Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 ####################################################################### # # 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_1 _database_code_depnum_ccdc_archive 'CCDC 289606' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 La N7 O11' _chemical_formula_weight 729.44 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.796(4) _cell_length_b 9.658(2) _cell_length_c 19.230(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.55(2) _cell_angle_gamma 90.00 _cell_volume 2839.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.516 _cell_measurement_theta_max 19.794 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5858 _exptl_absorpt_correction_T_max 0.9114 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 1 _diffrn_reflns_number 8049 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6513 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+14.9920P] 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 SHELXL _refine_ls_extinction_coef 0.0032(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6513 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 La1 La 0.26797(3) 0.34822(5) 0.58177(2) 0.03678(18) Uani 1 1 d . . . N10 N 0.2465(6) 0.2908(9) 0.7380(4) 0.0529(19) Uani 1 1 d . . . N20 N 0.4269(6) 0.5361(9) 0.6477(4) 0.055(2) Uani 1 1 d . . . N30 N 0.0980(7) 0.5120(10) 0.5945(7) 0.089(3) Uani 1 1 d . . . O11 O 0.2571(6) 0.4118(8) 0.7183(4) 0.080(2) Uani 1 1 d . . . O12 O 0.2536(4) 0.1964(7) 0.6944(3) 0.0588(17) Uani 1 1 d . . . O13 O 0.2331(7) 0.2619(9) 0.7955(4) 0.099(3) Uani 1 1 d . . . O21 O 0.3565(5) 0.5894(7) 0.6091(3) 0.068(2) Uani 1 1 d . . . O22 O 0.4276(4) 0.4083(7) 0.6599(4) 0.0614(18) Uani 1 1 d . . . O23 O 0.4929(5) 0.6080(8) 0.6713(4) 0.079(2) Uani 1 1 d . . . O31 O 0.1015(5) 0.3791(8) 0.5995(5) 0.092(3) Uani 1 1 d . . . O32 O 0.1667(5) 0.5672(8) 0.5796(4) 0.076(2) Uani 1 1 d . . . O33 O 0.0442(6) 0.5737(10) 0.6142(8) 0.148(5) Uani 1 1 d . . . O1 O 0.1726(4) 0.1494(6) 0.5473(3) 0.0470(14) Uani 1 1 d . . . O2 O 0.3595(3) 0.1496(6) 0.5922(3) 0.0402(12) Uani 1 1 d . . . N1 N 0.3646(4) 0.3679(8) 0.4885(4) 0.0449(17) Uani 1 1 d . . . N2 N 0.1708(4) 0.3714(7) 0.4472(4) 0.0440(17) Uani 1 1 d . . . N4 N 0.3768(4) -0.0456(7) 0.6920(3) 0.0411(16) Uani 1 1 d . . . H4B H 0.3402 0.0110 0.6647 0.049 Uiso 1 1 calc R . . N3 N 0.1637(4) -0.0654(8) 0.6281(4) 0.0454(17) Uani 1 1 d . . . H3C H 0.1843 0.0177 0.6265 0.055 Uiso 1 1 calc R . . C1 C 0.3391(6) 0.4665(10) 0.4273(5) 0.053(2) Uani 1 1 d . . . H1A H 0.3190 0.4141 0.3826 0.064 Uiso 1 1 calc R . . H1B H 0.3905 0.5202 0.4239 0.064 Uiso 1 1 calc R . . C2 C 0.2684(6) 0.5638(10) 0.4352(5) 0.055(2) Uani 1 1 d . . . H2A H 0.2706 0.6463 0.4061 0.067 Uiso 1 1 calc R . . H2B H 0.2805 0.5933 0.4855 0.067 Uiso 1 1 calc R . . C3 C 0.1763(6) 0.5048(10) 0.4134(5) 0.053(2) Uani 1 1 d . . . H3A H 0.1358 0.5698 0.4272 0.063 Uiso 1 1 calc R . . H3B H 0.1586 0.4939 0.3611 0.063 Uiso 1 1 calc R . . C4 C 0.1263(5) 0.2817(9) 0.4039(4) 0.0410(19) Uani 1 1 d . . . H4A H 0.1042 0.3097 0.3559 0.049 Uiso 1 1 calc R . . C5 C 0.1061(5) 0.1376(9) 0.4219(4) 0.0397(18) Uani 1 1 d . . . C6 C 0.0637(5) 0.0558(10) 0.3637(5) 0.045(2) Uani 1 1 d . . . H6A H 0.0508 0.0948 0.3175 0.054 Uiso 1 1 calc R . . C7 C 0.0396(6) -0.0813(11) 0.3712(5) 0.051(2) Uani 1 1 d . . . C8 C 0.0568(5) -0.1362(10) 0.4402(5) 0.047(2) Uani 1 1 d . . . H8A H 0.0380 -0.2262 0.4474 0.057 Uiso 1 1 calc R . . C9 C 0.1026(5) -0.0568(9) 0.4994(5) 0.0419(19) Uani 1 1 d . . . C10 C 0.1297(5) 0.0811(9) 0.4929(4) 0.0380(18) Uani 1 1 d . . . C11 C 0.1210(5) -0.1209(9) 0.5680(5) 0.044(2) Uani 1 1 d . . . H11A H 0.1005 -0.2117 0.5700 0.053 Uiso 1 1 calc R . . C12 C -0.0056(7) -0.1658(12) 0.3060(5) 0.070(3) Uani 1 1 d . . . H12A H 0.0151 -0.2606 0.3122 0.105 Uiso 1 1 calc R . . H12B H 0.0075 -0.1268 0.2634 0.105 Uiso 1 1 calc R . . H12C H -0.0683 -0.1639 0.3007 0.105 Uiso 1 1 calc R . . C13 C 0.1797(6) -0.1337(10) 0.6991(5) 0.052(2) Uani 1 1 d . . . H13A H 0.1329 -0.2007 0.6983 0.063 Uiso 1 1 calc R . . H13B H 0.1777 -0.0639 0.7356 0.063 Uiso 1 1 calc R . . C14 C 0.2684(6) -0.2086(10) 0.7201(5) 0.051(2) Uani 1 1 d . . . H14A H 0.2662 -0.2766 0.7574 0.061 Uiso 1 1 calc R . . H14B H 0.2756 -0.2601 0.6780 0.061 Uiso 1 1 calc R . . C15 C 0.3487(6) -0.1194(10) 0.7471(4) 0.050(2) Uani 1 1 d . . . H15A H 0.3366 -0.0523 0.7815 0.060 Uiso 1 1 calc R . . H15B H 0.3968 -0.1785 0.7729 0.060 Uiso 1 1 calc R . . C16 C 0.4555(6) -0.0595(9) 0.6810(4) 0.044(2) Uani 1 1 d . . . H16A H 0.4924 -0.1268 0.7082 0.053 Uiso 1 1 calc R . . C17 C 0.4891(5) 0.0186(9) 0.6315(4) 0.0375(18) Uani 1 1 d . . . C20 C 0.5646(5) 0.1617(10) 0.5379(5) 0.047(2) Uani 1 1 d . . . H20A H 0.5892 0.2078 0.5047 0.056 Uiso 1 1 calc R . . C18 C 0.5752(5) -0.0095(9) 0.6283(4) 0.0424(19) Uani 1 1 d . . . H18A H 0.6072 -0.0778 0.6586 0.051 Uiso 1 1 calc R . . C19 C 0.6144(5) 0.0606(10) 0.5816(5) 0.047(2) Uani 1 1 d . . . C21 C 0.4800(5) 0.1980(9) 0.5410(4) 0.0385(18) Uani 1 1 d . . . C22 C 0.4386(5) 0.1243(8) 0.5888(4) 0.0381(18) Uani 1 1 d . . . C23 C 0.4371(6) 0.3042(9) 0.4915(5) 0.045(2) Uani 1 1 d . . . H23A H 0.4663 0.3305 0.4565 0.054 Uiso 1 1 calc R . . C24 C 0.7060(6) 0.0237(11) 0.5769(6) 0.064(3) Uani 1 1 d . . . H24A H 0.7392 0.1078 0.5759 0.097 Uiso 1 1 calc R . . H24B H 0.7029 -0.0291 0.5335 0.097 Uiso 1 1 calc R . . H24C H 0.7345 -0.0312 0.6184 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0430(3) 0.0293(2) 0.0338(2) -0.0026(2) 0.00181(17) 0.0068(2) N10 0.072(5) 0.048(4) 0.040(4) -0.003(4) 0.018(4) -0.006(4) N20 0.058(5) 0.057(5) 0.048(4) -0.015(4) 0.010(4) 0.003(5) N30 0.091(8) 0.041(5) 0.155(10) 0.012(6) 0.068(8) 0.010(5) O11 0.129(7) 0.048(4) 0.065(5) -0.007(4) 0.026(5) -0.021(5) O12 0.076(5) 0.050(4) 0.056(4) -0.001(3) 0.027(3) 0.014(3) O13 0.166(9) 0.094(6) 0.062(5) 0.003(5) 0.076(5) 0.002(6) O21 0.080(5) 0.062(4) 0.055(4) 0.001(3) 0.004(4) 0.022(4) O22 0.060(4) 0.055(4) 0.061(4) -0.003(3) -0.001(3) 0.010(4) O23 0.085(6) 0.061(5) 0.083(5) 0.005(4) 0.007(4) -0.002(4) O31 0.067(5) 0.066(6) 0.147(8) 0.001(5) 0.035(5) -0.007(4) O32 0.062(5) 0.055(4) 0.115(6) 0.005(4) 0.029(4) -0.005(4) O33 0.081(6) 0.069(6) 0.336(17) -0.009(8) 0.131(9) 0.014(5) O1 0.042(3) 0.052(3) 0.043(3) 0.004(3) 0.004(2) -0.005(3) O2 0.036(3) 0.040(3) 0.048(3) 0.003(3) 0.016(2) 0.006(3) N1 0.040(4) 0.051(5) 0.043(4) 0.007(3) 0.010(3) -0.002(4) N2 0.037(4) 0.045(4) 0.049(4) 0.013(3) 0.009(3) 0.000(3) N4 0.038(4) 0.044(4) 0.040(4) 0.005(3) 0.008(3) 0.003(3) N3 0.043(4) 0.043(4) 0.052(4) 0.002(3) 0.017(3) 0.000(3) C1 0.044(5) 0.063(6) 0.057(5) 0.021(5) 0.023(4) 0.004(5) C2 0.066(6) 0.045(5) 0.050(5) 0.012(4) 0.006(5) 0.001(5) C3 0.057(6) 0.048(5) 0.056(5) 0.016(4) 0.020(5) 0.003(5) C4 0.029(4) 0.054(5) 0.039(4) 0.007(4) 0.007(3) 0.010(4) C5 0.027(4) 0.052(5) 0.041(4) 0.003(4) 0.011(3) 0.008(4) C6 0.033(4) 0.057(6) 0.047(5) -0.004(4) 0.016(4) 0.008(4) C7 0.039(5) 0.059(6) 0.053(5) -0.010(5) 0.010(4) 0.005(4) C8 0.043(5) 0.045(5) 0.058(5) -0.006(4) 0.018(4) -0.003(4) C9 0.038(4) 0.039(4) 0.051(5) 0.001(4) 0.016(4) 0.005(4) C10 0.020(4) 0.052(5) 0.042(4) -0.002(4) 0.009(3) 0.003(4) C11 0.035(4) 0.042(5) 0.060(5) -0.001(4) 0.020(4) -0.001(4) C12 0.071(7) 0.070(7) 0.068(6) -0.015(6) 0.016(5) -0.015(6) C13 0.051(5) 0.060(6) 0.047(5) 0.017(5) 0.016(4) 0.000(5) C14 0.060(6) 0.046(5) 0.048(5) 0.012(4) 0.017(4) -0.004(5) C15 0.055(5) 0.062(6) 0.034(4) 0.007(4) 0.013(4) 0.003(5) C16 0.043(5) 0.043(5) 0.044(5) -0.005(4) 0.005(4) 0.004(4) C17 0.031(4) 0.042(5) 