# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_ARCakhdt_1 _database_code_depnum_ccdc_archive 'CCDC 866033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 La N5 O13' _chemical_formula_sum 'C42 H36 La N5 O13' _chemical_formula_weight 957.67 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' La La -0.2871 2.4523 '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 10.7473(6) _cell_length_b 12.5084(8) _cell_length_c 15.0670(9) _cell_angle_alpha 86.953(5) _cell_angle_beta 89.168(5) _cell_angle_gamma 79.358(5) _cell_volume 1987.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.8027 _exptl_absorpt_process_details ? _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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29817 _diffrn_reflns_av_R_equivalents 0.1366 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6983 _reflns_number_gt 4980 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0473P)^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 6983 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 La1 La 0.28179(3) 0.31461(3) 0.21637(2) 0.04103(16) Uani 1 1 d . . . O1 O 0.1606(4) 0.2275(4) 0.1195(3) 0.0502(12) Uani 1 1 d . . . O9 O -0.3338(4) 0.2135(4) -0.3048(3) 0.0588(13) Uani 1 1 d . . . H09 H -0.3848 0.1734 -0.2931 0.088 Uiso 1 1 calc R . . O3 O 0.4505(5) 0.2623(4) 0.0898(3) 0.0611(13) Uani 1 1 d . . . O2 O 0.2293(4) 0.1577(4) 0.2979(3) 0.0535(13) Uani 1 1 d . . . O11 O 0.1734(4) -0.2957(4) 0.7229(3) 0.0600(13) Uani 1 1 d . . . H011 H 0.1267 -0.3384 0.7122 0.090 Uiso 1 1 calc R . . O12 O 0.0369(5) -0.3085(4) 0.5787(3) 0.0773(17) Uani 1 1 d . . . O5 O 0.4887(5) 0.1682(4) 0.2126(3) 0.0669(14) Uani 1 1 d . . . N2 N 0.4278(4) 0.4681(4) 0.2140(3) 0.0349(12) Uani 1 1 d . . . O6 O 0.0431(4) 0.4044(4) 0.2326(3) 0.0606(13) Uani 1 1 d . . . C14 C 0.5838(6) 0.6268(5) 0.2089(4) 0.0400(15) Uani 1 1 d . . . C17 C 0.3367(5) 0.5357(5) 0.0718(3) 0.0330(14) Uani 1 1 d . . . N3 N 0.2570(5) 0.4638(4) 0.0848(3) 0.0447(14) Uani 1 1 d . . . N1 N 0.4278(5) 0.3254(4) 0.3559(3) 0.0462(14) Uani 1 1 d . . . O10 O -0.3652(5) 0.0919(4) -0.1618(3) 0.0675(15) Uani 1 1 d . . . O8 O 0.1667(5) 0.4611(4) 0.3221(3) 0.0650(14) Uani 1 1 d . . . C5 C 0.5077(6) 0.3965(5) 0.3595(4) 0.0400(15) Uani 1 1 d . . . C42 C -0.0350(10) -0.3206(8) 0.5036(5) 0.118(4) Uani 1 1 d . . . H42A H -0.0779 -0.3809 0.5148 0.177 Uiso 1 1 calc R . . H42B H 0.0201 -0.3340 0.4531 0.177 Uiso 1 1 calc R . . H42C H -0.0962 -0.2552 0.4919 0.177 Uiso 1 1 calc R . . C13 C 0.6595(6) 0.7154(5) 0.2085(4) 0.0398(15) Uani 1 1 d . . . C16 C 0.4266(5) 0.5406(4) 0.1453(3) 0.0323(13) Uani 1 1 d . . . C36 C 0.1844(6) -0.0753(5) 0.5086(4) 0.0391(15) Uani 1 1 d . . . C39 C 0.1746(6) -0.2231(5) 0.6518(4) 0.0452(16) Uani 1 1 d . . . C6 C 0.5094(6) 0.4722(5) 0.2809(4) 0.0397(15) Uani 1 1 d . . . C34 C 0.1315(5) 0.0191(5) 0.3584(3) 0.0403(15) Uani 1 1 d . . . H34 H 0.0721 -0.0249 0.3500 0.048 Uiso 1 1 calc R . . C31 C 0.0818(6) 0.1633(5) 0.1336(4) 0.0406(15) Uani 1 1 d . . . O4 O 0.6305(5) 0.1504(5) 0.1086(4) 0.0777(16) Uani 1 1 d . . . C30 C -0.0073(6) 0.1543(5) 0.0622(4) 0.0473(17) Uani 1 1 d . . . H30 H -0.0656 0.1087 0.0731 0.057 Uiso 1 1 calc R . . C21 C 0.1760(6) 0.4581(5) 0.0192(4) 0.0511(18) Uani 1 1 d . . . H21 H 0.1202 0.4098 0.0279 0.061 Uiso 1 1 calc R . . C28 C -0.0946(6) 0.2077(5) -0.0909(4) 0.0420(16) Uani 1 1 d . . . C7 C 0.5877(6) 0.5503(5) 0.2780(4) 0.0415(16) Uani 1 1 d . . . H7 H 0.6439 0.5503 0.3243 0.050 Uiso 1 1 calc R . . O7 O -0.0339(6) 0.5328(5) 0.3197(4) 0.0874(18) Uani 1 1 d . . . C3 C 0.5732(7) 0.3248(6) 0.5042(4) 0.059(2) Uani 1 1 d . . . H3 H 0.6224 0.3249 0.5544 0.070 Uiso 1 1 calc R . . C35 C 0.1925(6) 0.0031(5) 0.4343(4) 0.0428(16) Uani 1 1 d . . . H35 H 0.2501 0.0490 0.4420 0.051 Uiso 1 1 calc R . . C27 C -0.1887(6) 0.1467(5) -0.0880(4) 0.0419(16) Uani 1 1 d . . . H27 H -0.1986 0.1038 -0.0369 0.050 Uiso 1 1 calc R . . C41 C 0.1063(6) -0.2272(5) 0.5754(4) 0.0409(15) Uani 1 1 d . . . C29 C -0.0099(6) 0.2066(5) -0.0161(4) 0.0442(16) Uani 1 1 d . . . H29 H 0.0518 0.2493 -0.0251 