# 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_r80209b _audit_creation_date 2013-05-14 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H18 Cd N2 O8, 0.5(C2 H6 O2), H2 O' _chemical_formula_sum 'C22 H23 Cd N2 O10' _chemical_formula_weight 587.82 _chemical_melting_point ? 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' Cd Cd -0.8075 1.2024 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 10.099(2) _cell_length_b 16.811(3) _cell_length_c 15.251(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.81(3) _cell_angle_gamma 90.00 _cell_volume 2571.0(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_T_max 0.9821 _exptl_absorpt_correction_T_min 0.9150 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1188 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_unetI/netI 0.1244 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14376 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.03 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3946 _reflns_number_total 4482 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.874 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.156 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 4482 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0733 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+42.7714P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1709 _refine_ls_wR_factor_ref 0.1761 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Others Fixed Sof: C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) O8(0.5) H8A(0.5) O9(0.5) H9A(0.5) 4.a Riding coordinates: O1(H1A,H1B), O8(H8A), O9(H9A), O10(H10A,H10B), O11(H11) 4.b Secondary CH2 refined with riding coordinates: C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B) 4.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C17(H17), C18(H18), C19(H19) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cd1 Cd 0.74744(6) 0.51744(3) 0.68121(4) 0.01545(19) Uani 1 1 d . . . C1 C 0.8603(9) 0.3663(5) 0.8050(6) 0.0267(19) Uani 1 1 d . . . H1 H 0.9372 0.3801 0.7806 0.032 Uiso 1 1 calc R . . C2 C 0.6425(9) 0.3910(5) 0.8222(6) 0.0280(19) Uani 1 1 d . . . H2 H 0.5663 0.4219 0.8097 0.034 Uiso 1 1 calc R . . C3 C 0.6374(10) 0.3252(5) 0.8784(6) 0.031(2) Uani 1 1 d . . . H3 H 0.5597 0.3136 0.9030 0.037 Uiso 1 1 calc R . . C4 C 0.8635(9) 0.2995(5) 0.8599(5) 0.0260(19) Uani 1 1 d . . . H4 H 0.9415 0.2701 0.8716 0.031 Uiso 1 1 calc R . . C5 C 0.7501(9) 0.2774(5) 0.8968(5) 0.0227(18) Uani 1 1 d . . . C6 C 0.7482(8) 0.2070(5) 0.9552(5) 0.0205(17) Uani 1 1 d . . . C7 C 0.6300(8) 0.1677(5) 0.9677(5) 0.0189(16) Uani 1 1 d . . . H7 H 0.5496 0.1833 0.9363 0.023 Uiso 1 1 calc R . . C8 C 0.8670(8) 0.1791(5) 1.0026(5) 0.0192(16) Uani 1 1 d . . . H8 H 0.9479 0.2030 0.9949 0.023 Uiso 1 1 calc R . . C9 C 0.8636(8) 0.1169(5) 1.0601(5) 0.0220(17) Uani 1 1 d . . . H9 H 0.9432 0.0991 1.0909 0.026 Uiso 1 1 calc R . . H10 H 0.558(10) 0.085(6) 1.039(6) 0.026 Uiso 1 1 d . . . C10 C 0.6337(8) 0.1056(5) 1.0269(5) 0.0195(17) Uani 1 1 d . . . C11 C 0.5039(8) 0.5631(5) 0.7283(5) 0.0189(16) Uani 1 1 d . . . C12 C 0.3802(7) 0.5980(4) 0.7578(5) 0.0157(15) Uani 1 1 d . . . C13 C 0.2536(8) 0.5659(4) 0.7314(5) 0.0144(15) Uani 1 1 d . . . C14 C 0.2397(8) 0.4927(5) 0.6758(5) 0.0204(17) Uani 1 1 d . . . C15 C 0.0028(8) 0.5723(5) 0.7309(5) 0.0212(17) Uani 1 1 d . . . C16 C 0.1398(8) 0.6033(5) 0.7578(5) 0.0190(16) Uani 1 1 d . . . C17 C 0.1547(8) 0.6724(5) 0.8088(5) 0.0209(17) Uani 1 1 d . . . H17 H 0.0798 0.6980 0.8252 0.025 Uiso 1 1 calc R . . C18 C 0.2828(8) 0.7035(5) 0.8356(6) 0.0239(18) Uani 1 1 d . . . H18 H 0.2924 0.7491 0.8704 0.029 Uiso 1 1 calc R . . C19 C 0.3932(8) 0.6666(5) 0.8105(5) 0.0216(17) Uani 1 1 d . . . H19 H 0.4776 0.6872 0.8285 0.026 Uiso 1 1 calc R . . C20 C 0.302(3) 0.0215(10) 0.4759(10) 0.041(6) Uani 0.50 1 d P . . H20A H 0.2677 -0.0259 0.4449 0.049 Uiso 0.50 1 calc PR . . H20B H 0.3732 0.0047 0.5204 0.049 Uiso 0.50 1 calc PR . . C21 C 0.1989(18) 0.0543(11) 0.5196(11) 0.030(4) Uani 0.50 1 d P . . H21A H 0.1679 0.0147 0.5587 0.036 Uiso 0.50 1 calc PR . . H21B H 0.1245 0.0688 0.4764 0.036 Uiso 0.50 1 calc PR . . C22 C 0.2636(10) 0.3526(5) 0.6734(6) 0.029(2) Uani 1 1 d . . . H22A H 0.3380 0.3524 0.6387 0.035 Uiso 1 1 calc R . . H22B H 0.1817 0.3477 0.6336 0.035 Uiso 1 1 calc R . . C23 C 0.2762(10) 0.2846(5) 0.7377(7) 0.034(2) Uani 1 1 d . . . H23A H 0.2925 0.2359 0.7068 0.041 Uiso 1 1 calc R . . H23B H 0.3518 0.2939 0.7820 0.041 Uiso 1 1 calc R . . N1 N 0.7479(7) 0.0802(4) 1.0738(4) 0.0204(14) Uani 1 1 d . . . N2 N 0.7510(7) 0.4111(4) 0.7862(4) 0.0214(15) Uani 1 1 d . . . O1 O 0.7114(6) 0.5936(3) 0.5503(4) 0.0278(14) Uani 1 1 d . . . H1A H 0.7372 0.6405 0.5403 0.033 Uiso 1 1 d R . . H1B H 0.7281 0.5645 0.5073 0.033 Uiso 1 1 d R . . O2 O 0.4968(6) 0.5097(3) 0.6711(4) 0.0211(12) Uani 1 1 d . . . O3 O 0.6161(6) 0.5904(3) 0.7640(4) 0.0248(13) Uani 1 1 d . . . O4 O 0.2627(5) 0.4257(3) 0.7232(3) 0.0181(11) Uani 1 1 d . . . O5 O 0.2122(6) 0.4927(3) 0.5960(3) 0.0213(12) Uani 1 1 d . . . O6 O -0.0120(6) 0.5017(3) 0.7056(4) 0.0253(13) Uani 1 1 d . . . O7 O -0.0960(6) 0.6188(4) 0.7323(5) 0.0342(15) Uani 1 1 d . . . O8 O 0.3597(14) 0.0722(8) 0.4133(7) 0.037(3) Uani 0.50 1 d P . . H8A H 0.3002 0.0896 0.3772 0.045 Uiso 0.50 1 d PR . . O9 O 0.2453(13) 0.1244(6) 0.5707(6) 0.024(3) Uani 0.50 1 d PU . . H9A H 0.3268 0.1272 0.5741 0.029 Uiso 0.50 1 d PR . . O10 O 0.2028(10) 0.2465(5) 0.9614(5) 0.063(3) Uani 1 1 d . . . H10A H 0.1797 0.2692 0.9029 0.076 Uiso 1 1 d R . . H10B H 0.2258 0.2926 1.0010 0.076 Uiso 1 1 d R . . O11 O 0.1594(7) 0.2760(4) 0.7797(4) 0.0360(16) Uani 1 1 d . . . H11 H 0.1247 0.2329 0.7663 0.043 Uiso 1 1 d 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 Cd1 0.0147(3) 0.0124(3) 0.0196(3) -0.0010(2) 0.0037(2) 0.0001(2) C1 0.024(5) 0.025(5) 0.033(5) 0.003(4) 0.012(4) 0.003(4) C2 0.024(5) 0.026(5) 0.035(5) 0.009(4) 0.007(4) 0.004(4) C3 0.031(5) 0.026(5) 0.037(5) 0.010(4) 0.013(4) 0.001(4) C4 0.018(4) 0.030(5) 0.030(4) 0.012(4) 0.005(4) 0.006(4) C5 0.030(5) 0.021(4) 0.017(4) 0.000(3) -0.001(3) -0.001(4) C6 0.025(4) 0.019(4) 0.018(4) -0.006(3) 0.003(3) 0.003(3) C7 0.016(4) 0.020(4) 0.020(4) -0.002(3) -0.002(3) -0.003(3) C8 0.012(4) 0.019(4) 0.028(4) 0.003(3) 0.009(3) 0.000(3) C9 0.020(4) 0.022(4) 0.025(4) 0.000(3) 0.006(3) -0.003(3) C10 0.013(4) 0.024(4) 0.022(4) -0.002(3) 0.003(3) 0.001(3) C11 0.015(4) 0.018(4) 0.026(4) 0.004(3) 0.008(3) 0.000(3) C12 0.012(4) 0.014(4) 0.021(4) 0.003(3) 0.004(3) -0.002(3) C13 0.017(4) 0.014(4) 0.013(3) 0.000(3) 0.005(3) 0.000(3) C14 0.021(4) 0.013(4) 0.028(4) -0.002(3) 0.005(3) -0.002(3) C15 0.020(4) 0.020(4) 0.024(4) -0.003(3) 0.004(3) -0.001(3) C16 0.014(4) 0.022(4) 0.022(4) 0.000(3) 0.007(3) 0.000(3) C17 0.012(4) 0.020(4) 0.032(4) -0.009(3) 0.010(3) 0.000(3) C18 0.015(4) 0.024(4) 0.033(4) -0.008(4) 0.003(4) -0.005(3) C19 0.018(4) 0.021(4) 0.027(4) -0.004(3) 0.008(3) -0.003(3) C20 0.111(19) 0.008(8) 0.005(7) 0.003(6) 0.010(9) 0.014(10) C21 0.031(10) 0.030(10) 0.024(8) 0.002(7) -0.022(8) 0.012(8) C22 0.034(5) 0.022(4) 0.032(5) -0.007(4) 0.008(4) -0.003(4) C23 0.033(5) 0.020(5) 0.050(6) 0.004(4) 0.010(4) 0.003(4) N1 0.024(4) 0.018(3) 0.018(3) 0.002(3) 0.000(3) 0.001(3) N2 0.028(4) 0.013(3) 0.024(3) 0.003(3) 0.006(3) 0.004(3) O1 0.043(4) 0.022(3) 0.020(3) 0.002(2) 0.011(3) -0.001(3) O2 0.022(3) 0.017(3) 0.025(3) -0.002(2) 0.008(2) 0.005(2) O3 0.015(3) 0.024(3) 0.036(3) -0.008(2) 0.006(2) -0.003(2) O4 0.026(3) 0.010(3) 0.019(3) 0.000(2) 0.008(2) 0.000(2) O5 0.026(3) 0.024(3) 0.014(3) -0.002(2) 0.002(2) -0.003(2) O6 0.023(3) 0.021(3) 0.033(3) -0.004(2) 0.005(3) -0.002(2) O7 0.016(3) 0.026(3) 0.061(4) -0.014(3) 0.003(3) -0.003(3) O8 0.040(8) 0.055(9) 0.016(6) 0.002(6) 0.003(5) -0.016(7) O9 0.057(8) 0.007(5) 0.004(4) 0.001(4) -0.009(5) 0.004(5) O10 0.110(8) 0.034(4) 0.043(4) -0.001(3) -0.001(5) -0.002(5) O11 0.037(4) 0.023(3) 0.051(4) -0.001(3) 0.016(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 C11 2.753(8) . ? Cd1 C15 2.760(8) 1_655 ? Cd1 N1 2.319(6) 4_565 ? Cd1 N2 2.397(6) . ? Cd1 O1 2.363(6) . ? Cd1 O2 2.521(6) . ? Cd1 O3 2.292(6) . ? Cd1 O6 2.429(6) 1_655 ? Cd1 O7 2.392(6) 1_655 ? C1 H1 0.9300 . ? C1 C4 1.398(12) . ? C1 N2 1.340(11) . ? C2 H2 0.9300 . ? C2 C3 1.404(12) . ? C2 N2 1.327(11) . ? C3 H3 0.9300 . ? C3 C5 1.394(12) . ? C4 H4 0.9300 . ? C4 C5 1.385(12) . ? C5 C6 1.483(11) . ? C6 C7 1.397(11) . ? C6 C8 1.405(11) . ? C7 H7 0.9300 . ? C7 C10 1.379(11) . ? C8 H8 0.9300 . ? C8 C9 1.368(11) . ? C9 H9 0.9300 . ? C9 N1 1.359(11) . ? C10 H10 0.87(10) . ? C10 N1 1.353(10) . ? C11 C12 1.496(11) . ? C11 O2 1.249(10) . ? C11 O3 1.282(10) . ? C12 C13 1.401(10) . ? C12 C19 1.403(11) . ? C13 C14 1.493(10) . ? C13 C16 1.409(11) . ? C14 O4 1.344(9) . ? C14 O5 1.216(10) . ? C15 Cd1 2.760(8) 1_455 ? C15 C16 1.489(11) . ? C15 O6 1.253(10) . ? C15 O7 1.270(10) . ? C16 C17 1.397(11) . ? C17 H17 0.9300 . ? C17 C18 1.410(11) . ? C18 H18 0.9300 . ? C18 C19 1.370(11) . ? C19 H19 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.41(3) . ? C20 O8 1.45(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 O9 1.46(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.502(12) . ? C22 O4 1.444(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 O11 1.415(11) . ? N1 Cd1 2.319(6) 4_566 ? O1 H1A 0.8509 . ? O1 H1B 0.8497 . ? O6 Cd1 2.429(6) 1_455 ? O7 Cd1 2.392(6) 1_455 ? O8 H8A 0.8201 . ? O9 H9A 0.8201 . ? O10 H10A 0.9729 . ? O10 H10B 0.9928 . ? O11 H11 0.8201 . ? 