# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2062 data_la-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1-La _chemical_formula_moiety LaL4(NO3)3(H2O)2 _chemical_formula_sum 'C13 H14 La N9 O11 ' _chemical_formula_weight 611.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.846(9) _cell_length_b 11.550(12) _cell_length_c 12.041(12) _cell_angle_alpha 89.475(10) _cell_angle_beta 77.162(10) _cell_angle_gamma 73.674(10) _cell_volume 1019.3(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.93 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 2.176 _exptl_absorpt_correction_type 'empirical (DIFABS)' _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3562 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.94 _reflns_number_total 3562 _reflns_number_gt 3333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. Hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. The hydrogen atoms bonded to water molecules were not located and not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+9.2825P] 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 SHELXL _refine_ls_extinction_coef 0.0116(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3562 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 0.510 _refine_ls_restrained_S_all 0.510 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.04853(2) 0.251162(17) 0.153689(15) 0.02518(11) Uani 1 d . . . N11 N 0.1665(4) 0.0105(3) 0.1965(3) 0.0302(7) Uani 1 d . . . C12 C 0.3055(5) -0.0707(4) 0.1272(3) 0.0376(9) Uani 1 d . . . H12 H 0.3835 -0.0422 0.0711 0.045 Uiso 1 calc R . . C13 C 0.2247(6) -0.2382(4) 0.2146(4) 0.0432(10) Uani 1 d . . . H13 H 0.2434 -0.3211 0.2195 0.052 Uiso 1 calc R . . C14 C 0.3389(6) -0.1932(4) 0.1342(4) 0.0452(10) Uani 1 d . . . H14 H 0.4386 -0.2455 0.0847 0.054 Uiso 1 calc R . . C15 C 0.0796(6) -0.1565(4) 0.2888(4) 0.0377(9) Uani 1 d . . . H15 H -0.0005 -0.1838 0.3445 0.045 Uiso 1 calc R . . C16 C 0.0568(5) -0.0341(3) 0.2783(3) 0.0268(7) Uani 1 d . . . N21 N -0.0983(4) 0.1724(3) 0.3472(2) 0.0271(6) Uani 1 d . . . C22 C -0.0885(5) 0.0558(3) 0.3604(3) 0.0253(7) Uani 1 d . . . N23 N -0.1909(4) 0.0131(3) 0.4444(3) 0.0319(7) Uani 1 d . . . C24 C -0.3141(5) 0.0987(4) 0.5193(3) 0.0312(8) Uani 1 d . . . N25 N -0.3228(5) 0.2174(3) 0.5206(3) 0.0354(7) Uani 1 d . . . C26 C -0.2129(5) 0.2485(4) 0.4341(3) 0.0285(7) Uani 1 d . . . N200 N -0.4320(5) 0.0633(4) 0.6007(3) 0.0452(9) Uani 1 d . . . H20A H -0.4276 -0.0119 0.6039 0.054 Uiso 1 calc R . . H20B H -0.5123 0.1157 0.6498 0.054 Uiso 1 calc R . . N31 N -0.1157(5) 0.4116(3) 0.3386(3) 0.0347(7) Uani 1 d . . . C32 C -0.2085(5) 0.3760(4) 0.4343(3) 0.0336(8) Uani 1 d . . . C33 C -0.2988(6) 0.4530(4) 0.5309(4) 0.0423(10) Uani 1 d . . . H33 H -0.3616 0.4253 0.5955 0.051 Uiso 1 calc R . . C34 C -0.2928(7) 0.5713(5) 0.5283(5) 0.0526(13) Uani 1 d . . . H34 H -0.3504 0.6246 0.5917 0.063 Uiso 1 calc R . . C35 C -0.2015(7) 0.6091(5) 0.4315(5) 0.0561(13) Uani 1 d . . . H35 H -0.1969 0.6887 0.4280 0.067 Uiso 1 calc R . . C36 C -0.1155(7) 0.5279(5) 0.3383(5) 0.0500(11) Uani 1 d . . . H36 H -0.0548 0.5552 0.2725 0.060 Uiso 1 calc R . . O41 O -0.3332(5) 0.3408(4) 0.2007(4) 0.0608(10) Uani 1 d . . . O42 O -0.1869(5) 0.4436(4) 0.0949(4) 0.0661(11) Uani 1 d . . . N43 N -0.3390(5) 0.4295(3) 0.1422(3) 0.0405(8) Uani 1 d . . . O44 O -0.4831(5) 0.4976(4) 0.1304(5) 0.0822(14) Uani 1 d . . . O51 O 0.0798(12) 0.2972(5) -0.0665(4) 0.119(3) Uani 1 d . . . O52 O 0.2271(8) 0.1274(6) -0.0409(4) 0.116(3) Uani 1 d . . . N53 N 0.1908(5) 0.2028(5) -0.1087(3) 0.0505(11) Uani 1 d . . . O54 O 0.2531(6) 0.1860(6) -0.2105(3) 0.0994(19) Uani 1 d . . . O61 O 0.2578(6) 0.2256(4) 0.3003(3) 0.0581(10) Uani 1 d . . . O62 O 0.4146(5) 0.1744(4) 0.1285(3) 0.0569(9) Uani 1 d . . . N63 N 0.4093(6) 0.1761(4) 0.2339(4) 0.0554(12) Uani 1 d . . . O64 O 0.5448(6) 0.1317(5) 0.2715(5) 0.097(2) Uani 1 d . . . O200 O -0.1363(6) 0.1189(4) 0.0886(4) 0.0706(12) Uani 1 d . . . O100 O 0.1977(5) 0.4245(3) 0.1081(3) 0.0496(8) Uani 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 La1 0.02481(14) 0.02688(17) 0.02422(14) 0.00214(8) -0.00534(8) -0.00822(10) N11 0.0270(14) 0.0310(19) 0.0292(15) 0.0002(12) -0.0049(12) -0.0040(14) C12 0.0290(18) 0.038(3) 0.037(2) -0.0003(16) -0.0012(15) -0.0003(18) C13 0.045(2) 0.027(3) 0.054(3) -0.0034(18) -0.016(2) -0.001(2) C14 0.041(2) 0.039(3) 0.044(2) -0.0100(18) -0.0052(18) 0.005(2) C15 0.037(2) 0.030(2) 0.045(2) 0.0023(16) -0.0081(17) -0.0097(19) C16 0.0267(16) 0.025(2) 0.0304(17) 0.0018(13) -0.0098(14) -0.0083(15) N21 0.0288(14) 0.0239(17) 0.0273(14) -0.0013(11) -0.0036(11) -0.0074(13) C22 0.0260(16) 0.027(2) 0.0257(16) 0.0047(13) -0.0093(13) -0.0093(15) N23 0.0306(15) 0.036(2) 0.0305(15) 0.0068(13) -0.0075(12) -0.0113(15) C24 0.0282(17) 0.043(3) 0.0245(16) 0.0068(14) -0.0070(13) -0.0129(17) N25 0.0377(17) 0.039(2) 0.0243(15) -0.0026(13) -0.0004(13) -0.0075(16) C26 0.0273(16) 0.030(2) 0.0270(17) -0.0017(14) -0.0050(13) -0.0065(16) N200 0.044(2) 0.059(3) 0.0341(18) 0.0032(16) 0.0017(15) -0.027(2) N31 0.0341(16) 0.032(2) 0.0377(17) -0.0036(13) -0.0051(13) -0.0120(16) C32 0.0354(19) 0.032(2) 0.0318(18) -0.0071(15) -0.0090(15) -0.0065(18) C33 0.042(2) 0.040(3) 0.040(2) -0.0110(18) -0.0080(18) -0.005(2) C34 0.046(2) 0.039(3) 0.067(3) -0.027(2) -0.012(2) -0.003(2) C35 0.048(3) 0.032(3) 0.085(4) -0.016(2) -0.009(3) -0.012(2) C36 0.052(3) 0.035(3) 0.062(3) -0.002(2) -0.006(2) -0.017(2) O41 0.056(2) 0.059(3) 0.077(3) 0.0257(19) -0.0209(18) -0.028(2) O42 0.0351(17) 0.085(3) 0.081(3) 0.045(2) -0.0183(17) -0.0204(19) N43 0.0349(18) 0.030(2) 0.056(2) -0.0002(15) -0.0140(16) -0.0053(17) O44 0.0401(19) 0.050(3) 0.153(5) 0.019(3) -0.033(2) 0.0011(19) O51 0.258(8) 0.054(3) 0.039(2) 0.0071(19) -0.031(3) -0.039(4) O52 0.128(4) 0.118(5) 0.038(2) -0.005(2) -0.015(2) 0.065(4) N53 0.0375(19) 0.089(4) 0.0258(17) -0.0014(19) -0.0027(14) -0.023(2) O54 0.071(3) 0.193(6) 0.0285(18) -0.002(2) 0.0013(17) -0.038(3) O61 0.070(2) 0.073(3) 0.0528(19) 0.0085(17) -0.0329(18) -0.040(2) O62 0.0369(16) 0.064(3) 0.069(2) 0.0234(18) -0.0099(15) -0.0154(17) N63 0.050(2) 0.054(3) 0.089(3) 0.041(2) -0.043(2) -0.038(2) O64 0.071(3) 0.103(4) 0.169(5) 0.093(4) -0.089(3) -0.062(3) O200 0.075(3) 0.055(3) 0.109(3) 0.018(2) -0.063(2) -0.031(2) O100 0.0469(17) 0.048(2) 0.066(2) 0.0227(15) -0.0227(15) -0.0257(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 La1 O100 2.587(4) . ? La1 O200 2.612(4) . ? La1 O61 2.628(4) . ? La1 N21 2.635(3) . ? La1 O52 2.640(5) . ? La1 O42 2.664(4) . ? La1 O51 2.670(5) . ? La1 O62 2.704(5) . ? La1 N31 2.741(4) . ? La1 N11 2.755(4) . ? La1 O41 2.807(5) . ? N11 C12 1.342(5) . ? N11 C16 1.356(5) . ? C12 C14 1.370(7) . ? C13 C14 1.371(7) . ? C13 C15 1.395(6) . ? C15 C16 1.382(6) . ? C16 C22 1.486(5) . ? N21 C22 1.337(5) . ? N21 C26 1.353(5) . ? C22 N23 1.328(5) . ? N23 C24 1.348(5) . ? C24 N200 1.336(5) . ? C24 N25 1.354(6) . ? N25 C26 1.313(5) . ? C26 C32 1.482(6) . ? N31 C36 1.343(6) . ? N31 C32 1.347(5) . ? C32 C33 1.394(6) . ? C33 C34 1.380(7) . ? C34 C35 1.363(8) . ? C35 C36 1.386(7) . ? O41 N43 1.234(5) . ? O42 N43 1.258(5) . ? N43 O44 1.219(5) . ? O51 N53 1.218(8) . ? O52 N53 1.207(7) . ? N53 O54 1.211(5) . ? O61 N63 1.258(6) . ? O62 N63 1.260(6) . ? N63 O64 1.226(5) . ? 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 O100 La1 O200 147.16(13) . . ? O100 La1 O61 77.42(12) . . ? O200 La1 O61 134.09(13) . . ? O100 La1 N21 132.50(10) . . ? O200 La1 N21 77.21(13) . . ? O61 La1 N21 68.46(13) . . ? O100 La1 O52 93.6(2) . . ? O200 La1 O52 68.5(2) . . ? O61 La1 O52 111.22(17) . . ? N21 La1 O52 128.75(18) . . ? O100 La1 O42 69.74(14) . . ? O200 La1 O42 87.78(15) . . ? O61 La1 O42 132.23(15) . . ? N21 La1 O42 110.98(12) . . ? O52 La1 O42 104.70(16) . . ? O100 La1 O51 70.09(15) . . ? O200 La1 O51 78.16(18) . . ? O61 La1 O51 136.2(2) . . ? N21 La1 O51 154.31(18) . . ? O52 La1 O51 45.10(18) . . ? O42 La1 O51 60.75(18) . . ? O100 La1 O62 67.75(13) . . ? O200 La1 O62 122.91(15) . . ? O61 La1 O62 47.54(13) . . ? N21 La1 O62 107.22(11) . . ? O52 La1 O62 65.77(17) . . ? O42 La1 O62 135.43(11) . . ? O51 La1 O62 92.2(2) . . ? O100 La1 N31 76.70(12) . . ? O200 La1 N31 118.78(14) . . ? O61 La1 N31 69.18(14) . . ? N21 La1 N31 61.02(12) . . ? O52 La1 N31 170.08(18) . . ? O42 La1 N31 70.16(14) . . ? O51 La1 N31 127.46(16) . . ? O62 La1 N31 111.51(12) . . ? O100 La1 N11 135.86(12) . . ? O200 La1 N11 66.06(13) . . ? O61 La1 N11 70.67(11) . . ? N21 La1 N11 60.16(10) . . ? O52 La1 N11 71.35(15) . . ? O42 La1 N11 153.37(11) . . ? O51 La1 N11 115.09(13) . . ? O62 La1 N11 68.25(11) . . ? N31 La1 N11 117.15(11) . . ? O100 La1 O41 110.74(13) . . ? O200 La1 O41 61.43(15) . . ? O61 La1 O41 127.11(14) . . ? N21 La1 O41 69.57(11) . . ? O52 La1 O41 119.83(17) . . ? O42 La1 O41 45.22(11) . . ? O51 La1 O41 92.2(2) . . ? O62 La1 O41 174.41(12) . . ? N31 La1 O41 63.00(12) . . ? N11 La1 O41 112.71(10) . . ? C12 N11 C16 116.6(4) . . ? C12 N11 La1 123.9(3) . . ? C16 N11 La1 118.1(2) . . ? N11 C12 C14 123.8(4) . . ? C14 C13 C15 118.2(4) . . ? C12 C14 C13 119.6(4) . . ? C16 C15 C13 118.9(4) . . ? N11 C16 C15 122.8(4) . . ? N11 C16 C22 116.5(3) . . ? C15 C16 C22 120.6(3) . . ? C22 N21 C26 114.6(3) . . ? C22 N21 La1 122.5(2) . . ? C26 N21 La1 122.1(3) . . ? N23 C22 N21 125.5(3) . . ? N23 C22 C16 117.1(3) . . ? N21 C22 C16 117.2(3) . . ? C22 N23 C24 114.4(3) . . ? N200 C24 N23 117.7(4) . . ? N200 C24 N25 117.5(4) . . ? N23 C24 N25 124.7(3) . . ? C26 N25 C24 114.9(3) . . ? N25 C26 N21 125.2(4) . . ? N25 C26 C32 117.3(3) . . ? N21 C26 C32 117.4(3) . . ? C36 N31 C32 116.9(4) . . ? C36 N31 La1 123.3(3) . . ? C32 N31 La1 119.7(3) . . ? N31 C32 C33 123.1(4) . . ? N31 C32 C26 117.1(3) . . ? C33 C32 C26 119.8(4) . . ? C34 C33 C32 118.5(4) . . ? C35 C34 C33 119.1(4) . . ? C34 C35 C36 119.4(5) . . ? N31 C36 C35 123.0(5) . . ? N43 O41 La1 96.4(3) . . ? N43 O42 La1 102.8(3) . . ? O44 N43 O41 121.9(4) . . ? O44 N43 O42 122.6(4) . . ? O41 N43 O42 115.5(4) . . ? N53 O51 La1 99.2(3) . . ? N53 O52 La1 101.1(4) . . ? O54 N53 O52 123.6(6) . . ? O54 N53 O51 122.1(5) . . ? O52 N53 O51 114.3(4) . . ? N63 O61 La1 98.9(3) . . ? N63 O62 La1 95.2(3) . . ? O64 N63 O61 120.6(6) . . ? O64 N63 O62 122.1(6) . . ? O61 N63 O62 117.3(4) . . ? _refine_diff_density_max 0.933 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.087 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON program, Utrecht University, The Netherlands Walker, N., and Stuart, D., (1983) Acta Cryst. A39 467. ; #===END data_2-La _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2-La, NCMe' _chemical_formula_moiety '[LaL4(NO3)3(H2O)] NCMe' _chemical_formula_sum 'C15 H15 La N10 O10 ' _chemical_formula_weight 634.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.943(9) _cell_length_b 11.172(12) _cell_length_c 11.871(12) _cell_angle_alpha 117.191(10) _cell_angle_beta 91.443(10) _cell_angle_gamma 100.283(10) _cell_volume 1145(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 25.96 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3977 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.96 _reflns_number_total 3977 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. The hydrogen atoms bonded to carbon were included in geometric positions and given thermal parameters equivalent to 1.2 times those of the atom to which they were attached. The hydrogen atoms bonded to water molecules were not located and not included ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.8991P] 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 SHELXL _refine_ls_extinction_coef 0.0074(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3977 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.25083(3) 0.26623(3) 0.16585(2) 0.02792(15) Uani 1 d . . . N11 N 0.0803(5) 0.4247(5) 0.2889(4) 0.0378(10) Uani 1 d . . . C12 C -0.0401(6) 0.3752(7) 0.3161(6) 0.0440(13) Uani 1 d . . . H12 H -0.0598 0.2832 0.2982 0.053 Uiso 1 calc R . . C13 C -0.1369(6) 0.4532(7) 0.3695(6) 0.0501(15) Uani 1 d . . . H13 H -0.2184 0.4146 0.3883 0.060 Uiso 1 calc R . . C14 C -0.1113(6) 0.5880(7) 0.3943(6) 0.0509(15) Uani 1 d . . . H14 H -0.1754 0.6421 0.4292 0.061 Uiso 1 calc R . . C15 C 0.0128(6) 0.6427(7) 0.3662(6) 0.0469(14) Uani 1 d . . . H15 H 0.0324 0.7334 0.3805 0.056 Uiso 1 calc R . . C16 C 0.1060(6) 0.5595(6) 0.3167(5) 0.0375(12) Uani 1 d . . . N21 N 0.3262(4) 0.5257(4) 0.2360(4) 0.0331(9) Uani 1 d . . . C22 C 0.2412(6) 0.6134(5) 0.2855(5) 0.0361(11) Uani 1 d . . . N23 N 0.2659(5) 0.7428(5) 0.3087(5) 0.0450(11) Uani 1 d . . . C24 C 0.3872(6) 0.7836(6) 0.2731(6) 0.0413(12) Uani 1 d . . . N25 N 0.4835(5) 0.7077(5) 0.2283(5) 0.0418(11) Uani 1 d . . . C26 C 0.4462(5) 0.5809(5) 0.2120(5) 0.0340(11) Uani 1 d . . . N31 N 0.5066(5) 0.3621(5) 0.1497(5) 0.0390(10) Uani 1 d . . . C32 C 0.5447(5) 0.4878(6) 0.1585(5) 0.0341(11) Uani 1 d . . . C33 C 0.6674(6) 0.5276(7) 0.1180(6) 0.0419(13) Uani 1 d . . . H33 H 0.6925 0.6156 0.1259 0.050 Uiso 1 calc R . . C34 C 0.7509(6) 0.4342(7) 0.0658(6) 0.0481(14) Uani 1 d . . . H34 H 0.8316 0.4578 0.0358 0.058 Uiso 1 calc R . . C35 C 0.7137(6) 0.3065(7) 0.0587(6) 0.0480(14) Uani 1 d . . . H35 H 0.7691 0.2424 0.0255 0.058 Uiso 1 calc R . . C36 C 0.5910(6) 0.2759(6) 0.1024(6) 0.0439(13) Uani 1 d . . . H36 H 0.5662 0.1896 0.0982 0.053 Uiso 1 calc R . . N27 N 0.4140(7) 0.9104(6) 0.2852(7) 0.0635(16) Uani 1 d . . . H27A H 0.4902 0.9407 0.2647 0.076 Uiso 1 calc R . . H27B H 0.3552 0.9619 0.3134 0.076 Uiso 1 calc R . . O41 O 0.3062(5) 0.1609(5) -0.0708(4) 0.0509(10) Uani 1 d . . . N43 N 0.3100(5) 0.0425(5) -0.0834(5) 0.0467(12) Uani 1 d . . . O44 O 0.3321(8) -0.0474(6) -0.1826(5) 0.0832(19) Uani 1 d . . . O42 O 0.2942(5) 0.0267(5) 0.0149(4) 0.0518(11) Uani 1 d . . . O51 O 0.0322(4) 0.1459(4) -0.0021(4) 0.0474(10) Uani 1 d . . . N53 N 0.0414(5) 0.2357(5) -0.0420(4) 0.0397(11) Uani 1 d . . . O54 O -0.0291(6) 0.2132(6) -0.1371(5) 0.0692(15) Uani 1 d . . . O52 O 0.1264(5) 0.3469(4) 0.0242(4) 0.0459(10) Uani 1 d . . . O61 O 0.4017(5) 0.1862(5) 0.2860(4) 0.0533(11) Uani 1 d . . . O62 O 0.3275(5) 0.3682(5) 0.4013(4) 0.0558(11) Uani 1 d . . . N63 N 0.4005(6) 0.2835(6) 0.3969(5) 0.0517(13) Uani 1 d . . . O64 O 0.4576(8) 0.2916(8) 0.4920(6) 0.097(2) Uani 1 d . . . O100 O 0.0886(5) 0.1058(4) 0.2159(4) 0.0454(9) Uani 1 d . . . N100 N 0.1512(8) 0.0697(7) 0.4300(6) 0.0711(19) Uani 1 d . . . C101 C 0.1776(7) 0.0532(8) 0.5134(6) 0.0562(16) Uani 1 d . . . C102 C 0.2088(12) 0.0306(13) 0.6195(10) 0.109(4) Uani 1 d . . . H10A H 0.2709 -0.0312 0.5978 0.131 Uiso 1 calc R . . H10B H 0.1254 -0.0090 0.6402 0.131 Uiso 1 calc R . . H10C H 0.2511 0.1167 0.6917 0.131 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0293(2) 0.0267(2) 0.02944(19) 0.01477(13) 0.00478(11) 0.00513(14) N11 0.037(2) 0.042(3) 0.039(2) 0.023(2) 0.0087(19) 0.008(2) C12 0.035(3) 0.048(3) 0.049(3) 0.023(3) 0.007(2) 0.008(3) C13 0.038(3) 0.064(4) 0.044(3) 0.022(3) 0.011(2) 0.010(3) C14 0.042(3) 0.053(4) 0.050(3) 0.015(3) 0.016(3) 0.019(3) C15 0.042(3) 0.045(3) 0.047(3) 0.015(3) 0.007(2) 0.011(3) C16 0.039(3) 0.038(3) 0.034(3) 0.015(2) 0.002(2) 0.011(3) N21 0.033(2) 0.032(2) 0.033(2) 0.0145(17) 0.0041(17) 0.006(2) C22 0.043(3) 0.033(3) 0.033(3) 0.015(2) 0.006(2) 0.009(3) N23 0.050(3) 0.036(3) 0.051(3) 0.020(2) 0.008(2) 0.014(3) C24 0.046(3) 0.033(3) 0.047(3) 0.020(2) 0.006(2) 0.008(3) N25 0.049(3) 0.033(2) 0.044(3) 0.020(2) 0.008(2) 0.008(2) C26 0.039(3) 0.035(3) 0.030(2) 0.016(2) 0.005(2) 0.008(2) N31 0.031(2) 0.041(3) 0.048(3) 0.023(2) 0.0065(19) 0.009(2) C32 0.032(3) 0.036(3) 0.034(3) 0.017(2) 0.003(2) 0.008(2) C33 0.041(3) 0.042(3) 0.047(3) 0.024(3) 0.013(2) 0.009(3) C34 0.039(3) 0.056(4) 0.061(4) 0.036(3) 0.017(3) 0.012(3) C35 0.036(3) 0.060(4) 0.056(4) 0.030(3) 0.011(3) 0.022(3) C36 0.037(3) 0.040(3) 0.059(4) 0.025(3) 0.010(3) 0.011(3) N27 0.075(4) 0.040(3) 0.091(5) 0.040(3) 0.030(3) 0.021(3) O41 0.063(3) 0.050(3) 0.046(2) 0.027(2) 0.013(2) 0.015(2) N43 0.054(3) 0.055(3) 0.037(3) 0.021(2) 0.012(2) 0.027(3) O44 0.137(5) 0.081(4) 0.046(3) 0.024(3) 0.033(3) 0.071(4) O42 0.075(3) 0.047(2) 0.041(2) 0.0227(19) 0.015(2) 0.024(2) O51 0.047(2) 0.048(2) 0.053(2) 0.033(2) -0.0029(19) -0.002(2) N53 0.036(2) 0.046(3) 0.038(2) 0.021(2) 0.0021(19) 0.008(2) O54 0.075(3) 0.079(4) 0.057(3) 0.038(3) -0.017(3) 0.010(3) O52 0.051(2) 0.035(2) 0.049(2) 0.0202(18) -0.0030(19) 0.002(2) O61 0.064(3) 0.054(3) 0.053(3) 0.030(2) 0.007(2) 0.023(2) O62 0.064(3) 0.060(3) 0.043(2) 0.022(2) 0.005(2) 0.017(3) N63 0.053(3) 0.057(3) 0.048(3) 0.029(3) -0.008(2) 0.005(3) O64 0.114(5) 0.110(5) 0.067(4) 0.045(4) -0.034(4) 0.019(4) O100 0.051(2) 0.042(2) 0.046(2) 0.0275(19) 0.0042(18) 0.000(2) N100 0.098(5) 0.074(4) 0.057(4) 0.042(3) 0.015(3) 0.024(4) C101 0.059(4) 0.063(4) 0.044(3) 0.026(3) 0.006(3) 0.004(4) C102 0.107(8) 0.147(10) 0.077(6) 0.073(7) -0.033(6) -0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O100 2.481(4) . ? La1 O62 2.523(5) . ? La1 O61 2.574(4) . ? La1 O42 2.575(5) . ? La1 N21 2.578(5) . ? La1 O51 2.607(5) . ? La1 O52 2.617(4) . ? La1 O41 2.621(5) . ? La1 N31 2.625(5) . ? La1 N11 2.641(5) . ? N11 C12 1.338(7) . ? N11 C16 1.359(7) . ? C12 C13 1.384(8) . ? C13 C14 1.369(10) . ? C14 C15 1.395(9) . ? C15 C16 1.379(8) . ? C16 C22 1.499(8) . ? N21 C26 1.341(7) . ? N21 C22 1.347(7) . ? C22 N23 1.317(7) . ? N23 C24 1.358(8) . ? C24 N27 1.332(8) . ? C24 N25 1.350(7) . ? N25 C26 1.319(7) . ? C26 C32 1.495(7) . ? N31 C36 1.328(7) . ? N31 C32 1.342(7) . ? C32 C33 1.396(8) . ? C33 C34 1.380(8) . ? C34 C35 1.371(9) . ? C35 C36 1.385(8) . ? O41 N43 1.269(7) . ? N43 O44 1.206(7) . ? N43 O42 1.268(6) . ? O51 N53 1.282(6) . ? N53 O54 1.211(7) . ? N53 O52 1.255(7) . ? O61 N63 1.270(7) . ? O62 N63 1.276(7) . ? N63 O64 1.208(7) . ? N100 C101 1.121(9) . ? C101 C102 1.430(10) . ? 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 O100 La1 O62 80.41(16) . . ? O100 La1 O61 74.56(16) . . ? O62 La1 O61 49.75(16) . . ? O100 La1 O42 75.64(16) . . ? O62 La1 O42 118.48(15) . . ? O61 La1 O42 69.36(16) . . ? O100 La1 N21 140.27(14) . . ? O62 La1 N21 77.12(15) . . ? O61 La1 N21 112.56(16) . . ? O42 La1 N21 144.09(15) . . ? O100 La1 O51 68.87(14) . . ? O62 La1 O51 142.10(15) . . ? O61 La1 O51 134.18(15) . . ? O42 La1 O51 75.50(15) . . ? N21 La1 O51 113.18(13) . . ? O100 La1 O52 111.95(15) . . ? O62 La1 O52 134.70(15) . . ? O61 La1 O52 171.83(14) . . ? O42 La1 O52 106.82(15) . . ? N21 La1 O52 65.98(14) . . ? O51 La1 O52 48.53(14) . . ? O100 La1 O41 114.67(15) . . ? O62 La1 O41 150.34(16) . . ? O61 La1 O41 107.44(15) . . ? O42 La1 O41 48.96(13) . . ? N21 La1 O41 100.69(14) . . ? O51 La1 O41 66.37(15) . . ? O52 La1 O41 65.69(15) . . ? O100 La1 N31 147.70(14) . . ? O62 La1 N31 85.52(16) . . ? O61 La1 N31 74.16(16) . . ? O42 La1 N31 86.04(16) . . ? N21 La1 N31 61.89(14) . . ? O51 La1 N31 132.07(15) . . ? O52 La1 N31 98.62(15) . . ? O41 La1 N31 68.15(15) . . ? O100 La1 N11 79.49(16) . . ? O62 La1 N11 72.69(15) . . ? O61 La1 N11 119.42(15) . . ? O42 La1 N11 150.03(16) . . ? N21 La1 N11 62.75(15) . . ? O51 La1 N11 80.15(16) . . ? O52 La1 N11 67.61(15) . . ? O41 La1 N11 133.13(13) . . ? N31 La1 N11 123.60(16) . . ? C12 N11 C16 116.7(5) . . ? C12 N11 La1 122.5(4) . . ? C16 N11 La1 120.5(3) . . ? N11 C12 C13 123.6(6) . . ? C14 C13 C12 119.2(6) . . ? C13 C14 C15 118.7(6) . . ? C16 C15 C14 118.7(6) . . ? N11 C16 C15 123.1(5) . . ? N11 C16 C22 116.0(5) . . ? C15 C16 C22 120.8(5) . . ? C26 N21 C22 114.5(5) . . ? C26 N21 La1 122.7(3) . . ? C22 N21 La1 122.3(3) . . ? N23 C22 N21 125.7(5) . . ? N23 C22 C16 116.7(5) . . ? N21 C22 C16 117.5(5) . . ? C22 N23 C24 113.9(5) . . ? N27 C24 N25 117.3(5) . . ? N27 C24 N23 117.0(5) . . ? N25 C24 N23 125.7(5) . . ? C26 N25 C24 113.7(5) . . ? N25 C26 N21 126.2(5) . . ? N25 C26 C32 117.4(5) . . ? N21 C26 C32 116.4(5) . . ? C36 N31 C32 117.7(5) . . ? C36 N31 La1 119.5(4) . . ? C32 N31 La1 120.8(3) . . ? N31 C32 C33 121.8(5) . . ? N31 C32 C26 115.7(4) . . ? C33 C32 C26 122.4(5) . . ? C34 C33 C32 119.0(6) . . ? C35 C34 C33 119.4(5) . . ? C34 C35 C36 117.9(5) . . ? N31 C36 C35 124.1(6) . . ? N43 O41 La1 96.3(3) . . ? O44 N43 O42 122.5(5) . . ? O44 N43 O41 121.2(5) . . ? O42 N43 O41 116.2(5) . . ? O44 N43 La1 179.2(5) . . ? O42 N43 La1 57.1(3) . . ? O41 N43 La1 59.2(3) . . ? N43 O42 La1 98.5(3) . . ? N53 O51 La1 97.1(3) . . ? O54 N53 O52 123.1(5) . . ? O54 N53 O51 121.2(5) . . ? O52 N53 O51 115.6(5) . . ? N53 O52 La1 97.3(3) . . ? N63 O61 La1 96.6(3) . . ? N63 O62 La1 98.9(3) . . ? O64 N63 O61 122.9(6) . . ? O64 N63 O62 122.3(6) . . ? O61 N63 O62 114.7(5) . . ? N100 C101 C102 178.9(9) . . ? _refine_diff_density_max 1.852 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.167 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_2-Pr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2-Pr, NCMe' _chemical_formula_moiety '[PrL4(NO3)3(H2O)] NCMe' _chemical_formula_sum 'C15 H15 N10 O10 Pr' _chemical_formula_weight 636.28 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' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.943(9) _cell_length_b 11.101(12) _cell_length_c 11.836(12) _cell_angle_alpha 117.279(10) _cell_angle_beta 91.323(10) _cell_angle_gamma 100.616(10) _cell_volume 1133(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 25.