0.053 Uiso 1 1 calc R . . C8 C 0.7168(6) 0.7368(6) 0.2861(5) 0.060(2) Uani 1 1 d . . . H8 H 0.7125 0.6928 0.3374 0.072 Uiso 1 1 calc R . . C33 C 0.1460(5) 0.0973(5) 0.2865(3) 0.0359(14) Uani 1 1 d . . . C1 C 0.4219(7) 0.2564(6) 0.4251(4) 0.061(2) Uani 1 1 d . . . H1 H 0.3662 0.2080 0.4221 0.073 Uiso 1 1 calc R . . C40 C 0.1118(6) -0.1558(5) 0.5048(4) 0.0437(16) Uani 1 1 d . . . H40 H 0.0665 -0.1610 0.4535 0.052 Uiso 1 1 calc R . . N4 N 0.5259(6) 0.1920(5) 0.1359(4) 0.0520(15) Uani 1 1 d . . . C37 C 0.2546(6) -0.0736(6) 0.5845(4) 0.0545(19) Uani 1 1 d . . . H37 H 0.3074 -0.0227 0.5872 0.065 Uiso 1 1 calc R . . C18 C 0.3316(6) 0.6016(5) -0.0060(4) 0.0410(15) Uani 1 1 d . . . H18 H 0.3845 0.6524 -0.0134 0.049 Uiso 1 1 calc R . . C38 C 0.2483(6) -0.1449(6) 0.6557(4) 0.0526(18) Uani 1 1 d . . . H38 H 0.2940 -0.1404 0.7069 0.063 Uiso 1 1 calc R . . C24 C -0.2546(6) 0.2110(5) -0.2341(4) 0.0456(16) Uani 1 1 d . . . C4 C 0.5817(7) 0.3971(5) 0.4344(4) 0.0522(18) Uani 1 1 d . . . H4 H 0.6364 0.4463 0.4369 0.063 Uiso 1 1 calc R . . C12 C 0.6732(6) 0.7786(5) 0.1325(5) 0.0563(19) Uani 1 1 d . . . H12 H 0.6397 0.7625 0.0793 0.068 Uiso 1 1 calc R . . C20 C 0.1695(6) 0.5180(5) -0.0594(4) 0.0518(18) Uani 1 1 d . . . H20 H 0.1130 0.5090 -0.1034 0.062 Uiso 1 1 calc R . . C26 C -0.0845(7) 0.2709(5) -0.1677(4) 0.0536(18) Uani 1 1 d . . . H26 H -0.0217 0.3131 -0.1711 0.064 Uiso 1 1 calc R . . C2 C 0.4926(7) 0.2517(6) 0.5010(4) 0.059(2) Uani 1 1 d . . . H2 H 0.4862 0.2015 0.5478 0.071 Uiso 1 1 calc R . . N5 N 0.0549(6) 0.4689(5) 0.2928(4) 0.0577(16) Uani 1 1 d . . . C19 C 0.2478(6) 0.5910(5) -0.0717(4) 0.0479(17) Uani 1 1 d . . . H19 H 0.2449 0.6338 -0.1243 0.058 Uiso 1 1 calc R . . C15 C 0.4987(5) 0.6219(5) 0.1411(4) 0.0405(15) Uani 1 1 d . . . H15 H 0.4903 0.6728 0.0933 0.049 Uiso 1 1 calc R . . C11 C 0.7359(7) 0.8656(6) 0.1342(5) 0.067(2) Uani 1 1 d . . . H11 H 0.7420 0.9093 0.0830 0.080 Uiso 1 1 calc R . . C32 C 0.0735(6) 0.1005(5) 0.2119(4) 0.0443(16) Uani 1 1 d . . . H32 H 0.0126 0.0563 0.2137 0.053 Uiso 1 1 calc R . . C25 C -0.1626(7) 0.2741(5) -0.2390(4) 0.0519(18) Uani 1 1 d . . . H25 H -0.1537 0.3180 -0.2896 0.062 Uiso 1 1 calc R . . C22 C -0.3888(7) 0.0248(6) -0.0869(4) 0.067(2) Uani 1 1 d . . . H22A H -0.4598 -0.0088 -0.0987 0.101 Uiso 1 1 calc R . . H22B H -0.4071 0.0684 -0.0361 0.101 Uiso 1 1 calc R . . H22C H -0.3155 -0.0305 -0.0751 0.101 Uiso 1 1 calc R . . C23 C -0.2680(6) 0.1473(5) -0.1579(4) 0.0443(16) Uani 1 1 d . . . C9 C 0.7807(7) 0.8241(6) 0.2871(6) 0.071(2) Uani 1 1 d . . . H9 H 0.8175 0.8391 0.3394 0.085 Uiso 1 1 calc R . . C10 C 0.7894(7) 0.8870(6) 0.2123(6) 0.068(2) Uani 1 1 d . . . H10 H 0.8318 0.9453 0.2136 0.081 Uiso 1 1 calc R . . OW1 O -0.4749(5) 0.0393(4) -0.3296(3) 0.0775(16) 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 La1 0.0466(3) 0.0445(3) 0.0356(2) 0.01192(17) -0.00971(17) -0.02099(19) O1 0.059(3) 0.057(3) 0.042(2) 0.011(2) -0.009(2) -0.036(3) O9 0.073(3) 0.068(3) 0.033(2) 0.012(2) -0.017(2) -0.010(3) O3 0.063(3) 0.073(4) 0.046(3) 0.017(3) -0.001(2) -0.016(3) O2 0.065(3) 0.059(3) 0.043(3) 0.015(2) -0.012(2) -0.032(3) O11 0.065(3) 0.069(3) 0.045(3) 0.025(2) -0.011(2) -0.017(3) O12 0.108(4) 0.083(4) 0.054(3) 0.027(3) -0.025(3) -0.058(4) O5 0.063(3) 0.083(4) 0.048(3) 0.020(3) -0.003(3) -0.002(3) N2 0.038(3) 0.034(3) 0.033(3) 0.005(2) -0.007(2) -0.010(2) O6 0.056(3) 0.074(4) 0.053(3) 0.002(3) -0.011(2) -0.017(3) C14 0.045(4) 0.040(4) 0.037(3) 0.001(3) -0.004(3) -0.014(3) C17 0.036(3) 0.036(3) 0.027(3) 0.003(3) -0.007(3) -0.006(3) N3 0.044(3) 0.053(4) 0.040(3) 0.014(2) -0.017(3) -0.019(3) N1 0.060(4) 0.046(3) 0.034(3) 0.011(2) -0.009(3) -0.016(3) O10 0.077(4) 0.087(4) 0.049(3) 0.011(3) -0.013(3) -0.044(3) O8 0.063(4) 0.068(4) 0.068(3) -0.007(3) -0.002(3) -0.022(3) C5 0.051(4) 0.032(4) 0.038(3) 0.001(3) -0.014(3) -0.009(3) C42 0.194(11) 0.132(9) 0.057(5) 0.031(5) -0.039(6) -0.112(9) C13 0.037(4) 0.033(4) 0.050(4) -0.003(3) -0.001(3) -0.008(3) C16 0.037(3) 0.029(3) 0.030(3) 0.003(2) -0.004(3) -0.005(3) C36 0.036(4) 0.040(4) 0.041(4) 