data_p21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H24 N9 Nd2 O16, N O3, 6(H2 O)' _chemical_formula_sum 'C30 H36 N10 Nd2 O25' _chemical_formula_weight 1225.17 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 p2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 10.550(2) _cell_length_b 22.245(4) _cell_length_c 19.971(4) _cell_angle_alpha 90.00 _cell_angle_beta 119.66(3) _cell_angle_gamma 90.00 _cell_volume 4072.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9255 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 2.630 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1241 _exptl_absorpt_correction_T_max 0.9400 _exptl_absorpt_process_details 'Process-auto' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 38514 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9255 _reflns_number_gt 8433 _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^)+(0.0254P)^2^+14.6619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9255 _refine_ls_number_parameters 646 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.006 _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 0.30932(2) 0.464131(7) 0.353834(9) 0.01940(5) Uani 1 1 d . . . Nd2 Nd 0.113537(19) 0.530935(7) 0.139007(9) 0.01848(5) Uani 1 1 d . . . O1 O 0.2113(3) 0.43635(10) 0.21334(13) 0.0252(5) Uani 1 1 d . . . O2 O 0.3148(3) 0.35889(11) 0.28907(13) 0.0309(6) Uani 1 1 d . . . O3 O 0.0586(3) 0.44921(11) 0.05456(14) 0.0338(6) Uani 1 1 d . . . O4 O -0.0164(3) 0.38919(11) -0.04524(13) 0.0276(5) Uani 1 1 d . . . O5 O 0.1993(3) 0.49893(11) 0.42649(16) 0.0337(6) Uani 1 1 d . . . O6 O 0.1734(3) 0.54772(11) 0.51540(14) 0.0295(6) Uani 1 1 d . . . H6 H 0.1879 0.5140 0.5344 0.080 Uiso 1 1 calc . . . O7 O 0.0808(3) 0.52019(11) 0.26829(14) 0.0280(5) Uani 1 1 d . . . O8 O 0.0223(3) 0.60454(12) 0.20233(14) 0.0335(6) Uani 1 1 d . . . O9 O 0.5224(4) 0.46272(11) 0.56531(15) 0.0402(7) Uani 1 1 d . . . O10 O 0.4235(3) 0.39885(11) 0.46720(13) 0.0310(6) Uani 1 1 d . . . O11 O 0.6634(3) 0.45198(10) 0.72411(13) 0.0261(5) Uani 1 1 d . . . O12 O 0.7083(3) 0.37621(11) 0.80266(13) 0.0282(5) Uani 1 1 d . . . O13 O 0.5450(3) 0.43948(14) 0.35858(17) 0.0409(7) Uani 1 1 d D . . O14 O 0.1002(4) 0.39438(14) 0.32662(18) 0.0422(7) Uani 1 1 d D . . O15 O -0.1443(3) 0.50692(11) 0.09077(16) 0.0315(6) Uani 1 1 d D . . O16 O 0.3095(3) 0.52705(11) 0.10991(18) 0.0342(6) Uani 1 1 d D . . N1 N 0.2210(3) 0.27935(11) 0.17016(15) 0.0201(5) Uani 1 1 d . . . H1 H 0.2698 0.2625 0.2146 0.080 Uiso 1 1 calc . . . N2 N 0.0921(3) 0.29000(12) 0.04332(15) 0.0205(6) Uani 1 1 d . . . N3 N 0.1740(4) 0.06715(13) 0.06025(19) 0.0323(7) Uani 1 1 d . . . N4 N 0.1854(3) 0.65721(12) 0.44986(16) 0.0230(6) Uani 1 1 d . . . N5 N 0.0998(3) 0.67498(12) 0.32595(16) 0.0234(6) Uani 1 1 d . . . H5 H 0.0701 0.6945 0.2836 0.080 Uiso 1 1 calc . . . N6 N 0.2336(4) 0.88714(14) 0.4428(2) 0.0373(8) Uani 1 1 d . . . N7 N 0.4814(3) 0.30304(12) 0.56191(15) 0.0216(6) Uani 1 1 d . . . H7 H 0.4421 0.2933 0.5141 0.080 Uiso 1 1 