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 2.226 _exptl_absorpt_correction_type 'empirical (DIFABS)' _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3993 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.95 _reflns_number_total 3993 _reflns_number_gt 3600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. Hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. Hydrogen atoms on the water molecules could not be located and were not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.8991P] 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 SHELXL _refine_ls_extinction_coef 0.0146(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3993 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.24870(3) 0.26736(3) 0.16487(3) 0.02939(18) Uani 1 d . . . N11 N 0.0791(6) 0.4209(6) 0.2865(5) 0.0405(12) Uani 1 d . . . C12 C -0.0416(7) 0.3687(8) 0.3128(7) 0.0468(16) Uani 1 d . . . H12 H -0.0616 0.2756 0.2932 0.056 Uiso 1 calc R . . C13 C -0.1384(8) 0.4483(8) 0.3683(7) 0.0492(16) Uani 1 d . . . H13 H -0.2201 0.4095 0.3874 0.059 Uiso 1 calc R . . C14 C -0.1111(8) 0.5845(8) 0.3941(8) 0.0533(18) Uani 1 d . . . H14 H -0.1752 0.6387 0.4293 0.064 Uiso 1 calc R . . C15 C 0.0125(8) 0.6410(8) 0.3676(7) 0.0502(17) Uani 1 d . . . H15 H 0.0329 0.7333 0.3843 0.060 Uiso 1 calc R . . C16 C 0.1055(7) 0.5562(7) 0.3153(6) 0.0400(14) Uani 1 d . . . N21 N 0.3238(6) 0.5233(5) 0.2360(5) 0.0364(11) Uani 1 d . . . C22 C 0.2399(7) 0.6124(7) 0.2859(6) 0.0401(14) Uani 1 d . . . N23 N 0.2667(6) 0.7439(6) 0.3107(6) 0.0459(13) Uani 1 d . . . C24 C 0.3886(8) 0.7854(7) 0.2755(7) 0.0443(15) Uani 1 d . . . N25 N 0.4835(6) 0.7074(6) 0.2297(6) 0.0422(13) Uani 1 d . . . C26 C 0.4459(7) 0.5806(7) 0.2128(6) 0.0379(13) Uani 1 d . . . N31 N 0.5022(6) 0.3579(6) 0.1493(6) 0.0427(13) Uani 1 d . . . C32 C 0.5432(7) 0.4857(6) 0.1586(6) 0.0377(13) Uani 1 d . . . C33 C 0.6636(7) 0.5246(7) 0.1175(7) 0.0407(14) Uani 1 d . . . H33 H 0.6881 0.6128 0.1241 0.049 Uiso 1 calc R . . C34 C 0.7490(7) 0.4302(8) 0.0656(7) 0.0476(16) Uani 1 d . . . H34 H 0.8309 0.4542 0.0370 0.057 Uiso 1 calc R . . C35 C 0.7089(7) 0.3012(8) 0.0577(7) 0.0486(17) Uani 1 d . . . H35 H 0.7633 0.2361 0.0238 0.058 Uiso 1 calc R . . C36 C 0.5858(7) 0.2698(7) 0.1014(7) 0.0446(15) Uani 1 d . . . H36 H 0.5602 0.1828 0.0971 0.053 Uiso 1 calc R . . N27 N 0.4170(8) 0.9142(7) 0.2891(8) 0.0649(19) Uani 1 d . . . H27A H 0.4935 0.9448 0.2689 0.078 Uiso 1 calc R . . H27B H 0.3587 0.9664 0.3180 0.078 Uiso 1 calc R . . O41 O 0.3025(6) 0.1656(5) -0.0707(5) 0.0526(12) Uani 1 d . . . N43 N 0.3082(6) 0.0477(6) -0.0830(5) 0.0473(14) Uani 1 d . . . O44 O 0.3304(8) -0.0442(7) -0.1830(6) 0.077(2) Uani 1 d . . . O42 O 0.2914(6) 0.0311(5) 0.0159(5) 0.0524(13) Uani 1 d . . . O51 O 0.0329(5) 0.1472(5) 0.0009(5) 0.0488(11) Uani 1 d . . . N53 N 0.0403(6) 0.2376(6) -0.0401(6) 0.0419(13) Uani 1 d . . . O54 O -0.0324(7) 0.2144(7) -0.1341(6) 0.0670(17) Uani 1 d . . . O52 O 0.1263(6) 0.3490(5) 0.0247(5) 0.0470(12) Uani 1 d . . . O61 O 0.3972(6) 0.1858(6) 0.2816(5) 0.0539(13) Uani 1 d . . . O62 O 0.3243(6) 0.3700(6) 0.3971(5) 0.0559(13) Uani 1 d . . . N63 N 0.3967(7) 0.2838(7) 0.3931(6) 0.0526(16) Uani 1 d . . . O64 O 0.4556(9) 0.2936(9) 0.4882(7) 0.094(3) Uani 1 d . . . O100 O 0.0906(5) 0.1061(5) 0.2134(5) 0.0464(11) Uani 1 d . . . N100 N 0.1499(11) 0.0706(9) 0.4286(8) 0.076(2) Uani 1 d . . . C101 C 0.1752(9) 0.0544(9) 0.5139(8) 0.0577(19) Uani 1 d . . . C102 C 0.2084(14) 0.0335(15) 0.6210(11) 0.105(4) Uani 1 d . . . H10A H 0.2764 -0.0222 0.6016 0.125 Uiso 1 calc R . . H10B H 0.1268 -0.0131 0.6386 0.125 Uiso 1 calc R . . H10C H 0.2444 0.1218 0.6947 0.125 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0311(2) 0.0254(2) 0.0326(2) 0.01446(16) 0.00452(13) 0.00609(14) N11 0.038(3) 0.040(3) 0.045(3) 0.021(2) 0.006(2) 0.009(2) C12 0.041(4) 0.050(4) 0.049(4) 0.023(3) 0.009(3) 0.008(3) C13 0.040(4) 0.059(4) 0.050(4) 0.027(3) 0.011(3) 0.011(3) C14 0.047(4) 0.050(4) 0.057(4) 0.017(3) 0.016(3) 0.021(3) C15 0.044(4) 0.045(4) 0.057(4) 0.017(3) 0.012(3) 0.017(3) C16 0.043(4) 0.035(3) 0.040(3) 0.015(3) 0.005(3) 0.009(3) N21 0.037(3) 0.031(2) 0.037(3) 0.015(2) 0.003(2) 0.003(2) C22 0.043(3) 0.040(3) 0.037(3) 0.016(3) 0.003(3) 0.014(3) N23 0.050(3) 0.034(3) 0.052(3) 0.018(3) 0.009(3) 0.012(3) C24 0.053(4) 0.029(3) 0.048(4) 0.016(3) 0.006(3) 0.008(3) N25 0.047(3) 0.030(3) 0.050(3) 0.019(2) 0.011(3) 0.007(2) C26 0.036(3) 0.037(3) 0.040(3) 0.018(3) 0.003(3) 0.007(3) N31 0.033(3) 0.043(3) 0.050(3) 0.020(3) 0.002(2) 0.011(2) C32 0.038(3) 0.033(3) 0.039(3) 0.014(3) -0.001(3) 0.008(3) C33 0.036(3) 0.037(3) 0.055(4) 0.029(3) 0.012(3) 0.001(3) C34 0.036(3) 0.055(4) 0.061(4) 0.034(4) 0.016(3) 0.011(3) C35 0.037(4) 0.058(4) 0.059(4) 0.032(4) 0.013(3) 0.018(3) C36 0.036(3) 0.037(3) 0.066(4) 0.027(3) 0.005(3) 0.009(3) N27 0.075(5) 0.039(3) 0.090(5) 0.034(4) 0.028(4) 0.023(3) O41 0.065(3) 0.049(3) 0.055(3) 0.029(2) 0.019(2) 0.021(3) N43 0.052(3) 0.051(3) 0.039(3) 0.017(3) 0.008(3) 0.025(3) O44 0.121(6) 0.074(4) 0.046(3) 0.021(3) 0.029(3) 0.061(4) O42 0.075(4) 0.048(3) 0.044(3) 0.025(2) 0.016(2) 0.025(3) O51 0.052(3) 0.045(3) 0.050(3) 0.026(2) -0.004(2) 0.003(2) N53 0.039(3) 0.043(3) 0.044(3) 0.020(3) 0.001(2) 0.011(2) O54 0.071(4) 0.075(4) 0.056(3) 0.034(3) -0.017(3) 0.009(3) O52 0.052(3) 0.035(2) 0.049(3) 0.019(2) -0.005(2) 0.003(2) O61 0.062(3) 0.052(3) 0.056(3) 0.029(3) 0.003(3) 0.019(3) O62 0.067(4) 0.054(3) 0.045(3) 0.020(2) 0.004(2) 0.019(3) N63 0.058(4) 0.055(4) 0.049(4) 0.029(3) -0.003(3) 0.009(3) O64 0.107(6) 0.107(6) 0.070(4) 0.044(4) -0.031(4) 0.024(5) O100 0.052(3) 0.041(2) 0.048(3) 0.026(2) 0.005(2) 0.003(2) N100 0.115(7) 0.071(5) 0.055(4) 0.037(4) 0.007(4) 0.029(5) C101 0.052(5) 0.063(5) 0.056(5) 0.029(4) 0.006(4) 0.003(4) C102 0.091(8) 0.147(11) 0.078(7) 0.073(8) -0.031(6) -0.019(8) _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 Pr1 O100 2.440(5) . ? Pr1 O62 2.477(6) . ? Pr1 N21 2.517(6) . ? Pr1 O42 2.525(5) . ? Pr1 O61 2.540(5) . ? Pr1 O51 2.555(5) . ? Pr1 N31 2.580(6) . ? Pr1 O41 2.597(6) . ? Pr1 O52 2.597(5) . ? Pr1 N11 2.597(6) . ? N11 C12 1.340(10) . ? N11 C16 1.350(9) . ? C12 C13 1.397(10) . ? C13 C14 1.369(12) . ? C14 C15 1.385(12) . ? C15 C16 1.392(9) . ? C16 C22 1.486(10) . ? N21 C22 1.347(8) . ? N21 C26 1.359(9) . ? C22 N23 1.322(9) . ? N23 C24 1.360(10) . ? C24 N27 1.338(9) . ? C24 N25 1.352(9) . ? N25 C26 1.307(9) . ? C26 C32 1.497(9) . ? N31 C36 1.335(8) . ? N31 C32 1.355(9) . ? C32 C33 1.373(10) . ? C33 C34 1.400(10) . ? C34 C35 1.372(11) . ? C35 C36 1.387(10) . ? O41 N43 1.262(8) . ? N43 O44 1.216(8) . ? N43 O42 1.276(8) . ? O51 N53 1.292(8) . ? N53 O54 1.207(8) . ? N53 O52 1.249(8) . ? O61 N63 1.269(9) . ? O62 N63 1.285(8) . ? N63 O64 1.207(9) . ? N100 C101 1.134(11) . ? C101 C102 1.431(13) . ? 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 O100 Pr1 O62 80.69(19) . . ? O100 Pr1 N21 140.57(18) . . ? O62 Pr1 N21 76.24(18) . . ? O100 Pr1 O42 75.23(19) . . ? O62 Pr1 O42 118.81(17) . . ? N21 Pr1 O42 144.16(19) . . ? O100 Pr1 O61 73.90(19) . . ? O62 Pr1 O61 50.63(18) . . ? N21 Pr1 O61 112.60(19) . . ? O42 Pr1 O61 68.74(18) . . ? O100 Pr1 O51 68.65(17) . . ? O62 Pr1 O51 141.71(19) . . ? N21 Pr1 O51 113.85(16) . . ? O42 Pr1 O51 75.66(18) . . ? O61 Pr1 O51 133.44(18) . . ? O100 Pr1 N31 145.72(18) . . ? O62 Pr1 N31 85.2(2) . . ? N21 Pr1 N31 63.18(17) . . ? O42 Pr1 N31 84.78(19) . . ? O61 Pr1 N31 73.0(2) . . ? O51 Pr1 N31 132.93(19) . . ? O100 Pr1 O41 114.93(18) . . ? O62 Pr1 O41 150.75(19) . . ? N21 Pr1 O41 100.37(17) . . ? O42 Pr1 O41 49.75(16) . . ? O61 Pr1 O41 107.73(18) . . ? O51 Pr1 O41 66.63(19) . . ? N31 Pr1 O41 68.03(18) . . ? O100 Pr1 O52 112.68(18) . . ? O62 Pr1 O52 134.13(17) . . ? N21 Pr1 O52 66.13(17) . . ? O42 Pr1 O52 107.06(17) . . ? O61 Pr1 O52 171.52(17) . . ? O51 Pr1 O52 49.20(16) . . ? N31 Pr1 O52 99.59(19) . . ? O41 Pr1 O52 65.00(18) . . ? O100 Pr1 N11 79.33(19) . . ? O62 Pr1 N11 72.51(18) . . ? N21 Pr1 N11 63.48(18) . . ? O42 Pr1 N11 149.5(2) . . ? O61 Pr1 N11 119.67(19) . . ? O51 Pr1 N11 79.55(18) . . ? N31 Pr1 N11 125.54(19) . . ? O41 Pr1 N11 132.59(17) . . ? O52 Pr1 N11 67.81(18) . . ? C12 N11 C16 117.5(6) . . ? C12 N11 Pr1 122.5(5) . . ? C16 N11 Pr1 119.7(5) . . ? N11 C12 C13 122.8(7) . . ? C14 C13 C12 118.9(8) . . ? C13 C14 C15 119.6(7) . . ? C14 C15 C16 118.3(7) . . ? N11 C16 C15 123.0(7) . . ? N11 C16 C22 116.8(6) . . ? C15 C16 C22 120.2(6) . . ? C22 N21 C26 113.9(5) . . ? C22 N21 Pr1 122.9(4) . . ? C26 N21 Pr1 122.8(4) . . ? N23 C22 N21 125.9(7) . . ? N23 C22 C16 117.8(6) . . ? N21 C22 C16 116.3(6) . . ? C22 N23 C24 114.2(6) . . ? N27 C24 N25 117.8(7) . . ? N27 C24 N23 117.1(7) . . ? N25 C24 N23 125.1(6) . . ? C26 N25 C24 114.4(6) . . ? N25 C26 N21 126.3(6) . . ? N25 C26 C32 117.9(6) . . ? N21 C26 C32 115.7(6) . . ? C36 N31 C32 117.4(6) . . ? C36 N31 Pr1 120.2(5) . . ? C32 N31 Pr1 120.3(4) . . ? N31 C32 C33 122.4(6) . . ? N31 C32 C26 115.4(6) . . ? C33 C32 C26 122.1(6) . . ? C32 C33 C34 119.3(6) . . ? C35 C34 C33 118.4(7) . . ? C34 C35 C36 118.8(6) . . ? N31 C36 C35 123.5(7) . . ? N43 O41 Pr1 95.5(4) . . ? O44 N43 O41 121.8(6) . . ? O44 N43 O42 122.0(6) . . ? O41 N43 O42 116.2(5) . . ? N43 O42 Pr1 98.5(4) . . ? N53 O51 Pr1 97.6(4) . . ? O54 N53 O52 123.4(6) . . ? O54 N53 O51 121.5(6) . . ? O52 N53 O51 115.2(5) . . ? N53 O52 Pr1 96.8(4) . . ? N63 O61 Pr1 96.2(4) . . ? N63 O62 Pr1 98.8(4) . . ? O64 N63 O61 123.2(7) . . ? O64 N63 O62 122.4(7) . . ? O61 N63 O62 114.3(6) . . ? N100 C101 C102 179.4(11) . . ? _refine_diff_density_max 2.132 _refine_diff_density_min -1.540 _refine_diff_density_rms 0.207 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_2-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2-Nd, 2NCMe' _chemical_formula_moiety '[NdL4(NO3)3(H2O)] 2NCMe' _chemical_formula_sum 'C17 H18 N11 Nd O10' _chemical_formula_weight 680.66 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.191(9) _cell_length_b 11.710(12) _cell_length_c 13.339(13) _cell_angle_alpha 109.893(10) _cell_angle_beta 103.994(10) _cell_angle_gamma 90.778(10) _cell_volume 1303(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.90 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4142 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.90 _reflns_number_total 4142 _reflns_number_gt 3811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. Hydrogen atoms bonded to water molecules were not located and not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+4.3356P] 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 SHELXL _refine_ls_extinction_coef 0.0015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4142 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.200 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd Nd 0.25459(3) 0.13774(2) 0.290246(18) 0.02989(11) Uani 1 d . . . O100 O 0.2918(5) 0.0470(4) 0.1030(3) 0.0492(10) Uani 1 d . . . H1 H 0.246(10) 0.064(8) 0.057(7) 0.09(3) Uiso 1 d . . . H2 H 0.340(10) -0.004(8) 0.070(7) 0.09(3) Uiso 1 d . . . N11 C 0.0860(5) 0.1599(3) 0.4296(3) 0.0234(8) Uani 1 d . . . C12 C -0.0492(6) 0.0981(5) 0.4019(4) 0.0436(12) Uani 1 d . . . H12 H -0.0843 0.0419 0.3305 0.052 Uiso 1 calc R . . C13 C -0.1403(6) 0.1125(5) 0.4730(5) 0.0476(13) Uani 1 d . . . H13 H -0.2334 0.0665 0.4501 0.057 Uiso 1 calc R . . C14 C -0.0900(7) 0.1965(5) 0.5786(5) 0.0507(13) Uani 1 d . . . H14 H -0.1492 0.2088 0.6282 0.061 Uiso 1 calc R . . C15 C 0.0490(6) 0.2622(5) 0.6098(4) 0.0467(12) Uani 1 d . . . H15 H 0.0849 0.3201 0.6804 0.056 Uiso 1 calc R . . C16 C 0.1349(5) 0.2404(4) 0.5335(4) 0.0332(10) Uani 1 d . . . N21 N 0.3625(4) 0.2871(3) 0.4873(3) 0.0293(8) Uani 1 d . . . C22 C 0.2875(5) 0.3073(4) 0.5663(4) 0.0311(9) Uani 1 d . . . N23 N 0.3373(5) 0.3810(4) 0.6692(3) 0.0360(9) Uani 1 d . . . C24 C 0.4753(6) 0.4415(4) 0.6954(4) 0.0354(10) Uani 1 d . . . N25 N 0.5606(5) 0.4300(3) 0.6233(3) 0.0336(8) Uani 1 d . . . C26 C 0.4997(5) 0.3517(4) 0.5225(3) 0.0290(9) Uani 1 d . . . N31 N 0.5241(5) 0.2505(4) 0.3384(3) 0.0364(9) Uani 1 d . . . C32 C 0.5881(5) 0.3335(4) 0.4400(3) 0.0283(9) Uani 1 d . . . C33 C 0.7282(6) 0.3983(4) 0.4664(4) 0.0371(10) Uani 1 d . . . H33 H 0.7700 0.4545 0.5370 0.044 Uiso 1 calc R . . C34 C 0.8037(6) 0.3774(5) 0.3852(5) 0.0448(12) Uani 1 d . . . H34 H 0.8968 0.4205 0.4001 0.054 Uiso 1 calc R . . C35 C 0.7400(6) 0.2925(5) 0.2823(4) 0.0486(13) Uani 1 d . . . H35 H 0.7902 0.2769 0.2271 0.058 Uiso 1 calc R . . C36 C 0.6018(6) 0.2308(5) 0.2615(4) 0.0463(12) Uani 1 d . . . H36 H 0.5601 0.1731 0.1916 0.056 Uiso 1 calc R . . N100 N 0.5295(6) 0.5168(4) 0.7986(3) 0.0499(11) Uani 1 d . . . H10A H 0.4773 0.5255 0.8457 0.060 Uiso 1 calc R . . H10B H 0.6169 0.5570 0.8186 0.060 Uiso 1 calc R . . O41 O -0.0080(4) 0.0750(3) 0.1491(3) 0.0506(9) Uani 1 d . . . N43 N -0.0111(5) -0.0360(4) 0.1380(3) 0.0433(10) Uani 1 d . . . O42 O 0.0891(5) -0.0653(3) 0.2056(3) 0.0492(9) Uani 1 d . . . O44 O -0.1077(5) -0.1130(4) 0.0660(3) 0.0670(13) Uani 1 d . . . O61 O 0.1139(4) 0.3291(3) 0.3150(3) 0.0468(9) Uani 1 d . . . O62 O 0.2299(5) 0.2927(3) 0.1881(3) 0.0459(8) Uani 1 d . . . N63 N 0.1428(5) 0.3582(4) 0.2386(4) 0.0420(10) Uani 1 d . . . O64 O 0.0918(6) 0.4436(4) 0.2158(4) 0.0710(13) Uani 1 d . . . O51 O 0.3297(5) 0.0043(3) 0.4067(3) 0.0467(9) Uani 1 d . . . N53 N 0.4092(5) -0.0606(4) 0.3499(3) 0.0423(10) Uani 1 d . . . O54 O 0.4494(6) -0.1552(4) 0.3603(4) 0.0725(14) Uani 1 d . . . O52 O 0.4417(5) -0.0228(4) 0.2791(4) 0.0622(12) Uani 1 d . . . C302 C -0.1450(16) 0.3457(12) -0.0750(11) 0.157(6) Uani 1 d . . . H30A H -0.2108 0.2984 -0.1457 0.188 Uiso 1 calc R . . H30B H -0.0829 0.2930 -0.0460 0.188 Uiso 1 calc R . . H30C H -0.0822 0.4065 -0.0830 0.188 Uiso 1 calc R . . C301 C -0.2336(11) 0.4046(7) -0.0004(7) 0.085(2) Uani 1 d . . . N300 N -0.3047(11) 0.4529(8) 0.0534(7) 0.106(3) Uani 1 d . . . N400 N 0.4739(10) -0.1435(7) 0.0231(6) 0.099(3) Uani 1 d . . . C401 C 0.5519(10) -0.1857(7) 0.0764(6) 0.076(2) Uani 1 d . . . C402 C 0.6489(11) -0.2369(8) 0.1465(8) 0.098(3) Uani 1 d . . . H40A H 0.7142 -0.1727 0.2073 0.118 Uiso 1 calc R . . H40B H 0.7084 -0.2912 0.1054 0.118 Uiso 1 calc R . . H40C H 0.5896 -0.2813 0.1740 0.118 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02782(17) 0.03105(16) 0.03286(15) 0.01299(10) 0.00926(9) 0.00319(9) O100 0.054(3) 0.058(3) 0.036(2) 0.0153(18) 0.0140(18) 0.0148(19) N11 0.032(2) 0.034(2) 0.042(2) 0.0172(16) 0.0137(15) -0.0001(14) C12 0.039(3) 0.043(3) 0.050(3) 0.017(2) 0.014(2) -0.003(2) C13 0.028(3) 0.060(3) 0.068(4) 0.035(3) 0.018(2) 0.002(2) C14 0.042(4) 0.064(4) 0.061(3) 0.029(3) 0.028(3) 0.000(2) C15 0.041(3) 0.062(3) 0.044(3) 0.020(2) 0.021(2) 0.006(2) C16 0.030(3) 0.038(2) 0.043(3) 0.025(2) 0.0161(19) 0.0104(18) N21 0.029(2) 0.032(2) 0.0313(18) 0.0149(15) 0.0119(14) 0.0074(15) C22 0.031(3) 0.035(2) 0.036(2) 0.0203(19) 0.0135(18) 0.0089(18) N23 0.034(2) 0.042(2) 0.036(2) 0.0155(17) 0.0167(16) 0.0039(16) C24 0.042(3) 0.034(2) 0.030(2) 0.0110(18) 0.0103(19) 0.0065(19) N25 0.034(2) 0.034(2) 0.034(2) 0.0120(16) 0.0105(15) 0.0005(15) C26 0.030(3) 0.028(2) 0.036(2) 0.0174(18) 0.0109(17) 0.0064(17) N31 0.030(2) 0.048(2) 0.0312(19) 0.0121(17) 0.0110(15) 0.0017(16) C32 0.028(3) 0.029(2) 0.035(2) 0.0170(18) 0.0108(17) 0.0096(16) C33 0.035(3) 0.034(2) 0.044(3) 0.013(2) 0.014(2) 0.0037(18) C34 0.030(3) 0.049(3) 0.064(3) 0.024(3) 0.021(2) 0.004(2) C35 0.040(4) 0.068(4) 0.046(3) 0.023(3) 0.023(2) 0.006(2) C36 0.038(3) 0.066(4) 0.033(2) 0.012(2) 0.015(2) 0.002(2) N100 0.049(3) 0.055(3) 0.040(2) 0.007(2) 0.017(2) -0.010(2) O41 0.043(2) 0.048(2) 0.060(2) 0.0248(18) 0.0049(17) 0.0058(16) N43 0.043(3) 0.049(3) 0.037(2) 0.0165(19) 0.0078(18) -0.0052(19) O42 0.053(3) 0.042(2) 0.047(2) 0.0187(16) -0.0004(17) -0.0022(16) O43 0.060(3) 0.069(3) 0.056(2) 0.022(2) -0.012(2) -0.027(2) O61 0.050(3) 0.044(2) 0.058(2) 0.0249(17) 0.0261(18) 0.0149(16) O62 0.054(3) 0.044(2) 0.048(2) 0.0199(16) 0.0223(17) 0.0076(16) N63 0.038(3) 0.039(2) 0.049(2) 0.0214(19) 0.0038(18) 0.0039(17) O64 0.075(3) 0.062(3) 0.090(3) 0.049(3) 0.013(2) 0.023(2) O51 0.053(3) 0.051(2) 0.050(2) 0.0289(17) 0.0212(17) 0.0123(17) N53 0.047(3) 0.043(2) 0.040(2) 0.0228(19) 0.0045(18) 0.0107(19) O54 0.090(4) 0.054(3) 0.090(3) 0.046(2) 0.022(3) 0.034(2) O52 0.075(3) 0.074(3) 0.067(3) 0.045(2) 0.041(2) 0.042(2) C302 0.165(14) 0.132(10) 0.170(12) 0.008(9) 0.104(11) 0.047(9) C301 0.094(7) 0.070(5) 0.089(6) 0.015(4) 0.037(5) 0.019(4) N300 0.116(7) 0.111(6) 0.092(5) 0.022(4) 0.050(5) 0.029(5) N400 0.143(8) 0.103(5) 0.078(4) 0.046(4) 0.060(5) 0.061(5) C401 0.105(7) 0.073(5) 0.077(5) 0.041(4) 0.052(4) 0.024(4) C402 0.116(8) 0.096(6) 0.121(7) 0.074(6) 0.048(6) 0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O100 2.470(4) . ? Nd O42 2.546(4) . ? Nd O51 2.548(4) . ? Nd N21 2.552(4) . ? Nd O52 2.557(4) . ? Nd O61 2.566(4) . ? Nd O41 2.592(4) . ? Nd O62 2.597(4) . ? Nd N31 2.618(5) . ? Nd N11 2.645(4) . ? N11 C12 1.333(7) . ? N11 C16 1.345(6) . ? C12 C13 1.381(7) . ? C13 C14 1.376(8) . ? C14 C15 1.377(8) . ? C15 C16 1.393(7) . ? C16 C22 1.488(7) . ? N21 C26 1.353(6) . ? N21 C22 1.352(6) . ? C22 N23 1.310(6) . ? N23 C24 1.351(7) . ? C24 N100 1.323(6) . ? C24 N25 1.356(6) . ? N25 C26 1.320(6) . ? C26 C32 1.482(6) . ? N31 C36 1.346(6) . ? N31 C32 1.353(6) . ? C32 C33 1.389(7) . ? C33 C34 1.378(7) . ? C34 C35 1.372(8) . ? C35 C36 1.371(8) . ? O41 N43 1.255(6) . ? N43 O44 1.225(6) . ? N42 O42 1.263(6) . ? O61 N63 1.261(6) . ? O62 N63 1.268(6) . ? N63 O64 1.209(6) . ? O52 N53 1.256(6) . ? N53 O51 1.214(6) . ? N53 O54 1.262(6) . ? C302 C301 1.438(12) . ? C301 N300 1.106(10) . ? N400 C401 1.125(10) . ? C401 C402 1.421(11) . ? 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 O100 Nd O43 75.63(14) . . ? O100 Nd O51 112.86(15) . . ? O43 Nd O51 69.10(14) . . ? O100 Nd N21 146.54(14) . . ? O42 Nd N21 134.20(12) . . ? O51 Nd N21 74.84(14) . . ? O100 Nd O52 67.78(15) . . ? O42 Nd O52 75.69(17) . . ? O51 Nd O52 49.36(13) . . ? N21 Nd O52 101.27(14) . . ? O100 Nd O61 112.84(14) . . ? O42 Nd O61 115.67(15) . . ? O51 Nd O61 133.59(12) . . ? N21 Nd O61 71.78(13) . . ? O52 Nd O61 168.60(15) . . ? O100 Nd O41 71.62(16) . . ? O42 Nd O41 49.40(12) . . ? O51 Nd O41 115.82(13) . . ? N21 Nd O41 136.45(13) . . ? O52 Nd O41 117.68(15) . . ? O61 Nd O41 72.19(13) . . ? O100 Nd O62 67.92(15) . . ? O42 Nd O62 120.59(13) . . ? O51 Nd O62 169.22(13) . . ? N21 Nd O62 98.62(14) . . ? O52 Nd O62 125.66(13) . . ? O61 Nd O62 48.95(12) . . ? O41 Nd O62 74.85(13) . . ? O100 Nd N31 84.08(14) . . ? O42 Nd N31 146.89(13) . . ? O51 Nd N31 96.09(13) . . ? N21 Nd N31 62.51(12) . . ? O52 Nd N31 72.48(17) . . ? O61 Nd N31 96.16(15) . . ? O41 Nd N31 145.30(13) . . ? O62 Nd N31 73.19(13) . . ? O100 Nd N11 150.17(14) . . ? O42 Nd N11 77.49(13) . . ? O51 Nd N11 68.25(13) . . ? N21 Nd N11 63.27(13) . . ? O52 Nd N11 117.29(13) . . ? O61 Nd N11 68.30(12) . . ? O41 Nd N11 81.16(15) . . ? O62 Nd N11 116.88(12) . . ? N31 Nd N11 125.75(13) . . ? C12 N11 C16 117.0(4) . . ? C12 N11 Nd 123.6(3) . . ? C16 N11 Nd 119.3(3) . . ? N11 C12 C13 124.0(5) . . ? C14 C13 C12 118.5(5) . . ? C15 C14 C13 119.1(5) . . ? C14 C15 C16 118.8(5) . . ? N11 C16 C15 122.7(5) . . ? N11 C16 C22 117.5(4) . . ? C15 C16 C22 119.8(4) . . ? C26 N21 C22 114.0(4) . . ? C26 N21 Nd 123.4(3) . . ? C22 N21 Nd 122.6(3) . . ? N23 C22 N21 125.8(4) . . ? N23 C22 C16 117.1(4) . . ? N21 C22 C16 117.1(4) . . ? C22 N23 C24 115.4(4) . . ? N100 C24 N23 117.2(4) . . ? N100 C24 N25 118.5(5) . . ? N23 C24 N25 124.3(4) . . ? C26 N25 C24 114.7(4) . . ? N25 C26 N21 125.8(4) . . ? N25 C26 C32 117.5(4) . . ? N21 C26 C32 116.7(4) . . ? C36 N31 C32 117.6(4) . . ? C36 N31 Nd 121.0(3) . . ? C32 N31 Nd 121.4(3) . . ? N31 C32 C33 122.5(4) . . ? N31 C32 C26 116.0(4) . . ? C33 C32 C26 121.5(4) . . ? C34 C33 C32 118.4(5) . . ? C35 C34 C33 119.3(5) . . ? C36 C35 C34 119.6(5) . . ? N31 C36 C35 122.6(5) . . ? N43 O41 Nd 95.1(3) . . ? O44 N43 O41 122.0(5) . . ? O44 N43 O42 120.9(5) . . ? O41 N43 O42 117.1(4) . . ? N43 O42 Nd 97.2(3) . . ? N63 O61 Nd 98.5(3) . . ? N63 O62 Nd 96.8(3) . . ? O64 N63 O61 122.1(5) . . ? O64 N63 O62 122.4(5) . . ? O61 N63 O62 115.5(4) . . ? N53 O51 Nd 97.0(3) . . ? O54 N53 O51 122.3(5) . . ? O54 N53 O52 121.9(5) . . ? O51 N53 O52 115.7(4) . . ? N53 O52 Nd 96.4(3) . . ? N300 C301 C302 176.4(12) . . ? N400 C401 C402 178.4(8) . . ? _refine_diff_density_max 1.189 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.104 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_2-Sm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-Sm,NCMe _chemical_formula_moiety '[SmL4(NO3)3(H2O)] NCMe' _chemical_formula_sum 'C15 H15 N10 O10 Sm' _chemical_formula_weight 647.74 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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.936(9) _cell_length_b 11.106(12) _cell_length_c 11.831(12) _cell_angle_alpha 117.346(10) _cell_angle_beta 91.333(10) _cell_angle_gamma 100.543(10) _cell_volume 1131(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.94 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 2.670 _exptl_absorpt_correction_type 'empirical (DIFABS)' _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3960 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.94 _reflns_number_total 3960 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. Hydrogen atoms on water molecules could not be located and were not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+2.3837P] 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 SHELXL _refine_ls_extinction_coef 0.0116(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3960 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.248754(15) 0.267347(15) 0.164871(15) 0.02447(10) Uani 1 d . . . N11 N 0.0788(3) 0.4212(3) 0.2873(3) 0.0317(7) Uani 1 d . . . C12 C -0.0416(4) 0.3698(4) 0.3135(4) 0.0369(8) Uani 1 d . . . H12 H -0.0612 0.2768 0.2942 0.044 Uiso 1 calc R . . C13 C -0.1386(4) 0.4475(5) 0.3679(4) 0.0425(9) Uani 1 d . . . H13 H -0.2202 0.4080 0.3865 0.051 Uiso 1 calc R . . C14 C -0.1120(4) 0.5842(5) 0.3940(4) 0.0469(10) Uani 1 d . . . H14 H -0.1765 0.6382 0.4284 0.056 Uiso 1 calc R . . C15 C 0.0118(4) 0.6401(4) 0.3682(4) 0.0418(9) Uani 1 d . . . H15 H 0.0323 0.7326 0.3859 0.050 Uiso 1 calc R . . C16 C 0.1052(4) 0.5568(4) 0.3157(3) 0.0323(8) Uani 1 d . . . N21 N 0.3243(3) 0.5237(3) 0.2360(3) 0.0280(6) Uani 1 d . . . C22 C 0.2400(4) 0.6119(4) 0.2865(3) 0.0297(7) Uani 1 d . . . N23 N 0.2672(3) 0.7433(3) 0.3100(3) 0.0378(7) Uani 1 d . . . C24 C 0.3883(4) 0.7853(4) 0.2758(4) 0.0370(8) Uani 1 d . . . N25 N 0.4838(3) 0.7076(3) 0.2301(3) 0.0350(7) Uani 1 d . . . C26 C 0.4455(4) 0.5795(3) 0.2125(3) 0.0284(7) Uani 1 d . . . N31 N 0.5023(3) 0.3583(3) 0.1495(3) 0.0311(6) Uani 1 d . . . C32 C 0.5431(3) 0.4856(4) 0.1585(3) 0.0278(7) Uani 1 d . . . C33 C 0.6647(4) 0.5249(4) 0.1184(4) 0.0357(8) Uani 1 d . . . H33 H 0.6903 0.6136 0.1265 0.043 Uiso 1 calc R . . C34 C 0.7485(4) 0.4302(4) 0.0656(4) 0.0398(9) Uani 1 d . . . H34 H 0.8299 0.4536 0.0360 0.048 Uiso 1 calc R . . C35 C 0.7085(4) 0.3013(4) 0.0581(4) 0.0389(9) Uani 1 d . . . H35 H 0.7633 0.2363 0.0243 0.047 Uiso 1 calc R . . C36 C 0.5861(4) 0.2697(4) 0.1012(4) 0.0368(8) Uani 1 d . . . H36 H 0.5604 0.1825 0.0966 0.044 Uiso 1 calc R . . N27 N 0.4171(4) 0.9137(4) 0.2885(4) 0.0549(10) Uani 1 d . . . H27A H 0.3592 0.9664 0.3175 0.066 Uiso 1 calc R . . H27B H 0.4935 0.9436 0.2675 0.066 Uiso 1 calc R . . O41 O 0.3032(3) 0.1654(3) -0.0706(3) 0.0419(6) Uani 1 d . . . N43 N 0.3081(4) 0.0478(4) -0.0826(3) 0.0387(8) Uani 1 d . . . O44 O 0.3305(5) -0.0449(4) -0.1831(3) 0.0666(11) Uani 1 d . . . O42 O 0.2912(3) 0.0307(3) 0.0153(3) 0.0425(7) Uani 1 d . . . O51 O 0.0325(3) 0.1476(3) 0.0005(3) 0.0385(6) Uani 1 d . . . N53 N 0.0402(3) 0.2374(3) -0.0395(3) 0.0335(7) Uani 1 d . . . O54 O -0.0334(4) 0.2147(4) -0.1335(3) 0.0588(9) Uani 1 d . . . O52 O 0.1270(3) 0.3490(3) 0.0247(3) 0.0378(6) Uani 1 d . . . O61 O 0.3978(3) 0.1857(3) 0.2820(3) 0.0455(7) Uani 1 d . . . O62 O 0.3261(3) 0.3704(3) 0.3970(3) 0.0463(7) Uani 1 d . . . N63 N 0.3967(4) 0.2842(4) 0.3924(4) 0.0435(8) Uani 1 d . . . O64 O 0.4558(5) 0.2939(5) 0.4884(4) 0.0805(13) Uani 1 d . . . O100 O 0.0908(3) 0.1065(3) 0.2136(3) 0.0376(6) Uani 1 d . . . N100 N 0.1511(6) 0.0709(5) 0.4288(4) 0.0646(12) Uani 1 d . . . C101 C 0.1750(5) 0.0550(5) 0.5131(5) 0.0490(11) Uani 1 d . . . C102 C 0.2098(8) 0.0344(9) 0.6192(7) 0.101(3) Uani 1 d . . . H10A H 0.2856 -0.0115 0.6031 0.121 Uiso 1 calc R . . H10B H 0.1317 -0.0218 0.6312 0.121 Uiso 1 calc R . . H10C H 0.2357 0.1227 0.6951 0.121 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02461(12) 0.02422(12) 0.02479(12) 0.01172(8) 0.00349(8) 0.00528(7) N11 0.0270(14) 0.0354(16) 0.0325(16) 0.0160(13) 0.0049(13) 0.0065(12) C12 0.0295(18) 0.044(2) 0.038(2) 0.0201(17) 0.0058(16) 0.0054(15) C13 0.0329(19) 0.056(2) 0.038(2) 0.0208(19) 0.0095(17) 0.0101(17) C14 0.037(2) 0.051(2) 0.048(2) 0.015(2) 0.0146(19) 0.0193(18) C15 0.038(2) 0.038(2) 0.046(2) 0.0141(18) 0.0097(18) 0.0153(17) C16 0.0308(17) 0.0332(18) 0.0283(17) 0.0092(15) 0.0027(15) 0.0108(14) N21 0.0267(14) 0.0251(13) 0.0293(14) 0.0105(12) 0.0021(12) 0.0056(11) C22 0.0316(17) 0.0286(16) 0.0265(16) 0.0103(14) 0.0014(14) 0.0088(13) N23 0.0402(17) 0.0293(15) 0.0439(18) 0.0156(14) 0.0074(15) 0.0119(13) C24 0.040(2) 0.0290(17) 0.041(2) 0.0157(16) 0.0049(17) 0.0087(15) N25 0.0370(16) 0.0313(15) 0.0399(18) 0.0192(14) 0.0080(15) 0.0075(13) C26 0.0262(16) 0.0284(16) 0.0284(17) 0.0120(14) -0.0006(14) 0.0051(13) N31 0.0224(13) 0.0331(15) 0.0411(17) 0.0202(13) 0.0058(13) 0.0058(11) C32 0.0248(16) 0.0323(17) 0.0265(16) 0.0145(14) 0.0001(14) 0.0052(13) C33 0.0304(18) 0.0335(18) 0.044(2) 0.0201(17) 0.0065(17) 0.0043(14) C34 0.0288(18) 0.051(2) 0.050(2) 0.030(2) 0.0135(18) 0.0139(16) C35 0.0278(18) 0.045(2) 0.048(2) 0.0220(18) 0.0104(17) 0.0161(16) C36 0.0309(18) 0.0316(18) 0.051(2) 0.0216(17) 0.0038(17) 0.0098(14) N27 0.060(2) 0.0319(18) 0.079(3) 0.0294(19) 0.022(2) 0.0157(16) O41 0.0522(17) 0.0422(15) 0.0385(15) 0.0226(13) 0.0135(14) 0.0158(13) N43 0.0401(18) 0.0460(18) 0.0312(16) 0.0144(15) 0.0079(15) 0.0220(15) O44 0.108(3) 0.067(2) 0.0361(16) 0.0193(16) 0.0280(19) 0.056(2) O42 0.0596(18) 0.0424(15) 0.0340(14) 0.0209(12) 0.0151(14) 0.0219(13) O51 0.0361(14) 0.0386(14) 0.0426(15) 0.0244(12) -0.0044(12) -0.0010(11) N53 0.0314(16) 0.0369(16) 0.0314(16) 0.0156(13) -0.0003(14) 0.0076(13) O54 0.059(2) 0.069(2) 0.0493(19) 0.0323(17) -0.0193(17) 0.0059(17) O52 0.0415(15) 0.0314(13) 0.0384(15) 0.0161(12) -0.0018(13) 0.0052(11) O61 0.0510(17) 0.0500(17) 0.0444(16) 0.0261(14) 0.0059(14) 0.0205(14) O62 0.0541(18) 0.0475(16) 0.0333(14) 0.0147(13) 0.0014(14) 0.0149(14) N63 0.0427(19) 0.051(2) 0.0383(19) 0.0258(17) -0.0050(16) 0.0032(16) O64 0.090(3) 0.097(3) 0.056(2) 0.040(2) -0.028(2) 0.016(2) O100 0.0407(14) 0.0381(14) 0.0364(14) 0.0225(12) 0.0046(12) 0.0010(11) N100 0.091(3) 0.068(3) 0.048(2) 0.036(2) 0.013(2) 0.021(2) C101 0.046(2) 0.054(3) 0.043(2) 0.022(2) 0.004(2) 0.0069(19) C102 0.084(5) 0.150(7) 0.071(4) 0.071(5) -0.031(4) -0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O100 2.439(3) . ? Sm1 O62 2.477(4) . ? Sm1 N21 2.523(4) . ? Sm1 O42 2.527(3) . ? Sm1 O61 2.546(3) . ? Sm1 O51 2.559(3) . ? Sm1 N31 2.580(4) . ? Sm1 O52 2.593(3) . ? Sm1 O41 2.595(4) . ? Sm1 N11 2.601(3) . ? N11 C12 1.335(5) . ? N11 C16 1.356(5) . ? C12 C13 1.382(6) . ? C13 C14 1.375(7) . ? C14 C15 1.380(6) . ? C15 C16 1.384(5) . ? C16 C22 1.484(6) . ? N21 C22 1.343(5) . ? N21 C26 1.346(5) . ? C22 N23 1.326(5) . ? N23 C24 1.349(6) . ? C24 N27 1.338(5) . ? C24 N25 1.354(5) . ? N25 C26 1.318(5) . ? C26 C32 1.491(5) . ? N31 C36 1.339(5) . ? N31 C32 1.351(5) . ? C32 C33 1.378(5) . ? C33 C34 1.389(6) . ? C34 C35 1.374(6) . ? C35 C36 1.379(6) . ? O41 N43 1.258(5) . ? N43 O44 1.223(5) . ? N43 O42 1.266(5) . ? O51 N53 1.278(4) . ? N53 O54 1.213(4) . ? N53 O52 1.253(4) . ? O61 N63 1.263(5) . ? O62 N63 1.269(5) . ? N63 O64 1.217(5) . ? N100 C101 1.117(7) . ? C101 C102 1.422(8) . ? 