0.006(3) -0.001(3) -0.005(3) C39 0.049(4) 0.048(4) 0.035(4) 0.011(3) -0.003(3) -0.004(3) C6 0.043(4) 0.035(4) 0.040(4) 0.001(3) -0.002(3) -0.004(3) C34 0.038(4) 0.058(4) 0.021(3) -0.001(3) -0.008(3) 0.002(3) C31 0.041(4) 0.046(4) 0.037(3) -0.002(3) -0.007(3) -0.012(3) O4 0.065(4) 0.086(4) 0.080(4) -0.012(3) 0.014(3) -0.006(3) C30 0.051(4) 0.052(4) 0.044(4) 0.008(3) -0.010(3) -0.025(3) C21 0.049(4) 0.051(4) 0.058(4) 0.019(3) -0.022(3) -0.024(4) C28 0.048(4) 0.047(4) 0.034(3) 0.002(3) -0.009(3) -0.017(3) C7 0.049(4) 0.045(4) 0.033(3) 0.002(3) -0.012(3) -0.017(3) O7 0.078(4) 0.080(4) 0.099(5) -0.008(4) 0.017(3) 0.000(4) C3 0.080(5) 0.064(5) 0.032(4) 0.009(3) -0.022(4) -0.016(4) C35 0.041(4) 0.035(4) 0.054(4) 0.004(3) 0.008(3) -0.014(3) C27 0.050(4) 0.048(4) 0.029(3) 0.010(3) -0.002(3) -0.015(3) C41 0.045(4) 0.044(4) 0.036(3) 0.011(3) -0.006(3) -0.015(3) C29 0.045(4) 0.045(4) 0.047(4) 0.000(3) 0.001(3) -0.020(3) C8 0.059(5) 0.071(5) 0.057(4) 0.005(4) -0.013(4) -0.033(4) C33 0.038(4) 0.043(4) 0.028(3) 0.011(3) 0.001(3) -0.013(3) C1 0.084(6) 0.065(5) 0.042(4) 0.022(3) -0.027(4) -0.038(4) C40 0.051(4) 0.048(4) 0.034(3) 0.013(3) -0.011(3) -0.016(3) N4 0.054(4) 0.055(4) 0.052(4) -0.004(3) -0.002(3) -0.021(3) C37 0.055(5) 0.059(5) 0.054(4) 0.008(4) -0.011(4) -0.023(4) C18 0.048(4) 0.044(4) 0.031(3) 0.007(3) 0.002(3) -0.012(3) C38 0.054(4) 0.064(5) 0.040(4) 0.009(3) -0.014(3) -0.014(4) C24 0.050(4) 0.050(4) 0.034(4) -0.001(3) -0.004(3) -0.003(3) C4 0.068(5) 0.053(4) 0.040(4) 0.006(3) -0.023(3) -0.022(4) C12 0.057(5) 0.052(5) 0.065(5) 0.012(4) -0.015(4) -0.027(4) C20 0.055(4) 0.053(5) 0.048(4) 0.006(3) -0.020(3) -0.012(4) C26 0.068(5) 0.047(4) 0.049(4) 0.006(3) -0.004(4) -0.022(4) C2 0.081(6) 0.056(5) 0.038(4) 0.019(3) -0.010(4) -0.013(4) N5 0.059(5) 0.058(4) 0.054(4) 0.014(3) 0.002(3) -0.010(4) C19 0.054(4) 0.053(4) 0.033(3) 0.015(3) -0.004(3) -0.006(4) C15 0.040(4) 0.036(4) 0.046(4) 0.006(3) 0.001(3) -0.010(3) C11 0.069(5) 0.059(5) 0.076(5) 0.012(4) -0.008(4) -0.025(4) C32 0.036(4) 0.055(4) 0.046(4) 0.006(3) -0.004(3) -0.020(3) C25 0.076(5) 0.047(4) 0.035(4) 0.013(3) 0.000(3) -0.022(4) C22 0.072(5) 0.080(6) 0.057(5) 0.014(4) -0.011(4) -0.038(5) C23 0.050(4) 0.049(4) 0.035(4) 0.003(3) -0.004(3) -0.012(3) C9 0.073(6) 0.067(6) 0.081(6) -0.006(4) -0.015(5) -0.033(5) C10 0.050(5) 0.062(5) 0.098(6) 0.003(5) -0.004(4) -0.028(4) OW1 0.080(4) 0.088(4) 0.069(3) 0.011(3) -0.017(3) -0.029(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 La1 O1 2.400(4) . ? La1 O2 2.410(4) . ? La1 O5 2.609(5) . ? La1 O8 2.615(5) . ? La1 O6 2.617(5) . ? La1 N3 2.631(5) . ? La1 O3 2.636(5) . ? La1 N1 2.665(5) . ? La1 N2 2.694(4) . ? La1 N4 3.053(7) . ? La1 N5 3.068(7) . ? O1 C31 1.279(6) . ? O9 C24 1.369(7) . ? O3 N4 1.265(7) . ? O2 C33 1.292(6) . ? O11 C39 1.368(7) . ? O12 C41 1.367(7) . ? O12 C42 1.409(8) . ? O5 N4 1.255(7) . ? N2 C16 1.338(7) . ? N2 C6 1.354(7) . ? O6 N5 1.269(7) . ? C14 C7 1.372(8) . ? C14 C15 1.391(7) . ? C14 C13 1.491(7) . ? C17 N3 1.357(7) . ? C17 C18 1.391(7) . ? C17 C16 1.491(7) . ? N3 C21 1.340(7) . ? N1 C1 1.326(7) . ? N1 C5 1.350(7) . ? O10 C23 1.360(7) . ? O10 C22 1.419(7) . ? O8 N5 1.271(7) . ? C5 C4 1.391(7) . ? C5 C6 1.479(8) . ? C13 C12 1.377(8) . ? C13 C8 1.392(8) . ? C16 C15 1.386(7) . ? C36 C37 1.382(8) . ? C36 C40 1.387(8) . ? C36 C35 1.461(8) . ? C39 C38 1.372(8) . ? C39 C41 1.381(8) . ? C6 C7 1.401(7) . ? C34 C35 1.314(8) . ? C34 C33 1.447(8) . ? C31 C32 1.393(8) . ? C31 C30 1.473(8) . ? O4 N4 1.223(7) . ? C30 C29 1.315(8) . ? C21 C20 1.363(8) . ? C28 C27 1.374(7) . ? C28 C26 1.381(8) . ? C28 C29 1.457(8) . ? O7 N5 1.206(7) . ? C3 C4 1.363(8) . ? C3 C2 1.373(8) . ? C27 C23 1.364(8) . ? C41 C40 1.361(8) . ? C8 C9 1.394(9) . ? C33 C32 1.373(7) . ? C1 C2 1.375(8) . ? C37 C38 1.368(9) . ? C18 C19 1.375(8) . ? C24 C25 1.374(8) . ? C24 C23 1.382(8) . ? C12 C11 1.384(8) . ? C20 C19 1.356(8) . ? C26 C25 1.368(8) . ? C11 C10 1.377(9) . ? C9 C10 1.352(10) . ? 