calc . . . N8 N 0.5760(3) 0.29383(12) 0.68801(16) 0.0221(6) Uani 1 1 d . . . N9 N 0.4235(4) 0.07766(14) 0.5986(2) 0.0396(8) Uani 1 1 d . . . C1 C 0.1607(4) 0.25147(14) 0.10111(18) 0.0203(6) Uani 1 1 d . . . C2 C 0.1901(4) 0.33952(13) 0.15647(17) 0.0181(6) Uani 1 1 d . . . C3 C 0.1095(4) 0.34511(13) 0.07666(17) 0.0181(6) Uani 1 1 d . . . C4 C 0.2184(6) 0.08500(18) 0.1315(2) 0.0441(11) Uani 1 1 d . . . H4 H 0.2517 0.0568 0.1710 0.080 Uiso 1 1 calc . . . C5 C 0.2158(5) 0.14537(17) 0.1480(2) 0.0374(9) Uani 1 1 d . . . H5A H 0.2464 0.1577 0.1983 0.080 Uiso 1 1 calc . . . C6 C 0.1670(4) 0.18692(14) 0.08900(19) 0.0219(6) Uani 1 1 d . . . C7 C 0.1213(5) 0.16618(17) 0.0150(2) 0.0359(9) Uani 1 1 d . . . H7A H 0.0881 0.1931 -0.0259 0.080 Uiso 1 1 calc . . . C8 C 0.1252(5) 0.10581(18) 0.0023(2) 0.0397(10) Uani 1 1 d . . . H8 H 0.0932 0.0919 -0.0475 0.080 Uiso 1 1 calc . . . C9 C 0.2421(4) 0.38087(14) 0.22314(18) 0.0200(6) Uani 1 1 d . . . C10 C 0.0461(3) 0.39882(14) 0.02557(17) 0.0184(6) Uani 1 1 d . . . C11 C 0.1540(4) 0.69927(14) 0.39674(19) 0.0218(6) Uani 1 1 d . . . C12 C 0.1527(4) 0.60355(14) 0.41084(18) 0.0206(6) Uani 1 1 d . . . C13 C 0.1001(4) 0.61351(14) 0.33319(19) 0.0211(6) Uani 1 1 d . . . C14 C 0.2775(5) 0.84703(17) 0.4994(2) 0.0372(9) Uani 1 1 d . . . H14 H 0.3258 0.8610 0.5499 0.080 Uiso 1 1 calc . . . C15 C 0.2552(5) 0.78552(16) 0.4874(2) 0.0319(8) Uani 1 1 d . . . H15 H 0.2890 0.7592 0.5289 0.080 Uiso 1 1 calc . . . C16 C 0.1818(4) 0.76392(15) 0.4124(2) 0.0239(7) Uani 1 1 d . . . C17 C 0.1376(5) 0.80555(17) 0.3533(2) 0.0368(9) Uani 1 1 d . . . H17 H 0.0888 0.7932 0.3021 0.080 Uiso 1 1 calc . . . C18 C 0.1674(6) 0.86580(17) 0.3720(3) 0.0416(10) Uani 1 1 d . . . H18 H 0.1386 0.8931 0.3318 0.080 Uiso 1 1 calc . . . C19 C 0.1771(4) 0.54567(14) 0.45360(19) 0.0215(6) Uani 1 1 d . . . C20 C 0.0613(4) 0.57677(15) 0.26347(19) 0.0231(7) Uani 1 1 d . . . C21 C 0.5168(4) 0.26473(14) 0.62148(19) 0.0215(6) Uani 1 1 d . . . C22 C 0.5190(4) 0.35986(14) 0.59122(18) 0.0195(6) Uani 1 1 d . . . C23 C 0.5790(4) 0.35342(14) 0.67040(18) 0.0196(6) Uani 1 1 d . . . C24 C 0.3831(6) 0.11189(19) 0.5373(3) 0.0444(11) Uani 1 1 d . . . H24 H 0.3323 0.0941 0.4889 0.080 Uiso 1 1 calc . . . C25 C 0.4122(5) 0.17307(17) 0.5413(2) 0.0371(9) Uani 1 1 d . . . H25 H 0.3807 0.1955 0.4965 0.080 Uiso 1 1 calc . . . C26 C 0.4888(4) 0.19992(14) 0.6127(2) 0.0234(7) Uani 1 1 d . . . C27 C 0.5346(5) 0.16374(17) 0.6777(2) 0.0341(9) Uani 1 1 d . . . H27 H 0.5882 0.1797 0.7270 0.080 Uiso 1 1 calc . . . C28 C 0.4983(5) 0.10378(18) 0.6669(3) 0.0391(9) Uani 1 1 d . . . H28 H 0.5281 0.0800 0.7105 0.080 Uiso 1 1 calc . . . C29 C 0.4874(4) 0.41143(15) 0.53753(18) 0.0221(6) Uani 1 1 d . . . C30 C 0.6513(4) 0.39675(14) 0.73557(18) 0.0201(6) Uani 1 1 d . . . N10 N 0.6536(8) 0.5803(4) 0.1651(4) 0.1051(9) Uani 1 1 d U . . O17 O 0.5654(7) 0.5927(3) 0.1904(3) 0.1051(9) Uani 1 1 d U . . O18 O 0.7112(7) 0.5297(3) 0.1793(4) 0.1051(9) Uani 1 1 d U . . O19 O 0.6872(6) 0.6267(3) 