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 O100 Sm1 O62 80.91(11) . . ? O100 Sm1 N21 140.66(10) . . ? O62 Sm1 N21 76.19(10) . . ? O100 Sm1 O42 75.25(12) . . ? O62 Sm1 O42 118.77(10) . . ? N21 Sm1 O42 144.05(11) . . ? O100 Sm1 O61 73.85(12) . . ? O62 Sm1 O61 50.41(11) . . ? N21 Sm1 O61 112.56(11) . . ? O42 Sm1 O61 68.87(12) . . ? O100 Sm1 O51 68.81(11) . . ? O62 Sm1 O51 142.13(11) . . ? N21 Sm1 O51 113.76(9) . . ? O42 Sm1 O51 75.66(11) . . ? O61 Sm1 O51 133.58(11) . . ? O100 Sm1 N31 145.81(10) . . ? O62 Sm1 N31 84.74(11) . . ? N21 Sm1 N31 62.92(9) . . ? O42 Sm1 N31 84.97(11) . . ? O61 Sm1 N31 73.07(12) . . ? O51 Sm1 N31 132.90(11) . . ? O100 Sm1 O52 112.86(11) . . ? O62 Sm1 O52 134.30(11) . . ? N21 Sm1 O52 66.08(10) . . ? O42 Sm1 O52 106.93(11) . . ? O61 Sm1 O52 171.39(10) . . ? O51 Sm1 O52 49.17(10) . . ? N31 Sm1 O52 99.36(11) . . ? O100 Sm1 O41 115.02(10) . . ? O62 Sm1 O41 150.21(11) . . ? N21 Sm1 O41 100.28(10) . . ? O42 Sm1 O41 49.62(9) . . ? O61 Sm1 O41 107.61(11) . . ? O51 Sm1 O41 66.76(11) . . ? N31 Sm1 O41 67.97(10) . . ? O52 Sm1 O41 65.04(11) . . ? O100 Sm1 N11 79.24(12) . . ? O62 Sm1 N11 72.71(11) . . ? N21 Sm1 N11 63.65(11) . . ? O42 Sm1 N11 149.39(10) . . ? O61 Sm1 N11 119.53(12) . . ? O51 Sm1 N11 79.55(11) . . ? N31 Sm1 N11 125.42(11) . . ? O52 Sm1 N11 68.04(12) . . ? O41 Sm1 N11 132.85(9) . . ? C12 N11 C16 117.4(3) . . ? C12 N11 Sm1 122.8(3) . . ? C16 N11 Sm1 119.5(2) . . ? N11 C12 C13 123.5(4) . . ? C14 C13 C12 118.7(4) . . ? C13 C14 C15 119.0(4) . . ? C14 C15 C16 119.2(4) . . ? N11 C16 C15 122.2(4) . . ? N11 C16 C22 116.4(3) . . ? C15 C16 C22 121.4(4) . . ? C22 N21 C26 114.7(3) . . ? C22 N21 Sm1 122.3(2) . . ? C26 N21 Sm1 122.5(2) . . ? N23 C22 N21 125.0(4) . . ? N23 C22 C16 117.8(3) . . ? N21 C22 C16 117.3(3) . . ? C22 N23 C24 114.9(3) . . ? N27 C24 N23 117.8(4) . . ? N27 C24 N25 117.3(4) . . ? N23 C24 N25 125.0(3) . . ? C26 N25 C24 114.2(4) . . ? N25 C26 N21 126.0(3) . . ? N25 C26 C32 117.5(3) . . ? N21 C26 C32 116.4(3) . . ? C36 N31 C32 117.5(3) . . ? C36 N31 Sm1 120.0(2) . . ? C32 N31 Sm1 120.5(2) . . ? N31 C32 C33 122.5(3) . . ? N31 C32 C26 115.0(3) . . ? C33 C32 C26 122.5(3) . . ? C32 C33 C34 119.1(4) . . ? C35 C34 C33 118.6(4) . . ? C34 C35 C36 119.0(4) . . ? N31 C36 C35 123.2(4) . . ? N43 O41 Sm1 95.2(2) . . ? O44 N43 O41 121.6(4) . . ? O44 N43 O42 121.5(4) . . ? O41 N43 O42 116.8(3) . . ? N43 O42 Sm1 98.3(2) . . ? N53 O51 Sm1 97.4(2) . . ? O54 N53 O52 122.9(4) . . ? O54 N53 O51 121.3(3) . . ? O52 N53 O51 115.8(3) . . ? N53 O52 Sm1 96.5(2) . . ? N63 O61 Sm1 95.5(2) . . ? N63 O62 Sm1 98.7(2) . . ? O64 N63 O61 122.5(4) . . ? O64 N63 O62 122.0(4) . . ? O61 N63 O62 115.4(3) . . ? N100 C101 C102 178.1(7) . . ? _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., (1983) Acta Cryst A39 158. ; #===END data_3-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3-Nd,H2O _chemical_formula_moiety [NdL4(NO3)2(H2O)3] [NO3] H2O _chemical_formula_sum 'C13 H18 N9 Nd O13' _chemical_formula_weight 652.60 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.332(9) _cell_length_b 9.521(9) _cell_length_c 13.622(12) _cell_angle_alpha 79.378(10) _cell_angle_beta 81.902(10) _cell_angle_gamma 73.879(10) _cell_volume 1137.6(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 2.368 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 0.577 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3610 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3610 _reflns_number_gt 3261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. hydrogen atoms bonded to oxygen atoms in water molecules could not be located. and were not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+2.6310P] 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 3610 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.16657(3) 0.19785(3) 0.201511(19) 0.02764(16) Uani 1 d . . . N11 N -0.0717(6) 0.1122(7) 0.2882(4) 0.0378(11) Uani 1 d . . . C12 C -0.1455(8) 0.0502(9) 0.2378(5) 0.0463(16) Uani 1 d . . . H12 H -0.1126 0.0409 0.1710 0.056 Uiso 1 calc R . . C13 C -0.2682(8) -0.0004(10) 0.2814(6) 0.069(2) Uani 1 d . . . H13 H -0.3128 -0.0398 0.2471 0.082 Uiso 1 calc R . . C14 C -0.3191(7) 0.0126(8) 0.3805(5) 0.0455(16) Uani 1 d . . . H14 H -0.4015 -0.0211 0.4110 0.055 Uiso 1 calc R . . C15 C -0.2451(7) 0.0765(8) 0.4327(5) 0.0391(15) Uani 1 d . . . H15 H -0.2773 0.0877 0.4993 0.047 Uiso 1 calc R . . C16 C -0.1219(6) 0.1240(6) 0.3851(4) 0.0291(11) Uani 1 d . . . C22 C -0.0358(6) 0.1944(7) 0.4385(4) 0.0295(12) Uani 1 d . . . N21 N 0.0881(5) 0.2259(6) 0.3873(4) 0.0300(10) Uani 1 d . . . C26 C 0.1578(6) 0.2928(6) 0.4382(4) 0.0295(11) Uani 1 d . . . N25 N 0.1138(6) 0.3267(6) 0.5286(4) 0.0381(11) Uani 1 d . . . C24 C -0.0114(7) 0.2887(7) 0.5725(4) 0.0372(13) Uani 1 d . . . N23 N -0.0902(6) 0.2195(6) 0.5297(4) 0.0348(11) Uani 1 d . . . C32 C 0.2971(6) 0.3315(7) 0.3852(5) 0.0327(12) Uani 1 d . . . N31 N 0.3259(5) 0.3180(6) 0.2867(4) 0.0329(11) Uani 1 d . . . C36 C 0.4486(8) 0.3551(8) 0.2387(6) 0.0459(16) Uani 1 d . . . H36 H 0.4695 0.3497 0.1705 0.055 Uiso 1 calc R . . C35 C 0.5462(8) 0.4014(9) 0.2861(7) 0.057(2) Uani 1 d . . . H35 H 0.6310 0.4255 0.2508 0.069 Uiso 1 calc R . . C34 C 0.5132(7) 0.4105(9) 0.3880(6) 0.0430(17) Uani 1 d . . . H34 H 0.5754 0.4421 0.4220 0.052 Uiso 1 calc R . . C33 C 0.3927(8) 0.3736(9) 0.4358(6) 0.0487(18) Uani 1 d . . . H33 H 0.3719 0.3759 0.5043 0.058 Uiso 1 calc R . . N27 N -0.0600(8) 0.3157(8) 0.6660(5) 0.0523(16) Uani 1 d . . . H10A H -0.0114 0.3564 0.6966 0.063 Uiso 1 calc R . . H10B H -0.1397 0.2924 0.6956 0.063 Uiso 1 calc R . . O41 O 0.2304(6) -0.0882(6) 0.2313(4) 0.0477(11) Uani 1 d . . . N43 N 0.3277(6) -0.1109(7) 0.2924(4) 0.0418(13) Uani 1 d . . . O42 O 0.3503(5) 0.0036(6) 0.3172(4) 0.0445(11) Uani 1 d . . . O44 O 0.3959(7) -0.2346(6) 0.3264(5) 0.0654(17) Uani 1 d . . . N53 N -0.0921(6) 0.4841(8) 0.1685(5) 0.0491(16) Uani 1 d . . . O52 O -0.0816(8) 0.3817(9) 0.1192(6) 0.0739(19) Uani 1 d . . . O51 O -0.0051(6) 0.4549(6) 0.2355(4) 0.0534(13) Uani 1 d . . . O54 O -0.1788(7) 0.6044(8) 0.1520(7) 0.098(3) Uani 1 d . . . N63 N -0.2406(12) 0.2528(9) -0.0501(7) 0.075(3) Uani 1 d . . . O62 O -0.2629(8) 0.1400(7) 0.0032(5) 0.0678(16) Uani 1 d . . . O61 O -0.3412(12) 0.3556(9) -0.0809(10) 0.127(4) Uani 1 d . . . O64 O -0.1087(10) 0.2648(10) -0.0772(6) 0.094(3) Uani 1 d . . . O100 O 0.2284(6) 0.3976(5) 0.0686(3) 0.0459(11) Uani 1 d . . . O200 O 0.1024(6) 0.1241(6) 0.0525(4) 0.0513(13) Uani 1 d . . . O300 O 0.4131(5) 0.1031(6) 0.1075(4) 0.0494(12) Uani 1 d . . . O400 O 0.4499(7) 0.1948(8) -0.1029(5) 0.076(2) Uani 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 0.0285(2) 0.0272(3) 0.0269(2) -0.00435(14) -0.00211(13) -0.00674(14) N11 0.034(3) 0.044(3) 0.038(3) -0.009(2) -0.005(2) -0.013(2) C12 0.049(4) 0.062(5) 0.039(3) -0.017(3) -0.005(3) -0.026(3) C13 0.047(4) 0.062(6) 0.064(5) -0.008(4) -0.022(4) -0.021(4) C14 0.040(3) 0.048(4) 0.054(4) -0.002(3) -0.006(3) -0.025(3) C15 0.034(3) 0.045(4) 0.037(3) 0.000(3) -0.004(2) -0.013(3) C16 0.027(3) 0.029(3) 0.033(3) -0.004(2) -0.006(2) -0.009(2) C22 0.021(2) 0.031(3) 0.031(3) -0.001(2) -0.003(2) -0.001(2) N21 0.026(2) 0.034(3) 0.030(2) -0.0066(19) -0.0036(17) -0.0065(19) C26 0.033(3) 0.027(3) 0.030(3) -0.008(2) -0.003(2) -0.008(2) N25 0.043(3) 0.036(3) 0.040(3) -0.013(2) -0.005(2) -0.013(2) C24 0.044(3) 0.038(4) 0.030(3) -0.013(2) -0.003(2) -0.007(3) N23 0.038(3) 0.031(3) 0.036(3) -0.009(2) 0.001(2) -0.010(2) C32 0.028(3) 0.025(3) 0.048(3) -0.009(2) -0.004(2) -0.009(2) N31 0.029(2) 0.032(3) 0.040(3) -0.007(2) 0.001(2) -0.011(2) C36 0.044(4) 0.044(4) 0.050(4) -0.001(3) 0.002(3) -0.019(3) C35 0.047(4) 0.052(5) 0.081(6) -0.006(4) -0.002(4) -0.031(3) C34 0.027(3) 0.044(4) 0.072(5) -0.036(3) 0.001(3) -0.019(3) C33 0.048(4) 0.059(5) 0.057(4) -0.028(3) 0.003(3) -0.034(3) N27 0.062(4) 0.065(5) 0.040(3) -0.023(3) 0.009(3) -0.032(3) O41 0.051(3) 0.044(3) 0.049(3) -0.008(2) -0.006(2) -0.013(2) N43 0.040(3) 0.037(3) 0.039(3) -0.002(2) 0.004(2) -0.001(2) O42 0.043(3) 0.041(3) 0.048(3) -0.005(2) -0.011(2) -0.006(2) O44 0.073(4) 0.037(3) 0.063(3) 0.007(2) 0.001(3) 0.010(3) N53 0.028(3) 0.051(4) 0.057(4) 0.011(3) -0.005(2) -0.004(3) O52 0.077(4) 0.078(5) 0.081(4) -0.012(4) -0.033(3) -0.032(4) O51 0.065(3) 0.044(3) 0.045(3) -0.010(2) -0.013(2) 0.004(2) O54 0.047(3) 0.060(4) 0.159(8) 0.024(4) -0.017(4) 0.008(3) N63 0.117(7) 0.039(4) 0.081(6) -0.008(4) -0.051(5) -0.018(5) O62 0.087(4) 0.044(3) 0.069(4) -0.009(3) -0.012(3) -0.009(3) O61 0.131(8) 0.047(5) 0.202(11) 0.005(5) -0.090(8) -0.003(5) O64 0.116(6) 0.099(6) 0.085(5) 0.029(4) -0.052(4) -0.065(5) O100 0.060(3) 0.035(3) 0.042(2) 0.0027(19) -0.002(2) -0.017(2) O200 0.071(3) 0.043(3) 0.045(3) -0.016(2) -0.018(2) -0.012(2) O300 0.044(3) 0.055(3) 0.042(2) -0.005(2) 0.0104(19) -0.009(2) O400 0.057(4) 0.066(4) 0.075(4) 0.010(3) 0.011(3) 0.009(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 O200 2.464(5) . ? Nd1 O300 2.488(5) . ? Nd1 O100 2.504(5) . ? Nd1 N21 2.575(5) . ? Nd1 O41 2.588(6) . ? Nd1 O42 2.602(5) . ? Nd1 N31 2.605(5) . ? Nd1 O51 2.608(5) . ? Nd1 N11 2.630(6) . ? Nd1 O52 2.728(7) . ? N11 C12 1.343(8) . ? N11 C16 1.352(8) . ? C12 C13 1.380(10) . ? C13 C14 1.383(11) . ? C14 C15 1.373(10) . ? C15 C16 1.384(9) . ? C16 C22 1.505(8) . ? C22 N23 1.313(8) . ? C22 N21 1.341(8) . ? N21 C26 1.352(7) . ? C26 N25 1.312(8) . ? C26 C32 1.500(8) . ? N25 C24 1.346(9) . ? C24 N27 1.337(9) . ? C24 N23 1.358(8) . ? C32 N31 1.354(8) . ? C32 C33 1.380(8) . ? N31 C36 1.338(8) . ? C36 C35 1.391(11) . ? C35 C34 1.392(12) . ? C34 C33 1.320(10) . ? O41 N43 1.265(8) . ? N43 O44 1.214(8) . ? N43 O42 1.277(8) . ? N53 O54 1.208(9) . ? N53 O51 1.249(8) . ? N53 O52 1.258(10) . ? N63 O61 1.210(11) . ? N63 O62 1.232(11) . ? N63 O64 1.264(13) . ? 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 O200 Nd1 O300 75.74(19) . . ? O200 Nd1 O100 79.96(19) . . ? O300 Nd1 O100 69.70(17) . . ? O200 Nd1 N21 145.33(18) . . ? O300 Nd1 N21 132.69(16) . . ? O100 Nd1 N21 124.48(17) . . ? O200 Nd1 O41 73.31(17) . . ? O300 Nd1 O41 71.73(17) . . ? O100 Nd1 O41 137.25(16) . . ? N21 Nd1 O41 95.33(16) . . ? O200 Nd1 O42 118.80(18) . . ? O300 Nd1 O42 68.62(17) . . ? O100 Nd1 O42 126.89(17) . . ? N21 Nd1 O42 68.95(16) . . ? O41 Nd1 O42 49.24(17) . . ? O200 Nd1 N31 151.28(18) . . ? O300 Nd1 N31 81.96(18) . . ? O100 Nd1 N31 75.43(18) . . ? N21 Nd1 N31 63.14(16) . . ? O41 Nd1 N31 116.52(16) . . ? O42 Nd1 N31 67.53(18) . . ? O200 Nd1 O51 111.46(17) . . ? O300 Nd1 O51 136.90(19) . . ? O100 Nd1 O51 70.05(18) . . ? N21 Nd1 O51 64.15(16) . . ? O41 Nd1 O51 151.26(19) . . ? O42 Nd1 O51 128.72(16) . . ? N31 Nd1 O51 73.64(18) . . ? O200 Nd1 N11 83.22(19) . . ? O300 Nd1 N11 140.88(18) . . ? O100 Nd1 N11 138.42(16) . . ? N21 Nd1 N11 62.15(16) . . ? O41 Nd1 N11 70.79(17) . . ? O42 Nd1 N11 94.51(18) . . ? N31 Nd1 N11 125.25(16) . . ? O51 Nd1 N11 81.5(2) . . ? O200 Nd1 O52 65.0(2) . . ? O300 Nd1 O52 125.5(2) . . ? O100 Nd1 O52 67.6(2) . . ? N21 Nd1 O52 99.4(2) . . ? O41 Nd1 O52 125.44(19) . . ? O42 Nd1 O52 164.7(2) . . ? N31 Nd1 O52 117.0(2) . . ? O51 Nd1 O52 46.83(19) . . ? N11 Nd1 O52 70.8(2) . . ? C12 N11 C16 117.4(5) . . ? C12 N11 Nd1 120.6(4) . . ? C16 N11 Nd1 122.0(4) . . ? N11 C12 C13 122.4(7) . . ? C12 C13 C14 119.8(6) . . ? C15 C14 C13 118.4(6) . . ? C14 C15 C16 119.2(6) . . ? N11 C16 C15 122.8(6) . . ? N11 C16 C22 115.5(5) . . ? C15 C16 C22 121.7(5) . . ? N23 C22 N21 126.8(6) . . ? N23 C22 C16 116.7(5) . . ? N21 C22 C16 116.5(5) . . ? C22 N21 C26 113.5(5) . . ? C22 N21 Nd1 123.7(4) . . ? C26 N21 Nd1 122.2(4) . . ? N25 C26 N21 125.7(5) . . ? N25 C26 C32 117.9(5) . . ? N21 C26 C32 116.3(5) . . ? C26 N25 C24 115.2(5) . . ? N27 C24 N25 118.4(6) . . ? N27 C24 N23 117.1(6) . . ? N25 C24 N23 124.5(5) . . ? C22 N23 C24 114.1(5) . . ? N31 C32 C33 122.2(6) . . ? N31 C32 C26 116.5(5) . . ? C33 C32 C26 121.3(6) . . ? C36 N31 C32 116.7(5) . . ? C36 N31 Nd1 121.9(4) . . ? C32 N31 Nd1 121.0(4) . . ? N31 C36 C35 123.0(7) . . ? C34 C35 C36 118.1(7) . . ? C33 C34 C35 119.1(6) . . ? C34 C33 C32 120.8(7) . . ? N43 O41 Nd1 97.6(4) . . ? O44 N43 O41 122.2(6) . . ? O44 N43 O42 121.3(6) . . ? O41 N43 O42 116.5(5) . . ? N43 O42 Nd1 96.6(3) . . ? O54 N53 O51 121.4(9) . . ? O54 N53 O52 122.8(8) . . ? O51 N53 O52 115.8(6) . . ? N53 O52 Nd1 95.3(4) . . ? N53 O51 Nd1 101.5(4) . . ? O61 N63 O62 122.7(12) . . ? O61 N63 O64 116.6(11) . . ? O62 N63 O64 120.7(8) . . ? _refine_diff_density_max 0.959 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.144 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_3-Sm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3-Sm,H2O _chemical_formula_moiety [SmL4(NO3)2(H2O)3] [NO3] H2O ? _chemical_formula_sum 'C13 H18 N9 O13 Sm ' _chemical_formula_weight 658.71 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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.361(9) _cell_length_b 9.454(9) _cell_length_c 13.611(12) _cell_angle_alpha 79.723(10) _cell_angle_beta 81.839(10) _cell_angle_gamma 74.112(10) _cell_volume 1134.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 26.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.674 _exptl_absorpt_correction_type empirical (DIFABS) _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3355 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3355 _reflns_number_gt 3073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms were fixed at ideal positions with isotropic displacement parameters fixed at 1.2* that of the carbon atom to which they were bonded. Hydrogen atoms bonded to oxygen in water molecules were not located and were not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+2.6310P] 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 3355 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.16771(4) 0.19539(4) 0.20272(2) 0.0417(2) Uani 1 d . . . N11 N -0.0675(9) 0.1110(8) 0.2864(5) 0.0514(16) Uani 1 d . . . C12 C -0.1423(13) 0.0493(13) 0.2367(7) 0.066(2) Uani 1 d . . . H12 H -0.1106 0.0414 0.1698 0.090 Uiso 1 calc R . . C13 C -0.2660(12) -0.0037(12) 0.2810(8) 0.075(2) Uani 1 d . . . H13 H -0.3093 -0.0454 0.2470 0.090 Uiso 1 calc R . . C14 C -0.3174(12) 0.0117(11) 0.3793(8) 0.061(2) Uani 1 d . . . H14 H -0.4005 -0.0209 0.4097 0.073 Uiso 1 calc R . . C15 C -0.2430(11) 0.0764(11) 0.4317(7) 0.055(2) Uani 1 d . . . H15 H -0.2749 0.0879 0.4984 0.066 Uiso 1 calc R . . C16 C -0.1208(9) 0.1240(8) 0.3840(5) 0.0437(16) Uani 1 d . . . C22 C -0.0346(9) 0.1929(8) 0.4367(6) 0.0435(16) Uani 1 d . . . N21 N 0.0893(8) 0.2263(7) 0.3863(5) 0.0427(13) Uani 1 d . . . C26 C 0.1585(9) 0.2931(9) 0.4358(6) 0.0465(16) Uani 1 d . . . N25 N 0.1178(10) 0.3270(8) 0.5271(5) 0.0526(16) Uani 1 d . . . C24 C -0.0078(11) 0.2872(9) 0.5727(6) 0.0517(19) Uani 1 d . . . N23 N -0.0887(9) 0.2198(9) 0.5290(5) 0.0498(16) Uani 1 d . . . C32 C 0.2998(9) 0.3302(8) 0.3830(6) 0.0459(16) Uani 1 d . . . N31 N 0.3255(8) 0.3155(7) 0.2849(5) 0.0511(18) Uani 1 d . . . C36 C 0.4505(11) 0.3516(10) 0.2339(8) 0.060(2) Uani 1 d . . . H36 H 0.4699 0.3448 0.1657 0.072 Uiso 1 calc R . . C35 C 0.5500(13) 0.3981(11) 0.2800(9) 0.068(3) Uani 1 d . . . H35 H 0.6368 0.4186 0.2453 0.082 Uiso 1 calc R . . C34 C 0.5108(12) 0.4122(11) 0.3838(7) 0.054(2) Uani 1 d . . . H34 H 0.5696 0.4492 0.4173 0.065 Uiso 1 calc R . . C33 C 0.3949(13) 0.3741(12) 0.4316(8) 0.064(2) Uani 1 d . . . H33 H 0.3755 0.3766 0.5003 0.076 Uiso 1 calc R . . N27 N -0.0554(13) 0.3174(11) 0.6643(6) 0.068(2) Uani 1 d . . . H10A H -0.1350 0.2947 0.6945 0.082 Uiso 1 calc R . . H10B H -0.0069 0.3599 0.6939 0.082 Uiso 1 calc R . . O41 O 0.2273(8) -0.0874(7) 0.2316(5) 0.0579(15) Uani 1 d . . . N43 N 0.3281(9) -0.1121(8) 0.2917(5) 0.0545(17) Uani 1 d . . . O42 O 0.3481(8) 0.0026(8) 0.3160(5) 0.0583(15) Uani 1 d . . . O44 O 0.3929(10) -0.2381(8) 0.3245(6) 0.079(2) Uani 1 d . . . N53 N -0.0954(10) 0.4890(10) 0.1703(7) 0.061(2) Uani 1 d . . . O52 O -0.0878(16) 0.3926(15) 0.1176(8) 0.110(4) Uani 1 d . . . O51 O -0.0071(9) 0.4500(8) 0.2369(5) 0.0656(17) Uani 1 d . . . O54 O -0.1814(12) 0.6102(12) 0.1612(13) 0.132(5) Uani 1 d . . . N63 N -0.2382(14) 0.2552(10) -0.0504(8) 0.074(3) Uani 1 d . . . O62 O -0.2595(10) 0.1395(8) 0.0017(6) 0.073(2) Uani 1 d . . . O61 O -0.3390(15) 0.3576(11) -0.0837(12) 0.116(4) Uani 1 d . . . O64 O -0.1064(15) 0.2674(13) -0.0765(8) 0.105(3) Uani 1 d . . . O100 O 0.2259(9) 0.3930(7) 0.0713(5) 0.0603(15) Uani 1 d . . . O200 O 0.1030(8) 0.1248(7) 0.0559(5) 0.0609(16) Uani 1 d . . . O300 O 0.4096(8) 0.1000(7) 0.1080(5) 0.0617(16) Uani 1 d . . . O400 O 0.4474(10) 0.1982(9) -0.0994(6) 0.076(2) Uani 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 Sm1 0.0457(3) 0.0385(3) 0.0394(3) -0.00316(17) -0.00496(18) -0.00937(19) N11 0.059(5) 0.050(4) 0.046(3) -0.006(3) -0.012(3) -0.013(3) C12 0.065(6) 0.090(7) 0.050(5) -0.018(5) -0.005(4) -0.028(5) C13 0.063(7) 0.073(6) 0.068(6) -0.012(5) -0.019(4) -0.033(5) C14 0.064(6) 0.057(5) 0.063(5) 0.002(4) -0.011(4) -0.024(4) C15 0.052(5) 0.059(5) 0.050(4) 0.001(4) -0.007(4) -0.014(4) C16 0.047(4) 0.039(4) 0.042(3) 0.001(3) -0.010(3) -0.007(3) C22 0.048(4) 0.037(3) 0.043(4) -0.004(3) -0.006(3) -0.006(3) N21 0.044(4) 0.040(3) 0.046(3) -0.005(2) -0.006(2) -0.012(3) C26 0.040(4) 0.051(4) 0.048(4) -0.009(3) -0.003(3) -0.011(3) N25 0.067(5) 0.045(4) 0.049(4) -0.008(3) -0.006(3) -0.017(3) C24 0.060(5) 0.048(4) 0.045(4) -0.010(3) -0.005(3) -0.008(4) N23 0.048(4) 0.056(4) 0.043(3) -0.010(3) -0.001(3) -0.010(3) C32 0.043(4) 0.038(4) 0.058(4) -0.013(3) -0.001(3) -0.011(3) N31 0.056(5) 0.043(4) 0.051(4) -0.002(3) -0.006(3) -0.010(3) C36 0.053(5) 0.050(5) 0.070(6) 0.005(4) 0.001(4) -0.013(4) C35 0.058(6) 0.053(5) 0.100(8) -0.001(5) -0.014(5) -0.030(4) C34 0.056(6) 0.053(5) 0.061(5) -0.010(4) -0.015(4) -0.021(4) C33 0.064(7) 0.069(6) 0.072(6) -0.016(4) -0.017(4) -0.030(5) N27 0.088(7) 0.076(6) 0.051(4) -0.021(4) 0.008(4) -0.038(5) O41 0.065(4) 0.051(3) 0.061(4) -0.004(3) -0.008(3) -0.021(3) N43 0.059(5) 0.048(4) 0.047(4) 0.000(3) -0.002(3) -0.005(3) O42 0.057(4) 0.060(4) 0.057(3) -0.003(3) -0.010(3) -0.015(3) O44 0.084(6) 0.051(4) 0.074(5) 0.011(3) 0.001(4) 0.012(4) N53 0.055(5) 0.057(5) 0.065(5) 0.009(4) -0.013(4) -0.013(4) O52 0.130(10) 0.145(10) 0.085(6) -0.014(6) -0.025(6) -0.079(8) O51 0.072(5) 0.059(4) 0.056(4) -0.006(3) -0.016(3) 0.002(3) O54 0.068(6) 0.074(6) 0.218(15) 0.035(7) -0.030(7) 0.014(5) N63 0.094(8) 0.047(4) 0.085(6) -0.005(4) -0.035(5) -0.015(4) O62 0.088(6) 0.052(4) 0.077(5) -0.004(3) -0.017(4) -0.013(3) O61 0.114(10) 0.057(5) 0.176(12) 0.001(6) -0.063(8) -0.005(5) O64 0.128(10) 0.110(8) 0.090(6) 0.031(5) -0.049(6) -0.063(7) O100 0.077(5) 0.047(3) 0.055(3) 0.003(2) -0.005(3) -0.020(3) O200 0.069(4) 0.055(3) 0.056(3) -0.012(3) -0.015(3) -0.006(3) O300 0.065(4) 0.057(4) 0.053(3) -0.002(3) 0.007(3) -0.008(3) O400 0.065(5) 0.064(4) 0.078(5) 0.004(3) 0.004(4) 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 Sm1 O200 2.417(6) . ? Sm1 O300 2.464(7) . ? Sm1 O100 2.465(6) . ? Sm1 N21 2.547(7) . ? Sm1 O41 2.547(7) . ? Sm1 N31 2.561(7) . ? Sm1 O42 2.569(7) . ? Sm1 N11 2.590(8) . ? Sm1 O51 2.591(7) . ? Sm1 O52 2.849(14) . ? N11 C12 1.336(13) . ? N11 C16 1.365(11) . ? C12 C13 1.403(16) . ? C13 C14 1.375(15) . ? C14 C15 1.378(14) . ? C15 C16 1.378(13) . ? C16 C22 1.486(11) . ? C22 N23 1.327(10) . ? C22 N21 1.347(11) . ? N21 C26 1.331(11) . ? C26 N25 1.317(11) . ? C26 C32 1.511(12) . ? N25 C24 1.364(13) . ? C24 N27 1.317(12) . ? C24 N23 1.364(12) . ? C32 N31 1.348(11) . ? C32 C33 1.368(12) . ? N31 C36 1.367(12) . ? C36 C35 1.395(16) . ? C35 C34 1.429(16) . ? C34 C33 1.288(15) . ? O41 N43 1.281(11) . ? N43 O44 1.216(11) . ? N43 O42 1.256(11) . ? N53 O54 1.204(13) . ? N53 O52 1.238(14) . ? N53 O51 1.252(12) . ? N63 O61 1.223(14) . ? N63 O62 1.242(14) . ? N63 O64 1.265(17) . ? 