data_fddd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C40 H23 N12 Nd3 O18' _chemical_formula_sum 'C40 H23 N12 Nd3 O18' _chemical_formula_weight 1392.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 16.847(2) _cell_length_b 20.710(4) _cell_length_c 22.468(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7839(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2453 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 28.34 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5368 _exptl_absorpt_coefficient_mu 4.020 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9241 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Process-auto' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean '10.0' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13232 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2453 _reflns_number_gt 1953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Process-auto' _computing_cell_refinement 'Process-auto' _computing_data_reduction 'Process-auto' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+192.1422P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2453 _refine_ls_number_parameters 198 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.3750 -0.1250 0.187897(15) 0.01773(11) Uani 1 2 d S . . Nd2 Nd 0.1250 0.1250 0.1250 0.01340(12) Uani 1 4 d S . . O1 O 0.2794(2) -0.04183(19) 0.18860(17) 0.0311(9) Uani 1 1 d . . . O2 O 0.2131(3) 0.0413(2) 0.15192(18) 0.0367(10) Uani 1 1 d . . . O3 O 0.1907(2) 0.08454(19) 0.03296(16) 0.0258(8) Uani 1 1 d . . . O4 O 0.2435(2) 0.0545(2) -0.05127(17) 0.0317(9) Uani 1 1 d . . . O1W O 0.097(2) 0.0223(18) 0.6231(18) 0.034(7) Uani 0.20 1 d PU . . O1W' O 0.115(3) 0.0097(11) 0.627(3) 0.045(8) Uani 0.30 1 d PU . . N1 N 0.3770(2) -0.0497(2) 0.09527(18) 0.0210(8) Uani 1 1 d . . . N2 N 0.3640(2) -0.0135(2) 0.00163(19) 0.0233(9) Uani 1 1 d . . . N3 N 0.5952(4) -0.1447(3) 0.0513(5) 0.078(3) Uani 1 1 d . . . C1 C 0.3126(3) -0.0085(2) 0.0927(2) 0.0198(9) Uani 1 1 d . . . C2 C 0.3039(3) 0.0135(2) 0.0349(2) 0.0199(9) Uani 1 1 d . . . C3 C 0.4062(3) -0.0503(2) 0.0396(2) 0.0218(10) Uani 1 1 d . . . C4 C 0.6115(8) -0.1628(7) 0.0048(9) 0.034(3) Uani 0.50 1 d P . . C4' C 0.5981(14) -0.1530(9) -0.0268(10) 0.045(4) Uani 0.50 1 d P . . C5 C 0.5617(11) -0.1450(9) -0.0442(8) 0.033(4) Uani 0.50 1 d PU . . C5' C 0.5515(10) -0.1263(8) -0.0641(7) 0.036(3) Uani 0.50 1 d PU . . C6 C 0.4926(5) -0.1026(5) -0.0369(3) 0.055(2) Uani 1 1 d . . . C7 C 0.4771(3) -0.0875(2) 0.0221(2) 0.0245(10) Uani 1 1 d . . . C8 C 0.5303(3) -0.1085(3) 0.0656(3) 0.0368(14) Uani 1 1 d . . . C9 C 0.2641(3) -0.0017(3) 0.1472(2) 0.0243(10) Uani 1 1 d . . . C10 C 0.2434(3) 0.0534(2) 0.0046(2) 0.0193(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01693(18) 0.01768(18) 0.01857(18) 0.000 0.000 0.00208(13) Nd2 0.0119(2) 0.0131(2) 0.0152(2) 0.000 0.000 0.000 O1 0.033(2) 0.030(2) 0.031(2) 0.0097(16) 0.0099(16) 0.0161(17) O2 0.038(2) 0.042(2) 0.029(2) 0.0050(18) 0.0052(17) 0.025(2) O3 0.0220(18) 0.032(2) 0.0233(18) 0.0023(15) -0.0006(14) 0.0108(16) O4 0.030(2) 0.042(2) 0.0233(18) 0.0068(17) 0.0038(15) 0.0166(18) O1W 0.039(11) 0.037(10) 0.026(9) 0.004(8) 0.006(8) 0.013(8) O1W' 0.045(14) 0.045(10) 0.044(10) 0.002(9) 0.002(10) 0.003(9) N1 0.0201(19) 0.020(2) 0.023(2) 0.0004(15) 0.0011(17) 0.0036(16) N2 0.024(2) 0.025(2) 0.0214(19) 0.0040(17) 0.0022(16) 0.0041(17) N3 0.023(3) 0.040(4) 0.171(10) 0.026(5) 0.006(4) 0.003(3) C1 0.016(2) 0.020(2) 0.023(2) -0.0006(18) -0.0010(17) 0.0015(18) C2 0.017(2) 0.021(2) 0.022(2) 0.0017(18) 0.0005(17) 0.0009(18) C3 0.019(2) 0.021(2) 0.026(2) -0.0005(19) 0.0023(18) 0.0017(19) C4 0.014(6) 0.032(7) 0.055(10) -0.011(8) 0.005(7) 0.003(4) C4' 0.046(12) 0.039(9) 0.050(12) -0.016(9) 0.017(10) 0.005(8) C5 0.022(6) 0.043(7) 0.034(7) -0.004(6) 0.004(6) 0.009(6) C5' 0.033(6) 0.039(6) 0.036(6) 0.002(6) 0.003(5) 0.006(5) C6 0.038(4) 0.082(6) 0.045(4) -0.025(4) 0.015(3) -0.004(4) C7 0.016(2) 0.022(2) 0.036(3) -0.001(2) 0.006(2) -0.0003(19) C8 0.017(2) 0.037(3) 0.057(4) 0.014(3) 0.003(2) 0.005(2) C9 0.026(2) 0.025(2) 0.023(2) 0.000(2) 0.0011(19) 0.004(2) C10 0.014(2) 0.019(2) 0.025(2) 0.0012(19) -0.0002(17) 0.0011(17) _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 Nd1 O1 2.359(4) . ? Nd1 O1 2.359(4) 2_545 ? Nd1 O4 2.486(4) 19_656 ? Nd1 O4 2.486(4) 32_556 ? Nd1 O3 2.547(3) 19_656 ? Nd1 O3 2.547(3) 32_556 ? Nd1 N1 2.601(4) 2_545 ? Nd1 N1 2.601(4) . ? Nd1 C10 2.902(5) 19_656 ? Nd1 C10 2.902(5) 32_556 ? Nd2 O2 2.361(4) 8_544 ? Nd2 O2 2.361(4) 14_445 ? Nd2 O2 2.361(4) 11_454 ? Nd2 O2 2.361(4) . ? Nd2 O3 2.490(4) 14_445 ? Nd2 O3 2.490(4) . ? Nd2 O3 2.490(4) 8_544 ? Nd2 O3 2.490(4) 11_454 ? O1 C9 1.273(6) . ? O2 C9 1.242(6) . ? O3 C10 1.270(6) . ? O3 Nd1 2.547(3) 27 ? O4 C10 1.254(6) . ? O4 Nd1 2.486(4) 27 ? O1W O1W' 0.69(5) 