# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sanping Chen' _publ_contact_author_email SANPINGCHEN@126.COM _publ_section_title ; Microporous Lanthanide-Carboxylate Frameworks based on 5-Nitroisophthalic acid ; loop_ _publ_author_name 'Sanping Chen' 'Shengli Gao' 'Yi-Xia Ren' 'Wei-Tao Wang' # Attachment 'revised3-Ho.cif' data_xb0628m _database_code_depnum_ccdc_archive 'CCDC 741283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 Ho2 N9 O24' _chemical_formula_weight 1395.78 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.719(2) _cell_length_b 16.6492(18) _cell_length_c 16.1955(17) _cell_angle_alpha 90.00 _cell_angle_beta 120.052(2) _cell_angle_gamma 90.00 _cell_volume 5069.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 3.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6634 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12684 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4506 _reflns_number_gt 3758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0673P)^2^+37.6279P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4506 _refine_ls_number_parameters 355 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _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 Ho1 Ho 0.691312(14) 0.354124(17) -0.002042(19) 0.02365(13) Uani 1 1 d . . . O1 O 0.7066(3) 0.4421(3) 0.1257(4) 0.0489(14) Uani 1 1 d . . . O2 O 0.7246(4) 0.4954(3) 0.0154(4) 0.0520(15) Uani 1 1 d . . . O3 O 0.8139(2) 0.3602(3) 0.0862(4) 0.0405(13) Uani 1 1 d . . . O4 O 0.8738(3) 0.2463(3) 0.1106(3) 0.0378(12) Uani 1 1 d . . . O5 O 0.5866(4) 0.3383(5) 0.0105(7) 0.085(2) Uani 1 1 d . . . O6 O 0.5972(4) 0.4278(4) -0.1248(5) 0.080(2) Uani 1 1 d . . . O7 O 0.7213(3) 0.6317(3) 0.3788(4) 0.0420(13) Uani 1 1 d . . . O8 O 0.7780(3) 0.7478(3) 0.4012(4) 0.0487(14) Uani 1 1 d . . . O9 O 0.8633(6) 0.8227(6) 0.1853(8) 0.122(4) Uani 1 1 d . . . O10 O 0.8354(4) 0.7527(4) 0.0611(5) 0.073(2) Uani 1 1 d . . . O11 O 0.9100(7) 0.5735(10) 0.4711(10) 0.173(6) Uani 1 1 d U . . O12 O 0.9436(4) 0.6078(4) 0.2026(7) 0.097(3) Uani 1 1 d . . . C13 C 0.8701(3) 0.3191(4) 0.1247(5) 0.0291(15) Uani 1 1 d . . . C1 C 0.7466(4) 0.5786(4) 0.1451(5) 0.0323(15) Uani 1 1 d . . . C2 C 0.7393(3) 0.5942(4) 0.2239(5) 0.0278(14) Uani 1 1 d . . . H2 H 0.7186 0.5557 0.2440 0.033 Uiso 1 1 calc R . . C3 C 0.7623(4) 0.6661(4) 0.2732(5) 0.0306(15) Uani 1 1 d . . . C4 C 0.7942(4) 0.7226(5) 0.2443(5) 0.0408(18) Uani 1 1 d . . . H4 H 0.8108 0.7708 0.2770 0.049 Uiso 1 1 calc R . . C5 C 0.8009(4) 0.7059(5) 0.1665(6) 0.0445(19) Uani 1 1 d . . . C6 C 0.7775(4) 0.6351(4) 0.1152(6) 0.0402(18) Uani 1 1 d . . . H6 H 0.7824 0.6261 0.0621 0.048 Uiso 1 1 calc R . . C7 C 0.7230(4) 0.5008(4) 0.0907(5) 0.0364(17) Uani 1 1 d . . . C8 C 0.7533(4) 0.6832(4) 0.3579(5) 0.0340(16) Uani 1 1 d . . . C9 C 1.0000 0.3224(6) 0.2500 0.028(2) Uani 1 2 d S . . H9 H 1.0000 0.2666 0.2500 0.034 Uiso 1 2 calc SR . . C10 C 0.9379(4) 0.3632(4) 0.1904(5) 0.0274(14) Uani 1 1 d . . . C11 C 0.9372(3) 0.4460(4) 0.1916(5) 0.0352(16) Uani 1 1 d . . . H11 H 0.8954 0.4744 0.1540 0.042 Uiso 1 1 calc R . . C12 C 1.0000 0.4855(6) 0.2500 0.041(3) Uani 1 2 d S . . C14 C 0.5941(7) 0.4778(7) -0.1875(8) 0.086(4) Uani 1 1 d . . . H14 H 0.6104 0.5299 -0.1681 0.103 Uiso 1 1 calc R . . C16 C 0.5599(11) 0.5224(13) -0.3457(13) 0.171(8) Uani 1 1 d U . . H16A H 0.5185 0.5091 -0.4055 0.256 Uiso 1 1 calc R . . H16B H 0.6008 0.5236 -0.3536 0.256 Uiso 1 1 calc R . . H16C H 0.5535 0.5742 -0.3250 0.256 Uiso 1 1 calc R . . C15 C 0.5610(12) 0.3728(12) -0.313(2) 0.227(14) Uani 1 1 d U . . H15A H 0.5833 0.3689 -0.3509 0.341 Uiso 1 1 calc R . . H15B H 0.5113 0.3610 -0.3513 0.341 Uiso 1 1 calc R . . H15C H 0.5827 0.3352 -0.2610 0.341 Uiso 1 1 calc R . . C17 C 0.5619(6) 0.2774(8) 0.0296(8) 0.083(3) Uani 1 1 d . . . H17 H 0.5863 0.2296 0.0366 0.100 Uiso 1 1 calc R . . C18 C 0.4639(14) 0.3365(14) 0.026(2) 0.232(12) Uani 1 1 d U . . H18A H 0.4920 0.3846 0.0467 0.348 Uiso 1 1 calc R . . H18B H 0.4401 0.3297 0.0625 0.348 Uiso 1 1 calc R . . H18C H 0.4292 0.3405 -0.0402 0.348 Uiso 1 1 calc R . . C19 C 0.4908(13) 0.1953(16) 0.066(2) 0.250(14) Uani 1 1 d U . . H19A H 0.4477 0.1748 0.0130 0.375 Uiso 1 1 calc R . . H19B H 0.4847 0.2012 0.1203 0.375 Uiso 1 1 calc R . . H19C H 0.5290 0.1585 0.0808 0.375 Uiso 1 1 calc R . . C20 C 0.8607(10) 0.5224(12) 0.4540(10) 0.122(5) Uani 1 1 d U . . H20 H 0.8319 0.5282 0.4809 0.146 Uiso 1 1 calc R . . C21 C 0.8889(12) 0.4515(16) 0.3507(14) 0.207(11) Uani 1 1 d U . . H21A H 0.8644 0.4781 0.2899 0.311 Uiso 1 1 calc R . . H21B H 0.8925 0.3952 0.3411 0.311 Uiso 1 1 calc R . . H21C H 0.9357 0.4739 0.3879 0.311 Uiso 1 1 calc R . . C22 C 0.7948(10) 0.4085(10) 0.3761(13) 0.139(6) Uani 1 1 d U . . H22A H 0.7685 0.4280 0.4052 0.208 Uiso 1 1 calc R . . H22B H 0.8133 0.3561 0.4006 0.208 Uiso 1 1 calc R . . H22C H 0.7639 0.4056 0.3083 0.208 Uiso 1 1 calc R . . N1 N 0.8366(4) 0.7643(5) 0.1343(7) 0.063(2) Uani 1 1 d . . . N2 N 0.5705(7) 0.4599(9) -0.2720(8) 0.129(5) Uani 1 1 d U . . N3 N 0.5072(7) 0.2719(9) 0.0411(10) 0.130(5) Uani 1 1 d U . . N4 N 0.8521(6) 0.4619(8) 0.3974(7) 0.095(3) Uani 1 1 d U . . N5 N 1.0000 0.5741(6) 0.2500 0.064(3) Uani 1 2 d S . . 