# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1507 data_1-La _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 1-La _chemical_formula_sum 'C11 H23 La N10 O15' _chemical_formula_weight 674.30 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.830(12) _cell_length_b 11.254(14) _cell_length_c 13.787(17) _cell_angle_alpha 73.957(10) _cell_angle_beta 79.888(10) _cell_angle_gamma 67.599(10) _cell_volume 1351(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.662 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3412 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.04 _reflns_number_total 3412 _reflns_number_gt 3085 _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^)+(0.1518P)^2^+42.4576P] 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 0.005(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3412 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.3220 _refine_ls_wR_factor_gt 0.3176 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.223 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.26396(14) 0.31955(11) 0.24379(7) 0.0318(5) Uani 1 d . . . N14 N 0.192(2) 0.5222(16) 0.3358(11) 0.035(4) Uani 1 d . . . C13 C 0.179(3) 0.492(2) 0.4406(15) 0.044(5) Uani 1 d . . . N12 N 0.137(3) 0.600(2) 0.4791(13) 0.049(5) Uani 1 d . . . N11 N 0.126(3) 0.7024(19) 0.3966(15) 0.052(5) Uani 1 d . . . H11 H 0.1027 0.7839 0.3977 0.062 Uiso 1 calc R . . C15 C 0.159(2) 0.652(2) 0.3108(15) 0.038(5) Uani 1 d . . . N21 N 0.2529(18) 0.2621(14) 0.4535(9) 0.026(3) Uani 1 d . . . C22 C 0.282(2) 0.137(2) 0.5082(12) 0.034(4) Uani 1 d . . . C23 C 0.274(3) 0.101(2) 0.6147(13) 0.047(6) Uani 1 d . . . H23 H 0.2943 0.0140 0.6507 0.057 Uiso 1 calc R . . C24 C 0.233(3) 0.207(2) 0.6639(13) 0.044(5) Uani 1 d . . . H24 H 0.2284 0.1896 0.7342 0.053 Uiso 1 calc R . . C25 C 0.200(3) 0.336(3) 0.6087(13) 0.044(5) Uani 1 d . . . H25 H 0.1709 0.4053 0.6411 0.053 Uiso 1 calc R . . C26 C 0.211(2) 0.360(2) 0.5026(12) 0.035(4) Uani 1 d . . . N34 N 0.341(2) 0.0629(17) 0.3488(11) 0.039(4) Uani 1 d . . . C33 C 0.331(3) 0.033(2) 0.4503(14) 0.036(4) Uani 1 d . . . N32 N 0.363(2) -0.0922(16) 0.4935(13) 0.042(4) Uani 1 d . . . N31 N 0.396(3) -0.1445(17) 0.4145(15) 0.047(5) Uani 1 d . . . H31 H 0.4228 -0.2279 0.4193 0.057 Uiso 1 calc R . . C35 C 0.386(3) -0.058(2) 0.3276(15) 0.036(4) Uani 1 d . . . O100 O 0.069(2) 0.5099(15) 0.1366(10) 0.049(4) Uani 1 d . . . O200 O 0.392(2) 0.4828(18) 0.1400(13) 0.070(6) Uani 1 d . . . O300 O -0.0090(18) 0.3559(16) 0.3245(10) 0.043(4) Uani 1 d . . . O400 O 0.517(2) 0.2664(18) 0.3081(10) 0.050(4) Uani 1 d . . . O500 O 0.139(2) 0.1926(19) 0.1829(12) 0.058(5) Uani 1 d . . . C100 C 0.157(5) 0.732(4) 0.203(2) 0.033(7) Uiso 0.50 d P A 1 H10A H 0.2543 0.7038 0.1694 0.040 Uiso 0.50 calc PR A 1 H10B H 0.1262 0.8237 0.2024 0.040 Uiso 0.50 calc PR A 1 H10C H 0.0895 0.7182 0.1683 0.040 Uiso 0.50 calc PR A 1 C101 C 0.025(3) 0.710(3) 0.2432(16) 0.010(4) Uiso 0.50 d P A 2 H10D H 0.0532 0.7548 0.1771 0.012 Uiso 0.50 calc PR A 2 H10E H -0.0566 0.7717 0.2738 0.012 Uiso 0.50 calc PR A 2 H10F H -0.0029 0.6398 0.2374 0.012 Uiso 0.50 calc PR A 2 C300 C 0.496(3) -0.072(2) 0.2432(15) 0.007(4) Uiso 0.50 d P B 1 H30A H 0.5550 -0.0203 0.2415 0.008 Uiso 0.50 calc PR B 1 H30B H 0.4477 -0.0411 0.1814 0.008 Uiso 0.50 calc PR B 1 H30C H 0.5572 -0.1629 0.2504 0.008 Uiso 0.50 calc PR B 1 C301 C 0.418(5) -0.087(4) 0.221(2) 0.031(7) Uiso 0.50 d P B 2 H30D H 0.4859 -0.1760 0.2247 0.038 Uiso 0.50 calc PR B 2 H30E H 0.4595 -0.0265 0.1754 0.038 Uiso 0.50 calc PR B 2 H30F H 0.3272 -0.0780 0.1972 0.038 Uiso 0.50 calc PR B 2 O51 O 0.484(3) 0.1827(19) 0.1379(13) 0.065(6) Uani 1 d . . . N53 N 0.445(5) 0.232(4) 0.0486(15) 0.083(11) Uani 1 d . . . O52 O 0.306(4) 0.321(3) 0.0428(14) 0.088(8) Uani 1 d . . . O54 O 0.509(4) 0.204(4) -0.0256(18) 0.122(13) Uani 1 d . . . N43 N -0.211(3) 0.344(2) 0.1071(16) 0.060(6) Uani 1 d . . . O42 O -0.217(4) 0.311(3) 0.2029(15) 0.108(11) Uani 1 d . . . O41 O -0.321(3) 0.389(3) 0.0632(15) 0.089(8) Uani 1 d . . . O44 O -0.089(2) 0.337(2) 0.0582(12) 0.069(6) Uani 1 d . . . N63 N 0.009(6) 0.001(2) 0.4511(14) 0.055(9) Uiso 0.50 d PD . . O61 O 0.032(8) 0.001(4) 0.3646(13) 0.095(14) Uiso 0.50 d PD . . O62 O -0.019(4) 0.0983(12) 0.4812(14) 0.101(8) Uiso 1 d D . . O71 O 0.475(5) -0.4126(16) 0.5182(18) 0.122(10) Uiso 1 d D . . N73 N 0.517(6) -0.473(2) 0.4517(16) 0.071(13) Uiso 0.50 d PD . . O72 O 0.489(11) -0.418(4) 0.3667(17) 0.13(2) Uiso 0.50 d PD . . O700 O -0.228(3) 0.620(3) 0.1655(14) 0.082(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 La1 0.0323(8) 0.0318(7) 0.0312(6) -0.0073(4) -0.0025(3) -0.0111(5) N14 0.034(12) 0.028(8) 0.040(7) -0.002(6) -0.006(6) -0.010(7) C13 0.033(16) 0.041(11) 0.056(11) -0.019(9) -0.003(9) -0.007(10) N12 0.045(16) 0.047(10) 0.060(10) -0.025(8) 0.003(8) -0.017(11) N11 0.046(17) 0.032(9) 0.081(12) -0.029(9) -0.001(9) -0.010(10) C15 0.000(11) 0.035(10) 0.064(11) -0.006(8) -0.004(7) 0.008(7) N21 0.022(10) 0.029(7) 0.026(6) -0.005(5) -0.001(5) -0.010(6) C22 0.026(13) 0.039(10) 0.031(8) -0.001(7) -0.001(6) -0.010(9) C23 0.057(18) 0.049(12) 0.033(9) 0.001(8) -0.017(9) -0.016(11) C24 0.039(15) 0.056(12) 0.027(8) -0.006(8) 0.001(7) -0.010(11) C25 0.043(17) 0.065(14) 0.033(9) -0.018(9) -0.001(8) -0.023(12) C26 0.024(13) 0.052(12) 0.031(8) -0.013(7) -0.005(6) -0.011(9) N34 0.045(14) 0.033(8) 0.043(8) -0.017(7) -0.005(7) -0.013(8) C33 0.021(13) 0.037(10) 0.052(10) -0.007(8) -0.011(7) -0.011(9) N32 0.038(13) 0.025(8) 0.052(9) 0.000(7) -0.001(7) -0.006(8) N31 0.032(15) 0.024(8) 0.086(13) -0.016(8) -0.013(9) -0.005(8) C35 0.013(13) 0.040(10) 0.059(11) -0.020(9) 0.000(7) -0.008(9) O100 0.047(12) 0.043(8) 0.045(7) 0.008(6) -0.011(6) -0.010(7) O200 0.063(15) 0.052(10) 0.073(10) 0.017(8) 0.010(9) -0.025(10) O300 0.028(10) 0.058(9) 0.046(7) -0.006(6) 0.005(5) -0.026(8) O400 0.026(11) 0.074(11) 0.051(7) -0.010(7) -0.005(6) -0.022(9) O500 0.045(14) 0.068(11) 0.074(10) -0.029(8) -0.021(8) -0.019(9) O51 0.063(18) 0.056(10) 0.064(10) -0.013(8) 0.007(9) -0.013(10) N53 0.11(4) 0.12(2) 0.046(12) -0.028(12) -0.018(13) -0.06(3) O52 0.10(3) 0.111(19) 0.060(11) -0.017(11) -0.014(11) -0.038(18) O54 0.08(3) 0.20(4) 0.090(16) -0.089(18) 0.021(14) -0.03(3) N43 0.043(19) 0.064(13) 0.063(12) -0.002(10) -0.004(10) -0.016(12) O42 0.07(2) 0.15(2) 0.053(10) 0.026(12) 0.010(10) -0.028(18) O41 0.07(2) 0.12(2) 0.074(11) 0.022(13) -0.032(11) -0.051(17) O44 0.034(14) 0.096(15) 0.061(9) 0.009(9) -0.004(7) -0.027(11) O700 0.047(17) 0.126(19) 0.068(11) -0.025(11) -0.012(8) -0.019(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O100 2.563(15) . ? La1 O500 2.573(17) . ? La1 O200 2.584(15) . ? La1 O400 2.586(17) . ? La1 O51 2.60(2) . ? La1 O300 2.641(15) . ? La1 N14 2.713(18) . ? La1 N34 2.724(17) . ? La1 O52 2.72(2) . ? La1 N21 2.774(12) . ? N14 C15 1.33(3) . ? N14 C13 1.38(3) . ? C13 N12 1.34(3) . ? C13 C26 1.44(3) . ? N12 N11 1.36(3) . ? N11 C15 1.39(3) . ? C15 C100 1.51(4) . ? C15 C101 1.57(3) . ? N21 C26 1.35(3) . ? N21 C22 1.35(2) . ? C22 C23 1.41(2) . ? C22 C33 1.48(3) . ? C23 C24 1.43(3) . ? C24 C25 1.38(3) . ? C25 C26 1.41(2) . ? N34 C33 1.34(2) . ? N34 C35 1.36(3) . ? C33 N32 1.31(3) . ? N32 N31 1.31(3) . ? N31 C35 1.31(3) . ? C35 C300 1.44(3) . ? C35 C301 1.55(4) . ? O51 N53 1.26(3) . ? N53 O54 1.16(4) . ? N53 O52 1.35(5) . ? N43 O41 1.19(4) . ? N43 O44 1.25(3) . ? N43 O42 1.27(3) . ? N63 O61 1.174(17) . ? N63 O62 1.196(17) . ? N63 O62 1.224(17) 2_556 ? O71 N73 1.209(18) 2_646 ? O71 N73 1.214(18) . ? N73 O72 1.190(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 La1 O500 78.9(6) . . ? O100 La1 O200 73.5(6) . . ? O500 La1 O200 129.7(6) . . ? O100 La1 O400 140.0(5) . . ? O500 La1 O400 136.1(6) . . ? O200 La1 O400 68.3(6) . . ? O100 La1 O51 113.9(6) . . ? O500 La1 O51 79.3(7) . . ? O200 La1 O51 74.9(6) . . ? O400 La1 O51 67.2(7) . . ? O100 La1 O300 66.4(5) . . ? O500 La1 O300 66.8(6) . . ? O200 La1 O300 132.1(6) . . ? O400 La1 O300 136.5(5) . . ? O51 La1 O300 