11_455 ? O1W O1W 0.94(7) 11_455 ? O1W' O1W' 0.36(10) 11_455 ? O1W' O1W 0.69(5) 11_455 ? N1 C3 1.343(6) . ? N1 C1 1.382(6) . ? N2 C3 1.347(6) . ? N2 C2 1.378(6) . ? N3 C4 1.143(19) . ? N3 C8 1.365(9) . ? N3 C4' 1.76(2) . ? C1 C2 1.382(7) . ? C1 C9 1.481(7) . ? C2 C10 1.478(6) . ? C3 C7 1.476(7) . ? C4 C4' 0.77(2) . ? C4 C5 1.43(2) . ? C4 C5' 2.00(2) . ? C4' C5 0.75(2) . ? C4' C5' 1.28(3) . ? C5 C5' 0.616(17) . ? C5 C6 1.467(19) . ? C5' C6 1.264(17) . ? C6 C7 1.387(8) . ? C7 C8 1.396(8) . ? C10 Nd1 2.902(5) 27 ? 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 Nd1 O1 179.24(19) . 2_545 ? O1 Nd1 O4 96.82(15) . 19_656 ? O1 Nd1 O4 83.10(15) 2_545 19_656 ? O1 Nd1 O4 83.10(15) . 32_556 ? O1 Nd1 O4 96.82(15) 2_545 32_556 ? O4 Nd1 O4 168.76(17) 19_656 32_556 ? O1 Nd1 O3 92.91(14) . 19_656 ? O1 Nd1 O3 86.45(13) 2_545 19_656 ? O4 Nd1 O3 51.38(12) 19_656 19_656 ? O4 Nd1 O3 117.39(12) 32_556 19_656 ? O1 Nd1 O3 86.45(13) . 32_556 ? O1 Nd1 O3 92.91(14) 2_545 32_556 ? O4 Nd1 O3 117.39(12) 19_656 32_556 ? O4 Nd1 O3 51.38(12) 32_556 32_556 ? O3 Nd1 O3 66.02(16) 19_656 32_556 ? O1 Nd1 N1 115.72(14) . 2_545 ? O1 Nd1 N1 64.95(13) 2_545 2_545 ? O4 Nd1 N1 116.19(13) 19_656 2_545 ? O4 Nd1 N1 73.46(13) 32_556 2_545 ? O3 Nd1 N1 150.94(13) 19_656 2_545 ? O3 Nd1 N1 117.91(13) 32_556 2_545 ? O1 Nd1 N1 64.95(13) . . ? O1 Nd1 N1 115.72(14) 2_545 . ? O4 Nd1 N1 73.46(13) 19_656 . ? O4 Nd1 N1 116.19(13) 32_556 . ? O3 Nd1 N1 117.91(13) 19_656 . ? O3 Nd1 N1 150.94(13) 32_556 . ? N1 Nd1 N1 73.68(18) 2_545 . ? O1 Nd1 C10 95.33(14) . 19_656 ? O1 Nd1 C10 84.27(13) 2_545 19_656 ? O4 Nd1 C10 25.45(13) 19_656 19_656 ? O4 Nd1 C10 143.31(13) 32_556 19_656 ? O3 Nd1 C10 25.93(12) 19_656 19_656 ? O3 Nd1 C10 91.94(13) 32_556 19_656 ? N1 Nd1 C10 136.76(13) 2_545 19_656 ? N1 Nd1 C10 95.59(13) . 19_656 ? O1 Nd1 C10 84.27(13) . 32_556 ? O1 Nd1 C10 95.33(14) 2_545 32_556 ? O4 Nd1 C10 143.31(13) 19_656 32_556 ? O4 Nd1 C10 25.45(13) 32_556 32_556 ? O3 Nd1 C10 91.94(13) 19_656 32_556 ? O3 Nd1 C10 25.93(12) 32_556 32_556 ? N1 Nd1 C10 95.59(13) 2_545 32_556 ? N1 Nd1 C10 136.76(13) . 32_556 ? C10 Nd1 C10 117.87(19) 19_656 32_556 ? O2 Nd2 O2 85.5(2) 8_544 14_445 ? O2 Nd2 O2 150.3(2) 8_544 11_454 ? O2 Nd2 O2 102.1(2) 14_445 11_454 ? O2 Nd2 O2 102.1(2) 8_544 . ? O2 Nd2 O2 150.3(2) 14_445 . ? O2 Nd2 O2 85.5(2) 11_454 . ? O2 Nd2 O3 79.59(14) 8_544 14_445 ? O2 Nd2 O3 71.73(13) 14_445 14_445 ? O2 Nd2 O3 75.82(14) 11_454 14_445 ? O2 Nd2 O3 137.65(13) . 