Supplementary data for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Feng Luo' _publ_contact_author_email 'LUOFENG 123456@MAIL.NANKAI.EDU.CN' _publ_section_title ; An unusual metal-organic framework showing both rotaxane- and cantenane-like motifs ; loop_ _publ_author_name 'Feng Luo.' 'Yunxia Che.' 'Yu-ting Yang.' 'Jimin Zheng.' # Attachment '071217D_R.cif' data_071217d _database_code_depnum_ccdc_archive 'CCDC 682871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H42 Cd2 N4 O12' _chemical_formula_weight 1187.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.427(3) _cell_length_b 11.482(4) _cell_length_c 12.836(4) _cell_angle_alpha 68.977(7) _cell_angle_beta 81.168(5) _cell_angle_gamma 65.834(4) _cell_volume 1183.2(7) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2923 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 26.25 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8445 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6561 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4703 _reflns_number_gt 3850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+2.0885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4703 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7653(5) 0.0605(4) 0.1546(4) 0.0318(10) Uani 1 1 d . . . C2 C 0.6329(5) 0.1010(4) 0.2335(3) 0.0285(10) Uani 1 1 d . . . C3 C 0.5236(5) 0.0450(4) 0.2539(4) 0.0328(10) Uani 1 1 d . . . H3 H 0.5290 -0.0103 0.2141 0.039 Uiso 1 1 calc R . . C4 C 0.4038(5) 0.0686(4) 0.3328(4) 0.0314(10) Uani 1 1 d . . . C5 C 0.2977(5) 0.0031(5) 0.3575(4) 0.0419(12) Uani 1 1 d . . . H5 H 0.3043 -0.0529 0.3181 0.050 Uiso 1 1 calc R . . C6 C 0.1865(6) 0.0208(5) 0.4380(5) 0.0482(14) Uani 1 1 d . . . H6 H 0.1173 -0.0223 0.4530 0.058 Uiso 1 1 calc R . . C7 C 0.1769(6) 0.1048(5) 0.4984(4) 0.0462(13) Uani 1 1 d . . . H7 H 0.1034 0.1141 0.5554 0.055 Uiso 1 1 calc R . . C8 C 0.2735(5) 0.1728(5) 0.4748(4) 0.0383(11) Uani 1 1 d . . . H8 H 0.2613 0.2308 0.5138 0.046 Uiso 1 1 calc R . . C9 C 0.3933(5) 0.1574(4) 0.3915(3) 0.0285(10) Uani 1 1 d . . . C10 C 0.5001(5) 0.2230(4) 0.3655(3) 0.0283(10) Uani 1 1 d . . . C11 C 0.6210(5) 0.1901(4) 0.2913(4) 0.0301(10) Uani 1 1 d . . . C12 C 0.4933(6) 0.3185(5) 0.4257(4) 0.0353(11) Uani 1 1 d . . . C13 C 0.4940(5) 0.4569(4) 0.3542(3) 0.0265(9) Uani 1 1 d . . . C14 C 0.3650(5) 