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 0.01912(18) 0.02747(19) 0.02095(18) -0.00103(12) 0.00748(14) -0.00129(12) O1 0.068(4) 0.043(3) 0.053(3) -0.019(3) 0.043(3) -0.017(3) O2 0.083(4) 0.039(3) 0.037(3) -0.003(2) 0.032(3) 0.001(3) O3 0.015(2) 0.048(3) 0.042(3) 0.000(2) 0.002(2) -0.003(2) O4 0.029(3) 0.034(3) 0.035(3) -0.008(2) 0.004(2) -0.005(2) O5 0.078(5) 0.087(5) 0.127(7) -0.022(5) 0.079(6) -0.003(4) O6 0.069(5) 0.075(5) 0.082(5) 0.013(4) 0.028(4) 0.005(4) O7 0.046(3) 0.055(3) 0.030(3) 0.004(2) 0.022(3) 0.010(3) O8 0.049(3) 0.053(3) 0.032(3) -0.016(2) 0.011(3) 0.009(3) O9 0.189(11) 0.081(6) 0.140(8) -0.035(6) 0.116(9) -0.078(7) O10 0.078(5) 0.092(5) 0.077(5) 0.024(4) 0.059(4) -0.003(4) O11 0.122(10) 0.216(15) 0.151(11) -0.005(10) 0.045(9) -0.060(11) O12 0.049(4) 0.035(4) 0.158(8) 0.006(4) 0.016(5) 0.013(3) C13 0.022(3) 0.034(4) 0.025(3) 0.000(3) 0.007(3) -0.004(3) C1 0.036(4) 0.032(4) 0.031(4) 0.002(3) 0.019(3) 0.003(3) C2 0.030(4) 0.027(3) 0.026(3) -0.003(3) 0.014(3) -0.002(3) C3 0.029(4) 0.037(4) 0.024(3) -0.005(3) 0.013(3) 0.000(3) C4 0.041(4) 0.035(4) 0.041(4) -0.009(3) 0.016(4) -0.010(3) C5 0.052(5) 0.039(4) 0.050(5) 0.008(4) 0.031(4) -0.009(4) C6 0.049(5) 0.043(4) 0.036(4) -0.005(3) 0.027(4) -0.002(4) C7 0.045(4) 0.039(4) 0.030(4) -0.007(3) 0.023(4) 0.001(3) C8 0.034(4) 0.038(4) 0.026(3) -0.008(3) 0.012(3) 0.004(3) C9 0.021(5) 0.027(5) 0.035(5) 0.000 0.013(4) 0.000 C10 0.022(3) 0.026(3) 0.028(3) -0.002(3) 0.008(3) -0.001(3) C11 0.017(3) 0.036(4) 0.041(4) 0.002(3) 0.005(3) 0.007(3) C12 0.035(6) 0.027(5) 0.050(6) 0.000 0.013(5) 0.000 C14 0.115(10) 0.058(6) 0.056(7) 0.016(5) 0.021(7) -0.003(7) C16 0.148(17) 0.193(16) 0.143(16) 0.061(13) 0.052(14) 0.004(15) C15 0.118(16) 0.138(12) 0.29(3) -0.032(14) 0.000(19) -0.023(14) C17 0.045(6) 0.108(9) 0.090(8) -0.005(7) 0.029(6) -0.022(6) C18 0.20(2) 0.187(16) 0.45(4) -0.02(2) 0.27(3) 0.008(14) C19 0.149(19) 0.243(19) 0.37(4) 0.11(3) 0.14(2) -0.022(18) C20 0.111(12) 0.159(15) 0.076(9) 0.007(10) 0.032(9) 0.043(11) C21 0.19(2) 0.36(3) 0.128(14) 0.000(18) 0.122(15) 0.09(2) C22 0.158(17) 0.101(12) 0.159(16) 0.029(11) 0.080(14) -0.006(12) N1 0.067(5) 0.049(5) 0.085(6) 0.010(4) 0.047(5) -0.012(4) N2 0.124(10) 0.144(10) 0.061(7) 0.008(6) 0.003(7) -0.018(9) N3 0.094(9) 0.154(11) 0.175(12) 0.018(10) 0.093(9) -0.006(8) N4 0.106(8) 0.117(9) 0.066(6) 0.001(6) 0.047(6) 0.019(7) N5 0.034(6) 0.036(6) 0.088(8) 0.000 0.005(6) 0.000 _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 O8 2.271(5) 4_645 ? Ho1 O3 2.309(5) . ? Ho1 O4 2.323(5) 7_655 ? Ho1 O7 2.338(5) 6_565 ? Ho1 O6 2.359(7) . ? Ho1 O5 2.396(7) . ? Ho1 O1 2.419(5) . ? Ho1 O2 2.435(5) . ? O1 C7 1.267(9) . ? O2 C7 1.240(8) . ? O3 C13 1.258(8) . ? O4 C13 1.243(8) . ? O4 Ho1 2.323(5) 7_655 ? O5 C17 1.258(13) . ? O6 C14 1.288(12) . ? O7 C8 1.253(9) . ? O7 Ho1 2.338(5) 6_566 ? O8 C8 1.248(9) . ? O8 Ho1 2.271(5) 4_655 ? O9 N1 1.218(11) . ? O10 N1 1.189(10) . ? O11 C20 1.28(2) . ? O12 N5 1.209(7) . ? C13 C10 1.507(9) . ? C1 C6 1.377(10) . ? C1 C2 1.388(9) . ? C1 C7 1.505(10) . ? C2 C3 1.387(9) . ? C2 H2 0.9300 . ? C3 C4 1.381(10) . ? C3 C8 1.506(9) . ? C4 C5 1.366(11) . ? C4 H4 0.9300 . ? C5 C6 1.383(11) . ? C5 N1 1.493(10) . ? C6 H6 0.9300 . ? C9 C10 1.381(8) 2_755 ? C9 C10 1.381(8) . ? C9 H9 0.9300 . ? C10 C11 1.380(9) . ? C11 C12 1.377(8) . ? C11 H11 0.9300 . ? C12 C11 1.377(8) 2_755 ? C12 N5 1.476(14) . ? C14 N2 1.235(15) . ? C14 H14 0.9300 . ? C16 N2 1.51(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15 N2 1.56(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C17 N3 1.294(15) . ? C17 H17 0.9300 . ? C18 N3 1.37(2) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.43(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.310(18) . ? C20 H20 0.9300 . ? C21 N4 1.359(17) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.424(18) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N5 O12 1.209(7) 2_755 ? 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 O8 Ho1 O3 75.93(19) 4_645 . ? O8 Ho1 O4 80.28(19) 4_645 7_655 ? O3 Ho1 O4 125.20(18) . 7_655 ? O8 Ho1 O7 124.7(2) 4_645 6_565 ? O3 Ho1 O7 78.16(19) . 