# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1281 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the three crystal structures in the paper 'Lanthanide complexes of a new sterically hindered potentially hexadentate podand ligand based on a tris(pyrazolyl)borate core....' (revised version) by Z. R. Reeves, K. L. V. Mann, J. C. Jeffery, J. A. McCleverty, M. D. Ward, F. Barigelletti and N. Armaroli submitted for publication to Dalton Transactions. ; #================================================================= data_bell _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H27 B Eu N11 O7' _chemical_formula_weight 780.37 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Eu' 'Eu' -0.1578 3.6682 '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 10.876(3) _cell_length_b 16.507(5) _cell_length_c 19.011(6) _cell_angle_alpha 70.302(5) _cell_angle_beta 82.212(5) _cell_angle_gamma 73.769(7) _cell_volume 3082.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method ? _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 2.099 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.60 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27838 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.45 _reflns_number_total 13136 _reflns_number_observed 8547 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0275P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13136 _refine_ls_number_parameters 865 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_obs 0.0453 _refine_ls_wR_factor_all 0.0856 _refine_ls_wR_factor_obs 0.0724 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_goodness_of_fit_obs 1.047 _refine_ls_restrained_S_all 0.982 _refine_ls_restrained_S_obs 1.048 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Eu1 Eu 0.04983(3) 0.24371(2) 0.03978(2) 0.01957(8) Uani 1 d . . O1 O 0.0436(4) 0.3887(2) 0.0435(2) 0.0265(9) Uani 1 d D . H1B H 0.0697(50) 0.4242(31) -0.0010(20) 0.050 Uiso 1 d D . H1A H -0.0242(38) 0.4267(31) 0.0553(29) 0.050 Uiso 1 d D . O111 O 0.0657(5) 0.0210(3) 0.2266(2) 0.0513(13) Uani 1 d . . O112 O -0.0315(3) 0.1155(2) 0.1269(2) 0.0260(9) Uani 1 d . . O113 O 0.1379(3) 0.1352(2) 0.1607(2) 0.0248(9) Uani 1 d . . O121 O 0.4154(4) 0.2533(3) -0.0542(2) 0.0361(10) Uani 1 d . . O122 O 0.2179(4) 0.2542(2) -0.0640(2) 0.0276(9) Uani 1 d . . O123 O 0.2761(3) 0.2539(2) 0.0407(2) 0.0274(9) Uani 1 d . . N11 N 0.0579(5) 0.0882(3) 0.1739(3) 0.0296(12) Uani 1 d . . N12 N 0.3071(4) 0.2534(3) -0.0273(3) 0.0262(11) Uani 1 d . . N111 N -0.1434(5) 0.3812(3) -0.1218(3) 0.0317(12) Uani 1 d . . N112 N -0.0299(4) 0.3749(3) -0.0949(2) 0.0264(11) Uani 1 d . . N122 N 0.1727(5) 0.4590(3) -0.0788(3) 0.0315(12) Uani 1 d . . N131 N -0.2687(4) 0.3065(3) -0.0067(3) 0.0292(12) Uani 1 d . . N132 N -0.1868(4) 0.2952(3) 0.0456(3) 0.0259(11) Uani 1 d . . N142 N -0.0683(4) 0.2839(3) 0.1651(2) 0.0242(11) Uani 1 d . . N151 N -0.1297(4) 0.2190(3) -0.0859(2) 0.0270(11) Uani 1 d . . N152 N -0.0237(4) 0.1818(3) -0.0445(2) 0.0242(11) Uani 1 d . . N162 N 0.2065(4) 0.0715(3) 0.0229(2) 0.0212(10) Uani 1 d . . C113 C 0.0220(7) 0.4359(4) -0.1480(3) 0.036(2) Uani 1 d . . C114 C -0.0571(8) 0.4803(4) -0.2082(4) 0.053(2) Uani 1 d . . H4B H -0.0426(8) 0.5259(4) -0.2525(4) 0.063 Uiso 1 calc R . C115 C -0.1600(8) 0.4439(4) -0.1897(4) 0.051(2) Uani 1 d . . H6A H -0.2316(8) 0.4599(4) -0.2197(4) 0.062 Uiso 1 calc R . C121 C 0.1464(6) 0.4522(4) -0.1428(4) 0.038(2) Uani 1 d . . C123 C 0.2873(6) 0.4729(4) -0.0705(4) 0.042(2) Uani 1 d . . C124 C 0.3758(7) 0.4836(5) -0.1296(5) 0.061(2) Uani 1 d . . H3C H 0.4552(7) 0.4938(5) -0.1241(5) 0.074 Uiso 1 calc R . C125 C 0.3485(8) 0.4795(5) -0.1968(5) 0.075(3) Uani 1 d . . H1E H 0.4083(8) 0.4887(5) -0.2383(5) 0.090 Uiso 1 calc R . C126 C 0.2358(8) 0.4622(5) -0.2041(4) 0.060(2) Uani 1 d . . H2A H 0.2181(8) 0.4570(5) -0.2497(4) 0.072 Uiso 1 calc R . C127 C 0.3083(6) 0.4759(4) 0.0039(4) 0.050(2) Uani 1 d . . H95A H 0.3818(24) 0.5008(25) 0.0001(6) 0.075 Uiso 1 calc R . H95B H 0.3254(38) 0.4156(5) 0.0395(7) 0.075 Uiso 1 calc R . H95C H 0.2316(15) 0.5133(22) 0.0212(11) 0.075 Uiso 1 calc R . C132 C -0.3848(5) 0.3029(4) 0.0991(3) 0.0333(15) Uani 1 d . . H24A H -0.4547(5) 0.3043(4) 0.1348(3) 0.040 Uiso 1 calc R . C133 C -0.2570(5) 0.2924(3) 0.1103(3) 0.0251(13) Uani 1 d . . C135 C -0.3883(6) 0.3107(4) 0.0241(4) 0.036(2) Uani 1 d . . H19A H -0.4623(6) 0.3179(4) -0.0010(4) 0.043 Uiso 1 calc R . C141 C -0.1938(5) 0.2856(3) 0.1766(3) 0.0251(13) Uani 1 d . . C143 C -0.0079(6) 0.2898(3) 0.2200(3) 0.0299(14) Uani 1 d . . C144 C -0.0718(7) 0.2933(4) 0.2885(3) 0.044(2) Uani 1 d . . H11A H -0.0278(7) 0.2972(4) 0.3267(3) 0.053 Uiso 1 calc R . C145 C -0.1969(7) 0.2909(4) 0.3000(4) 0.050(2) Uani 1 d . . H5A H -0.2404(7) 0.2918(4) 0.3467(4) 0.060 Uiso 1 calc R . C146 C -0.2608(6) 0.2872(4) 0.2434(3) 0.039(2) Uani 1 d . . H7C H -0.3484(6) 0.2858(4) 0.2504(3) 0.046 Uiso 1 calc R . C147 C 0.1303(6) 0.2931(4) 0.2066(3) 0.039(2) Uani 1 d . . H94A H 0.1742(10) 0.2634(21) 0.2537(5) 0.059 Uiso 1 calc R . H94B H 0.1352(6) 0.3552(4) 0.1875(19) 0.059 Uiso 1 calc R . H94C H 0.1714(10) 0.2629(21) 0.1700(16) 0.059 Uiso 1 calc R . C153 C 0.0372(5) 0.1066(3) -0.0609(3) 0.0219(12) Uani 1 d . . C154 C -0.0329(5) 0.0961(4) -0.1131(3) 0.0265(13) Uani 1 d . . H22A H -0.0127(5) 0.0490(4) -0.1340(3) 0.032 Uiso 1 calc R . C155 C -0.1355(5) 0.1676(4) -0.1270(3) 0.0276(13) Uani 1 d . . H18A H -0.2007(5) 0.1797(4) -0.1603(3) 0.033 Uiso 1 calc R . C161 C 0.1572(5) 0.0497(3) -0.0278(3) 0.0227(12) Uani 1 d . . C163 C 0.3186(5) 0.0160(4) 0.0540(3) 0.0257(13) Uani 1 d . . C164 C 0.3797(5) -0.0600(4) 0.0345(3) 0.0303(14) Uani 1 d . . H10A H 0.4574(5) -0.0974(4) 0.0567(3) 0.036 Uiso 1 calc R . C165 C 0.3272(6) -0.0808(4) -0.0173(3) 0.0325(15) Uani 1 d . . H21A H 0.3675(6) -0.1331(4) -0.0303(3) 0.039 Uiso 1 calc R . C166 C 0.2170(5) -0.0256(4) -0.0495(3) 0.0285(14) Uani 1 d . . H25A H 0.1811(5) -0.0381(4) -0.0863(3) 0.034 Uiso 1 calc R . C167 C 0.3765(5) 0.0356(4) 0.1114(3) 0.0323(14) Uani 1 d . . H91A H 0.4681(8) 0.0059(19) 0.1133(14) 0.048 Uiso 1 calc R . H91B H 0.3342(22) 0.0139(20) 0.1604(4) 0.048 Uiso 1 calc R . H91C H 0.3651(29) 0.0999(4) 0.0980(10) 0.048 Uiso 1 calc R . B1 B -0.2187(7) 0.3101(4) -0.0869(4) 0.033(2) Uani 1 d . . H1 H -0.2930(7) 0.3235(4) -0.1183(4) 0.040 Uiso 1 calc R . Eu2 Eu 0.29745(3) 0.27512(2) 0.46676(2) 0.02777(9) Uani 1 d . . O2 O 0.4613(4) 0.1459(3) 0.5117(2) 0.0380(11) Uani 1 d D . HA H 0.4625(59) 0.1186(32) 0.5621(15) 0.050 Uiso 1 d D . HB H 0.4687(56) 0.0952(26) 0.5008(27) 0.050 Uiso 1 d D . O211 O 0.4198(6) 0.3840(3) 0.6014(3) 0.080(2) Uani 1 d . . O212 O 0.4608(4) 0.3187(3) 0.5151(3) 0.0499(12) Uani 1 d . . O213 O 0.2692(4) 0.3457(3) 0.5652(2) 0.0414(11) Uani 1 d . . O221 O 0.4110(4) 0.3554(3) 0.2446(2) 0.0556(13) Uani 1 d . . O222 O 0.2631(4) 0.3279(3) 0.3313(2) 0.0363(10) Uani 1 d . . O223 O 0.4595(4) 0.2921(3) 0.3613(2) 0.0414(11) Uani 1 d . . N21 N 0.3840(6) 0.3508(4) 0.5622(3) 0.050(2) Uani 1 d . . N22 N 0.3790(5) 0.3258(3) 0.3096(3) 0.0357(13) Uani 1 d . . N211 N 0.0765(4) 0.1630(3) 0.5825(3) 0.0279(11) Uani 1 d . . N212 N 0.1873(4) 0.1846(3) 0.5871(3) 0.0273(11) Uani 1 d . . N222 N 0.4351(5) 0.1529(3) 0.6556(3) 0.0319(12) Uani 1 d . . N231 N -0.0266(4) 0.2935(3) 0.4764(3) 0.0286(11) Uani 1 d . . N232 N 0.0671(4) 0.3378(3) 0.4569(3) 0.0293(12) Uani 1 d . . N242 N 0.2148(5) 0.4607(3) 0.4069(3) 0.0381(13) Uani 1 d . . N251 N 0.0960(4) 0.1492(3) 0.4537(3) 0.0271(11) Uani 1 d . . N252 N 0.2188(4) 0.1560(3) 0.4334(2) 0.0263(11) Uani 1 d . . N262 N 0.4901(4) 0.0855(3) 0.3918(3) 0.0292(11) Uani 1 d . . C213 C 0.2106(5) 0.1537(4) 0.6609(3) 0.0303(14) Uani 1 d . . C214 C 0.1173(6) 0.1116(4) 0.7029(3) 0.036(2) Uani 1 d . . H17A H 0.1121(6) 0.0841(4) 0.7555(3) 0.044 Uiso 1 calc R . C215 C 0.0347(6) 0.1189(4) 0.6511(3) 0.035(2) Uani 1 d . . H20A H -0.0396(6) 0.0965(4) 0.6619(3) 0.043 Uiso 1 calc R . C221 C 0.3191(6) 0.1654(4) 0.6912(3) 0.0356(15) Uani 1 d . . C223 C 0.5336(6) 0.1639(4) 0.6835(4) 0.038(2) Uani 1 d . . C224 C 0.5177(7) 0.1884(5) 0.7488(4) 0.053(2) Uani 1 d . . H1D H 0.5886(7) 0.1961(5) 0.7678(4) 0.064 Uiso 1 calc R . C225 C 0.3987(7) 0.2010(5) 0.7851(4) 0.052(2) Uani 1 d . . H8D H 0.3865(7) 0.2179(5) 0.8292(4) 0.062 Uiso 1 calc R . C226 C 0.2981(6) 0.1890(4) 0.7568(3) 0.043(2) Uani 1 d . . H15A H 0.2155(6) 0.1967(4) 0.7813(3) 0.052 Uiso 1 calc R . C227 C 0.6603(6) 0.1531(5) 0.6399(4) 0.050(2) Uani 1 d . . H92A H 0.7292(7) 0.1439(27) 0.6722(7) 0.076 Uiso 1 calc R . H92B H 0.6590(15) 0.2066(12) 0.5968(13) 0.076 Uiso 1 calc R . H92C H 0.6751(19) 0.1015(17) 0.6223(20) 0.076 Uiso 1 calc R . C233 C 0.0083(6) 0.4256(4) 0.4311(3) 0.0307(14) Uani 1 d . . C234 C -0.1236(6) 0.4369(4) 0.4342(3) 0.037(2) Uani 1 d . . H7A H -0.1874(6) 0.4913(4) 0.4194(3) 0.044 Uiso 1 calc R . C235 C -0.1419(6) 0.3534(4) 0.4631(3) 0.035(2) Uani 1 d . . H26A H -0.2228(6) 0.3393(4) 0.4725(3) 0.042 Uiso 1 calc R . C241 C 0.0846(7) 0.4913(4) 0.4045(3) 0.036(2) Uani 1 d . . C243 C 0.2861(8) 0.5207(5) 0.3812(4) 0.048(2) Uani 1 d . . C244 C 0.2299(9) 0.6110(5) 0.3548(4) 0.055(2) Uani 1 d . . H4A H 0.2820(9) 0.6520(5) 0.3367(4) 0.066 Uiso 1 calc R . C245 C 0.0987(9) 0.6414(5) 0.3547(4) 0.059(2) Uani 1 d . . H3B H 0.0598(9) 0.7034(5) 0.3379(4) 0.071 Uiso 1 calc R . C246 C 0.0238(7) 0.5811(4) 0.3792(4) 0.050(2) Uani 1 d . . H7D H -0.0670(7) 0.6007(4) 0.3786(4) 0.059 Uiso 1 calc R . C247 C 