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 La1 O2 72.55(13) . . ? O1 La1 O5 96.66(16) . . ? O2 La1 O5 75.44(16) . . ? O1 La1 O8 120.01(15) . . ? O2 La1 O8 97.00(15) . . ? O5 La1 O8 138.82(15) . . ? O1 La1 O6 71.86(15) . . ? O2 La1 O6 86.78(15) . . ? O5 La1 O6 161.23(15) . . ? O8 La1 O6 48.33(14) . . ? O1 La1 N3 82.49(14) . . ? O2 La1 N3 154.10(14) . . ? O5 La1 N3 115.14(16) . . ? O8 La1 N3 89.40(16) . . ? O6 La1 N3 78.82(15) . . ? O1 La1 O3 80.12(14) . . ? O2 La1 O3 112.82(16) . . ? O5 La1 O3 48.20(14) . . ? O8 La1 O3 148.55(15) . . ? O6 La1 O3 139.07(15) . . ? N3 La1 O3 68.27(16) . . ? O1 La1 N1 155.30(15) . . ? O2 La1 N1 84.19(14) . . ? O5 La1 N1 68.85(16) . . ? O8 La1 N1 70.14(16) . . ? O6 La1 N1 115.88(16) . . ? N3 La1 N1 121.45(14) . . ? O3 La1 N1 102.09(15) . . ? O1 La1 N2 141.23(13) . . ? O2 La1 N2 144.85(13) . . ? O5 La1 N2 88.13(15) . . ? O8 La1 N2 75.12(14) . . ? O6 La1 N2 110.19(15) . . ? N3 La1 N2 61.04(13) . . ? O3 La1 N2 74.70(14) . . ? N1 La1 N2 60.80(14) . . ? O1 La1 N4 89.85(15) . . ? O2 La1 N4 95.20(16) . . ? O5 La1 N4 24.00(14) . . ? O8 La1 N4 149.95(14) . . ? O6 La1 N4 160.15(15) . . ? N3 La1 N4 91.48(17) . . ? O3 La1 N4 24.30(13) . . ? N1 La1 N4 83.96(16) . . ? N2 La1 N4 79.11(14) . . ? O1 La1 N5 95.97(17) . . ? O2 La1 N5 92.81(16) . . ? O5 La1 N5 159.24(15) . . ? O8 La1 N5 24.20(14) . . ? O6 La1 N5 24.15(14) . . ? N3 La1 N5 82.82(16) . . ? O3 La1 N5 151.08(15) . . ? N1 La1 N5 93.31(17) . . ? N2 La1 N5 92.27(16) . . ? N4 La1 N5 171.23(15) . . ? C31 O1 La1 133.1(4) . . ? N4 O3 La1 96.7(4) . . ? C33 O2 La1 133.3(3) . . ? C41 O12 C42 118.3(5) . . ? N4 O5 La1 98.3(4) . . ? C16 N2 C6 117.3(5) . . ? C16 N2 La1 121.5(3) . . ? C6 N2 La1 121.2(4) . . ? N5 O6 La1 98.3(4) . . ? C7 C14 C15 116.3(5) . . ? C7 C14 C13 122.3(5) . . ? C15 C14 C13 121.2(5) . . ? N3 C17 C18 120.7(5) . . ? N3 C17 C16 116.3(5) . . ? C18 C17 C16 122.9(5) . . ? C21 N3 C17 117.1(5) . . ? C21 N3 La1 118.8(4) . . ? C17 N3 La1 123.1(3) . . ? C1 N1 C5 118.4(5) . . ? C1 N1 La1 118.0(4) . . ? C5 N1 La1 123.6(4) . . ? C23 O10 C22 118.5(5) . . ? N5 O8 La1 98.3(4) . . ? N1 C5 C4 120.4(5) . . ? N1 C5 C6 116.1(5) . . ? C4 C5 C6 123.4(5) . . ? C12 C13 C8 118.5(6) . . ? C12 C13 C14 121.4(5) . . ? C8 C13 C14 120.1(6) . . ? N2 C16 C15 123.8(5) . . ? N2 C16 C17 117.1(5) . . ? C15 C16 C17 119.0(5) . . ? C37 C36 C40 117.8(5) . . ? C37 C36 C35 119.9(5) . . ? C40 C36 C35 122.2(5) . . ? O11 C39 C38 118.8(5) . . ? O11 C39 C41 122.4(6) . . ? C38 C39 C41 118.8(6) . . ? N2 C6 C7 120.9(5) . . ? N2 C6 C5 118.1(5) . . ? C7 C6 C5 120.9(5) . . ? C35 C34 C33 127.4(6) . . ? O1 C31 C32 124.9(5) . . ? O1 C31 C30 118.1(5) . . ? C32 C31 C30 117.0(5) . . ? C29 C30 C31 124.4(6) . . ? N3 C21 C20 124.7(6) . . ? C27 C28 C26 117.0(5) . . ? C27 C28 C29 121.5(5) . . ? C26 C28 C29 121.4(5) . . ? C14 C7 C6 121.9(5) . . ? C4 C3 C2 120.6(6) . . ? C34 C35 C36 130.3(6) . . ? C23 C27 C28 121.7(5) . . ? C40 C41 O12 125.0(5) . . ? C40 C41 C39 121.2(5) . . ? O12 C41 C39 113.8(5) . . ? C30 C29 C28 129.9(6) . . ? C13 C8 C9 120.0(7) . . ? O2 C33 C32 125.2(5) . . ? O2 C33 C34 116.3(5) . . ? C32 C33 C34 118.4(5) . . ? N1 C1 C2 124.4(6) . . ? C41 C40 C36 120.5(5) . . ? O4 N4 O5 121.3(6) . . ? O4 N4 O3 122.4(6) . . ? O5 N4 O3 116.4(6) . . ? O4 N4 La1 172.9(4) . . ? O5 N4 La1 57.7(4) . . ? O3 N4 La1 59.0(3) . . ? C38 C37 C36 121.5(6) . . ? C19 C18 C17 119.6(5) . . ? C37 C38 C39 120.1(6) . . ? O9 C24 C25 119.1(6) . . ? O9 C24 C23 120.7(6) . . ? C25 C24 C23 120.2(6) . . ? C3 C4 C5 119.4(6) . . ? C13 C12 C11 121.0(6) . . ? C19 C20 C21 118.0(6) . . ? C25 C26 C28 122.9(6) . . ? C3 C2 C1 116.7(6) . . ? O7 N5 O6 122.1(7) . . ? O7 N5 O8 122.9(7) . . ? O6 N5 O8 115.0(6) . . ? O7 N5 La1 177.1(5) . . ? O6 N5 La1 57.6(4) . . ? O8 N5 La1 57.5(4) . . ? C20 C19 C18 119.7(6) . . ? C16 C15 C14 119.6(5) . . ? C10 C11 C12 119.5(7) . . ? C33 C32 C31 126.5(5) . . ? C26 C25 C24 118.4(6) . . ? O10 C23 C27 126.7(6) . . ? O10 C23 C24 113.5(5) . . ? C27 C23 C24 119.7(6) . . ? C10 C9 C8 120.3(7) . . ? C9 C10 C11 120.6(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.595 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.112 data_ARCakhdt_2 _database_code_depnum_ccdc_archive 'CCDC 900324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Gd N5 O13' _chemical_formula_sum 'C42 H36 Gd N5 O13' _chemical_formula_weight 976.01 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 10.7275(6) _cell_length_b 12.4582(8) _cell_length_c 15.0207(9) _cell_angle_alpha 86.869(4) _cell_angle_beta 89.236(4) _cell_angle_gamma 80.443(4) _cell_volume 1976.