 N4 C10 59.3(2) . . . . ? N1 Cu1 N4 C10 -14.9(2) . . . . ? O1 Cu1 N4 C11 -11.0(4) 23_765 . . . ? N2 Cu1 N4 C11 102.3(4) . . . . ? N6 Cu1 N4 C11 -113.2(4) . . . . ? N1 Cu1 N4 C11 172.6(4) . . . . ? O1 Cu1 N6 C18 167.8(2) 23_765 . . . ? N2 Cu1 N6 C18 63.1(2) . . . . ? N4 Cu1 N6 C18 -85.7(2) . . . . ? N1 Cu1 N6 C18 -11.1(2) . . . . ? O1 Cu1 N6 C19 -24.1(3) 23_765 . . . ? N2 Cu1 N6 C19 -128.8(3) . . . . ? N4 Cu1 N6 C19 82.4(3) . . . . ? N1 Cu1 N6 C19 157.0(3) . . . . ? C17 N1 C1 C2 77.3(3) . . . . ? C9 N1 C1 C2 -158.3(3) . . . . ? Cu1 N1 C1 C2 -39.3(3) . . . . ? C3 N2 C2 N3 -1.0(4) . . . . ? Cu1 N2 C2 N3 178.6(2) . . . . ? C3 N2 C2 C1 178.2(3) . . . . ? Cu1 N2 C2 C1 -2.2(4) . . . . ? C8 N3 C2 N2 1.2(4) . . . . ? C8 N3 C2 C1 -178.0(3) . . . . ? N1 C1 C2 N2 29.2(4) . . . . ? N1 C1 C2 N3 -151.6(3) . . . . ? C2 N2 C3 C4 -179.2(3) . . . . ? Cu1 N2 C3 C4 1.4(6) . . . . ? C2 N2 C3 C8 0.4(3) . . . . ? Cu1 N2 C3 C8 -179.0(3) . . . . ? N2 C3 C4 C5 179.4(3) . . . . ? C8 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C7 0.0(6) . . . . ? C5 C6 C7 C8 0.0(6) . . . . ? C2 N3 C8 C7 178.7(4) . . . . ? C2 N3 C8 C3 -0.9(4) . . . . ? C6 C7 C8 N3 -179.7(4) . . . . ? C6 C7 C8 C3 -0.2(5) . . . . ? N2 C3 C8 N3 0.3(3) . . . . ? C4 C3 C8 N3 180.0(3) . . . . ? N2 C3 C8 C7 -179.4(3) . . . . ? C4 C3 C8 C7 0.3(5) . . . . ? C17 N1 C9 C10 -147.3(3) . . . . ? C1 N1 C9 C10 87.8(3) . . . . ? Cu1 N1 C9 C10 -30.1(3) . . . . ? C11 N4 C10 N5 -0.2(4) . . . . ? Cu1 N4 C10 N5 -175.4(2) . . . . ? C11 N4 C10 C9 176.4(3) . . . . ? Cu1 N4 C10 C9 1.2(4) . . . . ? C16 N5 C10 N4 0.7(4) . . . . ? C16 N5 C10 C9 -175.8(3) . . . . ? N1 C9 C10 N4 20.4(4) . . . . ? N1 C9 C10 N5 -163.5(3) . . . . ? C10 N4 C11 C12 -178.9(4) . . . . ? Cu1 N4 C11 C12 -6.1(7) . . . . ? C10 N4 C11 C16 -0.4(4) . . . . ? Cu1 N4 C11 C16 172.4(3) . . . . ? N4 C11 C12 C13 177.1(4) . . . . ? C16 C11 C12 C13 -1.3(6) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 -0.1(8) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C10 N5 C16 C15 177.4(4) . . . . ? C10 N5 C16 C11 -0.9(4) . . . . ? C14 C15 C16 N5 -178.3(4) . . . . ? C14 C15 C16 C11 -0.2(7) . . . . ? C12 C11 C16 N5 179.5(3) . . . . ? N4 C11 C16 N5 0.8(4) . . . . ? C12 C11 C16 C15 1.0(6) . . . . ? N4 C11 C16 C15 -177.7(4) . . . . ? C9 N1 C17 C18 78.7(3) . . . . ? C1 N1 C17 C18 -155.6(3) . . . . ? Cu1 N1 C17 C18 -39.3(3) . . . . ? C19 N6 C18 N7 -0.3(3) . . . . ? Cu1 N6 C18 N7 172.2(2) . . . . ? C19 N6 C18 C17 177.7(3) . . . . ? Cu1 N6 C18 C17 -9.8(3) . . . . ? C24 N7 C18 N6 -0.2(3) . . . . ? C25 N7 C18 N6 -169.5(3) . . . . ? C24 N7 C18 C17 -178.1(3) . . . . ? C25 N7 C18 C17 12.6(5) . . . . ? N1 C17 C18 N6 34.3(4) . . . . ? N1 C17 C18 N7 -147.9(3) . . . . ? C18 N6 C19 C24 0.8(3) . . . . ? Cu1 N6 C19 C24 -167.7(3) . . . . ? C18 N6 C19 C20 178.7(3) . . . . ? Cu1 N6 C19 C20 10.3(6) . . . . ? N6 C19 C20 C21 -179.3(3) . . . . ? C24 C19 C20 C21 -1.6(5) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 C23 1.3(5) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C22 C23 C24 C19 -0.6(5) . . . . ? C22 C23 C24 N7 -179.3(3) . . . . ? N6 C19 C24 C23 -179.9(3) . . . . ? C20 C19 C24 C23 1.9(5) . . . . ? N6 C19 C24 N7 -0.9(3) . . . . ? C20 C19 C24 N7 -179.1(3) . . . . ? C18 N7 C24 C23 179.6(3) . . . . ? C25 N7 C24 C23 -11.1(5) . . . . ? C18 N7 C24 C19 0.7(3) . . . . ? C25 N7 C24 C19 170.1(3) . . . . ? C18 N7 C25 C26 84.2(4) . . . . ? C24 N7 C25 C26 -83.0(4) . . . . ? N7 C25 C26 O1 -3.0(4) . . . . ? N7 C25 C26 O2 177.0(3) . . . . ? O2 C26 O1 Cu1 -3.9(4) . . . 20_575 ? C25 C26 O1 Cu1 176.0(2) . . . 