# 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_global data_1a #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H66 Gd2 N8 O12' _chemical_formula_weight 1405.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 10.5471(5) _cell_length_b 11.3694(6) _cell_length_c 12.8451(7) _cell_angle_alpha 105.5560(10) _cell_angle_beta 102.6370(10) _cell_angle_gamma 101.9690(10) _cell_volume 1388.74(12) _cell_formula_units_Z 1 _cell_measurement_temperature 191(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 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 2.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6411 _exptl_absorpt_correction_T_max 0.7111 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(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 ? _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 7716 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.15 _reflns_number_total 5416 _reflns_number_gt 4855 _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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5416 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.1028(4) 0.4335(3) 0.1437(3) 0.0264(8) Uani 1 1 d . . . C2 C -0.0123(4) 0.3639(3) 0.0485(3) 0.0280(8) Uani 1 1 d . . . C3 C 0.0014(5) 0.3236(4) -0.0601(4) 0.0356(9) Uani 1 1 d . . . H3 H -0.076(4) 0.277(4) -0.118(3) 0.029(11) Uiso 1 1 d . . . C4 C 0.1244(5) 0.3449(4) -0.0795(4) 0.0413(11) Uani 1 1 d . . . H4 H 0.133(4) 0.318(4) -0.154(4) 0.046(13) Uiso 1 1 d . . . C5 C 0.2394(5) 0.4122(4) 0.0114(4) 0.0363(10) Uani 1 1 d . . . H5 H 0.327(5) 0.434(4) 0.012(4) 0.039(12) Uiso 1 1 d . . . C6 C 0.2295(4) 0.4559(4) 0.1199(3) 0.0308(9) Uani 1 1 d . . . C7 C 0.3691(5) 0.6495(5) 0.2543(5) 0.0449(11) Uani 1 1 d . . . H7A H 0.296(6) 0.671(5) 0.267(4) 0.063(17) Uiso 1 1 d . . . H7B H 0.399(5) 0.680(5) 0.201(4) 0.059(16) Uiso 1 1 d . . . H7C H 0.448(5) 0.684(5) 0.319(4) 0.060(16) Uiso 1 1 d . . . C8 C -0.1481(4) 0.3412(3) 0.0596(3) 0.0274(8) Uani 1 1 d . . . H8 H -0.222(4) 0.320(4) -0.009(3) 0.030(11) Uiso 1 1 d . . . C9 C -0.3230(4) 0.3437(4) 0.1453(3) 0.0273(8) Uani 1 1 d . . . H9A H -0.377(4) 0.339(3) 0.075(3) 0.018(9) Uiso 1 1 d . . . H9B H -0.355(4) 0.277(4) 0.167(3) 0.022(10) Uiso 1 1 d . . . C10 C -0.3297(4) 0.4640(4) 0.2269(3) 0.0263(8) Uani 1 1 d . . . H10A H -0.287(4) 0.532(4) 0.206(3) 0.022(10) Uiso 1 1 d . . . H10B H -0.424(4) 0.463(4) 0.222(3) 0.040(12) Uiso 1 1 d . . . C11 C -0.3496(4) 0.4046(4) 0.3939(3) 0.0289(8) Uani 1 1 d . . . H11A H -0.342(5) 0.327(5) 0.385(4) 0.048(14) Uiso 1 1 d . . . H11B H -0.454(4) 0.398(4) 0.350(3) 0.030(10) Uiso 1 1 d . . . C12 C -0.3104(4) 0.4817(4) 0.5190(3) 0.0256(8) Uani 1 1 d . . . H12A H -0.395(4) 0.491(3) 0.541(3) 0.021(9) Uiso 1 1 d . . . H12B H -0.267(4) 0.442(4) 0.561(4) 0.043(13) Uiso 1 1 d . . . C13 C -0.2385(4) 0.6120(3) 0.4148(3) 0.0210(7) Uani 1 1 d . . . H13 H -0.321(4) 0.633(3) 0.393(3) 0.018(9) Uiso 1 1 d . . . C14 C -0.1253(4) 0.7086(3) 0.4035(3) 0.0212(7) Uani 1 1 d . . . C15 C -0.1517(4) 0.8093(4) 0.3690(3) 0.0284(8) Uani 1 1 d . . . H15 H -0.235(4) 0.814(4) 0.349(3) 0.022(10) Uiso 1 1 d . . . C16 C -0.0496(4) 0.9004(4) 0.3620(3) 0.0345(9) Uani 1 1 d . . . H16 H -0.064(4) 0.966(4) 0.341(3) 0.036(12) Uiso 1 1 d . . . C17 C 0.0837(4) 0.8938(4) 0.3919(3) 0.0323(9) Uani 1 1 d . . . H17 H 0.155(4) 0.955(4) 0.392(3) 0.023(10) Uiso 1 1 d . . . C18 C 0.1115(4) 0.7945(3) 0.4273(3) 0.0258(8) Uani 1 1 d . . . C19 C 0.0075(3) 0.6989(3) 0.4339(3) 0.0210(7) Uani 1 1 d . . . C20 C 0.3494(5) 0.8920(5) 0.4903(5) 0.0456(12) Uani 1 1 d . . . H20A H 0.340(4) 0.973(5) 0.544(4) 0.050(13) Uiso 1 1 d . . . H20B H 0.352(4) 0.916(4) 0.423(4) 0.044(13) Uiso 1 1 d . . . H20C H 0.426(5) 0.866(4) 0.521(4) 0.042(13) Uiso 1 1 d . . . C21 C -0.2603(4) 0.7174(4) 0.5952(3) 0.0256(8) Uani 1 1 d . . . H21A H -0.219(3) 0.787(3) 0.574(3) 0.013(8) Uiso 1 1 d . . . H21B H -0.354(4) 0.702(4) 0.571(3) 0.024(10) Uiso 1 1 d . . . C22 C -0.2068(4) 0.7480(4) 0.7213(3) 0.0271(8) Uani 1 1 d . . . H22A H -0.236(3) 0.816(4) 0.755(3) 0.018(9) Uiso 1 1 d . . . H22B H -0.233(3) 0.676(3) 0.744(3) 0.011(8) Uiso 1 1 d . . . C23 C 0.0075(4) 0.8944(3) 0.8202(3) 0.0255(8) Uani 1 1 d . . . H23 H -0.043(3) 0.947(4) 0.858(3) 0.021(9) Uiso 1 1 d . . . C24 C 0.1526(4) 0.9530(3) 0.8530(3) 0.0274(8) Uani 1 1 d . . . C25 C 0.2071(4) 1.0685(4) 0.9438(3) 0.0344(9) Uani 1 1 d . . . H25 H 0.149(4) 1.096(4) 0.980(3) 0.021(10) Uiso 1 1 d . . . C26 C 0.3416(5) 1.1303(4) 0.9763(4) 0.0413(11) Uani 1 1 d . . . H26 H 0.376(5) 1.201(5) 1.033(4) 0.049(14) Uiso 1 1 d . . . C27 C 0.4257(4) 1.0828(4) 0.9169(4) 0.0364(10) Uani 1 1 d . . . H27 H 0.519(5) 1.118(4) 0.932(4) 0.048(13) Uiso 1 1 d . . . C28 C 0.3739(4) 0.9731(4) 0.8251(3) 0.0303(8) Uani 1 1 d . . . C29 C 0.2346(4) 0.9028(3) 0.7896(3) 0.0260(8) Uani 1 1 d . . . C30 C 0.5856(5) 0.9949(5) 0.7834(5) 0.0425(11) Uani 1 1 d . . . H30A H 0.581(4) 1.068(5) 0.777(4) 0.035(12) Uiso 1 1 d . . . H30B H 0.618(5) 0.947(5) 0.729(4) 0.054(14) Uiso 1 1 d . . . H30C H 0.641(4) 1.012(4) 0.865(4) 0.043(13) Uiso 1 1 d . . . N1 N -0.1810(3) 0.3548(3) 0.1519(2) 0.0250(7) Uani 1 1 d . . . N2 N -0.2592(3) 0.4789(3) 0.3453(2) 0.0215(6) Uani 1 1 d . . . N3 N -0.2199(3) 0.6087(3) 0.5321(2) 0.0204(6) Uani 1 1 d . . . N4 N -0.0581(3) 0.7836(3) 0.7504(2) 0.0245(7) Uani 1 1 d . . . O1 O 0.0958(2) 0.4745(2) 0.2470(2) 0.0246(5) Uani 1 1 d . . . O2 O 0.3477(3) 0.5161(3) 0.2090(2) 0.0358(6) Uani 1 1 d . . . O3 O 0.0357(2) 0.6038(2) 0.46869(19) 0.0189(5) Uani 1 1 d . . . O4 O 0.2401(2) 0.7815(2) 0.4590(2) 0.0328(6) Uani 1 1 d . . . O5 O 0.1900(2) 0.7985(2) 0.7027(2) 0.0268(6) Uani 1 1 d . . . O6 O 0.4508(3) 0.9208(3) 0.7607(2) 0.0370(7) Uani 1 1 d . . . Gd1 Gd -0.032274(16) 0.391020(15) 0.345621(13) 0.01928(7) 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 0.034(2) 0.0239(19) 0.028(2) 