0.5514(4) 0.2900(4) 0.0271(9) Uani 1 1 d . . . C15 C 0.3531(5) 0.6852(4) 0.2279(3) 0.0284(9) Uani 1 1 d . . . C16 C 0.2119(5) 0.7887(5) 0.1575(4) 0.0358(11) Uani 1 1 d . . . C17 C 0.4732(5) 0.7222(4) 0.2315(4) 0.0301(10) Uani 1 1 d . . . H17 H 0.4657 0.8099 0.1912 0.036 Uiso 1 1 calc R . . C18 C 0.6072(5) 0.6305(4) 0.2946(3) 0.0268(9) Uani 1 1 d . . . C19 C 0.6183(5) 0.4966(4) 0.3573(4) 0.0288(10) Uani 1 1 d . . . C20 C 0.7571(6) 0.4081(5) 0.4190(4) 0.0468(13) Uani 1 1 d . . . H20 H 0.7693 0.3196 0.4607 0.056 Uiso 1 1 calc R . . C21 C 0.8735(6) 0.4516(6) 0.4180(5) 0.0549(15) Uani 1 1 d . . . H21 H 0.9628 0.3916 0.4593 0.066 Uiso 1 1 calc R . . C22 C 0.8614(6) 0.5822(6) 0.3570(4) 0.0450(13) Uani 1 1 d . . . H22 H 0.9420 0.6091 0.3573 0.054 Uiso 1 1 calc R . . C23 C 0.7311(5) 0.6707(5) 0.2970(4) 0.0367(11) Uani 1 1 d . . . H23 H 0.7223 0.7587 0.2568 0.044 Uiso 1 1 calc R . . C24 C 0.1036(6) 1.2796(5) 0.1413(4) 0.0407(12) Uani 1 1 d . . . H24 H 0.0562 1.2386 0.2044 0.049 Uiso 1 1 calc R . . C25 C 0.1655(6) 1.3695(5) 0.1349(4) 0.0485(14) Uani 1 1 d . . . H25 H 0.1687 1.4010 0.1915 0.058 Uiso 1 1 calc R . . C26 C 0.1939(6) 1.3362(5) -0.0252(4) 0.0431(13) Uani 1 1 d . . . H26 H 0.2210 1.3421 -0.0992 0.052 Uiso 1 1 calc R . . C27 C 0.2999(5) 1.5013(5) -0.0194(4) 0.0385(12) Uani 1 1 d . . . H27A H 0.2367 1.5846 -0.0041 0.046 Uiso 1 1 calc R . . H27B H 0.3066 1.5222 -0.0998 0.046 Uiso 1 1 calc R . . C28 C 0.4621(6) 1.4485(5) 0.0261(4) 0.0338(11) Uani 1 1 d . . . Cd1 Cd 0.05555(4) 1.11400(3) 0.00318(3) 0.02293(10) Uani 1 1 d . . . H1A H 0.185(6) 0.578(6) 0.246(5) 0.057(19) Uiso 1 1 d . . . H2A H 0.399(6) 0.336(5) 0.472(4) 0.047(14) Uiso 1 1 d . . . H3A H 0.576(6) 0.270(5) 0.483(4) 0.046(14) Uiso 1 1 d . . . H4A H 0.796(8) 0.201(7) 0.224(6) 0.10(2) Uiso 1 1 d . . . H5A H 0.456(6) 1.426(5) 0.104(5) 0.062(17) Uiso 1 1 d . . . H6A H 0.518(6) 1.369(5) 0.011(4) 0.047(15) Uiso 1 1 d . . . N1 N 0.1209(4) 1.2583(4) 0.0418(3) 0.0308(8) Uani 1 1 d . . . N2 N 0.2226(4) 1.4049(4) 0.0286(3) 0.0318(8) Uani 1 1 d . . . O1 O 0.1189(4) 0.7451(4) 0.1361(3) 0.0469(9) Uani 1 1 d . . . O2 O 0.1967(4) 0.9097(3) 0.1234(3) 0.0535(10) Uani 1 1 d . . . O3 O 0.2461(4) 0.5119(4) 0.2907(3) 0.0412(8) Uani 1 1 d . . . O4 O 0.7297(4) 0.2452(3) 0.2745(3) 0.0402(8) Uani 1 1 d . . . O5 O 0.7779(4) -0.0318(3) 0.1197(3) 