145.6(6) . . ? O100 La1 N14 75.8(5) . . ? O500 La1 N14 139.8(7) . . ? O200 La1 N14 71.1(6) . . ? O400 La1 N14 80.9(6) . . ? O51 La1 N14 139.9(7) . . ? O300 La1 N14 74.5(5) . . ? O100 La1 N34 144.7(6) . . ? O500 La1 N34 68.3(6) . . ? O200 La1 N34 138.5(7) . . ? O400 La1 N34 75.3(6) . . ? O51 La1 N34 73.1(5) . . ? O300 La1 N34 88.4(6) . . ? N14 La1 N34 122.4(4) . . ? O100 La1 O52 66.0(8) . . ? O500 La1 O52 63.1(7) . . ? O200 La1 O52 67.5(8) . . ? O400 La1 O52 108.1(8) . . ? O51 La1 O52 48.4(9) . . ? O300 La1 O52 115.3(8) . . ? N14 La1 O52 129.6(7) . . ? N34 La1 O52 107.6(7) . . ? O100 La1 N21 124.6(5) . . ? O500 La1 N21 111.4(5) . . ? O200 La1 N21 118.8(6) . . ? O400 La1 N21 67.9(5) . . ? O51 La1 N21 121.5(5) . . ? O300 La1 N21 68.9(5) . . ? N14 La1 N21 61.8(4) . . ? N34 La1 N21 60.7(5) . . ? O52 La1 N21 168.1(7) . . ? C15 N14 C13 103.7(18) . . ? C15 N14 La1 139.0(13) . . ? C13 N14 La1 117.3(13) . . ? N12 C13 N14 112.9(18) . . ? N12 C13 C26 123.2(19) . . ? N14 C13 C26 124(2) . . ? C13 N12 N11 104.8(17) . . ? N12 N11 C15 107.9(17) . . ? N14 C15 C100 124(2) . . ? N14 C15 N11 110.6(16) . . ? C100 C15 N11 126(2) . . ? N14 C15 C101 106(2) . . ? C100 C15 C101 54(2) . . ? N11 C15 C101 112.2(19) . . ? C26 N21 C22 118.8(14) . . ? C26 N21 La1 120.2(10) . . ? C22 N21 La1 120.9(12) . . ? N21 C22 C23 124(2) . . ? N21 C22 C33 116.4(15) . . ? C23 C22 C33 119.6(17) . . ? C22 C23 C24 115.6(18) . . ? C25 C24 C23 120.9(16) . . ? C24 C25 C26 119(2) . . ? N21 C26 C25 122.2(19) . . ? N21 C26 C13 116.6(15) . . ? C25 C26 C13 121(2) . . ? C33 N34 C35 102.3(16) . . ? C33 N34 La1 120.3(14) . . ? C35 N34 La1 137.4(12) . . ? N32 C33 N34 116(2) . . ? N32 C33 C22 122.9(18) . . ? N34 C33 C22 121.6(17) . . ? C33 N32 N31 101.4(16) . . ? N32 N31 C35 113.8(17) . . ? N31 C35 N34 107.0(17) . . ? N31 C35 C300 125(2) . . ? N34 C35 C300 112.4(18) . . ? N31 C35 C301 127(2) . . ? N34 C35 C301 126(2) . . ? C300 C35 C301 37.3(18) . . ? N53 O51 La1 103(2) . . ? O54 N53 O51 128(4) . . ? O54 N53 O52 118(3) . . ? O51 N53 O52 114(3) . . ? N53 O52 La1 94.6(14) . . ? O41 N43 O44 120(2) . . ? O41 N43 O42 121(3) . . ? O44 N43 O42 119(3) . . ? O61 N63 O62 122(2) . . ? O61 N63 O62 124(2) . 2_556 ? O62 N63 O62 113.7(18) . 2_556 ? O72 N73 O71 119(2) . 2_646 ? O72 N73 O71 120(2) . . ? O71 N73 O71 113(2) 2_646 . ? _refine_diff_density_max 2.742 _refine_diff_density_min -1.548 _refine_diff_density_rms 0.275 _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-Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 2-Tb _chemical_formula_sum 'C13 H20 N11 O12 Tb' _chemical_formula_weight 681.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' _cell_length_a 9.354(12) _cell_length_b 29.40(3) _cell_length_c 9.836(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.516(10) _cell_angle_gamma 90.00 _cell_volume 2499(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.908 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean ? _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 1132 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.89 _reflns_number_total 1132 _reflns_number_gt 1093 _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^)+(0.0894P)^2^+48.5199P] 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 0.0012(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1132 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Tb1 Tb 0.5000 0.36492(2) 0.7500 0.0364(8) Uani 1 d S . . O32 O 0.4487(16) 0.3318(4) 0.5026(13) 0.062(5) Uani 1 d . . . N33 N 0.358(3) 0.3625(4) 0.4299(19) 0.082(8) Uani 1 d . . . O34 O 0.344(2) 0.3934(3) 0.5086(12) 0.112(7) Uani 1 d . . . O31 O 0.295(3) 0.3629(5) 0.2963(16) 0.153(11) Uani 1 d . . . N14 N 0.3129(18) 0.4036(3) 0.8489(13) 0.039(5) Uani 1 d . . . C15 C 0.210(3) 0.3914(4) 0.9060(17) 0.069(8) Uani 1 d . . . N11 N 0.145(2) 0.4288(4) 0.9350(14) 0.062(5) Uani 1 d . . . H11 H 0.0765 0.4290 0.9740 0.074 Uiso 1 calc R . . N12 N 0.2004(19) 0.4655(4) 0.8946(14) 0.058(5) Uani 1 d . . . C13 C 0.299(2) 0.4495(4) 0.8441(15) 0.046(6) Uani 1 d . . . N21 N 0.5000 0.4535(4) 0.7500 0.040(6) Uani 1 d S . . C22 C 0.400(2) 0.4770(4) 0.7918(15) 0.033(5) Uani 1 d . . . C23 C 0.606(3) 0.5248(4) 0.7077(17) 0.065(7) Uani 1 d . . . H23 H 0.6779 0.5401 0.6803 0.078 Uiso 1 calc R . . C24 C 0.5000 0.5482(5) 0.7500 0.047(9) Uani 1 d S . . H24 H 0.5000 0.5798 0.7500 0.057 Uiso 1 calc SR . . C100 C 0.167(3) 0.3449(5) 0.942(2) 0.080(8) Uani 1 d . . . H10A H 0.0939 0.3312 0.8539 0.095 Uiso 1 calc R . . H10B H 0.1214 0.3475 1.0137 0.095 Uiso 1 calc R . . H10C H 0.2580 0.3263 0.9801 0.095 Uiso 1 calc R . . O200 O 0.301(5) 0.3089(9) 0.700(3) 0.063(8) Uiso 0.50 d P A 1 N23 N 0.250(6) 0.2976(11) 0.664(4) 0.057(8) Uiso 0.50 d P A 2 O21 O 0.368(4) 0.2886(7) 0.749(3) 0.058(6) Uiso 0.50 d P A 2 O22 O 0.220(3) 0.3376(6) 0.621(2) 0.058(5) Uiso 0.50 d P A 2 O24 O 0.136(3) 0.2696(6) 0.629(2) 0.064(5) Uiso 0.50 d P A 2 C102 C -0.126(6) 0.2448(13) 0.219(5) 0.091(12) Uiso 0.50 d P . . H10D H -0.0963 0.2135 0.2197 0.109 Uiso 0.50 calc PR . . H10E H -0.1393 0.2584 0.1265 0.109 Uiso 0.50 calc PR . . H10F H -0.2214 0.2465 0.2342 0.109 Uiso 0.50 calc PR . . C101 C -0.013(7) 0.2675(13) 0.330(5) 0.084(11) Uiso 0.50 d P . . N100 N 0.076(6) 0.2864(15) 0.421(5) 0.125(14) Uiso 0.50 d P . . O100 O 0.061(2) 0.4465(5) 0.4332(18) 0.107(5) 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 Tb1 0.041(2) 0.0336(4) 0.0357(8) 0.000 0.0161(11) 0.000 O32 0.048(16) 0.078(7) 0.059(8) -0.029(6) 0.018(10) -0.018(7) N33 0.12(3) 0.065(8) 0.058(13) -0.002(7) 0.036(16) -0.040(10) O34 0.19(2) 0.051(5) 0.050(8) -0.002(5) -0.004(11) 0.019(8) O31 0.26(3) 0.141(12) 0.021(8) -0.005(6) 0.015(14) -0.104(14) N14 0.023(16) 0.047(5) 0.045(8) -0.002(5) 0.011(10) -0.001(6) C15 0.12(3) 0.055(7) 0.055(10) 0.003(6) 0.065(15) -0.005(9) N11 0.056(19) 0.071(7) 0.052(9) 0.000(6) 0.015(12) 0.004(8) N12 0.069(18) 0.060(6) 0.054(8) -0.003(5) 0.032(11) 0.014(7) C13 0.05(2) 0.047(6) 0.033(8) 0.001(5) 0.010(12) 0.017(8) N21 0.04(2) 0.031(6) 0.050(10) 0.000 0.023(13) 0.000 C22 0.011(18) 0.044(5) 0.037(9) -0.002(5) 0.000(11) 0.008(7) C23 0.09(2) 0.039(6) 0.066(11) -0.002(6) 0.033(14) -0.017(8) C24 0.04(3) 0.038(8) 0.053(14) 0.000 0.003(18) 0.000 C100 0.09(3) 0.068(9) 0.076(14) 0.012(8) 0.033(17) -0.016(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O200 2.39(3) 6_657 ? Tb1 O200 2.39(3) . ? Tb1 O34 2.412(12) . ? Tb1 O34 2.412(12) 6_657 ? Tb1 O32 2.491(10) . ? Tb1 O32 2.491(10) 6_657 ? Tb1 O21 2.56(2) 6_657 ? Tb1 O21 2.56(2) . ? Tb1 O22 2.57(3) 6_657 ? Tb1 O22 2.57(3) . ? Tb1 N14 2.571(12) . ? Tb1 N14 2.571(12) 6_657 ? Tb1 N21 2.605(11) . ? O32 N33 1.26(2) . ? N33 O31 1.22(2) . ? N33 O34 1.235(18) . ? N14 C15 1.335(19) . ? N14 C13 1.355(14) . ? C15 N11 1.343(18) . ? C15 C100 1.504(19) . ? N11 N12 1.325(17) . ? N12 C13 1.296(18) . ? C13 C22 1.47(2) . ? N21 C22 1.350(14) 6_657 ? N21 C22 1.350(14) . ? C22 C23 1.406(15) 6_657 ? C23 C24 1.397(19) . ? C23 C22 1.406(15) 6_657 ? C24 C23 1.397(19) 6_657 ? N23 O21 1.13(5) . ? N23 O22 1.24(4) . ? N23 O24 1.28(4) . ? C102 C101 1.36(6) . ? C101 N100 1.11(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O200 Tb1 O200 92.9(17) 6_657 . ? O200 Tb1 O34 125.0(8) 6_657 . ? O200 Tb1 O34 84.5(9) . . ? O200 Tb1 O34 84.5(9) 6_657 6_657 ? O200 Tb1 O34 125.0(8) . 6_657 ? O34 Tb1 O34 139.4(5) . 6_657 ? O200 Tb1 O32 77.1(8) 6_657 . ? O200 Tb1 O32 71.6(7) . . ? O34 Tb1 O32 49.9(4) . . ? O34 Tb1 O32 156.1(6) 6_657 . ? O200 Tb1 O32 71.6(7) 6_657 6_657 ? O200 Tb1 O32 77.1(8) . 6_657 ? O34 Tb1 O32 156.1(6) . 6_657 ? O34 Tb1 O32 49.9(4) 6_657 6_657 ? O32 Tb1 O32 134.0(6) . 6_657 ? O200 Tb1 O21 19.8(12) 6_657 6_657 ? O200 Tb1 O21 74.5(10) . 6_657 ? O34 Tb1 O21 114.7(7) . 6_657 ? O34 Tb1 O21 101.0(8) 6_657 6_657 ? O32 Tb1 O21 64.8(7) . 6_657 ? O32 Tb1 O21 75.1(6) 6_657 6_657 ? O200 Tb1 O21 74.5(10) 6_657 . ? O200 Tb1 O21 19.8(12) . . ? O34 Tb1 O21 101.0(8) . . ? O34 Tb1 O21 114.7(7) 6_657 . ? O32 Tb1 O21 75.1(6) . . ? O32 Tb1 O21 64.8(7) 6_657 . ? O21 Tb1 O21 57.6(13) 6_657 . ? O200 Tb1 O22 27.7(9) 6_657 6_657 ? O200 Tb1 O22 116.9(11) . 