6_565 ? O4 Ho1 O7 76.33(18) 7_655 6_565 ? O8 Ho1 O6 146.1(2) 4_645 . ? O3 Ho1 O6 138.0(2) . . ? O4 Ho1 O6 78.1(2) 7_655 . ? O7 Ho1 O6 74.6(2) 6_565 . ? O8 Ho1 O5 78.6(3) 4_645 . ? O3 Ho1 O5 143.2(3) . . ? O4 Ho1 O5 75.0(2) 7_655 . ? O7 Ho1 O5 138.6(3) 6_565 . ? O6 Ho1 O5 70.7(3) . . ? O8 Ho1 O1 89.5(2) 4_645 . ? O3 Ho1 O1 79.7(2) . . ? O4 Ho1 O1 148.67(18) 7_655 . ? O7 Ho1 O1 132.03(18) 6_565 . ? O6 Ho1 O1 95.5(2) . . ? O5 Ho1 O1 74.0(2) . . ? O8 Ho1 O2 134.96(19) 4_645 . ? O3 Ho1 O2 72.7(2) . . ? O4 Ho1 O2 144.67(18) 7_655 . ? O7 Ho1 O2 78.98(18) 6_565 . ? O6 Ho1 O2 71.2(2) . . ? O5 Ho1 O2 109.6(2) . . ? O1 Ho1 O2 53.86(18) . . ? C7 O1 Ho1 91.9(4) . . ? C7 O2 Ho1 91.8(5) . . ? C13 O3 Ho1 144.5(5) . . ? C13 O4 Ho1 140.3(4) . 7_655 ? C17 O5 Ho1 130.6(8) . . ? C14 O6 Ho1 133.0(8) . . ? C8 O7 Ho1 125.2(5) . 6_566 ? C8 O8 Ho1 164.6(5) . 4_655 ? O4 C13 O3 125.1(6) . . ? O4 C13 C10 118.2(6) . . ? O3 C13 C10 116.6(6) . . ? C6 C1 C2 119.7(7) . . ? C6 C1 C7 117.8(6) . . ? C2 C1 C7 122.5(6) . . ? C3 C2 C1 121.1(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 C8 119.7(6) . . ? C2 C3 C8 120.9(6) . . ? C5 C4 C3 118.5(7) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 123.4(7) . . ? C4 C5 N1 120.2(7) . . ? C6 C5 N1 116.3(7) . . ? C1 C6 C5 117.9(7) . . ? C1 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? O2 C7 O1 122.5(7) . . ? O2 C7 C1 117.9(7) . . ? O1 C7 C1 119.4(6) . . ? O8 C8 O7 125.3(7) . . ? O8 C8 C3 117.3(7) . . ? O7 C8 C3 117.3(6) . . ? C10 C9 C10 121.1(9) 2_755 . ? C10 C9 H9 119.4 2_755 . ? C10 C9 H9 119.4 . . ? C11 C10 C9 119.7(6) . . ? C11 C10 C13 118.8(6) . . ? C9 C10 C13 121.4(6) . . ? C12 C11 C10 118.2(7) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C11 C12 C11 123.0(9) . 2_755 ? C11 C12 N5 118.5(5) . . ? C11 C12 N5 118.5(5) 2_755 . ? N2 C14 O6 123.1(12) . . ? N2 C14 H14 118.4 . . ? O6 C14 H14 118.4 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C17 N3 128.9(14) . . ? O5 C17 H17 115.5 . . ? N3 C17 H17 115.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O11 C20 N4 118.1(18) . . ? O11 C20 H20 121.0 . . ? N4 C20 H20 121.0 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O10 N1 O9 124.9(8) . . ? O10 N1 C5 119.2(8) . . ? O9 N1 C5 115.9(8) . . ? C14 N2 C16 121.6(15) . . ? C14 N2 C15 125.9(16) . . ? C16 N2 C15 111.7(17) . . ? C17 N3 C18 121.3(15) . . ? C17 N3 C19 118.4(17) . . ? C18 N3 C19 120.2(16) . . ? C20 N4 C21 124.7(19) . . ? C20 N4 C22 116.7(15) . . ? C21 N4 C22 118.2(17) . . ? O12 N5 O12 124.8(11) 2_755 . ? O12 N5 C12 117.6(5) 2_755 . ? O12 N5 C12 117.6(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 O8 Ho1 O1 C7 151.3(5) 4_645 . . . ? O3 Ho1 O1 C7 75.5(5) . . . . ? O4 Ho1 O1 C7 -138.5(5) 7_655 . . . ? O7 Ho1 O1 C7 11.9(6) 6_565 . . . ? O6 Ho1 O1 C7 -62.3(5) . . . . ? O5 Ho1 O1 C7 -130.4(5) . . . . ? O2 Ho1 O1 C7 -0.5(4) . . . . ? O8 Ho1 O2 C7 -41.5(6) 4_645 . . . ? O3 Ho1 O2 C7 -89.3(5) . . . . ? O4 Ho1 O2 C7 143.5(5) 7_655 . . . ? O7 Ho1 O2 C7 -170.2(5) 6_565 . . . ? O6 Ho1 O2 C7 112.5(5) . . . . ? O5 Ho1 O2 C7 51.9(6) . . . . ? O1 Ho1 O2 C7 0.5(5) . . . . ? O8 Ho1 O3 C13 37.8(8) 4_645 . . . ? O4 Ho1 O3 C13 -29.2(9) 7_655 . . . ? O7 Ho1 O3 C13 -92.9(8) 6_565 . . . ? O6 Ho1 O3 C13 -143.2(8) . . . . ? O5 Ho1 O3 C13 85.3(9) . . . . ? O1 Ho1 O3 C13 129.9(8) . . . . ? O2 Ho1 O3 C13 -174.9(9) . . . . ? O8 Ho1 O5 C17 -25.8(10) 4_645 . . . ? O3 Ho1 O5 C17 -72.6(11) . . . . ? O4 Ho1 O5 C17 57.0(10) 7_655 . . . ? O7 Ho1 O5 C17 104.7(11) 6_565 . . . ? O6 Ho1 O5 C17 139.4(11) . . . . ? O1 Ho1 O5 C17 -118.7(11) . . . . ? O2 Ho1 O5 C17 -159.7(10) . . . . ? O8 Ho1 O6 C14 -160.9(9) 4_645 . . . ? O3 Ho1 O6 C14 20.9(12) . . . . ? O4 Ho1 O6 C14 -109.4(10) 7_655 . . . ? O7 Ho1 O6 C14 -30.5(10) 6_565 . . . ? O5 Ho1 O6 C14 172.5(11) . . . . ? O1 Ho1 O6 C14 101.7(10) . . . . ? O2 Ho1 O6 C14 52.9(10) . . . . ? Ho1 O4 C13 O3 17.5(12) 7_655 . . . ? Ho1 O4 C13 C10 -160.4(5) 7_655 . . . ? Ho1 O3 C13 O4 12.4(13) . . . . ? Ho1 O3 C13 C10 -169.6(6) . . . . ? C6 C1 C2 C3 0.3(11) . . . . ? C7 C1 C2 C3 179.2(7) . . . . ? C1 C2 C3 C4 -1.2(11) . . . . ? C1 C2 C3 C8 179.1(6) . . . . ? C2 C3 C4 C5 1.1(11) . . . . ? C8 C3 C4 C5 -179.2(7) . . . . ? C3 C4 C5 C6 -0.2(13) . . . . ? C3 C4 C5 N1 -178.5(7) . . . . ? C2 C1 C6 C5 0.7(11) . . . . ? C7 C1 C6 C5 -178.4(7) . . . . ? C4 C5 C6 C1 -0.7(13) . . . . ? N1 C5 C6 C1 177.7(7) . . . . ? Ho1 O2 C7 O1 -0.9(8) . . . . ? Ho1 O2 C7 C1 174.7(6) . . . . ? Ho1 O1 C7 O2 0.9(8) . . . . ? Ho1 O1 C7 C1 -174.6(6) . . . . ? C6 C1 C7 O2 -8.6(11) . . . . ? C2 C1 C7 O2 172.5(7) . . . . ? C6 C1 C7 O1 167.1(7) . . . . ? C2 C1 C7 O1 -11.8(11) . . . . ? Ho1 O8 C8 O7 -5(2) 4_655 . . . ? Ho1 O8 C8 C3 174.8(15) 4_655 . . . ? Ho1 O7 C8 O8 4.8(11) 6_566 . . . ? Ho1 O7 C8 C3 -174.8(4) 6_566 . . . ? C4 C3 C8 O8 -2.7(10) . . . . ? C2 C3 C8 O8 177.0(7) . . . . ? C4 C3 C8 O7 177.0(7) . . . . ? C2 C3 C8 O7 -3.3(10) . . . . ? C10 C9 C10 C11 -1.5(5) 2_755 . . . ? C10 C9 C10 C13 179.7(7) 2_755 . . . ? O4 C13 C10 C11 166.7(7) . . . . ? O3 C13 C10 C11 -11.3(10) . . . . ? O4 C13 C10 C9 -14.4(9) . . . . ? O3 C13 C10 C9 167.5(6) . . . . ? C9 C10 C11 C12 2.8(10) . . . . ? C13 C10 C11 C12 -178.2(5) . . . . ? C10 C11 C12 C11 -1.4(5) . . . 