# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_3 _database_code_depnum_ccdc_archive 'CCDC 891154' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H24 Dy N3 O14' _chemical_formula_weight 752.97 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.798(3) _cell_length_b 12.935(4) _cell_length_c 13.396(4) _cell_angle_alpha 118.378(3) _cell_angle_beta 97.249(4) _cell_angle_gamma 99.837(4) _cell_volume 1429.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6079 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 26.75 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 2.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_correction_T_max 0.511 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8538 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_unetl/netI 0.0567 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.75 _reflns_number_total 6079 _reflns_number_gt 5381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C(17), C(18), C(19), C(20), C(21), C(22), C(23), C(24), N(3), O(9), O(10), O(11), O(12) atoms of one L^-1^ ligand are found to be disordered. Thermal (SIMU) restraints are placed on these atoms to obtain acceptable ADPs. ; _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^)+(0.0542P)^2^+2.0023P] 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 6079 _refine_ls_number_parameters 490 _refine_ls_number_restraints 656 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.247282(19) 0.495594(18) 0.480341(17) 0.02996(9) Uani 1 1 d . . . O1 O 0.3143(11) -0.1161(7) 0.3796(8) 0.147(4) Uani 1 1 d . . . O2 O 0.3916(7) -0.0975(6) 0.5452(8) 0.127(3) Uani 1 1 d . . . O3 O 0.2781(4) 0.2988(3) 0.4517(3) 0.0386(7) Uani 1 1 d . A . O4 O 0.1383(4) 0.3808(3) 0.5669(3) 0.0380(7) Uani 1 1 d . A . O5 O 0.1642(9) 0.4734(13) 0.8943(9) 0.214(7) Uani 1 1 d . . . O6 O 0.2032(10) 0.6356(13) 1.0483(8) 0.220(7) Uani 1 1 d . . . O7 O 0.4353(4) 0.5326(3) 0.6232(3) 0.0420(8) Uani 1 1 d . A . O8 O 0.6686(4) 0.5768(4) 0.6867(3) 0.0512(9) Uani 1 1 d . . . O1W O 0.4228(4) 0.6751(3) 0.5219(4) 0.0545(10) Uani 1 1 d . A . H3W H 0.5071 0.6936 0.5218 0.082 Uiso 1 1 d R . . H4W H 0.4054 0.7287 0.5102 0.082 Uiso 1 1 d R . . N1 N 0.3229(7) -0.0716(5) 0.4807(8) 0.081(2) Uani 1 1 d . . . N2 N 0.2397(8) 0.5669(12) 0.9666(7) 0.130(4) Uani 1 1 d . . . C1 C 0.1600(9) -0.0750(7) 0.6509(7) 0.078(2) Uani 1 1 d . . . H1A H 0.1448 -0.1539 0.5832 0.117 Uiso 1 1 calc R . . H1B H 0.0809 -0.0741 0.6866 0.117 Uiso 1 1 calc R . . H1C H 0.2461 -0.0573 0.7058 0.117 Uiso 1 1 calc R . . C2 C 0.2553(6) 0.1073(4) 0.5002(5) 0.0421(11) Uani 1 1 d . A . H2A H 0.3038 0.1021 0.4434 0.050 Uiso 1 1 calc R . . C3 C 0.2470(6) 0.0225(5) 0.5358(5) 0.0489(13) Uani 1 1 d . . . C4 C 0.1732(7) 0.0201(5) 0.6152(5) 0.0498(13) Uani 1 1 d . . . C5 C 0.1043(7) 0.1128(5) 0.6619(5) 0.0520(14) Uani 1 1 d . . . H5A H 0.0509 0.1149 0.7152 0.062 Uiso 1 1 calc R . . C6 C 0.1131(6) 0.2011(5) 0.6315(5) 0.0470(12) Uani 1 1 d . A . H6A H 0.0670 0.2621 0.6654 0.056 Uiso 1 1 calc R . . C7 C 0.1893(5) 0.2003(4) 0.5513(4) 0.0368(10) Uani 1 1 d . . . C8 C 0.2022(5) 0.2984(4) 0.5208(4) 0.0343(10) Uani 1 1 d . A . C9 C 0.4891(12) 0.7014(13) 1.1747(7) 0.148(6) Uani 1 1 d . . . H9A H 0.4064 0.6480 1.1728 0.221 Uiso 1 1 calc R . . H9B H 0.4817 0.7838 1.2150 0.221 Uiso 1 1 calc R . . H9C H 0.5731 0.6953 1.2147 0.221 Uiso 1 1 calc R . . C10 C 0.4988(9) 0.6649(12) 1.0496(6) 0.114(4) Uani 1 1 d . . . C11 C 0.3844(8) 0.6018(10) 0.9527(6) 0.093(3) Uani 1 1 d . . . C12 C 0.3950(6) 0.5698(7) 0.8399(5) 0.068(2) Uani 1 1 d . . . H12A H 0.3147 0.5278 0.7778 0.082 Uiso 1 1 calc R . . C13 C 0.5277(6) 0.6016(7) 0.8220(5) 0.0628(18) Uani 1 1 d . A . C14 C 0.6444(8) 0.6648(11) 0.9162(6) 0.103(4) Uani 1 1 d . . . H14A H 0.7337 0.6871 0.9045 0.124 Uiso 1 1 calc R . . C15 C 0.6307(9) 0.6954(13) 1.0268(7) 0.132(5) Uani 1 1 d . . . H15A H 0.7114 0.7376 1.0885 0.159 Uiso 1 1 calc R . . C16 C 0.5443(5) 0.5687(5) 0.7019(4) 0.0380(10) Uani 1 1 d . . . C17 C 0.4098(18) 0.9901(18) 1.1702(11) 0.167(8) Uani 0.723(5) 1 d PU A 1 H17A H 0.5085 0.9926 1.1713 0.251 Uiso 0.723(5) 1 calc PR A 1 H17B H 0.3793 0.9579 1.2176 0.251 Uiso 0.723(5) 1 calc PR A 1 H17C H 0.3978 1.0709 1.2005 0.251 Uiso 0.723(5) 1 calc PR A 1 C18 C 0.0959(5) 0.7997(6) 0.8989(5) 0.070(3) Uani 0.723(5) 1 d PGU A 1 H18A H -0.0034 0.7773 0.8800 0.084 Uiso 0.723(5) 1 calc PR A 1 C19 C 0.1708(7) 0.8739(7) 1.0150(4) 0.094(4) Uani 0.723(5) 1 d PGDU A 1 C20 C 0.3191(7) 0.9074(8) 1.0433(4) 0.100(4) Uani 0.723(5) 1 d PGU A 1 C21 C 0.3924(5) 0.8668(7) 0.9554(5) 0.085(3) Uani 0.723(5) 1 d PGU A 1 H21A H 0.4916 0.8892 0.9743 0.102 Uiso 0.723(5) 1 calc PR A 1 C22 C 0.3174(5) 0.7926(6) 0.8393(4) 0.061(2) Uani 0.723(5) 1 d PGU A 1 H22A H 0.3665 0.7654 0.7805 0.073 Uiso 0.723(5) 1 calc PR A 1 C23 C 0.1691(5) 0.7591(6) 0.8110(3) 0.0469(19) Uani 0.723(5) 1 d PGDU A 1 C24 C 0.088(2) 0.6726(13) 0.6871(7) 0.027(2) Uani 0.723(5) 1 d PDU A 1 N3 N 0.0875(13) 0.9091(14) 1.0987(7) 0.160(8) Uani 0.723(5) 1 d PD A 1 O9 O 0.1385(16) 0.9819(17) 1.1976(9) 0.219(8) Uani 0.723(5) 1 d PDU A 1 O10 O -0.0374(15) 0.8765(15) 1.0700(10) 0.202(7) Uani 0.723(5) 1 d PDU A 1 O11 O 0.1552(7) 0.6284(6) 0.6096(6) 0.0439(14) Uani 0.723(5) 1 d PU A 1 O12 O -0.0461(8) 0.6471(6) 0.6654(6) 0.0458(16) Uani 0.723(5) 1 d PU . 1 C17B C 0.149(5) 1.057(3) 1.166(3) 0.104(10) Uani 0.277(5) 1 d PU A 2 H17D H 0.2489 1.0902 1.2027 0.157 Uiso 0.277(5) 1 calc PR A 2 H17E H 0.1017 1.0275 1.2100 0.157 Uiso 0.277(5) 1 calc PR A 2 H17F H 0.1092 1.1189 1.1640 0.157 Uiso 0.277(5) 1 calc PR A 2 C18B C -0.0172(12) 0.7950(13) 0.8503(11) 0.051(4) Uani 0.277(5) 1 d PGU A 2 H18B H -0.1065 0.7512 0.7992 0.061 Uiso 0.277(5) 1 calc PR A 2 C19B C -0.0063(14) 0.8853(14) 0.9644(12) 0.064(5) Uani 0.277(5) 1 d PGDU A 2 C20B C 0.1271(17) 0.9507(14) 1.0407(10) 0.068(5) Uani 0.277(5) 1 d PGU A 2 C21B C 0.2496(14) 0.9258(16) 1.0029(12) 0.077(6) Uani 0.277(5) 1 d PGU A 2 H21B H 0.3388 0.9696 1.0539 0.093 Uiso 0.277(5) 1 calc PR A 2 C22B C 0.2387(13) 0.8355(16) 0.8887(13) 0.069(5) Uani 0.277(5) 1 d PGU A 2 H22B H 0.3207 0.8188 0.8634 0.082 Uiso 0.277(5) 1 calc PR A 2 C23B C 0.1053(15) 0.7701(14) 0.8124(10) 0.052(5) Uani 0.277(5) 1 d PGDU A 2 C24B C 0.088(9) 0.670(5) 0.690(2) 0.053(9) Uani 0.277(5) 1 d PDU A 2 N3B N -0.135(2) 0.902(2) 1.0012(18) 0.073(6) Uani 0.277(5) 1 d PDU A 2 O9B O -0.145(3) 0.927(4) 1.0970(18) 0.187(10) Uani 0.277(5) 1 d PDU A 2 O10B O -0.237(3) 0.882(3) 0.931(2) 0.170(11) Uani 0.277(5) 1 d PDU A 2 O11B O 0.1993(17) 0.6530(16) 0.6546(14) 0.037(3) Uani 0.277(5) 1 d PU A 2 O12B O -0.031(2) 0.6122(18) 0.6326(17) 0.043(3) Uani 0.277(5) 1 d PU . 2 O13 O 0.1388(4) 0.6045(4) 0.3962(4) 0.0539(11) Uani 1 1 d . A . H13 H 0.070(8) 0.617(6) 0.414(6) 0.065 Uiso 1 1 d . . . C25 C 0.1330(12) 0.5759(12) 0.2692(11) 0.131(4) Uani 1 1 d . . . H25A H 0.1237 0.6458 0.2637 0.196 Uiso 1 1 calc R A . H25B H 0.0526 0.5080 0.2169 0.196 Uiso 1 1 calc R . . H25C H 0.2192 0.5561 0.2483 0.196 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02153(12) 0.04182(14) 0.03552(13) 0.02448(10) 0.01097(8) 0.01169(9) O1 0.241(11) 0.116(6) 0.154(7) 0.077(5) 0.138(8) 0.120(7) O2 0.092(5) 0.094(4) 0.229(9) 0.102(5) 0.029(5) 0.055(4) O3 0.0378(18) 0.0468(19) 0.0437(18) 0.0275(15) 0.0212(15) 0.0189(15) O4 0.0337(18) 0.0442(18) 0.054(2) 0.0338(16) 0.0223(15) 0.0168(15) O5 0.071(5) 0.334(15) 0.111(6) 0.049(8) 0.035(5) -0.054(7) O6 0.114(7) 0.376(17) 0.118(7) 0.081(9) 0.089(6) 0.038(8) O7 0.0353(18) 0.062(2) 0.0343(17) 0.0287(16) 0.0068(14) 0.0148(16) O8 0.0336(19) 0.082(3) 0.046(2) 0.036(2) 0.0203(16) 0.0157(19) O1W 0.0299(19) 0.052(2) 0.098(3) 0.048(2) 0.019(2) 0.0158(17) N1 0.063(4) 0.051(3) 0.149(7) 0.058(4) 0.043(4) 0.029(3) N2 0.059(5) 0.242(12) 0.069(5) 0.072(6) 0.031(4) 0.004(6) C1 0.091(6) 0.065(4) 0.093(5) 0.058(4) 0.006(4) 0.013(4) C2 0.039(3) 0.037(2) 0.052(3) 0.024(2) 0.014(2) 0.011(2) C3 0.046(3) 0.036(3) 0.063(4) 0.025(2) 0.006(3) 0.012(2) C4 0.055(3) 0.041(3) 0.054(3) 0.030(2) 0.000(3) 0.004(2) C5 0.066(4) 0.051(3) 0.045(3) 