20_575 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 62.59 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.467 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.076 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 0.000 0.000 0.000 8 1 ' ' 2 0.500 0.000 0.000 1573 352 ' ' 3 1.000 0.000 0.500 1574 352 ' ' 4 0.500 0.000 0.500 8 2 ' ' 5 0.132 0.132 0.132 46 5 ' ' 6 0.632 0.132 0.368 46 5 ' ' 7 1.000 0.500 0.000 1574 352 ' ' 8 0.500 0.500 0.500 1574 350 ' ' 9 0.132 0.368 0.632 46 5 ' ' 10 0.632 0.368 0.868 46 5 ' ' 11 0.500 0.500 0.000 8 2 ' ' 12 0.000 0.500 0.500 8 2 ' ' 13 0.368 0.632 0.132 46 6 ' ' 14 0.868 0.632 0.368 46 6 ' ' 15 0.368 0.868 0.632 46 6 ' ' 16 0.868 0.868 0.868 46 6 ' ' #==================# data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H132 Cu6 I13.50 N42 O12' _chemical_formula_weight 4881.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 27.6501(3) _cell_length_b 27.6501(3) _cell_length_c 27.6501(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21139.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6199 _cell_measurement_theta_min 3.1940 _cell_measurement_theta_max 62.3483 _exptl_crystal_description Oxtahedral _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9390 _exptl_absorpt_coefficient_mu 16.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1360 _exptl_absorpt_correction_T_max 0.2876 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16597 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 62.43 _reflns_number_total 5566 _reflns_number_gt 3605 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The ClO~4~^-^ anions and water solvents are severely disordered and removed by using SQUEEZ program from PLUTON. I atom are refined by using ISOR and SIMU to simulate isotropic displacement, which give rise 36 restraints. Due to poor crystallinity and stron absorption effect after I uptake, the reflection intersity becomes week and gives low obervation data ratio, and therefore high R values ; _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^)+(0.0121P)^2^+620.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5566 _refine_ls_number_parameters 307 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.1299 _refine_ls_wR_factor_ref 0.2882 _refine_ls_wR_factor_gt 0.2826 _refine_ls_goodness_of_fit_ref 1.375 _refine_ls_restrained_S_all 1.379 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.14598(9) 0.84493(9) 0.91694(9) 0.0417(7) Uani 1 1 d . . . N1 N 0.1765(6) 0.8037(5) 0.9726(5) 0.049(4) Uani 1 1 d . . . N2 N 0.2080(5) 0.8237(5) 0.8843(6) 0.045(4) Uani 1 1 d . . . N3 N 0.2721(6) 0.7724(6) 0.8837(6) 0.058(5) Uani 1 1 d . . . H3A H 0.2926 0.7499 0.8931 0.069 Uiso 1 1 calc R . . N4 N 0.0876(7) 0.8011(6) 0.9328(7) 0.059(5) Uani 1 1 d . . . N5 N 0.0555(7) 0.7515(7) 0.9913(8) 0.077(6) Uani 1 1 d . . . H5A H 0.0521 0.7348 1.0182 0.092 Uiso 1 1 calc R . . N6 N 0.1605(5) 0.9006(5) 0.9684(5) 0.040(4) Uani 1 1 d . . . N7 N 0.1898(5) 0.9162(5) 1.0417(5) 0.041(4) Uani 1 1 d . . . C1 C 0.2034(8) 0.7628(7) 0.9492(7) 0.057(6) Uani 1 1 d . . . H1A H 0.2276 0.7491 0.9717 0.068 Uiso 1 1 calc R . . H1B H 0.1808 0.7369 0.9393 0.068 Uiso 1 1 calc R . . C2 C 0.2263(7) 0.7833(7) 0.9082(7) 0.050(5) Uani 1 1 d . . . C3 C 0.2399(3) 0.8326(3) 0.8465(3) 0.043(4) Uani 1 1 d G . . C4 C 0.2377(4) 0.8685(4) 0.8113(4) 0.050(5) Uani 1 1 d G . . H4A H 0.2115 0.8908 0.8112 0.060 Uiso 1 1 calc R . . C5 C 0.2737(4) 0.8718(4) 0.7765(4) 0.061(6) Uani 1 1 d G . . H5B H 0.2723 0.8963 0.7525 0.073 Uiso 1 1 calc R . . C6 C 0.3120(3) 0.8392(4) 0.7768(3) 0.066(7) Uani 1 1 d G . . H6A H 0.3367 0.8415 0.7529 0.079 Uiso 1 1 calc R . . C7 C 0.3142(4) 0.8033(4) 0.8119(4) 0.071(7) Uani 1 1 d G . . H7A H 0.3403 0.7810 0.8121 0.085 