2_755 ? C10 C11 C12 N5 178.6(5) . . . . ? Ho1 O6 C14 N2 103.2(16) . . . . ? Ho1 O5 C17 N3 175.7(11) . . . . ? C4 C5 N1 O10 -172.3(8) . . . . ? C6 C5 N1 O10 9.3(12) . . . . ? C4 C5 N1 O9 5.4(14) . . . . ? C6 C5 N1 O9 -173.0(10) . . . . ? O6 C14 N2 C16 172.9(14) . . . . ? O6 C14 N2 C15 -18(3) . . . . ? O5 C17 N3 C18 5(3) . . . . ? O5 C17 N3 C19 -178.0(19) . . . . ? O11 C20 N4 C21 -4(2) . . . . ? O11 C20 N4 C22 -177.1(14) . . . . ? C11 C12 N5 O12 -175.8(6) . . . 2_755 ? C11 C12 N5 O12 4.2(6) 2_755 . . 2_755 ? C11 C12 N5 O12 4.2(6) . . . . ? C11 C12 N5 O12 -175.8(6) 2_755 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.221 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.147 # Attachment 'revised2-Dy.cif' data_xb0600m _database_code_depnum_ccdc_archive 'CCDC 741284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 Dy2 N9 O24' _chemical_formula_weight 1390.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.746(3) _cell_length_b 16.682(2) _cell_length_c 16.2156(19) _cell_angle_alpha 90.00 _cell_angle_beta 120.009(2) _cell_angle_gamma 90.00 _cell_volume 5093.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 3.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5204 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15595 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6115 _reflns_number_gt 4721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0501P)^2^+43.0738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6115 _refine_ls_number_parameters 355 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _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 N5 N 0.8520(6) 0.0380(7) 0.8972(7) 0.099(3) Uani 1 1 d U . . Dy1 Dy 0.691182(12) 0.145806(15) 0.497776(17) 0.02313(9) Uani 1 1 d . . . O1 O 0.7241(3) 0.0042(3) 0.5147(3) 0.0517(13) Uani 1 1 d . . . O2 O 0.7058(3) 0.0567(3) 0.6250(3) 0.0478(12) Uani 1 1 d . . . O3 O 0.7215(2) -0.1317(3) 0.8780(3) 0.0420(11) Uani 1 1 d . . . O4 O 0.7786(3) -0.2479(3) 0.9009(3) 0.0487(12) Uani 1 1 d . . . O5 O 0.8358(3) -0.2531(4) 0.5614(5) 0.0739(18) Uani 1 1 d . . . O6 O 0.8637(6) -0.3223(5) 0.6861(7) 0.127(4) Uani 1 1 d . . . O7 O 0.8139(2) 0.1397(3) 0.5866(3) 0.0388(10) Uani 1 1 d . . . O8 O 0.8745(2) 0.2532(3) 0.6112(3) 0.0373(10) Uani 1 1 d . . . O11 O 0.5969(3) 0.0726(4) 0.3750(5) 0.0782(18) Uani 1 1 d . . . O10 O 0.5864(4) 0.1617(5) 0.5111(6) 0.089(2) Uani 1 1 d . . . O12 O 0.9104(6) -0.0720(9) 0.9717(8) 0.170(5) Uani 1 1 d U . . C1 C 0.7227(3) -0.0009(4) 0.5905(4) 0.0356(13) Uani 1 1 d . . . C2 C 0.7471(3) -0.0788(4) 0.6452(4) 0.0322(13) Uani 1 1 d . . . C3 C 0.7393(3) -0.0946(3) 0.7242(4) 0.0286(12) Uani 1 1 d . . . H3 H 0.7186 -0.0564 0.7443 0.034 Uiso 1 1 calc R . . C4 C 0.7622(3) -0.1666(4) 0.7732(4) 0.0305(12) Uani 1 1 d . . . C5 C 0.7943(3) -0.2228(4) 0.7443(5) 0.0388(14) Uani 1 1 d . . . H5 H 0.8105 -0.2710 0.7768 0.047 Uiso 1 1 calc R . . C6 C 0.8018(4) -0.2061(4) 0.6667(5) 0.0433(16) Uani 1 1 d . . . C7 C 0.7779(4) -0.1356(4) 0.6159(5) 0.0387(15) Uani 1 1 d . . . H7 H 0.7825 -0.1267 0.5626 0.046 Uiso 1 1 calc R . . C8 C 0.7537(3) -0.1827(4) 0.8578(4) 0.0326(13) Uani 1 1 d . . . C9 C 0.8700(3) 0.1805(4) 0.6242(4) 0.0305(12) Uani 1 1 d . . . C10 C 1.0000 0.1773(5) 0.7500 0.0287(16) Uani 1 2 d S . . H10 H 1.0000 0.2331 0.7500 0.034 Uiso 1 2 calc SR . . C11 C 0.9376(3) 0.1364(3) 0.6899(4) 0.0279(12) Uani 1 1 d . . . C12 C 0.9376(3) 0.0533(4) 0.6918(4) 0.0367(14) Uani 1 1 d . . . H12 H 0.8960 0.0248 0.6543 0.044 Uiso 1 1 calc R . . C13 C 1.0000 0.0137(5) 0.7500 0.041(2) Uani 1 2 d S . . C14 C 0.5932(6) 0.0223(6) 0.3124(7) 0.085(3) Uani 1 1 d . . . H14 H 0.6081 -0.0302 0.3314 0.103 Uiso 1 1 calc R . . C15 C 0.5624(10) 0.1283(11) 0.1845(19) 0.222(12) Uani 1 1 d U . . H15A H 0.5762 0.1673 0.2343 0.333 Uiso 1 1 calc R . . H15B H 0.5137 0.1371 0.1366 0.333 Uiso 1 1 calc R . . H15C H 0.5921 0.1334 0.1567 0.333 Uiso 1 1 calc R . . C16 C 0.5598(10) -0.0232(12) 0.1566(13) 0.192(8) Uani 1 1 d U . . H16A H 0.5629 -0.0750 0.1844 0.288 Uiso 1 1 calc R . . H16B H 0.5958 -0.0188 0.1391 0.288 Uiso 1 1 calc R . . H16C H 0.5139 -0.0170 0.1010 0.288 Uiso 1 1 calc R . . C17 C 0.5613(5) 0.2223(8) 0.5292(7) 0.084(3) Uani 1 1 d . . . H17 H 0.5854 0.2699 0.5349 0.101 Uiso 1 1 calc R . . C18 C 0.4646(13) 0.1626(13) 0.529(2) 0.261(13) Uani 1 1 d U . . H18A H 0.4319 0.1548 0.4624 0.392 Uiso 1 1 calc R . . H18B H 0.4387 0.1713 0.5618 0.392 Uiso 1 1 calc R . . H18C H 0.4940 0.1160 0.5545 0.392 Uiso 1 1 calc R . . C19 C 0.4891(11) 0.3056(14) 0.566(2) 0.246(12) Uani 1 