0.1411(3) 0.1051(9) Uani 1 1 d U . . O1W O 0.8682(4) 0.27095(13) 0.87696(17) 0.0430(7) Uani 1 1 d D . . O2W O 0.4668(5) 0.2208(2) 0.3016(2) 0.0654(11) Uani 1 1 d D . . O3W O 0.3657(5) 0.26905(17) 0.4031(2) 0.0671(11) Uani 1 1 d D . . O4W O 0.7400(5) 0.34139(18) 0.3824(2) 0.0718(12) Uani 1 1 d D . . O5W O 0.0500(5) 0.2598(3) 0.3202(3) 0.0876(15) Uani 1 1 d D . . O6W O -0.1485(5) 0.4376(3) 0.3199(3) 0.0967(16) Uani 1 1 d D . . H13A H 0.579(6) 0.3981(12) 0.359(3) 0.090 Uiso 1 1 d D . . H13B H 0.631(4) 0.456(2) 0.402(3) 0.090 Uiso 1 1 d D . . H14A H 0.101(6) 0.3507(9) 0.328(4) 0.090 Uiso 1 1 d D . . H14B H 0.005(4) 0.405(2) 0.322(4) 0.090 Uiso 1 1 d D . . H15A H -0.185(6) 0.4683(16) 0.065(3) 0.090 Uiso 1 1 d D . . H15B H -0.209(6) 0.523(2) 0.109(4) 0.090 Uiso 1 1 d D . . H16A H 0.350(6) 0.4886(15) 0.104(4) 0.090 Uiso 1 1 d D . . H16B H 0.396(4) 0.548(2) 0.146(3) 0.090 Uiso 1 1 d D . . H1A H 0.934(5) 0.291(2) 0.9263(19) 0.090 Uiso 1 1 d D . . H1B H 0.801(5) 0.303(2) 0.845(3) 0.090 Uiso 1 1 d D . . H2A H 0.471(7) 0.1790(13) 0.317(4) 0.090 Uiso 1 1 d D . . H2B H 0.541(6) 0.223(3) 0.287(4) 0.090 Uiso 1 1 d D . . H3A H 0.387(7) 0.2356(17) 0.377(3) 0.090 Uiso 1 1 d D . . H3B H 0.360(7) 0.3066(14) 0.375(3) 0.090 Uiso 1 1 d D . . H4A H 0.763(7) 0.2983(10) 0.384(4) 0.090 Uiso 1 1 d D . . H4B H 0.780(7) 0.362(2) 0.353(4) 0.090 Uiso 1 1 d D . . H5B H 0.050(6) 0.2137(11) 0.332(4) 0.090 Uiso 1 1 d D . . H5C H 0.160(3) 0.267(2) 0.356(3) 0.090 Uiso 1 1 d D . . H6A H -0.188(6) 0.469(2) 0.278(3) 0.090 Uiso 1 1 d D . . H6B H -0.223(5) 0.428(3) 0.333(4) 0.090 Uiso 1 1 d 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 0.02813(10) 0.01343(8) 0.01275(8) 0.00054(6) 0.00713(7) 0.00166(6) Nd2 0.02658(10) 0.01083(8) 0.01421(8) 0.00043(5) 0.00717(7) 0.00167(6) O1 0.0404(15) 0.0129(10) 0.0177(11) -0.0002(8) 0.0109(10) 0.0037(10) O2 0.0468(16) 0.0195(12) 0.0157(11) 0.0023(9) 0.0072(11) 0.0082(11) O3 0.0542(18) 0.0138(11) 0.0212(12) -0.0008(9) 0.0093(12) 0.0063(11) O4 0.0405(15) 0.0198(11) 0.0141(11) 0.0020(9) 0.0069(10) 0.0029(10) O5 0.0601(19) 0.0170(12) 0.0357(15) 0.0013(10) 0.0328(14) 0.0053(12) O6 0.0496(16) 0.0190(11) 0.0261(13) 0.0027(9) 0.0235(12) 0.0021(11) O7 0.0318(14) 0.0206(11) 0.0250(12) -0.0048(9) 0.0090(11) 0.0037(10) O8 0.0509(17) 0.0279(13) 0.0216(12) 0.0023(10) 0.0180(12) 0.0098(12) O9 0.0593(19) 0.0207(13) 0.0204(13) 0.0025(10) 0.0044(13) -0.0124(12) O10 0.0456(16) 0.0229(12) 0.0151(11) 0.0030(9) 0.0078(11) 0.0040(11) O11 0.0393(14) 0.0162(11) 0.0183(11) 0.0001(9) 0.0107(11) -0.0046(10) O12 0.0397(15) 0.0197(11) 0.0161(11) 0.0007(9) 0.0070(11) -0.0014(10) O13 0.0323(15) 0.0454(17) 0.0374(16) -0.0059(13) 0.0114(13) 0.0033(13) O14 0.0497(18) 0.0358(15) 0.0452(17) -0.0093(13) 0.0266(15) -0.0137(14) O15 0.0298(14) 0.0227(12) 0.0397(15) -0.0045(11) 0.0155(12) -0.0035(11) O16 0.0403(16) 0.0204(12) 0.0480(17) -0.0050(11) 0.0265(14) 0.0009(11) N1 0.0285(15) 0.0123(12) 0.0163(12) 0.0015(9) 0.0086(11) 0.0042(11) N2 0.0272(15) 0.0141(12) 