0.030(3) 0.017(3) 0.009(3) C6 0.055(3) 0.045(3) 0.051(3) 0.029(2) 0.020(3) 0.020(2) C7 0.033(2) 0.040(2) 0.041(3) 0.024(2) 0.007(2) 0.009(2) C8 0.029(2) 0.038(2) 0.042(2) 0.024(2) 0.0123(19) 0.0112(19) C9 0.113(8) 0.255(15) 0.049(5) 0.070(7) 0.025(5) 0.008(9) C10 0.067(5) 0.207(11) 0.041(4) 0.055(5) 0.013(3) -0.003(6) C11 0.051(4) 0.168(9) 0.049(4) 0.050(5) 0.024(3) 0.009(5) C12 0.035(3) 0.123(6) 0.041(3) 0.041(4) 0.012(2) 0.010(3) C13 0.029(3) 0.121(6) 0.039(3) 0.044(3) 0.009(2) 0.013(3) C14 0.041(4) 0.202(10) 0.046(4) 0.062(5) 0.005(3) -0.006(5) C15 0.057(5) 0.256(14) 0.047(4) 0.068(6) 0.001(4) -0.013(7) C16 0.032(2) 0.054(3) 0.036(2) 0.027(2) 0.0131(19) 0.016(2) C17 0.122(12) 0.227(17) 0.060(7) 0.055(9) -0.019(7) -0.086(11) C18 0.062(5) 0.081(5) 0.034(4) 0.016(4) 0.010(4) -0.018(4) C19 0.082(6) 0.112(7) 0.040(4) 0.023(5) 0.010(4) -0.037(6) C20 0.083(7) 0.125(8) 0.046(5) 0.035(5) -0.005(5) -0.043(6) C21 0.057(5) 0.102(7) 0.067(6) 0.039(5) -0.009(5) -0.021(5) C22 0.042(4) 0.078(5) 0.054(4) 0.036(4) -0.001(3) -0.005(4) C23 0.041(4) 0.057(4) 0.039(4) 0.028(3) 0.004(3) -0.004(4) C24 0.030(4) 0.031(3) 0.029(4) 0.020(3) 0.010(3) 0.013(3) N3 0.133(11) 0.194(14) 0.032(5) 0.002(6) 0.023(6) -0.073(10) O9 0.152(10) 0.294(15) 0.057(6) 0.000(8) 0.033(6) -0.033(11) O10 0.122(8) 0.267(13) 0.071(6) -0.003(7) 0.051(6) -0.040(9) O11 0.041(3) 0.050(3) 0.044(4) 0.022(3) 0.017(2) 0.021(3) O12 0.031(3) 0.054(4) 0.039(4) 0.015(3) 0.006(2) 0.006(3) C17B 0.13(2) 0.090(17) 0.050(14) 0.014(13) 0.013(15) -0.003(17) C18B 0.050(8) 0.056(8) 0.043(8) 0.023(6) 0.014(7) 0.007(7) C19B 0.071(9) 0.064(9) 0.044(8) 0.018(7) 0.025(7) 0.007(8) C20B 0.074(10) 0.075(9) 0.051(9) 0.036(8) 0.014(8) -0.003(9) C21B 0.070(10) 0.085(10) 0.056(9) 0.031(8) -0.004(9) 0.001(9) C22B 0.061(9) 0.072(9) 0.043(8) 0.016(7) 0.003(8) -0.004(8) C23B 0.047(9) 0.055(8) 0.047(8) 0.025(7) 0.011(7) 0.000(8) C24B 0.047(12) 0.061(12) 0.040(11) 0.023(10) 0.013(11) -0.006(11) N3B 0.081(10) 0.058(8) 0.073(9) 0.023(6) 0.039(8) 0.021(7) O9B 0.117(12) 0.253(16) 0.072(9) 0.003(11) 0.063(9) -0.014(12) O10B 0.094(12) 0.226(17) 0.091(11) 0.007(12) 0.064(10) 0.005(13) O11B 0.030(5) 0.044(5) 0.035(6) 0.014(5) 0.011(4) 0.020(4) O12B 0.032(5) 0.047(6) 0.042(6) 0.016(5) 0.011(5) 0.010(5) O13 0.036(2) 0.084(3) 0.078(3) 0.062(3) 0.024(2) 0.028(2) C25 0.110(9) 0.181(12) 0.159(11) 0.109(10) 0.054(8) 0.088(9) _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 O11 2.204(6) . ? Dy1 O12B 2.21(2) 2_566 ? Dy1 O7 2.286(3) . ? Dy1 O8 2.302(3) 2_666 ? Dy1 O12 2.338(7) 2_566 ? Dy1 O1W 2.413(4) . ? Dy1 O11B 2.429(16) . ? Dy1 O3 2.466(3) . ? Dy1 O4 2.469(3) . ? Dy1 O13 2.470(4) . ? Dy1 C8 2.826(5) . ? O1 N1 1.177(11) . ? O2 N1 1.232(10) . ? O3 C8 1.261(6) . ? O4 C8 1.269(5) . ? O5 N2 1.161(13) . ? O6 N2 1.183(12) . ? O7 C16 1.244(6) . ? O8 C16 1.255(6) . ? O8 Dy1 2.302(3) 2_666 ? O1W H3W 0.8200 . ? O1W H4W 0.8200 . ? N1 C3 1.475(7) . ? N2 C11 1.475(10) . ? C1 C4 1.510(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.384(8) . ? C2 C7 1.388(7) . ? C2 H2A 0.9300 . ? C3 C4 1.368(9) . ? C4 C5 1.398(9) . ? C5 C6 1.378(8) . ? C5 H5A 0.9300 . ? C6 C7 1.380(7) . ? C6 H6A 0.9300 . ? C7 C8 1.498(7) . ? C9 C10 1.530(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.386(11) . ? C10 C15 1.400(11) . ? C11 C12 1.387(9) . ? C12 C13 1.381(8) . ? C12 H12A 0.9300 . ? C13 C14 1.380(9) . ? C13 C16 1.495(7) . ? C14 C15 1.371(10) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 C20 1.546(13) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C18 H18A 0.9300 . ? C19 C20 1.3900 . ? C19 N3 1.416(12) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.497(10) . ? C24 O12 1.26(2) . ? C24 O11 1.256(18) . ? N3 O10 1.173(11) . ? N3 O9 1.174(10) . ? O12 Dy1 2.338(7) 2_566 ? C17B C20B 1.54(3) . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B C19B 1.3900 . ? C18B C23B 1.3900 . ? C18B H18B 0.9300 . ? C19B C20B 1.3900 . ? C19B N3B 1.427(14) . ? C20B C21B 1.3900 . ? C21B C22B 1.3900 . ? C21B H21B 0.9300 . ? C22B C23B 1.3900 . ? C22B H22B 0.9300 . ? C23B C24B 1.495(12) . ? C24B O12B 1.20(7) . ? C24B O11B 1.25(8) . ? N3B O9B 1.182(12) . ? N3B O10B 1.181(12) . ? O12B Dy1 2.21(2) 2_566 ? O13 C25 1.552(12) . ? O13 H13 0.75(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Dy1 O12B 90.3(5) . 2_566 ? O11 Dy1 O7 91.5(2) . . ? O12B Dy1 O7 149.9(7) 2_566 . ? O11 Dy1 O8 151.3(2) . 2_666 ? O12B Dy1 O8 87.7(5) 2_566 2_666 ? O7 Dy1 O8 104.35(13) . 2_666 ? O11 Dy1 O12 103.0(2) . 2_566 ? O12B Dy1 O12 12.7(4) 2_566 2_566 ? O7 Dy1 O12 146.5(2) . 2_566 ? O8 Dy1 O12 76.8(2) 2_666 2_566 ? O11 Dy1 O1W 83.8(2) . . ? O12B Dy1 O1W 137.8(6) 2_566 . ? O7 Dy1 O1W 72.15(14) . . ? O8 Dy1 O1W 78.67(15) 2_666 . ? O12 Dy1 O1W 138.6(2) 2_566 . ? O11 Dy1 O11B 13.7(3) . . ? O12B Dy1 O11B 102.9(6) 2_566 . ? O7 Dy1 O11B 77.9(4) . . ? O8 Dy1 O11B 154.5(5) 2_666 . ? O12 Dy1 O11B 115.5(4) 2_566 . ? O1W Dy1 O11B 78.0(5) . . ? O11 Dy1 O3 130.0(2) . . ? O12B Dy1 O3 84.6(6) 2_566 . ? O7 Dy1 O3 71.40(13) . . ? O8 Dy1 O3 78.35(13) 2_666 . ? O12 Dy1 O3 76.2(2) 2_566 . ? O1W Dy1 O3 129.89(12) . . ? O11B Dy1 O3 125.1(5) . . ? O11 Dy1 O4 77.8(2) . . ? O12B Dy1 O4 73.0(6) 2_566 . ? O7 Dy1 O4 78.03(13) . . ? O8 Dy1 O4 128.40(14) 2_666 . ? O12 Dy1 O4 75.9(2) 2_566 . ? O1W Dy1 O4 144.36(15) . . ? O11B Dy1 O4 77.0(5) . . ? O3 Dy1 O4 53.06(10) . . ? O11 Dy1 O13 70.5(2) . . ? O12B Dy1 O13 68.4(6) 2_566 . ? O7 Dy1 O13 139.65(15) . . ? O8 Dy1 O13 82.21(15) 2_666 . ? O12 Dy1 O13 73.8(2) 2_566 . ? O1W Dy1 O13 70.27(14) . . ? O11B Dy1 O13 80.4(4) . . ? O3 Dy1 O13 147.26(15) . . ? O4 Dy1 O13 129.05(12) . . ? O11 Dy1 C8 103.9(2) . . ? O12B Dy1 C8 78.7(6) 2_566 . ? O7 Dy1 C8 71.78(14) . . ? O8 Dy1 C8 103.81(14) 2_666 . ? O12 Dy1 C8 75.5(2) 2_566 . ? O1W Dy1 C8 143.27(14) . . ? O11B Dy1 C8 101.0(5) . . ? O3 Dy1 C8 26.46(12) . . ? O4 Dy1 C8 26.65(12) . . ? O13 Dy1 C8 146.34(14) . . ? C8 O3 Dy1 92.9(3) . . ? C8 O4 Dy1 92.6(3) . . ? C16 O7 Dy1 170.8(4) . . ? C16 O8 Dy1 131.8(3) . 2_666 ? Dy1 O1W H3W 137.5 . . ? Dy1 O1W H4W 124.8 . . ? H3W O1W H4W 92.6 . . ? O1 N1 O2 124.8(7) . . ? O1 N1 C3 118.4(8) . . ? O2 N1 C3 116.7(8) . . ? O5 N2 O6 122.4(9) . . ? O5 N2 C11 118.1(9) . . ? O6 N2 C11 119.5(10) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 118.4(5) . . ? C3 C2 H2A 120.8 . . ? C7 C2 H2A 120.8 . . ? C4 C3 C2 124.8(5) . . ? C4 C3 N1 119.6(6) . . ? C2 C3 N1 115.7(6) . . ? C3 C4 C5 115.1(5) . . ? C3 C4 C1 124.7(6) . . ? C5 C4 C1 120.1(6) . . ? C6 C5 C4 122.0(6) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C7 120.9(5) . . ? C5 C6 H6A 119.6 . . ? C7 C6 H6A 119.6 . . ? C6 C7 C2 118.7(5) . . ? C6 C7 C8 120.8(4) . . ? C2 C7 C8 120.5(5) . . ? O3 C8 O4 121.3(4) . . ? O3 C8 C7 119.5(4) . . ? O4 C8 C7 119.2(4) . . ? O3 C8 Dy1 60.6(2) . . ? O4 C8 Dy1 60.8(2) . . ? C7 C8 Dy1 175.0(3) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 115.2(6) . . ? C11 C10 C9 124.9(8) . . ? C15 C10 C9 119.9(8) . . ? C10 C11 C12 124.2(7) . . ? C10 C11 N2 119.9(6) . . ? C12 C11 N2 115.9(7) . . ? C13 C12 C11 118.4(6) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? C14 C13 C12 119.3(6) . . ? C14 C13 C16 120.5(5) . . ? C12 C13 C16 120.2(5) . . ? C15 C14 C13 121.1(7) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C10 121.9(7) . . ? C14 C15 H15A 119.0 . . ? C10 C15 H15A 119.0 . . ? O7 C16 O8 124.2(4) . . ? O7 C16 C13 118.6(4) . . ? O8 C16 C13 117.2(4) . . ? C19 C18 C23 120.0 . . ? C19 C18 H18A 120.0 . . ? C23 C18 H18A 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 N3 123.9(6) . . ? C18 C19 N3 116.1(6) . . ? C19 C20 C21 120.0 . . ? C19 C20 C17 123.0(8) . . ? C21 C20 C17 117.0(8) . . ? C22 C21 C20 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 C24 120.3(9) . . ? C18 C23 C24 119.6(10) . . ? O12 C24 O11 122.9(9) . . ? O12 C24 C23 118.0(11) . . ? O11 C24 C23 119.2(16) . . ? O10 N3 O9 116.7(14) . . ? O10 N3 C19 121.0(8) . . ? O9 N3 C19 121.8(11) . . ? C24 O11 Dy1 159.9(10) . . ? C24 O12 Dy1 140.9(5) . 