1 d U . . H19A H 0.5284 0.3419 0.5867 0.370 Uiso 1 1 calc R . . H19B H 0.4792 0.2980 0.6173 0.370 Uiso 1 1 calc R . . H19C H 0.4480 0.3275 0.5121 0.370 Uiso 1 1 calc R . . C20 C 0.8618(8) -0.0220(10) 0.9548(9) 0.110(4) Uani 1 1 d U . . H20 H 0.8336 -0.0277 0.9827 0.132 Uiso 1 1 calc R . . C21 C 0.7943(9) 0.0882(9) 0.8750(11) 0.137(5) Uani 1 1 d U . . H21A H 0.7676 0.0670 0.9027 0.206 Uiso 1 1 calc R . . H21B H 0.7643 0.0912 0.8071 0.206 Uiso 1 1 calc R . . H21C H 0.8112 0.1408 0.9000 0.206 Uiso 1 1 calc R . . C22 C 0.8917(11) 0.0495(15) 0.8537(13) 0.217(10) Uani 1 1 d U . . H22A H 0.9164 0.0008 0.8569 0.325 Uiso 1 1 calc R . . H22B H 0.9255 0.0916 0.8857 0.325 Uiso 1 1 calc R . . H22C H 0.8610 0.0640 0.7883 0.325 Uiso 1 1 calc R . . O9 O 1.0562(3) -0.1082(3) 0.7973(6) 0.098(3) Uani 1 1 d . . . N1 N 0.8367(4) -0.2643(4) 0.6348(6) 0.0658(19) Uani 1 1 d . . . N2 N 1.0000 -0.0742(5) 0.7500 0.065(3) Uani 1 2 d S . . N3 N 0.5707(7) 0.0408(8) 0.2276(8) 0.135(4) Uani 1 1 d U . . N4 N 0.5070(5) 0.2290(8) 0.5412(9) 0.121(4) Uani 1 1 d U . . 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 N5 0.117(8) 0.124(8) 0.071(6) -0.009(5) 0.057(6) -0.028(5) Dy1 0.01851(13) 0.02735(14) 0.02062(13) 0.00108(11) 0.00760(10) 0.00136(10) O1 0.089(4) 0.036(3) 0.034(2) 0.003(2) 0.033(3) -0.003(3) O2 0.068(3) 0.041(3) 0.049(3) 0.017(2) 0.041(3) 0.015(2) O3 0.042(3) 0.060(3) 0.029(2) -0.004(2) 0.021(2) -0.011(2) O4 0.045(3) 0.053(3) 0.036(2) 0.017(2) 0.011(2) -0.008(2) O5 0.079(4) 0.092(5) 0.077(4) -0.025(4) 0.059(4) 0.002(3) O6 0.202(10) 0.082(5) 0.144(8) 0.037(6) 0.122(8) 0.084(6) O7 0.0154(18) 0.045(3) 0.040(2) 0.003(2) 0.0025(18) 0.0018(17) O8 0.029(2) 0.034(2) 0.037(2) 0.0112(19) 0.0086(19) 0.0060(17) O11 0.062(4) 0.084(5) 0.073(4) -0.010(4) 0.022(3) -0.002(3) O10 0.077(5) 0.099(5) 0.124(6) 0.019(5) 0.076(5) 0.007(4) O12 0.126(9) 0.213(13) 0.142(9) 0.011(9) 0.045(8) 0.048(8) C1 0.041(3) 0.035(3) 0.032(3) 0.004(3) 0.019(3) -0.002(3) C2 0.036(3) 0.034(3) 0.029(3) 0.003(2) 0.018(3) 0.002(2) C3 0.030(3) 0.031(3) 0.026(3) 0.003(2) 0.014(2) 0.002(2) C4 0.032(3) 0.037(3) 0.021(3) 0.003(2) 0.012(2) -0.002(2) C5 0.041(3) 0.034(3) 0.038(3) 0.007(3) 0.018(3) 0.004(3) C6 0.046(4) 0.039(4) 0.051(4) -0.002(3) 0.029(3) 0.007(3) C7 0.053(4) 0.040(4) 0.035(3) 0.003(3) 0.031(3) 0.000(3) C8 0.031(3) 0.038(3) 0.024(3) 0.005(3) 0.010(2) -0.007(3) C9 0.018(3) 0.040(3) 0.025(3) 0.002(2) 0.005(2) 0.006(2) C10 0.018(4) 0.033(4) 0.029(4) 0.000 0.008(3) 0.000 C11 0.016(2) 0.031(3) 0.029(3) 0.000(2) 0.005(2) 0.000(2) C12 0.021(3) 0.035(3) 0.042(3) -0.005(3) 0.007(3) -0.005(2) C13 0.026(4) 0.032(5) 0.056(6) 0.000 0.015(4) 0.000 C14 0.103(8) 0.066(6) 0.059(6) -0.016(5) 0.019(6) -0.001(6) C15 0.098(12) 0.143(11) 0.33(3) 0.026(13) 0.034(16) 0.024(11) C16 0.178(18) 0.197(15) 0.164(17) -0.083(13) 0.058(14) -0.006(15) C17 0.046(5) 0.116(9) 0.086(7) 0.009(7) 0.029(5) 0.022(6) C18 0.23(2) 0.199(16) 0.52(4) -0.01(2) 0.31(3) -0.027(15) C19 0.152(17) 0.240(17) 0.37(3) -0.11(2) 0.15(2) 0.016(16) C20 0.100(9) 0.145(11) 0.083(8) 0.007(7) 0.045(7) -0.018(7) C21 0.163(13) 0.101(10) 0.132(12) -0.040(8) 0.061(11) -0.008(8) C22 0.223(19) 0.35(3) 0.159(15) -0.002(16) 0.158(16) -0.064(17) O9 0.042(3) 0.033(3) 0.166(7) 0.009(4) 0.012(4) 0.011(3) N1 0.075(5) 0.056(4) 0.082(5) -0.011(4) 0.050(4) 0.015(4) N2 0.037(5) 0.040(5) 0.086(7) 0.000 0.008(5) 0.000 N3 0.124(9) 0.153(10) 0.071(7) -0.013(6) 0.007(6) 0.035(8) N4 0.070(6) 0.158(10) 0.150(10) -0.026(8) 0.066(7) 0.006(6) _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 N5 C20 1.313(16) . ? N5 C22 1.374(15) . ? N5 C21 1.397(17) . ? Dy1 O4 2.279(4) 4_656 ? Dy1 O7 2.315(4) . ? Dy1 O8 2.339(4) 7_656 ? Dy1 O3 2.354(4) 6 ? Dy1 O11 2.361(6) . ? Dy1 O10 2.408(6) . ? Dy1 O2 2.432(4) . ? Dy1 O1 2.443(5) . ? O1 C1 1.247(7) . ? O2 C1 1.255(8) . ? O3 C8 1.246(8) . ? O3 Dy1 2.354(4) 6_556 ? O4 C8 1.260(8) . ? O4 Dy1 2.279(4) 4_646 ? O5 N1 1.195(9) . ? O6 N1 1.219(10) . ? O7 C9 1.257(7) . ? O8 C9 1.244(7) . ? O8 Dy1 2.339(4) 7_656 ? O11 C14 1.289(11) . ? O10 C17 1.252(12) . ? O12 C20 1.263(16) . ? C1 C2 1.512(8) . ? C2 C7 1.375(8) . ? C2 C3 1.399(8) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.381(9) . ? C4 C8 1.498(8) . ? C5 C6 1.375(9) . ? C5 H5 0.9300 . ? C6 C7 1.381(9) . ? C6 N1 1.477(9) . ? C7 H7 0.9300 . ? C9 C11 1.506(7) . ? C10 C11 1.391(7) . ? C10 C11 1.391(7) 2_756 ? C10 H10 0.9300 . ? C11 C12 1.387(8) . ? C12 C13 1.374(7) . ? C12 H12 0.9300 . ? C13 C12 1.374(7) 2_756 ? C13 N2 1.466(12) . ? C14 N3 1.246(14) . ? C14 H14 0.9300 . ? C15 N3 1.59(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N3 1.501(18) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N4 1.294(12) . ? C17 H17 0.9300 . ? C18 N4 1.39(2) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.45(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O9 N2 1.210(7) . ? N2 O9 1.210(7) 2_756 ? 