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Hexagonal _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 1.753 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6213 _exptl_absorpt_correction_T_max 0.8442 _exptl_absorpt_process_details ? _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 Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34953 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8503 _reflns_number_gt 4380 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0475P)^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 8503 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 0.78397(3) 0.31651(3) 0.71566(2) 0.04693(14) Uani 1 1 d . . . C34 C 0.6333(6) 0.0227(6) 0.8607(4) 0.0509(18) Uani 1 1 d . . . O2 O 0.7291(4) 0.1710(4) 0.8011(3) 0.0636(13) Uani 1 1 d . . . O1 O 0.6720(4) 0.2303(4) 0.6196(3) 0.0605(13) Uani 1 1 d . . . N2 N 0.9253(4) 0.4645(4) 0.7147(3) 0.0450(13) Uani 1 1 d . . . O11 O 0.6766(4) -0.2965(4) 1.2227(3) 0.0760(15) Uani 1 1 d . . . H39 H 0.6272 -0.3376 1.2116 0.114 Uiso 1 1 calc R . . N3 N 0.7525(5) 0.4601(4) 0.5873(3) 0.0511(14) Uani 1 1 d . . . O6 O 0.5532(5) 0.3955(5) 0.7306(3) 0.0723(14) Uani 1 1 d . . . O9 O 0.1691(5) 0.2115(4) 0.1964(3) 0.0756(15) Uani 1 1 d . . . H24 H 0.1179 0.1709 0.2089 0.113 Uiso 1 1 calc R . . O3 O 0.9429(4) 0.2720(4) 0.5925(3) 0.0666(14) Uani 1 1 d . . . O5 O 0.9753(5) 0.1726(4) 0.7120(3) 0.0796(15) Uani 1 1 d . . . O8 O 0.6780(5) 0.4561(4) 0.8166(3) 0.0730(14) Uani 1 1 d . . . C16 C 0.9219(5) 0.5394(5) 0.6457(4) 0.0442(16) Uani 1 1 d . . . O4 O 1.1165(6) 0.1557(5) 0.6081(4) 0.0912(18) Uani 1 1 d . . . N1 N 0.9202(5) 0.3206(4) 0.8549(3) 0.0572(15) Uani 1 1 d . . . O12 O 0.5393(5) -0.3088(5) 1.0781(3) 0.0952(19) Uani 1 1 d . . . O7 O 0.4775(6) 0.5239(5) 0.8167(4) 0.0951(19) Uani 1 1 d . . . C36 C 0.6906(6) -0.0714(5) 1.0098(4) 0.0513(17) Uani 1 1 d . . . C17 C 0.8317(5) 0.5335(5) 0.5732(4) 0.0433(16) Uani 1 1 d . . . C18 C 0.8293(6) 0.5960(6) 0.4954(4) 0.0533(18) Uani 1 1 d . . . O10 O 0.1403(5) 0.0899(5) 0.3402(3) 0.0909(18) Uani 1 1 d . . . C40 C 0.6150(7) -0.1518(6) 1.0040(5) 0.0563(19) Uani 1 1 d . . . C6 C 1.0055(6) 0.4701(5) 0.7815(4) 0.0462(16) Uani 1 1 d . . . C35 C 0.6992(7) 0.0078(6) 0.9357(4) 0.0516(18) Uani 1 1 d . . . C5 C 1.0014(6) 0.3917(5) 0.8595(4) 0.0477(16) Uani 1 1 d . . . C42 C 0.4635(11) -0.3189(9) 1.0021(6) 0.147(5) Uani 1 1 d . . . H42A H 0.4200 -0.3799 1.0125 0.220 Uiso 1 1 calc R . . H42B H 0.5168 -0.3301 0.9504 0.220 Uiso 1 1 calc R . . H42C H 0.4029 -0.2536 0.9923 0.220 Uiso 1 1 calc R . . C30 C 0.5008(6) 0.1585(6) 0.5623(4) 0.056(2) Uani 1 1 d . . . C33 C 0.6493(6) 0.1061(5) 0.7898(4) 0.0483(17) Uani 1 1 d . . . N4 N 1.0146(7) 0.1997(6) 0.6358(4) 0.0638(17) Uani 1 1 d . . . N5 N 0.5667(7) 0.4617(6) 0.7896(5) 0.0662(17) Uani 1 1 d . . . C14 C 1.0822(6) 0.6238(5) 0.7112(4) 0.0487(17) Uani 1 1 d . . . C331 C 0.5890(6) 0.1684(5) 0.6339(4) 0.0499(17) Uani 1 1 d . . . C27 C 0.3180(6) 0.1444(6) 0.4127(4) 0.0557(19) Uani 1 1 d . . . C19 C 0.7441(7) 0.5867(6) 0.4289(5) 0.060(2) Uani 1 1 d . . . C39 C 0.6793(6) -0.2214(6) 1.1524(4) 0.0550(19) Uani 1 1 d . . . C28 C 0.4127(6) 0.2101(5) 0.4093(4) 0.0513(17) Uani 1 1 d . . . C38 C 0.7546(7) -0.1445(6) 1.1582(5) 0.063(2) Uani 1 1 d . . . C13 C 1.1597(6) 0.7133(5) 0.7106(4) 0.0486(17) Uani 1 1 d . . . C29 C 0.4992(6) 0.2093(6) 0.4831(4) 0.0557(18) Uani 1 1 d . . . C7 C 1.0857(6) 0.5466(5) 0.7809(4) 0.0525(18) Uani 1 1 d . . . C24 C 0.2492(7) 0.2109(5) 0.2669(4) 0.0548(18) Uani 1 1 d . . . C37 C 0.7607(7) -0.0696(6) 1.0865(5) 0.061(2) Uani 1 1 d . . . C21 C 0.6700(7) 0.4541(6) 0.5230(5) 0.065(2) Uani 1 1 d . . . C41 C 0.6090(6) -0.2263(6) 