2_566 ? C20B C17B H17D 109.5 . . ? C20B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C20B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C19B C18B C23B 120.0 . . ? C19B C18B H18B 120.0 . . ? C23B C18B H18B 120.0 . . ? C20B C19B C18B 120.0 . . ? C20B C19B N3B 122.1(13) . . ? C18B C19B N3B 117.8(13) . . ? C19B C20B C21B 120.0 . . ? C19B C20B C17B 123(2) . . ? C21B C20B C17B 117(2) . . ? C20B C21B C22B 120.0 . . ? C20B C21B H21B 120.0 . . ? C22B C21B H21B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B H22B 120.0 . . ? C21B C22B H22B 120.0 . . ? C22B C23B C18B 120.0 . . ? C22B C23B C24B 122(3) . . ? C18B C23B C24B 118(3) . . ? O12B C24B O11B 124.9(16) . . ? O12B C24B C23B 118(5) . . ? O11B C24B C23B 117(5) . . ? O9B N3B O10B 120(2) . . ? O9B N3B C19B 122(2) . . ? O10B N3B C19B 117.8(18) . . ? C24B O11B Dy1 134(2) . . ? C24B O12B Dy1 177(3) . 2_566 ? C25 O13 Dy1 123.4(4) . . ? C25 O13 H13 112(6) . . ? Dy1 O13 H13 113(6) . . ? O13 C25 H25A 109.5 . . ? O13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 O11 Dy1 O3 C8 10.6(4) . . . . ? O12B Dy1 O3 C8 -75.3(6) 2_566 . . . ? O7 Dy1 O3 C8 86.3(3) . . . . ? O8 Dy1 O3 C8 -164.0(3) 2_666 . . . ? O12 Dy1 O3 C8 -85.0(3) 2_566 . . . ? O1W Dy1 O3 C8 131.7(3) . . . . ? O11B Dy1 O3 C8 26.8(6) . . . . ? O4 Dy1 O3 C8 -2.5(3) . . . . ? O13 Dy1 O3 C8 -109.2(3) . . . . ? O11 Dy1 O4 C8 -167.3(3) . . . . ? O12B Dy1 O4 C8 98.6(5) 2_566 . . . ? O7 Dy1 O4 C8 -73.1(3) . . . . ? O8 Dy1 O4 C8 25.8(3) 2_666 . . . ? O12 Dy1 O4 C8 85.7(3) 2_566 . . . ? O1W Dy1 O4 C8 -106.7(3) . . . . ? O11B Dy1 O4 C8 -153.3(5) . . . . ? O3 Dy1 O4 C8 2.5(3) . . . . ? O13 Dy1 O4 C8 140.6(3) . . . . ? O11 Dy1 O7 C16 -72(2) . . . . ? O12B Dy1 O7 C16 -165(2) 2_566 . . . ? O8 Dy1 O7 C16 84(2) 2_666 . . . ? O12 Dy1 O7 C16 171(2) 2_566 . . . ? O1W Dy1 O7 C16 11(2) . . . . ? O11B Dy1 O7 C16 -70(2) . . . . ? O3 Dy1 O7 C16 156(2) . . . . ? O4 Dy1 O7 C16 -149(2) . . . . ? O13 Dy1 O7 C16 -11(2) . . . . ? C8 Dy1 O7 C16 -176(2) . . . . ? C7 C2 C3 C4 2.8(9) . . . . ? C7 C2 C3 N1 -178.2(5) . . . . ? O1 N1 C3 C4 136.6(8) . . . . ? O2 N1 C3 C4 -43.5(9) . . . . ? O1 N1 C3 C2 -42.4(10) . . . . ? O2 N1 C3 C2 137.4(7) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? N1 C3 C4 C5 -179.7(6) . . . . ? C2 C3 C4 C1 177.8(6) . . . . ? N1 C3 C4 C1 -1.2(10) . . . . ? C3 C4 C5 C6 -1.2(9) . . . . ? C1 C4 C5 C6 -179.8(6) . . . . ? C4 C5 C6 C7 1.0(9) . . . . ? C5 C6 C7 C2 1.1(9) . . . . ? C5 C6 C7 C8 -178.3(5) . . . . ? C3 C2 C7 C6 -2.9(8) . . . . ? C3 C2 C7 C8 176.5(5) . . . . ? Dy1 O3 C8 O4 4.5(5) . . . . ? Dy1 O3 C8 C7 -174.2(4) . . . . ? Dy1 O4 C8 O3 -4.5(5) . . . . ? Dy1 O4 C8 C7 174.2(4) . . . . ? C6 C7 C8 O3 176.6(5) . . . . ? C2 C7 C8 O3 -2.8(7) . . . . ? C6 C7 C8 O4 -2.2(7) . . . . ? C2 C7 C8 O4 178.5(5) . . . . ? C6 C7 C8 Dy1 86(4) . . . . ? C2 C7 C8 Dy1 -93(4) . . . . ? O11 Dy1 C8 O3 -171.7(3) . . . . ? O12B Dy1 C8 O3 100.9(5) 2_566 . . . ? O7 Dy1 C8 O3 -84.7(3) . . . . ? O8 Dy1 C8 O3 16.1(3) 2_666 . . . ? O12 Dy1 C8 O3 88.2(3) 2_566 . . . ? O1W Dy1 C8 O3 -73.4(4) . . . . ? O11B Dy1 C8 O3 -158.0(5) . . . . ? O4 Dy1 C8 O3 175.6(5) . . . . ? O13 Dy1 C8 O3 112.9(3) . . . . ? O11 Dy1 C8 O4 12.8(3) . . . . ? O12B Dy1 C8 O4 -74.7(5) 2_566 . . . ? O7 Dy1 C8 O4 99.7(3) . . . . ? O8 Dy1 C8 O4 -159.4(3) 2_666 . . . ? O12 Dy1 C8 O4 -87.3(3) 2_566 . . . ? O1W Dy1 C8 O4 111.1(3) . . . . ? O11B Dy1 C8 O4 26.5(5) . . . . ? O3 Dy1 C8 O4 -175.6(5) . . . . ? O13 Dy1 C8 O4 -62.7(4) . . . . ? O11 Dy1 C8 C7 -79(4) . . . . ? O12B Dy1 C8 C7 -166(4) 2_566 . . . ? O7 Dy1 C8 C7 8(4) . . . . ? O8 Dy1 C8 C7 109(4) 2_666 . . . ? O12 Dy1 C8 C7 -179(100) 2_566 . . . ? O1W Dy1 C8 C7 20(4) . . . . ? O11B Dy1 C8 C7 -65(4) . . . . ? O3 Dy1 C8 C7 93(4) . . . . ? O4 Dy1 C8 C7 -91(4) . . . . ? O13 Dy1 C8 C7 -154(4) . . . . ? C15 C10 C11 C12 0(2) . . . . ? C9 C10 C11 C12 179.8(12) . . . . ? C15 C10 C11 N2 -178.9(12) . . . . ? C9 C10 C11 N2 1(2) . . . . ? O5 N2 C11 C10 -142.9(15) . . . . ? O6 N2 C11 C10 39.3(19) . . . . ? O5 N2 C11 C12 38.4(18) . . . . ? O6 N2 C11 C12 -139.5(12) . . . . ? C10 C11 C12 C13 0.5(17) . . . . ? N2 C11 C12 C13 179.2(9) . . . . ? C11 C12 C13 C14 -0.6(14) . . . . ? C11 C12 C13 C16 179.8(8) . . . . ? C12 C13 C14 C15 0.6(17) . . . . ? C16 C13 C14 C15 -179.9(11) . . . . ? C13 C14 C15 C10 0(2) . . . . ? C11 C10 C15 C14 0(2) . . . . ? C9 C10 C15 C14 -179.9(13) . . . . ? Dy1 O7 C16 O8 -72(2) . . . . ? Dy1 O7 C16 C13 110(2) . . . . ? Dy1 O8 C16 O7 -12.2(8) 2_666 . . . ? Dy1 O8 C16 C13 166.1(4) 2_666 . . . ? C14 C13 C16 O7 -166.7(8) . . . . ? C12 C13 C16 O7 12.8(10) . . . . ? C14 C13 C16 O8 14.9(11) . . . . ? C12 C13 C16 O8 -165.5(7) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C23 C18 C19 N3 -178.9(11) . . . . ? C18 C19 C20 C21 0.0 . . . . ? N3 C19 C20 C21 178.8(12) . . . . ? C18 C19 C20 C17 179.7(13) . . . . ? N3 C19 C20 C17 -1.4(15) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C17 C20 C21 C22 -179.7(12) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C21 C22 C23 C24 -175.9(10) . . . . ? C19 C18 C23 C22 0.0 . . . . ? C19 C18 C23 C24 175.9(10) . . . . ? C22 C23 C24 O12 -178.4(11) . . . . ? C18 C23 C24 O12 5.7(18) . . . . ? C22 C23 C24 O11 1.8(19) . . . . ? C18 C23 C24 O11 -174.1(11) . . . . ? C20 C19 N3 O10 -178.7(16) . . . . ? C18 C19 N3 O10 0(2) . . . . ? C20 C19 N3 O9 10(3) . . . . ? C18 C19 N3 O9 -171.6(19) . . . . ? O12 C24 O11 Dy1 -75(3) . . . . ? C23 C24 O11 Dy1 104(3) . . . . ? O12B Dy1 O11 C24 69(3) 2_566 . . . ? O7 Dy1 O11 C24 -81(2) . . . . ? O8 Dy1 O11 C24 155(2) 2_666 . . . ? O12 Dy1 O11 C24 68(2) 2_566 . . . ? O1W Dy1 O11 C24 -153(2) . . . . ? O11B Dy1 O11 C24 -89(4) . . . . ? O3 Dy1 O11 C24 -14(3) . . . . ? O4 Dy1 O11 C24 -4(2) . . . . ? O13 Dy1 O11 C24 136(2) . . . . ? C8 Dy1 O11 C24 -10(2) . . . . ? O11 C24 O12 Dy1 16(3) . . . 2_566 ? C23 C24 O12 Dy1 -164.0(7) . . . 2_566 ? C23B C18B C19B C20B 0.0 . . . . ? C23B C18B C19B N3B -175.8(18) . . . . ? C18B C19B C20B C21B 0.0 . . . . ? N3B C19B C20B C21B 175.6(18) . . . . ? C18B C19B C20B C17B 176(2) . . . . ? N3B C19B C20B C17B -8(3) . . . . ? C19B C20B C21B C22B 0.0 . . . . ? C17B C20B C21B C22B -177(2) . . . . ? C20B C21B C22B C23B 0.0 . . . . ? C21B C22B C23B C18B 0.0 . . . . ? C21B C22B C23B C24B -178(4) . . . . ? C19B C18B C23B C22B 0.0 . . . . ? C19B C18B C23B C24B 179(4) . . . . ? C22B C23B C24B O12B 175(4) . . . . ? C18B C23B C24B O12B -4(7) . . . . ? C22B C23B C24B O11B -5(7) . . . . ? C18B C23B C24B O11B 176(4) . . . . ? C20B C19B N3B O9B -32(4) . . . . ? C18B C19B N3B O9B 144(3) . . . . ? C20B C19B N3B O10B 152(3) . . . . ? C18B C19B N3B O10B -32(3) . . . . ? O12B C24B O11B Dy1 -9(10) . . . . ? C23B C24B O11B Dy1 171(2) . . . . ? O11 Dy1 O11B C24B 32(5) . . . . ? O12B Dy1 O11B C24B 9(5) 2_566 . . . ? O7 Dy1 O11B C24B -140(5) . . . . ? O8 Dy1 O11B C24B 122(5) 2_666 . . . ? O12 Dy1 O11B C24B 8(5) 2_566 . . . ? O1W Dy1 O11B C24B 146(5) . . . . ? O3 Dy1 O11B C24B -83(5) . . . . ? O4 Dy1 O11B C24B -60(5) . . . . ? O13 Dy1 O11B C24B 74(5) . . . . ? C8 Dy1 O11B C24B -71(5) . . . . ? O11B C24B O12B Dy1 -33(78) . . . 2_566 ? C23B C24B O12B Dy1 147(69) . . . 2_566 ? O11 Dy1 O13 C25 -177.4(7) . . . . ? O12B Dy1 O13 C25 -79.0(8) 2_566 . . . ? O7 Dy1 O13 C25 114.6(7) . . . . ? O8 Dy1 O13 C25 11.6(6) 2_666 . . . ? O12 Dy1 O13 C25 -66.8(7) 2_566 . . . ? O1W Dy1 O13 C25 92.3(6) . . . . ? O11B Dy1 O13 C25 172.9(8) . . . . ? O3 Dy1 O13 C25 -42.3(7) . . . . ? O4 Dy1 O13 C25 -122.5(6) . . . . ? C8 Dy1 O13 C25 -91.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H3W O3 0.82 2.07 2.848(5) 159.1 2_666 O1W H4W O2 0.82 2.10 2.881(7) 159.4 1_565 O13 H13 O4 0.75(7) 2.10(7) 2.842(5) 169(7) 2_566 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.647 _refine_diff_density_min -2.072 _refine_diff_density_rms 0.129 data_1 _database_code_depnum_ccdc_archive 'CCDC 891155' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H24 Gd N3 O14' _chemical_formula_weight 747.72 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8217(4) _cell_length_b 12.9436(7) _cell_length_c 13.4474(8) _cell_angle_alpha 118.500(6) _cell_angle_beta 97.591(4) _cell_angle_gamma 99.982(4) _cell_volume 1433.33(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6093 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 26.75 _exptl_crystal_description Rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 2.