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 C20 N5 C22 123.4(16) . . ? C20 N5 C21 116.5(12) . . ? C22 N5 C21 119.9(15) . . ? O4 Dy1 O7 76.00(16) 4_656 . ? O4 Dy1 O8 80.29(17) 4_656 7_656 ? O7 Dy1 O8 125.43(15) . 7_656 ? O4 Dy1 O3 124.98(18) 4_656 6 ? O7 Dy1 O3 78.36(16) . 6 ? O8 Dy1 O3 76.46(16) 7_656 6 ? O4 Dy1 O11 145.7(2) 4_656 . ? O7 Dy1 O11 138.3(2) . . ? O8 Dy1 O11 77.9(2) 7_656 . ? O3 Dy1 O11 74.7(2) 6 . ? O4 Dy1 O10 78.2(2) 4_656 . ? O7 Dy1 O10 142.8(2) . . ? O8 Dy1 O10 75.0(2) 7_656 . ? O3 Dy1 O10 138.8(2) 6 . ? O11 Dy1 O10 70.8(3) . . ? O4 Dy1 O2 89.80(18) 4_656 . ? O7 Dy1 O2 79.89(17) . . ? O8 Dy1 O2 148.46(15) 7_656 . ? O3 Dy1 O2 131.85(16) 6 . ? O11 Dy1 O2 95.1(2) . . ? O10 Dy1 O2 73.7(2) . . ? O4 Dy1 O1 135.10(16) 4_656 . ? O7 Dy1 O1 72.89(17) . . ? O8 Dy1 O1 144.56(16) 7_656 . ? O3 Dy1 O1 78.98(16) 6 . ? O11 Dy1 O1 71.2(2) . . ? O10 Dy1 O1 109.5(2) . . ? O2 Dy1 O1 53.62(15) . . ? C1 O1 Dy1 91.5(4) . . ? C1 O2 Dy1 91.9(4) . . ? C8 O3 Dy1 125.1(4) . 6_556 ? C8 O4 Dy1 164.0(5) . 4_646 ? C9 O7 Dy1 144.6(4) . . ? C9 O8 Dy1 139.5(4) . 7_656 ? C14 O11 Dy1 133.4(7) . . ? C17 O10 Dy1 130.8(7) . . ? O1 C1 O2 122.9(6) . . ? O1 C1 C2 117.5(6) . . ? O2 C1 C2 119.4(5) . . ? C7 C2 C3 119.3(6) . . ? C7 C2 C1 118.5(5) . . ? C3 C2 C1 122.2(5) . . ? C4 C3 C2 120.9(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 C8 120.3(5) . . ? C5 C4 C8 120.3(6) . . ? C6 C5 C4 119.0(6) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.4(6) . . ? C5 C6 N1 120.4(7) . . ? C7 C6 N1 117.2(6) . . ? C2 C7 C6 118.9(6) . . ? C2 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? O3 C8 O4 125.8(6) . . ? O3 C8 C4 117.6(5) . . ? O4 C8 C4 116.6(6) . . ? O8 C9 O7 125.8(5) . . ? O8 C9 C11 117.7(5) . . ? O7 C9 C11 116.5(5) . . ? C11 C10 C11 121.2(8) . 2_756 ? C11 C10 H10 119.4 . . ? C11 C10 H10 119.4 2_756 . ? C12 C11 C10 119.1(6) . . ? C12 C11 C9 119.5(5) . . ? C10 C11 C9 121.4(6) . . ? C13 C12 C11 119.0(6) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C12 122.5(8) 2_756 . ? C12 C13 N2 118.8(4) 2_756 . ? C12 C13 N2 118.8(4) . . ? N3 C14 O11 122.8(11) . . ? N3 C14 H14 118.6 . . ? O11 C14 H14 118.6 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O10 C17 N4 130.0(13) . . ? O10 C17 H17 115.0 . . ? N4 C17 H17 115.0 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O12 C20 N5 118.7(14) . . ? O12 C20 H20 120.7 . . ? N5 C20 H20 120.7 . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 N1 O6 124.6(7) . . ? O5 N1 C6 119.4(7) . . ? O6 N1 C6 116.0(7) . . ? O9 N2 O9 124.1(10) 2_756 . ? O9 N2 C13 117.9(5) 2_756 . ? O9 N2 C13 117.9(5) . . ? C14 N3 C16 119.6(14) . . ? C14 N3 C15 127.5(15) . . ? C16 N3 C15 112.2(15) . . ? C17 N4 C18 120.0(14) . . ? C17 N4 C19 120.7(14) . . ? C18 N4 C19 119.2(14) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.365 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.157 # Attachment 'revised1-Nd.cif' data_xb0700m _database_code_depnum_ccdc_archive 'CCDC 741285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 N9 Nd2 O24' _chemical_formula_weight 1354.40 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 monoclinic _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.854(3) _cell_length_b 17.034(2) _cell_length_c 16.445(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.559(2) _cell_angle_gamma 90.00 _cell_volume 5325.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 2.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16578 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.91 _reflns_number_total 6299 _reflns_number_gt 4395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00002(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6299 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Nd1 Nd 0.690041(11) 0.643695(13) 0.499353(15) 0.02107(9) Uani 1 1 d . . . O1 O 0.72894(17) 0.50048(18) 0.5194(2) 0.0376(8) Uani 1 1 d . . . O2 O 0.70316(17) 0.54799(18) 0.6232(2) 0.0402(8) Uani 1 1 d . . . O3 O 0.72279(16) 0.37018(18) 0.8775(2) 0.0330(8) Uani 1 1 d . . . O4 O 0.77696(16) 0.25450(19) 0.9005(2) 0.0392(8) Uani 1 1 d . . . O5 O 0.8717(3) 0.1825(3) 0.6960(4) 0.0936(17) Uani 1 1 d . . . O6 O 0.8370(2) 0.2438(2) 0.5668(3) 0.0641(11) Uani 1 1 d . . . O7 O 0.87678(15) 0.75145(17) 0.6105(2) 0.0330(7) Uani 1 1 d . . . O8 O 0.81599(14) 0.64100(18) 0.5891(2) 0.0349(8) Uani 1 1 d . . . O9 O 1.05633(18) 0.3963(2) 0.7938(3) 0.0595(12) Uani 1 1 d . . . O10 O 0.58595(17) 0.6679(2) 0.5204(3) 0.0472(9) Uani 1 1 d . . . O11 O 0.59650(15) 0.5690(2) 0.3754(2) 0.0426(8) Uani 1 1 d . . . O12 O 0.5948(2) -0.0702(3) 0.5287(4) 0.0956(17) Uani 1 1 d . . . N1 N 0.8408(2) 0.2354(3) 0.6421(4) 