Uiso 1 1 calc R . . C8 C 0.2781(3) 0.8000(4) 0.8467(4) 0.050(5) Uani 1 1 d G . . C9 C 0.1366(6) 0.7873(6) 1.0061(5) 0.047(5) Uani 1 1 d G . . H9A H 0.1464 0.7572 1.0229 0.057 Uiso 1 1 calc R . . H9B H 0.1303 0.8124 1.0309 0.057 Uiso 1 1 calc R . . C10 C 0.0935(7) 0.7788(7) 0.9783(7) 0.049(5) Uani 1 1 d . . . C11 C 0.0431(3) 0.7844(4) 0.9185(4) 0.063(6) Uani 1 1 d G . . C12 C 0.0166(4) 0.7969(5) 0.8777(4) 0.086(8) Uani 1 1 d G . . H12A H 0.0305 0.8171 0.8536 0.103 Uiso 1 1 calc R . . C13 C -0.0303(4) 0.7798(5) 0.8720(5) 0.075(6) Uani 1 1 d GU . . H13A H -0.0485 0.7883 0.8441 0.090 Uiso 1 1 calc R . . C14 C -0.0507(3) 0.7502(5) 0.9072(5) 0.098(7) Uani 1 1 d GU . . H14A H -0.0828 0.7385 0.9033 0.118 Uiso 1 1 calc R . . C15 C -0.0242(4) 0.7377(6) 0.9480(5) 0.088(9) Uani 1 1 d G . . H15A H -0.0381 0.7175 0.9720 0.105 Uiso 1 1 calc R . . C16 C 0.0227(4) 0.7549(4) 0.9537(4) 0.059(6) Uani 1 1 d G . . C17 C 0.2119(4) 0.8374(6) 1.0002(6) 0.046(5) Uani 1 1 d G . . H17A H 0.2196 0.8239 1.0324 0.056 Uiso 1 1 calc R . . H17B H 0.2423 0.8416 0.9818 0.056 Uiso 1 1 calc R . . C18 C 0.1860(6) 0.8841(7) 1.0048(7) 0.046(5) Uani 1 1 d . . . C19 C 0.1462(4) 0.9465(3) 0.9822(3) 0.047(5) Uani 1 1 d G . . C20 C 0.1164(4) 0.9802(4) 0.9597(3) 0.046(5) Uani 1 1 d G . . H20A H 0.1038 0.9737 0.9284 0.056 Uiso 1 1 calc R . . C21 C 0.1051(4) 1.0232(3) 0.9830(4) 0.056(6) Uani 1 1 d G . . H21A H 0.0848 1.0463 0.9676 0.068 Uiso 1 1 calc R . . C22 C 0.1236(5) 1.0327(3) 1.0288(4) 0.044(5) Uani 1 1 d G . . H22A H 0.1159 1.0621 1.0447 0.053 Uiso 1 1 calc R . . C23 C 0.1534(4) 0.9990(3) 1.0513(3) 0.061(6) Uani 1 1 d G . . H23A H 0.1660 1.0054 1.0826 0.073 Uiso 1 1 calc R . . C24 C 0.1647(3) 0.9559(3) 1.0280(3) 0.036(4) Uani 1 1 d G . . C25 C 0.2113(5) 0.9069(5) 1.0893(5) 0.043(5) Uani 1 1 d G . . H25A H 0.2263 0.9371 1.1015 0.052 Uiso 1 1 calc R . . H25B H 0.2371 0.8824 1.0860 0.052 Uiso 1 1 calc R . . C26 C 0.1729(6) 0.8886(5) 1.1271(6) 0.028(4) Uani 1 1 d . . . O1 O 0.1341(5) 0.8796(4) 1.1116(4) 0.043(3) Uani 1 1 d . . . O2 O 0.1884(5) 0.8863(5) 1.1689(5) 0.049(3) Uani 1 1 d . . . I1 I 0.24789(9) 0.52174(8) 0.17376(7) 0.0710(6) Uani 0.75 1 d PU . . I2 I 0.15175(8) 0.55780(7) 0.15863(7) 0.0660(6) Uani 0.75 1 d PU . . I3 I 0.05477(12) 0.58908(15) 0.14512(13) 0.1467(16) Uani 0.75 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0434(15) 0.0379(14) 0.0438(15) -0.0017(12) -0.0069(12) 0.0051(12) N1 0.069(11) 0.040(9) 0.039(9) 0.001(7) -0.007(8) 0.017(8) N2 0.040(9) 0.042(9) 0.053(10) 0.000(8) -0.008(8) 0.001(7) N3 0.071(12) 0.033(9) 0.069(12) -0.012(8) -0.014(10) 0.022(8) N4 0.073(12) 0.034(9) 0.071(13) -0.004(8) -0.001(10) 0.013(9) N5 0.071(13) 0.065(12) 0.095(16) -0.003(12) 0.021(12) -0.007(11) N6 0.040(9) 0.047(9) 0.033(8) -0.009(7) -0.005(7) 0.008(7) N7 0.048(9) 0.045(9) 0.030(8) -0.009(7) -0.001(7) 0.004(7) C1 0.074(15) 0.043(12) 0.053(13) -0.007(10) 0.003(11) 0.010(11) C2 0.044(11) 0.057(13) 0.050(12) -0.022(10) -0.013(10) 0.021(10) C3 0.034(10) 0.052(12) 0.043(11) -0.013(9) -0.004(8) 0.007(9) C4 0.046(12) 0.050(12) 0.054(12) -0.007(10) -0.004(10) 0.011(10) C5 0.070(15) 0.047(12) 0.065(14) -0.004(11) -0.008(12) 0.003(11) C6 0.042(12) 0.090(18) 0.065(15) -0.031(13) 0.007(11) -0.007(12) C7 0.057(15) 0.071(16) 0.084(18) -0.009(14) -0.017(13) 0.004(12) C8 0.049(12) 0.061(13) 0.040(11) -0.014(10) 0.000(10) 0.009(10) C9 0.049(12) 0.047(11) 0.047(11) 0.004(9) 0.006(9) -0.016(9) C10 0.046(12) 0.048(12) 0.052(12) -0.012(10) 0.012(10) -0.002(10) C11 0.033(11) 0.066(15) 0.090(18) -0.014(13) -0.019(12) -0.004(10) C12 0.079(18) 0.088(19) 0.09(2) -0.020(16) -0.009(15) -0.016(15) C13 0.044(10) 0.094(13) 