0.0176(13) 0.0000(10) 0.0090(11) 0.0020(11) N3 0.0375(18) 0.0190(14) 0.0385(18) -0.0046(12) 0.0174(15) 0.0009(13) N4 0.0300(15) 0.0167(13) 0.0232(14) -0.0015(10) 0.0139(12) 0.0008(11) N5 0.0320(16) 0.0179(13) 0.0220(14) 0.0013(10) 0.0148(12) 0.0034(11) N6 0.046(2) 0.0188(15) 0.047(2) -0.0023(13) 0.0233(17) 0.0007(14) N7 0.0264(15) 0.0183(13) 0.0162(13) -0.0005(10) 0.0077(11) -0.0039(11) N8 0.0284(15) 0.0162(13) 0.0199(13) 0.0009(10) 0.0105(12) -0.0025(11) N9 0.052(2) 0.0198(15) 0.053(2) -0.0031(14) 0.0310(19) -0.0080(15) C1 0.0256(17) 0.0144(14) 0.0193(15) -0.0001(11) 0.0098(13) 0.0018(12) C2 0.0236(16) 0.0124(13) 0.0166(14) 0.0015(11) 0.0086(13) 0.0020(12) C3 0.0223(16) 0.0132(13) 0.0160(14) 0.0008(11) 0.0074(12) 0.0018(12) C4 0.069(3) 0.0215(18) 0.034(2) 0.0055(15) 0.019(2) 0.0053(19) C5 0.057(3) 0.0218(18) 0.0267(19) 0.0015(14) 0.0159(19) 0.0058(17) C6 0.0251(17) 0.0149(14) 0.0261(17) -0.0019(12) 0.0131(14) 0.0016(12) C7 0.058(3) 0.0218(17) 0.0277(19) -0.0013(14) 0.0205(19) 0.0062(17) C8 0.060(3) 0.0259(19) 0.030(2) -0.0061(15) 0.020(2) 0.0037(18) C9 0.0265(17) 0.0156(14) 0.0161(14) 0.0001(11) 0.0092(13) 0.0009(12) C10 0.0206(15) 0.0158(14) 0.0162(14) 0.0033(11) 0.0071(12) 0.0024(12) C11 0.0258(17) 0.0183(15) 0.0235(16) -0.0018(12) 0.0137(14) 0.0011(13) C12 0.0267(17) 0.0161(14) 0.0204(15) -0.0013(12) 0.0126(13) 0.0013(13) C13 0.0274(17) 0.0151(14) 0.0222(16) -0.0004(12) 0.0133(14) 0.0007(12) C14 0.042(2) 0.0254(18) 0.037(2) -0.0081(15) 0.0137(18) -0.0026(17) C15 0.042(2) 0.0212(17) 0.0292(19) -0.0002(14) 0.0149(17) -0.0013(15) C16 0.0288(18) 0.0167(15) 0.0308(18) -0.0006(13) 0.0182(15) 0.0022(13) C17 0.057(3) 0.0218(18) 0.031(2) 0.0011(14) 0.0211(19) 0.0041(17) C18 0.063(3) 0.0209(18) 0.042(2) 0.0071(16) 0.027(2) 0.0035(18) C19 0.0254(17) 0.0183(15) 0.0209(15) 0.0007(12) 0.0115(13) -0.0010(13) C20 0.0239(16) 0.0239(16) 0.0218(16) -0.0035(13) 0.0115(14) 0.0018(13) C21 0.0238(17) 0.0180(15) 0.0211(16) 0.0012(12) 0.0098(13) -0.0020(13) C22 0.0202(16) 0.0171(14) 0.0173(15) -0.0009(11) 0.0063(12) -0.0026(12) C23 0.0218(16) 0.0163(14) 0.0178(15) 0.0013(11) 0.0075(13) -0.0014(12) C24 0.065(3) 0.028(2) 0.042(2) -0.0113(17) 0.027(2) -0.018(2) C25 0.056(3) 0.0233(18) 0.0291(19) -0.0047(14) 0.0189(19) -0.0114(17) C26 0.0278(17) 0.0169(15) 0.0267(17) -0.0009(12) 0.0143(15) -0.0033(13) C27 0.043(2) 0.0237(18) 0.031(2) 0.0041(15) 0.0144(17) -0.0037(16) C28 0.049(3) 0.0237(18) 0.046(2) 0.0086(17) 0.025(2) -0.0002(17) C29 0.0239(16) 0.0205(15) 0.0170(15) 0.0033(12) 0.0065(13) -0.0011(13) C30 0.0222(16) 0.0181(15) 0.0194(15) 0.0005(12) 0.0099(13) -0.0018(12) N10 0.1044(10) 0.1073(10) 0.1057(10) -0.0026(5) 0.0537(6) 0.0005(5) O17 0.1044(10) 0.1073(10) 0.1057(10) -0.0026(5) 0.0537(6) 0.0005(5) O18 0.1044(10) 0.1073(10) 0.1057(10) -0.0026(5) 0.0537(6) 0.0005(5) O19 0.1044(10) 0.1073(10) 0.1057(10) -0.0026(5) 0.0537(6) 0.0005(5) O1W 0.059(2) 0.0254(14) 0.0338(15) -0.0028(11) 0.0150(15) 0.0002(13) O2W 0.063(2) 0.078(3) 0.044(2) -0.0006(19) 