0.039(4) -0.005(4) 0.009(3) 0.007(4) C20 0.043(5) 0.048(5) 0.052(5) -0.015(4) 0.017(4) -0.004(4) C18 0.035(4) 0.041(5) 0.050(5) -0.001(4) 0.008(4) 0.005(4) C19 0.033(4) 0.053(5) 0.061(5) -0.006(5) 0.021(4) 0.000(4) C21 0.032(4) 0.045(5) 0.040(4) -0.005(4) 0.011(3) 0.000(4) C22 0.034(4) 0.043(5) 0.039(4) -0.006(4) 0.012(3) 0.003(4) C23 0.046(5) 0.045(5) 0.048(5) -0.003(4) 0.018(4) -0.010(4) C24 0.047(5) 0.062(7) 0.091(8) -0.010(6) 0.031(5) 0.008(5) _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 La1 O2 2.380(5) . ? La1 O1 2.428(6) . ? La1 N1 2.638(7) . ? La1 O32 2.646(7) . ? La1 O22 2.655(7) . ? La1 N2 2.666(7) . ? La1 O12 2.672(6) . ? La1 O21 2.700(8) . ? La1 O11 2.743(7) . ? La1 O31 2.752(8) . ? N10 O13 1.210(9) . ? N10 O11 1.252(10) . ? N10 O12 1.263(9) . ? N20 O23 1.239(10) . ? N20 O22 1.256(10) . ? N20 O21 1.280(10) . ? N30 O33 1.175(11) . ? N30 O31 1.288(11) . ? N30 O32 1.304(11) . ? O1 C10 1.278(9) . ? O2 C22 1.291(9) . ? N1 C23 1.288(11) . ? N1 C1 1.489(10) . ? N2 C4 1.283(10) . ? N2 C3 1.455(10) . ? N4 C16 1.320(10) . ? N4 C15 1.436(10) . ? N4 H4B 0.8700 . ? N3 C11 1.299(10) . ? N3 C13 1.480(10) . ? N3 H3C 0.8700 . ? C1 C2 1.496(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.519(13) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.488(12) . ? C4 H4A 0.9400 . ? C5 C6 1.395(11) . ? C5 C10 1.430(11) . ? C6 C7 1.395(13) . ? C6 H6A 0.9400 . ? C7 C8 1.391(12) . ? C7 C12 1.515(12) . ? C8 C9 1.412(11) . ? C8 H8A 0.9400 . ? C9 C10 1.414(12) . ? C9 C11 1.419(12) . ? C11 H11A 0.9400 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.538(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.513(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.418(11) . ? C16 H16A 0.9400 . ? C17 C18 1.404(10) . ? C17 C22 1.422(11) . ? C20 C19 1.395(12) . ? C20 C21 1.398(11) . ? C20 H20A 0.9400 . ? C18 C19 1.388(12) . ? C18 H18A 0.9400 . ? C19 C24 1.513(11) . ? C21 C22 1.442(11) . ? C21 C23 1.447(12) . ? C23 H23A 0.9400 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 O2 La1 O1 73.00(19) . . ? O2 La1 N1 70.8(2) . . ? O1 La1 N1 107.3(2) . . ? O2 La1 O32 176.1(2) . . ? O1 La1 O32 107.3(2) . . ? N1 La1 O32 112.5(2) . . ? O2 La1 O22 70.0(2) . . ? O1 La1 O22 139.7(2) . . ? N1 La1 O22 74.9(2) . . ? O32 La1 O22 108.6(2) . . ? O2 La1 N2 109.8(2) . . ? O1 La1 N2 68.6(2) . . ? N1 La1 N2 68.0(2) . . ? O32 La1 N2 73.7(2) . . ? O22 La1 N2 139.9(2) . . ? O2 La1 O12 70.31(18) . . ? O1 La1 O12 67.3(2) . . ? N1 La1 O12 140.5(2) . . ? O32 La1 O12 106.1(2) . . ? O22 La1 O12 85.6(2) . . ? N2 La1 O12 133.4(2) . . ? O2 La1 O21 113.9(2) . . ? O1 La1 O21 172.36(19) . . ? N1 La1 O21 73.1(2) . . ? O32 La1 O21 66.1(2) . . ? O22 La1 O21 47.9(2) . . ? N2 La1 O21 105.1(2) . . ? O12 La1 O21 117.5(2) . . ? O2 La1 O11 106.4(2) . . ? O1 La1 O11 104.8(2) . . ? N1 La1 O11 145.1(2) . . ? O32 La1 O11 69.7(3) . . ? O22 La1 O11 71.8(2) . . ? N2 La1 O11 138.7(2) . . ? O12 La1 O11 46.3(2) . . ? O21 La1 O11 77.0(2) . . ? O2 La1 O31 131.0(2) . . ? O1 La1 O31 64.7(2) . . ? N1 La1 O31 144.2(3) . . ? O32 La1 O31 47.4(2) . . ? O22 La1 O31 135.0(3) . . ? N2 La1 O31 77.1(3) . . ? O12 La1 O31 71.4(2) . . ? O21 La1 O31 110.3(2) . . ? O11 La1 O31 64.3(3) . . ? O13 N10 O11 124.0(9) . . ? O13 N10 O12 120.3(9) . . ? O11 N10 O12 115.6(7) . . ? O23 N20 O22 121.0(9) . . ? O23 N20 O21 121.0(9) . . ? O22 N20 O21 118.0(9) . . ? O33 N30 O31 120.1(11) . . ? O33 N30 O32 124.9(10) . . ? O31 N30 O32 113.7(9) . . ? N10 O11 La1 97.2(5) . . ? N10 O12 La1 100.4(5) . . ? N20 O21 La1 95.6(6) . . ? N20 O22 La1 98.4(5) . . ? N30 O31 La1 97.1(7) . . ? N30 O32 La1 101.7(6) . . ? C10 O1 La1 142.8(5) . . ? C22 O2 La1 136.4(5) . . ? C23 N1 C1 113.7(7) . . ? C23 N1 La1 126.6(6) . . ? C1 N1 La1 119.7(5) . . ? C4 N2 C3 113.1(7) . . ? C4 N2 La1 131.4(6) . . ? C3 N2 La1 115.0(5) . . ? C16 N4 C15 123.1(7) . . ? C16 N4 H4B 118.5 . . ? C15 N4 H4B 118.5 . . ? C11 N3 C13 124.6(8) . . ? C11 N3 H3C 117.7 . . ? C13 N3 H3C 117.7 . . ? N1 C1 C2 112.5(7) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 115.1(8) . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N2 C3 C2 111.7(7) . . ? N2 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C5 126.5(7) . . ? N2 C4 H4A 116.7 . . ? C5 C4 H4A 116.7 . . ? C6 C5 C10 120.4(8) . . ? C6 C5 C4 115.5(7) . . ? C10 C5 C4 124.0(8) . . ? C7 C6 C5 122.9(9) . . ? C7 C6 H6A 118.5 . . ? C5 C6 H6A 118.5 . . ? C8 C7 C6 117.8(9) . . ? C8 C7 C12 121.5(9) . . ? C6 C7 C12 120.7(9) . . ? C7 C8 C9 120.0(9) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 123.0(8) . . ? C8 C9 C11 117.1(8) . . ? C10 C9 C11 119.8(8) . . ? O1 C10 C9 121.6(8) . . ? O1 C10 C5 122.8(8) . . ? C9 C10 C5 115.6(8) . . ? N3 C11 C9 125.9(8) . . ? N3 C11 H11A 117.0 . . ? C9 C11 H11A 117.0 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 112.6(7) . . ? N3 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N3 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 116.9(8) . . ? C15 C14 H14A 108.1 . . ? C13 C14 H14A 108.1 . . ? C15 C14 H14B 108.1 . . ? C13 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? N4 C15 C14 114.6(7) . . ? N4 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? N4 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N4 C16 C17 125.5(8) . . ? N4 C16 H16A 117.3 . . ? C17 C16 H16A 117.3 . . ? C18 C17 C16 117.2(8) . . ? C18 C17 C22 121.5(8) . . ? C16 C17 C22 121.3(7) . . ? C19 C20 C21 123.5(8) . . ? C19 C20 H20A 118.3 . . ? C21 C20 H20A 118.3 . . ? C19 C18 C17 122.0(8) . . ? C19 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? C18 C19 C20 117.0(7) . . ? C18 C19 C24 120.8(9) . . ? C20 C19 C24 122.1(8) . . ? C20 C21 C22 119.6(8) . . ? C20 C21 C23 116.4(8) . . ? C22 C21 C23 123.9(7) . . ? O2 C22 C17 121.1(7) . . ? O2 C22 C21 122.5(7) . . ? C17 C22 C21 116.4(7) . . ? N1 C23 C21 129.1(8) . . ? N1 C23 H23A 115.4 . . ? C21 C23 H23A 115.4 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 N10 O11 La1 -175.8(9) . . . . ? O12 N10 O11 La1 6.6(9) . . . . ? O2 La1 O11 N10 -43.7(7) . . . . ? O1 La1 O11 N10 32.5(7) . . . . ? N1 La1 O11 N10 -123.6(6) . . . . ? O32 La1 O11 N10 135.8(7) . . . . ? O22 La1 O11 N10 -105.5(7) . . . . ? N2 La1 O11 N10 106.8(6) . . . . ? O12 La1 O11 N10 -3.9(5) . . . . ? O21 La1 O11 N10 -155.1(7) . . . . ? O31 La1 O11 N10 84.4(6) . . . . ? O13 N10 O12 La1 175.5(8) . . . . ? O11 N10 O12 La1 -6.8(9) . . . . ? O2 La1 O12 N10 143.2(6) . . . . ? O1 La1 O12 N10 -137.6(6) . . . . ? N1 La1 O12 N10 132.5(5) . . . . ? O32 La1 O12 N10 -35.2(6) . . . . ? O22 La1 O12 N10 72.8(6) . . . . ? N2 La1 O12 N10 -117.8(6) . . . . ? O21 La1 O12 N10 35.8(6) . . . . ? O11 La1 O12 N10 3.9(5) . . . . ? O31 La1 O12 N10 -68.0(6) . . . . ? O23 N20 O21 La1 176.0(8) . . . . ? O22 N20 O21 La1 -2.9(8) . . . . ? O2 La1 O21 N20 -23.6(5) . . . . ? O1 La1 O21 N20 -177.3(13) . . . . ? N1 La1 O21 N20 -83.0(5) . . . . ? O32 La1 O21 N20 152.1(6) . . . . ? O22 La1 O21 N20 1.6(5) . . . . ? N2 La1 O21 N20 -143.8(5) . . . . ? O12 La1 O21 N20 55.7(6) . . . . ? O11 La1 O21 N20 78.8(5) . . . . ? O31 La1 O21 N20 134.6(5) . . . . ? O23 N20 O22 La1 -175.9(7) . . . . ? O21 N20 O22 La1 2.9(9) . . . . ? O2 La1 O22 N20 153.8(6) . . . . ? O1 La1 O22 N20 178.1(5) . . . . ? N1 La1 O22 N20 79.1(6) . . . . ? O32 La1 O22 N20 -30.0(6) . . . . ? N2 La1 O22 N20 56.5(7) . . . . ? O12 La1 O22 N20 -135.6(6) . . . . ? O21 La1 O22 N20 -1.7(5) . . . . ? O11 La1 O22 N20 -90.3(6) . . . . ? O31 La1 O22 N20 -77.6(6) . . . . ? O33 N30 O31 La1 -163.6(13) . . . . ? O32 N30 O31 La1 4.0(12) . . . . ? O2 La1 O31 N30 172.8(7) . . . . ? O1 La1 