0.0451(9) Uani 1 1 d . . . O6 O 0.8554(4) 0.1252(3) 0.1267(3) 0.0417(8) 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 C1 0.030(2) 0.027(2) 0.035(3) -0.009(2) 0.0050(19) -0.0105(19) C2 0.029(2) 0.024(2) 0.030(2) -0.0066(18) 0.0048(19) -0.0119(18) C3 0.031(2) 0.032(2) 0.039(3) -0.017(2) 0.005(2) -0.013(2) C4 0.028(2) 0.027(2) 0.040(3) -0.013(2) 0.004(2) -0.0115(19) C5 0.036(3) 0.041(3) 0.060(3) -0.029(3) 0.010(2) -0.019(2) C6 0.037(3) 0.047(3) 0.071(4) -0.025(3) 0.018(3) -0.027(2) C7 0.038(3) 0.043(3) 0.056(3) -0.019(3) 0.019(2) -0.019(2) C8 0.039(3) 0.033(3) 0.042(3) -0.014(2) 0.009(2) -0.014(2) C9 0.028(2) 0.025(2) 0.030(2) -0.0072(18) 0.0044(18) -0.0105(18) C10 0.032(2) 0.021(2) 0.029(2) -0.0068(18) 0.0007(19) -0.0088(18) C11 0.034(2) 0.027(2) 0.032(2) -0.0072(19) 0.002(2) -0.018(2) C12 0.046(3) 0.033(3) 0.028(3) -0.010(2) 0.001(2) -0.018(2) C13 0.033(2) 0.023(2) 0.027(2) -0.0145(18) 0.0041(18) -0.0105(18) C14 0.026(2) 0.030(2) 0.034(2) -0.0169(19) 0.0032(18) -0.0139(18) C15 0.027(2) 0.029(2) 0.031(2) -0.0151(19) -0.0040(18) -0.0065(18) C16 0.028(2) 0.040(3) 0.033(3) -0.016(2) -0.002(2) -0.003(2) C17 0.036(2) 0.025(2) 0.032(2) -0.0094(19) -0.001(2) -0.0140(19) C18 0.025(2) 0.034(2) 0.026(2) -0.0164(19) -0.0012(17) -0.0103(18) C19 0.031(2) 0.028(2) 0.032(2) -0.0143(19) -0.0050(19) -0.0104(19) C20 0.042(3) 0.034(3) 0.059(3) -0.013(2) -0.022(3) -0.005(2) C21 0.034(3) 0.063(4) 0.070(4) -0.029(3) -0.023(3) -0.006(3) C22 0.030(3) 0.068(4) 0.055(3) -0.035(3) 0.005(2) -0.025(3) C23 0.035(3) 0.044(3) 0.043(3) -0.023(2) 0.006(2) -0.022(2) C24 0.059(3) 0.050(3) 0.031(3) -0.013(2) 0.000(2) -0.039(3) C25 0.074(4) 0.062(3) 0.037(3) -0.024(3) 0.004(3) -0.047(3) C26 0.053(3) 0.067(3) 0.035(3) -0.029(3) 0.018(2) -0.043(3) C27 0.043(3) 0.036(3) 0.046(3) -0.003(2) -0.009(2) -0.029(2) C28 0.035(3) 0.031(3) 0.041(3) -0.007(2) -0.005(2) -0.021(2) Cd1 0.01993(15) 0.02182(15) 0.03247(18) -0.01272(12) 0.00008(11) -0.01008(11) N1 0.037(2) 0.037(2) 0.033(2) -0.0150(17) 0.0036(17) -0.0266(18) N2 0.032(2) 0.034(2) 0.039(2) -0.0117(17) -0.0041(17) -0.0206(17) O1 0.0339(19) 0.054(2) 0.053(2) -0.0175(18) -0.0186(16) -0.0109(17) O2 0.051(2) 0.0313(19) 0.061(2) -0.0057(17) -0.0179(18) -0.0014(16) O3 0.0320(19) 0.045(2) 0.056(2) -0.0186(19) -0.0050(17) -0.0197(17) O4 0.0395(19) 0.043(2) 0.052(2) -0.0245(17) 