0.0178(18) 0.027(2) O3W 0.115(4) 0.047(2) 0.0377(19) 0.0034(15) 0.036(2) -0.008(2) O4W 0.095(3) 0.055(2) 0.042(2) -0.0031(17) 0.016(2) 0.025(2) O5W 0.073(3) 0.130(4) 0.051(2) 0.013(3) 0.024(2) -0.001(3) O6W 0.059(3) 0.131(5) 0.105(4) -0.005(3) 0.044(3) -0.001(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 Nd1 O9 2.360(3) 3_666 ? Nd1 O5 2.392(3) . ? Nd1 O10 2.447(2) . ? Nd1 O7 2.492(3) . ? Nd1 O13 2.502(3) . ? Nd1 O14 2.526(3) . ? Nd1 O11 2.536(2) 3_666 ? Nd1 O1 2.540(2) . ? Nd1 O2 2.689(2) . ? Nd1 C9 2.986(3) . ? Nd1 Nd2 4.0139(12) . ? Nd2 O3 2.349(2) . ? Nd2 O16 2.410(3) . ? Nd2 O4 2.411(2) 3_565 ? Nd2 O15 2.453(3) . ? Nd2 O1 2.486(2) . ? Nd2 O8 2.532(3) . ? Nd2 O11 2.605(3) 3_666 ? Nd2 O12 2.644(3) 3_666 ? Nd2 O7 2.779(3) . ? Nd2 C30 2.978(3) 3_666 ? Nd2 C20 2.980(3) . ? O1 C9 1.267(4) . ? O2 C9 1.249(4) . ? O3 C10 1.238(4) . ? O4 C10 1.248(4) . ? O4 Nd2 2.411(2) 3_565 ? O5 C19 1.247(4) . ? O6 C19 1.255(4) . ? O6 H6 0.8200 . ? O7 C20 1.271(4) . ? O8 C20 1.243(4) . ? O9 C29 1.242(4) . ? O9 Nd1 2.360(3) 3_666 ? O10 C29 1.252(4) . ? O11 C30 1.268(4) . ? O11 Nd1 2.536(2) 3_666 ? O11 Nd2 2.605(3) 3_666 ? O12 C30 1.252(4) . ? O12 Nd2 2.644(3) 3_666 ? O13 H13A 0.988(19) . ? O13 H13B 0.97(2) . ? O14 H14A 0.972(19) . ? O14 H14B 0.997(19) . ? O15 H15A 0.985(19) . ? O15 H15B 0.983(19) . ? O16 H16A 0.986(19) . ? O16 H16B 0.96(2) . ? N1 C1 1.350(4) . ? N1 C2 1.373(4) . ? N1 H1 0.8600 . ? N2 C1 1.328(4) . ? N2 C3 1.363(4) . ? N3 C4 1.320(5) . ? N3 C8 1.325(5) . ? N4 C11 1.328(4) . ? N4 C12 1.373(4) . ? N5 C11 1.348(4) . ? N5 C13 1.375(4) . ? N5 H5 0.8600 . ? N6 C18 1.317(6) . ? N6 C14 1.330(5) . ? N7 C21 1.357(4) . ? N7 C22 1.367(4) . ? N7 H7 0.8600 . ? N8 C21 1.324(4) . ? N8 C23 1.376(4) . ? N9 C24 1.320(6) . ? N9 C28 1.326(6) . ? C1 C6 1.463(4) . ? C2 C3 1.392(4) . ? C2 C9 1.482(4) . ? C3 C10 1.497(4) . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 C6 1.382(5) . ? C5 H5A 0.9300 . ? C6 C7 1.387(5) . ? C7 C8 1.371(5) . ? C7 H7A 0.9300 . ? C8 H8 0.9300 . ? C11 C16 1.470(4) . ? C12 C13 1.382(4) . ? C12 C19 1.495(4) . ? C13 C20 1.486(4) . ? C14 C15 1.389(5) . ? C14 H14 0.9300 . ? C15 C16 1.387(5) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C17 C18 1.385(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C21 C26 1.465(4) . ? C22 C23 1.390(4) . ? C22 C29 1.491(4) . ? C23 C30 1.491(4) . ? C24 C25 1.389(5) . ? C24 H24 0.9300 . ? C25 C26 1.380(5) . ? C25 H25 0.9300 . ? C26 C27 1.396(5) . ? C27 C28 1.375(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C30 Nd2 2.978(3) 3_666 ? N10 O18 1.244(8) . ? N10 O19 1.260(9) . ? N10 O17 1.289(8) . ? O1W H1A 0.98(2) . ? O1W H1B 0.979(19) . ? O2W H2A 0.969(19) . ? O2W H2B 0.964(19) . ? O3W H3A 0.992(19) . ? O3W H3B 0.985(19) . ? O4W H4A 0.986(19) . ? O4W H4B 0.997(19) . ? O5W H5B 1.052(19) . ? O5W H5C 1.03(2) . ? O6W H6A 1.010(19) . ? O6W H6B 0.97(2) . ? 