0.4306(7) 0.4875(5) 0.3818(4) 0.065(2) Uani 1 d . . H93A H 0.4580(8) 0.4692(29) 0.4331(5) 0.098 Uiso 1 calc R . H93B H 0.4695(7) 0.5352(12) 0.3500(21) 0.098 Uiso 1 calc R . H93C H 0.4579(8) 0.4366(21) 0.3628(26) 0.098 Uiso 1 calc R . C253 C 0.2620(5) 0.1099(3) 0.3845(3) 0.0262(13) Uani 1 d . . C254 C 0.1652(6) 0.0754(4) 0.3726(4) 0.039(2) Uani 1 d . . H13A H 0.1698(6) 0.0415(4) 0.3402(4) 0.047 Uiso 1 calc R . C256 C 0.0621(6) 0.1012(4) 0.4180(3) 0.036(2) Uani 1 d . . H19B H -0.0186(6) 0.0875(4) 0.4233(3) 0.044 Uiso 1 calc R . C261 C 0.3922(5) 0.0992(4) 0.3494(3) 0.0278(13) Uani 1 d . . C263 C 0.6100(6) 0.0771(4) 0.3600(3) 0.0317(14) Uani 1 d . . C264 C 0.6337(6) 0.0823(4) 0.2849(3) 0.038(2) Uani 1 d . . H11B H 0.7184(6) 0.0771(4) 0.2633(3) 0.046 Uiso 1 calc R . C265 C 0.5327(6) 0.0949(4) 0.2425(3) 0.041(2) Uani 1 d . . H16A H 0.5470(6) 0.0987(4) 0.1911(3) 0.050 Uiso 1 calc R . C266 C 0.4116(6) 0.1020(4) 0.2750(3) 0.036(2) Uani 1 d . . H18B H 0.3414(6) 0.1087(4) 0.2469(3) 0.043 Uiso 1 calc R . C267 C 0.7156(6) 0.0627(5) 0.4086(4) 0.049(2) Uani 1 d . . H90A H 0.7043(22) 0.1155(11) 0.4238(19) 0.073 Uiso 1 calc R . H90B H 0.7981(6) 0.0521(26) 0.3808(8) 0.073 Uiso 1 calc R . H90C H 0.7140(24) 0.0111(17) 0.4530(11) 0.073 Uiso 1 calc R . B2 B 0.0083(6) 0.1918(4) 0.5092(4) 0.028(2) Uani 1 d . . H2 H -0.0721(6) 0.1709(4) 0.5198(4) 0.034 Uiso 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 Eu1 0.0232(2) 0.0183(2) 0.0190(2) -0.00813(14) -0.00220(12) -0.00479(12) O1 0.035(2) 0.017(2) 0.026(2) -0.007(2) 0.004(2) -0.007(2) O111 0.091(4) 0.038(3) 0.025(3) 0.015(2) -0.022(2) -0.039(3) O112 0.028(2) 0.028(2) 0.028(2) -0.012(2) -0.005(2) -0.012(2) O113 0.031(2) 0.023(2) 0.026(2) -0.009(2) -0.002(2) -0.012(2) O121 0.022(2) 0.048(3) 0.045(3) -0.023(2) 0.009(2) -0.013(2) O122 0.029(2) 0.026(2) 0.031(2) -0.008(2) -0.002(2) -0.010(2) O123 0.030(2) 0.028(2) 0.028(2) -0.017(2) -0.002(2) -0.001(2) N11 0.044(3) 0.028(3) 0.020(3) -0.011(3) -0.003(2) -0.010(2) N12 0.031(3) 0.014(2) 0.034(3) -0.007(2) 0.000(2) -0.007(2) N111 0.044(3) 0.026(3) 0.023(3) -0.012(2) -0.008(2) 0.002(2) N112 0.037(3) 0.020(3) 0.019(3) -0.004(2) -0.003(2) -0.002(2) N122 0.038(3) 0.012(2) 0.040(3) -0.009(2) 0.010(2) -0.003(2) N131 0.026(3) 0.032(3) 0.034(3) -0.018(3) -0.007(2) -0.002(2) N132 0.028(3) 0.026(3) 0.026(3) -0.010(2) -0.009(2) -0.005(2) N142 0.035(3) 0.016(2) 0.022(3) -0.008(2) -0.002(2) -0.005(2) N151 0.030(3) 0.033(3) 0.026(3) -0.018(2) -0.008(2) -0.005(2) N152 0.029(3) 0.021(3) 0.022(3) -0.007(2) -0.003(2) -0.005(2) N162 0.025(3) 0.018(2) 0.020(2) -0.006(2) 0.001(2) -0.005(2) C113 0.064(5) 0.021(3) 0.018(3) -0.008(3) 0.000(3) 0.000(3) C114 0.106(7) 0.023(4) 0.028(4) -0.004(3) -0.006(4) -0.018(4) C115 0.096(6) 0.028(4) 0.025(4) -0.010(3) -0.033(4) 0.009(4) C121 0.053(4) 0.017(3) 0.035(4) -0.005(3) 0.010(3) -0.005(3) C123 0.030(4) 0.019(3) 0.071(5) -0.013(4) 0.010(4) -0.004(3) C124 0.052(5) 0.041(5) 0.084(7) -0.016(5) 0.026(5) -0.018(4) C125 0.075(6) 0.056(5) 0.074(7) -0.010(5) 0.053(5) -0.023(5) C126 0.081(6) 0.046(5) 0.047(5) -0.016(4) 0.030(4) -0.019(4) C127 0.034(4) 0.034(4) 0.085(6) -0.023(4) 0.000(4) -0.009(3) C132 0.030(3) 0.029(3) 0.043(4) -0.016(3) 0.003(3) -0.007(3) C133 0.023(3) 0.020(3) 0.029(3) -0.005(3) 0.000(3) -0.003(2) C135 0.026(3) 0.033(4) 0.054(5) -0.024(4) -0.013(3) 0.003(3) C141 0.029(3) 0.020(3) 0.020(3) -0.005(3) 0.000(2) 0.001(2) C143 0.048(4) 0.017(3) 0.027(3) -0.008(3) -0.013(3) -0.005(3) C144 0.070(5) 0.034(4) 0.027(4) -0.014(3) -0.010(3) -0.001(4) C145 0.068(5) 0.049(4) 0.029(4) -0.023(4) 0.003(4) 0.003(4) C146 0.043(4) 0.038(4) 0.029(4) -0.010(3) 0.006(3) -0.006(3) C147 0.051(4) 0.034(4) 0.043(4) -0.019(3) -0.027(3) -0.006(3) C153 0.029(3) 0.017(3) 0.020(3) -0.007(3) 0.005(2) -0.006(2) C154 0.037(3) 0.027(3) 0.024(3) -0.015(3) 0.004(3) -0.015(3) C155 0.035(3) 0.034(3) 0.020(3) -0.012(3) -0.006(3) -0.011(3) C161 0.029(3) 0.019(3) 0.022(3) -0.006(3) 0.005(2) -0.012(2) C163 0.029(3) 0.024(3) 0.021(3) -0.004(3) 0.003(2) -0.008(3) C164 0.025(3) 0.024(3) 0.040(4) -0.014(3) 0.001(3) 0.000(3) C165 0.040(4) 0.019(3) 0.041(4) -0.018(3) 0.006(3) -0.006(3) C166 0.035(4) 0.025(3) 0.028(3) -0.015(3) 0.002(3) -0.005(3) C167 0.027(3) 0.032(3) 0.037(4) -0.013(3) -0.008(3) 0.002(3) B1 0.036(4) 0.032(4) 0.031(4) -0.016(4) -0.015(3) 0.008(3) Eu2 0.0333(2) 0.0338(2) 0.0225(2) -0.0111(2) 0.00147(14) -0.0168(2) O2 0.037(2) 0.047(3) 0.035(3) -0.021(2) -0.003(2) -0.009(2) O211 0.119(5) 0.071(4) 0.081(4) -0.037(3) -0.039(4) -0.039(3) O212 0.051(3) 0.061(3) 0.049(3) -0.014(3) -0.005(2) -0.035(3) O213 0.061(3) 0.040(3) 0.028(3) -0.012(2) -0.008(2) -0.015(2) O221 0.051(3) 0.075(4) 0.022(3) -0.003(3) 0.014(2) -0.009(3) O222 0.039(3) 0.046(3) 0.030(2) -0.017(2) 0.003(2) -0.016(2) O223 0.039(3) 0.046(3) 0.032(3) -0.010(2) 0.003(2) -0.006(2) N21 0.072(5) 0.046(4) 0.043(4) -0.013(3) -0.019(3) -0.028(3) N22 0.044(3) 0.035(3) 0.027(3) -0.012(3) 0.009(3) -0.010(3) N211 0.026(3) 0.027(3) 0.030(3) -0.008(2) 0.002(2) -0.008(2) N212 0.028(3) 0.030(3) 0.027(3) -0.011(2) 0.001(2) -0.010(2) N222 0.035(3) 0.035(3) 0.026(3) -0.012(3) -0.005(2) -0.003(2) N231 0.032(3) 0.027(3) 0.026(3) -0.008(2) 0.000(2) -0.008(2) N232 0.036(3) 0.031(3) 0.022(3) -0.010(2) -0.002(2) -0.006(2) N242 0.067(4) 0.034(3) 0.024(3) -0.014(3) 0.006(3) -0.027(3) N251 0.032(3) 0.025(3) 0.028(3) -0.009(2) -0.002(2) -0.011(2) N252 0.026(3) 0.029(3) 0.024(3) -0.009(2) -0.004(2) -0.006(2) N262 0.033(3) 0.028(3) 0.027(3) -0.009(2) -0.001(2) -0.007(2) C213 0.031(3) 0.029(3) 0.025(3) -0.007(3) 0.002(3) -0.001(3) C214 0.044(4) 0.033(4) 0.022(3) -0.002(3) 0.006(3) -0.006(3) C215 0.034(4) 0.031(4) 0.033(4) -0.003(3) 0.010(3) -0.008(3) C221 0.039(4) 0.040(4) 0.024(3) -0.010(3) 0.002(3) -0.005(3) C223 0.040(4) 0.030(4) 0.038(4) -0.008(3) -0.011(3) 0.000(3) C224 0.051(5) 0.062(5) 0.048(5) -0.014(4) -0.028(4) -0.007(4) C225 0.059(5) 0.067(5) 0.028(4) -0.022(4) -0.006(4) -0.004(4) C226 0.043(4) 0.059(5) 0.023(3) -0.012(3) 0.000(3) -0.008(3) C227 0.033(4) 0.057(5) 0.067(5) -0.027(4) -0.009(4) -0.007(3) C233 0.049(4) 0.027(3) 0.016(3) -0.009(3) -0.003(3) -0.005(3) C234 0.051(4) 0.030(4) 0.029(4) -0.011(3) -0.007(3) -0.005(3) C235 0.034(4) 0.046(4) 0.027(4) -0.017(3) -0.007(3) -0.003(3) C241 0.061(5) 0.038(4) 0.016(3) -0.009(3) 0.001(3) -0.023(4) C243 0.085(6) 0.043(4) 0.029(4) -0.017(4) 0.013(4) -0.037(4) C244 0.107(7) 0.042(5) 0.031(4) -0.016(4) 0.015(4) -0.044(5) C245 0.108(7) 0.031(4) 0.041(5) -0.015(4) 0.007(5) -0.023(5) C246 0.082(6) 0.029(4) 0.035(4) -0.012(4) -0.001(4) -0.010(4) C247 0.086(6) 0.056(5) 0.073(6) -0.031(5) 0.027(5) -0.050(5) C253 0.032(3) 0.022(3) 0.025(3) -0.008(3) -0.005(3) -0.004(3) C254 0.040(4) 0.033(4) 0.053(4) -0.022(4) -0.014(3) -0.007(3) C256 0.037(4) 0.033(4) 0.045(4) -0.014(3) -0.013(3) -0.010(3) C261 0.035(3) 0.022(3) 0.028(3) -0.012(3) -0.001(3) -0.005(3) C263 0.037(4) 0.027(3) 0.029(3) -0.002(3) -0.007(3) -0.010(3) C264 0.040(4) 0.035(4) 0.037(4) -0.014(3) 0.003(3) -0.005(3) C265 0.048(4) 0.045(4) 0.028(4) -0.016(3) 0.002(3) -0.002(3) C266 0.036(4) 0.039(4) 0.036(4) -0.020(3) -0.008(3) -0.003(3) C267 0.038(4) 0.064(5) 0.049(5) -0.020(4) -0.004(3) -0.015(4) B2 0.026(4) 0.031(4) 0.026(4) -0.007(3) 0.006(3) -0.011(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 Eu1 O1 2.400(3) . ? Eu1 N132 2.474(4) . ? Eu1 N152 2.481(4) . ? Eu1 O122 2.496(4) . ? Eu1 O113 2.505(4) . ? Eu1 O112 2.508(4) . ? Eu1 O123 2.516(4) . ? Eu1 N142 2.743(4) . ? Eu1 N112 2.796(5) . ? Eu1 N11 2.936(5) . ? Eu1 N12 2.937(5) . ? Eu1 N162 2.974(4) . ? O1 H1B 0.91(3) . ? O1 H1A 0.88(3) . ? O111 N11 1.209(6) . ? O112 N11 1.291(5) . ? O113 N11 1.269(5) . ? O121 N12 1.218(5) . ? O122 N12 1.264(5) . ? O123 N12 1.291(5) . ? N111 C115 1.353(7) . ? N111 N112 1.363(6) . ? N111 B1 1.533(9) . ? N112 C113 1.352(7) . ? N122 C121 1.333(7) . ? N122 C123 1.368(7) . ? N131 C135 1.345(7) . ? N131 N132 1.355(6) . ? N131 B1 1.536(8) . ? N132 C133 1.351(6) . ? N142 C141 1.347(7) . ? N142 C143 1.349(6) . ? N151 C155 1.350(6) . ? N151 N152 1.360(6) . ? N151 B1 1.541(7) . ? N152 C153 1.350(6) . ? N162 C161 1.352(6) . ? N162 C163 1.372(6) . ? C113 C114 1.392(9) . ? C113 C121 1.473(9) . ? C114 C115 1.366(10) . ? C114 H4B 0.95 . ? C115 H6A 0.95 . ? C121 C126 1.408(9) . ? C123 C124 1.374(9) . ? C123 C127 1.481(9) . ? C124 C125 1.378(11) . ? C124 H3C 0.95 . ? C125 C126 1.369(10) . ? C125 H1E 0.95 . ? C126 H2A 0.95 . ? C127 H95A 0.98 . ? C127 H95B 0.98 . ? C127 H95C 0.98 . ? C132 C133 1.389(7) . ? C132 C135 1.392(8) . ? C132 H24A 0.95 . ? C133 C141 1.473(7) . ? C135 H19A 0.95 . ? C141 C146 1.380(7) . ? C143 C144 1.403(8) . ? C143 C147 1.503(8) . ? C144 C145 1.358(9) . ? C144 H11A 0.95 . ? C145 C146 1.384(8) . ? C145 H5A 0.95 . ? C146 H7C 0.95 . ? C147 H94A 0.98 . ? C147 H94B 0.98 . ? C147 H94C 0.98 . ? C153 C154 1.411(7) . ? C153 C161 1.456(7) . ? C154 C155 1.357(7) . ? C154 H22A 0.95 . ? C155 H18A 0.95 . ? C161 C166 1.400(6) . ? C163 C164 1.391(7) . ? C163 C167 1.492(7) . ? C164 C165 1.380(7) . ? C164 H10A 0.95 . ? C165 C166 1.361(7) . ? C165 H21A 0.95 . ? C166 H25A 0.95 . ? C167 H91A 0.98 . ? C167 H91B 0.98 . ? C167 H91C 0.98 . ? B1 H1 1.00 . ? Eu2 O2 2.349(4) . ? Eu2 N232 2.435(5) . ? Eu2 O213 2.463(4) . ? Eu2 O222 2.469(4) . ? Eu2 O212 2.474(4) . ? Eu2 O223 2.479(4) . ? Eu2 N212 2.619(5) . ? Eu2 N252 2.633(4) . ? Eu2 N242 2.807(5) . ? Eu2 N21 2.896(5) . ? Eu2 N22 2.903(5) . ? O2 HA 