6_657 ? O34 Tb1 O22 135.8(6) . 6_657 ? O34 Tb1 O22 60.1(6) 6_657 6_657 ? O32 Tb1 O22 98.1(5) . 6_657 ? O32 Tb1 O22 67.4(5) 6_657 6_657 ? O21 Tb1 O22 47.4(9) 6_657 6_657 ? O21 Tb1 O22 97.3(9) . 6_657 ? O200 Tb1 O22 116.9(11) 6_657 . ? O200 Tb1 O22 27.7(9) . . ? O34 Tb1 O22 60.1(6) . . ? O34 Tb1 O22 135.8(6) 6_657 . ? O32 Tb1 O22 67.4(5) . . ? O32 Tb1 O22 98.1(5) 6_657 . ? O21 Tb1 O22 97.3(9) 6_657 . ? O21 Tb1 O22 47.4(9) . . ? O22 Tb1 O22 143.5(9) 6_657 . ? O200 Tb1 N14 144.6(6) 6_657 . ? O200 Tb1 N14 78.2(7) . . ? O34 Tb1 N14 88.5(5) . . ? O34 Tb1 N14 73.6(6) 6_657 . ? O32 Tb1 N14 129.7(5) . . ? O32 Tb1 N14 73.0(4) 6_657 . ? O21 Tb1 N14 141.7(5) 6_657 . ? O21 Tb1 N14 89.5(6) . . ? O22 Tb1 N14 131.7(5) 6_657 . ? O22 Tb1 N14 67.2(5) . . ? O200 Tb1 N14 78.2(7) 6_657 6_657 ? O200 Tb1 N14 144.6(6) . 6_657 ? O34 Tb1 N14 73.6(6) . 6_657 ? O34 Tb1 N14 88.5(5) 6_657 6_657 ? O32 Tb1 N14 73.0(4) . 6_657 ? O32 Tb1 N14 129.7(5) 6_657 6_657 ? O21 Tb1 N14 89.5(6) 6_657 6_657 ? O21 Tb1 N14 141.7(5) . 6_657 ? O22 Tb1 N14 67.2(5) 6_657 6_657 ? O22 Tb1 N14 131.7(5) . 6_657 ? N14 Tb1 N14 127.5(4) . 6_657 ? O200 Tb1 N21 133.6(8) 6_657 . ? O200 Tb1 N21 133.6(8) . . ? O34 Tb1 N21 69.7(3) . . ? O34 Tb1 N21 69.7(3) 6_657 . ? O32 Tb1 N21 113.0(3) . . ? O32 Tb1 N21 113.0(3) 6_657 . ? O21 Tb1 N21 151.2(6) 6_657 . ? O21 Tb1 N21 151.2(6) . . ? O22 Tb1 N21 108.3(4) 6_657 . ? O22 Tb1 N21 108.3(4) . . ? N14 Tb1 N21 63.7(2) . . ? N14 Tb1 N21 63.7(2) 6_657 . ? N33 O32 Tb1 96.4(9) . . ? O31 N33 O34 123(2) . . ? O31 N33 O32 124.4(18) . . ? O34 N33 O32 112.5(16) . . ? N33 O34 Tb1 101.0(12) . . ? C15 N14 C13 102.1(12) . . ? C15 N14 Tb1 138.1(8) . . ? C13 N14 Tb1 119.7(9) . . ? N14 C15 N11 109.2(12) . . ? N14 C15 C100 130.1(15) . . ? N11 C15 C100 120.7(16) . . ? N12 N11 C15 109.9(14) . . ? C13 N12 N11 103.9(11) . . ? N12 C13 N14 114.8(13) . . ? N12 C13 C22 125.4(10) . . ? N14 C13 C22 119.7(12) . . ? C22 N21 C22 118.4(13) 6_657 . ? C22 N21 Tb1 120.8(7) 6_657 . ? C22 N21 Tb1 120.8(7) . . ? N21 C22 C23 123.1(15) . 6_657 ? N21 C22 C13 115.8(9) . . ? C23 C22 C13 121.0(14) 6_657 . ? C24 C23 C22 117.3(16) . 6_657 ? C23 C24 C23 120.9(15) 6_657 . ? O21 N23 O22 120(4) . . ? O21 N23 O24 121(4) . . ? O22 N23 O24 118(5) . . ? N23 O21 Tb1 98(2) . . ? N23 O22 Tb1 94(3) . . ? N100 C101 C102 178(6) . . ? _refine_diff_density_max 0.763 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.147 _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 2-Sm _chemical_formula_sum 'C13 H20 N11 O12 Sm' _chemical_formula_weight 672.75 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 monoclinic _symmetry_space_group_name_H-M I2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' _cell_length_a 9.353(12) _cell_length_b 29.59(3) _cell_length_c 9.889(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.946(10) _cell_angle_gamma 90.00 _cell_volume 2521(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.407 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2524 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.02 _reflns_number_total 1475 _reflns_number_gt 1259 _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^)+(0.0894P)^2^+48.5199P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1475 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1993 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _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 Sm1 Sm 0.5000 0.36457(3) 0.7500 0.0513(6) Uani 1 d S . . O32 O 0.4484(17) 0.3314(5) 0.4993(15) 0.085(4) Uani 1 d . . . N33 N 0.353(3) 0.3623(6) 0.425(2) 0.107(7) Uani 1 d . . . O34 O 0.338(2) 0.3934(4) 0.5031(15) 0.130(7) Uani 1 d . . . O31 O 0.298(3) 0.3623(6) 0.2912(18) 0.182(12) Uani 1 d . . . N14 N 0.3120(16) 0.4045(4) 0.8462(14) 0.057(3) Uani 1 d . . . C15 C 0.213(2) 0.3928(5) 0.9100(18) 0.058(4) Uani 1 d . . . N11 N 0.1422(19) 0.4295(5) 0.9319(17) 0.073(4) Uani 1 d . . . H11 H 0.0694 0.4294 0.9646 0.088 Uiso 1 calc R . . N12 N 0.2009(17) 0.4669(5) 0.8955(16) 0.067(4) Uani 1 d . . . C13 C 0.300(2) 0.4507(4) 0.8430(18) 0.060(5) Uani 1 d . . . N21 N 0.5000 0.4551(5) 0.7500 0.055(5) Uani 1 d S . . C22 C 0.4018(19) 0.4774(4) 0.7930(16) 0.050(4) Uani 1 d . . . C23 C 0.400(2) 0.5248(5) 0.796(2) 0.077(6) Uani 1 d . . . H23 H 0.3324 0.5401 0.8285 0.093 Uiso 1 calc R . . C24 C 0.5000 0.5483(7) 0.7500 0.070(7) Uani 1 d S . . H24 H 0.5000 0.5798 0.7500 0.084 Uiso 1 calc SR . . C100 C 0.173(2) 0.3454(6) 0.942(2) 0.077(5) Uani 1 d . . . H10A H 0.1037 0.3316 0.8529 0.092 Uiso 1 calc R . . H10B H 0.1244 0.3467 1.0113 0.092 Uiso 1 calc R . . H10C H 0.2666 0.3278 0.9828 0.092 Uiso 1 calc R . . O200 O 0.303(5) 0.3071(11) 0.705(4) 0.087(11) Uiso 0.50 d P A 1 N23 N 0.246(5) 0.2991(12) 0.665(4) 0.069(10) Uiso 0.50 d P A 2 O21 O 0.375(3) 0.2869(9) 0.753(3) 0.079(7) Uiso 0.50 d P A 2 O22 O 0.217(3) 0.3361(8) 0.620(3) 0.078(7) Uiso 0.50 d P A 2 O24 O 0.144(4) 0.2694(8) 0.629(3) 0.086(7) Uiso 0.50 d P A 2 C102 C -0.145(6) 0.2441(17) 0.215(6) 0.120(16) Uiso 0.50 d P . . H10D H -0.1130 0.2141 0.2023 0.144 Uiso 0.50 calc PR . . H10E H -0.1730 0.2605 0.1244 0.144 Uiso 0.50 calc PR . . H10F H -0.2331 0.2424 0.2417 0.144 Uiso 0.50 calc PR . . C101 C -0.018(6) 0.2671(12) 0.330(5) 0.081(10) Uiso 0.50 d P . . N100 N 0.060(7) 0.2849(18) 0.422(6) 0.156(19) Uiso 0.50 d P . . O100 O 0.058(2) 0.4461(6) 0.432(2) 0.125(6) 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 Sm1 0.0529(11) 0.0471(6) 0.0566(9) 0.000 0.0243(8) 0.000 O32 0.084(11) 0.097(9) 0.078(9) -0.037(7) 0.037(9) -0.025(8) N33 0.17(2) 0.082(11) 0.080(15) 0.005(10) 0.056(16) -0.033(12) O34 0.189(19) 0.064(7) 0.065(9) -0.003(6) -0.029(12) 0.016(9) O31 0.28(3) 0.173(17) 0.044(10) 0.010(9) 0.015(15) -0.105(18) N14 0.050(10) 0.064(7) 0.060(9) 0.005(6) 0.024(8) 0.005(6) C15 0.048(13) 0.075(10) 0.058(11) 0.005(7) 0.027(10) 0.008(8) N11 0.061(11) 0.090(10) 0.078(11) 0.005(7) 0.037(9) 0.003(8) N12 0.050(11) 0.086(9) 0.060(10) 0.002(7) 0.015(9) 0.021(7) C13 0.075(14) 0.055(8) 0.056(10) 0.002(6) 0.032(10) 0.009(8) N21 0.058(14) 0.043(8) 0.061(12) 0.000 0.021(11) 0.000 C22 0.054(12) 0.049(7) 0.052(10) 0.000(5) 0.027(9) 0.012(7) C23 0.107(18) 0.053(8) 0.092(14) 0.014(8) 0.060(14) 0.019(9) C24 0.08(2) 0.045(10) 0.076(17) 0.000 0.018(17) 0.000 C100 0.067(15) 0.095(12) 0.066(13) 0.012(9) 0.023(12) -0.011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O200 2.42(4) . ? Sm1 O200 2.42(3) 6_657 ? Sm1 O34 2.470(13) 6_657 ? Sm1 O34 2.470(13) . ? Sm1 O32 2.532(12) 6_657 ? Sm1 O32 2.533(12) . ? Sm1 O21 2.58(3) 6_657 ? Sm1 O21 2.58(3) . ? Sm1 N14 2.588(13) . ? Sm1 N14 2.588(13) 6_657 ? Sm1 O22 2.59(3) . ? Sm1 O22 2.59(3) 6_657 ? Sm1 N21 2.680(15) . ? O32 N33 1.29(2) . ? N33 O31 1.22(2) . ? N33 O34 1.24(2) . ? N14 C15 1.35(2) . ? N14 C13 1.373(17) . ? C15 N11 1.33(2) . ? C15 C100 1.52(2) . ? N11 N12 1.34(2) . ? N12 C13 1.32(2) . ? C13 C22 1.46(2) . ? N21 C22 1.327(15) 6_657 ? N21 C22 1.327(15) . ? C22 C23 1.404(19) . ? C23 C24 1.38(2) . ? C24 C23 1.38(2) 6_657 ? N23 O22 1.18(4) . ? N23 O21 1.23(5) . ? N23 O24 1.25(4) . ? C102 C101 1.45(6) . ? C101 N100 1.06(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O200 Sm1 O23 90.8(18) . 6_657 ? O200 Sm1 O34 123.6(10) . 6_657 ? O200 Sm1 O34 86.1(10) 6_657 6_657 ? O200 Sm1 O34 86.1(10) . . ? O200 Sm1 O34 123.6(10) 6_657 . ? O34 Sm1 O34 139.5(6) 6_657 . ? O200 Sm1 O32 75.3(10) . 6_657 ? O200 Sm1 O32 73.0(9) 6_657 6_657 ? O34 Sm1 O32 50.0(5) 6_657 6_657 ? O34 Sm1 O32 155.6(7) . 6_657 ? O200 Sm1 O32 73.0(9) . . ? O200 Sm1 O32 75.3(10) 6_657 . ? O34 Sm1 O32 155.6(7) 6_657 . ? O34 Sm1 O32 50.0(5) . . ? O32 Sm1 O32 134.3(7) 6_657 . ? O200 Sm1 O21 71.9(12) . 6_657 ? O200 Sm1 O21 20.2(9) 6_657 6_657 ? O34 Sm1 O21 102.3(8) 6_657 6_657 ? O34 Sm1 O21 113.7(7) . 6_657 ? O32 Sm1 O21 75.7(7) 6_657 6_657 ? O32 Sm1 O21 63.7(7) . 