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 O9 Nd1 O5 77.79(11) 3_666 . ? O9 Nd1 O10 85.23(9) 3_666 . ? O5 Nd1 O10 78.18(9) . . ? O9 Nd1 O7 105.61(9) 3_666 . ? O5 Nd1 O7 70.03(9) . . ? O10 Nd1 O7 142.90(9) . . ? O9 Nd1 O13 74.22(11) 3_666 . ? O5 Nd1 O13 145.06(10) . . ? O10 Nd1 O13 79.04(10) . . ? O7 Nd1 O13 137.89(10) . . ? O9 Nd1 O14 148.41(11) 3_666 . ? O5 Nd1 O14 72.24(10) . . ? O10 Nd1 O14 79.17(11) . . ? O7 Nd1 O14 73.40(10) . . ? O13 Nd1 O14 128.26(10) . . ? O9 Nd1 O11 68.73(9) 3_666 3_666 ? O5 Nd1 O11 111.76(8) . 3_666 ? O10 Nd1 O11 148.36(9) . 3_666 ? O7 Nd1 O11 64.91(9) . 3_666 ? O13 Nd1 O11 76.83(10) . 3_666 ? O14 Nd1 O11 132.22(10) . 3_666 ? O9 Nd1 O1 132.90(9) 3_666 . ? O5 Nd1 O1 133.98(10) . . ? O10 Nd1 O1 128.51(8) . . ? O7 Nd1 O1 68.75(8) . . ? O13 Nd1 O1 80.92(10) . . ? O14 Nd1 O1 77.18(10) . . ? O11 Nd1 O1 66.97(7) 3_666 . ? O9 Nd1 O2 137.84(11) 3_666 . ? O5 Nd1 O2 134.92(9) . . ? O10 Nd1 O2 79.08(8) . . ? O7 Nd1 O2 110.47(8) . . ? O13 Nd1 O2 64.52(10) . . ? O14 Nd1 O2 65.56(10) . . ? O11 Nd1 O2 108.02(8) 3_666 . ? O1 Nd1 O2 49.51(7) . . ? O9 Nd1 C9 142.99(11) 3_666 . ? O5 Nd1 C9 138.99(10) . . ? O10 Nd1 C9 103.65(9) . . ? O7 Nd1 C9 88.88(9) . . ? O13 Nd1 C9 72.46(10) . . ? O14 Nd1 C9 68.08(10) . . ? O11 Nd1 C9 88.28(8) 3_666 . ? O1 Nd1 C9 24.86(8) . . ? O2 Nd1 C9 24.73(8) . . ? O9 Nd1 Nd2 106.92(7) 3_666 . ? O5 Nd1 Nd2 112.40(7) . . ? O10 Nd1 Nd2 165.04(6) . . ? O7 Nd1 Nd2 43.15(6) . . ? O13 Nd1 Nd2 95.61(8) . . ? O14 Nd1 Nd2 93.71(8) . . ? O11 Nd1 Nd2 39.30(6) 3_666 . ? O1 Nd1 Nd2 36.54(5) . . ? O2 Nd1 Nd2 86.01(5) . . ? C9 Nd1 Nd2 61.40(6) . . ? O3 Nd2 O16 74.65(10) . . ? O3 Nd2 O4 98.84(8) . 3_565 ? O16 Nd2 O4 85.68(10) . 3_565 ? O3 Nd2 O15 73.62(10) . . ? O16 Nd2 O15 144.51(10) . . ? O4 Nd2 O15 83.86(9) 3_565 . ? O3 Nd2 O1 69.86(8) . . ? O16 Nd2 O1 87.81(9) . . ? O4 Nd2 O1 168.16(8) 3_565 . ? O15 Nd2 O1 95.85(9) . . ? O3 Nd2 O8 147.08(10) . . ? O16 Nd2 O8 136.63(9) . . ? O4 Nd2 O8 77.93(8) 3_565 . ? O15 Nd2 O8 73.47(9) . . ? O1 Nd2 O8 113.39(8) . . ? O3 Nd2 O11 129.79(9) . 3_666 ? O16 Nd2 O11 79.70(10) . 3_666 ? O4 Nd2 O11 121.56(8) 3_565 3_666 ? O15 Nd2 O11 133.94(9) . 3_666 ? O1 Nd2 O11 66.70(8) . 3_666 ? O8 Nd2 O11 75.56(9) . 3_666 ? O3 Nd2 O12 142.19(10) . 3_666 ? O16 Nd2 O12 68.08(9) . 3_666 ? O4 Nd2 O12 72.70(8) 3_565 3_666 ? O15 Nd2 O12 138.72(8) . 3_666 ? O1 Nd2 O12 113.81(8) . 3_666 ? O8 Nd2 O12 68.75(9) . 3_666 ? O11 Nd2 O12 49.28(7) 3_666 3_666 ? O3 Nd2 O7 120.04(9) . . ? O16 Nd2 O7 137.45(9) . . ? O4 Nd2 O7 125.76(8) 3_565 . ? O15 Nd2 O7 73.90(9) . . ? O1 Nd2 O7 65.04(7) . . ? O8 Nd2 O7 48.62(8) . . ? O11 Nd2 O7 60.05(8) 3_666 . ? O12 Nd2 O7 92.63(8) 3_666 . ? O3 Nd2 C30 145.98(10) . 3_666 ? O16 Nd2 C30 76.41(9) . 3_666 ? O4 Nd2 C30 96.44(9) 3_565 3_666 ? O15 Nd2 C30 138.45(9) . 3_666 ? O1 Nd2 C30 91.61(9) . 3_666 ? O8 Nd2 C30 66.10(9) . 3_666 ? O11 Nd2 C30 25.13(8) 3_666 3_666 ? O12 Nd2 C30 24.84(8) 3_666 3_666 ? O7 Nd2 C30 72.53(8) . 