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 C11 Cd1 C15 132.1(2) . 1_655 ? N1 Cd1 C11 117.3(2) 4_565 . ? N1 Cd1 C15 110.5(2) 4_565 1_655 ? N1 Cd1 N2 86.7(2) 4_565 . ? N1 Cd1 O1 78.4(2) 4_565 . ? N1 Cd1 O2 90.4(2) 4_565 . ? N1 Cd1 O6 86.8(2) 4_565 1_655 ? N1 Cd1 O7 132.7(2) 4_565 1_655 ? N2 Cd1 C11 88.7(2) . . ? N2 Cd1 C15 97.3(2) . 1_655 ? N2 Cd1 O2 86.4(2) . . ? N2 Cd1 O6 83.2(2) . 1_655 ? O1 Cd1 C11 91.0(2) . . ? O1 Cd1 C15 95.5(2) . 1_655 ? O1 Cd1 N2 163.1(2) . . ? O1 Cd1 O2 85.6(2) . . ? O1 Cd1 O6 103.9(2) . 1_655 ? O1 Cd1 O7 85.3(2) . 1_655 ? O2 Cd1 C11 26.9(2) . . ? O2 Cd1 C15 158.9(2) . 1_655 ? O3 Cd1 C11 27.6(2) . . ? O3 Cd1 C15 104.7(2) . 1_655 ? O3 Cd1 N1 144.8(2) . 4_565 ? O3 Cd1 N2 89.7(2) . . ? O3 Cd1 O1 97.7(2) . . ? O3 Cd1 O2 54.48(19) . . ? O3 Cd1 O6 127.4(2) . 1_655 ? O3 Cd1 O7 80.9(2) . 1_655 ? O6 Cd1 C11 154.1(2) 1_655 . ? O6 Cd1 C15 27.0(2) 1_655 1_655 ? O6 Cd1 O2 169.35(19) 1_655 . ? O7 Cd1 C11 107.0(2) 1_655 . ? O7 Cd1 C15 27.4(2) 1_655 1_655 ? O7 Cd1 N2 110.9(2) 1_655 . ? O7 Cd1 O2 132.61(19) 1_655 . ? O7 Cd1 O6 54.4(2) 1_655 1_655 ? C4 C1 H1 118.6 . . ? N2 C1 H1 118.6 . . ? N2 C1 C4 122.7(8) . . ? C3 C2 H2 118.4 . . ? N2 C2 H2 118.4 . . ? N2 C2 C3 123.1(8) . . ? C2 C3 H3 120.4 . . ? C5 C3 C2 119.2(8) . . ? C5 C3 H3 120.4 . . ? C1 C4 H4 120.1 . . ? C5 C4 C1 119.8(8) . . ? C5 C4 H4 120.1 . . ? C3 C5 C6 120.8(8) . . ? C4 C5 C3 117.3(8) . . ? C4 C5 C6 121.9(8) . . ? C7 C6 C5 122.1(7) . . ? C7 C6 C8 117.6(7) . . ? C8 C6 C5 120.3(7) . . ? C6 C7 H7 120.3 . . ? C10 C7 C6 119.4(8) . . ? C10 C7 H7 120.3 . . ? C6 C8 H8 120.0 . . ? C9 C8 C6 120.0(8) . . ? C9 C8 H8 120.0 . . ? C8 C9 H9 118.9 . . ? N1 C9 C8 122.2(8) . . ? N1 C9 H9 118.9 . . ? C7 C10 H10 119(6) . . ? N1 C10 C7 122.7(8) . . ? N1 C10 H10 118(6) . . ? C12 C11 Cd1 172.5(6) . . ? O2 C11 Cd1 66.1(4) . . ? O2 C11 C12 120.8(7) . . ? O2 C11 O3 121.8(7) . . ? O3 C11 Cd1 55.8(4) . . ? O3 C11 C12 117.4(7) . . ? C13 C12 C11 121.9(7) . . ? C13 C12 C19 120.1(7) . . ? C19 C12 C11 118.0(7) . . ? C12 C13 C14 120.1(7) . . ? C12 C13 C16 119.6(7) . . ? C16 C13 C14 120.3(7) . . ? O4 C14 C13 112.8(7) . . ? O5 C14 C13 124.3(7) . . ? O5 C14 O4 122.9(7) . . ? C16 C15 Cd1 179.1(6) . 1_455 ? O6 C15 Cd1 61.6(4) . 1_455 ? O6 C15 C16 119.3(7) . . ? O6 C15 O7 121.6(8) . . ? O7 C15 Cd1 60.0(4) . 1_455 ? O7 C15 C16 119.1(7) . . ? C13 C16 C15 121.9(7) . . ? C17 C16 C13 119.5(7) . . ? C17 C16 C15 118.6(7) . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.3(7) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.0(8) . . ? C19 C18 H18 120.0 . . ? C12 C19 H19 119.7 . . ? C18 C19 C12 120.6(8) . . ? C18 C19 H19 119.7 . . ? H20A C20 H20B 107.3 . . ? C21 C20 H20A 108.0 . . ? C21 C20 H20B 108.0 . . ? C21 C20 O8 117.2(15) . . ? O8 C20 H20A 108.0 . . ? O8 C20 H20B 108.0 . . ? C20 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C20 C21 O9 111.0(16) . . ? H21A C21 H21B 108.0 . . ? O9 C21 H21A 109.4 . . ? O9 C21 H21B 109.4 . . ? H22A C22 H22B 108.4 . . ? C23 C22 H22A 110.1 . . ? C23 C22 H22B 110.1 . . ? O4 C22 H22A 110.1 . . ? O4 C22 H22B 110.1 . . ? O4 C22 C23 108.0(7) . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O11 C23 C22 111.3(8) . . ? O11 C23 H23A 109.4 . . ? O11 C23 H23B 109.4 . . ? C9 N1 Cd1 120.3(5) . 4_566 ? C10 N1 Cd1 121.6(5) . 4_566 ? C10 N1 C9 118.0(7) . . ? C1 N2 Cd1 120.7(5) . . ? C2 N2 Cd1 121.3(5) . . ? C2 N2 C1 117.8(7) . . ? Cd1 O1 H1A 129.3 . . ? Cd1 O1 H1B 108.3 . . ? H1A O1 H1B 107.7 . . ? C11 O2 Cd1 86.9(5) . . ? C11 O3 Cd1 96.6(5) . . ? C14 O4 C22 116.2(6) . . ? C15 O6 Cd1 91.4(5) . 1_455 ? C15 O7 Cd1 92.7(5) . 1_455 ? C20 O8 H8A 109.5 . . ? C21 O9 H9A 109.7 . . ? H10A O10 H10B 105.4 . . ? C23 O11 H11 109.5 . . ? 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 Cd1 C11 C12 C13 164(4) . . . . ? Cd1 C11 C12 C19 -14(4) . . . . ? Cd1 C15 C16 C13 -152(35) 1_455 . . . ? Cd1 C15 C16 C17 26(36) 1_455 . . . ? C1 C4 C5 C3 -1.5(13) . . . . ? C1 C4 C5 C6 179.8(8) . . . . ? C2 C3 C5 C4 1.8(13) . . . . ? C2 C3 C5 C6 -179.4(8) . . . . ? C3 C2 N2 Cd1 174.7(7) . . . . ? C3 C2 N2 C1 -0.2(13) . . . . ? C3 C5 C6 C7 24.2(12) . . . . ? C3 C5 C6 C8 -153.5(8) . . . . ? C4 C1 N2 Cd1 -174.4(7) . . . . ? C4 C1 N2 C2 0.6(13) . . . . ? C4 C5 C6 C7 -157.1(8) . . . . ? C4 C5 C6 C8 25.2(12) . . . . ? C5 C6 C7 C10 -176.0(7) . . . . ? C5 C6 C8 C9 176.3(7) . . . . ? C6 C7 C10 N1 -0.4(12) . . . . ? C6 C8 C9 N1 -0.2(12) . . . . ? C7 C6 C8 C9 -1.5(11) . . . . ? C7 C10 N1 Cd1 174.8(6) . . . 4_566 ? C7 C10 N1 C9 -1.3(12) . . . . ? C8 C6 C7 C10 1.8(11) . . . . ? C8 C9 N1 Cd1 -174.6(6) . . . 4_566 ? C8 C9 N1 C10 1.6(12) . . . . ? C11 Cd1 N2 C1 -172.2(6) . . . . ? C11 Cd1 N2 C2 13.0(7) . . . . ? C11 C12 C13 C14 2.9(11) . . . . ? C11 C12 C13 C16 -177.1(7) . . . . ? C11 C12 C19 C18 176.6(7) . . . . ? C12 C11 O2 Cd1 176.6(6) . . . . ? C12 C11 O3 Cd1 -176.3(6) . . . . ? C12 C13 C14 O4 81.4(9) . . . . ? C12 C13 C14 O5 -97.8(10) . . . . ? C12 C13 C16 C15 179.3(7) . . . . ? C12 C13 C16 C17 0.9(11) . . . . ? C13 C12 C19 C18 -0.9(12) . . . . ? C13 C14 O4 C22 -174.4(7) . . . . ? C13 C16 C17 C18 -1.6(12) . . . . ? C14 C13 C16 C15 -0.7(11) . . . . ? C14 C13 C16 C17 -179.1(7) . . . . ? C15 Cd1 C11 C12 20(4) 1_655 . . . ? C15 Cd1 C11 O2 176.7(4) 1_655 . . . ? C15 Cd1 C11 O3 -6.7(6) 1_655 . . . ? C15 Cd1 N2 C1 -39.9(7) 1_655 . . . ? C15 Cd1 N2 C2 145.3(7) 1_655 . . . ? C15 Cd1 O2 C11 -6.9(8) 1_655 . . . ? C15 Cd1 O3 C11 174.9(5) 1_655 . . . ? C15 C16 C17 C18 180.0(8) . . . . ? C16 C13 C14 O4 -98.6(9) . . . . ? C16 C13 C14 O5 82.2(10) . . . . ? C16 C15 O6 Cd1 -179.9(6) . . . 1_455 ? C16 C15 O7 Cd1 179.9(6) . . . 1_455 ? C16 C17 C18 C19 1.0(13) . . . . ? C17 C18 C19 C12 0.2(13) . . . . ? C19 C12 C13 C14 -179.7(7) . . . . ? C19 C12 C13 C16 0.3(11) . . . . ? C23 C22 O4 C14 -174.1(7) . . . . ? N1 Cd1 C11 C12 -156(4) 4_565 . . . ? N1 Cd1 C11 O2 0.9(5) 4_565 . . . ? N1 Cd1 C11 O3 177.5(4) 4_565 . . . ? N1 Cd1 N2 C1 70.4(6) 4_565 . . . ? N1 Cd1 N2 C2 -104.4(7) 4_565 . . . ? N1 Cd1 O2 C11 -179.2(5) 4_565 . . . ? N1 Cd1 O3 C11 -3.8(7) 4_565 . . . ? N2 Cd1 C11 C12 118(4) . . . . ? N2 Cd1 C11 O2 -84.7(5) . . . . ? N2 Cd1 C11 O3 91.9(5) . . . . ? N2 Cd1 O2 C11 94.1(5) . . . . ? N2 Cd1 O3 C11 -87.7(5) . . . . ? N2 C1 C4 C5 0.3(14) . . . . ? N2 C2 C3 C5 -1.0(14) . . . . ? O1 Cd1 C11 C12 -79(4) . . . . ? O1 Cd1 C11 O2 78.4(4) . . . . ? O1 Cd1 C11 O3 -105.0(5) . . . . ? O1 Cd1 N2 C1 98.9(10) . . . . ? O1 Cd1 N2 C2 -75.9(10) . . . . ? O1 Cd1 O2 C11 -100.8(5) . . . . ? O1 Cd1 O3 C11 77.1(5) . . . . ? O2 Cd1 C11 C12 -157(4) . . . . ? O2 Cd1 C11 O3 176.6(8) . . . . ? O2 Cd1 N2 C1 160.9(6) . . . . ? O2 Cd1 N2 C2 -13.9(7) . . . . ? O2 Cd1 O3 C11 -1.9(4) . . . . ? O2 C11 C12 C13 8.2(11) . . . . ? O2 C11 C12 C19 -169.3(7) . . . . ? O2 C11 O3 Cd1 3.6(8) . . . . ? O3 Cd1 C11 C12 26(4) . . . . ? O3 Cd1 C11 O2 -176.6(8) . . . . ? O3 Cd1 N2 C1 -144.6(6) . . . . ? O3 Cd1 N2 C2 40.6(7) . . . . ? O3 Cd1 O2 C11 1.9(4) . . . . ? O3 C11 C12 C13 -171.9(7) . . . . ? O3 C11 C12 C19 10.6(11) . . . . ? O3 C11 O2 Cd1 -3.3(7) . . . . ? O4 C22 C23 O11 68.8(10) . . . . ? O5 C14 O4 C22 4.8(11) . . . . ? O6 Cd1 C11 C12 47(4) 1_655 . . . ? O6 Cd1 C11 O2 -156.0(4) 1_655 . . . ? O6 Cd1 C11 O3 20.6(8) 1_655 . . . ? O6 Cd1 N2 C1 -16.9(6) 1_655 . . . ? O6 Cd1 N2 C2 168.4(7) 1_655 . . . ? O6 Cd1 O2 C11 106.1(10) 1_655 . . . ? O6 Cd1 O3 C11 -168.8(4) 1_655 . . . ? O6 C15 C16 C13 19.8(12) . . . . ? O6 C15 C16 C17 -161.9(8) . . . . ? O6 C15 O7 Cd1 1.5(8) . . . 1_455 ? O7 Cd1 C11 C12 7(4) 1_655 . . . ? O7 Cd1 C11 O2 163.8(4) 1_655 . . . ? O7 Cd1 C11 O3 -19.6(5) 1_655 . . . ? O7 Cd1 N2 C1 -64.5(7) 1_655 . . . ? O7 Cd1 N2 C2 120.8(6) 1_655 . . . ? O7 Cd1 O2 C11 -21.3(6) 1_655 . . . ? O7 Cd1 O3 C11 161.1(5) 1_655 . . . ? O7 C15 C16 C13 -158.7(8) . . . . ? O7 C15 C16 C17 19.7(12) . . . . ? O7 C15 O6 Cd1 -1.4(8) . . . 