6_657 ? O200 Sm1 O21 20.2(9) . . ? O200 Sm1 O21 71.9(12) 6_657 . ? O34 Sm1 O21 113.7(7) 6_657 . ? O34 Sm1 O21 102.3(8) . . ? O32 Sm1 O21 63.7(7) 6_657 . ? O32 Sm1 O21 75.7(7) . . ? O21 Sm1 O21 54.4(13) 6_657 . ? O200 Sm1 N14 78.9(9) . . ? O200 Sm1 N14 146.4(9) 6_657 . ? O34 Sm1 N14 73.9(6) 6_657 . ? O34 Sm1 N14 87.8(6) . . ? O32 Sm1 N14 73.4(4) 6_657 . ? O32 Sm1 N14 129.8(5) . . ? O21 Sm1 N14 141.8(6) 6_657 . ? O21 Sm1 N14 91.5(7) . . ? O200 Sm1 N14 146.4(9) . 6_657 ? O200 Sm1 N14 78.9(9) 6_657 6_657 ? O34 Sm1 N14 87.8(6) 6_657 6_657 ? O34 Sm1 N14 73.9(6) . 6_657 ? O32 Sm1 N14 129.8(5) 6_657 6_657 ? O32 Sm1 N14 73.4(4) . 6_657 ? O21 Sm1 N14 91.5(7) 6_657 6_657 ? O21 Sm1 N14 141.8(6) . 6_657 ? N14 Sm1 N14 125.7(5) . 6_657 ? O200 Sm1 O22 28.6(10) . . ? O200 Sm1 O22 114.9(11) 6_657 . ? O34 Sm1 O22 135.9(8) 6_657 . ? O34 Sm1 O22 60.4(7) . . ? O32 Sm1 O22 97.4(6) 6_657 . ? O32 Sm1 O22 67.6(6) . . ? O21 Sm1 O22 94.8(9) 6_657 . ? O21 Sm1 O22 48.6(8) . . ? N14 Sm1 O22 67.8(6) . . ? N14 Sm1 O22 132.4(6) 6_657 . ? O200 Sm1 O22 114.9(11) . 6_657 ? O200 Sm1 O22 28.6(10) 6_657 6_657 ? O34 Sm1 O22 60.4(7) 6_657 6_657 ? O34 Sm1 O22 135.9(8) . 6_657 ? O32 Sm1 O22 67.6(6) 6_657 6_657 ? O32 Sm1 O22 97.4(6) . 6_657 ? O21 Sm1 O22 48.6(8) 6_657 6_657 ? O21 Sm1 O22 94.8(9) . 6_657 ? N14 Sm1 O22 132.4(6) . 6_657 ? N14 Sm1 O22 67.8(6) 6_657 6_657 ? O22 Sm1 O22 142.1(11) . 6_657 ? O200 Sm1 N21 134.6(9) . . ? O200 Sm1 N21 134.6(9) 6_657 . ? O34 Sm1 N21 69.8(3) 6_657 . ? O34 Sm1 N21 69.8(3) . . ? O32 Sm1 N21 112.8(4) 6_657 . ? O32 Sm1 N21 112.8(4) . . ? O21 Sm1 N21 152.8(6) 6_657 . ? O21 Sm1 N21 152.8(6) . . ? N14 Sm1 N21 62.9(3) . . ? N14 Sm1 N21 62.9(3) 6_657 . ? O22 Sm1 N21 109.0(5) . . ? O22 Sm1 N21 109.0(5) 6_657 . ? N33 O32 Sm1 96.0(11) . . ? O31 N33 O34 125(2) . . ? O31 N33 O32 121(2) . . ? O34 N33 O32 113.5(19) . . ? N33 O34 Sm1 100.3(13) . . ? C15 N14 C13 101.7(13) . . ? C15 N14 Sm1 137.9(10) . . ? C13 N14 Sm1 120.4(10) . . ? N11 C15 N14 109.9(14) . . ? N11 C15 C100 123.0(16) . . ? N14 C15 C100 126.9(15) . . ? C15 N11 N12 110.3(15) . . ? C13 N12 N11 103.4(13) . . ? N12 C13 N14 114.5(14) . . ? N12 C13 C22 126.1(13) . . ? N14 C13 C22 119.3(14) . . ? C22 N21 C22 120.6(16) 6_657 . ? C22 N21 Sm1 119.7(8) 6_657 . ? C22 N21 Sm1 119.7(8) . . ? N21 C22 C23 121.2(14) . . ? N21 C22 C13 117.6(12) . . ? C23 C22 C13 121.1(13) . . ? C24 C23 C22 118.8(16) . . ? C23 C24 C23 119(2) 6_657 . ? O22 N23 O21 124(4) . . ? O22 N23 O24 121(4) . . ? O21 N23 O24 115(3) . . ? N23 O21 Sm1 93(2) . . ? N23 O22 Sm1 94(3) . . ? N100 C101 C102 170(6) . . ? _refine_diff_density_max 0.754 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.154 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_2-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 2-Nd _chemical_formula_sum 'C13 H20 N11 Nd O12' _chemical_formula_weight 666.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' _cell_length_a 9.326(9) _cell_length_b 29.71(3) _cell_length_c 9.895(11) _cell_angle_alpha 90.00 _cell_angle_beta 113.030(10) _cell_angle_gamma 90.00 _cell_volume 2523(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 2.135 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2525 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.90 _reflns_number_total 1450 _reflns_number_gt 1314 _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^)+(0.0894P)^2^+48.5199P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1450 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1650 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.5000 0.36446(2) 0.7500 0.0387(5) Uani 1 d S . . O32 O 0.4458(15) 0.3322(4) 0.4939(13) 0.084(4) Uani 1 d . . . N33 N 0.352(2) 0.3630(4) 0.4264(15) 0.092(6) Uani 1 d . . . O34 O 0.3332(19) 0.3923(3) 0.5004(11) 0.120(6) Uani 1 d . . . O31 O 0.293(3) 0.3630(5) 0.2927(13) 0.191(11) Uani 1 d . . . N14 N 0.3082(14) 0.4057(3) 0.8453(10) 0.046(3) Uani 1 d . . . C15 C 0.2122(18) 0.3939(4) 0.9079(14) 0.055(4) Uani 1 d . . . N11 N 0.1449(15) 0.4314(4) 0.9326(12) 0.060(3) Uani 1 d . . . H11 H 0.0739 0.4319 0.9678 0.072 Uiso 1 calc R . . N12 N 0.2033(15) 0.4671(4) 0.8953(13) 0.061(3) Uani 1 d . . . C13 C 0.3042(17) 0.4509(4) 0.8449(12) 0.045(3) Uani 1 d . . . N21 N 0.5000 0.4553(4) 0.7500 0.043(4) Uani 1 d S . . C22 C 0.3989(16) 0.4775(4) 0.7919(12) 0.046(4) Uani 1 d . . . C23 C 0.6009(19) 0.5251(4) 0.7051(15) 0.063(4) Uani 1 d . . . H23 H 0.6686 0.5405 0.6729 0.076 Uiso 1 calc R . . C24 C 0.5000 0.5485(6) 0.7500 0.069(7) Uani 1 d S . . H24 H 0.5000 0.5798 0.7500 0.082 Uiso 1 calc SR . . C100 C 0.170(2) 0.3475(5) 0.9427(16) 0.074(5) Uani 1 d . . . H10A H 0.1050 0.3327 0.8532 0.088 Uiso 1 calc R . . H10B H 0.1137 0.3501 1.0058 0.088 Uiso 1 calc R . . H10C H 0.2627 0.3303 0.9910 0.088 Uiso 1 calc R . . O200 O 0.293(3) 0.3082(8) 0.696(3) 0.071(7) Uiso 0.50 d P A 1 N23 N 0.252(4) 0.2964(10) 0.667(3) 0.066(8) Uiso 0.50 d P A 2 O21 O 0.373(3) 0.2879(6) 0.752(2) 0.063(5) Uiso 0.50 d P A 2 O22 O 0.215(2) 0.3366(6) 0.616(2) 0.063(5) Uiso 0.50 d P A 2 O24 O 0.129(3) 0.2687(6) 0.625(2) 0.076(5) Uiso 0.50 d P A 2 C102 C -0.142(4) 0.2428(11) 0.212(4) 0.088(10) Uiso 0.50 d P . . H10D H -0.1008 0.2133 0.2099 0.106 Uiso 0.50 calc PR . . H10E H -0.1629 0.2578 0.1206 0.106 Uiso 0.50 calc PR . . H10F H -0.2366 0.2402 0.2285 0.106 Uiso 0.50 calc PR . . C101 C -0.027(5) 0.2690(13) 0.332(4) 0.097(11) Uiso 0.50 d P . . N100 N 0.073(5) 0.2860(14) 0.432(5) 0.135(14) Uiso 0.50 d P . . O100 O 0.0563(19) 0.4470(5) 0.4332(18) 0.124(5) 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 Nd1 0.0395(9) 0.0376(5) 0.0393(6) 0.000 0.0156(5) 0.000 O32 0.080(10) 0.092(7) 0.079(8) -0.041(6) 0.029(7) -0.029(7) N33 0.139(18) 0.074(8) 0.051(8) -0.003(6) 0.024(9) -0.037(9) O34 0.175(15) 0.060(6) 0.057(7) -0.004(5) -0.028(7) 0.013(7) O31 0.34(3) 0.160(14) 0.027(7) -0.001(6) 0.019(10) -0.108(15) N14 0.054(8) 0.054(5) 0.042(5) 0.004(4) 0.031(6) 0.000(5) C15 0.055(11) 0.073(8) 0.040(7) 0.001(5) 0.022(8) 0.001(7) N11 0.044(9) 0.089(8) 0.054(6) 0.002(5) 0.025(7) 0.009(6) N12 0.059(10) 0.073(7) 0.066(7) 0.005(5) 0.041(8) 0.015(6) C13 0.052(10) 0.056(6) 0.032(6) 0.004(4) 0.023(7) 0.012(6) N21 0.062(12) 0.039(6) 0.041(7) 0.000 0.032(9) 0.000 C22 0.049(11) 0.051(6) 0.036(6) -0.008(4) 0.014(7) 0.001(5) C23 0.092(14) 0.047(6) 0.066(8) -0.010(5) 0.047(10) -0.019(7) C24 0.11(2) 0.046(8) 0.055(11) 0.000 0.041(14) 0.000 C100 0.082(14) 0.086(9) 0.058(9) 0.006(7) 0.032(10) -0.017(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 Nd1 O200 2.45(3) . ? Nd1 O200 2.45(3) 6_657 ? Nd1 O34 2.490(10) . ? Nd1 O34 2.490(10) 6_657 ? Nd1 O32 2.568(10) . ? Nd1 O32 2.568(10) 6_657 ? Nd1 O21 2.569(19) . ? Nd1 O21 2.569(19) 6_657 ? Nd1 O22 2.60(2) . ? Nd1 O22 2.60(2) 6_657 ? Nd1 N14 2.628(11) 6_657 ? Nd1 N14 2.628(11) . ? Nd1 N21 2.700(12) . ? O32 N33 1.263(18) . ? N33 O34 1.193(18) . ? N33 O31 1.218(18) . ? N14 C15 1.320(17) . ? N14 C13 1.345(13) . ? C15 N11 1.348(17) . ? C15 C100 1.510(19) . ? N11 N12 1.308(16) . ? N12 C13 1.316(17) . ? C13 C22 1.429(18) . ? N21 C22 1.342(14) 6_657 ? N21 C22 1.343(14) . ? C22 C23 1.414(15) 6_657 ? C23 C24 1.377(16) . ? C23 C22 1.414(15) 6_657 ? C24 C23 1.377(17) 6_657 ? N23 O21 1.14(4) . ? N23 O22 1.29(3) . ? N23 O24 1.34(4) . ? C102 C101 1.47(5) . ? C101 N100 1.18(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O200 Nd1 O200 93.9(13) . 6_657 ? O200 Nd1 O34 82.9(7) . . ? O200 Nd1 O34 125.2(7) 6_657 . ? O200 Nd1 O34 125.2(7) . 6_657 ? O200 Nd1 O34 82.9(7) 6_657 6_657 ? O34 Nd1 O34 141.2(5) . 6_657 ? O200 Nd1 O32 72.2(7) . . ? O200 Nd1 O32 78.2(7) 6_657 . ? O34 Nd1 O32 48.7(4) . . ? O34 Nd1 O32 155.3(5) 6_657 . ? O200 Nd1 O32 78.2(7) . 6_657 ? O200 Nd1 O32 72.2(7) 6_657 6_657 ? O34 Nd1 O32 155.3(5) . 6_657 ? O34 Nd1 O32 48.7(4) 6_657 6_657 ? O32 Nd1 O32 136.1(6) . 6_657 ? O200 Nd1 O21 21.6(7) . . ? O200 Nd1 O21 73.7(9) 6_657 . ? O34 Nd1 O21 100.9(6) . . ? O34 Nd1 O21 113.5(5) 6_657 . ? O32 Nd1 O21 76.2(5) . . ? O32 Nd1 O21 64.9(5) 6_657 . ? O200 Nd1 O21 73.7(9) . 6_657 ? O200 Nd1 O21 21.6(7) 6_657 6_657 ? O34 Nd1 O21 113.5(5) . 