# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1805 data_1-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 N6 Nd O10 ' _chemical_formula_weight 581.56 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 8.327(9) _cell_length_b 10.985(12) _cell_length_c 11.160(14) _cell_angle_alpha 93.763(10) _cell_angle_beta 94.442(10) _cell_angle_gamma 101.419(10) _cell_volume 994(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 2.680 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.482 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 3414 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0617 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3414 _reflns_number_gt 2222 _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^)+(0.1487P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3414 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2179 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.23450(7) 0.17693(6) 0.23608(6) 0.0604(3) Uani 1 d . . . N11 N 0.0214(12) 0.3148(9) 0.1769(9) 0.063(2) Uani 1 d . . . C12 C -0.1340(15) 0.2656(13) 0.1310(13) 0.072(3) Uani 1 d . . . H12 H -0.1675 0.1793 0.1222 0.087 Uiso 1 calc R . . C13 C -0.2466(15) 0.3371(15) 0.0963(14) 0.078(4) Uani 1 d . . . H13 H -0.3533 0.3004 0.0652 0.094 Uiso 1 calc R . . C14 C -0.1947(17) 0.4630(14) 0.1094(14) 0.081(4) Uani 1 d . . . H14 H -0.2668 0.5135 0.0859 0.097 Uiso 1 calc R . . C15 C -0.0373(16) 0.5168(12) 0.1568(13) 0.072(3) Uani 1 d . . . H15 H -0.0042 0.6030 0.1679 0.086 Uiso 1 calc R . . C16 C 0.0696(14) 0.4420(11) 0.1873(10) 0.062(3) Uani 1 d . . . N21 N 0.3293(11) 0.4267(12) 0.2818(8) 0.068(3) Uani 1 d U . . C22 C 0.2488(16) 0.4937(11) 0.2411(15) 0.078(4) Uani 1 d U . . C23 C 0.3118(17) 0.6215(11) 0.2254(10) 0.068(3) Uani 1 d U . . H23 H 0.2485 0.6702 0.1860 0.082 Uiso 1 calc R . . C24 C 0.4713(16) 0.6686(12) 0.2717(12) 0.072(3) Uani 1 d U . . H24 H 0.5165 0.7528 0.2694 0.086 Uiso 1 calc R . . C25 C 0.5647(15) 0.5901(10) 0.3219(11) 0.062(3) Uani 1 d U . . H25 H 0.6745 0.6189 0.3507 0.075 Uiso 1 calc R . . C26 C 0.4868(14) 0.4657(11) 0.3273(12) 0.065(3) Uani 1 d U . . N31 N 0.5052(11) 0.2565(10) 0.3728(10) 0.067(3) Uani 1 d . . . C32 C 0.5827(15) 0.3770(11) 0.3855(10) 0.063(3) Uani 1 d . . . C33 C 0.7341(14) 0.4206(13) 0.4479(12) 0.070(3) Uani 1 d . . . H33 H 0.7814 0.5051 0.4545 0.085 Uiso 1 calc R . . C34 C 0.8147(16) 0.3366(14) 0.5005(13) 0.078(4) Uani 1 d . . . H34 H 0.9165 0.3636 0.5445 0.094 Uiso 1 calc R . . C35 C 0.7399(17) 0.2092(16) 0.4864(16) 0.087(4) Uani 1 d . . . H35 H 0.7930 0.1489 0.5159 0.104 Uiso 1 calc R . . C36 C 0.5864(16) 0.1784(13) 0.4274(15) 0.078(4) Uani 1 d . . . H36 H 0.5327 0.0954 0.4248 0.093 Uiso 1 calc R . . N43 N 0.4371(17) -0.0054(12) 0.1631(11) 0.088(4) Uani 1 d . . . O41 O 0.4723(12) 0.1058(10) 0.1444(11) 0.091(3) Uani 1 d . . . O42 O 0.3062(16) -0.0385(9) 0.2154(12) 0.108(4) Uani 1 d . . . O44 O 0.521(2) -0.0786(15) 0.1343(15) 0.149(6) Uani 1 d . . . N53 N 0.1586(14) 0.1578(10) 0.4927(10) 0.074(3) Uani 1 d . . . O51 O 0.1990(12) 0.0713(8) 0.4399(8) 0.073(2) Uani 1 d . . . O54 O 0.1246(14) 0.1591(10) 0.6003(8) 0.095(3) Uani 1 d . . . O52 O 0.1390(11) 0.2509(8) 0.4357(8) 0.072(2) Uani 1 d . . . O61 O 0.3147(10) 0.2923(7) 0.0497(7) 0.0621(19) Uani 1 d . . . O62 O 0.1422(10) 0.1146(8) 0.0129(8) 0.068(2) Uani 1 d . . . N63 N 0.2221(12) 0.2132(8) -0.0268(8) 0.060(2) Uani 1 d . . . O64 O 0.2030(13) 0.2326(10) -0.1332(8) 0.083(3) Uani 1 d . . . O100 O -0.0321(10) 0.0246(8) 0.2211(8) 0.072(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 0.0607(4) 0.0593(5) 0.0609(4) 0.0037(3) 0.0075(3) 0.0110(3) N11 0.065(5) 0.058(6) 0.066(6) 0.010(4) -0.003(5) 0.013(4) C12 0.069(7) 0.072(8) 0.077(8) 0.011(6) 0.014(6) 0.014(6) C13 0.049(6) 0.098(10) 0.090(9) 0.021(8) 0.006(6) 0.017(6) C14 0.083(8) 0.088(10) 0.089(9) 0.038(8) 0.024(8) 0.046(8) C15 0.079(8) 0.063(7) 0.082(8) 0.015(6) 0.013(7) 0.029(6) C16 0.063(6) 0.070(7) 0.058(6) 0.011(5) 0.005(5) 0.020(5) N21 0.048(4) 0.093(7) 0.053(5) 0.039(5) 0.001(4) -0.017(5) C22 0.070(7) 0.044(6) 0.112(10) -0.028(6) 0.050(8) -0.009(5) C23 0.095(8) 0.058(6) 0.051(5) 0.003(5) -0.002(6) 0.016(6) C24 0.076(7) 0.063(7) 0.074(7) 0.001(6) 0.014(7) 0.008(6) C25 0.069(6) 0.046(6) 0.069(7) 0.004(5) 0.013(6) 0.005(5) C26 0.068(6) 0.059(6) 0.078(7) 0.015(5) 0.025(6) 0.023(5) N31 0.056(5) 0.066(6) 0.084(7) 0.005(5) 0.002(5) 0.023(5) C32 0.077(7) 0.058(6) 0.058(6) 0.006(5) 0.016(6) 0.020(5) C33 0.052(6) 0.085(8) 0.076(8) -0.002(6) 0.014(6) 0.018(6) C34 0.059(6) 0.095(10) 0.081(9) -0.001(7) 0.001(6) 0.022(7) C35 0.066(7) 0.097(11) 0.106(11) 0.032(9) 0.002(7) 0.033(7) C36 0.067(7) 0.061(7) 0.109(11) 0.019(7) 0.007(7) 0.020(6) N43 0.116(10) 0.085(9) 0.081(7) 0.026(6) 0.030(7) 0.054(8) O41 0.080(6) 0.092(7) 0.113(8) 0.008(6) 0.041(6) 0.034(5) O42 0.140(9) 0.074(6) 0.132(9) 0.038(6) 0.078(9) 0.042(6) O44 0.190(14) 0.156(12) 0.159(13) 0.069(10) 0.103(12) 0.121(12) N53 0.086(7) 0.062(6) 0.062(6) 0.008(5) 0.003(6) -0.014(5) O51 0.098(6) 0.056(5) 0.070(5) 0.014(4) 0.013(5) 0.021(4) O52 0.117(8) 0.105(8) 0.048(4) 0.001(4) 0.010(5) -0.010(6) O54 0.085(5) 0.068(5) 0.062(5) 0.004(4) 0.016(4) 0.011(4) O61 0.073(5) 0.062(4) 0.050(4) 0.003(3) 0.008(4) 0.009(4) O64 0.074(5) 0.061(5) 0.067(5) 0.007(4) 0.011(4) 0.006(4) N63 0.072(6) 0.053(5) 0.051(5) -0.011(4) 0.005(5) 0.010(4) O62 0.106(7) 0.095(7) 0.057(5) 0.024(4) 0.016(5) 0.029(6) O100 0.060(4) 0.069(5) 0.076(5) 0.003(4) 0.002(4) -0.008(4) _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 O100 2.488(8) . ? Nd1 O41 2.530(9) . ? Nd1 O42 2.553(10) . ? Nd1 O62 2.556(9) . ? Nd1 O52 2.560(8) . ? Nd1 O61 2.570(8) . ? Nd1 N31 2.586(10) . ? Nd1 N11 2.625(10) . ? Nd1 O51 2.632(9) . ? Nd1 N21 2.703(13) . ? N11 C12 1.347(16) . ? N11 C16 1.370(16) . ? C12 C13 1.386(19) . ? C13 C14 1.36(2) . ? C14 C15 1.38(2) . ? C15 C16 1.364(17) . ? C16 C22 1.546(18) . ? N21 C22 1.179(18) . ? N21 C26 1.345(15) . ? C22 C23 1.425(17) . ? C23 C24 1.373(18) . ? C24 C25 1.388(19) . ? C25 C26 1.398(16) . ? C26 C32 1.523(17) . ? N31 C36 1.341(16) . ? N31 C32 1.346(16) . ? C32 C33 1.373(18) . ? C33 C34 1.38(2) . ? C34 C35 1.41(2) . ? C35 C36 1.36(2) . ? N43 O44 1.207(16) . ? N43 O41 1.234(15) . ? N43 O42 1.277(16) . ? N53 O51 1.203(14) . ? N53 O52 1.255(14) . ? N53 O54 1.270(14) . ? O61 N63 1.270(12) . ? O64 N63 1.279(12) . ? N63 O62 1.224(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 Nd1 O41 117.2(3) . . ? O100 Nd1 O42 74.0(4) . . ? O41 Nd1 O42 49.4(3) . . ? O100 Nd1 O62 71.7(3) . . ? O41 Nd1 O62 73.3(3) . . ? O42 Nd1 O62 79.8(4) . . ? O100 Nd1 O52 83.2(3) . . ? O41 Nd1 O52 142.9(4) . . ? O42 Nd1 O52 118.7(3) . . ? O62 Nd1 O52 143.6(3) . . ? O100 Nd1 O61 118.4(3) . . ? O41 Nd1 O61 68.2(3) . . ? O42 Nd1 O61 109.1(3) . . ? O62 Nd1 O61 50.2(3) . . ? O52 Nd1 O61 131.5(3) . . ? O100 Nd1 N31 142.8(3) . . ? O41 Nd1 N31 69.4(4) . . ? O42 Nd1 N31 89.1(4) . . ? O62 Nd1 N31 138.6(3) . . ? O52 Nd1 N31 76.1(3) . . ? O61 Nd1 N31 98.4(3) . . ? O100 Nd1 N11 77.6(3) . . ? O41 Nd1 N11 137.1(4) . . ? O42 Nd1 N11 146.4(4) . . ? O62 Nd1 N11 74.5(3) . . ? O52 Nd1 N11 74.7(3) . . ? O61 Nd1 N11 69.5(3) . . ? N31 Nd1 N11 124.5(3) . . ? O100 Nd1 O51 70.0(3) . . ? O41 Nd1 O51 106.9(3) . . ? O42 Nd1 O51 70.3(3) . . ? O62 Nd1 O51 136.4(3) . . ? O52 Nd1 O51 48.5(3) . . ? O61 Nd1 O51 171.3(3) . . ? N31 Nd1 O51 73.1(3) . . ? N11 Nd1 O51 116.0(3) . . ? O100 Nd1 N21 135.3(3) . . ? O41 Nd1 N21 105.8(3) . . ? O42 Nd1 N21 150.1(4) . . ? O62 Nd1 N21 111.9(3) . . ? O52 Nd1 N21 68.7(3) . . ? O61 Nd1 N21 66.1(3) . . ? N31 Nd1 N21 63.6(3) . . ? N11 Nd1 N21 62.1(3) . . ? O51 Nd1 N21 109.8(3) . . ? C12 N11 C16 117.6(10) . . ? C12 N11 Nd1 122.6(8) . . ? C16 N11 Nd1 119.7(7) . . ? N11 C12 C13 123.3(13) . . ? C14 C13 C12 117.3(13) . . ? C13 C14 C15 121.1(12) . . ? C16 C15 C14 119.2(13) . . ? C15 C16 N11 121.4(12) . . ? C15 C16 C22 123.0(12) . . ? N11 C16 C22 115.5(10) . . ? C22 N21 C26 123.2(12) . . ? C22 N21 Nd1 120.6(8) . . ? C26 N21 Nd1 114.4(9) . . ? N21 C22 C23 123.6(13) . . ? N21 C22 C16 120.5(10) . . ? C23 C22 C16 115.5(14) . . ? C24 C23 C22 116.3(13) . . ? C23 C24 C25 119.7(12) . . ? C24 C25 C26 117.1(12) . . ? N21 C26 C25 119.8(12) . . ? N21 C26 C32 121.2(11) . . ? C25 C26 C32 119.0(11) . . ? C36 N31 C32 115.0(11) . . ? C36 N31 Nd1 121.9(9) . . ? C32 N31 Nd1 122.8(8) . . ? N31 C32 C33 124.3(12) . . ? N31 C32 C26 114.7(11) . . ? C33 C32 C26 121.0(11) . . ? C32 C33 C34 118.8(13) . . ? C33 C34 C35 118.7(13) . . ? C36 C35 C34 116.9(13) . . ? N31 C36 C35 126.1(13) . . ? O44 N43 O41 122.5(14) . . ? O44 N43 O42 121.8(14) . . ? O41 N43 O42 115.7(11) . . ? O44 N43 Nd1 179.3(14) . . ? O41 N43 Nd1 57.2(6) . . ? O42 N43 Nd1 58.5(6) . . ? N43 O41 Nd1 98.6(7) . . ? N43 O42 Nd1 96.3(7) . . ? O51 N53 O54 123.8(12) . . ? O51 N53 O52 119.1(10) . . ? O52 N53 O54 117.0(12) . . ? N53 O51 Nd1 95.3(7) . . ? N53 O52 Nd1 97.0(7) . . ? N63 O61 Nd1 96.0(6) . . ? N63 O62 Nd1 96.4(6) . . ? O64 N63 O61 121.8(10) . . ? O62 N63 O64 120.9(10) . . ? O61 N63 O62 117.2(9) . . ? O62 N63 Nd1 58.4(5) . . ? _refine_diff_density_max 0.888 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.179 _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., (1983) Acta Cryst A39 158. ; #====END data_2-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 N17 Nd2 O18' _chemical_formula_weight 1442.45 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 11.189(14) _cell_length_b 16.059(17) _cell_length_c 16.320(17) _cell_angle_alpha 106.576(10) _cell_angle_beta 95.158(10) _cell_angle_gamma 95.872(10) _cell_volume 2774(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(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 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.940 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 8908 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.90 _reflns_number_total 8908 _reflns_number_gt 7076 _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^)+(0.1184P)^2^+6.2023P] 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 0.0037(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8908 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.07222(3) 0.35642(2) 0.22511(2) 0.03384(15) Uani 1 d . . . O11 O 0.1330(5) 0.5147(3) 0.3188(3) 0.0495(12) Uani 1 d . . . N13 N 0.0693(6) 0.5508(4) 0.2742(4) 0.0479(16) Uani 1 d . . . O12 O 0.0063(5) 0.5006(3) 0.2062(3) 0.0507(12) Uani 1 d . . . O14 O 0.0708(8) 0.6308(4) 0.2941(4) 0.075(2) Uani 1 d . . . O21 O 0.0820(6) 0.2011(3) 0.2419(4) 0.0562(14) Uani 1 d . . . O22 O 0.1395(6) 0.2225(3) 0.1257(4) 0.0584(15) Uani 1 d . . . N23 N 0.1289(8) 0.1719(4) 0.1736(5) 0.062(2) Uani 1 d . . . O24 O 0.1657(11) 0.1011(4) 0.1545(5) 0.107(3) Uani 1 d . . . N11 N 0.2173(6) 0.4345(4) 0.1432(4) 0.0501(15) Uani 1 d . . . C12 C 0.3184(8) 0.4863(5) 0.1864(6) 0.059(2) Uani 1 d . . . H12 H 0.3397 0.4878 0.2433 0.071 Uiso 1 calc R . . C13 C 0.3929(10) 0.5376(7) 0.1516(9) 0.086(3) Uani 1 d . . . H13 H 0.4631 0.5720 0.1832 0.103 Uiso 1 calc R . . C14 C 0.3590(12) 0.5354(10) 0.0698(10) 0.115(5) Uani 1 d . . . H14 H 0.4063 0.5696 0.0442 0.138 Uiso 1 calc R . . C15 C 0.2558(11) 0.4835(9) 0.0232(8) 0.100(4) Uani 1 d . . . H15 H 0.2348 0.4812 -0.0339 0.120 Uiso 1 calc R . . C16 C 0.1826(8) 0.4342(5) 0.0620(5) 0.0536(19) Uani 1 d . . . N21 N 0.0017(6) 0.3380(4) 0.0607(4) 0.0413(13) Uani 1 d . . . C26 C 0.0686(8) 0.3811(5) 0.0157(5) 0.0499(18) Uani 1 d . . . C24 C -0.0803(12) 0.3290(7) -0.1068(6) 0.081(3) Uani 1 d . . . H24 H -0.1077 0.3255 -0.1634 0.097 Uiso 1 calc R . . C25 C 0.0272(10) 0.3771(6) -0.0678(6) 0.070(3) Uani 1 d . . . H25 H 0.0732 0.4075 -0.0974 0.083 Uiso 1 calc R . . C22 C -0.1056(8) 0.2882(5) 0.0221(5) 0.0500(18) Uani 1 d . . . C23 C -0.1501(9) 0.2843(5) -0.0610(5) 0.062(2) Uani 1 d . . . H23 H -0.2251 0.2526 -0.0862 0.074 Uiso 1 calc R . . N31 N -0.1267(6) 0.2534(4) 0.1545(4) 0.0484(15) Uani 1 d . . . C32 C -0.1812(8) 0.2072(5) 0.2002(6) 0.0551(19) Uani 1 d . . . H32 H -0.1517 0.2187 0.2580 0.066 Uiso 1 calc R . . C33 C -0.2798(8) 0.1428(5) 0.1655(6) 0.057(2) Uani 1 d . . . H33 H -0.3179 0.1136 0.1997 0.068 Uiso 1 calc R . . C34 C -0.3193(9) 0.1237(6) 0.0802(6) 0.067(2) Uani 1 d . . . H34 H -0.3832 0.0794 0.0546 0.081 Uiso 1 calc R . . C35 C -0.2635(9) 0.1708(6) 0.0316(6) 0.062(2) Uani 1 d . . . H35 H -0.2892 0.1580 -0.0269 0.075 Uiso 1 calc R . . C36 C -0.1705(7) 0.2362(4) 0.0706(5) 0.0434(16) Uani 1 d . . . N41 N -0.1052(6) 0.4025(4) 0.3164(4) 0.0443(13) Uani 1 d . . . C42 C -0.2023(7) 0.4275(5) 0.2797(5) 0.0485(17) Uani 1 d . . . H42 H -0.2044 0.4271 0.2225 0.058 Uiso 1 calc R . . C43 C -0.2988(8) 0.4537(5) 0.3228(6) 0.058(2) Uani 1 d . . . H43 H -0.3646 0.4709 0.2959 0.070 Uiso 1 calc R . . C44 C -0.2941(8) 0.4534(6) 0.4067(6) 0.058(2) Uani 1 d . . . H44 H -0.3578 0.4706 0.4377 0.069 Uiso 1 calc R . . C45 C -0.1959(8) 0.4278(5) 0.4460(5) 0.0524(18) Uani 1 d . . . H45 H -0.1921 0.4281 0.5032 0.063 Uiso 1 calc R . . C46 C -0.1023(6) 0.4016(4) 0.3976(4) 0.0391(14) Uani 1 d . . . N51 N 0.0989(5) 0.3583(3) 0.3883(3) 0.0373(12) Uani 1 d . . . C52 C 0.0071(6) 0.3742(4) 0.4366(4) 0.0393(14) Uani 1 d . . . C53 C 0.0136(8) 0.3644(5) 0.5193(5) 0.0514(18) Uani 1 d . . . H53 H -0.0518 0.3734 0.5507 0.062 Uiso 1 calc R . . C54 C 0.1161(9) 0.3416(6) 0.5537(5) 0.058(2) Uani 1 d . . . H54 H 0.1218 0.3350 0.6086 0.070 Uiso 1 calc R . . C55 C 0.2112(8) 0.3284(5) 0.5055(5) 0.0539(19) Uani 1 d . . . H55 H 0.2830 0.3146 0.5284 0.065 Uiso 1 calc R . . C56 C 0.1993(6) 0.3359(4) 0.4228(4) 0.0407(15) Uani 1 d . . . N61 N 0.2853(6) 0.3332(4) 0.2920(4) 0.0463(14) Uani 1 d . . . C62 C 0.2980(6) 0.3167(4) 0.3676(5) 0.0401(15) Uani 1 d . . . C63 C 0.3981(8) 0.2805(6) 0.3913(6) 0.062(2) Uani 1 d . . . H63 H 0.4055 0.2693 0.4443 0.075 Uiso 1 calc R . . C64 C 0.4870(8) 0.2608(7) 0.3383(7) 0.073(3) Uani 1 d . . . H64 H 0.5550 0.2380 0.3551 0.088 Uiso 1 calc R . . C65 C 0.4710(8) 0.2764(7) 0.2597(8) 0.074(3) Uani 1 d . . . H65 H 0.5273 0.2619 0.2210 0.088 Uiso 1 calc R . . C66 C 0.3725(7) 0.3130(6) 0.2383(6) 0.059(2) Uani 1 d . . . H66 H 0.3643 0.3247 0.1856 0.071 Uiso 1 calc R . . Nd2 Nd -0.31941(3) -0.10176(2) 0.30324(2) 0.04189(16) Uani 1 d . . . O31 O -0.3791(7) 0.0464(5) 0.4006(5) 0.0778(19) Uani 1 d . . . O32 O -0.2131(5) 0.0552(4) 0.3445(4) 0.0604(15) Uani 1 d . . . N33 N -0.2910(8) 0.0946(5) 0.3869(5) 0.0613(19) Uani 1 d . . . O34 O -0.2776(8) 0.1749(5) 0.4130(6) 0.099(3) Uani 1 d . . . O41 O -0.2579(6) -0.2468(4) 0.2087(4) 0.0602(15) Uani 1 d . . . N43 N -0.2877(7) -0.2924(5) 0.2542(6) 0.065(2) Uani 1 d . . . O42 O -0.3178(6) -0.2531(4) 0.3272(5) 0.0685(17) Uani 1 d . . . O44 O -0.2874(9) -0.3724(5) 0.2344(7) 0.107(3) Uani 1 d . . . O52 O -0.5324(5) -0.1414(4) 0.3379(4) 0.0592(14) Uani 1 d . . . O51 O -0.4978(5) -0.2111(4) 0.2101(4) 0.0609(15) Uani 1 d . . . O54 O -0.6764(5) -0.2338(5) 0.2494(5) 0.0767(19) Uani 1 d . . . N53 N -0.5713(6) -0.1954(5) 0.2650(5) 0.0568(17) Uani 1 d . . . O61 O -0.4325(6) -0.0265(5) 0.2186(5) 0.084(2) Uani 1 d . . . N63 N -0.5297(7) -0.0381(5) 0.1712(5) 0.0652(19) Uani 1 d . . . O62 O -0.6293(7) -0.0576(6) 0.1901(6) 0.095(2) Uani 1 d . . . O64 O -0.5179(10) -0.0366(9) 0.0972(6) 0.155(5) Uani 1 d . . . N81 N -0.0946(5) -0.1039(4) 0.3560(4) 0.0428(13) Uani 1 d . . . C82 C -0.0637(6) -0.1142(4) 0.4326(5) 0.0450(16) Uani 1 d . . . C83 C 0.0507(7) -0.1358(5) 0.4560(6) 0.060(2) Uani 1 d . . . H83 H 0.0712 -0.1422 0.5102 0.072 Uiso 1 calc R . . C84 C 0.1329(8) -0.1472(6) 0.3947(7) 0.071(3) Uani 1 d . . . H84 H 0.2086 -0.1628 0.4073 0.086 Uiso 1 calc R . . C85 C 0.1011(8) -0.1353(6) 0.3175(7) 0.064(2) Uani 1 d . . . H85 H 0.1556 -0.1428 0.2771 0.076 Uiso 1 calc R . . C86 C -0.0105(6) -0.1124(5) 0.2976(5) 0.0471(17) Uani 1 d . . . C92 C -0.1548(7) -0.0993(4) 0.4951(5) 0.0433(16) Uani 1 d . . . C93 C -0.1275(8) -0.0975(5) 0.5801(6) 0.0551(19) Uani 1 d . . . H93 H -0.0514 -0.1078 0.5995 0.066 Uiso 1 calc R . . C94 C -0.2134(9) -0.0802(6) 0.6357(6) 0.062(2) Uani 1 d . . . H94 H -0.1961 -0.0788 0.6929 0.074 Uiso 1 calc R . . C95 C -0.3264(9) -0.0649(6) 0.6049(6) 0.063(2) Uani 1 d . . . H95 H -0.3856 -0.0515 0.6413 0.076 Uiso 1 calc R . . C96 C -0.3484(9) -0.0700(6) 0.5199(6) 0.062(2) Uani 1 d . . . H96 H -0.4252 -0.0623 0.4989 0.074 Uiso 1 calc R . . N91 N -0.2646(6) -0.0858(4) 0.4643(4) 0.0512(15) Uani 1 d . . . N71 N -0.1634(6) -0.0840(4) 0.1985(4) 0.0500(15) Uani 1 d . . . C72 C -0.0470(7) -0.0956(4) 0.2156(5) 0.0506(18) Uani 1 d . . . C73 C 0.0345(10) -0.0910(6) 0.1566(7) 0.075(3) Uani 1 d . . . H73 H 0.1155 -0.0966 0.1691 0.090 Uiso 1 calc R . . C74 C -0.0064(12) -0.0781(7) 0.0797(7) 0.086(3) Uani 1 d . . . H74 H 0.0466 -0.0771 0.0391 0.103 Uiso 1 calc R . . C75 C -0.1238(12) -0.0666(6) 0.0625(6) 0.076(3) Uani 1 d . . . H75 H -0.1520 -0.0575 0.0108 0.091 Uiso 1 calc R . . C76 C -0.1987(9) -0.0689(5) 0.1236(5) 0.060(2) Uani 1 d . . . H76 H -0.2785 -0.0595 0.1128 0.072 Uiso 1 calc R . . N100 N 0.4490(10) 0.5429(8) 0.4063(8) 0.106(4) Uani 1 d . . . C101 C 0.4171(9) 0.6071(7) 0.4089(7) 0.068(2) Uani 1 d . . . C102 C 0.3747(13) 0.6876(7) 0.4126(9) 0.099(4) Uani 1 d . . . H10A H 0.3571 0.7149 0.4699 0.118 Uiso 1 calc R . . H10B H 0.3025 0.6774 0.3727 0.118 Uiso 1 calc R . . H10C H 0.4357 0.7254 0.3977 0.118 Uiso 1 calc R . . N200 N -0.4185(11) 0.3592(8) 0.0899(8) 0.109(3) Uiso 1 d . . . C201 C -0.4915(12) 0.3151(8) 0.0474(9) 0.087(3) Uiso 1 d . . . C202 C -0.5879(16) 0.2532(12) -0.0061(12) 0.140(6) Uiso 1 d . . . H20A H -0.6182 0.2747 -0.0520 0.168 Uiso 1 calc R . . H20B H -0.6517 0.2449 0.0275 0.168 Uiso 1 calc R . . H20C H -0.5586 0.1983 -0.0298 0.168 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 Nd1 0.0424(2) 0.0320(2) 0.0265(2) 0.00810(13) 0.00341(15) 0.00490(14) O11 0.064(3) 0.041(3) 0.046(3) 0.015(2) 0.008(3) 0.013(2) N13 0.070(4) 0.037(3) 0.042(4) 0.014(3) 0.025(3) 0.011(3) O12 0.070(3) 0.045(3) 0.040(3) 0.016(2) 0.005(3) 0.012(2) O14 0.136(6) 0.033(3) 0.065(4) 0.017(3) 0.038(4) 0.019(3) O21 0.073(4) 0.048(3) 0.046(3) 0.013(2) 0.000(3) 0.006(3) O22 0.095(4) 0.043(3) 0.037(3) 0.007(2) 0.007(3) 0.021(3) N23 0.104(6) 0.036(3) 0.040(4) 0.006(3) -0.010(4) 0.019(3) O24 0.205(10) 0.051(4) 0.065(5) 0.008(3) 0.005(6) 0.056(5) N11 0.059(4) 0.042(3) 0.048(4) 0.009(3) 0.016(3) 0.005(3) C12 0.059(5) 0.052(4) 0.062(5) 0.012(4) 0.010(4) -0.002(4) C13 0.068(6) 0.076(7) 0.116(10) 0.040(6) 0.016(6) -0.015(5) C14 0.087(8) 0.148(12) 0.134(12) 0.090(10) 0.028(9) -0.022(8) C15 0.088(8) 0.142(11) 0.093(8) 0.080(8) 0.017(7) -0.021(7) C16 0.064(5) 0.054(4) 0.056(5) 0.028(4) 0.026(4) 0.012(4) N21 0.056(3) 0.041(3) 0.030(3) 0.014(2) 0.007(3) 0.009(3) C26 0.071(5) 0.046(4) 0.038(4) 0.019(3) 0.013(4) 0.011(4) C24 0.130(9) 0.077(6) 0.034(5) 0.025(4) -0.013(5) -0.002(6) C25 0.099(7) 0.070(6) 0.047(5) 0.028(4) 0.013(5) 0.010(5) C22 0.065(5) 0.036(3) 0.045(4) 0.002(3) 0.008(4) 0.011(3) C23 0.082(6) 0.051(4) 0.043(5) 0.007(3) -0.013(4) 0.005(4) N31 0.065(4) 0.044(3) 0.032(3) 0.011(2) 0.002(3) -0.008(3) C32 0.067(5) 0.044(4) 0.052(5) 0.011(3) 0.012(4) 0.001(4) C33 0.065(5) 0.047(4) 0.058(5) 0.019(3) 0.003(4) -0.001(4) C34 0.065(5) 0.057(5) 0.073(6) 0.020(4) 0.001(5) -0.019(4) C35 0.076(6) 0.058(5) 0.043(5) 0.008(3) -0.007(4) -0.005(4) C36 0.052(4) 0.025(3) 0.046(4) 0.006(3) -0.001(3) -0.005(3) N41 0.052(3) 0.039(3) 0.039(3) 0.005(2) 0.005(3) 0.011(3) C42 0.051(4) 0.055(4) 0.038(4) 0.010(3) 0.001(3) 0.012(3) C43 0.055(4) 0.049(4) 0.071(6) 0.016(4) 0.007(4) 0.011(4) C44 0.058(5) 0.060(5) 0.062(5) 0.020(4) 0.027(4) 0.016(4) C45 0.061(5) 0.051(4) 0.049(4) 0.015(3) 0.017(4) 0.011(4) C46 0.047(4) 0.030(3) 0.037(4) 0.007(2) 0.005(3) -0.003(3) N51 0.047(3) 0.033(3) 0.028(3) 0.006(2) -0.002(2) 0.004(2) C52 0.048(4) 0.035(3) 0.034(4) 0.009(3) 0.008(3) 0.004(3) C53 0.068(5) 0.053(4) 0.034(4) 0.013(3) 0.012(4) 0.006(4) C54 0.082(6) 0.065(5) 0.034(4) 0.022(3) 0.009(4) 0.015(4) C55 0.061(5) 0.056(5) 0.045(5) 0.018(3) -0.008(4) 0.013(4) C56 0.049(4) 0.037(3) 0.031(4) 0.004(3) -0.004(3) 0.009(3) N61 0.055(3) 0.056(4) 0.029(3) 0.010(2) 0.006(3) 0.013(3) C62 0.046(4) 0.028(3) 0.042(4) 0.009(3) -0.002(3) 0.000(3) C63 0.054(5) 0.072(5) 0.064(6) 0.027(4) -0.008(4) 0.019(4) C64 0.051(5) 0.085(7) 0.091(8) 0.033(5) 0.001(5) 0.028(5) C65 0.051(5) 0.078(6) 0.090(8) 0.020(5) 0.008(5) 0.020(4) C66 0.051(4) 0.078(6) 0.053(5) 0.021(4) 0.015(4) 0.023(4) Nd2 0.0391(2) 0.0475(3) 0.0402(3) 0.01603(17) 0.00262(17) 0.00466(16) O31 0.081(5) 0.096(5) 0.069(5) 0.030(4) 0.024(4) 0.040(4) O32 0.063(3) 0.046(3) 0.064(4) 0.003(2) 0.005(3) 0.014(3) N33 0.076(5) 0.060(4) 0.045(4) 0.008(3) -0.010(4) 0.028(4) O34 0.114(6) 0.064(4) 0.103(6) -0.002(4) -0.017(5) 0.044(4) O41 0.057(3) 0.053(3) 0.074(4) 0.022(3) 0.012(3) 0.008(3) N43 0.063(4) 0.044(4) 0.079(6) 0.014(4) -0.012(4) -0.001(3) O42 0.081(4) 0.064(4) 0.066(4) 0.035(3) -0.002(4) 0.002(3) O44 0.138(8) 0.044(4) 0.132(8) 0.025(4) -0.006(6) 0.006(4) O52 0.051(3) 0.075(4) 0.048(3) 0.014(3) 0.010(3) -0.001(3) O51 0.041(3) 0.082(4) 0.053(3) 0.011(3) 0.006(3) 0.007(3) O54 0.042(3) 0.099(5) 0.082(5) 0.025(4) 0.001(3) -0.008(3) N53 0.044(4) 0.066(4) 0.063(5) 0.026(3) 0.003(3) 0.003(3) O61 0.067(4) 0.093(5) 0.100(6) 0.062(4) -0.029(4) -0.015(4) N63 0.068(5) 0.073(5) 0.055(5) 0.029(4) -0.006(4) -0.005(4) O62 0.063(4) 0.128(7) 0.093(6) 0.033(5) 0.007(4) 0.017(4) O64 0.118(7) 0.259(14) 0.078(6) 0.082(8) -0.023(6) -0.075(8) N81 0.039(3) 0.036(3) 0.048(4) 0.006(2) 0.004(3) 0.003(2) C82 0.044(4) 0.034(3) 0.049(4) 0.004(3) -0.004(3) 0.002(3) C83 0.053(5) 0.054(5) 0.068(6) 0.012(4) -0.011(4) 0.018(4) C84 0.045(4) 0.061(5) 0.098(8) 0.006(5) -0.004(5) 0.020(4) C85 0.049(4) 0.061(5) 0.072(6) 0.002(4) 0.011(4) 0.016(4) C86 0.037(3) 0.045(4) 0.050(4) -0.002(3) 0.006(3) 0.007(3) C92 0.050(4) 0.034(3) 0.044(4) 0.009(3) -0.001(3) 0.005(3) C93 0.056(5) 0.050(4) 0.056(5) 0.016(3) -0.010(4) 0.005(3) C94 0.080(6) 0.054(5) 0.049(5) 0.016(4) 0.003(4) 0.001(4) C95 0.073(6) 0.064(5) 0.054(5) 0.017(4) 0.017(4) 0.007(4) C96 0.063(5) 0.080(6) 0.053(5) 0.029(4) 0.017(4) 0.020(4) N91 0.054(4) 0.058(4) 0.045(4) 0.019(3) 0.006(3) 0.012(3) N71 0.064(4) 0.038(3) 0.045(4) 0.007(2) 0.016(3) -0.001(3) C72 0.058(4) 0.032(3) 0.057(5) 0.002(3) 0.022(4) 0.004(3) C73 0.072(6) 0.070(6) 0.086(7) 0.018(5) 0.038(5) 0.011(5) C74 0.116(9) 0.078(7) 0.081(8) 0.030(5) 0.062(7) 0.027(6) C75 0.124(9) 0.066(6) 0.042(5) 0.015(4) 0.031(6) 0.017(6) C76 0.076(6) 0.055(5) 0.045(5) 0.010(3) 0.011(4) 0.003(4) N100 0.089(7) 0.120(9) 0.094(8) 0.001(6) -0.008(5) 0.052(7) C101 0.055(5) 0.079(6) 0.067(6) 0.014(5) 0.010(4) 0.009(5) C102 0.129(10) 0.069(7) 0.096(9) 0.038(6) -0.028(8) 0.002(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 Nd1 O22 2.526(5) . ? Nd1 O11 2.550(6) . ? Nd1 O12 2.591(6) . ? Nd1 N31 2.592(7) . ? Nd1 O21 2.598(6) . ? Nd1 N41 2.630(6) . ? Nd1 N11 2.631(6) . ? Nd1 N61 2.638(7) . ? Nd1 N51 2.645(6) . ? Nd1 N21 2.651(6) . ? O11 N13 1.268(9) . ? N13 O14 1.230(8) . ? N13 O12 1.269(9) . ? O21 N23 1.263(9) . ? O22 N23 1.283(9) . ? N23 O24 1.215(10) . ? N11 C12 1.342(11) . ? N11 C16 1.345(11) . ? C12 C13 1.381(13) . ? C13 C14 1.344(18) . ? C14 C15 1.375(19) . ? C15 C16 1.393(11) . ? C16 C26 1.470(12) . ? N21 C22 1.363(10) . ? N21 C26 1.365(9) . ? C26 C25 1.379(13) . ? C24 C25 1.357(15) . ? C24 C23 1.407(14) . ? C22 C23 1.383(12) . ? C22 C36 1.486(11) . ? N31 C32 1.336(10) . ? N31 C36 1.351(10) . ? C32 C33 1.388(11) . ? C33 C34 1.358(13) . ? C34 C35 1.388(13) . ? C35 C36 1.366(11) . ? N41 C46 1.326(9) . ? N41 C42 1.345(10) . ? C42 C43 1.378(11) . ? C43 C44 1.367(13) . ? C44 C45 1.379(12) . ? C45 C46 1.395(10) . ? C46 C52 1.492(10) . ? N51 C56 1.339(9) . ? N51 C52 1.351(9) . ? C52 C53 1.400(10) . ? C53 C54 1.360(12) . ? C54 C55 1.377(12) . ? C55 C56 1.384(11) . ? C56 C62 1.488(11) . ? N61 C62 1.333(9) . ? N61 C66 1.372(10) . ? C62 C63 1.388(11) . ? C63 C64 1.378(14) . ? C64 C65 1.376(15) . ? C65 C66 1.364(13) . ? Nd2 O61 2.434(7) . ? Nd2 O32 2.548(6) . ? Nd2 O52 2.559(6) . ? Nd2 O51 2.567(6) . ? Nd2 O42 2.571(7) . ? Nd2 N91 2.577(7) . ? Nd2 N81 2.591(7) . ? Nd2 O41 2.598(6) . ? Nd2 N71 2.600(6) . ? Nd2 O31 2.644(7) . ? O31 N33 1.266(11) . ? O32 