0.91(3) . ? O2 HB 0.91(3) . ? O211 N21 1.217(6) . ? O212 N21 1.284(7) . ? O213 N21 1.267(7) . ? O221 N22 1.206(6) . ? O222 N22 1.267(6) . ? O223 N22 1.278(6) . ? N211 C215 1.349(7) . ? N211 N212 1.371(6) . ? N211 B2 1.535(8) . ? N212 C213 1.354(7) . ? N222 C223 1.337(7) . ? N222 C221 1.346(7) . ? N231 C235 1.356(7) . ? N231 N232 1.357(6) . ? N231 B2 1.534(8) . ? N232 C233 1.355(7) . ? N242 C243 1.348(8) . ? N242 C241 1.366(8) . ? N251 C256 1.348(6) . ? N251 N252 1.363(6) . ? N251 B2 1.539(7) . ? N252 C253 1.349(6) . ? N262 C261 1.346(7) . ? N262 C263 1.351(7) . ? C213 C214 1.396(8) . ? C213 C221 1.465(8) . ? C214 C215 1.375(8) . ? C214 H17A 0.95 . ? C215 H20A 0.95 . ? C221 C226 1.401(7) . ? C223 C224 1.406(8) . ? C223 C227 1.507(8) . ? C224 C225 1.378(9) . ? C224 H1D 0.95 . ? C225 C226 1.370(8) . ? C225 H8D 0.95 . ? C226 H15A 0.95 . ? C227 H92A 0.98 . ? C227 H92B 0.98 . ? C227 H92C 0.98 . ? C233 C234 1.390(8) . ? C233 C241 1.464(8) . ? C234 C235 1.362(8) . ? C234 H7A 0.95 . ? C235 H26A 0.95 . ? C241 C246 1.387(8) . ? C243 C244 1.386(9) . ? C243 C247 1.514(9) . ? C244 C245 1.373(10) . ? C244 H4A 0.95 . ? C245 C246 1.381(9) . ? C245 H3B 0.95 . ? C246 H7D 0.95 . ? C247 H93A 0.98 . ? C247 H93B 0.98 . ? C247 H93C 0.98 . ? C253 C254 1.404(7) . ? C253 C261 1.471(7) . ? C254 C256 1.380(8) . ? C254 H13A 0.95 . ? C256 H19B 0.95 . ? C261 C266 1.388(7) . ? C263 C264 1.394(8) . ? C263 C267 1.488(8) . ? C264 C265 1.378(8) . ? C264 H11B 0.95 . ? C265 C266 1.369(8) . ? C265 H16A 0.95 . ? C266 H18B 0.95 . ? C267 H90A 0.98 . ? C267 H90B 0.98 . ? C267 H90C 0.98 . ? B2 H2 1.00 . ? 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 Eu1 N132 84.55(13) . . ? O1 Eu1 N152 136.65(14) . . ? N132 Eu1 N152 74.81(13) . . ? O1 Eu1 O122 91.74(12) . . ? N132 Eu1 O122 134.22(14) . . ? N152 Eu1 O122 77.30(13) . . ? O1 Eu1 O113 106.55(12) . . ? N132 Eu1 O113 112.93(14) . . ? N152 Eu1 O113 116.51(13) . . ? O122 Eu1 O113 111.83(12) . . ? O1 Eu1 O112 133.95(12) . . ? N132 Eu1 O112 73.37(13) . . ? N152 Eu1 O112 75.77(13) . . ? O122 Eu1 O112 132.42(11) . . ? O113 Eu1 O112 51.33(11) . . ? O1 Eu1 O123 71.46(12) . . ? N132 Eu1 O123 155.92(12) . . ? N152 Eu1 O123 124.55(12) . . ? O122 Eu1 O123 51.20(11) . . ? O113 Eu1 O123 73.43(12) . . ? O112 Eu1 O123 122.28(12) . . ? O1 Eu1 N142 64.09(12) . . ? N132 Eu1 N142 61.79(13) . . ? N152 Eu1 N142 130.32(14) . . ? O122 Eu1 N142 151.61(12) . . ? O113 Eu1 N142 65.37(12) . . ? O112 Eu1 N142 69.86(11) . . ? O123 Eu1 N142 104.13(12) . . ? O1 Eu1 N112 68.67(12) . . ? N132 Eu1 N112 70.97(14) . . ? N152 Eu1 N112 68.67(13) . . ? O122 Eu1 N112 65.32(13) . . ? O113 Eu1 N112 173.90(12) . . ? O112 Eu1 N112 134.70(13) . . ? O123 Eu1 N112 101.09(13) . . ? N142 Eu1 N112 114.28(12) . . ? O1 Eu1 N11 123.50(12) . . ? N132 Eu1 N11 94.06(14) . . ? N152 Eu1 N11 96.05(13) . . ? O122 Eu1 N11 124.54(12) . . ? O113 Eu1 N11 25.42(11) . . ? O112 Eu1 N11 25.93(11) . . ? O123 Eu1 N11 97.42(13) . . ? N142 Eu1 N11 65.92(12) . . ? N112 Eu1 N11 160.63(14) . . ? O1 Eu1 N12 81.98(12) . . ? N132 Eu1 N12 153.96(14) . . ? N152 Eu1 N12 100.38(13) . . ? O122 Eu1 N12 25.28(11) . . ? O113 Eu1 N12 92.29(13) . . ? O112 Eu1 N12 131.06(12) . . ? O123 Eu1 N12 25.96(11) . . ? N142 Eu1 N12 129.23(13) . . ? N112 Eu1 N12 83.37(14) . . ? N11 Eu1 N12 111.96(13) . . ? O1 Eu1 N162 148.03(13) . . ? N132 Eu1 N162 127.20(12) . . ? N152 Eu1 N162 61.56(13) . . ? O122 Eu1 N162 64.28(11) . . ? O113 Eu1 N162 67.51(11) . . ? O112 Eu1 N162 68.48(11) . . ? O123 Eu1 N162 76.88(11) . . ? N142 Eu1 N162 130.07(12) . . ? N112 Eu1 N162 114.34(12) . . ? N11 Eu1 N162 64.52(12) . . ? N12 Eu1 N162 67.35(11) . . ? Eu1 O1 H1B 112.6(33) . . ? Eu1 O1 H1A 126.1(37) . . ? H1B O1 H1A 100.3(32) . . ? N11 O112 Eu1 95.9(3) . . ? N11 O113 Eu1 96.6(3) . . ? N12 O122 Eu1 97.2(3) . . ? N12 O123 Eu1 95.5(3) . . ? O111 N11 O113 122.2(5) . . ? O111 N11 O112 121.8(5) . . ? O113 N11 O112 116.0(5) . . ? O111 N11 Eu1 176.1(4) . . ? O113 N11 Eu1 57.9(3) . . ? O112 N11 Eu1 58.2(3) . . ? O121 N12 O122 122.5(5) . . ? O121 N12 O123 121.7(5) . . ? O122 N12 O123 115.8(4) . . ? O121 N12 Eu1 177.1(3) . . ? O122 N12 Eu1 57.5(2) . . ? O123 N12 Eu1 58.5(2) . . ? C115 N111 N112 110.1(5) . . ? C115 N111 B1 126.4(5) . . ? N112 N111 B1 121.9(5) . . ? C113 N112 N111 105.3(5) . . ? C113 N112 Eu1 135.3(4) . . ? N111 N112 Eu1 119.1(3) . . ? C121 N122 C123 121.2(6) . . ? C135 N131 N132 110.0(5) . . ? C135 N131 B1 129.7(5) . . ? N132 N131 B1 120.3(5) . . ? C133 N132 N131 106.9(4) . . ? C133 N132 Eu1 123.1(4) . . ? N131 N132 Eu1 127.7(3) . . ? C141 N142 C143 118.1(5) . . ? C141 N142 Eu1 116.0(3) . . ? C143 N142 Eu1 125.2(4) . . ? C155 N151 N152 109.8(4) . . ? C155 N151 B1 128.1(5) . . ? N152 N151 B1 121.9(4) . . ? C153 N152 N151 106.5(4) . . ? C153 N152 Eu1 126.6(3) . . ? N151 N152 Eu1 126.9(3) . . ? C161 N162 C163 117.5(4) . . ? C161 N162 Eu1 111.0(3) . . ? C163 N162 Eu1 131.5(3) . . ? N112 C113 C114 111.0(6) . . ? N112 C113 C121 124.3(6) . . ? C114 C113 C121 124.7(6) . . ? C115 C114 C113 104.8(6) . . ? C115 C114 H4B 127.6(4) . . ? C113 C114 H4B 127.6(4) . . ? N111 C115 C114 108.8(6) . . ? N111 C115 H6A 125.6(4) . . ? C114 C115 H6A 125.6(4) . . ? N122 C121 C126 120.0(7) . . ? N122 C121 C113 118.6(5) . . ? C126 C121 C113 121.3(6) . . ? N122 C123 C124 120.0(7) . . ? N122 C123 C127 116.6(6) . . ? C124 C123 C127 123.4(7) . . ? C123 C124 C125 119.6(7) . . ? C123 C124 H3C 120.2(5) . . ? C125 C124 H3C 120.2(5) . . ? C126 C125 C124 120.3(7) . . ? C126 C125 H1E 119.9(5) . . ? C124 C125 H1E 119.9(5) . . ? C125 C126 C121 118.9(7) . . ? C125 C126 H2A 120.5(5) . . ? C121 C126 H2A 120.5(5) . . ? C123 C127 H95A 109.5(4) . . ? C123 C127 H95B 109.5(3) . . ? H95A C127 H95B 109.5 . . ? C123 C127 H95C 109.5(3) . . ? H95A C127 H95C 109.5 . . ? H95B C127 H95C 109.5 . . ? C133 C132 C135 105.1(5) . . ? C133 C132 H24A 127.4(3) . . ? C135 C132 H24A 127.4(4) . . ? N132 C133 C132 109.9(5) . . ? N132 C133 C141 119.0(5) . . ? C132 C133 C141 131.0(5) . . ? N131 C135 C132 108.1(5) . . ? N131 C135 H19A 125.9(3) . . ? C132 C135 H19A 125.9(4) . . ? N142 C141 C146 123.1(5) . . ? N142 C141 C133 114.6(5) . . ? C146 C141 C133 122.2(5) . . ? N142 C143 C144 121.2(6) . . ? N142 C143 C147 118.9(5) . . ? C144 C143 C147 119.9(5) . . ? C145 C144 C143 119.6(6) . . ? C145 C144 H11A 120.2(4) . . ? C143 C144 H11A 120.2(4) . . ? C144 C145 C146 119.7(6) . . ? C144 C145 H5A 120.2(4) . . ? C146 C145 H5A 120.2(4) . . ? C141 C146 C145 118.3(6) . . ? C141 C146 H7C 120.9(4) . . ? C145 C146 H7C 120.9(4) . . ? C143 C147 H94A 109.5(3) . . ? C143 C147 H94B 109.5(3) . . ? H94A C147 H94B 109.5 . . ? C143 C147 H94C 109.5(3) . . ? H94A C147 H94C 109.5 . . ? H94B C147 H94C 109.5 . . ? N152 C153 C154 109.3(5) . . ? N152 C153 C161 122.1(4) . . ? C154 C153 C161 128.6(4) . . ? C155 C154 C153 105.4(4) . . ? C155 C154 H22A 127.3(3) . . ? C153 C154 H22A 127.3(3) . . ? N151 C155 C154 108.9(5) . . ? N151 C155 H18A 125.5(3) . . ? C154 C155 H18A 125.5(3) . . ? N162 C161 C166 122.5(5) . . ? N162 C161 C153 118.7(4) . . ? C166 C161 C153 118.8(5) . . ? N162 C163 C164 121.6(5) . . ? N162 C163 C167 120.0(4) . . ? C164 C163 C167 118.4(5) . . ? C165 C164 C163 119.8(5) . . ? C165 C164 H10A 120.1(3) . . ? C163 C164 H10A 120.1(3) . . ? C166 C165 C164 119.3(5) . . ? C166 C165 H21A 120.3(3) . . ? C164 C165 H21A 120.3(3) . . ? C165 C166 C161 119.4(5) . . ? C165 C166 H25A 120.3(3) . . ? C161 C166 H25A 120.3(3) . . ? C163 C167 H91A 109.5(3) . . ? C163 C167 H91B 109.5(3) . . ? H91A C167 H91B 109.5 . . ? C163 C167 H91C 109.5(3) . . ? H91A C167 H91C 109.5 . . ? H91B C167 H91C 109.5 . . ? N111 B1 N131 112.0(4) . . ? N111 B1 N151 108.6(5) . . ? N131 B1 N151 109.0(5) . . ? N111 B1 H1 109.1(3) . . ? N131 B1 H1 109.1(3) . . ? N151 B1 H1 109.1(3) . . ? O2 Eu2 N232 145.7(2) . . ? O2 Eu2 O213 102.65(14) . . ? N232 Eu2 O213 83.57(14) . . ? O2 Eu2 O222 116.96(13) . . ? N232 Eu2 O222 75.23(14) . . ? O213 Eu2 O222 135.46(13) . . ? O2 Eu2 O212 73.10(15) . . ? N232 Eu2 O212 130.99(15) . . ? O213 Eu2 O212 51.96(15) . . ? O222 Eu2 O212 120.15(14) . . ? O2 Eu2 O223 78.50(14) . . ? N232 Eu2 O223 125.6(2) . . ? O213 Eu2 O223 124.95(14) . . ? O222 Eu2 O223 51.57(14) . . ? O212 Eu2 O223 77.57(15) . . ? O2 Eu2 N212 77.65(14) . . ? N232 Eu2 N212 72.92(15) . . ? O213 Eu2 N212 70.02(14) . . ? O222 Eu2 N212 135.49(14) . . ? O212 Eu2 N212 104.20(15) . . ? O223 Eu2 N212 154.33(13) . . ? O2 Eu2 N252 77.87(14) . . ? N232 Eu2 N252 76.50(14) . . ? O213 Eu2 N252 140.53(15) . . ? O222 Eu2 N252 71.26(13) . . ? O212 Eu2 N252 150.84(15) . . ? O223 Eu2 N252 94.15(14) . . ? N212 Eu2 N252 71.67(13) . . ? O2 Eu2 N242 150.3(2) . . ? N232 Eu2 N242 63.5(2) . . ? O213 Eu2 N242 69.11(13) . . ? O222 Eu2 N242 66.40(12) . . ? O212 Eu2 N242 80.2(2) . . ? O223 Eu2 N242 83.48(14) . . ? N212 Eu2 N242 122.18(14) . . ? N252 Eu2 N242 127.17(14) . . ? O2 Eu2 N21 88.1(2) . . ? N232 Eu2 N21 107.3(2) . . ? O213 Eu2 N21 25.77(15) . . ? O222 Eu2 N21 132.25(15) . . ? O212 Eu2 N21 26.19(15) . . ? O223 Eu2 N21 101.5(2) . . ? N212 Eu2 N21 87.0(2) . . ? N252 Eu2 N21 156.5(2) . . ? N242 Eu2 N21 72.55(15) . . ? O2 Eu2 N22 99.26(14) . . ? N232 Eu2 N22 100.0(2) . . ? O213 Eu2 N22 134.02(14) . . ? O222 Eu2 N22 25.69(13) . . ? O212 Eu2 N22 98.4(2) . . ? O223 Eu2 N22 25.98(13) . . ? N212 Eu2 N22 155.02(13) . . ? N252 Eu2 N22 83.42(14) . . ? N242 Eu2 N22 71.86(13) . . ? N21 Eu2 N22 117.8(2) . . ? Eu2 O2 HA 117.4(36) . . ? Eu2 O2 HB 122.9(36) . . ? HA