1.0757(4) 0.0570(19) Uani 1 1 d . . . C32 C 0.5782(6) 0.1082(5) 0.7132(4) 0.0523(18) Uani 1 1 d . . . H32 H 0.5161 0.0642 0.7152 0.063 Uiso 1 1 calc R . . C15 C 0.9969(6) 0.6191(6) 0.6431(4) 0.0515(18) Uani 1 1 d . . . C4 C 1.0751(7) 0.3924(6) 0.9356(4) 0.064(2) Uani 1 1 d . . . C20 C 0.6636(7) 0.5135(6) 0.4432(5) 0.062(2) Uani 1 1 d . . . C3 C 1.0666(8) 0.3187(7) 1.0046(5) 0.068(2) Uani 1 1 d . . . C1 C 0.9138(8) 0.2498(6) 0.9241(5) 0.072(2) Uani 1 1 d . . . C26 C 0.4224(7) 0.2713(6) 0.3320(4) 0.062(2) Uani 1 1 d . . . C8 C 1.2213(7) 0.7340(7) 0.7878(6) 0.075(2) Uani 1 1 d . . . C25 C 0.3416(7) 0.2721(6) 0.2613(5) 0.065(2) Uani 1 1 d . . . C11 C 1.2320(8) 0.8710(7) 0.6389(6) 0.079(2) Uani 1 1 d . . . C22 C 0.1148(8) 0.0230(7) 0.4174(5) 0.092(3) Uani 1 1 d . . . H22A H 0.0438 -0.0119 0.4057 0.137 Uiso 1 1 calc R . . H22B H 0.0960 0.0677 0.4675 0.137 Uiso 1 1 calc R . . H22C H 0.1876 -0.0314 0.4305 0.137 Uiso 1 1 calc R . . C23 C 0.2368(6) 0.1462(5) 0.3437(4) 0.0540(18) Uani 1 1 d . . . C10 C 1.2910(9) 0.8884(8) 0.7148(7) 0.081(3) Uani 1 1 d . . . C12 C 1.1683(7) 0.7810(7) 0.6365(5) 0.075(2) Uani 1 1 d . . . C2 C 0.9845(8) 0.2456(7) 1.0002(5) 0.075(2) Uani 1 1 d . . . C9 C 1.2865(9) 0.8207(8) 0.7888(6) 0.092(3) Uani 1 1 d . . . OW1 O 0.0202(5) 0.0409(5) 0.1756(4) 0.1010(19) Uani 1 1 d . . . H18 H 0.900(8) 0.663(7) 0.479(5) 0.13(3) Uiso 1 1 d . . . H40 H 0.573(6) -0.152(6) 0.950(5) 0.08(2) Uiso 1 1 d . . . H27 H 0.319(5) 0.109(4) 0.472(4) 0.046(16) Uiso 1 1 d . . . H19 H 0.736(5) 0.621(4) 0.377(4) 0.037(17) Uiso 1 1 d . . . H38 H 0.806(6) -0.129(5) 1.211(4) 0.08(2) Uiso 1 1 d . . . H7 H 1.139(5) 0.551(5) 0.838(4) 0.063(18) Uiso 1 1 d . . . H37 H 0.815(5) -0.011(5) 1.091(4) 0.062(19) Uiso 1 1 d . . . H21 H 0.629(6) 0.400(5) 0.535(4) 0.06(2) Uiso 1 1 d . . . H14 H 0.994(4) 0.681(4) 0.595(3) 0.032(14) Uiso 1 1 d . . . H4 H 1.141(6) 0.452(5) 0.941(4) 0.08(2) Uiso 1 1 d . . . H20 H 0.606(7) 0.500(6) 0.401(5) 0.09(2) Uiso 1 1 d . . . H3 H 1.111(5) 0.325(4) 1.054(3) 0.034(15) Uiso 1 1 d . . . H1 H 0.841(8) 0.197(7) 0.909(5) 0.12(3) Uiso 1 1 d . . . H26 H 0.491(6) 0.322(5) 0.333(4) 0.068(19) Uiso 1 1 d . . . H8 H 1.211(7) 0.683(7) 0.835(5) 0.11(3) Uiso 1 1 d . . . H25 H 0.339(6) 0.317(6) 0.206(4) 0.08(2) Uiso 1 1 d . . . H11 H 1.254(6) 0.918(5) 0.581(4) 0.08(2) Uiso 1 1 d . . . H10 H 1.330(7) 0.942(6) 0.709(5) 0.09(3) Uiso 1 1 d . . . H12 H 1.138(5) 0.758(5) 0.579(4) 0.06(2) Uiso 1 1 d . . . H2 H 0.980(5) 0.193(5) 1.049(4) 0.050(17) Uiso 1 1 d . . . H9 H 1.345(7) 0.833(6) 0.847(5) 0.11(3) Uiso 1 1 d . . . H30 H 0.438(5) 0.121(4) 0.575(3) 0.041(16) Uiso 1 1 d . . . H35 H 0.750(7) 0.065(6) 0.949(4) 0.09(3) Uiso 1 1 d . . . H29 H 0.565(6) 0.273(5) 0.476(4) 0.08(2) Uiso 1 1 d . . . H34 H 0.565(6) -0.014(5) 0.848(4) 0.07(2) Uiso 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 Gd1 0.0561(2) 0.0474(2) 0.04094(19) 0.01440(14) -0.01046(14) -0.02395(16) C34 0.047(4) 0.060(5) 0.047(4) 0.009(4) -0.005(3) -0.015(4) O2 0.082(3) 0.072(3) 0.046(3) 0.020(2) -0.017(2) -0.045(3) O1 0.071(3) 0.070(3) 0.048(3) 0.015(2) -0.010(2) -0.038(3) N2 0.047(3) 0.048(3) 0.041(3) 0.013(3) -0.015(2) -0.016(3) O11 0.086(4) 0.088(4) 0.055(3) 0.030(3) -0.020(3) -0.026(3) N3 0.052(3) 0.054(4) 0.050(3) 0.019(3) -0.014(3) -0.021(3) O6 0.075(4) 0.082(4) 0.062(3) 0.003(3) -0.006(3) -0.022(3) O9 0.090(4) 0.088(4) 0.047(3) 0.006(3) -0.024(3) -0.010(3) O3 0.071(3) 0.068(4) 0.058(3) 0.020(3) -0.003(3) -0.011(3) O5 0.086(4) 0.087(4) 0.060(3) 0.020(3) -0.001(3) -0.005(3) O8 0.069(4) 0.078(4) 0.077(3) -0.001(3) -0.010(3) -0.025(3) C16 0.046(4) 0.047(4) 0.041(4) 0.008(3) -0.007(3) -0.012(3) O4 0.076(4) 0.095(5) 0.098(4) -0.008(3) 0.013(3) 0.000(4) N1 0.075(4) 0.050(4) 0.048(3) 0.015(3) -0.019(3) -0.023(3) O12 0.126(5) 0.099(4) 0.073(4) 0.033(3) -0.026(3) -0.064(4) O7 0.090(4) 0.073(4) 0.118(5) -0.003(4) 0.022(4) -0.003(4) C36 0.056(4) 0.051(5) 0.046(4) 0.008(3) -0.007(3) -0.009(4) C17 0.042(4) 0.046(4) 0.042(4) 0.010(3) -0.007(3) -0.011(3) C18 0.062(5) 0.054(5) 0.045(4) 0.012(4) 0.000(4) -0.017(4) O10 0.095(4) 