N33 1.268(9) . ? N33 O34 1.226(10) . ? O41 N43 1.227(10) . ? N43 O44 1.232(10) . ? N43 O42 1.272(11) . ? O52 N53 1.264(9) . ? O51 N53 1.261(9) . ? O54 N53 1.239(9) . ? O61 N63 1.241(10) . ? N63 O64 1.218(11) . ? N63 O62 1.233(11) . ? N81 C82 1.328(10) . ? N81 C86 1.388(9) . ? C82 C83 1.408(11) . ? C82 C92 1.495(11) . ? C83 C84 1.405(15) . ? C84 C85 1.349(15) . ? C85 C86 1.375(12) . ? C86 C72 1.470(12) . ? C92 N91 1.347(10) . ? C92 C93 1.384(12) . ? C93 C94 1.375(13) . ? C94 C95 1.390(14) . ? C95 C96 1.364(13) . ? C96 N91 1.355(11) . ? N71 C76 1.347(12) . ? N71 C72 1.351(11) . ? C72 C73 1.396(12) . ? C73 C74 1.377(16) . ? C74 C75 1.360(17) . ? C75 C76 1.365(13) . ? N100 C101 1.115(14) . ? C101 C102 1.410(16) . ? N200 C201 1.071(15) . ? C201 C202 1.42(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 O22 Nd1 O11 146.5(2) . . ? O22 Nd1 O12 134.37(18) . . ? O11 Nd1 O12 49.67(18) . . ? O22 Nd1 N31 75.2(2) . . ? O11 Nd1 N31 137.2(2) . . ? O12 Nd1 N31 98.2(2) . . ? O22 Nd1 O21 49.89(19) . . ? O11 Nd1 O21 137.00(19) . . ? O12 Nd1 O21 166.0(2) . . ? N31 Nd1 O21 69.2(2) . . ? O22 Nd1 N41 140.6(2) . . ? O11 Nd1 N41 72.15(18) . . ? O12 Nd1 N41 69.65(18) . . ? N31 Nd1 N41 69.9(2) . . ? O21 Nd1 N41 99.56(19) . . ? O22 Nd1 N11 81.0(2) . . ? O11 Nd1 N11 72.50(19) . . ? O12 Nd1 N11 66.0(2) . . ? N31 Nd1 N11 124.9(2) . . ? O21 Nd1 N11 125.7(2) . . ? N41 Nd1 N11 134.64(19) . . ? O22 Nd1 N61 71.2(2) . . ? O11 Nd1 N61 83.81(19) . . ? O12 Nd1 N61 127.55(19) . . ? N31 Nd1 N61 134.3(2) . . ? O21 Nd1 N61 65.54(19) . . ? N41 Nd1 N61 123.5(2) . . ? N11 Nd1 N61 79.3(2) . . ? O22 Nd1 N51 112.79(19) . . ? O11 Nd1 N51 71.63(17) . . ? O12 Nd1 N51 112.40(16) . . ? N31 Nd1 N51 106.06(18) . . ? O21 Nd1 N51 67.58(17) . . ? N41 Nd1 N51 62.19(19) . . ? N11 Nd1 N51 129.0(2) . . ? N61 Nd1 N51 61.90(18) . . ? O22 Nd1 N21 67.82(19) . . ? O11 Nd1 N21 114.64(17) . . ? O12 Nd1 N21 69.24(17) . . ? N31 Nd1 N21 62.67(18) . . ? O21 Nd1 N21 107.93(17) . . ? N41 Nd1 N21 109.6(2) . . ? N11 Nd1 N21 62.4(2) . . ? N61 Nd1 N21 126.89(18) . . ? N51 Nd1 N21 168.54(18) . . ? N13 O11 Nd1 97.8(4) . . ? O14 N13 O11 121.9(7) . . ? O14 N13 O12 121.3(7) . . ? O11 N13 O12 116.7(6) . . ? N13 O12 Nd1 95.8(4) . . ? N23 O21 Nd1 95.3(4) . . ? N23 O22 Nd1 98.2(4) . . ? O24 N23 O21 122.8(8) . . ? O24 N23 O22 120.9(8) . . ? O21 N23 O22 116.3(6) . . ? C12 N11 C16 118.8(7) . . ? C12 N11 Nd1 119.7(6) . . ? C16 N11 Nd1 120.7(5) . . ? N11 C12 C13 123.9(10) . . ? C14 C13 C12 116.9(10) . . ? C13 C14 C15 121.1(10) . . ? C14 C15 C16 119.7(12) . . ? N11 C16 C15 119.5(9) . . ? N11 C16 C26 119.2(6) . . ? C15 C16 C26 121.3(9) . . ? C22 N21 C26 119.8(7) . . ? C22 N21 Nd1 119.4(5) . . ? C26 N21 Nd1 120.8(5) . . ? N21 C26 C25 120.8(8) . . ? N21 C26 C16 116.5(7) . . ? C25 C26 C16 122.7(7) . . ? C25 C24 C23 119.3(9) . . ? C24 C25 C26 120.3(9) . . ? N21 C22 C23 120.6(8) . . ? N21 C22 C36 118.1(7) . . ? C23 C22 C36 121.3(8) . . ? C22 C23 C24 119.2(9) . . ? C32 N31 C36 118.0(7) . . ? C32 N31 Nd1 118.4(6) . . ? C36 N31 Nd1 123.2(5) . . ? N31 C32 C33 123.0(8) . . ? C34 C33 C32 118.2(8) . . ? C33 C34 C35 119.5(8) . . ? C36 C35 C34 119.4(9) . . ? N31 C36 C35 121.7(7) . . ? N31 C36 C22 115.9(6) . . ? C35 C36 C22 122.2(8) . . ? C46 N41 C42 118.9(6) . . ? C46 N41 Nd1 122.1(5) . . ? C42 N41 Nd1 119.1(5) . . ? N41 C42 C43 123.1(7) . . ? C44 C43 C42 117.5(8) . . ? C43 C44 C45 120.7(8) . . ? C44 C45 C46 118.3(7) . . ? N41 C46 C45 121.6(7) . . ? N41 C46 C52 117.5(6) . . ? C45 C46 C52 120.9(6) . . ? C56 N51 C52 118.3(6) . . ? C56 N51 Nd1 120.8(4) . . ? C52 N51 Nd1 120.6(4) . . ? N51 C52 C53 121.5(7) . . ? N51 C52 C46 117.2(6) . . ? C53 C52 C46 121.3(7) . . ? C54 C53 C52 119.7(7) . . ? C53 C54 C55 118.7(7) . . ? C54 C55 C56 119.7(8) . . ? N51 C56 C55 122.1(7) . . ? N51 C56 C62 117.3(6) . . ? C55 C56 C62 120.6(7) . . ? C62 N61 C66 118.6(7) . . ? C62 N61 Nd1 120.6(5) . . ? C66 N61 Nd1 118.1(5) . . ? N61 C62 C63 120.3(8) . . ? N61 C62 C56 117.3(6) . . ? C63 C62 C56 122.4(7) . . ? C64 C63 C62 121.6(9) . . ? C65 C64 C63 117.3(8) . . ? C66 C65 C64 119.9(10) . . ? C65 C66 N61 122.2(9) . . ? O61 Nd2 O32 73.4(2) . . ? O61 Nd2 O52 80.8(2) . . ? O32 Nd2 O52 123.18(19) . . ? O61 Nd2 O51 72.0(2) . . ? O32 Nd2 O51 145.3(2) . . ? O52 Nd2 O51 49.80(19) . . ? O61 Nd2 O42 141.0(2) . . ? O32 Nd2 O42 145.6(2) . . ? O52 Nd2 O42 75.2(2) . . ? O51 Nd2 O42 69.1(2) . . ? O61 Nd2 N91 136.7(3) . . ? O32 Nd2 N91 83.9(2) . . ? O52 Nd2 N91 81.9(2) . . ? O51 Nd2 N91 122.2(2) . . ? O42 Nd2 N91 69.4(2) . . ? O61 Nd2 N81 137.2(2) . . ? O32 Nd2 N81 72.51(19) . . ? O52 Nd2 N81 140.4(2) . . ? O51 Nd2 N81 137.56(19) . . ? O42 Nd2 N81 76.1(2) . . ? N91 Nd2 N81 62.8(2) . . ? O61 Nd2 O41 112.5(3) . . ? O32 Nd2 O41 130.6(2) . . ? O52 Nd2 O41 105.9(2) . . ? O51 Nd2 O41 65.7(2) . . ? O42 Nd2 O41 48.6(2) . . ? N91 Nd2 O41 110.3(2) . . ? N81 Nd2 O41 73.29(19) . . ? O61 Nd2 N71 80.5(3) . . ? O32 Nd2 N71 68.66(19) . . ? O52 Nd2 N71 153.2(2) . . ? O51 Nd2 N71 105.8(2) . . ? O42 Nd2 N71 109.0(2) . . ? N91 Nd2 N71 124.7(2) . . ? N81 Nd2 N71 63.5(2) . . ? O41 Nd2 N71 64.52(19) . . ? O61 Nd2 O31 68.0(3) . . ? O32 Nd2 O31 48.9(2) . . ? O52 Nd2 O31 74.7(2) . . ? O51 Nd2 O31 115.0(2) . . ? O42 Nd2 O31 131.3(2) . . ? N91 Nd2 O31 69.2(2) . . ? N81 Nd2 O31 106.0(2) . . ? O41 Nd2 O31 179.3(2) . . ? N71 Nd2 O31 115.2(2) . . ? N33 O31 Nd2 94.9(5) . . ? N33 O32 Nd2 99.5(5) . . ? O34 N33 O31 123.7(9) . . ? O34 N33 O32 120.1(9) . . ? O31 N33 O32 116.3(7) . . ? N43 O41 Nd2 96.9(5) . . ? O41 N43 O44 124.2(10) . . ? O41 N43 O42 116.9(7) . . ? O44 N43 O42 118.9(9) . . ? N43 O42 Nd2 96.9(5) . . ? N53 O52 Nd2 96.5(4) . . ? N53 O51 Nd2 96.2(5) . . ? O54 N53 O51 121.4(8) . . ? O54 N53 O52 121.1(7) . . ? O51 N53 O52 117.4(6) . . ? N63 O61 Nd2 139.6(6) . . ? O64 N63 O62 120.2(9) . . ? O64 N63 O61 125.3(8) . . ? O62 N63 O61 114.1(9) . . ? C82 N81 C86 119.1(6) . . ? C82 N81 Nd2 120.4(5) . . ? C86 N81 Nd2 119.2(5) . . ? N81 C82 C83 122.3(8) . . ? N81 C82 C92 117.0(6) . . ? C83 C82 C92 120.7(8) . . ? C84 C83 C82 117.7(9) . . ? C85 C84 C83 119.5(8) . . ? C84 C85 C86 121.2(9) . . ? C85 C86 N81 120.2(8) . . ? C85 C86 C72 122.9(8) . . ? N81 C86 C72 116.9(6) . . ? N91 C92 C93 121.9(7) . . ? N91 C92 C82 116.0(7) . . ? C93 C92 C82 122.2(7) . . ? C94 C93 C92 119.8(8) . . ? C93 C94 C95 118.9(9) . . ? C96 C95 C94 118.3(9) . . ? N91 C96 C95 123.7(9) . . ? C92 N91 C96 117.4(7) . . ? C92 N91 Nd2 121.4(5) . . ? C96 N91 Nd2 121.0(6) . . ? C76 N71 C72 118.6(7) . . ? C76 N71 Nd2 120.7(6) . . ? C72 N71 Nd2 120.5(5) . . ? N71 C72 C73 120.2(9) . . ? N71 C72 C86 117.7(6) . . ? C73 C72 C86 122.1(8) . . ? C74 C73 C72 119.2(10) . . ? C75 C74 C73 120.6(9) . . ? C74 C75 C76 117.8(10) . . ? N71 C76 C75 123.6(10) . . ? N100 C101 C102 178.9(13) . . ? N200 C201 C202 176.8(18) . . ? _refine_diff_density_max 1.656 _refine_diff_density_min -2.125 _refine_diff_density_rms 0.186 _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 ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H33 N15 O18' _chemical_formula_weight 1372.54 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 10.518(12) _cell_length_b 15.595(17) _cell_length_c 16.116(17) _cell_angle_alpha 100.722(10) _cell_angle_beta 106.149(10) _cell_angle_gamma 95.784(10) _cell_volume 2462(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(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 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 2.455 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 7591 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1176 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7591 _reflns_number_gt 3598 _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^)+(0.1627P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7591 _refine_ls_number_parameters 721 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2471 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 0.30021(8) 0.01377(6) 0.20701(6) 0.0506(3) Uani 1 d . . . N11 N 0.2417(17) -0.1561(9) 0.1533(11) 0.069(4) Uani 1 d U . . C12 C 0.2159(18) -0.2061(13) 0.2065(13) 0.068(5) Uani 1 d U . . H12 H 0.2290 -0.1799 0.2657 0.081 Uiso 1 calc R . . C13 C 0.170(2) -0.2974(13) 0.1767(15) 0.075(5) Uani 1 d U . . H13 H 0.1526 -0.3307 0.2158 0.090 Uiso 1 calc R . . C14 C 0.150(2) -0.3367(15) 0.0912(17) 0.089(6) Uani 1 d U . . H14 H 0.1216 -0.3974 0.0712 0.107 Uiso 1 calc R . . C15 C 0.1719(18) -0.2861(11) 0.0350(14) 0.064(5) Uani 1 d U . . H15 H 0.1565 -0.3115 -0.0246 0.077 Uiso 1 calc R . . C16 C 0.2174(17) -0.1967(12) 0.0672(14) 0.065(5) Uani 1 d U . . N21 N 0.2965(13) -0.0513(9) 0.0485(9) 0.050(3) Uani 1 d . . . C22 C 0.2369(15) -0.1378(13) 0.0057(12) 0.061(5) Uani 1 d . . . C23 C 0.2064(17) -0.1662(12) -0.0844(12) 0.058(5) Uani 1 d . . . H23 H 0.1701 -0.2252 -0.1104 0.070 Uiso 1 calc R . . C24 C 0.2270(19) -0.1118(14) -0.1359(13) 0.075(6) Uani 1 d . . . H24 H 0.1988 -0.1305 -0.1973 0.090 Uiso 1 calc R . . C25 C 0.2903(19) -0.0287(13) -0.0956(11) 0.065(5) Uani 1 d . . . H25 H 0.3094 0.0096 -0.1300 0.078 Uiso 1 calc R . . C26 C 0.3282(15) 0.0016(11) -0.0036(11) 0.052(4) Uani 1 d . . . N31 N 0.4120(14) 0.1195(9) 0.1303(9) 0.056(4) Uani 1 d . . . C32 C 0.3942(14) 0.0924(10) 0.0386(12) 0.049(4) Uani 1 d . . . C33 C 0.4470(16) 0.1500(10) -0.0032(11) 0.053(4) Uani 1 d . . . H33 H 0.4440 0.1305 -0.0620 0.064 Uiso 1 calc R . . C34 C 0.5015(19) 0.2317(13) 0.0385(12) 0.067(5) Uani 1 d . . . H34 H 0.5323 0.2700 0.0079 0.080 Uiso 1 calc R . . C35 C 0.5141(19) 0.2621(14) 0.1281(15) 0.075(6) Uani 1 d . . . H35 H 0.5507 0.3201 0.1584 0.089 Uiso 1 calc R . . C36 C 0.4690(18) 0.2009(12) 0.1680(13) 0.062(5) Uani 1 d . . . H36 H 0.4800 0.2191 0.2282 0.074 Uiso 1 calc R . . N41 N 0.0519(14) -0.0467(9) 0.1800(9) 0.056(4) Uani 1 d . . . C42 C -0.0200(17) -0.0992(13) 0.1009(12) 0.067(5) Uani 1 d . . . H42 H 0.0041 -0.0908 0.0513 0.080 Uiso 1 calc R . . C43 C -0.1264(18) -0.1643(13) 0.0882(13) 0.063(5) Uani 1 d . . . H43 H -0.1697 -0.2005 0.0325 0.076 Uiso 1 calc R . . C44 C -0.1666(19) -0.1742(14) 0.1607(14) 0.078(6) Uani 1 d . . . H44 H -0.2379 -0.2175 0.1553 0.093 Uiso 1 calc R . . C45 C -0.0993(19) -0.1187(15) 0.2410(14) 0.079(6) Uani 1 d . . . H45 H -0.1266 -0.1240 0.2902 0.094 Uiso 1 calc R . . C46 C 0.0090(18) -0.0547(12) 0.2507(13) 0.065(5) Uani 1 d . . . N51 N 0.2107(13) 0.0382(10) 0.3446(9) 0.056(4) Uani 1 d . . . C53 C 0.016(2) 0.0384(13) 0.3958(14) 0.073(6) Uani 1 d . . . H53 H -0.0739 0.0179 0.3862 0.087 Uiso 1 calc R . . C52 C 0.0805(14) 0.0082(11) 0.3353(10) 0.047(4) Uani 1 d . . . C54 C 0.091(2) 0.1005(15) 0.4717(14) 0.074(6) Uani 1 d . . . H54 H 0.0505 0.1211 0.5145 0.089 Uiso 1 calc R . . C55 C 0.226(3) 0.1328(13) 0.4848(13) 0.085(7) Uani 1 d . . . H55 H 0.2764 0.1754 0.5349 0.102 Uiso 1 calc R . . C56 C 0.280(2) 0.0987(13) 0.4207(12) 0.068(5) Uani 1 d . . . N61 N 0.4652(15) 0.1189(10) 0.3568(10) 0.064(4) Uani 1 d . . . C62 C 0.4288(17) 0.1235(11) 0.4319(12) 0.055(4) Uani 1 d . . . C63 C 0.520(2) 0.1547(15) 0.5151(13) 0.082(6) Uani 1 d . . . H63 H 0.4930 0.1608 0.5657 0.099 Uiso 1 calc R . . C66 C 0.649(3) 0.1758(17) 0.5208(15) 0.101(9) Uani 1 d . . . H66 H 0.7112 0.1946 0.5768 0.122 Uiso 1 calc R . . C64 C 0.6912(19) 0.1715(14) 0.4520(16) 0.086(7) Uani 1 d . . . H64 H 0.7816 0.1868 0.4580 0.103 Uiso 1 calc R . . C65 C 0.5954(19) 0.1428(12) 0.3688(13) 0.069(5) Uani 1 d . . . H65 H 0.6241 0.1402 0.3188 0.083 Uiso 1 calc R . . O11 O 0.2113(13) 0.1553(8) 0.2272(8) 0.063(3) Uani 1 d . . . N13 N 0.1455(15) 0.1515(11) 0.1474(11) 0.062(4) Uani 1 d . . . O12 O 0.1360(13) 0.0812(8) 0.0937(8) 0.065(3) Uani 1 d . . . O14 O 0.0982(14) 0.2168(10) 0.1266(10) 0.085(4) Uani 1 d . . . O21 O 0.4414(12) -0.0662(9) 0.3144(8) 0.068(3) Uani 1 d . . . N23 N 0.5442(16) -0.0596(10) 0.2892(10) 0.063(4) Uani 1 d . . . O22 O 0.5244(12) -0.0281(9) 0.2191(8) 0.070(3) Uani 1 d . . . O24 O 0.6487(14) -0.0836(12) 0.3238(11) 0.100(5) Uani 1 d . . . Sm2 Sm 0.32036(8) 0.43202(6) 0.70307(6) 0.0514(3) Uani 1 d . . . N71 N 0.5478(14) 0.4995(10) 0.8171(10) 0.059(4) Uani 1 d . . . C72 C 0.5618(17) 0.5315(12) 0.9044(11) 0.059(4) Uani 1 d . . . H72 H 0.4867 0.5220 0.9232 0.071 Uiso 1 calc R . . C73 C 0.6761(18) 0.5757(13) 0.9655(14) 0.079(6) Uani 1 d . . . H73 H 0.6798 0.5971 1.0241 0.094 Uiso 1 calc R . . C74 C 0.7862(19) 0.5878(12) 0.9374(14) 0.070(5) Uani 1 d . . . H74 H 0.8664 0.6178 0.9787 0.084 Uiso 1 calc R . . C75 C 0.7848(18) 0.5582(14) 0.8522(12) 0.066(5) Uani 1 d . . . H75 H 0.8604 0.5683 0.8340 0.079 Uiso 1 calc R . . C76 C 0.6651(17) 0.5127(12) 0.7951(11) 0.062(5) Uani 1 d . . . N81 N 0.5239(15) 0.4450(9) 0.6428(10) 0.059(4) Uani 1 d . . . C82 C 0.6500(18) 0.4700(14) 0.6992(15) 0.074(6) Uani 1 d . . . C83 C 0.7659(19) 0.4589(13) 0.6717(15) 0.069(6) Uani 1 d . . . H83 H 0.8516 0.4766 0.7117 0.083 Uiso 1 calc R . . C84 C 0.747(2) 0.4218(15) 0.5854(15) 0.085(6) Uani 1 d . . . H84 H 0.8213 0.4129 0.5662 0.102 Uiso 1 calc R . . C85 C 0.621(2) 0.3972(11) 0.5258(14) 0.068(5) Uani 1 d . . . H85 H 0.6095 0.3740 0.4662 0.081 Uiso 1 calc R . . C86 C 0.512(2) 0.4079(13) 0.5569(13) 0.066(5) Uani 1 d . . . N91 N 0.2699(15) 0.3911(11) 0.5344(10) 0.068(4) Uani 1 d . . . C92 C 0.370(2) 0.3816(12) 0.4950(13) 0.065(5) Uani 1 d . . . C93 C 0.340(3) 0.3518(13) 0.4039(13) 0.079(7) Uani 1 d . . . H93 H 0.4075 0.3448 0.3774 0.094 Uiso 1 calc R . . C94 C 0.205(3) 0.3325(13) 0.3536(14) 0.082(6) Uani 1 d . . . H94 H 0.1828 0.3117 0.2926 0.099 Uiso 1 calc R . . C95 C 0.1064(19) 0.3431(13) 0.3901(13) 0.070(5) Uani 1 d . . . H95 H 0.0166 0.3297 0.3564 0.084 Uiso 1 calc R . . C96 C 0.145(2) 0.3743(14) 0.4789(13) 0.072(5) Uani 1 d . . . H96 H 0.0767 0.3853 0.5041 0.086 Uiso 1 calc R . . O31 O 0.4593(12) 0.3077(8) 0.7162(8) 0.063(3) Uani 1 d . . . N33 N 0.4432(14) 0.2963(11) 0.7879(13) 0.069(4) Uani 1 d . . . O32 O 0.3694(12) 0.3457(8) 0.8210(8) 0.059(3) Uani 1 d . . . O34 O 0.4922(16) 0.2431(11) 0.8295(12) 0.099(5) Uani 1 d . . . O41 O 0.1754(13) 0.2746(9) 0.6456(8) 0.071(4) Uani 1 d . . . N43 N 0.0652(17) 0.2965(14) 0.6482(12) 0.077(5) Uani 1 d . . . O44 O -0.0345(13) 0.2445(11) 0.6265(11) 0.101(5) Uani 1 d . . . O42 O 0.0694(12) 0.3801(11) 0.6754(11) 0.087(4) Uani 1 d . . . O61 O 0.2595(12) 0.5135(12) 0.8217(10) 0.099(5) Uani 1 d . . . N63 N 0.1605(16) 0.5371(12) 0.8359(11) 0.074(5) Uani 1 d . . . O62 O 0.0917(15) 0.5107(17) 0.8748(10) 0.160(11) Uani 1 d . . . O64 O 0.121(3) 0.6041(14) 0.8179(12) 0.148(9) Uani 1 d . . . O51 O 0.3750(12) 0.5843(8) 0.6814(9) 0.070(3) Uani 1 d U . . O52 O 0.1639(12) 0.5355(9) 0.6338(10) 0.080(4) Uani 1 d U . . O54 O 0.2335(16) 0.6716(11) 0.6412(12) 0.105(5) Uani 1 d U . . N53 N 0.2654(16) 0.6003(9) 0.6665(14) 0.083(4) Uani 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0530(5) 0.0498(6) 0.0499(6) 0.0126(4) 0.0164(4) 0.0074(4) N11 0.104(12) 0.042(9) 0.078(11) 0.015(7) 0.055(9) 0.010(8) C12 0.070(11) 0.075(13) 0.061(11) 0.033(9) 0.013(9) 0.012(9) C13 0.083(12) 0.060(12) 0.085(14) 0.032(10) 0.024(11) -0.002(9) C14 0.100(14) 0.056(13) 0.096(16) 0.007(12) 0.011(13) 0.015(11) C15 0.070(10) 0.037(10) 0.080(13) 0.003(9) 0.020(9) 0.009(8) C16 0.044(9) 0.062(12) 0.109(14) 0.032(10) 0.044(9) 0.018(7) N21 0.060(8) 0.042(8) 0.048(8) 0.008(6) 0.018(6) 0.009(6) C22 0.039(9) 0.076(14) 0.056(12) 0.016(10) -0.007(8) 0.005(8) C23 0.058(10) 0.039(11) 0.066(13) -0.003(9) 0.009(9) 0.011(8) C24 0.073(13) 0.082(16) 0.059(13) -0.007(11) 0.018(10) 0.009(11) C25 0.093(14) 0.060(13) 0.044(11) 0.008(9) 0.027(10) 0.012(10) C26 0.041(8) 0.061(12) 0.063(12) 0.025(9) 0.017(8) 0.020(7) N31 0.068(9) 0.055(10) 0.043(8) 0.004(7) 0.026(7) -0.005(7) C32 0.033(7) 0.039(10) 0.081(13) 0.021(8) 0.018(8) 0.015(6) C33 0.070(11) 0.034(10) 0.064(11) -0.002(8) 0.037(9) 0.015(8) C34 0.076(13) 0.080(15) 0.057(13) 0.044(11) 0.024(10) 0.006(10) C35 0.071(12) 0.063(13) 0.104(18) 0.051(12) 0.026(11) 0.013(9) C36 0.077(12) 0.051(12) 0.060(12) 0.012(9) 0.022(9) 0.020(9) N41 0.063(9) 0.049(9) 0.057(9) 0.019(7) 0.017(7) 0.004(7) C42 0.052(10) 0.089(15) 0.049(12) -0.003(10) 0.012(9) 0.004(9) C43 0.058(11) 0.067(13) 0.069(13) 0.020(10) 0.022(9) 0.018(9) C44 0.058(11) 0.077(15) 0.086(16) 0.020(12) 0.012(11) -0.020(10) C45 0.067(12) 0.104(18) 0.080(15) 0.039(13) 0.038(11) 0.007(11) C46 0.068(12) 0.055(12) 0.074(14) 0.011(10) 0.027(10) 0.009(9) N51 0.053(8) 0.067(10) 0.048(9) 0.015(7) 0.012(7) 0.009(7) C53 0.068(13) 0.084(15) 0.095(16) 0.030(12) 0.065(12) 0.008(10) C52 0.035(8) 0.066(12) 0.039(9) 0.024(8) 0.005(7) 0.001(7) C54 0.083(14) 0.095(17) 0.075(15) 0.038(12) 0.056(12) 0.024(12) C55 0.16(2) 0.049(12) 0.051(12) 0.012(9) 0.047(13) 0.001(12) C56 0.102(15) 0.059(13) 0.037(11) 0.018(9) 0.010(10) 0.008(10) N61 0.070(10) 0.074(11) 0.053(10) 0.021(8) 0.016(8) 0.018(8) C62 0.059(10) 0.039(10) 0.056(11) 0.012(8) 0.002(9) -0.003(7) C63 0.081(14) 0.112(19) 0.045(12) 0.032(11) -0.001(10) 0.002(12) C66 0.11(2) 0.11(2) 0.055(15) 0.016(13) 0.007(13) -0.037(15) C64 0.051(11) 0.070(15) 0.11(2) 0.016(13) -0.003(13) -0.020(9) C65 0.077(13) 0.062(13) 0.056(12) -0.003(9) 0.018(10) -0.013(10) O11 0.094(9) 0.058(8) 0.043(8) 0.014(6) 0.027(7) 0.020(6) N13 0.068(10) 0.064(12) 0.066(12) 0.026(9) 0.025(8) 0.030(8) O12 0.086(8) 0.047(8) 0.051(7) 0.008(6) 0.008(6) 0.006(6) O14 0.095(10) 0.085(11) 0.079(10) 0.038(8) 0.013(8) 0.039(8) O21 0.060(7) 0.081(10) 0.059(8) 0.031(7) 0.001(6) 0.014(6) N23 0.063(10) 0.064(11) 0.064(11) 0.019(8) 0.021(8) 0.010(7) O22 0.068(8) 0.080(10) 0.066(9) 0.020(7) 0.029(7) 0.004(6) O24 0.070(9) 0.125(14) 0.101(12) 0.037(10) 0.002(9) 0.050(9) Sm2 0.0467(5) 0.0528(6) 0.0563(6) 0.0113(4) 0.0180(4) 0.0095(4) N71 0.058(9) 0.060(10) 0.059(10) 0.013(7) 0.022(7) 0.007(7) C72 0.063(11) 0.065(12) 0.047(11) 0.023(9) 0.005(8) 0.018(9) C73 0.060(11) 0.072(15) 0.071(14) 0.011(11) -0.021(11) -0.016(9) C74 0.061(11) 0.057(13) 0.082(15) 0.016(10) 0.005(10) 0.015(9) C75 0.059(11) 0.095(15) 0.049(12) 0.020(10) 0.021(9) 0.021(10) C76 0.056(10) 0.072(13) 0.038(10) 0.017(8) -0.015(8) -0.005(8) N81 0.064(9) 0.052(9) 0.074(11) 0.020(7) 0.039(8) 0.013(7) C82 0.054(11) 0.088(15) 0.094(16) 0.037(12) 0.029(11) 0.030(10) C83 0.057(11) 0.077(14) 0.100(17) 0.051(12) 0.036(11) 0.030(9) C84 0.097(17) 0.093(18) 0.066(15) 0.034(13) 0.017(13) 0.007(13) C85 0.102(15) 0.039(11) 0.078(14) 0.011(9) 0.053(13) 0.017(10) C86 0.085(14) 0.063(13) 0.070(14) 0.030(10) 0.036(11) 0.041(10) N91 0.066(10) 0.073(12) 0.064(10) 0.012(8) 0.023(8) 0.013(8) C92 0.094(14) 0.042(11) 0.081(15) 0.027(9) 0.046(12) 0.027(9) C93 0.15(2) 0.053(13) 0.048(12) 0.005(9) 0.052(13) 0.033(13) C94 0.118(19) 0.057(14) 0.059(14) -0.004(10) 0.014(14) 0.016(12) C95 0.067(11) 0.065(13) 0.060(13) -0.001(10) -0.002(10) 0.021(9) C96 0.070(12) 0.093(16) 0.053(13) 0.018(10) 0.016(10) 0.020(10) O31 0.069(8) 0.065(8) 0.065(8) 0.022(6) 0.033(6) 0.008(6) N33 0.043(8) 0.066(11) 0.111(14) 0.038(10) 0.024(9) 0.031(7) O32 0.068(7) 0.056(8) 0.055(7) 0.014(6) 0.020(6) 0.006(6) O34 0.102(11) 0.088(12) 0.128(14) 0.058(11) 0.044(10) 0.024(9) O41 0.063(8) 0.085(10) 0.065(9) 0.002(7) 0.031(6) 0.003(7) N43 0.063(11) 0.090(15) 0.083(13) 0.024(11) 0.024(9) 0.014(10) O44 0.055(8) 0.102(12) 0.124(14) 0.022(10) 0.011(8) -0.030(8) O42 0.052(7) 0.084(12) 0.120(13) 0.011(9) 0.023(8) 0.008(7) O61 0.047(8) 0.149(15) 0.087(11) -0.008(10) 0.025(7) 0.006(8) N63 0.070(11) 0.087(13) 0.083(12) 0.004(10) 0.053(9) 0.033(9) O62 0.067(10) 0.36(3) 0.059(10) 0.106(15) 0.011(8) -0.031(13) O64 0.25(3) 0.118(17) 0.087(13) 0.030(12) 0.042(15) 0.100(18) O51 0.065(7) 0.066(8) 0.093(9) 0.020(7) 0.040(7) 0.018(6) O52 0.059(7) 0.078(9) 0.090(10) 0.015(7) -0.004(7) 0.024(6) O54 0.097(10) 0.076(11) 0.150(15) 0.052(10) 0.032(10) 0.019(8) N53 0.062(8) 0.019(7) 0.160(11) -0.002(8) 0.033(8) 0.021(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O22 2.475(13) . ? Sm1 O11 2.483(12) . ? Sm1 O21 2.550(12) . ? Sm1 N21 2.555(13) . ? Sm1 N41 2.572(14) . ? Sm1 N11 2.583(15) . ? Sm1 O12 2.598(13) . ? Sm1 N31 2.609(13) . ? Sm1 N51 2.621(13) . ? Sm1 N61 2.675(15) . ? N11 C12 1.32(2) . ? N11 C16 1.35(2) . ? C12 C13 1.40(3) . ? C13 C14 1.35(3) . ? C14 C15 1.36(3) . ? C15 C16 1.38(3) . ? C16 C22 1.51(3) . ? N21 C26 1.36(2) . ? N21 C22 1.39(2) . ? C22 C23 1.37(2) . ? C23 C24 1.33(3) . ? C24 C25 1.35(3) . ? C25 C26 1.40(2) . ? C26 C32 1.46(2) . ? N31 C36 1.30(2) . ? N31 C32 1.41(2) . ? C32 C33 1.38(2) . ? C33 C34 1.31(2) . ? C34 C35 1.40(3) . ? C35 C36 1.36(2) . ? N41 C42 1.35(2) . ? N41 C46 1.36(2) . ? C42 C43 1.38(2) . ? C43 C44 1.38(3) . ? C44 C45 1.37(3) . ? C45 C46 1.39(2) . ? C46 C52 1.47(2) . ? N51 C52 1.359(19) . ? N51 C56 1.36(2) . ? C53 C52 1.37(2) . ? C53 C54 1.39(3) . ? C54 C55 1.41(3) . ? C55 C56 1.36(3) . ? C56 C62 1.52(3) . ? N61 C65 1.33(2) . ? N61 C62 1.36(2) . ? C62 C63 1.38(2) . ? C63 C66 1.33(3) . ? C66 C64 1.30(3) . ? C64 C65 1.40(3) . ? O11 N13 1.267(19) . ? N13 O14 1.239(19) . ? N13 O12 1.240(18) . ? O21 N23 1.258(18) . ? N23 O24 1.216(19) . ? N23 O22 1.287(19) . ? Sm2 O61 2.370(14) . ? Sm2 O32 2.497(12) . ? Sm2 O51 2.497(13) . ? Sm2 O31 2.547(13) . ? Sm2 N71 2.556(14) . ? Sm2 N91 2.561(16) . ? Sm2 O42 2.570(13) . ? Sm2 N81 2.590(13) . ? Sm2 O52 2.596(13) . ? Sm2 O41 2.613(13) . ? N71 C72 1.36(2) . ? N71 C76 1.38(2) . ? C72 C73 1.35(2) . ? C73 C74 1.36(3) . ? C74 C75 1.36(3) . ? C75 C76 1.37(2) . ? C76 C82 1.52(3) . ? N81 C82 1.35(2) . ? N81 C86 1.36(2) . ? C82 C83 1.42(2) . ? C83 C84 1.35(3) . ? C84 C85 1.37(3) . ? C85 C86 1.39(2) . ? C86 C92 1.51(3) . ? N91 C96 1.34(2) . ? N91 C92 1.38(2) . ? C92 C93 1.39(3) . ? C93 C94 1.40(3) . ? C94 C95 1.34(3) . ? C95 C96 1.35(3) . ? O31 N33 1.25(2) . ? N33 O34 1.23(2) . ? N33 O32 1.296(18) . ? O41 N43 1.251(19) . ? N43 O44 1.183(19) . ? N43 O42 1.29(2) . ? O61 N63 1.204(17) . ? N63 O62 1.173(18) . ? N63 O64 1.22(2) . ? O51 N53 1.173(17) . ? O52 N53 1.308(19) . ? O54 N53 1.30(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 O22 Sm1 O11 135.3(4) . . ? O22 Sm1 O21 49.6(4) . . ? O11 Sm1 O21 133.3(4) . . ? O22 Sm1 N21 74.3(4) . . ? O11 Sm1 N21 114.9(4) . . ? O21 Sm1 N21 110.3(4) . . ? O22 Sm1 N41 144.2(4) . . ? O11 Sm1 N41 80.4(4) . . ? O21 Sm1 N41 107.8(4) . . ? N21 Sm1 N41 94.3(4) . . ? O22 Sm1 N11 78.3(5) . . ? O11 Sm1 N11 146.0(5) . . ? O21 Sm1 N11 67.5(5) . . ? N21 Sm1 N11 63.1(4) . . ? N41 Sm1 N11 66.4(5) . . ? O22 Sm1 O12 133.8(4) . . ? O11 Sm1 O12 49.5(4) . . ? O21 Sm1 O12 173.9(4) . . ? N21 Sm1 O12 68.8(4) . . ? N41 Sm1 O12 66.6(4) . . ? N11 Sm1 O12 107.3(5) . . ? O22 Sm1 N31 74.9(4) . . ? O11 Sm1 N31 71.9(4) . . ? O21 Sm1 N31 120.9(4) . . ? N21 Sm1 N31 63.9(4) . . ? N41 Sm1 N31 130.8(4) . . ? N11 Sm1 N31 125.2(4) . . ? O12 Sm1 N31 64.4(4) . . ? O22 Sm1 N51 121.0(4) . . ? O11 Sm1 N51 68.2(4) . . ? O21 Sm1 N51 75.1(4) . . ? N21 Sm1 N51 156.8(4) . . ? N41 Sm1 N51 63.0(4) . . ? N11 Sm1 N51 100.8(4) . . ? O12 Sm1 N51 103.4(4) . . ? N31 Sm1 N51 134.0(4) . . ? O22 Sm1 N61 74.5(4) . . ? O11 Sm1 N61 73.1(4) . . ? O21 Sm1 N61 65.0(4) . . ? N21 Sm1 N61 139.8(4) . . ? N41 Sm1 N61 125.7(5) . . ? N11 Sm1 N61 132.3(5) . . ? O12 Sm1 N61 119.8(4) . . ? N31 Sm1 N61 84.1(4) . . ? N51 Sm1 N61 63.3(4) . . ? C12 N11 C16 116.8(16) . . ? C12 N11 Sm1 120.7(13) . . ? C16 N11 Sm1 121.8(11) . . ? N11 C12 C13 122.1(19) . . ? C14 C13 C12 120.0(19) . . ? C13 C14 C15 119(2) . . ? C14 C15 C16 119(2) . . ? N11 C16 C15 123.0(18) . . ? N11 C16 C22 116.3(16) . . ? C15 C16 C22 120.6(19) . . ? C26 N21 C22 116.1(14) . . ? C26 N21 Sm1 121.0(11) . . ? C22 N21 Sm1 121.6(11) . . ? C23 C22 N21 121.5(17) . . ? C23 C22 C16 124.2(18) . . ? N21 C22 C16 114.2(16) . . ? C24 C23 C22 122.0(18) . . ? C23 C24 C25 117.6(19) . . ? C24 C25 C26 121.9(18) . . ? N21 C26 C25 120.6(16) . . ? N21 C26 C32 118.2(15) . . ? C25 C26 C32 121.1(16) . . ? C36 N31 C32 116.5(14) . . ? C36 N31 Sm1 124.2(11) . . ? C32 N31 Sm1 118.6(10) . . ? C33 C32 N31 118.8(14) . . ? C33 C32 C26 124.6(16) . . ? N31 C32 C26 116.4(14) . . ? C34 C33 C32 121.2(16) . . ? C33 C34 C35 121.1(16) . . ? C36 C35 C34 115.3(19) . . ? N31 C36 C35 126.7(19) . . ? C42 N41 C46 117.0(15) . . ? C42 N41 Sm1 119.5(11) . . ? C46 N41 Sm1 118.9(12) . . ? N41 C42 C43 124.7(17) . . ? C42 C43 C44 117.9(18) . . ? C45 C44 C43 118.4(16) . . ? C44 