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 O200 Sm1 O300 75.6(3) . . ? O200 Sm1 O100 79.0(3) . . ? O300 Sm1 O100 70.1(2) . . ? O200 Sm1 N21 145.3(3) . . ? O300 Sm1 N21 133.4(2) . . ? O100 Sm1 N21 124.3(2) . . ? O200 Sm1 O41 73.8(2) . . ? O300 Sm1 O41 71.9(2) . . ? O100 Sm1 O41 137.6(2) . . ? N21 Sm1 O41 95.7(2) . . ? O200 Sm1 N31 150.6(2) . . ? O300 Sm1 N31 82.1(2) . . ? O100 Sm1 N31 75.6(2) . . ? N21 Sm1 N31 63.6(2) . . ? O41 Sm1 N31 117.0(2) . . ? O200 Sm1 O42 119.3(2) . . ? O300 Sm1 O42 68.8(2) . . ? O100 Sm1 O42 127.6(3) . . ? N21 Sm1 O42 69.5(2) . . ? O41 Sm1 O42 49.4(2) . . ? N31 Sm1 O42 67.9(2) . . ? O200 Sm1 N11 82.7(2) . . ? O300 Sm1 N11 140.4(2) . . ? O100 Sm1 N11 137.3(2) . . ? N21 Sm1 N11 62.8(2) . . ? O41 Sm1 N11 70.4(2) . . ? N31 Sm1 N11 126.3(2) . . ? O42 Sm1 N11 95.0(2) . . ? O200 Sm1 O51 109.9(2) . . ? O300 Sm1 O51 138.2(2) . . ? O100 Sm1 O51 70.5(2) . . ? N21 Sm1 O51 63.7(2) . . ? O41 Sm1 O51 149.9(3) . . ? N31 Sm1 O51 75.0(2) . . ? O42 Sm1 O51 129.6(2) . . ? N11 Sm1 O51 80.3(3) . . ? O200 Sm1 O52 65.1(3) . . ? O300 Sm1 O52 125.1(3) . . ? O100 Sm1 O52 66.1(3) . . ? N21 Sm1 O52 98.9(3) . . ? O41 Sm1 O52 126.2(3) . . ? N31 Sm1 O52 115.9(3) . . ? O42 Sm1 O52 165.3(3) . . ? N11 Sm1 O52 71.2(3) . . ? O51 Sm1 O52 45.0(3) . . ? C12 N11 C16 116.0(8) . . ? C12 N11 Sm1 121.6(6) . . ? C16 N11 Sm1 122.3(5) . . ? N11 C12 C13 123.2(9) . . ? C14 C13 C12 119.4(9) . . ? C13 C14 C15 118.5(10) . . ? C14 C15 C16 119.1(9) . . ? N11 C16 C15 123.8(8) . . ? N11 C16 C22 114.4(7) . . ? C15 C16 C22 121.7(7) . . ? N23 C22 N21 125.4(8) . . ? N23 C22 C16 117.0(8) . . ? N21 C22 C16 117.6(7) . . ? C26 N21 C22 114.8(7) . . ? C26 N21 Sm1 122.0(5) . . ? C22 N21 Sm1 122.8(5) . . ? N25 C26 N21 126.5(8) . . ? N25 C26 C32 116.8(7) . . ? N21 C26 C32 116.7(7) . . ? C26 N25 C24 114.5(7) . . ? N27 C24 N23 117.7(9) . . ? N27 C24 N25 118.0(9) . . ? N23 C24 N25 124.3(7) . . ? C22 N23 C24 114.5(8) . . ? N31 C32 C33 122.6(8) . . ? N31 C32 C26 115.0(7) . . ? C33 C32 C26 122.3(8) . . ? C32 N31 C36 116.7(8) . . ? C32 N31 Sm1 121.7(5) . . ? C36 N31 Sm1 121.1(6) . . ? N31 C36 C35 122.7(10) . . ? C36 C35 C34 116.0(10) . . ? C33 C34 C35 120.6(9) . . ? C34 C33 C32 121.1(10) . . ? N43 O41 Sm1 98.0(5) . . ? O44 N43 O42 124.0(8) . . ? O44 N43 O41 121.2(8) . . ? O42 N43 O41 114.7(7) . . ? N43 O42 Sm1 97.7(5) . . ? O54 N53 O52 124.1(13) . . ? O54 N53 O51 121.3(12) . . ? O52 N53 O51 114.6(10) . . ? N53 O52 Sm1 93.6(8) . . ? N53 O51 Sm1 106.2(6) . . ? O61 N63 O62 123.3(14) . . ? O61 N63 O64 116.8(12) . . ? O62 N63 O64 119.8(10) . . ? _refine_diff_density_max 1.263 _refine_diff_density_min -1.619 _refine_diff_density_rms 0.193 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., (1983) Acta Cryst A39 158. ; #===END _data 4-eu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4-Eu _chemical_formula_moiety [EuL4(NO3)2(H2O)2](NO3)2H2O _chemical_formula_sum 'C13 H18 Eu N9 O13' _chemical_formula_weight 660.32 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.789(9) _cell_length_b 11.256(13) _cell_length_c 23.39(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(1) _cell_angle_gamma 90.00 _cell_volume 2314(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 25.95 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 2.793 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6372 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.95 _reflns_number_total 3650 _reflns_number_gt 2901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was used and refined to 0.45(1) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+2.1165P] 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 SHELXL _refine_ls_extinction_coef 0.0091(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3650 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.75843(5) 0.74553(3) 0.624166(18) 0.0337(2) Uani 1 d . . . O100 O 0.9414(11) 0.7274(6) 0.6985(3) 0.0573(18) Uani 1 d . . . O200 O 0.5859(10) 0.7619(5) 0.7012(3) 0.058(2) Uani 1 d . . . N43 N 0.6904(11) 0.9999(8) 0.6313(4) 0.062(2) Uani 1 d . . . O41 O 0.7910(9) 0.9530(6) 0.6610(3) 0.061(2) Uani 1 d . . . O42 O 0.6207(8) 0.9297(6) 0.5975(3) 0.0615(18) Uani 1 d . . . O44 O 0.6626(13) 1.1049(6) 0.6320(4) 0.105(3) Uani 1 d . . . O51 O 0.9010(8) 0.5653(6) 0.5953(3) 0.0597(18) Uani 1 d . . . N53 N 0.8299(10) 0.4893(7) 0.6266(4) 0.061(2) Uani 1 d . . . O52 O 0.7249(9) 0.5339(6) 0.6566(3) 0.0553(19) Uani 1 d . . . O54 O 0.8630(11) 0.3852(6) 0.6264(4) 0.090(2) Uani 1 d . . . N11 N 0.9950(7) 0.8335(7) 0.5744(3) 0.0455(18) Uani 1 d . . . C16 C 1.0066(9) 0.8342(8) 0.5164(4) 0.046(2) Uani 1 d . . . C15 C 1.1349(11) 0.8753(7) 0.4895(4) 0.052(2) Uani 1 d . . . H15 H 1.1398 0.8745 0.4498 0.062 Uiso 1 calc R . . C14 C 1.2559(16) 0.9175(9) 0.5202(5) 0.058(3) Uani 1 d . . . H14 H 1.3413 0.9484 0.5021 0.070 Uiso 1 calc R . . C13 C 1.2466(14) 0.9126(9) 0.5797(5) 0.056(3) Uani 1 d . . . H13 H 1.3290 0.9355 0.6020 0.067 Uiso 1 calc R . . C12 C 1.1144(11) 0.8736(8) 0.6051(4) 0.054(2) Uani 1 d . . . H12 H 1.1072 0.8749 0.6447 0.065 Uiso 1 calc R . . N21 N 0.7556(10) 0.7503(4) 0.5160(3) 0.0342(17) Uani 1 d . . . C22 C 0.8725(10) 0.7908(8) 0.4846(3) 0.0390(18) Uani 1 d . . . N23 N 0.8775(10) 0.7937(7) 0.4288(3) 0.0509(18) Uani 1 d . . . C24 C 0.752(3) 0.7542(6) 0.4006(4) 0.044(2) Uani 1 d . . . N25 N 0.6267(10) 0.7132(7) 0.4288(3) 0.0466(17) Uani 1 d . . . C26 C 0.6329(11) 0.7125(8) 0.4843(3) 0.0399(18) Uani 1 d . . . N31 N 0.5171(8) 0.6632(7) 0.5745(3) 0.0474(18) Uani 1 d . . . C32 C 0.5018(9) 0.6655(8) 0.5176(4) 0.044(2) Uani 1 d . . . C33 C 0.3723(11) 0.6284(7) 0.4898(4) 0.048(2) Uani 1 d . . . H33 H 0.3651 0.6336 0.4503 0.058 Uiso 1 calc R . . C34 C 0.2530(17) 0.5832(9) 0.5217(5) 0.059(3) Uani 1 d . . . H34 H 0.1652 0.5552 0.5041 0.070 Uiso 1 calc R . . C35 C 0.2681(13) 0.5810(9) 0.5806(5) 0.056(3) Uani 1 d . . . H35 H 0.1885 0.5549 0.6035 0.067 Uiso 1 calc R . . C36 C 0.4009(10) 0.6174(8) 0.6042(4) 0.047(2) Uani 1 d . . . H36 H 0.4120 0.6101 0.6436 0.057 Uiso 1 calc R . . N27 N 0.749(3) 0.7541(6) 0.3454(4) 0.062(3) Uiso 1 d . . . H27A H 0.6695 0.7287 0.3276 0.074 Uiso 1 calc R . . H27B H 0.8259 0.7795 0.3264 0.074 Uiso 1 calc R . . N63 N 0.6444(10) 1.0107(8) 0.2494(4) 0.0582(19) Uani 1 d . . . O61 O 0.6895(12) 0.9260(9) 0.2210(4) 0.098(4) Uani 1 d . . . O62 O 0.7314(15) 1.0810(10) 0.2700(4) 0.114(4) Uani 1 d . . . O64 O 0.5074(10) 1.0257(9) 0.2515(5) 0.102(3) Uani 1 d . . . O502 O 0.9311(10) 0.8216(8) 0.8018(3) 0.085(2) Uani 1 d . . . O503 O 1.0063(10) 1.0981(8) 0.7237(4) 0.092(3) Uani 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 Eu1 0.0322(3) 0.0383(3) 0.0305(3) -0.00114(16) 0.0000(3) 0.00052(14) O100 0.060(5) 0.064(4) 0.048(4) -0.003(3) -0.012(3) 0.011(4) O200 0.058(6) 0.061(5) 0.056(5) 0.001(3) 0.026(4) 0.007(3) N43 0.074(6) 0.048(5) 0.065(6) 0.001(5) 0.019(5) -0.004(4) O41 0.060(6) 0.052(4) 0.072(5) -0.018(3) -0.002(4) -0.003(4) O42 0.058(5) 0.065(5) 0.062(4) 0.007(3) 0.001(3) 0.015(4) O44 0.154(9) 0.037(4) 0.125(7) -0.002(5) 0.027(7) 0.023(5) O51 0.053(4) 0.063(5) 0.063(4) -0.011(3) 0.005(3) 0.009(3) N53 0.072(6) 0.040(5) 0.071(5) -0.017(5) -0.009(5) -0.001(4) O52 0.056(5) 0.045(4) 0.065(4) 0.013(3) 0.005(3) 0.004(3) O54 0.123(7) 0.046(4) 0.102(6) -0.005(4) -0.020(6) 0.013(4) N11 0.033(4) 0.051(5) 0.053(5) -0.004(3) -0.001(3) 0.003(3) C16 0.044(5) 0.043(5) 0.051(6) 0.008(4) 0.004(4) 0.001(4) C15 0.054(6) 0.041(5) 0.061(6) 0.007(4) 0.011(4) 0.008(4) C14 0.040(7) 0.060(6) 0.075(7) 0.019(5) 0.000(5) 0.008(5) C13 0.045(7) 0.055(6) 0.067(7) -0.007(5) -0.005(5) 0.001(5) C12 0.054(6) 0.045(5) 0.064(6) 0.003(4) -0.013(4) -0.001(4) N21 0.032(5) 0.032(4) 0.038(4) 0.000(2) -0.003(3) -0.006(2) C22 0.040(5) 0.030(4) 0.047(5) 0.000(4) -0.003(4) 0.009(4) N23 0.054(5) 0.055(5) 0.044(4) -0.005(4) 0.009(3) 0.008(4) C24 0.044(7) 0.049(6) 0.037(4) 0.007(3) -0.002(5) -0.002(4) N25 0.055(5) 0.044(4) 0.041(4) 0.000(3) -0.007(3) -0.004(4) C26 0.046(5) 0.034(4) 0.040(4) -0.005(4) -0.003(4) 0.018(4) N31 0.032(4) 0.056(5) 0.054(5) -0.003(4) 0.002(3) 0.000(3) C32 0.038(5) 0.045(5) 0.050(6) -0.003(4) 0.001(3) 0.001(4) C33 0.055(6) 0.039(5) 0.050(5) -0.008(4) -0.008(4) 0.000(4) C34 0.049(8) 0.051(6) 0.076(7) -0.010(5) -0.015(5) -0.013(5) C35 0.030(6) 0.062(6) 0.076(7) 0.003(5) 0.006(5) -0.011(5) C36 0.034(5) 0.054(6) 0.054(5) 0.005(4) 0.004(4) 0.004(4) N63 0.043(5) 0.065(6) 0.066(5) 0.000(4) 0.001(4) -0.001(4) O61 0.114(11) 0.089(6) 0.092(6) -0.018(5) 0.032(6) 0.026(6) O62 0.112(10) 0.125(8) 0.105(8) -0.014(6) -0.039(6) -0.059(7) O64 0.059(6) 0.092(7) 0.155(8) -0.035(6) 0.001(5) 0.000(4) O502 0.111(7) 0.085(6) 0.059(5) -0.009(4) -0.011(4) 0.020(5) O503 0.082(7) 0.099(7) 0.097(6) -0.035(5) 0.008(4) -0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O200 2.363(7) . ? Eu1 O100 2.378(8) . ? Eu1 O42 2.480(7) . ? Eu1 O51 2.478(7) . ? Eu1 O41 2.506(7) . ? Eu1 O52 2.517(7) . ? Eu1 N21 2.532(7) . ? Eu1 N11 2.580(7) . ? Eu1 N31 2.590(7) . ? N43 O44 1.208(10) . ? N43 O41 1.242(12) . ? N43 O42 1.274(11) . ? O51 N53 1.286(11) . ? N53 O54 1.207(10) . ? N53 O52 1.264(11) . ? N11 C12 1.349(11) . ? N11 C16 1.361(10) . ? C16 C15 1.372(12) . ? C16 C22 1.477(12) . ? C15 C14 1.369(16) . ? C14 C13 1.395(15) . ? C13 C12 1.376(15) . ? N21 C22 1.343(11) . ? N21 C26 1.376(12) . ? C22 N23 1.306(10) . ? N23 C24 1.36(2) . ? C24 N27 1.293(15) . ? C24 N25 1.36(2) . ? N25 C26 1.300(10) . ? C26 C32 1.487(12) . ? N31 C32 1.339(10) . ? N31 C36 1.338(11) . ? C32 C33 1.375(12) . ? C33 C34 1.383(16) . ? C34 C35 1.385(15) . ? C35 C36 1.356(15) . ? N63 O62 1.202(12) . ? N63 O64 1.216(11) . ? N63 O61 1.228(11) . ? 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 O200 Eu1 O100 83.3(3) . . ? O200 Eu1 O42 79.2(2) . . ? O100 Eu1 O42 125.9(2) . . ? O200 Eu1 O51 126.6(2) . . ? O100 Eu1 O51 77.7(2) . . ? O42 Eu1 O51 149.6(2) . . ? O200 Eu1 O41 74.8(2) . . ? O100 Eu1 O41 75.6(2) . . ? O42 Eu1 O41 50.5(3) . . ? O51 Eu1 O41 143.0(3) . . ? O200 Eu1 O52 76.6(2) . . ? O100 Eu1 O52 77.1(2) . . ? O42 Eu1 O52 144.0(3) . . ? O51 Eu1 O52 50.7(2) . . ? O41 Eu1 O52 142.3(3) . . ? O200 Eu1 N21 139.0(3) . . ? O100 Eu1 N21 137.7(3) . . ? O42 Eu1 N21 74.1(2) . . ? O51 Eu1 N21 75.5(2) . . ? O41 Eu1 N21 109.0(2) . . ? O52 Eu1 N21 108.7(2) . . ? O200 Eu1 N11 146.2(3) . . ? O100 Eu1 N11 79.5(3) . . ? O42 Eu1 N11 87.7(2) . . ? O51 Eu1 N11 77.5(2) . . ? O41 Eu1 N11 72.9(2) . . ? O52 Eu1 N11 126.4(2) . . ? N21 Eu1 N11 63.2(2) . . ? O200 Eu1 N31 81.1(3) . . ? O100 Eu1 N31 148.4(3) . . ? O42 Eu1 N31 77.7(3) . . ? O51 Eu1 N31 90.0(2) . . ? O41 Eu1 N31 125.5(3) . . ? O52 Eu1 N31 72.6(2) . . ? N21 Eu1 N31 63.3(2) . . ? N11 Eu1 N31 126.5(2) . . ? O44 N43 O41 123.5(11) . . ? O44 N43 O42 121.3(11) . . ? O41 N43 O42 115.2(8) . . ? O44 N43 Eu1 177.6(8) . . ? O41 N43 Eu1 58.1(5) . . ? O42 N43 Eu1 57.1(5) . . ? N43 O41 Eu1 97.0(6) . . ? N43 O42 Eu1 97.3(6) . . ? N53 O51 Eu1 98.3(5) . . ? O54 N53 O52 124.3(10) . . ? O54 N53 O51 121.8(10) . . ? O52 N53 O51 113.9(7) . . ? O54 N53 Eu1 177.9(8) . . ? O52 N53 Eu1 57.8(4) . . ? O51 N53 Eu1 56.1(4) . . ? N53 O52 Eu1 97.1(5) . . ? C12 N11 C16 118.1(8) . . ? C12 N11 Eu1 121.0(6) . . ? C16 N11 Eu1 120.8(6) . . ? N11 C16 C15 121.4(8) . . ? N11 C16 C22 116.2(7) . . ? C15 C16 C22 122.4(8) . . ? C16 C15 C14 120.9(9) . . ? C15 C14 C13 117.7(11) . . ? C12 C13 C14 119.4(11) . . ? N11 C12 C13 122.3(9) . . ? C22 N21 C26 114.3(7) . . ? C22 N21 Eu1 123.1(6) . . ? C26 N21 Eu1 122.6(6) . . ? N23 C22 N21 125.5(8) . . ? N23 C22 C16 118.0(8) . . ? N21 C22 C16 116.6(7) . . ? C22 N23 C24 116.6(10) . . ? N27 C24 N25 118(3) . . ? N27 C24 N23 120(3) . . ? N25 C24 N23 122.1(8) . . ? C26 N25 C24 116.9(10) . . ? N25 C26 N21 124.6(9) . . ? N25 C26 C32 119.5(9) . . ? N21 C26 C32 115.9(7) . . ? C32 N31 C36 116.6(8) . . ? C32 N31 Eu1 121.4(5) . . ? C36 N31 Eu1 122.0(6) . . ? N31 C32 C33 123.2(8) . . ? N31 C32 C26 116.7(8) . . ? C33 C32 C26 120.1(8) . . ? C32 C33 C34 119.0(8) . . ? C35 C34 C33 118.0(11) . . ? C36 C35 C34 119.0(10) . . ? N31 C36 C35 124.1(8) . . ? O62 N63 O64 121.5(11) . . ? O62 N63 O61 121.5(11) . . ? O64 N63 O61 116.7(10) . . ? _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END _data_4_Gd _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 4-Gd _chemical_formula_moiety [GdL4(NO3)2(H2O)2][NO3],2H2O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 Gd N9 O13' _chemical_formula_weight 665.61 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.767(9) _cell_length_b 11.205(13) _cell_length_c 23.295(27) _cell_angle_alpha 90.00 _cell_angle_beta 90.456(10) _cell_angle_gamma 90.00 _cell_volume 2288.3(44) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method ? _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 2.982 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6376 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3710 _reflns_number_gt 2471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was not necessary in this structure ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1409P)^2^+1.3175P] 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 SHELXL _refine_ls_extinction_coef 0.0003(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3710 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.2326 _refine_ls_wR_factor_gt 0.1937 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.75809(5) 0.74739(4) 0.623178(16) 0.0393(3) Uani 1 d . . . O100 O 0.9368(11) 0.7303(7) 0.6972(3) 0.065(2) Uani 1 d . . . O200 O 0.5895(12) 0.7646(6) 0.6994(4) 0.067(2) Uani 1 d . . . N43 N 0.6893(15) 1.0002(11) 0.6299(5) 0.075(3) Uani 1 d . . . O41 O 0.7904(10) 0.9538(8) 0.6605(4) 0.066(2) Uani 1 d . . . O42 O 0.6212(9) 0.9281(8) 0.5965(3) 0.070(2) Uani 1 d . . . O44 O 0.6611(13) 1.1042(9) 0.6304(5) 0.105(3) Uani 1 d . . . O51 O 0.9016(8) 0.5710(8) 0.5948(3) 0.068(2) Uani 1 d . . . N53 N 0.8283(13) 0.4945(10) 0.6268(5) 0.070(3) Uani 1 d . . . O52 O 0.7244(9) 0.5384(7) 0.6559(4) 0.062(2) Uani 1 d . . . O54 O 0.8639(12) 0.3899(9) 0.6269(4) 0.100(3) Uani 1 d . . . N11 N 0.9941(9) 0.8330(8) 0.5758(3) 0.055(2) Uani 1 d . . . C16 C 1.0076(10) 0.8353(9) 0.5183(4) 0.050(2) Uani 1 d . . . C15 C 1.1379(12) 0.8749(10) 0.4905(5) 0.060(3) Uani 1 d . . . H15 H 1.1436 0.8733 0.4506 0.073 Uiso 1 calc R . . C14 C 1.2572(14) 0.9161(12) 0.5229(6) 0.066(3) Uani 1 d . . . H14 H 1.3454 0.9433 0.5052 0.079 Uiso 1 calc R . . C13 C 1.2462(13) 0.9171(12) 0.5820(6) 0.065(3) Uani 1 d . . . H13 H 1.3266 0.9446 0.6047 0.078 Uiso 1 calc R . . C12 C 1.1143(11) 0.8767(10) 0.6066(5) 0.061(3) Uani 1 d . . . H12 H 1.1066 0.8793 0.6463 0.074 Uiso 1 calc R . . N21 N 0.7550(10) 0.7501(6) 0.5176(4) 0.042(2) Uani 1 d . . . C22 C 0.8745(11) 0.7913(10) 0.4846(4) 0.048(2) Uani 1 d . . . N23 N 0.8783(10) 0.7928(9) 0.4288(4) 0.056(2) Uani 1 d . . . C24 C 0.7519(18) 0.7538(8) 0.3999(7) 0.056(3) Uani 1 d . . . N25 N 0.6240(11) 0.7120(10) 0.4296(4) 0.060(2) Uani 1 d . . . C26 C 0.6346(12) 0.7134(10) 0.4838(4) 0.047(2) Uani 1 d . . . N31 N 0.5181(8) 0.6645(8) 0.5752(3) 0.054(2) Uani 1 d . . . C32 C 0.5022(11) 0.6662(9) 0.5182(4) 0.053(3) Uani 1 d . . . C33 C 0.3709(11) 0.6280(10) 0.4902(5) 0.060(3) Uani 1 d . . . H33 H 0.3631 0.6323 0.4505 0.072 Uiso 1 calc R . . C34 C 0.2531(13) 0.5840(13) 0.5219(5) 0.065(3) Uani 1 d . . . H34 H 0.1640 0.5582 0.5038 0.078 Uiso 1 calc R . . C35 C 0.2672(12) 0.5780(11) 0.5804(5) 0.059(3) Uani 1 d . . . H35 H 0.1892 0.5471 0.6028 0.071 Uiso 1 calc R . . C36 C 0.4023(12) 0.6196(9) 0.6054(5) 0.061(3) Uani 1 d . . . H36 H 0.4123 0.6159 0.6451 0.073 Uiso 1 calc R . . N27 N 0.7516(16) 0.7532(8) 0.3452(5) 0.071(4) Uani 1 d . . . H27A H 0.8306 0.7773 0.3268 0.086 Uiso 1 calc R . . H27B H 0.6724 0.7287 0.3266 0.086 Uiso 1 calc R . . N63 N 0.6420(12) 1.0066(10) 0.2486(4) 0.073(3) Uani 1 d . . . O61 O 0.6852(12) 0.9220(11) 0.2198(5) 0.101(4) Uani 1 d . . . O62 O 0.7331(14) 1.0758(13) 0.2711(5) 0.126(5) Uani 1 d . . . O64 O 0.5045(12) 1.0228(11) 0.2528(6) 0.118(4) Uani 1 d . . . O502 O 0.9243(12) 0.8212(11) 0.8021(4) 0.106(3) Uani 1 d . . . O503 O 1.0042(11) 1.0992(10) 0.7253(4) 0.098(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0375(5) 0.0434(5) 0.0369(4) -0.00131(19) -0.0003(2) 0.00115(18) O100 0.070(6) 0.077(6) 0.050(4) -0.006(4) -0.021(4) 0.014(4) O200 0.080(7) 0.072(6) 0.050(5) -0.002(3) 0.011(4) -0.001(4) N43 0.104(9) 0.052(7) 0.068(7) -0.013(6) 0.011(6) -0.001(7) O41 0.066(6) 0.068(6) 0.065(5) -0.014(4) 0.003(4) -0.015(4) O42 0.072(5) 0.074(6) 0.065(5) 0.004(4) 0.001(4) 0.017(4) O44 0.132(9) 0.051(7) 0.132(9) -0.003(6) 0.042(7) 0.009(6) O51 0.064(5) 0.081(6) 0.060(5) -0.003(4) 0.009(4) 0.001(4) N53 0.081(8) 0.054(7) 0.075(7) -0.012(5) -0.012(5) 0.006(6) O52 0.065(5) 0.049(5) 0.070(5) 0.013(4) 0.009(4) 0.005(4) O54 0.113(8) 0.066(7) 0.120(8) -0.003(6) -0.011(6) 0.021(6) N11 0.045(5) 0.065(7) 0.054(5) -0.002(4) -0.003(4) 0.002(4) C16 0.046(5) 0.050(7) 0.054(6) 0.003(5) 0.006(4) 0.006(5) C15 0.050(7) 0.061(8) 0.070(7) 0.002(6) 0.007(5) 0.006(5) C14 0.046(8) 0.054(8) 0.097(10) 0.014(7) 0.019(6) 0.003(5) C13 0.040(7) 0.077(9) 0.077(8) -0.005(7) -0.003(5) -0.007(5) C12 0.050(6) 0.072(8) 0.061(7) -0.003(6) -0.007(5) 0.005(5) N21 0.039(5) 0.038(5) 0.049(5) 0.003(3) 0.002(3) 0.000(3) C22 0.045(6) 0.041(6) 0.058(6) -0.007(5) -0.001(4) 0.009(5) N23 0.056(5) 0.066(6) 0.045(5) -0.001(4) 0.009(4) 0.004(5) C24 0.062(10) 0.049(8) 0.058(8) -0.001(5) 0.000(6) 0.009(5) N25 0.060(6) 0.082(6) 0.038(5) 0.010(5) 0.000(4) -0.004(5) C26 0.051(6) 0.046(6) 0.045(6) 0.006(5) -0.001(4) 0.007(5) N31 0.044(5) 0.066(6) 0.053(5) -0.004(4) 0.003(3) 0.003(4) C32 0.049(6) 0.049(7) 0.062(7) -0.009(5) -0.004(4) 0.006(5) C33 0.045(6) 0.069(8) 0.067(7) -0.004(6) -0.007(5) -0.005(5) C34 0.048(7) 0.077(9) 0.071(8) -0.007(7) -0.016(5) -0.005(6) C35 0.036(6) 0.063(8) 0.077(8) -0.005(6) 0.000(5) -0.001(5) C36 0.058(7) 0.050(7) 0.074(7) 0.008(6) 0.010(5) -0.003(5) N27 0.063(9) 0.102(11) 0.049(6) -0.001(5) 0.009(5) -0.012(4) N63 0.062(7) 0.075(8) 0.083(7) -0.004(6) 0.001(5) -0.003(5) O61 0.098(8) 0.109(9) 0.098(7) -0.027(6) 0.022(6) 0.020(6) O62 0.124(10) 0.134(11) 0.120(9) -0.022(8) -0.040(7) -0.050(8) O64 0.073(7) 0.116(10) 0.166(10) -0.036(8) 0.014(6) 0.010(6) O502 0.130(8) 0.110(9) 0.079(6) -0.016(6) -0.012(5) 0.020(7) O503 0.083(6) 0.112(9) 0.100(7) -0.037(6) 0.011(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O100 2.328(8) . ? Gd1 O200 2.328(9) . ? Gd1 O42 2.433(8) . ? Gd1 O51 2.438(8) . ? Gd1 N21 2.460(9) . ? Gd1 O52 2.480(8) . ? Gd1 O41 2.486(9) . ? Gd1 N11 2.541(8) . ? Gd1 N31 2.549(8) . ? N43 O44 1.191(14) . ? N43 O41 1.247(15) . ? N43 O42 1.268(13) . ? O51 N53 1.308(12) . ? N53 O54 1.213(13) . ? N53 O52 1.242(13) . ? N11 C16 1.344(12) . ? N11 C12 1.362(12) . ? C16 C15 1.391(13) . ? C16 C22 1.486(14) . ? C15 C14 1.366(17) . ? C14 C13 1.383(18) . ? C13 C12 1.370(15) . ? N21 C26 1.374(14) . ? N21 C22 1.382(13) . ? C22 N23 1.302(13) . ? N23 C24 1.364(18) . ? C24 N27 1.27(2) . ? C24 N25 1.404(17) . ? N25 C26 1.266(13) . ? C26 C32 1.511(14) . ? N31 C32 1.336(12) . ? N31 C36 1.338(12) . ? C32 C33 1.386(14) . ? C33 C34 1.365(16) . ? C34 C35 1.370(17) . ? C35 C36 1.396(15) . ? N63 O61 1.223(13) . ? N63 O64 1.223(13) . ? N63 O62 1.229(13) . ? 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 O100 Gd1 O200 82.5(3) . . ? O100 Gd1 O42 125.8(3) . . ? O200 Gd1 O42 79.1(3) . . ? O100 Gd1 O51 77.8(3) . . ? O200 Gd1 O51 127.4(3) . . ? O42 Gd1 O51 149.3(3) . . ? O100 Gd1 N21 138.0(3) . . ? O200 Gd1 N21 139.5(3) . . ? O42 Gd1 N21 74.5(2) . . ? O51 Gd1 N21 74.9(2) . . ? O100 Gd1 O52 77.1(3) . . ? O200 Gd1 O52 76.5(3) . . ? O42 Gd1 O52 143.6(3) . . ? O51 Gd1 O52 51.8(3) . . ? N21 Gd1 O52 108.6(3) . . ? O100 Gd1 O41 75.1(3) . . ? O200 Gd1 O41 74.2(3) . . ? O42 Gd1 O41 50.9(3) . . ? O51 Gd1 O41 142.3(3) . . ? N21 Gd1 O41 109.7(3) . . ? O52 Gd1 O41 141.7(3) . . ? O100 Gd1 N11 78.9(3) . . ? O200 Gd1 N11 145.5(3) . . ? O42 Gd1 N11 88.6(3) . . ? O51 Gd1 N11 76.4(3) . . ? N21 Gd1 N11 64.1(3) . . ? O52 Gd1 N11 126.1(3) . . ? O41 Gd1 N11 73.1(3) . . ? O100 Gd1 N31 147.4(3) . . ? O200 Gd1 N31 80.7(3) . . ? O42 Gd1 N31 77.7(3) . . ? O51 Gd1 N31 90.7(3) . . ? N21 Gd1 N31 64.2(3) . . ? O52 Gd1 N31 72.0(3) . . ? O41 Gd1 N31 125.7(3) . . ? N11 Gd1 N31 128.2(3) . . ? O44 N43 O41 123.4(13) . . ? O44 N43 O42 122.2(13) . . ? O41 N43 O42 114.4(11) . . ? O44 N43 Gd1 177.4(9) . . ? O41 N43 Gd1 58.4(6) . . ? O42 N43 Gd1 56.1(6) . . ? N43 O41 Gd1 96.3(7) . . ? N43 O42 Gd1 98.3(7) . . ? N53 O51 Gd1 96.9(6) . . ? O54 N53 O52 124.8(12) . . ? O54 N53 O51 120.5(12) . . ? O52 N53 O51 114.7(10) . . ? O54 N53 Gd1 177.0(10) . . ? O52 N53 Gd1 58.1(6) . . ? O51 N53 Gd1 56.6(5) . . ? N53 O52 Gd1 96.7(7) . . ? C16 N11 C12 116.4(8) . . ? C16 N11 Gd1 121.2(6) . . ? C12 N11 Gd1 122.4(7) . . ? N11 C16 C15 123.3(9) . . ? N11 C16 C22 116.4(8) . . ? C15 C16 C22 120.3(9) . . ? C14 C15 C16 118.6(11) . . ? C15 C14 C13 119.6(10) . . ? C12 C13 C14 118.6(11) . . ? N11 C12 C13 123.4(10) . . ? C26 N21 C22 111.4(9) . . ? C26 N21 Gd1 124.8(6) . . ? C22 N21 Gd1 123.9(7) . . ? N23 C22 N21 125.8(9) . . ? N23 C22 C16 119.8(9) . . ? N21 C22 C16 114.4(9) . . ? C22 N23 C24 117.5(10) . . ? N27 C24 N23 119.4(15) . . ? N27 C24 N25 119.8(16) . . ? N23 C24 N25 120.8(12) . . ? C26 N25 C24 115.8(11) . . ? N25 C26 N21 128.6(10) . . ? N25 C26 C32 118.2(10) . . ? N21 C26 C32 113.1(9) . . ? C32 N31 C36 117.0(9) . . ? C32 N31 Gd1 120.7(6) . . ? C36 N31 Gd1 122.3(7) . . ? N31 C32 C33 122.9(10) . . ? N31 C32 C26 117.2(9) . . ? C33 C32 C26 119.9(10) . . ? C34 C33 C32 119.2(11) . . ? C33 C34 C35 119.5(11) . . ? C34 C35 C36 117.9(11) . . ? N31 C36 C35 123.5(11) . . ? O61 N63 O64 118.0(12) . . ? O61 N63 O62 121.3(13) . . ? O64 N63 O62 120.6(13) . . ? _refine_diff_density_max 2.343 _refine_diff_density_min -2.278 _refine_diff_density_rms 0.195 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END _data_4-tb _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 4-tb _chemical_formula_moiety [Tb(L4)(NO3)2(H2O)2](NO3)2(H2O) _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 N9 O13 Tb' _chemical_formula_weight 667.28 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.777(9) _cell_length_b 11.223(13) _cell_length_c 23.336(27) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(1) _cell_angle_gamma 90.00 _cell_volume 2298.7(44) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.90 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method ? _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 3.160 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7614 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.13 _reflns_number_total 4019 _reflns_number_observed 3473 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was used and refined to 0.44(1) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1405P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4019 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_all 0.1928 _refine_ls_wR_factor_obs 0.1798 _refine_ls_goodness_of_fit_all 1.152 _refine_ls_goodness_of_fit_obs 1.160 _refine_ls_restrained_S_all 1.152 _refine_ls_restrained_S_obs 1.160 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tb1 Tb 0.75815(6) 0.74602(3) 0.62360(2) 0.0278(2) Uani 1 d . . O100 O 0.9413(14) 0.7296(6) 0.6968(4) 0.048(2) Uani 1 d . . O200 O 0.5875(12) 0.7620(6) 0.7002(4) 0.043(2) Uani 1 d . . N43 N 0.6910(12) 0.9985(8) 0.6311(5) 0.055(3) Uani 1 d . . O41 O 0.7925(8) 0.9505(6) 0.6613(3) 0.042(2) Uani 1 d . . O42 O 0.6192(9) 0.9279(6) 0.5962(3) 0.047(2) Uani 1 d . . O44 O 0.6584(13) 1.1030(6) 0.6310(4) 0.083(3) Uani 1 d . . O51 O 0.8994(8) 0.5686(6) 0.5956(3) 0.044(2) Uani 1 d . . N53 N 0.8284(10) 0.4921(7) 0.6259(5) 0.051(2) Uani 1 d . . O52 O 0.7282(11) 0.5362(6) 0.6565(4) 0.049(2) Uani 1 d . . O54 O 0.8619(11) 0.3899(6) 0.6254(4) 0.073(2) Uani 1 d . . N11 N 0.9972(8) 0.8331(7) 0.5752(3) 0.034(2) Uani 1 d . . C16 C 1.0066(10) 0.8318(8) 0.5170(4) 0.035(2) Uani 1 d . . C15 C 1.1387(12) 0.8738(9) 0.4917(5) 0.049(3) Uani 1 d . . H15 H 1.1448(12) 0.8727(9) 0.4520(5) 0.059 Uiso 1 calc R . C14 C 1.2595(17) 0.9164(10) 0.5213(6) 0.050(3) Uani 1 d . . H14 H 1.3463(17) 0.9447(10) 0.5029(6) 0.060 Uiso 1 calc R . C13 C 1.2466(15) 0.9153(10) 0.5821(5) 0.045(3) Uani 1 d . . H13 H 1.3252(15) 0.9438(10) 0.6050(5) 0.054 Uiso 1 calc R . C12 C 1.1201(11) 0.8729(7) 0.6053(4) 0.039(2) Uani 1 d . . H12 H 1.1146(11) 0.8700(7) 0.6451(4) 0.046 Uiso 1 calc R . N21 N 0.7576(13) 0.7489(5) 0.5158(4) 0.031(2) Uani 1 d . . C22 C 0.8725(11) 0.7907(10) 0.4852(4) 0.035(2) Uani 1 d . . N23 N 0.8762(11) 0.7944(9) 0.4294(4) 0.046(2) Uani 1 d . . C24 C 0.7509(39) 0.7554(8) 0.4010(5) 0.039(3) Uani 1 d . . N25 N 0.6292(10) 0.7122(8) 0.4292(4) 0.039(2) Uani 1 d . . C26 C 0.6367(10) 0.7135(8) 0.4850(3) 0.027(2) Uani 1 d . . N31 N 0.5175(9) 0.6633(7) 0.5754(3) 0.038(2) Uani 1 d . . C32 C 0.5012(11) 0.6665(7) 0.5172(4) 0.037(2) Uani 1 d . . C33 C 0.3699(13) 0.6289(9) 0.4899(4) 0.045(2) Uani 1 d . . H33 H 0.3616(13) 0.6341(9) 0.4502(4) 0.054 Uiso 1 calc R . C34 C 0.2551(16) 0.5848(11) 0.5211(5) 0.046(3) Uani 1 d . . H34 H 0.1664(16) 0.5586(11) 0.5034(5) 0.056 Uiso 1 calc R . C35 C 0.2692(16) 0.5788(13) 0.5795(5) 0.053(3) Uani 1 d . . H35 H 0.1898(16) 0.5495(13) 0.6018(5) 0.063 Uiso 1 calc R . C36 C 0.4044(13) 0.6174(10) 0.6053(5) 0.051(3) Uani 1 d . . H36 H 0.4148(13) 0.6103(10) 0.6448(5) 0.061 Uiso 1 calc R . N27 N 0.7554(46) 0.7537(7) 0.3445(5) 0.067(5) Uani 1 d . . H27A H 0.6802(46) 0.7248(7) 0.3254(5) 0.080 Uiso 1 calc R . H27B H 0.8336(46) 0.7815(7) 0.3267(5) 0.080 Uiso 1 calc R . N63 N 0.6407(11) 1.0105(8) 0.2487(4) 0.052(2) Uani 1 d . . O61 O 0.6845(13) 0.9234(10) 0.2200(5) 0.078(3) Uani 1 d . . O62 O 0.7347(14) 1.0798(10) 0.2690(5) 0.091(4) Uani 1 d . . O64 O 0.5037(11) 1.0213(10) 0.2525(6) 0.096(3) Uani 1 d . . O502 O 0.9287(12) 0.8206(9) 0.8021(3) 0.075(3) Uani 1 d . . O503 O 1.0030(11) 1.1011(10) 0.7235(4) 0.082(3) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0270(4) 0.0287(3) 0.0275(3) -0.00137(15) 0.0016(4) 0.00071(13) O100 0.050(7) 0.045(4) 0.048(5) 0.003(3) -0.001(4) 0.026(4) O200 0.033(6) 0.061(5) 0.035(5) -0.002(3) 0.011(4) -0.008(3) N43 0.057(7) 0.026(4) 0.082(7) 0.005(5) 0.035(6) 0.022(4) O41 0.022(5) 0.023(3) 0.080(5) -0.014(3) 0.008(3) -0.003(3) O42 0.049(5) 0.019(4) 0.074(5) 0.002(3) 0.002(4) 0.015(3) O44 0.110(8) 0.021(4) 0.118(7) 0.006(4) 0.028(6) 0.032(4) O51 0.043(5) 0.039(4) 0.052(4) -0.003(3) 0.005(3) 0.007(3) N53 0.053(6) 0.019(4) 0.081(6) -0.004(5) -0.014(5) 0.023(4) O52 0.047(6) 0.025(4) 0.075(5) 0.006(3) 0.004(4) -0.013(3) O54 0.076(6) 0.031(4) 0.113(7) -0.003(5) -0.007(6) 0.012(4) N11 0.031(5) 0.023(4) 0.049(5) 0.002(3) 0.005(3) 0.006(3) C16 0.031(6) 0.027(5) 0.047(6) 0.006(4) 0.006(4) 0.007(3) C15 0.025(6) 0.044(6) 0.079(7) 0.019(5) 0.015(5) -0.011(4) C14 0.028(8) 0.038(6) 0.084(9) 0.017(5) 0.008(6) 0.002(5) C13 0.021(7) 0.041(6) 0.074(7) -0.011(5) -0.013(5) -0.023(5) C12 0.037(6) 0.017(4) 0.062(6) -0.006(4) -0.003(4) -0.008(4) N21 0.023(7) 0.037(5) 0.035(4) 0.000(2) 0.000(4) 0.011(3) C22 0.022(5) 0.036(5) 0.048(6) 0.000(4) 0.002(4) 0.005(4) N23 0.047(6) 0.052(5) 0.040(5) -0.001(4) 0.008(4) 0.006(5) C24 0.040(9) 0.052(7) 0.026(6) 0.005(3) 0.000(8) 0.011(4) N25 0.035(5) 0.027(4) 0.053(5) 0.001(4) -0.009(4) 0.001(4) C26 0.024(5) 0.028(4) 0.027(5) 0.000(4) -0.004(3) 0.001(4) N31 0.042(5) 0.029(4) 0.043(5) 0.001(3) 0.006(3) -0.003(3) C32 0.044(6) 0.014(4) 0.053(6) -0.007(4) -0.004(4) 0.000(3) C33 0.054(7) 0.044(6) 0.039(5) -0.005(4) -0.005(5) 0.007(5) C34 0.021(7) 0.051(6) 0.068(8) -0.011(5) -0.005(5) -0.021(5) C35 0.019(7) 0.085(9) 0.053(7) -0.004(6) 0.002(5) 0.010(6) C36 0.039(7) 0.067(8) 0.046(6) 0.009(5) 0.004(4) 0.002(5) N27 0.082(13) 0.094(10) 0.024(5) -0.006(4) 0.003(11) -0.015(5) N63 0.031(6) 0.053(6) 0.072(6) 0.005(5) -0.004(4) 0.003(4) O61 0.061(8) 0.075(7) 0.100(7) -0.012(5) 0.024(5) 0.031(5) O62 0.064(9) 0.077(7) 0.131(9) -0.017(6) -0.007(7) -0.029(6) O64 0.043(7) 0.082(8) 0.164(10) -0.046(7) 0.000(6) 0.009(5) O502 0.089(7) 0.078(7) 0.059(5) -0.008(4) -0.008(4) 0.028(6) O503 0.060(7) 0.085(8) 0.102(7) -0.040(6) 0.013(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O200 2.336(8) . ? Tb1 O100 2.354(11) . ? Tb1 O42 2.463(7) . ? Tb1 O51 2.432(7) . ? Tb1 O41 2.475(7) . ? Tb1 O52 2.492(7) . ? Tb1 N21 2.515(9) . ? Tb1 N11 2.575(7) . ? Tb1 N31 2.569(9) . ? N43 O44 1.206(10) . ? N43 O42 1.300(13) . ? N43 O41 1.258(13) . ? O51 N53 1.275(11) . ? N53 O54 1.184(10) . ? N53 O52 1.236(12) . ? N11 C16 1.359(11) . ? N11 C12 1.364(12) . ? C16 C15 1.383(12) . ? C16 C22 1.467(14) . ? C15 C14 1.35(2) . ? C14 C13 1.42(2) . ? C13 C12 1.32(2) . ? N21 C26 1.343(14) . ? N21 C22 1.321(14) . ? C22 N23 1.305(12) . ? N23 C24 1.36(3) . ? C24 N27 1.32(2) . ? C24 N25 1.34(3) . ? N25 C26 1.304(12) . ? C26 C32 1.501(13) . ? N31 C36 1.317(13) . ? N31 C32 1.367(12) . ? C32 C33 1.384(14) . ? C33 C34 1.34(2) . ? C34 C35 1.37(2) . ? C35 C36 1.40(2) . ? N63 O61 1.245(13) . ? N63 O64 1.211(13) . ? N63 O62 1.229(13) . ? 