0.115(5) 0.073(4) 0.016(3) -0.020(3) -0.054(4) C40 0.065(5) 0.057(5) 0.051(4) 0.017(4) -0.007(4) -0.026(4) C6 0.058(4) 0.043(4) 0.039(4) 0.006(3) -0.009(3) -0.013(3) C35 0.061(5) 0.047(5) 0.048(4) 0.007(3) -0.002(4) -0.013(4) C5 0.057(4) 0.045(4) 0.040(4) 0.008(3) -0.012(3) -0.008(3) C42 0.220(12) 0.181(11) 0.075(6) 0.033(7) -0.059(7) -0.142(10) C30 0.054(5) 0.067(5) 0.053(4) 0.016(4) -0.014(4) -0.035(4) C33 0.060(4) 0.042(4) 0.043(4) 0.017(3) 0.002(3) -0.014(4) N4 0.065(5) 0.067(5) 0.065(5) 0.001(4) -0.006(4) -0.027(4) N5 0.073(5) 0.056(5) 0.068(5) 0.016(4) 0.006(4) -0.013(4) C14 0.047(4) 0.048(4) 0.052(4) 0.004(3) -0.010(3) -0.012(3) C331 0.052(4) 0.047(4) 0.051(4) 0.005(3) 0.000(3) -0.013(3) C27 0.071(5) 0.065(5) 0.035(4) 0.007(4) -0.014(4) -0.021(4) C19 0.071(5) 0.071(6) 0.036(4) 0.011(4) -0.011(4) -0.007(4) C39 0.055(4) 0.065(5) 0.046(4) 0.025(4) -0.006(3) -0.020(4) C28 0.056(4) 0.057(5) 0.044(4) 0.005(3) -0.005(3) -0.021(4) C38 0.072(5) 0.078(6) 0.041(4) 0.012(4) -0.016(4) -0.021(4) C13 0.051(4) 0.044(4) 0.055(4) 0.001(3) -0.004(3) -0.020(3) C29 0.065(5) 0.050(5) 0.056(5) 0.001(4) -0.009(4) -0.022(4) C7 0.065(5) 0.052(5) 0.045(4) 0.004(3) -0.015(3) -0.023(4) C24 0.072(5) 0.051(5) 0.039(4) 0.012(3) -0.017(3) -0.008(4) C37 0.063(5) 0.065(5) 0.056(5) 0.007(4) -0.014(4) -0.019(4) C21 0.068(5) 0.063(5) 0.069(5) 0.029(4) -0.030(4) -0.034(4) C41 0.063(5) 0.060(5) 0.052(4) 0.011(4) -0.006(4) -0.025(4) C32 0.057(4) 0.059(5) 0.046(4) 0.014(3) -0.011(3) -0.029(4) C15 0.054(4) 0.053(5) 0.049(4) 0.017(4) -0.004(3) -0.018(4) C4 0.089(6) 0.057(5) 0.048(4) 0.010(4) -0.025(4) -0.024(4) C20 0.064(5) 0.062(5) 0.061(5) 0.012(4) -0.028(4) -0.018(4) C3 0.093(6) 0.067(6) 0.041(4) 0.007(4) -0.028(4) -0.008(5) C1 0.092(6) 0.072(6) 0.055(5) 0.028(4) -0.025(4) -0.028(5) C26 0.079(5) 0.063(5) 0.051(4) 0.013(4) -0.011(4) -0.028(4) C8 0.078(6) 0.082(6) 0.074(6) 0.011(5) -0.017(4) -0.044(5) C25 0.088(6) 0.058(5) 0.051(5) 0.016(4) -0.013(4) -0.020(4) C11 0.084(6) 0.067(6) 0.091(6) 0.013(5) -0.008(5) -0.038(5) C22 0.106(7) 0.099(7) 0.081(6) 0.006(5) -0.001(5) -0.053(6) C23 0.062(5) 0.058(5) 0.044(4) 0.007(3) -0.004(4) -0.020(4) C10 0.084(6) 0.063(6) 0.103(8) -0.001(5) -0.004(5) -0.034(5) C12 0.089(6) 0.080(6) 0.067(5) 0.009(5) -0.014(4) -0.047(5) C2 0.098(6) 0.072(6) 0.055(5) 0.028(4) -0.012(5) -0.024(5) C9 0.106(7) 0.093(7) 0.093(7) 0.001(6) -0.018(6) -0.060(6) OW1 0.101(4) 0.110(5) 0.100(4) 0.020(4) -0.028(3) -0.046(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.307(4) . ? Gd1 O2 2.315(4) . ? Gd1 O8 2.491(5) . ? Gd1 O5 2.493(5) . ? Gd1 O6 2.519(5) . ? Gd1 O3 2.520(5) . ? Gd1 N3 2.544(5) . ? Gd1 N2 2.574(5) . ? Gd1 N1 2.575(5) . ? Gd1 N4 2.931(8) . ? Gd1 N5 2.948(8) . ? C34 C35 1.325(9) . ? C34 C33 1.476(8) . ? O2 C33 1.289(7) . ? O1 C331 1.280(7) . ? N2 C6 1.342(7) . ? N2 C16 1.353(7) . ? O11 C39 1.375(7) . ? N3 C21 1.332(8) . ? N3 C17 1.355(7) . ? O6 N5 1.268(7) . ? O9 C24 1.373(7) . ? O3 N4 1.243(7) . ? O5 N4 1.263(7) . ? O8 N5 1.257(7) . ? C16 C15 1.376(8) . ? C16 C17 1.480(8) . ? O4 N4 1.218(7) . ? N1 C1 1.334(8) . ? N1 C5 1.347(7) . ? O12 C41 1.367(7) . ? O12 C42 1.434(9) . ? O7 N5 1.208(8) . ? C36 C37 1.388(9) . ? C36 C40 1.396(9) . ? C36 C35 1.460(8) . ? C17 C18 1.367(8) . ? C18 C19 1.385(9) . ? O10 C23 1.346(7) . ? O10 C22 1.441(8) . ? C40 C41 1.391(9) . ? C6 C7 1.385(8) . ? C6 C5 1.489(8) . ? C5 C4 1.400(8) . ? C30 C29 1.316(8) . ? C30 C331 1.465(8) . ? C33 C32 1.385(8) . ? C14 C7 1.379(8) . ? C14 C15 1.392(8) . ? C14 C13 1.498(8) . ? C331 C32 1.387(8) . ? C27 C23 1.360(8) . ? C27 C28 1.405(8) . ? C19 C20 1.363(9) . ? C39 C38 1.359(9) . ? C39 C41 1.395(8) . ? C28 C26 1.366(8) . ? C28 C29 1.454(8) . ? C38 C37 1.393(9) . ? C13 C12 1.371(9) . ? C13 C8 1.399(9) . ? C24 C25 1.346(9) . ? C24 C23 1.389(8) . ? C21 C20 1.370(9) . ? C4 C3 1.359(9) . ? C3 C2 1.373(10) . ? C1 C2 1.373(10) . ? C26 C25 1.379(9) . ? C8 C9 1.382(10) . ? C11 C10 1.358(11) . ? C11 C12 1.409(10) . ? C10 C9 1.363(11) . ? 