0.0122(16) 0.0130(16) 0.0113(16) C2 0.038(2) 0.0257(19) 0.026(2) 0.0112(16) 0.0128(17) 0.0128(16) C3 0.049(3) 0.032(2) 0.027(2) 0.0098(18) 0.013(2) 0.013(2) C4 0.069(3) 0.035(2) 0.028(2) 0.0089(18) 0.029(2) 0.017(2) C5 0.043(3) 0.039(2) 0.041(3) 0.020(2) 0.026(2) 0.018(2) C6 0.036(2) 0.034(2) 0.034(2) 0.0180(18) 0.0177(18) 0.0175(17) C7 0.035(3) 0.046(3) 0.051(3) 0.016(2) 0.011(2) 0.006(2) C8 0.034(2) 0.0238(19) 0.0186(19) 0.0030(15) 0.0016(17) 0.0085(16) C9 0.0244(19) 0.030(2) 0.023(2) 0.0074(17) 0.0025(16) 0.0066(16) C10 0.0194(18) 0.032(2) 0.024(2) 0.0064(16) 0.0022(15) 0.0070(16) C11 0.027(2) 0.026(2) 0.034(2) 0.0099(17) 0.0134(17) 0.0037(16) C12 0.0176(18) 0.028(2) 0.030(2) 0.0098(16) 0.0075(16) 0.0030(15) C13 0.0212(18) 0.0247(18) 0.0174(17) 0.0062(14) 0.0033(14) 0.0106(14) C14 0.0305(19) 0.0179(17) 0.0137(16) 0.0032(13) 0.0059(14) 0.0070(14) C15 0.035(2) 0.030(2) 0.0204(19) 0.0077(16) 0.0049(17) 0.0150(17) C16 0.051(3) 0.027(2) 0.030(2) 0.0158(18) 0.012(2) 0.0129(19) C17 0.041(2) 0.022(2) 0.032(2) 0.0101(17) 0.0139(19) 0.0019(17) C18 0.032(2) 0.0235(19) 0.0219(19) 0.0055(15) 0.0122(16) 0.0054(15) C19 0.0277(18) 0.0219(18) 0.0128(16) 0.0035(13) 0.0077(14) 0.0062(14) C20 0.037(3) 0.035(3) 0.060(3) 0.021(2) 0.010(2) -0.002(2) C21 0.0231(19) 0.030(2) 0.030(2) 0.0120(17) 0.0119(16) 0.0130(16) C22 0.032(2) 0.026(2) 0.028(2) 0.0070(17) 0.0137(17) 0.0143(16) C23 0.036(2) 0.0251(19) 0.0226(19) 0.0097(15) 0.0126(16) 0.0162(16) C24 0.033(2) 0.0235(19) 0.025(2) 0.0079(15) 0.0056(16) 0.0107(16) C25 0.042(2) 0.028(2) 0.030(2) 0.0024(17) 0.0102(19) 0.0124(18) C26 0.047(3) 0.027(2) 0.035(2) -0.0026(19) 0.003(2) 0.0050(19) C27 0.033(2) 0.027(2) 0.036(2) 0.0009(17) 0.0021(19) 0.0008(17) C28 0.033(2) 0.0234(19) 0.033(2) 0.0096(16) 0.0085(17) 0.0057(16) C29 0.031(2) 0.0206(18) 0.0230(19) 0.0066(15) 0.0049(16) 0.0043(15) C30 0.034(2) 0.035(3) 0.060(3) 0.018(2) 0.016(2) 0.009(2) N1 0.0268(16) 0.0236(16) 0.0231(16) 0.0062(13) 0.0051(13) 0.0079(13) N2 0.0201(15) 0.0227(15) 0.0211(16) 0.0058(12) 0.0070(12) 0.0057(12) N3 0.0215(15) 0.0196(15) 0.0202(15) 0.0064(12) 0.0056(12) 0.0068(12) N4 0.0269(16) 0.0244(16) 0.0232(16) 0.0073(13) 0.0082(13) 0.0090(13) O1 0.0255(13) 0.0269(13) 0.0223(13) 0.0078(11) 0.0092(11) 0.0069(10) O2 0.0295(15) 0.0431(17) 0.0441(17) 0.0219(14) 0.0148(13) 0.0150(12) O3 0.0224(12) 0.0157(11) 0.0198(12) 0.0065(9) 0.0077(10) 0.0050(9) O4 0.0232(13) 0.0280(14) 0.0468(17) 0.0143(12) 0.0127(12) 0.0010(11) O5 0.0283(13) 0.0226(13) 0.0253(14) 0.0038(11) 0.0079(11) 0.0036(10) O6 0.0289(14) 0.0291(15) 0.0442(18) 0.0034(12) 0.0110(13) 0.0012(12) Gd1 0.02004(10) 0.01902(10) 0.01829(10) 0.00505(7) 0.00613(7) 0.00537(7) _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 O1 1.308(4) . ? C1 C6 1.423(5) . ? C1 C2 1.424(5) . ? C2 C3 1.396(5) . ? C2 C8 1.447(5) . ? C3 C4 1.358(6) . ? C3 H3 0.92(4) . ? C4 C5 1.392(7) . ? C4 H4 0.95(4) . ? C5 C6 1.384(5) . ? C5 H5 0.90(4) . ? C6 O2 1.391(5) . ? C7 O2 1.420(6) . ? C7 H7A 0.89(5) . ? C7 H7B 0.93(5) . ? C7 H7C 0.96(5) . ? C8 N1 1.286(5) . ? C8 H8 0.97(4) . ? C9 N1 1.458(5) . ? C9 C10 1.510(5) . ? C9 H9A 0.94(4) . ? C9 H9B 0.90(4) . ? C10 N2 1.487(5) . ? C10 H10A 0.95(4) . ? C10 H10B 0.98(4) . ? C11 N2 1.490(5) . ? C11 C12 1.525(5) . ? C11 H11A 0.88(5) . ? C11 H11B 1.10(4) . ? C12 N3 1.501(4) . ? C12 H12A 1.01(4) . ? C12 H12B 0.90(5) . ? C13 N2 1.479(4) . ? C13 N3 1.488(4) . ? C13 C14 1.506(5) . ? C13 H13 0.95(4) . ? C14 C15 1.391(5) . ? C14 C19 1.405(5) . ? C15 C16 1.367(6) . ? C15 H15 0.87(4) . ? C16 C17 1.398(6) . ? C16 H16 0.89(4) . ? C17 C18 1.386(5) . ? C17 H17 0.91(4) . ? C18 O4 1.379(4) . ? C18 C19 1.410(5) . ? C19 O3 1.338(4) . ? C20 O4 1.412(5) . ? C20 H20A 1.03(5) . ? C20 H20B 0.98(5) . ? C20 H20C 0.95(5) . ? C21 N3 1.483(4) . ? C21 C22 1.509(5) . ? C21 H21A 0.96(4) . ? C21 H21B 0.93(4) . ? C22 N4 1.470(5) . ? C22 H22A 0.92(4) . ? C22 H22B 0.95(4) . ? C23 N4 1.277(5) . ? C23 C24 1.452(5) . ? C23 H23 0.98(4) . ? C24 C25 1.409(5) . ? C24 C29 1.414(5) . ? C25 C26 1.360(6) . ? C25 H25 0.91(4) . ? C26 C27 1.391(6) . ? C26 H26 0.87(5) . ? C27 C28 1.376(5) . ? C27 H27 0.94(5) . ? C28 O6 1.387(5) . ? C28 C29 1.425(5) . ? C29 O5 1.304(4) . ? C30 O6 1.417(5) . ? C30 H30A 0.87(5) . ? C30 H30B 0.93(5) . ? C30 H30C 1.03(5) . ? N1 Gd1 2.510(3) . ? N2 Gd1 2.777(3) . ? N3 Gd1 2.777(3) 2_566 ? N4 Gd1 2.521(3) 2_566 ? O1 Gd1 2.278(2) . ? O3 Gd1 2.366(2) . ? O3 Gd1 2.379(2) 2_566 ? O5 Gd1 2.267(2) 2_566 ? Gd1 O5 2.267(2) 2_566 ? Gd1 O3 2.379(2) 2_566 ? Gd1 N4 2.521(3) 2_566 ? Gd1 N3 2.777(3) 2_566 ? Gd1 Gd1 3.8963(4) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 120.9(3) . . ? O1 C1 C2 123.6(3) . . ? C6 C1 C2 115.5(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 C8 117.6(4) . . ? C1 C2 C8 121.2(3) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3 121(2) . . ? C2 C3 H3 117(3) . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 121(3) . . ? C5 C4 H4 120(3) . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 110(3) . . ? C4 C5 H5 129(3) . . ? C5 C6 O2 118.9(3) . . ? C5 C6 C1 121.9(4) . . ? O2 C6 C1 119.1(3) . . ? O2 C7 H7A 113(4) . . ? O2 C7 H7B 103(3) . . ? H7A C7 H7B 114(5) . . ? O2 C7 H7C 109(3) . . ? H7A C7 H7C 114(5) . . ? H7B C7 H7C 103(4) . . ? N1 C8 C2 126.7(3) . . ? N1 C8 H8 116(2) . . ? C2 C8 H8 117(2) . . ? N1 C9 C10 107.9(3) . . ? N1 C9 H9A 114(2) . . ? C10 C9 H9A 105(2) . . ? N1 C9 H9B 108(2) . . ? C10 C9 H9B 109(2) . . ? H9A C9 H9B 113(3) . . ? N2 C10 C9 111.2(3) . . ? N2 C10 H10A 110(2) . . ? C9 C10 H10A 106(2) . . ? N2 C10 H10B 108(2) . . ? C9 C10 H10B 111(2) . . ? H10A C10 H10B 110(3) . . ? N2 C11 C12 105.6(3) . . ? N2 C11 H11A 114(3) . . ? C12 C11 H11A 111(3) . . ? N2 C11 H11B 107(2) . . ? C12 C11 H11B 111(2) . . ? H11A C11 H11B 109(4) . . ? N3 C12 C11 105.7(3) . . ? N3 C12 H12A 111(2) . . ? C11 C12 H12A 109(2) . . ? N3 C12 H12B 111(3) . . ? C11 C12 H12B 110(3) . . ? H12A C12 H12B 109(3) . . ? N2 C13 N3 104.7(3) . . ? N2 C13 C14 114.9(3) . . ? N3 C13 C14 113.5(3) . . ? N2 C13 H13 108(2) . . ? N3 C13 H13 107(2) . . ? C14 C13 H13 109(2) . . ? C15 C14 C19 120.8(3) . . ? C15 C14 C13 120.1(3) . . ? C19 C14 C13 119.0(3) . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 119(3) . . ? C14 C15 H15 120(3) . . ? C15 C16 C17 119.6(4) . . ? C15 C16 H16 123(3) . . ? C17 C16 H16 118(3) . . ? C18 C17 C16 120.0(4) . . ? C18 C17 H17 117(2) . . ? C16 C17 H17 123(2) . . ? O4 C18 C17 123.6(3) . . ? O4 C18 C19 115.1(3) . . ? C17 C18 C19 121.3(4) . . ? O3 C19 C14 122.0(3) . . ? O3 C19 C18 120.7(3) . . ? C14 C19 C18 117.3(3) . . ? O4 C20 H20A 116(3) . . ? O4 C20 H20B 108(3) . . ? H20A C20 H20B 102(4) . . ? O4 C20 H20C 103(3) . . ? H20A C20 H20C 113(4) . . ? H20B C20 H20C 115(4) . . ? N3 C21 C22 111.7(3) . . ? N3 C21 H21A 104(2) . . ? C22 C21 H21A 109(2) . . ? N3 C21 H21B 110(2) . . ? C22 C21 H21B 113(2) . . ? H21A C21 H21B 108(3) . . ? N4 C22 C21 107.3(3) . . ? N4 C22 H22A 111(2) . . ? C21 C22 H22A 107(2) . . ? N4 C22 H22B 106(2) . . ? C21 C22 H22B 112(2) . . ? H22A C22 H22B 113(3) . . ? N4 C23 C24 127.0(3) . . ? N4 C23 H23 118(2) . . ? C24 C23 H23 115(2) . . ? C25 C24 C29 120.9(4) . . ? C25 C24 C23 117.7(3) . . ? C29 C24 C23 121.2(3) . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25 123(2) . . ? C24 C25 H25 116(2) . . ? C25 C26 C27 120.1(4) . . ? C25 C26 H26 121(3) . . ? C27 C26 H26 119(3) . . ? C28 C27 C26 120.4(4) . . ? C28 C27 H27 113(3) . . ? C26 C27 H27 127(3) . . ? C27 C28 O6 123.9(4) . . ? C27 C28 C29 121.6(4) . . ? O6 C28 C29 114.5(3) . . ? O5 C29 C24 124.1(3) . . ? O5 C29 C28 119.6(3) . . ? C24 C29 C28 116.3(3) . . ? O6 C30 H30A 107(3) . . ? O6 C30 H30B 104(3) . . ? H30A C30 H30B 114(4) . . ? O6 C30 H30C 111(3) . . ? H30A C30 H30C 107(4) . . ? H30B C30 H30C 114(4) . . ? C8 N1 C9 117.5(3) . . ? C8 N1 Gd1 128.2(3) . . ? C9 N1 Gd1 114.3(2) . . ? C13 N2 C10 107.4(3) . . ? C13 N2 C11 102.8(3) . . ? C10 N2 C11 111.0(3) . . ? C13 N2 Gd1 117.9(2) . . ? C10 N2 Gd1 108.34(19) . . ? C11 N2 Gd1 109.4(2) . . ? C21 N3 C13 107.2(3) . . ? C21 N3 C12 113.1(3) . . ? C13 N3 C12 104.8(3) . . ? C21 N3 Gd1 109.6(2) . 2_566 ? C13 N3 Gd1 118.61(19) . 2_566 ? C12 N3 Gd1 103.5(2) . 2_566 ? C23 N4 C22 117.8(3) . . ? C23 N4 Gd1 128.8(2) . 2_566 ? C22 N4 Gd1 113.4(2) . 2_566 ? C1 O1 Gd1 133.4(2) . . ? C6 O2 C7 113.0(3) . . ? C19 O3 Gd1 122.2(2) . . ? C19 O3 Gd1 118.38(19) . 2_566 ? Gd1 O3 Gd1 110.40(9) . 2_566 ? C18 O4 C20 116.8(3) . . ? C29 O5 Gd1 135.2(2) . 2_566 ? C28 O6 C30 116.7(3) . . ? O5 Gd1 O1 131.56(9) 2_566 . ? O5 Gd1 O3 142.27(8) 2_566 . ? O1 Gd1 O3 83.67(8) . . ? O5 Gd1 O3 82.44(8) 2_566 2_566 ? O1 Gd1 O3 142.95(8) . 2_566 ? O3 Gd1 O3 69.60(9) . 2_566 ? O5 Gd1 N1 73.96(9) 2_566 . ? O1 Gd1 N1 71.01(9) . . ? O3 Gd1 N1 114.72(9) . . ? O3 Gd1 N1 143.30(9) 2_566 . ? O5 Gd1 N4 71.26(9) 2_566 2_566 ? O1 Gd1 N4 73.81(9) . 2_566 ? O3 Gd1 N4 142.71(9) . 2_566 ? O3 Gd1 N4 112.94(9) 2_566 2_566 ? N1 Gd1 N4 85.82(9) . 2_566 ? O5 Gd1 N3 112.16(9) 2_566 2_566 ? O1 Gd1 N3 81.32(8) . 2_566 ? O3 Gd1 N3 82.34(8) . 2_566 ? O3 Gd1 N3 70.39(8) 2_566 2_566 ? N1 Gd1 N3 144.79(9) . 2_566 ? N4 Gd1 N3 65.40(9) 2_566 2_566 ? O5 Gd1 N2 81.39(9) 2_566 . ? O1 Gd1 N2 112.38(9) . . ? O3 Gd1 N2 70.87(8) . . ? O3 Gd1 N2 83.20(8) 2_566 . ? N1 Gd1 N2 65.99(9) . . ? N4 Gd1 N2 145.32(9) 2_566 . ? N3 Gd1 N2 147.64(8) 2_566 . ? O5 Gd1 Gd1 113.58(6) 2_566 2_566 ? O1 Gd1 Gd1 114.85(6) . 2_566 ? O3 Gd1 Gd1 34.90(5) . 2_566 ? O3 Gd1 Gd1 34.70(5) 2_566 2_566 ? N1 Gd1 Gd1 138.03(7) . 2_566 ? N4 Gd1 Gd1 136.15(7) 2_566 2_566 ? N3 Gd1 Gd1 73.39(6) 2_566 2_566 ? N2 Gd1 Gd1 74.26(6) . 2_566 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.744 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 921077' ####################################################################### # # 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_global # Attachment '1.cif' data_1b #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H66 N8 O12 Tb2' _chemical_formula_weight 1409.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 10.5341(4) _cell_length_b 11.3689(5) _cell_length_c 12.8170(6) _cell_angle_alpha 105.5600(10) _cell_angle_beta 102.8740(10) _cell_angle_gamma 101.8150(10) _cell_volume 1383.19(10) _cell_formula_units_Z 1 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6104 _exptl_absorpt_correction_T_max 0.6957 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(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 ? _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 7686 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.08 _reflns_number_total 5385 _reflns_number_gt 4779 _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^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5385 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.1031(4) 0.4347(4) 0.1449(3) 0.0243(9) Uani 1 1 d . . . C2 C -0.0119(4) 0.3637(4) 0.0493(3) 0.0268(9) Uani 1 1 d . . . C3 C 0.0024(5) 0.3230(4) -0.0602(4) 0.0330(10) Uani 1 1 d . . . H3 H -0.074(4) 0.284(4) -0.116(4) 0.019(11) Uiso 1 1 d . . . C4 C 0.1264(5) 0.3468(5) -0.0779(4) 0.0394(12) Uani 1 1 d . . . H4 H 0.132(5) 0.315(4) -0.150(4) 0.040(13) Uiso 1 1 d . . . C5 C 0.2414(5) 0.4148(5) 0.0145(4) 0.0358(11) Uani 1 1 d . . . H5 H 0.332(5) 0.431(5) 0.009(4) 0.051(15) Uiso 1 1 d . . . C6 C 0.2309(4) 0.4583(4) 0.1227(4) 0.0298(10) Uani 1 1 d . . . C7 C 0.3694(6) 0.6520(5) 0.2560(5) 0.0414(12) Uani 1 1 d . . . H7A H 0.290(5) 0.672(4) 0.264(4) 0.034(13) Uiso 1 1 d . . . H7B H 0.398(5) 0.697(5) 0.200(4) 0.047(14) Uiso 1 1 d . . . H7C H 0.444(5) 0.682(5) 0.317(4) 0.040(14) Uiso 1 1 d . . . C8 C -0.1480(4) 0.3404(4) 0.0601(3) 0.0243(9) Uani 1 1 d . . . H8 H -0.224(4) 0.316(4) -0.016(4) 0.037(13) Uiso 