0.0128(16) -0.0265(16) O5 0.048(2) 0.043(2) 0.053(2) -0.0287(17) 0.0209(17) -0.0217(17) O6 0.0376(19) 0.0402(19) 0.054(2) -0.0205(16) 0.0180(16) -0.0233(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O5 1.249(5) . ? C1 O6 1.278(5) . ? C1 C2 1.509(6) . ? C2 C3 1.372(6) . ? C2 C11 1.426(6) . ? C3 C4 1.404(6) . ? C4 C5 1.420(6) . ? C4 C9 1.436(6) . ? C5 C6 1.360(7) . ? C6 C7 1.409(7) . ? C7 C8 1.364(6) . ? C8 C9 1.432(6) . ? C9 C10 1.425(6) . ? C10 C11 1.386(6) . ? C10 C12 1.529(6) . ? C11 O4 1.365(5) . ? C12 C13 1.526(6) . ? C13 C14 1.386(6) . ? C13 C19 1.431(6) . ? C14 O3 1.368(5) . ? C14 C15 1.420(6) . ? C15 C17 1.374(6) . ? C15 C16 1.518(6) . ? C16 O2 1.250(6) . ? C16 O1 1.275(5) . ? C17 C18 1.405(6) . ? C18 C19 1.424(6) . ? C18 C23 1.428(6) . ? C19 C20 1.423(6) . ? C20 C21 1.375(7) . ? C21 C22 1.386(7) . ? C22 C23 1.358(7) . ? C24 C25 1.353(6) . ? C24 N1 1.359(6) . ? C25 N2 1.367(6) . ? C26 N1 1.335(5) . ? C26 N2 1.340(6) . ? C27 N2 1.473(5) . ? C27 C28 1.519(6) . ? C28 C28 1.528(8) 2_685 ? Cd1 N1 2.211(3) . ? Cd1 O5 2.222(3) 2_665 ? Cd1 O6 2.263(3) 1_465 ? Cd1 O2 2.265(3) . ? Cd1 O1 2.274(3) 2_575 ? Cd1 Cd1 3.2221(11) 2_575 ? O1 Cd1 2.274(3) 2_575 ? O5 Cd1 2.222(3) 2_665 ? O6 Cd1 2.263(3) 1_645 ? 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 C1 O6 124.6(4) . . ? O5 C1 C2 118.0(4) . . ? O6 C1 C2 117.3(4) . . ? C3 C2 C11 119.0(4) . . ? C3 C2 C1 118.4(4) . . ? C11 C2 C1 122.6(4) . . ? C2 C3 C4 122.1(4) . . ? C3 C4 C5 121.2(4) . . ? C3 C4 C9 118.7(4) . . ? C5 C4 C9 120.1(4) . . ? C6 C5 C4 121.1(5) . . ? C5 C6 C7 119.6(5) . . ? C8 C7 C6 121.1(4) . . ? C7 C8 C9 121.7(4) . . ? C10 C9 C8 124.1(4) . . ? C10 C9 C4 119.6(4) . . ? C8 C9 C4 116.3(4) . . ? C11 C10 C9 119.0(4) . . ? C11 C10 C12 119.3(4) . . ? C9 C10 C12 121.4(4) . . ? O4 C11 C10 118.2(4) . . ? O4 C11 C2 120.3(4) . . ? C10 C11 C2 121.4(4) . . ? C13 C12 C10 117.7(4) . . ? C14 C13 C19 118.5(4) . . ? C14 C13 C12 119.0(4) . . ? C19 C13 C12 122.3(4) . . ? O3 C14 C13 117.3(4) . . ? O3 C14 C15 120.7(4) . . ? C13 C14 C15 122.0(4) . . ? C17 C15 C14 119.0(4) . . ? C17 C15 C16 118.9(4) . . ? C14 C15 C16 122.1(4) . . ? O2 C16 O1 124.9(4) . . ? O2 C16 C15 117.7(4) . . ? O1 C16 C15 117.3(4) . . ? C15 C17 C18 121.4(4) . . ? C17 C18 C19 119.4(4) . . ? C17 C18 C23 120.6(4) . . ? C19 C18 C23 120.0(4) . . ? C20 C19 C18 116.8(4) . . ? C20 C19 C13 123.5(4) . . ? C18 C19 C13 119.7(4) . . ? C21 C20 C19 120.9(5) . . ? C20 C21 C22 121.9(5) . . ? C23 C22 C21 119.4(5) . . ? C22 C23 C18 121.0(4) . . ? C25 C24 N1 109.8(4) . . ? C24 C25 N2 106.5(4) . . ? N1 C26 N2 110.7(4) . . ? N2 C27 C28 113.2(4) . . ? C27 C28 C28 111.4(5) . 