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 O200 Tb1 O100 83.6(3) . . ? O200 Tb1 O42 79.6(3) . . ? O100 Tb1 O42 126.3(2) . . ? O200 Tb1 O51 126.3(2) . . ? O100 Tb1 O51 77.4(2) . . ? O42 Tb1 O51 149.3(2) . . ? O200 Tb1 O41 74.7(2) . . ? O100 Tb1 O41 74.4(3) . . ? O42 Tb1 O41 52.1(3) . . ? O51 Tb1 O41 142.3(3) . . ? O200 Tb1 O52 76.6(3) . . ? O100 Tb1 O52 76.9(3) . . ? O42 Tb1 O52 144.2(3) . . ? O51 Tb1 O52 50.5(3) . . ? O41 Tb1 O52 141.2(3) . . ? O200 Tb1 N21 139.6(4) . . ? O100 Tb1 N21 136.8(4) . . ? O42 Tb1 N21 74.1(2) . . ? O51 Tb1 N21 75.2(2) . . ? O41 Tb1 N21 110.0(2) . . ? O52 Tb1 N21 108.7(2) . . ? O200 Tb1 N11 145.8(3) . . ? O100 Tb1 N11 78.0(3) . . ? O42 Tb1 N11 88.5(3) . . ? O51 Tb1 N11 77.2(2) . . ? O41 Tb1 N11 72.7(2) . . ? O52 Tb1 N11 125.5(3) . . ? N21 Tb1 N11 63.8(3) . . ? O200 Tb1 N31 80.6(3) . . ? O100 Tb1 N31 148.5(3) . . ? O42 Tb1 N31 77.2(3) . . ? O51 Tb1 N31 90.3(3) . . ? O41 Tb1 N31 126.3(3) . . ? O52 Tb1 N31 72.9(3) . . ? N21 Tb1 N31 64.1(3) . . ? N11 Tb1 N31 128.0(2) . . ? O44 N43 O42 118.5(11) . . ? O44 N43 O41 125.8(12) . . ? O42 N43 O41 115.7(8) . . ? N43 O41 Tb1 96.4(6) . . ? N43 O42 Tb1 95.8(6) . . ? N53 O51 Tb1 98.9(5) . . ? O54 N53 O52 124.7(11) . . ? O54 N53 O51 121.8(10) . . ? O52 N53 O51 113.5(7) . . ? N53 O52 Tb1 97.1(6) . . ? C16 N11 C12 118.1(8) . . ? C16 N11 Tb1 118.8(6) . . ? C12 N11 Tb1 122.9(6) . . ? N11 C16 C15 118.2(9) . . ? N11 C16 C22 117.4(8) . . ? C15 C16 C22 124.3(9) . . ? C16 C15 C14 124.0(11) . . ? C13 C14 C15 116.3(12) . . ? C12 C13 C14 118.5(11) . . ? C13 C12 N11 124.8(10) . . ? C26 N21 C22 114.8(8) . . ? C26 N21 Tb1 122.3(7) . . ? C22 N21 Tb1 122.8(8) . . ? N23 C22 N21 124.7(10) . . ? N23 C22 C16 118.5(9) . . ? N21 C22 C16 116.8(9) . . ? C22 N23 C24 117.2(12) . . ? N27 C24 N25 120.5(35) . . ? N27 C24 N23 117.9(37) . . ? N25 C24 N23 121.5(10) . . ? C26 N25 C24 116.3(11) . . ? N25 C26 N21 125.4(9) . . ? N25 C26 C32 117.0(8) . . ? N21 C26 C32 117.6(8) . . ? C36 N31 C32 117.2(9) . . ? C36 N31 Tb1 121.9(7) . . ? C32 N31 Tb1 120.8(6) . . ? N31 C32 C33 122.5(9) . . ? N31 C32 C26 115.0(8) . . ? C33 C32 C26 122.5(8) . . ? C34 C33 C32 119.3(9) . . ? C33 C34 C35 119.4(12) . . ? C34 C35 C36 119.4(12) . . ? N31 C36 C35 122.1(10) . . ? O61 N63 O64 115.0(11) . . ? O61 N63 O62 119.8(12) . . ? O64 N63 O62 125.2(12) . . ? _refine_diff_density_max 1.204 _refine_diff_density_min -1.878 _refine_diff_density_rms 0.145 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_4-Dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Dy(L4)(NO3)2(H2O)2, NO3, 2H2O _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 Dy N9 O13' _chemical_formula_weight 670.86 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.780(9) _cell_length_b 11.219(13) _cell_length_c 23.33(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.306(10) _cell_angle_gamma 90.00 _cell_volume 2298(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.97 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 3.335 _exptl_absorpt_correction_type n/a _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5336 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.97 _reflns_number_total 3257 _reflns_number_gt 2363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was used and refined to 0.31(1) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+8.2208P] 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 SHELXL _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3257 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.75776(7) 0.74735(6) 0.62331(2) 0.0371(3) Uani 1 d . . . O100 O 0.9359(14) 0.7300(9) 0.6972(4) 0.057(3) Uani 1 d . . . O200 O 0.5882(11) 0.7666(9) 0.6998(4) 0.054(3) Uani 1 d . . . N43 N 0.6891(18) 0.9976(14) 0.6295(6) 0.059(4) Uani 1 d . . . O41 O 0.7937(14) 0.9513(10) 0.6616(5) 0.062(3) Uani 1 d . . . O42 O 0.6203(12) 0.9268(11) 0.5960(5) 0.060(3) Uani 1 d . . . O44 O 0.6637(18) 1.1019(14) 0.6296(6) 0.100(5) Uani 1 d . . . O51 O 0.8995(11) 0.5706(10) 0.5953(4) 0.058(3) Uani 1 d . . . N53 N 0.8284(14) 0.4953(14) 0.6250(7) 0.062(3) Uani 1 d . . . O52 O 0.7252(14) 0.5380(10) 0.6553(4) 0.062(3) Uani 1 d . . . O54 O 0.8659(14) 0.3910(11) 0.6274(6) 0.083(4) Uani 1 d . . . N11 N 0.9952(12) 0.8319(12) 0.5762(5) 0.046(3) Uani 1 d . . . C16 C 1.0076(15) 0.8338(14) 0.5184(6) 0.044(4) Uani 1 d . . . C15 C 1.1403(19) 0.8735(14) 0.4914(8) 0.064(5) Uani 1 d . . . H15 H 1.1499 0.8681 0.4518 0.077 Uiso 1 calc R . . C14 C 1.2576(18) 0.9210(14) 0.5245(8) 0.063(5) Uani 1 d . . . H14 H 1.3425 0.9549 0.5074 0.076 Uiso 1 calc R . . C13 C 1.245(2) 0.9166(13) 0.5824(6) 0.050(4) Uani 1 d . . . H13 H 1.3255 0.9414 0.6054 0.059 Uiso 1 calc R . . C12 C 1.1152(17) 0.8764(13) 0.6068(7) 0.055(4) Uani 1 d . . . H12 H 1.1074 0.8792 0.6465 0.066 Uiso 1 calc R . . N21 N 0.7528(14) 0.7510(10) 0.5166(3) 0.038(2) Uani 1 d . . . C22 C 0.8722(16) 0.7900(13) 0.4851(5) 0.038(3) Uani 1 d . . . N23 N 0.8766(16) 0.7944(14) 0.4295(5) 0.060(4) Uani 1 d . . . C24 C 0.753(3) 0.7544(14) 0.4013(5) 0.049(3) Uani 1 d . . . N25 N 0.6259(14) 0.7145(12) 0.4282(5) 0.045(3) Uani 1 d . . . C26 C 0.6366(17) 0.7160(14) 0.4849(6) 0.045(3) Uani 1 d . . . N31 N 0.5197(13) 0.6667(13) 0.5749(5) 0.052(3) Uani 1 d . . . C32 C 0.5020(16) 0.6662(17) 0.5175(6) 0.054(4) Uani 1 d . . . C33 C 0.3701(16) 0.6265(13) 0.4900(6) 0.047(4) Uani 1 d . . . H33 H 0.3633 0.6286 0.4503 0.057 Uiso 1 calc R . . C34 C 0.2512(18) 0.5849(14) 0.5214(6) 0.053(4) Uani 1 d . . . H34 H 0.1615 0.5602 0.5037 0.063 Uiso 1 calc R . . C35 C 0.2677(19) 0.5804(15) 0.5794(7) 0.061(5) Uani 1 d . . . H35 H 0.1885 0.5518 0.6019 0.073 Uiso 1 calc R . . C36 C 0.4027(16) 0.6187(14) 0.6056(6) 0.054(4) Uani 1 d . . . H36 H 0.4132 0.6112 0.6451 0.064 Uiso 1 calc R . . N27 N 0.746(3) 0.7520(13) 0.3450(4) 0.072(4) Uani 1 d . . . H20A H 0.8223 0.7764 0.3251 0.087 Uiso 1 calc R . . H20B H 0.6658 0.7259 0.3280 0.087 Uiso 1 calc R . . N63 N 0.6422(13) 1.0070(14) 0.2483(6) 0.055(3) Uani 1 d . . . O61 O 0.6879(16) 0.9230(14) 0.2197(6) 0.102(5) Uani 1 d . . . O62 O 0.727(2) 1.0791(17) 0.2700(7) 0.133(7) Uani 1 d . . . O64 O 0.5044(13) 1.0224(16) 0.2533(8) 0.109(5) Uani 1 d . . . O502 O 0.9237(15) 0.8213(12) 0.8013(5) 0.087(4) Uani 1 d . . . O503 O 1.0024(13) 1.1004(14) 0.7237(5) 0.096(5) Uani 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 Dy1 0.0399(4) 0.0407(5) 0.0308(3) -0.0004(3) 0.0059(4) 0.0008(2) O100 0.067(7) 0.071(8) 0.033(5) -0.002(5) -0.005(5) 0.008(6) O200 0.046(6) 0.072(8) 0.043(6) -0.005(5) 0.023(5) 0.003(5) N43 0.100(11) 0.028(10) 0.050(8) 0.002(7) 0.040(9) 0.007(8) O41 0.064(8) 0.040(8) 0.082(8) -0.014(6) 0.012(6) -0.001(6) O42 0.067(7) 0.056(8) 0.056(7) 0.003(6) 0.004(6) 0.011(6) O44 0.150(13) 0.053(10) 0.099(10) 0.006(8) 0.037(10) 0.012(8) O51 0.051(6) 0.070(8) 0.053(6) -0.003(6) 0.012(5) -0.003(5) N53 0.061(8) 0.057(11) 0.069(9) -0.006(9) 0.002(8) 0.004(7) O52 0.080(8) 0.056(7) 0.050(5) 0.016(5) 0.023(6) 0.003(6) O54 0.100(9) 0.045(9) 0.103(9) 0.005(7) -0.011(8) 0.027(6) N11 0.047(8) 0.043(9) 0.049(7) -0.014(6) 0.008(5) 0.009(5) C16 0.051(9) 0.045(11) 0.037(7) -0.002(7) 0.020(6) 0.007(6) C15 0.066(11) 0.048(12) 0.080(11) 0.018(9) 0.033(9) 0.021(9) C14 0.037(9) 0.035(10) 0.118(15) 0.000(9) 0.017(10) -0.018(7) C13 0.054(10) 0.041(10) 0.054(9) 0.000(7) 0.010(7) -0.017(8) C12 0.068(10) 0.043(11) 0.055(9) -0.008(7) 0.003(8) -0.017(8) N21 0.038(5) 0.040(7) 0.036(4) 0.012(5) -0.007(6) -0.008(4) C22 0.044(8) 0.041(8) 0.031(7) 0.005(6) 0.002(6) 0.021(6) N23 0.061(9) 0.085(10) 0.033(6) 0.004(7) 0.011(6) 0.012(7) C24 0.067(9) 0.052(10) 0.029(5) 0.006(7) 0.004(9) 0.002(7) N25 0.050(7) 0.047(7) 0.037(6) -0.007(6) -0.012(5) 0.008(5) C26 0.043(8) 0.050(10) 0.041(8) -0.001(7) -0.008(6) 0.016(7) N31 0.045(7) 0.064(11) 0.048(7) -0.012(6) 0.006(5) -0.003(6) C32 0.055(11) 0.067(13) 0.039(8) -0.008(8) 0.010(6) 0.007(7) C33 0.051(9) 0.054(11) 0.037(7) -0.005(7) 0.017(6) -0.011(7) C34 0.035(8) 0.060(11) 0.063(10) -0.004(7) -0.009(7) -0.008(7) C35 0.041(9) 0.066(12) 0.076(11) -0.005(9) 0.017(8) 0.006(8) C36 0.042(8) 0.081(13) 0.038(8) -0.003(7) -0.002(6) -0.008(8) N27 0.091(11) 0.093(11) 0.033(5) -0.002(7) -0.003(10) -0.027(7) N63 0.055(7) 0.063(8) 0.047(6) 0.001(6) 0.009(7) 0.006(8) O61 0.104(11) 0.110(12) 0.093(9) -0.030(9) 0.044(8) 0.031(9) O62 0.151(16) 0.141(15) 0.106(12) -0.013(10) -0.060(11) -0.067(13) O64 0.067(8) 0.112(13) 0.149(11) -0.042(10) 0.017(9) 0.006(7) O502 0.097(10) 0.101(11) 0.063(7) -0.018(7) 0.000(7) 0.019(8) O503 0.074(9) 0.125(13) 0.088(9) -0.040(8) 0.007(6) 0.009(7) _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 Dy1 O100 2.329(12) . ? Dy1 O200 2.339(8) . ? Dy1 O42 2.428(11) . ? Dy1 O51 2.431(11) . ? Dy1 O41 2.476(11) . ? Dy1 O52 2.482(11) . ? Dy1 N21 2.490(9) . ? Dy1 N31 2.540(12) . ? Dy1 N11 2.548(11) . ? N43 O44 1.191(16) . ? N43 O42 1.266(17) . ? N43 O41 1.291(18) . ? O51 N53 1.262(17) . ? N53 O54 1.216(16) . ? N53 O52 1.247(17) . ? N11 C16 1.353(16) . ? N11 C12 1.365(18) . ? C16 C15 1.401(19) . ? C16 C22 1.50(2) . ? C15 C14 1.39(2) . ? C14 C13 1.36(2) . ? C13 C12 1.35(2) . ? N21 C26 1.317(19) . ? N21 C22 1.356(17) . ? C22 N23 1.297(16) . ? N23 C24 1.34(3) . ? C24 N27 1.316(16) . ? C24 N25 1.36(3) . ? N25 C26 1.325(17) . ? C26 C32 1.52(2) . ? N31 C32 1.347(18) . ? N31 C36 1.367(17) . ? C32 C33 1.39(2) . ? C33 C34 1.36(2) . ? C34 C35 1.36(2) . ? C35 C36 1.40(2) . ? N63 O61 1.223(17) . ? N63 O64 1.228(15) . ? N63 O62 1.211(19) . ? 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 O100 Dy1 O200 82.6(4) . . ? O100 Dy1 O42 126.4(4) . . ? O200 Dy1 O42 78.9(4) . . ? O100 Dy1 O51 77.8(3) . . ? O200 Dy1 O51 127.5(4) . . ? O42 Dy1 O51 149.2(3) . . ? O100 Dy1 O41 74.0(4) . . ? O200 Dy1 O41 73.8(3) . . ? O42 Dy1 O41 52.5(4) . . ? O51 Dy1 O41 141.8(4) . . ? O100 Dy1 O52 77.1(4) . . ? O200 Dy1 O52 77.4(3) . . ? O42 Dy1 O52 143.6(4) . . ? O51 Dy1 O52 50.9(4) . . ? O41 Dy1 O52 141.3(4) . . ? O100 Dy1 N21 138.5(4) . . ? O200 Dy1 N21 138.9(4) . . ? O42 Dy1 N21 73.6(4) . . ? O51 Dy1 N21 75.5(4) . . ? O41 Dy1 N21 110.3(4) . . ? O52 Dy1 N21 108.4(4) . . ? O100 Dy1 N31 148.0(4) . . ? O200 Dy1 N31 81.2(4) . . ? O42 Dy1 N31 76.9(4) . . ? O51 Dy1 N31 90.6(4) . . ? O41 Dy1 N31 126.5(4) . . ? O52 Dy1 N31 72.5(4) . . ? N21 Dy1 N31 63.3(4) . . ? O100 Dy1 N11 78.6(4) . . ? O200 Dy1 N11 145.2(4) . . ? O42 Dy1 N11 89.1(4) . . ? O51 Dy1 N11 76.5(4) . . ? O41 Dy1 N11 73.0(4) . . ? O52 Dy1 N11 125.4(4) . . ? N21 Dy1 N11 64.7(4) . . ? N31 Dy1 N11 128.0(3) . . ? O44 N43 O42 122.1(18) . . ? O44 N43 O41 121.6(17) . . ? O42 N43 O41 116.2(14) . . ? O44 N43 Dy1 177.0(11) . . ? O42 N43 Dy1 57.0(8) . . ? O41 N43 Dy1 59.2(8) . . ? N43 O41 Dy1 94.2(9) . . ? N43 O42 Dy1 97.1(10) . . ? N53 O51 Dy1 98.2(9) . . ? O54 N53 O52 122.7(16) . . ? O54 N53 O51 122.3(15) . . ? O52 N53 O51 114.7(14) . . ? N53 O52 Dy1 96.1(9) . . ? C16 N11 C12 116.8(12) . . ? C16 N11 Dy1 120.4(10) . . ? C12 N11 Dy1 122.8(9) . . ? N11 C16 C15 121.6(15) . . ? N11 C16 C22 116.3(12) . . ? C15 C16 C22 122.1(13) . . ? C14 C15 C16 119.3(15) . . ? C13 C14 C15 118.3(15) . . ? C14 C13 C12 120.4(16) . . ? C13 C12 N11 123.4(14) . . ? C26 N21 C22 113.1(9) . . ? C26 N21 Dy1 124.4(9) . . ? C22 N21 Dy1 122.5(9) . . ? N23 C22 N21 125.5(15) . . ? N23 C22 C16 118.5(14) . . ? N21 C22 C16 116.0(11) . . ? C22 N23 C24 116.7(14) . . ? N27 C24 N23 122(3) . . ? N27 C24 N25 115(3) . . ? N23 C24 N25 123.1(10) . . ? C26 N25 C24 113.7(14) . . ? N21 C26 N25 127.8(15) . . ? N21 C26 C32 115.7(12) . . ? N25 C26 C32 116.4(14) . . ? C32 N31 C36 115.8(13) . . ? C32 N31 Dy1 122.3(10) . . ? C36 N31 Dy1 121.8(9) . . ? N31 C32 C33 123.3(13) . . ? N31 C32 C26 114.2(14) . . ? C33 C32 C26 122.5(13) . . ? C34 C33 C32 120.1(13) . . ? C33 C34 C35 117.9(15) . . ? C34 C35 C36 120.5(15) . . ? N31 C36 C35 122.1(13) . . ? O61 N63 O64 119.0(17) . . ? O61 N63 O62 122.7(15) . . ? O64 N63 O62 118.2(17) . . ? _diffrn_measured_fraction_theta_max 0.686 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.686 _refine_diff_density_max 1.444 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.137 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_4-ho _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 4-ho _chemical_formula_moiety [HoL4(NO3)2(H2O)2](NO3)2(H2O) _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 Ho N9 O13' _chemical_formula_weight 673.29 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.763(9) _cell_length_b 11.195(13) _cell_length_c 23.234(27) _cell_angle_alpha 90 _cell_angle_beta 90.144(10) _cell_angle_gamma 90 _cell_volume 2279.3(44) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.93 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 3.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5417 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.93 _reflns_number_total 3097 _reflns_number_observed 2232 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was used for 1 0 0 / -1 0 0 and refined to 0.47(1) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0050(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3097 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1957 _refine_ls_wR_factor_obs 0.1765 _refine_ls_goodness_of_fit_all 1.175 _refine_ls_goodness_of_fit_obs 1.273 _refine_ls_restrained_S_all 1.175 _refine_ls_restrained_S_obs 1.273 _refine_ls_shift/esd_max -0.019 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ho1 Ho 0.75762(8) 0.74785(5) 0.62287(2) 0.0368(3) Uani 1 d . . O100 O 0.9307(12) 0.7306(8) 0.6958(5) 0.047(3) Uani 1 d . . O200 O 0.5860(12) 0.7645(7) 0.6985(4) 0.044(3) Uani 1 d . . N43 N 0.6935(22) 0.9979(14) 0.6300(8) 0.076(5) Uani 1 d . . O41 O 0.7908(16) 0.9533(11) 0.6599(6) 0.065(4) Uani 1 d . . O42 O 0.6232(13) 0.9288(11) 0.5958(4) 0.063(3) Uani 1 d . . O44 O 0.6654(18) 1.1024(11) 0.6296(5) 0.093(4) Uani 1 d . . O51 O 0.9029(13) 0.5710(10) 0.5948(5) 0.064(3) Uani 1 d . . N53 N 0.8315(16) 0.4959(14) 0.6268(6) 0.059(3) Uani 1 d . . O52 O 0.7226(15) 0.5389(10) 0.6564(5) 0.053(3) Uani 1 d . . O54 O 0.8602(17) 0.3910(10) 0.6274(5) 0.088(4) Uani 1 d . . N11 N 0.9962(12) 0.8357(12) 0.5755(4) 0.047(3) Uani 1 d . . C16 C 1.0018(14) 0.8346(15) 0.5191(6) 0.050(4) Uani 1 d . . C15 C 1.1335(18) 0.8737(14) 0.4900(6) 0.057(4) Uani 1 d . . H15 H 1.1404(18) 0.8716(14) 0.4501(6) 0.069 Uiso 1 calc R . C14 C 1.2457(29) 0.9132(15) 0.5222(7) 0.062(5) Uani 1 d . . H14 H 1.3304(29) 0.9424(15) 0.5026(7) 0.074 Uiso 1 calc R . C13 C 1.2537(23) 0.9169(16) 0.5820(7) 0.055(5) Uani 1 d . . H13 H 1.3381(23) 0.9436(16) 0.6027(7) 0.066 Uiso 1 calc R . C12 C 1.1176(19) 0.8752(13) 0.6072(6) 0.057(4) Uani 1 d . . H12 H 1.1102(19) 0.8745(13) 0.6471(6) 0.069 Uiso 1 calc R . N21 N 0.7513(18) 0.7508(10) 0.5169(4) 0.040(3) Uani 1 d . . C22 C 0.8729(18) 0.7910(14) 0.4852(6) 0.046(4) Uani 1 d . . N23 N 0.8752(13) 0.7967(12) 0.4300(5) 0.048(3) Uani 1 d . . C24 C 0.7372(29) 0.7546(12) 0.4006(5) 0.036(4) Uani 1 d . . N25 N 0.6236(17) 0.7118(12) 0.4283(5) 0.053(3) Uani 1 d . . C26 C 0.6363(18) 0.7168(13) 0.4834(6) 0.042(4) Uani 1 d . . N31 N 0.5219(12) 0.6676(13) 0.5759(5) 0.055(4) Uani 1 d . . C32 C 0.4970(14) 0.6650(14) 0.5171(6) 0.046(4) Uani 1 d . . C33 C 0.3693(18) 0.6275(13) 0.4905(6) 0.052(4) Uani 1 d . . H33 H 0.3645(18) 0.6290(13) 0.4506(6) 0.062 Uiso 1 calc R . C34 C 0.2404(30) 0.5853(15) 0.5224(8) 0.065(5) Uani 1 d . . H34 H 0.1473(30) 0.5647(15) 0.5058(8) 0.078 Uiso 1 calc R . C35 C 0.2711(21) 0.5788(17) 0.5814(6) 0.057(5) Uani 1 d . . H35 H 0.1977(21) 0.5468(17) 0.6057(6) 0.068 Uiso 1 calc R . C36 C 0.4048(17) 0.6179(13) 0.6039(7) 0.055(4) Uani 1 d . . H36 H 0.4165(17) 0.6091(13) 0.6435(7) 0.066 Uiso 1 calc R . N27 N 0.7675(34) 0.7513(10) 0.3449(6) 0.059(4) Uiso 1 d . . H27A H 0.7206(34) 0.7985(10) 0.3218(6) 0.070 Uiso 1 calc R . H27B H 0.8341(34) 0.7018(10) 0.3319(6) 0.070 Uiso 1 calc R . N63 N 0.6416(15) 1.0077(17) 0.2506(6) 0.066(3) Uani 1 d . . O61 O 0.6875(23) 0.9214(14) 0.2192(6) 0.117(8) Uani 1 d . . O62 O 0.7271(20) 1.0780(15) 0.2699(7) 0.109(6) Uani 1 d . . O64 O 0.5078(16) 1.0216(17) 0.2516(9) 0.116(5) Uani 1 d . . O502 O 0.9246(16) 0.8218(11) 0.8015(4) 0.086(4) Uani 1 d . . O503 O 1.0050(13) 1.0969(13) 0.7253(5) 0.087(4) Uani 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 Ho1 0.0413(5) 0.0360(6) 0.0332(4) -0.0010(3) -0.0056(5) 0.0006(2) O100 0.027(7) 0.072(8) 0.041(6) -0.016(5) 0.001(4) 0.003(4) O200 0.032(6) 0.065(8) 0.036(6) 0.001(4) 0.019(4) 0.002(4) N43 0.109(14) 0.037(9) 0.083(12) -0.013(10) 0.023(11) -0.029(13) O41 0.069(11) 0.045(8) 0.082(9) -0.017(6) -0.001(7) -0.002(7) O42 0.068(8) 0.059(8) 0.062(7) 0.000(6) -0.009(5) 0.025(6) O44 0.136(12) 0.048(8) 0.096(8) 0.006(8) 0.030(10) -0.007(9) O51 0.065(7) 0.059(8) 0.068(7) 0.003(6) -0.006(6) 0.016(6) N53 0.081(10) 0.058(10) 0.037(7) -0.008(7) -0.012(7) -0.013(9) O52 0.050(8) 0.054(7) 0.055(6) 0.017(5) 0.000(5) -0.001(6) O54 0.117(11) 0.036(7) 0.112(9) -0.002(7) 0.006(9) -0.005(8) N11 0.053(7) 0.055(9) 0.035(6) -0.012(6) 0.012(5) 0.017(6) C16 0.049(9) 0.048(11) 0.053(9) -0.004(8) 0.030(6) 0.004(7) C15 0.058(10) 0.067(12) 0.047(8) 0.002(8) -0.009(7) -0.011(9) C14 0.075(14) 0.045(11) 0.066(10) 0.006(8) 0.011(9) -0.003(11) C13 0.046(11) 0.056(12) 0.064(10) -0.014(8) -0.011(7) -0.002(10) C12 0.081(12) 0.047(11) 0.044(8) -0.009(7) -0.016(8) -0.006(9) N21 0.048(9) 0.042(8) 0.031(4) 0.005(5) -0.002(6) -0.009(4) C22 0.058(10) 0.041(9) 0.039(9) -0.012(7) -0.014(7) 0.020(9) N23 0.035(7) 0.058(8) 0.051(8) -0.003(7) 0.000(5) 0.007(6) C24 0.031(11) 0.040(9) 0.038(6) -0.009(6) 0.002(6) 0.021(5) N25 0.066(10) 0.049(8) 0.045(8) 0.010(6) -0.008(6) 0.011(7) C26 0.052(9) 0.035(8) 0.040(8) -0.007(6) -0.016(6) 0.017(8) N31 0.013(5) 0.074(11) 0.078(9) -0.005(8) 0.018(5) -0.006(6) C32 0.051(9) 0.032(10) 0.054(10) -0.008(8) 0.006(6) -0.009(7) C33 0.062(10) 0.039(10) 0.055(9) -0.025(7) -0.012(7) 0.009(9) C34 0.061(13) 0.026(9) 0.107(15) 0.001(9) -0.024(10) 0.017(10) C35 0.029(9) 0.089(15) 0.052(9) 0.005(8) -0.011(7) -0.001(10) C36 0.032(8) 0.049(11) 0.084(11) 0.010(8) -0.001(7) 0.016(7) N63 0.044(7) 0.095(12) 0.060(6) -0.005(7) 0.011(7) 0.005(8) O61 0.177(23) 0.086(11) 0.088(9) -0.025(8) 0.035(11) 0.028(13) O62 0.101(14) 0.106(12) 0.120(12) -0.026(9) -0.057(10) -0.040(10) O64 0.069(10) 0.093(14) 0.187(14) -0.020(11) 0.009(10) -0.009(8) O502 0.121(11) 0.079(10) 0.058(6) -0.001(6) -0.011(6) 0.019(9) O503 0.075(9) 0.103(12) 0.083(8) -0.026(7) -0.005(6) 0.002(8) _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 O100 2.280(11) . ? Ho1 O200 2.324(8) . ? Ho1 O42 2.427(11) . ? Ho1 O51 2.444(11) . ? Ho1 N21 2.463(9) . ? Ho1 O41 2.471(12) . ? Ho1 O52 2.486(11) . ? Ho1 N31 2.499(12) . ? Ho1 N11 2.561(11) . ? N43 O44 1.20(2) . ? N43 O41 1.21(2) . ? N43 O42 1.27(2) . ? N53 O51 1.29(2) . ? N53 O54 1.20(2) . ? N53 O52 1.27(2) . ? N11 C16 1.313(15) . ? N11 C12 1.36(2) . ? C16 C15 1.41(2) . ? C16 C22 1.46(2) . ? C15 C14 1.31(2) . ? C14 C13 1.39(2) . ? C13 C12 1.41(3) . ? N21 C26 1.33(2) . ? N21 C22 1.37(2) . ? C22 N23 1.28(2) . ? N23 C24 1.46(2) . ? C24 N25 1.28(3) . ? C24 N27 1.32(3) . ? N25 C26 1.29(2) . ? C26 C32 1.56(2) . ? N31 C36 1.34(2) . ? N31 C32 1.38(2) . ? C32 C33 1.34(2) . ? C33 C34 1.43(3) . ? C34 C35 1.40(2) . ? C35 C36 1.35(2) . ? N63 O62 1.17(2) . ? N63 O64 1.18(2) . ? N63 O61 1.28(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 O100 Ho1 O200 82.8(4) . . ? O100 Ho1 O42 125.9(4) . . ? O200 Ho1 O42 79.3(4) . . ? O100 Ho1 O51 77.4(3) . . ? O200 Ho1 O51 127.2(4) . . ? O42 Ho1 O51 149.4(3) . . ? O100 Ho1 N21 139.3(5) . . ? O200 Ho1 N21 137.9(5) . . ? O42 Ho1 N21 73.7(4) . . ? O51 Ho1 N21 75.9(4) . . ? O100 Ho1 O41 75.2(4) . . ? O200 Ho1 O41 74.8(4) . . ? O42 Ho1 O41 50.9(4) . . ? O51 Ho1 O41 141.8(5) . . ? N21 Ho1 O41 109.7(4) . . ? O100 Ho1 O52 76.6(4) . . ? O200 Ho1 O52 75.9(4) . . ? O42 Ho1 O52 143.9(4) . . ? O51 Ho1 O52 52.1(4) . . ? N21 Ho1 O52 109.0(4) . . ? O41 Ho1 O52 141.3(4) . . ? O100 Ho1 N31 147.2(4) . . ? O200 Ho1 N31 79.8(4) . . ? O42 Ho1 N31 77.6(4) . . ? O51 Ho1 N31 91.4(4) . . ? N21 Ho1 N31 63.4(4) . . ? O41 Ho1 N31 125.5(5) . . ? O52 Ho1 N31 72.4(4) . . ? O100 Ho1 N11 79.1(4) . . ? O200 Ho1 N11 145.6(4) . . ? O42 Ho1 N11 87.9(4) . . ? O51 Ho1 N11 76.7(4) . . ? N21 Ho1 N11 65.2(4) . . ? O41 Ho1 N11 72.4(4) . . ? O52 Ho1 N11 126.7(4) . . ? N31 Ho1 N11 128.7(3) . . ? O44 N43 O41 123.8(18) . . ? O44 N43 O42 119.4(20) . . ? O41 N43 O42 116.7(16) . . ? O54 N53 O52 121.3(15) . . ? O54 N53 O51 123.0(16) . . ? O52 N53 O51 115.6(14) . . ? C16 N11 C12 120.1(12) . . ? C16 N11 Ho1 117.2(9) . . ? C12 N11 Ho1 122.7(9) . . ? N11 C16 C15 120.7(13) . . ? N11 C16 C22 120.9(12) . . ? C15 C16 C22 118.4(13) . . ? C14 C15 C16 116.5(15) . . ? C15 C14 C13 127.6(20) . . ? C14 C13 C12 111.9(16) . . ? N11 C12 C13 123.2(13) . . ? C26 N21 C22 112.3(10) . . ? C26 N21 Ho1 125.2(11) . . ? C22 N21 Ho1 122.4(10) . . ? N23 C22 N21 124.5(14) . . ? N23 C22 C16 121.0(15) . . ? N21 C22 C16 114.4(12) . . ? C22 N23 C24 116.8(15) . . ? N25 C24 N27 127.0(32) . . ? N25 C24 N23 121.2(11) . . ? N27 C24 N23 111.2(35) . . ? C24 N25 C26 115.6(14) . . ? N25 C26 N21 129.4(15) . . ? N25 C26 C32 115.7(13) . . ? N21 C26 C32 114.8(12) . . ? C36 N31 C32 111.2(13) . . ? C36 N31 Ho1 124.6(10) . . ? C32 N31 Ho1 124.2(8) . . ? C33 C32 N31 126.0(13) . . ? C33 C32 C26 122.2(13) . . ? N31 C32 C26 111.8(12) . . ? C32 C33 C34 121.5(14) . . ? C35 C34 C33 111.0(19) . . ? C36 C35 C34 123.0(19) . . ? N31 C36 C35 127.0(15) . . ? O62 N63 O64 120.7(21) . . ? O62 N63 O61 121.8(17) . . ? O64 N63 O61 116.6(21) . . ? _refine_diff_density_max 1.255 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.149 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END ; _data_4-er _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 Er N9 O13' _chemical_formula_weight 675.62 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' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.759(9) _cell_length_b 11.176(13) _cell_length_c 23.25(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.494(10) _cell_angle_gamma 90.00 _cell_volume 2276(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 3.