0.0515(12) Uani 1 1 d . . . N2 N 1.0000 0.4308(3) 0.7500 0.0391(14) Uani 1 2 d S . . N3 N 0.5053(2) 0.7402(3) 0.5355(4) 0.0559(13) Uani 1 1 d . . . N4 N 0.5750(2) 0.5463(3) 0.2283(3) 0.0499(12) Uani 1 1 d . . . N5 N 0.6552(3) 0.0376(3) 0.6065(4) 0.0580(13) Uani 1 1 d . . . C1 C 0.7493(2) 0.4174(3) 0.6471(3) 0.0291(10) Uani 1 1 d . . . C2 C 0.7411(2) 0.4032(2) 0.7244(3) 0.0275(10) Uani 1 1 d . . . H2 H 0.7192 0.4407 0.7424 0.033 Uiso 1 1 calc R . . C3 C 0.7646(2) 0.3343(3) 0.7750(3) 0.0276(10) Uani 1 1 d . . . C4 C 0.7976(2) 0.2789(3) 0.7483(3) 0.0320(11) Uani 1 1 d . . . H4 H 0.8144 0.2324 0.7817 0.038 Uiso 1 1 calc R . . C5 C 0.8052(2) 0.2941(3) 0.6709(3) 0.0333(11) Uani 1 1 d . . . C6 C 0.7816(2) 0.3615(3) 0.6196(3) 0.0322(10) Uani 1 1 d . . . H6 H 0.7870 0.3697 0.5676 0.039 Uiso 1 1 calc R . . C7 C 0.7256(2) 0.4938(3) 0.5928(3) 0.0302(10) Uani 1 1 d . . . C8 C 0.7547(2) 0.3188(3) 0.8584(3) 0.0297(10) Uani 1 1 d . . . C9 C 1.0000 0.6773(4) 0.7500 0.0256(13) Uani 1 2 d S . . H9 H 1.0000 0.7319 0.7500 0.031 Uiso 1 2 calc SR . . C10 C 0.9385(2) 0.6373(2) 0.6909(3) 0.0249(9) Uani 1 1 d . . . C11 C 0.93826(19) 0.5554(2) 0.6916(3) 0.0251(9) Uani 1 1 d . . . H11 H 0.8974 0.5274 0.6536 0.030 Uiso 1 1 calc R . . C12 C 1.0000 0.5171(3) 0.7500 0.0250(13) Uani 1 2 d S . . C13 C 0.8714(2) 0.6804(3) 0.6250(3) 0.0249(9) Uani 1 1 d . . . C14 C 0.5617(3) 0.7314(3) 0.5269(4) 0.0474(14) Uani 1 1 d . . . H14 H 0.5851 0.7767 0.5257 0.057 Uiso 1 1 calc R . . C15 C 0.4835(4) 0.8156(4) 0.5507(7) 0.108(3) Uani 1 1 d . . . H15A H 0.5147 0.8553 0.5505 0.161 Uiso 1 1 calc R . . H15B H 0.4850 0.8158 0.6100 0.161 Uiso 1 1 calc R . . H15C H 0.4365 0.8262 0.5018 0.161 Uiso 1 1 calc R . . C16 C 0.4648(4) 0.6733(4) 0.5372(6) 0.089(3) Uani 1 1 d . . . H16A H 0.4799 0.6269 0.5189 0.134 Uiso 1 1 calc R . . H16B H 0.4158 0.6822 0.4946 0.134 Uiso 1 1 calc R . . H16C H 0.4720 0.6666 0.5993 0.134 Uiso 1 1 calc R . . C17 C 0.5907(3) 0.5243(3) 0.3121(4) 0.0511(15) Uani 1 1 d . . . H17 H 0.5983 0.4711 0.3259 0.061 Uiso 1 1 calc R . . C18 C 0.5648(3) 0.4907(4) 0.1558(5) 0.084(2) Uani 1 1 d . . . H18A H 0.5776 0.4390 0.1822 0.126 Uiso 1 1 calc R . . H18B H 0.5937 0.5053 0.1294 0.126 Uiso 1 1 calc R . . H18C H 0.5163 0.4909 0.1077 0.126 Uiso 1 1 calc R . . C19 C 0.5645(3) 0.6284(3) 0.2012(4) 0.0567(16) Uani 1 1 d . . . H19A H 0.5728 0.6601 0.2540 0.085 Uiso 1 1 calc R . . H19B H 0.5170 0.6361 0.1518 0.085 Uiso 1 1 calc R . . H19C H 0.5965 0.6434 0.1799 0.085 Uiso 1 1 calc R . . C20 C 0.6411(3) -0.0211(4) 0.5475(4) 0.0640(18) Uani 1 1 d . . . H20 H 0.6680 -0.0256 0.5182 0.077 Uiso 1 1 calc R . . C21 C 0.7153(4) 0.0884(4) 0.6293(5) 0.082(2) Uani 1 1 d . . . H21A H 0.7450 0.0906 0.6959 0.123 Uiso 1 1 calc R . . H21B H 0.6989 0.1402 0.6056 0.123 Uiso 1 1 calc R . . H21C H 0.7414 0.0678 0.6013 0.123 Uiso 1 1 calc R . . C22 C 0.6173(4) 0.0466(5) 0.6566(6) 0.113(3) Uani 1 1 d . . . H22A H 0.5695 0.0300 0.6177 0.169 Uiso 1 1 calc R . . H22B H 0.6181 0.1007 0.6734 0.169 Uiso 1 1 calc R . . H22C H 0.6390 0.0150 0.7121 0.169 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 Nd1 0.01894(12) 0.02171(13) 0.02179(14) 0.00026(11) 0.00946(10) 0.00021(10) O1 0.053(2) 0.0337(19) 0.0334(19) 0.0058(15) 0.0274(17) 0.0020(16) O2 0.057(2) 0.0320(19) 0.044(2) 0.0109(16) 0.0347(18) 0.0121(16) O3 0.0345(17) 0.040(2) 0.0281(18) 0.0050(15) 0.0182(15) 0.0014(15) O4 0.0428(19) 0.036(2) 0.036(2) 0.0143(16) 0.0170(16) 0.0027(15) O5 0.144(5) 0.063(3) 0.113(4) 0.039(3) 0.094(4) 0.065(3) O6 0.080(3) 0.071(3) 0.068(3) -0.007(2) 0.056(3) 0.014(2) O7 0.0288(16) 0.0273(18) 0.0332(19) 0.0047(14) 0.0079(14) -0.0001(13) O8 0.0175(15) 0.0360(19) 0.039(2) -0.0009(16) 0.0044(14) -0.0010(14) O9 0.043(2) 0.028(2) 0.092(3) 0.006(2) 0.021(2) 0.0091(17) O10 0.038(2) 0.054(2) 0.062(3) 0.0041(19) 0.034(2) 0.0093(17) O11 0.0292(17) 0.046(2) 0.043(2) -0.0096(18) 0.0100(16) -0.0079(16) O12 0.081(3) 0.112(4) 0.098(4) -0.019(3) 0.047(3) -0.032(3) N1 0.061(3) 0.041(3) 0.067(4) 0.000(3) 0.043(3) 0.010(2) N2 0.033(3) 0.028(3) 0.057(4) 0.000 0.023(3) 0.000 N3 0.041(2) 0.054(3) 0.087(4) 0.000(3) 0.043(3) 0.015(2) N4 0.036(2) 0.054(3) 0.041(3) -0.013(2) 0.005(2) 0.008(2) N5 0.071(3) 0.063(3) 0.055(3) -0.003(3) 0.043(3) 0.000(3) C1 0.029(2) 0.026(2) 0.034(3) 0.004(2) 0.017(2) 0.0037(19) C2 0.029(2) 0.025(2) 0.032(3) 0.003(2) 0.018(2) 0.0022(19) C3 0.029(2) 0.029(2) 0.028(3) 0.0016(19) 0.017(2) 0.0040(19) C4 0.036(2) 0.022(2) 0.042(3) 0.007(2) 0.022(2) 0.001(2) C5 0.038(3) 0.030(3) 0.041(3) -0.001(2) 0.027(2) 0.007(2) C6 0.037(2) 0.038(3) 0.031(3) 0.001(2) 0.023(2) 0.001(2) C7 0.029(2) 0.031(3) 0.033(3) 0.008(2) 0.017(2) 0.000(2) C8 0.021(2) 0.032(3) 0.028(3) 0.010(2) 0.006(2) -0.003(2) C9 0.024(3) 0.020(3) 0.025(3) 0.000 0.007(3) 0.000 C10 