O2 HB 94.3(31) . . ? N21 O212 Eu2 95.6(3) . . ? N21 O213 Eu2 96.5(3) . . ? N22 O222 Eu2 96.7(3) . . ? N22 O223 Eu2 95.9(3) . . ? O211 N21 O213 122.3(6) . . ? O211 N21 O212 121.9(6) . . ? O213 N21 O212 115.9(5) . . ? O211 N21 Eu2 178.9(5) . . ? O213 N21 Eu2 57.7(3) . . ? O212 N21 Eu2 58.2(3) . . ? O221 N22 O222 122.3(6) . . ? O221 N22 O223 122.2(5) . . ? O222 N22 O223 115.5(5) . . ? O221 N22 Eu2 173.3(4) . . ? O222 N22 Eu2 57.6(3) . . ? O223 N22 Eu2 58.1(3) . . ? C215 N211 N212 110.3(5) . . ? C215 N211 B2 126.5(5) . . ? N212 N211 B2 123.1(5) . . ? C213 N212 N211 105.2(5) . . ? C213 N212 Eu2 134.4(4) . . ? N211 N212 Eu2 120.3(3) . . ? C223 N222 C221 119.0(5) . . ? C235 N231 N232 108.8(5) . . ? C235 N231 B2 131.1(5) . . ? N232 N231 B2 120.0(5) . . ? C233 N232 N231 106.9(5) . . ? C233 N232 Eu2 125.4(4) . . ? N231 N232 Eu2 127.7(3) . . ? C243 N242 C241 118.1(6) . . ? C243 N242 Eu2 128.6(5) . . ? C241 N242 Eu2 113.3(4) . . ? C256 N251 N252 110.8(4) . . ? C256 N251 B2 125.0(5) . . ? N252 N251 B2 124.2(4) . . ? C253 N252 N251 105.9(4) . . ? C253 N252 Eu2 133.6(4) . . ? N251 N252 Eu2 118.6(3) . . ? C261 N262 C263 118.6(5) . . ? N212 C213 C214 111.1(5) . . ? N212 C213 C221 123.4(5) . . ? C214 C213 C221 125.6(6) . . ? C215 C214 C213 104.6(5) . . ? C215 C214 H17A 127.7(4) . . ? C213 C214 H17A 127.7(4) . . ? N211 C215 C214 108.8(5) . . ? N211 C215 H20A 125.6(3) . . ? C214 C215 H20A 125.6(4) . . ? N222 C221 C226 122.1(6) . . ? N222 C221 C213 119.4(5) . . ? C226 C221 C213 118.5(6) . . ? N222 C223 C224 121.2(6) . . ? N222 C223 C227 117.1(5) . . ? C224 C223 C227 121.6(6) . . ? C225 C224 C223 119.6(6) . . ? C225 C224 H1D 120.2(4) . . ? C223 C224 H1D 120.2(4) . . ? C226 C225 C224 119.1(6) . . ? C226 C225 H8D 120.5(4) . . ? C224 C225 H8D 120.5(4) . . ? C225 C226 C221 119.0(6) . . ? C225 C226 H15A 120.5(4) . . ? C221 C226 H15A 120.5(4) . . ? C223 C227 H92A 109.5(3) . . ? C223 C227 H92B 109.5(4) . . ? H92A C227 H92B 109.5 . . ? C223 C227 H92C 109.5(3) . . ? H92A C227 H92C 109.5 . . ? H92B C227 H92C 109.5 . . ? N232 C233 C234 109.6(5) . . ? N232 C233 C241 120.1(6) . . ? C234 C233 C241 130.3(6) . . ? C235 C234 C233 105.4(6) . . ? C235 C234 H7A 127.3(4) . . ? C233 C234 H7A 127.3(4) . . ? N231 C235 C234 109.3(6) . . ? N231 C235 H26A 125.4(3) . . ? C234 C235 H26A 125.4(4) . . ? N242 C241 C246 122.5(6) . . ? N242 C241 C233 117.6(6) . . ? C246 C241 C233 119.8(6) . . ? N242 C243 C244 121.5(7) . . ? N242 C243 C247 118.6(6) . . ? C244 C243 C247 119.8(7) . . ? C245 C244 C243 120.0(7) . . ? C245 C244 H4A 120.0(4) . . ? C243 C244 H4A 120.0(5) . . ? C244 C245 C246 119.5(7) . . ? C244 C245 H3B 120.2(4) . . ? C246 C245 H3B 120.2(5) . . ? C245 C246 C241 118.3(7) . . ? C245 C246 H7D 120.9(5) . . ? C241 C246 H7D 120.9(4) . . ? C243 C247 H93A 109.5(4) . . ? C243 C247 H93B 109.5(4) . . ? H93A C247 H93B 109.5 . . ? C243 C247 H93C 109.5(3) . . ? H93A C247 H93C 109.5 . . ? H93B C247 H93C 109.5 . . ? N252 C253 C254 110.1(5) . . ? N252 C253 C261 123.8(5) . . ? C254 C253 C261 126.1(5) . . ? C256 C254 C253 105.2(5) . . ? C256 C254 H13A 127.4(3) . . ? C253 C254 H13A 127.4(3) . . ? N251 C256 C254 107.9(5) . . ? N251 C256 H19B 126.0(3) . . ? C254 C256 H19B 126.0(3) . . ? N262 C261 C266 121.9(5) . . ? N262 C261 C253 117.9(5) . . ? C266 C261 C253 120.2(5) . . ? N262 C263 C264 121.5(5) . . ? N262 C263 C267 117.1(5) . . ? C264 C263 C267 121.4(6) . . ? C265 C264 C263 119.2(6) . . ? C265 C264 H11B 120.4(4) . . ? C263 C264 H11B 120.4(4) . . ? C266 C265 C264 119.3(6) . . ? C266 C265 H16A 120.4(4) . . ? C264 C265 H16A 120.4(4) . . ? C265 C266 C261 119.4(6) . . ? C265 C266 H18B 120.3(4) . . ? C261 C266 H18B 120.3(4) . . ? C263 C267 H90A 109.5(3) . . ? C263 C267 H90B 109.5(3) . . ? H90A C267 H90B 109.5 . . ? C263 C267 H90C 109.5(4) . . ? H90A C267 H90C 109.5 . . ? H90B C267 H90C 109.5 . . ? N231 B2 N211 109.8(5) . . ? N231 B2 N251 110.8(5) . . ? N211 B2 N251 109.5(5) . . ? N231 B2 H2 108.9(3) . . ? N211 B2 H2 108.9(3) . . ? N251 B2 H2 108.9(3) . . ? _refine_diff_density_max 1.649 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.129 #=END data_choc _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H54 B2 Gd2 N22 O14' _chemical_formula_weight 1571.31 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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 10.870(2) _cell_length_b 16.4827(13) _cell_length_c 18.996(2) _cell_angle_alpha 70.356(7) _cell_angle_beta 82.054(8) _cell_angle_gamma 73.900(13) _cell_volume 3076.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method ? _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.64 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31882 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13905 _reflns_number_observed 11633 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0334P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13905 _refine_ls_number_parameters 853 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_obs 0.0226 _refine_ls_wR_factor_all 0.0579 _refine_ls_wR_factor_obs 0.0557 _refine_ls_goodness_of_fit_all 0.916 _refine_ls_goodness_of_fit_obs 0.971 _refine_ls_restrained_S_all 0.916 _refine_ls_restrained_S_obs 0.971 _refine_ls_shift/esd_max 0.143 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Gd1 Gd 0.049257(11) 0.244055(7) 0.039413(6) 0.01932(3) Uani 1 d . . Gd2 Gd 0.296178(12) 0.275286(8) 0.466772(6) 0.02544(4) Uani 1 d . . B1 B -0.2183(3) 0.3101(2) -0.0875(2) 0.0334(7) Uani 1 d . . H1 H -0.2923(3) 0.3233(2) -0.1189(2) 0.040 Uiso 1 calc R . B2 B 0.0070(3) 0.1921(2) 0.5083(2) 0.0291(6) Uani 1 d . . H2 H -0.0736(3) 0.1711(2) 0.5189(2) 0.035 Uiso 1 calc R . N11 N -0.0227(2) 0.18195(13) -0.04471(10) 0.0244(4) Uani 1 d . . N12 N -0.1285(2) 0.21831(14) -0.08592(11) 0.0277(5) Uani 1 d . . C13 C -0.1338(3) 0.1668(2) -0.12705(13) 0.0310(6) Uani 1 d . . H13B H -0.1988(3) 0.1785(2) -0.16041(13) 0.037 Uiso 1 calc R . C14 C -0.0304(3) 0.0949(2) -0.11281(13) 0.0288(6) Uani 1 d . . H14G H -0.0095(3) 0.0474(2) -0.13340(13) 0.035 Uiso 1 calc R . C15 C 0.0382(2) 0.10684(15) -0.06107(12) 0.0233(5) Uani 1 d . . N21 N 0.2072(2) 0.07162(12) 0.02347(10) 0.0239(4) Uani 1 d . . C22 C 0.1579(2) 0.0495(2) -0.02753(13) 0.0243(5) Uani 1 d . . C23 C 0.2173(3) -0.0257(2) -0.04922(14) 0.0298(6) Uani 1 d . . H23A H 0.1811(3) -0.0384(2) -0.08587(14) 0.036 Uiso 1 calc R . C24 C 0.3286(3) -0.0813(2) -0.0171(2) 0.0354(6) Uani 1 d . . H24A H 0.3696(3) -0.1334(2) -0.0303(2) 0.042 Uiso 1 calc R . C25 C 0.3793(3) -0.0597(2) 0.03462(15) 0.0328(6) Uani 1 d . . H25A H 0.4566(3) -0.0968(2) 0.05715(15) 0.039 Uiso 1 calc R . C26 C 0.3178(2) 0.0163(2) 0.05404(13) 0.0271(5) Uani 1 d . . C27 C 0.3759(3) 0.0362(2) 0.11190(14) 0.0333(6) Uani 1 d . . H27A H 0.3699(16) 0.1001(2) 0.0969(5) 0.050 Uiso 1 calc R . H27B H 0.4662(5) 0.0033(9) 0.1162(7) 0.050 Uiso 1 calc R . H27C H 0.3296(11) 0.0180(11) 0.1603(3) 0.050 Uiso 1 calc R . N31 N -0.1868(2) 0.29502(13) 0.04585(11) 0.0257(4) Uani 1 d . . N32 N -0.2684(2) 0.30673(14) -0.00694(12) 0.0301(5) Uani 1 d . . C33 C -0.3873(3) 0.3106(2) 0.0241(2) 0.0365(6) Uani 1 d . . H33A H -0.4611(3) 0.3181(2) -0.0012(2) 0.044 Uiso 1 calc R . C34 C -0.3858(3) 0.3020(2) 0.0985(2) 0.0347(6) Uani 1 d . . H34A H -0.4560(3) 0.3022(2) 0.1344(2) 0.042 Uiso 1 calc R . C35 C -0.2578(2) 0.2930(2) 0.10942(14) 0.0272(5) Uani 1 d . . N41 N -0.0688(2) 0.28417(12) 0.16511(10) 0.0245(4) Uani 1 d . . C42 C -0.1943(3) 0.2866(2) 0.17557(13) 0.0276(5) Uani 1 d . . C43 C -0.2630(3) 0.2883(2) 0.24241(15) 0.0408(7) Uani 1 d . . H43A H -0.3508(3) 0.2873(2) 0.24890(15) 0.049 Uiso 1 calc R . C44 C -0.1991(4) 0.2913(2) 0.2998(2) 0.0504(9) Uani 1 d . . H44A H -0.2427(4) 0.2918(2) 0.3466(2) 0.060 Uiso 1 calc R . C45 C -0.0734(3) 0.2936(2) 0.28817(15) 0.0441(8) Uani 1 d . . H45A H -0.0301(3) 0.2980(2) 0.32635(15) 0.053 Uiso 1 calc R . C46 C -0.0078(3) 0.2894(2) 0.22020(13) 0.0313(6) Uani 1 d . . C47 C 0.1289(3) 0.2937(2) 0.2065(2) 0.0389(7) Uani 1 d . . H47A H 0.1691(6) 0.2662(11) 0.1679(8) 0.058 Uiso 1 calc R . H47B H 0.1740(5) 0.2618(11) 0.2530(3) 0.058 Uiso 1 calc R . H47C H 0.1333(3) 0.3560(2) 0.1897(10) 0.058 Uiso 1 calc R . N51 N -0.0284(2) 0.37526(13) -0.09521(11) 0.0297(5) Uani 1 d . . N52 N -0.1418(2) 0.38050(14) -0.12217(11) 0.0340(5) Uani 1 d . . C53 C -0.1575(4) 0.4439(2) -0.1908(2) 0.0504(9) Uani 1 d . . H53A H -0.2290(4) 0.4604(2) -0.2208(2) 0.061 Uiso 1 calc R . C54 C -0.0536(4) 0.4795(2) -0.2091(2) 0.0497(9) Uani 1 d . . H54A H -0.0381(4) 0.5245(2) -0.2537(2) 0.060 Uiso 1 calc R . C55 C 0.0251(3) 0.4359(2) -0.14873(14) 0.0373(7) Uani 1 d . . N61 N 0.1744(2) 0.45862(13) -0.07800(12) 0.0334(5) Uani 1 d . . C62 C 0.1491(3) 0.4520(2) -0.1428(2) 0.0400(7) Uani 1 d . . C63 C 0.2386(4) 0.4624(2) -0.2037(2) 0.0611(10) Uani 1 d . . H63A H 0.2213(4) 0.4586(2) -0.2500(2) 0.073 Uiso 1 calc R . C64 C 0.3527(4) 0.4783(3) -0.1946(2) 0.0752(13) Uani 1 d . . H64A H 0.4144(4) 0.4858(3) -0.2353(2) 0.090 Uiso 1 calc R . C65 C 0.3785(4) 0.4835(2) -0.1275(2) 0.0607(10) Uani 1 d . . H65A H 0.4573(4) 0.4942(2) -0.1216(2) 0.073 Uiso 1 calc R . C66 C 0.2876(3) 0.4729(2) -0.0693(2) 0.0418(7) Uani 1 d . . C67 C 0.3077(3) 0.4754(2) 0.0059(2) 0.0463(8) Uani 1 d . . H67A H 0.2329(9) 0.5157(11) 0.0219(5) 0.069 Uiso 1 calc R . H67B H 0.3844(12) 0.4967(13) 0.0033(3) 0.069 Uiso 1 calc R . H67C H 0.3188(21) 0.4156(3) 0.0420(3) 0.069 Uiso 1 calc R . N71 N 0.3062(2) 0.25349(13) -0.02682(11) 