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 0.500 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9776 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_unetl/netI 0.0542 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 26.75 _reflns_number_total 6093 _reflns_number_gt 5425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction,2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C(17), C(18), C(19), C(20), C(21), C(22), C(23), C(24), N(3), O(9), O(10), O(11), O(12) atoms of one L^-1^ ligand are found to be disordered. Thermal (SIMU) restraints are placed on these atoms to obtain acceptable ADPs. ; _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^)+(0.0367P)^2^+1.5000P] 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 6093 _refine_ls_number_parameters 496 _refine_ls_number_restraints 637 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.248236(17) 0.496522(17) 0.480365(16) 0.03168(8) Uani 1 1 d . . . O1 O 0.3150(8) -0.1159(6) 0.3825(7) 0.140(3) Uani 1 1 d . . . O2 O 0.3931(5) -0.0949(5) 0.5483(6) 0.118(2) Uani 1 1 d . . . O3 O 0.2778(3) 0.2984(3) 0.4527(2) 0.0389(6) Uani 1 1 d . A . O4 O 0.1401(3) 0.3806(3) 0.5674(3) 0.0402(7) Uani 1 1 d . A . O5 O 0.1629(7) 0.4756(10) 0.8910(7) 0.227(6) Uani 1 1 d . . . O6 O 0.2026(8) 0.6368(10) 1.0444(7) 0.212(5) Uani 1 1 d . . . O7 O 0.4402(3) 0.5354(3) 0.6253(2) 0.0446(7) Uani 1 1 d . A . O8 O 0.6728(3) 0.5787(3) 0.6905(3) 0.0524(8) Uani 1 1 d . . . O1W O 0.4263(3) 0.6776(3) 0.5197(4) 0.0546(9) Uani 1 1 d . A . H3W H 0.515(7) 0.682(6) 0.526(5) 0.082 Uiso 1 1 d . . . H4W H 0.413(7) 0.734(6) 0.517(6) 0.082 Uiso 1 1 d . . . N1 N 0.3235(6) -0.0703(5) 0.4830(6) 0.0796(16) Uani 1 1 d . . . N2 N 0.2384(7) 0.5686(9) 0.9628(6) 0.135(3) Uani 1 1 d . . . C1 C 0.1599(7) -0.0748(5) 0.6521(6) 0.0742(17) Uani 1 1 d . . . H1A H 0.1502 -0.1533 0.5852 0.111 Uiso 1 1 calc R . . H1B H 0.0777 -0.0777 0.6831 0.111 Uiso 1 1 calc R . . H1C H 0.2440 -0.0539 0.7106 0.111 Uiso 1 1 calc R . . C2 C 0.2555(4) 0.1078(4) 0.5020(4) 0.0429(10) Uani 1 1 d . A . H2A H 0.3047 0.1030 0.4460 0.051 Uiso 1 1 calc R . . C3 C 0.2467(5) 0.0223(4) 0.5368(4) 0.0485(12) Uani 1 1 d . . . C4 C 0.1726(5) 0.0208(4) 0.6164(4) 0.0489(11) Uani 1 1 d . . . C5 C 0.1046(6) 0.1119(5) 0.6617(4) 0.0533(12) Uani 1 1 d . . . H5A H 0.0509 0.1133 0.7141 0.064 Uiso 1 1 calc R . . C6 C 0.1131(5) 0.2013(4) 0.6325(4) 0.0449(10) Uani 1 1 d . A . H6A H 0.0675 0.2622 0.6667 0.054 Uiso 1 1 calc R . . C7 C 0.1899(4) 0.2004(4) 0.5519(4) 0.0365(9) Uani 1 1 d . . . C8 C 0.2026(4) 0.2983(4) 0.5218(3) 0.0332(8) Uani 1 1 d . A . C9 C 0.4871(10) 0.7006(12) 1.1737(6) 0.177(6) Uani 1 1 d . . . H9A H 0.4281 0.6320 1.1718 0.266 Uiso 1 1 calc R . . H9B H 0.4454 0.7679 1.2044 0.266 Uiso 1 1 calc R . . H9C H 0.5805 0.7238 1.2225 0.266 Uiso 1 1 calc R . . C10 C 0.4985(8) 0.6658(10) 1.0496(6) 0.130(4) Uani 1 1 d . . . C11 C 0.3837(6) 0.6041(8) 0.9524(5) 0.100(3) Uani 1 1 d . . . C12 C 0.3975(5) 0.5718(6) 0.8402(5) 0.0732(19) Uani 1 1 d . . . H12A H 0.3178 0.5288 0.7771 0.088 Uiso 1 1 calc R . . C13 C 0.5293(5) 0.6037(6) 0.8236(4) 0.0655(17) Uani 1 1 d . A . C14 C 0.6459(6) 0.6652(9) 0.9194(5) 0.115(3) Uani 1 1 d . . . H14A H 0.7361 0.6870 0.9094 0.138 Uiso 1 1 calc R . . C15 C 0.6300(8) 0.6947(11) 1.0291(6) 0.155(5) Uani 1 1 d . . . H15A H 0.7104 0.7353 1.0915 0.186 Uiso 1 1 calc R . . C16 C 0.5480(4) 0.5700(4) 0.7045(4) 0.0394(10) Uani 1 1 d . . . C17 C 0.4130(15) 0.9917(16) 1.1754(10) 0.193(8) Uani 0.680(5) 1 d PU A 1 H17A H 0.5123 0.9963 1.1788 0.289 Uiso 0.680(5) 1 calc PR A 1 H17B H 0.3818 0.9590 1.2219 0.289 Uiso 0.680(5) 1 calc PR A 1 H17C H 0.3997 1.0720 1.2051 0.289 Uiso 0.680(5) 1 calc PR A 1 C18 C 0.0999(4) 0.7985(6) 0.8995(4) 0.068(2) Uani 0.680(5) 1 d PGU A 1 H18A H 0.0006 0.7752 0.8800 0.082 Uiso 0.680(5) 1 calc PR A 1 C19 C 0.1751(6) 0.8716(7) 1.0160(4) 0.093(3) Uani 0.680(5) 1 d PGU A 1 C20 C 0.3234(6) 0.9064(7) 1.0451(3) 0.105(4) Uani 0.680(5) 1 d PGU A 1 C21 C 0.3965(4) 0.8680(7) 0.9577(5) 0.094(3) Uani 0.680(5) 1 d PGU A 1 H21A H 0.4958 0.8913 0.9772 0.113 Uiso 0.680(5) 1 calc PR A 1 C22 C 0.3213(5) 0.7949(6) 0.8413(4) 0.066(2) Uani 0.680(5) 1 d PGU A 1 H22A H 0.3703 0.7693 0.7828 0.079 Uiso 0.680(5) 1 calc PR A 1 C23 C 0.1730(5) 0.7602(5) 0.8121(3) 0.0479(19) Uani 0.680(5) 1 d PGDU A 1 C24 C 0.089(3) 0.6737(15) 0.6881(8) 0.033(4) Uani 0.680(5) 1 d PDU A 1 N3 N 0.0911(14) 0.9079(12) 1.1001(8) 0.159(6) Uani 0.680(5) 1 d P A 1 O9 O 0.1444(14) 0.9751(15) 1.2001(8) 0.210(7) Uani 0.680(5) 1 d PU A 1 O10 O -0.0297(13) 0.8699(14) 1.0730(8) 0.192(6) Uani 0.680(5) 1 d PU A 1 O11 O 0.1597(7) 0.6321(7) 0.6128(6) 0.0471(15) Uani 0.680(5) 1 d PU A 1 O12 O -0.0435(9) 0.6477(8) 0.6671(6) 0.0488(18) Uani 0.680(5) 1 d PU . 1 C17B C 0.140(3) 1.055(2) 1.1697(16) 0.089(7) Uani 0.320(5) 1 d PU A 2 H17D H 0.2384 1.1001 1.2078 0.133 Uiso 0.320(5) 1 calc PR A 2 H17E H 0.1031 1.0201 1.2128 0.133 Uiso 0.320(5) 1 calc PR A 2 H17F H 0.0862 1.1088 1.1663 0.133 Uiso 0.320(5) 1 calc PR A 2 C18B C -0.0149(8) 0.7958(10) 0.8521(8) 0.054(4) Uani 0.320(5) 1 d PGU A 2 H18B H -0.1042 0.7513 0.8005 0.065 Uiso 0.320(5) 1 calc PR A 2 C19B C -0.0041(10) 0.8848(10) 0.9667(8) 0.059(4) Uani 0.320(5) 1 d PGU A 2 C20B C 0.1294(12) 0.9513(10) 1.0437(7) 0.066(4) Uani 0.320(5) 1 d PGU A 2 C21B C 0.2520(9) 0.9289(11) 1.0063(9) 0.073(5) Uani 0.320(5) 1 d PGU A 2 H21B H 0.3413 0.9734 1.0578 0.088 Uiso 0.320(5) 1 calc PR A 2 C22B C 0.2412(9) 0.8399(12) 0.8917(9) 0.062(4) Uani 0.320(5) 1 d PGU A 2 H22B H 0.3233 0.8249 0.8666 0.075 Uiso 0.320(5) 1 calc PR A 2 C23B C 0.1078(10) 0.7734(10) 0.8146(7) 0.047(4) Uani 0.320(5) 1 d PGDU A 2 C24B C 0.098(7) 0.674(3) 0.6928(14) 0.035(7) Uani 0.320(5) 1 d PDU A 2 N3B N -0.128(3) 0.9026(15) 1.008(2) 0.085(6) Uani 0.320(5) 1 d P A 2 O9B O -0.141(2) 0.927(2) 1.0998(15) 0.141(7) Uani 0.320(5) 1 d PU A 2 O10B O -0.2399(19) 0.8814(18) 0.9259(18) 0.115(6) Uani 0.320(5) 1 d PU A 2 O11B O 0.2041(14) 0.6571(14) 0.6579(11) 0.039(3) Uani 0.320(5) 1 d PU A 2 O12B O -0.0289(18) 0.6151(15) 0.6291(13) 0.041(3) Uani 0.320(5) 1 d PU . 2 O13 O 0.1380(4) 0.6070(4) 0.3977(4) 0.0586(9) Uani 1 1 d . A . H13 H 0.054(6) 0.616(5) 0.413(5) 0.070 Uiso 1 1 d . . . C25 C 0.1352(10) 0.5760(12) 0.2600(14) 0.211(7) Uani 1 1 d . . . H25A H 0.1210 0.6441 0.2532 0.316 Uiso 1 1 calc R A . H25B H 0.0588 0.5046 0.2058 0.316 Uiso 1 1 calc R . . H25C H 0.2243 0.5618 0.2429 0.316 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02376(12) 0.04260(13) 0.03858(13) 0.02655(10) 0.01041(8) 0.01228(9) O1 0.225(7) 0.108(5) 0.155(6) 0.075(4) 0.129(6) 0.117(5) O2 0.088(3) 0.082(3) 0.210(7) 0.092(4) 0.018(4) 0.043(3) O3 0.0372(15) 0.0442(16) 0.0451(17) 0.0265(14) 0.0190(13) 0.0159(13) O4 0.0403(16) 0.0417(16) 0.0539(18) 0.0303(15) 0.0233(13) 0.0203(13) O5 0.076(4) 0.334(12) 0.125(6) 0.040(7) 0.042(4) -0.055(6) O6 0.124(6) 0.354(13) 0.130(6) 0.094(7) 0.093(5) 0.046(7) O7 0.0358(15) 0.061(2) 0.0362(16) 0.0257(15) 0.0030(12) 0.0145(14) O8 0.0348(16) 0.083(2) 0.0524(19) 0.0418(19) 0.0218(14) 0.0165(16) O1W 0.0317(16) 0.050(2) 0.101(3) 0.050(2) 0.0194(17) 0.0176(15) N1 0.067(3) 0.054(3) 0.135(5) 0.054(4) 0.042(3) 0.025(2) N2 0.069(4) 0.238(10) 0.073(4) 0.071(5) 0.038(4) -0.004(5) C1 0.085(4) 0.062(4) 0.088(4) 0.057(3) 0.002(3) 0.006(3) C2 0.037(2) 0.043(2) 0.053(3) 0.027(2) 0.0106(19) 0.0130(19) C3 0.043(3) 0.032(2) 0.064(3) 0.021(2) 0.007(2) 0.0128(19) C4 0.056(3) 0.040(2) 0.051(3) 0.030(2) -0.001(2) 0.004(2) C5 0.069(3) 0.053(3) 0.046(3) 0.033(2) 0.016(2) 0.010(2) C6 0.051(3) 0.048(3) 0.048(3) 0.030(2) 0.021(2) 0.020(2) C7 0.030(2) 0.037(2) 0.042(2) 0.0211(19) 0.0043(16) 0.0078(16) C8 0.0264(19) 0.035(2) 0.039(2) 0.0208(18) 0.0065(16) 0.0065(16) C9 0.128(7) 0.321(16) 0.047(4) 0.086(7) 0.029(4) 0.003(8) C10 0.079(5) 