0.023(2) 0.024(2) 0.027(2) -0.0006(19) 0.0118(19) -0.0013(18) C11 0.016(2) 0.029(2) 0.026(2) -0.0009(19) 0.0072(18) -0.0018(17) C12 0.022(3) 0.019(3) 0.033(4) 0.000 0.012(3) 0.000 C13 0.020(2) 0.025(2) 0.024(2) -0.0015(19) 0.0072(19) 0.0015(18) C14 0.040(3) 0.057(4) 0.045(3) -0.005(3) 0.021(3) 0.006(3) C15 0.101(6) 0.075(5) 0.193(10) -0.028(6) 0.109(7) 0.002(5) C16 0.096(5) 0.077(5) 0.144(8) 0.023(5) 0.097(6) 0.021(4) C17 0.029(3) 0.043(3) 0.058(4) -0.016(3) 0.003(3) 0.001(2) C18 0.068(4) 0.097(6) 0.069(5) -0.051(4) 0.020(4) 0.001(4) C19 0.040(3) 0.079(5) 0.044(4) -0.002(3) 0.015(3) 0.006(3) C20 0.059(4) 0.088(5) 0.054(4) -0.001(4) 0.035(3) 0.006(4) C21 0.102(6) 0.069(5) 0.079(5) -0.007(4) 0.047(5) -0.013(4) C22 0.107(6) 0.175(9) 0.089(6) 0.000(6) 0.074(5) 0.034(6) _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 O4 2.372(3) 4_656 ? Nd1 O8 2.398(3) . ? Nd1 O11 2.417(3) . ? Nd1 O7 2.446(3) 7_666 ? Nd1 O3 2.449(3) 6_565 ? Nd1 O10 2.499(3) . ? Nd1 O2 2.513(3) . ? Nd1 O1 2.551(3) . ? O1 C7 1.249(5) . ? O2 C7 1.259(5) . ? O3 C8 1.252(5) . ? O3 Nd1 2.449(3) 6_566 ? O4 C8 1.258(5) . ? O4 Nd1 2.372(3) 4_646 ? O5 N1 1.210(6) . ? O6 N1 1.208(6) . ? O7 C13 1.250(5) . ? O7 Nd1 2.446(3) 7_666 ? O8 C13 1.249(5) . ? O9 N2 1.227(4) . ? O10 C14 1.233(6) . ? O11 C17 1.245(6) . ? O12 C20 1.228(7) . ? N1 C5 1.481(6) . ? N2 O9 1.227(4) 2_756 ? N2 C12 1.471(8) . ? N3 C14 1.317(6) . ? N3 C15 1.434(7) . ? N3 C16 1.451(7) . ? N4 C17 1.300(7) . ? N4 C19 1.451(7) . ? N4 C18 1.453(7) . ? N5 C20 1.320(8) . ? N5 C22 1.435(8) . ? N5 C21 1.458(7) . ? C1 C6 1.389(6) . ? C1 C2 1.390(6) . ? C1 C7 1.518(6) . ? C2 C3 1.383(6) . ? C2 H2 0.9300 . ? C3 C4 1.384(6) . ? C3 C8 1.512(6) . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.367(6) . ? C6 H6 0.9300 . ? C9 C10 1.388(5) . ? C9 C10 1.388(5) 2_756 ? C9 H9 0.9300 . ? C10 C11 1.396(6) . ? C10 C13 1.515(5) . ? C11 C12 1.374(5) . ? C11 H11 0.9300 . ? C12 C11 1.374(5) 2_756 ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd1 O8 73.99(11) 4_656 . ? O4 Nd1 O11 147.73(11) 4_656 . ? O8 Nd1 O11 138.23(11) . . ? O4 Nd1 O7 78.34(11) 4_656 7_666 ? O8 Nd1 O7 123.68(10) . 7_666 ? O11 Nd1 O7 79.22(11) . 7_666 ? O4 Nd1 O3 122.26(11) 4_656 6_565 ? O8 Nd1 O3 77.99(11) . 6_565 ? O11 Nd1 O3 74.10(11) . 6_565 ? O7 Nd1 O3 77.02(10) 7_666 6_565 ? O4 Nd1 O10 76.00(12) 4_656 . ? O8 Nd1 O10 139.90(12) . . ? O11 Nd1 O10 75.79(12) . . ? O7 Nd1 O10 74.29(11) 7_666 . ? O3 Nd1 O10 141.53(11) 6_565 . ? O4 Nd1 O2 94.54(12) 4_656 . ? O8 Nd1 O2 81.44(11) . . ? O11 Nd1 O2 93.05(12) . . ? O7 Nd1 O2 149.34(10) 7_666 . ? O3 Nd1 O2 129.66(10) 6_565 . ? O10 Nd1 O2 75.05(11) . . ? O4 Nd1 O1 134.71(11) 4_656 . ? O8 Nd1 O1 72.18(10) . . ? O11 Nd1 O1 72.25(11) . . ? O7 Nd1 O1 146.46(10) 7_666 . ? O3 Nd1 O1 78.49(10) 6_565 . ? O10 Nd1 O1 114.07(11) . . ? O2 Nd1 O1 51.47(10) . . ? C7 O1 Nd1 92.1(3) . . ? C7 O2 Nd1 93.7(3) . . ? C8 O3 Nd1 124.2(3) . 6_566 ? C8 O4 Nd1 167.8(3) . 4_646 ? C13 O7 Nd1 140.3(3) . 7_666 ? C13 O8 Nd1 146.2(3) . . ? C14 O10 Nd1 128.0(4) . . ? C17 O11 Nd1 136.2(3) . . ? O6 N1 O5 124.8(5) . . ? O6 N1 C5 117.9(5) . . ? O5 N1 C5 117.4(5) . . ? O9 N2 O9 122.8(6) . 2_756 ? O9 N2 C12 118.6(3) . . ? O9 N2 C12 118.6(3) 2_756 . ? C14 N3 C15 121.9(5) . . ? C14 N3 C16 121.7(5) . . ? C15 N3 C16 116.3(5) . . ? C17 N4 C19 121.5(5) . . ? C17 N4 C18 122.4(5) . . ? C19 N4 C18 116.1(5) . . ? C20 N5 C22 120.7(6) . . ? C20 N5 C21 119.5(6) . . ? C22 N5 C21 119.4(6) . . ? C6 C1 C2 119.6(4) . . ? C6 C1 C7 118.5(4) . . ? C2 C1 C7 121.9(4) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 C8 121.1(4) . . ? C4 C3 C8 120.0(4) . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 122.9(4) . . ? C6 C5 N1 117.9(4) . . ? C4 C5 N1 119.2(4) . . ? C5 C6 C1 118.2(4) . . ? C5 C6 H6 120.9 . . ? C1 C6 H6 120.9 . . ? O1 C7 O2 122.5(4) . . ? O1 C7 C1 118.8(4) . . ? O2 C7 C1 118.7(4) . . ? O3 C8 O4 125.6(4) . . ? O3 C8 C3 116.9(4) . . ? O4 C8 C3 117.4(4) . . ? C10 C9 C10 121.2(6) . 2_756 ? C10 C9 H9 119.4 . . ? C10 C9 H9 119.4 2_756 . ? C9 C10 C11 119.4(4) . . ? C9 C10 C13 121.6(4) . . ? C11 C10 C13 119.0(4) . . ? C12 C11 C10 118.3(4) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C11 C12 C11 123.4(5) 2_756 . ? C11 C12 N2 118.3(3) 2_756 . ? C11 C12 N2 118.3(3) . . ? O8 C13 O7 126.2(4) . . ? O8 C13 C10 116.6(4) . . ? O7 C13 C10 117.2(4) . . ? O10 C14 N3 125.0(6) . . ? O10 C14 H14 117.5 . . ? N3 C14 H14 117.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O11 C17 N4 125.1(5) . . ? O11 C17 H17 117.5 . . ? N4 C17 H17 117.5 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O12 C20 N5 124.5(6) . . ? O12 C20 H20 117.7 . . ? N5 C20 H20 117.7 . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.387 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.132