0.0255(4) Uani 1 d . . O72 O 0.4151(2) 0.25246(13) -0.05386(11) 0.0381(4) Uani 1 d . . O73 O 0.2175(2) 0.25411(11) -0.06391(9) 0.0271(4) Uani 1 d . . O74 O 0.2760(2) 0.25412(11) 0.04031(9) 0.0282(4) Uani 1 d . . N81 N 0.0567(2) 0.08989(13) 0.17261(11) 0.0292(5) Uani 1 d . . O82 O 0.0656(2) 0.02187(13) 0.22626(11) 0.0521(6) Uani 1 d . . O83 O 0.1363(2) 0.13645(10) 0.15968(9) 0.0250(4) Uani 1 d . . O84 O -0.0315(2) 0.11571(11) 0.12645(9) 0.0278(4) Uani 1 d . . O91 O 0.0429(2) 0.38819(10) 0.04276(9) 0.0275(4) Uani 1 d . . N111 N 0.2188(2) 0.15646(13) 0.43285(11) 0.0261(4) Uani 1 d . . N112 N 0.0953(2) 0.14970(13) 0.45256(12) 0.0280(5) Uani 1 d . . C113 C 0.0636(3) 0.1016(2) 0.4161(2) 0.0344(6) Uani 1 d . . H11B H -0.0170(3) 0.0877(2) 0.4208(2) 0.041 Uiso 1 calc R . C114 C 0.1662(3) 0.0760(2) 0.3712(2) 0.0353(6) Uani 1 d . . H11A H 0.1712(3) 0.0421(2) 0.3387(2) 0.042 Uiso 1 calc R . C115 C 0.2621(3) 0.1104(2) 0.38369(13) 0.0278(5) Uani 1 d . . N121 N 0.4912(2) 0.08476(14) 0.39167(11) 0.0295(5) Uani 1 d . . C122 C 0.3926(3) 0.0999(2) 0.34852(14) 0.0282(5) Uani 1 d . . C123 C 0.4121(3) 0.1036(2) 0.27395(15) 0.0373(7) Uani 1 d . . H12B H 0.3418(3) 0.1121(2) 0.24531(15) 0.045 Uiso 1 calc R . C124 C 0.5351(3) 0.0946(2) 0.2419(2) 0.0422(7) Uani 1 d . . H12D H 0.5505(3) 0.0971(2) 0.1909(2) 0.051 Uiso 1 calc R . C125 C 0.6351(3) 0.0820(2) 0.2848(2) 0.0377(6) Uani 1 d . . H12C H 0.7200(3) 0.0773(2) 0.2632(2) 0.045 Uiso 1 calc R . C126 C 0.6108(3) 0.0764(2) 0.35968(15) 0.0326(6) Uani 1 d . . C127 C 0.7166(3) 0.0601(2) 0.4096(2) 0.0466(8) Uani 1 d . . H12E H 0.7142(13) 0.0076(9) 0.4532(6) 0.070 Uiso 1 calc R . H12F H 0.7053(12) 0.1120(6) 0.4263(10) 0.070 Uiso 1 calc R . H12G H 0.7995(3) 0.0501(14) 0.3819(4) 0.070 Uiso 1 calc R . N131 N 0.0673(2) 0.33845(14) 0.45651(11) 0.0294(5) Uani 1 d . . N132 N -0.0272(2) 0.29482(14) 0.47574(11) 0.0281(5) Uani 1 d . . C133 C -0.1422(3) 0.3535(2) 0.46277(14) 0.0349(6) Uani 1 d . . H13C H -0.2230(3) 0.3392(2) 0.47209(14) 0.042 Uiso 1 calc R . C134 C -0.1226(3) 0.4379(2) 0.43365(14) 0.0379(7) Uani 1 d . . H13A H -0.1857(3) 0.4926(2) 0.41877(14) 0.046 Uiso 1 calc R . C135 C 0.0099(3) 0.4257(2) 0.43075(13) 0.0321(6) Uani 1 d . . N141 N 0.2171(3) 0.45969(15) 0.40739(11) 0.0364(6) Uani 1 d . . C142 C 0.0885(3) 0.4912(2) 0.40528(13) 0.0357(7) Uani 1 d . . C143 C 0.0279(4) 0.5811(2) 0.3794(2) 0.0484(8) Uani 1 d . . H14F H -0.0629(4) 0.6005(2) 0.3787(2) 0.058 Uiso 1 calc R . C144 C 0.1030(5) 0.6415(2) 0.3546(2) 0.0601(11) Uani 1 d . . H14A H 0.0646(5) 0.7036(2) 0.3370(2) 0.072 Uiso 1 calc R . C145 C 0.2338(4) 0.6105(2) 0.3558(2) 0.0569(10) Uani 1 d . . H14E H 0.2866(4) 0.6512(2) 0.3382(2) 0.068 Uiso 1 calc R . C146 C 0.2895(4) 0.5197(2) 0.38250(15) 0.0454(8) Uani 1 d . . C147 C 0.4324(4) 0.4874(2) 0.3831(2) 0.0632(10) Uani 1 d . . H14B H 0.4602(4) 0.4373(11) 0.3630(13) 0.095 Uiso 1 calc R . H14C H 0.4594(4) 0.4680(15) 0.4345(3) 0.095 Uiso 1 calc R . H14D H 0.4713(4) 0.5356(5) 0.3521(11) 0.095 Uiso 1 calc R . N151 N 0.1856(2) 0.18482(14) 0.58647(11) 0.0274(5) Uani 1 d . . N152 N 0.0753(2) 0.16332(14) 0.58139(11) 0.0282(5) Uani 1 d . . C153 C 0.0323(3) 0.1189(2) 0.64993(15) 0.0354(6) Uani 1 d . . H15B H -0.0417(3) 0.0960(2) 0.66062(15) 0.042 Uiso 1 calc R . C154 C 0.1140(3) 0.1127(2) 0.70103(15) 0.0374(7) Uani 1 d . . H15A H 0.1074(3) 0.0859(2) 0.75372(15) 0.045 Uiso 1 calc R . C155 C 0.2091(3) 0.1537(2) 0.66000(14) 0.0311(6) Uani 1 d . . N161 N 0.4332(2) 0.15204(15) 0.65555(12) 0.0322(5) Uani 1 d . . C162 C 0.3173(3) 0.1650(2) 0.69136(14) 0.0328(6) Uani 1 d . . C163 C 0.2968(3) 0.1879(2) 0.7567(2) 0.0467(8) Uani 1 d . . H16G H 0.2141(3) 0.1957(2) 0.7813(2) 0.056 Uiso 1 calc R . C164 C 0.3983(3) 0.1991(2) 0.7855(2) 0.0538(9) Uani 1 d . . H16B H 0.3864(3) 0.2154(2) 0.8299(2) 0.065 Uiso 1 calc R . C165 C 0.5164(3) 0.1865(2) 0.7491(2) 0.0509(8) Uani 1 d . . H16F H 0.5875(3) 0.1935(2) 0.7685(2) 0.061 Uiso 1 calc R . C166 C 0.5324(3) 0.1633(2) 0.6835(2) 0.0389(7) Uani 1 d . . C167 C 0.6586(3) 0.1517(2) 0.6405(2) 0.0534(8) Uani 1 d . . H16C H 0.6739(10) 0.0990(9) 0.6243(11) 0.080 Uiso 1 calc R . H16D H 0.7270(4) 0.1441(15) 0.6724(4) 0.080 Uiso 1 calc R . H16E H 0.6575(8) 0.2043(7) 0.5965(7) 0.080 Uiso 1 calc R . N171 N 0.3776(2) 0.32653(15) 0.31003(12) 0.0349(5) Uani 1 d . . O172 O 0.4103(2) 0.3559(2) 0.24473(11) 0.0587(7) Uani 1 d . . O173 O 0.2615(2) 0.32912(12) 0.33129(9) 0.0343(4) Uani 1 d . . O174 O 0.4580(2) 0.29154(13) 0.36184(10) 0.0387(5) Uani 1 d . . N181 N 0.3812(3) 0.3501(2) 0.56247(14) 0.0473(7) Uani 1 d . . O182 O 0.4159(3) 0.3829(2) 0.60255(15) 0.0751(8) Uani 1 d . . O183 O 0.4584(2) 0.31844(15) 0.51562(12) 0.0477(5) Uani 1 d . . O184 O 0.2664(2) 0.34552(13) 0.56511(10) 0.0398(5) Uani 1 d . . O191 O 0.4593(2) 0.14664(13) 0.51074(10) 0.0371(4) Uani 1 d . . H191 H 0.4620 0.1297 0.5614 0.050 Uiso 1 d . . H91B H 0.0826 0.4203 0.0000 0.050 Uiso 1 d . . H192 H 0.4614 0.1129 0.5013 0.050 Uiso 1 d . . H91A H 0.0000 0.4224 0.0600 0.050 Uiso 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 0.02173(6) 0.01804(6) 0.01982(6) -0.00771(4) -0.00192(4) -0.00486(5) Gd2 0.02832(7) 0.02979(7) 0.02315(6) -0.01093(5) 0.00192(5) -0.01327(6) B1 0.030(2) 0.037(2) 0.037(2) -0.0197(13) -0.0175(13) 0.0030(14) B2 0.027(2) 0.0294(15) 0.0327(15) -0.0095(12) 0.0005(12) -0.0107(13) N11 0.0263(11) 0.0241(10) 0.0249(10) -0.0113(8) -0.0035(8) -0.0040(9) N12 0.0298(12) 0.0317(11) 0.0277(11) -0.0163(9) -0.0078(9) -0.0055(9) C13 0.037(2) 0.0391(15) 0.0248(12) -0.0155(11) -0.0031(11) -0.0143(12) C14 0.037(2) 0.0308(13) 0.0263(12) -0.0166(10) 0.0060(11) -0.0147(12) C15 0.0297(13) 0.0217(11) 0.0220(11) -0.0101(9) 0.0045(10) -0.0108(10) N21 0.0272(11) 0.0208(10) 0.0246(10) -0.0084(8) 0.0015(8) -0.0071(9) C22 0.0292(13) 0.0222(11) 0.0244(12) -0.0093(9) 0.0054(10) -0.0119(10) C23 0.0344(15) 0.0267(13) 0.0325(13) -0.0157(10) 0.0053(11) -0.0095(11) C24 0.039(2) 0.0242(13) 0.045(2) -0.0187(12) 0.0082(13) -0.0057(12) C25 0.0289(14) 0.0253(13) 0.0402(15) -0.0105(11) 0.0019(11) -0.0020(11) C26 0.0278(14) 0.0237(12) 0.0292(13) -0.0079(10) 0.0030(10) -0.0082(10) C27 0.0311(15) 0.0315(14) 0.0357(14) -0.0122(11) -0.0055(11) -0.0012(12) N31 0.0261(11) 0.0271(11) 0.0255(10) -0.0124(8) -0.0047(8) -0.0024(9) N32 0.0244(12) 0.0318(12) 0.0370(12) -0.0176(9) -0.0105(9) 0.0013(9) C33 0.0237(14) 0.0337(15) 0.060(2) -0.0259(13) -0.0095(13) -0.0015(12) C34 0.0260(14) 0.0328(14) 0.047(2) -0.0185(12) 0.0025(12) -0.0054(12) C35 0.0254(13) 0.0228(12) 0.0333(13) -0.0110(10) 0.0008(10) -0.0039(10) N41 0.0349(12) 0.0192(10) 0.0210(10) -0.0081(8) -0.0043(8) -0.0055(9) C42 0.0343(15) 0.0210(12) 0.0253(12) -0.0088(9) 0.0005(10) -0.0026(11) C43 0.044(2) 0.038(2) 0.0332(15) -0.0120(12) 0.0078(12) -0.0027(14) C44 0.071(2) 0.049(2) 0.0226(14) -0.0132(13) 0.0054(14) -0.002(2) C45 0.068(2) 0.036(2) 0.0253(14) -0.0141(12) -0.0118(14) 0.001(2) C46 0.048(2) 0.0189(12) 0.0264(13) -0.0081(10) -0.0107(11) -0.0019(12) C47 0.050(2) 0.0300(14) 0.044(2) -0.0158(12) -0.0220(14) -0.0060(13) N51 0.0364(13) 0.0260(11) 0.0240(10) -0.0085(8) -0.0041(9) -0.0015(10) N52 0.0468(15) 0.0258(11) 0.0257(11) -0.0095(9) -0.0120(10) 0.0034(10) C53 0.086(3) 0.031(2) 0.0298(15) -0.0104(12) -0.028(2) 0.006(2) C54 0.091(3) 0.0289(15) 0.0255(14) -0.0023(11) -0.011(2) -0.013(2) C55 0.060(2) 0.0225(13) 0.0246(13) -0.0085(10) 0.0008(12) -0.0025(13) N61 0.0369(13) 0.0181(10) 0.0393(13) -0.0072(9) 0.0102(10) -0.0053(9) C62 0.054(2) 0.0187(12) 0.039(2) -0.0047(11) 0.0127(13) -0.0074(13) C63 0.083(3) 0.053(2) 0.041(2) -0.014(2) 0.022(2) -0.020(2) C64 0.073(3) 0.064(3) 0.075(3) -0.013(2) 0.043(2) -0.029(2) C65 0.049(2) 0.041(2) 0.086(3) -0.019(2) 0.025(2) -0.017(2) C66 0.032(2) 0.0178(12) 0.066(2) -0.0074(12) 0.0119(14) -0.0046(11) C67 0.032(2) 0.034(2) 0.075(2) -0.0200(15) -0.0021(15) -0.0091(13) N71 0.0259(11) 0.0167(9) 0.0339(11) -0.0090(8) -0.0009(9) -0.0040(8) O72 0.0225(10) 0.0481(12) 0.0500(12) -0.0246(9) 0.0046(8) -0.0102(9) O73 0.0269(10) 0.0266(9) 0.0292(9) -0.0084(7) -0.0030(7) -0.0088(7) O74 0.0286(10) 0.0288(9) 0.0308(9) -0.0140(7) -0.0017(7) -0.0070(8) N81 0.0434(14) 0.0244(10) 0.0229(10) -0.0090(8) -0.0018(9) -0.0113(10) O82 0.090(2) 0.0376(11) 0.0313(11) 0.0084(9) -0.0181(11) -0.0366(12) O83 0.0289(10) 0.0220(8) 0.0261(8) -0.0081(7) -0.0041(7) -0.0075(7) O84 0.0319(10) 0.0270(9) 0.0297(9) -0.0112(7) -0.0030(7) -0.0120(8) O91 0.0334(10) 0.0196(8) 0.0298(9) -0.0092(7) 0.0027(7) -0.0072(7) N111 0.0262(11) 0.0273(11) 0.0274(10) -0.0100(8) -0.0034(8) -0.0082(9) N112 0.0267(12) 0.0256(11) 0.0343(11) -0.0110(9) -0.0039(9) -0.0073(9) C113 0.0315(15) 0.0324(14) 0.047(2) -0.0168(12) -0.0105(12) -0.0099(12) C114 0.037(2) 0.0307(14) 0.045(2) -0.0196(12) -0.0120(13) -0.0045(12) C115 0.0321(14) 0.0245(12) 0.0281(13) -0.0097(10) -0.0070(11) -0.0046(11) N121 0.0325(13) 0.0274(11) 0.0297(11) -0.0106(9) -0.0039(9) -0.0059(10) C122 0.0322(14) 0.0227(12) 0.0305(13) -0.0110(10) -0.0061(11) -0.0026(11) C123 0.042(2) 0.039(2) 0.0323(14) -0.0181(12) -0.0087(12) 0.0006(13) C124 0.049(2) 0.044(2) 0.0314(15) -0.0177(13) 0.0002(13) -0.0032(14) C125 0.035(2) 0.037(2) 0.041(2) -0.0172(12) 0.0058(12) -0.0067(13) C126 0.0299(15) 0.0292(13) 0.0388(15) -0.0120(11) -0.0028(11) -0.0052(11) C127 0.035(2) 0.058(2) 0.050(2) -0.020(2) -0.0050(14) -0.0103(15) N131 0.0362(13) 0.0263(11) 0.0253(11) -0.0100(8) 0.0012(9) -0.0060(10) N132 0.0278(12) 0.0304(11) 0.0264(11) -0.0103(9) 