3_666 ? O3 Nd2 C20 141.45(10) . . ? O16 Nd2 C20 138.45(10) . . ? O4 Nd2 C20 102.29(9) 3_565 . ? O15 Nd2 C20 77.01(10) . . ? O1 Nd2 C20 89.13(9) . . ? O8 Nd2 C20 24.37(9) . . ? O11 Nd2 C20 61.23(9) 3_666 . ? O12 Nd2 C20 75.51(9) 3_666 . ? O7 Nd2 C20 25.19(8) . . ? C30 Nd2 C20 62.26(9) 3_666 . ? O3 Nd2 Nd1 107.13(6) . . ? O16 Nd2 Nd1 101.27(8) . . ? O4 Nd2 Nd1 154.03(6) 3_565 . ? O15 Nd2 Nd1 102.90(7) . . ? O1 Nd2 Nd1 37.47(5) . . ? O8 Nd2 Nd1 80.05(6) . . ? O11 Nd2 Nd1 38.06(5) 3_666 . ? O12 Nd2 Nd1 86.60(6) 3_666 . ? O7 Nd2 Nd1 37.82(5) . . ? C30 Nd2 Nd1 61.77(6) 3_666 . ? C20 Nd2 Nd1 56.28(7) . . ? C9 O1 Nd2 156.3(2) . . ? C9 O1 Nd1 97.66(19) . . ? Nd2 O1 Nd1 105.99(8) . . ? C9 O2 Nd1 91.04(19) . . ? C10 O3 Nd2 165.4(2) . . ? C10 O4 Nd2 122.5(2) . 3_565 ? C19 O5 Nd1 141.7(2) . . ? C19 O6 H6 109.5 . . ? C20 O7 Nd1 127.8(2) . . ? C20 O7 Nd2 86.3(2) . . ? Nd1 O7 Nd2 99.04(9) . . ? C20 O8 Nd2 98.4(2) . . ? C29 O9 Nd1 153.6(3) . 3_666 ? C29 O10 Nd1 130.6(2) . . ? C30 O11 Nd1 151.2(2) . 3_666 ? C30 O11 Nd2 94.10(19) . 3_666 ? Nd1 O11 Nd2 102.65(9) 3_666 3_666 ? C30 O12 Nd2 92.7(2) . 3_666 ? Nd1 O13 H13A 124(4) . . ? Nd1 O13 H13B 115(4) . . ? H13A O13 H13B 100(2) . . ? Nd1 O14 H14A 128(3) . . ? Nd1 O14 H14B 128(3) . . ? H14A O14 H14B 104(3) . . ? Nd2 O15 H15A 120(3) . . ? Nd2 O15 H15B 128(3) . . ? H15A O15 H15B 108(3) . . ? Nd2 O16 H16A 122(4) . . ? Nd2 O16 H16B 115(4) . . ? H16A O16 H16B 101(3) . . ? C1 N1 C2 107.4(3) . . ? C1 N1 H1 126.3 . . ? C2 N1 H1 126.3 . . ? C1 N2 C3 105.8(3) . . ? C4 N3 C8 121.6(3) . . ? C11 N4 C12 105.4(3) . . ? C11 N5 C13 108.1(3) . . ? C11 N5 H5 126.0 . . ? C13 N5 H5 125.9 . . ? C18 N6 C14 116.5(3) . . ? C21 N7 C22 108.0(3) . . ? C21 N7 H7 126.0 . . ? C22 N7 H7 126.0 . . ? C21 N8 C23 105.9(3) . . ? C24 N9 C28 117.1(3) . . ? N2 C1 N1 111.7(3) . . ? N2 C1 C6 122.6(3) . . ? N1 C1 C6 125.6(3) . . ? N1 C2 C3 105.4(3) . . ? N1 C2 C9 118.7(3) . . ? C3 C2 C9 135.9(3) . . ? N2 C3 C2 109.7(3) . . ? N2 C3 C10 118.6(3) . . ? C2 C3 C10 131.7(3) . . ? N3 C4 C5 120.7(4) . . ? N3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.2(4) . . ? C6 C5 H5A 120.4 . . ? C4 C5 H5A 120.4 . . ? C5 C6 C7 118.2(3) . . ? C5 C6 C1 122.9(3) . . ? C7 C6 C1 118.8(3) . . ? C8 C7 C6 119.8(4) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? N3 C8 C7 120.6(4) . . ? N3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? O2 C9 O1 121.4(3) . . ? O2 C9 C2 117.7(3) . . ? O1 C9 C2 120.9(3) . . ? O2 C9 Nd1 64.23(17) . . ? O1 C9 Nd1 57.48(16) . . ? C2 C9 Nd1 173.0(2) . . ? O3 C10 O4 124.0(3) . . ? O3 C10 C3 119.7(3) . . ? O4 C10 C3 116.3(3) . . ? N4 C11 N5 111.4(3) . . ? N4 C11 C16 125.1(3) . . ? N5 C11 C16 123.5(3) . . ? N4 C12 C13 110.3(3) . . ? N4 C12 C19 120.0(3) . . ? C13 C12 C19 129.7(3) . . ? N5 C13 C12 104.8(3) . . ? N5 C13 C20 117.6(3) . . ? C12 C13 C20 137.2(3) . . ? N6 C14 C15 123.8(4) . . ? N6 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 117.4(3) . . ? C15 C16 C11 121.0(3) . . ? C17 C16 C11 121.6(3) . . ? C18 C17 C16 118.8(4) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? N6 C18 C17 124.6(4) . . ? N6 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? O5 C19 O6 