0.231(11) 0.050(4) 0.068(5) 0.009(3) -0.013(5) C11 0.052(3) 0.182(8) 0.053(4) 0.057(4) 0.027(3) 0.003(4) C12 0.040(3) 0.130(6) 0.042(3) 0.043(3) 0.012(2) 0.011(3) C13 0.029(2) 0.127(5) 0.040(3) 0.046(3) 0.0087(19) 0.010(3) C14 0.047(3) 0.222(10) 0.053(4) 0.072(5) 0.004(3) -0.012(4) C15 0.066(4) 0.300(14) 0.052(4) 0.082(6) 0.000(3) -0.027(6) C16 0.034(2) 0.057(3) 0.038(2) 0.030(2) 0.0128(17) 0.0159(19) C17 0.135(11) 0.266(17) 0.061(7) 0.066(9) -0.038(7) -0.113(11) C18 0.050(4) 0.089(5) 0.038(4) 0.027(4) 0.005(3) -0.022(4) C19 0.078(6) 0.121(7) 0.039(4) 0.030(5) 0.007(4) -0.030(5) C20 0.083(6) 0.137(8) 0.048(5) 0.041(5) -0.011(4) -0.040(6) C21 0.055(5) 0.131(7) 0.063(5) 0.051(5) -0.013(4) -0.034(5) C22 0.037(4) 0.098(6) 0.056(4) 0.046(4) 0.000(3) -0.008(4) C23 0.038(4) 0.063(4) 0.041(4) 0.031(3) 0.007(3) -0.002(3) C24 0.033(6) 0.034(5) 0.029(5) 0.013(4) 0.008(4) 0.013(4) N3 0.124(9) 0.197(13) 0.039(5) 0.011(6) 0.018(5) -0.073(8) O9 0.170(10) 0.284(15) 0.049(5) 0.019(7) 0.026(6) -0.026(10) O10 0.117(8) 0.268(12) 0.065(5) 0.013(7) 0.043(5) -0.030(9) O11 0.050(4) 0.055(4) 0.047(4) 0.027(4) 0.020(3) 0.027(3) O12 0.035(3) 0.064(5) 0.035(4) 0.017(3) 0.010(3) 0.007(3) C17B 0.121(16) 0.068(12) 0.028(9) -0.001(8) 0.012(9) -0.006(11) C18B 0.043(7) 0.063(7) 0.051(7) 0.023(6) 0.025(5) 0.012(6) C19B 0.068(8) 0.066(8) 0.041(7) 0.025(6) 0.025(6) 0.016(7) C20B 0.066(8) 0.076(9) 0.053(8) 0.039(7) 0.009(7) 0.001(7) C21B 0.055(8) 0.089(9) 0.063(8) 0.036(7) -0.003(7) 0.013(7) C22B 0.054(7) 0.065(8) 0.044(7) 0.015(6) 0.002(6) 0.006(7) C23B 0.053(8) 0.049(7) 0.036(7) 0.023(5) 0.013(6) 0.002(6) C24B 0.037(11) 0.043(9) 0.047(10) 0.041(8) 0.010(9) 0.006(9) N3B 0.132(17) 0.055(9) 0.089(14) 0.031(9) 0.091(14) 0.047(11) O9B 0.121(11) 0.194(14) 0.074(9) 0.038(9) 0.060(8) 0.034(11) O10B 0.091(10) 0.130(12) 0.126(12) 0.049(10) 0.064(9) 0.059(9) O11B 0.036(6) 0.048(6) 0.028(6) 0.011(5) 0.011(4) 0.020(5) O12B 0.030(5) 0.049(7) 0.034(7) 0.015(5) 0.004(5) 0.011(5) O13 0.0398(18) 0.090(3) 0.082(3) 0.066(2) 0.0215(17) 0.0298(18) C25 0.091(7) 0.225(14) 0.37(2) 0.189(16) 0.052(10) 0.073(8) _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 Gd1 O12B 2.224(17) 2_566 ? Gd1 O11 2.227(7) . ? Gd1 O7 2.317(3) . ? Gd1 O8 2.329(3) 2_666 ? Gd1 O12 2.361(8) 2_566 ? Gd1 O1W 2.446(3) . ? Gd1 O11B 2.462(14) . ? Gd1 O3 2.485(3) . ? Gd1 O13 2.487(3) . ? Gd1 O4 2.490(3) . ? Gd1 C8 2.851(4) . ? O1 N1 1.173(8) . ? O2 N1 1.234(8) . ? O3 C8 1.262(5) . ? O4 C8 1.261(5) . ? O5 N2 1.150(10) . ? O6 N2 1.180(10) . ? O7 C16 1.241(5) . ? O8 C16 1.259(5) . ? O8 Gd1 2.329(3) 2_666 ? O1W H3W 0.85(6) . ? O1W H4W 0.78(7) . ? N1 C3 1.470(6) . ? N2 C11 1.468(8) . ? C1 C4 1.519(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.385(6) . ? C2 C3 1.387(6) . ? C2 H2A 0.9300 . ? C3 C4 1.377(7) . ? C4 C5 1.380(7) . ? C5 C6 1.381(6) . ? C5 H5A 0.9300 . ? C6 C7 1.397(6) . ? C6 H6A 0.9300 . ? C7 C8 1.494(6) . ? C9 C10 1.532(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.382(9) . ? C10 C11 1.386(9) . ? C11 C12 1.393(7) . ? C12 C13 1.370(6) . ? C12 H12A 0.9300 . ? C13 C14 1.385(7) . ? C13 C16 1.492(6) . ? C14 C15 1.375(9) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 C20 1.573(11) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C18 H18A 0.9300 . ? C19 C20 1.3900 . ? C19 N3 1.434(11) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.500(12) . ? C24 O12 1.24(3) . ? C24 O11 1.26(2) . ? N3 O10 1.138(13) . ? N3 O9 1.174(12) . ? O12 Gd1 2.361(8) 2_566 ? C17B C20B 1.553(19) . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B C19B 1.3900 . ? C18B C23B 1.3900 . ? C18B H18B 0.9300 . ? C19B C20B 1.3900 . ? C19B N3B 1.406(19) . ? C20B C21B 1.3900 . ? C21B C22B 1.3900 . ? C21B H21B 0.9300 . ? C22B C23B 1.3900 . ? C22B H22B 0.9300 . ? C23B C24B 1.499(14) . ? C24B O11B 1.21(6) . ? C24B O12B 1.27(6) . ? N3B O9B 1.16(2) . ? N3B O10B 1.34(3) . ? O12B Gd1 2.224(17) 2_566 ? O13 C25 1.693(15) . ? O13 H13 0.89(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12B Gd1 O11 90.6(4) 2_566 . ? O12B Gd1 O7 148.1(5) 2_566 . ? O11 Gd1 O7 90.68(19) . . ? O12B Gd1 O8 88.0(4) 2_566 2_666 ? O11 Gd1 O8 151.3(2) . 2_666 ? O7 Gd1 O8 105.31(10) . 2_666 ? O12B Gd1 O12 13.2(3) 2_566 2_566 ? O11 Gd1 O12 103.6(2) . 2_566 ? O7 Gd1 O12 147.0(3) . 2_566 ? O8 Gd1 O12 75.78(18) 2_666 2_566 ? O12B Gd1 O1W 139.2(5) 2_566 . ? O11 Gd1 O1W 84.0(2) . . ? O7 Gd1 O1W 72.57(12) . . ? O8 Gd1 O1W 78.56(13) 2_666 . ? O12 Gd1 O1W 137.7(3) 2_566 . ? O12B Gd1 O11B 102.8(4) 2_566 . ? O11 Gd1 O11B 13.5(3) . . ? O7 Gd1 O11B 77.3(3) . . ? O8 Gd1 O11B 154.8(4) 2_666 . ? O12 Gd1 O11B 116.0(3) 2_566 . ? O1W Gd1 O11B 78.4(4) . . ? O12B Gd1 O3 83.4(5) 2_566 . ? O11 Gd1 O3 129.3(2) . . ? O7 Gd1 O3 71.40(10) . . ? O8 Gd1 O3 78.90(11) 2_666 . ? O12 Gd1 O3 76.6(2) 2_566 . ? O1W Gd1 O3 130.07(10) . . ? O11B Gd1 O3 124.5(4) . . ? O12B Gd1 O13 70.2(5) 2_566 . ? O11 Gd1 O13 70.4(2) . . ? O7 Gd1 O13 139.28(12) . . ? O8 Gd1 O13 82.25(13) 2_666 . ? O12 Gd1 O13 73.7(3) 2_566 . ? O1W Gd1 O13 69.89(12) . . ? O11B Gd1 O13 80.2(4) . . ? O3 Gd1 O13 147.91(12) . . ? O12B Gd1 O4 71.2(5) 2_566 . ? O11 Gd1 O4 78.0(2) . . ? O7 Gd1 O4 77.96(10) . . ? O8 Gd1 O4 128.02(11) 2_666 . ? O12 Gd1 O4 76.2(2) 2_566 . ? O1W Gd1 O4 145.10(12) . . ? O11B Gd1 O4 77.2(4) . . ? O3 Gd1 O4 52.41(9) . . ? O13 Gd1 O4 128.98(10) . . ? O12B Gd1 C8 76.9(5) 2_566 . ? O11 Gd1 C8 103.5(2) . . ? O7 Gd1 C8 71.86(11) . . ? O8 Gd1 C8 104.00(12) 2_666 . ? O12 Gd1 C8 75.8(3) 2_566 . ? O1W Gd1 C8 143.67(11) . . ? O11B Gd1 C8 100.6(4) . . ? O3 Gd1 C8 26.22(10) . . ? O13 Gd1 C8 146.30(11) . . ? O4 Gd1 C8 26.22(10) . . ? C8 O3 Gd1 93.3(2) . . ? C8 O4 Gd1 93.1(2) . . ? C16 O7 Gd1 172.3(3) . . ? C16 O8 Gd1 130.2(3) . 2_666 ? Gd1 O1W H3W 124(4) . . ? Gd1 O1W H4W 127(5) . . ? H3W O1W H4W 108(6) . . ? O1 N1 O2 124.4(6) . . ? O1 N1 C3 118.8(6) . . ? O2 N1 C3 116.7(7) . . ? O5 N2 O6 122.1(8) . . ? O5 N2 C11 119.1(8) . . ? O6 N2 C11 118.8(8) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.8(4) . . ? C7 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 124.2(4) . . ? C4 C3 N1 120.2(5) . . ? C2 C3 N1 115.6(5) . . ? C3 C4 C5 115.5(4) . . ? C3 C4 C1 124.1(5) . . ? C5 C4 C1 120.4(5) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C7 120.3(4) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C2 C7 C6 118.4(4) . . ? C2 C7 C8 120.9(4) . . ? C6 C7 C8 120.7(4) . . ? O3 C8 O4 121.0(4) . . ? O3 C8 C7 119.4(4) . . ? O4 C8 C7 119.5(4) . . ? O3 C8 Gd1 60.5(2) . . ? O4 C8 Gd1 60.7(2) . . ? C7 C8 Gd1 175.1(3) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 115.8(6) . . ? C15 C10 C9 120.0(7) . . ? C11 C10 C9 124.3(7) . . ? C10 C11 C12 123.1(5) . . ? C10 C11 N2 121.0(5) . . ? C12 C11 N2 115.9(5) . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 118.5(5) . . ? C12 C13 C16 120.8(4) . . ? C14 C13 C16 120.6(4) . . ? C15 C14 C13 121.0(6) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C10 122.2(6) . . ? C14 C15 H15A 118.9 . . ? C10 C15 H15A 118.9 . . ? O7 C16 O8 123.8(4) . . ? O7 C16 C13 118.3(4) . . ? O8 C16 C13 117.9(4) . . ? C19 C18 C23 120.0 . . ? C19 C18 H18A 120.0 . . ? C23 C18 H18A 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 N3 116.2(6) . . ? C20 C19 N3 123.8(6) . . ? C19 C20 C21 120.0 . . ? C19 C20 C17 121.8(7) . . ? C21 C20 C17 118.2(7) . . ? C22 C21 C20 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 C24 121.2(10) . . ? C18 C23 C24 118.7(10) . . ? O12 C24 O11 125.0(10) . . ? O12 C24 C23 118.2(12) . . ? O11 C24 C23 117(2) . . ? O10 N3 O9 117.3(12) . . ? O10 N3 C19 121.3(9) . . ? O9 N3 C19 121.4(12) . . ? C24 O11 Gd1 158.7(11) . . ? C24 O12 Gd1 140.9(5) . 