0.086(13) -0.010(11) -0.011(10) -0.019(10) C14 0.077(12) 0.117(14) 0.101(14) -0.028(12) -0.011(11) -0.014(12) C15 0.038(13) 0.11(2) 0.12(2) -0.014(18) 0.007(14) 0.013(14) C16 0.067(15) 0.060(14) 0.051(13) -0.002(11) 0.011(11) -0.020(12) C17 0.039(10) 0.050(12) 0.050(12) 0.004(9) -0.019(9) 0.019(9) C18 0.032(10) 0.063(13) 0.043(11) 0.009(10) 0.005(9) -0.009(9) C19 0.040(11) 0.050(12) 0.052(12) 0.004(10) 0.005(9) 0.006(9) C20 0.076(14) 0.029(10) 0.034(10) 0.004(8) 0.009(10) 0.000(9) C21 0.075(15) 0.046(12) 0.048(12) 0.005(10) 0.016(11) 0.005(11) C22 0.054(12) 0.028(10) 0.050(12) -0.002(8) -0.004(10) 0.007(9) C23 0.069(15) 0.083(16) 0.031(11) 0.006(11) -0.007(10) -0.021(13) C24 0.051(11) 0.027(9) 0.031(9) 0.002(7) 0.005(8) 0.003(8) C25 0.019(8) 0.055(12) 0.056(12) -0.007(10) -0.010(8) 0.000(8) C26 0.031(9) 0.019(8) 0.034(10) 0.000(7) -0.011(8) 0.000(7) O1 0.056(8) 0.046(8) 0.028(6) 0.008(6) 0.003(6) 0.001(6) O2 0.047(8) 0.051(8) 0.048(8) 0.007(6) -0.003(6) -0.017(6) I1 0.0912(15) 0.0794(14) 0.0424(10) 0.0011(10) 0.0176(10) -0.0033(12) I2 0.0856(15) 0.0566(12) 0.0557(12) 0.0056(9) 0.0223(10) 0.0097(10) I3 0.101(2) 0.194(4) 0.145(3) 0.093(3) 0.044(2) 0.066(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.985(12) 21_676 ? Cu1 N2 2.025(16) . ? Cu1 N4 2.066(19) . ? Cu1 N1 2.093(15) . ? Cu1 N6 2.133(14) . ? N1 C1 1.50(2) . ? N1 C9 1.511(19) . ? N1 C17 1.551(19) . ? N2 C3 1.390(18) . ? N2 C2 1.39(2) . ? N3 C8 1.288(19) . ? N3 C2 1.47(2) . ? N3 H3A 0.8800 . ? N4 C11 1.37(2) . ? N4 C10 1.41(3) . ? N5 C10 1.34(3) . ? N5 C16 1.38(2) . ? N5 H5A 0.8800 . ? N6 C18 1.31(2) . ? N6 C19 1.383(16) . ? N7 C24 1.353(16) . ? N7 C18 1.36(2) . ? N7 C25 1.467(17) . ? C1 C2 1.42(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 H5B 0.9500 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 C8 1.3900 . ? C7 H7A 0.9500 . ? C9 C10 1.44(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9500 . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 H15A 0.9500 . ? C17 C18 1.48(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C25 C26 1.57(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O1 1.183(19) . ? C26 O2 1.233(19) . ? O1 Cu1 1.985(12) 17_667 ? I1 I2 2.870(3) . ? I2 I3 2.842(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 99.2(6) 21_676 . ? O1 Cu1 N4 103.2(6) 21_676 . ? N2 Cu1 N4 125.9(6) . . ? O1 Cu1 N1 175.4(6) 21_676 . ? N2 Cu1 N1 80.1(6) . . ? N4 Cu1 N1 80.7(7) . . ? O1 Cu1 N6 96.0(5) 21_676 . ? N2 Cu1 N6 110.3(6) . . ? N4 Cu1 N6 115.4(6) . . ? N1 Cu1 N6 80.0(6) . . ? C1 N1 C9 113.6(15) . . ? C1 N1 C17 110.7(15) . . ? C9 N1 C17 109.9(13) . . ? C1 N1 Cu1 107.0(11) . . ? C9 N1 Cu1 108.7(11) . . ? C17 N1 Cu1 106.7(10) . . ? C3 N2 C2 105.6(14) . . ? C3 N2 Cu1 145.2(11) . . ? C2 N2 Cu1 109.2(12) . . ? C8 N3 C2 110.9(14) . . ? C8 N3 H3A 124.5 . . ? C2 N3 H3A 124.5 . . ? C11 N4 C10 102.4(15) . . ? C11 N4 Cu1 146.7(13) . . ? C10 N4 Cu1 110.8(14) . . ? C10 N5 C16 105.9(18) . . ? C10 N5 H5A 127.0 . . ? C16 N5 H5A 127.0 . . ? C18 N6 C19 105.1(13) . . ? C18 N6 Cu1 111.3(13) . . ? C19 N6 Cu1 142.4(10) . . ? C24 N7 C18 106.3(13) . . ? C24 N7 C25 127.0(13) . . ? C18 N7 C25 126.3(15) . . ? C2 C1 N1 105.5(16) . . ? C2 C1 H1A 110.6 . . ? N1 C1 H1A 110.6 . . ? C2 C1 H1B 110.6 . . ? N1 C1 H1B 110.6 . . ? H1A C1 H1B 108.8 . . ? N2 C2 C1 122.4(17) . . ? N2 C2 N3 105.0(17) . . ? C1 C2 N3 132.4(18) . . ? N2 C3 C4 128.7(7) . . ? N2 C3 C8 111.3(7) . . ? C4 C3 C8 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5B 120.0 . . ? C6 C5 H5B 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? N3 C8 C7 133.1(9) . . ? N3 C8 C3 106.9(8) . . ? C7 C8 C3 120.0 . . ? C10 C9 N1 109.1(13) . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? N1 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N5 C10 N4 113.1(19) . . ? N5 C10 C9 126.7(19) . . ? N4 C10 C9 120.1(16) . . ? N4 C11 C12 128.7(9) . . ? N4 C11 C16 111.0(9) . . ? C12 C11 C16 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? N5 C16 C15 132.3(9) . . ? N5 C16 C11 107.5(9) . . ? C15 C16 C11 120.0 . . ? C18 C17 N1 105.2(11) . . ? C18 C17 H17A 110.7 . . ? N1 C17 H17A 110.7 . . ? C18 C17 H17B 110.7 . . ? N1 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? N6 C18 N7 113.1(17) . . ? N6 C18 C17 119.7(17) . . ? N7 C18 C17 126.8(16) . . ? N6 C19 C20 131.3(8) . . ? N6 C19 C24 108.6(8) . . ? C20 C19 C24 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? N7 C24 C23 132.9(7) . . ? N7 C24 C19 107.0(7) . . ? C23 C24 C19 120.0 . . ? N7 C25 C26 112.3(12) . . ? N7 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N7 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? O1 C26 O2 130.1(16) . . ? O1 C26 C25 116.0(14) . . ? O2 C26 C25 113.9(13) . . ? C26 O1 Cu1 120.0(11) . 17_667 ? I3 I2 I1 177.22(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 62.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.114 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.252 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 0.000 0.000 0.000 7 4 ' ' 2 0.500 0.000 0.000 1202 486 ' ' 3 0.000 0.000 0.500 1202 484 ' ' 4 0.500 0.000 0.500 7 3 ' ' 5 0.137 0.137 0.137 58 24 ' ' 6 0.637 0.137 0.363 58 31 ' ' 7 1.000 0.500 0.000 1202 491 ' ' 8 0.500 0.500 0.500 1202 503 ' ' 9 0.137 0.363 0.637 58 23 ' ' 10 0.637 0.363 0.863 58 29 ' ' 11 0.500 0.500 0.000 7 5 ' ' 12 0.000 0.500 0.500 7 4 ' ' 13 0.363 0.637 0.137 58 20 ' ' 14 0.863 0.637 0.363 58 30 ' ' 15 0.363 0.863 0.637 58 18 ' ' 16 0.863 0.863 0.863 58 29 ' ' #==========================# data_1c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H132 Cu6 I9 N42 O12' _chemical_formula_weight 4310.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 27.6270(2) _cell_length_b 27.6270(2) _cell_length_c 27.6270(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21086.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Octahedral _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8436 _exptl_absorpt_coefficient_mu 11.460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2077 _exptl_absorpt_correction_T_max 0.3936 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _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 11810 _diffrn_reflns_av_R_equivalents 0.1783 _diffrn_reflns_av_sigmaI/netI 0.2352 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 61.66 _reflns_number_total 5330 _reflns_number_gt 1800 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The ClO~4~^-^ anions and water solvents are severely disordered and removed by using SQUEEZ program from PLUTON. Phenly rings are restricted to be coplanar by FLAT, and C and I atom are refined by using ISOR and SIMU to simulate isotropic displacement, which give rise 354 restraints. Due to poor crystallinity and stron absorption effect after I uptake, the reflection intersity becomes week and gives low obervation data ratio, and therefore high R values ; _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^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5330 _refine_ls_number_parameters 334 _refine_ls_number_restraints 390 _refine_ls_R_factor_all 0.2380 _refine_ls_R_factor_gt 0.1589 _refine_ls_wR_factor_ref 0.3631 _refine_ls_wR_factor_gt 0.3242 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.020 _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 Cu1 Cu 0.34477(7) 0.58281(7) -0.14591(7) 