1 1 d . . . C9 C -0.3234(4) 0.3427(4) 0.1440(3) 0.0247(9) Uani 1 1 d . . . H9A H -0.380(4) 0.336(4) 0.063(3) 0.017(10) Uiso 1 1 d . . . H9B H -0.364(4) 0.270(4) 0.167(3) 0.015(10) Uiso 1 1 d . . . C10 C -0.3294(4) 0.4624(4) 0.2256(3) 0.0245(9) Uani 1 1 d . . . H10A H -0.287(4) 0.537(4) 0.211(3) 0.019(10) Uiso 1 1 d . . . H10B H -0.425(4) 0.463(4) 0.221(4) 0.030(12) Uiso 1 1 d . . . C11 C -0.3500(4) 0.4033(4) 0.3934(4) 0.0259(9) Uani 1 1 d . . . H11A H -0.344(4) 0.329(4) 0.386(4) 0.026(12) Uiso 1 1 d . . . H11B H -0.448(4) 0.399(4) 0.353(4) 0.027(11) Uiso 1 1 d . . . C12 C -0.3100(4) 0.4814(4) 0.5182(4) 0.0243(9) Uani 1 1 d . . . H12A H -0.392(4) 0.493(4) 0.538(4) 0.037(13) Uiso 1 1 d . . . H12B H -0.274(4) 0.441(4) 0.563(3) 0.019(11) Uiso 1 1 d . . . C13 C -0.2390(4) 0.6111(4) 0.4141(3) 0.0216(8) Uani 1 1 d . . . H13 H -0.325(4) 0.635(3) 0.385(3) 0.015(10) Uiso 1 1 d . . . C14 C -0.1268(4) 0.7068(4) 0.4033(3) 0.0213(8) Uani 1 1 d . . . C15 C -0.1532(4) 0.8077(4) 0.3681(3) 0.0266(9) Uani 1 1 d . . . H15 H -0.246(4) 0.811(4) 0.345(3) 0.017(10) Uiso 1 1 d . . . C16 C -0.0509(5) 0.8991(4) 0.3619(4) 0.0329(11) Uani 1 1 d . . . H16 H -0.066(4) 0.963(4) 0.338(3) 0.022(11) Uiso 1 1 d . . . C17 C 0.0825(5) 0.8931(4) 0.3918(4) 0.0297(10) Uani 1 1 d . . . H17 H 0.156(4) 0.958(4) 0.389(4) 0.032(12) Uiso 1 1 d . . . C18 C 0.1104(4) 0.7939(4) 0.4276(3) 0.0236(9) Uani 1 1 d . . . C19 C 0.0074(4) 0.6982(4) 0.4339(3) 0.0205(8) Uani 1 1 d . . . C20 C 0.3493(5) 0.8920(5) 0.4897(5) 0.0426(13) Uani 1 1 d . . . H20A H 0.333(5) 0.951(5) 0.544(5) 0.051(17) Uiso 1 1 d . . . H20B H 0.350(5) 0.918(5) 0.421(4) 0.051(15) Uiso 1 1 d . . . H20C H 0.427(5) 0.872(5) 0.527(4) 0.046(15) Uiso 1 1 d . . . C21 C -0.2610(4) 0.7163(4) 0.5949(3) 0.0244(9) Uani 1 1 d . . . H21A H -0.220(4) 0.792(4) 0.580(3) 0.016(10) Uiso 1 1 d . . . H21B H -0.358(4) 0.697(4) 0.568(3) 0.028(11) Uiso 1 1 d . . . C22 C -0.2064(4) 0.7471(4) 0.7210(4) 0.0259(9) Uani 1 1 d . . . H22A H -0.236(4) 0.818(4) 0.754(4) 0.031(12) Uiso 1 1 d . . . H22B H -0.232(4) 0.676(4) 0.744(3) 0.021(11) Uiso 1 1 d . . . C23 C 0.0076(4) 0.8929(4) 0.8204(3) 0.0244(9) Uani 1 1 d . . . H23 H -0.041(3) 0.939(3) 0.855(3) 0.008(9) Uiso 1 1 d . . . C24 C 0.1530(4) 0.9514(4) 0.8530(3) 0.0271(9) Uani 1 1 d . . . C25 C 0.2073(5) 1.0671(4) 0.9438(4) 0.0342(11) Uani 1 1 d . . . H25 H 0.148(3) 1.100(3) 0.984(3) 0.009(9) Uiso 1 1 d . . . C26 C 0.3414(5) 1.1301(5) 0.9751(4) 0.0421(12) Uani 1 1 d . . . H26 H 0.377(4) 1.202(4) 1.033(4) 0.023(11) Uiso 1 1 d . . . C27 C 0.4254(5) 1.0821(4) 0.9148(4) 0.0365(11) Uani 1 1 d . . . H27 H 0.521(4) 1.121(4) 0.935(4) 0.030(12) Uiso 1 1 d . . . C28 C 0.3740(4) 0.9724(4) 0.8234(4) 0.0284(9) Uani 1 1 d . . . C29 C 0.2345(4) 0.9003(4) 0.7892(3) 0.0238(9) Uani 1 1 d . . . C30 C 0.5840(5) 0.9927(5) 0.7818(5) 0.0420(12) Uani 1 1 d . . . H30A H 0.583(5) 1.066(5) 0.769(4) 0.050(16) Uiso 1 1 d . . . H30B H 0.615(5) 0.942(5) 0.728(4) 0.048(15) Uiso 1 1 d . . . H30C H 0.644(5) 1.010(4) 0.863(4) 0.041(13) Uiso 1 1 d . . . N1 N -0.1805(3) 0.3547(3) 0.1519(3) 0.0233(7) Uani 1 1 d . . . N2 N -0.2596(3) 0.4782(3) 0.3448(3) 0.0199(7) Uani 1 1 d . . . N3 N -0.2201(3) 0.6081(3) 0.5314(3) 0.0207(7) Uani 1 1 d . . . N4 N -0.0581(3) 0.7820(3) 0.7505(3) 0.0226(7) Uani 1 1 d . . . O1 O 0.0955(3) 0.4753(3) 0.2487(2) 0.0238(6) Uani 1 1 d . . . O2 O 0.3485(3) 0.5193(3) 0.2122(3) 0.0347(7) Uani 1 1 d . . . O3 O 0.0353(2) 0.6028(2) 0.4692(2) 0.0178(5) Uani 1 1 d . . . O4 O 0.2396(3) 0.7817(3) 0.4607(3) 0.0302(7) Uani 1 1 d . . . O5 O 0.1882(3) 0.7964(3) 0.7022(2) 0.0239(6) Uani 1 1 d . . . O6 O 0.4499(3) 0.9197(3) 0.7596(3) 0.0358(7) Uani 1 1 d . . . Tb1 Tb -0.032129(18) 0.391685(17) 0.345863(15) 0.01835(7) 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 0.031(2) 0.029(2) 0.021(2) 0.0126(18) 0.0137(18) 0.0144(19) C2 0.036(2) 0.027(2) 0.022(2) 0.0114(18) 0.0121(19) 0.0116(19) C3 0.047(3) 0.032(3) 0.021(2) 0.009(2) 0.012(2) 0.011(2) C4 0.060(3) 0.038(3) 0.028(3) 0.010(2) 0.025(3) 0.019(3) C5 0.047(3) 0.037(3) 0.044(3) 0.022(2) 0.033(3) 0.022(2) C6 0.032(2) 0.035(2) 0.033(2) 0.018(2) 0.017(2) 0.015(2) C7 0.032(3) 0.042(3) 0.045(3) 0.013(3) 0.004(3) 0.008(2) C8 0.033(2) 0.018(2) 0.019(2) 0.0040(17) 0.0043(18) 0.0084(18) C9 0.020(2) 0.030(2) 0.018(2) 0.0048(18) -0.0001(17) 0.0041(18) C10 0.021(2) 0.034(2) 0.020(2) 0.0092(19) 0.0057(17) 0.0099(19) C11 0.023(2) 0.024(2) 0.028(2) 0.0075(19) 0.0116(19) 0.0008(18) C12 0.017(2) 0.031(2) 0.026(2) 0.0114(19) 0.0077(18) 0.0068(18) C13 0.021(2) 0.027(2) 0.019(2) 0.0064(17) 0.0067(16) 0.0117(17) C14 0.025(2) 0.020(2) 0.0157(19) 0.0028(16) 0.0039(16) 0.0069(17) C15 0.029(2) 0.030(2) 0.021(2) 0.0070(18) 0.0058(18) 0.0119(19) C16 0.052(3) 0.025(2) 0.028(2) 0.014(2) 0.012(2) 0.017(2) C17 0.042(3) 0.023(2) 0.028(2) 0.0118(19) 0.017(2) 0.006(2) C18 0.028(2) 0.025(2) 0.0181(19) 0.0058(17) 0.0100(17) 0.0055(18) C19 0.028(2) 0.020(2) 0.0141(18) 0.0043(16) 0.0080(16) 0.0081(17) C20 0.031(3) 0.037(3) 0.051(3) 0.015(3) 0.009(3) -0.006(2) C21 0.023(2) 0.029(2) 0.023(2) 0.0063(19) 0.0079(18) 0.0124(19) C22 0.029(2) 0.028(2) 0.023(2) 0.0071(19) 0.0096(18) 0.015(2) C23 0.034(2) 0.025(2) 0.019(2) 0.0069(18) 0.0125(18) 0.0123(19) C24 0.036(2) 0.023(2) 0.022(2) 0.0090(18) 0.0054(18) 0.0089(19) C25 0.041(3) 0.029(2) 0.029(2) 0.002(2) 0.011(2) 0.011(2) C26 0.045(3) 0.028(3) 0.035(3) -0.007(2) 0.000(2) 0.007(2) C27 0.029(3) 0.026(2) 0.044(3) 0.006(2) 0.005(2) 0.000(2) C28 0.028(2) 0.023(2) 0.032(2) 0.0096(19) 0.0062(19) 0.0046(18) C29 0.032(2) 0.018(2) 0.022(2) 0.0073(17) 0.0078(18) 0.0071(17) C30 0.031(3) 0.036(3) 0.054(4) 0.013(3) 0.010(3) 0.004(2) N1 0.0254(18) 0.0200(17) 0.0209(17) 0.0040(14) 0.0035(14) 0.0062(14) N2 0.0192(16) 0.0224(17) 0.0156(16) 0.0038(14) 0.0044(13) 0.0048(14) N3 0.0207(17) 0.0212(17) 0.0211(17) 0.0064(14) 