2_566 ? C20B C17B H17D 109.5 . . ? C20B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C20B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C19B C18B C23B 120.0 . . ? C19B C18B H18B 120.0 . . ? C23B C18B H18B 120.0 . . ? C18B C19B C20B 120.0 . . ? C18B C19B N3B 120.4(13) . . ? C20B C19B N3B 119.5(13) . . ? C21B C20B C19B 120.0 . . ? C21B C20B C17B 120.4(12) . . ? C19B C20B C17B 119.5(12) . . ? C20B C21B C22B 120.0 . . ? C20B C21B H21B 120.0 . . ? C22B C21B H21B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B H22B 120.0 . . ? C21B C22B H22B 120.0 . . ? C22B C23B C18B 120.0 . . ? C22B C23B C24B 119(3) . . ? C18B C23B C24B 121(3) . . ? O11B C24B O12B 123.6(12) . . ? O11B C24B C23B 121(4) . . ? O12B C24B C23B 115(4) . . ? O9B N3B O10B 119(2) . . ? O9B N3B C19B 127(3) . . ? O10B N3B C19B 113.7(15) . . ? C24B O11B Gd1 133.7(15) . . ? C24B O12B Gd1 177(3) . 2_566 ? C25 O13 Gd1 121.9(4) . . ? C25 O13 H13 110(4) . . ? Gd1 O13 H13 114(4) . . ? O13 C25 H25A 109.5 . . ? O13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 O12B Gd1 O3 C8 -73.7(4) 2_566 . . . ? O11 Gd1 O3 C8 11.6(3) . . . . ? O7 Gd1 O3 C8 86.5(2) . . . . ? O8 Gd1 O3 C8 -163.0(2) 2_666 . . . ? O12 Gd1 O3 C8 -85.1(3) 2_566 . . . ? O1W Gd1 O3 C8 132.4(2) . . . . ? O11B Gd1 O3 C8 27.3(4) . . . . ? O13 Gd1 O3 C8 -107.8(3) . . . . ? O4 Gd1 O3 C8 -2.4(2) . . . . ? O12B Gd1 O4 C8 98.6(4) 2_566 . . . ? O11 Gd1 O4 C8 -166.6(3) . . . . ? O7 Gd1 O4 C8 -73.3(2) . . . . ? O8 Gd1 O4 C8 26.9(3) 2_666 . . . ? O12 Gd1 O4 C8 86.0(3) 2_566 . . . ? O1W Gd1 O4 C8 -106.0(3) . . . . ? O11B Gd1 O4 C8 -152.8(4) . . . . ? O3 Gd1 O4 C8 2.4(2) . . . . ? O13 Gd1 O4 C8 141.2(2) . . . . ? O12B Gd1 O7 C16 -160(2) 2_566 . . . ? O11 Gd1 O7 C16 -68(2) . . . . ? O8 Gd1 O7 C16 88(2) 2_666 . . . ? O12 Gd1 O7 C16 176(2) 2_566 . . . ? O1W Gd1 O7 C16 16(2) . . . . ? O11B Gd1 O7 C16 -66(2) . . . . ? O3 Gd1 O7 C16 161(2) . . . . ? O13 Gd1 O7 C16 -8(2) . . . . ? O4 Gd1 O7 C16 -145(2) . . . . ? C8 Gd1 O7 C16 -172(2) . . . . ? C7 C2 C3 C4 2.0(7) . . . . ? C7 C2 C3 N1 -177.9(4) . . . . ? O1 N1 C3 C4 136.5(6) . . . . ? O2 N1 C3 C4 -43.4(7) . . . . ? O1 N1 C3 C2 -43.6(8) . . . . ? O2 N1 C3 C2 136.5(5) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? N1 C3 C4 C5 179.9(5) . . . . ? C2 C3 C4 C1 178.4(5) . . . . ? N1 C3 C4 C1 -1.7(8) . . . . ? C3 C4 C5 C6 -1.8(7) . . . . ? C1 C4 C5 C6 179.7(5) . . . . ? C4 C5 C6 C7 1.6(8) . . . . ? C3 C2 C7 C6 -2.2(6) . . . . ? C3 C2 C7 C8 176.8(4) . . . . ? C5 C6 C7 C2 0.5(7) . . . . ? C5 C6 C7 C8 -178.6(4) . . . . ? Gd1 O3 C8 O4 4.4(4) . . . . ? Gd1 O3 C8 C7 -174.4(3) . . . . ? Gd1 O4 C8 O3 -4.4(4) . . . . ? Gd1 O4 C8 C7 174.4(3) . . . . ? C2 C7 C8 O3 -2.2(6) . . . . ? C6 C7 C8 O3 176.9(4) . . . . ? C2 C7 C8 O4 179.1(4) . . . . ? C6 C7 C8 O4 -1.9(6) . . . . ? C2 C7 C8 Gd1 -89(3) . . . . ? C6 C7 C8 Gd1 90(3) . . . . ? O12B Gd1 C8 O3 101.8(4) 2_566 . . . ? O11 Gd1 C8 O3 -170.8(3) . . . . ? O7 Gd1 C8 O3 -84.6(2) . . . . ? O8 Gd1 C8 O3 17.2(2) 2_666 . . . ? O12 Gd1 C8 O3 88.3(3) 2_566 . . . ? O1W Gd1 C8 O3 -72.4(3) . . . . ? O11B Gd1 C8 O3 -157.3(4) . . . . ? O13 Gd1 C8 O3 114.3(3) . . . . ? O4 Gd1 C8 O3 175.7(4) . . . . ? O12B Gd1 C8 O4 -73.9(4) 2_566 . . . ? O11 Gd1 C8 O4 13.5(3) . . . . ? O7 Gd1 C8 O4 99.7(2) . . . . ? O8 Gd1 C8 O4 -158.5(2) 2_666 . . . ? O12 Gd1 C8 O4 -87.4(3) 2_566 . . . ? O1W Gd1 C8 O4 111.9(3) . . . . ? O11B Gd1 C8 O4 26.9(4) . . . . ? O3 Gd1 C8 O4 -175.7(4) . . . . ? O13 Gd1 C8 O4 -61.4(3) . . . . ? O12B Gd1 C8 C7 -168(3) 2_566 . . . ? O11 Gd1 C8 C7 -81(3) . . . . ? O7 Gd1 C8 C7 5(3) . . . . ? O8 Gd1 C8 C7 107(3) 2_666 . . . ? O12 Gd1 C8 C7 178(3) 2_566 . . . ? O1W Gd1 C8 C7 18(3) . . . . ? O11B Gd1 C8 C7 -67(3) . . . . ? O3 Gd1 C8 C7 90(3) . . . . ? O13 Gd1 C8 C7 -156(3) . . . . ? O4 Gd1 C8 C7 -94(3) . . . . ? C15 C10 C11 C12 0.2(16) . . . . ? C9 C10 C11 C12 -178.9(10) . . . . ? C15 C10 C11 N2 -179.8(10) . . . . ? C9 C10 C11 N2 1.0(17) . . . . ? O5 N2 C11 C10 -141.3(12) . . . . ? O6 N2 C11 C10 39.1(15) . . . . ? O5 N2 C11 C12 38.6(15) . . . . ? O6 N2 C11 C12 -141.0(10) . . . . ? C10 C11 C12 C13 -1.3(14) . . . . ? N2 C11 C12 C13 178.7(8) . . . . ? C11 C12 C13 C14 1.4(11) . . . . ? C11 C12 C13 C16 179.7(7) . . . . ? C12 C13 C14 C15 -0.5(14) . . . . ? C16 C13 C14 C15 -178.8(9) . . . . ? C13 C14 C15 C10 -0.6(18) . . . . ? C11 C10 C15 C14 0.7(18) . . . . ? C9 C10 C15 C14 179.9(12) . . . . ? Gd1 O7 C16 O8 -76(2) . . . . ? Gd1 O7 C16 C13 104(2) . . . . ? Gd1 O8 C16 O7 -13.4(7) 2_666 . . . ? Gd1 O8 C16 C13 166.8(4) 2_666 . . . ? C12 C13 C16 O7 14.6(9) . . . . ? C14 C13 C16 O7 -167.1(7) . . . . ? C12 C13 C16 O8 -165.6(6) . . . . ? C14 C13 C16 O8 12.7(9) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C23 C18 C19 N3 179.4(9) . . . . ? C18 C19 C20 C21 0.0 . . . . ? N3 C19 C20 C21 -179.3(10) . . . . ? C18 C19 C20 C17 178.4(11) . . . . ? N3 C19 C20 C17 -0.9(13) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C17 C20 C21 C22 -178.5(10) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C21 C22 C23 C24 -175.3(12) . . . . ? C19 C18 C23 C22 0.0 . . . . ? C19 C18 C23 C24 175.4(12) . . . . ? C22 C23 C24 O12 -178.7(13) . . . . ? C18 C23 C24 O12 6(2) . . . . ? C22 C23 C24 O11 2(2) . . . . ? C18 C23 C24 O11 -173.5(13) . . . . ? C18 C19 N3 O10 7(2) . . . . ? C20 C19 N3 O10 -174.1(15) . . . . ? C18 C19 N3 O9 -175.7(16) . . . . ? C20 C19 N3 O9 4(2) . . . . ? O12 C24 O11 Gd1 -69(4) . . . . ? C23 C24 O11 Gd1 111(3) . . . . ? O12B Gd1 O11 C24 60(3) 2_566 . . . ? O7 Gd1 O11 C24 -88(3) . . . . ? O8 Gd1 O11 C24 147(3) 2_666 . . . ? O12 Gd1 O11 C24 62(3) 2_566 . . . ? O1W Gd1 O11 C24 -160(3) . . . . ? O11B Gd1 O11 C24 -96(4) . . . . ? O3 Gd1 O11 C24 -22(3) . . . . ? O13 Gd1 O11 C24 129(3) . . . . ? O4 Gd1 O11 C24 -11(3) . . . . ? C8 Gd1 O11 C24 -17(3) . . . . ? O11 C24 O12 Gd1 15(4) . . . 2_566 ? C23 C24 O12 Gd1 -164.4(8) . . . 2_566 ? C23B C18B C19B C20B 0.0 . . . . ? C23B C18B C19B N3B -175.8(14) . . . . ? C18B C19B C20B C21B 0.0 . . . . ? N3B C19B C20B C21B 175.8(14) . . . . ? C18B C19B C20B C17B 176.9(15) . . . . ? N3B C19B C20B C17B -7.3(17) . . . . ? C19B C20B C21B C22B 0.0 . . . . ? C17B C20B C21B C22B -176.9(15) . . . . ? C20B C21B C22B C23B 0.0 . . . . ? C21B C22B C23B C18B 0.0 . . . . ? C21B C22B C23B C24B -177(2) . . . . ? C19B C18B C23B C22B 0.0 . . . . ? C19B C18B C23B C24B 177(2) . . . . ? C22B C23B C24B O11B -5(5) . . . . ? C18B C23B C24B O11B 177(3) . . . . ? C22B C23B C24B O12B 178(2) . . . . ? C18B C23B C24B O12B 0(4) . . . . ? C18B C19B N3B O9B 143(2) . . . . ? C20B C19B N3B O9B -32(3) . . . . ? C18B C19B N3B O10B -33.0(19) . . . . ? C20B C19B N3B O10B 151.3(14) . . . . ? O12B C24B O11B Gd1 -12(6) . . . . ? C23B C24B O11B Gd1 171.2(16) . . . . ? O12B Gd1 O11B C24B 7(3) 2_566 . . . ? O11 Gd1 O11B C24B 32(3) . . . . ? O7 Gd1 O11B C24B -140(3) . . . . ? O8 Gd1 O11B C24B 121(3) 2_666 . . . ? O12 Gd1 O11B C24B 8(3) 2_566 . . . ? O1W Gd1 O11B C24B 145(3) . . . . ? O3 Gd1 O11B C24B -84(3) . . . . ? O13 Gd1 O11B C24B 74(3) . . . . ? O4 Gd1 O11B C24B -60(3) . . . . ? C8 Gd1 O11B C24B -72(3) . . . . ? O11B C24B O12B Gd1 81(33) . . . 2_566 ? C23B C24B O12B Gd1 -102(33) . . . 2_566 ? O12B Gd1 O13 C25 -81.6(6) 2_566 . . . ? O11 Gd1 O13 C25 -179.6(6) . . . . ? O7 Gd1 O13 C25 113.6(5) . . . . ? O8 Gd1 O13 C25 9.1(5) 2_666 . . . ? O12 Gd1 O13 C25 -68.2(5) 2_566 . . . ? O1W Gd1 O13 C25 89.7(5) . . . . ? O11B Gd1 O13 C25 170.9(6) . . . . ? O3 Gd1 O13 C25 -45.2(6) . . . . ? O4 Gd1 O13 C25 -124.4(5) . . . . ? C8 Gd1 O13 C25 -94.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H3W O3 0.85(6) 1.97(6) 2.824(4) 177(6) 2_666 O1W H4W O2 0.78(7) 2.10(7) 2.865(6) 168(7) 1_565 O13 H13 O4 0.89(6) 1.97(6) 2.850(4) 174(5) 2_566 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.941 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.104 data_2 _database_code_depnum_ccdc_archive 'CCDC 892519' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H34 Gd N5 O15' _chemical_formula_weight 921.92 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8528(6) _cell_length_b 13.4639(8) _cell_length_c 14.2272(10) _cell_angle_alpha 92.229(5) _cell_angle_beta 90.403(5) _cell_angle_gamma 96.000(5) _cell_volume 1875.