6_657 ? O34 Nd1 O21 100.9(5) 6_657 6_657 ? O32 Nd1 O21 64.9(5) . 6_657 ? O32 Nd1 O21 76.2(5) 6_657 6_657 ? O21 Nd1 O21 55.3(10) . 6_657 ? O200 Nd1 O22 27.1(7) . . ? O200 Nd1 O22 117.1(8) 6_657 . ? O34 Nd1 O22 58.8(6) . . ? O34 Nd1 O22 136.8(6) 6_657 . ? O32 Nd1 O22 67.1(5) . . ? O32 Nd1 O22 98.7(5) 6_657 . ? O21 Nd1 O22 48.6(6) . . ? O21 Nd1 O22 95.6(7) 6_657 . ? O200 Nd1 O22 117.1(8) . 6_657 ? O200 Nd1 O22 27.1(7) 6_657 6_657 ? O34 Nd1 O22 136.8(6) . 6_657 ? O34 Nd1 O22 58.8(6) 6_657 6_657 ? O32 Nd1 O22 98.7(5) . 6_657 ? O32 Nd1 O22 67.1(5) 6_657 6_657 ? O21 Nd1 O22 95.6(7) . 6_657 ? O21 Nd1 O22 48.6(6) 6_657 6_657 ? O22 Nd1 O22 142.8(8) . 6_657 ? O200 Nd1 N14 145.9(6) . 6_657 ? O200 Nd1 N14 78.9(7) 6_657 6_657 ? O34 Nd1 N14 74.8(5) . 6_657 ? O34 Nd1 N14 87.3(4) 6_657 6_657 ? O32 Nd1 N14 73.7(3) . 6_657 ? O32 Nd1 N14 129.0(4) 6_657 6_657 ? O21 Nd1 N14 142.7(5) . 6_657 ? O21 Nd1 N14 91.7(5) 6_657 6_657 ? O22 Nd1 N14 132.0(5) . 6_657 ? O22 Nd1 N14 68.1(5) 6_657 6_657 ? O200 Nd1 N14 78.9(7) . . ? O200 Nd1 N14 145.9(6) 6_657 . ? O34 Nd1 N14 87.3(4) . . ? O34 Nd1 N14 74.8(5) 6_657 . ? O32 Nd1 N14 129.0(4) . . ? O32 Nd1 N14 73.7(3) 6_657 . ? O21 Nd1 N14 91.7(5) . . ? O21 Nd1 N14 142.7(5) 6_657 . ? O22 Nd1 N14 68.1(5) . . ? O22 Nd1 N14 132.0(5) 6_657 . ? N14 Nd1 N14 124.5(4) 6_657 . ? O200 Nd1 N21 133.1(6) . . ? O200 Nd1 N21 133.1(6) 6_657 . ? O34 Nd1 N21 70.6(2) . . ? O34 Nd1 N21 70.6(2) 6_657 . ? O32 Nd1 N21 111.9(3) . . ? O32 Nd1 N21 111.9(3) 6_657 . ? O21 Nd1 N21 152.4(5) . . ? O21 Nd1 N21 152.4(5) 6_657 . ? O22 Nd1 N21 108.6(4) . . ? O22 Nd1 N21 108.6(4) 6_657 . ? N14 Nd1 N21 62.2(2) 6_657 . ? N14 Nd1 N21 62.2(2) . . ? N33 O32 Nd1 94.6(9) . . ? O34 N33 O31 123.7(19) . . ? O34 N33 O32 116.2(14) . . ? O31 N33 O32 120.0(18) . . ? N33 O34 Nd1 100.5(10) . . ? C15 N14 C13 104.1(11) . . ? C15 N14 Nd1 136.6(8) . . ? C13 N14 Nd1 119.1(9) . . ? N14 C15 N11 108.4(12) . . ? N14 C15 C100 129.5(13) . . ? N11 C15 C100 122.0(15) . . ? N12 N11 C15 110.1(12) . . ? N11 N12 C13 104.5(11) . . ? N12 C13 N14 112.7(12) . . ? N12 C13 C22 125.0(11) . . ? N14 C13 C22 122.2(12) . . ? C22 N21 C22 121.1(13) 6_657 . ? C22 N21 Nd1 119.5(7) 6_657 . ? C22 N21 Nd1 119.5(7) . . ? N21 C22 C23 120.2(13) . 6_657 ? N21 C22 C13 116.8(10) . . ? C23 C22 C13 122.7(12) 6_657 . ? C24 C23 C22 119.6(14) . 6_657 ? C23 C24 C23 119.3(16) . 6_657 ? O21 N23 O22 122(3) . . ? O21 N23 O24 125(3) . . ? O22 N23 O24 113(3) . . ? N23 O21 Nd1 97(2) . . ? N23 O22 Nd1 92(2) . . ? N100 C101 C102 173(4) . . ? _refine_diff_density_max 0.645 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.138 _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(DMTZP),H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 2(DMTZP),H2O _chemical_formula_sum 'C34 H48 N14 O' _chemical_formula_weight 668.86 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 11.320(14) _cell_length_b 21.98(2) _cell_length_c 16.689(18) _cell_angle_alpha 90 _cell_angle_beta 109.698(10) _cell_angle_gamma 90 _cell_volume 3910(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 5 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 6415 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.08 _reflns_number_total 3713 _reflns_number_gt 1199 _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^)+(0.2000P)^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 0.003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3713 _refine_ls_number_parameters 205 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.2222 _refine_ls_R_factor_gt 0.1345 _refine_ls_wR_factor_ref 0.3765 _refine_ls_wR_factor_gt 0.3144 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.236 _refine_ls_shift/su_max 0.119 _refine_ls_shift/su_mean 0.012 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 O100 O 0.0000 -0.12473(19) 0.2500 0.0917(16) Uani 1 d S . . N21A N 0.0000 0.0149(3) 0.2500 0.0921(18) Uani 1 d S . . C22A C -0.0991(6) 0.0480(3) 0.1997(3) 0.0986(18) Uani 1 d . . . C23A C -0.1030(7) 0.1094(3) 0.1981(4) 0.121(2) Uani 1 d . . . H23A H -0.1730 0.1302 0.1631 0.146 Uiso 1 calc R . . C24A C 0.0000 0.1401(4) 0.2500 0.141(4) Uani 1 d S . . H24A H -0.0003 0.1824 0.2499 0.169 Uiso 1 calc SR . . N14A N -0.2006(5) -0.0497(2) 0.1460(3) 0.1066(16) Uani 1 d . . . C13A C -0.2041(6) 0.0113(3) 0.1483(4) 0.1010(18) Uani 1 d . . . N12A N -0.3128(5) 0.0347(2) 0.0959(3) 0.1171(18) Uani 1 d . . . N11A N -0.3808(6) -0.0157(3) 0.0612(3) 0.130(2) Uani 1 d . . . H11A H -0.4562 -0.0152 0.0256 0.156 Uiso 1 calc R . . C15A C -0.3159(8) -0.0642(3) 0.0894(5) 0.126(2) Uani 1 d D . . C16A C -0.3659(11) -0.1279(4) 0.0638(6) 0.194(4) Uiso 0.473(10) d PD A 1 H16A H -0.4493 -0.1286 0.0680 0.233 Uiso 0.473(10) calc PR A 1 H16B H -0.3772 -0.1315 0.0038 0.233 Uiso 0.473(10) calc PR A 1 C17A C -0.305(2) -0.1844(7) 0.1035(19) 0.252(6) Uiso 0.473(10) d PD A 1 H17A H -0.2678 -0.1772 0.1642 0.302 Uiso 0.473(10) calc PR A 1 H17B H -0.2367 -0.1927 0.0823 0.302 Uiso 0.473(10) calc PR A 1 C18A C -0.387(3) -0.2435(9) 0.091(2) 0.252(6) Uiso 0.473(10) d PD A 1 H18A H -0.4456 -0.2376 0.1214 0.302 Uiso 0.473(10) calc PR A 1 H18B H -0.4358 -0.2463 0.0312 0.302 Uiso 0.473(10) calc PR A 1 C19A C -0.325(3) -0.3028(11) 0.1178(18) 0.252(6) Uiso 0.473(10) d PD A 1 H19A H -0.2545 -0.3063 0.0989 0.302 Uiso 0.473(10) calc PR A 1 H19B H -0.3839 -0.3347 0.0932 0.302 Uiso 0.473(10) calc PR A 1 H19C H -0.2978 -0.3059 0.1787 0.302 Uiso 0.473(10) calc PR A 1 C16C C -0.3659(11) -0.1279(4) 0.0638(6) 0.194(4) Uiso 0.527(10) d PD A 2 H16C H -0.3075 -0.1503 0.0438 0.233 Uiso 0.527(10) calc PR A 2 H16D H -0.4455 -0.1254 0.0176 0.233 Uiso 0.527(10) calc PR A 2 C17C C -0.384(3) -0.1624(7) 0.1407(12) 0.252(6) Uiso 0.527(10) d PD A 2 H17C H -0.3174 -0.1507 0.1922 0.302 Uiso 0.527(10) calc PR A 2 H17D H -0.4629 -0.1490 0.1465 0.302 Uiso 0.527(10) calc PR A 2 C18C C -0.386(3) -0.2332(8) 0.1346(16) 0.252(6) Uiso 0.527(10) d PD A 2 H18C H -0.3359 -0.2499 0.1894 0.302 Uiso 0.527(10) calc PR A 2 H18D H -0.4717 -0.2471 0.1227 0.302 Uiso 0.527(10) calc PR A 2 C19C C -0.337(3) -0.2584(10) 0.0670(17) 0.252(6) Uiso 0.527(10) d PD A 2 H19C H -0.3507 -0.2290 0.0221 0.302 Uiso 0.527(10) calc PR A 2 H19D H -0.3811 -0.2952 0.0443 0.302 Uiso 0.527(10) calc PR A 2 H19E H -0.2492 -0.2668 0.0919 0.302 Uiso 0.527(10) calc PR A 2 N21B N 0.0000 -0.2652(3) 0.2500 0.0912(19) Uani 1 d S . . C22B C 0.0490(6) -0.2973(3) 0.1997(4) 0.0995(18) Uani 1 d . . . C23B C 0.0492(7) -0.3598(3) 0.1975(4) 0.122(2) Uani 1 d . . . H23B H 0.0819 -0.3808 0.1614 0.147 Uiso 1 calc R . . C24B C 0.0000 -0.3894(5) 0.2500 0.140(4) Uani 1 d S . . H24B H 0.0000 -0.4317 0.2500 0.168 Uiso 1 calc SR . . N14B N 0.0977(5) -0.2004(2) 0.1457(3) 0.1088(17) Uani 1 d . . . C13B C 0.1030(6) -0.2602(3) 0.1472(4) 0.0995(19) Uani 1 d . . . N12B N 0.1575(5) -0.2845(2) 0.0962(3) 0.1157(18) Uani 1 d . . . N11B N 0.1911(6) -0.2350(3) 0.0606(4) 0.130(2) Uani 1 d . . . C15B C 0.1559(8) -0.1867(3) 0.0901(5) 0.127(2) Uani 1 d D . . C16B C 0.1806(11) -0.1228(4) 0.0666(6) 0.193(4) Uiso 0.556(10) d PD B 1 H16B H 0.1023 -0.1002 0.0475 0.232 Uiso 0.556(10) calc PR B 1 H16C H 0.2133 -0.1243 0.0198 0.232 Uiso 0.556(10) calc PR B 1 C17B C 0.275(2) -0.0896(7) 0.1422(12) 0.241(5) Uiso 0.556(10) d PD B 1 H17B H 0.2562 -0.1008 0.1929 0.289 Uiso 0.556(10) calc PR B 1 H17B H 0.3577 -0.1054 0.1490 0.289 Uiso 0.556(10) calc PR B 1 C18B C 0.281(2) -0.0205(8) 0.1394(15) 0.241(5) Uiso 0.556(10) d PD B 1 H18B H 0.2979 -0.0050 0.1965 0.289 Uiso 0.556(10) calc PR B 1 H18B H 0.3514 -0.0092 0.1216 0.289 Uiso 0.556(10) calc PR B 1 C19B C 0.163(2) 0.0104(10) 0.0804(16) 0.241(5) Uiso 0.556(10) d PD B 1 H19A H 0.1105 -0.0193 0.0435 0.289 Uiso 0.556(10) calc PR B 1 H19B H 0.1865 0.0407 0.0469 0.289 Uiso 0.556(10) calc PR B 1 H19C H 0.1191 0.0294 0.1136 0.289 Uiso 0.556(10) calc PR B 1 C16D C 0.1806(11) -0.1228(4) 0.0666(6) 0.193(4) Uiso 0.444(10) d PD B 2 H16D H 0.2665 -0.1231 0.0671 0.232 Uiso 0.444(10) calc PR B 2 H16D H 0.1283 -0.1176 0.0075 0.232 Uiso 0.444(10) calc PR