O31 N30 -154.3(9) . . . . ? N1 La1 O31 N30 -69.7(9) . . . . ? O32 La1 O31 N30 -2.5(7) . . . . ? O22 La1 O31 N30 69.5(9) . . . . ? N2 La1 O31 N30 -82.1(8) . . . . ? O12 La1 O31 N30 132.6(8) . . . . ? O21 La1 O31 N30 19.4(9) . . . . ? O11 La1 O31 N30 83.0(8) . . . . ? O33 N30 O32 La1 162.7(14) . . . . ? O31 N30 O32 La1 -4.3(12) . . . . ? O2 La1 O32 N30 -64(3) . . . . ? O1 La1 O32 N30 29.0(8) . . . . ? N1 La1 O32 N30 146.8(7) . . . . ? O22 La1 O32 N30 -132.3(7) . . . . ? N2 La1 O32 N30 89.8(7) . . . . ? O12 La1 O32 N30 -41.6(8) . . . . ? O21 La1 O32 N30 -155.0(8) . . . . ? O11 La1 O32 N30 -70.7(7) . . . . ? O31 La1 O32 N30 2.5(7) . . . . ? O2 La1 O1 C10 -97.2(9) . . . . ? N1 La1 O1 C10 -34.2(9) . . . . ? O32 La1 O1 C10 86.9(9) . . . . ? O22 La1 O1 C10 -121.1(8) . . . . ? N2 La1 O1 C10 22.8(8) . . . . ? O12 La1 O1 C10 -172.5(9) . . . . ? O21 La1 O1 C10 57.7(19) . . . . ? O11 La1 O1 C10 159.8(8) . . . . ? O31 La1 O1 C10 108.2(9) . . . . ? O1 La1 O2 C22 153.5(7) . . . . ? N1 La1 O2 C22 37.7(7) . . . . ? O32 La1 O2 C22 -112(3) . . . . ? O22 La1 O2 C22 -42.7(7) . . . . ? N2 La1 O2 C22 94.5(7) . . . . ? O12 La1 O2 C22 -135.2(7) . . . . ? O21 La1 O2 C22 -23.0(7) . . . . ? O11 La1 O2 C22 -105.7(7) . . . . ? O31 La1 O2 C22 -175.6(7) . . . . ? O2 La1 N1 C23 -21.2(7) . . . . ? O1 La1 N1 C23 -85.6(7) . . . . ? O32 La1 N1 C23 156.7(7) . . . . ? O22 La1 N1 C23 52.4(7) . . . . ? N2 La1 N1 C23 -143.1(8) . . . . ? O12 La1 N1 C23 -10.6(9) . . . . ? O21 La1 N1 C23 102.4(7) . . . . ? O11 La1 N1 C23 70.2(9) . . . . ? O31 La1 N1 C23 -156.1(6) . . . . ? O2 La1 N1 C1 162.5(7) . . . . ? O1 La1 N1 C1 98.1(6) . . . . ? O32 La1 N1 C1 -19.6(7) . . . . ? O22 La1 N1 C1 -123.8(7) . . . . ? N2 La1 N1 C1 40.7(6) . . . . ? O12 La1 N1 C1 173.1(6) . . . . ? O21 La1 N1 C1 -73.9(6) . . . . ? O11 La1 N1 C1 -106.1(7) . . . . ? O31 La1 N1 C1 27.6(8) . . . . ? O2 La1 N2 C4 45.8(7) . . . . ? O1 La1 N2 C4 -15.8(7) . . . . ? N1 La1 N2 C4 104.3(7) . . . . ? O32 La1 N2 C4 -132.4(7) . . . . ? O22 La1 N2 C4 127.9(7) . . . . ? O12 La1 N2 C4 -35.4(8) . . . . ? O21 La1 N2 C4 168.7(7) . . . . ? O11 La1 N2 C4 -104.0(7) . . . . ? O31 La1 N2 C4 -83.5(7) . . . . ? O2 La1 N2 C3 -126.2(6) . . . . ? O1 La1 N2 C3 172.1(6) . . . . ? N1 La1 N2 C3 -67.7(6) . . . . ? O32 La1 N2 C3 55.6(6) . . . . ? O22 La1 N2 C3 -44.1(7) . . . . ? O12 La1 N2 C3 152.5(5) . . . . ? O21 La1 N2 C3 -3.4(6) . . . . ? O11 La1 N2 C3 83.9(6) . . . . ? O31 La1 N2 C3 104.5(6) . . . . ? C23 N1 C1 C2 -165.6(8) . . . . ? La1 N1 C1 C2 11.1(10) . . . . ? N1 C1 C2 C3 -80.8(10) . . . . ? C4 N2 C3 C2 -136.3(8) . . . . ? La1 N2 C3 C2 37.2(9) . . . . ? C1 C2 C3 N2 50.4(11) . . . . ? C3 N2 C4 C5 -178.1(7) . . . . ? La1 N2 C4 C5 9.8(12) . . . . ? N2 C4 C5 C6 -173.9(8) . . . . ? N2 C4 C5 C10 4.2(12) . . . . ? C10 C5 C6 C7 2.2(12) . . . . ? C4 C5 C6 C7 -179.6(7) . . . . ? C5 C6 C7 C8 1.8(12) . . . . ? C5 C6 C7 C12 -179.4(8) . . . . ? C6 C7 C8 C9 -4.1(12) . . . . ? C12 C7 C8 C9 177.1(8) . . . . ? C7 C8 C9 C10 2.6(12) . . . . ? C7 C8 C9 C11 -177.6(8) . . . . ? La1 O1 C10 C9 160.2(6) . . . . ? La1 O1 C10 C5 -19.5(13) . . . . ? C8 C9 C10 O1 -178.5(7) . . . . ? C11 C9 C10 O1 1.8(11) . . . . ? C8 C9 C10 C5 1.3(11) . . . . ? C11 C9 C10 C5 -178.5(7) . . . . ? C6 C5 C10 O1 176.2(7) . . . . ? C4 C5 C10 O1 -1.9(12) . . . . ? C6 C5 C10 C9 -3.6(10) . . . . ? C4 C5 C10 C9 178.4(7) . . . . ? C13 N3 C11 C9 178.2(8) . . . . ? C8 C9 C11 N3 178.6(8) . . . . ? C10 C9 C11 N3 -1.7(13) . . . . ? C11 N3 C13 C14 94.2(10) . . . . ? N3 C13 C14 C15 77.6(10) . . . . ? C16 N4 C15 C14 -121.8(9) . . . . ? C13 C14 C15 N4 -76.7(10) . . . . ? C15 N4 C16 C17 -174.7(8) . . . . ? N4 C16 C17 C18 178.9(8) . . . . ? N4 C16 C17 C22 1.1(13) . . . . ? C16 C17 C18 C19 179.8(8) . . . . ? C22 C17 C18 C19 -2.3(13) . . . . ? C17 C18 C19 C20 0.4(13) . . . . ? C17 C18 C19 C24 -177.3(8) . . . . ? C21 C20 C19 C18 2.4(13) . . . . ? C21 C20 C19 C24 180.0(8) . . . . ? C19 C20 C21 C22 -3.2(13) . . . . ? C19 C20 C21 C23 -179.5(8) . . . . ? La1 O2 C22 C17 146.7(6) . . . . ? La1 O2 C22 C21 -34.9(11) . . . . ? C18 C17 C22 O2 -179.9(7) . . . . ? C16 C17 C22 O2 -2.2(12) . . . . ? C18 C17 C22 C21 1.5(11) . . . . ? C16 C17 C22 C21 179.3(7) . . . . ? C20 C21 C22 O2 -177.4(7) . . . . ? C23 C21 C22 O2 -1.4(13) . . . . ? C20 C21 C22 C17 1.1(11) . . . . ? C23 C21 C22 C17 177.1(7) . . . . ? C1 N1 C23 C21 -177.1(8) . . . . ? La1 N1 C23 C21 6.4(13) . . . . ? C20 C21 C23 N1 -171.0(9) . . . . ? C22 C21 C23 N1 12.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.086 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.137 data_10 _database_code_depnum_ccdc_archive 'CCDC 289607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Ho N7 O11' _chemical_formula_weight 755.46 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' Ho Ho -0.2175 4.6783 '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 15.594(2) _cell_length_b 9.5218(12) _cell_length_c 18.669(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.532(3) _cell_angle_gamma 90.00 _cell_volume 2695.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5337 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.61 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_absorpt_correction_T_min 0.4103 _exptl_absorpt_correction_T_max 0.6132 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 5340 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26821 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.20 _reflns_number_total 6637 _reflns_number_gt 5196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXTL (Bruker, 2002)' _computing_structure_refinement 'SHELXTL (Bruker, 2002)' _computing_molecular_graphics 'SHELXTL (Bruker, 2002)' _computing_publication_material 'SHELXTL (Bruker, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6637 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.002 _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 Ho1 Ho 0.263432(13) 0.33390(2) 0.583166(11) 0.02089(7) Uani 1 1 d . . . N10 N 0.2486(2) 0.2917(4) 0.7364(2) 0.0278(9) Uani 1 1 d . . . N20 N 0.4169(3) 0.5151(4) 0.6482(2) 0.0301(9) Uani 1 1 d . . . N30 N 0.1050(3) 0.4919(4) 0.5956(2) 0.0356(10) Uani 1 1 d . . . O11 O 0.2574(2) 0.4133(3) 0.71352(17) 0.0338(8) Uani 1 1 d . . . O12 O 0.2527(2) 0.1935(3) 0.69128(16) 0.0270(7) Uani 1 1 d . . . O13 O 0.2375(2) 0.2676(4) 0.79685(18) 0.0447(9) Uani 1 1 d . . . O21 O 0.3472(2) 0.5651(3) 0.60870(17) 0.0323(8) Uani 1 1 d . . . O22 O 0.4159(2) 0.3857(4) 0.66164(18) 0.0328(8) Uani 1 1 d . . . O23 O 0.4818(2) 0.5869(4) 0.6718(2) 0.0440(9) Uani 1 1 d . . . O31 O 0.1085(2) 0.3608(3) 0.60026(19) 0.0336(8) Uani 1 1 d . . . O32 O 0.1718(2) 0.5520(3) 0.58149(18) 0.0325(8) Uani 1 1 d . . . O33 O 0.0424(2) 0.5583(4) 0.6049(2) 0.0568(12) Uani 1 1 d . . . O1 O 0.17972(19) 0.1369(3) 0.54910(16) 0.0236(7) Uani 1 1 d . . . O2 O 0.35526(18) 0.1447(3) 0.59297(16) 0.0249(7) Uani 1 1 d . . . N1 N 0.3604(2) 0.3687(4) 0.4923(2) 0.0248(8) Uani 1 1 d . . . N2 N 0.1715(2) 0.3713(4) 0.4540(2) 0.0250(8) Uani 1 1 d . . . N4 N 0.3739(2) -0.0527(4) 0.69454(19) 0.0248(8) Uani 1 1 d . . . H4B H 0.3372 0.0062 0.6666 0.030 Uiso 1 1 calc R . . N3 N 0.1630(2) -0.0784(4) 0.6299(2) 0.0255(8) Uani 1 1 d . . . H3C H 0.1863 0.0055 0.6287 0.031 Uiso 1 1 calc R . . C1 C 0.3355(3) 0.4717(5) 0.4311(3) 0.0333(11) Uani 1 1 d . . . H1A H 0.3887 0.5253 0.4274 0.040 Uiso 1 1 calc R . . H1B H 0.3148 0.4197 0.3843 0.040 Uiso 1 1 calc R . . C2 C 0.2660(3) 0.5722(5) 0.4394(3) 0.0318(11) Uani 1 1 d . . . H2A H 0.2674 0.6539 0.4069 0.038 Uiso 1 1 calc R . . H2B H 0.2796 