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6659 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3956 _reflns_number_gt 2498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1257P)^2^+9.7614P] 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 SHELXL _refine_ls_extinction_coef 0.0016(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3956 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2457 _refine_ls_wR_factor_gt 0.2147 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.75745(8) 0.74827(6) 0.62260(2) 0.0417(3) Uani 1 d . . . O100 O 0.9324(14) 0.7301(9) 0.6963(5) 0.054(3) Uani 1 d . . . O200 O 0.5854(17) 0.7647(9) 0.6981(5) 0.060(3) Uani 1 d . . . N43 N 0.683(2) 0.9982(15) 0.6274(9) 0.075(5) Uani 1 d . . . O41 O 0.7920(15) 0.9526(12) 0.6592(6) 0.068(4) Uani 1 d . . . O42 O 0.6183(15) 0.9236(11) 0.5954(6) 0.064(3) Uani 1 d . . . O44 O 0.6588(17) 1.1049(12) 0.6291(6) 0.085(4) Uani 1 d . . . O51 O 0.9020(13) 0.5744(11) 0.5934(5) 0.062(3) Uani 1 d . . . N53 N 0.8321(16) 0.4953(15) 0.6273(6) 0.058(4) Uani 1 d . . . O52 O 0.7227(15) 0.5415(12) 0.6560(6) 0.070(4) Uani 1 d . . . O54 O 0.8649(18) 0.3922(11) 0.6267(7) 0.094(5) Uani 1 d . . . N11 N 0.9914(15) 0.8347(12) 0.5759(5) 0.048(3) Uani 1 d . . . C16 C 1.0078(17) 0.8355(15) 0.5196(7) 0.049(4) Uani 1 d . . . C15 C 1.137(2) 0.8732(16) 0.4904(8) 0.060(4) Uani 1 d . . . H15 H 1.1424 0.8696 0.4505 0.072 Uiso 1 calc R . . C14 C 1.260(2) 0.9170(15) 0.5236(9) 0.060(5) Uani 1 d . . . H14 H 1.3489 0.9456 0.5066 0.072 Uiso 1 calc R . . C13 C 1.2436(18) 0.9154(15) 0.5820(8) 0.054(4) Uani 1 d . . . H13 H 1.3239 0.9413 0.6053 0.065 Uiso 1 calc R . . C12 C 1.1098(18) 0.8760(13) 0.6075(8) 0.054(4) Uani 1 d . . . H12 H 1.1018 0.8783 0.6474 0.064 Uiso 1 calc R . . N21 N 0.7528(15) 0.7505(11) 0.5168(5) 0.042(3) Uani 1 d . . . C22 C 0.8744(19) 0.7903(15) 0.4853(7) 0.047(4) Uani 1 d . . . N23 N 0.8801(17) 0.7920(14) 0.4300(6) 0.057(4) Uani 1 d . . . C24 C 0.754(3) 0.7514(16) 0.4010(7) 0.057(4) Uani 1 d . . . N25 N 0.6296(16) 0.7109(13) 0.4274(6) 0.047(3) Uani 1 d . . . C26 C 0.636(2) 0.7124(14) 0.4833(7) 0.047(4) Uani 1 d . . . N31 N 0.5158(17) 0.6661(14) 0.5746(6) 0.061(4) Uani 1 d . . . C32 C 0.5041(19) 0.6677(15) 0.5176(7) 0.052(4) Uani 1 d . . . C33 C 0.370(2) 0.6303(15) 0.4907(7) 0.056(4) Uani 1 d . . . H33 H 0.3594 0.6374 0.4510 0.068 Uiso 1 calc R . . C34 C 0.254(2) 0.5841(15) 0.5213(9) 0.066(5) Uani 1 d . . . H34 H 0.1671 0.5538 0.5033 0.080 Uiso 1 calc R . . C35 C 0.2697(18) 0.5832(16) 0.5818(8) 0.057(4) Uani 1 d . . . H35 H 0.1907 0.5556 0.6048 0.069 Uiso 1 calc R . . C36 C 0.4008(17) 0.6232(15) 0.6058(7) 0.053(4) Uani 1 d . . . H36 H 0.4116 0.6208 0.6456 0.063 Uiso 1 calc R . . N27 N 0.755(3) 0.7512(14) 0.3452(7) 0.081(6) Uani 1 d . . . H20A H 0.6768 0.7254 0.3263 0.097 Uiso 1 calc R . . H20B H 0.8338 0.7768 0.3271 0.097 Uiso 1 calc R . . N63 N 0.6362(16) 1.0045(18) 0.2494(7) 0.064(4) Uani 1 d . . . O61 O 0.6856(19) 0.9179(17) 0.2204(7) 0.102(6) Uani 1 d . . . O62 O 0.733(2) 1.075(2) 0.2695(8) 0.124(7) Uani 1 d . . . O64 O 0.5015(17) 1.0202(18) 0.2524(10) 0.117(6) Uani 1 d . . . O502 O 0.9251(19) 0.8210(14) 0.8018(6) 0.092(4) Uani 1 d . . . O503 O 1.0041(18) 1.1015(16) 0.7242(7) 0.104(5) Uani 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 Er1 0.0436(5) 0.0445(5) 0.0369(4) -0.0011(3) 0.0001(4) 0.0005(3) O100 0.050(7) 0.067(8) 0.043(6) -0.004(5) -0.024(5) 0.006(5) O200 0.079(10) 0.070(9) 0.030(5) -0.004(5) 0.015(6) -0.006(6) N43 0.066(11) 0.049(10) 0.112(15) 0.022(10) 0.048(11) 0.024(8) O41 0.064(8) 0.057(8) 0.084(9) -0.036(7) 0.008(7) -0.013(7) O42 0.072(8) 0.036(7) 0.084(9) 0.003(6) -0.003(7) 0.000(6) O44 0.103(11) 0.060(9) 0.093(10) 0.004(8) 0.013(9) 0.015(8) O51 0.064(8) 0.059(8) 0.062(7) -0.002(6) 0.018(6) 0.011(6) N53 0.054(8) 0.073(10) 0.048(8) -0.020(8) -0.020(7) 0.010(8) O52 0.055(8) 0.066(8) 0.089(9) 0.016(7) 0.008(7) 0.008(7) O54 0.117(12) 0.039(8) 0.125(12) -0.016(8) -0.014(10) 0.025(8) N11 0.058(9) 0.041(8) 0.046(7) -0.009(6) -0.007(6) -0.006(6) C16 0.041(9) 0.051(10) 0.055(9) -0.009(8) 0.016(7) 0.002(7) C15 0.059(11) 0.056(11) 0.066(11) -0.004(9) -0.013(9) 0.009(9) C14 0.044(10) 0.054(11) 0.082(13) -0.011(9) 0.007(9) -0.012(8) C13 0.025(8) 0.053(10) 0.084(12) -0.009(9) -0.020(8) 0.008(7) C12 0.058(10) 0.032(8) 0.072(11) -0.002(7) 0.011(9) 0.011(8) N21 0.025(6) 0.046(7) 0.056(7) -0.007(6) 0.004(6) 0.000(5) C22 0.044(9) 0.056(9) 0.040(8) 0.007(7) 0.002(7) 0.013(8) N23 0.046(8) 0.074(9) 0.052(8) 0.012(7) 0.009(7) 0.010(7) C24 0.067(12) 0.072(11) 0.033(7) 0.005(8) 0.000(9) 0.023(9) N25 0.043(8) 0.058(8) 0.041(7) -0.001(6) -0.006(6) 0.009(6) C26 0.054(10) 0.030(7) 0.058(10) 0.001(7) -0.004(8) 0.010(7) N31 0.061(10) 0.058(10) 0.065(9) -0.005(8) 0.017(8) 0.013(8) C32 0.060(11) 0.047(10) 0.049(9) 0.002(7) 0.008(8) 0.011(8) C33 0.055(10) 0.058(11) 0.056(10) -0.003(8) -0.023(8) 0.012(9) C34 0.051(11) 0.045(10) 0.102(15) -0.005(10) -0.034(11) -0.011(9) C35 0.027(8) 0.069(12) 0.076(12) -0.006(9) -0.003(8) -0.009(8) C36 0.044(9) 0.055(11) 0.059(10) -0.002(8) 0.000(8) -0.009(8) N27 0.113(16) 0.086(12) 0.043(8) 0.021(8) -0.013(11) -0.016(9) N63 0.046(8) 0.095(12) 0.052(7) 0.008(7) -0.010(8) -0.018(9) O61 0.088(11) 0.109(13) 0.110(12) -0.027(10) 0.030(10) 0.020(10) O62 0.114(14) 0.144(17) 0.112(13) -0.002(12) -0.054(12) -0.022(13) O64 0.071(10) 0.093(13) 0.187(17) -0.025(12) 0.007(12) -0.002(8) O502 0.101(12) 0.087(11) 0.089(10) -0.006(8) 0.008(9) 0.003(9) O503 0.100(12) 0.114(14) 0.098(11) -0.046(10) 0.011(9) -0.002(10) _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was used and refined to 0.14(1) ; 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 Er1 O100 2.298(11) . ? Er1 O200 2.331(12) . ? Er1 O42 2.392(12) . ? Er1 O51 2.420(11) . ? Er1 O41 2.453(12) . ? Er1 N21 2.460(13) . ? Er1 O52 2.457(13) . ? Er1 N11 2.519(13) . ? Er1 N31 2.553(16) . ? N43 O44 1.212(18) . ? N43 O42 1.25(2) . ? N43 O41 1.31(2) . ? O51 N53 1.336(19) . ? N53 O54 1.188(18) . ? N53 O52 1.281(19) . ? N11 C16 1.317(19) . ? N11 C12 1.35(2) . ? C16 C15 1.39(2) . ? C16 C22 1.50(2) . ? C15 C14 1.41(2) . ? C14 C13 1.37(3) . ? C13 C12 1.39(2) . ? N21 C26 1.35(2) . ? N21 C22 1.37(2) . ? C22 N23 1.29(2) . ? N23 C24 1.36(3) . ? C24 N27 1.30(3) . ? C24 N25 1.34(3) . ? N25 C26 1.30(2) . ? C26 C32 1.49(2) . ? N31 C32 1.33(2) . ? N31 C36 1.33(2) . ? C32 C33 1.39(2) . ? C33 C34 1.34(3) . ? C34 C35 1.41(3) . ? C35 C36 1.35(2) . ? N63 O64 1.196(19) . ? N63 O62 1.24(2) . ? N63 O61 1.26(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 O100 Er1 O200 82.9(4) . . ? O100 Er1 O42 127.3(4) . . ? O200 Er1 O42 78.6(4) . . ? O100 Er1 O51 77.9(4) . . ? O200 Er1 O51 128.2(4) . . ? O42 Er1 O51 148.4(4) . . ? O100 Er1 O41 75.3(4) . . ? O200 Er1 O41 75.1(4) . . ? O42 Er1 O41 52.4(5) . . ? O51 Er1 O41 141.4(4) . . ? O100 Er1 N21 138.7(5) . . ? O200 Er1 N21 138.4(5) . . ? O42 Er1 N21 73.9(4) . . ? O51 Er1 N21 74.5(4) . . ? O41 Er1 N21 109.7(4) . . ? O100 Er1 O52 76.3(4) . . ? O200 Er1 O52 75.8(4) . . ? O42 Er1 O52 142.2(4) . . ? O51 Er1 O52 53.1(4) . . ? O41 Er1 O52 141.3(5) . . ? N21 Er1 O52 109.0(4) . . ? O100 Er1 N11 79.4(4) . . ? O200 Er1 N11 145.9(4) . . ? O42 Er1 N11 89.3(4) . . ? O51 Er1 N11 75.9(4) . . ? O41 Er1 N11 72.2(4) . . ? N21 Er1 N11 64.6(4) . . ? O52 Er1 N11 126.8(4) . . ? O100 Er1 N31 147.0(5) . . ? O200 Er1 N31 79.5(5) . . ? O42 Er1 N31 76.1(5) . . ? O51 Er1 N31 91.4(4) . . ? O41 Er1 N31 125.7(5) . . ? N21 Er1 N31 64.0(4) . . ? O52 Er1 N31 72.3(5) . . ? N11 Er1 N31 128.6(4) . . ? O44 N43 O42 127(2) . . ? O44 N43 O41 120(2) . . ? O42 N43 O41 113.6(14) . . ? N43 O41 Er1 94.7(11) . . ? N43 O42 Er1 99.3(10) . . ? N53 O51 Er1 97.0(8) . . ? O54 N53 O52 125.5(18) . . ? O54 N53 O51 121.5(16) . . ? O52 N53 O51 112.8(14) . . ? N53 O52 Er1 96.9(10) . . ? C16 N11 C12 116.7(14) . . ? C16 N11 Er1 121.8(11) . . ? C12 N11 Er1 121.4(10) . . ? N11 C16 C15 125.7(16) . . ? N11 C16 C22 115.9(14) . . ? C15 C16 C22 118.5(15) . . ? C16 C15 C14 117.4(17) . . ? C13 C14 C15 116.9(17) . . ? C14 C13 C12 121.7(16) . . ? N11 C12 C13 121.6(16) . . ? C26 N21 C22 112.6(13) . . ? C26 N21 Er1 125.3(11) . . ? C22 N21 Er1 122.0(10) . . ? N23 C22 N21 125.1(17) . . ? N23 C22 C16 119.4(16) . . ? N21 C22 C16 115.5(13) . . ? C22 N23 C24 116.8(17) . . ? N27 C24 N25 118(3) . . ? N27 C24 N23 119(3) . . ? N25 C24 N23 123.1(14) . . ? C26 N25 C24 115.3(16) . . ? N25 C26 N21 127.1(17) . . ? N25 C26 C32 120.3(17) . . ? N21 C26 C32 112.6(15) . . ? C32 N31 C36 119.6(16) . . ? C32 N31 Er1 119.1(12) . . ? C36 N31 Er1 121.2(11) . . ? N31 C32 C33 120.1(17) . . ? N31 C32 C26 118.9(16) . . ? C33 C32 C26 121.0(15) . . ? C34 C33 C32 120.9(16) . . ? C33 C34 C35 117.7(16) . . ? C36 C35 C34 118.9(17) . . ? N31 C36 C35 122.6(17) . . ? O64 N63 O62 124(2) . . ? O64 N63 O61 119.2(19) . . ? O62 N63 O61 116.7(18) . . ? _refine_diff_density_max 3.137 _refine_diff_density_min -2.502 _refine_diff_density_rms 0.208 _refine_diff_density_max 3.657 _refine_diff_density_min -2.058 _refine_diff_density_rms 0.227 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_4-tm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4-tm _chemical_formula_moiety [TmL4(NO3)2(H2O)2](NO3)(H2O)2 _chemical_formula_sum 'C13 H18 N9 O13 Tm' _chemical_formula_weight 677.29 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' 'Tm' 'Tm' -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.745(9) _cell_length_b 11.172(13) _cell_length_c 23.22(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.619(10) _cell_angle_gamma 90.00 _cell_volume 2268(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.996 _exptl_absorpt_correction_type all _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean n/a _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5533 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3129 _reflns_number_gt 1756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was not necessary ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+5.5468P] 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 3129 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2156 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.75709(6) 0.74893(7) 0.62239(2) 0.0418(3) Uani 1 d . . . O100 O 0.9325(13) 0.7308(11) 0.6959(4) 0.060(3) Uani 1 d . . . O200 O 0.5890(13) 0.7689(10) 0.6976(4) 0.056(3) Uani 1 d . . . N43 N 0.689(2) 0.9985(17) 0.6268(7) 0.067(4) Uani 1 d . . . O41 O 0.7916(18) 0.9575(15) 0.6587(7) 0.092(5) Uani 1 d . . . O42 O 0.6192(12) 0.9275(13) 0.5943(5) 0.071(4) Uani 1 d . . . O44 O 0.6550(17) 1.1048(14) 0.6296(7) 0.098(5) Uani 1 d . . . O51 O 0.8970(13) 0.5744(12) 0.5950(5) 0.069(4) Uani 1 d . . . N53 N 0.8347(19) 0.4948(17) 0.6270(6) 0.066(5) Uani 1 d . . . O52 O 0.7232(13) 0.5411(11) 0.6549(5) 0.062(3) Uani 1 d . . . O54 O 0.8661(18) 0.3921(14) 0.6266(7) 0.094(5) Uani 1 d . . . N11 N 0.9904(14) 0.8340(14) 0.5753(6) 0.059(4) Uani 1 d . . . C16 C 1.0062(18) 0.8367(18) 0.5189(6) 0.061(5) Uani 1 d . . . C15 C 1.137(2) 0.8783(16) 0.4919(8) 0.060(5) Uani 1 d . . . H15 H 1.1433 0.8804 0.4519 0.072 Uiso 1 calc R . . C14 C 1.258(2) 0.9167(16) 0.5267(10) 0.066(6) Uani 1 d . . . H14 H 1.3487 0.9416 0.5098 0.079 Uiso 1 calc R . . C13 C 1.2455(18) 0.9181(19) 0.5841(7) 0.067(6) Uani 1 d . . . H13 H 1.3258 0.9449 0.6073 0.080 Uiso 1 calc R . . C12 C 1.110(2) 0.879(2) 0.6081(8) 0.074(6) Uani 1 d . . . H12 H 1.0995 0.8824 0.6479 0.089 Uiso 1 calc R . . N21 N 0.7544(14) 0.7497(11) 0.5176(5) 0.045(3) Uani 1 d . . . C22 C 0.8750(19) 0.7871(15) 0.4845(7) 0.050(4) Uani 1 d . . . N23 N 0.8780(15) 0.7932(15) 0.4303(6) 0.063(4) Uani 1 d . . . C24 C 0.750(2) 0.7550(16) 0.4015(6) 0.050(4) Uani 1 d . . . N25 N 0.6297(16) 0.7140(13) 0.4277(6) 0.056(4) Uani 1 d . . . C26 C 0.629(2) 0.7130(16) 0.4845(7) 0.055(5) Uani 1 d . . . N31 N 0.5177(14) 0.6643(15) 0.5748(6) 0.062(4) Uani 1 d . . . C32 C 0.5043(17) 0.6690(17) 0.5171(6) 0.052(4) Uani 1 d . . . C33 C 0.371(2) 0.6283(17) 0.4892(9) 0.068(5) Uani 1 d . . . H33 H 0.3619 0.6315 0.4493 0.081 Uiso 1 calc R . . C34 C 0.256(2) 0.5851(19) 0.5208(7) 0.070(6) Uani 1 d . . . H34 H 0.1688 0.5563 0.5024 0.084 Uiso 1 calc R . . C35 C 0.2658(19) 0.5823(17) 0.5801(8) 0.064(5) Uani 1 d . . . H35 H 0.1838 0.5557 0.6018 0.077 Uiso 1 calc R . . C36 C 0.4039(17) 0.6210(16) 0.6074(7) 0.056(5) Uani 1 d . . . H36 H 0.4153 0.6165 0.6473 0.067 Uiso 1 calc R . . N27 N 0.753(2) 0.7514(14) 0.3442(6) 0.079(5) Uani 1 d . . . H27A H 0.6764 0.7224 0.3252 0.095 Uiso 1 calc R . . H27B H 0.8313 0.7779 0.3261 0.095 Uiso 1 calc R . . N63 N 0.6399(17) 1.0049(18) 0.2476(6) 0.067(5) Uani 1 d . . . O61 O 0.6821(17) 0.9150(17) 0.2197(6) 0.107(6) Uani 1 d . . . O62 O 0.726(2) 1.0764(17) 0.2708(7) 0.124(7) Uani 1 d . . . O64 O 0.5068(19) 1.0182(17) 0.2540(8) 0.111(5) Uani 1 d . . . O502 O 0.9251(19) 0.8272(19) 0.8017(6) 0.115(6) Uani 1 d . . . O503 O 1.0051(16) 1.1016(18) 0.7245(7) 0.125(7) Uani 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 Tm1 0.0402(5) 0.0464(6) 0.0388(4) -0.0009(4) 0.0004(2) 0.0011(4) O100 0.052(7) 0.082(11) 0.047(5) -0.002(6) -0.014(4) 0.008(6) O200 0.067(8) 0.059(9) 0.041(5) 0.001(5) 0.023(5) -0.004(6) N43 0.079(12) 0.050(12) 0.073(11) -0.018(9) 0.003(8) -0.023(11) O41 0.107(13) 0.077(13) 0.091(11) -0.032(9) -0.014(8) -0.014(10) O42 0.047(7) 0.075(11) 0.091(9) 0.006(8) -0.006(6) 0.009(6) O44 0.120(12) 0.043(10) 0.130(13) -0.028(9) 0.010(9) 0.023(10) O51 0.066(8) 0.076(11) 0.067(8) 0.006(7) 0.017(6) 0.005(7) N53 0.084(12) 0.059(12) 0.055(9) -0.031(9) 0.014(7) 0.004(11) O52 0.069(8) 0.041(8) 0.075(8) 0.032(6) -0.013(6) -0.003(6) O54 0.135(13) 0.050(10) 0.097(11) -0.011(9) 0.016(8) 0.029(10) N11 0.049(9) 0.065(12) 0.062(9) -0.008(8) 0.001(6) 0.016(8) C16 0.067(11) 0.071(14) 0.044(8) 0.007(9) 0.026(7) 0.013(10) C15 0.068(12) 0.037(12) 0.077(12) 0.003(9) 0.024(9) 0.015(9) C14 0.044(12) 0.037(13) 0.117(17) -0.005(12) 0.014(9) -0.010(9) C13 0.048(10) 0.11(2) 0.045(9) -0.010(10) -0.017(7) -0.018(10) C12 0.061(13) 0.087(18) 0.075(12) 0.006(11) -0.007(9) 0.013(11) N21 0.047(7) 0.046(9) 0.041(6) 0.003(7) 0.003(4) 0.005(7) C22 0.056(11) 0.044(12) 0.050(9) -0.015(7) -0.003(7) 0.015(8) N23 0.053(9) 0.091(13) 0.044(7) 0.007(7) 0.005(6) 0.003(8) C24 0.068(11) 0.053(11) 0.028(6) 0.005(9) 0.005(5) 0.013(10) N25 0.056(9) 0.063(11) 0.048(7) -0.005(7) -0.013(6) -0.006(7) C26 0.065(12) 0.044(12) 0.054(9) 0.016(7) -0.019(7) 0.002(8) N31 0.048(8) 0.071(12) 0.067(9) 0.004(9) 0.011(6) 0.006(8) C32 0.061(11) 0.055(12) 0.039(8) -0.006(8) -0.001(6) 0.012(9) C33 0.069(13) 0.056(15) 0.077(13) 0.005(10) -0.014(9) 0.008(10) C34 0.074(13) 0.085(18) 0.050(11) -0.024(11) -0.019(8) 0.019(12) C35 0.054(12) 0.050(14) 0.089(14) 0.003(10) 0.025(9) 0.004(10) C36 0.042(10) 0.063(14) 0.062(10) -0.006(9) 0.006(7) 0.002(8) N27 0.110(14) 0.082(14) 0.045(8) -0.006(9) -0.019(7) -0.038(9) N63 0.040(9) 0.109(16) 0.053(8) -0.010(9) 0.002(6) -0.012(9) O61 0.108(12) 0.130(16) 0.085(10) -0.031(10) 0.035(8) 0.025(11) O62 0.149(15) 0.109(16) 0.114(12) -0.033(11) -0.070(11) -0.029(12) O64 0.090(12) 0.099(15) 0.144(14) -0.018(11) -0.014(9) -0.007(9) O502 0.129(13) 0.139(17) 0.076(10) -0.006(11) 0.006(8) 0.034(12) O503 0.098(12) 0.161(18) 0.118(13) -0.070(12) 0.029(9) -0.049(11) _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 Tm1 O100 2.292(10) . ? Tm1 O200 2.306(9) . ? Tm1 O51 2.392(12) . ? Tm1 O42 2.418(13) . ? Tm1 N21 2.434(11) . ? Tm1 O52 2.460(12) . ? Tm1 O41 2.495(15) . ? Tm1 N11 2.512(14) . ? Tm1 N31 2.539(15) . ? N43 O44 1.22(2) . ? N43 O42 1.248(18) . ? N43 O41 1.25(2) . ? O51 N53 1.284(19) . ? N53 O54 1.179(19) . ? N53 O52 1.285(18) . ? N11 C16 1.317(18) . ? N11 C12 1.38(2) . ? C16 C15 1.39(2) . ? C16 C22 1.50(2) . ? C15 C14 1.39(3) . ? C14 C13 1.34(2) . ? C13 C12 1.39(2) . ? N21 C22 1.38(2) . ? N21 C26 1.39(2) . ? C22 N23 1.261(19) . ? N23 C24 1.36(2) . ? C24 N27 1.33(2) . ? C24 N25 1.30(2) . ? N25 C26 1.32(2) . ? C26 C32 1.42(2) . ? N31 C36 1.348(19) . ? N31 C32 1.343(18) . ? C32 C33 1.41(2) . ? C33 C34 1.34(2) . ? C34 C35 1.38(2) . ? C35 C36 1.42(2) . ? N63 O64 1.185(18) . ? N63 O62 1.219(19) . ? N63 O61 1.25(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 O100 Tm1 O200 82.6(4) . . ? O100 Tm1 O51 77.6(4) . . ? O200 Tm1 O51 127.8(4) . . ? O100 Tm1 O42 127.1(4) . . ? O200 Tm1 O42 78.7(4) . . ? O51 Tm1 O42 148.9(4) . . ? O100 Tm1 N21 138.1(4) . . ? O200 Tm1 N21 139.3(4) . . ? O51 Tm1 N21 74.7(4) . . ? O42 Tm1 N21 74.2(4) . . ? O100 Tm1 O52 76.7(4) . . ? O200 Tm1 O52 77.2(4) . . ? O51 Tm1 O52 51.4(4) . . ? O42 Tm1 O52 143.2(4) . . ? N21 Tm1 O52 108.1(4) . . ? O100 Tm1 O41 75.8(5) . . ? O200 Tm1 O41 74.3(5) . . ? O51 Tm1 O41 142.3(5) . . ? O42 Tm1 O41 51.6(5) . . ? N21 Tm1 O41 109.5(5) . . ? O52 Tm1 O41 142.4(5) . . ? O100 Tm1 N11 79.5(4) . . ? O200 Tm1 N11 145.2(4) . . ? O51 Tm1 N11 76.8(4) . . ? O42 Tm1 N11 88.6(4) . . ? N21 Tm1 N11 64.0(4) . . ? O52 Tm1 N11 126.2(4) . . ? O41 Tm1 N11 72.5(5) . . ? O100 Tm1 N31 146.4(5) . . ? O200 Tm1 N31 80.6(4) . . ? O51 Tm1 N31 90.2(5) . . ? O42 Tm1 N31 77.4(5) . . ? N21 Tm1 N31 64.4(4) . . ? O52 Tm1 N31 71.4(5) . . ? O41 Tm1 N31 126.2(5) . . ? N11 Tm1 N31 128.4(4) . . ? O44 N43 O42 122(2) . . ? O44 N43 O41 119.8(18) . . ? O42 N43 O41 117.9(19) . . ? N43 O41 Tm1 93.4(12) . . ? N43 O42 Tm1 97.1(12) . . ? N53 O51 Tm1 100.9(9) . . ? O54 N53 O52 124.9(18) . . ? O54 N53 O51 124.8(16) . . ? O52 N53 O51 109.9(16) . . ? N53 O52 Tm1 97.6(10) . . ? C16 N11 C12 116.9(15) . . ? C16 N11 Tm1 122.4(12) . . ? C12 N11 Tm1 120.7(11) . . ? N11 C16 C15 123.5(17) . . ? N11 C16 C22 115.7(14) . . ? C15 C16 C22 120.7(15) . . ? C14 C15 C16 117.7(17) . . ? C13 C14 C15 120.7(15) . . ? C14 C13 C12 118.5(15) . . ? C13 C12 N11 122.5(17) . . ? C22 N21 C26 112.6(13) . . ? C22 N21 Tm1 124.1(10) . . ? C26 N21 Tm1 123.3(10) . . ? N23 C22 N21 126.7(15) . . ? N23 C22 C16 119.3(15) . . ? N21 C22 C16 113.6(13) . . ? C22 N23 C24 116.5(14) . . ? N27 C24 N25 118.6(18) . . ? N27 C24 N23 118.4(17) . . ? N25 C24 N23 122.9(13) . . ? C26 N25 C24 118.8(14) . . ? N25 C26 N21 122.5(15) . . ? N25 C26 C32 123.1(15) . . ? N21 C26 C32 114.3(14) . . ? C36 N31 C32 121.2(15) . . ? C36 N31 Tm1 119.9(11) . . ? C32 N31 Tm1 118.8(10) . . ? N31 C32 C33 120.7(15) . . ? N31 C32 C26 119.0(14) . . ? C33 C32 C26 120.3(15) . . ? C34 C33 C32 119.1(18) . . ? C33 C34 C35 121.3(18) . . ? C34 C35 C36 118.6(15) . . ? N31 C36 C35 119.1(15) . . ? O64 N63 O62 117.8(19) . . ? O64 N63 O61 117.4(18) . . ? O62 N63 O61 124.7(17) . . ? _refine_diff_density_max 1.860 _refine_diff_density_min -2.236 _refine_diff_density_rms 0.206 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_4-yb _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 4-yb _chemical_formula_moiety [YbL4(NO3)2(H2O)],2H2O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 N9 O13 Yb' _chemical_formula_weight 681.40 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.745(9) _cell_length_b 11.183(13) _cell_length_c 23.23(3) _cell_angle_alpha 89.96 _cell_angle_beta 91.016(10) _cell_angle_gamma 90.03 _cell_volume 2272(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 4.201 _exptl_absorpt_correction_type empirical (DIFABS) _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7228 _diffrn_reflns_av_R_equivalents 0.1204 _diffrn_reflns_av_sigmaI/netI 0.1175 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.10 _reflns_number_total 4044 _reflns_number_gt 2405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.1284P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00001(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4044 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_obs 0.0719 _refine_ls_wR_factor_all 0.1705 _refine_ls_wR_factor_obs 0.1479 _refine_ls_goodness_of_fit_all 1.253 _refine_ls_goodness_of_fit_obs 1.543 _refine_ls_restrained_S_all 1.321 _refine_ls_restrained_S_obs 1.543 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Yb1 Yb 0.75628(8) 0.74598(9) 0.62219(3) 0.0420(3) Uani 1 d . . O100 O 0.9327(12) 0.7361(12) 0.6978(4) 0.049(3) Uani 1 d . . O200 O 0.5846(12) 0.7597(13) 0.6972(4) 0.051(3) Uani 1 d . . N43 N 0.6925(16) 0.9958(15) 0.6279(6) 0.046(4) Uani 1 d . . O41 O 0.7934(13) 0.9543(11) 0.6608(5) 0.051(3) Uani 1 d . . O42 O 0.6175(12) 0.9241(10) 0.5938(5) 0.046(3) Uani 1 d . . O44 O 0.6566(15) 1.0986(11) 0.6306(5) 0.058(3) Uani 1 d . . O51 O 0.8961(12) 0.5730(11) 0.5956(5) 0.047(3) Uani 1 d . . N53 N 0.8305(18) 0.4989(14) 0.6262(7) 0.052(4) Uani 1 d . . O52 O 0.7184(13) 0.5378(10) 0.6555(5) 0.042(3) Uani 1 d . . O54 O 0.8656(13) 0.3914(10) 0.6269(5) 0.052(3) Uani 1 d . . N11 N 0.9969(16) 0.8320(11) 0.5791(6) 0.041(3) Uani 1 d . . C16 C 1.0074(18) 0.8331(14) 0.5172(7) 0.042(4) Uani 1 d . . C15 C 1.1422(21) 0.8760(15) 0.4910(8) 0.052(5) Uani 1 d . . H15 H 1.1573(21) 0.8784(15) 0.4515(8) 0.062 Uiso 1 calc R . C14 C 1.2530(19) 0.9155(15) 0.5338(7) 0.040(4) Uani 1 d . . H14 H 1.3447(19) 0.9446(15) 0.5197(7) 0.048 Uiso 1 calc R . C13 C 1.2403(19) 0.9154(16) 0.5927(7) 0.040(4) Uani 1 d . . H13 H 1.3174(19) 0.9399(16) 0.6182(7) 0.048 Uiso 1 calc R . C12 C 1.1075(20) 0.8770(15) 0.6084(8) 0.047(4) Uani 1 d . . H12 H 1.0898(20) 0.8834(15) 0.6476(8) 0.056 Uiso 1 calc R . N21 N 0.7505(13) 0.7330(10) 0.5225(6) 0.037(3) Uani 1 d . . C22 C 0.8678(19) 0.7914(14) 0.4858(7) 0.041(4) Uani 1 d . . N23 N 0.8785(17) 0.7909(12) 0.4287(6) 0.047(4) Uani 1 d . . C24 C 0.7585(17) 0.7460(21) 0.4013(6) 0.043(3) Uani 1 d . . N25 N 0.6330(16) 0.7105(11) 0.4283(6) 0.045(4) Uani 1 d . . C26 C 0.6418(17) 0.7129(13) 0.4840(7) 0.034(4) Uani 1 d . . N31 N 0.5158(15) 0.6698(11) 0.5769(6) 0.037(3) Uani 1 d . . C32 C 0.5013(17) 0.6710(13) 0.5150(7) 0.035(4) Uani 1 d . . C33 C 0.3811(20) 0.6294(17) 0.4918(8) 0.052(5) Uani 1 d . . H33 H 0.3762(20) 0.6338(17) 0.4519(8) 0.063 Uiso 1 calc R . C34 C 0.2543(21) 0.5777(14) 0.5179(7) 0.038(4) Uani 1 d . . H34 H 0.1702(21) 0.5475(14) 0.4975(7) 0.045 Uiso 1 calc R . C35 C 0.2681(19) 0.5765(14) 0.5783(8) 0.041(5) Uani 1 d . . H35 H 0.1890(19) 0.5440(14) 0.5996(8) 0.049 Uiso 1 calc R . C36 C 0.4008(19) 0.6238(16) 0.6088(7) 0.048(4) Uani 1 d . . H36 H 0.4073(19) 0.6228(16) 0.6488(7) 0.058 Uiso 1 calc R . N27 N 0.7575(15) 0.7480(16) 0.3442(5) 0.053(3) Uani 1 d . . H27A H 0.8337(15) 0.7779(16) 0.3263(5) 0.064 Uiso 1 calc R . H27B H 0.6807(15) 0.7193(16) 0.3252(5) 0.064 Uiso 1 calc R . N63 N 0.6489(18) 1.0028(15) 0.2506(6) 0.050(4) Uani 1 d . . O61 O 0.6772(14) 0.9220(12) 0.2162(5) 0.060(3) Uani 1 d . . O62 O 0.7291(15) 1.0811(12) 0.2659(5) 0.058(4) Uani 1 d . . O64 O 0.5083(15) 1.0214(12) 0.2586(6) 0.064(4) Uani 1 d . . O502 O 0.9229(14) 0.8224(11) 0.8016(5) 0.053(3) Uani 1 d . . O503 O 1.0007(14) 1.1022(12) 0.7239(5) 0.059(3) Uani 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 Yb1 0.0406(4) 0.0433(4) 0.0421(4) -0.0006(5) 0.0005(2) 0.0003(4) O100 0.048(7) 0.050(7) 0.049(6) 0.000(7) -0.003(5) -0.010(6) O200 0.051(7) 0.055(7) 0.048(6) -0.001(7) 0.008(5) -0.008(7) N43 0.036(10) 0.075(12) 0.025(8) -0.004(8) 0.000(6) -0.012(8) O41 0.034(8) 0.057(8) 0.061(9) -0.021(7) -0.011(6) 