1_455 ? O8 C20 C21 O9 -60(2) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 939638' ####################################################################### # # 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_c090213l _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H53 Cd6 N9 O29.50' _chemical_formula_weight 2322.74 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' Cd Cd -0.8075 1.2024 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5925(10) _cell_length_b 19.4409(18) _cell_length_c 23.682(2) _cell_angle_alpha 73.7440(10) _cell_angle_beta 83.661(2) _cell_angle_gamma 89.712(2) _cell_volume 4651.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2276 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28772 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 16243 _reflns_number_gt 12788 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+30.3027P] 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 16243 _refine_ls_number_parameters 1181 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1997 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Cd1 Cd 0.24644(6) 0.45473(4) 0.22671(3) 0.02463(18) Uani 1 1 d . . . Cd3 Cd 0.69694(7) 0.15655(4) 0.25871(3) 0.02577(18) Uani 1 1 d . . . Cd2 Cd 1.08562(7) -0.34242(4) 0.25296(3) 0.02547(18) Uani 1 1 d . . . Cd4 Cd 0.67852(7) -0.28748(4) 0.26708(3) 0.02701(18) Uani 1 1 d . . . Cd5 Cd 0.54994(6) -0.04090(4) 0.23950(3) 0.02612(18) Uani 1 1 d . . . Cd6 Cd 1.10640(7) 0.22381(4) 0.24030(3) 0.02983(19) Uani 1 1 d . . . C1 C 0.4831(9) 0.8327(5) 0.2093(4) 0.030(2) Uani 1 1 d . . . C2 C 0.4458(8) 0.7851(5) 0.1732(4) 0.0235(19) Uani 1 1 d . . . C6 C 0.3824(8) 0.6711(5) 0.1638(4) 0.023(2) Uani 1 1 d . . . C7 C 0.4027(9) 0.7144(5) 0.1993(4) 0.027(2) Uani 1 1 d . . . C8 C 0.3331(9) 0.5957(5) 0.1896(4) 0.028(2) Uani 1 1 d . . . C9 C 0.3813(9) 0.6854(5) 0.2654(4) 0.027(2) Uani 1 1 d . . . C10 C 0.3383(9) 0.3425(5) 0.1844(4) 0.028(2) Uani 1 1 d . . . C11 C 0.4000(8) 0.2914(5) 0.1536(4) 0.0234(19) Uani 1 1 d . . . C15 C 0.4719(9) 0.1750(5) 0.1526(4) 0.024(2) Uani 1 1 d . . . C16 C 0.4244(9) 0.2222(5) 0.1840(4) 0.026(2) Uani 1 1 d . . . C17 C 0.4002(9) 0.1966(5) 0.2504(4) 0.026(2) Uani 1 1 d . . . C18 C 0.4990(9) 0.0987(6) 0.1834(4) 0.033(2) Uani 1 1 d . . . C19 C 0.8330(10) 0.5649(5) 0.2537(4) 0.031(2) Uani 1 1 d . . . C20 C 0.7782(9) 0.4971(5) 0.2474(4) 0.030(2) Uani 1 1 d . . . C21 C 0.6463(11) 0.4910(7) 0.2511(5) 0.047(3) Uani 1 1 d . . . H21 H 0.5970 0.5291 0.2559 0.056 Uiso 1 1 calc R . . C22 C 0.5876(10) 0.4293(7) 0.2478(6) 0.052(3) Uani 1 1 d . . . H22 H 0.4999 0.4268 0.2481 0.063 Uiso 1 1 calc R . . C23 C 0.6600(10) 0.3716(6) 0.2442(5) 0.041(3) Uani 1 1 d . . . H23 H 0.6198 0.3291 0.2445 0.050 Uiso 1 1 calc R . . C24 C 0.7922(9) 0.3752(5) 0.2400(4) 0.028(2) Uani 1 1 d . . . C25 C 0.8520(9) 0.4405(5) 0.2388(4) 0.024(2) Uani 1 1 d . . . C26 C 0.9938(9) 0.4460(5) 0.2333(4) 0.027(2) Uani 1 1 d . . . C27 C 0.8646(10) 0.3091(5) 0.2416(4) 0.030(2) Uani 1 1 d . . . C28 C 0.9523(11) 0.0649(5) 0.2597(4) 0.033(2) Uani 1 1 d . . . C29 C 1.0083(10) -0.0056(5) 0.2589(5) 0.035(2) Uani 1 1 d . . . C30 C 1.1394(12) -0.0114(8) 0.2569(7) 0.068(4) Uani 1 1 d . . . H30 H 1.1887 0.0287 0.2554 0.082 Uiso 1 1 calc R . . C31 C 1.1957(13) -0.0718(10) 0.2572(9) 0.092(6) Uani 1 1 d . . . H31 H 1.2838 -0.0735 0.2553 0.111 Uiso 1 1 calc R . . C32 C 1.1256(12) -0.1333(7) 0.2604(7) 0.065(4) Uani 1 1 d . . . H32 H 1.1659 -0.1764 0.2627 0.078 Uiso 1 1 calc R . . C33 C 0.9940(10) -0.1297(6) 0.2601(5) 0.035(2) Uani 1 1 d . . . C34 C 0.9357(9) -0.0651(5) 0.2590(4) 0.028(2) Uani 1 1 d . . . C35 C 0.7960(9) -0.0597(5) 0.2578(4) 0.028(2) Uani 1 1 d . . . C36 C 0.9215(11) -0.1971(5) 0.2629(4) 0.033(2) Uani 1 1 d . . . C37 C 0.3432(12) 0.4685(7) 0.3494(5) 0.049(3) Uani 1 1 d . . . H37 H 0.3621 0.5155 0.3269 0.059 Uiso 1 1 calc R . . C38 C 0.3569(12) 0.4506(6) 0.4088(5) 0.050(3) Uani 1 1 d . . . H38 H 0.3853 0.4848 0.4255 0.060 Uiso 1 1 calc R . . C39 C 0.3279(12) 0.3808(7) 0.4435(5) 0.051(3) Uani 1 1 d . . . C40 C 0.2908(15) 0.3337(7) 0.4136(5) 0.065(4) Uani 1 1 d . . . H40 H 0.2725 0.2859 0.4340 0.079 Uiso 1 1 calc R . . C41 C 0.2811(13) 0.3566(7) 0.3551(5) 0.057(4) Uani 1 1 d . . . H41 H 0.2559 0.3235 0.3365 0.069 Uiso 1 1 calc R . . C42 C 0.3341(14) 0.3881(7) 0.6004(5) 0.059(4) Uani 1 1 d . . . H42 H 0.3406 0.4227 0.6203 0.071 Uiso 1 1 calc R . . C43 C 0.3324(13) 0.4098(7) 0.5397(5) 0.056(3) Uani 1 1 d . . . H43 H 0.3330 0.4583 0.5196 0.068 Uiso 1 1 calc R . . C44 C 0.3300(12) 0.3589(7) 0.5092(5) 0.048(3) Uani 1 1 d . . . C45 C 0.3270(14) 0.2894(6) 0.5414(5) 0.057(4) Uani 1 1 d . . . H45 H 0.3269 0.2537 0.5222 0.068 Uiso 1 1 calc R . . C46 C 0.3243(13) 0.2706(7) 0.6019(5) 0.054(3) Uani 1 1 d . . . H46 H 0.3206 0.2222 0.6227 0.065 Uiso 1 1 calc R . . C47 C 0.5688(13) 0.1222(6) 0.6332(5) 0.051(3) Uani 1 1 d . . . H47 H 0.5578 0.1603 0.6496 0.061 Uiso 1 1 calc R . . C48 C 0.5956(14) 0.1377(7) 0.5727(5) 0.057(4) Uani 1 1 d . . . H48 H 0.5997 0.1851 0.5495 0.068 Uiso 1 1 calc R . . C49 C 0.6163(11) 0.0829(6) 0.5466(4) 0.040(3) Uani 1 1 d . . . C50 C 0.6090(12) 0.0157(6) 0.5853(5) 0.050(3) Uani 1 1 d . . . H50 H 0.6243 -0.0236 0.5707 0.060 Uiso 1 1 calc R . . C51 C 0.5797(11) 0.0049(6) 0.6449(5) 0.042(3) Uani 1 1 d . . . H51 H 0.5750 -0.0418 0.6695 0.051 Uiso 1 1 calc R . . C52 C 0.6160(16) 0.1708(8) 0.3860(5) 0.070(4) Uani 1 1 d . . . H52 H 0.5894 0.2139 0.3624 0.084 Uiso 1 1 calc R . . C53 C 0.6002(17) 0.1595(7) 0.4460(5) 0.076(5) Uani 1 1 d . . . H53 H 0.5649 0.1950 0.4618 0.091 Uiso 1 1 calc R . . C54 C 0.6358(11) 0.0962(6) 0.4835(4) 0.038(3) Uani 1 1 d . . . C55 C 0.6875(13) 0.0486(7) 0.4558(5) 0.055(3) Uani 1 1 d . . . H55 H 0.7137 0.0047 0.4784 0.066 Uiso 1 1 calc R . . C56 C 0.7018(12) 0.0637(6) 0.3952(5) 0.048(3) Uani 1 1 d . . . H56 H 0.7382 0.0294 0.3784 0.058 Uiso 1 1 calc R . . C57 C 1.0253(13) -0.3697(6) 0.3918(5) 0.052(3) Uani 1 1 d . . . H57 H 1.0229 -0.3200 0.3811 0.062 Uiso 1 1 calc R . . C58 C 1.0100(13) -0.4069(6) 0.4509(5) 0.053(3) Uani 1 1 d . . . H58 H 0.9997 -0.3818 0.4792 0.064 Uiso 1 1 calc R . . C59 C 1.0099(10) -0.4796(6) 0.4687(4) 0.035(2) Uani 1 1 d . . . C60 C 1.0239(13) -0.5127(6) 0.4246(4) 0.048(3) Uani 1 1 d . . . H60 H 1.0235 -0.5625 0.4340 0.058 Uiso 1 1 calc R . . C61 C 1.0387(13) -0.4730(6) 0.3669(5) 0.051(3) Uani 1 1 d . . . H61 H 1.0461 -0.4969 0.3378 0.061 Uiso 1 1 calc R . . C62 C 0.7797(10) -0.2124(6) 0.1303(5) 0.039(3) Uani 1 1 d . . . H62 H 0.7970 -0.1753 0.1462 0.047 Uiso 1 1 calc R . . C63 C 0.8107(10) -0.2018(6) 0.0703(5) 0.039(3) Uani 1 1 d . . . H63 H 0.8430 -0.1575 0.0466 0.047 Uiso 1 1 calc R . . C64 C 0.7942(9) -0.2563(7) 0.0457(5) 0.039(3) Uani 1 1 d . . . C65 C 0.7395(11) -0.3186(6) 0.0836(5) 0.042(3) Uani 1 1 d . . . H65 H 0.7240 -0.3570 0.0688 0.051 Uiso 1 1 calc R . . C66 C 0.7078(10) -0.3252(6) 0.1419(4) 0.034(2) Uani 1 1 d . . . H66 H 0.6714 -0.3683 0.1661 0.041 Uiso 1 1 calc R . . C67 C 0.8280(10) -0.2466(6) -0.0180(4) 0.038(3) Uani 1 1 d . . . C68 C 0.8191(11) -0.1830(6) -0.0593(5) 0.045(3) Uani 1 1 d . . . H68 H 0.7982 -0.1423 -0.0474 0.054 Uiso 1 1 calc R . . C69 C 0.8407(10) -0.1782(7) -0.1182(5) 0.046(3) Uani 1 1 d . . . H69 H 0.8300 -0.1340 -0.1452 0.055 Uiso 1 1 calc R . . C70 C 0.8873(10) -0.2943(6) -0.0993(5) 0.040(3) Uani 1 1 d . . . H70 H 0.9119 -0.3335 -0.1128 0.048 Uiso 1 1 calc R . . C71 C 0.8657(10) -0.3049(6) -0.0396(5) 0.041(3) Uani 1 1 d . . . H71 H 0.8758 -0.3498 -0.0136 0.049 Uiso 1 1 calc R . . C72 C 0.7587(11) 0.2623(6) 0.1254(4) 0.038(3) Uani 1 1 d . . . H72 H 0.7306 0.2966 0.1441 0.045 Uiso 1 1 calc R . . C73 C 0.7921(10) 0.2838(6) 0.0652(5) 0.041(3) Uani 1 1 d . . . H73 H 0.7880 0.3318 0.0440 0.049 Uiso 1 1 calc R . . C74 C 0.8326(9) 0.2325(6) 0.0359(4) 0.032(2) Uani 1 1 d . . . C75 C 0.8392(10) 0.1632(6) 0.0705(4) 0.037(2) Uani 1 1 d . . . H75 H 0.8686 0.1275 0.0536 0.045 Uiso 1 1 calc R . . C76 C 0.8025(10) 0.1471(6) 0.1296(4) 0.039(3) Uani 1 1 d . . . H76 H 0.8037 0.0994 0.1518 0.047 Uiso 1 1 calc R . . C77 C 0.9196(10) 0.3414(6) -0.1206(5) 0.038(3) Uani 1 1 d . . . H77 H 0.9430 0.3886 -0.1411 0.045 Uiso 1 1 calc R . . C78 C 0.8990(9) 0.3238(6) -0.0609(4) 0.034(2) Uani 1 1 d . . . H78 H 0.9085 0.3585 -0.0414 0.041 Uiso 1 1 calc R . . C79 C 0.8634(9) 0.2533(6) -0.0284(4) 0.033(2) Uani 1 1 d . . . C80 C 0.8552(10) 0.2045(6) -0.0601(4) 0.036(2) Uani 1 1 d . . . H80 H 0.8349 0.1566 -0.0407 0.044 Uiso 1 1 calc R . . C81 C 0.8777(10) 0.2275(6) -0.1219(4) 0.038(3) Uani 1 1 d . . . H81 H 0.8710 0.1941 -0.1429 0.045 Uiso 1 1 calc R . . C87 C 1.0277(18) 0.1624(12) 0.3899(7) 0.113(7) Uani 1 1 d . . . H87A H 0.9442 0.1424 0.3895 0.135 Uiso 1 1 calc R . . H87B H 1.0258 0.1787 0.4251 0.135 Uiso 1 1 calc R . . C88 C 1.122(2) 0.1063(13) 0.3927(9) 0.121(5) Uani 1 1 d U . . H88A H 1.0994 0.0663 0.4276 0.145 Uiso 1 1 calc R . . H88B H 1.1236 0.0888 0.3581 0.145 Uiso 1 1 calc R . . N1 N 0.3051(8) 0.4231(5) 0.3226(3) 0.037(2) Uani 