C45 C46 121.6(17) . . ? N41 C46 C45 120.2(17) . . ? N41 C46 C52 116.8(15) . . ? C45 C46 C52 123.0(17) . . ? C52 N51 C56 116.6(15) . . ? C52 N51 Sm1 120.3(10) . . ? C56 N51 Sm1 121.1(11) . . ? C52 C53 C54 117.6(16) . . ? N51 C52 C53 123.6(16) . . ? N51 C52 C46 114.4(14) . . ? C53 C52 C46 121.8(14) . . ? C53 C54 C55 120.9(16) . . ? C56 C55 C54 117(2) . . ? C55 C56 N51 124.4(19) . . ? C55 C56 C62 121.1(18) . . ? N51 C56 C62 114.4(16) . . ? C65 N61 C62 115.8(15) . . ? C65 N61 Sm1 122.6(12) . . ? C62 N61 Sm1 117.8(11) . . ? N61 C62 C63 121.9(17) . . ? N61 C62 C56 117.2(15) . . ? C63 C62 C56 120.7(17) . . ? C66 C63 C62 118(2) . . ? C64 C66 C63 123(2) . . ? C66 C64 C65 117(2) . . ? N61 C65 C64 123.6(19) . . ? N13 O11 Sm1 99.3(10) . . ? O14 N13 O12 123.8(17) . . ? O14 N13 O11 119.9(16) . . ? O12 N13 O11 116.3(15) . . ? N13 O12 Sm1 94.4(10) . . ? N23 O21 Sm1 97.4(10) . . ? O24 N23 O21 124.7(17) . . ? O24 N23 O22 123.2(16) . . ? O21 N23 O22 112.1(15) . . ? N23 O22 Sm1 100.2(10) . . ? O61 Sm2 O32 75.0(5) . . ? O61 Sm2 O51 80.9(5) . . ? O32 Sm2 O51 140.2(4) . . ? O61 Sm2 O31 124.4(5) . . ? O32 Sm2 O31 51.0(4) . . ? O51 Sm2 O31 131.1(4) . . ? O61 Sm2 N71 77.4(4) . . ? O32 Sm2 N71 70.4(4) . . ? O51 Sm2 N71 73.7(5) . . ? O31 Sm2 N71 73.1(4) . . ? O61 Sm2 N91 145.0(5) . . ? O32 Sm2 N91 133.5(5) . . ? O51 Sm2 N91 82.5(5) . . ? O31 Sm2 N91 89.5(5) . . ? N71 Sm2 N91 126.5(5) . . ? O61 Sm2 O42 72.7(5) . . ? O32 Sm2 O42 88.2(5) . . ? O51 Sm2 O42 114.4(5) . . ? O31 Sm2 O42 113.1(5) . . ? N71 Sm2 O42 146.9(5) . . ? N91 Sm2 O42 86.6(5) . . ? O61 Sm2 N81 135.6(5) . . ? O32 Sm2 N81 108.4(4) . . ? O51 Sm2 N81 68.9(4) . . ? O31 Sm2 N81 64.6(4) . . ? N71 Sm2 N81 63.6(5) . . ? N91 Sm2 N81 63.3(5) . . ? O42 Sm2 N81 149.4(5) . . ? O61 Sm2 O52 74.4(6) . . ? O32 Sm2 O52 144.4(4) . . ? O51 Sm2 O52 49.7(4) . . ? O31 Sm2 O52 160.7(4) . . ? N71 Sm2 O52 119.4(5) . . ? N91 Sm2 O52 71.3(5) . . ? O42 Sm2 O52 65.4(5) . . ? N81 Sm2 O52 106.2(5) . . ? O61 Sm2 O41 110.2(5) . . ? O32 Sm2 O41 69.8(4) . . ? O51 Sm2 O41 149.6(5) . . ? O31 Sm2 O41 66.7(4) . . ? N71 Sm2 O41 135.5(5) . . ? N91 Sm2 O41 72.4(4) . . ? O42 Sm2 O41 48.6(4) . . ? N81 Sm2 O41 112.3(4) . . ? O52 Sm2 O41 104.6(4) . . ? C72 N71 C76 114.0(14) . . ? C72 N71 Sm2 122.5(11) . . ? C76 N71 Sm2 123.4(11) . . ? C73 C72 N71 125.0(19) . . ? C72 C73 C74 117(2) . . ? C75 C74 C73 123.3(19) . . ? C74 C75 C76 115.7(18) . . ? C75 C76 N71 124.9(17) . . ? C75 C76 C82 121.9(17) . . ? N71 C76 C82 113.2(14) . . ? C82 N81 C86 116.8(16) . . ? C82 N81 Sm2 120.5(12) . . ? C86 N81 Sm2 121.0(12) . . ? N81 C82 C83 123(2) . . ? N81 C82 C76 117.3(16) . . ? C83 C82 C76 120.1(18) . . ? C84 C83 C82 118(2) . . ? C83 C84 C85 121(2) . . ? C84 C85 C86 118(2) . . ? N81 C86 C85 123.1(19) . . ? N81 C86 C92 115.8(16) . . ? C85 C86 C92 121.1(18) . . ? C96 N91 C92 115.6(17) . . ? C96 N91 Sm2 122.3(12) . . ? C92 N91 Sm2 122.0(13) . . ? N91 C92 C93 121(2) . . ? N91 C92 C86 115.6(17) . . ? C93 C92 C86 123.2(18) . . ? C92 C93 C94 118(2) . . ? C95 C94 C93 122.2(19) . . ? C94 C95 C96 116.3(18) . . ? N91 C96 C95 126.9(19) . . ? N33 O31 Sm2 95.4(9) . . ? O34 N33 O32 117.4(18) . . ? O34 N33 O31 125.7(16) . . ? O32 N33 O31 116.9(15) . . ? N33 O32 Sm2 96.6(10) . . ? N43 O41 Sm2 97.9(12) . . ? O44 N43 O41 122(2) . . ? O42 N43 O44 123.2(18) . . ? O41 N43 O42 114.5(15) . . ? N43 O44 Sm2 99.0(10) . . ? N63 O61 Sm2 138.5(12) . . ? O62 N63 O61 131(2) . . ? O62 N63 O64 105.5(19) . . ? O61 N63 O64 123(2) . . ? N53 O51 Sm2 96.4(10) . . ? N53 O52 Sm2 88.4(9) . . ? O51 N53 O54 122.4(17) . . ? O51 N53 O52 119.4(14) . . ? O54 N53 O52 110.9(16) . . ? _refine_diff_density_max 2.719 _refine_diff_density_min -1.477 _refine_diff_density_rms 0.205 #====END data_2-Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 N17 O18 Tb2' _chemical_formula_weight 1471.81 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.087(12) _cell_length_b 16.01(2) _cell_length_c 16.226(17) _cell_angle_alpha 106.012(10) _cell_angle_beta 95.798(10) _cell_angle_gamma 95.867(10) _cell_volume 2728(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 2.662 _exptl_absorpt_correction_type 'DIFABS, (Walker and Stuart, 1983) ' _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 8460 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.90 _reflns_number_total 8460 _reflns_number_gt 6876 _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^)+(0.0700P)^2^+10.1260P] 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(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8460 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.022 _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 Tb1 Tb 0.06998(3) 0.356778(19) 0.226276(17) 0.03387(12) Uani 1 d . . . O11 O 0.1295(5) 0.5095(3) 0.3200(3) 0.0461(11) Uani 1 d . . . N13 N 0.0678(6) 0.5469(4) 0.2733(4) 0.0460(14) Uani 1 d . . . O12 O 0.0044(5) 0.4975(3) 0.2047(3) 0.0483(12) Uani 1 d . . . O14 O 0.0712(7) 0.6272(4) 0.2949(4) 0.0712(17) Uani 1 d . . . O21 O 0.0755(5) 0.2055(3) 0.2471(3) 0.0532(13) Uani 1 d . . . O22 O 0.1308(5) 0.2247(3) 0.1297(3) 0.0542(13) Uani 1 d . . . N23 N 0.1184(7) 0.1744(4) 0.1781(4) 0.0576(17) Uani 1 d . . . O24 O 0.1502(10) 0.1022(4) 0.1577(4) 0.107(3) Uani 1 d . . . N11 N 0.2178(6) 0.4351(4) 0.1508(4) 0.0479(14) Uani 1 d . . . C12 C 0.3182(7) 0.4867(5) 0.1972(5) 0.0556(19) Uani 1 d . . . H12 H 0.3369 0.4867 0.2544 0.067 Uiso 1 calc R . . C13 C 0.3969(10) 0.5404(7) 0.1656(8) 0.082(3) Uani 1 d . . . H13 H 0.4671 0.5742 0.1994 0.099 Uiso 1 calc R . . C14 C 0.3650(13) 0.5406(10) 0.0825(10) 0.119(5) Uani 1 d . . . H14 H 0.4143 0.5758 0.0587 0.143 Uiso 1 calc R . . C15 C 0.2617(11) 0.4899(9) 0.0331(8) 0.098(4) Uani 1 d . . . H15 H 0.2418 0.4897 -0.0240 0.118 Uiso 1 calc R . . C16 C 0.1869(7) 0.4386(5) 0.0698(5) 0.0522(18) Uani 1 d . . . N21 N 0.0033(6) 0.3407(4) 0.0646(3) 0.0426(13) Uani 1 d . . . C26 C 0.0717(7) 0.3838(5) 0.0207(4) 0.0488(18) Uani 1 d . . . C24 C -0.0753(11) 0.3303(7) -0.1053(5) 0.078(3) Uani 1 d . . . H24 H -0.1016 0.3266 -0.1626 0.094 Uiso 1 calc R . . C25 C 0.0342(10) 0.3789(6) -0.0645(5) 0.069(2) Uani 1 d . . . H25 H 0.0828 0.4083 -0.0940 0.083 Uiso 1 calc R . . C22 C -0.1020(7) 0.2909(5) 0.0239(4) 0.0469(17) Uani 1 d . . . C23 C -0.1463(8) 0.2869(6) -0.0610(5) 0.061(2) Uani 1 d . . . H23 H -0.2222 0.2555 -0.0871 0.073 Uiso 1 calc R . . N31 N -0.1279(6) 0.2561(4) 0.1563(3) 0.0454(14) Uani 1 d . . . C32 C -0.1842(7) 0.2096(5) 0.2018(5) 0.0511(18) Uani 1 d . . . H32 H -0.1556 0.2215 0.2603 0.061 Uiso 1 calc R . . C33 C -0.2828(8) 0.1447(5) 0.1663(5) 0.0573(19) Uani 1 d . . . H33 H -0.3217 0.1149 0.2001 0.069 Uiso 1 calc R . . C34 C -0.3206(8) 0.1263(6) 0.0801(6) 0.067(2) Uani 1 d . . . H34 H -0.3841 0.0812 0.0535 0.081 Uiso 1 calc R . . C35 C -0.2658(8) 0.1736(6) 0.0318(5) 0.060(2) Uani 1 d . . . H35 H -0.2935 0.1624 -0.0267 0.072 Uiso 1 calc R . . C36 C -0.1685(7) 0.2381(4) 0.0719(4) 0.0428(16) Uani 1 d . . . N41 N -0.1066(5) 0.4020(4) 0.3118(3) 0.0415(13) Uani 1 d . . . C42 C -0.2041(7) 0.4276(5) 0.2752(5) 0.0480(17) Uani 1 d . . . H42 H -0.2062 0.4285 0.2180 0.058 Uiso 1 calc R . . C43 C -0.3009(7) 0.4525(5) 0.3176(5) 0.0535(18) Uani 1 d . . . H43 H -0.3677 0.4689 0.2893 0.064 Uiso 1 calc R . . C44 C -0.2982(7) 0.4530(5) 0.4017(6) 0.058(2) Uani 1 d . . . H44 H -0.3632 0.4698 0.4317 0.070 Uiso 1 calc R . . C45 C -0.1993(7) 0.4286(5) 0.4417(5) 0.0516(18) Uani 1 d . . . H45 H -0.1955 0.4297 0.4995 0.062 Uiso 1 calc R . . C46 C -0.1031(6) 0.4018(4) 0.3949(4) 0.0379(14) Uani 1 d . . . N51 N 0.0969(5) 0.3592(3) 0.3871(3) 0.0327(11) Uani 1 d . . . C52 C 0.0054(6) 0.3743(4) 0.4349(4) 0.0360(14) Uani 1 d . . . C53 C 0.0149(7) 0.3660(5) 0.5179(4) 0.0484(17) Uani 1 d . . . H53 H -0.0502 0.3763 0.5496 0.058 Uiso 1 calc R . . C54 C 0.1177(8) 0.3431(5) 0.5538(4) 0.0540(19) Uani 1 d . . . H54 H 0.1239 0.3375 0.6096 0.065 Uiso 1 calc R . . C55 C 0.2123(7) 0.3283(5) 0.5054(4) 0.0494(18) Uani 1 d . . . H55 H 0.2844 0.3134 0.5286 0.059 Uiso 1 calc R . . C56 C 0.2000(6) 0.3356(4) 0.4216(4) 0.0382(14) Uani 1 d . . . N61 N 0.2826(5) 0.3317(4) 0.2887(4) 0.0426(13) Uani 1 d . . . C62 C 0.2991(6) 0.3163(4) 0.3660(4) 0.0399(15) Uani 1 d . . . C63 C 0.3963(8) 0.2788(5) 0.3904(5) 0.057(2) Uani 1 d . . . H63 H 0.4046 0.2683 0.4442 0.068 Uiso 1 calc R . . C64 C 0.4830(8) 0.2561(6) 0.3353(6) 0.069(2) Uani 1 d . . . H64 H 0.5498 0.2305 0.3511 0.082 Uiso 1 calc R . . C65 C 0.4673(8) 0.2726(7) 0.2570(6) 0.069(2) Uani 1 d . . . H65 H 0.5241 0.2591 0.2187 0.083 Uiso 1 calc R . . C66 C 0.3665(7) 0.3094(6) 0.2356(5) 0.057(2) Uani 1 d . . . H66 H 0.3560 0.3193 0.1816 0.069 Uiso 1 calc R . . Tb2 Tb -0.31883(3) -0.10233(2) 0.301056(19) 0.04170(13) Uani 1 d . . . O31 O -0.3821(7) 0.0449(5) 0.3968(4) 0.0803(19) Uani 1 d . . . O32 O -0.2140(5) 0.0499(3) 0.3447(3) 0.0540(13) Uani 1 d . . . N33 N -0.2908(7) 0.0907(5) 0.3854(4) 0.0603(18) Uani 1 d . . . O34 O -0.2754(8) 0.1711(5) 0.4106(5) 0.095(2) Uani 1 d . . . O41 O -0.2588(5) -0.2450(4) 0.2067(4) 0.0608(14) Uani 1 d . . . N43 N -0.2882(7) -0.2908(5) 0.2548(5) 0.0618(18) Uani 1 d . . . O42 O -0.3192(6) -0.2499(4) 0.3273(4) 0.0704(17) Uani 1 d . . . O44 O -0.2861(8) -0.3702(5) 0.2355(6) 0.102(3) Uani 1 d . . . O52 O -0.5247(5) -0.1400(4) 0.3366(3) 0.0587(14) Uani 1 d . . . O51 O -0.4974(5) -0.2076(4) 0.2080(3) 0.0580(14) Uani 1 d . . . O54 O -0.6739(5) -0.2330(4) 0.2497(4) 0.0728(17) Uani 1 d . . . N53 N -0.5687(6) -0.1946(5) 0.2644(4) 0.0546(16) Uani 1 d . . . O61 O -0.4309(6) -0.0290(5) 0.2167(4) 0.0766(19) Uani 1 d . . . N63 N -0.5320(7) -0.0344(5) 0.1739(4) 0.0618(19) Uani 1 d . . . O64 O -0.6304(6) -0.0573(6) 0.1954(5) 0.091(2) Uani 1 d . . . O62 O -0.5295(9) -0.0251(9) 0.1026(6) 0.168(6) Uani 1 d . . . N81 N -0.0975(5) -0.1060(4) 0.3500(4) 0.0422(13) Uani 1 d . . . C82 C -0.0629(7) -0.1135(5) 0.4295(4) 0.0446(16) Uani 1 d . . . C83 C 0.0499(7) -0.1359(5) 0.4504(6) 0.058(2) Uani 1 d . . . H83 H 0.0708 -0.1437 0.5045 0.070 Uiso 1 calc R . . C84 C 0.1320(8) -0.1469(6) 0.3916(6) 0.067(2) Uani 1 d . . . H84 H 0.2085 -0.1624 0.4052 0.080 Uiso 1 calc R . . C85 C 0.0988(8) -0.1343(6) 0.3115(6) 0.066(2) Uani 1 d . . . H85 H 0.1536 -0.1399 0.2712 0.079 Uiso 1 calc R . . C86 C -0.0161(7) -0.1136(5) 0.2925(5) 0.0486(17) Uani 1 d . . . C92 C -0.1551(6) -0.0998(4) 0.4908(4) 0.0425(15) Uani 1 d . . . C93 C -0.1265(8) -0.0968(5) 0.5773(5) 0.056(2) Uani 1 d . . . H93 H -0.0491 -0.1063 0.5974 0.067 Uiso 1 calc R . . C94 C -0.2116(9) -0.0800(6) 0.6321(5) 0.061(2) Uani 1 d . . . H94 H -0.1937 -0.0787 0.6897 0.073 Uiso 1 calc R . . C95 C -0.3242(8) -0.0650(6) 0.6010(5) 0.061(2) Uani 1 d . . . H95 H -0.3833 -0.0521 0.6376 0.074 Uiso 1 calc R . . C96 C -0.3489(8) -0.0692(6) 0.5153(5) 0.058(2) Uani 1 d . . . H96 H -0.4260 -0.0594 0.4948 0.070 Uiso 1 calc R . . N91 N -0.2664(5) -0.0869(4) 0.4597(4) 0.0461(14) Uani 1 d . . . N71 N -0.1735(6) -0.0839(4) 0.1950(4) 0.0470(14) Uani 1 d . . . C72 C -0.0568(7) -0.0961(5) 0.2095(5) 0.0502(18) Uani 1 d . . . C73 C 0.0239(9) -0.0935(6) 0.1484(6) 0.070(2) Uani 1 d . . . H73 H 0.1052 -0.1013 0.1597 0.084 Uiso 1 calc R . . C74 C -0.0196(11) -0.0793(6) 0.0720(6) 0.078(3) Uani 1 d . . . H74 H 0.0326 -0.0772 0.0309 0.093 Uiso 1 calc R . . C75 C -0.1388(11) -0.0682(6) 0.0561(5) 0.074(3) Uani 1 d . . . H75 H -0.1698 -0.0599 0.0039 0.089 Uiso 1 calc R . . C76 C -0.2113(8) -0.0695(5) 0.1184(5) 0.0566(19) Uani 1 d . . . H76 H -0.2920 -0.0600 0.1080 0.068 Uiso 1 calc R . . N100 N 0.4498(10) 0.5492(8) 0.4126(7) 0.110(4) Uani 1 d . . . C101 C 0.4159(8) 0.6138(8) 0.4144(5) 0.067(2) Uani 1 d . . . C102 C 0.3698(12) 0.6938(8) 0.4175(8) 0.098(4) Uani 1 d . . . H10A H 0.3456 0.7179 0.4735 0.118 Uiso 1 calc R . . H10B H 0.3003 0.6833 0.3738 0.118 Uiso 1 calc R . . H10C H 0.4322 0.7346 0.4074 0.118 Uiso 1 calc R . . N200 N -0.4155(11) 0.3671(8) 0.0882(7) 0.108(3) Uiso 1 d . . . C201 C -0.4920(11) 0.3184(8) 0.0464(7) 0.082(3) Uiso 1 d . . . C202 C -0.5922(13) 0.2531(10) -0.0074(9) 0.122(5) Uiso 1 d . . . H20A H -0.6215 0.2715 -0.0564 0.147 Uiso 1 calc R . . H20B H -0.6576 0.2476 0.0261 0.147 Uiso 1 calc R . . H20C H -0.5631 0.1975 -0.0270 0.147 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 Tb1 0.0375(2) 0.03325(19) 0.03051(16) 0.00874(11) 0.00400(12) 0.00511(12) O11 0.055(3) 0.037(3) 0.043(2) 0.0087(19) 0.004(2) 0.006(2) N13 0.063(4) 0.035(4) 0.046(3) 0.015(2) 0.022(3) 0.013(3) O12 0.055(3) 0.049(3) 0.045(3) 0.018(2) 0.007(2) 0.010(2) O14 0.123(6) 0.038(4) 0.062(3) 0.017(2) 0.033(3) 0.022(3) O21 0.068(4) 0.049(3) 0.041(3) 0.015(2) -0.003(2) 0.007(2) O22 0.078(4) 0.045(3) 0.038(2) 0.006(2) 0.003(2) 0.022(3) N23 0.085(5) 0.040(4) 0.045(3) 0.010(3) -0.007(3) 0.018(3) O24 0.211(10) 0.048(4) 0.065(4) 0.010(3) 0.005(5) 0.060(5) N11 0.051(4) 0.051(4) 0.045(3) 0.018(3) 0.015(3) 0.005(3) C12 0.049(5) 0.047(5) 0.062(4) 0.005(3) 0.008(4) -0.005(3) C13 0.067(7) 0.078(7) 0.109(8) 0.041(6) 0.019(6) -0.005(5) C14 0.101(10) 0.143(13) 0.141(11) 0.094(10) 0.033(9) -0.022(9) C15 0.085(8) 0.131(11) 0.104(8) 0.079(8) 0.024(6) -0.009(7) C16 0.055(5) 0.055(5) 0.056(4) 0.024(3) 0.022(4) 0.015(4) N21 0.064(4) 0.035(3) 0.030(3) 0.010(2) 0.006(2) 0.012(3) C26 0.066(5) 0.049(5) 0.039(3) 0.019(3) 0.015(3) 0.018(4) C24 0.117(9) 0.073(7) 0.040(4) 0.022(4) -0.011(5) -0.002(6) C25 0.103(8) 0.066(6) 0.046(4) 0.026(4) 0.020(4) 0.008(5) C22 0.056(5) 0.042(4) 0.042(3) 0.008(3) 0.002(3) 0.015(3) C23 0.071(6) 0.068(6) 0.040(4) 0.014(3) -0.003(4) 0.008(4) N31 0.048(4) 0.044(4) 0.040(3) 0.008(2) 0.000(2) -0.001(3) C32 0.051(5) 0.053(5) 0.048(4) 0.015(3) 0.008(3) -0.006(3) C33 0.058(5) 0.045(5) 0.065(5) 0.014(3) 0.008(4) -0.003(3) C34 0.050(6) 0.063(6) 0.079(6) 0.020(4) -0.009(4) -0.017(4) C35 0.060(6) 0.058(5) 0.049(4) 0.001(3) -0.012(4) 0.007(4) C36 0.053(5) 0.025(4) 0.045(3) 0.003(2) 0.001(3) 0.002(3) N41 0.040(4) 0.043(3) 0.041(3) 0.012(2) 0.001(2) 0.006(2) C42 0.051(5) 0.044(4) 0.047(4) 0.012(3) 0.000(3) 0.007(3) C43 0.040(5) 0.047(5) 0.074(5) 0.017(4) 0.008(4) 0.012(3) C44 0.041(5) 0.057(5) 0.080(5) 0.015(4) 0.027(4) 0.014(4) C45 0.058(5) 0.050(5) 0.051(4) 0.015(3) 0.021(3) 0.014(4) C46 0.039(4) 0.036(4) 0.037(3) 0.009(2) 0.009(3) 0.001(3) N51 0.035(3) 0.030(3) 0.032(2) 0.0073(19) 0.001(2) 0.004(2) C52 0.040(4) 0.030(4) 0.035(3) 0.006(2) 0.006(3) 0.004(3) C53 0.056(5) 0.050(4) 0.040(3) 0.012(3) 0.011(3) 0.009(3) C54 0.072(6) 0.059(5) 0.032(3) 0.017(3) 0.005(3) 0.007(4) C55 0.058(5) 0.051(5) 0.039(3) 0.015(3) -0.006(3) 0.015(3) C56 0.043(4) 0.031(4) 0.036(3) 0.004(2) 0.000(3) 0.007(3) N61 0.036(3) 0.046(4) 0.049(3) 0.016(2) 0.008(2) 0.011(2) C62 0.035(4) 0.039(4) 0.040(3) 0.007(3) -0.006(3) 0.004(3) C63 0.049(5) 0.060(5) 0.056(4) 0.014(4) -0.006(4) 0.010(4) C64 0.044(5) 0.076(6) 0.087(6) 0.025(5) 0.001(4) 0.019(4) C65 0.048(6) 0.087(7) 0.077(6) 0.018(5) 0.024(4) 0.027(5) C66 0.046(5) 0.065(6) 0.068(5) 0.024(4) 0.020(4) 0.017(4) TB2 0.0344(2) 0.0494(2) 0.04229(19) 0.01571(14) 0.00307(14) 0.00533(14) O31 0.063(5) 0.105(6) 0.087(5) 0.036(4) 0.024(4) 0.039(4) O32 0.042(3) 0.050(3) 0.062(3) 0.002(2) 0.005(2) 0.010(2) N33 0.058(5) 0.073(6) 0.051(4) 0.015(3) 0.000(3) 0.031(4) O34 0.116(6) 0.065(5) 0.091(5) -0.001(3) -0.011(4) 0.050(4) O41 0.056(4) 0.051(4) 0.075(4) 0.018(3) 0.007(3) 0.006(3) N43 0.057(5) 0.051(5) 0.073(5) 0.020(3) -0.014(4) 0.002(3) O42 0.074(4) 0.072(4) 0.071(4) 0.039(3) -0.002(3) 0.002(3) O44 0.117(7) 0.039(5) 0.143(7) 0.026(4) -0.004(5) 0.009(4) O52 0.046(3) 0.081(4) 0.048(3) 0.016(3) 0.008(2) 0.008(3) O51 0.042(3) 0.077(4) 0.054(3) 0.019(3) 0.004(2) 0.007(3) O54 0.036(4) 0.088(5) 0.086(4) 0.021(3) 0.003(3) -0.011(3) N53 0.040(4) 0.068(5) 0.056(4) 0.024(3) 0.004(3) -0.003(3) O61 0.051(4) 0.105(5) 0.083(4) 0.054(4) -0.013(3) -0.001(3) N63 0.067(6) 0.068(5) 0.049(4) 0.026(3) -0.011(3) -0.006(4) O64 0.051(4) 0.140(7) 0.091(5) 0.044(5) 0.015(4) 0.025(4) O62 0.125(8) 0.274(14) 0.102(6) 0.113(8) -0.046(6) -0.097(8) N81 0.026(3) 0.034(3) 0.063(3) 0.009(2) 0.002(2) 0.005(2) C82 0.036(4) 0.037(4) 0.052(4) 0.005(3) -0.006(3) 0.001(3) C83 0.040(5) 0.050(5) 0.079(5) 0.013(4) -0.006(4) 0.011(3) C84 0.037(5) 0.060(6) 0.096(7) 0.008(4) -0.006(4) 0.021(4) C85 0.044(6) 0.056(6) 0.093(6) 0.006(4) 0.018(4) 0.017(4) C86 0.029(4) 0.041(4) 0.070(5) 0.005(3) 0.011(3) 0.004(3) C92 0.037(4) 0.038(4) 0.050(4) 0.013(3) -0.005(3) 0.004(3) C93 0.054(5) 0.054(5) 0.054(4) 0.017(3) -0.013(4) 0.003(4) C94 0.078(7) 0.058(5) 0.045(4) 0.017(3) 0.002(4) 0.003(4) C95 0.065(6) 0.068(6) 0.051(4) 0.016(4) 0.013(4) 0.004(4) C96 0.052(5) 0.073(6) 0.052(4) 0.021(4) 0.010(4) 0.012(4) N91 0.038(4) 0.055(4) 0.045(3) 0.017(3) -0.001(3) 0.007(3) N71 0.053(4) 0.042(4) 0.045(3) 0.009(2) 0.013(3) 0.006(3) C72 0.047(5) 0.033(4) 0.067(5) 0.006(3) 0.019(4) 0.003(3) C73 0.060(6) 0.069(6) 0.082(6) 0.014(4) 0.036(5) 0.013(4) C74 0.102(9) 0.063(6) 0.070(6) 0.014(4) 0.044(6) 0.009(5) C75 0.114(9) 0.064(6) 0.049(4) 0.015(4) 0.032(5) 0.017(5) C76 0.055(5) 0.053(5) 0.058(4) 0.008(3) 0.009(4) 0.009(4) N100 0.087(8) 0.129(10) 0.098(7) 0.002(6) -0.007(5) 0.049(7) C101 0.041(5) 0.096(8) 0.057(5) 0.011(4) 0.000(4) 0.013(5) C102 0.117(10) 0.078(8) 0.100(8) 0.035(6) -0.014(7) 0.011(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 Tb1 O22 2.462(5) . ? Tb1 O11 2.479(5) . ? Tb1 O12 2.539(6) . ? Tb1 O21 2.541(6) . ? Tb1 N31 2.542(6) . ? Tb1 N41 2.563(6) . ? Tb1 N11 2.567(6) . ? Tb1 N61 2.585(6) . ? Tb1 N51 2.585(5) . ? Tb1 N21 2.586(6) . ? O11 N13 1.276(7) . ? N13 O14 1.232(8) . ? N13 O12 1.266(8) . ? O21 N23 1.256(8) . ? O22 N23 1.278(8) . ? N23 O24 1.209(9) . ? N11 C12 1.337(10) . ? N11 C16 1.343(9) . ? C12 C13 1.394(12) . ? C13 C14 1.360(16) . ? C14 C15 1.370(18) . ? C15 C16 1.395(12) . ? C16 C26 1.488(12) . ? N21 C22 1.341(10) . ? N21 C26 1.355(9) . ? C26 C25 1.381(10) . ? C24 C25 1.370(14) . ? C24 C23 1.377(13) . ? C22 C23 1.397(10) . ? C22 C36 1.489(10) . ? N31 C32 1.336(9) . ? N31 C36 1.339(8) . ? C32 C33 1.385(11) . ? C33 C34 1.360(11) . ? C34 C35 1.372(12) . ? C35 C36 1.383(11) . ? N41 C42 1.336(9) . ? N41 C46 1.345(8) . ? C42 C43 1.367(11) . ? C43 C44 1.361(11) . ? C44 C45 1.364(11) . ? C45 C46 1.405(10) . ? C46 C52 1.473(9) . ? N51 C52 1.340(8) . ? N51 C56 1.355(8) . ? C52 C53 1.384(9) . ? C53 C54 1.357(11) . ? C54 C55 1.374(11) . ? C55 C56 1.392(9) . ? C56 C62 1.494(10) . ? N61 C66 1.341(9) . ? N61 C62 1.342(8) . ? C62 C63 1.363(10) . ? C63 C64 1.386(12) . ? C64 C65 1.364(13) . ? C65 C66 1.372(12) . ? TB2 O61 2.374(6) . ? TB2 O52 2.466(6) . ? TB2 O32 2.468(6) . ? TB2 N81 2.513(6) . ? TB2 O42 2.514(7) . ? TB2 O51 2.520(6) . ? TB2 N91 2.519(6) . ? TB2 N71 2.528(6) . ? TB2 O41 2.567(6) . ? TB2 O31 2.645(7) . ? O31 N33 1.248(10) . ? O32 N33 1.255(8) . ? N33 O34 1.226(10) . ? O41 N43 1.255(9) . ? N43 O44 1.225(10) . ? N43 O42 1.278(10) . ? O52 N53 1.268(8) . ? O51 N53 1.257(8) . ? O54 N53 1.229(8) . ? O61 N63 1.239(9) . ? N63 O62 1.208(10) . ? N63 O64 1.230(10) . ? N81 C82 1.349(9) . ? N81 C86 1.353(9) . ? C82 C83 1.371(11) . ? C82 C92 1.489(10) . ? C83 C84 1.373(13) . ? C84 C85 1.388(13) . ? C85 C86 1.375(11) . ? C86 C72 1.485(11) . ? C92 N91 1.343(9) . ? C92 C93 1.393(10) . ? C93 C94 1.357(12) . ? C94 C95 1.367(12) . ? C95 C96 1.371(11) . ? C96 N91 1.345(10) . ? N71 C72 1.336(10) . ? N71 C76 1.358(10) . ? C72 C73 1.406(11) . ? C73 C74 1.372(14) . ? C74 C75 1.360(15) . ? C75 C76 1.357(12) . ? N100 C101 1.131(13) . ? C101 C102 1.417(15) . ? N200 C201 1.116(14) . ? C201 C202 1.466(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 O22 Tb1 O11 148.29(18) . . ? O22 Tb1 O12 133.96(17) . . ? O11 Tb1 O12 51.11(17) . . ? O22 Tb1 O21 50.87(18) . . ? O11 Tb1 O21 135.09(16) . . ? O12 Tb1 O21 164.88(18) . . ? O22 Tb1 N31 74.1(2) . . ? O11 Tb1 N31 136.93(18) . . ? O12 Tb1 N31 97.7(2) . . ? O21 Tb1 N31 68.90(19) . . ? O22 Tb1 N41 139.28(19) . . ? O11 Tb1 N41 71.66(18) . . ? O12 Tb1 N41 69.19(17) . . ? O21 Tb1 N41 98.60(18) . . ? N31 Tb1 N41 69.2(2) . . ? O22 Tb1 N11 82.6(2) . . ? O11 Tb1 N11 72.45(19) . . ? O12 Tb1 N11 66.22(19) . . ? O21 Tb1 N11 127.10(19) . . ? N31 Tb1 N11 126.81(19) . . ? N41 Tb1 N11 134.1(2) . . ? O22 Tb1 N61 70.64(18) . . ? O11 Tb1 N61 84.55(18) . . ? O12 Tb1 N61 128.20(18) . . ? O21 Tb1 N61 65.99(18) . . ? N31 Tb1 N61 133.9(2) . . ? N41 Tb1 N61 126.42(18) . . ? N11 Tb1 N61 76.7(2) . . ? O22 Tb1 N51 113.14(16) . . ? O11 Tb1 N51 70.03(16) . . ? O12 Tb1 N51 112.64(15) . . ? O21 Tb1 N51 66.75(15) . . ? N31 Tb1 N51 106.22(17) . . ? N41 Tb1 N51 63.17(17) . . ? N11 Tb1 N51 126.93(18) . . ? N61 Tb1 N51 63.70(17) . . ? O22 Tb1 N21 67.49(17) . . ? O11 Tb1 N21 115.32(17) . . ? O12 Tb1 N21 68.43(16) . . ? O21 Tb1 N21 109.33(16) . . ? N31 Tb1 N21 63.62(19) . . ? N41 Tb1 N21 109.12(19) . . ? N11 Tb1 N21 63.3(2) . . ? N61 Tb1 N21 124.46(18) . . ? N51 Tb1 N21 169.59(18) . . ? N13 O11 Tb1 97.3(4) . . ? O14 N13 O12 122.4(6) . . ? O14 N13 O11 120.7(6) . . ? O12 N13 O11 116.9(6) . . ? N13 O12 Tb1 94.7(4) . . ? N23 O21 Tb1 94.8(4) . . ? N23 O22 Tb1 98.0(4) . . ? O24 N23 O21 123.6(7) . . ? O24 N23 O22 120.2(7) . . ? O21 N23 O22 116.1(6) . . ? C12 N11 C16 118.0(7) . . ? C12 N11 Tb1 119.4(5) . . ? C16 N11 Tb1 121.5(5) . . ? N11 C12 C13 124.4(8) . . ? C14 C13 C12 116.2(10) . . ? C13 C14 C15 121.3(9) . . ? C14 C15 C16 119.1(10) . . ? N11 C16 C15 121.0(9) . . ? N11 C16 C26 117.1(6) . . ? C15 C16 C26 122.0(8) . . ? C22 N21 C26 119.1(6) . . ? C22 N21 Tb1 119.9(4) . . ? C26 N21 Tb1 120.9(5) . . ? N21 C26 C25 121.4(8) . . ? N21 C26 C16 116.5(6) . . ? C25 C26 C16 122.1(7) . . ? C25 C24 C23 119.7(7) . . ? C24 C25 C26 119.4(8) . . ? N21 C22 C23 121.5(7) . . ? N21 C22 C36 117.4(6) . . ? C23 C22 C36 121.1(7) . . ? C24 C23 C22 118.7(8) . . ? C32 N31 C36 118.1(6) . . ? C32 N31 Tb1 119.0(5) . . ? C36 N31 Tb1 122.2(5) . . ? N31 C32 C33 123.4(7) . . ? C34 C33 C32 117.4(7) . . ? C33 C34 C35 120.6(8) . . ? C34 C35 C36 118.7(7) . . ? N31 C36 C35 121.7(7) . . ? N31 C36 C22 116.1(6) . . ? C35 C36 C22 122.2(6) . . ? C42 N41 C46 118.2(6) . . ? C42 N41 Tb1 120.6(4) . . ? C46 N41 Tb1 121.1(4) . . ? N41 C42 C43 123.3(7) . . ? C44 C43 C42 119.0(7) . . ? C43 C44 C45 119.3(7) . . ? C44 C45 C46 119.5(7) . . ? N41 C46 C45 120.6(6) . . ? N41 C46 C52 117.8(6) . . ? C45 C46 C52 121.6(6) . . ? C52 N51 C56 118.7(5) . . ? C52 N51 Tb1 121.1(4) . . ? C56 N51 Tb1 119.8(4) . . ? N51 C52 C53 121.1(6) . . ? N51 C52 C46 116.3(5) . . ? C53 C52 C46 122.6(6) . . ? C54 C53 C52 121.0(7) . . ? C53 C54 C55 118.2(6) . . ? C54 C55 C56 119.8(7) . . ? N51 C56 C55 121.1(6) . . ? N51 C56 C62 117.8(5) . . ? C55 C56 C62 121.1(6) . . ? C66 N61 C62 117.5(6) . . ? C66 N61 Tb1 119.4(5) . . ? C62 N61 Tb1 120.4(4) . . ? N61 C62 C63 122.0(7) . . ? N61 C62 C56 116.6(6) . . ? C63 C62 C56 121.2(6) . . ? C62 C63 C64 120.2(8) . . ? C65 C64 C63 117.9(8) . . ? C64 C65 C66 119.3(8) . . ? N61 C66 C65 123.1(8) . . ? O61 TB2 O52 81.4(2) . . ? O61 TB2 O32 74.6(2) . . ? O52 TB2 O32 122.22(18) . . ? O61 TB2 N81 136.8(2) . . ? O52 TB2 N81 140.58(19) . . ? O32 TB2 N81 72.39(18) . . ? O61 TB2 O42 140.9(2) . . ? O52 TB2 O42 74.3(2) . . ? O32 TB2 O42 144.5(2) . . ? N81 TB2 O42 76.5(2) . . ? O61 TB2 O51 70.9(2) . . ? O52 TB2 O51 50.74(18) . . ? O32 TB2 O51 145.43(18) . . ? N81 TB2 O51 137.51(19) . . ? O42 TB2 O51 70.0(2) . . ? O61 TB2 N91 136.4(2) . . ? O52 TB2 N91 80.24(19) . . ? O32 TB2 N91 82.57(19) . . ? N81 TB2 N91 64.75(19) . . ? O42 TB2 N91 68.9(2) . . ? O51 TB2 N91 122.37(19) . . ? O61 TB2 N71 78.3(2) . . ? O52 TB2 N71 152.01(19) . . ? O32 TB2 N71 70.12(18) . . ? N81 TB2 N71 64.8(2) . . ? O42 TB2 N71 111.0(2) . . ? O51 TB2 N71 103.9(2) . . ? N91 TB2 N71 127.7(2) . . ? O61 TB2 O41 111.6(2) . . ? O52 TB2 O41 106.5(2) . . ? O32 TB2 O41 131.07(19) . . ? N81 TB2 O41 72.61(18) . . ? O42 TB2 O41 50.1(2) . . ? O51 TB2 O41 66.0(2) . . ? N91 TB2 O41 111.4(2) . . ? N71 TB2 O41 64.5(2) . . ? O61 TB2 O31 67.7(2) . . ? O52 TB2 O31 73.4(2) . . ? O32 TB2 O31 49.0(2) . . ? N81 TB2 O31 107.9(2) . . ? O42 TB2 O31 130.3(2) . . ? O51 TB2 O31 113.6(2) . . ? N91 TB2 O31 69.2(2) . . ? N71 TB2 O31 115.3(2) . . ? O41 TB2 O31 179.37(18) . . ? N33 O31 TB2 93.0(5) . . ? N33 O32 TB2 101.5(5) . . ? O34 N33 O31 123.3(8) . . ? O34 N33 O32 120.5(9) . . ? O31 N33 O32 