Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ahrens, Birte' 'Cotton, S.' 'Noy, Oliver E.' 'Raithby, P.' 'Teat, Simon J.' _publ_contact_author_name 'Prof P Raithby' _publ_contact_author_address ; Prof P Raithby Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_section_title ; Structural variety in nitrate complexes of the heavy lanthanides with 2,2':6',2''-terpyridine, and stereoselective placement of nitrate. ; data_pr9966 _database_code_CSD 169191 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H11 Lu N6 O9' _chemical_formula_weight 594.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0435(4) _cell_length_b 16.5688(6) _cell_length_c 13.2564(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.591(3) _cell_angle_gamma 90.00 _cell_volume 1882.69(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24357 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description colourless _exptl_crystal_colour needle _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 5.309 _exptl_absorpt_correction_type 'semi-empirical multiple scans (SORTAV)' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 1.127 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not applicable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47367 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4289 _reflns_number_gt 3929 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius' B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+1.1902P] 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 'all riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4289 _refine_ls_number_parameters 280 _refine_ls_number_restraints 166 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0455 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.236209(10) 0.153221(5) 0.207604(7) 0.01795(4) Uani 1 1 d . . . N1 N 0.0630(2) 0.14199(12) 0.31092(17) 0.0238(4) Uani 1 1 d U . . C1 C -0.0183(3) 0.20536(17) 0.3277(2) 0.0312(6) Uani 1 1 d U . . H1 H 0.0117 0.2579 0.3132 0.037 Uiso 1 1 calc R . . C2 C -0.1437(3) 0.19775(18) 0.3652(2) 0.0349(6) Uani 1 1 d U . . H2 H -0.1983 0.2441 0.3764 0.042 Uiso 1 1 calc R . . C3 C -0.1880(3) 0.12181(19) 0.3860(2) 0.0337(6) Uani 1 1 d U . . H3 H -0.2753 0.1148 0.4102 0.040 Uiso 1 1 calc R . . C4 C -0.1036(3) 0.05560(17) 0.37115(19) 0.0296(5) Uani 1 1 d U . . H4 H -0.1311 0.0027 0.3863 0.035 Uiso 1 1 calc R . . C5 C 0.0220(3) 0.06767(15) 0.33373(18) 0.0230(5) Uani 1 1 d U . . N2 N 0.2299(2) 0.01999(12) 0.27293(15) 0.0204(4) Uani 1 1 d U . . C6 C 0.1221(3) 0.00070(14) 0.31968(18) 0.0224(5) Uani 1 1 d U . . C7 C 0.1111(3) -0.07726(15) 0.3560(2) 0.0295(5) Uani 1 1 d U . . H7 H 0.0305 -0.0910 0.3845 0.035 Uiso 1 1 calc R . . C8 C 0.2192(3) -0.13415(16) 0.3497(2) 0.0342(6) Uani 1 1 d U . . H8 H 0.2154 -0.1872 0.3758 0.041 Uiso 1 1 calc R . . C9 C 0.3329(3) -0.11382(15) 0.3054(2) 0.0294(5) Uani 1 1 d U . . H9 H 0.4101 -0.1520 0.3029 0.035 Uiso 1 1 calc R . . C10 C 0.3328(2) -0.03671(14) 0.26455(18) 0.0220(4) Uani 1 1 d U . . N3 N 0.4332(2) 0.06774(12) 0.17751(15) 0.0220(4) Uani 1 1 d U . . C11 C 0.4447(3) -0.01001(14) 0.20978(18) 0.0214(4) Uani 1 1 d U . . C12 C 0.5527(3) -0.06210(16) 0.1903(2) 0.0300(5) Uani 1 1 d U . . H12 H 0.5576 -0.1169 0.2124 0.036 Uiso 1 1 calc R . . C13 C 0.6531(3) -0.03382(17) 0.1387(2) 0.0317(6) Uani 1 1 d U . . H13 H 0.7283 -0.0687 0.1255 0.038 Uiso 1 1 calc R . . C14 C 0.6428(3) 0.04528(17) 0.1068(2) 0.0319(6) Uani 1 1 d U . . H14 H 0.7110 0.0663 0.0716 0.038 Uiso 1 1 calc R . . C15 C 0.5305(3) 0.09392(16) 0.1270(2) 0.0274(5) Uani 1 1 d U . . H15 H 0.5223 0.1485 0.1037 0.033 Uiso 1 1 calc R . . N4 N 0.4376(2) 0.22612(13) 0.39232(17) 0.0281(4) Uani 1 1 d . . . O41 O 0.3117(2) 0.26094(11) 0.33961(15) 0.0312(4) Uani 1 1 d . . . O42 O 0.4528(2) 0.15426(10) 0.36337(16) 0.0338(4) Uani 1 1 d . . . O43 O 0.5379(2) 0.25904(13) 0.46358(16) 0.0444(5) Uani 1 1 d . . . N5 N 0.0203(2) 0.10774(13) 0.01174(17) 0.0314(5) Uani 1 1 d . . . O51 O 0.1606(2) 0.12538(13) 0.02083(15) 0.0365(4) Uani 1 1 d . . . O52 O -0.0126(2) 0.11046(13) 0.09804(14) 0.0366(4) Uani 1 1 d . . . O53 O -0.0747(3) 0.09044(15) -0.07295(16) 0.0555(6) Uani 1 1 d . . . N6 N 0.2372(2) 0.30111(12) 0.10831(16) 0.0292(5) Uani 1 1 d . . . O61 O 0.35873(19) 0.25609(10) 0.14000(15) 0.0303(4) Uani 1 1 d . . . O62 O 0.11569(19) 0.27383(10) 0.12519(15) 0.0311(4) Uani 1 1 d . . . O63 O 0.2392(3) 0.36607(12) 0.06644(17) 0.0447(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01719(6) 0.01572(6) 0.02264(6) -0.00038(3) 0.00873(4) 0.00058(3) N1 0.0240(10) 0.0256(10) 0.0247(11) -0.0001(8) 0.0119(9) 0.0021(8) C1 0.0316(13) 0.0317(14) 0.0343(14) -0.0009(11) 0.0161(11) 0.0079(11) C2 0.0290(13) 0.0461(16) 