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 Gd1 O2 75.59(14) . . ? O1 Gd1 O8 122.23(17) . . ? O2 Gd1 O8 94.23(16) . . ? O1 Gd1 O5 93.62(17) . . ? O2 Gd1 O5 75.51(17) . . ? O8 Gd1 O5 139.39(17) . . ? O1 Gd1 O6 72.05(18) . . ? O2 Gd1 O6 83.97(16) . . ? O8 Gd1 O6 50.23(17) . . ? O5 Gd1 O6 157.49(17) . . ? O1 Gd1 O3 78.36(15) . . ? O2 Gd1 O3 116.94(16) . . ? O8 Gd1 O3 147.11(16) . . ? O5 Gd1 O3 50.12(15) . . ? O6 Gd1 O3 137.95(16) . . ? O1 Gd1 N3 80.40(15) . . ? O2 Gd1 N3 153.39(15) . . ? O8 Gd1 N3 88.90(17) . . ? O5 Gd1 N3 117.75(17) . . ? O6 Gd1 N3 77.80(16) . . ? O3 Gd1 N3 68.21(17) . . ? O1 Gd1 N2 140.68(14) . . ? O2 Gd1 N2 142.60(14) . . ? O8 Gd1 N2 74.30(16) . . ? O5 Gd1 N2 90.18(17) . . ? O6 Gd1 N2 111.97(17) . . ? O3 Gd1 N2 74.37(16) . . ? N3 Gd1 N2 63.46(15) . . ? O1 Gd1 N1 152.86(16) . . ? O2 Gd1 N1 79.44(15) . . ? O8 Gd1 N1 69.79(18) . . ? O5 Gd1 N1 69.71(17) . . ? O6 Gd1 N1 115.86(18) . . ? O3 Gd1 N1 104.15(17) . . ? N3 Gd1 N1 126.02(16) . . ? N2 Gd1 N1 63.16(15) . . ? O1 Gd1 N4 87.22(16) . . ? O2 Gd1 N4 97.56(18) . . ? O8 Gd1 N4 150.26(16) . . ? O5 Gd1 N4 25.31(15) . . ? O6 Gd1 N4 158.23(17) . . ? O3 Gd1 N4 24.92(14) . . ? N3 Gd1 N4 92.53(18) . . ? N2 Gd1 N4 79.82(16) . . ? N1 Gd1 N4 85.64(17) . . ? O1 Gd1 N5 97.35(19) . . ? O2 Gd1 N5 89.91(17) . . ? O8 Gd1 N5 24.95(16) . . ? O5 Gd1 N5 158.98(17) . . ? O6 Gd1 N5 25.30(15) . . ? O3 Gd1 N5 150.07(16) . . ? N3 Gd1 N5 81.87(16) . . ? N2 Gd1 N5 92.57(18) . . ? N1 Gd1 N5 93.06(19) . . ? N4 Gd1 N5 172.04(17) . . ? C35 C34 C33 123.7(6) . . ? C33 O2 Gd1 133.0(3) . . ? C331 O1 Gd1 131.7(4) . . ? C6 N2 C16 117.5(5) . . ? C6 N2 Gd1 121.8(4) . . ? C16 N2 Gd1 120.7(4) . . ? C21 N3 C17 116.9(5) . . ? C21 N3 Gd1 120.3(4) . . ? C17 N3 Gd1 121.9(4) . . ? N5 O6 Gd1 96.6(4) . . ? N4 O3 Gd1 96.4(4) . . ? N4 O5 Gd1 97.2(5) . . ? N5 O8 Gd1 98.3(5) . . ? N2 C16 C15 122.0(5) . . ? N2 C16 C17 117.0(5) . . ? C15 C16 C17 121.0(5) . . ? C1 N1 C5 118.2(6) . . ? C1 N1 Gd1 120.3(5) . . ? C5 N1 Gd1 121.5(4) . . ? C41 O12 C42 118.2(6) . . ? C37 C36 C40 118.9(6) . . ? C37 C36 C35 120.2(6) . . ? C40 C36 C35 120.9(6) . . ? N3 C17 C18 121.3(5) . . ? N3 C17 C16 116.0(5) . . ? C18 C17 C16 122.6(5) . . ? C17 C18 C19 120.5(6) . . ? C23 O10 C22 118.5(5) . . ? C41 C40 C36 119.6(6) . . ? N2 C6 C7 122.8(5) . . ? N2 C6 C5 116.5(5) . . ? C7 C6 C5 120.6(5) . . ? C34 C35 C36 128.2(7) . . ? N1 C5 C4 120.6(6) . . ? N1 C5 C6 116.8(5) . . ? C4 C5 C6 122.5(6) . . ? C29 C30 C331 124.9(6) . . ? O2 C33 C32 123.7(5) . . ? O2 C33 C34 119.2(6) . . ? C32 C33 C34 117.1(6) . . ? O4 N4 O3 123.6(7) . . ? O4 N4 O5 120.5(7) . . ? O3 N4 O5 115.8(7) . . ? O4 N4 Gd1 174.0(5) . . ? O3 N4 Gd1 58.7(4) . . ? O5 N4 Gd1 57.5(4) . . ? O7 N5 O8 124.0(8) . . ? O7 N5 O6 121.2(7) . . ? O8 N5 O6 114.7(7) . . ? O7 N5 Gd1 177.3(5) . . ? O8 N5 Gd1 56.7(4) . . ? O6 N5 Gd1 58.1(4) . . ? C7 C14 C15 116.9(6) . . ? C7 C14 C13 122.2(6) . . ? C15 C14 C13 120.8(6) . . ? O1 C331 C32 123.9(6) . . ? O1 C331 C30 118.7(5) . . ? C32 C331 C30 117.4(6) . . ? C23 C27 C28 121.2(6) . . ? C20 C19 C18 118.3(7) . . ? C38 C39 O11 118.7(6) . . ? C38 C39 C41 120.8(6) . . ? O11 C39 C41 120.5(6) . . ? C26 C28 C27 116.7(6) . . ? C26 C28 C29 121.8(6) . . ? C27 C28 C29 121.5(6) . . ? C39 C38 C37 119.3(6) . . ? C12 C13 C8 117.5(6) . . ? C12 C13 C14 121.7(6) . . ? C8 C13 C14 120.7(6) . . ? C30 C29 C28 129.6(6) . . ? C14 C7 C6 120.0(6) . . ? C25 C24 O9 119.9(6) . . ? C25 C24 C23 119.8(6) . . ? O9 C24 C23 120.3(6) . . ? C36 C37 C38 121.4(7) . . ? N3 C21 C20 124.6(7) . . ? O12 C41 C40 125.2(6) . . ? O12 C41 C39 114.7(6) . . ? C40 C41 C39 120.1(6) . . ? C33 C32 C331 127.5(6) . . ? C16 C15 C14 120.7(6) . . ? C3 C4 C5 119.5(7) . . ? C19 C20 C21 118.3(7) . . ? C4 C3 C2 120.0(7) . . ? N1 C1 C2 123.9(7) . . ? C28 C26 C25 122.4(7) . . ? C9 C8 C13 120.7(8) . . ? C24 C25 C26 120.0(7) . . ? C10 C11 C12 119.5(8) . . ? O10 C23 C27 126.7(6) . . ? O10 C23 C24 113.3(6) . . ? C27 C23 C24 120.0(6) . . ? C11 C10 C9 120.3(8) . . ? C13 C12 C11 121.4(7) . . ? C3 C2 C1 117.7(7) . . ? C10 C9 C8 120.6(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.750 _refine_diff_density_min -1.473 _refine_diff_density_rms 0.116