0.6069 0.4908 0.038 Uiso 1 1 calc R . . C3 C 0.1744(3) 0.5116(5) 0.4215(3) 0.0301(10) Uani 1 1 d . . . H3A H 0.1345 0.5755 0.4401 0.036 Uiso 1 1 calc R . . H3B H 0.1529 0.5051 0.3673 0.036 Uiso 1 1 calc R . . C4 C 0.1274(3) 0.2818(5) 0.4094(2) 0.0240(9) Uani 1 1 d . . . H4A H 0.1046 0.3143 0.3606 0.029 Uiso 1 1 calc R . . C5 C 0.1076(3) 0.1375(4) 0.4232(2) 0.0209(9) Uani 1 1 d . . . C6 C 0.0629(3) 0.0593(5) 0.3638(2) 0.0263(10) Uani 1 1 d . . . H6A H 0.0489 0.1025 0.3167 0.032 Uiso 1 1 calc R . . C7 C 0.0375(3) -0.0789(5) 0.3693(3) 0.0280(10) Uani 1 1 d . . . C8 C 0.0557(3) -0.1371(5) 0.4384(3) 0.0263(10) Uani 1 1 d . . . H8A H 0.0361 -0.2300 0.4443 0.032 Uiso 1 1 calc R . . C9 C 0.1024(3) -0.0637(5) 0.5008(2) 0.0220(9) Uani 1 1 d . . . C10 C 0.1326(3) 0.0747(5) 0.4940(2) 0.0217(9) Uani 1 1 d . . . C11 C 0.1183(3) -0.1321(4) 0.5690(3) 0.0247(10) Uani 1 1 d . . . H11A H 0.0948 -0.2238 0.5705 0.030 Uiso 1 1 calc R . . C12 C -0.0095(3) -0.1596(5) 0.3020(3) 0.0386(12) Uani 1 1 d . . . H12A H 0.0036 -0.2599 0.3096 0.058 Uiso 1 1 calc R . . H12B H 0.0107 -0.1267 0.2590 0.058 Uiso 1 1 calc R . . H12C H -0.0732 -0.1446 0.2938 0.058 Uiso 1 1 calc R . . C13 C 0.1767(3) -0.1502(5) 0.7006(3) 0.0303(11) Uani 1 1 d . . . H13A H 0.1296 -0.2211 0.6978 0.036 Uiso 1 1 calc R . . H13B H 0.1711 -0.0810 0.7388 0.036 Uiso 1 1 calc R . . C14 C 0.2656(3) -0.2225(5) 0.7242(2) 0.0287(10) Uani 1 1 d . . . H14A H 0.2624 -0.2906 0.7636 0.034 Uiso 1 1 calc R . . H14B H 0.2759 -0.2767 0.6818 0.034 Uiso 1 1 calc R . . C15 C 0.3443(3) -0.1288(5) 0.7519(2) 0.0304(11) Uani 1 1 d . . . H15A H 0.3293 -0.0600 0.7868 0.036 Uiso 1 1 calc R . . H15B H 0.3937 -0.1869 0.7795 0.036 Uiso 1 1 calc R . . C16 C 0.4519(3) -0.0680(5) 0.6829(2) 0.0269(10) Uani 1 1 d . . . H16A H 0.4887 -0.1391 0.7096 0.032 Uiso 1 1 calc R . . C17 C 0.4860(3) 0.0148(5) 0.6329(2) 0.0245(9) Uani 1 1 d . . . C20 C 0.5621(3) 0.1646(5) 0.5392(2) 0.0274(10) Uani 1 1 d . . . H20A H 0.5879 0.2150 0.5056 0.033 Uiso 1 1 calc R . . C18 C 0.5728(3) -0.0120(5) 0.6281(2) 0.0296(10) Uani 1 1 d . . . H18A H 0.6054 -0.0833 0.6582 0.036 Uiso 1 1 calc R . . C19 C 0.6119(3) 0.0613(5) 0.5814(3) 0.0277(10) Uani 1 1 d . . . C21 C 0.4772(3) 0.1992(4) 0.5427(2) 0.0237(10) Uani 1 1 d . . . C22 C 0.4358(3) 0.1220(5) 0.5898(2) 0.0225(9) Uani 1 1 d . . . C23 C 0.4338(3) 0.3081(5) 0.4938(2) 0.0270(10) Uani 1 1 d . . . H23A H 0.4638 0.3388 0.4579 0.032 Uiso 1 1 calc R . . C24 C 0.7045(3) 0.0280(5) 0.5750(3) 0.0364(12) Uani 1 1 d . . . H24A H 0.7465 0.0571 0.6202 0.055 Uiso 1 1 calc R . . H24B H 0.7170 0.0786 0.5329 0.055 Uiso 1 1 calc R . . H24C H 0.7100 -0.0732 0.5679 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.02143(11) 0.01844(11) 0.02197(11) -0.00003(9) 0.00340(7) 0.00138(9) N10 0.026(2) 0.032(2) 0.026(2) -0.0038(18) 0.0056(17) -0.0026(17) N20 0.028(2) 0.033(2) 0.027(2) -0.0046(19) 0.0019(17) 0.0016(19) N30 0.031(2) 0.027(2) 0.051(3) 0.001(2) 0.014(2) 0.0004(19) O11 0.045(2) 0.0255(19) 0.0305(18) -0.0018(15) 0.0088(16) -0.0064(16) O12 0.0305(17) 0.0250(18) 0.0267(17) -0.0030(14) 0.0092(14) 0.0018(13) O13 0.065(3) 0.048(2) 0.0273(19) 0.0015(17) 0.0224(18) -0.001(2) O21 0.0296(18) 0.032(2) 0.0331(19) -0.0028(15) 0.0017(15) 0.0022(15) O22 0.0349(19) 0.0272(19) 0.0338(19) -0.0018(15) 0.0031(15) 0.0013(15) O23 0.034(2) 0.043(2) 0.049(2) -0.0002(19) -0.0030(17) -0.0087(18) O31 0.0291(18) 0.0229(19) 0.049(2) -0.0012(15) 0.0085(16) -0.0036(14) O32 0.0247(17) 0.0279(19) 0.046(2) 0.0041(16) 0.0107(15) 0.0010(14) O33 0.031(2) 0.034(2) 0.115(4) 0.002(2) 0.037(2) 0.0069(17) O1 0.0244(16) 0.0217(17) 0.0229(16) 0.0023(13) 0.0019(13) -0.0024(13) O2 0.0203(15) 0.0254(18) 0.0295(16) 0.0034(14) 0.0068(13) 0.0046(13) N1 0.0234(19) 0.025(2) 0.025(2) 0.0052(16) 0.0037(16) -0.0023(16) N2 0.0197(19) 0.023(2) 0.032(2) 0.0028(17) 0.0066(16) 0.0020(15) N4 0.0244(19) 0.026(2) 0.0228(19) 0.0050(16) 0.0034(16) 0.0033(16) N3 0.025(2) 0.021(2) 0.030(2) 0.0042(17) 0.0061(17) 0.0003(16) C1 0.033(3) 0.038(3) 0.030(3) 0.012(2) 0.011(2) -0.001(2) C2 0.037(3) 0.025(3) 0.032(3) 0.007(2) 0.006(2) -0.003(2) C3 0.033(3) 0.022(2) 0.033(3) 0.006(2) 0.004(2) 0.002(2) C4 0.021(2) 0.026(2) 0.025(2) 0.0004(19) 0.0040(19) 0.0031(18) C5 0.015(2) 0.023(2) 0.024(2) -0.0013(18) 0.0049(17) 0.0001(17) C6 0.021(2) 0.032(3) 0.024(2) 0.001(2) 0.0022(18) 0.0046(19) C7 0.023(2) 0.030(3) 0.031(3) -0.009(2) 0.008(2) -0.003(2) C8 0.023(2) 0.020(2) 0.038(3) -0.005(2) 0.010(2) -0.0004(18) C9 0.017(2) 0.025(2) 0.024(2) -0.0018(19) 0.0058(18) 0.0018(18) C10 0.014(2) 0.023(2) 0.029(2) -0.0056(19) 0.0061(18) -0.0009(17) C11 0.021(2) 0.017(2) 0.036(3) -0.0011(19) 0.008(2) -0.0003(17) C12 0.040(3) 0.041(3) 0.033(3) -0.009(3) 0.005(2) -0.005(3) C13 0.030(2) 0.031(3) 0.031(2) 0.003(2) 0.008(2) -0.001(2) C14 0.034(3) 0.029(3) 0.022(2) 0.004(2) 0.006(2) 0.002(2) C15 0.038(3) 0.030(3) 0.023(2) 0.004(2) 0.007(2) 0.002(2) C16 0.028(2) 0.024(3) 0.025(2) -0.0032(19) -0.0013(19) 0.004(2) C17 0.021(2) 0.026(2) 0.024(2) -0.003(2) 0.0009(18) 0.0012(19) C20 0.026(2) 0.030(3) 0.027(2) -0.005(2) 0.0066(19) -0.005(2) C18 0.021(2) 0.031(3) 0.033(3) -0.007(2) -0.0006(19) 0.004(2) C19 0.023(2) 0.027(3) 0.033(3) -0.010(2) 0.005(2) 0.0012(19) C21 0.023(2) 0.023(2) 0.026(2) -0.0021(18) 0.0063(19) -0.0021(18) C22 0.024(2) 0.022(2) 0.021(2) -0.0071(18) 0.0043(18) -0.0009(18) C23 0.026(2) 0.029(3) 0.026(2) -0.003(2) 0.0081(19) -0.006(2) C24 0.025(2) 0.037(3) 0.047(3) -0.005(2) 0.010(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O2 2.282(3) . ? Ho1 O1 2.289(3) . ? Ho1 O12 2.459(3) . ? Ho1 O32 2.517(3) . ? Ho1 O31 2.523(3) . ? Ho1 N2 2.526(4) . ? Ho1 O22 2.532(3) . ? Ho1 N1 2.545(3) . ? Ho1 O21 2.548(3) . ? Ho1 O11 2.571(3) . ? N10 O13 1.204(5) . ? N10 O11 1.252(5) . ? N10 O12 1.270(4) . ? N20 O23 1.216(5) . ? N20 O21 1.256(5) . ? N20 O22 1.259(5) . ? N30 O33 1.209(5) . ? N30 O31 1.251(5) . ? N30 O32 1.269(5) . ? O1 C10 1.263(5) . ? O2 C22 1.290(5) . ? N1 C23 1.275(6) . ? N1 C1 1.487(5) . ? N2 C4 1.274(5) . ? N2 C3 1.473(5) . ? N4 C16 1.293(5) . ? N4 C15 1.455(5) . ? N3 C11 1.293(5) . ? N3 C13 1.457(5) . ? C1 C2 1.481(6) . ? C2 C3 1.504(6) . ? C4 C5 1.444(6) . ? C5 C6 1.381(6) . ? C5 C10 1.420(6) . ? C6 C7 1.384(6) . ? C7 C8 1.371(6) . ? C7 C12 1.508(6) . ? C8 C9 1.408(6) . ? C9 C11 1.398(6) . ? C9 C10 1.416(6) . ? C13 C14 1.518(6) . ? C14 C15 1.507(6) . ? C16 C17 1.417(6) . ? C17 C18 1.400(6) . ? C17 C22 1.417(6) . ? C20 C19 1.379(6) . ? C20 C21 1.382(6) . ? C18 C19 1.367(6) . ? C19 C24 1.509(6) . ? C21 C22 1.412(6) . ? C21 C23 1.441(6) . ? 