0.0328(14) -0.0018(12) 0.0144(11) 0.0118(12) C3 0.0241(12) 0.0551(17) 0.0241(13) 0.0003(12) 0.0108(10) 0.0021(12) C4 0.0229(11) 0.0422(15) 0.0253(12) 0.0016(11) 0.0102(10) -0.0047(10) C5 0.0212(11) 0.0313(12) 0.0166(11) -0.0007(9) 0.0060(9) -0.0016(9) N2 0.0205(9) 0.0189(10) 0.0213(9) -0.0010(7) 0.0058(7) -0.0019(7) C6 0.0227(11) 0.0254(12) 0.0195(11) -0.0013(9) 0.0072(9) -0.0041(9) C7 0.0339(13) 0.0279(13) 0.0279(13) 0.0041(10) 0.0116(11) -0.0053(10) C8 0.0458(16) 0.0216(12) 0.0341(15) 0.0058(11) 0.0113(12) -0.0034(11) C9 0.0321(13) 0.0212(12) 0.0336(14) 0.0022(10) 0.0086(11) 0.0047(10) C10 0.0219(10) 0.0206(11) 0.0214(11) -0.0032(9) 0.0040(9) -0.0005(9) N3 0.0222(9) 0.0214(10) 0.0236(10) -0.0019(8) 0.0092(8) 0.0016(8) C11 0.0217(11) 0.0196(11) 0.0218(11) -0.0021(9) 0.0054(9) 0.0029(9) C12 0.0317(12) 0.0272(13) 0.0299(13) -0.0034(10) 0.0083(11) 0.0086(10) C13 0.0256(12) 0.0411(15) 0.0289(13) -0.0061(11) 0.0094(10) 0.0114(11) C14 0.0231(11) 0.0474(16) 0.0279(13) -0.0066(12) 0.0121(10) -0.0002(11) C15 0.0265(12) 0.0274(13) 0.0317(13) -0.0008(10) 0.0142(10) -0.0002(10) N4 0.0267(10) 0.0292(11) 0.0302(11) -0.0073(9) 0.0118(9) -0.0040(9) O41 0.0306(9) 0.0254(9) 0.0372(10) -0.0042(8) 0.0102(8) 0.0024(7) O42 0.0297(10) 0.0288(11) 0.0381(11) -0.0100(7) 0.0038(9) 0.0065(7) O43 0.0378(10) 0.0482(13) 0.0400(11) -0.0201(10) 0.0023(9) -0.0076(9) N5 0.0317(11) 0.0292(12) 0.0291(11) -0.0013(9) 0.0038(9) -0.0006(9) O51 0.0277(9) 0.0497(12) 0.0336(10) -0.0105(9) 0.0122(8) 0.0009(9) O52 0.0281(9) 0.0526(13) 0.0284(10) 0.0012(9) 0.0081(8) -0.0126(9) O53 0.0511(13) 0.0704(16) 0.0312(11) -0.0108(11) -0.0063(10) -0.0123(11) N6 0.0387(12) 0.0195(10) 0.0273(11) 0.0009(8) 0.0073(9) 0.0002(9) O61 0.0280(8) 0.0228(9) 0.0429(11) 0.0025(8) 0.0155(8) -0.0006(7) O62 0.0267(9) 0.0262(9) 0.0408(10) 0.0027(8) 0.0112(8) 0.0039(7) O63 0.0633(14) 0.0236(10) 0.0439(12) 0.0115(9) 0.0125(11) -0.0014(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 Lu1 O42 2.3498(19) . ? Lu1 O61 2.3599(16) . ? Lu1 O52 2.3643(17) . ? Lu1 O62 2.3697(17) . ? Lu1 N2 2.3786(19) . ? Lu1 O51 2.3940(18) . ? Lu1 N1 2.3945(19) . ? Lu1 N3 2.4065(18) . ? Lu1 O41 2.4397(18) . ? Lu1 N6 2.783(2) . ? Lu1 N5 2.809(2) . ? Lu1 N4 2.816(2) . ? N1 C1 1.340(3) . ? N1 C5 1.348(3) . ? C1 C2 1.382(3) . ? C2 C3 1.374(4) . ? C3 C4 1.386(4) . ? C4 C5 1.391(3) . ? C5 C6 1.480(3) . ? N2 C6 1.350(3) . ? N2 C10 1.352(3) . ? C6 C7 1.393(3) . ? C7 C8 1.380(4) . ? C8 C9 1.378(4) . ? C9 C10 1.388(3) . ? C10 C11 1.488(3) . ? N3 C15 1.337(3) . ? N3 C11 1.351(3) . ? C11 C12 1.388(3) . ? C12 C13 1.382(4) . ? C13 C14 1.371(4) . ? C14 C15 1.388(3) . ? N4 O43 1.211(3) . ? N4 O41 1.269(3) . ? N4 O42 1.272(3) . ? N5 O53 1.211(3) . ? N5 O51 1.270(3) . ? N5 O52 1.272(3) . ? N6 O63 1.214(3) . ? N6 O62 1.273(3) . ? N6 O61 1.283(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O42 Lu1 O61 88.15(7) . . ? O42 Lu1 O52 154.88(7) . . ? O61 Lu1 O52 116.95(6) . . ? O42 Lu1 O62 122.07(6) . . ? O61 Lu1 O62 54.44(6) . . ? O52 Lu1 O62 76.21(7) . . ? O42 Lu1 N2 78.28(6) . . ? O61 Lu1 N2 151.31(6) . . ? O52 Lu1 N2 79.45(7) . . ? O62 Lu1 N2 152.81(6) . . ? O42 Lu1 O51 142.51(6) . . ? O61 Lu1 O51 76.13(7) . . ? O52 Lu1 O51 53.48(6) . . ? O62 Lu1 O51 75.40(7) . . ? N2 Lu1 O51 99.54(7) . . ? O42 Lu1 N1 90.69(7) . . ? O61 Lu1 N1 138.19(6) . . ? O52 Lu1 N1 70.12(7) . . ? O62 Lu1 N1 92.33(6) . . ? N2 Lu1 N1 67.89(6) . . ? O51 Lu1 N1 123.60(7) . . ? O42 Lu1 N3 72.32(6) . . ? O61 Lu1 N3 84.27(6) . . ? O52 Lu1 N3 109.36(7) . . ? O62 Lu1 N3 132.52(6) . . ? N2 Lu1 N3 67.62(6) . . ? O51 Lu1 N3 72.39(6) . . ? N1 Lu1 N3 134.67(7) . . ? O42 Lu1 O41 53.14(6) . . ? O61 Lu1 O41 71.71(6) . . ? O52 Lu1 O41 130.82(6) . . ? O62 Lu1 O41 72.31(6) . . ? N2 Lu1 O41 116.84(6) . . ? O51 Lu1 O41 143.62(7) . . ? N1 Lu1 O41 74.40(6) . . ? N3 Lu1 O41 119.79(6) . . ? O42 Lu1 N6 106.36(6) . . ? O61 Lu1 N6 27.34(6) . . ? O52 Lu1 N6 96.85(6) . . ? O62 Lu1 N6 27.11(6) . . ? N2 Lu1 N6 173.44(6) . . ? O51 Lu1 N6 73.94(7) . . ? N1 Lu1 N6 116.13(6) . . ? N3 Lu1 N6 109.00(6) . . ? O41 Lu1 N6 69.68(6) . . ? O42 Lu1 N5 162.42(6) . . ? O61 Lu1 N5 96.59(6) . . ? O52 Lu1 N5 26.73(6) . . ? O62 Lu1 N5 73.63(6) . . ? N2 Lu1 N5 89.84(6) . . ? O51 Lu1 N5 26.76(6) . . ? N1 Lu1 N5 96.85(7) . . ? N3 Lu1 N5 91.25(6) . . ? O41 Lu1 N5 144.33(6) . . ? N6 Lu1 N5 84.56(6) . . ? O42 Lu1 N4 26.60(6) . . ? O61 Lu1 N4 76.62(6) . . ? O52 Lu1 N4 152.59(6) . . ? O62 Lu1 N4 96.55(6) . . ? N2 Lu1 N4 99.52(6) . . ? O51 Lu1 N4 150.97(6) . . ? N1 Lu1 N4 84.01(6) . . ? N3 Lu1 N4 95.11(6) . . ? O41 Lu1 N4 26.73(6) . . ? N6 Lu1 N4 86.26(6) . . ? N5 Lu1 N4 170.15(6) . . ? C1 N1 C5 118.3(2) . . ? C1 N1 Lu1 121.85(17) . . ? C5 N1 Lu1 118.41(15) . . ? N1 