0.0743(6) Uani 1 1 d . . . I1 I 0.34079(6) 0.65151(7) -0.44182(6) 0.0716(5) Uani 0.50 1 d PU . . I2 I 0.35271(10) 0.55602(9) -0.40852(12) 0.1465(10) Uani 0.50 1 d PU . . I3 I 0.32640(6) 0.74817(7) -0.47838(7) 0.0775(5) Uani 0.50 1 d PU . . O1 O 0.3793(3) 0.3891(3) -0.1321(3) 0.078(3) Uani 1 1 d . . . O2 O 0.3849(4) 0.3317(4) -0.1906(4) 0.111(4) Uani 1 1 d U . . N1 N 0.3034(4) 0.5261(4) -0.1774(4) 0.086(4) Uani 1 1 d . . . N5 N 0.3229(4) 0.6154(4) -0.2077(4) 0.079(4) Uani 1 1 d . . . N2 N 0.2725(5) 0.6149(5) -0.2710(5) 0.105(4) Uani 1 1 d U . . H2A H 0.2496 0.6055 -0.2910 0.125 Uiso 1 1 calc R . . N3 N 0.3964(4) 0.5318(3) -0.1585(4) 0.079(3) Uani 1 1 d . . . N4 N 0.4153(4) 0.4599(4) -0.1898(4) 0.082(4) Uani 1 1 d . . . N6 N 0.3007(5) 0.5652(5) -0.0898(5) 0.111(4) Uani 1 1 d U . . N7 N 0.2489(6) 0.5109(5) -0.0558(5) 0.124(5) Uani 1 1 d . . . H7A H 0.2291 0.4861 -0.0533 0.149 Uiso 1 1 calc R . . C1 C 0.2663(5) 0.5483(5) -0.2031(5) 0.081(4) Uani 1 1 d U . . H1A H 0.2393 0.5565 -0.1810 0.097 Uiso 1 1 calc R . . H1B H 0.2540 0.5263 -0.2285 0.097 Uiso 1 1 calc R . . C2 C 0.2853(6) 0.5913(6) -0.2245(6) 0.096(4) Uani 1 1 d U . . C9 C 0.3378(5) 0.4979(6) -0.2092(5) 0.086(4) Uani 1 1 d U . . H9A H 0.3254 0.4647 -0.2143 0.103 Uiso 1 1 calc R . . H9B H 0.3411 0.5139 -0.2411 0.103 Uiso 1 1 calc R . . C10 C 0.3828(5) 0.4965(5) -0.1854(5) 0.070(3) Uani 1 1 d U . . C17 C 0.2882(6) 0.4955(6) -0.1391(6) 0.103(5) Uani 1 1 d U . . H17A H 0.3132 0.4705 -0.1335 0.123 Uiso 1 1 calc R . . H17B H 0.2580 0.4787 -0.1489 0.123 Uiso 1 1 calc R . . C18 C 0.2794(6) 0.5220(7) -0.0934(6) 0.102(4) Uani 1 1 d U . . C19 C 0.2841(3) 0.5827(3) -0.0442(2) 0.124(4) Uani 1 1 d GDU . . C20 C 0.2934(3) 0.6244(3) -0.0176(2) 0.145(5) Uani 1 1 d GDU . . H20A H 0.3125 0.6495 -0.0311 0.174 Uiso 1 1 calc R . . C21 C 0.2746(3) 0.6293(3) 0.0288(2) 0.160(5) Uani 1 1 d GDU . . H21A H 0.2809 0.6578 0.0470 0.192 Uiso 1 1 calc R . . C22 C 0.2466(3) 0.5925(3) 0.0487(2) 0.158(5) Uani 1 1 d GDU . . H22A H 0.2338 0.5958 0.0804 0.189 Uiso 1 1 calc R . . C23 C 0.2374(3) 0.5508(3) 0.0221(3) 0.145(5) Uani 1 1 d GDU . . H23A H 0.2183 0.5256 0.0357 0.174 Uiso 1 1 calc R . . C24 C 0.2561(3) 0.5459(3) -0.0243(2) 0.122(4) Uani 1 1 d GDU . . C3 C 0.3344(3) 0.6526(3) -0.2397(2) 0.061(3) Uani 1 1 d GDU . . C4 C 0.3681(4) 0.6876(4) -0.2369(3) 0.073(3) Uani 1 1 d GDU . . H4A H 0.3897 0.6882 -0.2101 0.088 Uiso 1 1 calc R . . C5 C 0.3719(4) 0.7235(4) -0.2731(4) 0.089(4) Uani 1 1 d DU . . H5A H 0.3959 0.7481 -0.2715 0.107 Uiso 1 1 calc R . . C6 C 0.3389(4) 0.7214(4) -0.3113(4) 0.098(4) Uani 1 1 d DU . . H6A H 0.3416 0.7441 -0.3370 0.117 Uiso 1 1 calc R . . C7 C 0.3024(4) 0.6871(4) -0.3129(4) 0.091(4) Uani 1 1 d DU . . H7B H 0.2787 0.6875 -0.3378 0.110 Uiso 1 1 calc R . . C8 C 0.3016(4) 0.6528(4) -0.2773(4) 0.080(3) Uani 1 1 d DU . . C11 C 0.4456(3) 0.5181(3) -0.1465(3) 0.064(3) Uani 1 1 d DU . . C12 C 0.4788(3) 0.5399(4) -0.1173(3) 0.072(3) Uani 1 1 d DU . . H12A H 0.4719 0.5713 -0.1050 0.087 Uiso 1 1 calc R . . C13 C 0.5230(4) 0.5176(4) -0.1047(4) 0.089(4) Uani 1 1 d DU . . H13 H 0.5451 0.5324 -0.0829 0.107 Uiso 1 1 calc R . . C14 C 0.5325(4) 0.4727(4) -0.1260(4) 0.082(4) Uani 1 1 d DU . . H14A H 0.5633 0.4582 -0.1214 0.099 Uiso 1 1 calc R . . C15 C 0.4977(3) 0.4489(4) -0.1537(4) 0.078(3) Uani 1 1 d DU . . H15 H 0.5026 0.4166 -0.1644 0.094 Uiso 1 1 calc R . . C16 C 0.4559(4) 0.4738(3) -0.1650(4) 0.066(3) Uani 1 1 d DU . . C25 C 0.4084(6) 0.4137(5) -0.2105(5) 0.086(4) Uani 1 1 d U . . H25A H 0.4398 0.4025 -0.2236 0.103 Uiso 1 1 calc R . . H25B H 0.3859 0.4172 -0.2383 0.103 Uiso 1 1 calc R . . C26 C 0.3877(5) 0.3725(4) -0.1760(5) 