116.2(8) . . ? N43 O41 TB2 95.6(5) . . ? O44 N43 O41 123.0(9) . . ? O44 N43 O42 120.7(8) . . ? O41 N43 O42 116.3(7) . . ? N43 O42 TB2 97.5(5) . . ? N53 O52 TB2 98.0(4) . . ? N53 O51 TB2 95.7(4) . . ? O54 N53 O51 121.5(7) . . ? O54 N53 O52 122.9(7) . . ? O51 N53 O52 115.6(6) . . ? N63 O61 TB2 141.9(5) . . ? O62 N63 O64 119.4(8) . . ? O62 N63 O61 115.7(9) . . ? O64 N63 O61 124.4(7) . . ? C82 N81 C86 119.4(6) . . ? C82 N81 TB2 120.1(5) . . ? C86 N81 TB2 119.7(5) . . ? N81 C82 C83 121.0(7) . . ? N81 C82 C92 116.4(6) . . ? C83 C82 C92 122.5(7) . . ? C82 C83 C84 120.1(8) . . ? C83 C84 C85 118.8(8) . . ? C86 C85 C84 119.3(8) . . ? N81 C86 C85 121.2(8) . . ? N81 C86 C72 116.3(6) . . ? C85 C86 C72 122.4(7) . . ? N91 C92 C93 121.3(7) . . ? N91 C92 C82 116.8(6) . . ? C93 C92 C82 121.9(7) . . ? C94 C93 C92 120.0(8) . . ? C93 C94 C95 118.8(7) . . ? C94 C95 C96 119.3(8) . . ? N91 C96 C95 122.8(8) . . ? C96 N91 C92 117.8(6) . . ? C96 N91 TB2 121.9(5) . . ? C92 N91 TB2 120.3(5) . . ? C72 N71 C76 117.2(7) . . ? C72 N71 TB2 120.0(5) . . ? C76 N71 TB2 122.5(5) . . ? N71 C72 C73 121.4(8) . . ? N71 C72 C86 117.2(6) . . ? C73 C72 C86 121.4(8) . . ? C74 C73 C72 118.8(9) . . ? C75 C74 C73 120.1(8) . . ? C76 C75 C74 118.2(9) . . ? C75 C76 N71 124.2(9) . . ? N100 C101 C102 178.2(13) . . ? N200 C201 C202 178.8(14) . . ? _refine_diff_density_max 1.976 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.128 _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-Dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H33 Dy2 N15 O18 ' _chemical_formula_weight 1396.86 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.452(13) _cell_length_b 15.531(17) _cell_length_c 16.107(19) _cell_angle_alpha 101.062(10) _cell_angle_beta 106.144(10) _cell_angle_gamma 95.838(10) _cell_volume 2431(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 3.144 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983) ' _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 8252 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.91 _reflns_number_total 8252 _reflns_number_gt 5291 _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^)+(0.1683P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8252 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2306 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.342 _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 Dy1 Dy 0.30268(6) 0.01143(4) 0.20652(4) 0.0413(2) Uani 1 d . . . N11 N 0.2417(11) -0.1599(6) 0.1543(7) 0.049(3) Uani 1 d . . . C12 C 0.2168(16) -0.2094(9) 0.2095(10) 0.060(4) Uani 1 d . . . H12 H 0.2322 -0.1818 0.2688 0.072 Uiso 1 calc R . . C13 C 0.1693(18) -0.2992(13) 0.1818(13) 0.082(5) Uani 1 d . . . H13 H 0.1515 -0.3317 0.2213 0.098 Uiso 1 calc R . . C14 C 0.1482(19) -0.3407(11) 0.0928(12) 0.077(5) Uani 1 d . . . H14 H 0.1184 -0.4016 0.0721 0.092 Uiso 1 calc R . . C15 C 0.1724(15) -0.2900(9) 0.0378(11) 0.061(4) Uani 1 d . . . H15 H 0.1572 -0.3163 -0.0218 0.074 Uiso 1 calc R . . C16 C 0.2198(12) -0.1987(8) 0.0688(8) 0.045(3) Uani 1 d . . . N21 N 0.2958(10) -0.0555(7) 0.0491(6) 0.044(2) Uani 1 d . . . C22 C 0.2405(12) -0.1402(8) 0.0090(9) 0.043(3) Uani 1 d . . . C23 C 0.2037(14) -0.1694(9) -0.0829(9) 0.055(3) Uani 1 d . . . H23 H 0.1615 -0.2277 -0.1095 0.066 Uiso 1 calc R . . C24 C 0.2282(15) -0.1143(10) -0.1336(9) 0.058(4) Uani 1 d . . . H24 H 0.2024 -0.1341 -0.1951 0.070 Uiso 1 calc R . . C25 C 0.2914(14) -0.0288(9) -0.0939(8) 0.053(3) Uani 1 d . . . H25 H 0.3103 0.0102 -0.1277 0.064 Uiso 1 calc R . . C26 C 0.3268(14) -0.0013(9) -0.0018(9) 0.055(3) Uani 1 d . . . N31 N 0.4115(11) 0.1150(6) 0.1320(6) 0.043(2) Uani 1 d . . . C32 C 0.3950(13) 0.0893(9) 0.0418(8) 0.052(3) Uani 1 d . . . C33 C 0.4447(14) 0.1482(9) -0.0017(9) 0.052(3) Uani 1 d . . . H33 H 0.4388 0.1283 -0.0611 0.063 Uiso 1 calc R . . C34 C 0.5013(15) 0.2338(10) 0.0402(9) 0.058(4) Uani 1 d . . . H34 H 0.5308 0.2728 0.0097 0.070 Uiso 1 calc R . . C35 C 0.5143(14) 0.2622(10) 0.1317(9) 0.055(3) Uani 1 d . . . H35 H 0.5522 0.3202 0.1629 0.066 Uiso 1 calc R . . C36 C 0.4678(14) 0.1993(9) 0.1734(9) 0.054(3) Uani 1 d . . . H36 H 0.4768 0.2173 0.2335 0.064 Uiso 1 calc R . . N41 N 0.0548(10) -0.0472(7) 0.1790(7) 0.044(2) Uani 1 d . . . C42 C -0.0158(12) -0.0992(8) 0.1005(8) 0.046(3) Uani 1 d . . . H42 H 0.0105 -0.0914 0.0514 0.055 Uiso 1 calc R . . C43 C -0.1264(15) -0.1645(9) 0.0863(10) 0.061(4) Uani 1 d . . . H43 H -0.1732 -0.1995 0.0301 0.073 Uiso 1 calc R . . C44 C -0.1617(15) -0.1741(11) 0.1593(10) 0.067(4) Uani 1 d . . . H44 H -0.2313 -0.2192 0.1537 0.081 Uiso 1 calc R . . C45 C -0.0987(14) -0.1200(10) 0.2398(10) 0.060(4) Uani 1 d . . . H45 H -0.1270 -0.1255 0.2887 0.072 Uiso 1 calc R . . C46 C 0.0080(13) -0.0567(8) 0.2479(8) 0.049(3) Uani 1 d . . . N51 N 0.2176(10) 0.0328(7) 0.3424(6) 0.046(3) Uani 1 d . . . C53 C 0.023(2) 0.0358(12) 0.3974(12) 0.083(5) Uani 1 d . . . H53 H -0.0688 0.0170 0.3877 0.099 Uiso 1 calc R . . C52 C 0.0910(15) 0.0047(8) 0.3341(9) 0.049(3) Uani 1 d . . . C54 C 0.104(2) 0.0967(11) 0.4747(11) 0.081(5) Uani 1 d . . . H54 H 0.0676 0.1171 0.5199 0.097 Uiso 1 calc R . . C55 C 0.2389(19) 0.1269(11) 0.4847(10) 0.077(5) Uani 1 d . . . H55 H 0.2916 0.1694 0.5348 0.092 Uiso 1 calc R . . C56 C 0.2933(16) 0.0922(9) 0.4179(8) 0.056(3) Uani 1 d . . . N61 N 0.4722(11) 0.1135(7) 0.3518(7) 0.052(3) Uani 1 d . . . C62 C 0.4339(15) 0.1184(9) 0.4268(9) 0.055(3) Uani 1 d . . . C63 C 0.5276(19) 0.1554(13) 0.5086(11) 0.085(5) Uani 1 d . . . H63 H 0.4995 0.1685 0.5589 0.102 Uiso 1 calc R . . C66 C 0.6656(18) 0.1735(13) 0.5160(11) 0.084(6) Uani 1 d . . . H66 H 0.7307 0.1891 0.5714 0.101 Uiso 1 calc R . . C64 C 0.7018(18) 0.1677(11) 0.4413(12) 0.080(5) Uani 1 d . . . H64 H 0.7914 0.1840 0.4444 0.096 Uiso 1 calc R . . C65 C 0.6032(14) 0.1371(10) 0.3597(10) 0.060(4) Uani 1 d . . . H65 H 0.6288 0.1327 0.3084 0.072 Uiso 1 calc R . . O11 O 0.2161(9) 0.1495(6) 0.2291(6) 0.054(2) Uani 1 d . . . N13 N 0.1516(12) 0.1509(7) 0.1505(8) 0.051(3) Uani 1 d . . . O12 O 0.1368(9) 0.0780(6) 0.0931(6) 0.052(2) Uani 1 d . . . O14 O 0.1029(11) 0.2141(7) 0.1303(8) 0.076(3) Uani 1 d . . . O21 O 0.4408(10) -0.0687(7) 0.3159(6) 0.059(2) Uani 1 d . . . N23 N 0.5401(13) -0.0619(7) 0.2834(7) 0.055(3) Uani 1 d . . . O22 O 0.5226(10) -0.0321(6) 0.2137(6) 0.058(2) Uani 1 d . . . O24 O 0.6470(13) -0.0846(9) 0.3195(8) 0.091(4) Uani 1 d . . . Dy2 Dy 0.32380(6) 0.43259(4) 0.70276(4) 0.0423(2) Uani 1 d . . . N71 N 0.5490(11) 0.5014(6) 0.8169(7) 0.045(2) Uani 1 d . . . C72 C 0.5590(13) 0.5319(9) 0.9052(9) 0.056(3) Uani 1 d . . . H72 H 0.4823 0.5220 0.9228 0.067 Uiso 1 calc R . . C73 C 0.6758(15) 0.5758(10) 0.9678(10) 0.062(4) Uani 1 d . . . H73 H 0.6791 0.5955 1.0268 0.074 Uiso 1 calc R . . C74 C 0.7871(15) 0.5899(11) 0.9417(10) 0.072(4) Uani 1 d . . . H74 H 0.8678 0.6207 0.9829 0.087 Uiso 1 calc R . . C75 C 0.7815(16) 0.5592(10) 0.8548(12) 0.070(4) Uani 1 d . . . H75 H 0.8580 0.5687 0.8368 0.085 Uiso 1 calc R . . C76 C 0.6625(13) 0.5146(8) 0.7953(9) 0.046(3) Uani 1 d . . . N81 N 0.5260(11) 0.4451(6) 0.6435(7) 0.047(2) Uani 1 d . . . C82 C 0.6493(12) 0.4718(9) 0.7008(9) 0.050(3) Uani 1 d . . . C83 C 0.7651(15) 0.4618(10) 0.6715(12) 0.064(4) Uani 1 d . . . H83 H 0.8518 0.4826 0.7104 0.076 Uiso 1 calc R . . C84 C 0.7455(18) 0.4221(12) 0.5876(11) 0.075(5) Uani 1 d . . . H84 H 0.8203 0.4130 0.5685 0.089 Uiso 1 calc R . . C85 C 0.6211(16) 0.3945(11) 0.5288(10) 0.063(4) Uani 1 d . . . H85 H 0.6099 0.3676 0.4699 0.075 Uiso 1 calc R . . C86 C 0.5087(18) 0.4073(10) 0.5587(11) 0.067(4) Uani 1 d . . . N91 N 0.2712(11) 0.3920(7) 0.5372(7) 0.049(3) Uani 1 d . . . C92 C 0.3744(17) 0.3791(8) 0.4978(10) 0.059(4) Uani 1 d . . . C93 C 0.3397(19) 0.3521(11) 0.4073(10) 0.070(4) Uani 1 d . . . H93 H 0.4082 0.3496 0.3809 0.085 Uiso 1 calc R . . C94 C 0.208(2) 0.3285(9) 0.3542(10) 0.076(5) Uani 1 d . . . H94 H 0.1885 0.3027 0.2940 0.092 Uiso 1 calc R . . C95 C 0.1053(18) 0.3435(10) 0.3909(10) 0.069(4) Uani 1 d . . . H95 H 0.0157 0.3347 0.3559 0.083 Uiso 1 calc R . . C96 C 0.1425(14) 0.3718(10) 0.4815(9) 0.059(4) Uani 1 d . . . H96 H 0.0734 0.3778 0.5072 0.070 Uiso 1 calc R . . O31 O 0.4623(10) 0.3110(6) 0.7219(7) 0.055(2) Uani 1 d . . . N33 N 0.4417(11) 0.2993(8) 0.7924(8) 0.054(3) Uani 1 d . . . O32 O 0.3621(10) 0.3493(6) 0.8180(6) 0.054(2) Uani 1 d . . . O34 O 0.4904(12) 0.2478(8) 0.8347(8) 0.078(3) Uani 1 d . . . O41 O 0.1840(11) 0.2747(7) 0.6436(7) 0.071(3) Uani 1 d . . . N43 N 0.0724(12) 0.2984(10) 0.6491(9) 0.068(3) Uani 1 d . . . O44 O -0.0282(11) 0.2431(9) 0.6245(9) 0.096(4) Uani 1 d . . . O42 O 0.0804(10) 0.3796(7) 0.6778(8) 0.078(3) Uani 1 d . . . O61 O 0.2640(10) 0.5175(8) 0.8189(7) 0.080(4) Uani 1 d . . . N63 N 0.1589(14) 0.5359(9) 0.8350(8) 0.063(3) Uani 1 d . . . O62 O 0.0982(16) 0.4997(15) 0.8712(10) 0.165(9) Uani 1 d . . . O64 O 0.1149(19) 0.6026(10) 0.8151(12) 0.130(6) Uani 1 d . . . O51 O 0.3747(11) 0.5833(6) 0.6811(7) 0.063(3) Uani 1 d . . . O52 O 0.1656(12) 0.5338(8) 0.6338(7) 0.076(3) Uani 1 d . . . O54 O 0.2339(16) 0.6696(8) 0.6372(11) 0.109(5) Uani 1 d . . . N53 N 0.2613(13) 0.5959(8) 0.6607(14) 0.105(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 Dy1 0.0456(4) 0.0402(4) 0.0374(4) 0.0090(2) 0.0119(3) 0.0061(3) N11 0.060(7) 0.027(5) 0.055(7) 0.014(4) 0.010(5) 0.007(5) C12 0.073(10) 0.050(8) 0.053(8) 0.023(6) 0.006(7) 0.013(7) C13 0.070(11) 0.092(13) 0.086(13) 0.043(10) 0.015(9) 0.006(10) C14 0.088(12) 0.056(9) 0.079(12) 0.015(8) 0.012(10) 0.013(9) C15 0.057(9) 0.038(7) 0.082(11) 0.004(7) 0.017(8) 0.009(6) C16 0.040(7) 0.038(6) 0.045(7) 0.005(5) 0.004(5) -0.005(5) N21 0.049(6) 0.050(6) 0.029(5) 0.004(4) 0.012(4) 0.000(5) C22 0.041(7) 0.035(6) 0.056(8) 0.017(5) 0.014(6) 0.007(5) C23 0.051(8) 0.060(8) 0.042(7) -0.008(6) 0.011(6) 0.002(6) C24 0.059(9) 0.077(10) 0.045(8) 0.017(7) 0.020(7) 0.026(8) C25 0.058(8) 0.059(8) 0.035(7) 0.007(6) 0.008(6) -0.003(7) C26 0.053(8) 0.059(8) 0.046(8) 0.011(6) 0.007(6) -0.001(7) N31 0.065(7) 0.035(5) 0.028(5) 0.008(4) 0.013(5) 0.010(5) C32 0.049(7) 0.066(8) 0.030(6) 0.005(6) -0.003(5) 0.019(6) C33 0.066(9) 0.049(7) 0.057(8) 0.020(6) 0.032(7) 0.025(7) C34 0.063(9) 0.067(9) 0.053(8) 0.029(7) 0.022(7) 0.008(7) C35 0.051(8) 0.060(8) 0.050(8) 0.011(6) 0.011(6) 0.010(7) C36 0.066(9) 0.052(8) 0.051(8) 0.021(6) 0.021(7) 0.013(7) N41 0.034(5) 0.050(6) 0.046(6) 0.012(5) 0.006(4) 0.007(5) C42 0.036(6) 0.057(8) 0.038(7) 0.010(5) 0.002(5) 0.008(6) C43 0.064(9) 0.045(8) 0.059(9) 0.015(6) -0.002(7) -0.005(7) C44 0.055(9) 0.075(10) 0.057(9) 0.026(8) -0.005(7) -0.011(8) C45 0.053(8) 0.082(10) 0.055(9) 0.028(7) 0.021(7) 0.012(7) C46 0.053(8) 0.050(7) 0.046(7) 0.017(6) 0.018(6) 0.003(6) N51 0.043(6) 0.065(7) 0.020(5) 0.008(4) 0.003(4) -0.009(5) C53 0.107(14) 0.080(12) 0.081(12) 0.020(9) 0.062(11) 0.015(10) C52 0.079(10) 0.051(7) 0.050(7) 0.038(6) 0.041(7) 0.041(7) C54 0.116(15) 0.083(11) 0.055(10) 0.008(8) 0.051(10) 0.018(11) C55 0.092(13) 0.084(12) 0.041(8) 0.002(7) 0.013(8) -0.005(10) C56 0.079(10) 0.058(8) 0.037(7) 0.019(6) 0.021(7) 0.020(7) N61 0.051(7) 0.062(7) 0.037(6) 0.009(5) 0.005(5) 0.005(5) C62 0.062(9) 0.051(8) 0.045(8) 0.013(6) 0.005(6) 0.004(7) C63 0.087(13) 0.111(14) 0.041(9) 0.013(9) -0.002(8) 0.008(11) C66 0.067(11) 0.111(14) 0.049(9) 0.019(9) -0.012(8) -0.024(10) C64 0.079(11) 0.072(11) 0.078(12) 0.034(9) 0.006(9) -0.022(9) C65 0.054(9) 0.065(9) 0.050(8) 0.010(7) 0.004(7) -0.001(7) O11 0.059(6) 0.061(6) 0.044(5) 0.014(4) 0.022(5) 0.005(5) N13 0.068(8) 0.036(6) 0.052(7) 0.012(5) 0.022(6) 0.007(5) O12 0.060(6) 0.055(5) 0.042(5) 0.011(4) 0.014(4) 0.012(4) O14 0.069(7) 0.077(7) 0.078(8) 0.026(6) 0.003(6) 0.035(6) O21 0.066(6) 0.073(6) 0.044(5) 0.017(5) 0.021(5) 0.018(5) N23 0.065(8) 0.045(6) 0.038(6) 0.001(5) -0.006(6) 0.003(6) O22 0.069(6) 0.067(6) 0.041(5) 0.022(4) 0.015(5) 0.016(5) O24 0.080(8) 0.117(10) 0.065(8) 0.035(7) -0.013(6) 0.037(7) Dy2 0.0404(4) 0.0423(4) 0.0425(4) 0.0051(2) 0.0131(3) 0.0071(3) N71 0.047(6) 0.038(5) 0.042(6) 0.005(4) 0.005(5) -0.001(5) C72 0.039(7) 0.068(9) 0.056(9) 0.022(7) 0.001(6) 0.008(7) C73 0.053(9) 0.065(9) 0.047(8) 0.008(7) -0.013(7) 0.009(7) C74 0.051(9) 0.087(11) 0.050(9) 0.001(8) -0.012(7) -0.014(8) C75 0.060(10) 0.062(9) 0.091(13) 0.019(8) 0.027(9) 0.004(8) C76 0.042(7) 0.045(7) 0.051(8) 0.019(5) 0.007(6) 0.012(6) N81 0.045(6) 0.040(5) 0.056(7) 0.017(5) 0.011(5) 0.015(5) C82 0.037(7) 0.060(8) 0.066(9) 0.034(7) 0.019(6) 0.026(6) C83 0.055(9) 0.064(9) 0.100(13) 0.046(9) 0.043(9) 0.031(7) C84 0.071(11) 0.113(14) 0.070(11) 0.047(10) 0.043(9) 0.044(10) C85 0.064(10) 0.086(11) 0.050(8) 0.025(7) 0.025(8) 0.026(8) C86 0.090(12) 0.052(8) 0.076(11) 0.015(7) 0.048(10) 0.030(8) N91 0.060(7) 0.040(6) 0.040(6) -0.004(4) 0.015(5) -0.001(5) C92 0.088(11) 0.032(7) 0.060(9) 0.011(6) 0.023(8) 0.016(7) C93 0.095(13) 0.075(10) 0.049(9) 0.007(7) 0.036(9) 0.019(9) C94 0.131(16) 0.043(8) 0.048(9) -0.002(6) 0.024(10) 0.011(9) C95 0.082(11) 0.068(10) 0.051(9) 0.008(7) 0.013(8) 0.013(8) C96 0.045(8) 0.077(10) 0.044(8) 0.007(7) 0.001(6) 0.012(7) O31 0.059(6) 0.051(5) 0.063(6) 0.023(5) 0.025(5) 0.010(5) N33 0.037(6) 0.065(8) 0.061(7) 0.028(6) 0.006(5) 0.011(6) O32 0.063(6) 0.045(5) 0.060(6) 0.014(4) 0.026(5) 0.009(4) O34 0.077(8) 0.098(8) 0.067(7) 0.039(6) 0.018(6) 0.025(7) O41 0.062(7) 0.074(7) 0.066(7) 0.000(5) 0.014(5) 0.004(5) N43 0.040(7) 0.086(10) 0.061(8) 0.016(7) -0.006(6) 0.000(7) O44 0.052(7) 0.099(9) 0.108(10) 0.020(7) -0.006(6) -0.025(6) O42 0.047(6) 0.061(7) 0.112(10) -0.010(6) 0.022(6) 0.006(5) O61 0.046(6) 0.107(9) 0.062(7) -0.028(6) 0.010(5) 0.014(6) N63 0.076(9) 0.064(8) 0.046(7) 0.002(6) 0.016(6) 0.029(7) O62 0.100(11) 0.31(3) 0.102(11) 0.127(15) 0.037(9) -0.028(13) O64 0.171(17) 0.089(10) 0.134(14) 0.016(9) 0.047(12) 0.055(11) O51 0.079(7) 0.051(5) 0.076(7) 0.019(5) 0.046(6) 0.010(5) O52 0.068(7) 0.100(9) 0.059(7) 0.015(6) 0.011(6) 0.042(7) O54 0.146(13) 0.065(7) 0.164(14) 0.059(8) 0.086(11) 0.060(9) N53 0.035(7) 0.036(7) 0.24(2) -0.003(9) 0.070(10) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O22 2.440(10) . ? Dy1 O11 2.413(10) . ? Dy1 N11 2.587(10) . ? Dy1 N21 2.528(9) . ? Dy1 O21 2.555(10) . ? Dy1 N41 2.543(10) . ? Dy1 O12 2.596(9) . ? Dy1 N31 2.539(9) . ? Dy1 N51 2.560(9) . ? Dy1 N61 2.613(11) . ? N11 C12 1.341(17) . ? N11 C16 1.338(16) . ? C12 C13 1.37(2) . ? C13 C14 1.40(2) . ? C14 C15 1.35(2) . ? C15 C16 1.398(17) . ? C16 C22 1.488(17) . ? N21 C26 1.358(16) . ? N21 C22 1.338(15) . ? C22 C23 1.390(18) . ? C23 C24 1.34(2) . ? C24 C25 1.367(19) . ? C25 C26 1.392(18) . ? C26 C32 1.456(19) . ? N31 C36 1.340(16) . ? N31 C32 1.387(15) . ? C32 C33 1.396(19) . ? C33 C34 1.359(19) . ? C34 C35 1.418(19) . ? C35 C36 1.407(19) . ? N41 C42 1.328(15) . ? N41 C46 1.358(16) . ? C42 C43 1.395(18) . ? C43 C44 1.36(2) . ? C44 C45 1.35(2) . ? C45 C46 1.369(18) . ? C46 C52 1.497(19) . ? N51 C52 1.312(17) . ? N51 C56 1.356(17) . ? C53 C54 1.40(2) . ? C53 C52 1.439(19) . ? C54 C55 1.40(2) . ? C55 C56 1.40(2) . ? C56 C62 1.44(2) . ? N61 C65 1.345(18) . ? N61 C62 1.365(17) . ? C62 C63 1.38(2) . ? C63 C66 1.41(2) . ? C66 C64 1.35(2) . ? C64 C65 1.39(2) . ? O11 N13 1.264(14) . ? N13 O14 1.209(14) . ? N13 O12 1.281(13) . ? O21 N23 1.289(15) . ? N23 O24 1.229(16) . ? N23 O22 1.268(14) . ? Dy2 O61 2.346(10) . ? Dy2 O51 2.460(9) . ? Dy2 O32 2.428(9) . ? Dy2 N71 2.527(10) . ? Dy2 O31 2.507(10) . ? Dy2 O42 2.488(10) . ? Dy2 N91 2.506(10) . ? Dy2 N81 2.554(11) . ? Dy2 O41 2.580(11) . ? Dy2 O52 2.573(11) . ? N71 C72 1.381(17) . ? N71 C76 1.333(16) . ? C72 C73 1.362(18) . ? C73 C74 1.35(2) . ? C74 C75 1.37(2) . ? C75 C76 1.36(2) . ? C76 C82 1.502(19) . ? N81 C82 1.329(17) . ? N81 C86 1.334(18) . ? C82 C83 1.427(17) . ? C83 C84 1.32(2) . ? C84 C85 1.35(2) . ? C85 C86 1.41(2) . ? C86 C92 1.44(2) . ? N91 C96 1.360(17) . ? N91 C92 1.407(18) . ? C92 C93 1.37(2) . ? C93 C94 1.37(2) . ? C94 C95 1.38(2) . ? C95 C96 1.37(2) . ? O31 N33 1.255(14) . ? N33 O34 1.210(15) . ? N33 O32 1.290(14) . ? O41 N43 1.280(16) . ? N43 O44 1.205(15) . ? N43 O42 1.244(16) . ? O61 N63 1.244(15) . ? N63 O62 1.148(16) . ? N63 O64 1.238(18) . ? O51 N53 1.186(16) . ? O52 N53 1.233(16) . ? O54 N53 1.307(18) . ? 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 O22 Dy1 O11 136.3(3) . . ? O22 Dy1 N11 77.9(3) . . ? O11 Dy1 N11 145.7(3) . . ? O22 Dy1 N21 73.0(3) . . ? O11 Dy1 N21 116.1(3) . . ? N11 Dy1 N21 63.4(3) . . ? O22 Dy1 O21 52.0(3) . . ? O11 Dy1 O21 131.7(3) . . ? N11 Dy1 O21 67.1(3) . . ? N21 Dy1 O21 111.2(3) . . ? O22 Dy1 N41 144.1(3) . . ? O11 Dy1 N41 79.6(3) . . ? N11 Dy1 N41 66.5(3) . . ? N21 Dy1 N41 93.5(3) . . ? O21 Dy1 N41 107.3(3) . . ? O22 Dy1 O12 132.7(3) . . ? O11 Dy1 O12 50.4(3) . . ? N11 Dy1 O12 107.4(3) . . ? N21 Dy1 O12 68.7(3) . . ? O21 Dy1 O12 172.9(3) . . ? N41 Dy1 O12 65.7(3) . . ? O22 Dy1 N31 74.8(3) . . ? O11 Dy1 N31 72.5(3) . . ? N11 Dy1 N31 126.2(3) . . ? N21 Dy1 N31 64.7(3) . . ? O21 Dy1 N31 122.4(3) . . ? N41 Dy1 N31 129.9(3) . . ? O12 Dy1 N31 64.4(3) . . ? O22 Dy1 N51 121.3(3) . . ? O11 Dy1 N51 68.6(3) . . ? N11 Dy1 N51 98.9(3) . . ? N21 Dy1 N51 155.9(3) . . ? O21 Dy1 N51 72.5(3) . . ? N41 Dy1 N51 63.4(3) . . ? O12 Dy1 N51 104.6(3) . . ? N31 Dy1 N51 134.8(3) . . ? O22 Dy1 N61 74.2(3) . . ? O11 Dy1 N61 74.0(3) . . ? N11 Dy1 N61 131.2(4) . . ? N21 Dy1 N61 138.9(3) . . ? O21 Dy1 N61 64.1(3) . . ? N41 Dy1 N61 127.5(3) . . ? O12 Dy1 N61 121.0(3) . . ? N31 Dy1 N61 83.3(3) . . ? N51 Dy1 N61 64.9(3) . . ? C12 N11 C16 119.4(11) . . ? C12 N11 Dy1 120.6(9) . . ? C16 N11 Dy1 119.6(8) . . ? N11 C12 C13 122.5(14) . . ? C14 C13 C12 118.6(16) . . ? C13 C14 C15 118.3(15) . . ? C14 C15 C16 121.2(15) . . ? N11 C16 C15 120.1(12) . . ? N11 C16 C22 117.3(10) . . ? C15 C16 C22 122.5(12) . . ? C26 N21 C22 117.8(10) . . ? C26 N21 Dy1 119.3(8) . . ? C22 N21 Dy1 121.9(8) . . ? C23 C22 N21 121.1(11) . . ? C23 C22 C16 123.3(11) . . ? N21 C22 C16 115.6(11) . . ? C24 C23 C22 120.9(12) . . ? C23 C24 C25 119.2(13) . . ? C24 C25 C26 118.7(13) . . ? N21 C26 C25 122.0(12) . . ? N21 C26 C32 118.4(12) . . ? C25 C26 C32 119.6(12) . . ? C36 N31 C32 117.6(10) . . ? C36 N31 Dy1 122.1(7) . . ? C32 N31 Dy1 119.6(8) . . ? C33 C32 N31 120.3(12) . . ? C33 C32 C26 123.7(12) . . ? N31 C32 C26 115.9(12) . . ? C34 C33 C32 122.0(12) . . ? C33 C34 C35 118.3(12) . . ? C36 C35 C34 117.5(13) . . ? N31 C36 C35 124.1(12) . . ? C42 N41 C46 115.8(11) . . ? C42 N41 Dy1 118.9(8) . . ? C46 N41 Dy1 120.4(8) . . ? N41 C42 C43 124.7(13) . . ? C42 C43 C44 116.0(13) . . ? C45 C44 C43 121.9(14) . . ? C44 C45 C46 118.4(13) . . ? N41 C46 C45 123.0(12) . . ? N41 C46 C52 112.9(11) . . ? C45 C46 C52 123.9(11) . . ? C52 N51 C56 118.5(11) . . ? C52 N51 Dy1 120.5(8) . . ? C56 N51 Dy1 118.8(8) . . ? C54 C53 C52 114.9(17) . . ? N51 C52 C53 124.8(14) . . ? N51 C52 C46 117.3(10) . . ? C53 C52 C46 117.5(14) . . ? C53 C54 C55 120.8(14) . . ? C56 C55 C54 118.7(14) . . ? C55 C56 N51 122.0(14) . . ? C55 C56 C62 120.9(13) . . ? N51 C56 C62 117.1(11) . . ? C65 N61 C62 119.1(12) . . ? C65 N61 Dy1 122.0(9) . . ? C62 N61 Dy1 115.8(9) . . ? N61 C62 C63 119.4(15) . . ? N61 C62 C56 118.9(12) . . ? C63 C62 C56 121.5(14) . . ? C66 C63 C62 120.1(16) . . ? C64 C66 C63 118.8(15) . . ? C66 C64 C65 118.9(16) . . ? N61 C65 C64 122.7(15) . . ? N13 O11 Dy1 101.6(7) . . ? O14 N13 O12 121.8(12) . . ? O14 N13 O11 123.6(11) . . ? O12 N13 O11 114.6(10) . . ? N13 O12 Dy1 92.3(7) . . ? N23 O21 Dy1 91.8(7) . . ? O24 N23 O21 119.9(12) . . ? O24 N23 O22 122.1(13) . . ? O21 N23 O22 118.0(11) . . ? N23 O22 Dy1 97.7(8) . . ? O61 Dy2 O51 79.1(4) . . ? O61 Dy2 O32 74.8(4) . . ? O51 Dy2 O32 141.1(3) . . ? O61 Dy2 N71 76.6(3) . . ? O51 Dy2 N71 74.2(4) . . ? O32 Dy2 N71 72.0(3) . . ? O61 Dy2 O31 123.3(4) . . ? O51 Dy2 O31 132.5(3) . . ? O32 Dy2 O31 51.0(3) . . ? N71 Dy2 O31 72.4(3) . . ? O61 Dy2 O42 73.1(4) . . ? O51 Dy2 O42 114.6(4) . . ? O32 Dy2 O42 84.8(4) . . ? N71 Dy2 O42 145.7(4) . . ? O31 Dy2 O42 112.0(3) . . ? O61 Dy2 N91 143.4(4) . . ? O51 Dy2 N91 82.3(3) . . ? O32 Dy2 N91 134.4(3) . . ? N71 Dy2 N91 127.6(3) . . ? O31 Dy2 N91 92.3(3) . . ? O42 Dy2 N91 86.7(4) . . ? O61 Dy2 N81 134.7(4) . . ? O51 Dy2 N81 69.6(3) . . ? O32 Dy2 N81 110.7(3) . . ? N71 Dy2 N81 64.1(3) . . ? O31 Dy2 N81 65.8(3) . . ? O42 Dy2 N81 150.0(4) . . ? N91 Dy2 N81 63.9(4) . . ? O61 Dy2 O41 112.8(4) . . ? O51 Dy2 O41 149.1(4) . . ? O32 Dy2 O41 69.2(3) . . ? N71 Dy2 O41 135.3(4) . . ? O31 Dy2 O41 66.2(4) . . ? O42 Dy2 O41 49.3(3) . . ? N91 Dy2 O41 71.4(3) . . ? N81 Dy2 O41 110.8(3) . . ? O61 Dy2 O52 73.3(4) . . ? O51 Dy2 O52 49.6(4) . . ? O32 Dy2 O52 141.7(3) . . ? N71 Dy2 O52 119.5(4) . . ? O31 Dy2 O52 162.7(3) . . ? O42 Dy2 O52 66.0(4) . . ? N91 Dy2 O52 70.6(4) . . ? N81 Dy2 O52 106.7(4) . . ? O41 Dy2 O52 104.7(4) . . ? C72 N71 C76 116.3(11) . . ? C72 N71 Dy2 121.0(8) . . ? C76 N71 Dy2 122.6(8) . . ? C73 C72 N71 123.2(14) . . ? C72 C73 C74 118.0(15) . . ? C73 C74 C75 120.4(13) . . ? C76 C75 C74 119.0(14) . . ? C75 C76 N71 123.0(13) . . ? C75 C76 C82 122.8(12) . . ? N71 C76 C82 114.1(11) . . ? C82 N81 C86 120.6(12) . . ? C82 N81 Dy2 119.1(8) . . ? C86 N81 Dy2 118.7(9) . . ? N81 C82 C83 120.2(14) . . ? N81 C82 C76 118.2(11) . . ? C83 C82 C76 121.6(13) . . ? C84 C83 C82 118.1(16) . . ? C83 C84 C85 122.3(14) . . ? C84 C85 C86 118.4(15) . . ? N81 C86 C85 120.2(16) . . ? N81 C86 C92 119.7(13) . . ? C85 C86 C92 120.1(14) . . ? C96 N91 C92 116.5(12) . . ? C96 N91 Dy2 122.3(9) . . ? C92 N91 Dy2 120.8(9) . . ? N91 C92 C93 118.6(15) . . ? N91 C92 C86 114.2(12) . . ? C93 C92 C86 126.7(15) . . ? C94 C93 C92 122.7(15) . . ? C95 C94 C93 119.3(14) . . ? C94 C95 C96 116.5(16) . . ? N91 C96 C95 125.8(14) . . ? N33 O31 Dy2 96.4(7) . . ? O34 N33 O31 125.4(12) . . ? O34 N33 O32 121.3(12) . . ? O31 N33 O32 113.3(10) . . ? O34 N33 Dy2 175.7(10) . . ? O31 N33 Dy2 58.4(6) . . ? O32 N33 Dy2 55.0(6) . . ? N33 O32 Dy2 99.2(7) . . ? N43 O41 Dy2 95.5(8) . . ? O44 N43 O41 119.2(15) . . ? O42 N43 O44 126.7(15) . . ? O41 N43 O42 114.0(11) . . ? N43 O42 Dy2 101.1(8) . . ? N63 O61 Dy2 137.8(9) . . ? O62 N63 O61 127.2(18) . . ? O62 N63 O64 113.6(18) . . ? O61 N63 O64 119.1(16) . . ? N53 O51 Dy2 96.0(8) . . ? N53 O52 Dy2 89.4(9) . . ? O51 N53 O52 121.5(12) . . ? O51 N53 O54 119.6(13) . . ? O52 N53 O54 114.9(16) . . ? O51 N53 Dy2 59.4(8) . . ? O52 N53 Dy2 64.9(8) . . ? O54 N53 Dy2 176.8(14) . . ? _refine_diff_density_max 2.767 _refine_diff_density_min -1.650 _refine_diff_density_rms 0.190 _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-Ho _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H33 Ho2 N15 O18 ' _chemical_formula_weight 1401.72 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.463(11) _cell_length_b 15.525(17) _cell_length_c 16.131(17) _cell_angle_alpha 100.88(1) _cell_angle_beta 106.22(1) _cell_angle_gamma 95.81(1) _cell_volume 2437.6 _cell_formula_units_Z 2 _cell_measurement_temperature 298(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 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 3.316 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8371 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.88 _reflns_number_total 8371 _reflns_number_gt 6381 _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^)+(0.0804P)^2^+16.6184P] 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 8371 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.005 _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 Ho1 Ho 0.30335(4) 0.01072(2) 0.20629(2) 0.03610(13) Uani 1 d . . . Ho2 Ho 0.32467(4) 0.43282(2) 0.70258(2) 0.03638(13) Uani 1 d . . . N11 N 0.2406(8) -0.1585(4) 0.1550(5) 0.0440(17) Uani 1 d . . . C12 C 0.2181(11) -0.2094(7) 0.2099(8) 0.060(3) Uani 1 d . . . H12 H 0.2381 -0.1827 0.2697 0.072 Uiso 1 calc R . . C13 C 0.1677(13) -0.2977(7) 0.1828(9) 0.073(3) Uani 1 d . . . H13 H 0.1471 -0.3285 0.2228 0.088 Uiso 1 calc R . . C14 C 0.1469(12) -0.3414(7) 0.0970(9) 0.071(3) Uani 1 d . . . H14 H 0.1170 -0.4024 0.0779 0.086 Uiso 1 calc R . . C15 C 0.1727(10) -0.2900(6) 0.0394(8) 0.058(3) Uani 1 d . . . H15 H 0.1594 -0.3170 -0.0196 0.070 Uiso 1 calc R . . C16 C 0.2183(9) -0.1988(6) 0.0692(6) 0.044(2) Uani 1 d . . . N21 N 0.2960(7) -0.0547(4) 0.0480(5) 0.0373(15) Uani 1 d . . . C22 C 