0.0007(9) -0.0072(9) C133 0.032(2) 0.043(2) 0.0306(14) -0.0180(12) -0.0030(11) -0.0029(13) C134 0.047(2) 0.0321(14) 0.0314(14) -0.0128(11) -0.0074(12) 0.0018(13) C135 0.047(2) 0.0279(13) 0.0208(12) -0.0103(10) -0.0008(11) -0.0056(12) N141 0.063(2) 0.0299(12) 0.0241(11) -0.0117(9) 0.0036(11) -0.0218(12) C142 0.061(2) 0.0293(14) 0.0179(12) -0.0110(10) 0.0031(12) -0.0113(14) C143 0.076(2) 0.0305(15) 0.035(2) -0.0120(12) 0.0026(15) -0.008(2) C144 0.112(4) 0.027(2) 0.042(2) -0.0124(13) 0.006(2) -0.020(2) C145 0.105(3) 0.042(2) 0.038(2) -0.0184(14) 0.015(2) -0.043(2) C146 0.077(2) 0.043(2) 0.0284(14) -0.0167(12) 0.0101(14) -0.032(2) C147 0.079(3) 0.056(2) 0.068(2) -0.020(2) 0.016(2) -0.046(2) N151 0.0284(12) 0.0298(11) 0.0244(10) -0.0083(8) 0.0014(9) -0.0093(9) N152 0.0254(11) 0.0281(11) 0.0291(11) -0.0061(9) 0.0035(9) -0.0095(9) C153 0.0318(15) 0.0330(14) 0.0336(14) -0.0020(11) 0.0066(11) -0.0102(12) C154 0.036(2) 0.038(2) 0.0268(13) -0.0020(11) 0.0043(11) -0.0051(13) C155 0.0316(15) 0.0311(14) 0.0265(13) -0.0076(10) 0.0018(11) -0.0048(11) N161 0.0307(13) 0.0356(12) 0.0305(11) -0.0120(9) -0.0045(9) -0.0053(10) C162 0.035(2) 0.0349(14) 0.0240(12) -0.0065(11) -0.0018(11) -0.0047(12) C163 0.043(2) 0.064(2) 0.0311(15) -0.0193(14) -0.0012(13) -0.005(2) C164 0.057(2) 0.072(2) 0.033(2) -0.025(2) -0.0118(15) -0.003(2) C165 0.050(2) 0.059(2) 0.047(2) -0.018(2) -0.023(2) -0.005(2) C166 0.035(2) 0.038(2) 0.042(2) -0.0133(13) -0.0089(13) -0.0018(13) C167 0.033(2) 0.062(2) 0.072(2) -0.033(2) -0.004(2) -0.007(2) N171 0.0376(14) 0.0376(13) 0.0286(12) -0.0126(10) 0.0066(10) -0.0093(11) O172 0.0523(15) 0.079(2) 0.0271(11) -0.0046(10) 0.0124(10) -0.0107(13) O173 0.0359(11) 0.0450(11) 0.0286(9) -0.0167(8) 0.0032(8) -0.0161(9) O174 0.0323(11) 0.0457(12) 0.0343(10) -0.0101(9) 0.0034(8) -0.0091(9) N181 0.068(2) 0.0384(14) 0.0454(15) -0.0146(12) -0.0169(14) -0.0207(14) O182 0.106(2) 0.067(2) 0.080(2) -0.0392(14) -0.035(2) -0.030(2) O183 0.0478(14) 0.0546(13) 0.0512(13) -0.0181(11) -0.0057(10) -0.0257(11) O184 0.0543(14) 0.0380(11) 0.0330(10) -0.0155(8) -0.0042(9) -0.0147(10) O191 0.0390(12) 0.0416(11) 0.0373(10) -0.0212(9) -0.0035(8) -0.0083(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 Gd1 O91 2.380(2) . ? Gd1 N31 2.468(2) . ? Gd1 N11 2.471(2) . ? Gd1 O73 2.486(2) . ? Gd1 O83 2.490(2) . ? Gd1 O84 2.501(2) . ? Gd1 O74 2.518(2) . ? Gd1 N41 2.744(2) . ? Gd1 N51 2.792(2) . ? Gd1 N81 2.913(2) . ? Gd1 N71 2.923(2) . ? Gd1 N21 2.974(2) . ? Gd2 O191 2.339(2) . ? Gd2 N131 2.424(2) . ? Gd2 O184 2.452(2) . ? Gd2 O183 2.463(2) . ? Gd2 O174 2.464(2) . ? Gd2 O173 2.470(2) . ? Gd2 N151 2.607(2) . ? Gd2 N111 2.621(2) . ? Gd2 N141 2.786(2) . ? Gd2 N181 2.878(2) . ? Gd2 N171 2.891(2) . ? B1 N52 1.531(4) . ? B1 N32 1.539(4) . ? B1 N12 1.550(4) . ? B2 N112 1.540(4) . ? B2 N152 1.534(4) . ? B2 N132 1.549(3) . ? N11 C15 1.347(3) . ? N11 N12 1.358(3) . ? N12 C13 1.350(3) . ? C13 C14 1.367(4) . ? C14 C15 1.405(3) . ? C15 C22 1.461(3) . ? N21 C22 1.359(3) . ? N21 C26 1.358(3) . ? C22 C23 1.397(3) . ? C23 C24 1.374(4) . ? C24 C25 1.374(4) . ? C25 C26 1.389(3) . ? C26 C27 1.505(4) . ? N31 C35 1.335(3) . ? N31 N32 1.361(3) . ? N32 C33 1.338(3) . ? C33 C34 1.374(4) . ? C34 C35 1.395(4) . ? C35 C42 1.475(3) . ? N41 C42 1.343(3) . ? N41 C46 1.351(3) . ? C42 C43 1.385(4) . ? C43 C44 1.392(4) . ? C44 C45 1.362(5) . ? C45 C46 1.399(4) . ? C46 C47 1.490(4) . ? N51 C55 1.359(3) . ? N51 N52 1.369(3) . ? N52 C53 1.367(3) . ? C53 C54 1.366(5) . ? C54 C55 1.393(4) . ? C55 C62 1.470(4) . ? N61 C62 1.342(4) . ? N61 C66 1.357(4) . ? C62 C63 1.401(4) . ? C63 C64 1.381(6) . ? C64 C65 1.377(5) . ? C65 C66 1.376(4) . ? C66 C67 1.490(4) . ? N71 O72 1.222(3) . ? N71 O73 1.266(3) . ? N71 O74 1.275(3) . ? N81 O82 1.226(2) . ? N81 O83 1.257(3) . ? N81 O84 1.274(3) . ? N111 C115 1.352(3) . ? N111 N112 1.368(3) . ? N112 C113 1.348(3) . ? C113 C114 1.366(4) . ? C114 C115 1.398(4) . ? C115 C122 1.472(4) . ? N121 C126 1.348(3) . ? N121 C122 1.356(3) . ? C122 C123 1.386(3) . ? C123 C124 1.381(4) . ? C124 C125 1.376(4) . ? C125 C126 1.387(4) . ? C126 C127 1.501(4) . ? N131 C135 1.345(3) . ? N131 N132 1.355(3) . ? N132 C133 1.346(3) . ? C133 C134 1.379(4) . ? C134 C135 1.394(4) . ? C135 C142 1.476(4) . ? N141 C142 1.351(4) . ? N141 C146 1.354(4) . ? C142 C143 1.388(4) . ? C143 C144 1.382(5) . ? C144 C145 1.372(5) . ? C145 C146 1.391(5) . ? C146 C147 1.497(5) . ? N151 C155 1.350(3) . ? N151 N152 1.365(3) . ? N152 C153 1.353(3) . ? C153 C154 1.364(4) . ? C154 C155 1.395(4) . ? C155 C162 1.469(4) . ? N161 C162 1.345(3) . ? N161 C166 1.347(4) . ? C162 C163 1.388(4) . ? C163 C164 1.377(5) . ? C164 C165 1.368(5) . ? C165 C166 1.399(4) . ? C166 C167 1.495(4) . ? N171 O172 1.212(3) . ? N171 O173 1.265(3) . ? N171 O174 1.281(3) . ? N181 O182 1.217(3) . ? N181 O184 1.264(3) . ? N181 O183 1.277(3) . ? 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 O91 Gd1 N31 84.48(6) . . ? O91 Gd1 N11 136.52(6) . . ? N31 Gd1 N11 75.19(7) . . ? O91 Gd1 O73 91.79(6) . . ? N31 Gd1 O73 134.56(6) . . ? N11 Gd1 O73 77.06(6) . . ? O91 Gd1 O83 106.70(6) . . ? N31 Gd1 O83 112.75(6) . . ? N11 Gd1 O83 116.53(6) . . ? O73 Gd1 O83 111.66(6) . . ? O91 Gd1 O84 134.16(5) . . ? N31 Gd1 O84 73.47(6) . . ? N11 Gd1 O84 75.94(6) . . ? O73 Gd1 O84 132.11(6) . . ? O83 Gd1 O84 51.18(5) . . ? O91 Gd1 O74 71.67(6) . . ? N31 Gd1 O74 156.02(6) . . ? N11 Gd1 O74 124.26(6) . . ? O73 Gd1 O74 51.17(5) . . ? O83 Gd1 O74 73.27(6) . . ? O84 Gd1 O74 121.92(6) . . ? O91 Gd1 N41 64.22(6) . . ? N31 Gd1 N41 61.76(6) . . ? N11 Gd1 N41 130.68(7) . . ? O73 Gd1 N41 151.57(6) . . ? O83 Gd1 N41 65.22(6) . . ? O84 Gd1 N41 69.94(6) . . ? O74 Gd1 N41 104.00(6) . . ? O91 Gd1 N51 68.30(6) . . ? N31 Gd1 N51 71.43(7) . . ? N11 Gd1 N51 68.88(6) . . ? O73 Gd1 N51 65.26(6) . . ? O83 Gd1 N51 173.56(6) . . ? O84 Gd1 N51 135.20(6) . . ? O74 Gd1 N51 100.91(6) . . ? N41 Gd1 N51 114.48(6) . . ? O91 Gd1 N81 123.61(6) . . ? N31 Gd1 N81 93.92(7) . . ? N11 Gd1 N81 96.18(6) . . ? O73 Gd1 N81 124.38(6) . . ? O83 Gd1 N81 25.39(5) . . ? O84 Gd1 N81 25.82(6) . . ? O74 Gd1 N81 97.23(6) . . ? N41 Gd1 N81 65.79(6) . . ? N51 Gd1 N81 161.01(7) . . ? O91 Gd1 N71 81.99(6) . . ? N31 Gd1 N71 154.37(6) . . ? N11 Gd1 N71 100.30(6) . . ? O73 Gd1 N71 25.47(5) . . ? O83 Gd1 N71 92.00(6) . . ? O84 Gd1 N71 130.66(6) . . ? O74 Gd1 N71 25.75(5) . . ? N41 Gd1 N71 128.92(6) . . ? N51 Gd1 N71 83.35(6) . . ? N81 Gd1 N71 111.69(6) . . ? O91 Gd1 N21 147.81(6) . . ? N31 Gd1 N21 127.54(6) . . ? N11 Gd1 N21 61.87(6) . . ? O73 Gd1 N21 64.22(5) . . ? O83 Gd1 N21 67.09(5) . . ? O84 Gd1 N21 68.26(5) . . ? O74 Gd1 N21 76.43(6) . . ? N41 Gd1 N21 129.65(5) . . ? N51 Gd1 N21 114.74(6) . . ? N81 Gd1 N21 64.28(5) . . ? N71 Gd1 N21 67.15(5) . . ? O191 Gd2 N131 146.21(7) . . ? O191 Gd2 O184 103.04(6) . . ? N131 Gd2 O184 83.25(7) . . ? O191 Gd2 O183 73.09(7) . . ? N131 Gd2 O183 130.76(7) . . ? O184 Gd2 O183 52.11(7) . . ? O191 Gd2 O174 78.04(7) . . ? N131 Gd2 O174 125.45(6) . . ? O184 Gd2 O174 125.46(7) . . ? O183 Gd2 O174 77.95(7) . . ? O191 Gd2 O173 117.10(6) . . ? N131 Gd2 O173 74.71(6) . . ? O184 Gd2 O173 135.04(6) . . ? O183 Gd2 O173 120.37(7) . . ? O174 Gd2 O173 51.83(6) . . ? O191 Gd2 N151 77.86(7) . . ? N131 Gd2 N151 73.25(7) . . ? O184 Gd2 N151 69.92(7) . . ? O183 Gd2 N151 104.03(7) . . ? O174 Gd2 N151 154.01(7) . . ? O173 Gd2 N151 135.40(6) . . ? O191 Gd2 N111 77.67(6) . . ? N131 Gd2 N111 76.95(7) . . ? O184 Gd2 N111 140.53(7) . . ? O183 Gd2 N111 150.64(7) . . ? O174 Gd2 N111 93.62(7) . . ? O173 Gd2 N111 71.35(6) . . ? N151 Gd2 N111 71.80(6) . . ? O191 Gd2 N141 149.72(7) . . ? N131 Gd2 N141 63.69(7) . . ? O184 Gd2 N141 69.09(6) . . ? O183 Gd2 N141 79.84(7) . . ? O174 Gd2 N141 83.35(7) . . ? O173 Gd2 N141 66.06(6) . . ? N151 Gd2 N141 122.63(7) . . ? N111 Gd2 N141 127.58(7) . . ? O191 Gd2 N181 88.22(7) . . ? N131 Gd2 N181 107.09(8) . . ? O184 Gd2 N181 25.89(7) . . ? O183 Gd2 N181 26.22(8) . . ? O174 Gd2 N181 101.98(8) . . ? O173 Gd2 N181 132.28(7) . . ? N151 Gd2 N181 86.86(7) . . ? N111 Gd2 N181 156.37(7) . . ? N141 Gd2 N181 72.45(7) . . ? O191 Gd2 N171 99.20(7) . . ? N131 Gd2 N171 99.60(7) . . ? O184 Gd2 N171 134.05(6) . . ? O183 Gd2 N171 98.67(7) . . ? O174 Gd2 N171 26.15(6) . . ? O173 Gd2 N171 25.78(6) . . ? N151 Gd2 N171 154.99(7) . . ? N111 Gd2 N171 83.28(6) . . ? N141 Gd2 N171 71.45(6) . . ? N181 Gd2 N171 118.02(7) . . ? N52 B1 N32 111.9(2) . . ? N52 B1 N12 108.1(2) . . ? N32 B1 N12 108.7(2) . . ? N112 B2 N152 109.3(2) . . ? N112 B2 N132 110.8(2) . . ? N152 B2 N132 109.3(2) . . ? C15 N11 N12 106.3(2) . . ? C15 N11 Gd1 126.6(2) . . ? N12 N11 Gd1 126.99(14) . . ? C13 N12 N11 110.0(2) . . ? C13 N12 B1 127.8(2) . . ? N11 N12 B1 122.0(2) . . ? N12 C13 C14 108.8(2) . . ? C13 C14 C15 104.9(2) . . ? N11 C15 C14 110.0(2) . . ? N11 C15 C22 122.2(2) . . ? C14 C15 C22 127.8(2) . . ? C22 N21 C26 117.0(2) . . ? C22 N21 Gd1 110.48(15) . . ? C26 N21 Gd1 132.4(2) . . ? N21 C22 C23 122.6(2) . . ? N21 C22 C15 118.7(2) . . ? C23 C22 C15 118.7(2) . . ? C24 C23 C22 119.4(2) . . ? C23 C24 C25 118.5(2) . . ? C24 C25 C26 120.2(3) . . ? N21 C26 C25 122.2(2) . . ? N21 C26 C27 119.6(2) . . ? C25 C26 C27 118.1(2) . . ? C35 N31 N32 106.5(2) . . ? C35 N31 Gd1 124.0(2) . . ? N32 N31 Gd1 127.36(15) . . ? C33 N32 N31 109.4(2) . . ? C33 N32 B1 129.8(2) . . ? N31 N32 B1 120.8(2) . . ? N32 C33 C34 109.2(2) . . ? C33 C34 C35 104.3(2) . . ? N31 C35 C34 110.5(2) . . ? N31 C35 C42 118.1(2) . . ? C34 