0.0090(14) 0.0054(14) N4 0.0261(18) 0.0252(19) 0.0173(16) 0.0057(15) 0.0079(14) 0.0091(15) O1 0.0252(15) 0.0302(16) 0.0190(14) 0.0099(12) 0.0094(12) 0.0085(12) O2 0.0258(16) 0.0449(19) 0.0409(19) 0.0200(16) 0.0137(14) 0.0137(14) O3 0.0195(13) 0.0191(14) 0.0170(13) 0.0073(11) 0.0069(11) 0.0066(11) O4 0.0219(15) 0.0280(16) 0.0404(18) 0.0127(14) 0.0109(13) 0.0022(13) O5 0.0262(15) 0.0231(15) 0.0202(14) 0.0036(12) 0.0079(12) 0.0055(12) O6 0.0284(16) 0.0301(17) 0.0427(19) 0.0037(15) 0.0140(14) 0.0020(14) Tb1 0.01908(11) 0.02033(11) 0.01552(10) 0.00475(8) 0.00620(7) 0.00561(7) _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 O1 1.313(4) . ? C1 C2 1.424(6) . ? C1 C6 1.425(6) . ? C2 C3 1.408(6) . ? C2 C8 1.448(6) . ? C3 C4 1.361(7) . ? C3 H3 0.88(4) . ? C4 C5 1.397(7) . ? C4 H4 0.91(5) . ? C5 C6 1.379(6) . ? C5 H5 0.95(5) . ? C6 O2 1.385(5) . ? C7 O2 1.412(6) . ? C7 H7A 0.94(4) . ? C7 H7B 1.05(5) . ? C7 H7C 0.91(5) . ? C8 N1 1.276(5) . ? C8 H8 1.04(5) . ? C9 N1 1.461(5) . ? C9 C10 1.501(6) . ? C9 H9A 1.04(4) . ? C9 H9B 1.00(4) . ? C10 N2 1.485(5) . ? C10 H10A 0.96(4) . ? C10 H10B 1.00(4) . ? C11 N2 1.495(5) . ? C11 C12 1.519(6) . ? C11 H11A 0.84(4) . ? C11 H11B 1.03(4) . ? C12 N3 1.497(5) . ? C12 H12A 0.98(4) . ? C12 H12B 0.89(4) . ? C13 N2 1.476(5) . ? C13 N3 1.483(5) . ? C13 C14 1.493(5) . ? C13 H13 1.02(4) . ? C14 C15 1.396(6) . ? C14 C19 1.411(5) . ? C15 C16 1.368(6) . ? C15 H15 0.97(4) . ? C16 C17 1.393(6) . ? C16 H16 0.89(4) . ? C17 C18 1.386(6) . ? C17 H17 0.97(4) . ? C18 O4 1.380(5) . ? C18 C19 1.404(5) . ? C19 O3 1.342(4) . ? C20 O4 1.418(5) . ? C20 H20A 0.90(5) . ? C20 H20B 1.01(5) . ? C20 H20C 0.96(5) . ? C21 N3 1.482(5) . ? C21 C22 1.506(6) . ? C21 H21A 0.97(4) . ? C21 H21B 0.96(4) . ? C22 N4 1.464(5) . ? C22 H22A 0.95(4) . ? C22 H22B 0.94(4) . ? C23 N4 1.278(5) . ? C23 C24 1.453(6) . ? C23 H23 0.91(3) . ? C24 C25 1.409(6) . ? C24 C29 1.417(5) . ? C25 C26 1.359(7) . ? C25 H25 0.97(3) . ? C26 C27 1.398(7) . ? C26 H26 0.89(4) . ? C27 C28 1.370(6) . ? C27 H27 0.96(4) . ? C28 O6 1.376(5) . ? C28 C29 1.431(6) . ? C29 O5 1.301(5) . ? C30 O6 1.407(6) . ? C30 H30A 0.89(6) . ? C30 H30B 0.94(5) . ? C30 H30C 1.03(5) . ? N1 Tb1 2.497(3) . ? N2 Tb1 2.769(3) . ? N3 Tb1 2.769(3) 2_566 ? N4 Tb1 2.512(3) 2_566 ? O1 Tb1 2.263(3) . ? O3 Tb1 2.351(2) . ? O3 Tb1 2.362(2) 2_566 ? O5 Tb1 2.249(3) 2_566 ? Tb1 O5 2.249(3) 2_566 ? Tb1 O3 2.362(2) 2_566 ? Tb1 N4 2.512(3) 2_566 ? Tb1 N3 2.769(3) 2_566 ? Tb1 Tb1 3.8782(4) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 123.3(4) . . ? O1 C1 C6 120.5(4) . . ? C2 C1 C6 116.1(4) . . ? C3 C2 C1 120.8(4) . . ? C3 C2 C8 117.8(4) . . ? C1 C2 C8 121.2(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 123(3) . . ? C2 C3 H3 116(3) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 119(3) . . ? C5 C4 H4 122(3) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 H5 115(3) . . ? C4 C5 H5 124(3) . . ? C5 C6 O2 118.9(4) . . ? C5 C6 C1 121.5(4) . . ? O2 C6 C1 119.5(4) . . ? O2 C7 H7A 112(3) . . ? O2 C7 H7B 111(3) . . ? H7A C7 H7B 105(4) . . ? O2 C7 H7C 106(3) . . ? H7A C7 H7C 119(4) . . ? H7B C7 H7C 104(4) . . ? N1 C8 C2 126.6(4) . . ? N1 C8 H8 119(2) . . ? C2 C8 H8 114(2) . . ? N1 C9 C10 107.1(3) . . ? N1 C9 H9A 112(2) . . ? C10 C9 H9A 107(2) . . ? N1 C9 H9B 111(2) . . ? C10 C9 H9B 108(2) . . ? H9A C9 H9B 111(3) . . ? N2 C10 C9 112.0(3) . . ? N2 C10 H10A 107(2) . . ? C9 C10 H10A 112(2) . . ? N2 C10 H10B 107(2) . . ? C9 C10 H10B 111(2) . . ? H10A C10 H10B 107(3) . . ? N2 C11 C12 104.9(3) . . ? N2 C11 H11A 115(3) . . ? C12 C11 H11A 110(3) . . ? N2 C11 H11B 107(2) . . ? C12 C11 H11B 111(2) . . ? H11A C11 H11B 109(4) . . ? N3 C12 C11 106.4(3) . . ? N3 C12 H12A 109(3) . . ? C11 C12 H12A 109(3) . . ? N3 C12 H12B 115(3) . . ? C11 C12 H12B 112(3) . . ? H12A C12 H12B 106(4) . . ? N2 C13 N3 104.6(3) . . ? N2 C13 C14 115.1(3) . . ? N3 C13 C14 113.3(3) . . ? N2 C13 H13 107(2) . . ? N3 C13 H13 112(2) . . ? C14 C13 H13 105(2) . . ? C15 C14 C19 120.1(4) . . ? C15 C14 C13 120.3(4) . . ? C19 C14 C13 119.6(3) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 120(2) . . ? C14 C15 H15 119(2) . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 122(3) . . ? C17 C16 H16 118(3) . . ? C18 C17 C16 119.5(4) . . ? C18 C17 H17 120(3) . . ? C16 C17 H17 121(3) . . ? O4 C18 C17 123.4(4) . . ? O4 C18 C19 114.8(3) . . ? C17 C18 C19 121.8(4) . . ? O3 C19 C18 121.4(3) . . ? O3 C19 C14 121.1(3) . . ? C18 C19 C14 117.5(4) . . ? O4 C20 H20A 105(3) . . ? O4 C20 H20B 110(3) . . ? H20A C20 H20B 112(4) . . ? O4 C20 H20C 105(3) . . ? H20A C20 H20C 106(5) . . ? H20B C20 H20C 119(4) . . ? N3 C21 C22 111.7(3) . . ? N3 C21 H21A 108(2) . . ? C22 C21 H21A 105(2) . . ? N3 C21 H21B 108(2) . . ? C22 C21 H21B 114(2) . . ? H21A C21 H21B 110(3) . . ? N4 C22 C21 107.7(3) . . ? N4 C22 H22A 111(3) . . ? C21 C22 H22A 105(3) . . ? N4 C22 H22B 106(2) . . ? C21 C22 H22B 112(3) . . ? H22A C22 H22B 115(4) . . ? N4 C23 C24 126.8(4) . . ? N4 C23 H23 117(2) . . ? C24 C23 H23 116(2) . . ? C25 C24 C29 121.2(4) . . ? C25 C24 C23 117.4(4) . . ? C29 C24 C23 121.1(4) . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25 121(2) . . ? C24 C25 H25 119(2) . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26 121(3) . . ? C27 C26 H26 119(3) . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 116(3) . . ? C26 C27 H27 123(3) . . ? C27 C28 O6 124.2(4) . . ? C27 C28 C29 121.5(4) . . ? O6 C28 C29 114.3(3) . . ? O5 C29 C24 123.6(4) . . ? O5 C29 C28 120.3(4) . . ? C24 C29 C28 116.0(4) . . ? O6 C30 H30A 110(3) . . ? O6 C30 H30B 103(3) . . ? H30A C30 H30B 110(5) . . ? O6 C30 H30C 114(3) . . ? H30A C30 H30C 110(4) . . ? H30B C30 H30C 111(4) . . ? C8 N1 C9 117.1(3) . . ? C8 N1 Tb1 128.3(3) . . ? C9 N1 Tb1 114.6(2) . . ? C13 N2 C10 107.8(3) . . ? C13 N2 C11 103.1(3) . . ? C10 N2 C11 111.2(3) . . ? C13 N2 Tb1 117.7(2) . . ? C10 N2 Tb1 107.7(2) . . ? C11 N2 Tb1 109.4(2) . . ? C21 N3 C13 107.5(3) . . ? C21 N3 C12 113.0(3) . . ? C13 N3 C12 104.7(3) . . ? C21 N3 Tb1 109.7(2) . 