0.2377(9) -0.1408(6) 0.0092(6) 0.0419(19) Uani 1 d . . . C23 C 0.2025(9) -0.1721(6) -0.0836(6) 0.049(2) Uani 1 d . . . H23 H 0.1624 -0.2309 -0.1097 0.059 Uiso 1 calc R . . C24 C 0.2276(10) -0.1156(7) -0.1349(6) 0.056(2) Uani 1 d . . . H24 H 0.2010 -0.1348 -0.1963 0.067 Uiso 1 calc R . . C25 C 0.2926(10) -0.0303(7) -0.0947(6) 0.052(2) Uani 1 d . . . H25 H 0.3141 0.0079 -0.1286 0.063 Uiso 1 calc R . . C26 C 0.3268(9) -0.0004(5) -0.0020(6) 0.0406(19) Uani 1 d . . . N31 N 0.4109(7) 0.1152(4) 0.1322(4) 0.0400(16) Uani 1 d . . . C32 C 0.3971(9) 0.0903(6) 0.0435(6) 0.0409(19) Uani 1 d . . . C33 C 0.4439(9) 0.1483(5) -0.0009(6) 0.0411(19) Uani 1 d . . . H33 H 0.4350 0.1291 -0.0607 0.049 Uiso 1 calc R . . C34 C 0.5031(10) 0.2335(6) 0.0424(7) 0.053(2) Uani 1 d . . . H34 H 0.5355 0.2724 0.0129 0.063 Uiso 1 calc R . . C35 C 0.5139(10) 0.2608(6) 0.1314(7) 0.053(2) Uani 1 d . . . H35 H 0.5507 0.3191 0.1621 0.064 Uiso 1 calc R . . C36 C 0.4688(10) 0.1998(6) 0.1737(6) 0.048(2) Uani 1 d . . . H36 H 0.4790 0.2180 0.2339 0.058 Uiso 1 calc R . . N41 N 0.0544(7) -0.0489(5) 0.1787(5) 0.0414(16) Uani 1 d . . . C42 C -0.0154(9) -0.0985(6) 0.0985(6) 0.048(2) Uani 1 d . . . H42 H 0.0100 -0.0894 0.0496 0.057 Uiso 1 calc R . . C43 C -0.1259(10) -0.1637(7) 0.0860(7) 0.057(3) Uani 1 d . . . H43 H -0.1721 -0.1987 0.0298 0.068 Uiso 1 calc R . . C44 C -0.1644(11) -0.1750(7) 0.1582(8) 0.067(3) Uani 1 d . . . H44 H -0.2351 -0.2197 0.1518 0.080 Uiso 1 calc R . . C45 C -0.0996(10) -0.1210(7) 0.2389(8) 0.060(3) Uani 1 d . . . H45 H -0.1278 -0.1263 0.2878 0.072 Uiso 1 calc R . . C46 C 0.0099(9) -0.0578(6) 0.2472(6) 0.046(2) Uani 1 d . . . N51 N 0.2202(8) 0.0323(5) 0.3426(5) 0.0434(17) Uani 1 d . . . C53 C 0.0300(14) 0.0352(8) 0.3993(8) 0.071(3) Uani 1 d . . . H53 H -0.0595 0.0140 0.3927 0.085 Uiso 1 calc R . . C52 C 0.0881(10) 0.0037(6) 0.3326(6) 0.047(2) Uani 1 d . . . C54 C 0.1068(14) 0.0976(8) 0.4746(7) 0.074(3) Uani 1 d . . . H54 H 0.0687 0.1204 0.5180 0.089 Uiso 1 calc R . . C55 C 0.2395(14) 0.1255(8) 0.4843(7) 0.070(3) Uani 1 d . . . H55 H 0.2926 0.1667 0.5351 0.084 Uiso 1 calc R . . C56 C 0.2955(11) 0.0921(6) 0.4180(6) 0.054(2) Uani 1 d . . . N61 N 0.4741(8) 0.1119(5) 0.3501(5) 0.0447(17) Uani 1 d . . . C62 C 0.4369(10) 0.1194(6) 0.4255(6) 0.048(2) Uani 1 d . . . C63 C 0.5335(14) 0.1508(9) 0.5087(7) 0.082(4) Uani 1 d . . . H63 H 0.5071 0.1559 0.5597 0.098 Uiso 1 calc R . . C64 C 0.6668(14) 0.1743(9) 0.5161(8) 0.090(5) Uani 1 d . . . H64 H 0.7313 0.1951 0.5713 0.108 Uiso 1 calc R . . C65 C 0.7023(13) 0.1663(8) 0.4397(8) 0.078(4) Uani 1 d . . . H65 H 0.7918 0.1814 0.4423 0.094 Uiso 1 calc R . . C66 C 0.6042(10) 0.1357(6) 0.3593(7) 0.056(2) Uani 1 d . . . H66 H 0.6301 0.1314 0.3082 0.06(3) Uiso 1 calc R . . O11 O 0.2179(7) 0.1485(4) 0.2293(4) 0.0511(16) Uani 1 d . . . N13 N 0.1500(8) 0.1485(5) 0.1502(5) 0.0465(18) Uani 1 d . . . O12 O 0.1363(7) 0.0777(4) 0.0936(4) 0.0521(16) Uani 1 d . . . O14 O 0.1046(8) 0.2135(5) 0.1306(5) 0.068(2) Uani 1 d . . . O21 O 0.4420(7) -0.0694(4) 0.3147(4) 0.0522(16) Uani 1 d . . . N23 N 0.5404(8) -0.0646(5) 0.2837(5) 0.0496(19) Uani 1 d . . . O22 O 0.5212(6) -0.0328(4) 0.2132(4) 0.0514(15) Uani 1 d . . . O24 O 0.6478(8) -0.0855(6) 0.3173(6) 0.085(3) Uani 1 d . . . N71 N 0.5491(7) 0.5020(5) 0.8174(5) 0.0416(16) Uani 1 d . . . C72 C 0.5575(9) 0.5326(6) 0.9045(6) 0.045(2) Uani 1 d . . . H72 H 0.4807 0.5231 0.9220 0.054 Uiso 1 calc R . . C73 C 0.6763(11) 0.5771(7) 0.9670(7) 0.061(3) Uani 1 d . . . H73 H 0.6792 0.5972 1.0257 0.073 Uiso 1 calc R . . C74 C 0.7886(11) 0.5913(8) 0.9422(8) 0.067(3) Uani 1 d . . . H74 H 0.8689 0.6219 0.9836 0.080 Uiso 1 calc R . . C75 C 0.7835(9) 0.5605(7) 0.8562(8) 0.056(2) Uani 1 d . . . H75 H 0.8599 0.5704 0.8384 0.067 Uiso 1 calc R . . C76 C 0.6630(9) 0.5141(6) 0.7953(6) 0.045(2) Uani 1 d . . . N81 N 0.5262(7) 0.4442(5) 0.6440(5) 0.0421(16) Uani 1 d . . . C82 C 0.6516(9) 0.4731(6) 0.7010(6) 0.045(2) Uani 1 d . . . C83 C 0.7672(10) 0.4623(7) 0.6730(8) 0.058(3) Uani 1 d . . . H83 H 0.8537 0.4825 0.7122 0.069 Uiso 1 calc R . . C84 C 0.7477(11) 0.4216(8) 0.5870(8) 0.064(3) Uani 1 d . . . H84 H 0.8222 0.4124 0.5678 0.077 Uiso 1 calc R . . C85 C 0.6200(11) 0.3938(7) 0.5277(7) 0.061(3) Uani 1 d . . . H85 H 0.6078 0.3669 0.4688 0.073 Uiso 1 calc R . . C86 C 0.5105(10) 0.4068(6) 0.5579(6) 0.048(2) Uani 1 d . . . N91 N 0.2722(8) 0.3908(5) 0.5369(5) 0.0493(19) Uani 1 d . . . C92 C 0.3698(10) 0.3793(6) 0.4991(6) 0.047(2) Uani 1 d . . . C93 C 0.3407(13) 0.3492(7) 0.4069(7) 0.065(3) Uani 1 d . . . H93 H 0.4103 0.3424 0.3820 0.078 Uiso 1 calc R . . C94 C 0.2089(14) 0.3300(7) 0.3539(7) 0.071(3) Uani 1 d . . . H94 H 0.1876 0.3083 0.2931 0.086 Uiso 1 calc R . . C95 C 0.1091(13) 0.3433(7) 0.3927(7) 0.065(3) Uani 1 d . . . H95 H 0.0192 0.3327 0.3579 0.079 Uiso 1 calc R . . C96 C 0.1425(11) 0.3721(7) 0.4824(7) 0.061(3) Uani 1 d . . . H96 H 0.0734 0.3794 0.5076 0.073 Uiso 1 calc R . . O31 O 0.4628(6) 0.3109(4) 0.7223(4) 0.0484(15) Uani 1 d . . . N33 N 0.4402(8) 0.3005(5) 0.7937(5) 0.0485(18) Uani 1 d . . . O32 O 0.3618(6) 0.3493(4) 0.8187(4) 0.0472(14) Uani 1 d . . . O34 O 0.4902(8) 0.2489(5) 0.8344(5) 0.071(2) Uani 1 d . . . O41 O 0.1868(7) 0.2746(5) 0.6427(5) 0.0640(19) Uani 1 d . . . N43 N 0.0770(9) 0.2980(6) 0.6482(6) 0.057(2) Uani 1 d . . . O44 O -0.0278(8) 0.2436(6) 0.6244(7) 0.091(3) Uani 1 d . . . O42 O 0.0806(8) 0.3786(5) 0.6755(6) 0.076(2) Uani 1 d . . . O61 O 0.2658(7) 0.5187(5) 0.8163(5) 0.067(2) Uani 1 d . . . N63 N 0.1596(9) 0.5377(6) 0.8331(6) 0.059(2) Uani 1 d . . . O62 O 0.0972(12) 0.4943(11) 0.8661(8) 0.139(5) Uani 1 d . . . O64 O 0.1156(13) 0.6038(7) 0.8132(8) 0.117(4) Uani 1 d . . . O51 O 0.3765(7) 0.5829(4) 0.6834(5) 0.0538(16) Uani 1 d . . . O52 O 0.1648(7) 0.5320(5) 0.6338(5) 0.0638(19) Uani 1 d . . . O54 O 0.2356(10) 0.6690(6) 0.6366(7) 0.091(3) Uani 1 d . . . N53 N 0.2561(10) 0.5960(5) 0.6493(6) 0.056(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 Ho1 0.0396(2) 0.0350(2) 0.0341(2) 0.00964(15) 0.01094(17) 0.00517(16) Ho2 0.0334(2) 0.0365(2) 0.0378(2) 0.00506(16) 0.01087(17) 0.00579(16) N11 0.046(4) 0.036(4) 0.049(4) 0.015(3) 0.010(4) 0.005(3) C12 0.060(6) 0.052(6) 0.066(7) 0.026(5) 0.007(5) 0.006(5) C13 0.078(8) 0.051(6) 0.096(9) 0.038(6) 0.023(7) 0.004(5) C14 0.062(7) 0.039(5) 0.109(10) 0.022(6) 0.016(7) 0.003(5) C15 0.047(5) 0.035(5) 0.080(7) 0.000(5) 0.011(5) -0.003(4) C16 0.034(4) 0.041(4) 0.052(5) 0.008(4) 0.008(4) 0.007(4) N21 0.031(3) 0.037(3) 0.041(4) 0.005(3) 0.010(3) 0.002(3) C22 0.035(4) 0.045(5) 0.047(5) 0.013(4) 0.013(4) 0.008(4) C23 0.043(5) 0.051(5) 0.040(5) -0.009(4) 0.009(4) -0.006(4) C24 0.056(6) 0.071(7) 0.040(5) 0.007(5) 0.018(5) 0.006(5) C25 0.060(6) 0.066(6) 0.030(4) 0.010(4) 0.014(4) 0.005(5) C26 0.042(5) 0.035(4) 0.045(5) 0.011(4) 0.013(4) 0.008(4) N31 0.044(4) 0.040(4) 0.035(4) 0.013(3) 0.007(3) 0.007(3) C32 0.038(5) 0.043(4) 0.046(5) 0.014(4) 0.016(4) 0.012(4) C33 0.044(5) 0.037(4) 0.044(5) 0.015(4) 0.012(4) 0.008(4) C34 0.055(6) 0.056(6) 0.058(6) 0.031(5) 0.024(5) 0.008(5) C35 0.055(6) 0.033(4) 0.067(6) 0.016(4) 0.012(5) -0.003(4) C36 0.054(6) 0.041(5) 0.047(5) 0.009(4) 0.012(4) 0.010(4) N41 0.039(4) 0.042(4) 0.042(4) 0.010(3) 0.011(3) 0.005(3) C42 0.041(5) 0.053(5) 0.046(5) 0.015(4) 0.005(4) 0.010(4) C43 0.045(6) 0.056(6) 0.058(6) 0.014(5) 0.000(5) 0.003(4) C44 0.056(7) 0.057(6) 0.078(8) 0.024(6) 0.006(6) -0.008(5) C45 0.047(6) 0.076(7) 0.069(7) 0.035(6) 0.024(5) 0.007(5) C46 0.038(5) 0.048(5) 0.057(6) 0.020(4) 0.017(4) 0.006(4) N51 0.050(4) 0.045(4) 0.033(4) 0.006(3) 0.010(3) 0.005(3) C53 0.092(9) 0.070(7) 0.065(7) 0.020(6) 0.044(7) 0.014(6) C52 0.055(6) 0.051(5) 0.051(5) 0.028(4) 0.029(5) 0.019(4) C54 0.099(10) 0.080(8) 0.051(6) 0.007(6) 0.037(7) 0.016(7) C55 0.100(10) 0.071(7) 0.040(5) 0.003(5) 0.032(6) 0.003(7) C56 0.076(7) 0.044(5) 0.042(5) 0.021(4) 0.013(5) 0.002(5) N61 0.044(4) 0.048(4) 0.044(4) 0.016(3) 0.014(4) 0.005(3) C62 0.056(6) 0.040(5) 0.043(5) 0.014(4) 0.008(4) -0.002(4) C63 0.097(10) 0.101(9) 0.025(5) 0.015(5) -0.004(6) -0.015(8) C64 0.080(9) 0.109(10) 0.046(7) 0.021(7) -0.021(7) -0.032(8) C65 0.064(7) 0.074(8) 0.076(8) 0.024(6) -0.005(7) -0.016(6) C66 0.050(6) 0.054(6) 0.058(6) 0.018(5) 0.009(5) -0.005(4) O11 0.066(4) 0.055(4) 0.038(3) 0.014(3) 0.019(3) 0.018(3) N13 0.047(4) 0.036(4) 0.059(5) 0.014(4) 0.017(4) 0.012(3) O12 0.064(4) 0.040(3) 0.049(4) 0.008(3) 0.015(3) 0.006(3) O14 0.076(5) 0.062(4) 0.073(5) 0.028(4) 0.019(4) 0.034(4) O21 0.056(4) 0.061(4) 0.046(4) 0.023(3) 0.018(3) 0.012(3) N23 0.055(5) 0.054(4) 0.040(4) 0.015(4) 0.008(4) 0.019(4) O22 0.048(4) 0.063(4) 0.050(4) 0.021(3) 0.018(3) 0.014(3) O24 0.064(5) 0.106(7) 0.088(6) 0.040(5) 0.006(5) 0.040(5) N71 0.037(4) 0.043(4) 0.045(4) 0.012(3) 0.013(3) 0.004(3) C72 0.033(4) 0.055(5) 0.049(5) 0.015(4) 0.015(4) 0.004(4) C73 0.059(7) 0.062(6) 0.046(6) 0.006(5) -0.001(5) 0.002(5) C74 0.044(6) 0.073(7) 0.066(7) 0.006(6) -0.003(5) 0.003(5) C75 0.031(5) 0.063(6) 0.076(7) 0.021(5) 0.017(5) 0.005(4) C76 0.041(5) 0.038(4) 0.055(5) 0.018(4) 0.006(4) 0.007(4) N81 0.045(4) 0.042(4) 0.042(4) 0.015(3) 0.012(3) 0.016(3) C82 0.043(5) 0.046(5) 0.056(5) 0.020(4) 0.021(4) 0.018(4) C83 0.040(5) 0.067(6) 0.087(8) 0.040(6) 0.034(5) 0.016(5) C84 0.051(6) 0.090(8) 0.080(8) 0.040(6) 0.045(6) 0.031(6) C85 0.066(7) 0.078(7) 0.054(6) 0.018(5) 0.035(6) 0.031(6) C86 0.063(6) 0.047(5) 0.049(5) 0.022(4) 0.029(5) 0.028(5) N91 0.050(5) 0.050(4) 0.041(4) 0.000(3) 0.010(4) 0.007(4) C92 0.065(6) 0.038(4) 0.040(5) 0.011(4) 0.016(4) 0.021(4) C93 0.095(9) 0.063(6) 0.041(5) 0.010(5) 0.025(6) 0.027(6) C94 0.106(10) 0.053(6) 0.043(6) -0.006(5) 0.015(6) 0.017(6) C95 0.076(8) 0.065(7) 0.046(6) 0.007(5) 0.009(5) 0.010(6) C96 0.054(6) 0.063(6) 0.057(6) 0.009(5) 0.007(5) 0.010(5) O31 0.045(4) 0.046(3) 0.060(4) 0.016(3) 0.024(3) 0.006(3) N33 0.049(5) 0.045(4) 0.052(5) 0.016(4) 0.015(4) 0.004(4) O32 0.050(4) 0.045(3) 0.050(4) 0.010(3) 0.021(3) 0.004(3) O34 0.074(5) 0.074(5) 0.078(5) 0.045(4) 0.022(4) 0.023(4) O41 0.051(4) 0.068(5) 0.064(5) 0.006(4) 0.011(4) 0.003(4) N43 0.046(5) 0.063(5) 0.049(5) 0.014(4) -0.004(4) -0.005(4) O44 0.048(4) 0.094(6) 0.103(7) 0.013(5) -0.004(5) -0.023(4) O42 0.055(4) 0.054(4) 0.108(7) -0.001(4) 0.023(5) 0.003(3) O61 0.043(4) 0.093(5) 0.058(4) -0.014(4) 0.023(3) 0.019(4) N63 0.061(6) 0.064(5) 0.046(5) 0.001(4) 0.010(4) 0.020(5) O62 0.090(8) 0.241(15) 0.109(9) 0.085(10) 0.050(7) -0.009(9) O64 0.158(11) 0.084(7) 0.122(9) 0.019(6) 0.047(8) 0.070(7) O51 0.046(4) 0.053(4) 0.068(4) 0.018(3) 0.019(3) 0.020(3) O52 0.053(4) 0.067(5) 0.065(5) 0.014(4) 0.007(4) 0.016(4) O54 0.097(7) 0.078(6) 0.128(8) 0.056(6) 0.048(6) 0.045(5) N53 0.076(6) 0.049(5) 0.065(5) 0.026(4) 0.039(5) 0.028(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 Ho1 O11 2.405(6) . ? Ho1 O22 2.421(6) . ? Ho1 N31 2.538(7) . ? Ho1 N21 2.541(7) . ? Ho1 O21 2.545(6) . ? Ho1 N11 2.558(7) . ? Ho1 N41 2.559(7) . ? Ho1 N51 2.560(7) . ? Ho1 O12 2.598(6) . ? Ho1 N61 2.605(7) . ? Ho2 O61 2.323(6) . ? Ho2 O51 2.435(7) . ? Ho2 O32 2.439(6) . ? Ho2 O42 2.495(8) . ? Ho2 O31 2.509(6) . ? Ho2 N91 2.514(7) . ? Ho2 N71 2.531(7) . ? Ho2 N81 2.544(7) . ? Ho2 O52 2.556(7) . ? Ho2 O41 2.580(7) . ? N11 C16 1.351(12) . ? N11 C12 1.345(12) . ? C12 C13 1.358(15) . ? C13 C14 1.369(18) . ? C14 C15 1.396(16) . ? C15 C16 1.392(12) . ? C16 C22 1.480(13) . ? N21 C26 1.345(11) . ? N21 C22 1.363(11) . ? C22 C23 1.412(12) . ? C23 C24 1.369(14) . ? C24 C25 1.373(14) . ? C25 C26 1.408(12) . ? C26 C32 1.471(12) . ? N31 C36 1.349(11) . ? N31 C32 1.372(11) . ? C32 C33 1.383(12) . ? C33 C34 1.365(13) . ? C34 C35 1.386(14) . ? C35 C36 1.386(13) . ? N41 C42 1.335(11) . ? N41 C46 1.338(12) . ? C42 C43 1.399(14) . ? C43 C44 1.369(16) . ? C44 C45 1.356(15) . ? C45 C46 1.390(13) . ? C46 C52 1.481(13) . ? N51 C52 1.363(12) . ? N51 C56 1.361(12) . ? C53 C54 1.382(17) . ? C53 C52 1.412(14) . ? C54 C55 1.368(17) . ? C55 C56 1.400(15) . ? C56 C62 1.462(14) . ? N61 C66 1.333(12) . ? N61 C62 1.365(12) . ? C62 C63 1.399(13) . ? C63 C64 1.371(18) . ? C64 C65 1.370(19) . ? C65 C66 1.374(15) . ? O11 N13 1.276(10) . ? N13 O14 1.216(9) . ? N13 O12 1.256(9) . ? O21 N23 1.265(10) . ? N23 O24 1.209(10) . ? N23 O22 1.296(10) . ? N71 C76 1.341(12) . ? N71 C72 1.370(11) . ? C72 C73 1.379(13) . ? C73 C74 1.354(16) . ? C74 C75 1.363(16) . ? C75 C76 1.389(13) . ? C76 C82 1.501(13) . ? N81 C82 1.349(12) . ? N81 C86 1.356(11) . ? C82 C83 1.419(12) . ? C83 C84 1.359(16) . ? C84 C85 1.379(16) . ? C85 C86 1.383(13) . ? C86 C92 1.480(14) . ? N91 C92 1.338(12) . ? N91 C96 1.362(13) . ? C92 C93 1.407(13) . ? C93 C94 1.372(17) . ? C94 C95 1.372(17) . ? C95 C96 1.363(14) . ? O31 N33 1.273(10) . ? N33 O34 1.199(10) . ? N33 O32 1.268(10) . ? O41 N43 1.261(11) . ? N43 O44 1.232(11) . ? N43 O42 1.238(11) . ? O61 N63 1.265(10) . ? N63 O62 1.186(13) . ? N63 O64 1.227(12) . ? O51 N53 1.279(11) . ? O52 N53 1.242(11) . ? O54 N53 1.218(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 O11 Ho1 O22 136.2(2) . . ? O11 Ho1 N31 72.1(2) . . ? O22 Ho1 N31 75.1(2) . . ? O11 Ho1 N21 115.8(2) . . ? O22 Ho1 N21 73.2(2) . . ? N31 Ho1 N21 64.5(2) . . ? O11 Ho1 O21 131.6(2) . . ? O22 Ho1 O21 51.7(2) . . ? N31 Ho1 O21 122.3(2) . . ? N21 Ho1 O21 111.5(2) . . ? O11 Ho1 N11 145.2(2) . . ? O22 Ho1 N11 78.4(2) . . ? N31 Ho1 N11 126.9(2) . . ? N21 Ho1 N11 64.2(2) . . ? O21 Ho1 N11 67.4(2) . . ? O11 Ho1 N41 80.0(2) . . ? O22 Ho1 N41 143.8(2) . . ? N31 Ho1 N41 129.9(2) . . ? N21 Ho1 N41 93.5(2) . . ? O21 Ho1 N41 107.4(2) . . ? N11 Ho1 N41 65.6(2) . . ? O11 Ho1 N51 68.5(2) . . ? O22 Ho1 N51 121.1(2) . . ? N31 Ho1 N51 134.3(2) . . ? N21 Ho1 N51 156.5(2) . . ? O21 Ho1 N51 72.6(2) . . ? N11 Ho1 N51 98.7(2) . . ? N41 Ho1 N51 63.9(2) . . ? O11 Ho1 O12 50.5(2) . . ? O22 Ho1 O12 133.0(2) . . ? N31 Ho1 O12 64.5(2) . . ? N21 Ho1 O12 68.5(2) . . ? O21 Ho1 O12 172.9(2) . . ? N11 Ho1 O12 107.1(2) . . ? N41 Ho1 O12 65.7(2) . . ? N51 Ho1 O12 104.5(2) . . ? O11 Ho1 N61 74.0(2) . . ? O22 Ho1 N61 73.8(2) . . ? N31 Ho1 N61 82.8(2) . . ? N21 Ho1 N61 138.2(2) . . ? O21 Ho1 N61 64.0(2) . . ? N11 Ho1 N61 131.4(2) . . ? N41 Ho1 N61 128.1(2) . . ? N51 Ho1 N61 65.0(2) . . ? O12 Ho1 N61 121.1(2) . . ? O61 Ho2 O51 77.6(3) . . ? O61 Ho2 O32 75.3(3) . . ? O51 Ho2 O32 140.1(2) . . ? O61 Ho2 O42 74.2(3) . . ? O51 Ho2 O42 115.1(2) . . ? O32 Ho2 O42 84.8(3) . . ? O61 Ho2 O31 123.9(3) . . ? O51 Ho2 O31 132.6(2) . . ? O32 Ho2 O31 51.3(2) . . ? O42 Ho2 O31 111.6(2) . . ? O61 Ho2 N91 143.3(3) . . ? O51 Ho2 N91 83.7(2) . . ? O32 Ho2 N91 134.1(2) . . ? O42 Ho2 N91 85.9(3) . . ? O31 Ho2 N91 91.9(2) . . ? O61 Ho2 N71 76.1(2) . . ? O51 Ho2 N71 73.4(2) . . ? O32 Ho2 N71 72.1(2) . . ? O42 Ho2 N71 146.1(3) . . ? O31 Ho2 N71 72.7(2) . . ? N91 Ho2 N71 128.0(3) . . ? O61 Ho2 N81 134.4(2) . . ? O51 Ho2 N81 70.3(2) . . ? O32 Ho2 N81 110.8(2) . . ? O42 Ho2 N81 149.1(3) . . ? O31 Ho2 N81 65.6(2) . . ? N91 Ho2 N81 64.0(2) . . ? N71 Ho2 N81 64.4(2) . . ? O61 Ho2 O52 72.5(3) . . ? O51 Ho2 O52 50.8(2) . . ? O32 Ho2 O52 140.7(2) . . ? O42 Ho2 O52 65.3(3) . . ? O31 Ho2 O52 162.7(2) . . ? N91 Ho2 O52 71.1(2) . . ? N71 Ho2 O52 120.0(2) . . ? N81 Ho2 O52 107.7(2) . . ? O61 Ho2 O41 114.1(3) . . ? O51 Ho2 O41 149.8(2) . . ? O32 Ho2 O41 69.4(2) . . ? O42 Ho2 O41 49.3(2) . . ? O31 Ho2 O41 65.7(2) . . ? N91 Ho2 O41 70.6(3) . . ? N71 Ho2 O41 135.3(2) . . ? N81 Ho2 O41 109.9(2) . . ? O52 Ho2 O41 104.2(2) . . ? C16 N11 C12 117.7(8) . . ? C16 N11 Ho1 120.4(6) . . ? C12 N11 Ho1 121.6(7) . . ? N11 C12 C13 123.6(11) . . ? C12 C13 C14 120.4(11) . . ? C13 C14 C15 116.7(10) . . ? C16 C15 C14 121.0(11) . . ? N11 C16 C15 120.5(9) . . ? N11 C16 C22 116.7(8) . . ? C15 C16 C22 122.7(9) . . ? C26 N21 C22 119.7(7) . . ? C26 N21 Ho1 119.5(5) . . ? C22 N21 Ho1 119.7(6) . . ? N21 C22 C23 120.5(8) . . ? N21 C22 C16 116.8(8) . . ? C23 C22 C16 122.7(8) . . ? C24 C23 C22 119.7(8) . . ? C23 C24 C25 119.2(9) . . ? C24 C25 C26 120.0(9) . . ? N21 C26 C25 120.7(8) . . ? N21 C26 C32 117.7(8) . . ? C25 C26 C32 121.6(8) . . ? C36 N31 C32 116.9(8) . . ? C36 N31 Ho1 122.6(6) . . ? C32 N31 Ho1 120.0(5) . . ? N31 C32 C33 121.7(8) . . ? N31 C32 C26 116.3(8) . . ? C33 C32 C26 122.0(8) . . ? C34 C33 C32 120.5(9) . . ? C33 C34 C35 118.7(9) . . ? C36 C35 C34 118.8(9) . . ? N31 C36 C35 123.4(9) . . ? C42 N41 C46 118.3(8) . . ? C42 N41 Ho1 117.9(6) . . ? C46 N41 Ho1 119.7(6) . . ? N41 C42 C43 121.9(9) . . ? C44 C43 C42 118.5(10) . . ? C45 C44 C43 120.0(10) . . ? C44 C45 C46 118.7(10) . . ? N41 C46 C45 122.4(9) . . ? N41 C46 C52 114.8(8) . . ? C45 C46 C52 122.8(9) . . ? C52 N51 C56 118.9(8) . . ? C52 N51 Ho1 119.3(5) . . ? C56 N51 Ho1 119.3(6) . . ? C54 C53 C52 119.7(12) . . ? N51 C52 C53 120.7(10) . . ? N51 C52 C46 116.3(7) . . ? C53 C52 C46 122.9(10) . . ? C55 C54 C53 119.1(10) . . ? C54 C55 C56 120.1(11) . . ? N51 C56 C55 121.4(10) . . ? N51 C56 C62 116.4(9) . . ? C55 C56 C62 122.2(10) . . ? C66 N61 C62 117.6(8) . . ? C66 N61 Ho1 123.4(6) . . ? C62 N61 Ho1 116.4(6) . . ? N61 C62 C63 120.3(10) . . ? N61 C62 C56 119.1(8) . . ? C63 C62 C56 120.6(10) . . ? C64 C63 C62 120.8(11) . . ? C63 C64 C65 118.1(11) . . ? C64 C65 C66 119.3(12) . . ? N61 C66 C65 123.9(11) . . ? N13 O11 Ho1 101.0(5) . . ? O14 N13 O12 122.3(8) . . ? O14 N13 O11 122.1(8) . . ? O12 N13 O11 115.6(7) . . ? N13 O12 Ho1 92.2(5) . . ? N23 O21 Ho1 93.6(4) . . ? O24 N23 O21 123.8(8) . . ? O24 N23 O22 120.6(9) . . ? O21 N23 O22 115.6(7) . . ? N23 O22 Ho1 98.7(5) . . ? C76 N71 C72 117.3(8) . . ? C76 N71 Ho2 121.8(6) . . ? C72 N71 Ho2 120.8(6) . . ? N71 C72 C73 122.0(9) . . ? C74 C73 C72 119.4(10) . . ? C73 C74 C75 119.8(10) . . ? C74 C75 C76 119.3(10) . . ? N71 C76 C75 122.1(9) . . ? N71 C76 C82 115.5(8) . . ? C75 C76 C82 122.4(9) . . ? C82 N81 C86 119.4(8) . . ? C82 N81 Ho2 119.9(6) . . ? C86 N81 Ho2 119.7(6) . . ? N81 C82 C83 121.0(9) . . ? N81 C82 C76 117.1(8) . . ? C83 C82 C76 121.8(9) . . ? C84 C83 C82 117.9(10) . . ? C83 C84 C85 121.5(9) . . ? C84 C85 C86 118.3(10) . . ? N81 C86 C85 121.7(10) . . ? N81 C86 C92 116.1(8) . . ? C85 C86 C92 122.2(9) . . ? C92 N91 C96 117.3(8) . . ? C92 N91 Ho2 121.3(6) . . ? C96 N91 Ho2 121.2(7) . . ? N91 C92 C93 121.8(10) . . ? N91 C92 C86 116.8(8) . . ? C93 C92 C86 121.3(10) . . ? C94 C93 C92 119.5(11) . . ? C95 C94 C93 118.6(10) . . ? C96 C95 C94 119.6(11) . . ? C95 C96 N91 123.2(11) . . ? N33 O31 Ho2 95.2(5) . . ? O34 N33 O32 122.6(9) . . ? O34 N33 O31 122.5(8) . . ? O32 N33 O31 114.8(7) . . ? N33 O32 Ho2 98.7(5) . . ? N43 O41 Ho2 94.9(6) . . ? O42 N43 O44 122.8(10) . . ? O44 N43 O41 121.2(10) . . ? O42 N43 O41 116.0(8) . . ? N43 O42 Ho2 99.8(6) . . ? N63 O61 Ho2 138.2(6) . . ? O62 N63 O64 117.0(12) . . ? O62 N63 O61 123.8(11) . . ? O64 N63 O61 119.2(11) . . ? N63 O61 Ho2 98.8(6) . . ? N63 O62 Ho2 94.0(5) . . ? O54 N53 O52 123.5(10) . . ? O54 N53 O51 120.1(10) . . ? O52 N53 O51 116.3(7) . . ? _refine_diff_density_max 1.542 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.140 #====END data_3-Ho _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 Ho N12 O10' _chemical_formula_weight 958.67 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.994(12) _cell_length_b 14.697(17) _cell_length_c 14.954(17) _cell_angle_alpha 70.007(10) _cell_angle_beta 78.049(10) _cell_angle_gamma 79.783(10) _cell_volume 2006(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 2.043 _exptl_absorpt_correction_type DIFABS, (Walker and Stuart, 1983 ) _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 5583 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.03 _reflns_number_total 5583 _reflns_number_gt 3536 _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^)+(0.1295P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5583 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 Ho1 Ho 0.24988(5) 0.25530(4) 0.20274(4) 0.0497(2) Uani 1 d . . . O100 O 0.3744(7) 0.3172(6) 0.2799(6) 0.057(2) Uani 1 d . . . O41 O 0.2528(9) 0.3098(7) 0.0263(7) 0.070(2) Uani 1 d . . . O42 O 0.4337(7) 0.3218(6) 0.0701(6) 0.059(2) Uani 1 d . . . N43 N 0.3708(10) 0.3314(9) 0.0021(8) 0.064(3) Uani 1 d . . . O44 O 0.4202(11) 0.3681(10) -0.0817(7) 0.099(4) Uani 1 d . . . N63 N 0.4828(10) 0.1046(8) 0.1632(9) 0.063(3) Uani 1 d . . . O64 O 0.5893(11) 0.0547(10) 0.1517(11) 0.120(5) Uani 1 d . . . O61 O 0.4580(12) 0.1422(8) 0.2293(7) 0.091(4) Uani 1 d . . . O62 O 0.3884(12) 0.1219(9) 0.1169(8) 0.097(3) Uani 1 d . . . O52 O 0.0916(8) 0.2832(6) 0.3409(6) 0.060(2) Uani 1 d . . . O54 O 0.0964(11) 0.1973(10) 0.4917(7) 0.092(4) Uani 1 d . . . N53 N 0.1407(9) 0.2084(8) 0.4070(7) 0.050(2) Uani 1 d . . . O51 O 0.2320(9) 0.1526(6) 0.3774(6) 0.055(2) Uani 1 d . . . C12 C -0.0805(16) 0.0595(14) 0.2114(14) 0.092(5) Uani 1 d . . . H12 H -0.1650 0.0709 0.1902 0.111 Uiso 1 calc R . . C16 C -0.0158(12) 0.1356(10) 0.2047(9) 0.058(3) Uani 1 d . . . C13 C 0.1644(15) 0.0252(10) 0.2712(12) 0.075(4) Uani 1 d . . . H13 H 0.2489 0.0144 0.2922 0.090 Uiso 1 calc R . . C15 C -0.0211(19) -0.0359(13) 0.2498(14) 0.093(5) Uani 1 d . . . H15 H -0.0659 -0.0881 0.2549 0.112 Uiso 1 calc R . . C14 C 0.1041(19) -0.0520(11) 0.2801(12) 0.087(4) Uani 1 d . . . H14 H 0.1456 -0.1150 0.3061 0.104 Uiso 1 calc R . . N11 N 0.1085(10) 0.1203(8) 0.2324(8) 0.061(3) Uani 1 d . . . N21 N 0.0055(8) 0.3065(7) 0.1651(7) 0.047(2) Uani 1 d . . . C22 C -0.0764(12) 0.2386(10) 0.1736(9) 0.063(3) Uani 1 d . . . C23 C -0.2129(12) 0.2643(12) 0.1576(10) 0.070(4) Uani 1 d . . . H23 H -0.2674 0.2171 0.1627 0.084 Uiso 1 calc R . . C24 C -0.2650(12) 0.3619(14) 0.1339(12) 0.081(5) Uani 1 d . . . H24 H -0.3565 0.3811 0.1253 0.097 Uiso 1 calc R . . C25 C -0.1812(12) 0.4288(11) 0.1233(10) 0.069(3) Uani 1 d . . . H25 H -0.2143 0.4947 0.1032 0.083 Uiso 1 calc R . . C26 C -0.0447(10) 0.4014(9) 0.1422(8) 0.052(3) Uani 1 d . . . C32 C 0.0475(12) 0.4727(9) 0.1330(9) 0.055(3) Uani 1 d . . . N31 N 0.1790(9) 0.4358(7) 0.1466(7) 0.051(2) Uani 1 d . . . C33 C 0.0983(15) 0.6358(10) 0.1002(12) 0.077(4) Uani 1 d . . . H33 H 0.0717 0.7024 0.0860 0.093 Uiso 1 calc R . . C34 C 0.2333(13) 0.5964(9) 0.1118(11) 0.068(3) Uani 1 d . . . H34 H 0.2991 0.6366 0.1053 0.082 Uiso 1 calc R . . C35 C 0.2681(12) 0.4979(9) 0.1328(10) 0.061(3) Uani 1 d . . . H35 H 0.3596 0.4731 0.1377 0.073 Uiso 1 calc R . . C36 C 0.0044(15) 0.5721(10) 0.1106(11) 0.073(4) Uani 1 d . . . H36 H -0.0865 0.5957 0.1026 0.088 Uiso 1 calc R . . N51 N 0.5146(9) 0.3966(7) 0.3859(7) 0.052(2) Uani 1 d . . . C52 C 0.6496(11) 0.3589(9) 0.3823(8) 0.051(3) Uani 1 d . . . C53 C 0.7515(13) 0.4189(14) 0.3577(12) 0.083(5) Uani 1 d . . . H53 H 0.8431 0.3919 0.3558 0.099 Uiso 1 calc R . . C54 C 0.7197(14) 0.5186(13) 0.3357(13) 0.088(5) Uani 1 d . . . H54 H 0.7890 0.5583 0.3220 0.106 Uiso 1 calc R . . C55 C 0.5829(16) 0.5593(12) 0.3340(13) 0.085(4) Uani 1 d . . . H55 H 0.5583 0.6264 0.3146 0.102 Uiso 1 calc R . . C56 C 0.4851(11) 0.4942(9) 0.3629(10) 0.060(3) Uani 1 d . . . N41 N 0.2543(9) 0.4702(8) 0.3608(8) 0.060(3) Uani 1 d . . . C42 C 0.1173(13) 0.4973(12) 0.3688(13) 0.084(5) Uani 1 d . . . H42 H 0.0598 0.4547 0.3673 0.101 Uiso 1 calc R . . C43 C 0.0584(17) 0.5887(12) 0.3793(13) 0.086(5) Uani 1 d . . . H43 H -0.0351 0.6091 0.3786 0.103 Uiso 1 calc R . . C44 C 0.1420(17) 0.6455(11) 0.3905(13) 0.086(5) Uani 1 d . . . H44 H 0.1065 0.7038 0.4025 0.103 Uiso 1 calc R . . C45 C 0.2804(16) 0.6151(10) 0.3838(12) 0.076(4) Uani 1 d . . . H45 H 0.3383 0.6549 0.3901 0.092 Uiso 1 calc R . . C46 C 0.3371(12) 0.5297(9) 0.3684(10) 0.061(3) Uani 1 d . . . N61 N 0.5865(10) 0.2071(7) 0.3825(7) 0.056(2) Uani 1 d . . . C62 C 0.6770(10) 0.2521(9) 0.4050(9) 0.056(3) Uani 1 d . . . C63 C 0.6094(15) 0.1119(10) 0.4029(11) 0.072(4) Uani 1 d . . . H63 H 0.5474 0.0803 0.3889 0.087 Uiso 1 calc R . . C64 C 0.7222(19) 0.0560(11) 0.4445(11) 0.088(5) Uani 1 d . . . H64 H 0.7359 -0.0112 0.4571 0.105 Uiso 1 calc R . . C65 C 0.8114(16) 0.1017(13) 0.4662(11) 0.085(5) Uani 1 d . . . H65 H 0.8860 0.0659 0.4957 0.102 Uiso 1 calc R . . C66 C 0.7913(13) 0.2004(12) 0.4449(10) 0.076(4) Uani 1 d . . . H66 H 0.8542 0.2327 0.4570 0.092 Uiso 1 calc R . . N200 N 0.200(2) 0.2462(17) -0.2127(15) 0.145(8) Uani 1 d . . . C201 C 0.1987(17) 0.1857(16) -0.1382(17) 0.098(6) Uani 1 d . . . C202 C 