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7952 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.00 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.559 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13349 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetl/netI 0.0869 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7952 _reflns_number_gt 6462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction,2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0423P)^2^+0.2000P] 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 8197 _refine_ls_number_parameters 520 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Gd1 Gd 0.74812(2) 0.493301(17) 0.487944(18) 0.03344(10) Uani 1 1 d D . . O1 O 0.9688(8) 0.7023(6) 0.9173(6) 0.173(4) Uani 1 1 d . . . O2 O 0.9243(8) 0.5692(6) 0.8523(8) 0.201(6) Uani 1 1 d . . . O3 O 0.5866(4) 0.5390(3) 0.5966(3) 0.0459(9) Uani 1 1 d . . . O4 O 0.3910(4) 0.6008(3) 0.6274(3) 0.0490(10) Uani 1 1 d . . . O5 O 0.5043(8) 0.0455(6) 0.8976(6) 0.150(3) Uani 1 1 d . . . O6 O 0.4685(8) 0.0564(5) 0.7569(6) 0.149(3) Uani 1 1 d . . . O7 O 0.6564(4) 0.3418(3) 0.5779(3) 0.0459(9) Uani 1 1 d . . . O8 O 0.8341(4) 0.4352(2) 0.6391(3) 0.0425(9) Uani 1 1 d . . . O9 O 1.1802(10) 0.0138(6) 0.1740(6) 0.169(4) Uani 1 1 d . . . O10 O 1.2607(9) 0.0529(6) 0.3069(7) 0.156(3) Uani 1 1 d . . . O11 O 0.9022(4) 0.3805(3) 0.4506(3) 0.0566(11) Uani 1 1 d . . . O12 O 1.1238(4) 0.3663(3) 0.4442(3) 0.0487(10) Uani 1 1 d . . . O13 O 0.8773(4) 0.5548(4) 0.3540(3) 0.0565(11) Uani 1 1 d D . . H13B H 0.9610(11) 0.559(5) 0.3543(19) 0.085 Uiso 1 1 d D . . H13C H 0.841(2) 0.553(5) 0.3013(11) 0.085 Uiso 1 1 d D . . O14 O 0.6363(4) 0.6264(3) 0.4162(3) 0.0537(11) Uani 1 1 d D . . H14B H 0.676(6) 0.683(2) 0.410(5) 0.081 Uiso 1 1 d D . . H14C H 0.553(5) 0.622(4) 0.405(5) 0.081 Uiso 1 1 d D . . N1 N 0.8919(6) 0.6439(5) 0.8754(5) 0.0756(18) Uani 1 1 d . . . N2 N 0.5271(7) 0.0865(5) 0.8276(6) 0.0813(19) Uani 1 1 d . . . N3 N 1.1728(8) 0.0541(5) 0.2493(5) 0.0815(19) Uani 1 1 d . . . N4 N 0.2071(9) 0.1966(5) 0.6194(6) 0.108(3) Uani 1 1 d . . . N5 N 0.2562(7) 0.4457(6) 0.8168(5) 0.090(2) Uani 1 1 d . . . C1 C 0.7555(10) 0.8015(6) 0.9846(6) 0.108(3) Uani 1 1 d . . . H1A H 0.7702 0.7556 1.0327 0.162 Uiso 1 1 calc R . . H1B H 0.6930 0.8471 1.0069 0.162 Uiso 1 1 calc R . . H1C H 0.8408 0.8383 0.9695 0.162 Uiso 1 1 calc R . . C2 C 0.6958(7) 0.7436(5) 0.8969(5) 0.0661(19) Uani 1 1 d . . . C3 C 0.7571(6) 0.6710(4) 0.8461(4) 0.0474(14) Uani 1 1 d . . . C4 C 0.7009(5) 0.6219(4) 0.7664(4) 0.0403(12) Uani 1 1 d . . . H4A H 0.7472 0.5743 0.7346 0.048 Uiso 1 1 calc R . . C5 C 0.5752(5) 0.6435(4) 0.7335(4) 0.0383(12) Uani 1 1 d . . . C6 C 0.5110(7) 0.7153(5) 0.7829(5) 0.077(2) Uani 1 1 d . . . H6A H 0.4260 0.7306 0.7625 0.092 Uiso 1 1 calc R . . C7 C 0.5706(9) 0.7646(6) 0.8618(6) 0.097(3) Uani 1 1 d . . . H7A H 0.5254 0.8135 0.8926 0.116 Uiso 1 1 calc R . . C8 C 0.5135(5) 0.5905(4) 0.6457(4) 0.0353(12) Uani 1 1 d . . . C9 C 0.7343(9) 0.1348(6) 0.9863(5) 0.084(2) Uani 1 1 d . . . H9A H 0.6608 0.0819 0.9858 0.126 Uiso 1 1 calc R . . H9B H 0.7249 0.1799 1.0391 0.126 Uiso 1 1 calc R . . H9C H 0.8197 0.1069 0.9910 0.126 Uiso 1 1 calc R . . C10 C 0.7301(7) 0.1911(5) 0.8956(4) 0.0564(16) Uani 1 1 d . . . C11 C 0.6371(6) 0.1690(4) 0.8214(5) 0.0531(15) Uani 1 1 d . . . C12 C 0.6398(6) 0.2225(4) 0.7397(4) 0.0502(15) Uani 1 1 d . . . H12A H 0.5754 0.2050 0.6922 0.060 Uiso 1 1 calc R . . C13 C 0.7388(6) 0.3017(4) 0.7296(4) 0.0423(13) Uani 1 1 d . . . C14 C 0.8328(6) 0.3250(4) 0.8019(4) 0.0511(15) Uani 1 1 d . . . H14A H 0.9002 0.3781 0.7963 0.061 Uiso 1 1 calc R . . C15 C 0.8278(7) 0.2704(5) 0.8822(5) 0.0613(18) Uani 1 1 d . . . H15A H 0.8930 0.2878 0.9293 0.074 Uiso 1 1 calc R . . C16 C 0.7433(5) 0.3629(4) 0.6438(4) 0.0389(12) Uani 1 1 d . . . C17 C 0.8949(10) -0.0154(5) 0.1713(6) 0.102(3) Uani 1 1 d . . . H17A H 0.7980 -0.0334 0.1681 0.153 Uiso 1 1 calc R . . H17B H 0.9385 -0.0695 0.1961 0.153 Uiso 1 1 calc R . . H17C H 0.9285 -0.0020 0.1094 0.153 Uiso 1 1 calc R . . C18 C 0.9258(8) 0.0772(4) 0.2350(5) 0.0637(19) Uani 1 1 d . . . C19 C 1.0548(7) 0.1091(4) 0.2730(4) 0.0511(15) Uani 1 1 d . . . C20 C 1.0810(6) 0.1913(4) 0.3332(4) 0.0416(13) Uani 1 1 d . . . H20A H 1.1686 0.2088 0.3573 0.050 Uiso 1 1 calc R . . C21 C 0.9771(5) 0.2474(4) 0.3576(4) 0.0372(12) Uani 1 1 d . . . C22 C 0.8471(6) 0.2172(4) 0.3215(5) 0.0608(18) Uani 1 1 d . . . H22A H 0.7746 0.2532 0.3379 0.073 Uiso 1 1 calc R . . C23 C 0.8255(7) 0.1342(5) 0.2614(5) 0.074(2) Uani 1 1 d . . . H23A H 0.7378 0.1163 0.2377 0.089 Uiso 1 1 calc R . . C24 C 1.0019(6) 0.3386(4) 0.4223(4) 0.0360(12) Uani 1 1 d . . . C25 C 0.0720(10) 0.1948(7) 0.6107(7) 0.106(3) Uani 1 1 d . . . H25A H 0.0326 0.2493 0.6366 0.127 Uiso 1 1 calc R . . C26 C -0.0110(10) 0.1230(6) 0.5689(6) 0.090(3) Uani 1 1 d . . . H26A H -0.1047 0.1268 0.5680 0.108 Uiso 1 1 calc R . . C27 C 0.0442(9) 0.0407(5) 0.5258(6) 0.073(2) Uani 1 1 d . . . C28 C 0.1816(11) 0.0391(7) 0.5372(7) 0.107(3) Uani 1 1 d . . . H28A H 0.2236 -0.0159 0.5153 0.128 Uiso 1 1 calc R . . C29 C 0.2576(11) 0.1193(7) 0.5815(8) 0.115(4) Uani 1 1 d . . . H29A H 0.3518 0.1182 0.5844 0.138 Uiso 1 1 calc R . . C30 C 0.2398(10) 0.5115(9) 0.8836(8) 0.139(5) Uani 1 1 d . . . H30A H 0.1620 0.5450 0.8824 0.167 Uiso 1 1 calc R . . C31 C 0.4489(7) 0.4879(5) 0.9617(5) 0.0622(18) Uani 1 1 d . . . C32 C 0.4622(9) 0.4185(6) 0.8918(6) 0.093(3) Uani 1 1 d . . . H32A H 0.5384 0.3831 0.8910 0.112 Uiso 1 1 calc R . . C33 C 0.3655(11) 0.3997(7) 0.8224(6) 0.106(3) Uani 1 1 d . . . H33A H 0.3785 0.3509 0.7762 0.128 Uiso 1 1 calc R . . C34 C 0.3331(10) 0.5342(8) 0.9568(7) 0.124(4) Uani 1 1 d . . . H34A H 0.3161 0.5818 1.0032 0.149 Uiso 1 1 calc R . . O15 O 0.6030(12) 0.1397(7) 0.5035(9) 0.213(5) Uani 1 1 d . . . H15 H 0.6025 0.1986 0.5203 0.319 Uiso 1 1 calc R . . C35 C 0.514(2) 0.1176(18) 0.4248(14) 0.344(17) Uani 1 1 d . . . H35C H 0.5550 0.1477 0.3703 0.516 Uiso 1 1 calc R . . H35A H 0.4288 0.1437 0.4371 0.516 Uiso 1 1 calc R . . H35B H 0.4989 0.0465 0.4138 0.516 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02009(13) 0.04429(16) 0.03509(17) -0.00956(10) -0.00529(10) 0.00388(10) O1 0.092(5) 0.234(8) 0.188(9) -0.106(7) -0.096(6) 0.041(5) O2 0.123(7) 0.169(7) 0.316(13) -0.128(8) -0.154(8) 0.094(6) O3 0.032(2) 0.062(2) 0.042(2) -0.0224(18) -0.0019(17) 0.0046(17) O4 0.025(2) 0.070(2) 0.052(3) -0.0167(19) -0.0167(18) 0.0109(17) O5 0.128(7) 0.179(7) 0.134(7) 0.081(6) -0.005(5) -0.059(5) O6 0.135(7) 0.144(6) 0.151(7) 0.051(5) -0.051(6) -0.079(5) O7 0.035(2) 0.055(2) 0.046(2) -0.0021(18) -0.0132(18) -0.0027(17) O8 0.032(2) 0.046(2) 0.048(2) -0.0016(17) -0.0075(17) -0.0006(16) O9 0.193(9) 0.174(7) 0.146(7) -0.090(6) 0.000(6) 0.081(6) O10 0.120(7) 0.193(8) 0.167(8) -0.061(6) -0.024(6) 0.101(6) O11 0.046(3) 0.070(3) 0.056(3) -0.024(2) -0.008(2) 0.027(2) O12 0.034(2) 0.056(2) 0.053(3) -0.0171(18) -0.0090(18) -0.0029(17) O13 0.023(2) 0.100(3) 0.046(3) 0.004(2) -0.0036(18) 0.006(2) O14 0.027(2) 0.061(3) 0.073(3) 0.009(2) -0.007(2) 0.0008(18) N1 0.058(4) 0.092(4) 0.075(4) -0.019(3) -0.043(3) 0.010(3) N2 0.067(5) 0.084(4) 0.091(6) 0.023(4) -0.002(4) -0.005(4) N3 0.098(6) 0.075(4) 0.076(5) -0.025(3) 0.000(4) 0.039(4) N4 0.098(7) 0.078(5) 0.145(8) 0.003(5) -0.015(6) -0.009(4) N5 0.063(5) 0.147(6) 0.062(5) -0.005(4) -0.024(4) 0.027(4) C1 0.116(8) 0.121(7) 0.082(6) -0.061(5) -0.045(6) 0.019(6) C2 0.061(5) 0.082(4) 0.054(4) -0.026(3) -0.024(3) 0.009(4) C3 0.037(3) 0.058(3) 0.046(4) -0.006(3) -0.016(3) 0.002(3) C4 0.029(3) 0.049(3) 0.041(3) -0.012(2) -0.006(2) 0.003(2) C5 0.030(3) 0.045(3) 0.039(3) -0.012(2) -0.010(2) 0.006(2) C6 0.046(4) 0.105(5) 0.082(5) -0.046(4) -0.019(4) 0.035(4) C7 0.084(6) 0.118(6) 0.090(6) -0.070(5) -0.037(5) 0.047(5) C8 0.022(3) 0.050(3) 0.032(3) -0.006(2) -0.005(2) 0.000(2) C9 0.103(7) 0.086(5) 0.067(5) 0.021(4) 0.013(5) 0.021(5) C10 0.065(5) 0.062(4) 0.046(4) 0.000(3) 0.004(3) 0.023(3) C11 0.049(4) 0.051(3) 0.060(4) 0.001(3) 0.007(3) 0.009(3) C12 0.037(3) 0.058(4) 0.056(4) -0.002(3) -0.005(3) 0.010(3) C13 0.036(3) 0.048(3) 0.044(3) -0.004(2) -0.003(3) 0.008(2) C14 0.047(4) 0.058(4) 0.048(4) 0.002(3) -0.007(3) 0.002(3) C15 0.068(5) 0.070(4) 0.046(4) -0.003(3) -0.020(3) 0.009(4) C16 0.027(3) 0.045(3) 