C1 C2 123.0(3) . . ? C3 C2 C1 118.7(2) . . ? C2 C3 C4 119.2(2) . . ? C3 C4 C5 119.1(2) . . ? N1 C5 C4 121.7(2) . . ? N1 C5 C6 115.74(19) . . ? C4 C5 C6 122.6(2) . . ? C6 N2 C10 119.4(2) . . ? C6 N2 Lu1 119.45(15) . . ? C10 N2 Lu1 121.20(14) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 116.1(2) . . ? C7 C6 C5 122.5(2) . . ? C8 C7 C6 118.9(2) . . ? C9 C8 C7 119.9(2) . . ? C8 C9 C10 118.9(2) . . ? N2 C10 C9 121.5(2) . . ? N2 C10 C11 115.2(2) . . ? C9 C10 C11 123.2(2) . . ? C15 N3 C11 118.15(19) . . ? C15 N3 Lu1 122.17(16) . . ? C11 N3 Lu1 119.66(14) . . ? N3 C11 C12 121.4(2) . . ? N3 C11 C10 116.26(19) . . ? C12 C11 C10 122.3(2) . . ? C13 C12 C11 119.6(2) . . ? C14 C13 C12 119.1(2) . . ? C13 C14 C15 118.5(2) . . ? N3 C15 C14 123.2(2) . . ? O43 N4 O41 122.8(2) . . ? O43 N4 O42 122.1(2) . . ? O41 N4 O42 115.1(2) . . ? O43 N4 Lu1 170.97(17) . . ? O41 N4 Lu1 59.88(11) . . ? O42 N4 Lu1 55.82(12) . . ? N4 O41 Lu1 93.39(13) . . ? N4 O42 Lu1 97.58(14) . . ? O53 N5 O51 122.4(2) . . ? O53 N5 O52 122.8(2) . . ? O51 N5 O52 114.8(2) . . ? O53 N5 Lu1 178.0(2) . . ? O51 N5 Lu1 58.10(12) . . ? O52 N5 Lu1 56.76(11) . . ? N5 O51 Lu1 95.15(14) . . ? N5 O52 Lu1 96.51(13) . . ? O63 N6 O62 122.3(2) . . ? O63 N6 O61 122.0(2) . . ? O62 N6 O61 115.69(19) . . ? O63 N6 Lu1 179.02(19) . . ? O62 N6 Lu1 58.05(11) . . ? O61 N6 Lu1 57.65(11) . . ? N6 O61 Lu1 95.02(13) . . ? N6 O62 Lu1 94.85(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O42 Lu1 N1 C1 102.87(19) . . . . ? O61 Lu1 N1 C1 14.9(2) . . . . ? O52 Lu1 N1 C1 -93.7(2) . . . . ? O62 Lu1 N1 C1 -19.3(2) . . . . ? N2 Lu1 N1 C1 179.9(2) . . . . ? O51 Lu1 N1 C1 -93.2(2) . . . . ? N3 Lu1 N1 C1 168.35(17) . . . . ? O41 Lu1 N1 C1 51.65(19) . . . . ? N6 Lu1 N1 C1 -5.8(2) . . . . ? N5 Lu1 N1 C1 -93.0(2) . . . . ? N4 Lu1 N1 C1 77.1(2) . . . . ? O42 Lu1 N1 C5 -91.00(17) . . . . ? O61 Lu1 N1 C5 -178.99(15) . . . . ? O52 Lu1 N1 C5 72.42(17) . . . . ? O62 Lu1 N1 C5 146.86(17) . . . . ? N2 Lu1 N1 C5 -13.95(16) . . . . ? O51 Lu1 N1 C5 72.88(19) . . . . ? N3 Lu1 N1 C5 -25.5(2) . . . . ? O41 Lu1 N1 C5 -142.23(18) . . . . ? N6 Lu1 N1 C5 160.36(16) . . . . ? N5 Lu1 N1 C5 73.08(18) . . . . ? N4 Lu1 N1 C5 -116.79(18) . . . . ? C5 N1 C1 C2 -1.4(4) . . . . ? Lu1 N1 C1 C2 164.8(2) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C1 N1 C5 C4 1.7(4) . . . . ? Lu1 N1 C5 C4 -164.92(17) . . . . ? C1 N1 C5 C6 -176.4(2) . . . . ? Lu1 N1 C5 C6 17.0(3) . . . . ? C3 C4 C5 N1 -0.5(4) . . . . ? C3 C4 C5 C6 177.5(2) . . . . ? O42 Lu1 N2 C6 104.94(17) . . . . ? O61 Lu1 N2 C6 168.34(15) . . . . ? O52 Lu1 N2 C6 -63.34(16) . . . . ? O62 Lu1 N2 C6 -36.6(2) . . . . ? O51 Lu1 N2 C6 -113.17(16) . . . . ? N1 Lu1 N2 C6 9.34(16) . . . . ? N3 Lu1 N2 C6 -179.54(18) . . . . ? O41 Lu1 N2 C6 67.27(17) . . . . ? N6 Lu1 N2 C6 -119.5(5) . . . . ? N5 Lu1 N2 C6 -88.12(17) . . . . ? N4 Lu1 N2 C6 88.83(16) . . . . ? O42 Lu1 N2 C10 -74.75(17) . . . . ? O61 Lu1 N2 C10 -11.4(2) . . . . ? O52 Lu1 N2 C10 116.97(17) . . . . ? O62 Lu1 N2 C10 143.70(16) . . . . ? O51 Lu1 N2 C10 67.14(17) . . . . ? N1 Lu1 N2 C10 -170.35(18) . . . . ? N3 Lu1 N2 C10 0.77(16) . . . . ? O41 Lu1 N2 C10 -112.42(16) . . . . ? N6 Lu1 N2 C10 60.8(6) . . . . ? N5 Lu1 N2 C10 92.19(17) . . . . ? N4 Lu1 N2 C10 -90.86(17) . . . . ? C10 N2 C6 C7 -2.4(3) . . . . ? Lu1 N2 C6 C7 177.92(17) . . . . ? C10 N2 C6 C5 175.2(2) . . . . ? Lu1 N2 C6 C5 -4.5(3) . . . . ? N1 C5 C6 N2 -8.2(3) . . . . ? C4 C5 C6 N2 173.7(2) . . . . ? N1 C5 C6 C7 169.3(2) . . . . ? C4 C5 C6 C7 -8.8(4) . . . . ? N2 C6 C7 C8 4.1(4) . . . . ? C5 C6 C7 C8 -173.3(2) . . . . ? C6 C7 C8 C9 -1.7(4) . . . . ? C7 C8 C9 C10 -2.2(4) . . . . ? C6 N2 C10 C9 -1.7(3) . . . . ? Lu1 N2 C10 C9 177.97(17) . . . . ? C6 N2 C10 C11 178.76(19) . . . . ? Lu1 N2 C10 C11 -1.5(3) . . . . ? C8 C9 C10 N2 4.0(4) . . . . ? C8 C9 C10 C11 -176.5(2) . . . . ? O42 Lu1 N3 C15 -97.29(19) . . . . ? O61 Lu1 N3 C15 -7.41(18) . . . . ? O52 Lu1 N3 C15 109.17(18) . . . . ? O62 Lu1 N3 C15 20.3(2) . . . . ? N2 Lu1 N3 C15 178.4(2) . . . . ? O51 Lu1 N3 C15 69.82(18) . . . . ? N1 Lu1 N3 C15 -170.00(17) . . . . ? O41 Lu1 N3 C15 -72.52(19) . . . . ? N6 Lu1 N3 C15 4.41(19) . . . . ? N5 Lu1 N3 C15 89.09(18) . . . . ? N4 Lu1 N3 C15 -83.39(18) . . . . ? O42 Lu1 N3 C11 84.50(17) . . . . ? O61 Lu1 N3 C11 174.38(17) . . . . ? O52 Lu1 N3 C11 -69.04(17) . . . . ? O62 Lu1 N3 C11 -157.86(15) . . . . ? N2 Lu1 N3 C11 0.20(16) . . . . ? O51 Lu1 N3 C11 -108.39(17) . . . . ? N1 Lu1 N3 C11 11.8(2) . . . . ? O41 Lu1 N3 C11 109.27(17) . . . . ? N6 Lu1 N3 C11 -173.79(16) . . . . ? N5 Lu1 N3 C11 -89.12(17) . . . . ? N4 Lu1 N3 C11 98.41(17) . . . . ? C15 N3 C11 C12 -0.8(3) . . . . ? Lu1 N3 C11 C12 177.52(17) . . . . ? C15 N3 C11 C10 -179.3(2) . . . . ? Lu1 N3 C11 C10 -1.0(3) . . . . ? N2 C10 C11 N3 1.7(3) . . . . ? C9 C10 C11 N3 -177.9(2) . . . . ? N2 C10 C11 C12 -176.9(2) . . . . ? C9 C10 C11 C12 3.6(4) . . . . ? N3 C11 C12 C13 1.3(4) . . . . ? C10 C11 C12 C13 179.7(2) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? C11 N3 C15 C14 -0.4(4) . . . . ? Lu1 N3 C15 C14 -178.63(18) . . . . ? C13 C14 C15 N3 1.0(4) . . . . ? O42 Lu1 N4 O43 79.3(11) . . . . ? O61 Lu1 N4 O43 -34.3(12) . . . . ? O52 Lu1 N4 O43 -157.9(11) . . . . ? O62 Lu1 N4 O43 -85.3(12) . . . . ? N2 Lu1 N4 O43 116.7(12) . . . . ? O51 Lu1 N4 O43 -13.7(12) . . . . ? N1 Lu1 N4 O43 -177.0(12) . . . . ? N3 Lu1 N4 O43 48.6(12) . . . . ? O41 Lu1 N4 O43 -110.1(12) . . . . ? N6 Lu1 N4 O43 -60.2(12) . . . . ? N5 Lu1 N4 O43 -81.4(12) . . . . ? O42 Lu1 N4 O41 -170.6(2) . . . . ? O61 Lu1 N4 O41 75.81(13) . . . . ? O52 Lu1 N4 O41 -47.8(2) . . . . ? O62 Lu1 N4 O41 24.79(13) . . . . ? N2 Lu1 N4 O41 -133.21(13) . . . . ? O51 Lu1 N4 O41 96.37(17) . . . . ? N1 Lu1 N4 O41 -66.87(13) . . . . ? N3 Lu1 N4 O41 158.67(13) . . . . ? N6 Lu1 N4 O41 49.91(13) . . . . ? N5 Lu1 N4 O41 28.6(4) . . . . ? O61 Lu1 N4 O42 -113.62(15) . . . . ? O52 Lu1 N4 O42 122.78(18) . . . . ? O62 Lu1 N4 O42 -164.65(15) . . . . ? N2 Lu1 N4 O42 37.36(15) . . . . ? O51 Lu1 N4 O42 -93.07(19) . . . . ? N1 Lu1 N4 O42 103.69(15) . . . . ? N3 Lu1 N4 O42 -30.76(15) . . . . ? O41 Lu1 N4 O42 170.6(2) . . . . ? N6 Lu1 N4 O42 -139.53(15) . . . . ? N5 Lu1 N4 O42 -160.8(3) . . . . ? O43 N4 O41 Lu1 169.9(2) . . . . ? O42 N4 O41 Lu1 -8.6(2) . . . . ? O42 Lu1 O41 N4 5.26(12) . . . . ? O61 Lu1 O41 N4 -96.58(13) . . . . ? O52 Lu1 O41 N4 153.22(12) . . . . ? O62 Lu1 O41 N4 -154.07(14) . . . . ? N2 Lu1 O41 N4 53.67(14) . . . . ? O51 Lu1 O41 N4 -125.60(14) . . . . ? N1 Lu1 O41 N4 108.27(14) . . . . ? N3 Lu1 O41 N4 -24.67(15) . . . . ? N6 Lu1 O41 N4 -125.50(14) . . . . ? N5 Lu1 O41 N4 -171.92(12) . . . . ? O43 N4 O42 Lu1 -169.5(2) . . . . ? O41 N4 O42 Lu1 9.0(2) . . . . ? O61 Lu1 O42 N4 63.10(14) . . . . ? O52 Lu1 O42 N4 -114.28(18) . . . . ? O62 Lu1 O42 N4 18.08(17) . . . . ? N2 Lu1 O42 N4 -142.33(15) . . . . ? O51 Lu1 O42 N4 127.23(15) . . . . ? N1 Lu1 O42 N4 -75.09(15) . . . . ? N3 Lu1 O42 N4 147.68(16) . . . . ? O41 Lu1 O42 N4 -5.29(12) . . . . ? N6 Lu1 O42 N4 42.46(15) . . . . ? N5 Lu1 O42 N4 169.26(18) . . . . ? O42 Lu1 N5 O53 -168(5) . . . . ? O61 Lu1 N5 O53 -64(6) . . . . ? O52 Lu1 N5 O53 78(6) . . . . ? O62 Lu1 N5 O53 -14(6) . . . . ? N2 Lu1 N5 O53 144(6) . . . . ? O51 Lu1 N5 O53 -104(6) . . . . ? N1 Lu1 N5 O53 77(6) . . . . ? N3 Lu1 N5 O53 -148(6) . . . . ? O41 Lu1 N5 O53 4(6) . . . . ? N6 Lu1 N5 O53 -39(6) . . . . ? N4 Lu1 N5 O53 -18(6) . . . . ? O42 Lu1 N5 O51 -64.8(3) . . . . ? O61 Lu1 N5 O51 40.05(15) . . . . ? O52 Lu1 N5 O51 -178.3(2) . . . . ? O62 Lu1 N5 O51 89.96(15) . . . . ? N2 Lu1 N5 O51 -111.93(15) . . . . ? N1 Lu1 N5 O51 -179.62(15) . . . . ? N3 Lu1 N5 O51 -44.32(15) . . . . ? O41 Lu1 N5 O51 107.67(16) . . . . ? N6 Lu1 N5 O51 64.64(15) . . . . ? N4 Lu1 N5 O51 86.0(4) . . . . ? O42 Lu1 N5 O52 113.4(2) . . . . ? O61 Lu1 N5 O52 -141.70(15) . . . . ? O62 Lu1 N5 O52 -91.79(15) . . . . ? N2 Lu1 N5 O52 66.32(15) . . . . ? O51 Lu1 N5 O52 178.3(2) . . . . ? N1 Lu1 N5 O52 -1.37(16) . . . . ? N3 Lu1 N5 O52 133.93(15) . . . . ? O41 Lu1 N5 O52 -74.08(18) . . . . ? N6 Lu1 N5 O52 -117.10(15) . . . . ? N4 Lu1 N5 O52 -95.8(4) . . . . ? O53 N5 O51 Lu1 177.7(2) . . . . ? O52 N5 O51 Lu1 -1.6(2) . . . . ? O42 Lu1 O51 N5 153.31(13) . . . . ? O61 Lu1 O51 N5 -138.82(15) . . . . ? O52 Lu1 O51 N5 0.98(14) . . . . ? O62 Lu1 O51 N5 -82.50(15) . . . . ? N2 Lu1 O51 N5 70.16(15) . . . . ? N1 Lu1 O51 N5 0.45(18) . . . . ? N3 Lu1 O51 N5 132.88(16) . . . . ? O41 Lu1 O51 N5 -110.50(16) . . . . ? N6 Lu1 O51 N5 -110.59(15) . . . . ? N4 Lu1 O51 N5 -159.42(14) . . . . ? O53 N5 O52 Lu1 -177.7(2) . . . . ? O51 N5 O52 Lu1 1.6(2) . . . . ? O42 Lu1 O52 N5 -139.25(16) . . . . ? O61 Lu1 O52 N5 43.69(17) . . . . ? O62 Lu1 O52 N5 80.90(15) . . . . ? N2 Lu1 O52 N5 -111.32(15) . . . . ? O51 Lu1 O52 N5 -0.98(14) . . . . ? N1 Lu1 O52 N5 178.55(17) . . . . ? N3 Lu1 O52 N5 -49.75(16) . . . . ? O41 Lu1 O52 N5 132.19(14) . . . . ? N6 Lu1 O52 N5 63.19(15) . . . . ? N4 Lu1 O52 N5 158.31(14) . . . . ? O42 Lu1 N6 O63 -18(11) . . . . ? O61 Lu1 N6 O63 -68(11) . . . . ? O52 Lu1 N6 O63 152(11) . . . . ? O62 Lu1 N6 O63 112(11) . . . . ? N2 Lu1 N6 O63 -152(11) . . . . ? O51 Lu1 N6 O63 -159(11) . . . . ? N1 Lu1 N6 O63 81(11) . . . . ? N3 Lu1 N6 O63 -95(11) . . . . ? O41 Lu1 N6 O63 21(11) . . . . ? N5 Lu1 N6 O63 176(100) . . . . ? N4 Lu1 N6 O63 0(11) . . . . ? O42 Lu1 N6 O62 -129.87(13) . . . . ? O61 Lu1 N6 O62 -180.0(2) . . . . ? O52 Lu1 N6 O62 