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 O2 Ho1 O1 71.44(11) . . ? O2 Ho1 O12 70.55(10) . . ? O1 Ho1 O12 68.81(10) . . ? O2 Ho1 O32 175.03(11) . . ? O1 Ho1 O32 112.79(10) . . ? O12 Ho1 O32 108.12(10) . . ? O2 Ho1 O31 132.18(10) . . ? O1 Ho1 O31 67.51(10) . . ? O12 Ho1 O31 72.54(10) . . ? O32 Ho1 O31 50.21(10) . . ? O2 Ho1 N2 113.16(11) . . ? O1 Ho1 N2 71.99(11) . . ? O12 Ho1 N2 136.70(11) . . ? O32 Ho1 N2 71.21(11) . . ? O31 Ho1 N2 76.11(11) . . ? O2 Ho1 O22 67.70(11) . . ? O1 Ho1 O22 135.85(11) . . ? O12 Ho1 O22 82.31(10) . . ? O32 Ho1 O22 107.48(11) . . ? O31 Ho1 O22 134.79(11) . . ? N2 Ho1 O22 140.46(11) . . ? O2 Ho1 N1 72.32(11) . . ? O1 Ho1 N1 108.10(11) . . ? O12 Ho1 N1 141.55(11) . . ? O32 Ho1 N1 107.99(11) . . ? O31 Ho1 N1 143.83(11) . . ? N2 Ho1 N1 68.80(11) . . ? O22 Ho1 N1 74.70(11) . . ? O2 Ho1 O21 112.49(11) . . ? O1 Ho1 O21 173.96(10) . . ? O12 Ho1 O21 116.54(10) . . ? O32 Ho1 O21 63.53(10) . . ? O31 Ho1 O21 110.67(10) . . ? N2 Ho1 O21 102.03(11) . . ? O22 Ho1 O21 49.65(10) . . ? N1 Ho1 O21 69.73(11) . . ? O2 Ho1 O11 108.52(11) . . ? O1 Ho1 O11 111.04(10) . . ? O12 Ho1 O11 50.07(10) . . ? O32 Ho1 O11 67.83(11) . . ? O31 Ho1 O11 66.55(11) . . ? N2 Ho1 O11 136.37(11) . . ? O22 Ho1 O11 68.46(10) . . ? N1 Ho1 O11 138.77(11) . . ? O21 Ho1 O11 72.53(10) . . ? O13 N10 O11 123.2(4) . . ? O13 N10 O12 121.4(4) . . ? O11 N10 O12 115.4(4) . . ? O23 N20 O21 122.1(4) . . ? O23 N20 O22 121.8(4) . . ? O21 N20 O22 116.1(4) . . ? O33 N30 O31 122.4(4) . . ? O33 N30 O32 121.6(4) . . ? O31 N30 O32 116.1(4) . . ? N10 O11 Ho1 94.7(2) . . ? N10 O12 Ho1 99.6(2) . . ? N20 O21 Ho1 96.7(3) . . ? N20 O22 Ho1 97.4(3) . . ? N30 O31 Ho1 96.9(2) . . ? N30 O32 Ho1 96.7(3) . . ? C10 O1 Ho1 142.8(3) . . ? C22 O2 Ho1 136.8(3) . . ? C23 N1 C1 112.8(4) . . ? C23 N1 Ho1 126.6(3) . . ? C1 N1 Ho1 120.6(3) . . ? C4 N2 C3 113.7(4) . . ? C4 N2 Ho1 128.9(3) . . ? C3 N2 Ho1 117.1(3) . . ? C16 N4 C15 122.7(4) . . ? C11 N3 C13 123.1(4) . . ? C2 C1 N1 114.3(4) . . ? C1 C2 C3 114.1(4) . . ? N2 C3 C2 112.1(4) . . ? N2 C4 C5 128.7(4) . . ? C6 C5 C10 119.8(4) . . ? C6 C5 C4 117.3(4) . . ? C10 C5 C4 122.8(4) . . ? C5 C6 C7 123.6(4) . . ? C8 C7 C6 117.0(4) . . ? C8 C7 C12 122.0(4) . . ? C6 C7 C12 121.0(4) . . ? C7 C8 C9 122.1(4) . . ? C11 C9 C8 118.0(4) . . ? C11 C9 C10 121.6(4) . . ? C8 C9 C10 120.4(4) . . ? O1 C10 C9 120.4(4) . . ? O1 C10 C5 122.8(4) . . ? C9 C10 C5 116.8(4) . . ? N3 C11 C9 124.1(4) . . ? N3 C13 C14 114.0(4) . . ? C15 C14 C13 116.5(4) . . ? N4 C15 C14 114.6(4) . . ? N4 C16 C17 124.1(4) . . ? C18 C17 C22 120.6(4) . . ? C18 C17 C16 117.3(4) . . ? C22 C17 C16 122.1(4) . . ? C19 C20 C21 124.1(4) . . ? C19 C18 C17 122.0(4) . . ? C18 C19 C20 116.9(4) . . ? C18 C19 C24 121.4(4) . . ? C20 C19 C24 121.7(4) . . ? C20 C21 C22 119.2(4) . . ? C20 C21 C23 117.1(4) . . ? C22 C21 C23 123.6(4) . . ? O2 C22 C21 122.2(4) . . ? O2 C22 C17 120.6(4) . . ? C21 C22 C17 117.1(4) . . ? N1 C23 C21 128.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 N10 O11 Ho1 -175.9(4) . . . . ? O12 N10 O11 Ho1 4.4(4) . . . . ? O2 Ho1 O11 N10 -45.1(3) . . . . ? O1 Ho1 O11 N10 31.5(3) . . . . ? O12 Ho1 O11 N10 -2.7(2) . . . . ? O32 Ho1 O11 N10 138.5(3) . . . . ? O31 Ho1 O11 N10 83.7(2) . . . . ? N2 Ho1 O11 N10 117.1(3) . . . . ? O22 Ho1 O11 N10 -100.9(3) . . . . ? N1 Ho1 O11 N10 -129.2(2) . . . . ? O21 Ho1 O11 N10 -153.6(3) . . . . ? O13 N10 O12 Ho1 175.6(4) . . . . ? O11 N10 O12 Ho1 -4.7(4) . . . . ? O2 Ho1 O12 N10 140.0(3) . . . . ? O1 Ho1 O12 N10 -143.1(3) . . . . ? O32 Ho1 O12 N10 -35.0(3) . . . . ? O31 Ho1 O12 N10 -71.0(2) . . . . ? N2 Ho1 O12 N10 -116.5(3) . . . . ? O22 Ho1 O12 N10 71.0(2) . . . . ? N1 Ho1 O12 N10 124.2(3) . . . . ? O21 Ho1 O12 N10 33.9(3) . . . . ? O11 Ho1 O12 N10 2.7(2) . . . . ? O23 N20 O21 Ho1 175.9(4) . . . . ? O22 N20 O21 Ho1 -3.7(4) . . . . ? O2 Ho1 O21 N20 -24.9(3) . . . . ? O1 Ho1 O21 N20 -154.6(9) . . . . ? O12 Ho1 O21 N20 53.8(3) . . . . ? O32 Ho1 O21 N20 151.8(3) . . . . ? O31 Ho1 O21 N20 134.0(2) . . . . ? N2 Ho1 O21 N20 -146.5(2) . . . . ? O22 Ho1 O21 N20 2.1(2) . . . . ? N1 Ho1 O21 N20 -84.7(2) . . . . ? O11 Ho1 O21 N20 78.4(2) . . . . ? O23 N20 O22 Ho1 -175.8(4) . . . . ? O21 N20 O22 Ho1 3.7(4) . . . . ? O2 Ho1 O22 N20 150.9(3) . . . . ? O1 Ho1 O22 N20 174.4(2) . . . . ? O12 Ho1 O22 N20 -137.1(2) . . . . ? O32 Ho1 O22 N20 -30.4(3) . . . . ? O31 Ho1 O22 N20 -81.2(3) . . . . ? N2 Ho1 O22 N20 51.0(3) . . . . ? N1 Ho1 O22 N20 74.0(2) . . . . ? O21 Ho1 O22 N20 -2.1(2) . . . . ? O11 Ho1 O22 N20 -87.1(2) . . . . ? O33 N30 O31 Ho1 -175.5(4) . . . . ? O32 N30 O31 Ho1 3.5(4) . . . . ? O2 Ho1 O31 N30 172.2(2) . . . . ? O1 Ho1 O31 N30 -155.0(3) . . . . ? O12 Ho1 O31 N30 131.3(3) . . . . ? O32 Ho1 O31 N30 -2.0(2) . . . . ? N2 Ho1 O31 N30 -79.0(3) . . . . ? O22 Ho1 O31 N30 71.9(3) . . . . ? N1 Ho1 O31 N30 -64.8(3) . . . . ? O21 Ho1 O31 N30 18.8(3) . . . . ? O11 Ho1 O31 N30 77.9(3) . . . . ? O33 N30 O32 Ho1 175.5(4) . . . . ? O31 N30 O32 Ho1 -3.5(4) . . . . ? O2 Ho1 O32 N30 -118.6(11) . . . . ? O1 Ho1 O32 N30 29.2(3) . . . . ? O12 Ho1 O32 N30 -44.9(3) . . . . ? O31 Ho1 O32 N30 2.0(2) . . . . ? N2 Ho1 O32 N30 89.4(3) . . . . ? O22 Ho1 O32 N30 -132.3(3) . . . . ? N1 Ho1 O32 N30 148.5(3) . . . . ? O21 Ho1 O32 N30 -156.1(3) . . . . ? O11 Ho1 O32 N30 -75.3(3) . . . . ? O2 Ho1 O1 C10 -108.6(4) . . . . ? O12 Ho1 O1 C10 175.7(5) . . . . ? O32 Ho1 O1 C10 74.2(4) . . . . ? O31 Ho1 O1 C10 96.5(4) . . . . ? N2 Ho1 O1 C10 14.4(4) . . . . ? O22 Ho1 O1 C10 -131.6(4) . . . . ? N1 Ho1 O1 C10 -45.1(4) . . . . ? O21 Ho1 O1 C10 22.8(12) . . . . ? O11 Ho1 O1 C10 148.1(4) . . . . ? O1 Ho1 O2 C22 153.3(4) . . . . ? O12 Ho1 O2 C22 -133.3(4) . . . . ? O32 Ho1 O2 C22 -58.0(13) . . . . ? O31 Ho1 O2 C22 -174.8(4) . . . . ? N2 Ho1 O2 C22 93.2(4) . . . . ? O22 Ho1 O2 C22 -43.8(4) . . . . ? N1 Ho1 O2 C22 36.5(4) . . . . ? O21 Ho1 O2 C22 -21.8(4) . . . . ? O11 Ho1 O2 C22 -100.1(4) . . . . ? O2 Ho1 N1 C23 -19.6(4) . . . . ? O1 Ho1 N1 C23 -82.5(4) . . . . ? O12 Ho1 N1 C23 -4.0(5) . . . . ? O32 Ho1 N1 C23 155.2(4) . . . . ? O31 Ho1 N1 C23 -158.9(3) . . . . ? N2 Ho1 N1 C23 -144.1(4) . . . . ? O22 Ho1 N1 C23 51.4(4) . . . . ? O21 Ho1 N1 C23 103.5(4) . . . . ? O11 Ho1 N1 C23 78.6(4) . . . . ? O2 Ho1 N1 C1 162.7(3) . . . . ? O1 Ho1 N1 C1 99.8(3) . . . . ? O12 Ho1 N1 C1 178.3(3) . . . . ? O32 Ho1 N1 C1 -22.5(3) . . . . ? O31 Ho1 N1 C1 23.4(4) . . . . ? N2 Ho1 N1 C1 38.2(3) . . . . ? O22 Ho1 N1 C1 -126.3(3) . . . . ? O21 Ho1 N1 C1 -74.2(3) . . . . ? O11 Ho1 N1 C1 -99.1(3) . . . . ? O2 Ho1 N2 C4 46.7(4) . . . . ? O1 Ho1 N2 C4 -13.1(3) . . . . ? O12 Ho1 N2 C4 -39.0(4) . . . . ? O32 Ho1 N2 C4 -135.8(4) . . . . ? O31 Ho1 N2 C4 -83.6(4) . . . . ? O22 Ho1 N2 C4 129.2(3) . . . . ? N1 Ho1 N2 C4 105.4(4) . . . . ? O21 Ho1 N2 C4 167.8(3) . . . . ? O11 Ho1 N2 C4 -115.0(3) . . . . ? O2 Ho1 N2 C3 -126.8(3) . . . . ? O1 Ho1 N2 C3 173.4(3) . . . . ? O12 Ho1 N2 C3 147.4(3) . . . . ? O32 Ho1 N2 C3 50.6(3) . . . . ? O31 Ho1 N2 C3 102.9(3) . . . . ? O22 Ho1 N2 C3 -44.3(4) . . . . ? N1 Ho1 N2 C3 -68.2(3) . . . . ? O21 Ho1 N2 C3 -5.7(3) . . . . ? O11 Ho1 N2 C3 71.5(3) . . . . ? C23 N1 C1 C2 -163.3(4) . . . . ? Ho1 N1 C1 C2 14.6(5) . . . . ? N1 C1 C2 C3 -77.1(5) . . . . ? C4 N2 C3 C2 -134.1(4) . . . . ? Ho1 N2 C3 C2 40.5(5) . . . . ? C1 C2 C3 N2 44.6(5) . . . . ? C3 N2 C4 C5 -177.0(4) . . . . ? Ho1 N2 C4 C5 9.3(6) . . . . ? N2 C4 C5 C6 -176.0(4) . . . . ? N2 C4 C5 C10 3.5(7) . . . . ? C10 C5 C6 C7 2.4(6) . . . . ? C4 C5 C6 C7 -178.1(4) . . . . ? C5 C6 C7 C8 2.3(6) . . . . ? C5 C6 C7 C12 -178.7(4) . . . . ? C6 C7 C8 C9 -3.5(6) . . . . ? C12 C7 C8 C9 177.5(4) . . . . ? C7 C8 C9 C11 -179.6(4) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? Ho1 O1 C10 C9 170.9(3) . . . . ? Ho1 O1 C10 C5 -8.8(7) . . . . ? C11 C9 C10 O1 4.5(6) . . . . ? C8 C9 C10 O1 -175.1(4) . . . . ? C11 C9 C10 C5 -175.8(4) . . . . ? C8 C9 C10 C5 4.6(6) . . . . ? C6 C5 C10 O1 174.0(4) . . . . ? C4 C5 C10 O1 -5.4(6) . . . . ? C6 C5 C10 C9 -5.7(6) . . . . ? C4 C5 C10 C9 174.8(4) . . . . ? C13 N3 C11 C9 178.3(4) . . . . ? C8 C9 C11 N3 177.5(4) . . . . ? C10 C9 C11 N3 -2.1(6) . . . . ? C11 N3 C13 C14 99.2(5) . . . . ? N3 C13 C14 C15 74.9(5) . . . . ? C16 N4 C15 C14 -119.2(5) . . . . ? C13 C14 C15 N4 -75.8(5) . . . . ? C15 N4 C16 C17 -173.2(4) . . . . ? N4 C16 C17 C18 178.2(4) . . . . ? N4 C16 C17 C22 -0.9(7) . . . . ? C22 C17 C18 C19 -1.1(7) . . . . ? C16 C17 C18 C19 179.7(4) . . . . ? C17 C18 C19 C20 0.5(7) . . . . ? C17 C18 C19 C24 -178.0(4) . . . . ? C21 C20 C19 C18 1.4(7) . . . . ? C21 C20 C19 C24 179.9(4) . . . . ? C19 C20 C21 C22 -2.7(7) . . . . ? C19 C20 C21 C23 -178.9(4) . . . . ? Ho1 O2 C22 C21 -34.1(6) . . . . ? Ho1 O2 C22 C17 147.3(3) . . . . ? C20 C21 C22 O2 -176.6(4) . . . . ? C23 C21 C22 O2 -0.7(7) . . . . ? C20 C21 C22 C17 1.9(6) . . . . ? C23 C21 C22 C17 177.8(4) . . . . ? C18 C17 C22 O2 178.5(4) . . . . ? C16 C17 C22 O2 -2.4(7) . . . . ? C18 C17 C22 C21 -0.1(6) . . . . ? C16 C17 C22 C21 179.0(4) . . . . ? C1 N1 C23 C21 -177.3(4) . . . . ? Ho1 N1 C23 C21 4.9(7) . . . . ? C20 C21 C23 N1 -171.5(5) . . . . ? C22 C21 C23 N1 12.