0.186(3) 0.1075(16) -0.0445(15) 0.126(8) Uani 1 d . . . H20A H 0.0905 0.1066 -0.0158 0.151 Uiso 1 calc R . . H20B H 0.2370 0.1193 -0.0027 0.151 Uiso 1 calc R . . H20C H 0.2212 0.0458 -0.0541 0.151 Uiso 1 calc R . . N100 N 0.820(2) 0.1471(14) -0.064(2) 0.161(9) Uani 1 d . . . C101 C 0.715(2) 0.1434(14) -0.0841(17) 0.106(6) Uani 1 d . . . C102 C 0.590(2) 0.1394(18) -0.1052(16) 0.132(9) Uani 1 d . . . H10A H 0.5199 0.1394 -0.0504 0.158 Uiso 1 calc R . . H10B H 0.5924 0.0809 -0.1208 0.158 Uiso 1 calc R . . H10C H 0.5689 0.1950 -0.1592 0.158 Uiso 1 calc R . . C302 C 0.3516(18) 0.213(2) 0.5774(15) 0.136(10) Uani 1 d . . . H30A H 0.3060 0.2737 0.5858 0.163 Uiso 1 calc R . . H30B H 0.2891 0.1646 0.6036 0.163 Uiso 1 calc R . . H30C H 0.3812 0.2222 0.5099 0.163 Uiso 1 calc R . . C301 C 0.4649(18) 0.1835(14) 0.6246(11) 0.086(5) Uani 1 d . . . N300 N 0.5617(18) 0.1641(17) 0.6599(14) 0.132(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 Ho1 0.0504(3) 0.0465(3) 0.0541(4) -0.0159(2) -0.0130(2) -0.0049(2) O100 0.059(4) 0.056(5) 0.066(5) -0.030(5) -0.016(4) -0.001(4) O41 0.079(6) 0.072(6) 0.063(6) -0.024(5) -0.012(5) -0.011(5) O42 0.050(4) 0.057(5) 0.067(6) -0.017(5) 0.000(4) -0.013(3) N43 0.053(5) 0.077(8) 0.046(7) -0.009(6) -0.002(5) 0.002(5) O44 0.096(7) 0.124(11) 0.043(6) -0.003(7) 0.016(5) -0.006(7) N63 0.056(5) 0.065(7) 0.073(7) -0.032(7) -0.006(6) -0.001(5) O64 0.086(7) 0.118(11) 0.152(12) -0.074(10) -0.004(7) 0.042(8) O61 0.121(8) 0.080(7) 0.068(7) -0.039(6) -0.026(6) 0.045(7) O62 0.104(7) 0.113(9) 0.082(8) -0.026(8) -0.031(7) -0.026(7) O52 0.054(4) 0.066(5) 0.058(5) -0.023(5) -0.011(4) 0.006(4) O54 0.081(6) 0.135(11) 0.056(6) -0.029(7) -0.023(5) 0.003(6) N53 0.055(5) 0.051(6) 0.038(6) -0.004(5) 0.000(4) -0.021(5) O51 0.076(5) 0.034(4) 0.054(5) -0.002(4) -0.024(4) -0.009(4) C12 0.086(9) 0.117(15) 0.097(13) -0.058(13) -0.014(9) -0.025(9) C16 0.064(6) 0.074(8) 0.043(7) -0.022(7) 0.002(6) -0.028(6) C13 0.086(9) 0.055(8) 0.090(11) -0.028(8) -0.017(8) -0.010(7) C15 0.116(12) 0.074(11) 0.102(14) -0.043(11) -0.003(11) -0.032(9) C14 0.120(12) 0.058(9) 0.077(11) -0.015(9) -0.004(9) -0.025(8) N11 0.068(6) 0.064(7) 0.057(6) -0.029(6) 0.005(5) -0.017(5) N21 0.046(4) 0.057(6) 0.043(5) -0.016(5) -0.009(4) -0.010(4) C22 0.063(7) 0.092(10) 0.043(7) -0.025(7) -0.015(6) -0.019(6) C23 0.060(7) 0.106(12) 0.049(7) -0.022(8) -0.003(6) -0.034(7) C24 0.047(6) 0.123(14) 0.081(10) -0.039(11) -0.018(7) -0.006(7) C25 0.049(6) 0.084(10) 0.062(8) -0.006(8) -0.010(6) -0.008(6) C26 0.048(5) 0.065(8) 0.048(7) -0.020(6) -0.020(5) 0.001(5) C32 0.064(6) 0.051(7) 0.048(7) -0.016(6) -0.012(6) 0.001(5) N31 0.054(5) 0.045(5) 0.052(6) -0.015(5) -0.008(4) -0.003(4) C33 0.084(8) 0.048(8) 0.089(11) -0.016(8) -0.006(8) -0.001(7) C34 0.075(7) 0.047(7) 0.078(10) -0.017(8) -0.006(7) -0.010(6) C35 0.064(6) 0.043(6) 0.074(9) -0.017(7) -0.007(6) -0.011(5) C36 0.079(8) 0.061(8) 0.070(9) -0.023(8) -0.012(7) 0.018(7) N51 0.055(5) 0.053(6) 0.048(5) -0.009(5) -0.012(4) -0.012(4) C52 0.051(5) 0.064(7) 0.039(6) -0.014(6) -0.002(5) -0.021(5) C53 0.057(7) 0.125(15) 0.087(11) -0.062(12) -0.007(7) -0.012(8) C54 0.075(8) 0.096(12) 0.105(13) -0.033(12) -0.004(8) -0.048(8) C55 0.102(10) 0.069(9) 0.094(12) -0.033(10) -0.012(9) -0.025(8) C56 0.057(6) 0.053(7) 0.070(9) -0.015(7) -0.010(6) -0.014(5) N41 0.055(5) 0.060(6) 0.073(7) -0.028(6) -0.015(5) -0.008(4) C42 0.062(7) 0.087(11) 0.113(13) -0.051(11) -0.015(8) 0.006(8) C43 0.090(9) 0.075(11) 0.096(12) -0.040(10) -0.021(9) 0.015(9) C44 0.103(11) 0.065(9) 0.102(13) -0.046(10) -0.014(9) -0.003(8) C45 0.098(10) 0.044(7) 0.087(11) -0.019(9) -0.013(9) -0.015(7) C46 0.065(6) 0.058(8) 0.071(9) -0.032(8) -0.018(7) 0.001(6) N61 0.068(5) 0.056(6) 0.044(6) -0.011(5) -0.016(5) -0.007(5) C62 0.043(5) 0.076(9) 0.052(7) -0.028(7) -0.004(5) -0.002(5) C63 0.086(8) 0.050(7) 0.077(10) -0.011(8) -0.022(8) -0.005(7) C64 0.128(13) 0.058(9) 0.060(9) -0.009(8) -0.025(9) 0.025(9) C65 0.077(8) 0.106(13) 0.060(9) -0.020(9) -0.024(8) 0.022(9) C66 0.055(6) 0.106(13) 0.065(8) -0.025(9) -0.019(7) 0.009(7) N200 0.166(17) 0.130(18) 0.113(15) -0.039(16) 0.000(13) 0.024(15) C201 0.082(9) 0.112(16) 0.116(16) -0.073(15) -0.009(11) 0.009(10) C202 0.17(2) 0.094(14) 0.096(15) -0.012(14) -0.048(14) 0.008(15) N100 0.149(16) 0.087(12) 0.25(3) -0.052(18) -0.016(18) -0.040(13) C101 0.117(14) 0.079(12) 0.117(16) -0.016(13) -0.013(13) -0.032(11) C102 0.143(18) 0.17(2) 0.101(16) -0.070(18) -0.021(14) 0.002(16) C302 0.093(12) 0.25(3) 0.095(14) -0.095(19) -0.018(11) -0.023(14) C301 0.090(10) 0.117(14) 0.054(9) -0.025(10) -0.005(8) -0.031(9) N300 0.107(11) 0.18(2) 0.108(14) -0.065(15) 0.006(11) -0.018(12) _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 2.328(7) . ? Ho1 O61 2.431(8) . ? Ho1 O52 2.436(8) . ? Ho1 O42 2.463(9) . ? Ho1 O41 2.478(10) . ? Ho1 N11 2.503(11) . ? Ho1 N31 2.510(9) . ? Ho1 O51 2.518(9) . ? Ho1 N21 2.545(8) . ? Ho1 O62 2.725(11) . ? O41 N43 1.225(14) . ? O42 N43 1.259(12) . ? N43 O44 1.217(15) . ? N63 O64 1.198(12) . ? N63 O62 1.225(13) . ? N63 O61 1.251(12) . ? O52 N53 1.301(12) . ? O54 N53 1.217(13) . ? N53 O51 1.231(11) . ? C12 C16 1.35(2) . ? C12 C15 1.39(3) . ? C16 N11 1.346(15) . ? C16 C22 1.478(19) . ? C13 C14 1.33(2) . ? C13 N11 1.381(18) . ? C15 C14 1.37(2) . ? N21 C26 1.346(15) . ? N21 C22 1.357(16) . ? C22 C23 1.397(16) . ? C23 C24 1.38(2) . ? C24 C25 1.35(2) . ? C25 C26 1.410(15) . ? C26 C32 1.467(17) . ? C32 N31 1.359(13) . ? C32 C36 1.391(18) . ? N31 C35 1.323(16) . ? C33 C36 1.39(2) . ? C33 C34 1.391(18) . ? C34 C35 1.368(18) . ? N51 C56 1.348(16) . ? N51 C52 1.362(13) . ? C52 C53 1.38(2) . ? C52 C62 1.476(18) . ? C53 C54 1.38(2) . ? C54 C55 1.39(2) . ? C55 C56 1.39(2) . ? C56 C46 1.474(15) . ? N41 C42 1.349(15) . ? N41 C46 1.352(16) . ? C42 C43 1.415(18) . ? C43 C44 1.35(2) . ? C44 C45 1.37(2) . ? C45 C46 1.356(16) . ? N61 C63 1.315(17) . ? N61 C62 1.363(15) . ? C62 C66 1.380(15) . ? C63 C64 1.395(19) . ? C64 C65 1.35(2) . ? C65 C66 1.36(2) . ? N200 C201 1.16(3) . ? C201 C202 1.48(3) . ? N100 C101 1.17(3) . ? C101 C102 1.37(3) . ? C302 C301 1.38(2) . ? C301 N300 1.14(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 O61 73.9(3) . . ? O100 Ho1 O52 73.8(3) . . ? O61 Ho1 O52 119.2(3) . . ? O100 Ho1 O42 79.0(3) . . ? O61 Ho1 O42 72.7(4) . . ? O52 Ho1 O42 144.7(3) . . ? O100 Ho1 O41 124.6(3) . . ? O61 Ho1 O41 105.0(3) . . ? O52 Ho1 O41 135.7(3) . . ? O42 Ho1 O41 50.3(3) . . ? O100 Ho1 N11 141.9(3) . . ? O61 Ho1 N11 92.1(4) . . ? O52 Ho1 N11 83.4(3) . . ? O42 Ho1 N11 131.2(3) . . ? O41 Ho1 N11 93.0(3) . . ? O100 Ho1 N31 75.8(3) . . ? O61 Ho1 N31 139.1(4) . . ? O52 Ho1 N31 76.7(3) . . ? O42 Ho1 N31 75.1(3) . . ? O41 Ho1 N31 71.3(3) . . ? N11 Ho1 N31 128.3(3) . . ? O100 Ho1 O51 71.0(3) . . ? O61 Ho1 O51 70.0(3) . . ? O52 Ho1 O51 51.3(3) . . ? O42 Ho1 O51 137.1(3) . . ? O41 Ho1 O51 162.5(3) . . ? N11 Ho1 O51 70.9(3) . . ? N31 Ho1 O51 123.8(3) . . ? O100 Ho1 N21 130.4(2) . . ? O61 Ho1 N21 154.3(4) . . ? O52 Ho1 N21 69.1(3) . . ? O42 Ho1 N21 115.7(3) . . ? O41 Ho1 N21 69.8(3) . . ? N11 Ho1 N21 63.8(3) . . ? N31 Ho1 N21 64.6(3) . . ? O51 Ho1 N21 107.0(3) . . ? O100 Ho1 O62 117.4(3) . . ? O61 Ho1 O62 47.0(3) . . ? O52 Ho1 O62 146.7(4) . . ? O42 Ho1 O62 67.1(3) . . ? O41 Ho1 O62 66.5(3) . . ? N11 Ho1 O62 69.0(3) . . ? N31 Ho1 O62 135.3(3) . . ? O51 Ho1 O62 100.4(3) . . ? N21 Ho1 O62 111.7(3) . . ? N43 O41 Ho1 97.2(7) . . ? N43 O42 Ho1 96.9(7) . . ? O44 N43 O41 122.6(11) . . ? O44 N43 O42 121.6(12) . . ? O41 N43 O42 115.5(11) . . ? O62 N63 O64 126.0(12) . . ? O64 N63 O61 120.3(12) . . ? O62 N63 O61 113.7(9) . . ? N63 O61 Ho1 106.2(7) . . ? N63 O62 Ho1 92.1(6) . . ? N53 O52 Ho1 97.4(5) . . ? O54 N53 O51 124.2(10) . . ? O54 N53 O52 120.1(9) . . ? O51 N53 O52 115.7(8) . . ? N53 O51 Ho1 95.4(6) . . ? C16 C12 C15 120.2(16) . . ? N11 C16 C12 120.6(14) . . ? N11 C16 C22 115.2(11) . . ? C12 C16 C22 124.1(13) . . ? C14 C13 N11 123.6(15) . . ? C14 C15 C12 119.5(15) . . ? C13 C14 C15 118.0(16) . . ? C16 N11 C13 118.0(12) . . ? C16 N11 Ho1 122.8(9) . . ? C13 N11 Ho1 118.9(9) . . ? C26 N21 C22 120.2(9) . . ? C26 N21 Ho1 119.2(7) . . ? C22 N21 Ho1 120.5(8) . . ? N21 C22 C23 121.7(13) . . ? N21 C22 C16 116.7(10) . . ? C23 C22 C16 121.6(13) . . ? C24 C23 C22 118.4(13) . . ? C25 C24 C23 119.1(12) . . ? C24 C25 C26 121.7(14) . . ? N21 C26 C25 118.8(11) . . ? N21 C26 C32 118.5(9) . . ? C25 C26 C32 122.7(11) . . ? N31 C32 C36 121.5(12) . . ? N31 C32 C26 115.9(10) . . ? C36 C32 C26 122.6(11) . . ? C35 N31 C32 118.0(10) . . ? C35 N31 Ho1 120.6(7) . . ? C32 N31 Ho1 121.3(8) . . ? C36 C33 C34 117.8(12) . . ? C35 C34 C33 119.3(13) . . ? N31 C35 C34 123.7(11) . . ? C33 C36 C32 119.5(12) . . ? C56 N51 C52 117.7(11) . . ? N51 C52 C53 120.7(12) . . ? N51 C52 C62 115.8(10) . . ? C53 C52 C62 123.5(11) . . ? C52 C53 C54 120.9(12) . . ? C53 C54 C55 119.4(14) . . ? C56 C55 C54 116.4(14) . . ? N51 C56 C55 124.6(11) . . ? N51 C56 C46 114.8(11) . . ? C55 C56 C46 120.6(12) . . ? C42 N41 C46 119.0(10) . . ? N41 C42 C43 121.9(15) . . ? C44 C43 C42 118.0(13) . . ? C43 C44 C45 118.5(12) . . ? C46 C45 C44 123.1(14) . . ? N41 C46 C45 119.3(11) . . ? N41 C46 C56 116.4(9) . . ? C45 C46 C56 124.3(12) . . ? C63 N61 C62 117.7(9) . . ? N61 C62 C66 121.5(12) . . ? N61 C62 C52 117.1(8) . . ? C66 C62 C52 121.4(11) . . ? N61 C63 C64 123.1(14) . . ? C65 C64 C63 118.5(14) . . ? C64 C65 C66 119.7(11) . . ? C65 C66 C62 119.5(14) . . ? N200 C201 C202 175(3) . . ? N100 C101 C102 178(3) . . ? N300 C301 C302 176(2) . . ? _refine_diff_density_max 1.993 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.123 _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-Er _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 Er N12 O10 ' _chemical_formula_weight 961.00 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.017(12) _cell_length_b 14.742(17) _cell_length_c 14.936(17) _cell_angle_alpha 69.486(10) _cell_angle_beta 78.106(10) _cell_angle_gamma 79.783(10) _cell_volume 2008(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 962 _exptl_absorpt_coefficient_mu 2.161 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 6861 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.98 _reflns_number_total 6861 _reflns_number_gt 5731 _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^)+(0.1243P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0119(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6861 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.442 _refine_ls_restrained_S_all 1.442 _refine_ls_shift/su_max 0.052 _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 0.24723(3) 0.25692(2) 0.20441(3) 0.0509(2) Uani 1 d . . . O100 O 0.3737(6) 0.3180(5) 0.2802(5) 0.0617(15) Uani 1 d . . . O41 O 0.2528(8) 0.3068(7) 0.0291(6) 0.085(2) Uani 1 d . . . O42 O 0.4310(6) 0.3241(5) 0.0720(5) 0.0630(15) Uani 1 d . . . N43 N 0.3704(9) 0.3320(7) 0.0042(7) 0.069(2) Uani 1 d . . . O44 O 0.4173(10) 0.3654(8) -0.0808(6) 0.103(3) Uani 1 d . . . N63 N 0.4823(8) 0.1032(6) 0.1666(6) 0.0662(19) Uani 1 d . . . O64 O 0.5910(10) 0.0563(8) 0.1598(9) 0.123(4) Uani 1 d . . . O61 O 0.4504(10) 0.1418(6) 0.2323(6) 0.088(2) Uani 1 d . . . O62 O 0.3945(10) 0.1196(8) 0.1134(7) 0.105(3) Uani 1 d . . . O52 O 0.0907(6) 0.2851(5) 0.3426(5) 0.0613(14) Uani 1 d . . . O54 O 0.0898(9) 0.1970(8) 0.4937(6) 0.088(3) Uani 1 d . . . N53 N 0.1360(8) 0.2106(6) 0.4094(6) 0.0629(19) Uani 1 d . . . O51 O 0.2304(9) 0.1531(5) 0.3803(5) 0.0734(19) Uani 1 d . . . C12 C -0.0767(12) 0.0559(10) 0.2112(8) 0.080(3) Uani 1 d . . . H12 H -0.1605 0.0666 0.1895 0.096 Uiso 1 calc R . . C16 C -0.0128(10) 0.1357(7) 0.2057(6) 0.060(2) Uani 1 d . . . C13 C 0.1681(11) 0.0273(7) 0.2708(8) 0.067(2) Uani 1 d . . . H13 H 0.2516 0.0159 0.2931 0.080 Uiso 1 calc R . . C15 C -0.0171(16) -0.0364(9) 0.2480(11) 0.098(4) Uani 1 d . . . H15 H -0.0603 -0.0890 0.2524 0.117 Uiso 1 calc R . . C14 C 0.1056(13) -0.0514(8) 0.2781(9) 0.079(3) Uani 1 d . . . H14 H 0.1476 -0.1144 0.3035 0.095 Uiso 1 calc R . . N11 N 0.1132(7) 0.1207(5) 0.2325(5) 0.0553(16) Uani 1 d . . . N21 N 0.0069(7) 0.3051(6) 0.1673(5) 0.0521(15) Uani 1 d . . . C22 C -0.0748(9) 0.2395(8) 0.1731(6) 0.061(2) Uani 1 d . . . C23 C -0.2090(11) 0.2622(9) 0.1580(8) 0.074(3) Uani 1 d . . . H23 H -0.2619 0.2138 0.1644 0.089 Uiso 1 calc R . . C24 C -0.2636(11) 0.3595(11) 0.1329(8) 0.079(3) Uani 1 d . . . H24 H -0.3539 0.3771 0.1213 0.095 Uiso 1 calc R . . C25 C -0.1840(9) 0.4301(8) 0.1253(8) 0.074(3) Uani 1 d . . . H25 H -0.2206 0.4952 0.1111 0.089 Uiso 1 calc R . . C26 C -0.0464(9) 0.4013(7) 0.1395(7) 0.059(2) Uani 1 d . . . C32 C 0.0463(8) 0.4716(6) 0.1328(6) 0.0519(17) Uani 1 d . . . N31 N 0.1777(7) 0.4359(5) 0.1454(5) 0.0498(14) Uani 1 d . . . C33 C 0.0971(12) 0.6361(7) 0.1011(8) 0.074(3) Uani 1 d . . . H33 H 0.0688 0.7021 0.0906 0.088 Uiso 1 calc R . . C34 C 0.2323(11) 0.5993(7) 0.1088(8) 0.073(3) Uani 1 d . . . H34 H 0.2979 0.6407 0.0987 0.088 Uiso 1 calc R . . C35 C 0.2684(9) 0.4999(7) 0.1319(7) 0.060(2) Uani 1 d . . . H35 H 0.3593 0.4754 0.1385 0.072 Uiso 1 calc R . . C36 C 0.0021(10) 0.5724(7) 0.1091(8) 0.071(2) Uani 1 d . . . H36 H -0.0878 0.5964 0.0990 0.085 Uiso 1 calc R . . N51 N 0.5152(8) 0.3965(6) 0.3851(5) 0.0572(17) Uani 1 d . . . C52 C 0.6476(9) 0.3600(8) 0.3816(7) 0.062(2) Uani 1 d . . . C53 C 0.7543(11) 0.4185(10) 0.3583(9) 0.081(3) Uani 1 d . . . H53 H 0.8454 0.3911 0.3590 0.098 Uiso 1 calc R . . C54 C 0.7200(12) 0.5172(10) 0.3346(9) 0.085(3) Uani 1 d . . . H54 H 0.7885 0.5581 0.3169 0.102 Uiso 1 calc R . . C55 C 0.5845(13) 0.5560(9) 0.3369(9) 0.084(3) Uani 1 d . . . H55 H 0.5605 0.6230 0.3199 0.100 Uiso 1 calc R . . C56 C 0.4836(10) 0.4929(7) 0.3650(7) 0.062(2) Uani 1 d . . . N41 N 0.2525(8) 0.4701(6) 0.3605(6) 0.0654(19) Uani 1 d . . . C42 C 0.1190(10) 0.4998(8) 0.3668(9) 0.079(3) Uani 1 d . . . H42 H 0.0618 0.4582 0.3635 0.095 Uiso 1 calc R . . C43 C 0.0589(12) 0.5870(9) 0.3779(10) 0.088(3) Uani 1 d . . . H43 H -0.0349 0.6053 0.3784 0.105 Uiso 1 calc R . . C44 C 0.1404(14) 0.6456(9) 0.3880(11) 0.095(4) Uani 1 d . . . H44 H 0.1030 0.7039 0.3990 0.114 Uiso 1 calc R . . C45 C 0.2795(12) 0.6175(8) 0.3816(9) 0.078(3) Uani 1 d . . . H45 H 0.3368 0.6582 0.3866 0.094 Uiso 1 calc R . . C46 C 0.3357(10) 0.5298(7) 0.3679(7) 0.060(2) Uani 1 d . . . N61 N 0.5881(8) 0.2099(6) 0.3801(6) 0.0604(17) Uani 1 d . . . C62 C 0.6778(9) 0.2527(7) 0.4034(6) 0.058(2) Uani 1 d . . . C63 C 0.6115(13) 0.1116(8) 0.4010(8) 0.076(3) Uani 1 d . . . H63 H 0.5505 0.0803 0.3860 0.091 Uiso 1 calc R . . C64 C 0.7197(13) 0.0575(9) 0.4425(8) 0.089(4) Uani 1 d . . . H64 H 0.7315 -0.0095 0.4545 0.107 Uiso 1 calc R . . C65 C 0.8114(11) 0.0981(10) 0.4672(8) 0.088(4) Uani 1 d . . . H65 H 0.8859 0.0606 0.4959 0.105 Uiso 1 calc R . . C66 C 0.7895(10) 0.1987(10) 0.4477(8) 0.076(3) Uani 1 d . . . H66 H 0.8492 0.2298 0.4642 0.092 Uiso 1 calc R . . N200 N 0.1897(16) 0.2437(11) -0.2127(11) 0.123(4) Uiso 1 d . . . C201 C 0.2007(13) 0.1841(9) -0.1383(9) 0.084(3) Uiso 1 d . . . C202 C 0.1952(19) 0.1098(13) -0.0463(12) 0.124(5) Uiso 1 d . . . H20A H 0.1011 0.1009 -0.0185 0.149 Uiso 1 calc R . . H20B H 0.2377 0.1285 -0.0044 0.149 Uiso 1 calc R . . H20C H 0.2431 0.0498 -0.0539 0.149 Uiso 1 calc R . . N100 N 0.826(2) 0.1423(14) -0.0558(13) 0.144(6) Uiso 1 d . . . C101 C 0.7281(19) 0.1448(12) -0.0845(12) 0.109(4) Uiso 1 d . . . C102 C 0.5980(19) 0.1425(14) -0.1076(14) 0.126(5) Uiso 1 d . . . H10A H 0.5310 0.1877 -0.0844 0.151 Uiso 1 calc R . . H10B H 0.5712 0.0780 -0.0774 0.151 Uiso 1 calc R . . H10C H 0.6042 0.1604 -0.1765 0.151 Uiso 1 calc R . . C302 C 0.3517(18) 0.2144(13) 0.5788(12) 0.120(5) Uiso 1 d . . . H30A H 0.2956 0.2639 0.6021 0.144 Uiso 1 calc R . . H30B H 0.3000 0.1608 0.5924 0.144 Uiso 1 calc R . . H30C H 0.3800 0.2410 0.5102 0.144 Uiso 1 calc R . . C301 C 0.4697(15) 0.1809(10) 0.6257(10) 0.092(3) Uiso 1 d . . . N300 N 0.5641(17) 0.1626(12) 0.6617(11) 0.125(4) Uiso 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 0.0449(3) 0.0471(3) 0.0649(3) -0.01955(17) -0.01342(19) -0.00801(15) O100 0.056(3) 0.062(3) 0.080(4) -0.040(3) -0.003(3) -0.014(3) O41 0.071(5) 0.120(7) 0.084(5) -0.050(5) -0.021(4) -0.015(4) O42 0.046(3) 0.068(4) 0.073(4) -0.022(3) -0.004(3) -0.011(3) N43 0.051(4) 0.076(5) 0.082(6) -0.033(4) -0.006(4) 0.000(4) O44 0.081(5) 0.148(9) 0.057(4) -0.021(5) 0.008(4) 0.002(5) N63 0.062(4) 0.064(4) 0.078(5) -0.031(4) -0.008(4) -0.007(4) O64 0.080(6) 0.114(7) 0.174(10) -0.077(7) 0.000(6) 0.029(5) O61 0.108(6) 0.076(5) 0.087(5) -0.045(4) -0.031(5) 0.025(4) O62 0.104(7) 0.126(8) 0.095(5) -0.022(5) -0.036(5) -0.047(6) O52 0.050(3) 0.064(4) 0.069(3) -0.022(3) -0.007(3) -0.007(3) O54 0.062(4) 0.131(8) 0.062(4) -0.027(4) 0.004(4) -0.017(4) N53 0.050(4) 0.065(5) 0.075(5) -0.021(4) -0.004(4) -0.021(4) O51 0.098(5) 0.046(3) 0.076(4) -0.024(3) -0.008(4) -0.004(3) C12 0.074(7) 0.098(8) 0.087(7) -0.034(6) -0.023(6) -0.037(6) C16 0.064(5) 0.069(5) 0.055(4) -0.021(4) -0.002(4) -0.033(4) C13 0.066(6) 0.054(5) 0.076(6) -0.013(4) -0.020(5) -0.002(4) C15 0.104(10) 0.062(7) 0.133(11) -0.029(7) -0.012(9) -0.040(6) C14 0.088(7) 0.052(5) 0.096(7) -0.018(5) -0.014(6) -0.020(5) N11 0.055(4) 0.052(4) 0.065(4) -0.023(3) -0.008(3) -0.015(3) N21 0.040(3) 0.073(4) 0.047(3) -0.023(3) -0.003(3) -0.012(3) C22 0.049(4) 0.086(6) 0.052(4) -0.024(4) 0.001(4) -0.028(4) C23 0.059(5) 0.094(8) 0.069(6) -0.024(5) 0.007(5) -0.034(5) C24 0.047(5) 0.123(10) 0.073(6) -0.032(6) -0.015(5) -0.017(6) C25 0.037(4) 0.082(6) 0.087(6) -0.002(5) -0.041(5) 0.020(4) C26 0.046(4) 0.067(5) 0.060(5) -0.016(4) 0.001(4) -0.013(4) C32 0.047(4) 0.062(5) 0.049(4) -0.019(3) -0.018(4) 0.000(3) N31 0.043(3) 0.050(3) 0.057(3) -0.014(3) -0.017(3) -0.004(3) C33 0.076(6) 0.050(5) 0.087(6) -0.016(4) -0.009(6) -0.006(4) C34 0.073(6) 0.055(5) 0.089(7) -0.022(5) 0.006(5) -0.026(4) C35 0.051(5) 0.060(5) 0.070(5) -0.024(4) -0.007(4) -0.009(4) C36 0.055(5) 0.056(5) 0.096(7) -0.022(5) -0.012(5) 0.004(4) N51 0.053(4) 0.070(5) 0.055(4) -0.026(3) 0.001(3) -0.023(3) C52 0.050(4) 0.079(6) 0.067(5) -0.032(4) 0.000(4) -0.024(4) C53 0.058(6) 0.099(8) 0.093(7) -0.040(6) 0.015(5) -0.038(6) C54 0.073(7) 0.100(8) 0.095(7) -0.029(6) -0.016(6) -0.046(6) C55 0.090(8) 0.069(6) 0.095(7) -0.020(6) -0.005(6) -0.042(6) C56 0.068(6) 0.063(5) 0.064(5) -0.027(4) -0.002(4) -0.027(4) N41 0.058(4) 0.061(4) 0.086(5) -0.033(4) -0.012(4) -0.011(3) C42 0.058(5) 0.075(6) 0.120(9) -0.054(6) -0.016(6) 0.000(5) C43 0.062(6) 0.096(8) 0.122(10) -0.061(8) -0.022(7) 0.009(6) C44 0.095(8) 0.071(7) 0.128(10) -0.054(7) -0.011(8) 0.002(6) C45 0.084(7) 0.059(5) 0.104(8) -0.041(6) -0.008(6) -0.017(5) C46 0.064(5) 0.057(5) 0.067(5) -0.028(4) -0.012(4) -0.013(4) N61 0.055(4) 0.061(4) 0.065(4) -0.017(3) -0.012(4) -0.010(3) C62 0.048(4) 0.068(5) 0.059(4) -0.022(4) -0.008(4) -0.006(4) C63 0.091(8) 0.067(6) 0.074(6) -0.022(5) -0.027(6) -0.007(5) C64 0.084(8) 0.091(8) 0.082(6) -0.011(5) -0.060(7) 0.037(6) C65 0.057(6) 0.117(9) 0.075(6) -0.020(6) -0.044(6) 0.044(6) C66 0.042(4) 0.109(9) 0.082(6) -0.038(6) -0.017(5) 0.003(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 Er1 O100 2.326(6) . ? Er1 O61 2.414(8) . ? Er1 O52 2.435(6) . ? Er1 O41 2.451(8) . ? Er1 O42 2.460(7) . ? Er1 N11 2.478(7) . ? Er1 N31 2.489(7) . ? Er1 N21 2.505(7) . ? Er1 O51 2.523(7) . ? Er1 O62 2.858(12) . ? O41 N43 1.242(12) . ? O42 N43 1.247(11) . ? N43 O44 1.213(12) . ? N63 O64 1.187(12) . ? N63 O62 1.242(11) . ? N63 O61 1.259(11) . ? O52 N53 1.284(11) . ? O54 N53 1.205(11) . ? N53 O51 1.268(11) . ? C12 C15 1.353(19) . ? C12 C16 1.406(13) . ? C16 N11 1.361(12) . ? C16 C22 1.492(15) . ? C13 N11 1.354(11) . ? C13 C14 1.375(14) . ? C15 C14 1.351(19) . ? N21 C22 1.343(11) . ? N21 C26 1.372(12) . ? C22 C23 1.373(15) . ? C23 C24 1.388(18) . ? C24 C25 1.381(17) . ? C25 C26 1.405(12) . ? C26 C32 1.475(13) . ? C32 N31 1.353(10) . ? C32 C36 1.412(12) . ? N31 C35 1.361(11) . ? C33 C34 1.379(16) . ? C33 C36 1.411(15) . ? C34 C35 1.381(14) . ? N51 C56 1.338(13) . ? N51 C52 1.338(12) . ? C52 C53 1.404(13) . ? C52 C62 1.486(14) . ? C53 C54 1.368(18) . ? C54 C55 1.375(18) . ? C55 C56 1.396(14) . ? C56 C46 1.483(14) . ? N41 C42 1.326(13) . ? N41 C46 1.359(12) . ? C42 C43 1.369(15) . ? C43 C44 1.352(18) . ? C44 C45 1.375(18) . ? C45 C46 1.382(14) . ? N61 C62 1.345(12) . ? N61 C63 1.359(13) . ? C62 C66 1.394(14) . ? C63 C64 1.348(15) . ? C64 C65 1.35(2) . ? C65 C66 1.393(19) . ? N200 C201 1.163(17) . ? C201 C202 1.423(19) . ? N100 C101 1.14(2) . ? C101 C102 1.42(2) . ? C302 C301 1.42(2) . ? C301 N300 1.128(18) . ? 