40.41(14) . . . . ? N2 Lu1 N6 O62 95.7(5) . . . . ? O51 Lu1 N6 O62 89.24(14) . . . . ? N1 Lu1 N6 O62 -30.78(15) . . . . ? N3 Lu1 N6 O62 153.64(13) . . . . ? O41 Lu1 N6 O62 -90.71(14) . . . . ? N5 Lu1 N6 O62 64.19(14) . . . . ? N4 Lu1 N6 O62 -112.24(14) . . . . ? O42 Lu1 N6 O61 50.12(14) . . . . ? O52 Lu1 N6 O61 -139.60(14) . . . . ? O62 Lu1 N6 O61 180.0(2) . . . . ? N2 Lu1 N6 O61 -84.3(6) . . . . ? O51 Lu1 N6 O61 -90.77(14) . . . . ? N1 Lu1 N6 O61 149.21(13) . . . . ? N3 Lu1 N6 O61 -26.37(15) . . . . ? O41 Lu1 N6 O61 89.28(13) . . . . ? N5 Lu1 N6 O61 -115.82(14) . . . . ? N4 Lu1 N6 O61 67.75(13) . . . . ? O63 N6 O61 Lu1 178.9(2) . . . . ? O62 N6 O61 Lu1 0.0(2) . . . . ? O42 Lu1 O61 N6 -132.54(14) . . . . ? O52 Lu1 O61 N6 46.21(15) . . . . ? O62 Lu1 O61 N6 0.00(12) . . . . ? N2 Lu1 O61 N6 166.29(13) . . . . ? O51 Lu1 O61 N6 81.80(14) . . . . ? N1 Lu1 O61 N6 -43.58(18) . . . . ? N3 Lu1 O61 N6 155.04(14) . . . . ? O41 Lu1 O61 N6 -80.97(13) . . . . ? N5 Lu1 O61 N6 64.43(14) . . . . ? N4 Lu1 O61 N6 -108.31(14) . . . . ? O63 N6 O62 Lu1 -178.9(2) . . . . ? O61 N6 O62 Lu1 0.0(2) . . . . ? O42 Lu1 O62 N6 60.35(15) . . . . ? O61 Lu1 O62 N6 0.01(12) . . . . ? O52 Lu1 O62 N6 -138.50(14) . . . . ? N2 Lu1 O62 N6 -165.59(14) . . . . ? O51 Lu1 O62 N6 -83.20(14) . . . . ? N1 Lu1 O62 N6 152.62(14) . . . . ? N3 Lu1 O62 N6 -34.72(17) . . . . ? O41 Lu1 O62 N6 79.81(14) . . . . ? N5 Lu1 O62 N6 -110.92(14) . . . . ? N4 Lu1 O62 N6 68.39(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.990 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.088 ####END data_pr9928 _database_code_CSD 169192 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 N6 O10 Yb' _chemical_formula_weight 638.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6800(10) _cell_length_b 21.8770(10) _cell_length_c 11.2990(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.590(10) _cell_angle_gamma 90.00 _cell_volume 2144.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 33287 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 4.429 _exptl_absorpt_correction_type 'semi empirical multiple scans' _exptl_absorpt_correction_T_min 0.6913 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not applicable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7217 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3735 _reflns_number_gt 3280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius HKL Scalepack' _computing_data_reduction 'Nonius HKL Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. One Oxygen Atom of one of the Nitrate Anions (O63) was refined as disorderd on two positions, with occupancies 0.4 and 0.6. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0015P)^2^+7.3432P] 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 'methyl and OH rigid, others riding' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00182(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3735 _refine_ls_number_parameters 318 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.57301(2) 0.622268(9) 0.323145(18) 0.02693(11) Uani 1 1 d . . . N1 N 0.7905(5) 0.68684(18) 0.2649(4) 0.0311(9) Uani 1 1 d DU . . C1 C 0.9181(6) 0.6622(3) 0.2176(5) 0.0398(13) Uani 1 1 d DU . . H1 H 0.9232 0.6191 0.2091 0.048 Uiso 1 1 calc R . . C2 C 1.0405(6) 0.6967(3) 0.1811(5) 0.0413(13) Uani 1 1 d DU . . H2 H 1.1275 0.6776 0.1479 0.050 Uiso 1 1 calc R . . C3 C 1.0350(6) 0.7593(3) 0.1936(5) 0.0386(12) Uani 1 1 d DU . . H3 H 1.1189 0.7840 0.1703 0.046 Uiso 1 1 calc R . . C4 C 0.9051(6) 0.7855(2) 0.2407(4) 0.0345(11) Uani 1 1 d DU . . H4 H 0.8986 0.8286 0.2496 0.041 Uiso 1 1 calc R . . C5 C 0.7846(5) 0.7483(2) 0.2748(4) 0.0280(10) Uani 1 1 d DU . . N2 N 0.5341(4) 0.73235(18) 0.3534(3) 0.0268(9) Uani 1 1 d DU . . C6 C 0.6399(5) 0.7734(2) 0.3217(4) 0.0286(10) Uani 1 1 d DU . . C7 C 0.6117(6) 0.8362(2) 0.3283(5) 0.0397(13) Uani 1 1 d DU . . H7 H 0.6894 0.8647 0.3087 0.048 Uiso 1 1 calc R . . C8 C 0.4710(6) 0.8559(3) 0.3631(5) 0.0479(14) Uani 1 1 d DU . . H8 H 0.4487 0.8984 0.3643 0.058 Uiso 1 1 calc R . . C9 C 0.3630(6) 0.8149(2) 0.3960(5) 0.0409(13) Uani 1 1 d DU . . H9 H 0.2651 0.8285 0.4210 0.049 Uiso 1 1 calc R . . C10 C 0.3971(5) 0.7527(2) 0.3928(4) 0.0305(11) Uani 1 1 d DU . . N3 N 0.3363(4) 0.64681(19) 0.4256(3) 0.0317(9) Uani 1 1 d U . . C11 C 0.2902(5) 0.7049(2) 0.4335(4) 0.0317(11) Uani 1 1 d U . . C12 C 0.1477(6) 0.7200(3) 0.4824(5) 0.0407(13) Uani 1 1 d U . . H12 H 0.1152 0.7614 0.4869 0.049 Uiso 1 1 calc R . . C13 C 0.0559(6) 0.6736(3) 0.5237(5) 0.0488(14) Uani 1 1 d U . . H13 H -0.0410 0.6827 0.5566 0.059 Uiso 1 1 calc R . . C14 C 0.1046(7) 0.6154(3) 0.5170(5) 0.0504(15) Uani 1 1 d U . . H14 H 0.0429 0.5832 0.5462 0.061 Uiso 1 1 calc R . . C15 C 0.2451(6) 0.6027(3) 0.4675(5) 0.0418(13) Uani 1 1 d U . . H15 H 0.2780 0.5613 0.4629 0.050 Uiso 1 1 calc R . . N4 N 0.6531(5) 0.6004(2) 0.5644(4) 0.0379(10) Uani 1 1 d . . . O41 O 0.6963(4) 0.64725(15) 0.5050(3) 0.0346(8) Uani 1 1 d . . . O42 O 0.5732(4) 0.56162(17) 0.5092(3) 0.0453(9) Uani 1 1 d . . . O43 O 0.6860(6) 0.5959(2) 0.6698(4) 0.0632(12) Uani 1 1 d . . . N5 N 0.4931(6) 0.6382(2) 0.0803(4) 0.0473(13) Uani 1 1 d . . . O51 O 0.6126(4) 0.6090(2) 0.1111(4) 0.0526(11) Uani 1 1 d . . . O52 O 0.4158(4) 0.66037(17) 0.1650(3) 0.0400(9) Uani 1 1 d . . . O53 O 0.4522(6) 0.6447(2) -0.0228(4) 0.0666(13) Uani 1 1 d . . . N6 N 0.7779(6) 0.4977(2) 0.2655(4) 0.0445(12) Uani 1 1 d . . . O61 O 0.7583(4) 0.55003(17) 0.3123(4) 0.0499(10) Uani 1 1 d . A . O62 O 0.6688(5) 0.46194(18) 0.2585(4) 0.0564(11) Uani 1 1 d . A . O63 O 0.914(3) 0.4803(16) 0.268(2) 0.062(7) Uani 0.40 1 d P A 1 O63' O 0.902(3) 0.4876(11) 0.2153(12) 0.059(4) Uani 0.60 1 d P A 2 O98 O 0.4205(4) 0.53998(15) 0.2710(3) 0.0357(8) Uani 1 1 d . . . H98 H 0.4619 0.5059 0.2846 0.054 Uiso 1 1 calc R . . C98 C 0.2714(6) 0.5309(3) 0.2099(5) 0.0467(14) Uani 1 1 d U . . H98A H 0.2193 0.5709 0.1999 0.056 Uiso 1 1 calc R . . H98B H 0.2057 0.5047 0.2591 0.056 Uiso 1 1 calc R . . C99 C 0.2879(9) 0.5016(4) 0.0902(6) 0.073(2) Uani 1 1 d U . . H99A H 0.3581 0.5260 0.0429 0.109 Uiso 1 1 calc R . . H99B H 0.1868 0.4994 0.0496 0.109 Uiso 1 1 calc R . . H99C H 0.3296 0.4602 0.1002 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02362(13) 0.02312(14) 0.03414(15) -0.00137(10) 0.00234(8) 0.00061(9) N1 0.030(2) 0.030(2) 0.033(2) -0.0001(19) 0.0034(17) -0.0008(18) C1 0.029(3) 0.041(3) 0.049(3) 0.002(3) 0.004(2) -0.001(2) C2 0.031(3) 0.056(3) 0.037(3) 0.002(3) 0.006(2) 0.003(2) C3 0.031(3) 0.050(3) 0.034(3) 0.010(3) 0.000(2) -0.008(2) C4 0.036(3) 0.036(3) 0.031(3) 0.002(2) -0.002(2) -0.006(2) C5 0.030(2) 0.028(3) 0.026(2) 0.002(2) 0.002(2) -0.004(2) N2 0.025(2) 0.028(2) 0.028(2) 0.0002(17) -0.0007(16) 0.0021(16) C6 0.030(2) 0.028(2) 0.028(3) 0.000(2) -0.002(2) 0.002(2) C7 0.043(3) 0.030(3) 0.046(3) 0.005(2) 0.005(3) 0.000(2) C8 0.052(3) 0.028(3) 0.064(4) 0.001(3) 0.010(3) 0.011(2) C9 0.041(3) 0.035(3) 0.047(3) 0.001(3) 0.006(3) 0.012(2) C10 0.029(2) 0.034(3) 0.028(3) -0.003(2) -0.002(2) 0.006(2) N3 0.028(2) 0.035(2) 0.032(2) -0.0004(19) 0.0063(17) -0.0018(18) C11 0.026(2) 0.040(3) 0.029(3) -0.001(2) -0.002(2) 0.001(2) C12 0.031(3) 0.055(3) 0.036(3) -0.010(3) 0.000(2) 0.006(2) C13 0.024(3) 0.077(4) 0.045(3) -0.013(3) 0.004(2) -0.001(3) C14 0.041(3) 0.063(4) 0.047(3) -0.004(3) 0.011(3) -0.018(3) C15 0.037(3) 0.045(3) 0.044(3) 0.003(3) 0.011(2) -0.008(2) N4 0.040(3) 0.035(3) 0.039(3) 0.005(2) -0.005(2) 0.002(2) O41 0.037(2) 0.0271(19) 0.040(2) 0.0009(16) -0.0007(16) -0.0005(15) O42 0.051(2) 0.034(2) 0.050(2) 0.0034(18) -0.0113(19) -0.0104(18) O43 0.091(3) 0.050(3) 0.047(3) 0.014(2) -0.022(2) -0.008(2) N5 0.061(3) 0.048(3) 0.033(3) 0.005(2) 0.001(2) -0.031(3) O51 0.032(2) 0.080(3) 0.046(2) -0.013(2) 0.0056(18) -0.006(2) O52 0.040(2) 0.044(2) 0.036(2) 0.0011(18) -0.0031(17) -0.0007(17) O53 0.095(4) 0.074(3) 0.030(2) 0.011(2) -0.011(2) -0.034(3) N6 0.043(3) 0.027(3) 0.064(3) -0.001(2) 0.008(2) 0.005(2) O61 0.039(2) 0.032(2) 0.078(3) -0.016(2) -0.004(2) 0.0085(17) O62 0.041(2) 0.032(2) 0.097(4) -0.007(2) 0.009(2) -0.0018(19) O63 0.029(8) 0.054(10) 0.10(2) -0.016(16) 0.033(14) 0.008(6) O63' 0.045(6) 0.063(9) 0.071(10) -0.021(9) 0.027(8) 0.000(5) O98 0.0302(18) 0.0257(19) 0.051(2) 0.0001(16) -0.0040(16) 0.0018(14) C98 0.042(3) 0.037(3) 0.061(4) 0.004(3) -0.007(3) -0.007(3) C99 0.089(5) 0.075(5) 0.054(4) 0.002(4) -0.004(4) -0.044(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O61 2.261(4) . ? Yb1 O41 2.355(3) . ? Yb1 O52 2.370(3) . ? Yb1 N3 2.446(4) . ? Yb1 O51 2.447(4) . ? Yb1 N2 2.457(4) . ? Yb1 N1 2.462(4) . ? Yb1 O42 2.486(4) . ? Yb1 N5 2.833(5) . ? Yb1 N4 2.835(5) . ? N1 C5 1.351(6) . ? N1 C1 1.355(6) . ? C1 C2 1.375(7) . ? C2 C3 1.378(8) . ? C3 C4 1.385(7) . ? C4 C5 1.387(7) . ? C5 C6 1.482(7) . ? N2 C6 1.340(6) . ? N2 C10 1.356(6) . ? C6 C7 1.397(7) . ? C7 C8 1.363(7) . ? C8 C9 1.357(7) . ? C9 C10 1.394(7) . ? C10 C11 1.479(7) . ? N3 C11 1.337(6) . ? N3 C15 1.344(6) . ? C11 C12 1.408(7) . ? C12 C13 1.380(8) . ? C13 C14 1.344(9) . ? C14 C15 1.384(8) . ? N4 O43 1.221(6) . ? N4 O42 1.250(5) . ? N4 O41 1.287(5) . ? N5 O53 1.216(6) . ? N5 O51 1.259(6) . ? N5 O52 1.279(6) . ? N6 O62 1.229(6) . ? N6 O63 1.24(3) . ? N6 O63' 1.25(2) . ? N6 O61 1.275(6) . ? O98 C98 1.464(6) . ? C98 C99 1.507(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 O61 Yb1 O41 84.41(13) . . ? O61 Yb1 O52 126.93(14) . . ? O41 Yb1 O52 144.57(12) . . ? O61 Yb1 