B 2 C17D C 0.167(3) -0.0672(7) 0.1083(19) 0.241(5) Uiso 0.444(10) d PD B 2 H17D H 0.2057 -0.0730 0.1692 0.289 Uiso 0.444(10) calc PR B 2 H17D H 0.0786 -0.0596 0.0966 0.289 Uiso 0.444(10) calc PR B 2 C18D C 0.227(3) -0.0092(9) 0.082(2) 0.241(5) Uiso 0.444(10) d PD B 2 H18D H 0.3129 -0.0188 0.0878 0.289 Uiso 0.444(10) calc PR B 2 H18E H 0.1825 -0.0018 0.0215 0.289 Uiso 0.444(10) calc PR B 2 C19D C 0.226(3) 0.0476(10) 0.1272(18) 0.241(5) Uiso 0.444(10) d PD B 2 H19D H 0.1416 0.0582 0.1217 0.289 Uiso 0.444(10) calc PR B 2 H19E H 0.2621 0.0795 0.1034 0.289 Uiso 0.444(10) calc PR B 2 H19F H 0.2749 0.0423 0.1862 0.289 Uiso 0.444(10) calc PR B 2 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 O100 0.093(4) 0.085(3) 0.094(3) 0.000 0.028(3) 0.000 N21A 0.073(5) 0.113(4) 0.076(4) 0.000 0.006(3) 0.000 C22A 0.070(4) 0.117(5) 0.097(4) 0.005(3) 0.013(3) 0.004(3) C23A 0.097(6) 0.103(5) 0.142(6) -0.004(4) 0.011(4) 0.009(4) C24A 0.135(11) 0.099(6) 0.180(10) 0.000 0.042(8) 0.000 N14A 0.077(4) 0.118(4) 0.101(3) -0.004(3) -0.001(3) -0.008(3) C13A 0.080(4) 0.112(4) 0.098(4) -0.001(3) 0.012(3) 0.017(4) N12A 0.085(4) 0.133(4) 0.112(4) -0.001(3) 0.004(3) 0.015(4) N11A 0.084(4) 0.149(5) 0.124(4) -0.009(4) -0.009(3) 0.016(4) C15A 0.114(7) 0.125(5) 0.123(5) -0.002(4) 0.018(5) 0.009(5) N21B 0.092(5) 0.104(4) 0.087(4) 0.000 0.043(4) 0.000 C22B 0.088(4) 0.117(5) 0.100(4) -0.001(3) 0.041(4) 0.002(3) C23B 0.141(7) 0.106(5) 0.142(6) 0.002(4) 0.077(5) 0.012(4) C24B 0.134(10) 0.110(7) 0.184(10) 0.000 0.064(8) 0.000 N14B 0.122(5) 0.119(4) 0.101(3) 0.005(3) 0.057(3) -0.008(3) C13B 0.109(5) 0.104(4) 0.095(4) -0.001(3) 0.047(4) 0.017(3) N12B 0.116(5) 0.137(4) 0.112(4) 0.005(3) 0.062(3) 0.017(3) N11B 0.150(6) 0.142(4) 0.123(4) -0.003(4) 0.078(4) 0.021(4) C15B 0.143(7) 0.130(5) 0.118(5) 0.008(4) 0.057(5) 0.007(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 N21A C22A 1.361(6) . ? N21A C22A 1.366(6) 6_556 ? C22A C23A 1.349(8) . ? C22A C13A 1.456(8) . ? C23A C24A 1.375(7) . ? C24A C23A 1.370(7) 6_556 ? N14A C13A 1.342(7) . ? N14A C15A 1.367(8) . ? C13A N12A 1.345(7) . ? N12A N11A 1.365(7) . ? N11A C15A 1.286(8) . ? C15A C16C 1.520(8) . ? C15A C16A 1.520(8) . ? C16A C17A 1.463(15) . ? C17A C18A 1.570(18) . ? C18A C19A 1.470(17) . ? C16C C17C 1.563(15) . ? C17C C18C 1.561(16) . ? C18C C19C 1.519(17) . ? N21B C22B 1.351(6) 6_556 ? N21B C22B 1.352(6) . ? C22B C23B 1.374(8) . ? C22B C13B 1.471(8) . ? C23B C24B 1.353(7) . ? C24B C23B 1.354(7) 6_556 ? N14B C13B 1.317(7) . ? N14B C15B 1.339(8) . ? C13B N12B 1.321(7) . ? N12B N11B 1.355(7) . ? N11B C15B 1.288(8) . ? C15B C16D 1.511(8) . ? C15B C16B 1.511(8) . ? C16B C17B 1.536(15) . ? C17B C18B 1.524(15) . ? C18B C19B 1.521(17) . ? C16D C17D 1.440(15) . ? C17D C18D 1.574(18) . ? C18D C19D 1.465(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 C22A N21A C22A 115.5(7) . 6_556 ? C23A C22A N21A 123.9(6) . . ? C23A C22A C13A 122.1(6) . . ? N21A C22A C13A 114.0(5) . . ? C22A C23A C24A 117.9(7) . . ? C23A C24A C23A 121.1(9) 6_556 . ? C13A N14A C15A 103.1(5) . . ? N14A C13A N12A 112.8(6) . . ? N14A C13A C22A 123.2(6) . . ? N12A C13A C22A 123.9(6) . . ? C13A N12A N11A 103.3(5) . . ? C15A N11A N12A 110.3(6) . . ? N11A C15A N14A 110.5(6) . . ? N11A C15A C16C 123.2(8) . . ? N14A C15A C16C 126.3(8) . . ? N11A C15A C16A 123.2(8) . . ? N14A C15A C16A 126.3(8) . . ? C16C C15A C16A 0.0(14) . . ? C17A C16A C15A 125.5(13) . . ? C16A C17A C18A 118.4(18) . . ? C19A C18A C17A 120(2) . . ? C15A C16C C17C 110.8(9) . . ? C18C C17C C16C 115.5(11) . . ? C19C C18C C17C 114.4(12) . . ? C22B N21B C22B 117.0(6) 6_556 . ? N21B C22B C23B 122.9(5) . . ? N21B C22B C13B 114.9(5) . . ? C23B C22B C13B 122.2(5) . . ? C24B C23B C22B 117.4(6) . . ? C23B C24B C23B 122.4(9) . 6_556 ? C13B N14B C15B 101.9(5) . . ? N14B C13B N12B 114.9(5) . . ? N14B C13B C22B 122.6(5) . . ? N12B C13B C22B 122.5(6) . . ? C13B N12B N11B 102.6(5) . . ? C15B N11B N12B 109.0(5) . . ? N11B C15B N14B 111.7(6) . . ? N11B C15B C16D 123.9(8) . . ? N14B C15B C16D 124.4(8) . . ? N11B C15B C16B 123.9(8) . . ? N14B C15B C16B 124.4(8) . . ? C16D C15B C16B 0.0(13) . . ? C15B C16B C17B 111.7(9) . . ? C18B C17B C16B 118.6(12) . . ? C19B C18B C17B 114.9(12) . . ? C17D C16D C15B 127.3(12) . . ? C16D C17D C18D 115.3(17) . . ? C19D C18D C17D 118.0(18) . . ? _refine_diff_density_max 0.464 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.071 _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 ; #====END data_3-Ho _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 3-Ho _chemical_formula_sum 'C13 H16 Ho N10 O11 ' _chemical_formula_weight 653.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 8.563(9) _cell_length_b 11.095(14) _cell_length_c 13.346(16) _cell_angle_alpha 96.979(10) _cell_angle_beta 98.063(10) _cell_angle_gamma 114.596(10) _cell_volume 1118(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 3.614 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.398 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3873 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.93 _reflns_number_total 3873 _reflns_number_gt 3609 _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^)+(0.0709P)^2^+2.4269P] 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 0.0115(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3873 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _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 Ho1 Ho 0.01284(2) 0.278586(17) 0.231992(14) 0.02742(11) Uani 1 d . . . N21 N 0.2340(5) 0.4865(4) 0.1852(3) 0.0309(8) Uani 1 d . . . C22 C 0.3595(6) 0.5862(5) 0.2599(4) 0.0341(10) Uani 1 d . . . C23 C 0.4948(7) 0.6962(6) 0.2372(5) 0.0511(13) Uani 1 d . . . H23 H 0.5808 0.7640 0.2896 0.061 Uiso 1 calc R . . C24 C 0.4983(8) 0.7022(6) 0.1347(5) 0.0574(16) Uani 1 d . . . H24 H 0.5885 0.7739 0.1175 0.069 Uiso 1 calc R . . C25 C 0.3682(7) 0.6018(5) 0.0576(5) 0.0481(13) Uani 1 d . . . H25 H 0.3680 0.6055 -0.0117 0.058 Uiso 1 calc R . . C26 C 0.2375(6) 0.4950(5) 0.0865(4) 0.0330(9) Uani 1 d . . . N34 N -0.0138(5) 0.2686(4) 0.0447(3) 0.0334(8) Uani 1 d . . . C33 C 0.0939(6) 0.3801(5) 0.0124(4) 0.0314(9) Uani 1 d . . . N32 N 0.0573(6) 0.3737(4) -0.0867(3) 0.0417(10) Uani 1 d . . . N31 N -0.0839(6) 0.2489(4) -0.1214(3) 0.0418(9) Uani 1 d . . . H31 H -0.1385 0.2154 -0.1848 0.050 Uiso 1 calc R . . C35 C -0.1236(7) 0.1876(5) -0.0426(4) 0.0383(11) Uani 1 d . . . N14 N 0.2087(5) 0.4549(4) 0.3828(3) 0.0332(8) Uani 1 d . . . C13 C 0.3440(6) 0.5660(4) 0.3647(4) 0.0336(10) Uani 1 d . . . N12 N 0.4553(6) 0.6491(4) 0.4486(3) 0.0411(9) Uani 1 d . . . N11 N 0.3859(6) 0.5867(4) 0.5246(3) 0.0406(9) Uani 1 d . . . H11 H 0.4304 0.6168 0.5896 0.049 Uiso 1 calc R . . C15 C 0.2402(6) 0.4728(5) 0.4850(4) 0.0384(11) Uani 1 d . . . O41 O -0.3003(5) 0.1332(4) 0.2019(3) 0.0494(9) Uani 1 d . . . O42 O -0.1843(5) 0.2629(4) 0.3520(3) 0.0438(8) Uani 1 d . . . N43 N -0.3202(6) 0.1671(5) 0.2915(4) 0.0429(11) Uani 1 d . . . O44 O -0.4583(6) 0.1131(5) 0.3181(5) 0.0731(15) Uani 1 d . . . O51 O -0.0473(6) 0.0437(4) 0.1655(4) 0.0538(10) Uani 1 d . . . O52 O 0.0020(5) 0.1084(4) 0.3304(3) 0.0462(9) Uani 1 d . . . N53 N -0.0445(6) 0.0111(5) 0.2528(4) 0.0497(12) Uani 1 d . . . O54 O -0.0841(7) -0.1041(4) 0.2640(5) 0.0812(16) Uani 1 d . . . O61 O 0.3811(6) 0.2823(5) 0.1062(3) 0.0612(11) Uani 1 d . . . O62 O 0.2888(5) 0.2689(4) 0.2502(4) 0.0512(11) Uani 1 d . . . N63 O 0.4114(5) 0.3081(4) 0.2008(4) 0.0503(10) Uani 1 d . . . O64 O 0.5630(5) 0.3748(4) 0.2543(3) 0.0532(10) Uani 1 d . . . O100 O -0.1223(5) 0.4222(4) 0.2024(3) 0.0431(8) Uani 1 d . . . C100 C 0.1352(8) 0.3819(6) 0.5492(5) 0.0535(14) Uani 1 d . . . H10A H 0.0630 0.4187 0.5768 0.064 Uiso 1 calc R . . H10B H 0.2131 0.3749 0.6048 0.064 Uiso 1 calc R . . H10C H 0.0619 0.2938 0.5072 0.064 Uiso 1 calc R . . C200 C -0.2684(9) 0.0501(6) -0.0547(6) 0.0602(16) Uani 1 d . . . H20A H -0.2205 -0.0108 -0.0373 0.072 Uiso 1 calc R . . H20B H -0.3330 0.0193 -0.1250 0.072 Uiso 1 calc R . . H20C H -0.3457 0.0527 -0.0098 0.072 Uiso 1 calc R . . N100 N 0.2244(8) -0.1806(7) 0.3416(5) 0.0703(16) Uani 1 d . . . C101 C 0.2441(7) -0.0987(6) 0.4065(5) 0.0491(13) Uani 1 d . . . C102 C 0.2687(10) 0.0072(7) 0.4917(6) 0.0650(17) Uani 1 d . . . H10D H 0.1661 -0.0210 0.5211 0.078 Uiso 1 calc R . . H10E H 0.2873 0.0886 0.4667 0.078 Uiso 1 calc R . . H10F H 0.3691 0.0238 0.5435 0.078 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 Ho1 0.02720(14) 0.02749(14) 0.02723(17) 0.00603(9) 0.00582(9) 0.01157(9) N21 0.0309(17) 0.0286(18) 0.032(2) 0.0063(15) 0.0057(15) 0.0121(15) C22 0.033(2) 0.032(2) 0.033(3) 0.0064(19) 0.0048(19) 0.0120(18) C23 0.045(3) 0.040(3) 0.047(4) 0.005(2) 0.006(2) 0.001(2) C24 0.050(3) 0.047(3) 0.057(4) 0.021(3) 0.019(3) -0.001(2) C25 0.046(3) 0.040(3) 0.051(4) 0.016(2) 0.018(3) 0.009(2) C26 0.039(2) 0.033(2) 0.029(3) 0.0090(19) 0.0080(19) 0.0170(19) N34 0.0346(18) 0.0333(19) 0.031(2) 0.0054(16) 0.0073(16) 0.0143(16) C33 0.042(2) 0.035(2) 0.021(3) 0.0057(18) 0.0050(18) 0.0208(19) N32 0.052(2) 0.037(2) 0.034(3) 0.0082(18) 0.012(2) 0.0172(19) N31 0.057(3) 0.038(2) 0.023(2) -0.0022(17) -0.0001(19) 0.0193(19) C35 0.047(3) 0.036(2) 0.029(3) 0.002(2) 0.004(2) 0.017(2) N14 0.0344(19) 0.0342(19) 0.029(2) 0.0033(16) 0.0087(16) 0.0131(16) C13 0.034(2) 0.028(2) 0.034(3) 0.0007(18) 0.0040(19) 0.0114(18) N12 0.045(2) 0.036(2) 0.034(3) 0.0010(17) 0.0040(19) 0.0119(18) N11 0.052(2) 0.040(2) 0.022(2) -0.0011(17) 0.0024(18) 0.0169(19) C15 0.038(2) 0.040(3) 0.038(3) 0.006(2) 0.010(2) 0.017(2) O41 0.0347(17) 0.049(2) 0.054(3) 0.0053(18) 0.0054(17) 0.0107(16) O42 0.0420(18) 0.052(2) 0.044(2) 0.0136(17) 0.0158(16) 0.0235(17) N43 0.035(2) 0.043(2) 0.057(3) 0.024(2) 0.014(2) 0.0175(19) O44 0.043(2) 0.085(3) 0.096(4) 0.043(3) 0.036(3) 0.019(2) O51 0.061(2) 0.045(2) 0.054(3) 0.0017(18) 0.006(2) 0.0266(19) O52 0.058(2) 0.046(2) 0.047(3) 0.0211(18) 0.0178(18) 0.0305(18) N53 0.041(2) 0.040(2) 0.076(4) 0.018(2) 0.014(2) 0.0243(19) O54 0.086(3) 0.039(2) 0.130(5) 0.032(3) 0.020(3) 0.036(2) O61 0.080(3) 0.074(3) 0.026(3) 0.0031(19) 0.003(2) 0.035(2) O62 0.0359(18) 0.066(2) 0.074(3) 0.037(2) 0.0267(19) 0.0329(18) N63 0.048(2) 0.043(2) 0.068(3) 0.0134(19) 0.015(2) 0.0265(17) O64 0.0329(18) 0.071(3) 0.045(3) 0.0045(19) 0.0028(16) 0.0164(17) O100 0.0448(18) 0.0445(19) 0.056(3) 0.0259(17) 0.0196(17) 0.0281(16) C100 0.056(3) 0.057(3) 0.039(4) 0.014(3) 0.014(3) 0.015(3) C200 0.060(4) 0.049(3) 0.046(4) -0.002(3) -0.001(3) 0.006(3) N100 0.080(4) 0.078(4) 0.049(4) -0.004(3) 0.008(3) 0.038(3) C101 0.049(3) 0.056(3) 0.040(4) 0.016(3) 0.004(2) 0.021(3) C102 0.076(4) 0.052(4) 0.064(5) 0.004(3) 0.014(4) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O100 2.365(4) . ? Ho1 O62 2.390(4) . ? Ho1 O52 2.405(4) . ? Ho1 O41 2.427(4) . ? Ho1 O42 2.455(4) . ? Ho1 O51 2.458(5) . ? Ho1 N14 2.461(4) . ? Ho1 N34 2.462(5) . ? Ho1 N21 2.518(4) . ? N21 C26 1.336(6) . ? N21 C22 1.347(6) . ? C22 C23 1.391(7) . ? C22 C13 1.459(7) . ? C23 C24 1.381(9) . ? C24 C25 1.381(9) . ? C25 C26 1.391(7) . ? C26 C33 1.471(7) . ? N34 C35 1.336(7) . ? N34 C33 1.364(6) . ? C33 N32 1.301(7) . ? N32 N31 1.373(6) . ? N31 C35 1.329(7) . ? C35 C200 1.483(8) . ? N14 C15 1.325(7) . ? N14 C13 1.372(6) . ? C13 N12 1.315(7) . ? N12 N11 1.364(6) . ? N11 C15 1.331(7) . ? C15 C100 1.494(7) . ? O41 N43 1.266(7) . ? O42 N43 1.278(6) . ? N43 O44 1.208(6) . ? O51 N53 1.262(7) . ? O52 N53 1.285(6) . ? N53 O54 1.213(6) . ? O61 N63 1.225(6) . ? O62 N63 1.269(6) . ? N63 O64 1.247(6) . ? N100 C101 1.116(8) . ? C101 C102 1.456(9) . ? 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 O62 142.81(13) . . ? O100 Ho1 O52 140.72(13) . . ? O62 Ho1 O52 71.79(13) . . ? O100 Ho1 O41 75.08(16) . . ? O62 Ho1 O41 141.28(16) . . ? O52 Ho1 O41 77.63(15) . . ? O100 Ho1 O42 70.61(13) . . ? O62 Ho1 O42 132.10(15) . . ? O52 Ho1 O42 70.40(13) . . ? O41 Ho1 O42 52.25(15) . . ? O100 Ho1 O51 136.95(15) . . ? O62 Ho1 O51 72.49(15) . . ? O52 Ho1 O51 52.57(16) . . ? O41 Ho1 O51 70.17(15) . . ? O42 Ho1 O51 105.12(14) . . ? O100 Ho1 N14 86.70(15) . . ? O62 Ho1 N14 73.83(16) . . ? O52 Ho1 N14 89.47(16) . . ? O41 Ho1 N14 129.64(13) . . ? O42 Ho1 N14 77.49(15) . . ? O51 Ho1 N14 135.41(14) . . ? O100 Ho1 N34 77.79(13) . . ? O62 Ho1 N34 92.23(14) . . ? O52 Ho1 N34 129.66(14) . . ? O41 Ho1 N34 89.32(13) . . ? O42 Ho1 N34 134.87(13) . . ? O51 Ho1 N34 77.19(14) . . ? N14 Ho1 N34 132.51(13) . . ? O100 Ho1 N21 72.19(15) . . ? O62 Ho1 N21 71.03(14) . . ? O52 Ho1 N21 140.01(14) . . ? O41 Ho1 N21 142.34(13) . . ? O42 Ho1 N21 128.83(13) . . ? O51 Ho1 N21 126.05(15) . . ? N14 Ho1 N21 66.46(15) . . ? N34 Ho1 N21 66.07(13) . . ? C26 N21 C22 119.0(4) . . ? C26 N21 Ho1 120.8(3) . . ? C22 N21 Ho1 120.0(3) . . ? N21 C22 C23 121.9(5) . . ? N21 C22 C13 114.4(4) . . ? C23 C22 C13 123.7(5) . . ? C24 C23 C22 118.3(5) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 118.1(5) . . ? N21 C26 C25 122.5(5) . . ? N21 C26 C33 113.9(4) . . ? C25 C26 C33 123.6(5) . . ? C35 N34 C33 103.5(4) . . ? C35 N34 Ho1 138.0(3) . . ? C33 N34 Ho1 117.9(3) . . ? N32 C33 N34 114.3(4) . . ? N32 C33 C26 125.0(4) . . ? N34 C33 C26 120.8(4) . . ? C33 N32 N31 103.0(4) . . ? C35 N31 N32 109.9(5) . . ? N31 C35 N34 109.3(5) . . ? N31 C35 C200 123.2(5) . . ? N34 C35 C200 127.5(5) . . ? C15 N14 C13 103.3(4) . . ? C15 N14 Ho1 138.9(3) . . ? C13 N14 Ho1 117.3(3) . . ? N12 C13 N14 114.4(4) . . ? N12 C13 C22 124.2(4) . . ? N14 C13 C22 121.3(4) . . ? C13 N12 N11 102.0(4) . . ? C15 N11 N12 111.0(5) . . ? N14 C15 N11 109.3(4) . . ? N14 C15 C100 127.3(5) . . ? N11 C15 C100 123.4(5) . . ? N43 O41 Ho1 96.9(3) . . ? N43 O42 Ho1 95.2(3) . . ? O44 N43 O41 122.4(5) . . ? O44 N43 O42 122.3(5) . . ? O41 N43 O42 115.3(4) . . ? O44 N43 Ho1 175.7(4) . . ? O41 N43 Ho1 57.1(2) . . ? O42 N43 Ho1 58.4(2) . . ? N53 O51 Ho1 94.8(3) . . ? N53 O52 Ho1 96.7(3) . . ? O54 N53 O51 122.9(6) . . ? O54 N53 O52 121.5(6) . . ? O51 N53 O52 115.5(4) . . ? O54 N53 Ho1 173.7(4) . . ? O51 N53 Ho1 59.1(2) . . ? O52 N53 Ho1 56.8(2) . . ? N63 O62 Ho1 132.6(3) . . ? O61 N63 O64 122.5(5) . . ? O61 N63 O62 121.6(5) . . ? O64 N63 O62 115.9(5) . . ? N100 C101 C102 179.4(7) . . ? _refine_diff_density_max 1.188 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.158 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_4-yb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 4-yb _chemical_formula_sum 'C13 H14 N11 O9 Yb' _chemical_formula_weight 641.39 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 16.102(18) _cell_length_b 8.179(10) _cell_length_c 16.571(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.689(10) _cell_angle_gamma 90.00 _cell_volume 2137(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 4.448 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6452 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.08 _reflns_number_total 3898 _reflns_number_gt 3074 _reflns_threshold_expression >2sigma(I) _refine_special_details ? _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_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+10.8015P] 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(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3898 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.017 _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 Yb1 Yb 0.23700(2) 0.16331(4) 0.008244(19) 0.03496(17) Uani 1 d . . . N14 N 0.1260(5) 0.1199(9) 0.0861(4) 0.0439(16) Uani 1 d . . . C15 C 0.1155(6) 0.0361(11) 0.1520(5) 0.049(2) Uani 1 d . . . N11 N 0.0349(5) 0.0482(10) 0.1575(5) 0.0550(19) Uani 1 d . . . H11 H 0.0142 0.0042 0.1963 0.066 Uiso 1 calc R . . N12 N -0.0116(5) 0.1376(10) 0.0954(5) 0.055(2) Uani 1 d . . . C13 C 0.0466(6) 0.1767(10) 0.0519(5) 0.0414(18) Uani 1 d . . . N21 N 0.0984(4) 0.2788(8) -0.0607(4) 0.0382(14) Uani 1 d . . . C22 C 0.0313(5) 0.2685(10) -0.0246(5) 0.0410(18) Uani 1 d . . . C23 C -0.0474(5) 0.3414(10) -0.0595(6) 0.046(2) Uani 1 d . . . H23 H -0.0936 0.3335 -0.0338 0.055 Uiso 1 calc R . . C24 C -0.0534(6) 