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 O61 74.4(3) . . ? O100 Er1 O52 74.0(2) . . ? O61 Er1 O52 119.0(2) . . ? O100 Er1 O41 124.9(3) . . ? O61 Er1 O41 103.7(3) . . ? O52 Er1 O41 137.0(3) . . ? O100 Er1 O42 78.1(2) . . ? O61 Er1 O42 73.4(3) . . ? O52 Er1 O42 144.0(2) . . ? O41 Er1 O42 50.6(3) . . ? O100 Er1 N11 142.4(2) . . ? O61 Er1 N11 89.5(3) . . ? O52 Er1 N11 85.3(2) . . ? O41 Er1 N11 91.6(3) . . ? O42 Er1 N11 130.2(2) . . ? O100 Er1 N31 76.5(2) . . ? O61 Er1 N31 140.3(3) . . ? O52 Er1 N31 77.1(2) . . ? O41 Er1 N31 72.2(3) . . ? O42 Er1 N31 74.6(2) . . ? N11 Er1 N31 129.5(2) . . ? O100 Er1 N21 131.5(2) . . ? O61 Er1 N21 152.4(3) . . ? O52 Er1 N21 69.5(2) . . ? O41 Er1 N21 70.7(2) . . ? O42 Er1 N21 116.4(2) . . ? N11 Er1 N21 64.2(2) . . ? N31 Er1 N21 65.3(2) . . ? O100 Er1 O51 71.3(3) . . ? O61 Er1 O51 69.3(3) . . ? O52 Er1 O51 51.5(2) . . ? O41 Er1 O51 161.1(3) . . ? O42 Er1 O51 136.6(3) . . ? N11 Er1 O51 71.2(2) . . ? N31 Er1 O51 124.6(2) . . ? N21 Er1 O51 106.9(2) . . ? O100 Er1 O62 116.4(2) . . ? O61 Er1 O62 46.3(3) . . ? O52 Er1 O62 147.7(2) . . ? O41 Er1 O62 64.4(3) . . ? O42 Er1 O62 66.4(3) . . ? N11 Er1 O62 68.2(3) . . ? N31 Er1 O62 133.9(3) . . ? N21 Er1 O62 111.5(2) . . ? O51 Er1 O62 100.8(2) . . ? N43 O41 Er1 97.4(6) . . ? N43 O42 Er1 96.8(5) . . ? O44 N43 O41 120.7(10) . . ? O44 N43 O42 124.1(9) . . ? O41 N43 O42 115.1(9) . . ? O62 N63 O64 125.9(11) . . ? O64 N63 O61 119.0(10) . . ? O62 N63 O61 115.1(9) . . ? N63 O61 Er1 109.7(6) . . ? N63 O62 Er1 88.0(7) . . ? N53 O52 Er1 98.3(5) . . ? O54 N53 O51 123.1(9) . . ? O54 N53 O52 121.5(9) . . ? O51 N53 O52 115.4(8) . . ? O54 N53 Er1 176.3(7) . . ? O51 N53 Er1 59.7(5) . . ? O52 N53 Er1 55.8(4) . . ? N53 O51 Er1 94.6(6) . . ? C15 C12 C16 120.5(11) . . ? N11 C16 C12 120.0(10) . . ? N11 C16 C22 115.5(7) . . ? C12 C16 C22 124.5(10) . . ? N11 C13 C14 122.8(10) . . ? C12 C15 C14 119.4(10) . . ? C15 C14 C13 119.5(10) . . ? C13 N11 C16 117.6(8) . . ? C13 N11 Er1 120.1(6) . . ? C16 N11 Er1 122.2(6) . . ? C22 N21 C26 117.2(8) . . ? C22 N21 Er1 122.4(6) . . ? C26 N21 Er1 120.4(6) . . ? N21 C22 C23 124.3(10) . . ? N21 C22 C16 115.0(8) . . ? C23 C22 C16 120.5(9) . . ? C22 C23 C24 118.1(10) . . ? C25 C24 C23 120.0(10) . . ? C24 C25 C26 118.5(10) . . ? N21 C26 C25 121.7(9) . . ? N21 C26 C32 115.8(8) . . ? C25 C26 C32 122.3(9) . . ? N31 C32 C36 121.3(8) . . ? N31 C32 C26 117.1(8) . . ? C36 C32 C26 121.5(8) . . ? C35 N31 C32 118.4(7) . . ? C35 N31 Er1 120.7(6) . . ? C32 N31 Er1 120.7(5) . . ? C34 C33 C36 119.2(9) . . ? C33 C34 C35 118.8(9) . . ? N31 C35 C34 123.3(9) . . ? C33 C36 C32 118.7(9) . . ? C56 N51 C52 118.4(8) . . ? N51 C52 C53 122.8(10) . . ? N51 C52 C62 116.5(8) . . ? C53 C52 C62 120.8(9) . . ? C54 C53 C52 117.8(11) . . ? C55 C54 C53 120.2(10) . . ? C54 C55 C56 118.8(11) . . ? N51 C56 C55 122.0(10) . . ? N51 C56 C46 116.3(8) . . ? C55 C56 C46 121.6(10) . . ? C42 N41 C46 117.4(8) . . ? N41 C42 C43 125.0(10) . . ? C42 C43 C44 117.9(11) . . ? C43 C44 C45 118.8(11) . . ? C44 C45 C46 121.1(10) . . ? N41 C46 C45 119.7(9) . . ? N41 C46 C56 116.3(8) . . ? C45 C46 C56 123.9(9) . . ? C62 N61 C63 117.1(8) . . ? N61 C62 C66 121.6(10) . . ? N61 C62 C52 115.8(8) . . ? C66 C62 C52 122.6(9) . . ? C64 C63 N61 122.7(11) . . ? C65 C64 C63 121.8(12) . . ? C64 C65 C66 117.0(9) . . ? C62 C66 C65 119.8(11) . . ? N200 C201 C202 172.2(16) . . ? N100 C101 C102 173(2) . . ? N300 C301 C302 174.1(18) . . ? _refine_diff_density_max 1.924 _refine_diff_density_min -2.492 _refine_diff_density_rms 0.142 _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-Tm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 N11 O10 Tm ' _chemical_formula_weight 919.60 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' 'Tm' 'Tm' -0.3139 5.2483 '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 10.263(13) _cell_length_b 14.487(17) _cell_length_c 14.816(17) _cell_angle_alpha 64.871(10) _cell_angle_beta 73.936(10) _cell_angle_gamma 78.876(10) _cell_volume 1909(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(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 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 5396 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1988 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.05 _reflns_number_total 5396 _reflns_number_gt 2039 _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^)+(0.1494P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5396 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2745 _refine_ls_R_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.2859 _refine_ls_wR_factor_gt 0.2208 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.021 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 0.25930(11) 0.28038(9) 0.19949(9) 0.0917(6) Uani 1 d . . . O100 O 0.3758(13) 0.3372(9) 0.2770(10) 0.083(4) Uani 1 d . . . O41 O 0.2784(16) 0.3110(11) 0.0236(11) 0.094(4) Uani 1 d . . . O42 O 0.4387(13) 0.3633(10) 0.0529(11) 0.083(4) Uani 1 d . . . N43 N 0.3879(18) 0.3574(15) -0.011(2) 0.105(8) Uani 1 d . . . O44 O 0.4417(18) 0.3805(16) -0.0996(15) 0.121(7) Uani 1 d . . . N63 N 0.537(2) 0.1328(15) 0.1491(19) 0.099(6) Uani 1 d . . . O62 O 0.6464(19) 0.0889(17) 0.1711(19) 0.164(9) Uani 1 d . . . O61 O 0.4506(18) 0.1652(12) 0.2138(13) 0.111(5) Uani 1 d . . . O64 O 0.504(2) 0.1414(18) 0.0731(19) 0.175(10) Uani 1 d . . . O52 O 0.0824(14) 0.2914(13) 0.3476(12) 0.091(4) Uani 1 d . . . O54 O 0.0746(14) 0.1767(13) 0.5059(14) 0.106(5) Uani 1 d . . . N53 N 0.136(2) 0.207(2) 0.4095(17) 0.099(7) Uani 1 d . . . O51 O 0.2301(12) 0.1633(9) 0.3824(10) 0.054(3) Uani 1 d . . . C12 C -0.034(3) 0.066(2) 0.192(2) 0.123(10) Uani 1 d . . . H12 H -0.1181 0.0784 0.1755 0.148 Uiso 1 calc R . . C16 C 0.027(2) 0.1440(18) 0.1924(16) 0.092(7) Uani 1 d . . . C13 C 0.219(2) 0.0386(19) 0.2494(19) 0.103(7) Uani 1 d . . . H13 H 0.2963 0.0275 0.2750 0.123 Uiso 1 calc R . . C15 C 0.035(3) -0.029(3) 0.218(3) 0.142(11) Uani 1 d . . . H15 H -0.0050 -0.0835 0.2220 0.171 Uiso 1 calc R . . C14 C 0.165(3) -0.046(2) 0.2398(18) 0.119(8) Uani 1 d . . . H14 H 0.2168 -0.1081 0.2478 0.143 Uiso 1 calc R . . N11 N 0.1462(18) 0.1339(15) 0.2176(13) 0.093(5) Uani 1 d . . . N21 N 0.0287(17) 0.3217(14) 0.1657(11) 0.081(5) Uani 1 d . . . C22 C -0.0508(19) 0.2481(18) 0.1755(14) 0.085(7) Uani 1 d . . . C23 C -0.177(2) 0.2729(18) 0.1591(15) 0.091(7) Uani 1 d . . . H23 H -0.2225 0.2230 0.1597 0.109 Uiso 1 calc R . . C24 C -0.242(2) 0.370(2) 0.1411(18) 0.099(8) Uani 1 d . . . H24 H -0.3330 0.3827 0.1372 0.119 Uiso 1 calc R . . C25 C -0.171(2) 0.4458(19) 0.1293(16) 0.088(7) Uani 1 d . . . H25 H -0.2082 0.5134 0.1105 0.106 Uiso 1 calc R . . C26 C -0.039(3) 0.4172(18) 0.1468(15) 0.090(6) Uani 1 d . . . C32 C 0.0527(17) 0.498(2) 0.1281(15) 0.081(7) Uani 1 d . . . N31 N 0.185(2) 0.4656(12) 0.1377(13) 0.091(6) Uani 1 d . . . C33 C 0.091(4) 0.667(2) 0.0987(18) 0.121(9) Uani 1 d . . . H33 H 0.0577 0.7330 0.0922 0.145 Uiso 1 calc R . . C34 C 0.227(2) 0.6356(19) 0.0970(16) 0.093(7) Uani 1 d . . . H34 H 0.2911 0.6815 0.0796 0.112 Uiso 1 calc R . . C35 C 0.262(3) 0.535(2) 0.122(2) 0.106(8) Uani 1 d . . . H35 H 0.3515 0.5120 0.1291 0.127 Uiso 1 calc R . . C36 C 0.004(2) 0.596(2) 0.1105(16) 0.089(7) Uani 1 d . . . H36 H -0.0862 0.6170 0.1062 0.106 Uiso 1 calc R . . N51 N 0.505(2) 0.4088(14) 0.3849(13) 0.085(5) Uani 1 d . . . C52 C 0.635(2) 0.376(2) 0.3859(16) 0.097(7) Uani 1 d . . . C53 C 0.734(2) 0.443(2) 0.365(2) 0.113(8) Uani 1 d . . . H53 H 0.8239 0.4164 0.3654 0.135 Uiso 1 calc R . . C54 C 0.701(3) 0.542(2) 0.345(2) 0.134(10) Uani 1 d . . . H54 H 0.7649 0.5856 0.3337 0.161 Uiso 1 calc R . . C55 C 0.564(2) 0.5763(19) 0.3437(19) 0.107(8) Uani 1 d . . . H55 H 0.5361 0.6454 0.3276 0.128 Uiso 1 calc R . . C56 C 0.466(3) 0.508(2) 0.3657(15) 0.098(7) Uani 1 d . . . N41 N 0.244(2) 0.4830(15) 0.3610(16) 0.112(7) Uani 1 d . . . C42 C 0.110(2) 0.512(2) 0.3649(19) 0.106(8) Uani 1 d . . . H42 H 0.0553 0.4697 0.3619 0.127 Uiso 1 calc R . . C43 C 0.050(2) 0.605(2) 0.3736(19) 0.112(8) Uani 1 d . . . H43 H -0.0422 0.6248 0.3769 0.135 Uiso 1 calc R . . C44 C 0.134(3) 0.6653(19) 0.377(2) 0.124(9) Uani 1 d . . . H44 H 0.0954 0.7271 0.3815 0.149 Uiso 1 calc R . . C45 C 0.264(2) 0.644(2) 0.3741(17) 0.104(8) Uani 1 d . . . H45 H 0.3173 0.6871 0.3777 0.125 Uiso 1 calc R . . C46 C 0.319(2) 0.5462(18) 0.3646(16) 0.084(6) Uani 1 d . . . N61 N 0.5827(18) 0.2228(16) 0.3784(14) 0.096(5) Uani 1 d . . . C62 C 0.6650(19) 0.263(2) 0.4078(16) 0.085(6) Uani 1 d . . . C63 C 0.610(3) 0.1233(19) 0.396(2) 0.133(11) Uani 1 d . . . H63 H 0.5574 0.0929 0.3760 0.159 Uiso 1 calc R . . C64 C 0.711(3) 0.066(2) 0.443(2) 0.126(10) Uani 1 d . . . H64 H 0.7191 -0.0044 0.4597 0.152 Uiso 1 calc R . . C65 C 0.803(2) 0.106(2) 0.466(2) 0.111(8) Uani 1 d . . . H65 H 0.8781 0.0666 0.4907 0.133 Uiso 1 calc R . . C66 C 0.777(2) 0.2091(19) 0.4499(16) 0.095(7) Uani 1 d . . . H66 H 0.8313 0.2410 0.4666 0.114 Uiso 1 calc R . . N200 N 0.153(4) 0.188(3) -0.179(3) 0.230(15) Uiso 1 d . . . C201 C 0.221(5) 0.148(4) -0.128(4) 0.214(18) Uiso 1 d . . . C202 C 0.336(4) 0.101(3) -0.067(3) 0.212(17) Uiso 1 d . . . H20A H 0.4228 0.1119 -0.1136 0.255 Uiso 1 calc R . . H20B H 0.3278 0.0293 -0.0287 0.255 Uiso 1 calc R . . H20C H 0.3268 0.1341 -0.0211 0.255 Uiso 1 calc R . . C302 C 0.321(3) 0.194(3) 0.598(3) 0.181(13) Uiso 1 d . . . H30A H 0.3017 0.1347 0.5917 0.217 Uiso 1 calc R . . H30B H 0.3336 0.2496 0.5322 0.217 Uiso 1 calc R . . H30C H 0.2453 0.2127 0.6441 0.217 Uiso 1 calc R . . C301 C 0.439(4) 0.171(3) 0.636(3) 0.155(11) Uiso 1 d . . . N300 N 0.527(3) 0.151(2) 0.679(2) 0.186(11) Uiso 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 0.0902(8) 0.0911(9) 0.0959(9) -0.0381(6) -0.0225(5) -0.0065(5) O100 0.114(10) 0.055(9) 0.087(10) -0.039(8) -0.018(8) -0.006(7) O41 0.099(11) 0.081(11) 0.100(11) -0.035(9) -0.013(9) -0.018(8) O42 0.060(9) 0.071(10) 0.102(11) -0.018(8) -0.013(8) -0.015(6) N43 0.042(13) 0.102(17) 0.18(3) -0.045(18) -0.060(15) 0.008(10) O44 0.100(13) 0.152(18) 0.092(13) -0.038(13) 0.004(11) -0.026(11) N63 0.102(16) 0.086(15) 0.126(19) -0.069(14) -0.012(14) 0.000(11) O62 0.104(14) 0.18(2) 0.26(3) -0.129(19) -0.067(16) 0.018(13) O61 0.140(13) 0.093(12) 0.111(13) -0.046(10) -0.064(11) 0.034(10) O64 0.21(2) 0.19(2) 0.18(2) -0.133(19) -0.106(18) 0.081(17) O52 0.097(11) 0.085(12) 0.071(10) -0.024(9) 0.000(8) -0.007(9) O54 0.076(10) 0.145(15) 0.087(13) -0.043(12) -0.022(9) 0.016(9) N53 0.091(16) 0.13(2) 0.067(17) -0.019(16) 0.011(15) -0.074(17) O51 0.044(7) 0.049(8) 0.059(9) -0.017(7) -0.009(6) 0.006(6) C12 0.15(2) 0.10(2) 0.19(3) -0.09(2) -0.10(2) 0.007(19) C16 0.084(15) 0.093(19) 0.073(15) -0.016(13) -0.019(12) 0.014(14) C13 0.114(17) 0.070(18) 0.111(19) -0.043(16) 0.021(15) -0.027(15) C15 0.13(2) 0.12(3) 0.20(3) -0.07(2) -0.06(2) -0.02(2) C14 0.16(3) 0.11(2) 0.087(18) -0.041(16) -0.020(17) -0.014(18) N11 0.095(14) 0.106(17) 0.089(14) -0.043(12) -0.032(10) -0.001(11) N21 0.086(12) 0.072(14) 0.062(11) -0.017(9) -0.002(9) -0.001(10) C22 0.051(13) 0.12(2) 0.066(14) 0.001(12) -0.028(10) -0.024(12) C23 0.102(17) 0.10(2) 0.079(16) -0.049(14) -0.026(13) 0.010(14) C24 0.051(13) 0.10(2) 0.11(2) -0.026(16) -0.005(13) 0.010(14) C25 0.053(13) 0.10(2) 0.080(16) -0.024(14) 0.018(11) -0.003(12) C26 0.13(2) 0.065(17) 0.060(14) -0.012(12) -0.004(13) -0.021(16) C32 0.026(10) 0.12(2) 0.080(15) -0.023(13) -0.022(9) 0.016(11) N31 0.139(17) 0.040(11) 0.085(13) -0.029(10) -0.006(11) -0.003(11) C33 0.17(3) 0.12(2) 0.081(17) -0.055(17) -0.027(18) 0.00(2) C34 0.076(16) 0.08(2) 0.102(18) 0.000(14) -0.038(13) -0.012(12) C35 0.113(18) 0.07(2) 0.14(2) -0.024(17) -0.057(16) 0.002(16) C36 0.048(11) 0.12(2) 0.092(17) -0.040(15) -0.013(11) 0.007(13) N51 0.115(16) 0.047(12) 0.081(13) -0.017(10) -0.009(10) -0.020(10) C52 0.061(15) 0.13(3) 0.084(16) -0.025(15) -0.014(12) -0.022(15) C53 0.093(17) 0.10(2) 0.13(2) -0.054(19) 0.008(15) -0.016(16) C54 0.13(2) 0.11(3) 0.16(3) -0.05(2) 0.005(19) -0.037(19) C55 0.075(15) 0.090(19) 0.14(2) -0.048(16) 0.006(14) -0.026(13) C56 0.13(2) 0.11(2) 0.040(13) -0.029(14) 0.018(12) -0.048(18) N41 0.136(19) 0.097(16) 0.136(18) -0.061(14) -0.048(14) -0.020(14) C42 0.075(15) 0.12(2) 0.14(2) -0.074(18) -0.021(14) 0.006(14) C43 0.079(15) 0.12(2) 0.13(2) -0.038(18) -0.045(15) 0.009(15) C44 0.14(2) 0.10(2) 0.18(3) -0.10(2) -0.05(2) 0.024(17) C45 0.071(15) 0.12(2) 0.11(2) -0.032(16) -0.019(13) -0.014(14) C46 0.068(13) 0.087(18) 0.095(17) -0.035(14) -0.031(11) 0.021(12) N61 0.094(13) 0.105(17) 0.108(15) -0.057(13) -0.022(11) -0.010(11) C62 0.064(13) 0.11(2) 0.096(17) -0.062(16) -0.017(12) -0.002(13) C63 0.17(3) 0.045(17) 0.12(2) -0.027(15) 0.03(2) 0.023(16) C64 0.10(2) 0.11(2) 0.13(2) -0.012(18) -0.047(17) 0.024(18) C65 0.070(15) 0.11(2) 0.14(2) -0.044(18) -0.035(15) 0.020(14) C66 0.085(15) 0.10(2) 0.080(16) -0.037(14) -0.010(12) 0.028(13) _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 O61 2.313(16) . ? Tm1 O100 2.317(12) . ? Tm1 O41 2.407(14) . ? Tm1 O42 2.444(13) . ? Tm1 N21 2.463(17) . ? Tm1 O52 2.473(14) . ? Tm1 N31 2.475(16) . ? Tm1 O51 2.480(12) . ? Tm1 N11 2.494(19) . ? O41 N43 1.29(2) . ? O42 N43 1.24(2) . ? N43 O44 1.20(3) . ? N63 O64 1.21(2) . ? N63 O62 1.24(2) . ? N63 O61 1.29(2) . ? O52 N53 1.30(3) . ? O54 N53 1.31(2) . ? N53 O51 1.13(2) . ? C12 C15 1.37(3) . ? C12 C16 1.39(3) . ? C16 N11 1.34(3) . ? C16 C22 1.51(3) . ? C13 N11 1.39(3) . ? C13 C14 1.51(3) . ? C15 C14 1.41(3) . ? N21 C26 1.37(3) . ? N21 C22 1.40(2) . ? C22 C23 1.34(3) . ? C23 C24 1.38(3) . ? C24 C25 1.36(3) . ? C25 C26 1.40(3) . ? C26 C32 1.53(3) . ? C32 C36 1.35(3) . ? C32 N31 1.38(2) . ? N31 C35 1.30(3) . ? C33 C34 1.38(3) . ? C33 C36 1.41(3) . ? C34 C35 1.35(3) . ? N51 C52 1.33(2) . ? N51 C56 1.35(3) . ? C52 C53 1.41(3) . ? C52 C62 1.52(3) . ? C53 C54 1.33(3) . ? C54 C55 1.40(3) . ? C55 C56 1.41(3) . ? C56 C46 1.51(3) . ? N41 C46 1.33(3) . ? N41 C42 1.35(3) . ? C42 C43 1.41(3) . ? C43 C44 1.36(3) . ? C44 C45 1.30(3) . ? C45 C46 1.47(3) . ? N61 C63 1.34(3) . ? N61 C62 1.36(2) . ? C62 C66 1.40(3) . ? C63 C64 1.35(3) . ? C64 C65 1.39(3) . ? C65 C66 1.39(3) . ? N200 C201 1.08(5) . ? C201 C202 1.56(5) . ? C302 C301 1.40(4) . ? C301 N300 1.17(4) . ? 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 Tm1 O100 78.2(5) . . ? O61 Tm1 O41 93.3(6) . . ? O100 Tm1 O41 132.3(5) . . ? O61 Tm1 O42 73.7(6) . . ? O100 Tm1 O42 80.3(5) . . ? O41 Tm1 O42 52.6(5) . . ? O61 Tm1 N21 146.8(6) . . ? O100 Tm1 N21 133.8(5) . . ? O41 Tm1 N21 71.8(5) . . ? O42 Tm1 N21 114.8(5) . . ? O61 Tm1 O52 123.7(6) . . ? O100 Tm1 O52 77.7(5) . . ? O41 Tm1 O52 138.9(5) . . ? O42 Tm1 O52 147.5(5) . . ? N21 Tm1 O52 67.3(5) . . ? O61 Tm1 N31 142.7(7) . . ? O100 Tm1 N31 78.0(6) . . ? O41 Tm1 N31 82.1(5) . . ? O42 Tm1 N31 74.3(5) . . ? N21 Tm1 N31 66.3(7) . . ? O52 Tm1 N31 78.0(6) . . ? O61 Tm1 O51 73.3(5) . . ? O100 Tm1 O51 71.3(4) . . ? O41 Tm1 O51 150.8(4) . . ? O42 Tm1 O51 139.9(4) . . ? N21 Tm1 O51 105.3(4) . . ? O52 Tm1 O51 51.0(5) . . ? N31 Tm1 O51 124.3(5) . . ? O61 Tm1 N11 84.2(6) . . ? O100 Tm1 N11 144.8(5) . . ? O41 Tm1 N11 78.4(5) . . ? O42 Tm1 N11 123.5(5) . . ? N21 Tm1 N11 64.1(6) . . ? O52 Tm1 N11 87.5(5) . . ? N31 Tm1 N11 130.2(7) . . ? O51 Tm1 N11 74.5(5) . . ? N43 O41 Tm1 95.4(15) . . ? N43 O42 Tm1 95.0(15) . . ? O44 N43 O42 124(2) . . ? O44 N43 O41 118(2) . . ? O42 N43 O41 117(3) . . ? O64 N63 O62 123(2) . . ? O64 N63 O61 119(2) . . ? O62 N63 O61 118(2) . . ? N63 O61 Tm1 132.5(15) . . ? N53 O52 Tm1 91.2(13) . . ? O51 N53 O52 122(2) . . ? O51 N53 O54 121(2) . . ? O52 N53 O54 116(2) . . ? N53 O51 Tm1 95.4(14) . . ? C15 C12 C16 118(2) . . ? N11 C16 C12 126(2) . . ? N11 C16 C22 114(2) . . ? C12 C16 C22 120(2) . . ? N11 C13 C14 116(2) . . ? C12 C15 C14 121(3) . . ? C15 C14 C13 119(3) . . ? C16 N11 C13 120(2) . . ? C16 N11 Tm1 123.8(17) . . ? C13 N11 Tm1 115.9(15) . . ? C26 N21 C22 114.0(19) . . ? C26 N21 Tm1 122.3(16) . . ? C22 N21 Tm1 123.3(13) . . ? C23 C22 N21 122(2) . . ? C23 C22 C16 125(2) . . ? N21 C22 C16 113.3(18) . . ? C22 C23 C24 123(2) . . ? C25 C24 C23 119(2) . . ? C24 C25 C26 117(2) . . ? N21 C26 C25 126(2) . . ? N21 C26 C32 113(2) . . ? C25 C26 C32 120(2) . . ? C36 C32 N31 121(2) . . ? C36 C32 C26 121.9(18) . . ? N31 C32 C26 117(2) . . ? C35 N31 C32 116.9(19) . . ? C35 N31 Tm1 123.2(17) . . ? C32 N31 Tm1 119.6(16) . . ? C34 C33 C36 119(2) . . ? C35 C34 C33 116(2) . . ? N31 C35 C34 127(2) . . ? C32 C36 C33 120(2) . . ? C52 N51 C56 118(2) . . ? N51 C52 C53 122(3) . . ? N51 C52 C62 113(2) . . ? C53 C52 C62 125(2) . . ? C54 C53 C52 122(3) . . ? C53 C54 C55 116(3) . . ? C54 C55 C56 122(2) . . ? N51 C56 C55 120(2) . . ? N51 C56 C46 119(2) . . ? C55 C56 C46 121(3) . . ? C46 N41 C42 117(2) . . ? N41 C42 C43 122(2) . . ? C44 C43 C42 117(2) . . ? C45 C44 C43 126(2) . . ? C44 C45 C46 114(2) . . ? N41 C46 C45 124.0(18) . . ? N41 C46 C56 116(2) . . ? C45 C46 C56 120(2) . . ? C63 N61 C62 116(2) . . ? N61 C62 C66 125(2) . . ? N61 C62 C52 115.8(18) . . ? C66 C62 C52 119(2) . . ? N61 C63 C64 122(3) . . ? C63 C64 C65 123(3) . . ? C64 C65 C66 116(2) . . ? C62 C66 C65 117(2) . . ? N200 C201 C202 171(5) . . ? N300 C301 C302 172(4) . . ? _refine_diff_density_max 0.927 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.134 _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 ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 N6 O10 Tm' _chemical_formula_weight 606.24 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' '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 8.655(10) _cell_length_b 8.833(10) _cell_length_c 25.31(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.863(10) _cell_angle_gamma 90.00 _cell_volume 1934(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(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 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 4.657 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.349 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 3494 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2111 _reflns_number_gt 1767 _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^)+(0.1281P)^2^+23.8873P] 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(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2111 _refine_ls_number_parameters 290 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1822 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.017 _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 Tm Tm 0.31431(8) 0.20412(11) 0.14336(2) 0.0400(5) Uani 1 d . . . N11 N 0.5011(15) 0.054(2) 0.1939(5) 0.044(5) Uani 1 d . . . C12 C 0.5579(18) 0.098(2) 0.2418(6) 0.041(5) Uani 1 d . . . H12 H 0.5539 0.2005 0.2508 0.049 Uiso 1 calc R . . C13 C 0.6231(19) -0.006(3) 0.2784(6) 0.049(7) Uani 1 d . . . H13 H 0.6588 0.0275 0.3112 0.058 Uiso 1 calc R . . C14 C 0.633(2) -0.157(3) 0.2650(8) 0.052(6) Uani 1 d . . . H14 H 0.6721 -0.2281 0.2889 0.062 Uiso 1 calc R . . C15 C 0.585(2) -0.198(3) 0.2160(8) 0.065(7) Uani 1 d . . . H15 H 0.5932 -0.2983 0.2054 0.078 Uiso 1 calc R . . C16 C 0.5233(17) -0.092(3) 0.1815(6) 0.048(7) Uani 1 d . . . N21 N 0.3815(16) -0.039(2) 0.1005(5) 0.051(5) Uani 1 d . . . C22 C 0.4690(19) -0.141(3) 0.1273(6) 0.049(5) Uani 1 d . . . C23 C 0.509(3) -0.271(3) 0.1042(8) 0.068(7) Uani 1 d U . . H23 H 0.5711 -0.3395 0.1227 0.082 Uiso 1 calc R . . C24 C 0.461(3) -0.305(3) 0.0557(9) 0.076(7) Uani 1 d U . . H24 H 0.4917 -0.3952 0.0401 0.091 Uiso 1 calc R . . C25 C 0.364(3) -0.204(3) 0.0275(7) 0.060(7) Uani 1 d U . . H25 H 0.3206 -0.2288 -0.0052 0.072 Uiso 1 calc R . . C26 C 0.337(2) -0.066(2) 0.0510(5) 0.039(5) Uani 1 d . . . N31 N 0.2162(18) 0.179(2) 0.0493(5) 0.057(5) Uani 1 d U . . C36 C 0.133(3) 0.285(3) 0.0245(7) 0.064(6) Uani 1 d U . . H36 H 0.1043 0.3709 0.0433 0.077 Uiso 1 calc R . . C35 C 0.090(3) 0.273(3) -0.0264(8) 0.080(8) Uani 1 d U . . H35 H 0.0371 0.3538 -0.0420 0.096 Uiso 1 calc R . . C34 C 0.117(3) 0.160(4) -0.0533(8) 0.091(8) Uani 1 d U . . H34 H 0.0829 0.1540 -0.0882 0.109 Uiso 1 calc R . . C33 C 0.202(2) 0.042(3) -0.0298(6) 0.068(6) Uani 1 d U . . H33 H 0.2298 -0.0426 -0.0497 0.081 Uiso 1 calc R . . C32 C 0.2437(19) 0.051(2) 0.0220(6) 0.045(5) Uani 1 d U . . O61 O 0.2203(15) 0.4364(16) 0.1252(4) 0.049(4) Uani 1 d . . . O62 O 0.2767(13) 0.5809(17) 0.1932(4) 0.056(4) Uani 1 d . . . O64 O 0.124(2) 0.669(2) 0.1322(5) 0.072(5) Uani 1 d . . . N63 N 0.2016(17) 0.565(2) 0.1499(5) 0.053(5) Uani 1 d . . . N53 N 0.0452(16) 0.038(2) 0.1754(5) 0.052(4) Uani 1 d U . . O51 O 0.1819(14) 0.0100(17) 0.1914(4) 0.054(4) Uani 1 d U . . O52 O 0.0416(14) 0.149(2) 0.1426(5) 0.062(4) Uani 1 d U . . O54 O -0.0702(17) -0.0226(19) 0.1904(6) 0.078(5) Uani 1 d U . . O41 O 0.5394(14) 0.375(2) 0.1616(4) 0.061(4) Uani 1 d . . . O44 O 0.7177(15) 0.4112(18) 0.1024(5) 0.066(5) Uani 1 d . . . N43 N 0.5974(15) 0.3471(19) 0.1159(5) 0.039(4) Uani 1 d . . . O42 O 0.5202(16) 0.2585(19) 0.0855(5) 0.061(4) Uani 1 d . . . O100 O 0.2704(14) 0.2903(14) 0.2281(4) 0.046(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 Tm 0.0375(5) 0.0455(13) 0.0370(4) -0.0006(3) 0.0010(3) 0.0003(4) N11 0.032(7) 0.042(17) 0.059(7) 0.010(8) 0.000(5) 0.017(8) C12 0.037(9) 0.014(17) 0.071(9) -0.009(9) -0.011(7) -0.013(9) C13 0.040(10) 0.05(2) 0.057(8) 0.028(10) -0.011(7) -0.022(11) C14 0.053(12) 0.02(2) 0.081(12) 0.012(12) -0.001(9) 0.004(12) C15 0.038(11) 0.07(2) 0.082(12) 0.007(11) -0.005(9) -0.007(11) C16 0.032(9) 0.05(2) 0.058(8) 0.006(10) 0.010(7) 0.016(10) N21 0.041(8) 0.065(15) 0.046(6) 0.003(7) 0.010(6) -0.010(8) C22 0.040(10) 0.052(18) 0.054(8) 0.009(10) 0.008(7) -0.001(10) C23 0.081(14) 0.06(2) 0.064(10) -0.014(11) 0.019(9) 0.018(13) C24 0.123(17) 0.025(19) 0.082(12) -0.020(10) 0.035(12) 0.029(13) C25 0.090(15) 0.04(2) 0.050(8) -0.005(9) 0.006(9) 0.024(12) C26 0.060(10) 0.019(17) 0.038(6) -0.003(8) 0.011(6) -0.009(9) N31 0.045(9) 0.070(16) 0.054(7) 0.005(8) -0.013(6) 0.014(9) C36 0.077(14) 0.038(18) 0.076(11) -0.025(9) -0.040(10) 0.016(12) C35 0.097(17) 0.07(2) 0.069(11) -0.008(11) -0.049(11) 0.014(14) C34 0.075(15) 0.14(2) 0.057(10) -0.011(13) -0.029(9) -0.001(15) C33 0.067(13) 0.083(18) 0.053(8) -0.024(10) -0.004(8) -0.007(12) C32 0.050(9) 0.028(15) 0.057(8) -0.024(9) 0.017(7) -0.033(9) O61 0.083(9) 0.021(12) 0.042(5) -0.014(6) -0.008(5) 0.024(7) O62 0.045(7) 0.075(13) 0.047(5) 0.001(6) -0.006(4) -0.003(7) O64 0.086(12) 0.058(16) 0.070(8) 0.010(8) -0.021(7) 0.005(10) N63 0.053(10) 0.057(19) 0.050(7) 0.023(9) 0.000(6) 0.001(9) N53 0.038(8) 0.061(14) 0.057(7) -0.003(8) -0.001(6) -0.011(8) O51 0.055(8) 0.044(12) 0.063(6) 0.002(6) 0.006(5) 0.019(7) O52 0.042(7) 0.069(13) 0.076(7) 0.014(8) -0.015(6) -0.002(8) O54 0.069(9) 0.054(14) 0.111(10) 0.000(9) 0.027(8) -0.011(9) O41 0.058(8) 0.081(13) 0.046(5) 0.004(6) 0.003(5) -0.012(8) O44 0.055(8) 0.066(14) 0.079(7) -0.013(7) 0.013(6) -0.031(8) N43 0.031(7) 0.023(13) 0.064(7) 0.004(7) 0.003(6) -0.009(7) O42 0.053(8) 0.045(12) 0.083(8) -0.031(8) -0.008(7) -0.020(8) O100 0.050(7) 0.048(13) 0.040(5) 0.002(5) 0.002(4) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm O61 2.251(13) . ? Tm O100 2.313(10) . ? Tm O42 2.371(14) . ? Tm O51 2.402(14) . ? Tm O52 2.410(13) . ? Tm N11 2.441(15) . ? Tm N21 2.482(17) . ? Tm O41 2.500(14) . ? Tm N31 2.526(14) . ? N11 C16 1.33(2) . ? N11 C12 1.36(2) . ? C12 C13 1.42(3) . ? C13 C14 1.38(3) . ? C14 C15 1.35(3) . ? C15 C16 1.38(3) . ? C16 C22 1.51(2) . ? N21 C26 1.325(19) . ? N21 C22 1.35(2) . ? C22 C23 1.34(3) . ? C23 C24 1.32(3) . ? C24 C25 1.41(3) . ? C25 C26 1.38(3) . ? C26 C32 1.50(3) . ? N31 C36 1.33(3) . ? N31 C32 1.35(2) . ? C36 C35 1.34(2) . ? C35 C34 1.23(4) . ? C34 C33 1.41(4) . ? C33 C32 1.36(2) . ? O61 N63 1.31(2) . ? O62 N63 1.274(18) . ? O64 N63 1.22(2) . ? N53 O54 1.200(19) . ? N53 O51 1.269(18) . ? N53 O52 1.28(2) . ? O41 N43 1.290(15) . ? O44 N43 1.238(17) . ? N43 O42 1.279(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 O61 Tm O100 79.9(4) . . ? O61 Tm O42 87.8(5) . . ? O100 Tm O42 129.9(4) . . ? O61 Tm O51 125.4(4) . . ? O100 Tm O51 71.3(4) . . ? O42 Tm O51 145.6(5) . . ? O61 Tm O52 80.4(5) . . ? O100 Tm O52 84.3(4) . . ? O42 Tm O52 141.3(4) . . ? O51 Tm O52 52.0(5) . . ? O61 Tm N11 146.9(5) . . ? O100 Tm N11 79.0(5) . . ? O42 Tm N11 86.3(5) . . ? O51 Tm N11 70.3(5) . . ? O52 Tm N11 122.3(5) . . ? O61 Tm N21 141.9(4) . . ? O100 Tm N21 137.2(4) . . ? O42 Tm N21 73.9(5) . . ? O51 Tm N21 73.7(4) . . ? O52 Tm N21 93.2(5) . . ? N11 Tm N21 66.4(5) . . ? O61 Tm O41 76.5(5) . . ? O100 Tm O41 76.6(4) . . ? O42 Tm O41 53.2(4) . . ? O51 Tm O41 135.5(4) . . ? O52 Tm O41 152.2(5) . . ? N11 Tm O41 73.9(6) . . ? N21 Tm O41 114.6(5) . . ? O61 Tm N31 76.8(5) . . ? O100 Tm N31 147.7(5) . . ? O42 Tm N31 71.4(5) . . ? O51 Tm N31 105.0(5) . . ? O52 Tm N31 70.1(5) . . ? N11 Tm N31 131.1(6) . . ? N21 Tm N31 65.8(5) . . ? O41 Tm N31 118.4(4) . . ? C16 N11 C12 116.1(16) . . ? C16 N11 Tm 119.7(11) . . ? C12 N11 Tm 122.4(14) . . ? N11 C12 C13 122(2) . . ? C14 C13 C12 119.7(19) . . ? C15 C14 C13 117(2) . . ? C14 C15 C16 121(2) . . ? N11 C16 C15 123.9(18) . . ? N11 C16 C22 116.7(17) . . ? C15 C16 C22 119(2) . . ? C26 N21 C22 120.6(17) . . ? C26 N21 Tm 120.0(13) . . ? C22 N21 Tm 119.3(12) . . ? C23 C22 N21 119.9(17) . . ? C23 C22 C16 125(2) . . ? N21 C22 C16 115.5(19) . . ? C24 C23 C22 121(2) . . ? C23 C24 C25 120(2) . . ? C26 C25 C24 116.3(19) . . ? N21 C26 C25 121.1(18) . . ? N21 C26 C32 119.2(16) . . ? C25 C26 C32 119.4(15) . . ? C36 N31 C32 116.6(15) . . ? C36 N31 Tm 123.7(13) . . ? C32 N31 Tm 119.6(12) . . ? C35 C36 N31 123(2) . . ? C34 C35 C36 123(3) . . ? C35 C34 C33 118.2(19) . . ? C32 C33 C34 119(2) . . ? N31 C32 C33 120(2) . . ? N31 C32 C26 115.3(14) . . ? C33 C32 C26 124.3(18) . . ? N63 O61 Tm 137.8(10) . . ? O64 N63 O62 120.1(19) . . ? O64 N63 O61 123.4(15) . . ? O62 N63 O61 116.4(17) . . ? O54 N53 O51 126.1(18) . . ? O54 N53 O52 122.2(17) . . ? O51 N53 O52 111.6(14) . . ? N53 O51 Tm 98.6(11) . . ? N53 O52 Tm 97.8(9) . . ? N43 O41 Tm 91.9(9) . . ? O44 N43 O41 120.1(14) . . ? O42 N43 O44 123.2(13) . . ? O41 N43 O42 116.6(12) . . ? N43 O42 Tm 98.3(9) . . ? _refine_diff_density_max 1.180 _refine_diff_density_min -1.505 _refine_diff_density_rms 0.225 _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 ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H11 N6 O9 Yb' _chemical_formula_weight 592.34 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 9.090(9) _cell_length_b 16.693(17) _cell_length_c 13.636(15) _cell_angle_alpha 90.00 _cell_angle_beta 111.110(10) _cell_angle_gamma 90.00 _cell_volume 1930(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(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 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 4.909 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '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 5514 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.89 _reflns_number_total 3449 _reflns_number_gt 2726 _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^)+(0.1507P)^2^+1.3917P] 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 0.0026(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3449 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1852 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Yb Yb 0.46701(4) 0.84449(2) 0.20474(3) 0.0355(3) Uani 1 d . . . N43 N 0.3735(12) 0.6956(5) 0.1063(7) 0.054(2) Uani 1 d . . . O42 O 0.5097(10) 0.7241(5) 0.1276(7) 0.062(2) Uani 1 d . . . O41 O 0.2780(9) 0.7404(4) 0.1362(7) 0.062(2) Uani 1 d . . . O44 O 0.3296(14) 0.6315(5) 0.0657(9) 0.084(3) Uani 1 d . . . N53 N 0.4488(11) 0.7748(6) 0.3889(8) 0.057(2) Uani 1 d . . . O52 O 0.4033(13) 0.8439(5) 0.3596(9) 0.071(3) Uani 1 d . . . O51 O 0.5225(9) 0.7380(5) 0.3375(7) 0.060(2) Uani 1 d . . . O54 O 0.4152(12) 