C35 C42 131.3(2) . . ? C42 N41 C46 118.9(2) . . ? C42 N41 Gd1 115.37(15) . . ? C46 N41 Gd1 125.1(2) . . ? N41 C42 C43 122.9(2) . . ? N41 C42 C35 115.6(2) . . ? C43 C42 C35 121.4(3) . . ? C42 C43 C44 117.9(3) . . ? C45 C44 C43 119.4(3) . . ? C44 C45 C46 120.3(3) . . ? N41 C46 C45 120.4(3) . . ? N41 C46 C47 119.0(2) . . ? C45 C46 C47 120.5(3) . . ? C55 N51 N52 105.8(2) . . ? C55 N51 Gd1 135.3(2) . . ? N52 N51 Gd1 118.56(15) . . ? C53 N52 N51 109.5(3) . . ? C53 N52 B1 126.4(3) . . ? N51 N52 B1 122.6(2) . . ? N52 C53 C54 108.7(3) . . ? C53 C54 C55 105.5(3) . . ? N51 C55 C54 110.5(3) . . ? N51 C55 C62 124.1(2) . . ? C54 C55 C62 125.5(3) . . ? C62 N61 C66 121.2(2) . . ? N61 C62 C63 120.2(3) . . ? N61 C62 C55 118.7(2) . . ? C63 C62 C55 121.1(3) . . ? C64 C63 C62 118.1(4) . . ? C65 C64 C63 121.1(3) . . ? C64 C65 C66 118.6(4) . . ? N61 C66 C65 120.7(3) . . ? N61 C66 C67 116.7(2) . . ? C65 C66 C67 122.7(3) . . ? O72 N71 O73 121.9(2) . . ? O72 N71 O74 121.6(2) . . ? O73 N71 O74 116.5(2) . . ? O72 N71 Gd1 176.4(2) . . ? O73 N71 Gd1 57.60(11) . . ? O74 N71 Gd1 59.09(11) . . ? N71 O73 Gd1 96.94(13) . . ? N71 O74 Gd1 95.17(13) . . ? O82 N81 O83 121.3(2) . . ? O82 N81 O84 121.8(2) . . ? O83 N81 O84 116.8(2) . . ? O82 N81 Gd1 175.9(2) . . ? O83 N81 Gd1 58.16(10) . . ? O84 N81 Gd1 58.73(11) . . ? N81 O83 Gd1 96.45(13) . . ? N81 O84 Gd1 95.46(13) . . ? C115 N111 N112 105.4(2) . . ? C115 N111 Gd2 134.0(2) . . ? N112 N111 Gd2 118.58(15) . . ? C113 N112 N111 110.1(2) . . ? C113 N112 B2 125.8(2) . . ? N111 N112 B2 124.0(2) . . ? N112 C113 C114 108.8(2) . . ? C113 C114 C115 105.0(2) . . ? N111 C115 C114 110.6(2) . . ? N111 C115 C122 123.6(2) . . ? C114 C115 C122 125.9(2) . . ? C126 N121 C122 118.4(2) . . ? N121 C122 C123 122.0(3) . . ? N121 C122 C115 117.9(2) . . ? C123 C122 C115 120.0(2) . . ? C124 C123 C122 119.0(3) . . ? C125 C124 C123 119.3(3) . . ? C124 C125 C126 119.4(3) . . ? N121 C126 C125 121.9(3) . . ? N121 C126 C127 116.4(2) . . ? C125 C126 C127 121.7(3) . . ? C135 N131 N132 106.7(2) . . ? C135 N131 Gd2 125.4(2) . . ? N132 N131 Gd2 127.8(2) . . ? C133 N132 N131 110.0(2) . . ? C133 N132 B2 130.2(2) . . ? N131 N132 B2 119.8(2) . . ? N132 C133 C134 108.3(3) . . ? C133 C134 C135 105.1(2) . . ? N131 C135 C134 109.9(2) . . ? N131 C135 C142 119.7(3) . . ? C134 C135 C142 130.4(3) . . ? C142 N141 C146 117.5(3) . . ? C142 N141 Gd2 113.6(2) . . ? C146 N141 Gd2 128.8(2) . . ? N141 C142 C143 123.5(3) . . ? N141 C142 C135 117.5(2) . . ? C143 C142 C135 119.1(3) . . ? C144 C143 C142 118.3(4) . . ? C145 C144 C143 118.9(3) . . ? C144 C145 C146 120.4(3) . . ? N141 C146 C145 121.4(3) . . ? N141 C146 C147 119.1(3) . . ? C145 C146 C147 119.4(3) . . ? C155 N151 N152 105.7(2) . . ? C155 N151 Gd2 134.2(2) . . ? N152 N151 Gd2 120.02(14) . . ? C153 N152 N151 110.3(2) . . ? C153 N152 B2 125.8(2) . . ? N151 N152 B2 123.7(2) . . ? N152 C153 C154 108.0(2) . . ? C153 C154 C155 105.9(2) . . ? N151 C155 C154 110.0(2) . . ? N151 C155 C162 124.2(2) . . ? C154 C155 C162 125.7(2) . . ? C162 N161 C166 118.7(2) . . ? N161 C162 C163 122.3(3) . . ? N161 C162 C155 118.4(2) . . ? C163 C162 C155 119.2(3) . . ? C164 C163 C162 119.0(3) . . ? C165 C164 C163 119.0(3) . . ? C164 C165 C166 120.0(3) . . ? N161 C166 C165 121.0(3) . . ? N161 C166 C167 117.1(3) . . ? C165 C166 C167 121.9(3) . . ? O172 N171 O173 121.9(2) . . ? O172 N171 O174 122.3(2) . . ? O173 N171 O174 115.8(2) . . ? O172 N171 Gd2 173.9(2) . . ? O173 N171 Gd2 58.16(11) . . ? O174 N171 Gd2 57.99(12) . . ? N171 O173 Gd2 96.05(14) . . ? N171 O174 Gd2 95.85(14) . . ? O182 N181 O184 121.6(3) . . ? O182 N181 O183 122.1(3) . . ? O184 N181 O183 116.3(2) . . ? O182 N181 Gd2 179.1(2) . . ? O184 N181 Gd2 57.89(13) . . ? O183 N181 Gd2 58.45(13) . . ? N181 O183 Gd2 95.3(2) . . ? N181 O184 Gd2 96.2(2) . . ? _refine_diff_density_max 1.621 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.072 #=END data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H29 B Cl2 N11 O7 Tb' _chemical_formula_weight 872.25 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.588(2) _cell_length_b 16.3820(12) _cell_length_c 11.3938(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.099(7) _cell_angle_gamma 90.00 _cell_volume 3333.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method ? _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.345 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.78 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20996 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7578 _reflns_number_observed 6065 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0272P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7578 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_obs 0.0259 _refine_ls_wR_factor_all 0.0591 _refine_ls_wR_factor_obs 0.0559 _refine_ls_goodness_of_fit_all 0.970 _refine_ls_goodness_of_fit_obs 1.035 _refine_ls_restrained_S_all 0.970 _refine_ls_restrained_S_obs 1.035 _refine_ls_shift/esd_max -0.014 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tb1 Tb 0.261312(7) -0.981925(8) 0.283509(12) 0.01561(4) Uani 1 d . . B1 B 0.2430(2) -0.7882(2) 0.4299(3) 0.0199(7) Uani 1 d . . H1 H 0.2361(2) -0.7343(2) 0.4667(3) 0.024 Uiso 1 calc R . N11 N 0.34418(13) -0.85345(14) 0.3474(2) 0.0186(5) Uani 1 d . . N12 N 0.31740(13) -0.78714(14) 0.3947(2) 0.0194(5) Uani 1 d . . C13 C 0.3642(2) -0.7238(2) 0.4062(3) 0.0251(7) Uani 1 d . . H13 H 0.3572(2) -0.6715(2) 0.4375(3) 0.030 Uiso 1 calc R . C14 C 0.4242(2) -0.7469(2) 0.3652(3) 0.0265(7) Uani 1 d . . H14 H 0.4661(2) -0.7146(2) 0.3619(3) 0.032 Uiso 1 calc R . C15 C 0.4098(2) -0.8285(2) 0.3293(2) 0.0199(6) Uani 1 d . . N21 N 0.47240(13) -0.95804(15) 0.3272(2) 0.0214(5) Uani 1 d . . C22 C 0.4581(2) -0.8825(2) 0.2798(3) 0.0216(6) Uani 1 d . . C23 C 0.4894(2) -0.8543(2) 0.1897(3) 0.0294(7) Uani 1 d . . H23 H 0.4795(2) -0.8004(2) 0.1583(3) 0.035 Uiso 1 calc R . C24 C 0.5351(2) -0.9062(2) 0.1467(3) 0.0345(8) Uani 1 d . . H24 H 0.5568(2) -0.8883(2) 0.0848(3) 0.041 Uiso 1 calc R . C25 C 0.5491(2) -0.9837(2) 0.1941(3) 0.0312(7) Uani 1 d . . H25 H 0.5802(2) -1.0198(2) 0.1650(3) 0.037 Uiso 1 calc R . C26 C 0.5173(2) -1.0086(2) 0.2849(3) 0.0248(7) Uani 1 d . . C27 C 0.5303(2) -1.0924(2) 0.3410(3) 0.0348(8) Uani 1 d . . H27A H 0.5751(7) -1.1164(5) 0.3254(17) 0.052 Uiso 1 calc R . H27B H 0.4869(5) -1.1271(4) 0.3047(14) 0.052 Uiso 1 calc R . H27C H 0.5374(12) -1.0884(2) 0.4293(4) 0.052 Uiso 1 calc R . N31 N 0.25782(13) -0.93672(14) 0.5047(2) 0.0176(5) Uani 1 d . . N32 N 0.24629(13) -0.85597(14) 0.5243(2) 0.0198(5) Uani 1 d . . C33 C 0.2419(2) -0.8442(2) 0.6389(3) 0.0256(7) Uani 1 d . . H33 H 0.2346(2) -0.7932(2) 0.6735(3) 0.031 Uiso 1 calc R . C34 C 0.2495(2) -0.9178(2) 0.6973(3) 0.0261(7) Uani 1 d . . H34 H 0.2485(2) -0.9283(2) 0.7788(3) 0.031 Uiso 1 calc R . C35 C 0.2592(2) -0.9742(2) 0.6110(2) 0.0196(6) Uani 1 d . . N41 N 0.31435(13) -1.10336(14) 0.5753(2) 0.0201(5) Uani 1 d . . C42 C 0.2711(2) -1.0627(2) 0.6330(2) 0.0200(6) Uani 1 d . . C43 C 0.2394(2) -1.1014(2) 0.7156(3) 0.0262(7) Uani 1 d . . H43 H 0.2090(2) -1.0717(2) 0.7553(3) 0.031 Uiso 1 calc R . C44 C 0.2528(2) -1.1837(2) 0.7386(3) 0.0301(8) Uani 1 d . . H44 H 0.2321(2) -1.2112(2) 0.7951(3) 0.036 Uiso 1 calc R . C45 C 0.2969(2) -1.2255(2) 0.6783(3) 0.0262(7) Uani 1 d . . H45 H 0.3070(2) -1.2820(2) 0.6932(3) 0.031 Uiso 1 calc R . C46 C 0.3260(2) -1.1838(2) 0.5964(3) 0.0209(6) Uani 1 d . . C47 C 0.3721(2) -1.2262(2) 0.5260(3) 0.0291(7) Uani 1 d . . H47A H 0.3778(10) -1.2838(3) 0.5497(14) 0.044 Uiso 1 calc R . H47B H 0.4215(4) -1.2005(8) 0.5437(14) 0.044 Uiso 1 calc R . H47C H 0.3470(6) -1.2220(11) 0.4383(3) 0.044 Uiso 1 calc R . N51 N 0.17761(13) -0.86800(14) 0.2414(2) 0.0192(5) Uani 1 d . . N52 N 0.17721(13) -0.80288(14) 0.3149(2) 0.0184(5) Uani 1 d . . C53 C 0.1155(2) -0.7582(2) 0.2677(3) 0.0259(7) Uani 1 d . . H53 H 0.1024(2) -0.7096(2) 0.3023(3) 0.031 Uiso 1 calc R . C54 C 0.0743(2) -0.7943(2) 0.1612(3) 0.0264(7) Uani 1 d . . H54 H 0.0280(2) -0.7763(2) 0.1084(3) 0.032 Uiso 1 calc R . C55 C 0.1156(2) -0.8632(2) 0.1475(3) 0.0194(6) Uani 1 d . . N61 N 0.14354(13) -0.99352(14) 0.0716(2) 0.0192(5) Uani 1 d . . C62 C 0.1007(2) -0.9248(2) 0.0501(3) 0.0197(6) Uani 1 d . . C63 C 0.0446(2) -0.9115(2) -0.0574(3) 0.0248(7) Uani 1 d . . H63 H 0.0161(2) -0.8625(2) -0.0686(3) 0.030 Uiso 1 calc R . C64 C 0.0305(2) -0.9698(2) -0.1476(3) 0.0299(7) Uani 1 d . . H64 H -0.0070(2) -0.9616(2) -0.2224(3) 0.036 Uiso 1 calc R . C65 C 0.0725(2) -1.0410(2) -0.1268(3) 0.0262(7) Uani 1 d . . H65 H 0.0634(2) -1.0825(2) -0.1874(3) 0.031 Uiso 1 calc R . C66 C 0.1278(2) -1.0516(2) -0.0174(3) 0.0220(6) Uani 1 d . . C67 C 0.1708(2) -1.1305(2) 0.0053(3) 0.0299(7) Uani 1 d . . H67A H 0.2213(4) -1.1216(3) -0.0032(18) 0.045 Uiso 1 calc R . H67B H 0.1449(6) -1.1714(4) -0.0541(11) 0.045 Uiso 1 calc R . H67C H 0.1743(10) -1.1498(6) 0.0881(7) 0.045 Uiso 1 calc R . N1 N 0.16649(15) -1.11287(15) 0.3249(2) 0.0239(6) Uani 1 d . . O1 O 0.12689(14) -1.16945(14) 0.3383(2) 0.0459(7) Uani 1 d . . O2 O 0.14819(12) -1.03904(12) 0.3333(2) 0.0255(5) Uani 1 d . . O3 O 0.22873(11) -1.12453(12) 0.3014(2) 0.0234(5) Uani 1 d . . N2 N 0.32144(14) -0.9903(2) 0.0759(2) 0.0259(6) Uani 1 d . . O4 O 0.34394(15) -0.9969(2) -0.0151(2) 0.0453(7) Uani 1 d . . O5 O 0.29520(12) -0.92460(13) 0.1043(2) 0.0276(5) Uani 1 d . . O6 O 0.32335(12) -1.05094(13) 0.1478(2) 0.0268(5) Uani 1 d . . O7 O 0.36862(13) -1.03975(13) 