124.1(3) . . ? O5 C19 C12 119.1(3) . . ? O6 C19 C12 116.8(3) . . ? O8 C20 O7 121.9(3) . . ? O8 C20 C13 116.8(3) . . ? O7 C20 C13 120.9(3) . . ? O8 C20 Nd2 57.18(17) . . ? O7 C20 Nd2 68.55(18) . . ? C13 C20 Nd2 152.9(2) . . ? N8 C21 N7 111.2(3) . . ? N8 C21 C26 124.7(3) . . ? N7 C21 C26 124.1(3) . . ? N7 C22 C23 105.3(3) . . ? N7 C22 C29 119.3(3) . . ? C23 C22 C29 135.4(3) . . ? N8 C23 C22 109.6(3) . . ? N8 C23 C30 117.8(3) . . ? C22 C23 C30 132.4(3) . . ? N9 C24 C25 123.5(4) . . ? N9 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C26 C25 C24 118.9(4) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 117.9(3) . . ? C25 C26 C21 122.0(3) . . ? C27 C26 C21 120.0(3) . . ? C28 C27 C26 118.2(4) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? N9 C28 C27 124.4(4) . . ? N9 C28 H28 117.8 . . ? C27 C28 H28 117.8 . . ? O9 C29 O10 125.6(3) . . ? O9 C29 C22 118.3(3) . . ? O10 C29 C22 116.1(3) . . ? O12 C30 O11 120.6(3) . . ? O12 C30 C23 117.7(3) . . ? O11 C30 C23 121.5(3) . . ? O12 C30 Nd2 62.48(17) . 3_666 ? O11 C30 Nd2 60.77(17) . 3_666 ? C23 C30 Nd2 159.6(2) . 3_666 ? O18 N10 O19 129.1(8) . . ? O18 N10 O17 118.1(8) . . ? O19 N10 O17 111.5(8) . . ? H1A O1W H1B 105(3) . . ? H2A O2W H2B 103(3) . . ? H3A O3W H3B 108(3) . . ? H4A O4W H4B 108(3) . . ? H5B O5W H5C 97(2) . . ? H6A O6W H6B 109(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 N3 0.82 1.90 2.707(4) 166.2 4_566 N1 H1 O2W 0.86 2.15 2.928(5) 150.1 . N5 H5 O5W 0.86 2.33 3.164(6) 164.7 2 N7 H7 O3W 0.86 2.02 2.880(4) 175.5 . O13 H13A O4W 0.988(19) 1.97(4) 2.872(5) 150(5) . O13 H13B O6 0.97(2) 1.90(3) 2.800(4) 153(5) 3_666 O14 H14A O5W 0.972(19) 2.08(3) 3.033(7) 167(5) . O14 H14B O6W 0.997(19) 1.75(2) 2.735(6) 169(5) . O15 H15A N6 0.985(19) 1.86(3) 2.795(4) 157(6) 2_545 O15 H15B O18 0.983(19) 1.97(3) 2.894(7) 155(6) 1_455 O15 H15B N10 0.983(19) 2.57(2) 3.542(8) 170(4) 1_455 O16 H16A N9 0.986(19) 1.70(2) 2.682(4) 178(6) 4_565 O16 H16B O17 0.96(2) 1.84(3) 2.777(7) 164(6) . O16 H16B N10 0.96(2) 2.64(4) 3.440(8) 141(5) . O1W H1A N2 0.98(2) 2.10(3) 3.005(4) 153(5) 1_656 O1W H1A O4 0.98(2) 2.26(5) 2.990(4) 130(4) 1_656 O1W H1B O12 0.979(19) 1.88(3) 2.838(4) 165(5) . O2W H2A O17 0.969(19) 1.95(3) 2.882(8) 161(6) 2_645 O2W H2A O19 0.969(19) 2.50(4) 3.190(8) 128(4) 2_645 O2W H2A N10 0.969(19) 2.68(3) 3.558(10) 151(5) 2_645 O2W H2B N8 0.964(19) 2.22(5) 3.027(5) 141(6) 4_565 O3W H3A O2W 0.992(19) 2.09(4) 2.922(6) 140(4) . O3W H3A O19 0.992(19) 2.52(4) 3.261(7) 132(4) 2_645 O3W H3B O2 0.985(19) 1.94(3) 2.873(4) 158(5) . O3W H3B O10 0.985(19) 2.61(5) 3.095(5) 111(4) . O4W H4A O1W 0.986(19) 1.94(3) 2.869(5) 155(5) 4_565 O4W H4B O6W 0.997(19) 2.07(3) 2.997(8) 153(5) 1_655 O5W H5B O8 1.052(19) 2.54(3) 3.517(6) 155(5) 2_545 O5W H5C O3W 1.03(2) 1.89(3) 2.902(7) 166(6) . O6W H6A O18 1.010(19) 2.18(2) 3.185(9) 174(6) 1_455 O6W H6B O4W 0.97(2) 2.28(5) 2.997(8) 130(5) 1_455 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.822 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.109