0.045(3) -0.006(2) -0.002(2) 0.006(2) C17 0.141(9) 0.069(5) 0.091(7) -0.036(4) -0.024(6) 0.001(5) C18 0.084(6) 0.047(3) 0.058(4) -0.012(3) -0.015(4) 0.005(3) C19 0.062(4) 0.043(3) 0.049(4) -0.007(3) 0.005(3) 0.013(3) C20 0.035(3) 0.040(3) 0.050(4) -0.004(2) 0.000(3) 0.004(2) C21 0.032(3) 0.041(3) 0.037(3) -0.009(2) -0.008(2) 0.002(2) C22 0.036(3) 0.064(4) 0.081(5) -0.024(3) -0.010(3) 0.006(3) C23 0.052(4) 0.075(4) 0.089(6) -0.029(4) -0.034(4) -0.001(4) C24 0.037(3) 0.043(3) 0.028(3) -0.002(2) -0.006(2) 0.006(2) C25 0.079(7) 0.098(6) 0.135(9) -0.009(6) 0.006(6) -0.014(5) C26 0.104(7) 0.066(5) 0.095(7) -0.003(4) 0.005(5) -0.009(5) C27 0.080(6) 0.067(5) 0.072(5) 0.018(4) -0.002(4) -0.003(4) C28 0.098(8) 0.100(6) 0.118(8) 0.009(6) -0.021(6) -0.008(6) C29 0.093(8) 0.089(6) 0.161(11) -0.028(6) -0.037(7) 0.014(6) C30 0.080(7) 0.227(12) 0.121(9) -0.057(9) -0.052(7) 0.088(8) C31 0.051(4) 0.096(5) 0.044(4) 0.002(4) -0.009(3) 0.028(4) C32 0.091(6) 0.136(7) 0.059(5) -0.028(5) -0.034(5) 0.063(5) C33 0.110(8) 0.152(8) 0.064(6) -0.023(5) -0.030(5) 0.052(7) C34 0.081(7) 0.183(9) 0.115(8) -0.074(7) -0.045(6) 0.078(7) O15 0.233(13) 0.155(8) 0.249(14) -0.011(8) 0.015(11) 0.018(7) C35 0.29(3) 0.52(4) 0.19(2) -0.09(2) -0.13(2) -0.07(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 Gd1 O11 2.308(4) . ? Gd1 O12 2.332(3) 2_766 ? Gd1 O3 2.338(4) . ? Gd1 O4 2.371(3) 2_666 ? Gd1 O13 2.424(4) . ? Gd1 O14 2.451(4) . ? Gd1 O8 2.490(4) . ? Gd1 O7 2.539(4) . ? Gd1 C16 2.879(5) . ? O1 N1 1.174(8) . ? O2 N1 1.125(8) . ? O3 C8 1.250(6) . ? O4 C8 1.256(6) . ? O4 Gd1 2.371(3) 2_666 ? O5 N2 1.170(8) . ? O6 N2 1.192(9) . ? O7 C16 1.270(6) . ? O8 C16 1.255(6) . ? O9 N3 1.189(9) . ? O10 N3 1.189(9) . ? O11 C24 1.244(6) . ? O12 C24 1.254(6) . ? O12 Gd1 2.332(3) 2_766 ? O13 H13B 0.820(10) . ? O13 H13C 0.825(10) . ? O14 H14B 0.823(10) . ? O14 H14C 0.83(5) . ? N1 C3 1.475(8) . ? N2 C11 1.474(8) . ? N3 C19 1.476(9) . ? N4 C29 1.300(12) . ? N4 C25 1.333(11) . ? N5 C30 1.296(11) . ? N5 C33 1.300(10) . ? C1 C2 1.526(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.384(9) . ? C2 C7 1.388(10) . ? C3 C4 1.374(7) . ? C4 C5 1.384(7) . ? C4 H4A 0.9300 . ? C5 C6 1.382(8) . ? C5 C8 1.505(7) . ? C6 C7 1.377(9) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.524(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.382(9) . ? C10 C11 1.395(9) . ? C11 C12 1.391(8) . ? C12 C13 1.381(7) . ? C12 H12A 0.9300 . ? C13 C14 1.384(8) . ? C13 C16 1.497(7) . ? C14 C15 1.381(8) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 C18 1.515(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.360(10) . ? C18 C19 1.396(9) . ? C19 C20 1.374(7) . ? C20 C21 1.373(7) . ? C20 H20A 0.9300 . ? C21 C22 1.391(7) . ? C21 C24 1.504(7) . ? C22 C23 1.377(8) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.319(11) . ? C25 H25A 0.9300 . ? C26 C27 1.407(11) . ? C26 H26A 0.9300 . ? C27 C28 1.365(12) . ? C27 C27 1.493(15) 2_556 ? C28 C29 1.377(11) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C34 1.388(12) . ? C30 H30A 0.9300 . ? C31 C32 1.354(10) . ? C31 C34 1.359(10) . ? C31 C31 1.483(12) 2_667 ? C32 C33 1.365(11) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? O15 C35 1.418(17) . ? O15 H15 0.8200 . ? C35 H35C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Gd1 O12 105.94(14) . 2_766 ? O11 Gd1 O3 145.39(15) . . ? O12 Gd1 O3 82.18(13) 2_766 . ? O11 Gd1 O4 83.83(13) . 2_666 ? O12 Gd1 O4 156.70(14) 2_766 2_666 ? O3 Gd1 O4 101.94(13) . 2_666 ? O11 Gd1 O13 72.46(16) . . ? O12 Gd1 O13 78.89(15) 2_766 . ? O3 Gd1 O13 141.67(15) . . ? O4 Gd1 O13 84.25(14) 2_666 . ? O11 Gd1 O14 139.96(16) . . ? O12 Gd1 O14 79.73(13) 2_766 . ? O3 Gd1 O14 74.14(15) . . ? O4 Gd1 O14 79.43(13) 2_666 . ? O13 Gd1 O14 69.88(15) . . ? O11 Gd1 O8 72.97(14) . . ? O12 Gd1 O8 75.57(12) 2_766 . ? O3 Gd1 O8 76.88(13) . . ? O4 Gd1 O8 127.73(12) 2_666 . ? O13 Gd1 O8 128.70(12) . . ? O14 Gd1 O8 144.01(14) . . ? O11 Gd1 O7 77.74(14) . . ? O12 Gd1 O7 124.30(13) 2_766 . ? O3 Gd1 O7 70.37(13) . . ? O4 Gd1 O7 78.05(13) 2_666 . ? O13 Gd1 O7 146.70(15) . . ? O14 Gd1 O7 132.42(13) . . ? O8 Gd1 O7 51.86(11) . . ? O11 Gd1 C16 74.65(15) . . ? O12 Gd1 C16 99.54(14) 2_766 . ? O3 Gd1 C16 70.81(14) . . ? O4 Gd1 C16 103.47(14) 2_666 . ? O13 Gd1 C16 145.13(14) . . ? O14 Gd1 C16 144.67(15) . . ? O8 Gd1 C16 25.74(12) . . ? O7 Gd1 C16 26.15(12) . . ? C8 O3 Gd1 161.6(4) . . ? C8 O4 Gd1 125.9(3) . 2_666 ? C16 O7 Gd1 92.0(3) . . ? C16 O8 Gd1 94.7(3) . . ? C24 O11 Gd1 165.4(4) . . ? C24 O12 Gd1 138.4(4) . 2_766 ? Gd1 O13 H13B 120.9(17) . . ? Gd1 O13 H13C 120.4(17) . . ? H13B O13 H13C 115(2) . . ? Gd1 O14 H14B 122(5) . . ? Gd1 O14 H14C 123(4) . . ? H14B O14 H14C 114(5) . . ? O2 N1 O1 119.9(8) . . ? O2 N1 C3 119.5(6) . . ? O1 N1 C3 120.3(7) . . ? O5 N2 O6 119.8(8) . . ? O5 N2 C11 121.8(8) . . ? O6 N2 C11 118.0(7) . . ? O9 N3 O10 121.2(9) . . ? O9 N3 C19 120.5(8) . . ? O10 N3 C19 118.2(7) . . ? C29 N4 C25 114.7(8) . . ? C30 N5 C33 116.2(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 115.3(6) . . ? C3 C2 C1 125.6(6) . . ? C7 C2 C1 119.1(7) . . ? C4 C3 C2 123.8(5) . . ? C4 C3 N1 116.0(6) . . ? C2 C3 N1 120.2(5) . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 117.8(5) . . ? C6 C5 C8 122.1(5) . . ? C4 C5 C8 120.1(5) . . ? C7 C6 C5 121.2(6) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C2 122.1(7) . . ? C6 C7 H7A 118.9 . . ? C2 C7 H7A 118.9 . . ? O3 C8 O4 124.5(5) . . ? O3 C8 C5 118.2(4) . . ? O4 C8 C5 117.3(5) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 115.2(6) . . ? C15 C10 C9 118.7(6) . . ? C11 C10 C9 126.1(6) . . ? C12 C11 C10 123.4(6) . . ? C12 C11 N2 116.3(6) . . ? C10 C11 N2 120.3(6) . . ? C13 C12 C11 119.5(6) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 118.3(5) . . ? C12 C13 C16 121.3(5) . . ? C14 C13 C16 120.4(5) . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C10 122.7(6) . . ? C14 C15 H15A 118.7 . . ? C10 C15 H15A 118.7 . . ? O8 C16 O7 121.2(5) . . ? O8 C16 C13 118.6(5) . . ? O7 C16 C13 120.2(4) . . ? O8 C16 Gd1 59.5(3) . . ? O7 C16 Gd1 61.8(3) . . ? C13 C16 Gd1 175.7(4) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 115.0(5) . . ? C23 C18 C17 121.0(7) . . ? C19 C18 C17 124.0(7) . . ? C20 C19 C18 123.6(6) . . ? C20 C19 N3 116.0(6) . . ? C18 C19 N3 120.4(6) . . ? C21 C20 C19 119.6(5) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 118.2(5) . . ? C20 C21 C24 121.3(5) . . ? C22 C21 C24 120.5(5) . . ? C23 C22 C21 120.1(6) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C18 C23 C22 123.4(6) . . ? C18 C23 H23A 118.3 . . ? C22 C23 H23A 118.3 . . ? O11 C24 O12 124.8(5) . . ? O11 C24 C21 118.8(5) . . ? O12 C24 C21 116.4(5) . . ? C26 C25 N4 126.2(10) . . ? C26 C25 H25A 116.9 . . ? N4 C25 H25A 116.9 . . ? C25 C26 C27 119.0(10) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C28 C27 C26 115.7(8) . . ? C28 C27 C27 122.9(10) . 2_556 ? C26 C27 C27 121.4(10) . 2_556 ? C27 C28 C29 119.6(10) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? N4 C29 C28 124.6(10) . . ? N4 C29 H29A 117.7 . . ? C28 C29 H29A 117.7 . . ? N5 C30 C34 123.0(9) . . ? N5 C30 H30A 118.5 . . ? C34 C30 H30A 118.5 . . ? C32 C31 C34 114.8(7) . . ? C32 C31 C31 123.4(8) . 2_667 ? C34 C31 C31 121.9(9) . 2_667 ? C31 C32 C33 121.0(8) . . ? C31 C32 H32A 119.5 . . ? C33 C32 H32A 119.5 . . ? N5 C33 C32 124.2(9) . . ? N5 C33 H33A 117.9 . . ? C32 C33 H33A 117.9 . . ? C31 C34 C30 120.9(9) . . ? C31 C34 H34A 119.6 . . ? C30 C34 H34A 119.6 . . ? C35 O15 H15 109.5 . . ? O15 C35 H35C 109.5 . . ? O15 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? O15 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13B O8 0.820(10) 2.014(11) 2.833(5) 177(3) 2_766 O13 H13C N5 0.825(10) 1.931(13) 2.754(7) 174(5) 2_666 O14 H14B N4 0.823(10) 1.953(19) 2.766(8) 170(7) 2_666 O14 H14C O7 0.83(5) 2.19(6) 2.961(6) 156(7) 2_666 O14 H14C O3 0.83(5) 2.44(4) 2.960(5) 122(6) 2_666 O15 H15 O7 0.82 2.08 2.876(11) 163.5 . _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.568 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.119