0.4056(2) 0.0231(5) Uani 1 d . . C1 C -0.0332(2) -0.6197(2) -0.0338(4) 0.0525(11) Uani 1 d . . H1A H -0.0292(2) -0.6340(2) 0.0522(4) 0.063 Uiso 0.63(4) calc PR 1 H1B H -0.0716(2) -0.5765(2) -0.0594(4) 0.063 Uiso 0.63(4) calc PR 1 H1A H -0.0643(2) -0.5728(2) -0.0730(4) 0.063 Uiso 0.37(4) calc PR 2 H1B H -0.0436(2) -0.6296(2) 0.0457(4) 0.063 Uiso 0.37(4) calc PR 2 Cl1 Cl 0.0546(3) -0.5824(4) -0.0450(5) 0.0436(14) Uani 0.63(4) d P 1 Cl1' Cl 0.0559(6) -0.5947(10) -0.0080(35) 0.091(4) Uani 0.37(4) d P 2 Cl2 Cl -0.06087(5) -0.70620(5) -0.12631(9) 0.0444(2) Uani 1 d . . H72 H 0.4072(22) -1.0160(22) 0.4076(33) 0.041(11) Uiso 1 d . . H71 H 0.3615(21) -1.0581(24) 0.4818(37) 0.057(12) Uiso 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 Tb1 0.01723(7) 0.01410(7) 0.01671(7) -0.00017(6) 0.00674(5) 0.00145(6) B1 0.025(2) 0.015(2) 0.020(2) -0.0033(13) 0.0071(14) 0.0006(13) N11 0.0197(13) 0.0185(12) 0.0187(12) -0.0015(10) 0.0069(10) -0.0011(10) N12 0.0208(13) 0.0155(12) 0.0213(12) -0.0013(9) 0.0046(10) -0.0014(10) C13 0.024(2) 0.017(2) 0.030(2) 0.0016(12) 0.0004(13) -0.0016(12) C14 0.023(2) 0.022(2) 0.033(2) 0.0043(13) 0.0054(14) -0.0048(13) C15 0.017(2) 0.023(2) 0.0176(14) 0.0040(11) 0.0019(11) -0.0007(12) N21 0.0193(13) 0.0263(14) 0.0200(12) -0.0027(10) 0.0076(10) -0.0014(10) C22 0.018(2) 0.027(2) 0.0187(14) 0.0010(12) 0.0027(12) -0.0024(12) C23 0.028(2) 0.036(2) 0.026(2) 0.0046(14) 0.0098(14) -0.0050(14) C24 0.024(2) 0.058(2) 0.025(2) 0.003(2) 0.0119(14) -0.007(2) C25 0.023(2) 0.048(2) 0.025(2) -0.008(2) 0.0115(13) -0.002(2) C26 0.020(2) 0.033(2) 0.0223(15) -0.0068(13) 0.0060(12) -0.0015(13) C27 0.039(2) 0.034(2) 0.037(2) -0.0043(15) 0.018(2) 0.009(2) N31 0.0186(13) 0.0155(12) 0.0194(12) -0.0017(9) 0.0067(10) -0.0004(10) N32 0.0236(14) 0.0191(13) 0.0182(12) -0.0040(10) 0.0083(10) 0.0002(10) C33 0.032(2) 0.027(2) 0.0199(15) -0.0062(12) 0.0102(13) 0.0042(13) C34 0.034(2) 0.031(2) 0.0148(15) -0.0023(12) 0.0099(13) 0.0028(14) C35 0.0190(15) 0.021(2) 0.0191(14) 0.0009(12) 0.0061(11) -0.0004(12) N41 0.0211(13) 0.0222(13) 0.0159(12) -0.0017(10) 0.0033(10) -0.0014(10) C42 0.020(2) 0.022(2) 0.0162(14) -0.0013(12) 0.0035(11) -0.0019(12) C43 0.029(2) 0.027(2) 0.026(2) 0.0010(14) 0.0139(13) -0.0033(14) C44 0.033(2) 0.030(2) 0.031(2) 0.0069(14) 0.0137(15) -0.0056(14) C45 0.030(2) 0.020(2) 0.027(2) 0.0019(13) 0.0050(13) -0.0015(13) C46 0.020(2) 0.021(2) 0.0201(15) -0.0005(12) 0.0025(12) -0.0017(12) C47 0.031(2) 0.025(2) 0.031(2) -0.0010(13) 0.0087(14) 0.0021(14) N51 0.0228(14) 0.0165(12) 0.0191(12) -0.0015(10) 0.0071(10) 0.0014(10) N52 0.0212(13) 0.0150(12) 0.0201(12) -0.0003(9) 0.0078(10) 0.0031(10) C53 0.026(2) 0.021(2) 0.032(2) 0.0021(13) 0.0109(14) 0.0084(13) C54 0.021(2) 0.025(2) 0.031(2) 0.0040(13) 0.0031(13) 0.0089(13) C55 0.018(2) 0.021(2) 0.0202(14) 0.0034(12) 0.0068(12) 0.0020(12) N61 0.0189(13) 0.0199(13) 0.0191(12) -0.0004(9) 0.0058(10) -0.0021(10) C62 0.0151(15) 0.024(2) 0.0217(15) 0.0022(12) 0.0080(12) -0.0015(12) C63 0.020(2) 0.029(2) 0.025(2) 0.0028(13) 0.0056(13) 0.0000(13) C64 0.023(2) 0.042(2) 0.022(2) 0.0036(14) 0.0012(13) -0.0007(14) C65 0.026(2) 0.034(2) 0.0180(15) -0.0056(13) 0.0044(13) -0.0068(13) C66 0.022(2) 0.026(2) 0.0203(15) -0.0033(12) 0.0093(12) -0.0046(13) C67 0.037(2) 0.025(2) 0.027(2) -0.0069(13) 0.0075(14) 0.0000(14) N1 0.031(2) 0.0218(14) 0.0214(13) -0.0045(10) 0.0110(11) -0.0065(11) O1 0.052(2) 0.0304(13) 0.068(2) -0.0104(12) 0.0382(14) -0.0196(12) O2 0.0272(12) 0.0206(11) 0.0316(12) -0.0045(9) 0.0129(9) 0.0005(9) O3 0.0229(12) 0.0191(11) 0.0313(12) 0.0000(9) 0.0130(9) 0.0017(9) N2 0.0221(14) 0.036(2) 0.0204(13) -0.0027(11) 0.0076(11) -0.0040(12) O4 0.057(2) 0.061(2) 0.0295(13) -0.0026(12) 0.0304(13) 0.0010(13) O5 0.0317(13) 0.0255(12) 0.0279(12) 0.0003(9) 0.0122(10) -0.0021(10) O6 0.0314(13) 0.0287(12) 0.0233(11) 0.0018(9) 0.0125(9) 0.0061(10) O7 0.0198(12) 0.0276(12) 0.0232(11) 0.0032(9) 0.0082(9) 0.0016(9) C1 0.061(3) 0.041(2) 0.067(3) -0.003(2) 0.036(2) -0.006(2) Cl1 0.0333(14) 0.041(2) 0.059(3) -0.0149(14) 0.0183(10) -0.0080(11) Cl1' 0.049(3) 0.053(3) 0.169(11) 0.003(7) 0.027(5) -0.003(2) Cl2 0.0422(5) 0.0338(5) 0.0550(6) 0.0041(4) 0.0098(4) 0.0010(4) _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 Tb1 O7 2.296(2) . ? Tb1 N51 2.392(2) . ? Tb1 O3 2.436(2) . ? Tb1 O6 2.447(2) . ? Tb1 O5 2.482(2) . ? Tb1 O2 2.506(2) . ? Tb1 N11 2.590(2) . ? Tb1 N31 2.644(2) . ? Tb1 N61 2.780(2) . ? Tb1 N2 2.887(2) . ? Tb1 N1 2.897(2) . ? B1 N32 1.536(4) . ? B1 N12 1.542(4) . ? B1 N52 1.544(4) . ? N11 C15 1.356(3) . ? N11 N12 1.366(3) . ? N12 C13 1.337(4) . ? C13 C14 1.377(4) . ? C14 C15 1.402(4) . ? C15 C22 1.479(4) . ? N21 C22 1.346(4) . ? N21 C26 1.355(4) . ? C22 C23 1.392(4) . ? C23 C24 1.384(4) . ? C24 C25 1.376(5) . ? C25 C26 1.387(4) . ? C26 C27 1.506(4) . ? N31 C35 1.352(3) . ? N31 N32 1.369(3) . ? N32 C33 1.344(3) . ? C33 C34 1.364(4) . ? C34 C35 1.397(4) . ? C35 C42 1.478(4) . ? N41 C42 1.346(3) . ? N41 C46 1.347(4) . ? C42 C43 1.394(4) . ? C43 C44 1.382(4) . ? C44 C45 1.388(4) . ? C45 C46 1.382(4) . ? C46 C47 1.495(4) . ? N51 C55 1.340(4) . ? N51 N52 1.357(3) . ? N52 C53 1.341(4) . ? C53 C54 1.377(4) . ? C54 C55 1.397(4) . ? C55 C62 1.468(4) . ? N61 C62 1.362(4) . ? N61 C66 1.362(4) . ? C62 C63 1.388(4) . ? C63 C64 1.374(4) . ? C64 C65 1.386(4) . ? C65 C66 1.390(4) . ? C66 C67 1.503(4) . ? N1 O1 1.219(3) . ? N1 O2 1.267(3) . ? N1 O3 1.272(3) . ? N2 O4 1.225(3) . ? N2 O5 1.261(3) . ? N2 O6 1.282(3) . ? C1 Cl1' 1.652(13) . ? C1 Cl2 1.755(4) . ? C1 Cl1 1.781(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Tb1 N51 148.31(8) . . ? O7 Tb1 O3 75.40(8) . . ? N51 Tb1 O3 127.02(7) . . ? O7 Tb1 O6 73.13(7) . . ? N51 Tb1 O6 128.93(7) . . ? O3 Tb1 O6 77.38(7) . . ? O7 Tb1 O5 106.18(8) . . ? N51 Tb1 O5 80.76(7) . . ? O3 Tb1 O5 123.88(7) . . ? O6 Tb1 O5 51.94(7) . . ? O7 Tb1 O2 110.56(8) . . ? N51 Tb1 O2 78.27(7) . . ? O3 Tb1 O2 51.63(6) . . ? O6 Tb1 O2 122.86(7) . . ? O5 Tb1 O2 138.40(7) . . ? O7 Tb1 N11 79.39(8) . . ? N51 Tb1 N11 74.06(8) . . ? O3 Tb1 N11 153.87(7) . . ? O6 Tb1 N11 101.85(7) . . ? O5 Tb1 N11 69.96(7) . . ? O2 Tb1 N11 135.27(7) . . ? O7 Tb1 N31 77.58(7) . . ? N51 Tb1 N31 77.64(7) . . ? O3 Tb1 N31 96.68(7) . . ? O6 Tb1 N31 150.67(7) . . ? O5 Tb1 N31 139.19(7) . . ? O2 Tb1 N31 69.20(7) . . ? N11 Tb1 N31 70.99(7) . . ? O7 Tb1 N61 147.21(7) . . ? N51 Tb1 N61 64.37(7) . . ? O3 Tb1 N61 81.55(7) . . ? O6 Tb1 N61 79.36(7) . . ? O5 Tb1 N61 68.27(7) . . ? O2 Tb1 N61 70.30(7) . . ? N11 Tb1 N61 124.29(7) . . ? N31 Tb1 N61 128.70(7) . . ? O7 Tb1 N2 90.48(8) . . ? N51 Tb1 N2 104.54(8) . . ? O3 Tb1 N2 100.65(7) . . ? O6 Tb1 N2 26.20(7) . . ? O5 Tb1 N2 25.77(7) . . ? O2 Tb1 N2 135.05(7) . . ? N11 Tb1 N2 86.21(7) . . ? N31 Tb1 N2 155.75(7) . . ? N61 Tb1 N2 71.07(7) . . ? O7 Tb1 N1 93.51(8) . . ? N51 Tb1 N1 102.66(8) . . ? O3 Tb1 N1 25.79(6) . . ? O6 Tb1 N1 100.10(7) . . ? O5 Tb1 N1 135.96(7) . . ? O2 Tb1 N1 25.85(6) . . ? N11 Tb1 N1 153.76(7) . . ? N31 Tb1 N1 82.84(7) . . ? N61 Tb1 N1 73.90(7) . . ? N2 Tb1 N1 119.32(7) . . ? N32 B1 N12 109.0(2) . . ? N32 B1 N52 110.5(2) . . ? N12 B1 N52 109.7(2) . . ? C15 N11 N12 105.2(2) . . ? C15 N11 Tb1 133.8(2) . . ? N12 N11 Tb1 120.2(2) . . ? C13 N12 N11 110.9(2) . . ? C13 N12 B1 126.1(2) . . ? N11 N12 B1 123.0(2) . . ? N12 C13 C14 108.7(3) . . ? C13 C14 C15 104.7(3) . . ? N11 C15 C14 110.5(3) . . ? N11 C15 C22 123.0(3) . . ? C14 C15 C22 126.5(3) . . ? C22 N21 C26 119.4(2) . . ? N21 C22 C23 121.7(3) . . ? N21 C22 C15 118.0(2) . . ? C23 C22 C15 120.2(3) . . ? C24 C23 C22 118.6(3) . . ? C25 C24 C23 119.7(3) . . ? C24 C25 C26 119.4(3) . . ? N21 C26 C25 121.2(3) . . ? N21 C26 C27 116.7(3) . . ? C25 C26 C27 122.2(3) . . ? C35 N31 N32 104.9(2) . . ? C35 N31 Tb1 136.7(2) . . ? N32 N31 Tb1 118.2(2) . . ? C33 N32 N31 110.6(2) . . ? C33 N32 B1 125.1(2) . . ? N31 N32 B1 124.2(2) . . ? N32 C33 C34 108.7(3) . . ? C33 C34 C35 104.9(2) . . ? N31 C35 C34 110.9(3) . . ? N31 C35 C42 124.2(2) . . ? C34 C35 C42 124.9(2) . . ? C42 N41 C46 119.1(2) . . ? N41 C42 C43 121.8(3) . . ? N41 C42 C35 118.9(2) . . ? C43 C42 C35 119.3(3) . . ? C44 C43 C42 118.9(3) . . ? C43 C44 C45 119.2(3) . . ? C46 C45 C44 119.1(3) . . ? N41 C46 C45 121.9(3) . . ? N41 C46 C47 116.5(2) . . ? C45 C46 C47 121.5(3) . . ? C55 N51 N52 107.2(2) . . ? C55 N51 Tb1 125.0(2) . . ? N52 N51 Tb1 127.2(2) . . ? C53 N52 N51 109.4(2) . . ? C53 N52 B1 130.0(2) . . ? N51 N52 B1 120.5(2) . . ? N52 C53 C54 108.8(3) . . ? C53 C54 C55 104.9(3) . . ? N51 C55 C54 109.6(3) . . ? N51 C55 C62 120.3(2) . . ? C54 C55 C62 130.1(3) . . ? C62 N61 C66 116.7(2) . . ? C62 N61 Tb1 112.4(2) . . ? C66 N61 Tb1 130.5(2) . . ? N61 C62 C63 123.2(3) . . ? N61 C62 C55 117.0(2) . . ? C63 C62 C55 119.8(3) . . ? C64 C63 C62 119.4(3) . . ? C63 C64 C65 118.4(3) . . ? C64 C65 C66 120.0(3) . . ? N61 C66 C65 122.2(3) . . ? N61 C66 C67 118.6(3) . . ? C65 C66 C67 119.2(3) . . ? O1 N1 O2 122.1(3) . . ? O1 N1 O3 121.9(3) . . ? O2 N1 O3 116.0(2) . . ? O1 N1 Tb1 177.5(2) . . ? O2 N1 Tb1 59.59(13) . . ? O3 N1 Tb1 56.43(13) . . ? N1 O2 Tb1 94.6(2) . . ? N1 O3 Tb1 97.8(2) . . ? O4 N2 O5 122.6(3) . . ? O4 N2 O6 121.2(3) . . ? O5 N2 O6 116.2(2) . . ? O4 N2 Tb1 176.5(2) . . ? O5 N2 Tb1 58.90(13) . . ? O6 N2 Tb1 57.38(13) . . ? N2 O5 Tb1 95.3(2) . . ? N2 O6 Tb1 96.4(2) . . ? Cl1' C1 Cl2 114.8(6) . . ? Cl2 C1 Cl1 110.8(2) . . ? _refine_diff_density_max 0.438 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.105