2_566 ? C13 N3 Tb1 118.6(2) . 2_566 ? C12 N3 Tb1 103.4(2) . 2_566 ? C23 N4 C22 117.6(3) . . ? C23 N4 Tb1 128.8(3) . 2_566 ? C22 N4 Tb1 113.6(2) . 2_566 ? C1 O1 Tb1 133.5(3) . . ? C6 O2 C7 113.2(4) . . ? C19 O3 Tb1 122.0(2) . . ? C19 O3 Tb1 118.5(2) . 2_566 ? Tb1 O3 Tb1 110.74(10) . 2_566 ? C18 O4 C20 117.0(4) . . ? C29 O5 Tb1 135.7(2) . 2_566 ? C28 O6 C30 116.7(4) . . ? O5 Tb1 O1 131.86(9) 2_566 . ? O5 Tb1 O3 142.13(9) 2_566 . ? O1 Tb1 O3 83.63(9) . . ? O5 Tb1 O3 82.44(9) 2_566 2_566 ? O1 Tb1 O3 142.68(9) . 2_566 ? O3 Tb1 O3 69.26(10) . 2_566 ? O5 Tb1 N1 73.93(10) 2_566 . ? O1 Tb1 N1 71.22(10) . . ? O3 Tb1 N1 115.18(9) . . ? O3 Tb1 N1 143.35(10) 2_566 . ? O5 Tb1 N4 71.27(10) 2_566 2_566 ? O1 Tb1 N4 73.79(10) . 2_566 ? O3 Tb1 N4 142.75(10) . 2_566 ? O3 Tb1 N4 113.28(9) 2_566 2_566 ? N1 Tb1 N4 85.38(10) . 2_566 ? O5 Tb1 N3 112.03(10) 2_566 2_566 ? O1 Tb1 N3 81.15(9) . 2_566 ? O3 Tb1 N3 82.27(9) . 2_566 ? O3 Tb1 N3 70.48(9) 2_566 2_566 ? N1 Tb1 N3 144.58(10) . 2_566 ? N4 Tb1 N3 65.50(10) 2_566 2_566 ? O5 Tb1 N2 81.24(9) 2_566 . ? O1 Tb1 N2 112.55(9) . . ? O3 Tb1 N2 71.10(9) . . ? O3 Tb1 N2 83.07(9) 2_566 . ? N1 Tb1 N2 66.16(10) . . ? N4 Tb1 N2 145.05(10) 2_566 . ? N3 Tb1 N2 147.79(9) 2_566 . ? O5 Tb1 Tb1 113.48(7) 2_566 2_566 ? O1 Tb1 Tb1 114.65(7) . 2_566 ? O3 Tb1 Tb1 34.72(6) . 2_566 ? O3 Tb1 Tb1 34.54(6) 2_566 2_566 ? N1 Tb1 Tb1 138.29(7) . 2_566 ? N4 Tb1 Tb1 136.32(7) 2_566 2_566 ? N3 Tb1 Tb1 73.44(6) 2_566 2_566 ? N2 Tb1 Tb1 74.34(6) . 2_566 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.702 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 921078' ####################################################################### # # 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_global # Attachment '1.cif' data_1c #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H78 Dy2 N12 O12' _chemical_formula_weight 1580.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2399(5) _cell_length_b 18.9948(8) _cell_length_c 14.4502(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7800(10) _cell_angle_gamma 90.00 _cell_volume 3342.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 2.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5279 _exptl_absorpt_correction_T_max 0.6574 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(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 ? _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 18462 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.13 _reflns_number_total 6664 _reflns_number_gt 5713 _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^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6664 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.003 _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 Dy1 Dy 0.139398(10) 0.043335(6) 0.036088(8) 0.01648(5) Uani 1 1 d . . . N1 N 0.21297(18) 0.16371(12) 0.07244(16) 0.0223(5) Uani 1 1 d . . . N2 N 0.01698(18) -0.13807(11) -0.08092(15) 0.0182(5) Uani 1 1 d . . . N3 N 0.18651(18) -0.08474(11) -0.03494(15) 0.0189(5) Uani 1 1 d . . . N4 N 0.33504(18) 0.00735(12) 0.07451(16) 0.0226(5) Uani 1 1 d . . . N5 N 0.7953(3) 0.77402(19) 0.3685(3) 0.0698(11) Uani 1 1 d . . . N6 N 0.2175(4) 0.8982(3) 0.5263(3) 0.0970(15) Uani 1 1 d . . . O1 O 0.22478(15) 0.08210(10) -0.08435(13) 0.0233(4) Uani 1 1 d . . . O2 O 0.31873(19) 0.05938(12) -0.23899(15) 0.0360(5) Uani 1 1 d . . . O3 O 0.00882(15) -0.03696(9) 0.07730(12) 0.0167(4) Uani 1 1 d . . . O4 O -0.02790(18) -0.04354(10) 0.25503(14) 0.0281(5) Uani 1 1 d . . . O5 O 0.17921(16) 0.04519(9) 0.19010(13) 0.0228(4) Uani 1 1 d . . . O6 O 0.13443(17) 0.09603(12) 0.35025(14) 0.0347(5) Uani 1 1 d . . . C1 C 0.3100(2) 0.12011(15) -0.09769(19) 0.0228(6) Uani 1 1 d . . . C2 C 0.3638(2) 0.11050(15) -0.1802(2) 0.0269(7) Uani 1 1 d . . . C3 C 0.4533(3) 0.15106(17) -0.1967(2) 0.0351(8) Uani 1 1 d . . . H3 H 0.4878 0.1435 -0.2519 0.042 Uiso 1 1 calc R . . C4 C 0.4938(3) 0.20265(18) -0.1344(2) 0.0384(8) Uani 1 1 d . . . H4 H 0.5558 0.2300 -0.1467 0.046 Uiso 1 1 calc R . . C5 C 0.4437(2) 0.21371(17) -0.0553(2) 0.0339(7) Uani 1 1 d . . . H5 H 0.4710 0.2492 -0.0127 0.041 Uiso 1 1 calc R . . C6 C 0.3525(2) 0.17353(15) -0.03597(19) 0.0248(6) Uani 1 1 d . . . C7 C 0.3476(3) 0.06033(19) -0.3323(2) 0.0417(9) Uani 1 1 d . . . H7A H 0.3316 0.1069 -0.3596 0.063 Uiso 1 1 calc R . . H7B H 0.3048 0.0246 -0.3690 0.063 Uiso 1 1 calc R . . H7C H 0.4261 0.0502 -0.3323 0.063 Uiso 1 1 calc R . . C8 C 0.2936(2) 0.19552(15) 0.04069(19) 0.0247(6) Uani 1 1 d . . . H8 H 0.3171 0.2381 0.0708 0.030 Uiso 1 1 calc R . . C9 C 0.1516(2) 0.20289(15) 0.13791(19) 0.0235(6) Uani 1 1 d . . . H9A H 0.1836 0.2503 0.1493 0.028 Uiso 1 1 calc R . . H9B H 0.1538 0.1776 0.1980 0.028 Uiso 1 1 calc R . . C10 C -0.0347(2) -0.20841(14) -0.0931(2) 0.0252(6) Uani 1 1 d . . . H10A H -0.0345 -0.2316 -0.0317 0.030 Uiso 1 1 calc R . . H10B H 0.0086 -0.2379 -0.1325 0.030 Uiso 1 1 calc R . . C11 C 0.0605(2) -0.11327(15) -0.16878(19) 0.0245(6) Uani 1 1 d . . . H11A H 0.0091 -0.0793 -0.2019 0.029 Uiso 1 1 calc R . . H11B H 0.0707 -0.1535 -0.2106 0.029 Uiso 1 1 calc R . . C12 C 0.1703(2) -0.07808(15) -0.13827(19) 0.0247(6) Uani 1 1 d . . . H12A H 0.2305 -0.1019 -0.1669 0.030 Uiso 1 1 calc R . . H12B H 0.1688 -0.0279 -0.1569 0.030 Uiso 1 1 calc R . . C13 C 0.1168(2) -0.14556(14) -0.01446(19) 0.0198(6) Uani 1 1 d . . . H13 H 0.1556 -0.1897 -0.0302 0.024 Uiso 1 1 calc R . . C14 C 0.0938(2) -0.14993(14) 0.08535(19) 0.0199(6) Uani 1 1 d . . . C15 C 0.1248(2) -0.21005(15) 0.1374(2) 0.0269(7) Uani 1 1 d . . . H15 H 0.1604 -0.2476 0.1090 0.032 Uiso 1 1 calc R . . C16 C 0.1046(2) -0.21555(16) 0.2282(2) 0.0322(7) Uani 1 1 d . . . H16 H 0.1258 -0.2569 0.2625 0.039 Uiso 1 1 calc R . . C17 C 0.0531(2) -0.16070(16) 0.2708(2) 0.0303(7) Uani 1 1 d . . . H17 H 0.0388 -0.1646 0.3340 0.036 Uiso 1 1 calc R . . C18 C 0.0228(2) -0.10039(15) 0.22069(19) 0.0236(6) Uani 1 1 d . . . C19 C 0.0411(2) -0.09461(14) 0.12655(18) 0.0185(6) Uani 1 1 d . . . C20 C -0.0508(3) -0.04625(17) 0.3490(2) 0.0386(8) Uani 1 1 d . . . H20A H -0.0974 -0.0871 0.3582 0.058 Uiso 1 1 calc R . . H20B H -0.0890 -0.0031 0.3644 0.058 Uiso 1 1 calc R . . H20C H 0.0181 -0.0504 0.3894 0.058 Uiso 1 1 calc R . . C21 C 0.3011(2) -0.10330(15) -0.0017(2) 0.0235(6) Uani 1 1 d . . . H21A H 0.3289 -0.1379 -0.0449 0.028 Uiso 1 1 calc R . . H21B H 0.3028 -0.1257 0.0603 0.028 Uiso 1 1 calc R . . C22 C 0.3747(2) -0.03990(14) 0.0049(2) 0.0235(6) Uani 1 1 d . . . H22A H 0.4515 -0.0541 0.0239 0.028 Uiso 1 1 calc R . . H22B H 0.3720 -0.0159 -0.0562 0.028 Uiso 1 1 calc R . . C23 C 0.4007(2) 0.02181(15) 0.1462(2) 0.0238(6) Uani 1 1 d . . . H23 H 0.4751 0.0078 0.1450 0.029 Uiso 1 1 calc R . . C24 C 0.3730(2) 0.05732(15) 0.2288(2) 0.0235(6) Uani 1 1 d . . . C25 C 0.4590(3) 0.07702(16) 0.2968(2) 0.0309(7) Uani 1 1 d . . . H25 H 0.5330 0.0725 0.2833 0.037 Uiso 1 1 calc R . . C26 C 0.4375(3) 0.10229(17) 0.3815(2) 0.0362(8) Uani 1 1 d . . . H26 H 0.4960 0.1155 0.4262 0.043 Uiso 1 1 calc R . . C27 C 0.3286(3) 0.10860(16) 0.4020(2) 0.0309(7) Uani 1 1 d . . . H27 H 0.3135 0.1255 0.4612 0.037 Uiso 1 1 calc R . . C28 C 0.2438(2) 0.09071(15) 0.3375(2) 0.0267(7) Uani 1 1 d . . . C29 C 0.2623(2) 0.06374(14) 0.24799(19) 0.0221(6) Uani 1 1 d . . . C30 C 0.1081(3) 0.1152(2) 0.4400(2) 0.0472(9) Uani 1 1 d . . . H30A H 0.1413 0.0815 0.4858 0.071 Uiso 1 1 calc R . . H30B H 0.0281 0.1149 0.4411 0.071 Uiso 1 1 calc R . . H30C H 0.1365 0.1625 0.4552 0.071 Uiso 1 1 calc R . . C31 C 0.8204(3) 0.7336(2) 0.2022(3) 0.0640(12) Uani 1 1 d . . . H31A H 0.8788 0.6982 0.2047 0.096 Uiso 1 1 calc R . . H31B H 0.8406 0.7739 0.1651 0.096 Uiso 1 1 calc R . . H31C H 0.7517 0.7131 0.1736 0.096 Uiso 1 1 calc R . . C32 C 0.8058(3) 0.7568(2) 0.2954(3) 0.0503(10) Uani 1 1 d . . . C33 C 0.3122(4) 0.9140(2) 0.3775(4) 0.0753(15) Uani 1 1 d . . . H33A H 0.2566 0.9129 0.3238 0.113 Uiso 1 1 calc R . . H33B H 0.3652 0.8759 0.3721 0.113 Uiso 1 1 calc R . . H33C H 0.3505 0.9594 0.3794 0.113 Uiso 1 1 calc R . . C34 C 0.2597(4) 0.9050(2) 0.4620(4) 0.0627(12) 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 Dy1 0.01572(8) 0.01742(8) 0.01637(8) -0.00012(5) 0.00184(5) -0.00150(5) N1 0.0203(13) 0.0230(12) 0.0228(13) -0.0005(10) -0.0022(10) -0.0005(10) N2 0.0182(12) 0.0174(11) 0.0191(12) -0.0038(9) 0.0019(9) -0.0014(10) N3 0.0152(12) 0.0202(12) 0.0218(12) -0.0019(10) 0.0035(9) -0.0010(10) N4 0.0220(13) 0.0226(12) 0.0241(13) -0.0011(10) 0.0070(10) -0.0037(10) N5 0.097(3) 0.051(2) 0.060(2) 0.0070(19) 0.004(2) -0.016(2) N6 0.097(4) 0.108(4) 0.088(4) 0.004(3) 0.019(3) -0.008(3) O1 0.0220(11) 0.0244(10) 0.0240(11) 0.0011(8) 0.0052(8) -0.0035(9) O2 0.0404(14) 0.0424(13) 0.0274(12) -0.0027(10) 0.0136(10) -0.0074(11) O3 0.0163(10) 0.0168(9) 0.0172(10) 0.0014(7) 0.0018(7) -0.0006(7) O4 0.0359(13) 0.0310(12) 0.0188(11) 0.0024(9) 0.0089(9) 0.0028(9) O5 0.0192(11) 0.0293(11) 0.0196(10) -0.0024(8) 0.0010(8) -0.0020(8) O6 0.0351(13) 0.0493(14) 0.0202(11) -0.0063(10) 0.0057(9) 0.0024(11) C1 0.0198(15) 0.0261(15) 0.0223(15) 0.0099(12) 0.0012(11) 0.0007(12) C2 0.0254(16) 0.0284(16) 0.0272(16) 0.0063(13) 0.0038(12) 0.0022(13) C3 0.0289(18) 0.0430(19) 0.0354(18) 0.0099(15) 0.0128(14) 0.0007(15) C4 0.0276(18) 0.043(2) 0.046(2) 0.0075(17) 0.0101(15) -0.0118(16) C5 0.0264(17) 0.0337(17) 0.0410(19) 0.0028(15) 0.0009(14) -0.0106(14) C6 0.0232(16) 0.0246(15) 0.0263(16) 0.0053(12) 0.0015(12) -0.0063(13) C7 0.047(2) 0.053(2) 0.0262(18) -0.0007(16) 0.0108(15) 0.0053(18) C8 0.0256(16) 0.0227(15) 0.0245(15) -0.0001(12) -0.0041(12) -0.0059(13) C9 0.0246(16) 0.0203(14) 0.0251(15) -0.0056(12) 0.0009(12) -0.0034(12) C10 0.0252(16) 0.0193(14) 0.0307(16) -0.0040(12) 0.0011(12) -0.0011(12) C11 0.0234(16) 0.0315(16) 0.0193(15) -0.0045(12) 0.0052(12) -0.0016(13) C12 0.0254(16) 0.0283(16) 0.0211(15) -0.0036(12) 0.0059(12) -0.0025(13) C13 0.0178(14) 0.0165(13) 0.0250(15) -0.0016(11) 0.0017(11) 0.0021(11) C14 0.0157(14) 0.0199(14) 0.0234(15) 0.0016(11) -0.0010(11) -0.0027(11) C15 0.0271(16) 0.0221(15) 0.0309(17) 0.0052(13) -0.0004(12) 0.0028(13) C16 0.0341(18) 0.0282(17) 0.0332(18) 0.0129(14) -0.0028(14) 0.0023(14) C17 0.0329(18) 0.0331(17) 0.0247(16) 0.0090(13) 0.0020(13) -0.0041(14) C18 0.0235(16) 0.0252(15) 0.0221(15) 0.0030(12) 0.0030(12) -0.0014(13) C19 0.0148(14) 0.0205(14) 0.0194(14) 0.0037(11) -0.0021(10) -0.0035(11) C20 0.048(2) 0.050(2) 0.0189(16) 0.0018(15) 0.0110(14) 0.0034(17) C21 0.0160(14) 0.0250(15) 0.0294(16) -0.0027(13) 0.0020(12) 0.0019(12) C22 0.0144(14) 0.0277(16) 0.0288(16) -0.0036(13) 0.0047(12) 0.0001(12) C23 0.0158(14) 0.0271(15) 0.0283(16) 0.0038(13) 0.0012(12) -0.0023(12) C24 0.0208(15) 0.0242(15) 0.0243(15) 0.0015(12) -0.0029(12) -0.0028(12) C25 0.0258(17) 0.0310(17) 0.0345(18) -0.0015(14) -0.0038(13) -0.0013(14) C26 0.0355(19) 0.0376(18) 0.0325(18) -0.0045(15) -0.0119(14) -0.0071(15) C27 0.045(2) 0.0288(16) 0.0183(15) -0.0014(13) -0.0010(13) 0.0007(15) C28 0.0326(18) 0.0264(16) 0.0207(15) 0.0015(12) 0.0009(12) 0.0025(14) C29 0.0285(16) 0.0183(14) 0.0188(14) 0.0033(11) -0.0004(12) -0.0010(12) C30 0.054(2) 0.064(2) 0.0254(18) -0.0074(17) 0.0133(16) 0.008(2) C31 0.064(3) 0.064(3) 0.060(3) -0.003(2) -0.015(2) 0.018(2) C32 0.052(3) 0.036(2) 0.061(3) 0.009(2) -0.005(2) -0.0050(18) C33 0.082(4) 0.043(3) 0.104(4) 0.002(3) 0.028(3) -0.014(2) C34 0.053(3) 0.048(3) 0.085(4) 0.002(2) 0.002(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O5 2.2300(19) . ? Dy1 O1 2.2427(17) . ? Dy1 O3 2.3220(19) 3 ? Dy1 O3 2.3296(17) . ? Dy1 N1 2.494(2) . ? Dy1 N4 