0.073(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0730(12) 0.0747(12) 0.0752(12) -0.0040(11) -0.0047(11) -0.0016(11) I1 0.0636(9) 0.0884(11) 0.0629(9) 0.0155(9) -0.0085(8) -0.0278(9) I2 0.1388(17) 0.1148(16) 0.186(2) 0.0685(17) -0.0846(17) -0.0472(16) I3 0.0535(8) 0.0804(11) 0.0986(12) -0.0081(11) 0.0004(10) -0.0183(9) O1 0.067(5) 0.067(5) 0.099(6) -0.016(5) -0.004(5) -0.010(5) O2 0.112(7) 0.088(6) 0.133(7) -0.015(6) 0.056(6) -0.016(6) N1 0.053(6) 0.105(8) 0.100(8) 0.040(8) -0.019(6) -0.007(7) N5 0.069(6) 0.062(6) 0.107(8) -0.016(7) -0.015(7) -0.014(6) N2 0.096(6) 0.112(6) 0.105(6) 0.001(6) -0.007(6) 0.014(6) N3 0.115(8) 0.046(5) 0.075(6) 0.009(5) -0.052(7) -0.021(6) N4 0.094(8) 0.078(7) 0.075(7) -0.011(6) -0.018(7) -0.012(7) N6 0.099(6) 0.116(7) 0.117(7) 0.013(6) -0.003(6) -0.007(6) N7 0.157(12) 0.097(9) 0.119(10) -0.026(9) 0.051(10) -0.032(10) C1 0.073(7) 0.094(7) 0.076(7) 0.010(7) -0.012(6) -0.030(6) C2 0.092(7) 0.106(7) 0.092(7) -0.002(7) -0.013(6) -0.010(7) C9 0.085(7) 0.091(7) 0.081(7) -0.003(7) 0.004(7) 0.006(7) C10 0.066(6) 0.073(6) 0.071(7) 0.022(6) 0.003(6) 0.007(6) C17 0.098(8) 0.102(8) 0.108(8) 0.011(7) 0.009(7) -0.012(7) C18 0.091(7) 0.111(7) 0.105(7) 0.015(7) 0.012(7) -0.013(7) C19 0.127(7) 0.127(7) 0.118(7) -0.007(6) 0.027(6) -0.005(6) C20 0.144(8) 0.156(8) 0.136(8) -0.019(7) 0.023(7) -0.011(8) C21 0.164(8) 0.167(8) 0.148(8) -0.003(8) 0.020(8) -0.024(8) C22 0.174(8) 0.163(8) 0.137(8) 0.007(8) 0.020(8) -0.012(8) C23 0.160(8) 0.147(8) 0.129(8) 0.002(7) 0.018(7) -0.010(8) C24 0.134(8) 0.118(8) 0.114(7) -0.005(7) 0.023(7) -0.010(7) C3 0.066(6) 0.057(5) 0.061(5) -0.003(5) -0.009(5) 0.002(5) C4 0.074(6) 0.078(6) 0.067(6) -0.021(5) 0.000(6) 0.008(6) C5 0.085(6) 0.098(7) 0.083(6) -0.008(6) -0.009(6) 0.001(6) C6 0.093(7) 0.109(7) 0.090(7) -0.004(7) -0.012(6) -0.001(7) C7 0.091(7) 0.093(7) 0.091(7) 0.018(6) -0.013(6) 0.007(6) C8 0.080(6) 0.080(6) 0.080(6) 0.021(5) -0.008(6) 0.007(6) C11 0.069(6) 0.062(6) 0.060(6) 0.002(5) 0.007(5) 0.001(5) C12 0.067(6) 0.075(6) 0.075(6) -0.003(6) -0.007(5) -0.007(6) C13 0.085(6) 0.094(7) 0.088(7) -0.015(6) -0.001(6) 0.003(6) C14 0.074(6) 0.093(6) 0.081(6) -0.022(6) -0.013(6) 0.003(6) C15 0.073(6) 0.080(6) 0.081(6) -0.020(6) 0.000(6) -0.001(6) C16 0.064(6) 0.068(6) 0.065(6) -0.016(5) -0.003(5) -0.005(5) C25 0.110(8) 0.067(7) 0.080(7) -0.006(6) 0.014(7) 0.000(7) C26 0.096(7) 0.040(5) 0.083(7) -0.013(6) 0.034(6) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.960(9) 22_565 ? Cu1 N5 2.022(12) . ? Cu1 N6 2.030(14) . ? Cu1 N3 2.035(11) . ? Cu1 N1 2.125(12) . ? I1 I2 2.813(3) . ? I1 I3 2.883(3) . ? O1 C26 1.317(16) . ? O1 Cu1 1.960(9) 19_656 ? O2 C26 1.199(15) . ? N1 C1 1.389(16) . ? N1 C17 1.419(19) . ? N1 C9 1.509(18) . ? N5 C2 1.318(18) . ? N5 C3 1.393(13) . ? N2 C8 1.330(16) . ? N2 C2 1.48(2) . ? N2 H2A 0.8800 . ? N3 C10 1.283(16) . ? N3 C11 1.450(14) . ? N4 C10 1.358(17) . ? N4 C16 1.369(15) . ? N4 C25 1.412(17) . ? N6 C18 1.33(2) . ? N6 C19 1.425(16) . ? N7 C24 1.315(15) . ? N7 C18 1.37(2) . ? N7 H7A 0.8800 . ? C1 C2 1.43(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C9 C10 1.409(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C17 C18 1.48(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C3 C4 1.3468 . ? C3 C8 1.377(11) . ? C4 C5 1.412(11) . ? C4 H4A 0.9500 . ? C5 C6 1.398(12) . ? C5 H5A 0.9500 . ? C6 C7 1.384(12) . ? C6 H6A 0.9500 . ? C7 C8 1.367(12) . ? C7 H7B 0.9500 . ? C11 C16 1.355(11) . ? C11 C12 1.361(11) . ? C12 C13 1.412(11) . ? C12 H12A 0.9500 . ? C13 C14 1.396(12) . ? C13 H13 0.9500 . ? C14 C15 1.393(12) . ? C14 H14A 0.9500 . ? C15 C16 1.379(11) . ? C15 H15 0.9500 . ? C25 C26 1.591(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N5 100.2(4) 22_565 . ? O1 Cu1 N6 105.7(5) 22_565 . ? N5 Cu1 N6 124.9(5) . . ? O1 Cu1 N3 95.9(4) 22_565 . ? N5 Cu1 N3 111.9(4) . . ? N6 Cu1 N3 112.7(5) . . ? O1 Cu1 N1 173.6(4) 22_565 . ? N5 Cu1 N1 79.7(4) . . ? N6 Cu1 N1 79.3(5) . . ? N3 Cu1 N1 78.3(4) . . ? I2 I1 I3 178.08(9) . . ? C26 O1 Cu1 119.0(8) . 