1 1 d . . . N2 N 0.3266(9) 0.3190(5) 0.6313(4) 0.041(2) Uani 1 1 d . . . N3 N 0.5580(8) 0.0577(5) 0.6688(3) 0.0322(19) Uani 1 1 d . . . N4 N 0.6673(9) 0.1236(5) 0.3597(4) 0.042(2) Uani 1 1 d . . . N5 N 0.7647(8) 0.1958(5) 0.1576(3) 0.033(2) Uani 1 1 d . . . N6 N 0.9078(8) 0.2944(5) -0.1515(3) 0.034(2) Uani 1 1 d . . . N7 N 0.7268(8) -0.2723(5) 0.1663(4) 0.036(2) Uani 1 1 d . . . N8 N 0.8759(9) -0.2326(5) -0.1394(4) 0.040(2) Uani 1 1 d . . . N9 N 1.0429(8) -0.4022(5) 0.3503(4) 0.0334(19) Uani 1 1 d . . . O1 O 0.5322(7) 0.8074(4) 0.2552(3) 0.0379(17) Uani 1 1 d . . . O2 O 0.4636(8) 0.8973(4) 0.1887(3) 0.048(2) Uani 1 1 d . . . O3 O 0.2730(7) 0.6933(4) 0.2900(3) 0.0375(17) Uani 1 1 d . . . O4 O 0.4724(7) 0.6549(4) 0.2908(3) 0.0356(17) Uani 1 1 d . . . O5 O 0.2452(7) 0.5818(4) 0.2321(3) 0.0335(16) Uani 1 1 d . . . O6 O 0.3758(8) 0.5498(4) 0.1682(4) 0.058(2) Uani 1 1 d . . . O7 O 0.3696(8) 0.4058(4) 0.1648(3) 0.047(2) Uani 1 1 d . . . O8 O 0.2554(7) 0.3198(4) 0.2286(3) 0.0386(17) Uani 1 1 d . . . O9 O 0.2951(7) 0.1695(4) 0.2734(3) 0.0369(17) Uani 1 1 d . . . O10 O 0.4907(7) 0.2033(4) 0.2781(3) 0.0398(18) Uani 1 1 d . . . O11 O 0.5532(6) 0.0856(4) 0.2303(3) 0.0318(16) Uani 1 1 d . . . O12 O 0.4678(10) 0.0507(4) 0.1630(4) 0.061(3) Uani 1 1 d . . . O13 O 0.8352(7) 0.0683(4) 0.2651(3) 0.0427(18) Uani 1 1 d . . . O14 O 1.0256(9) 0.1158(5) 0.2554(5) 0.071(3) Uani 1 1 d . . . O15 O 0.7237(7) -0.0749(4) 0.3038(3) 0.0427(18) Uani 1 1 d . . . O16 O 0.7572(7) -0.0394(4) 0.2077(3) 0.0382(17) Uani 1 1 d . . . O17 O 0.8078(8) -0.1926(4) 0.2585(4) 0.053(2) Uani 1 1 d . . . O18 O 0.9826(10) -0.2521(5) 0.2711(5) 0.072(3) Uani 1 1 d . . . O19 O 0.9775(7) 0.3159(4) 0.2216(3) 0.0444(19) Uani 1 1 d . . . O20 O 0.8074(8) 0.2517(4) 0.2643(4) 0.050(2) Uani 1 1 d . . . O21 O 1.0564(6) 0.4695(4) 0.1849(3) 0.0329(16) Uani 1 1 d . . . O22 O 1.0457(6) 0.4255(4) 0.2798(3) 0.0314(15) Uani 1 1 d . . . O23 O 0.9496(7) 0.5757(4) 0.2399(3) 0.0357(17) Uani 1 1 d . . . O24 O 0.7577(8) 0.6025(4) 0.2753(4) 0.049(2) Uani 1 1 d . . . O27 O 1.0547(9) 0.2225(6) 0.3385(4) 0.068(3) Uani 1 1 d . . . O28 O 1.2409(14) 0.1353(9) 0.3951(5) 0.120(5) Uani 1 1 d U . . H28 H 1.2795 0.1477 0.3617 0.180 Uiso 1 1 calc R . . O30 O 0.025(3) 0.2252(16) 0.5268(15) 0.048(8) Uani 0.25 1 d P . . C3 C 0.4070(9) 0.6973(6) 0.1031(4) 0.032(2) Uani 1 1 d . . . H3 H 0.3967 0.6676 0.0791 0.038 Uiso 1 1 calc R . . C4 C 0.4646(9) 0.8112(5) 0.1120(4) 0.032(2) Uani 1 1 d . . . H4 H 0.4894 0.8589 0.0944 0.039 Uiso 1 1 calc R . . C5 C 0.4284(10) 0.3156(6) 0.0933(4) 0.035(2) Uani 1 1 d . . . H5 H 0.4178 0.3636 0.0737 0.042 Uiso 1 1 calc R . . C12 C 0.4933(10) 0.1974(5) 0.0920(4) 0.035(2) Uani 1 1 d . . . H12 H 0.5213 0.1650 0.0711 0.042 Uiso 1 1 calc R . . C13 C 0.4731(11) 0.2686(6) 0.0613(4) 0.040(3) Uani 1 1 d . . . H13 H 0.4893 0.2842 0.0202 0.048 Uiso 1 1 calc R . . O1A O 0.9359(15) 0.3308(7) 0.3781(5) 0.081(4) Uani 0.75 1 d P A 1 C1A C 0.4470(11) 0.7679(6) 0.0782(4) 0.038(3) Uani 1 1 d . . . H1A H 0.4621 0.7857 0.0372 0.045 Uiso 1 1 calc R . . O1B O 0.843(3) 0.8948(11) 0.4121(8) 0.093(7) Uani 0.50 1 d PU . . O1C O 0.661(2) 0.3260(12) 0.5927(10) 0.085(6) Uani 0.50 1 d PU . . O1E O 0.783(3) 0.3070(17) 0.4898(13) 0.126(10) Uani 0.50 1 d PU . . O1F O 0.705(4) 0.4872(18) 0.0714(16) 0.167(13) Uani 0.50 1 d PU . . O1D O 0.796(3) 0.3391(18) 0.3929(11) 0.041(7) Uani 0.25 1 d PU B 2 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 Cd1 0.0248(4) 0.0233(4) 0.0265(3) -0.0085(3) -0.0025(3) 0.0020(3) Cd3 0.0331(4) 0.0214(4) 0.0228(3) -0.0064(3) -0.0022(3) -0.0007(3) Cd2 0.0336(4) 0.0201(4) 0.0214(3) -0.0045(3) -0.0014(3) 0.0027(3) Cd4 0.0339(4) 0.0217(4) 0.0273(4) -0.0095(3) -0.0050(3) 0.0036(3) Cd5 0.0279(4) 0.0227(4) 0.0289(4) -0.0093(3) -0.0029(3) 0.0008(3) Cd6 0.0331(4) 0.0232(4) 0.0352(4) -0.0117(3) -0.0035(3) 0.0020(3) C1 0.025(5) 0.029(6) 0.041(6) -0.016(5) -0.001(4) 0.003(4) C2 0.025(5) 0.014(5) 0.034(5) -0.012(4) 0.000(4) -0.001(4) C6 0.019(4) 0.020(5) 0.037(5) -0.016(4) -0.006(4) 0.002(4) C7 0.023(5) 0.032(6) 0.029(5) -0.014(4) -0.009(4) 0.006(4) C8 0.030(5) 0.025(5) 0.032(5) -0.013(4) -0.006(4) 0.005(4) C9 0.036(6) 0.022(5) 0.025(5) -0.009(4) -0.003(4) -0.009(4) C10 0.029(5) 0.025(6) 0.036(5) -0.013(4) -0.013(4) 0.004(4) C11 0.022(5) 0.021(5) 0.030(5) -0.011(4) 0.000(4) 0.001(4) C15 0.035(5) 0.018(5) 0.022(4) -0.011(4) -0.009(4) 0.002(4) C16 0.027(5) 0.023(5) 0.027(5) -0.007(4) -0.005(4) 0.001(4) C17 0.034(6) 0.020(5) 0.029(5) -0.016(4) 0.000(4) 0.008(4) C18 0.030(5) 0.031(6) 0.036(6) -0.008(5) 0.002(4) 0.008(5) C19 0.044(6) 0.017(5) 0.027(5) 0.002(4) -0.004(4) 0.005(5) C20 0.032(5) 0.022(5) 0.034(5) -0.007(4) -0.001(4) 0.001(4) C21 0.037(6) 0.044(7) 0.063(8) -0.023(6) -0.002(6) 0.006(6) C22 0.022(6) 0.064(9) 0.077(9) -0.031(7) -0.002(6) 0.006(6) C23 0.029(6) 0.042(7) 0.059(7) -0.023(6) -0.006(5) -0.010(5) C24 0.027(5) 0.029(5) 0.031(5) -0.014(4) -0.003(4) 0.000(4) C25 0.030(5) 0.019(5) 0.023(4) -0.007(4) -0.008(4) 0.009(4) C26 0.022(5) 0.018(5) 0.041(6) -0.008(4) -0.005(4) 0.004(4) C27 0.034(6) 0.027(6) 0.035(5) -0.018(4) -0.008(4) 0.005(5) C28 0.044(7) 0.023(6) 0.030(5) -0.006(4) 0.001(5) -0.003(5) C29 0.038(6) 0.025(6) 0.046(6) -0.015(5) -0.005(5) -0.005(5) C30 0.039(7) 0.058(9) 0.127(13) -0.058(9) -0.005(8) -0.007(7) C31 0.031(7) 0.106(14) 0.176(19) -0.094(14) -0.024(9) 0.008(8) C32 0.052(8) 0.052(9) 0.108(12) -0.047(8) -0.022(8) 0.029(7) C33 0.036(6) 0.031(6) 0.043(6) -0.015(5) -0.010(5) 0.007(5) C34 0.037(6) 0.013(5) 0.035(5) -0.005(4) -0.011(4) 0.004(4) C35 0.032(5) 0.013(5) 0.040(6) -0.010(4) -0.002(5) -0.001(4) C36 0.052(7) 0.023(6) 0.027(5) -0.009(4) -0.006(5) 0.009(5) C37 0.063(8) 0.040(7) 0.041(6) -0.002(5) -0.008(6) -0.013(6) C38 0.072(9) 0.039(7) 0.040(6) -0.006(5) -0.020(6) -0.012(6) C39 0.067(8) 0.055(8) 0.030(6) -0.006(5) -0.015(6) 0.003(7) C40 0.119(13) 0.045(8) 0.033(6) -0.008(6) -0.018(7) -0.019(8) C41 0.087(10) 0.055(8) 0.033(6) -0.013(6) -0.020(6) -0.013(7) C42 0.097(11) 0.040(7) 0.036(6) -0.005(5) -0.007(7) -0.011(7) C43 0.088(10) 0.037(7) 0.043(7) -0.004(5) -0.019(7) -0.008(7) C44 0.055(7) 0.059(8) 0.036(6) -0.018(6) -0.019(5) -0.001(6) C45 0.107(11) 0.034(7) 0.035(6) -0.016(5) -0.015(7) 0.004(7) C46 0.095(10) 0.035(7) 0.038(6) -0.016(5) -0.021(6) 0.002(7) C47 0.083(9) 0.038(7) 0.035(6) -0.016(5) -0.005(6) 0.015(6) C48 0.097(11) 0.033(7) 0.034(6) -0.002(5) -0.003(6) -0.003(7) C49 0.049(7) 0.040(7) 0.029(5) -0.007(5) -0.001(5) -0.001(5) C50 0.072(9) 0.040(7) 0.040(6) -0.017(5) -0.001(6) 0.008(6) C51 0.056(7) 0.039(7) 0.031(5) -0.009(5) -0.005(5) 0.007(6) C52 0.124(13) 0.053(9) 0.034(6) -0.014(6) -0.012(7) 0.033(9) C53 0.147(15) 0.052(9) 0.033(6) -0.018(6) -0.017(8) 0.041(9) C54 0.055(7) 0.031(6) 0.028(5) -0.006(4) -0.006(5) 0.009(5) C55 0.083(10) 0.042(7) 0.034(6) -0.002(5) -0.002(6) 0.017(7) C56 0.075(9) 0.035(7) 0.035(6) -0.012(5) -0.005(6) 0.023(6) C57 0.094(10) 0.025(6) 0.033(6) -0.009(5) 0.007(6) -0.009(6) C58 0.094(10) 0.038(7) 0.031(6) -0.017(5) -0.005(6) -0.005(7) C59 0.047(6) 0.032(6) 0.023(5) -0.004(4) -0.002(4) -0.006(5) C60 0.087(9) 0.027(6) 0.030(5) -0.010(5) 0.002(6) 0.009(6) C61 0.079(9) 0.042(7) 0.032(6) -0.015(5) -0.002(6) 0.003(7) C62 0.039(6) 0.042(7) 0.042(6) -0.020(5) -0.004(5) 0.000(5) C63 0.040(6) 0.044(7) 0.035(6) -0.015(5) -0.001(5) -0.006(5) C64 0.023(5) 0.060(8) 0.040(6) -0.024(6) -0.009(4) 0.007(5) C65 0.052(7) 0.041(7) 0.039(6) -0.020(5) -0.006(5) 0.009(6) C66 0.036(6) 0.033(6) 0.032(5) -0.004(4) -0.004(4) 0.000(5) C67 0.036(6) 0.052(7) 0.033(5) -0.022(5) -0.008(5) 0.005(5) C68 0.058(8) 0.042(7) 0.038(6) -0.020(5) -0.002(5) -0.003(6) C69 0.039(6) 0.049(7) 0.045(7) -0.009(6) -0.002(5) 0.001(6) C70 0.040(6) 0.045(7) 0.036(6) -0.014(5) -0.006(5) 0.012(5) C71 0.042(6) 0.044(7) 0.039(6) -0.014(5) -0.008(5) 0.009(5) C72 0.053(7) 0.027(6) 0.029(5) -0.003(4) -0.003(5) -0.004(5) C73 0.045(6) 0.031(6) 0.041(6) -0.001(5) -0.008(5) -0.002(5) C74 0.026(5) 0.040(6) 0.026(5) -0.005(4) 0.000(4) -0.004(5) C75 0.051(7) 0.029(6) 0.028(5) -0.003(4) -0.002(5) 0.004(5) C76 0.048(7) 0.032(6) 0.032(5) -0.002(5) 0.000(5) 0.002(5) C77 0.038(6) 0.030(6) 0.040(6) 0.002(5) -0.007(5) -0.009(5) C78 0.034(6) 0.040(6) 0.025(5) -0.004(4) 0.001(4) -0.003(5) C79 0.025(5) 0.041(6) 0.029(5) -0.004(5) -0.005(4) 0.006(5) C80 0.044(6) 0.026(6) 0.031(5) 0.005(4) -0.001(5) 0.006(5) C81 0.044(6) 0.036(6) 0.030(5) -0.005(5) -0.006(5) 0.012(5) C87 0.087(13) 0.17(2) 0.060(10) -0.004(12) 0.010(9) 0.000(14) C88 0.113(9) 0.151(12) 0.076(6) 0.004(7) -0.012(8) 0.046(10) N1 0.037(5) 0.048(6) 0.025(4) -0.007(4) -0.007(4) -0.003(4) N2 0.056(6) 0.039(6) 0.032(5) -0.011(4) -0.013(4) 0.006(5) N3 0.033(5) 0.038(5) 0.028(4) -0.012(4) -0.003(4) -0.001(4) N4 0.060(6) 0.037(5) 