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.623 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.210 data_14 _database_code_depnum_ccdc_archive 'CCDC 289608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Lu N7 O12' _chemical_formula_weight 783.52 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6659(8) _cell_length_b 10.0860(8) _cell_length_c 15.6100(13) _cell_angle_alpha 94.750(2) _cell_angle_beta 105.067(2) _cell_angle_gamma 97.636(2) _cell_volume 1445.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2064 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 20.18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 3.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 2091 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14662 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1376 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6874 _reflns_number_gt 4316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXTL (Bruker, 2002)' _computing_structure_refinement 'SHELXTL (Bruker, 2002)' _computing_molecular_graphics 'SHELXTL (Bruker, 2002)' _computing_publication_material 'SHELXTL (Bruker, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6874 _refine_ls_number_parameters 403 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.923 _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 Lu1 Lu 0.81435(4) 0.79642(3) 0.25351(2) 0.04107(12) Uani 1 1 d . . . O1 O 0.7819(5) 0.6344(4) 0.1444(3) 0.0446(12) Uani 1 1 d . A . O2 O 0.8660(5) 0.6231(4) 0.3269(3) 0.0462(12) Uani 1 1 d . A . N101 N 0.8351(17) 0.9960(15) 0.3945(10) 0.057(4) Uiso 0.50 1 d P A 1 O111 O 0.8380(13) 0.8729(11) 0.4098(7) 0.053(3) Uiso 0.50 1 d P A 1 O121 O 0.8237(15) 1.0793(12) 0.4528(9) 0.080(4) Uiso 0.50 1 d P A 1 N102 N 0.7519(17) 0.9853(15) 0.3775(10) 0.056(4) Uiso 0.50 1 d P A 2 O112 O 0.7594(13) 0.8648(11) 0.3916(7) 0.053(3) Uiso 0.50 1 d P A 2 O122 O 0.7190(13) 1.0647(11) 0.4297(8) 0.063(3) Uiso 0.50 1 d P A 2 O13 O 0.8101(8) 1.0201(5) 0.3126(4) 0.082(2) Uani 1 1 d . A . N20 N 0.6917(8) 0.0565(7) -0.0301(5) 0.064(2) Uani 1 1 d . . . O211 O 0.7202(17) 0.1038(14) 0.0510(10) 0.089(4) Uiso 0.50 1 d P B 3 O212 O 0.6346(14) 0.0831(12) 0.0331(9) 0.067(3) Uiso 0.50 1 d P B 4 O22 O 0.7537(7) -0.0420(6) -0.0345(5) 0.087(2) Uani 1 1 d . B . O23 O 0.6539(6) 0.1165(5) -0.0970(4) 0.0696(16) Uani 1 1 d . B . N30 N 0.4969(10) 0.6974(7) 0.2775(4) 0.070(2) Uani 1 1 d D . . O31 O 0.5908(9) 0.6550(6) 0.2443(4) 0.077(2) Uani 1 1 d . A . O321 O 0.5346(17) 0.8292(12) 0.2945(9) 0.084(4) Uiso 0.50 1 d PD A 5 O331 O 0.3946(14) 0.6455(16) 0.2951(10) 0.080(5) Uiso 0.50 1 d PD A 5 O322 O 0.4538(19) 0.8032(15) 0.2804(11) 0.107(6) Uiso 0.50 1 d PD A 6 O332 O 0.4250(16) 0.5929(14) 0.2968(10) 0.084(5) Uiso 0.50 1 d PD A 6 N1 N 0.9538(7) 0.8913(5) 0.1594(4) 0.0481(16) Uani 1 1 d . A . N2 N 1.0755(8) 0.8550(6) 0.3430(4) 0.0553(18) Uani 1 1 d . A . N3 N 0.6917(7) 0.3960(6) 0.3171(4) 0.0453(15) Uani 1 1 d . A . H3C H 0.6961 0.4808 0.3069 0.054 Uiso 1 1 calc R . . N4 N 0.5958(6) 0.4078(6) 0.1029(4) 0.0456(15) Uani 1 1 d . A . H4B H 0.6353 0.4774 0.1439 0.055 Uiso 1 1 calc R . . C1 C 1.0326(9) 1.0314(7) 0.1885(5) 0.060(2) Uani 1 1 d . . . H1A H 0.9686 1.0878 0.2095 0.072 Uiso 1 1 calc R A . H1B H 1.0578 1.0695 0.1371 0.072 Uiso 1 1 calc R . . C2 C 1.1697(10) 1.0350(8) 0.2631(5) 0.068(3) Uani 1 1 d . A . H2A H 1.2256 1.1274 0.2745 0.082 Uiso 1 1 calc R . . H2B H 1.2298 0.9738 0.2425 0.082 Uiso 1 1 calc R . . C3 C 1.1462(10) 0.9954(7) 0.3503(5) 0.072(3) Uani 1 1 d . . . H3A H 1.2412 1.0084 0.3960 0.087 Uiso 1 1 calc R A . H3B H 1.0857 1.0559 0.3711 0.087 Uiso 1 1 calc R . . C4 C 1.1586(9) 0.7771(7) 0.3823(4) 0.049(2) Uani 1 1 d . . . H4A H 1.2576 0.8157 0.4074 0.059 Uiso 1 1 calc R A . C5 C 1.1199(8) 0.6369(7) 0.3931(4) 0.0410(18) Uani 1 1 d . A . C6 C 1.2289(8) 0.5695(7) 0.4336(4) 0.0443(18) Uani 1 1 d . . . H6A H 1.3254 0.6171 0.4528 0.053 Uiso 1 1 calc R A . C7 C 1.2048(8) 0.4354(7) 0.4480(4) 0.0401(17) Uani 1 1 d . A . C8 C 1.0673(8) 0.3710(7) 0.4246(4) 0.0401(17) Uani 1 1 d . . . H8A H 1.0490 0.2803 0.4364 0.048 Uiso 1 1 calc R A . C9 C 0.9506(8) 0.4322(6) 0.3836(4) 0.0335(16) Uani 1 1 d . A . C10 C 0.9761(8) 0.5665(7) 0.3667(4) 0.0386(17) Uani 1 1 d . . . C11 C 0.8103(8) 0.3560(7) 0.3570(4) 0.0423(18) Uani 1 1 d . . . H11A H 0.8021 0.2653 0.3699 0.051 Uiso 1 1 calc R A . C12 C 1.3322(8) 0.3681(7) 0.4908(5) 0.056(2) Uani 1 1 d . . . H12A H 1.2964 0.2823 0.5089 0.084 Uiso 1 1 calc R A . H12B H 1.3949 0.4270 0.5434 0.084 Uiso 1 1 calc R . . H12C H 1.3877 0.3514 0.4477 0.084 Uiso 1 1 calc R . . C13 C 0.5519(8) 0.3100(7) 0.2882(4) 0.0497(19) Uani 1 1 d . . . H13A H 0.4748 0.3658 0.2875 0.060 Uiso 1 1 calc R A . H13B H 0.5464 0.2447 0.3316 0.060 Uiso 1 1 calc R . . C14 C 0.5241(9) 0.2326(7) 0.1947(5) 0.057(2) Uani 1 1 d . A . H14A H 0.6136 0.1971 0.1914 0.068 Uiso 1 1 calc R . . H14B H 0.4470 0.1542 0.1878 0.068 Uiso 1 1 calc R . . C15 C 0.4804(9) 0.3112(8) 0.1174(5) 0.057(2) Uani 1 1 d . . . H15A H 0.4391 0.2467 0.0624 0.068 Uiso 1 1 calc R A . H15B H 0.4023 0.3604 0.1266 0.068 Uiso 1 1 calc R . . C16 C 0.6428(8) 0.3962(7) 0.0327(5) 0.0481(19) Uani 1 1 d . . . H16A H 0.6043 0.3166 -0.0081 0.058 Uiso 1 1 calc R A . C17 C 0.7468(8) 0.4915(7) 0.0109(4) 0.0387(16) Uani 1 1 d . A . C18 C 0.7828(8) 0.4649(7) -0.0702(4) 0.0447(18) Uani 1 1 d . . . H18A H 0.7402 0.3820 -0.1069 0.054 Uiso 1 1 calc R A . C19 C 0.8757(8) 0.5532(7) -0.0977(4) 0.0372(16) Uani 1 1 d . A . C20 C 0.9323(8) 0.6722(7) -0.0434(4) 0.0447(18) Uani 1 1 d . . . H20A H 0.9954 0.7362 -0.0627 0.054 Uiso 1 1 calc R A . C21 C 0.9040(8) 0.7062(7) 0.0383(4) 0.0403(17) Uani 1 1 d . A . C22 C 0.8092(8) 0.6132(7) 0.0680(5) 0.0432(18) Uani 1 1 d . . . C23 C 0.9698(8) 0.8380(7) 0.0852(5) 0.0464(18) Uani 1 1 d . . . H23A H 1.0317 0.8915 0.0586 0.056 Uiso 1 1 calc R A . C24 C 0.9088(8) 0.5250(7) -0.1858(4) 0.053(2) Uani 1 1 d . . . H24A H 0.8937 0.4274 -0.2030 0.079 Uiso 1 1 calc R A . H24B H 1.0100 0.5629 -0.1801 0.079 Uiso 1 1 calc R . . H24C H 0.8443 0.5663 -0.2316 0.079 Uiso 1 1 calc R . . O100 O 0.6535(6) 0.8829(5) 0.1437(3) 0.0571(14) Uani 1 1 d . A . 