14_445 ? O2 Nd2 O3 75.82(14) 8_544 . ? O2 Nd2 O3 137.65(13) 14_445 . ? O2 Nd2 O3 79.59(14) 11_454 . ? O2 Nd2 O3 71.73(13) . . ? O3 Nd2 O3 67.72(16) 14_445 . ? O2 Nd2 O3 71.73(13) 8_544 8_544 ? O2 Nd2 O3 79.59(14) 14_445 8_544 ? O2 Nd2 O3 137.65(13) 11_454 8_544 ? O2 Nd2 O3 75.82(14) . 8_544 ? O3 Nd2 O3 140.68(18) 14_445 8_544 ? O3 Nd2 O3 127.27(17) . 8_544 ? O2 Nd2 O3 137.65(13) 8_544 11_454 ? O2 Nd2 O3 75.82(14) 14_445 11_454 ? O2 Nd2 O3 71.73(13) 11_454 11_454 ? O2 Nd2 O3 79.59(14) . 11_454 ? O3 Nd2 O3 127.27(17) 14_445 11_454 ? O3 Nd2 O3 140.68(18) . 11_454 ? O3 Nd2 O3 67.72(16) 8_544 11_454 ? C9 O1 Nd1 127.6(3) . . ? C9 O2 Nd2 160.0(4) . . ? C10 O3 Nd2 154.0(3) . . ? C10 O3 Nd1 92.8(3) . 27 ? Nd2 O3 Nd1 113.13(13) . 27 ? C10 O4 Nd1 96.2(3) . 27 ? O1W' O1W O1W 23(4) 11_455 11_455 ? O1W' O1W' O1W 27(10) 11_455 11_455 ? C3 N1 C1 104.6(4) . . ? C3 N1 Nd1 138.1(3) . . ? C1 N1 Nd1 113.2(3) . . ? C3 N2 C2 105.8(4) . . ? C4 N3 C8 125.9(11) . . ? C4 N3 C4' 18.6(10) . . ? C8 N3 C4' 108.0(9) . . ? N1 C1 C2 109.1(4) . . ? N1 C1 C9 117.2(4) . . ? C2 C1 C9 133.4(4) . . ? N2 C2 C1 107.3(4) . . ? N2 C2 C10 118.8(4) . . ? C1 C2 C10 133.7(4) . . ? N1 C3 N2 113.1(4) . . ? N1 C3 C7 123.3(5) . . ? N2 C3 C7 123.5(5) . . ? C4' C4 N3 133(2) . . ? C4' C4 C5 19.0(18) . . ? N3 C4 C5 118.6(13) . . ? C4' C4 C5' 16.3(17) . . ? N3 C4 C5' 117.6(11) . . ? C5 C4 C5' 8.4(10) . . ? C5 C4' C4 141(4) . . ? C5 C4' C5' 19(2) . . ? C4 C4' C5' 154(3) . . ? C5 C4' N3 119(2) . . ? C4 C4' N3 28.2(15) . . ? C5' C4' N3 126.5(14) . . ? C5' C5 C4' 138(4) . . ? C5' C5 C4 152(3) . . ? C4' C5 C4 19.7(18) . . ? C5' C5 C6 59(2) . . ? C4' C5 C6 137(2) . . ? C4 C5 C6 122.2(13) . . ? C5 C5' C6 96(3) . . ? C5 C5' C4' 23(2) . . ? C6 C5' C4' 109.6(15) . . ? C5 C5' C4 20(2) . . ? C6 C5' C4 99.8(11) . . ? C4' C5' C4 9.8(10) . . ? C5' C6 C7 134.2(11) . . ? C5' C6 C5 24.7(8) . . ? C7 C6 C5 113.0(10) . . ? C6 C7 C8 118.6(6) . . ? C6 C7 C3 121.7(6) . . ? C8 C7 C3 119.7(5) . . ? N3 C8 C7 121.4(7) . . ? O2 C9 O1 123.1(5) . . ? O2 C9 C1 121.4(5) . . ? O1 C9 C1 115.5(4) . . ? O4 C10 O3 119.6(4) . . ? O4 C10 C2 118.1(4) . . ? O3 C10 C2 122.3(4) . . ? O4 C10 Nd1 58.4(3) . 27 ? O3 C10 Nd1 61.2(2) . 27 ? C2 C10 Nd1 175.9(3) . 27 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.591 _refine_diff_density_min -0.918 _refine_diff_density_rms 0.189