0.028(4) -0.010(4) -0.001(4) 0.000(5) N5 0.035(5) 0.036(5) 0.026(4) -0.005(4) -0.001(4) -0.002(4) N6 0.043(5) 0.029(5) 0.026(4) 0.001(4) -0.007(4) 0.004(4) N7 0.041(5) 0.030(5) 0.036(5) -0.008(4) -0.005(4) 0.004(4) N8 0.043(5) 0.047(6) 0.036(5) -0.022(4) -0.008(4) 0.005(5) N9 0.039(5) 0.029(5) 0.034(4) -0.011(4) 0.001(4) -0.005(4) O1 0.045(4) 0.037(4) 0.038(4) -0.019(3) -0.016(3) 0.010(3) O2 0.071(6) 0.019(4) 0.059(5) -0.013(4) -0.025(4) 0.001(4) O3 0.034(4) 0.046(5) 0.032(4) -0.014(3) 0.005(3) 0.000(3) O4 0.039(4) 0.031(4) 0.031(4) 0.003(3) -0.010(3) 0.001(3) O5 0.043(4) 0.021(4) 0.036(4) -0.007(3) -0.001(3) 0.001(3) O6 0.062(5) 0.025(4) 0.087(6) -0.029(4) 0.025(5) -0.012(4) O7 0.054(5) 0.025(4) 0.060(5) -0.019(4) 0.012(4) 0.001(4) O8 0.048(4) 0.029(4) 0.044(4) -0.020(3) 0.001(4) 0.010(3) O9 0.031(4) 0.042(5) 0.033(4) -0.006(3) 0.003(3) 0.003(3) O10 0.041(4) 0.057(5) 0.028(4) -0.022(3) -0.012(3) 0.015(4) O11 0.038(4) 0.024(4) 0.030(4) -0.004(3) -0.006(3) 0.002(3) O12 0.107(8) 0.023(4) 0.071(6) -0.025(4) -0.051(5) 0.013(4) O13 0.046(5) 0.032(4) 0.055(5) -0.020(4) -0.009(4) 0.014(4) O14 0.069(6) 0.031(5) 0.118(8) -0.030(5) -0.004(6) -0.016(5) O15 0.034(4) 0.040(5) 0.051(5) -0.014(4) 0.009(4) -0.005(4) O16 0.039(4) 0.037(4) 0.045(4) -0.019(3) -0.012(3) 0.009(3) O17 0.048(5) 0.023(4) 0.092(7) -0.018(4) -0.020(5) -0.001(4) O18 0.079(7) 0.028(5) 0.112(8) -0.025(5) -0.008(6) 0.019(5) O19 0.046(5) 0.028(4) 0.058(5) -0.014(4) 0.002(4) 0.014(4) O20 0.065(5) 0.018(4) 0.067(5) -0.009(4) -0.009(4) -0.012(4) O21 0.029(4) 0.034(4) 0.033(4) -0.009(3) 0.003(3) 0.003(3) O22 0.029(4) 0.036(4) 0.034(4) -0.015(3) -0.006(3) 0.005(3) O23 0.040(4) 0.029(4) 0.039(4) -0.013(3) 0.004(3) -0.008(3) O24 0.063(5) 0.031(4) 0.058(5) -0.023(4) 0.000(4) 0.020(4) O27 0.080(7) 0.079(7) 0.045(5) -0.020(5) -0.001(5) 0.014(6) O28 0.112(9) 0.151(12) 0.076(6) 0.004(7) -0.012(7) 0.046(9) O30 0.047(18) 0.041(19) 0.07(2) -0.032(16) -0.021(16) 0.025(15) C3 0.035(6) 0.036(6) 0.025(5) -0.010(4) -0.003(4) 0.003(5) C4 0.037(6) 0.026(5) 0.032(5) -0.007(4) -0.001(4) -0.002(5) C5 0.043(6) 0.027(6) 0.035(5) -0.008(4) 0.000(5) 0.007(5) C12 0.045(6) 0.028(6) 0.035(5) -0.016(4) -0.001(5) 0.009(5) C13 0.058(7) 0.039(6) 0.020(5) -0.007(4) 0.003(5) -0.003(6) O1A 0.121(13) 0.059(9) 0.054(7) 0.003(6) -0.014(8) -0.006(8) C1A 0.053(7) 0.032(6) 0.027(5) -0.009(4) 0.004(5) -0.006(5) O1B 0.168(17) 0.068(12) 0.038(9) -0.011(8) -0.002(10) 0.023(12) O1C 0.085(6) 0.085(6) 0.084(6) -0.024(2) -0.0097(12) 0.0021(10) O1E 0.132(13) 0.127(13) 0.125(12) -0.048(9) -0.001(9) -0.008(9) O1F 0.23(2) 0.117(18) 0.158(19) -0.047(15) -0.013(16) -0.027(16) O1D 0.038(13) 0.067(16) 0.017(11) -0.010(11) 0.004(10) -0.017(12) _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 Cd1 O7 2.258(7) . ? Cd1 O6 2.321(8) . ? Cd1 O21 2.322(7) 1_455 ? Cd1 O22 2.334(7) 1_455 ? Cd1 N1 2.335(8) . ? Cd1 O5 2.508(7) . ? Cd1 O8 2.611(7) . ? Cd1 C26 2.667(9) 1_455 ? Cd3 O13 2.233(7) . ? Cd3 O20 2.236(7) . ? Cd3 N4 2.282(8) . ? Cd3 N5 2.330(8) . ? Cd3 O11 2.333(7) . ? Cd3 O10 2.409(7) . ? Cd2 O18 2.182(8) . ? Cd2 O23 2.259(7) 1_545 ? Cd2 N9 2.268(8) . ? Cd2 N6 2.314(8) 2_755 ? Cd2 O5 2.339(7) 1_645 ? Cd2 O3 2.436(7) 1_645 ? Cd4 O17 2.252(7) . ? Cd4 O24 2.258(7) 1_545 ? Cd4 N2 2.305(8) 2_656 ? Cd4 N7 2.320(8) . ? Cd4 O1 2.379(7) 1_545 ? Cd4 O4 2.396(7) 1_545 ? Cd5 O2 2.188(7) 1_545 ? Cd5 O16 2.239(7) . ? Cd5 N3 2.278(8) 2_656 ? Cd5 O12 2.394(8) . ? Cd5 O11 2.407(7) . ? Cd5 O15 2.488(8) . ? Cd6 O14 2.191(8) . ? Cd6 O19 2.221(7) . ? Cd6 O27 2.322(8) . ? Cd6 N8 2.334(8) 2_755 ? Cd6 O9 2.364(7) 1_655 ? Cd6 O8 2.387(8) 1_655 ? C1 O1 1.232(12) . ? C1 O2 1.240(12) . ? C1 C2 1.504(13) . ? C2 C4 1.386(13) . ? C2 C7 1.395(13) . ? C6 C3 1.378(13) . ? C6 C7 1.379(12) . ? C6 C8 1.493(13) . ? C7 C9 1.500(13) . ? C8 O6 1.207(12) . ? C8 O5 1.263(11) . ? C9 O4 1.252(11) . ? C9 O3 1.257(11) . ? C10 O7 1.221(12) . ? C10 O8 1.267(12) . ? C10 C11 1.497(13) . ? C11 C5 1.373(13) . ? C11 C16 1.375(13) . ? C15 C12 1.373(13) . ? C15 C16 1.394(13) . ? C15 C18 1.499(13) . ? C16 C17 1.504(12) . ? C17 O9 1.235(11) . ? C17 O10 1.246(11) . ? C18 O12 1.228(13) . ? C18 O11 1.267(12) . ? C19 O24 1.244(12) . ? C19 O23 1.246(12) . ? C19 C20 1.494(14) . ? C20 C21 1.394(15) . ? C20 C25 1.396(13) . ? C21 C22 1.379(17) . ? C21 H21 0.9300 . ? C22 C23 1.372(16) . ? C22 H22 0.9300 . ? C23 C24 1.393(14) . ? C23 H23 0.9300 . ? C24 C25 1.412(13) . ? C24 C27 1.489(14) . ? C25 C26 1.495(13) . ? C26 O21 1.227(11) . ? C26 O22 1.249(11) . ? C26 Cd1 2.667(9) 1_655 ? C27 O20 1.224(12) . ? C27 O19 1.230(12) . ? C28 O14 1.235(13) . ? C28 O13 1.236(13) . ? C28 C29 1.495(14) . ? C29 C30 1.390(16) . ? C29 C34 1.392(14) . ? C30 C31 1.31(2) . ? C30 H30 0.9300 . ? C31 C32 1.39(2) . ? C31 H31 0.9300 . ? C32 C33 1.395(16) . ? C32 H32 0.9300 . ? C33 C34 1.393(13) . ? C33 C36 1.502(15) . ? C34 C35 1.486(14) . ? C35 O15 1.224(12) . ? C35 O16 1.256(12) . ? C36 O17 1.221(13) . ? C36 O18 1.227(13) . ? C37 N1 1.309(14) . ? C37 C38 1.375(15) . ? C37 H37 0.9300 . ? C38 C39 1.391(16) . ? C38 H38 0.9300 . ? C39 C40 1.388(17) . ? C39 C44 1.496(15) . ? C40 C41 1.347(16) . ? C40 H40 0.9300 . ? C41 N1 1.316(15) . ? C41 H41 0.9300 . ? C42 N2 1.337(15) . ? C42 C43 1.382(16) . ? C42 H42 0.9300 . ? C43 C44 1.380(17) . ? C43 H43 0.9300 . ? C44 C45 1.352(16) . ? C45 C46 1.372(15) . ? C45 H45 0.9300 . ? C46 N2 1.321(14) . ? C46 H46 0.9300 . ? C47 N3 1.298(14) . ? C47 C48 1.376(15) . ? C47 H47 0.9300 . ? C48 C49 1.379(16) . ? C48 H48 0.9300 . ? C49 C50 1.367(16) . ? C49 C54 1.434(14) . ? C50 C51 1.368(15) . ? C50 H50 0.9300 . ? C51 N3 1.311(13) . ? C51 H51 0.9300 . ? C52 N4 1.329(15) . ? C52 C53 1.366(16) . ? C52 H52 0.9300 . ? C53 C54 1.378(16) . ? C53 H53 0.9300 . ? C54 C55 1.358(16) . ? C55 C56 1.374(15) . ? C55 H55 0.9300 . ? C56 N4 1.309(14) . ? C56 H56 0.9300 . ? C57 N9 1.306(13) . ? C57 C58 1.376(15) . ? C57 H57 0.9300 . ? C58 C59 1.356(15) . ? C58 H58 0.9300 . ? C59 C60 1.366(14) . ? C59 C59 1.467(18) 2_746 ? C60 C61 1.359(15) . ? C60 H60 0.9300 . ? C61 N9 1.321(14) . ? C61 H61 0.9300 . ? C62 N7 1.319(14) . ? C62 C63 1.378(14) . ? C62 H62 0.9300 . ? C63 C64 1.364(15) . ? C63 H63 0.9300 . ? C64 C65 1.375(16) . ? C64 C67 1.470(14) . ? C65 C66 1.356(14) . ? C65 H65 0.9300 . ? C66 N7 1.339(13) . ? C66 H66 0.9300 . ? C67 C68 1.356(16) . ? C67 C71 1.407(15) . ? C68 C69 1.365(15) . ? C68 H68 0.9300 . ? C69 N8 1.327(14) . ? C69 H69 0.9300 . ? C70 N8 1.320(14) . ? C70 C71 1.364(14) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 N5 1.311(13) . ? C72 C73 1.374(14) . ? C72 H72 0.9300 . ? C73 C74 1.406(15) . ? C73 H73 0.9300 . ? C74 C75 1.375(14) . ? C74 C79 1.460(13) . ? C75 C76 1.357(14) . ? C75 H75 0.9300 . ? C76 N5 1.337(13) . ? C76 H76 0.9300 . ? C77 N6 1.337(13) . ? C77 C78 1.350(14) . ? C77 H77 0.9300 . ? C78 C79 1.402(14) . ? C78 H78 0.9300 . ? C79 C80 1.374(15) . ? C80 C81 1.397(13) . ? C80 H80 0.9300 . ? C81 N6 1.314(13) . ? C81 H81 0.9300 . ? C87 O27 1.435(19) . ? C87 C88 1.47(3) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 O28 1.40(3) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? N2 Cd4 2.305(8) 2_656 ? N3 Cd5 2.278(8) 2_656 ? N6 Cd2 2.314(8) 2_755 ? N8 Cd6 2.334(8) 2_755 ? O1 Cd4 2.379(7) 1_565 ? O2 Cd5 2.188(7) 1_565 ? O3 Cd2 2.436(7) 1_465 ? O4 Cd4 2.396(7) 1_565 ? O5 Cd2 2.339(7) 1_465 ? O8 Cd6 2.387(8) 1_455 ? O9 Cd6 2.364(7) 1_455 ? O21 Cd1 2.322(7) 1_655 ? O22 Cd1 2.334(7) 1_655 ? O23 Cd2 2.259(7) 1_565 ? O24 Cd4 2.258(7) 1_565 ? O28 H28 0.8200 . ? C3 C1A 1.382(14) . ? C3 H3 0.9300 . ? C4 C1A 1.341(14) . ? C4 H4 0.9300 . ? C5 C13 1.393(14) . ? C5 H5 0.9300 . ? C12 C13 1.400(14) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C1A H1A 0.9300 . ? 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 O7 Cd1 O6 76.1(3) . . ? O7 Cd1 O21 102.2(3) . 1_455 ? O6 Cd1 O21 104.4(3) . 1_455 ? O7 Cd1 O22 133.8(3) . 1_455 ? O6 Cd1 O22 143.3(3) . 1_455 ? O21 Cd1 O22 55.3(2) 1_455 1_455 ? O7 Cd1 N1 113.1(3) . . ? O6 Cd1 N1 109.0(3) . . ? O21 Cd1 N1 135.9(3) 1_455 . ? O22 Cd1 N1 80.9(3) 1_455 . ? O7 Cd1 O5 129.0(2) . . ? O6 Cd1 O5 52.9(2) . . ? O21 Cd1 O5 91.2(2) 1_455 . ? O22 Cd1 O5 94.2(2) 1_455 . ? N1 Cd1 O5 86.8(3) . . ? O7 Cd1 O8 52.5(2) . . ? O6 Cd1 O8 128.4(2) . . ? O21 Cd1 O8 92.4(2) 1_455 . ? O22 Cd1 O8 85.8(2) 1_455 . ? N1 Cd1 O8 88.9(3) . . ? O5 Cd1 O8 175.7(2) . . ? O7 Cd1 C26 120.5(3) . 1_455 ? O6 Cd1 C26 126.1(3) . 1_455 ? O21 Cd1 C26 27.4(3) 1_455 1_455 ? O22 Cd1 C26 27.9(3) 1_455 1_455 ? N1 Cd1 C26 108.7(3) . 1_455 ? O5 Cd1 C26 92.9(3) . 1_455 ? O8 Cd1 C26 89.1(3) . 