0.7412(6) 0.4589(8) 0.077(3) Uani 1 d . . . N63 N 0.4881(13) 0.8904(6) 0.0106(8) 0.061(2) Uani 1 d . . . O61 O 0.6064(10) 0.8869(7) 0.0965(8) 0.074(3) Uani 1 d . . . O62 O 0.3609(9) 0.8748(6) 0.0199(8) 0.073(3) Uani 1 d . . . O64 O 0.5016(15) 0.9087(8) -0.0727(9) 0.103(4) Uani 1 d . . . N11 N 0.2385(9) 0.9290(5) 0.1727(8) 0.048(2) Uani 1 d . . . C16 C 0.2586(10) 1.0076(5) 0.2055(8) 0.040(2) Uani 1 d . . . C12 C 0.0917(11) 0.9022(7) 0.1241(10) 0.059(3) Uani 1 d . . . H12 H 0.0762 0.8489 0.1026 0.071 Uiso 1 calc R . . C13 C -0.0394(11) 0.9521(8) 0.1048(10) 0.063(3) Uani 1 d . . . H13 H -0.1403 0.9322 0.0697 0.075 Uiso 1 calc R . . N21 N 0.5368(8) 0.9776(5) 0.2705(6) 0.0364(16) Uani 1 d . . . C22 C 0.4234(12) 1.0338(6) 0.2607(8) 0.045(2) Uani 1 d . . . C26 C 0.6893(12) 0.9979(6) 0.3171(8) 0.044(2) Uani 1 d . . . C32 C 0.8434(12) 0.7960(8) 0.3263(10) 0.058(3) Uani 1 d . . . H32 H 0.8005 0.7450 0.3097 0.069 Uiso 1 calc R . . C33 C 1.0059(13) 0.8024(8) 0.3656(10) 0.063(3) Uani 1 d . . . H33 H 1.0706 0.7575 0.3786 0.076 Uiso 1 calc R . . N31 N 0.7442(9) 0.8568(5) 0.3104(8) 0.0430(19) Uani 1 d . . . C36 C 0.8056(11) 0.9316(7) 0.3316(9) 0.046(2) Uani 1 d . . . C15 C 0.1308(14) 1.0587(7) 0.1891(9) 0.055(3) Uani 1 d . . . H15 H 0.1470 1.1113 0.2128 0.066 Uiso 1 calc R . . C14 C -0.0196(13) 1.0305(8) 0.1373(11) 0.065(3) Uani 1 d . . . H14 H -0.1063 1.0639 0.1247 0.077 Uiso 1 calc R . . C34 C 1.0676(13) 0.8791(9) 0.3848(9) 0.063(3) Uani 1 d . . . H34 H 1.1761 0.8869 0.4077 0.075 Uiso 1 calc R . . C35 C 0.9686(12) 0.9434(7) 0.3698(10) 0.056(3) Uani 1 d . . . H36 H 1.0097 0.9948 0.3852 0.067 Uiso 1 calc R . . C25 C 0.7358(14) 1.0751(7) 0.3545(11) 0.062(3) Uani 1 d . . . H25 H 0.8423 1.0880 0.3842 0.074 Uiso 1 calc R . . C24 C 0.6244(16) 1.1312(8) 0.3470(11) 0.066(3) Uani 1 d . . . H24 H 0.6537 1.1830 0.3716 0.080 Uiso 1 calc R . . C23 C 0.4604(16) 1.1099(7) 0.3007(10) 0.063(3) Uani 1 d . . . H23 H 0.3818 1.1465 0.2979 0.075 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 Yb 0.0324(3) 0.0331(4) 0.0419(4) 0.00068(14) 0.0143(2) 0.00156(12) N43 0.076(6) 0.039(4) 0.043(5) -0.007(4) 0.018(5) -0.003(4) O42 0.064(5) 0.051(4) 0.080(6) -0.015(4) 0.036(4) 0.002(4) O41 0.049(4) 0.051(4) 0.086(7) -0.012(4) 0.024(4) -0.005(3) O44 0.126(9) 0.050(4) 0.073(7) -0.018(5) 0.032(6) -0.020(5) N53 0.053(5) 0.063(6) 0.054(6) 0.009(5) 0.018(4) 0.008(4) O52 0.082(7) 0.076(7) 0.072(7) 0.017(4) 0.046(6) 0.022(4) O51 0.057(4) 0.057(5) 0.063(6) 0.000(4) 0.019(4) 0.001(3) O54 0.097(7) 0.077(6) 0.070(6) 0.028(5) 0.044(6) 0.007(5) N63 0.078(7) 0.061(6) 0.048(6) 0.001(5) 0.028(5) -0.015(5) O61 0.061(5) 0.106(8) 0.062(6) 0.006(5) 0.032(5) -0.019(5) O62 0.050(4) 0.091(6) 0.072(6) 0.024(5) 0.015(4) -0.003(4) O64 0.126(9) 0.135(10) 0.064(7) 0.022(7) 0.053(7) -0.002(8) N11 0.036(4) 0.049(4) 0.061(6) 0.007(4) 0.019(4) 0.013(3) C16 0.041(4) 0.039(4) 0.044(6) 0.005(4) 0.021(4) 0.006(4) C12 0.037(5) 0.066(7) 0.069(8) 0.006(6) 0.013(5) 0.004(5) C13 0.025(4) 0.085(8) 0.075(8) 0.027(7) 0.014(5) 0.023(5) N21 0.046(4) 0.039(4) 0.029(4) 0.003(3) 0.019(3) 0.001(3) C22 0.052(5) 0.041(5) 0.041(6) 0.002(4) 0.017(4) -0.001(4) C26 0.058(6) 0.042(5) 0.035(5) -0.005(4) 0.020(5) -0.010(4) C32 0.043(5) 0.068(7) 0.064(8) -0.006(6) 0.023(5) 0.006(5) C33 0.050(6) 0.083(8) 0.050(7) 0.002(6) 0.009(5) 0.024(6) N31 0.027(4) 0.047(4) 0.044(5) -0.001(4) -0.001(3) 0.000(3) C36 0.036(4) 0.062(6) 0.041(6) 0.005(5) 0.014(4) -0.006(4) C15 0.067(6) 0.052(6) 0.043(6) 0.006(5) 0.018(5) 0.031(5) C14 0.048(6) 0.078(8) 0.068(8) -0.002(7) 0.021(6) 0.022(6) C34 0.044(5) 0.097(10) 0.042(7) 0.002(6) 0.009(5) 0.000(6) C35 0.048(5) 0.061(6) 0.060(7) -0.007(6) 0.022(5) -0.021(5) C25 0.061(6) 0.058(6) 0.064(8) -0.002(6) 0.021(6) -0.003(5) C24 0.075(8) 0.055(6) 0.061(8) 0.000(6) 0.015(6) -0.029(6) C23 0.083(8) 0.045(6) 0.065(8) -0.015(6) 0.033(7) -0.009(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 Yb O42 2.364(8) . ? Yb O61 2.373(8) . ? Yb O52 2.382(10) . ? Yb O41 2.385(7) . ? Yb N21 2.395(8) . ? Yb O62 2.406(10) . ? Yb N11 2.417(7) . ? Yb N31 2.419(8) . ? Yb O51 2.456(9) . ? N43 O44 1.205(13) . ? N43 O42 1.259(12) . ? N43 O41 1.317(12) . ? N53 O54 1.237(12) . ? N53 O52 1.241(12) . ? N53 O51 1.286(13) . ? N63 O64 1.225(14) . ? N63 O62 1.235(12) . ? N63 O61 1.275(13) . ? N11 C12 1.335(13) . ? N11 C16 1.377(13) . ? C16 C15 1.393(13) . ? C16 C22 1.480(14) . ? C12 C13 1.400(14) . ? C13 C14 1.372(19) . ? N21 C26 1.344(12) . ? N21 C22 1.364(12) . ? C22 C23 1.376(15) . ? C26 C25 1.394(15) . ? C26 C36 1.493(14) . ? C32 N31 1.323(14) . ? C32 C33 1.383(16) . ? C33 C34 1.38(2) . ? N31 C36 1.356(13) . ? C36 C35 1.396(14) . ? C15 C14 1.377(18) . ? C34 C35 1.368(18) . ? C25 C24 1.357(19) . ? C24 C23 1.438(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 O42 Yb O61 76.5(3) . . ? O42 Yb O52 121.5(3) . . ? O61 Yb O52 155.1(4) . . ? O42 Yb O41 54.4(3) . . ? O61 Yb O41 116.4(3) . . ? O52 Yb O41 88.5(4) . . ? O42 Yb N21 153.1(3) . . ? O61 Yb N21 80.1(3) . . ? O52 Yb N21 77.8(3) . . ? O41 Yb N21 151.5(2) . . ? O42 Yb O62 77.3(4) . . ? O61 Yb O62 52.3(3) . . ? O52 Yb O62 142.7(3) . . ? O41 Yb O62 77.4(3) . . ? N21 Yb O62 98.6(3) . . ? O42 Yb N11 133.1(3) . . ? O61 Yb N11 109.3(3) . . ? O52 Yb N11 72.3(3) . . ? O41 Yb N11 84.4(3) . . ? N21 Yb N11 67.7(3) . . ? O62 Yb N11 72.2(3) . . ? O42 Yb N31 92.0(3) . . ? O61 Yb N31 70.7(3) . . ? O52 Yb N31 90.3(4) . . ? O41 Yb N31 138.1(3) . . ? N21 Yb N31 67.6(3) . . ? O62 Yb N31 123.0(3) . . ? N11 Yb N31 134.5(3) . . ? O42 Yb O51 72.0(3) . . ? O61 Yb O51 131.3(3) . . ? O52 Yb O51 52.7(3) . . ? O41 Yb O51 71.9(3) . . ? N21 Yb O51 116.0(3) . . ? O62 Yb O51 145.4(3) . . ? N11 Yb O51 119.4(3) . . ? N31 Yb O51 74.3(3) . . ? O44 N43 O42 125.2(10) . . ? O44 N43 O41 120.1(10) . . ? O42 N43 O41 114.7(8) . . ? N43 O42 Yb 96.8(6) . . ? N43 O41 Yb 94.2(6) . . ? O54 N53 O52 121.6(10) . . ? O54 N53 O51 121.7(10) . . ? O52 N53 O51 116.6(10) . . ? N53 O52 Yb 97.5(7) . . ? N53 O51 Yb 92.7(6) . . ? O64 N63 O62 123.9(12) . . ? O64 N63 O61 122.1(11) . . ? O62 N63 O61 114.0(9) . . ? N63 O61 Yb 97.0(6) . . ? N63 O62 Yb 96.6(7) . . ? C12 N11 C16 118.2(8) . . ? C12 N11 Yb 122.3(7) . . ? C16 N11 Yb 119.5(6) . . ? N11 C16 C15 121.7(9) . . ? N11 C16 C22 116.0(8) . . ? C15 C16 C22 122.2(9) . . ? N11 C12 C13 121.6(12) . . ? C14 C13 C12 120.3(11) . . ? C26 N21 C22 119.2(8) . . ? C26 N21 Yb 120.0(6) . . ? C22 N21 Yb 120.9(6) . . ? N21 C22 C23 121.9(10) . . ? N21 C22 C16 115.9(8) . . ? C23 C22 C16 122.2(10) . . ? N21 C26 C25 122.1(10) . . ? N21 C26 C36 115.9(8) . . ? C25 C26 C36 121.9(10) . . ? N31 C32 C33 125.1(12) . . ? C32 C33 C34 116.6(11) . . ? C32 N31 C36 117.9(9) . . ? C32 N31 Yb 122.3(7) . . ? C36 N31 Yb 117.8(6) . . ? N31 C36 C35 120.6(10) . . ? N31 C36 C26 115.8(8) . . ? C35 C36 C26 123.4(10) . . ? C14 C15 C16 119.3(11) . . ? C13 C14 C15 118.8(9) . . ? C35 C34 C33 119.8(10) . . ? C34 C35 C36 119.9(11) . . ? C24 C25 C26 119.4(11) . . ? C25 C24 C23 119.3(12) . . ? C22 C23 C24 118.0(12) . . ? _refine_diff_density_max 3.447 _refine_diff_density_min -3.278 _refine_diff_density_rms 0.289 _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-La _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H29 La N14 O21' _chemical_formula_weight 542.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 10.385(14) _cell_length_b 41.89(5) _cell_length_c 10.757(12) _cell_angle_alpha 90.00 _cell_angle_beta 115.700(10) _cell_angle_gamma 90.00 _cell_volume 4216(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11752 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.95 _reflns_number_total 6846 _reflns_number_gt 5752 _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_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0004P)^2^+91.3352P] 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 6860 _refine_ls_number_parameters 623 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2245 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.275 _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 La1 La 0.00826(9) 0.135346(18) 0.22545(9) 0.0334(2) Uani 1 d . . . O11 O 0.1079(12) 0.1230(3) 0.4949(11) 0.055(3) Uani 1 d . . . O12 O 0.2715(11) 0.1298(3) 0.4246(11) 0.052(3) Uani 1 d . . . N13 N 0.2393(15) 0.1254(3) 0.5255(15) 0.052(4) Uani 1 d . . . O14 O 0.3315(14) 0.1231(4) 0.6435(13) 0.092(5) Uani 1 d . . . O21 O -0.0056(12) 0.1456(2) -0.0228(11) 0.051(3) Uani 1 d . . . O22 O 0.1830(11) 0.1201(2) 0.1121(11) 0.049(3) Uani 1 d . . . N23 N 0.1113(14) 0.1330(3) -0.0054(13) 0.044(3) Uani 1 d . . . O24 O 0.1542(13) 0.1331(3) -0.0946(12) 0.059(3) Uani 1 d . . . O31 O -0.1758(11) 0.1028(2) 0.2908(12) 0.052(3) Uani 1 d . . . O32 O -0.1680(11) 0.1533(2) 0.3322(9) 0.044(2) Uani 1 d . . . O34 O -0.2863(15) 0.1220(3) 0.4080(15) 0.086(5) Uani 1 d . . . N33 N -0.2132(14) 0.1254(3) 0.3461(14) 0.050(3) Uani 1 d . . . O41 O 0.0817(12) 0.0743(2) 0.2806(11) 0.052(3) Uani 1 d . . . O42 O -0.0776(12) 0.0837(2) 0.0736(10) 0.049(3) Uani 1 d . . . N43 N 0.0034(16) 0.0638(3) 0.1622(15) 0.050(3) Uani 1 d . . . O44 O 0.0019(16) 0.0351(2) 0.1329(12) 0.073(4) Uani 1 d . . . O51 O -0.2545(11) 0.1418(2) 0.0285(11) 0.049(3) Uani 1 d . . . O52 O -0.1468(11) 0.1867(2) 0.0965(10) 0.049(3) Uani 1 d . . . N53 N -0.2586(13) 0.1720(3) 0.0193(11) 0.044(3) Uani 1 d . . . O54 O -0.3641(13) 0.1866(3) -0.0603(12) 0.072(4) Uani 1 d . . . O61 O 0.1653(11) 0.1875(2) 0.2194(10) 0.043(2) Uani 1 d . . . O62 O 0.0850(10) 0.1880(2) 0.3785(9) 0.040(2) Uani 1 d . . . N63 N 0.1504(12) 0.2018(3) 0.3156(12) 0.041(3) Uani 1 d . . . O64 O 0.2034(12) 0.2288(2) 0.3550(11) 0.056(3) Uani 1 d . . . N11 N -0.0055(12) 0.3002(3) -0.1244(11) 0.037(3) Uani 1 d . . . H11 H -0.0323 0.3047 -0.2100 0.044 Uiso 1 calc R . . C12 C 0.0174(19) 0.3245(4) -0.0365(17) 0.054(4) Uani 1 d . . . H12 H 0.0038 0.3454 -0.0682 0.064 Uiso 1 calc R . . C13 C 0.0611(17) 0.3181(3) 0.1013(18) 0.053(4) Uani 1 d . . . H13 H 0.0776 0.3345 0.1645 0.063 Uiso 1 calc R . . C14 C 0.0799(17) 0.2867(4) 0.1432(14) 0.045(4) Uani 1 d . . . H14 H 0.1079 0.2822 0.2360 0.054 Uiso 1 calc R . . C15 C 0.0589(16) 0.2616(3) 0.0534(13) 0.040(3) Uani 1 d . . . H15 H 0.0760 0.2407 0.0850 0.048 Uiso 1 calc R . . C16 C 0.0110(15) 0.2687(3) -0.0867(15) 0.037(3) Uani 1 d . . . N21 N -0.0635(12) 0.2576(2) -0.3257(10) 0.0300(16) Uani 1 d U . . C23 C -0.0224(14) 0.2126(3) -0.1790(13) 0.0311(17) Uani 1 d U . . H23 H 0.0031 0.2044 -0.0912 0.037 Uiso 1 calc R . . C22 C -0.0246(14) 0.2452(3) -0.1999(12) 0.0301(16) Uani 1 d U . . C24 C -0.0591(18) 0.1925(3) -0.2916(17) 0.053(4) Uani 1 d . . . H24 H -0.0579 0.1705 -0.2789 0.063 Uiso 1 calc R . . C25 C -0.0977(17) 0.2047(3) -0.4229(16) 0.045(4) Uani 1 d . . . H25 H -0.1210 0.1915 -0.4991 0.054 Uiso 1 calc R . . C26 C -0.0997(14) 0.2380(3) -0.4347(12) 0.030(3) Uani 1 d . . . C33 C -0.1866(17) 0.2377(4) -0.6947(16) 0.048(4) Uani 1 d . . . H33 H -0.1853 0.2155 -0.6972 0.04(4) Uiso 1 calc R . . C34 C -0.2323(14) 0.2553(4) -0.8174(15) 0.048(4) Uani 1 d . . . H34 H -0.2642 0.2449 -0.9020 0.058 Uiso 1 calc R . . N31 N -0.1409(13) 0.2861(3) -0.5688(12) 0.040(3) Uani 1 d . . . H31 H -0.1122 0.2959 -0.4911 0.048 Uiso 1 calc R . . C36 C -0.1812(16) 0.3035(4) -0.6840(15) 0.049(4) Uani 1 d . . . H36 H -0.1767 0.3257 -0.6781 0.059 Uiso 1 calc R . . C35 C -0.2290(16) 0.2891(4) -0.8107(14) 0.047(4) Uani 1 d . . . H35 H -0.2587 0.3012 -0.8906 0.056 Uiso 1 calc R . . C32 C -0.1432(13) 0.2535(3) -0.5693(13) 0.033(3) Uani 1 d . . . N41 N 0.4673(15) 0.0529(3) 0.5450(12) 0.048(3) Uani 1 d . . . H41 H 0.4065 0.0427 0.4745 0.057 Uiso 1 calc R . . C42 C 0.5546(18) 0.0739(4) 0.5268(16) 0.051(4) Uani 1 d . . . H42 H 0.5489 0.0770 0.4389 0.061 Uiso 1 calc R . . C43 C 0.6540(19) 0.0913(4) 0.6374(17) 0.053(4) Uani 1 d . . . H43 H 0.7147 0.1059 0.6247 0.064 Uiso 1 calc R . . C44 C 0.6596(19) 0.0861(4) 0.7672(16) 0.051(4) Uani 1 d . . . H44 H 0.7230 0.0979 0.8418 0.062 Uiso 1 calc R . . C45 C 0.5729(19) 0.0637(4) 0.7874(16) 0.053(4) Uani 1 d . . . H45 H 0.5810 0.0596 0.8756 0.064 Uiso 1 calc R . . C46 C 0.4713(17) 0.0469(3) 0.6718(15) 0.046(4) Uani 1 d . . . N51 N 0.2922(13) 0.0071(3) 0.5616(12) 0.040(3) Uani 1 d . . . C52 C 0.3705(19) 0.0222(4) 0.6775(16) 0.049(4) Uani 1 d . . . C53 C 0.359(2) 0.0160(4) 0.7994(18) 0.059(5) Uani 1 d . . . H53 H 0.4144 0.0273 0.8792 0.071 Uiso 1 calc R . . C54 C 0.265(2) -0.0071(4) 0.8010(14) 0.060(5) Uani 1 d . . . H54 H 0.2574 -0.0118 0.8820 0.072 Uiso 1 calc R . . C55 C 0.184(2) -0.0228(4) 0.6821(17) 0.058(4) Uani 1 d . . . H55 H 0.1177 -0.0381 0.6794 0.069 Uiso 1 calc R . . C56 C 0.2022(15) -0.0155(3) 0.5638(16) 0.041(3) Uani 1 d . . . C62 C 0.1151(18) -0.0320(3) 0.4326(15) 0.045(4) Uani 1 d . . . N61 N 0.1322(14) -0.0224(2) 0.3204(11) 0.040(3) Uani 1 d . . . H61 H 0.1938 -0.0076 0.3316 0.048 Uiso 1 calc R . . C66 C 0.0198(19) -0.0564(4) 0.4165(15) 0.051(4) Uani 1 d . . . H66 H 0.0067 -0.0639 0.4917 0.061 Uiso 1 calc R . . C65 C -0.0561(19) -0.0697(4) 0.2871(14) 0.052(4) Uani 1 d . . . H65 H -0.1188 -0.0865 0.2769 0.062 Uiso 1 calc R . . C64 C -0.0413(18) -0.0588(3) 0.1730(14) 0.046(4) Uani 1 d . . . H64 H -0.0958 -0.0672 0.0856 0.055 Uiso 1 calc R . . C63 C 0.0607(18) -0.0343(3) 0.1946(17) 0.050(4) Uani 1 d . . . H63 H 0.0770 -0.0266 0.1216 0.060 Uiso 1 calc R . . O71 O 0.6549(12) -0.0161(3) 0.6864(10) 0.054(3) Uani 1 d . . . O72 O 0.7176(16) -0.0101(4) 0.8998(11) 0.091(5) Uani 1 d . . . N73 N 0.6517(18) -0.0248(4) 0.7968(12) 0.059(4) Uani 1 d . . . O74 O 0.582(2) -0.0483(4) 0.7952(18) 0.128(7) Uani 1 d . . . N100 N -0.0356(14) 0.3370(3) -0.3653(13) 0.050(3) Uani 1 d . . . C101 C -0.0317(17) 0.3621(4) -0.4058(17) 0.049(4) Uani 1 d . . . C102 C -0.017(2) 0.3941(4) -0.456(2) 0.066(5) Uani 1 d . . . H10A H -0.11(2) 0.405(4) -0.475(19) 0.080 Uiso 1 d . . . H10B H -0.06(2) 0.393(4) -0.551(19) 0.080 Uiso 1 d . . . H10C H 0.056(19) 0.406(4) -0.351(19) 0.080 Uiso 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 0.0353(4) 0.0323(4) 0.0302(4) 0.0016(3) 0.0121(3) 0.0001(4) O11 0.044(7) 0.059(7) 0.056(7) 0.005(5) 0.016(6) -0.002(5) O12 0.047(7) 0.064(7) 0.038(6) 0.014(5) 0.011(5) 0.001(5) N13 0.049(9) 0.039(7) 0.053(9) 0.014(6) 0.009(8) 0.002(6) O14 0.057(9) 0.138(13) 0.050(8) 0.019(8) -0.005(7) 0.008(8) O21 0.057(7) 0.040(6) 0.064(8) 0.012(5) 0.033(6) 0.013(5) O22 0.048(7) 0.061(7) 0.050(7) 0.014(5) 0.031(6) 0.010(5) N23 0.056(8) 0.031(6) 0.057(9) -0.002(6) 0.036(7) -0.003(6) O24 0.073(8) 0.068(7) 0.064(8) -0.001(6) 0.057(7) 0.007(6) O31 0.047(6) 0.044(6) 0.072(8) -0.007(5) 0.033(6) -0.001(5) O32 0.042(6) 0.059(7) 0.027(5) -0.006(4) 0.010(5) 0.001(5) O34 0.085(10) 0.104(10) 0.121(12) 0.035(9) 0.092(10) 0.016(8) N33 0.044(8) 0.062(9) 0.050(8) 0.009(6) 0.027(7) 0.000(6) O41 0.059(7) 0.046(6) 0.046(7) 0.010(5) 0.018(6) 0.008(5) O42 0.060(7) 0.038(5) 0.039(6) 0.001(5) 0.011(5) 0.004(5) N43 0.072(10) 0.029(6) 0.060(9) -0.001(6) 0.038(8) -0.003(6) O44 0.142(13) 0.030(6) 0.058(8) -0.001(5) 0.053(8) -0.002(6) O51 0.052(6) 0.032(6) 0.057(7) 0.001(5) 0.018(6) 0.002(4) O52 0.048(7) 0.047(6) 0.038(6) -0.003(5) 0.007(5) 0.002(5) N53 0.034(7) 0.067(9) 0.019(6) 0.019(6) -0.001(6) 0.018(6) O54 0.053(8) 0.097(10) 0.050(7) 0.037(7) 0.009(6) 0.019(7) O61 0.050(6) 0.051(6) 0.032(6) -0.011(5) 0.024(5) -0.007(5) O62 0.043(6) 0.048(6) 0.027(5) 0.006(4) 0.013(5) -0.012(4) N63 0.032(7) 0.037(6) 0.039(7) 0.001(5) 0.003(6) -0.002(5) O64 0.062(7) 0.034(5) 0.060(7) -0.004(5) 0.017(6) -0.016(5) N11 0.046(7) 0.045(7) 0.017(6) 0.003(5) 0.011(5) 0.007(5) C12 0.065(11) 0.050(9) 0.052(11) 0.000(8) 0.031(9) 0.003(8) C13 0.055(10) 0.037(8) 0.063(11) -0.004(7) 0.023(9) -0.004(7) C14 0.062(11) 0.062(10) 0.020(7) -0.007(6) 0.025(7) 0.002(8) C15 0.051(9) 0.048(8) 0.021(7) 0.012(6) 0.017(7) 0.006(7) C16 0.035(8) 0.036(7) 0.046(9) -0.001(6) 0.023(7) -0.003(6) N21 0.035(4) 0.042(4) 0.015(3) 0.001(3) 0.013(3) 0.001(3) C23 0.036(4) 0.042(4) 0.016(3) 0.001(3) 0.012(3) 0.001(3) C22 0.035(4) 0.042(4) 0.015(3) 0.001(3) 0.013(3) 0.001(3) C24 0.069(11) 0.027(7) 0.060(11) 0.000(7) 0.027(9) 0.000(7) C25 0.057(10) 0.043(8) 0.044(9) 0.007(7) 0.031(8) 0.010(7) C26 0.032(7) 0.048(8) 0.012(6) 0.009(5) 0.012(6) 0.009(6) C33 0.048(10) 0.050(9) 0.048(10) 0.003(7) 0.022(8) 0.009(7) C34 0.017(7) 0.072(11) 0.036(9) 0.009(7) -0.007(7) 0.009(6) N31 0.051(8) 0.044(7) 0.031(7) 0.001(5) 0.023(6) -0.001(5) C36 0.038(9) 0.056(9) 0.039(9) 0.017(7) 0.004(7) -0.012(7) C35 0.048(10) 0.057(10) 0.024(8) 0.015(7) 0.006(7) 0.009(7) C32 0.019(7) 0.048(8) 0.024(7) -0.001(6) 0.002(6) 0.002(5) N41 0.068(9) 0.040(7) 0.027(7) -0.002(5) 0.013(6) -0.009(6) C42 0.070(12) 0.056(10) 0.033(9) -0.007(7) 0.027(8) -0.004(8) C43 0.068(11) 0.042(8) 0.055(11) -0.005(7) 0.031(9) -0.011(8) C44 0.065(11) 0.047(9) 0.046(10) -0.016(7) 0.028(9) -0.009(8) C45 0.084(13) 0.048(9) 0.032(9) -0.008(7) 0.029(9) 0.001(8) C46 0.057(10) 0.038(8) 0.033(8) 0.008(6) 0.011(7) 0.012(7) N51 0.054(8) 0.036(6) 0.033(7) 0.000(5) 0.022(6) 0.003(5) C52 0.064(11) 0.048(9) 0.038(9) -0.001(7) 0.025(8) 0.000(7) C53 0.074(13) 0.049(10) 0.057(11) -0.007(8) 0.032(10) 0.005(8) C54 0.093(14) 0.074(11) 0.005(7) 0.010(7) 0.013(8) 0.001(10) C55 0.076(13) 0.051(9) 0.057(11) 0.000(8) 0.039(10) -0.009(8) C56 0.035(8) 0.044(8) 0.053(10) 0.012(7) 0.027(8) 0.012(6) C62 0.065(11) 0.029(7) 0.043(9) 0.003(6) 0.024(8) 0.005(7) N61 0.069(9) 0.029(6) 0.027(6) -0.003(5) 0.025(6) -0.007(5) C66 0.082(13) 0.050(9) 0.034(9) 0.004(7) 0.037(9) 0.003(8) C65 0.088(13) 0.049(9) 0.021(8) 0.010(6) 0.026(8) -0.001(8) C64 0.078(12) 0.045(8) 0.023(8) -0.013(6) 0.031(8) -0.004(8) C63 0.069(11) 0.034(8) 0.048(10) 0.005(7) 0.026(9) 0.010(7) O71 0.066(8) 0.065(7) 0.033(6) -0.007(5) 0.024(6) -0.014(6) O72 0.121(13) 0.139(13) 0.006(6) 0.000(7) 0.021(7) -0.009(10) N73 0.097(12) 0.075(10) 0.010(7) 0.014(6) 0.027(7) 0.004(9) O74 0.22(2) 0.081(11) 0.122(15) 0.006(10) 0.111(15) -0.042(12) N100 0.057(9) 0.049(8) 0.041(8) 0.002(6) 0.018(7) -0.006(6) C101 0.049(9) 0.047(9) 0.057(10) -0.003(8) 0.027(8) 0.004(7) C102 0.077(14) 0.044(10) 0.067(13) 0.009(9) 0.022(12) 0.001(9) _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 O42 2.624(10) . ? La1 O21 2.646(11) . ? La1 O51 2.645(10) . ? La1 O12 2.653(10) . ? La1 O32 2.658(10) . ? La1 O62 2.659(9) . ? La1 O41 2.660(10) . ? La1 O22 2.667(10) . ? La1 O11 2.672(11) . ? La1 O31 2.678(11) . ? La1 O52 2.685(10) . ? La1 O61 2.742(10) . ? O11 N13 1.262(16) . ? O12 N13 1.280(16) . ? N13 O14 1.218(16) . ? O21 N23 1.261(15) . ? O22 N23 1.277(15) . ? N23 O24 1.220(14) . ? O31 N33 1.267(16) . ? O32 N33 1.290(15) . ? O34 N33 1.216(16) . ? O41 N43 1.258(16) . ? O42 N43 1.271(15) . ? N43 O44 1.239(14) . ? O51 N53 1.267(15) . ? O52 N53 1.257(15) . ? N53 O54 1.224(14) . ? O61 N63 1.262(15) . ? O62 N63 1.285(14) . ? N63 O64 1.248(14) . ? N11 C12 1.338(18) . ? N11 C16 1.370(16) . ? C12 C13 1.38(2) . ? C13 C14 1.38(2) . ? C14 C15 1.379(19) . ? C15 C16 1.399(18) . ? C16 C22 1.481(17) . ? N21 C22 1.336(15) . ? N21 C26 1.344(15) . ? C23 C22 1.383(17) . ? C23 C24 1.387(19) . ? C24 C25 1.39(2) . ? C25 C26 1.400(18) . ? C26 C32 1.469(17) . ? C33 C32 1.392(19) . ? C33 C34 1.40(2) . ? C34 C35 1.42(2) . ? N31 C36 1.338(17) . ? N31 C32 1.365(16) . ? C36 C35 1.37(2) . ? N41 C42 1.337(19) . ? N41 C46 1.370(18) . ? C42 C43 1.39(2) . ? C43 C44 1.39(2) . ? C44 C45 1.38(2) . ? C45 C46 1.42(2) . ? C46 C52 1.49(2) . ? N51 C52 1.318(18) . ? N51 C56 1.337(18) . ? C52 C53 1.39(2) . ? C53 C54 1.38(2) . ? C54 C55 1.36(2) . ? C55 C56 1.40(2) . ? C56 C62 1.48(2) . ? C62 N61 1.356(18) . ? C62 C66 1.38(2) . ? N61 C63 1.325(18) . ? C66 C65 1.38(2) . ? C65 C64 1.380(18) . ? C64 C63 1.42(2) . ? O71 N73 1.257(14) . ? O72 N73 1.192(17) . ? N73 O74 1.218(19) . ? N100 C101 1.144(19) . ? C101 C102 1.48(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 O42 La1 O21 69.5(3) . . ? O42 La1 O51 68.4(3) . . ? O21 La1 O51 65.7(3) . . ? O42 La1 O12 112.5(3) . . ? O21 La1 O12 114.5(3) . . ? O51 La1 O12 179.0(3) . . ? O42 La1 O32 113.0(3) . . ? O21 La1 O32 130.1(3) . . ? O51 La1 O32 69.7(3) . . ? O12 La1 O32 109.7(3) . . ? O42 La1 O62 177.8(3) . . ? O21 La1 O62 111.2(3) . . ? O51 La1 O62 109.8(3) . . ? O12 La1 O62 69.3(3) . . ? O32 La1 O62 64.8(3) . . ? O42 La1 O41 48.2(3) . . ? O21 La1 O41 105.4(3) . . ? O51 La1 O41 112.0(3) . . ? O12 La1 O41 68.9(3) . . ? O32 La1 O41 111.2(3) . . ? O62 La1 O41 132.8(3) . . ? O42 La1 O22 68.4(3) . . ? O21 La1 O22 47.7(3) . . ? O51 La1 O22 109.2(3) . . ? O12 La1 O22 71.4(3) . . ? O32 La1 O22 177.2(3) . . ? O62 La1 O22 113.7(3) . . ? O41 La1 O22 71.6(3) . . ? O42 La1 O11 112.5(3) . . ? O21 La1 O11 162.2(3) . . ? O51 La1 O11 132.0(3) . . ? O12 La1 O11 47.8(3) . . ? O32 La1 O11 66.5(3) . . ? O62 La1 O11 67.6(3) . . ? O41 La1 O11 68.4(3) . . ? O22 La1 O11 115.4(3) . . ? O42 La1 O31 69.8(3) . . ? O21 La1 O31 127.9(3) . . ? O51 La1 O31 69.9(3) . . ? O12 La1 O31 110.3(3) . . ? O32 La1 O31 47.7(3) . . ? O62 La1 O31 108.4(3) . . ? O41 La1 O31 67.7(3) . . ? O22 La1 O31 134.6(3) . . ? O11 La1 O31 66.5(3) . . ? O42 La1 O52 111.9(3) . . ? O21 La1 O52 65.9(3) . . ? O51 La1 O52 47.5(3) . . ? O12 La1 O52 131.7(3) . . ? O32 La1 O52 67.9(3) . . ? O62 La1 O52 66.8(3) . . ? O41 La1 O52 159.2(3) . . ? O22 La1 O52 109.4(3) . . ? O11 La1 O52 125.4(3) . . ? O31 La1 O52 101.9(3) . . ? O42 La1 O61 133.4(3) . . ? O21 La1 O61 67.7(3) . . ? O51 La1 O61 108.4(3) . . ? O12 La1 O61 71.0(3) . . ? O32 La1 O61 108.2(3) . . ? O62 La1 O61 48.2(3) . . ? O41 La1 O61 130.9(3) . . ? O22 La1 O61 69.6(3) . . ? O11 La1 O61 103.1(3) . . ? O31 La1 O61 155.6(3) . . ? O52 La1 O61 65.1(3) . . ? N13 O11 La1 97.6(9) . . ? N13 O12 La1 98.1(8) . . ? O14 N13 O11 122.5(15) . . ? O14 N13 O12 121.3(14) . . ? O11 N13 O12 116.2(13) . . ? N23 O21 La1 99.0(8) . . ? N23 O22 La1 97.5(8) . . ? O24 N23 O21 122.6(13) . . ? O24 N23 O22 121.6(12) . . ? O21 N23 O22 115.8(11) . . ? N33 O31 La1 98.1(8) . . ? N33 O32 La1 98.4(8) . . ? O34 N33 O31 124.1(14) . . ? O34 N33 O32 120.9(14) . . ? O31 N33 O32 115.0(13) . . ? N43 O41 La1 96.6(8) . . ? N43 O42 La1 98.0(8) . . ? O44 N43 O41 122.0(13) . . ? O44 N43 O42 120.9(14) . . ? O41 N43 O42 117.1(11) . . ? N53 O51 La1 98.9(8) . . ? N53 O52 La1 97.2(7) . . ? O54 N53 O52 120.5(13) . . ? O54 N53 O51 123.1(14) . . ? O52 N53 O51 116.4(10) . . ? N63 O61 La1 94.2(7) . . ? N63 O62 La1 97.6(7) . . ? O64 N63 O61 121.1(13) . . ? O64 N63 O62 118.9(12) . . ? O61 N63 O62 119.9(11) . . ? C12 N11 C16 124.2(12) . . ? N11 C12 C13 119.2(14) . . ? C14 C13 C12 118.2(15) . . ? C15 C14 C13 122.8(14) . . ? C14 C15 C16 117.9(13) . . ? N11 C16 C15 117.6(12) . . ? N11 C16 C22 116.2(12) . . ? C15 C16 C22 126.2(12) . . ? C22 N21 C26 119.7(11) . . ? C22 C23 C24 118.7(12) . . ? N21 C22 C23 121.5(11) . . ? N21 C22 C16 115.7(11) . . ? C23 C22 C16 122.7(11) . . ? C23 C24 C25 120.8(13) . . ? C24 C25 C26 116.5(13) . . ? N21 C26 C25 122.8(11) . . ? N21 C26 C32 116.1(11) . . ? C25 C26 C32 121.1(12) . . ? C32 C33 C34 119.9(14) . . ? C33 C34 C35 119.0(14) . . ? C36 N31 C32 122.9(13) . . ? N31 C36 C35 120.9(14) . . ? C36 C35 C34 118.8(13) . . ? N31 C32 C33 118.5(12) . . ? N31 C32 C26 116.3(11) . . ? C33 C32 C26 125.2(13) . . ? C42 N41 C46 122.5(13) . . ? N41 C42 C43 121.0(14) . . ? C44 C43 C42 118.0(15) . . ? C45 C44 C43 121.2(15) . . ? C44 C45 C46 119.0(14) . . ? N41 C46 C45 118.2(14) . . ? N41 C46 C52 116.7(13) . . ? C45 C46 C52 125.0(14) . . ? C52 N51 C56 118.2(13) . . ? N51 C52 C53 122.1(15) . . ? N51 C52 C46 116.7(13) . . ? C53 C52 C46 121.1(15) . . ? C54 C53 C52 119.5(16) . . ? C55 C54 C53 118.8(14) . . ? C54 C55 C56 118.5(15) . . ? N51 C56 C55 122.8(15) . . ? N51 C56 C62 117.2(13) . . ? C55 C56 C62 119.9(14) . . ? N61 C62 C66 118.1(14) . . ? N61 C62 C56 116.7(13) . . ? C66 C62 C56 125.1(14) . . ? C63 N61 C62 124.5(13) . . ? C62 C66 C65 119.3(14) . . ? C64 C65 C66 121.8(15) . . ? C65 C64 C63 117.1(14) . . ? N61 C63 C64 119.1(14) . . ? O72 N73 O74 122.0(14) . . ? O72 N73 O71 119.2(15) . . ? O74 N73 O71 118.8(15) . . ? N100 C101 C102 176.3(18) . . ? _refine_diff_density_max 1.214 _refine_diff_density_min -2.924 _refine_diff_density_rms 0.165 _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