0.4244(12) -0.1328(6) 0.055(2) Uani 1 d . . . H24 H -0.1045 0.4729 -0.1573 0.066 Uiso 1 calc R . . C25 C 0.0158(6) 0.4366(11) -0.1703(6) 0.052(2) Uani 1 d . . . H25 H 0.0120 0.4927 -0.2198 0.063 Uiso 1 calc R . . C26 C 0.0909(6) 0.3622(10) -0.1316(5) 0.0407(18) Uani 1 d . . . N34 N 0.2419(4) 0.2963(8) -0.1207(4) 0.0391(15) Uani 1 d . . . C33 C 0.1696(6) 0.3619(10) -0.1648(5) 0.0411(18) Uani 1 d . . . N32 N 0.1759(5) 0.4196(10) -0.2374(4) 0.0506(18) Uani 1 d . . . N31 N 0.2583(5) 0.3871(10) -0.2384(5) 0.0530(19) Uani 1 d . . . H31 H 0.2824 0.4111 -0.2787 0.064 Uiso 1 calc R . . C35 C 0.2980(6) 0.3128(9) -0.1686(5) 0.0408(18) Uani 1 d . . . C100 C 0.1801(8) -0.0572(17) 0.2110(8) 0.073(3) Uani 1 d . . . H10A H 0.224(8) 0.014(16) 0.250(8) 0.087 Uiso 1 d . . . H10B H 0.218(9) -0.118(16) 0.190(8) 0.087 Uiso 1 d . . . H10C H 0.152(8) -0.123(16) 0.252(8) 0.087 Uiso 1 d . . . C200 C 0.3873(6) 0.2563(14) -0.1508(7) 0.055(2) Uani 1 d . . . H20A H 0.422(7) 0.292(13) -0.088(7) 0.066 Uiso 1 d . . . H20B H 0.408(8) 0.286(14) -0.185(7) 0.066 Uiso 1 d . . . H20C H 0.388(7) 0.144(14) -0.150(7) 0.066 Uiso 1 d . . . O41 O 0.2320(4) 0.4125(8) 0.0784(4) 0.0561(16) Uani 1 d . . . O42 O 0.3475(4) 0.3706(8) 0.0359(4) 0.0583(17) Uani 1 d . . . N43 N 0.3054(5) 0.4657(10) 0.0742(5) 0.0529(18) Uani 1 d . . . O44 O 0.3328(5) 0.5946(9) 0.1038(5) 0.079(2) Uani 1 d . . . N53 N 0.3852(5) 0.0151(10) 0.0943(5) 0.058(2) Uani 1 d . . . O54 O 0.4480(5) -0.0503(12) 0.1315(5) 0.090(3) Uani 1 d . . . O51 O 0.3690(4) 0.0290(8) 0.0162(4) 0.0550(16) Uani 1 d . . . O52 O 0.3300(4) 0.0798(8) 0.1303(4) 0.0545(15) Uani 1 d . . . O61 O 0.2113(5) -0.1311(7) 0.0159(4) 0.0498(15) Uani 1 d . . . O62 O 0.2064(4) -0.0289(7) -0.1038(3) 0.0463(13) Uani 1 d . . . N63 N 0.2054(5) -0.1586(8) -0.0586(5) 0.0464(18) Uani 1 d . . . O64 O 0.2009(5) -0.2932(9) -0.0895(5) 0.0675(19) Uani 1 d . . . N100 N 0.5268(7) 0.3916(13) 0.2080(6) 0.074(3) Uani 1 d . . . C101 C 0.5431(7) 0.3422(11) 0.1504(7) 0.054(2) Uani 1 d . . . C102 C 0.5646(10) 0.280(2) 0.0752(8) 0.077(3) Uani 1 d . . . H10A H 0.522(9) 0.194(16) 0.041(8) 0.093 Uiso 1 d . . . H10B H 0.618(9) 0.260(18) 0.095(9) 0.093 Uiso 1 d . . . H10C H 0.569(9) 0.357(16) 0.039(9) 0.093 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 Yb1 0.0346(2) 0.0370(2) 0.0334(2) -0.00035(12) 0.00719(14) 0.00271(13) N14 0.048(4) 0.049(4) 0.038(4) 0.006(3) 0.016(3) 0.003(3) C15 0.051(5) 0.056(5) 0.040(5) -0.002(4) 0.012(4) 0.001(4) N11 0.058(5) 0.061(5) 0.051(4) 0.004(4) 0.023(4) 0.002(4) N12 0.052(5) 0.059(5) 0.061(5) 0.006(4) 0.025(4) 0.002(4) C13 0.046(5) 0.038(4) 0.043(5) -0.004(3) 0.015(4) -0.002(3) N21 0.039(4) 0.038(3) 0.038(4) -0.001(3) 0.008(3) -0.002(3) C22 0.039(4) 0.034(4) 0.051(5) -0.001(3) 0.012(3) 0.004(3) C23 0.028(4) 0.049(5) 0.060(6) 0.003(4) 0.009(4) 0.002(3) C24 0.046(5) 0.055(6) 0.060(6) -0.001(4) 0.002(4) 0.011(4) C25 0.059(6) 0.049(5) 0.046(5) 0.007(4) 0.004(4) 0.008(4) C26 0.051(5) 0.040(4) 0.030(4) 0.000(3) 0.005(3) -0.001(3) N34 0.040(4) 0.040(4) 0.038(4) 0.005(3) 0.009(3) 0.002(3) C33 0.044(5) 0.041(4) 0.038(4) 0.000(3) 0.008(3) -0.004(3) N32 0.055(5) 0.061(5) 0.036(4) 0.005(3) 0.010(3) -0.001(4) N31 0.055(5) 0.063(5) 0.042(4) 0.004(4) 0.013(3) -0.002(4) C35 0.048(5) 0.032(4) 0.044(5) -0.001(3) 0.013(4) -0.005(3) C100 0.071(7) 0.088(9) 0.057(7) 0.035(6) 0.006(5) 0.001(6) C200 0.047(5) 0.058(6) 0.064(7) 0.000(5) 0.022(5) -0.010(4) O41 0.055(4) 0.044(4) 0.070(4) -0.019(3) 0.013(3) 0.004(3) O42 0.052(4) 0.056(4) 0.068(4) -0.013(3) 0.014(3) -0.012(3) N43 0.056(5) 0.049(5) 0.049(4) 0.003(3) 0.000(3) -0.004(4) O44 0.087(6) 0.042(4) 0.098(6) -0.010(4) -0.003(4) -0.018(4) N53 0.049(4) 0.053(5) 0.066(5) -0.012(4) 0.001(4) 0.007(4) O54 0.061(5) 0.111(7) 0.080(5) 0.000(5) -0.025(4) 0.039(5) O51 0.050(3) 0.064(4) 0.051(4) -0.013(3) 0.010(3) 0.008(3) O52 0.054(4) 0.058(4) 0.048(4) -0.003(3) 0.002(3) 0.005(3) O61 0.071(4) 0.043(3) 0.040(3) -0.003(2) 0.022(3) 0.009(3) O62 0.058(4) 0.038(3) 0.044(3) -0.004(2) 0.015(3) -0.004(3) N63 0.036(4) 0.038(4) 0.069(5) -0.004(3) 0.021(3) -0.002(3) O64 0.085(5) 0.041(4) 0.080(5) -0.020(3) 0.023(4) -0.008(3) N100 0.097(8) 0.077(6) 0.056(5) -0.009(5) 0.031(5) 0.009(6) C101 0.065(6) 0.041(5) 0.058(6) -0.001(4) 0.016(5) 0.005(4) C102 0.084(9) 0.087(9) 0.064(8) -0.017(7) 0.022(7) 0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O41 2.356(6) . ? Yb1 O52 2.360(6) . ? Yb1 O51 2.372(6) . ? Yb1 O62 2.407(6) . ? Yb1 N34 2.414(7) . ? Yb1 O42 2.433(7) . ? Yb1 N14 2.433(7) . ? Yb1 O61 2.451(7) . ? Yb1 N21 2.479(7) . ? N14 C15 1.328(11) . ? N14 C13 1.371(11) . ? C15 N11 1.323(12) . ? C15 C100 1.486(14) . ? N11 N12 1.357(11) . ? N12 C13 1.332(12) . ? C13 C22 1.450(12) . ? N21 C22 1.340(10) . ? N21 C26 1.343(10) . ? C22 C23 1.414(12) . ? C23 C24 1.378(14) . ? C24 C25 1.385(14) . ? C25 C26 1.390(12) . ? C26 C33 1.480(13) . ? N34 C35 1.323(11) . ? N34 C33 1.355(11) . ? C33 N32 1.316(11) . ? N32 N31 1.357(11) . ? N31 C35 1.347(12) . ? C35 C200 1.482(13) . ? O41 N43 1.275(10) . ? O42 N43 1.281(10) . ? N43 O44 1.207(10) . ? N53 O54 1.199(10) . ? N53 O51 1.271(10) . ? N53 O52 1.280(10) . ? O61 N63 1.240(10) . ? O62 N63 1.300(9) . ? N63 O64 1.210(9) . ? N100 C101 1.115(13) . ? C101 C102 1.452(16) . ? 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 O41 Yb1 O52 84.6(2) . . ? O41 Yb1 O51 119.5(2) . . ? O52 Yb1 O51 54.0(2) . . ? O41 Yb1 O62 157.5(2) . . ? O52 Yb1 O62 117.9(2) . . ? O51 Yb1 O62 77.4(2) . . ? O41 Yb1 N34 93.3(2) . . ? O52 Yb1 N34 139.5(2) . . ? O51 Yb1 N34 93.9(2) . . ? O62 Yb1 N34 69.5(2) . . ? O41 Yb1 O42 53.2(2) . . ? O52 Yb1 O42 74.2(2) . . ? O51 Yb1 O42 72.5(2) . . ? O62 Yb1 O42 128.9(2) . . ? N34 Yb1 O42 72.5(2) . . ? O41 Yb1 N14 76.3(2) . . ? O52 Yb1 N14 84.9(2) . . ? O51 Yb1 N14 130.5(2) . . ? O62 Yb1 N14 104.8(2) . . ? N34 Yb1 N14 134.0(2) . . ? O42 Yb1 N14 126.1(2) . . ? O41 Yb1 O61 143.3(2) . . ? O52 Yb1 O61 75.9(2) . . ? O51 Yb1 O61 72.6(2) . . ? O62 Yb1 O61 52.3(2) . . ? N34 Yb1 O61 121.7(2) . . ? O42 Yb1 O61 143.1(2) . . ? N14 Yb1 O61 71.3(2) . . ? O41 Yb1 N21 77.3(2) . . ? O52 Yb1 N21 149.4(2) . . ? O51 Yb1 N21 156.2(2) . . ? O62 Yb1 N21 82.5(2) . . ? N34 Yb1 N21 66.9(2) . . ? O42 Yb1 N21 112.1(2) . . ? N14 Yb1 N21 67.1(2) . . ? O61 Yb1 N21 104.6(2) . . ? C15 N14 C13 104.6(7) . . ? C15 N14 Yb1 137.8(6) . . ? C13 N14 Yb1 117.1(5) . . ? N11 C15 N14 108.0(8) . . ? N11 C15 C100 123.9(9) . . ? N14 C15 C100 128.1(9) . . ? C15 N11 N12 112.7(7) . . ? C13 N12 N11 101.5(8) . . ? N12 C13 N14 113.2(8) . . ? N12 C13 C22 125.8(8) . . ? N14 C13 C22 121.0(7) . . ? C22 N21 C26 119.0(7) . . ? C22 N21 Yb1 120.2(5) . . ? C26 N21 Yb1 120.7(5) . . ? N21 C22 C23 121.9(8) . . ? N21 C22 C13 114.4(7) . . ? C23 C22 C13 123.7(8) . . ? C24 C23 C22 117.7(8) . . ? C23 C24 C25 120.9(8) . . ? C24 C25 C26 117.7(8) . . ? N21 C26 C25 122.8(8) . . ? N21 C26 C33 113.1(7) . . ? C25 C26 C33 124.0(8) . . ? C35 N34 C33 104.7(7) . . ? C35 N34 Yb1 136.5(6) . . ? C33 N34 Yb1 118.5(5) . . ? N32 C33 N34 114.7(8) . . ? N32 C33 C26 124.8(8) . . ? N34 C33 C26 120.5(7) . . ? C33 N32 N31 101.4(7) . . ? C35 N31 N32 111.9(7) . . ? N34 C35 N31 107.4(8) . . ? N34 C35 C200 126.9(8) . . ? N31 C35 C200 125.7(8) . . ? N43 O41 Yb1 98.3(5) . . ? N43 O42 Yb1 94.4(5) . . ? O44 N43 O41 122.9(9) . . ? O44 N43 O42 123.0(9) . . ? O41 N43 O42 114.1(7) . . ? O44 N43 Yb1 178.1(7) . . ? O41 N43 Yb1 55.3(4) . . ? O42 N43 Yb1 58.8(4) . . ? O54 N53 O51 122.7(9) . . ? O54 N53 O52 122.6(9) . . ? O51 N53 O52 114.7(7) . . ? O54 N53 Yb1 179.1(8) . . ? O51 N53 Yb1 57.6(4) . . ? O52 N53 Yb1 57.1(4) . . ? N53 O51 Yb1 95.5(5) . . ? N53 O52 Yb1 95.8(5) . . ? N63 O61 Yb1 96.1(5) . . ? N63 O62 Yb1 96.5(5) . . ? O64 N63 O61 124.9(8) . . ? O64 N63 O62 120.4(8) . . ? O61 N63 O62 114.7(6) . . ? O64 N63 Yb1 172.5(6) . . ? O61 N63 Yb1 58.4(4) . . ? O62 N63 Yb1 56.7(4) . . ? N100 C101 C102 179.3(13) . . ? _refine_diff_density_max 2.085 _refine_diff_density_min -1.573 _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