2_685 ? N1 Cd1 O5 110.06(13) . 2_665 ? N1 Cd1 O6 95.04(12) . 1_465 ? O5 Cd1 O6 154.65(12) 2_665 1_465 ? N1 Cd1 O2 104.39(14) . . ? O5 Cd1 O2 81.98(13) 2_665 . ? O6 Cd1 O2 88.56(13) 1_465 . ? N1 Cd1 O1 101.42(13) . 2_575 ? O5 Cd1 O1 89.50(13) 2_665 2_575 ? O6 Cd1 O1 88.94(13) 1_465 2_575 ? O2 Cd1 O1 154.20(13) . 2_575 ? N1 Cd1 Cd1 169.09(9) . 2_575 ? O5 Cd1 Cd1 78.56(9) 2_665 2_575 ? O6 Cd1 Cd1 76.10(8) 1_465 2_575 ? O2 Cd1 Cd1 69.50(10) . 2_575 ? O1 Cd1 Cd1 84.98(9) 2_575 2_575 ? C26 N1 C24 105.8(4) . . ? C26 N1 Cd1 127.3(3) . . ? C24 N1 Cd1 126.8(3) . . ? C26 N2 C25 107.2(4) . . ? C26 N2 C27 125.7(4) . . ? C25 N2 C27 127.0(4) . . ? C16 O1 Cd1 117.7(3) . 2_575 ? C16 O2 Cd1 141.5(3) . . ? C1 O5 Cd1 129.9(3) . 2_665 ? C1 O6 Cd1 130.7(3) . 1_645 ? 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 O5 C1 C2 C3 -6.8(6) . . . . ? O6 C1 C2 C3 172.0(4) . . . . ? O5 C1 C2 C11 170.3(4) . . . . ? O6 C1 C2 C11 -10.8(6) . . . . ? C11 C2 C3 C4 -2.5(7) . . . . ? C1 C2 C3 C4 174.8(4) . . . . ? C2 C3 C4 C5 -176.0(4) . . . . ? C2 C3 C4 C9 1.8(7) . . . . ? C3 C4 C5 C6 176.7(5) . . . . ? C9 C4 C5 C6 -1.2(7) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C5 C6 C7 C8 2.5(8) . . . . ? C6 C7 C8 C9 -2.9(8) . . . . ? C7 C8 C9 C10 -178.2(4) . . . . ? C7 C8 C9 C4 1.3(7) . . . . ? C3 C4 C9 C10 2.4(6) . . . . ? C5 C4 C9 C10 -179.7(4) . . . . ? C3 C4 C9 C8 -177.1(4) . . . . ? C5 C4 C9 C8 0.8(6) . . . . ? C8 C9 C10 C11 173.6(4) . . . . ? C4 C9 C10 C11 -5.9(6) . . . . ? C8 C9 C10 C12 -0.6(7) . . . . ? C4 C9 C10 C12 179.9(4) . . . . ? C9 C10 C11 O4 -174.6(4) . . . . ? C12 C10 C11 O4 -0.3(6) . . . . ? C9 C10 C11 C2 5.4(6) . . . . ? C12 C10 C11 C2 179.7(4) . . . . ? C3 C2 C11 O4 178.7(4) . . . . ? C1 C2 C11 O4 1.6(6) . . . . ? C3 C2 C11 C10 -1.3(6) . . . . ? C1 C2 C11 C10 -178.4(4) . . . . ? C11 C10 C12 C13 55.6(6) . . . . ? C9 C10 C12 C13 -130.2(5) . . . . ? C10 C12 C13 C14 69.2(6) . . . . ? C10 C12 C13 C19 -115.5(5) . . . . ? C19 C13 C14 O3 -178.4(4) . . . . ? C12 C13 C14 O3 -3.0(6) . . . . ? C19 C13 C14 