1_455 ? O13 Cd3 O20 106.0(3) . . ? O13 Cd3 N4 87.7(3) . . ? O20 Cd3 N4 86.9(3) . . ? O13 Cd3 N5 87.9(3) . . ? O20 Cd3 N5 85.2(3) . . ? N4 Cd3 N5 169.6(3) . . ? O13 Cd3 O11 88.1(3) . . ? O20 Cd3 O11 161.7(3) . . ? N4 Cd3 O11 105.5(3) . . ? N5 Cd3 O11 83.8(3) . . ? O13 Cd3 O10 153.4(3) . . ? O20 Cd3 O10 95.6(3) . . ? N4 Cd3 O10 78.0(3) . . ? N5 Cd3 O10 109.5(3) . . ? O11 Cd3 O10 74.5(2) . . ? O18 Cd2 O23 110.6(3) . 1_545 ? O18 Cd2 N9 88.4(4) . . ? O23 Cd2 N9 84.2(3) 1_545 . ? O18 Cd2 N6 92.8(4) . 2_755 ? O23 Cd2 N6 84.3(3) 1_545 2_755 ? N9 Cd2 N6 168.1(3) . 2_755 ? O18 Cd2 O5 163.9(3) . 1_645 ? O23 Cd2 O5 85.3(2) 1_545 1_645 ? N9 Cd2 O5 95.8(3) . 1_645 ? N6 Cd2 O5 86.4(3) 2_755 1_645 ? O18 Cd2 O3 90.6(3) . 1_645 ? O23 Cd2 O3 153.3(3) 1_545 1_645 ? N9 Cd2 O3 80.3(3) . 1_645 ? N6 Cd2 O3 111.5(3) 2_755 1_645 ? O5 Cd2 O3 74.9(2) 1_645 1_645 ? O17 Cd4 O24 120.9(3) . 1_545 ? O17 Cd4 N2 90.6(3) . 2_656 ? O24 Cd4 N2 84.7(3) 1_545 2_656 ? O17 Cd4 N7 88.7(3) . . ? O24 Cd4 N7 83.8(3) 1_545 . ? N2 Cd4 N7 166.3(3) 2_656 . ? O17 Cd4 O1 78.4(3) . 1_545 ? O24 Cd4 O1 160.5(3) 1_545 1_545 ? N2 Cd4 O1 98.8(3) 2_656 1_545 ? N7 Cd4 O1 94.5(3) . 1_545 ? O17 Cd4 O4 150.8(3) . 1_545 ? O24 Cd4 O4 86.8(3) 1_545 1_545 ? N2 Cd4 O4 82.4(3) 2_656 1_545 ? N7 Cd4 O4 104.5(3) . 1_545 ? O1 Cd4 O4 74.8(2) 1_545 1_545 ? O2 Cd5 O16 103.3(3) 1_545 . ? O2 Cd5 N3 111.8(3) 1_545 2_656 ? O16 Cd5 N3 132.6(3) . 2_656 ? O2 Cd5 O12 77.4(3) 1_545 . ? O16 Cd5 O12 103.3(3) . . ? N3 Cd5 O12 114.5(3) 2_656 . ? O2 Cd5 O11 131.2(2) 1_545 . ? O16 Cd5 O11 92.5(2) . . ? N3 Cd5 O11 87.7(3) 2_656 . ? O12 Cd5 O11 54.0(2) . . ? O2 Cd5 O15 128.9(3) 1_545 . ? O16 Cd5 O15 54.5(2) . . ? N3 Cd5 O15 78.5(3) 2_656 . ? O12 Cd5 O15 146.0(3) . . ? O11 Cd5 O15 97.9(2) . . ? O14 Cd6 O19 118.4(3) . . ? O14 Cd6 O27 92.8(4) . . ? O19 Cd6 O27 84.3(3) . . ? O14 Cd6 N8 86.9(4) . 2_755 ? O19 Cd6 N8 87.3(3) . 2_755 ? O27 Cd6 N8 170.3(3) . 2_755 ? O14 Cd6 O9 87.7(3) . 1_655 ? O19 Cd6 O9 152.0(3) . 1_655 ? O27 Cd6 O9 84.5(3) . 1_655 ? N8 Cd6 O9 105.2(3) 2_755 1_655 ? O14 Cd6 O8 161.4(3) . 1_655 ? O19 Cd6 O8 80.2(3) . 1_655 ? O27 Cd6 O8 89.2(3) . 1_655 ? N8 Cd6 O8 94.2(3) 2_755 1_655 ? O9 Cd6 O8 74.1(2) 1_655 1_655 ? O1 C1 O2 124.0(9) . . ? O1 C1 C2 120.5(9) . . ? O2 C1 C2 115.4(9) . . ? C4 C2 C7 119.5(8) . . ? C4 C2 C1 118.2(8) . . ? C7 C2 C1 122.1(8) . . ? C3 C6 C7 120.0(9) . . ? C3 C6 C8 118.7(8) . . ? C7 C6 C8 121.3(8) . . ? C6 C7 C2 119.4(9) . . ? C6 C7 C9 120.3(9) . . ? C2 C7 C9 120.2(8) . . ? O6 C8 O5 121.5(9) . . ? O6 C8 C6 119.0(9) . . ? O5 C8 C6 119.4(8) . . ? O4 C9 O3 126.1(9) . . ? O4 C9 C7 117.1(9) . . ? O3 C9 C7 116.9(8) . . ? O7 C10 O8 122.2(9) . . ? O7 C10 C11 117.7(9) . . ? O8 C10 C11 120.1(9) . . ? C5 C11 C16 121.0(9) . . ? C5 C11 C10 117.3(8) . . ? C16 C11 C10 121.7(8) . . ? C12 C15 C16 120.2(9) . . ? C12 C15 C18 118.1(8) . . ? C16 C15 C18 121.6(8) . . ? C11 C16 C15 119.3(8) . . ? C11 C16 C17 121.1(8) . . ? C15 C16 C17 119.5(8) . . ? O9 C17 O10 125.0(9) . . ? O9 C17 C16 118.7(9) . . ? O10 C17 C16 116.3(9) . . ? O12 C18 O11 121.6(10) . . ? O12 C18 C15 119.5(9) . . ? O11 C18 C15 118.9(9) . . ? O24 C19 O23 127.1(10) . . ? O24 C19 C20 115.9(10) . . ? O23 C19 C20 116.8(9) . . ? C21 C20 C25 119.3(10) . . ? C21 C20 C19 117.3(9) . . ? C25 C20 C19 123.4(9) . . ? C22 C21 C20 121.1(11) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 119.3(10) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.7(10) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C25 118.6(9) . . ? C23 C24 C27 119.0(9) . . ? C25 C24 C27 122.2(8) . . ? C20 C25 C24 119.6(9) . . ? C20 C25 C26 120.7(9) . . ? C24 C25 C26 119.5(8) . . ? O21 C26 O22 121.5(9) . . ? O21 C26 C25 121.1(8) . . ? O22 C26 C25 117.4(8) . . ? O21 C26 Cd1 60.5(5) . 1_655 ? O22 C26 Cd1 61.0(5) . 1_655 ? C25 C26 Cd1 178.4(7) . 1_655 ? O20 C27 O19 125.0(10) . . ? O20 C27 C24 117.0(9) . . ? O19 C27 C24 118.0(9) . . ? O14 C28 O13 124.2(10) . . ? O14 C28 C29 118.1(10) . . ? O13 C28 C29 117.7(9) . . ? C30 C29 C34 118.6(10) . . ? C30 C29 C28 118.2(10) . . ? C34 C29 C28 123.2(10) . . ? C31 C30 C29 121.9(12) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 121.0(13) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C33 119.4(12) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 118.9(10) . . ? C34 C33 C36 123.1(9) . . ? C32 C33 C36 117.9(10) . . ? C29 C34 C33 120.0(9) . . ? C29 C34 C35 120.0(9) . . ? C33 C34 C35 119.9(9) . . ? O15 C35 O16 122.5(10) . . ? O15 C35 C34 120.8(9) . . ? O16 C35 C34 116.7(9) . . ? O17 C36 O18 126.1(11) . . ? O17 C36 C33 117.7(9) . . ? O18 C36 C33 116.2(10) . . ? N1 C37 C38 123.8(11) . . ? N1 C37 H37 118.1 . . ? C38 C37 H37 118.1 . . ? C37 C38 C39 119.3(11) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 115.5(10) . . ? C40 C39 C44 122.2(11) . . ? C38 C39 C44 122.2(11) . . ? C41 C40 C39 120.5(12) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? N1 C41 C40 123.8(12) . . ? N1 C41 H41 118.1 . . ? C40 C41 H41 118.1 . . ? N2 C42 C43 122.0(12) . . ? N2 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C44 C43 C42 119.6(12) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 117.1(10) . . ? C45 C44 C39 122.1(11) . . ? C43 C44 C39 120.8(11) . . ? C44 C45 C46 121.2(11) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? N2 C46 C45 122.0(11) . . ? N2 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? N3 C47 C48 124.1(11) . . ? N3 C47 H47 118.0 . . ? C48 C47 H47 118.0 . . ? C47 C48 C49 120.0(11) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 114.6(10) . . ? C50 C49 C54 123.4(11) . . ? C48 C49 C54 121.9(10) . . ? C49 C50 C51 121.7(11) . . ? C49 C50 H50 119.2 . . ? C51 C50 H50 119.2 . . ? N3 C51 C50 122.7(11) . . ? N3 C51 H51 118.6 . . ? C50 C51 H51 118.6 . . ? N4 C52 C53 123.6(12) . . ? N4 C52 H52 118.2 . . ? C53 C52 H52 118.2 . . ? C52 C53 C54 120.9(12) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 114.7(10) . . ? C55 C54 C49 123.9(10) . . ? C53 C54 C49 121.4(10) . . ? C54 C55 C56 121.4(11) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? N4 C56 C55 123.8(11) . . ? N4 C56 H56 118.1 . . ? C55 C56 H56 118.1 . . ? N9 C57 C58 122.0(11) . . ? N9 C57 H57 119.0 . . ? C58 C57 H57 119.0 . . ? C59 C58 C57 121.1(10) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C58 C59 C60 116.1(9) . . ? C58 C59 C59 122.0(12) . 2_746 ? C60 C59 C59 121.9(12) . 2_746 ? C61 C60 C59 120.1(11) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? N9 C61 C60 123.2(11) . . ? N9 C61 H61 118.4 . . ? C60 C61 H61 118.4 . . ? N7 C62 C63 123.6(10) . . ? N7 C62 H62 118.2 . . ? C63 C62 H62 118.2 . . ? C64 C63 C62 120.1(11) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 115.8(10) . . ? C63 C64 C67 121.2(11) . . ? C65 C64 C67 122.9(10) . . ? C66 C65 C64 121.3(11) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? N7 C66 C65 122.8(10) . . ? N7 C66 H66 118.6 . . ? C65 C66 H66 118.6 . . ? C68 C67 C71 116.1(10) . . ? C68 C67 C64 122.8(10) . . ? C71 C67 C64 121.0(11) . . ? C67 C68 C69 120.6(11) . . ? C67 C68 H68 119.7 . . ? C69 C68 H68 119.7 . . ? N8 C69 C68 124.0(11) . . ? N8 C69 H69 118.0 . . ? C68 C69 H69 118.0 . . ? N8 C70 C71 124.8(11) . . ? N8 C70 H70 117.6 . . ? C71 C70 H70 117.6 . . ? C70 C71 C67 118.8(11) . . ? C70 C71 H71 120.6 . . ? C67 C71 H71 120.6 . . ? N5 C72 C73 123.2(10) . . ? N5 C72 H72 118.4 . . ? C73 C72 H72 118.4 . . ? C72 C73 C74 119.3(10) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C75 C74 C73 116.7(9) . . ? C75 C74 C79 122.8(10) . . ? C73 C74 C79 120.5(9) . . ? C76 C75 C74 119.5(10) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? N5 C76 C75 123.9(10) . . ? N5 C76 H76 118.1 . . ? C75 C76 H76 118.1 . . ? N6 C77 C78 123.2(10) . . ? N6 C77 H77 118.4 . . ? C78 C77 H77 118.4 . . ? C77 C78 C79 120.1(10) . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C80 C79 C78 116.6(9) . . ? C80 C79 C74 121.1(10) . . ? C78 C79 C74 122.2(10) . . ? C79 C80 C81 119.3(10) . . ? C79 C80 H80 120.3 . . ? C81 C80 H80 120.3 . . ? N6 C81 C80 122.9(10) . . ? N6 C81 H81 118.5 . . ? C80 C81 H81 118.5 . . ? O27 C87 C88 112.5(15) . . ? O27 C87 H87A 109.1 . . ? C88 C87 H87A 109.1 . . ? O27 C87 H87B 109.1 . . ? C88 C87 H87B 109.1 . . ? H87A C87 H87B 107.8 . . ? O28 C88 C87 109(2) . . ? O28 C88 H88A 110.0 . . ? C87 C88 H88A 110.0 . . ? O28 C88 H88B 110.0 . . ? C87 C88 H88B 110.0 . . ? H88A C88 H88B 108.4 . . ? C37 N1 C41 117.0(9) . . ? C37 N1 Cd1 124.9(8) . . ? C41 N1 Cd1 117.4(7) . . ? C46 N2 C42 118.1(10) . . ? C46 N2 Cd4 122.1(8) . 2_656 ? C42 N2 Cd4 119.8(8) . 2_656 ? C47 N3 C51 116.8(9) . . ? C47 N3 Cd5 118.4(7) . 2_656 ? C51 N3 Cd5 122.3(7) . 2_656 ? C56 N4 C52 115.5(10) . . ? C56 N4 Cd3 126.6(8) . . ? C52 N4 Cd3 117.8(8) . . ? C72 N5 C76 117.4(9) . . ? C72 N5 Cd3 123.8(7) . . ? C76 N5 Cd3 118.6(7) . . ? C81 N6 C77 117.8(9) . . ? C81 N6 Cd2 125.8(7) . 2_755 ? C77 N6 Cd2 115.8(7) . 2_755 ? C62 N7 C66 116.2(9) . . ? C62 N7 Cd4 122.1(7) . . ? C66 N7 Cd4 121.6(7) . . ? C70 N8 C69 115.6(9) . . ? C70 N8 Cd6 121.6(7) . 