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 Lu1 0.0658(2) 0.03076(17) 0.03270(16) 0.00710(12) 0.02073(15) 0.01265(15) O1 0.060(3) 0.042(3) 0.034(3) 0.001(2) 0.018(2) 0.006(2) O2 0.063(3) 0.039(3) 0.036(3) 0.008(2) 0.012(2) 0.005(3) O13 0.158(6) 0.057(4) 0.050(3) 0.020(3) 0.054(4) 0.031(4) N20 0.083(6) 0.049(4) 0.061(5) 0.005(4) 0.021(4) 0.010(4) O22 0.064(4) 0.066(4) 0.125(6) 0.030(4) 0.008(4) 0.018(4) O23 0.086(5) 0.063(4) 0.066(4) 0.024(3) 0.023(3) 0.020(3) N30 0.094(7) 0.069(6) 0.051(4) 0.021(4) 0.014(4) 0.030(5) O31 0.089(6) 0.093(5) 0.069(4) 0.016(4) 0.043(4) 0.039(4) N1 0.069(5) 0.039(3) 0.040(3) 0.016(3) 0.018(3) 0.007(3) N2 0.096(6) 0.034(3) 0.031(3) 0.007(3) 0.018(3) -0.009(4) N3 0.055(4) 0.043(4) 0.039(3) 0.000(3) 0.020(3) -0.001(3) N4 0.052(4) 0.046(4) 0.037(3) 0.002(3) 0.014(3) -0.001(3) C1 0.098(7) 0.031(4) 0.059(5) 0.014(4) 0.035(5) 0.006(4) C2 0.097(7) 0.043(5) 0.057(5) 0.009(4) 0.016(5) -0.007(5) C3 0.113(8) 0.037(4) 0.050(5) 0.010(4) 0.005(5) -0.016(5) C4 0.068(6) 0.041(4) 0.035(4) 0.004(3) 0.017(4) -0.005(4) C5 0.059(5) 0.039(4) 0.026(3) 0.003(3) 0.019(3) -0.003(4) C6 0.050(5) 0.055(5) 0.027(3) 0.004(3) 0.017(3) -0.005(4) C7 0.055(5) 0.038(4) 0.033(4) 0.005(3) 0.022(3) 0.006(4) C8 0.052(5) 0.033(4) 0.039(4) 0.003(3) 0.019(4) 0.009(4) C9 0.055(5) 0.028(3) 0.022(3) 0.004(3) 0.018(3) 0.004(3) C10 0.056(5) 0.039(4) 0.025(3) -0.002(3) 0.015(3) 0.013(4) C11 0.058(5) 0.040(4) 0.029(4) 0.002(3) 0.014(4) 0.006(4) C12 0.067(6) 0.052(5) 0.057(5) 0.014(4) 0.028(4) 0.009(4) C13 0.046(5) 0.062(5) 0.039(4) 0.012(4) 0.012(4) -0.001(4) C14 0.060(5) 0.059(5) 0.047(4) 0.013(4) 0.010(4) -0.004(4) C15 0.057(5) 0.061(5) 0.047(4) 0.009(4) 0.009(4) -0.001(4) C16 0.055(5) 0.047(4) 0.040(4) 0.002(3) 0.007(4) 0.015(4) C17 0.041(4) 0.039(4) 0.037(4) 0.006(3) 0.008(3) 0.014(3) C18 0.060(5) 0.043(4) 0.035(4) 0.007(3) 0.013(4) 0.025(4) C19 0.049(5) 0.044(4) 0.029(3) 0.016(3) 0.019(3) 0.019(4) C20 0.048(5) 0.051(4) 0.044(4) 0.022(4) 0.018(4) 0.019(4) C21 0.048(5) 0.044(4) 0.031(4) 0.010(3) 0.010(3) 0.018(4) C22 0.058(5) 0.038(4) 0.042(4) 0.012(3) 0.019(4) 0.019(4) C23 0.055(5) 0.046(4) 0.044(4) 0.022(3) 0.017(4) 0.013(4) C24 0.064(5) 0.071(5) 0.031(4) 0.010(4) 0.019(4) 0.024(4) O100 0.071(4) 0.060(3) 0.057(3) 0.018(3) 0.032(3) 0.034(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 Lu1 O1 2.191(4) . ? Lu1 O2 2.210(4) . ? Lu1 O100 2.311(5) . ? Lu1 O13 2.375(5) . ? Lu1 O31 2.389(7) . ? Lu1 N1 2.411(6) . ? Lu1 O112 2.418(10) . ? Lu1 O111 2.439(10) . ? Lu1 N2 2.511(7) . ? Lu1 N101 2.805(14) . ? Lu1 N102 2.836(15) . ? O1 C22 1.293(7) . ? O2 C10 1.312(8) . ? N101 O121 1.223(16) . ? N101 O111 1.286(15) . ? N101 O13 1.289(15) . ? N102 O122 1.225(15) . ? N102 O112 1.260(15) . ? N102 O13 1.331(15) . ? N20 O22 1.232(8) . ? N20 O23 1.247(8) . ? N20 O211 1.261(15) . ? N20 O212 1.277(13) . ? N30 O331 1.163(11) . ? N30 O322 1.198(12) . ? N30 O31 1.260(10) . ? N30 O332 1.285(12) . ? N30 O321 1.316(11) . ? N1 C23 1.290(8) . ? N1 C1 1.487(8) . ? N2 C4 1.277(9) . ? N2 C3 1.470(8) . ? N3 C11 1.287(8) . ? N3 C13 1.446(8) . ? N4 C16 1.294(8) . ? N4 C15 1.457(9) . ? C1 C2 1.513(11) . ? C2 C3 1.515(10) . ? C4 C5 1.450(9) . ? C5 C6 1.373(9) . ? C5 C10 1.413(9) . ? C6 C7 1.388(9) . ? C7 C8 1.342(9) . ? C7 C12 1.514(10) . ? C8 C9 1.392(9) . ? C9 C10 1.403(8) . ? C9 C11 1.407(9) . ? C13 C14 1.537(9) . ? C14 C15 1.498(9) . ? C16 C17 1.423(9) . ? C17 C18 1.413(9) . ? C17 C22 1.417(9) . ? C18 C19 1.354(9) . ? C19 C20 1.368(9) . ? C19 C24 1.504(8) . ? C20 C21 1.397(9) . ? C21 C22 1.415(9) . ? C21 C23 1.442(9) . ? 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 Lu1 O2 77.97(16) . . ? O1 Lu1 O100 81.57(17) . . ? O2 Lu1 O100 147.98(18) . . ? O1 Lu1 O13 153.61(17) . . ? O2 Lu1 O13 128.34(17) . . ? O100 Lu1 O13 73.80(19) . . ? O1 Lu1 O31 72.9(2) . . ? O2 Lu1 O31 72.2(2) . . ? O100 Lu1 O31 78.5(2) . . ? O13 Lu1 O31 110.3(2) . . ? O1 Lu1 N1 76.15(18) . . ? O2 Lu1 N1 123.57(19) . . ? O100 Lu1 N1 73.87(19) . . ? O13 Lu1 N1 87.88(19) . . ? O31 Lu1 N1 140.9(2) . . ? O1 Lu1 O112 146.0(3) . . ? O2 Lu1 O112 79.7(3) . . ? O100 Lu1 O112 105.4(3) . . ? O13 Lu1 O112 53.4(3) . . ? O31 Lu1 O112 76.0(3) . . ? N1 Lu1 O112 137.9(3) . . ? O1 Lu1 O111 150.9(3) . . ? O2 Lu1 O111 74.3(3) . . ? O100 Lu1 O111 118.7(3) . . ? O13 Lu1 O111 54.4(3) . . ? O31 Lu1 O111 90.1(3) . . ? N1 Lu1 O111 127.4(3) . . ? O112 Lu1 O111 17.3(3) . . ? O1 Lu1 N2 111.99(18) . . ? O2 Lu1 N2 73.37(18) . . ? O100 Lu1 N2 137.84(18) . . ? O13 Lu1 N2 81.6(2) . . ? O31 Lu1 N2 143.1(2) . . ? N1 Lu1 N2 71.46(19) . . ? O112 Lu1 N2 85.5(3) . . ? O111 Lu1 N2 68.2(3) . . ? O1 Lu1 N101 175.7(3) . . ? O2 Lu1 N101 101.2(3) . . ? O100 Lu1 N101 97.4(3) . . ? O13 Lu1 N101 27.2(3) . . ? O31 Lu1 N101 102.8(3) . . ? N1 Lu1 N101 107.6(3) . . ? O112 Lu1 N101 30.3(4) . . ? O111 Lu1 N101 27.3(3) . . ? N2 Lu1 N101 71.6(3) . . ? O1 Lu1 N102 160.4(3) . . ? O2 Lu1 N102 105.3(3) . . ? O100 Lu1 N102 86.6(3) . . ? O13 Lu1 N102 27.8(3) . . ? O31 Lu1 N102 89.5(4) . . ? N1 Lu1 N102 115.4(3) . . ? O112 Lu1 N102 26.2(3) . . ? O111 Lu1 N102 32.8(4) . . ? N2 Lu1 N102 87.2(3) . . ? N101 Lu1 N102 15.6(3) . . ? C22 O1 Lu1 140.1(4) . . ? C10 O2 Lu1 141.7(4) . . ? O121 N101 O111 119.5(14) . . ? O121 N101 O13 121.0(14) . . ? O111 N101 O13 117.5(12) . . ? O121 N101 Lu1 171.2(13) . . ? O111 N101 Lu1 60.3(7) . . ? O13 N101 Lu1 57.4(6) . . ? N101 O111 Lu1 92.4(9) . . ? O122 N102 O112 121.5(14) . . ? O122 N102 O13 124.7(13) . . ? O112 N102 O13 112.5(12) . . ? O122 N102 Lu1 177.4(13) . . ? O112 N102 Lu1 58.0(8) . . ? O13 N102 Lu1 56.4(6) . . ? N102 O112 Lu1 95.7(9) . . ? N101 O13 N102 34.1(8) . . ? N101 O13 Lu1 95.3(7) . . ? N102 O13 Lu1 95.7(7) . . ? O22 N20 O23 120.1(7) . . ? O22 N20 O211 108.1(10) . . ? O23 N20 O211 127.6(9) . . ? O22 N20 O212 122.3(9) . . ? O23 N20 O212 115.8(9) . . ? O211 N20 O212 36.5(8) . . ? O331 N30 O322 90.2(14) . . ? O331 N30 O31 134.0(11) . . ? O322 N30 O31 133.1(12) . . ? O331 N30 O332 29.7(10) . . ? O322 N30 O332 119.7(15) . . ? O31 N30 O332 106.0(10) . . ? O331 N30 O321 119.8(13) . . ? O322 N30 O321 34.7(9) . . ? O31 N30 O321 106.2(10) . . ? O332 N30 O321 145.4(12) . . ? N30 O31 Lu1 121.0(5) . . ? C23 N1 C1 113.9(6) . . ? C23 N1 Lu1 129.1(5) . . ? C1 N1 Lu1 117.0(4) . . ? C4 N2 C3 114.2(7) . . ? C4 N2 Lu1 128.3(5) . . ? C3 N2 Lu1 117.5(5) . . ? C11 N3 C13 123.9(6) . . ? C16 N4 C15 123.1(6) . . ? N1 C1 C2 111.2(6) . . ? C1 C2 C3 115.1(8) . . ? N2 C3 C2 113.2(6) . . ? N2 C4 C5 127.8(7) . . ? C6 C5 C10 118.0(6) . . ? C6 C5 C4 118.1(7) . . ? C10 C5 C4 123.8(7) . . ? C5 C6 C7 123.2(7) . . ? C8 C7 C6 118.0(7) . . ? C8 C7 C12 122.4(6) . . ? C6 C7 C12 119.6(7) . . ? C7 C8 C9 122.3(6) . . ? C8 C9 C10 119.3(6) . . ? C8 C9 C11 119.0(6) . . ? C10 C9 C11 121.6(7) . . ? O2 C10 C9 119.1(6) . . ? O2 C10 C5 121.8(6) . . ? C9 C10 C5 119.0(7) . . ? N3 C11 C9 127.0(7) . . ? N3 C13 C14 112.5(6) . . ? C15 C14 C13 116.1(6) . . ? N4 C15 C14 115.8(6) . . ? N4 C16 C17 126.1(7) . . ? C18 C17 C22 120.6(7) . . ? C18 C17 C16 118.8(6) . . ? C22 C17 C16 120.6(6) . . ? C19 C18 C17 122.4(7) . . ? C18 C19 C20 116.7(6) . . ? C18 C19 C24 121.6(6) . . ? C20 C19 C24 121.6(6) . . ? C19 C20 C21 124.7(7) . . ? C20 C21 C22 118.8(6) . . ? C20 C21 C23 117.1(7) . . ? C22 C21 C23 124.1(6) . . ? O1 C22 C21 122.7(6) . . ? O1 C22 C17 120.5(7) . . ? C21 C22 C17 116.8(6) . . ? N1 C23 C21 127.