0.007(6) O42 0.031(7) 0.055(8) 0.051(7) 0.009(6) -0.003(5) 0.004(5) O44 0.078(10) 0.033(7) 0.063(9) -0.002(6) 0.006(7) 0.013(6) O51 0.032(7) 0.056(8) 0.053(8) -0.003(6) 0.000(5) 0.005(5) N53 0.063(12) 0.045(10) 0.049(10) 0.005(8) -0.005(8) 0.010(8) O52 0.036(8) 0.046(7) 0.044(8) -0.006(6) -0.001(5) -0.008(5) O54 0.053(8) 0.033(7) 0.070(9) -0.005(6) 0.002(6) 0.000(6) N11 0.049(10) 0.032(8) 0.042(8) -0.004(6) -0.004(6) 0.001(6) C16 0.030(11) 0.035(10) 0.060(12) 0.005(8) 0.001(8) 0.004(7) C15 0.054(12) 0.045(11) 0.057(12) 0.000(9) -0.012(9) 0.000(9) C14 0.027(10) 0.056(11) 0.036(11) 0.016(9) 0.007(7) 0.005(8) C13 0.026(10) 0.055(11) 0.040(10) 0.006(8) -0.008(7) -0.015(8) C12 0.045(12) 0.046(11) 0.050(11) 0.002(9) -0.001(8) -0.005(8) N21 0.023(7) 0.004(6) 0.084(9) -0.004(6) -0.007(6) 0.003(5) C22 0.035(11) 0.037(9) 0.050(11) -0.001(7) 0.008(7) 0.007(6) N23 0.050(10) 0.042(9) 0.049(9) -0.002(6) 0.010(7) 0.004(6) C24 0.036(9) 0.057(10) 0.036(7) -0.005(12) -0.001(6) -0.003(10) N25 0.046(10) 0.042(9) 0.048(9) -0.003(6) -0.001(7) -0.001(6) C26 0.025(10) 0.038(10) 0.040(9) 0.002(6) -0.004(6) -0.003(6) N31 0.037(9) 0.028(7) 0.046(8) -0.002(6) -0.009(6) 0.005(6) C32 0.031(10) 0.029(9) 0.045(10) -0.002(7) -0.014(7) 0.007(6) C33 0.045(12) 0.069(13) 0.043(11) -0.001(9) 0.004(8) -0.015(9) C34 0.059(12) 0.036(9) 0.018(8) -0.010(7) -0.008(7) 0.012(8) C35 0.034(11) 0.033(9) 0.056(13) -0.015(8) 0.018(8) 0.000(7) C36 0.034(11) 0.066(12) 0.045(11) 0.004(9) -0.001(7) -0.003(8) N27 0.050(9) 0.059(9) 0.051(8) -0.014(11) 0.006(6) 0.009(9) N63 0.046(11) 0.065(11) 0.040(9) -0.005(8) 0.011(7) 0.002(8) O61 0.056(9) 0.064(9) 0.060(9) -0.005(7) 0.014(6) 0.003(7) O62 0.057(9) 0.062(9) 0.056(8) 0.000(7) -0.012(6) -0.015(7) O64 0.052(9) 0.060(9) 0.079(10) -0.004(7) 0.014(7) -0.005(7) O502 0.056(9) 0.060(8) 0.045(7) -0.007(6) -0.005(6) 0.012(6) O503 0.053(8) 0.077(9) 0.045(7) -0.006(7) -0.003(6) -0.009(7) _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 Yb1 N21 2.320(14) . ? Yb1 O100 2.319(10) . ? Yb1 O200 2.326(10) . ? Yb1 O51 2.377(11) . ? Yb1 O42 2.418(11) . ? Yb1 O52 2.476(12) . ? Yb1 N31 2.485(13) . ? Yb1 O41 2.515(12) . ? Yb1 N11 2.534(14) . ? N43 O44 1.19(2) . ? N43 O41 1.25(2) . ? N43 O42 1.30(2) . ? O51 N53 1.24(2) . ? N53 O54 1.24(2) . ? N53 O52 1.28(2) . ? N11 C12 1.28(2) . ? N11 C16 1.44(2) . ? C16 C15 1.42(2) . ? C16 C22 1.49(2) . ? C15 C14 1.45(2) . ? C14 C13 1.37(2) . ? C13 C12 1.30(2) . ? N21 C26 1.31(2) . ? N21 C22 1.49(2) . ? C22 N23 1.33(2) . ? N23 C24 1.32(2) . ? C24 N27 1.33(2) . ? C24 N25 1.33(2) . ? N25 C26 1.29(2) . ? C26 C32 1.51(2) . ? N31 C36 1.36(2) . ? N31 C32 1.44(2) . ? C32 C33 1.26(2) . ? C33 C34 1.40(2) . ? C34 C35 1.41(2) . ? C35 C36 1.45(2) . ? N63 O62 1.17(2) . ? N63 O61 1.23(2) . ? N63 O64 1.26(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 N21 Yb1 O100 139.0(4) . . ? N21 Yb1 O200 138.6(4) . . ? O100 Yb1 O200 82.2(4) . . ? N21 Yb1 O51 72.0(4) . . ? O100 Yb1 O51 79.6(4) . . ? O200 Yb1 O51 126.2(5) . . ? N21 Yb1 O42 77.2(4) . . ? O100 Yb1 O42 124.7(4) . . ? O200 Yb1 O42 79.7(4) . . ? O51 Yb1 O42 149.1(4) . . ? N21 Yb1 O52 104.6(4) . . ? O100 Yb1 O52 79.1(4) . . ? O200 Yb1 O52 74.8(4) . . ? O51 Yb1 O52 52.3(4) . . ? O42 Yb1 O52 142.2(4) . . ? N21 Yb1 N31 63.4(4) . . ? O100 Yb1 N31 148.3(4) . . ? O200 Yb1 N31 77.8(4) . . ? O51 Yb1 N31 92.7(4) . . ? O42 Yb1 N31 75.5(4) . . ? O52 Yb1 N31 72.2(4) . . ? N21 Yb1 O41 114.5(4) . . ? O100 Yb1 O41 72.2(4) . . ? O200 Yb1 O41 75.6(5) . . ? O51 Yb1 O41 141.5(4) . . ? O42 Yb1 O41 52.8(4) . . ? O52 Yb1 O41 140.9(4) . . ? N31 Yb1 O41 124.8(4) . . ? N21 Yb1 N11 68.5(4) . . ? O100 Yb1 N11 76.8(4) . . ? O200 Yb1 N11 145.3(4) . . ? O51 Yb1 N11 76.8(4) . . ? O42 Yb1 N11 89.8(4) . . ? O52 Yb1 N11 126.6(4) . . ? N31 Yb1 N11 131.6(5) . . ? O41 Yb1 N11 71.7(4) . . ? O44 N43 O41 120.7(15) . . ? O44 N43 O42 119.9(15) . . ? O41 N43 O42 119.2(16) . . ? N43 O41 Yb1 92.3(10) . . ? N43 O42 Yb1 95.6(9) . . ? N53 O51 Yb1 98.6(10) . . ? O51 N53 O54 122.5(16) . . ? O51 N53 O52 116.4(14) . . ? O54 N53 O52 121.0(16) . . ? O51 N53 Yb1 55.8(8) . . ? O54 N53 Yb1 178.4(13) . . ? O52 N53 Yb1 60.6(8) . . ? N53 O52 Yb1 92.7(9) . . ? C12 N11 C16 117.8(14) . . ? C12 N11 Yb1 124.5(12) . . ? C16 N11 Yb1 117.7(10) . . ? C15 C16 N11 119.9(15) . . ? C15 C16 C22 125.2(16) . . ? N11 C16 C22 114.8(13) . . ? C16 C15 C14 111.1(16) . . ? C13 C14 C15 128.3(16) . . ? C12 C13 C14 111.5(15) . . ? N11 C12 C13 131.1(18) . . ? C26 N21 C22 100.5(13) . . ? C26 N21 Yb1 133.9(11) . . ? C22 N21 Yb1 122.6(9) . . ? N23 C22 C16 114.8(14) . . ? N23 C22 N21 128.8(15) . . ? C16 C22 N21 115.0(14) . . ? C24 N23 C22 114.4(14) . . ? N23 C24 N27 117.9(15) . . ? N23 C24 N25 122.7(14) . . ? N27 C24 N25 119.0(14) . . ? C26 N25 C24 115.4(13) . . ? N25 C26 N21 135.5(15) . . ? N25 C26 C32 115.8(13) . . ? N21 C26 C32 108.3(13) . . ? C36 N31 C32 119.6(13) . . ? C36 N31 Yb1 121.7(11) . . ? C32 N31 Yb1 118.6(9) . . ? C33 C32 N31 118.7(15) . . ? C33 C32 C26 126.2(16) . . ? N31 C32 C26 114.8(12) . . ? C32 C33 C34 129.1(18) . . ? C33 C34 C35 112.4(15) . . ? C34 C35 C36 122.5(15) . . ? N31 C36 C35 117.7(15) . . ? O62 N63 O61 128.1(16) . . ? O62 N63 O64 114.2(16) . . ? O61 N63 O64 115.1(16) . . ? _refine_diff_density_max 1.952 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.153 O52 Yb1 N11 126.6(4) . . ? N31 Yb1 N11 131.6(5) . . ? O41 Yb1 N11 71.7(4) . . ? O44 N43 O41 120.7(15) . . ? O44 N43 O42 119.9(15) . . ? O41 N43 O42 119.2(16) . . ? N43 O41 Yb1 92.3(10) . . ? N43 O42 Yb1 95.6(9) . . ? N53 O51 Yb1 98.6(10) . . ? O51 N53 O54 122.5(16) . . ? O51 N53 O52 116.4(14) . . ? O54 N53 O52 121.0(16) . . ? O51 N53 Yb1 55.8(8) . . ? O54 N53 Yb1 178.4(13) . . ? O52 N53 Yb1 60.6(8) . . ? N53 O52 Yb1 92.7(9) . . ? C12 N11 C16 117.8(14) . . ? C12 N11 Yb1 124.5(12) . . ? C16 N11 Yb1 117.7(10) . . ? C15 C16 N11 119.9(15) . . ? C15 C16 C22 125.2(16) . . ? N11 C16 C22 114.8(13) . . ? C16 C15 C14 111.1(16) . . ? C13 C14 C15 128.3(16) . . ? C12 C13 C14 111.5(15) . . ? N11 C12 C13 131.1(18) . . ? C26 N21 C22 100.5(13) . . ? C26 N21 Yb1 133.9(11) . . ? C22 N21 Yb1 122.6(9) . . ? N23 C22 C16 114.8(14) . . ? N23 C22 N21 128.8(15) . . ? C16 C22 N21 115.0(14) . . ? C24 N23 C22 114.4(14) . . ? N23 C24 N27 117.9(15) . . ? N23 C24 N25 122.7(14) . . ? N27 C24 N25 119.0(14) . . ? C26 N25 C24 115.4(13) . . ? N25 C26 N21 135.5(15) . . ? N25 C26 C32 115.8(13) . . ? N21 C26 C32 108.3(13) . . ? C36 N31 C32 119.6(13) . . ? C36 N31 Yb1 121.7(11) . . ? C32 N31 Yb1 118.6(9) . . ? C33 C32 N31 118.7(15) . . ? C33 C32 C26 126.2(16) . . ? N31 C32 C26 114.8(12) . . ? C32 C33 C34 129.1(18) . . ? C33 C34 C35 112.4(15) . . ? C34 C35 C36 122.5(15) . . ? N31 C36 C35 117.7(15) . . ? O62 N63 O61 128.1(16) . . ? O62 N63 O64 114.2(16) . . ? O61 N63 O64 115.1(16) . . ? _refine_diff_density_max 1.952 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.153 ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END _data_4-lu _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 4-lu _chemical_formula_moiety [LuL4(NO3)2(H2O)2]NO3,2H2O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H18 Lu N9 O13' _chemical_formula_weight 683.33 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.733(9) _cell_length_b 11.162(13) _cell_length_c 23.191(27) _cell_angle_alpha 90.00 _cell_angle_beta 90.734(10) _cell_angle_gamma 90.00 _cell_volume 2260.4(44) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.86 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method ? _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.452 _exptl_absorpt_correction_type empirical (DIFABS) _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7271 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.86 _reflns_number_total 3996 _reflns_number_observed 2923 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. A twin factor was not necessary ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+33.3248P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3996 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_obs 0.0621 _refine_ls_wR_factor_all 0.1209 _refine_ls_wR_factor_obs 0.1125 _refine_ls_goodness_of_fit_all 1.192 _refine_ls_goodness_of_fit_obs 1.315 _refine_ls_restrained_S_all 1.192 _refine_ls_restrained_S_obs 1.315 _refine_ls_shift/esd_max 0.027 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Lu1 Lu 0.75536(5) 0.74760(5) 0.62195(2) 0.0320(2) Uani 1 d . . O100 O 0.9303(8) 0.7270(5) 0.6955(3) 0.028(2) Uani 1 d . . O200 O 0.5858(9) 0.7664(8) 0.6964(3) 0.047(2) Uani 1 d . . N43 N 0.6895(13) 0.9978(10) 0.6295(6) 0.056(3) Uani 1 d . . O41 O 0.7904(9) 0.9541(8) 0.6590(4) 0.047(2) Uani 1 d . . O42 O 0.6177(10) 0.9230(7) 0.5938(4) 0.050(2) Uani 1 d . . O44 O 0.6489(11) 1.1030(9) 0.6271(4) 0.065(3) Uani 1 d . . O51 O 0.8962(8) 0.5760(7) 0.5939(3) 0.037(2) Uani 1 d . . N53 N 0.8275(14) 0.5010(10) 0.6265(5) 0.054(3) Uani 1 d . . O52 O 0.7245(8) 0.5448(7) 0.6569(3) 0.035(2) Uani 1 d . . O54 O 0.8697(11) 0.3948(8) 0.6271(4) 0.061(3) Uani 1 d . . N11 N 0.9942(11) 0.8326(8) 0.5767(4) 0.040(2) Uani 1 d . . C16 C 1.0116(12) 0.8367(10) 0.5204(5) 0.036(3) Uani 1 d . . C15 C 1.1367(15) 0.8745(10) 0.4920(6) 0.046(3) Uani 1 d . . H15 H 1.1445(15) 0.8714(10) 0.4520(6) 0.055 Uiso 1 calc R . C14 C 1.2477(17) 0.9164(13) 0.5262(7) 0.062(4) Uani 1 d . . H14 H 1.3351(17) 0.9484(13) 0.5096(7) 0.074 Uiso 1 calc R . C13 C 1.2379(13) 0.9140(9) 0.5844(5) 0.034(3) Uani 1 d . . H13 H 1.3208(13) 0.9378(9) 0.6072(5) 0.041 Uiso 1 calc R . C12 C 1.1091(14) 0.8774(10) 0.6088(6) 0.045(3) Uani 1 d . . H12 H 1.0987(14) 0.8831(10) 0.6485(6) 0.054 Uiso 1 calc R . N21 N 0.7546(9) 0.7484(9) 0.5169(3) 0.033(2) Uani 1 d . . C22 C 0.8708(12) 0.7884(8) 0.4844(4) 0.027(2) Uani 1 d . . N23 N 0.8805(11) 0.7899(8) 0.4301(4) 0.039(2) Uani 1 d . . C24 C 0.7538(13) 0.7515(13) 0.4013(4) 0.041(2) Uani 1 d . . N25 N 0.6261(10) 0.7115(7) 0.4307(4) 0.030(2) Uani 1 d . . C26 C 0.6330(11) 0.7151(7) 0.4844(4) 0.021(2) Uani 1 d . . N31 N 0.5175(11) 0.6697(8) 0.5746(4) 0.039(2) Uani 1 d . . C32 C 0.5051(12) 0.6666(10) 0.5187(4) 0.033(2) Uani 1 d . . C33 C 0.3696(15) 0.6306(12) 0.4911(6) 0.054(3) Uani 1 d . . H33 H 0.3580(15) 0.6389(12) 0.4514(6) 0.064 Uiso 1 calc R . C34 C 0.2599(14) 0.5855(10) 0.5216(5) 0.038(3) Uani 1 d . . H34 H 0.1717(14) 0.5584(10) 0.5029(5) 0.046 Uiso 1 calc R . C35 C 0.2701(16) 0.5764(14) 0.5823(7) 0.064(4) Uani 1 d . . H35 H 0.1935(16) 0.5419(14) 0.6043(7) 0.076 Uiso 1 calc R . C36 C 0.4040(13) 0.6233(10) 0.6064(6) 0.041(3) Uani 1 d . . H36 H 0.4156(13) 0.6225(10) 0.6463(6) 0.049 Uiso 1 calc R . N27 N 0.7534(13) 0.7464(12) 0.3444(4) 0.064(3) Uani 1 d . . H27A H 0.8335(13) 0.7674(12) 0.3257(4) 0.076 Uiso 1 calc R . H27B H 0.6730(13) 0.7221(12) 0.3261(4) 0.076 Uiso 1 calc R . N63 N 0.6377(14) 1.0045(11) 0.2500(5) 0.051(3) Uani 1 d . . O61 O 0.6842(13) 0.9205(11) 0.2200(5) 0.085(4) Uani 1 d . . O62 O 0.7283(14) 1.0797(12) 0.2700(5) 0.092(4) Uani 1 d . . O64 O 0.4991(15) 1.0163(12) 0.2533(6) 0.102(4) Uani 1 d . . O502 O 0.9258(14) 0.8203(12) 0.8010(5) 0.095(4) Uani 1 d . . O503 O 0.9970(15) 1.1035(13) 0.7263(6) 0.103(4) Uani 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 Lu1 0.0332(3) 0.0306(2) 0.0321(2) -0.0014(3) 0.00033(14) 0.0018(3) O100 0.036(4) 0.011(4) 0.035(3) 0.001(3) -0.005(3) -0.001(3) O200 0.050(5) 0.045(6) 0.045(4) 0.002(4) 0.005(3) -0.003(4) N43 0.046(8) 0.033(6) 0.089(9) -0.001(6) 0.017(6) 0.014(5) O41 0.024(5) 0.044(5) 0.072(6) -0.012(5) 0.000(4) 0.004(4) O42 0.053(6) 0.035(5) 0.061(5) -0.002(4) -0.006(4) 0.001(4) O44 0.064(7) 0.055(6) 0.077(7) 0.001(5) 0.007(5) 0.012(5) O51 0.027(5) 0.036(5) 0.047(5) 0.001(4) 0.004(3) 0.000(3) N53 0.061(8) 0.039(7) 0.062(7) -0.005(6) -0.009(6) 0.010(5) O52 0.022(5) 0.030(4) 0.052(5) 0.008(4) -0.002(3) -0.006(3) O54 0.070(7) 0.034(5) 0.079(7) 0.000(5) 0.001(5) 0.011(4) N11 0.041(6) 0.032(5) 0.046(6) 0.001(4) -0.005(4) 0.006(4) C16 0.028(7) 0.033(6) 0.046(7) -0.001(5) 0.004(5) 0.000(5) C15 0.049(8) 0.033(7) 0.056(8) 0.009(6) 0.003(6) 0.003(5) C14 0.053(10) 0.056(10) 0.076(12) -0.011(9) 0.009(8) -0.006(7) C13 0.032(7) 0.020(6) 0.049(7) -0.003(5) -0.009(5) -0.002(4) C12 0.048(8) 0.033(7) 0.053(7) -0.004(5) 0.000(6) 0.007(5) N21 0.033(5) 0.031(4) 0.036(4) -0.002(5) -0.001(3) 0.017(5) C22 0.027(6) 0.020(5) 0.033(5) 0.000(4) 0.004(4) 0.001(4) N23 0.039(6) 0.036(5) 0.041(5) 0.003(4) 0.006(4) 0.007(4) C24 0.043(7) 0.043(6) 0.037(5) -0.003(7) -0.002(4) -0.012(7) N25 0.023(5) 0.025(5) 0.044(5) -0.001(3) -0.007(4) 0.000(3) C26 0.015(6) 0.013(5) 0.036(5) 0.000(3) -0.001(4) 0.001(3) N31 0.032(6) 0.038(6) 0.047(6) -0.003(4) -0.003(4) 0.001(4) C32 0.021(6) 0.039(7) 0.040(6) 0.001(5) -0.004(4) 0.005(4) C33 0.045(9) 0.057(9) 0.059(8) 0.003(7) 0.000(6) -0.002(6) C34 0.037(8) 0.030(7) 0.048(8) -0.011(6) -0.005(5) -0.003(5) C35 0.040(9) 0.071(11) 0.080(11) -0.007(9) 0.015(7) 0.011(7) C36 0.026(7) 0.035(7) 0.060(8) -0.002(6) 0.001(5) 0.003(5) N27 0.071(8) 0.069(7) 0.051(6) 0.005(8) 0.004(5) -0.009(8) N63 0.039(8) 0.060(8) 0.055(7) 0.001(6) 0.002(5) -0.010(6) O61 0.083(9) 0.086(9) 0.087(8) -0.014(7) 0.018(6) 0.013(7) O62 0.078(9) 0.095(10) 0.102(9) 0.003(8) -0.014(7) -0.021(7) O64 0.070(10) 0.095(10) 0.141(12) -0.004(9) 0.012(8) 0.000(7) O502 0.087(10) 0.097(10) 0.101(9) -0.014(8) -0.007(7) 0.024(7) O503 0.091(10) 0.107(11) 0.113(10) -0.030(8) 0.016(7) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O100 2.286(7) . ? Lu1 O200 2.298(8) . ? Lu1 O51 2.373(8) . ? Lu1 O42 2.385(9) . ? Lu1 O52 2.420(8) . ? Lu1 N21 2.435(8) . ? Lu1 O41 2.478(9) . ? Lu1 N31 2.493(10) . ? Lu1 N11 2.530(10) . ? N43 O41 1.211(13) . ? N43 O44 1.228(13) . ? N43 O42 1.327(14) . ? O51 N53 1.280(13) . ? N53 O54 1.242(13) . ? N53 O52 1.252(13) . ? N11 C16 1.316(14) . ? N11 C12 1.339(15) . ? C16 C15 1.35(2) . ? C16 C22 1.572(15) . ? C15 C14 1.33(2) . ? C14 C13 1.35(2) . ? C13 C12 1.33(2) . ? N21 C26 1.347(12) . ? N21 C22 1.347(13) . ? C22 N23 1.265(13) . ? N23 C24 1.354(14) . ? C24 N27 1.320(14) . ? C24 N25 1.388(13) . ? N25 C26 1.247(12) . ? C26 C32 1.481(14) . ? N31 C32 1.301(13) . ? N31 C36 1.346(14) . ? C32 C33 1.40(2) . ? C33 C34 1.30(2) . ? C34 C35 1.41(2) . ? C35 C36 1.39(2) . ? N63 O64 1.222(15) . ? N63 O61 1.240(15) . ? N63 O62 1.239(15) . ? 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 O100 Lu1 O200 83.1(3) . . ? O100 Lu1 O51 77.2(2) . . ? O200 Lu1 O51 128.4(3) . . ? O100 Lu1 O42 128.1(3) . . ? O200 Lu1 O42 78.6(3) . . ? O51 Lu1 O42 148.2(3) . . ? O100 Lu1 O52 74.4(2) . . ? O200 Lu1 O52 76.1(3) . . ? O51 Lu1 O52 52.9(3) . . ? O42 Lu1 O52 143.3(3) . . ? O100 Lu1 N21 137.7(3) . . ? O200 Lu1 N21 139.2(3) . . ? O51 Lu1 N21 73.9(3) . . ? O42 Lu1 N21 74.3(3) . . ? O52 Lu1 N21 109.8(3) . . ? O100 Lu1 O41 75.9(3) . . ? O200 Lu1 O41 74.4(3) . . ? O51 Lu1 O41 141.7(3) . . ? O42 Lu1 O41 52.4(3) . . ? O52 Lu1 O41 140.1(3) . . ? N21 Lu1 O41 110.0(3) . . ? O100 Lu1 N31 147.0(3) . . ? O200 Lu1 N31 79.7(3) . . ? O51 Lu1 N31 91.7(3) . . ? O42 Lu1 N31 75.6(3) . . ? O52 Lu1 N31 74.1(3) . . ? N21 Lu1 N31 64.5(3) . . ? O41 Lu1 N31 125.1(3) . . ? O100 Lu1 N11 78.5(3) . . ? O200 Lu1 N11 145.0(3) . . ? O51 Lu1 N11 75.9(3) . . ? O42 Lu1 N11 89.7(3) . . ? O52 Lu1 N11 125.8(3) . . ? N21 Lu1 N11 64.9(3) . . ? O41 Lu1 N11 72.4(3) . . ? N31 Lu1 N11 129.3(3) . . ? O41 N43 O44 128.1(13) . . ? O41 N43 O42 115.7(10) . . ? O44 N43 O42 116.1(12) . . ? N43 O41 Lu1 95.4(7) . . ? N43 O42 Lu1 96.5(7) . . ? N53 O51 Lu1 96.8(6) . . ? O54 N53 O52 125.7(12) . . ? O54 N53 O51 119.3(12) . . ? O52 N53 O51 115.0(10) . . ? O54 N53 Lu1 175.4(10) . . ? O52 N53 Lu1 58.5(5) . . ? O51 N53 Lu1 56.5(5) . . ? N53 O52 Lu1 95.4(7) . . ? C16 N11 C12 116.3(10) . . ? C16 N11 Lu1 122.0(7) . . ? C12 N11 Lu1 121.6(8) . . ? N11 C16 C15 126.8(11) . . ? N11 C16 C22 114.5(9) . . ? C15 C16 C22 118.6(10) . . ? C14 C15 C16 113.9(13) . . ? C15 C14 C13 122.2(14) . . ? C12 C13 C14 119.7(12) . . ? C13 C12 N11 120.7(12) . . ? C26 N21 C22 111.8(8) . . ? C26 N21 Lu1 123.5(6) . . ? C22 N21 Lu1 124.6(7) . . ? N23 C22 N21 128.5(10) . . ? N23 C22 C16 117.6(9) . . ? N21 C22 C16 113.9(8) . . ? C22 N23 C24 115.0(9) . . ? N27 C24 N23 119.9(10) . . ? N27 C24 N25 119.0(10) . . ? N23 C24 N25 121.0(9) . . ? C26 N25 C24 116.8(8) . . ? N25 C26 N21 126.6(9) . . ? N25 C26 C32 119.8(9) . . ? N21 C26 C32 113.2(8) . . ? C32 N31 C36 118.9(10) . . ? C32 N31 Lu1 120.5(7) . . ? C36 N31 Lu1 120.5(8) . . ? N31 C32 C33 121.5(10) . . ? N31 C32 C26 118.1(9) . . ? C33 C32 C26 120.0(10) . . ? C34 C33 C32 119.3(13) . . ? C33 C34 C35 122.1(13) . . ? C36 C35 C34 114.6(13) . . ? N31 C36 C35 123.0(12) . . ? O64 N63 O61 116.7(13) . . ? O64 N63 O62 122.1(14) . . ? O61 N63 O62 120.7(13) . . ? _refine_diff_density_max 1.530 _refine_diff_density_min -2.027 _refine_diff_density_rms 0.127 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_5-yb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5-yb _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 N11 O10 Yb ' _chemical_formula_weight 709.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.034(9) _cell_length_b 11.667(14) _cell_length_c 13.156(18) _cell_angle_alpha 107.499(10) _cell_angle_beta 103.277(10) _cell_angle_gamma 90.956(10) _cell_volume 1282(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.04 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 3.721 _exptl_absorpt_correction_type empirical (DIFABS) _exptl_absorpt_correction_T_min 0.292 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean n/a _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4353 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.04 _reflns_number_total 4353 _reflns_number_gt 3196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+8.4556P] 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 SHELXL _refine_ls_extinction_coef 0.0002(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4353 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.22616(5) 0.34255(4) 0.20787(4) 0.0498(2) Uani 1 d . . . O41 O 0.2489(11) 0.5486(7) 0.2053(8) 0.068(2) Uani 1 d . . . N43 N 0.1104(14) 0.5478(8) 0.1551(9) 0.062(3) Uani 1 d . . . O42 O 0.0282(10) 0.4506(7) 0.1309(8) 0.069(2) Uani 1 d . . . O44 O 0.0606(14) 0.6389(8) 0.1386(10) 0.088(3) Uani 1 d . . . O51 O 0.3654(10) 0.1657(7) 0.1892(7) 0.060(2) Uani 1 d . . . N53 N 0.3400(12) 0.1382(10) 0.2695(9) 0.065(3) Uani 1 d . . . O52 O 0.2512(11) 0.2054(9) 0.3207(8) 0.071(2) Uani 1 d . . . O54 O 0.3938(13) 0.0551(9) 0.2969(10) 0.093(4) Uani 1 d . . . O61 O 0.4483(10) 0.4304(10) 0.3325(9) 0.092(3) Uani 1 d . . . N63 N 0.5666(13) 0.4216(11) 0.3973(9) 0.065(3) Uani 1 d . . . O62 O 0.5780(18) 0.3276(15) 0.4215(12) 0.137(6) Uani 1 d . . . O64 O 0.6644(17) 0.4989(17) 0.4335(11) 0.157(8) Uani 1 d . . . O100 O 0.1425(11) 0.4483(8) 0.3615(7) 0.070(2) Uani 1 d . . . N21 N 0.1330(10) 0.2179(7) 0.0178(6) 0.0412(18) Uani 1 d . . . C22 C 0.2125(12) 0.2078(8) -0.0595(9) 0.044(2) Uani 1 d . . . N23 N 0.1669(11) 0.1431(8) -0.1624(8) 0.051(2) Uani 1 d . . . C24 C 0.0267(14) 0.0835(10) -0.1918(9) 0.053(3) Uani 1 d . . . N25 N -0.0614(11) 0.0832(8) -0.1227(8) 0.052(2) Uani 1 d . . . C26 C -0.0039(12) 0.1523(8) -0.0194(8) 0.043(2) Uani 1 d . . . N27 N -0.0224(14) 0.0156(10) -0.2961(8) 0.071(3) Uani 1 d . . . H27A H -0.1089 -0.0272 -0.3179 0.086 Uiso 1 calc R . . H27B H 0.0323 0.0143 -0.3420 0.086 Uiso 1 calc R . . C32 C -0.0968(12) 0.1584(8) 0.0618(9) 0.044(2) Uani 1 d . . . C33 C -0.2365(12) 0.0959(9) 0.0319(9) 0.049(2) Uani 1 d . . . H33 H -0.2772 0.0482 -0.0405 0.059 Uiso 1 calc R . . N31 N -0.0299(10) 0.2292(8) 0.1662(7) 0.047(2) Uani 1 d . . . C35 C -0.2508(15) 0.1763(10) 0.2187(10) 0.060(3) Uani 1 d . . . H35 H -0.3023 0.1838 0.2736 0.072 Uiso 1 calc R . . C34 C -0.3185(14) 0.1046(10) 0.1122(11) 0.060(3) Uani 1 d . . . H34 H -0.4148 0.0636 0.0946 0.072 Uiso 1 calc R . . C36 C -0.1086(14) 0.2366(10) 0.2441(10) 0.055(3) Uani 1 d . . . H36 H -0.0652 0.2835 0.3163 0.066 Uiso 1 calc R . . C16 C 0.3671(13) 0.2765(10) -0.0179(10) 0.050(3) Uani 1 d . . . N11 N 0.4018(11) 0.3503(8) 0.0862(9) 0.056(2) Uani 1 d . . . C12 C 0.5388(14) 0.4159(12) 0.1219(12) 0.065(3) Uani 1 d . . . H12 H 0.5641 0.4696 0.1930 0.079 Uiso 1 calc R . . C13 C 0.6428(17) 0.4078(13) 0.0591(14) 0.074(4) Uani 1 d . . . H13 H 0.7354 0.4555 0.0870 0.089 Uiso 1 calc R . . C14 C 0.6077(15) 0.3283(13) -0.0448(13) 0.070(4) Uani 1 d . . . H14 H 0.6776 0.3194 -0.0880 0.084 Uiso 1 calc R . . C15 C 0.4661(16) 0.2603(12) -0.0860(13) 0.069(3) Uani 1 d . . . H15 H 0.4393 0.2060 -0.1569 0.082 Uiso 1 calc R . . N300 N 0.179(2) -0.0679(16) 0.5453(12) 0.111(5) Uani 1 d . . . C301 C 0.244(2) -0.1174(15) 0.4877(16) 0.091(5) Uani 1 d . . . C302 C 0.326(3) -0.181(2) 0.4098(19) 0.139(9) Uani 1 d . . . H30A H 0.3819 -0.1244 0.3896 0.167 Uiso 1 calc R . . H30B H 0.2556 -0.2333 0.3455 0.167 Uiso 1 calc R . . H30C H 0.3962 -0.2288 0.4425 0.167 Uiso 1 calc R . . N400 N -0.053(3) 0.625(2) 0.363(2) 0.159(9) Uani 1 d . . . C401 C -0.153(3) 0.6803(16) 0.3763(16) 0.101(6) Uani 1 d . . . C402 C -0.272(3) 0.7572(19) 0.3969(19) 0.139(9) Uani 1 d . . . H40A H -0.3239 0.7329 0.4442 0.167 Uiso 1 calc R . . H40B H -0.3435 0.7509 0.3286 0.167 Uiso 1 calc R . . H40C H -0.2287 0.8393 0.4317 0.167 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0481(3) 0.0493(3) 0.0520(3) 0.0163(2) 0.0117(2) 0.00401(18) O41 0.061(6) 0.054(5) 0.091(7) 0.025(4) 0.020(5) 0.003(4) N43 0.078(8) 0.047(5) 0.077(7) 0.028(5) 0.041(6) 0.010(5) O42 0.067(6) 0.059(5) 0.076(6) 0.026(4) 0.003(4) 0.009(4) O44 0.119(9) 0.062(5) 0.110(8) 0.050(6) 0.047(7) 0.042(5) O51 0.063(6) 0.064(5) 0.066(5) 0.031(4) 0.024(4) 0.015(4) N53 0.051(7) 0.072(7) 0.067(7) 0.028(6) -0.002(5) 0.001(5) O52 0.064(6) 0.095(7) 0.065(6) 0.041(5) 0.018(4) 0.007(5) O54 0.095(8) 0.073(6) 0.120(9) 0.065(6) -0.003(6) 0.012(5) O61 0.031(6) 0.132(9) 0.093(7) 0.031(6) -0.019(5) -0.017(5) N63 0.067(8) 0.079(7) 0.048(6) 0.014(5) 0.018(5) 0.006(6) O62 0.133(13) 0.148(13) 0.097(10) 0.019(9) -0.013(8) 0.036(10) O64 0.121(12) 0.236(17) 0.093(9) 0.079(10) -0.039(8) -0.102(12) O100 0.069(6) 0.078(6) 0.058(5) 0.006(4) 0.027(4) 0.006(4) N21 0.049(5) 0.045(4) 0.031(4) 0.013(3) 0.011(3) 0.002(3) C22 0.050(6) 0.035(5) 0.049(6) 0.016(4) 0.015(5) 0.010(4) N23 0.061(6) 0.045(5) 0.053(6) 0.016(4) 0.023(4) 0.005(4) C24 0.067(8) 0.049(6) 0.051(7) 0.022(5) 0.021(5) 0.012(5) N25 0.049(6) 0.055(5) 0.055(6) 0.016(4) 0.019(4) 0.006(4) C26 0.046(6) 0.034(5) 0.044(6) 0.013(4) 0.001(4) 0.012(4) N27 0.079(8) 0.083(7) 0.046(6) 0.007(5) 0.022(5) -0.011(6) C32 0.051(6) 0.037(5) 0.050(6) 0.017(4) 0.019(5) 0.011(4) C33 0.043(6) 0.052(6) 0.051(6) 0.018(5) 0.007(4) 0.007(4) N31 0.046(5) 0.053(5) 0.045(5) 0.021(4) 0.012(4) 0.001(4) C35 0.077(9) 0.056(7) 0.057(7) 0.020(6) 0.033(6) 0.005(6) C34 0.048(7) 0.057(7) 0.079(9) 0.019(6) 0.028(6) 0.007(5) C36 0.058(8) 0.058(6) 0.054(7) 0.019(5) 0.021(5) 0.007(5) C16 0.047(7) 0.054(6) 0.067(8) 0.034(6) 0.026(5) 0.016(4) N11 0.054(6) 0.051(5) 0.067(7) 0.025(5) 0.014(5) 0.001(4) C12 0.044(7) 0.072(8) 0.087(10) 0.039(7) 0.009(6) -0.004(5) C13 0.064(9) 0.072(8) 0.100(12) 0.044(8) 0.025(7) 0.001(6) C14 0.052(8) 0.093(10) 0.092(11) 0.053(9) 0.039(7) 0.026(6) C15 0.061(9) 0.073(8) 0.089(10) 0.037(7) 0.035(7) 0.016(6) N300 0.136(14) 0.131(13) 0.072(9) 0.027(9) 0.039(9) 0.044(11) C301 0.116(14) 0.085(10) 0.099(12) 0.041(9) 0.062(11) 0.035(9) C302 0.21(3) 0.121(16) 0.132(18) 0.049(14) 0.108(19) 0.066(17) N400 0.18(2) 0.146(17) 0.19(2) 0.058(16) 0.101(19) 0.064(16) C401 0.134(18) 0.086(11) 0.094(13) 0.017(9) 0.063(12) 0.016(11) C402 0.21(3) 0.119(16) 0.135(19) 0.057(14) 0.109(19) 0.086(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 Yb1 O61 2.275(8) . ? Yb1 O100 2.326(8) . ? Yb1 O42 2.413(8) . ? Yb1 O51 2.414(8) . ? Yb1 O41 2.420(8) . ? Yb1 N21 2.425(8) . ? Yb1 O52 2.470(9) . ? Yb1 N31 2.506(9) . ? Yb1 N11 2.517(10) . ? O41 N43 1.272(14) . ? N43 O44 