C15 -0.1(6) . . . . ? C12 C13 C14 C15 175.4(4) . . . . ? O3 C14 C15 C17 178.4(4) . . . . ? C13 C14 C15 C17 0.1(6) . . . . ? O3 C14 C15 C16 -1.7(6) . . . . ? C13 C14 C15 C16 179.9(4) . . . . ? C17 C15 C16 O2 -13.8(6) . . . . ? C14 C15 C16 O2 166.4(4) . . . . ? C17 C15 C16 O1 165.2(4) . . . . ? C14 C15 C16 O1 -14.7(6) . . . . ? C14 C15 C17 C18 0.3(6) . . . . ? C16 C15 C17 C18 -179.6(4) . . . . ? C15 C17 C18 C19 -0.7(6) . . . . ? C15 C17 C18 C23 179.8(4) . . . . ? C17 C18 C19 C20 179.6(4) . . . . ? C23 C18 C19 C20 -0.9(6) . . . . ? C17 C18 C19 C13 0.7(6) . . . . ? C23 C18 C19 C13 -179.8(4) . . . . ? C14 C13 C19 C20 -179.2(4) . . . . ? C12 C13 C19 C20 5.6(6) . . . . ? C14 C13 C19 C18 -0.3(6) . . . . ? C12 C13 C19 C18 -175.6(4) . . . . ? C18 C19 C20 C21 0.5(7) . . . . ? C13 C19 C20 C21 179.3(5) . . . . ? C19 C20 C21 C22 -0.2(8) . . . . ? C20 C21 C22 C23 0.4(8) . . . . ? C21 C22 C23 C18 -0.8(7) . . . . ? C17 C18 C23 C22 -179.4(4) . . . . ? C19 C18 C23 C22 1.1(6) . . . . ? N1 C24 C25 N2 0.1(6) . . . . ? N2 C27 C28 C28 179.9(5) . . . 2_685 ? N2 C26 N1 C24 0.1(6) . . . . ? N2 C26 N1 Cd1 -176.2(3) . . . . ? C25 C24 N1 C26 -0.1(6) . . . . ? C25 C24 N1 Cd1 176.3(4) . . . . ? O5 Cd1 N1 C26 29.4(4) 2_665 . . . ? O6 Cd1 N1 C26 -154.2(4) 1_465 . . . ? O2 Cd1 N1 C26 116.0(4) . . . . ? O1 Cd1 N1 C26 -64.3(4) 2_575 . . . ? Cd1 Cd1 N1 C26 170.6(4) 2_575 . . . ? O5 Cd1 N1 C24 -146.1(4) 2_665 . . . ? O6 Cd1 N1 C24 30.3(4) 1_465 . . . ? O2 Cd1 N1 C24 -59.5(4) . . . . ? O1 Cd1 N1 C24 120.2(4) 2_575 . . . ? Cd1 Cd1 N1 C24 -5.0(8) 2_575 . . . ? N1 C26 N2 C25 0.0(6) . . . . ? N1 C26 N2 C27 -179.4(4) . . . . ? C24 C25 N2 C26 0.0(6) . . . . ? C24 C25 N2 C27 179.3(4) . . . . ? C28 C27 N2 C26 -109.2(5) . . . . ? C28 C27 N2 C25 71.6(6) . . . . ? O2 C16 O1 Cd1 14.3(6) . . . 2_575 ? C15 C16 O1 Cd1 -164.6(3) . . . 2_575 ? O1 C16 O2 Cd1 -10.2(8) . . . . ? C15 C16 O2 Cd1 168.7(3) . . . . ? N1 Cd1 O2 C16 171.4(5) . . . . ? O5 Cd1 O2 C16 -79.8(5) 2_665 . . . ? O6 Cd1 O2 C16 76.6(5) 1_465 . . . ? O1 Cd1 O2 C16 -8.0(7) 2_575 . . . ? Cd1 Cd1 O2 C16 0.9(5) 2_575 . . . ? O6 C1 O5 Cd1 -2.7(7) . . . 2_665 ? C2 C1 O5 Cd1 176.1(3) . . . 2_665 ? O5 C1 O6 Cd1 3.9(7) . . . 1_645 ? C2 C1 O6 Cd1 -174.9(3) . . . 1_645 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.647 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.105