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Lu1 O1 C22 -137.4(7) . . . . ? O100 Lu1 O1 C22 67.4(7) . . . . ? O13 Lu1 O1 C22 46.4(9) . . . . ? O31 Lu1 O1 C22 147.9(7) . . . . ? N1 Lu1 O1 C22 -7.9(7) . . . . ? O112 Lu1 O1 C22 172.5(8) . . . . ? O111 Lu1 O1 C22 -155.5(8) . . . . ? N2 Lu1 O1 C22 -71.0(7) . . . . ? N101 Lu1 O1 C22 143(4) . . . . ? N102 Lu1 O1 C22 120.7(11) . . . . ? O1 Lu1 O2 C10 96.5(6) . . . . ? O100 Lu1 O2 C10 147.9(6) . . . . ? O13 Lu1 O2 C10 -85.7(7) . . . . ? O31 Lu1 O2 C10 172.2(7) . . . . ? N1 Lu1 O2 C10 32.3(7) . . . . ? O112 Lu1 O2 C10 -109.4(7) . . . . ? O111 Lu1 O2 C10 -92.6(7) . . . . ? N2 Lu1 O2 C10 -21.1(6) . . . . ? N101 Lu1 O2 C10 -87.9(7) . . . . ? N102 Lu1 O2 C10 -103.4(7) . . . . ? O1 Lu1 N101 O121 -23(11) . . . . ? O2 Lu1 N101 O121 -101(8) . . . . ? O100 Lu1 N101 O121 53(8) . . . . ? O13 Lu1 N101 O121 83(8) . . . . ? O31 Lu1 N101 O121 -27(8) . . . . ? N1 Lu1 N101 O121 128(8) . . . . ? O112 Lu1 N101 O121 -55(7) . . . . ? O111 Lu1 N101 O121 -91(8) . . . . ? N2 Lu1 N101 O121 -169(8) . . . . ? N102 Lu1 N101 O121 6(6) . . . . ? O1 Lu1 N101 O111 69(5) . . . . ? O2 Lu1 N101 O111 -9.9(10) . . . . ? O100 Lu1 N101 O111 143.9(9) . . . . ? O13 Lu1 N101 O111 173.9(15) . . . . ? O31 Lu1 N101 O111 64.1(10) . . . . ? N1 Lu1 N101 O111 -140.8(9) . . . . ? O112 Lu1 N101 O111 35.8(7) . . . . ? N2 Lu1 N101 O111 -78.0(9) . . . . ? N102 Lu1 N101 O111 97(2) . . . . ? O1 Lu1 N101 O13 -105(4) . . . . ? O2 Lu1 N101 O13 176.2(7) . . . . ? O100 Lu1 N101 O13 -30.0(8) . . . . ? O31 Lu1 N101 O13 -109.8(8) . . . . ? N1 Lu1 N101 O13 45.3(8) . . . . ? O112 Lu1 N101 O13 -138.1(14) . . . . ? O111 Lu1 N101 O13 -173.9(15) . . . . ? N2 Lu1 N101 O13 108.1(8) . . . . ? N102 Lu1 N101 O13 -76.9(18) . . . . ? O121 N101 O111 Lu1 169.8(15) . . . . ? O13 N101 O111 Lu1 5.8(14) . . . . ? O1 Lu1 O111 N101 -171.7(8) . . . . ? O2 Lu1 O111 N101 169.9(10) . . . . ? O100 Lu1 O111 N101 -41.8(10) . . . . ? O13 Lu1 O111 N101 -3.4(9) . . . . ? O31 Lu1 O111 N101 -118.7(9) . . . . ? N1 Lu1 O111 N101 49.4(10) . . . . ? O112 Lu1 O111 N101 -83.8(16) . . . . ? N2 Lu1 O111 N101 91.9(9) . . . . ? N102 Lu1 O111 N101 -29.6(8) . . . . ? O1 Lu1 N102 O122 3(25) . . . . ? O2 Lu1 N102 O122 -94(25) . . . . ? O100 Lu1 N102 O122 56(25) . . . . ? O13 Lu1 N102 O122 116(25) . . . . ? O31 Lu1 N102 O122 -23(25) . . . . ? N1 Lu1 N102 O122 126(25) . . . . ? O112 Lu1 N102 O122 -81(25) . . . . ? O111 Lu1 N102 O122 -114(25) . . . . ? N2 Lu1 N102 O122 -166(25) . . . . ? N101 Lu1 N102 O122 -171(26) . . . . ? O1 Lu1 N102 O112 83.7(13) . . . . ? O2 Lu1 N102 O112 -13.5(10) . . . . ? O100 Lu1 N102 O112 136.3(10) . . . . ? O13 Lu1 N102 O112 -162.7(15) . . . . ? O31 Lu1 N102 O112 57.9(10) . . . . ? N1 Lu1 N102 O112 -153.3(9) . . . . ? O111 Lu1 N102 O112 -33.0(8) . . . . ? N2 Lu1 N102 O112 -85.4(10) . . . . ? N101 Lu1 N102 O112 -90.1(19) . . . . ? O1 Lu1 N102 O13 -113.6(9) . . . . ? O2 Lu1 N102 O13 149.2(7) . . . . ? O100 Lu1 N102 O13 -61.0(7) . . . . ? O31 Lu1 N102 O13 -139.4(8) . . . . ? N1 Lu1 N102 O13 9.4(9) . . . . ? O112 Lu1 N102 O13 162.7(15) . . . . ? O111 Lu1 N102 O13 129.7(13) . . . . ? N2 Lu1 N102 O13 77.3(7) . . . . ? N101 Lu1 N102 O13 72.6(18) . . . . ? O122 N102 O112 Lu1 177.0(15) . . . . ? O13 N102 O112 Lu1 -15.5(13) . . . . ? O1 Lu1 O112 N102 -143.5(8) . . . . ? O2 Lu1 O112 N102 166.8(10) . . . . ? O100 Lu1 O112 N102 -45.7(10) . . . . ? O13 Lu1 O112 N102 9.9(9) . . . . ? O31 Lu1 O112 N102 -119.2(10) . . . . ? N1 Lu1 O112 N102 37.2(12) . . . . ? O111 Lu1 O112 N102 96.8(17) . . . . ? N2 Lu1 O112 N102 92.9(10) . . . . ? N101 Lu1 O112 N102 32.3(8) . . . . ? O121 N101 O13 N102 -77(2) . . . . ? O111 N101 O13 N102 86(2) . . . . ? Lu1 N101 O13 N102 92.4(18) . . . . ? O121 N101 O13 Lu1 -169.8(15) . . . . ? O111 N101 O13 Lu1 -6.0(15) . . . . ? O122 N102 O13 N101 92(2) . . . . ? O112 N102 O13 N101 -75(2) . . . . ? Lu1 N102 O13 N101 -91.0(18) . . . . ? O122 N102 O13 Lu1 -177.2(15) . . . . ? O112 N102 O13 Lu1 15.8(14) . . . . ? O1 Lu1 O13 N101 170.6(8) . . . . ? O2 Lu1 O13 N101 -4.8(9) . . . . ? O100 Lu1 O13 N101 148.9(8) . . . . ? O31 Lu1 O13 N101 78.1(8) . . . . ? N1 Lu1 O13 N101 -137.3(8) . . . . ? O112 Lu1 O13 N101 24.8(8) . . . . ? O111 Lu1 O13 N101 3.4(9) . . . . ? N2 Lu1 O13 N101 -65.7(8) . . . . ? N102 Lu1 O13 N101 34.2(8) . . . . ? O1 Lu1 O13 N102 136.3(7) . . . . ? O2 Lu1 O13 N102 -39.0(9) . . . . ? O100 Lu1 O13 N102 114.7(8) . . . . ? O31 Lu1 O13 N102 43.9(8) . . . . ? N1 Lu1 O13 N102 -171.5(8) . . . . ? O112 Lu1 O13 N102 -9.4(8) . . . . ? O111 Lu1 O13 N102 -30.8(8) . . . . ? N2 Lu1 O13 N102 -100.0(8) . . . . ? N101 Lu1 O13 N102 -34.2(8) . . . . ? O331 N30 O31 Lu1 -164.8(13) . . . . ? O322 N30 O31 Lu1 39.7(17) . . . . ? O332 N30 O31 Lu1 -153.1(8) . . . . ? O321 N30 O31 Lu1 13.9(10) . . . . ? O1 Lu1 O31 N30 -160.0(6) . . . . ? O2 Lu1 O31 N30 117.5(6) . . . . ? O100 Lu1 O31 N30 -75.4(6) . . . . ? O13 Lu1 O31 N30 -7.6(6) . . . . ? N1 Lu1 O31 N30 -120.8(6) . . . . ? O112 Lu1 O31 N30 33.9(6) . . . . ? O111 Lu1 O31 N30 44.0(6) . . . . ? N2 Lu1 O31 N30 96.0(6) . . . . ? N101 Lu1 O31 N30 19.7(7) . . . . ? N102 Lu1 O31 N30 11.3(6) . . . . ? O1 Lu1 N1 C23 1.0(6) . . . . ? O2 Lu1 N1 C23 66.1(7) . . . . ? O100 Lu1 N1 C23 -84.0(6) . . . . ? O13 Lu1 N1 C23 -157.8(6) . . . . ? O31 Lu1 N1 C23 -37.4(8) . . . . ? O112 Lu1 N1 C23 -179.3(7) . . . . ? O111 Lu1 N1 C23 161.8(6) . . . . ? N2 Lu1 N1 C23 120.3(6) . . . . ? N101 Lu1 N1 C23 -176.8(7) . . . . ? N102 Lu1 N1 C23 -162.1(7) . . . . ? O1 Lu1 N1 C1 -179.6(5) . . . . ? O2 Lu1 N1 C1 -114.5(5) . . . . ? O100 Lu1 N1 C1 95.3(5) . . . . ? O13 Lu1 N1 C1 21.5(5) . . . . ? O31 Lu1 N1 C1 141.9(5) . . . . ? O112 Lu1 N1 C1 0.0(7) . . . . ? O111 Lu1 N1 C1 -18.8(7) . . . . ? N2 Lu1 N1 C1 -60.3(5) . . . . ? N101 Lu1 N1 C1 2.5(6) . . . . ? N102 Lu1 N1 C1 17.2(6) . . . . ? O1 Lu1 N2 C4 -55.4(6) . . . . ? O2 Lu1 N2 C4 13.8(6) . . . . ? O100 Lu1 N2 C4 -157.5(5) . . . . ? O13 Lu1 N2 C4 148.1(6) . . . . ? O31 Lu1 N2 C4 35.2(8) . . . . ? N1 Lu1 N2 C4 -121.3(6) . . . . ? O112 Lu1 N2 C4 94.5(6) . . . . ? O111 Lu1 N2 C4 93.2(6) . . . . ? N101 Lu1 N2 C4 122.0(7) . . . . ? N102 Lu1 N2 C4 120.7(7) . . . . ? O1 Lu1 N2 C3 122.8(5) . . . . ? O2 Lu1 N2 C3 -168.0(5) . . . . ? O100 Lu1 N2 C3 20.6(6) . . . . ? O13 Lu1 N2 C3 -33.7(5) . . . . ? O31 Lu1 N2 C3 -146.6(5) . . . . ? N1 Lu1 N2 C3 56.8(5) . . . . ? O112 Lu1 N2 C3 -87.4(6) . . . . ? O111 Lu1 N2 C3 -88.6(6) . . . . ? N101 Lu1 N2 C3 -59.8(6) . . . . ? N102 Lu1 N2 C3 -61.1(6) . . . . ? C23 N1 C1 C2 -103.0(8) . . . . ? Lu1 N1 C1 C2 77.6(7) . . . . ? N1 C1 C2 C3 -66.2(9) . . . . ? C4 N2 C3 C2 109.2(8) . . . . ? Lu1 N2 C3 C2 -69.2(9) . . . . ? C1 C2 C3 N2 63.4(10) . . . . ? C3 N2 C4 C5 175.0(6) . . . . ? Lu1 N2 C4 C5 -6.8(10) . . . . ? N2 C4 C5 C6 176.4(7) . . . . ? N2 C4 C5 C10 -5.5(11) . . . . ? C10 C5 C6 C7 1.5(9) . . . . ? C4 C5 C6 C7 179.7(6) . . . . ? C5 C6 C7 C8 -3.2(9) . . . . ? C5 C6 C7 C12 178.2(6) . . . . ? C6 C7 C8 C9 2.7(9) . . . . ? C12 C7 C8 C9 -178.7(6) . . . . ? C7 C8 C9 C10 -0.7(9) . . . . ? C7 C8 C9 C11 176.9(6) . . . . ? Lu1 O2 C10 C9 -162.3(4) . . . . ? Lu1 O2 C10 C5 17.7(10) . . . . ? C8 C9 C10 O2 179.0(5) . . . . ? C11 C9 C10 O2 1.5(9) . . . . ? C8 C9 C10 C5 -1.0(8) . . . . ? C11 C9 C10 C5 -178.5(6) . . . . ? C6 C5 C10 O2 -179.4(6) . . . . ? C4 C5 C10 O2 2.5(9) . . . . ? C6 C5 C10 C9 0.5(9) . . . . ? C4 C5 C10 C9 -177.5(6) . . . . ? C13 N3 C11 C9 177.1(6) . . . . ? C8 C9 C11 N3 -178.7(6) . . . . ? C10 C9 C11 N3 -1.1(10) . . . . ? C11 N3 C13 C14 -86.4(8) . . . . ? N3 C13 C14 C15 -78.0(9) . . . . ? C16 N4 C15 C14 114.4(8) . . . . ? C13 C14 C15 N4 74.1(9) . . . . ? C15 N4 C16 C17 174.9(7) . . . . ? N4 C16 C17 C18 -178.0(7) . . . . ? N4 C16 C17 C22 -0.3(11) . . . . ? C22 C17 C18 C19 -0.7(10) . . . . ? C16 C17 C18 C19 177.0(6) . . . . ? C17 C18 C19 C20 -1.1(10) . . . . ? C17 C18 C19 C24 -177.9(6) . . . . ? C18 C19 C20 C21 1.9(10) . . . . ? C24 C19 C20 C21 178.7(6) . . . . ? C19 C20 C21 C22 -0.7(10) . . . . ? C19 C20 C21 C23 -178.2(6) . . . . ? Lu1 O1 C22 C21 11.4(11) . . . . ? Lu1 O1 C22 C17 -170.4(5) . . . . ? C20 C21 C22 O1 177.1(6) . . . . ? C23 C21 C22 O1 -5.7(11) . . . . ? C20 C21 C22 C17 -1.2(9) . . . . ? C23 C21 C22 C17 176.1(6) . . . . ? C18 C17 C22 O1 -176.4(6) . . . . ? C16 C17 C22 O1 5.9(10) . . . . ? C18 C17 C22 C21 1.8(10) . . . . ? C16 C17 C22 C21 -175.8(6) . . . . ? C1 N1 C23 C21 -177.9(7) . . . . ? Lu1 N1 C23 C21 1.5(11) . . . . ? C20 C21 C23 N1 177.2(7) . . . . ? C22 C21 C23 N1 0.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.927 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.168 #===End of cif