1.221(13) . ? N43 O42 1.259(13) . ? O51 N53 1.260(14) . ? N53 O54 1.204(13) . ? N53 O52 1.290(15) . ? O61 N63 1.231(14) . ? N63 O64 1.159(15) . ? N63 O62 1.230(18) . ? N21 C26 1.350(13) . ? N21 C22 1.353(13) . ? C22 N23 1.301(14) . ? C22 C16 1.497(15) . ? N23 C24 1.349(15) . ? C24 N27 1.328(15) . ? C24 N25 1.340(15) . ? N25 C26 1.330(13) . ? C26 C32 1.489(15) . ? C32 C33 1.360(15) . ? C32 N31 1.362(14) . ? C33 C34 1.405(16) . ? N31 C36 1.359(14) . ? C35 C36 1.374(17) . ? C35 C34 1.386(18) . ? C16 N11 1.342(15) . ? C16 C15 1.382(17) . ? N11 C12 1.350(15) . ? C12 C13 1.374(19) . ? C13 C14 1.36(2) . ? C14 C15 1.395(19) . ? N300 C301 1.09(2) . ? C301 C302 1.44(2) . ? N400 C401 1.13(2) . ? C401 C402 1.43(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O61 Yb1 O100 77.4(4) . . ? O61 Yb1 O42 124.9(4) . . ? O100 Yb1 O42 77.9(3) . . ? O61 Yb1 O51 81.8(4) . . ? O100 Yb1 O51 126.3(3) . . ? O42 Yb1 O51 149.8(3) . . ? O61 Yb1 O41 74.2(4) . . ? O100 Yb1 O41 77.5(3) . . ? O42 Yb1 O41 52.7(3) . . ? O51 Yb1 O41 141.3(3) . . ? O61 Yb1 N21 140.6(4) . . ? O100 Yb1 N21 142.0(3) . . ? O42 Yb1 N21 75.5(3) . . ? O51 Yb1 N21 74.4(3) . . ? O41 Yb1 N21 106.2(3) . . ? O61 Yb1 O52 81.2(4) . . ? O100 Yb1 O52 75.9(4) . . ? O42 Yb1 O52 137.1(3) . . ? O51 Yb1 O52 52.3(3) . . ? O41 Yb1 O52 147.0(3) . . ? N21 Yb1 O52 106.8(3) . . ? O61 Yb1 N31 148.6(4) . . ? O100 Yb1 N31 79.9(3) . . ? O42 Yb1 N31 69.9(3) . . ? O51 Yb1 N31 94.8(3) . . ? O41 Yb1 N31 121.3(3) . . ? N21 Yb1 N31 65.7(3) . . ? O52 Yb1 N31 72.5(3) . . ? O61 Yb1 N11 77.8(4) . . ? O100 Yb1 N11 145.6(3) . . ? O42 Yb1 N11 97.4(3) . . ? O51 Yb1 N11 72.6(3) . . ? O41 Yb1 N11 73.0(3) . . ? N21 Yb1 N11 65.4(3) . . ? O52 Yb1 N11 123.0(3) . . ? N31 Yb1 N11 131.1(3) . . ? N43 O41 Yb1 95.4(6) . . ? O44 N43 O42 123.2(13) . . ? O44 N43 O41 120.9(11) . . ? O42 N43 O41 115.8(10) . . ? N43 O42 Yb1 96.1(7) . . ? N53 O51 Yb1 98.0(7) . . ? O54 N53 O51 122.8(13) . . ? O54 N53 O52 122.1(12) . . ? O51 N53 O52 115.1(10) . . ? N53 O52 Yb1 94.5(7) . . ? N63 O61 Yb1 149.5(10) . . ? O64 N63 O62 121.1(15) . . ? O64 N63 O61 121.0(15) . . ? O62 N63 O61 117.8(13) . . ? C26 N21 C22 114.3(8) . . ? C26 N21 Yb1 122.2(6) . . ? C22 N21 Yb1 123.5(7) . . ? N23 C22 N21 125.7(10) . . ? N23 C22 C16 119.6(10) . . ? N21 C22 C16 114.7(9) . . ? C22 N23 C24 115.3(9) . . ? N27 C24 N25 118.4(11) . . ? N27 C24 N23 116.7(10) . . ? N25 C24 N23 124.8(10) . . ? C26 N25 C24 115.0(10) . . ? N25 C26 N21 124.9(10) . . ? N25 C26 C32 118.0(9) . . ? N21 C26 C32 117.1(9) . . ? C33 C32 N31 123.7(10) . . ? C33 C32 C26 121.4(10) . . ? N31 C32 C26 114.9(9) . . ? C32 C33 C34 118.9(11) . . ? C36 N31 C32 117.4(9) . . ? C36 N31 Yb1 122.6(7) . . ? C32 N31 Yb1 120.0(7) . . ? C36 C35 C34 120.9(11) . . ? C35 C34 C33 117.6(11) . . ? N31 C36 C35 121.5(11) . . ? N11 C16 C15 123.7(11) . . ? N11 C16 C22 116.7(9) . . ? C15 C16 C22 119.6(11) . . ? C16 N11 C12 116.5(11) . . ? C16 N11 Yb1 119.2(7) . . ? C12 N11 Yb1 124.0(9) . . ? N11 C12 C13 123.7(14) . . ? C14 C13 C12 118.7(13) . . ? C13 C14 C15 119.6(12) . . ? C16 C15 C14 117.7(13) . . ? N300 C301 C302 179(2) . . ? N400 C401 C402 176(3) . . ? _refine_diff_density_max 2.767 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.168 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_5-y _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 5-y _chemical_formula_moiety [YL4(NO3)3(H2O)]2NCMe _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H18 N11 O10 Y ' _chemical_formula_weight 625.34 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.047(9) _cell_length_b 11.668(14) _cell_length_c 13.209(18) _cell_angle_alpha 107.480(10) _cell_angle_beta 103.473(10) _cell_angle_gamma 90.448(10) _cell_volume 1289(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.03 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 2.335 _exptl_absorpt_correction_type empirical (DIFABS) _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4225 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4225 _reflns_number_observed 3246 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1989)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. hydrogen atoms bonded to carbon and nitrogen atoms were added in geometrical positions and given a thermal parameter equivalent to 1.2 times that of the atom to which they were bonded. Hydrogen atoms bonded to oxygen as part of water molecules were not located and not included. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+2.8942P] 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 SHELXL _refine_ls_extinction_coef 0.002(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4225 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2574 _refine_ls_wR_factor_gt 0.2310 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.22820(8) 0.34191(6) 0.20765(5) 0.0473(3) Uani 1 d . . . O41 O 0.2463(8) 0.5497(6) 0.2023(7) 0.0751(18) Uani 1 d . . . N43 N 0.1086(10) 0.5502(7) 0.1559(6) 0.0661(19) Uani 1 d . . . O42 O 0.0271(8) 0.4522(6) 0.1334(6) 0.0727(17) Uani 1 d . . . O44 O 0.0560(11) 0.6376(7) 0.1351(8) 0.095(2) Uani 1 d . . . O51 O 0.3672(7) 0.1612(6) 0.1886(5) 0.0660(15) Uani 1 d . . . N53 N 0.3417(9) 0.1352(7) 0.2690(6) 0.0633(19) Uani 1 d . . . O52 O 0.2543(8) 0.2034(7) 0.3193(5) 0.0695(16) Uani 1 d . . . O54 O 0.3970(9) 0.0526(7) 0.2982(8) 0.095(3) Uani 1 d . . . O61 O 0.4522(8) 0.4291(9) 0.3298(7) 0.098(3) Uani 1 d . . . N63 N 0.5684(9) 0.4240(9) 0.3944(6) 0.072(2) Uani 1 d . . . O62 O 0.5854(17) 0.3302(13) 0.4203(10) 0.158(5) Uani 1 d . . . O64 O 0.6642(14) 0.5020(16) 0.4347(10) 0.189(8) Uani 1 d . . . O100 O 0.1436(8) 0.4460(6) 0.3632(5) 0.0714(16) Uani 1 d . . . N21 N 0.1322(6) 0.2158(5) 0.0166(4) 0.0413(12) Uani 1 d . . . C22 C 0.2108(8) 0.2058(7) -0.0606(6) 0.0470(16) Uani 1 d . . . N23 N 0.1664(8) 0.1430(6) -0.1638(5) 0.0494(14) Uani 1 d . . . C24 C 0.0264(9) 0.0825(7) -0.1927(6) 0.0499(17) Uani 1 d . . . N25 N -0.0623(7) 0.0843(6) -0.1227(5) 0.0490(14) Uani 1 d . . . C26 C -0.0048(7) 0.1519(6) -0.0218(5) 0.0408(14) Uani 1 d . . . N27 N -0.0280(10) 0.0163(7) -0.2967(6) 0.071(2) Uani 1 d . . . H27A H -0.1161 -0.0231 -0.3171 0.10(4) Uiso 1 calc R . . H27B H 0.0250 0.0129 -0.3437 0.06(2) Uiso 1 calc R . . C32 C -0.0964(8) 0.1582(6) 0.0621(5) 0.0404(14) Uani 1 d . . . C33 C -0.2375(8) 0.0954(7) 0.0308(6) 0.0483(16) Uani 1 d . . . H33 H -0.2784 0.0481 -0.0413 0.028(15) Uiso 1 calc R . . N31 N -0.0297(7) 0.2264(6) 0.1636(5) 0.0494(14) Uani 1 d . . . C35 C -0.2522(10) 0.1755(8) 0.2163(7) 0.0595(19) Uani 1 d . . . H35 H -0.3041 0.1848 0.2710 0.09(3) Uiso 1 calc R . . C34 C -0.3164(10) 0.1053(7) 0.1113(7) 0.0574(19) Uani 1 d . . . H34 H -0.4121 0.0645 0.0938 0.11(4) Uiso 1 calc R . . C36 C -0.1070(10) 0.2327(7) 0.2396(6) 0.0573(19) Uani 1 d . . . H36 H -0.0616 0.2777 0.3117 0.09(3) Uiso 1 calc R . . C16 C 0.3642(9) 0.2723(7) -0.0225(6) 0.0502(17) Uani 1 d . . . N11 N 0.4014(7) 0.3475(6) 0.0816(6) 0.0507(14) Uani 1 d . . . C12 C 0.5380(10) 0.4100(8) 0.1147(8) 0.066(2) Uani 1 d . . . H12 H 0.5656 0.4627 0.1858 0.08(3) Uiso 1 calc R . . C13 C 0.6389(10) 0.4018(10) 0.0517(10) 0.074(3) Uani 1 d . . . H13 H 0.7310 0.4494 0.0791 0.07(3) Uiso 1 calc R . . C14 C 0.6039(11) 0.3228(10) -0.0525(10) 0.075(3) Uani 1 d . . . H14 H 0.6728 0.3134 -0.0963 0.15(6) Uiso 1 calc R . . C15 C 0.4637(11) 0.2579(9) -0.0906(8) 0.066(2) Uani 1 d . . . H15 H 0.4356 0.2046 -0.1615 0.06(3) Uiso 1 calc R . . N300 N 0.1785(16) -0.0703(12) 0.5462(9) 0.114(4) Uani 1 d . . . C301 C 0.2436(15) -0.1213(11) 0.4885(9) 0.085(3) Uani 1 d . . . C302 C 0.327(3) -0.1859(18) 0.4120(15) 0.124(6) Uani 1 d . . . H30A H 0.3013 -0.1611 0.3475 0.15(6) Uiso 1 calc R . . H30B H 0.2999 -0.2708 0.3926 0.27(15) Uiso 1 calc R . . H30C H 0.4340 -0.1689 0.4449 0.20(11) Uiso 1 calc R . . N400 N -0.058(2) 0.6229(17) 0.3646(18) 0.163(7) Uani 1 d . . . C401 C -0.1504(19) 0.6832(12) 0.3801(12) 0.102(4) Uani 1 d . . . C402 C -0.261(2) 0.7596(14) 0.4014(14) 0.131(6) Uani 1 d . . . H40A H -0.2674 0.7739 0.4758 0.157 Uiso 1 calc R . . H40B H -0.3578 0.7238 0.3526 0.157 Uiso 1 calc R . . H40C H -0.2367 0.8347 0.3909 0.157 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0450(5) 0.0502(5) 0.0447(4) 0.0146(3) 0.0074(3) 0.0029(3) O41 0.068(4) 0.061(4) 0.108(5) 0.036(4) 0.033(4) 0.013(3) N43 0.082(6) 0.062(4) 0.066(4) 0.030(4) 0.025(4) 0.013(4) O42 0.068(4) 0.066(4) 0.077(4) 0.023(3) 0.002(3) 0.008(3) O44 0.111(6) 0.075(5) 0.127(7) 0.059(5) 0.043(5) 0.042(4) O51 0.073(4) 0.064(3) 0.067(4) 0.029(3) 0.019(3) 0.013(3) N53 0.058(4) 0.069(4) 0.061(4) 0.032(4) -0.004(3) 0.008(3) O52 0.071(4) 0.087(4) 0.057(3) 0.036(3) 0.010(3) 0.008(3) O54 0.092(5) 0.080(5) 0.117(6) 0.059(5) -0.005(5) 0.016(4) O61 0.061(4) 0.137(7) 0.080(5) 0.029(5) -0.009(4) -0.017(4) N63 0.065(5) 0.099(6) 0.041(3) 0.010(4) 0.004(3) 0.000(4) O62 0.200(13) 0.146(10) 0.109(8) 0.038(8) 0.001(8) 0.069(9) O64 0.148(10) 0.285(18) 0.109(8) 0.094(10) -0.051(7) -0.133(12) O100 0.072(4) 0.076(4) 0.055(3) 0.002(3) 0.018(3) 0.005(3) N21 0.039(3) 0.046(3) 0.041(3) 0.018(2) 0.010(2) 0.008(2) C22 0.045(4) 0.054(4) 0.052(4) 0.026(3) 0.018(3) 0.012(3) N23 0.058(4) 0.054(3) 0.042(3) 0.017(3) 0.018(3) 0.008(3) C24 0.054(4) 0.060(4) 0.040(4) 0.022(3) 0.011(3) 0.008(3) N25 0.051(4) 0.051(3) 0.045(3) 0.016(3) 0.010(3) 0.004(3) C26 0.036(3) 0.045(3) 0.043(3) 0.017(3) 0.009(3) 0.015(3) N27 0.083(6) 0.083(5) 0.041(4) 0.009(3) 0.018(3) -0.006(4) C32 0.042(4) 0.038(3) 0.043(3) 0.012(3) 0.014(3) 0.011(3) C33 0.042(4) 0.051(4) 0.050(4) 0.012(3) 0.012(3) 0.007(3) N31 0.050(3) 0.061(4) 0.039(3) 0.019(3) 0.010(2) 0.001(3) C35 0.058(5) 0.070(5) 0.061(5) 0.026(4) 0.026(4) 0.007(4) C34 0.055(5) 0.057(4) 0.063(5) 0.019(4) 0.020(4) 0.002(4) C36 0.071(5) 0.056(4) 0.042(4) 0.010(3) 0.017(3) 0.002(4) C16 0.050(4) 0.053(4) 0.056(4) 0.027(3) 0.016(3) 0.015(3) N11 0.041(3) 0.048(3) 0.065(4) 0.020(3) 0.013(3) 0.007(2) C12 0.052(5) 0.069(5) 0.075(6) 0.033(5) 0.000(4) -0.011(4) C13 0.051(5) 0.080(6) 0.106(8) 0.054(6) 0.016(5) -0.008(4) C14 0.057(5) 0.092(7) 0.098(8) 0.051(6) 0.032(5) 0.016(5) C15 0.068(6) 0.077(6) 0.069(6) 0.037(5) 0.026(4) 0.008(4) N300 0.143(11) 0.140(10) 0.078(7) 0.036(7) 0.058(7) 0.050(8) C301 0.098(8) 0.097(8) 0.068(6) 0.026(6) 0.035(6) 0.023(6) C302 0.143(17) 0.136(14) 0.129(13) 0.052(11) 0.089(12) 0.059(11) N400 0.154(15) 0.160(14) 0.209(19) 0.067(14) 0.095(14) 0.063(12) C401 0.124(12) 0.087(8) 0.101(9) 0.023(7) 0.048(8) 0.023(8) C402 0.177(17) 0.110(11) 0.124(12) 0.044(10) 0.060(12) 0.060(11) _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 Y1 O61 2.281(7) . ? Y1 O100 2.352(7) . ? Y1 O42 2.427(6) . ? Y1 O51 2.441(7) . ? Y1 O41 2.452(7) . ? Y1 N21 2.452(6) . ? Y1 O52 2.473(6) . ? Y1 N31 2.539(7) . ? Y1 N11 2.552(7) . ? O41 N43 1.254(10) . ? N43 O44 1.208(10) . ? N43 O42 1.273(10) . ? O51 N53 1.257(10) . ? N53 O54 1.212(9) . ? N53 O52 1.280(11) . ? O61 N63 1.204(11) . ? N63 O64 1.159(13) . ? N63 O62 1.242(14) . ? N21 C26 1.347(9) . ? N21 C22 1.352(9) . ? C22 N23 1.302(10) . ? C22 C16 1.485(11) . ? N23 C24 1.359(10) . ? C24 N27 1.330(11) . ? C24 N25 1.354(10) . ? N25 C26 1.306(9) . ? C26 C32 1.516(10) . ? C32 N31 1.331(9) . ? C32 C33 1.377(10) . ? C33 C34 1.391(11) . ? N31 C36 1.336(10) . ? C35 C34 1.366(12) . ? C35 C36 1.393(12) . ? C16 N11 1.352(11) . ? C16 C15 1.392(12) . ? N11 C12 1.338(10) . ? C12 C13 1.357(14) . ? C13 C14 1.370(16) . ? C14 C15 1.377(14) . ? N300 C301 1.106(15) . ? C301 C302 1.434(18) . ? N400 C401 1.116(18) . ? C401 C402 1.37(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 O61 Y1 O100 78.3(3) . . ? O61 Y1 O42 124.6(3) . . ? O100 Y1 O42 77.6(3) . . ? O61 Y1 O51 82.1(3) . . ? O100 Y1 O51 125.3(2) . . ? O42 Y1 O51 150.2(2) . . ? O61 Y1 O41 74.8(3) . . ? O100 Y1 O41 78.7(3) . . ? O42 Y1 O41 51.9(2) . . ? O51 Y1 O41 142.4(2) . . ? O61 Y1 N21 140.2(3) . . ? O100 Y1 N21 141.5(2) . . ? O42 Y1 N21 76.2(2) . . ? O51 Y1 N21 74.2(2) . . ? O41 Y1 N21 105.7(2) . . ? O61 Y1 O52 82.0(3) . . ? O100 Y1 O52 75.2(3) . . ? O42 Y1 O52 136.4(2) . . ? O51 Y1 O52 51.7(2) . . ? O41 Y1 O52 148.1(3) . . ? N21 Y1 O52 106.2(2) . . ? O61 Y1 N31 150.0(3) . . ? O100 Y1 N31 80.1(2) . . ? O42 Y1 N31 69.8(2) . . ? O51 Y1 N31 93.8(2) . . ? O41 Y1 N31 120.8(2) . . ? N21 Y1 N31 64.58(19) . . ? O52 Y1 N31 72.5(2) . . ? O61 Y1 N11 77.9(3) . . ? O100 Y1 N11 147.0(2) . . ? O42 Y1 N11 97.7(2) . . ? O51 Y1 N11 73.1(2) . . ? O41 Y1 N11 73.2(2) . . ? N21 Y1 N11 64.9(2) . . ? O52 Y1 N11 123.2(2) . . ? N31 Y1 N11 129.4(2) . . ? N43 O41 Y1 96.1(5) . . ? O44 N43 O41 122.7(8) . . ? O44 N43 O42 122.0(9) . . ? O41 N43 O42 115.3(7) . . ? N43 O42 Y1 96.8(5) . . ? N53 O51 Y1 97.6(5) . . ? O54 N53 O51 122.9(10) . . ? O54 N53 O52 122.0(9) . . ? O51 N53 O52 115.2(7) . . ? N53 O52 Y1 95.4(4) . . ? N63 O61 Y1 151.3(8) . . ? O64 N63 O61 123.9(12) . . ? O64 N63 O62 118.2(12) . . ? O61 N63 O62 117.9(11) . . ? C26 N21 C22 113.6(6) . . ? C26 N21 Y1 123.3(4) . . ? C22 N21 Y1 123.1(5) . . ? N23 C22 N21 126.7(7) . . ? N23 C22 C16 117.3(7) . . ? N21 C22 C16 116.0(6) . . ? C22 N23 C24 114.2(6) . . ? N27 C24 N25 117.3(7) . . ? N27 C24 N23 118.2(7) . . ? N25 C24 N23 124.5(7) . . ? C26 N25 C24 114.9(6) . . ? N25 C26 N21 126.0(6) . . ? N25 C26 C32 118.3(6) . . ? N21 C26 C32 115.7(6) . . ? N31 C32 C33 124.8(6) . . ? N31 C32 C26 115.2(6) . . ? C33 C32 C26 120.0(6) . . ? C32 C33 C34 117.3(7) . . ? C32 N31 C36 116.6(6) . . ? C32 N31 Y1 121.1(5) . . ? C36 N31 Y1 122.3(5) . . ? C34 C35 C36 118.4(7) . . ? C35 C34 C33 119.5(7) . . ? N31 C36 C35 123.4(7) . . ? N11 C16 C15 122.0(8) . . ? N11 C16 C22 116.4(7) . . ? C15 C16 C22 121.6(8) . . ? C12 N11 C16 116.2(7) . . ? C12 N11 Y1 124.3(6) . . ? C16 N11 Y1 119.0(5) . . ? N11 C12 C13 124.7(9) . . ? C12 C13 C14 119.4(8) . . ? C13 C14 C15 118.0(9) . . ? C14 C15 C16 119.7(10) . . ? N300 C301 C302 178.7(14) . . ? N400 C401 C402 178(2) . . ? _refine_diff_density_max 1.014 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.135 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_6-Sc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H16 N9 O10 Sc' _chemical_formula_weight 527.33 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' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.891(11) _cell_length_b 10.784(12) _cell_length_c 11.785(14) _cell_angle_alpha 100.657(10) _cell_angle_beta 92.604(10) _cell_angle_gamma 93.970(10) _cell_volume 1106(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3944 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.87 _reflns_number_total 3944 _reflns_number_gt 3007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.6366P] 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 SHELXL _refine_ls_extinction_coef 0.011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3944 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.69308(7) 0.70164(6) 0.77421(5) 0.0344(2) Uani 1 d . . . N11 N 0.8846(3) 0.5630(3) 0.7129(2) 0.0377(6) Uani 1 d . . . C12 C 1.0172(4) 0.5986(4) 0.6747(3) 0.0468(9) Uani 1 d . . . H12 H 1.0380 0.6833 0.6707 0.056 Uiso 1 calc R . . C13 C 1.1254(4) 0.5140(4) 0.6406(3) 0.0530(10) Uani 1 d . . . H13 H 1.2159 0.5420 0.6135 0.064 Uiso 1 calc R . . C14 C 1.0973(4) 0.3894(4) 0.6472(3) 0.0538(10) Uani 1 d . . . H14 H 1.1689 0.3319 0.6258 0.065 Uiso 1 calc R . . C15 C 0.9612(4) 0.3499(4) 0.6861(3) 0.0467(8) Uani 1 d . . . H15 H 0.9392 0.2657 0.6915 0.056 Uiso 1 calc R . . C16 C 0.8579(4) 0.4397(3) 0.7170(3) 0.0358(7) Uani 1 d . . . N21 N 0.6211(3) 0.5021(2) 0.7886(2) 0.0321(6) Uani 1 d . . . N23 N 0.6696(3) 0.2857(3) 0.7576(2) 0.0398(6) Uani 1 d . . . C22 C 0.7075(3) 0.4044(3) 0.7559(2) 0.0334(7) Uani 1 d . . . C24 C 0.5274(4) 0.2634(3) 0.7930(3) 0.0422(8) Uani 1 d . . . N25 N 0.4363(3) 0.3553(3) 0.8358(2) 0.0416(7) Uani 1 d . . . C26 C 0.4896(3) 0.4713(3) 0.8310(3) 0.0341(7) Uani 1 d . . . N31 N 0.4671(3) 0.6946(3) 0.8694(2) 0.0378(6) Uani 1 d . . . C32 C 0.4024(3) 0.5801(3) 0.8783(3) 0.0345(7) Uani 1 d . . . C33 C 0.2658(4) 0.5648(4) 0.9279(3) 0.0450(8) Uani 1 d . . . H33 H 0.2240 0.4848 0.9331 0.054 Uiso 1 calc R . . C34 C 0.1922(4) 0.6731(4) 0.9699(3) 0.0539(10) Uani 1 d . . . H34 H 0.1017 0.6663 1.0058 0.065 Uiso 1 calc R . . C35 C 0.2547(4) 0.7886(4) 0.9577(3) 0.0573(10) Uani 1 d . . . H35 H 0.2051 0.8612 0.9820 0.069 Uiso 1 calc R . . C36 C 0.3916(4) 0.7967(4) 0.9091(3) 0.0512(9) Uani 1 d . . . H36 H 0.4344 0.8763 0.9033 0.061 Uiso 1 calc R . . O41 O 0.8821(3) 0.8445(2) 0.7645(3) 0.0547(7) Uani 1 d . . . O42 O 0.6549(3) 0.9000(2) 0.7491(3) 0.0592(7) Uani 1 d . . . N43 N 0.7972(4) 0.9323(3) 0.7526(3) 0.0616(9) Uani 1 d . . . O44 O 0.8461(4) 1.0365(3) 0.7454(4) 0.1067(14) Uani 1 d . . . O61 O 0.8194(3) 0.6848(3) 0.9361(2) 0.0515(6) Uani 1 d . . . N63 N 0.8110(3) 0.7880(3) 1.0064(3) 0.0531(8) Uani 1 d . . . O64 O 0.8787(4) 0.8064(4) 1.0997(3) 0.0929(12) Uani 1 d . . . O62 O 0.7276(4) 0.8635(3) 0.9702(3) 0.0839(10) Uani 1 d . . . N53 N 0.5681(4) 0.6644(3) 0.5544(3) 0.0528(8) Uani 1 d . . . O51 O 0.7082(3) 0.6846(3) 0.5792(2) 0.0662(8) Uani 1 d . . . O54 O 0.5145(4) 0.6467(4) 0.4555(2) 0.0856(10) Uani 1 d . . . O52 O 0.4894(3) 0.6630(3) 0.6412(2) 0.0573(7) Uani 1 d . . . N27 N 0.4789(4) 0.1447(3) 0.7876(3) 0.0598(9) Uani 1 d . . . H27A H 0.3913 0.1262 0.8108 0.072 Uiso 1 calc R . . H27B H 0.5348 0.0853 0.7609 0.072 Uiso 1 calc R . . O100 O 1.2089(6) 0.9715(7) 0.7199(5) 0.180(3) Uani 1 d . . . C101 C 1.1873(12) 0.9425(14) 0.6026(8) 0.215(7) Uani 1 d . . . H10A H 1.1268 0.8622 0.5846 0.257 Uiso 1 calc R . . H10B H 1.1248 1.0053 0.5803 0.257 Uiso 1 calc R . . C102 C 1.2888(13) 0.9341(13) 0.5390(8) 0.226(6) Uani 1 d . . . H10C H 1.3131 1.0147 0.5180 0.271 Uiso 1 calc R . . H10D H 1.2590 0.8723 0.4707 0.271 Uiso 1 calc R . . H10E H 1.3758 0.9086 0.5774 0.271 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0300(3) 0.0377(4) 0.0364(3) 0.0076(2) 0.0053(3) 0.0048(2) N11 0.0370(15) 0.0441(17) 0.0326(14) 0.0066(11) 0.0080(12) 0.0068(12) C12 0.0382(18) 0.055(2) 0.048(2) 0.0078(16) 0.0148(17) 0.0029(16) C13 0.0331(18) 0.080(3) 0.046(2) 0.0066(18) 0.0167(17) 0.0063(18) C14 0.042(2) 0.061(3) 0.059(2) 0.0055(19) 0.0135(18) 0.0177(18) C15 0.0415(19) 0.050(2) 0.051(2) 0.0069(16) 0.0141(17) 0.0145(16) C16 0.0341(16) 0.0444(19) 0.0299(15) 0.0063(13) 0.0043(14) 0.0100(13) N21 0.0261(13) 0.0387(15) 0.0320(13) 0.0061(11) 0.0042(11) 0.0063(11) N23 0.0405(15) 0.0386(16) 0.0404(15) 0.0055(12) 0.0037(13) 0.0082(12) C22 0.0341(16) 0.0401(19) 0.0263(14) 0.0047(12) 0.0042(13) 0.0066(13) C24 0.0417(19) 0.040(2) 0.0438(19) 0.0070(15) 0.0026(16) -0.0005(15) N25 0.0376(15) 0.0436(17) 0.0438(16) 0.0089(12) 0.0046(13) 0.0018(12) C26 0.0293(16) 0.0458(19) 0.0278(15) 0.0090(13) 0.0005(13) 0.0027(13) N31 0.0380(15) 0.0417(16) 0.0358(14) 0.0079(11) 0.0102(12) 0.0117(12) C32 0.0284(15) 0.0474(19) 0.0280(15) 0.0067(13) 0.0020(13) 0.0046(13) C33 0.0355(17) 0.059(2) 0.0427(18) 0.0123(16) 0.0073(16) 0.0076(15) C34 0.0363(18) 0.083(3) 0.047(2) 0.0137(19) 0.0144(17) 0.0186(19) C35 0.048(2) 0.068(3) 0.057(2) 0.0055(19) 0.0128(19) 0.026(2) C36 0.051(2) 0.050(2) 0.054(2) 0.0063(17) 0.0127(18) 0.0178(17) O41 0.0391(13) 0.0439(15) 0.0822(19) 0.0136(13) 0.0066(13) 0.0039(11) O42 0.0466(15) 0.0472(16) 0.083(2) 0.0080(13) -0.0006(14) 0.0094(12) N43 0.056(2) 0.040(2) 0.088(3) 0.0135(17) -0.0002(19) -0.0022(16) O44 0.092(3) 0.0423(19) 0.187(4) 0.034(2) 0.000(3) -0.0114(18) O61 0.0511(15) 0.0631(17) 0.0363(13) -0.0004(12) 0.0011(12) 0.0031(12) N63 0.0380(16) 0.069(2) 0.0471(18) -0.0013(16) 0.0038(15) 0.0030(15) O64 0.076(2) 0.136(3) 0.0491(18) -0.0234(19) -0.0152(17) 0.001(2) O62 0.064(2) 0.076(2) 0.115(3) 0.016(2) 0.0134(19) 0.0250(17) N53 0.062(2) 0.057(2) 0.0406(17) 0.0084(14) -0.0022(17) 0.0165(16) O51 0.0517(17) 0.107(2) 0.0429(15) 0.0126(14) 0.0090(13) 0.0257(15) O54 0.101(3) 0.115(3) 0.0375(15) 0.0078(16) -0.0201(16) 0.021(2) O52 0.0513(15) 0.0735(19) 0.0473(15) 0.0175(13) -0.0019(13) -0.0065(13) N27 0.0529(19) 0.0441(19) 0.082(2) 0.0087(16) 0.0170(18) 0.0018(15) O100 0.100(3) 0.286(8) 0.123(4) -0.018(5) 0.024(3) -0.062(4) C101 0.138(8) 0.389(19) 0.088(6) 0.000(8) 0.037(6) -0.080(9) C102 0.195(11) 0.342(19) 0.103(7) -0.041(9) 0.002(8) -0.006(11) _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 Sc1 O61 2.213(3) . ? Sc1 O41 2.222(3) . ? Sc1 N21 2.242(4) . ? Sc1 O42 2.259(4) . ? Sc1 O51 2.283(4) . ? Sc1 O52 2.304(3) . ? Sc1 N31 2.349(3) . ? Sc1 N11 2.392(3) . ? Sc1 O62 2.617(4) . ? N11 C12 1.338(4) . ? N11 C16 1.344(4) . ? C12 C13 1.393(5) . ? C13 C14 1.367(6) . ? C14 C15 1.381(5) . ? C15 C16 1.391(5) . ? C16 C22 1.481(5) . ? N21 C26 1.337(4) . ? N21 C22 1.356(4) . ? N23 C22 1.305(4) . ? N23 C24 1.368(5) . ? C24 N27 1.312(5) . ? C24 N25 1.362(5) . ? N25 C26 1.318(4) . ? C26 C32 1.487(5) . ? N31 C36 1.350(4) . ? N31 C32 1.350(4) . ? C32 C33 1.385(5) . ? C33 C34 1.399(5) . ? C34 C35 1.364(6) . ? C35 C36 1.372(6) . ? O41 N43 1.274(4) . ? O42 N43 1.286(4) . ? N43 O44 1.196(4) . ? O61 N63 1.268(4) . ? N63 O64 1.206(4) . ? N63 O62 1.255(5) . ? N53 O54 1.215(4) . ? N53 O51 1.262(4) . ? N53 O52 1.267(4) . ? O100 C101 1.361(9) . ? C101 C102 1.197(11) . ? 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 O61 Sc1 O41 82.94(12) . . ? O61 Sc1 N21 78.76(10) . . ? O41 Sc1 N21 147.55(10) . . ? O61 Sc1 O42 116.42(10) . . ? O41 Sc1 O42 57.51(11) . . ? N21 Sc1 O42 154.83(11) . . ? O61 Sc1 O51 144.09(11) . . ? O41 Sc1 O51 78.16(11) . . ? N21 Sc1 O51 101.80(11) . . ? O42 Sc1 O51 77.89(12) . . ? O61 Sc1 O52 154.71(10) . . ? O41 Sc1 O52 122.05(11) . . ? N21 Sc1 O52 80.44(10) . . ? O42 Sc1 O52 78.97(10) . . ? O51 Sc1 O52 55.12(11) . . ? O61 Sc1 N31 89.36(13) . . ? O41 Sc1 N31 137.00(11) . . ? N21 Sc1 N31 69.62(10) . . ? O42 Sc1 N31 89.70(10) . . ? O51 Sc1 N31 124.94(11) . . ? O52 Sc1 N31 69.92(13) . . ? O61 Sc1 N11 75.37(11) . . ? O41 Sc1 N11 80.57(13) . . ? N21 Sc1 N11 69.03(11) . . ? O42 Sc1 N11 132.28(10) . . ? O51 Sc1 N11 71.61(10) . . ? O52 Sc1 N11 110.11(12) . . ? N31 Sc1 N11 137.92(11) . . ? O61 Sc1 O62 51.29(12) . . ? O41 Sc1 O62 70.83(12) . . ? N21 Sc1 O62 115.30(12) . . ? O42 Sc1 O62 68.54(13) . . ? O51 Sc1 O62 142.90(13) . . ? O52 Sc1 O62 128.84(11) . . ? N31 Sc1 O62 71.48(11) . . ? N11 Sc1 O62 121.02(10) . . ? C12 N11 C16 117.1(3) . . ? C12 N11 Sc1 125.0(2) . . ? C16 N11 Sc1 117.9(2) . . ? N11 C12 C13 122.7(4) . . ? C14 C13 C12 119.3(3) . . ? C13 C14 C15 119.2(3) . . ? C14 C15 C16 118.1(4) . . ? N11 C16 C15 123.6(3) . . ? N11 C16 C22 114.9(3) . . ? C15 C16 C22 121.5(3) . . ? C26 N21 C22 115.2(3) . . ? C26 N21 Sc1 122.1(2) . . ? C22 N21 Sc1 122.7(2) . . ? C22 N23 C24 114.2(3) . . ? N23 C22 N21 125.6(3) . . ? N23 C22 C16 119.1(3) . . ? N21 C22 C16 115.3(3) . . ? N27 C24 N25 118.6(3) . . ? N27 C24 N23 116.7(3) . . ? N25 C24 N23 124.6(3) . . ? C26 N25 C24 114.6(3) . . ? N25 C26 N21 125.3(3) . . ? N25 C26 C32 119.6(3) . . ? N21 C26 C32 115.2(3) . . ? C36 N31 C32 117.3(3) . . ? C36 N31 Sc1 124.5(3) . . ? C32 N31 Sc1 118.0(2) . . ? N31 C32 C33 122.7(3) . . ? N31 C32 C26 114.8(3) . . ? C33 C32 C26 122.5(3) . . ? C32 C33 C34 118.3(4) . . ? C35 C34 C33 119.2(4) . . ? C34 C35 C36 119.3(4) . . ? N31 C36 C35 123.1(4) . . ? N43 O41 Sc1 94.9(2) . . ? N43 O42 Sc1 92.8(2) . . ? O44 N43 O41 122.6(4) . . ? O44 N43 O42 122.7(4) . . ? O41 N43 O42 114.7(3) . . ? O44 N43 Sc1 178.4(3) . . ? O41 N43 Sc1 56.51(18) . . ? O42 N43 Sc1 58.21(17) . . ? N63 O61 Sc1 106.7(2) . . ? O64 N63 O62 125.5(4) . . ? O64 N63 O61 120.0(4) . . ? O62 N63 O61 114.5(3) . . ? N63 O62 Sc1 87.3(2) . . ? O54 N53 O51 122.4(4) . . ? O54 N53 O52 123.4(4) . . ? O51 N53 O52 114.2(3) . . ? O54 N53 Sc1 178.8(3) . . ? O51 N53 Sc1 56.59(17) . . ? O52 N53 Sc1 57.56(18) . . ? N53 O51 Sc1 95.9(2) . . ? N53 O52 Sc1 94.8(2) . . ? C102 C101 O100 123.2(10) . . ? _refine_diff_density_max 0.481 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.059 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Cryst. 1983 A39 158. ; #===END