2_755 ? C69 N8 Cd6 122.4(8) . 2_755 ? C57 N9 C61 117.4(9) . . ? C57 N9 Cd2 122.9(7) . . ? C61 N9 Cd2 119.7(7) . . ? C1 O1 Cd4 123.4(6) . 1_565 ? C1 O2 Cd5 109.9(7) . 1_565 ? C9 O3 Cd2 119.2(6) . 1_465 ? C9 O4 Cd4 119.3(6) . 1_565 ? C8 O5 Cd2 127.7(6) . 1_465 ? C8 O5 Cd1 87.6(5) . . ? Cd2 O5 Cd1 134.0(3) 1_465 . ? C8 O6 Cd1 98.0(7) . . ? C10 O7 Cd1 101.6(6) . . ? C10 O8 Cd6 124.7(6) . 1_455 ? C10 O8 Cd1 83.7(6) . . ? Cd6 O8 Cd1 136.9(3) 1_455 . ? C17 O9 Cd6 120.8(6) . 1_455 ? C17 O10 Cd3 122.1(6) . . ? C18 O11 Cd3 129.5(6) . . ? C18 O11 Cd5 91.4(6) . . ? Cd3 O11 Cd5 130.7(3) . . ? C18 O12 Cd5 93.0(6) . . ? C28 O13 Cd3 135.2(7) . . ? C28 O14 Cd6 163.2(9) . . ? C35 O15 Cd5 86.1(6) . . ? C35 O16 Cd5 96.9(6) . . ? C36 O17 Cd4 123.7(7) . . ? C36 O18 Cd2 160.0(9) . . ? C27 O19 Cd6 121.2(7) . . ? C27 O20 Cd3 151.9(7) . . ? C26 O21 Cd1 92.2(6) . 1_655 ? C26 O22 Cd1 91.0(6) . 1_655 ? C19 O23 Cd2 132.0(7) . 1_565 ? C19 O24 Cd4 147.1(7) . 1_565 ? C87 O27 Cd6 129.1(11) . . ? C88 O28 H28 109.5 . . ? C6 C3 C1A 119.6(9) . . ? C6 C3 H3 120.2 . . ? C1A C3 H3 120.2 . . ? C1A C4 C2 120.2(9) . . ? C1A C4 H4 119.9 . . ? C2 C4 H4 119.9 . . ? C11 C5 C13 120.1(9) . . ? C11 C5 H5 119.9 . . ? C13 C5 H5 119.9 . . ? C15 C12 C13 120.3(9) . . ? C15 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C5 C13 C12 118.9(9) . . ? C5 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C4 C1A C3 121.1(9) . . ? C4 C1A H1A 119.4 . . ? C3 C1A H1A 119.4 . . ? 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 C1 C2 C4 -141.6(10) . . . . ? O2 C1 C2 C4 36.8(13) . . . . ? O1 C1 C2 C7 33.4(14) . . . . ? O2 C1 C2 C7 -148.3(10) . . . . ? C3 C6 C7 C2 1.2(13) . . . . ? C8 C6 C7 C2 -178.3(8) . . . . ? C3 C6 C7 C9 -177.5(9) . . . . ? C8 C6 C7 C9 3.0(13) . . . . ? C4 C2 C7 C6 1.6(14) . . . . ? C1 C2 C7 C6 -173.3(8) . . . . ? C4 C2 C7 C9 -179.7(9) . . . . ? C1 C2 C7 C9 5.4(14) . . . . ? C3 C6 C8 O6 39.9(14) . . . . ? C7 C6 C8 O6 -140.5(10) . . . . ? C3 C6 C8 O5 -138.0(9) . . . . ? C7 C6 C8 O5 41.5(13) . . . . ? C6 C7 C9 O4 86.8(11) . . . . ? C2 C7 C9 O4 -91.9(11) . . . . ? C6 C7 C9 O3 -92.3(11) . . . . ? C2 C7 C9 O3 89.0(11) . . . . ? O7 C10 C11 C5 -34.8(13) . . . . ? O8 C10 C11 C5 144.1(9) . . . . ? O7 C10 C11 C16 146.9(10) . . . . ? O8 C10 C11 C16 -34.2(13) . . . . ? C5 C11 C16 C15 -3.7(14) . . . . ? C10 C11 C16 C15 174.5(9) . . . . ? C5 C11 C16 C17 176.6(9) . . . . ? C10 C11 C16 C17 -5.2(14) . . . . ? C12 C15 C16 C11 -0.4(14) . . . . ? C18 C15 C16 C11 -179.3(9) . . . . ? C12 C15 C16 C17 179.3(9) . . . . ? C18 C15 C16 C17 0.4(14) . . . . ? C11 C16 C17 O9 90.6(11) . . . . ? C15 C16 C17 O9 -89.1(11) . . . . ? C11 C16 C17 O10 -90.8(11) . . . . ? C15 C16 C17 O10 89.5(11) . . . . ? C12 C15 C18 O12 -42.0(14) . . . . ? C16 C15 C18 O12 136.9(11) . . . . ? C12 C15 C18 O11 138.4(10) . . . . ? C16 C15 C18 O11 -42.7(14) . . . . ? O24 C19 C20 C21 16.4(14) . . . . ? O23 C19 C20 C21 -167.4(9) . . . . ? O24 C19 C20 C25 -163.0(9) . . . . ? O23 C19 C20 C25 13.2(14) . . . . ? C25 C20 C21 C22 1.6(17) . . . . ? C19 C20 C21 C22 -177.8(11) . . . . ? C20 C21 C22 C23 3.7(19) . . . . ? C21 C22 C23 C24 -4.1(19) . . . . ? C22 C23 C24 C25 -0.9(16) . . . . ? C22 C23 C24 C27 174.6(10) . . . . ? C21 C20 C25 C24 -6.5(14) . . . . ? C19 C20 C25 C24 172.8(8) . . . . ? C21 C20 C25 C26 178.6(9) . . . . ? C19 C20 C25 C26 -2.0(14) . . . . ? C23 C24 C25 C20 6.2(14) . . . . ? C27 C24 C25 C20 -169.2(9) . . . . ? C23 C24 C25 C26 -178.9(9) . . . . ? C27 C24 C25 C26 5.7(14) . . . . ? C20 C25 C26 O21 -90.5(12) . . . . ? C24 C25 C26 O21 94.7(11) . . . . ? C20 C25 C26 O22 89.8(11) . . . . ? C24 C25 C26 O22 -85.1(11) . . . . ? C20 C25 C26 Cd1 82(24) . . . 1_655 ? C24 C25 C26 Cd1 -92(24) . . . 1_655 ? C23 C24 C27 O20 -22.1(14) . . . . ? C25 C24 C27 O20 153.3(9) . . . . ? C23 C24 C27 O19 159.8(10) . . . . ? C25 C24 C27 O19 -24.9(14) . . . . ? O14 C28 C29 C30 3.9(17) . . . . ? O13 C28 C29 C30 -175.7(11) . . . . ? O14 C28 C29 C34 -175.1(10) . . . . ? O13 C28 C29 C34 5.3(15) . . . . ? C34 C29 C30 C31 -2(2) . . . . ? C28 C29 C30 C31 178.7(15) . . . . ? C29 C30 C31 C32 -1(3) . . . . ? C30 C31 C32 C33 3(3) . . . . ? C31 C32 C33 C34 -3(2) . . . . ? C31 C32 C33 C36 179.4(14) . . . . ? C30 C29 C34 C33 3.0(17) . . . . ? C28 C29 C34 C33 -178.0(9) . . . . ? C30 C29 C34 C35 -176.7(11) . . . . ? C28 C29 C34 C35 2.3(15) . . . . ? C32 C33 C34 C29 -0.6(16) . . . . ? C36 C33 C34 C29 177.3(9) . . . . ? C32 C33 C34 C35 179.2(11) . . . . ? C36 C33 C34 C35 -2.9(15) . . . . ? C29 C34 C35 O15 -92.6(12) . . . . ? C33 C34 C35 O15 87.7(12) . . . . ? C29 C34 C35 O16 87.8(12) . . . . ? C33 C34 C35 O16 -91.9(11) . . . . ? C34 C33 C36 O17 6.9(15) . . . . ? C32 C33 C36 O17 -175.2(11) . . . . ? C34 C33 C36 O18 -171.0(10) . . . . ? C32 C33 C36 O18 6.9(16) . . . . ? N1 C37 C38 C39 -1(2) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C37 C38 C39 C44 -174.7(12) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C44 C39 C40 C41 175.1(14) . . . . ? C39 C40 C41 N1 0(2) . . . . ? N2 C42 C43 C44 -4(2) . . . . ? C42 C43 C44 C45 1(2) . . . . ? C42 C43 C44 C39 179.9(13) . . . . ? C40 C39 C44 C45 17(2) . . . . ? C38 C39 C44 C45 -166.5(14) . . . . ? C40 C39 C44 C43 -161.9(14) . . . . ? C38 C39 C44 C43 15(2) . . . . ? C43 C44 C45 C46 1(2) . . . . ? C39 C44 C45 C46 -177.5(13) . . . . ? C44 C45 C46 N2 -1(2) . . . . ? N3 C47 C48 C49 -2(2) . . . . ? C47 C48 C49 C50 -1(2) . . . . ? C47 C48 C49 C54 175.6(12) . . . . ? C48 C49 C50 C51 1.7(19) . . . . ? C54 C49 C50 C51 -174.4(12) . . . . ? C49 C50 C51 N3 -1(2) . . . . ? N4 C52 C53 C54 -1(3) . . . . ? C52 C53 C54 C55 1(2) . . . . ? C52 C53 C54 C49 -178.2(15) . . . . ? C50 C49 C54 C55 -21(2) . . . . ? C48 C49 C54 C55 162.7(14) . . . . ? C50 C49 C54 C53 157.3(14) . . . . ? C48 C49 C54 C53 -19(2) . . . . ? C53 C54 C55 C56 0(2) . . . . ? C49 C54 C55 C56 178.8(13) . . . . ? C54 C55 C56 N4 0(2) . . . . ? N9 C57 C58 C59 -2(2) . . . . ? C57 C58 C59 C60 -1(2) . . . . ? C57 C58 C59 C59 -178.2(14) . . . 2_746 ? C58 C59 C60 C61 0.8(19) . . . . ? C59 C59 C60 C61 178.2(14) 2_746 . . . ? C59 C60 C61 N9 1(2) . . . . ? N7 C62 C63 C64 -4.0(17) . . . . ? C62 C63 C64 C65 3.4(15) . . . . ? C62 C63 C64 C67 -179.3(10) . . . . ? C63 C64 C65 C66 -1.7(16) . . . . ? C67 C64 C65 C66 -179.0(10) . . . . ? C64 C65 C66 N7 0.2(17) . . . . ? C63 C64 C67 C68 -31.9(16) . . . . ? C65 C64 C67 C68 145.2(12) . . . . ? C63 C64 C67 C71 151.3(11) . . . . ? C65 C64 C67 C71 -31.6(16) . . . . ? C71 C67 C68 C69 2.8(17) . . . . ? C64 C67 C68 C69 -174.1(10) . . . . ? C67 C68 C69 N8 -2.8(19) . . . . ? N8 C70 C71 C67 0.3(18) . . . . ? C68 C67 C71 C70 -1.6(16) . . . . ? C64 C67 C71 C70 175.3(10) . . . . ? N5 C72 C73 C74 1.2(17) . . . . ? C72 C73 C74 C75 -1.6(15) . . . . ? C72 C73 C74 C79 177.3(10) . . . . ? C73 C74 C75 C76 2.5(16) . . . . ? C79 C74 C75 C76 -176.4(10) . . . . ? C74 C75 C76 N5 -3.1(18) . . . . ? N6 C77 C78 C79 -0.1(16) . . . . ? C77 C78 C79 C80 2.0(15) . . . . ? C77 C78 C79 C74 -176.2(9) . . . . ? C75 C74 C79 C80 24.3(15) . . . . ? C73 C74 C79 C80 -154.6(10) . . . . ? C75 C74 C79 C78 -157.6(10) . . . . ? C73 C74 C79 C78 23.5(15) . . . . ? C78 C79 C80 C81 -2.3(15) . . . . ? C74 C79 C80 C81 175.9(9) . . . . ? C79 C80 C81 N6 0.7(16) . . . . ? O27 C87 C88 O28 61(2) . . . . ? C38 C37 N1 C41 -1.2(19) . . . . ? C38 C37 N1 Cd1 168.7(10) . . . . ? C40 C41 N1 C37 2(2) . . . . ? C40 C41 N1 Cd1 -169.1(12) . . . . ? O7 Cd1 N1 C37 118.9(9) . . . . ? O6 Cd1 N1 C37 36.3(10) . . . . ? O21 Cd1 N1 C37 -100.9(10) 1_455 . . . ? O22 Cd1 N1 C37 -107.3(10) 1_455 . . . ? O5 Cd1 N1 C37 -12.5(9) . . . . ? O8 Cd1 N1 C37 166.8(9) . . . . ? C26 Cd1 N1 C37 -104.5(9) 1_455 . . . ? O7 Cd1 N1 C41 -71.3(10) . . . . ? O6 Cd1 N1 C41 -153.9(9) . . . . ? O21 Cd1 N1 C41 69.0(10) 1_455 . . . ? O22 Cd1 N1 C41 62.6(9) 1_455 . . . ? O5 Cd1 N1 C41 157.3(9) . . . . ? O8 Cd1 N1 C41 -23.3(9) . . . . ? C26 Cd1 N1 C41 65.4(10) 1_455 . . . ? C45 C46 N2 C42 -1(2) . . . . ? C45 C46 N2 Cd4 179.8(11) . . . 2_656 ? C43 C42 N2 C46 4(2) . . . . ? C43 C42 N2 Cd4 -177.4(11) . . . 2_656 ? C48 C47 N3 C51 3.0(19) . . . . ? C48 C47 N3 Cd5 -159.5(11) . . . 2_656 ? C50 C51 N3 C47 -1.8(18) . . . . ? C50 C51 N3 Cd5 159.9(9) . . . 2_656 ? C55 C56 N4 C52 0(2) . . . . ? C55 C56 N4 Cd3 176.3(10) . . . . ? C53 C52 N4 C56 1(2) . . . . ? C53 C52 N4 Cd3 -176.0(14) . . . . ? O13 Cd3 N4 C56 -14.8(11) . . . . ? O20 Cd3 N4 C56 -121.0(11) . . . . ? N5 Cd3 N4 C56 -80(2) . . . . ? O11 Cd3 N4 C56 72.7(11) . . . . ? O10 Cd3 N4 C56 142.6(11) . . . . ? O13 Cd3 N4 C52 161.4(11) . . . . ? O20 Cd3 N4 C52 55.2(11) . . . . ? N5 Cd3 N4 C52 96(2) . . . . ? O11 Cd3 N4 C52 -111.2(11) . . . . ? O10 Cd3 N4 C52 -41.2(11) . . . . ? C73 C72 N5 C76 -1.5(16) . . . . ? C73 C72 N5 Cd3 -176.1(8) . . . . ? C75 C76 N5 C72 2.5(17) . . . . ? C75 C76 N5 Cd3 177.4(9) . . . . ? O13 Cd3 N5 C72 -153.7(9) . . . . ? O20 Cd3 N5 C72 -47.4(9) . . . . ? N4 Cd3 N5 C72 -88(2) . . . . ? O11 Cd3 N5 C72 118.0(9) . . . . ? O10 Cd3 N5 C72 46.9(9) . . . . ? O13 Cd3 N5 C76 31.9(8) . . . . ? O20 Cd3 N5 C76 138.1(8) . . . . ? N4 Cd3 N5 C76 97.2(19) . . . . ? O11 Cd3 N5 C76 -56.5(8) . . . . ? O10 Cd3 N5 C76 -127.6(8) . . . . ? C80 C81 N6 C77 1.3(16) . . . . ? C80 C81 N6 Cd2 -169.2(8) . . . 