2.498(2) . ? Dy1 N3 2.725(2) . ? Dy1 N2 2.752(2) 3 ? Dy1 Dy1 3.8374(3) 3 ? N1 C8 1.281(3) . ? N1 C9 1.468(3) . ? N2 C10 1.481(3) . ? N2 C13 1.483(3) . ? N2 C11 1.501(3) . ? N2 Dy1 2.752(2) 3 ? N3 C21 1.478(3) . ? N3 C13 1.483(3) . ? N3 C12 1.492(3) . ? N4 C23 1.276(4) . ? N4 C22 1.467(3) . ? N5 C32 1.126(5) . ? N6 C34 1.115(5) . ? O1 C1 1.299(3) . ? O2 C2 1.369(4) . ? O2 C7 1.428(4) . ? O3 C19 1.344(3) . ? O3 Dy1 2.3220(19) 3 ? O4 C18 1.364(3) . ? O4 C20 1.415(3) . ? O5 C29 1.299(3) . ? O6 C28 1.373(3) . ? O6 C30 1.415(3) . ? C1 C6 1.415(4) . ? C1 C2 1.430(4) . ? C2 C3 1.379(4) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.368(4) . ? C4 H4 0.9500 . ? C5 C6 1.403(4) . ? C5 H5 0.9500 . ? C6 C8 1.443(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 C10 1.513(4) 3 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C9 1.513(4) 3 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.526(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.499(4) . ? C13 H13 1.0000 . ? C14 C19 1.397(4) . ? C14 C15 1.399(4) . ? C15 C16 1.364(4) . ? C15 H15 0.9500 . ? C16 C17 1.393(4) . ? C16 H16 0.9500 . ? C17 C18 1.386(4) . ? C17 H17 0.9500 . ? C18 C19 1.405(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.501(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.440(4) . ? C23 H23 0.9500 . ? C24 C25 1.416(4) . ? C24 C29 1.416(4) . ? C25 C26 1.364(4) . ? C25 H25 0.9500 . ? C26 C27 1.399(4) . ? C26 H26 0.9500 . ? C27 C28 1.366(4) . ? C27 H27 0.9500 . ? C28 C29 1.431(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.444(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.446(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 Dy1 O1 134.20(7) . . ? O5 Dy1 O3 141.41(7) . 3 ? O1 Dy1 O3 82.04(7) . 3 ? O5 Dy1 O3 80.90(7) . . ? O1 Dy1 O3 143.00(7) . . ? O3 Dy1 O3 68.83(7) 3 . ? O5 Dy1 N1 74.77(7) . . ? O1 Dy1 N1 71.08(7) . . ? O3 Dy1 N1 115.87(7) 3 . ? O3 Dy1 N1 142.08(7) . . ? O5 Dy1 N4 70.99(7) . . ? O1 Dy1 N4 75.59(7) . . ? O3 Dy1 N4 143.69(7) 3 . ? O3 Dy1 N4 115.53(7) . . ? N1 Dy1 N4 83.47(7) . . ? O5 Dy1 N3 110.90(7) . . ? O1 Dy1 N3 82.42(7) . . ? O3 Dy1 N3 82.39(6) 3 . ? O3 Dy1 N3 71.84(6) . . ? N1 Dy1 N3 144.32(7) . . ? N4 Dy1 N3 66.73(7) . . ? O5 Dy1 N2 80.90(7) . 3 ? O1 Dy1 N2 110.95(7) . 3 ? O3 Dy1 N2 71.80(6) 3 3 ? O3 Dy1 N2 81.75(6) . 3 ? N1 Dy1 N2 66.16(7) . 3 ? N4 Dy1 N2 143.18(7) . 3 ? N3 Dy1 N2 148.35(6) . 3 ? O5 Dy1 Dy1 112.15(5) . 3 ? O1 Dy1 Dy1 113.65(5) . 3 ? O3 Dy1 Dy1 34.48(4) 3 3 ? O3 Dy1 Dy1 34.35(5) . 3 ? N1 Dy1 Dy1 137.98(5) . 3 ? N4 Dy1 Dy1 138.52(5) . 3 ? N3 Dy1 Dy1 74.38(5) . 3 ? N2 Dy1 Dy1 73.97(4) 3 3 ? C8 N1 C9 117.0(2) . . ? C8 N1 Dy1 129.19(19) . . ? C9 N1 Dy1 113.77(16) . . ? C10 N2 C13 107.7(2) . . ? C10 N2 C11 111.5(2) . . ? C13 N2 C11 103.8(2) . . ? C10 N2 Dy1 108.59(15) . 3 ? C13 N2 Dy1 117.24(15) . 3 ? C11 N2 Dy1 107.96(16) . 3 ? C21 N3 C13 107.2(2) . . ? C21 N3 C12 111.8(2) . . ? C13 N3 C12 104.2(2) . . ? C21 N3 Dy1 108.69(16) . . ? C13 N3 Dy1 118.19(15) . . ? C12 N3 Dy1 106.83(16) . . ? C23 N4 C22 117.7(2) . . ? C23 N4 Dy1 129.27(19) . . ? C22 N4 Dy1 113.00(17) . . ? C1 O1 Dy1 137.87(18) . . ? C2 O2 C7 117.0(2) . . ? C19 O3 Dy1 119.90(15) . 3 ? C19 O3 Dy1 119.75(15) . . ? Dy1 O3 Dy1 111.17(7) 3 . ? C18 O4 C20 117.5(2) . . ? C29 O5 Dy1 136.49(18) . . ? C28 O6 C30 117.2(2) . . ? O1 C1 C6 123.7(2) . . ? O1 C1 C2 119.8(3) . . ? C6 C1 C2 116.5(2) . . ? O2 C2 C3 124.5(3) . . ? O2 C2 C1 114.7(2) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 120.9(3) . . ? C5 C6 C8 117.7(3) . . ? C1 C6 C8 120.7(2) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C6 126.9(3) . . ? N1 C8 H8 116.5 . . ? C6 C8 H8 116.5 . . ? N1 C9 C10 106.4(2) . 3 ? N1 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 3 . ? N1 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 3 . ? H9A C9 H9B 108.6 . . ? N2 C10 C9 111.3(2) . 3 ? N2 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 3 . ? N2 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 3 . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 105.7(2) . . ? N2 C11 H11A 110.6 . . ? C12 C11 H11A 110.6 . . ? N2 C11 H11B 110.6 . . ? C12 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? N3 C12 C11 106.0(2) . . ? N3 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? N3 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? N2 C13 N3 104.4(2) . . ? N2 C13 C14 113.9(2) . . ? N3 C13 C14 113.8(2) . . ? N2 C13 H13 108.2 . . ? N3 C13 H13 108.2 . . ? C14 C13 H13 108.2 . . ? C19 C14 C15 119.8(2) . . ? C19 C14 C13 120.5(2) . . ? C15 C14 C13 119.7(2) . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? O4 C18 C17 124.9(3) . . ? O4 C18 C19 114.4(2) . . ? C17 C18 C19 120.7(3) . . ? O3 C19 C14 120.7(2) . . ? O3 C19 C18 120.6(2) . . ? C14 C19 C18 118.6(2) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 111.9(2) . . ? N3 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N3 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N4 C22 C21 107.2(2) . . ? N4 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? N4 C22 H22B 110.3 . . ? C21 C22 H22B 110.3 . . ? H22A C22 H22B 108.5 . . ? N4 C23 C24 126.3(3) . . ? N4 C23 H23 116.8 . . ? C24 C23 H23 116.8 . . ? C25 C24 C29 120.0(3) . . ? C25 C24 C23 118.6(3) . . ? C29 C24 C23 120.8(3) . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.6(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 O6 125.1(3) . . ? C27 C28 C29 121.8(3) . . ? O6 C28 C29 113.1(3) . . ? O5 C29 C24 123.6(3) . . ? O5 C29 C28 119.6(3) . . ? C24 C29 C28 116.8(3) . . ? O6 C30 H30A 109.5 . . ? O6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C32 C31 179.0(5) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 C33 178.8(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.454 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.133 _database_code_depnum_ccdc_archive 'CCDC 921079'