19_656 ? C1 N1 C17 115.1(11) . . ? C1 N1 C9 113.3(12) . . ? C17 N1 C9 108.2(12) . . ? C1 N1 Cu1 106.3(9) . . ? C17 N1 Cu1 107.2(9) . . ? C9 N1 Cu1 106.4(8) . . ? C2 N5 C3 109.2(12) . . ? C2 N5 Cu1 108.0(10) . . ? C3 N5 Cu1 142.8(8) . . ? C8 N2 C2 108.4(12) . . ? C8 N2 H2A 125.8 . . ? C2 N2 H2A 125.8 . . ? C10 N3 C11 102.0(10) . . ? C10 N3 Cu1 114.8(9) . . ? C11 N3 Cu1 143.2(7) . . ? C10 N4 C16 106.7(10) . . ? C10 N4 C25 128.3(12) . . ? C16 N4 C25 124.6(12) . . ? C18 N6 C19 103.2(12) . . ? C18 N6 Cu1 114.9(12) . . ? C19 N6 Cu1 141.9(10) . . ? C24 N7 C18 104.1(12) . . ? C24 N7 H7A 128.0 . . ? C18 N7 H7A 128.0 . . ? N1 C1 C2 107.9(12) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N5 C2 C1 124.3(14) . . ? N5 C2 N2 105.7(13) . . ? C1 C2 N2 129.7(14) . . ? C10 C9 N1 107.4(12) . . ? C10 C9 H9A 110.2 . . ? N1 C9 H9A 110.2 . . ? C10 C9 H9B 110.2 . . ? N1 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N3 C10 N4 115.1(12) . . ? N3 C10 C9 120.5(13) . . ? N4 C10 C9 124.3(13) . . ? N1 C17 C18 112.8(14) . . ? N1 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N1 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N6 C18 N7 114.5(16) . . ? N6 C18 C17 115.8(15) . . ? N7 C18 C17 129.4(16) . . ? C20 C19 C24 120.0 . . ? C20 C19 N6 133.6(6) . . ? C24 C19 N6 106.2(6) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? N7 C24 C23 128.7(7) . . ? N7 C24 C19 111.2(7) . . ? C23 C24 C19 120.0 . . ? C4 C3 C8 119.8(6) . . ? C4 C3 N5 130.6(5) . . ? C8 C3 N5 109.3(9) . . ? C3 C4 C5 121.0(6) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 117.2(10) . . ? C6 C5 H5A 121.4 . . ? C4 C5 H5A 121.4 . . ? C7 C6 C5 122.0(11) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C8 C7 C6 117.6(10) . . ? C8 C7 H7B 121.2 . . ? C6 C7 H7B 121.2 . . ? N2 C8 C7 130.5(11) . . ? N2 C8 C3 107.2(10) . . ? C7 C8 C3 122.3(10) . . ? C16 C11 C12 118.9(9) . . ? C16 C11 N3 110.3(8) . . ? C12 C11 N3 130.4(9) . . ? C11 C12 C13 122.2(9) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C14 C13 C12 116.6(9) . . ? C14 C13 H13 121.7 . . ? C12 C13 H13 121.7 . . ? C15 C14 C13 121.4(10) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C16 C15 C14 117.8(10) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C11 C16 N4 105.6(9) . . ? C11 C16 C15 122.7(9) . . ? N4 C16 C15 131.2(10) . . ? N4 C25 C26 116.8(12) . . ? N4 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? N4 C25 H25B 108.1 . . ? C26 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? O2 C26 O1 128.7(13) . . ? O2 C26 C25 119.6(13) . . ? O1 C26 C25 111.5(10) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 61.66 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.334 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.175 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 0.000 0.000 0.000 7 2 ' ' 2 0.500 0.000 0.000 1193 467 ' ' 3 0.000 0.000 0.500 1193 464 ' ' 4 0.500 0.000 0.500 7 2 ' ' 5 0.139 0.139 0.139 72 63 ' ' 6 0.639 0.139 0.361 72 84 ' ' 7 1.000 0.500 0.000 1193 483 ' ' 8 0.500 0.500 0.500 1193 495 ' ' 9 0.139 0.361 0.639 72 48 ' ' 10 0.639 0.361 0.861 72 58 ' ' 11 0.500 0.500 0.000 7 3 ' ' 12 0.000 0.500 0.500 7 2 ' ' 13 0.361 0.639 0.139 72 60 ' ' 14 0.861 0.639 0.361 72 74 ' ' 15 0.361 0.861 0.639 72 43 ' ' 16 0.861 0.861 0.861 72 61 ' ' #=======================END