2_755 ? C78 C77 N6 C81 -1.6(16) . . . . ? C78 C77 N6 Cd2 169.8(8) . . . 2_755 ? C63 C62 N7 C66 2.4(16) . . . . ? C63 C62 N7 Cd4 179.4(8) . . . . ? C65 C66 N7 C62 -0.5(15) . . . . ? C65 C66 N7 Cd4 -177.5(8) . . . . ? O17 Cd4 N7 C62 -16.2(8) . . . . ? O24 Cd4 N7 C62 -137.5(8) 1_545 . . . ? N2 Cd4 N7 C62 -103.6(15) 2_656 . . . ? O1 Cd4 N7 C62 62.0(8) 1_545 . . . ? O4 Cd4 N7 C62 137.5(8) 1_545 . . . ? O17 Cd4 N7 C66 160.6(8) . . . . ? O24 Cd4 N7 C66 39.4(8) 1_545 . . . ? N2 Cd4 N7 C66 73.3(17) 2_656 . . . ? O1 Cd4 N7 C66 -121.1(8) 1_545 . . . ? O4 Cd4 N7 C66 -45.7(8) 1_545 . . . ? C71 C70 N8 C69 -0.1(17) . . . . ? C71 C70 N8 Cd6 -173.1(8) . . . 2_755 ? C68 C69 N8 C70 1.3(17) . . . . ? C68 C69 N8 Cd6 174.3(9) . . . 2_755 ? C58 C57 N9 C61 3.7(19) . . . . ? C58 C57 N9 Cd2 -174.5(10) . . . . ? C60 C61 N9 C57 -3.7(19) . . . . ? C60 C61 N9 Cd2 174.5(10) . . . . ? O18 Cd2 N9 C57 -27.7(10) . . . . ? O23 Cd2 N9 C57 -138.6(10) 1_545 . . . ? N6 Cd2 N9 C57 -123.6(15) 2_755 . . . ? O5 Cd2 N9 C57 136.7(10) 1_645 . . . ? O3 Cd2 N9 C57 63.2(10) 1_645 . . . ? O18 Cd2 N9 C61 154.2(9) . . . . ? O23 Cd2 N9 C61 43.3(9) 1_545 . . . ? N6 Cd2 N9 C61 58.3(19) 2_755 . . . ? O5 Cd2 N9 C61 -41.4(9) 1_645 . . . ? O3 Cd2 N9 C61 -114.9(9) 1_645 . . . ? O2 C1 O1 Cd4 -141.4(9) . . . 1_565 ? C2 C1 O1 Cd4 36.8(12) . . . 1_565 ? O1 C1 O2 Cd5 7.0(13) . . . 1_565 ? C2 C1 O2 Cd5 -171.3(6) . . . 1_565 ? O4 C9 O3 Cd2 -128.8(8) . . . 1_465 ? C7 C9 O3 Cd2 50.2(10) . . . 1_465 ? O3 C9 O4 Cd4 -132.3(8) . . . 1_565 ? C7 C9 O4 Cd4 48.7(10) . . . 1_565 ? O6 C8 O5 Cd2 -148.9(8) . . . 1_465 ? C6 C8 O5 Cd2 29.0(12) . . . 1_465 ? O6 C8 O5 Cd1 -1.1(10) . . . . ? C6 C8 O5 Cd1 176.7(8) . . . . ? O7 Cd1 O5 C8 0.1(7) . . . . ? O6 Cd1 O5 C8 0.6(6) . . . . ? O21 Cd1 O5 C8 -106.6(6) 1_455 . . . ? O22 Cd1 O5 C8 -161.9(5) 1_455 . . . ? N1 Cd1 O5 C8 117.5(6) . . . . ? O8 Cd1 O5 C8 109(3) . . . . ? C26 Cd1 O5 C8 -133.9(6) 1_455 . . . ? O7 Cd1 O5 Cd2 144.2(4) . . . 1_465 ? O6 Cd1 O5 Cd2 144.7(6) . . . 1_465 ? O21 Cd1 O5 Cd2 37.5(4) 1_455 . . 1_465 ? O22 Cd1 O5 Cd2 -17.8(4) 1_455 . . 1_465 ? N1 Cd1 O5 Cd2 -98.4(4) . . . 1_465 ? O8 Cd1 O5 Cd2 -107(3) . . . 1_465 ? C26 Cd1 O5 Cd2 10.2(4) 1_455 . . 1_465 ? O5 C8 O6 Cd1 1.2(11) . . . . ? C6 C8 O6 Cd1 -176.6(7) . . . . ? O7 Cd1 O6 C8 178.9(8) . . . . ? O21 Cd1 O6 C8 79.7(7) 1_455 . . . ? O22 Cd1 O6 C8 29.5(10) 1_455 . . . ? N1 Cd1 O6 C8 -71.1(8) . . . . ? O5 Cd1 O6 C8 -0.7(6) . . . . ? O8 Cd1 O6 C8 -175.4(6) . . . . ? C26 Cd1 O6 C8 61.0(8) 1_455 . . . ? O8 C10 O7 Cd1 0.3(11) . . . . ? C11 C10 O7 Cd1 179.2(7) . . . . ? O6 Cd1 O7 C10 174.3(7) . . . . ? O21 Cd1 O7 C10 -83.7(7) 1_455 . . . ? O22 Cd1 O7 C10 -30.6(8) 1_455 . . . ? N1 Cd1 O7 C10 69.2(7) . . . . ? O5 Cd1 O7 C10 174.7(6) . . . . ? O8 Cd1 O7 C10 -0.1(6) . . . . ? C26 Cd1 O7 C10 -61.8(7) 1_455 . . . ? O7 C10 O8 Cd6 144.4(8) . . . 1_455 ? C11 C10 O8 Cd6 -34.5(12) . . . 1_455 ? O7 C10 O8 Cd1 -0.2(9) . . . . ? C11 C10 O8 Cd1 -179.1(8) . . . . ? O7 Cd1 O8 C10 0.1(5) . . . . ? O6 Cd1 O8 C10 -6.8(7) . . . . ? O21 Cd1 O8 C10 103.7(5) 1_455 . . . ? O22 Cd1 O8 C10 158.6(6) 1_455 . . . ? N1 Cd1 O8 C10 -120.5(6) . . . . ? O5 Cd1 O8 C10 -112(3) . . . . ? C26 Cd1 O8 C10 130.8(6) 1_455 . . . ? O7 Cd1 O8 Cd6 -135.8(6) . . . 1_455 ? O6 Cd1 O8 Cd6 -142.8(5) . . . 1_455 ? O21 Cd1 O8 Cd6 -32.3(5) 1_455 . . 1_455 ? O22 Cd1 O8 Cd6 22.6(4) 1_455 . . 1_455 ? N1 Cd1 O8 Cd6 103.6(5) . . . 1_455 ? O5 Cd1 O8 Cd6 112(3) . . . 1_455 ? C26 Cd1 O8 Cd6 -5.1(5) 1_455 . . 1_455 ? O10 C17 O9 Cd6 135.7(8) . . . 1_455 ? C16 C17 O9 Cd6 -45.8(11) . . . 1_455 ? O9 C17 O10 Cd3 124.9(9) . . . . ? C16 C17 O10 Cd3 -53.6(10) . . . . ? O13 Cd3 O10 C17 -76.9(9) . . . . ? O20 Cd3 O10 C17 138.4(8) . . . . ? N4 Cd3 O10 C17 -136.0(8) . . . . ? N5 Cd3 O10 C17 51.5(8) . . . . ? O11 Cd3 O10 C17 -25.9(7) . . . . ? O12 C18 O11 Cd3 150.7(9) . . . . ? C15 C18 O11 Cd3 -29.7(12) . . . . ? O12 C18 O11 Cd5 0.8(11) . . . . ? C15 C18 O11 Cd5 -179.6(8) . . . . ? O13 Cd3 O11 C18 -121.6(8) . . . . ? O20 Cd3 O11 C18 19.8(14) . . . . ? N4 Cd3 O11 C18 151.3(8) . . . . ? N5 Cd3 O11 C18 -33.5(8) . . . . ? O10 Cd3 O11 C18 78.8(8) . . . . ? O13 Cd3 O11 Cd5 17.1(4) . . . . ? O20 Cd3 O11 Cd5 158.5(7) . . . . ? N4 Cd3 O11 Cd5 -70.0(4) . . . . ? N5 Cd3 O11 Cd5 105.2(4) . . . . ? O10 Cd3 O11 Cd5 -142.5(4) . . . . ? O2 Cd5 O11 C18 -5.9(7) 1_545 . . . ? O16 Cd5 O11 C18 104.2(6) . . . . ? N3 Cd5 O11 C18 -123.2(6) 2_656 . . . ? O12 Cd5 O11 C18 -0.4(6) . . . . ? O15 Cd5 O11 C18 158.7(6) . . . . ? O2 Cd5 O11 Cd3 -155.2(4) 1_545 . . . ? O16 Cd5 O11 Cd3 -45.1(4) . . . . ? N3 Cd5 O11 Cd3 87.4(4) 2_656 . . . ? O12 Cd5 O11 Cd3 -149.8(5) . . . . ? O15 Cd5 O11 Cd3 9.4(4) . . . . ? O11 C18 O12 Cd5 -0.8(11) . . . . ? C15 C18 O12 Cd5 179.6(8) . . . . ? O2 Cd5 O12 C18 176.2(8) 1_545 . . . ? O16 Cd5 O12 C18 -82.9(7) . . . . ? N3 Cd5 O12 C18 67.7(8) 2_656 . . . ? O11 Cd5 O12 C18 0.4(6) . . . . ? O15 Cd5 O12 C18 -38.7(10) . . . . ? O14 C28 O13 Cd3 9.3(17) . . . . ? C29 C28 O13 Cd3 -171.1(7) . . . . ? O20 Cd3 O13 C28 -16.2(10) . . . . ? N4 Cd3 O13 C28 -102.3(10) . . . . ? N5 Cd3 O13 C28 68.2(10) . . . . ? O11 Cd3 O13 C28 152.1(10) . . . . ? O10 Cd3 O13 C28 -159.4(8) . . . . ? O13 C28 O14 Cd6 -20(4) . . . . ? C29 C28 O14 Cd6 161(3) . . . . ? O19 Cd6 O14 C28 7(3) . . . . ? O27 Cd6 O14 C28 92(3) . . . . ? N8 Cd6 O14 C28 -79(3) 2_755 . . . ? O9 Cd6 O14 C28 176(3) 1_655 . . . ? O8 Cd6 O14 C28 -172(3) 1_655 . . . ? O16 C35 O15 Cd5 -1.8(9) . . . . ? C34 C35 O15 Cd5 178.7(8) . . . . ? O2 Cd5 O15 C35 78.7(6) 1_545 . . . ? O16 Cd5 O15 C35 1.1(5) . . . . ? N3 Cd5 O15 C35 -172.4(6) 2_656 . . . ? O12 Cd5 O15 C35 -55.4(8) . . . . ? O11 Cd5 O15 C35 -86.4(6) . . . . ? O15 C35 O16 Cd5 2.0(10) . . . . ? C34 C35 O16 Cd5 -178.4(7) . . . . ? O2 Cd5 O16 C35 -129.7(6) 1_545 . . . ? N3 Cd5 O16 C35 7.7(7) 2_656 . . . ? O12 Cd5 O16 C35 150.4(6) . . . . ? O11 Cd5 O16 C35 96.9(6) . . . . ? O15 Cd5 O16 C35 -1.0(5) . . . . ? O18 C36 O17 Cd4 1.6(17) . . . . ? C33 C36 O17 Cd4 -176.1(7) . . . . ? O24 Cd4 O17 C36 -6.3(10) 1_545 . . . ? N2 Cd4 O17 C36 77.9(9) 2_656 . . . ? N7 Cd4 O17 C36 -88.4(9) . . . . ? O1 Cd4 O17 C36 176.7(10) 1_545 . . . ? O4 Cd4 O17 C36 153.3(7) 1_545 . . . ? O17 C36 O18 Cd2 78(3) . . . . ? C33 C36 O18 Cd2 -104(3) . . . . ? O23 Cd2 O18 C36 -73(3) 1_545 . . . ? N9 Cd2 O18 C36 -157(3) . . . . ? N6 Cd2 O18 C36 11(3) 2_755 . . . ? O5 Cd2 O18 C36 98(3) 1_645 . . . ? O3 Cd2 O18 C36 123(3) 1_645 . . . ? O20 C27 O19 Cd6 -12.8(14) . . . . ? C24 C27 O19 Cd6 165.2(6) . . . . ? O14 Cd6 O19 C27 29.4(9) . . . . ? O27 Cd6 O19 C27 -60.7(8) . . . . ? N8 Cd6 O19 C27 114.4(8) 2_755 . . . ? O9 Cd6 O19 C27 -127.5(8) 1_655 . . . ? O8 Cd6 O19 C27 -150.9(8) 1_655 . . . ? O19 C27 O20 Cd3 -85.6(18) . . . . ? C24 C27 O20 Cd3 96.4(16) . . . . ? O13 Cd3 O20 C27 99.7(16) . . . . ? N4 Cd3 O20 C27 -173.5(16) . . . . ? N5 Cd3 O20 C27 13.3(16) . . . . ? O11 Cd3 O20 C27 -40(2) . . . . ? O10 Cd3 O20 C27 -95.9(16) . . . . ? O22 C26 O21 Cd1 -0.5(9) . . . 1_655 ? C25 C26 O21 Cd1 179.8(8) . . . 1_655 ? O21 C26 O22 Cd1 0.5(9) . . . 1_655 ? C25 C26 O22 Cd1 -179.8(7) . . . 1_655 ? O24 C19 O23 Cd2 6.3(15) . . . 1_565 ? C20 C19 O23 Cd2 -169.4(6) . . . 1_565 ? O23 C19 O24 Cd4 54.5(19) . . . 1_565 ? C20 C19 O24 Cd4 -129.8(12) . . . 1_565 ? C88 C87 O27 Cd6 48(2) . . . . ? O14 Cd6 O27 C87 20.5(13) . . . . ? O19 Cd6 O27 C87 138.8(13) . . . . ? N8 Cd6 O27 C87 108(2) 2_755 . . . ? O9 Cd6 O27 C87 -66.9(13) 1_655 . . . ? O8 Cd6 O27 C87 -141.0(13) 1_655 . . . ? C7 C6 C3 C1A -2.6(14) . . . . ? C8 C6 C3 C1A 177.0(9) . . . . ? C7 C2 C4 C1A -3.0(15) . . . . ? C1 C2 C4 C1A 172.0(9) . . . . ? C16 C11 C5 C13 5.2(16) . . . . ? C10 C11 C5 C13 -173.1(9) . . . . ? C16 C15 C12 C13 2.9(16) . . . . ? C18 C15 C12 C13 -178.1(10) . . . . ? C11 C5 C13 C12 -2.6(17) . . . . ? C15 C12 C13 C5 -1.5(17) . . . . ? C2 C4 C1A C3 1.7(16) . . . . ? C6 C3 C1A C4 1.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.844 _refine_diff_density_min -1.475 _refine_diff_density_rms 0.219 # 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 -0.012 0.000 0.000 308 61 ' ' 2 0.013 0.500 0.000 178 32 ' ' 3 0.099 0.917 0.432 36 7 ' ' 4 0.182 0.782 0.385 7 0 ' ' 5 0.372 0.570 0.555 18 2 ' ' 6 0.627 0.430 0.445 18 2 ' ' 7 0.821 0.209 0.615 10 1 ' ' 8 0.904 0.079 0.566 33 5 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 939639'