N3 141.95(15) . . ? O41 Yb1 N3 84.46(12) . . ? O52 Yb1 N3 78.81(13) . . ? O61 Yb1 O51 75.21(15) . . ? O41 Yb1 O51 144.00(12) . . ? O52 Yb1 O51 52.91(13) . . ? N3 Yb1 O51 129.21(13) . . ? O61 Yb1 N2 142.50(13) . . ? O41 Yb1 N2 73.26(12) . . ? O52 Yb1 N2 71.44(12) . . ? N3 Yb1 N2 66.33(13) . . ? O51 Yb1 N2 106.01(14) . . ? O61 Yb1 N1 80.48(14) . . ? O41 Yb1 N1 76.52(13) . . ? O52 Yb1 N1 91.51(13) . . ? N3 Yb1 N1 131.38(13) . . ? O51 Yb1 N1 71.12(13) . . ? N2 Yb1 N1 65.42(13) . . ? O61 Yb1 O42 71.87(15) . . ? O41 Yb1 O42 52.85(12) . . ? O52 Yb1 O42 144.34(12) . . ? N3 Yb1 O42 72.42(13) . . ? O51 Yb1 O42 140.17(14) . . ? N2 Yb1 O42 113.72(12) . . ? N1 Yb1 O42 123.35(13) . . ? O61 Yb1 N5 100.90(16) . . ? O41 Yb1 N5 155.49(12) . . ? O52 Yb1 N5 26.61(14) . . ? N3 Yb1 N5 104.18(15) . . ? O51 Yb1 N5 26.31(14) . . ? N2 Yb1 N5 89.05(14) . . ? N1 Yb1 N5 80.76(13) . . ? O42 Yb1 N5 151.54(12) . . ? O61 Yb1 N4 77.18(14) . . ? O41 Yb1 N4 26.72(12) . . ? O52 Yb1 N4 154.85(13) . . ? N3 Yb1 N4 76.63(13) . . ? O51 Yb1 N4 152.13(14) . . ? N2 Yb1 N4 93.59(13) . . ? N1 Yb1 N4 100.64(13) . . ? O42 Yb1 N4 26.14(12) . . ? N5 Yb1 N4 177.33(14) . . ? C5 N1 C1 117.5(4) . . ? C5 N1 Yb1 121.2(3) . . ? C1 N1 Yb1 121.2(3) . . ? N1 C1 C2 123.2(5) . . ? C1 C2 C3 119.0(5) . . ? C2 C3 C4 118.8(5) . . ? C3 C4 C5 119.5(5) . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 122.4(4) . . ? C6 N2 C10 118.8(4) . . ? C6 N2 Yb1 121.5(3) . . ? C10 N2 Yb1 119.5(3) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 116.2(4) . . ? C7 C6 C5 122.3(4) . . ? C8 C7 C6 119.1(5) . . ? C9 C8 C7 120.1(5) . . ? C8 C9 C10 119.3(5) . . ? N2 C10 C9 121.2(5) . . ? N2 C10 C11 115.7(4) . . ? C9 C10 C11 123.1(4) . . ? C11 N3 C15 118.7(4) . . ? C11 N3 Yb1 119.8(3) . . ? C15 N3 Yb1 121.3(3) . . ? N3 C11 C12 121.1(5) . . ? N3 C11 C10 117.4(4) . . ? C12 C11 C10 121.5(5) . . ? C13 C12 C11 118.8(5) . . ? C14 C13 C12 119.5(5) . . ? C13 C14 C15 119.8(6) . . ? N3 C15 C14 122.1(6) . . ? O43 N4 O42 122.9(5) . . ? O43 N4 O41 120.6(4) . . ? O42 N4 O41 116.5(4) . . ? O43 N4 Yb1 174.8(4) . . ? O42 N4 Yb1 61.2(2) . . ? O41 N4 Yb1 55.4(2) . . ? N4 O41 Yb1 97.9(3) . . ? N4 O42 Yb1 92.7(3) . . ? O53 N5 O51 122.7(5) . . ? O53 N5 O52 121.8(6) . . ? O51 N5 O52 115.5(4) . . ? O53 N5 Yb1 177.2(4) . . ? O51 N5 Yb1 59.5(3) . . ? O52 N5 Yb1 56.1(2) . . ? N5 O51 Yb1 94.2(3) . . ? N5 O52 Yb1 97.3(3) . . ? O62 N6 O63 122.6(17) . . ? O62 N6 O63' 122.1(12) . . ? O63 N6 O63' 28.7(13) . . ? O62 N6 O61 119.1(5) . . ? O63 N6 O61 113.9(16) . . ? O63' N6 O61 118.2(12) . . ? N6 O61 Yb1 138.9(3) . . ? O98 C98 C99 112.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O61 Yb1 N1 C5 -165.0(4) . . . . ? O41 Yb1 N1 C5 -78.5(4) . . . . ? O52 Yb1 N1 C5 67.8(4) . . . . ? N3 Yb1 N1 C5 -8.6(4) . . . . ? O51 Yb1 N1 C5 117.5(4) . . . . ? N2 Yb1 N1 C5 -1.0(3) . . . . ? O42 Yb1 N1 C5 -104.2(4) . . . . ? N5 Yb1 N1 C5 92.2(4) . . . . ? N4 Yb1 N1 C5 -90.1(4) . . . . ? O61 Yb1 N1 C1 17.5(4) . . . . ? O41 Yb1 N1 C1 104.0(4) . . . . ? O52 Yb1 N1 C1 -109.7(4) . . . . ? N3 Yb1 N1 C1 173.9(3) . . . . ? O51 Yb1 N1 C1 -60.0(4) . . . . ? N2 Yb1 N1 C1 -178.5(4) . . . . ? O42 Yb1 N1 C1 78.3(4) . . . . ? N5 Yb1 N1 C1 -85.3(4) . . . . ? N4 Yb1 N1 C1 92.4(4) . . . . ? C5 N1 C1 C2 0.7(7) . . . . ? Yb1 N1 C1 C2 178.4(4) . . . . ? N1 C1 C2 C3 0.4(8) . . . . ? C1 C2 C3 C4 -1.0(8) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C1 N1 C5 C4 -1.4(7) . . . . ? Yb1 N1 C5 C4 -179.0(4) . . . . ? C1 N1 C5 C6 177.2(4) . . . . ? Yb1 N1 C5 C6 -0.4(6) . . . . ? C3 C4 C5 N1 0.8(7) . . . . ? C3 C4 C5 C6 -177.7(4) . . . . ? O61 Yb1 N2 C6 29.1(4) . . . . ? O41 Yb1 N2 C6 85.1(3) . . . . ? O52 Yb1 N2 C6 -98.1(3) . . . . ? N3 Yb1 N2 C6 176.3(4) . . . . ? O51 Yb1 N2 C6 -57.4(3) . . . . ? N1 Yb1 N2 C6 2.5(3) . . . . ? O42 Yb1 N2 C6 119.9(3) . . . . ? N5 Yb1 N2 C6 -77.7(3) . . . . ? N4 Yb1 N2 C6 102.6(3) . . . . ? O61 Yb1 N2 C10 -157.1(3) . . . . ? O41 Yb1 N2 C10 -101.1(3) . . . . ? O52 Yb1 N2 C10 75.7(3) . . . . ? N3 Yb1 N2 C10 -9.9(3) . . . . ? O51 Yb1 N2 C10 116.4(3) . . . . ? N1 Yb1 N2 C10 176.3(4) . . . . ? O42 Yb1 N2 C10 -66.3(4) . . . . ? N5 Yb1 N2 C10 96.1(3) . . . . ? N4 Yb1 N2 C10 -83.6(3) . . . . ? C10 N2 C6 C7 -0.1(6) . . . . ? Yb1 N2 C6 C7 173.7(3) . . . . ? C10 N2 C6 C5 -177.6(4) . . . . ? Yb1 N2 C6 C5 -3.7(5) . . . . ? N1 C5 C6 N2 2.6(6) . . . . ? C4 C5 C6 N2 -178.8(4) . . . . ? N1 C5 C6 C7 -174.8(4) . . . . ? C4 C5 C6 C7 3.8(7) . . . . ? N2 C6 C7 C8 -2.7(7) . . . . ? C5 C6 C7 C8 174.6(5) . . . . ? C6 C7 C8 C9 3.0(9) . . . . ? C7 C8 C9 C10 -0.5(9) . . . . ? C6 N2 C10 C9 2.7(7) . . . . ? Yb1 N2 C10 C9 -171.3(4) . . . . ? C6 N2 C10 C11 -176.1(4) . . . . ? Yb1 N2 C10 C11 9.9(5) . . . . ? C8 C9 C10 N2 -2.4(8) . . . . ? C8 C9 C10 C11 176.3(5) . . . . ? O61 Yb1 N3 C11 156.8(3) . . . . ? O41 Yb1 N3 C11 83.3(4) . . . . ? O52 Yb1 N3 C11 -65.4(4) . . . . ? O51 Yb1 N3 C11 -82.7(4) . . . . ? N2 Yb1 N3 C11 9.1(3) . . . . ? N1 Yb1 N3 C11 16.7(4) . . . . ? O42 Yb1 N3 C11 136.0(4) . . . . ? N5 Yb1 N3 C11 -73.4(4) . . . . ? N4 Yb1 N3 C11 109.2(4) . . . . ? O61 Yb1 N3 C15 -27.8(5) . . . . ? O41 Yb1 N3 C15 -101.4(4) . . . . ? O52 Yb1 N3 C15 110.0(4) . . . . ? O51 Yb1 N3 C15 92.7(4) . . . . ? N2 Yb1 N3 C15 -175.5(4) . . . . ? N1 Yb1 N3 C15 -168.0(4) . . . . ? O42 Yb1 N3 C15 -48.7(4) . . . . ? N5 Yb1 N3 C15 101.9(4) . . . . ? N4 Yb1 N3 C15 -75.5(4) . . . . ? C15 N3 C11 C12 -1.3(7) . . . . ? Yb1 N3 C11 C12 174.2(4) . . . . ? C15 N3 C11 C10 176.7(4) . . . . ? Yb1 N3 C11 C10 -7.9(6) . . . . ? N2 C10 C11 N3 -1.4(6) . . . . ? C9 C10 C11 N3 179.9(5) . . . . ? N2 C10 C11 C12 176.5(4) . . . . ? C9 C10 C11 C12 -2.2(8) . . . . ? N3 C11 C12 C13 0.7(8) . . . . ? C10 C11 C12 C13 -177.1(5) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C12 C13 C14 C15 -0.9(9) . . . . ? C11 N3 C15 C14 0.8(8) . . . . ? Yb1 N3 C15 C14 -174.6(4) . . . . ? C13 C14 C15 N3 0.3(9) . . . . ? O61 Yb1 N4 O43 142(4) . . . . ? O41 Yb1 N4 O43 39(4) . . . . ? O52 Yb1 N4 O43 -53(4) . . . . ? N3 Yb1 N4 O43 -65(4) . . . . ? O51 Yb1 N4 O43 135(4) . . . . ? N2 Yb1 N4 O43 -1(4) . . . . ? N1 Yb1 N4 O43 65(4) . . . . ? O42 Yb1 N4 O43 -143(4) . . . . ? N5 Yb1 N4 O43 -173(4) . . . . ? O61 Yb1 N4 O42 -74.9(3) . . . . ? O41 Yb1 N4 O42 -178.2(5) . . . . ? O52 Yb1 N4 O42 90.0(4) . . . . ? N3 Yb1 N4 O42 77.3(3) . . . . ? O51 Yb1 N4 O42 -82.9(4) . . . . ? N2 Yb1 N4 O42 141.9(3) . . . . ? N1 Yb1 N4 O42 -152.5(3) . . . . ? N5 Yb1 N4 O42 -31(3) . . . . ? O61 Yb1 N4 O41 103.3(3) . . . . ? O52 Yb1 N4 O41 -91.9(4) . . . . ? N3 Yb1 N4 O41 -104.6(3) . . . . ? O51 Yb1 N4 O41 95.3(4) . . . . ? N2 Yb1 N4 O41 -39.9(3) . . . . ? N1 Yb1 N4 O41 25.7(3) . . . . ? O42 Yb1 N4 O41 178.2(5) . . . . ? N5 Yb1 N4 O41 147(3) . . . . ? O43 N4 O41 Yb1 -176.2(4) . . . . ? O42 N4 O41 Yb1 1.8(4) . . . . ? O61 Yb1 O41 N4 -72.5(3) . . . . ? O52 Yb1 O41 N4 132.9(3) . . . . ? N3 Yb1 O41 N4 71.1(3) . . . . ? O51 Yb1 O41 N4 -127.6(3) . . . . ? N2 Yb1 O41 N4 138.0(3) . . . . ? N1 Yb1 O41 N4 -154.0(3) . . . . ? O42 Yb1 O41 N4 -1.0(3) . . . . ? N5 Yb1 O41 N4 -176.5(3) . . . . ? O43 N4 O42 Yb1 176.3(5) . . . . ? O41 N4 O42 Yb1 -1.7(4) . . . . ? O61 Yb1 O42 N4 97.9(3) . . . . ? O41 Yb1 O42 N4 1.0(3) . . . . ? O52 Yb1 O42 N4 -133.2(3) . . . . ? N3 Yb1 O42 N4 -95.5(3) . . . . ? O51 Yb1 O42 N4 133.6(3) . . . . ? N2 Yb1 O42 N4 -42.3(3) . . . . ? N1 Yb1 O42 N4 33.0(3) . . . . ? N5 Yb1 O42 N4 177.1(3) . . . . ? O61 Yb1 N5 O53 130(9) . . . . ? O41 Yb1 N5 O53 -129(9) . . . . ? O52 Yb1 N5 O53 -39(9) . . . . ? N3 Yb1 N5 O53 -21(9) . . . . ? O51 Yb1 N5 O53 143(9) . . . . ? N2 Yb1 N5 O53 -86(9) . . . . ? N1 Yb1 N5 O53 -151(9) . . . . ? O42 Yb1 N5 O53 58(9) . . . . ? N4 Yb1 N5 O53 87(10) . . . . ? O61 Yb1 N5 O51 -12.6(3) . . . . ? O41 Yb1 N5 O51 88.0(4) . . . . ? O52 Yb1 N5 O51 178.3(5) . . . . ? N3 Yb1 N5 O51 -163.7(3) . . . . ? N2 Yb1 N5 O51 131.0(3) . . . . ? N1 Yb1 N5 O51 65.8(3) . . . . ? O42 Yb1 N5 O51 -84.5(4) . . . . ? N4 Yb1 N5 O51 -56(3) . . . . ? O61 Yb1 N5 O52 169.1(3) . . . . ? O41 Yb1 N5 O52 -90.4(4) . . . . ? N3 Yb1 N5 O52 17.9(3) . . . . ? O51 Yb1 N5 O52 -178.3(5) . . . . ? N2 Yb1 N5 O52 -47.3(3) . . . . ? N1 Yb1 N5 O52 -112.6(3) . . . . ? O42 Yb1 N5 O52 97.1(4) . . . . ? N4 Yb1 N5 O52 125(3) . . . . ? O53 N5 O51 Yb1 -178.0(4) . . . . ? O52 N5 O51 Yb1 1.5(4) . . . . ? O61 Yb1 O51 N5 167.2(3) . . . . ? O41 Yb1 O51 N5 -135.1(3) . . . . ? O52 Yb1 O51 N5 -0.9(3) . . . . ? N3 Yb1 O51 N5 20.5(4) . . . . ? N2 Yb1 O51 N5 -51.7(3) . . . . ? N1 Yb1 O51 N5 -108.0(3) . . . . ? O42 Yb1 O51 N5 132.2(3) . . . . ? N4 Yb1 O51 N5 175.3(3) . . . . ? O53 N5 O52 Yb1 178.0(4) . . . . ? O51 N5 O52 Yb1 -1.6(4) . . . . ? O61 Yb1 O52 N5 -13.5(3) . . . . ? O41 Yb1 O52 N5 134.3(3) . . . . ? N3 Yb1 O52 N5 -162.3(3) . . . . ? O51 Yb1 O52 N5 0.9(3) . . . . ? N2 Yb1 O52 N5 129.1(3) . . . . ? N1 Yb1 O52 N5 65.7(3) . . . . ? O42 Yb1 O52 N5 -125.8(3) . . . . ? N4 Yb1 O52 N5 -174.9(3) . . . . ? O62 N6 O61 Yb1 -35.5(8) . . . . ? O63 N6 O61 Yb1 167.4(12) . . . . ? O63' N6 O61 Yb1 135.7(9) . . . . ? O41 Yb1 O61 N6 152.7(6) . . . . ? O52 Yb1 O61 N6 -45.4(6) . . . . ? N3 Yb1 O61 N6 79.1(6) . . . . ? O51 Yb1 O61 N6 -57.2(5) . . . . ? N2 Yb1 O61 N6 -154.4(5) . . . . ? N1 Yb1 O61 N6 -130.1(6) . . . . ? O42 Yb1 O61 N6 100.0(6) . . . . ? N5 Yb1 O61 N6 -51.5(6) . . . . ? N4 Yb1 O61 N6 126.6(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O98 H98 O62 0.84 2.07 2.756(5) 139.1 . C3 H3 O41 0.95 2.50 3.294(6) 140.6 4_675 C13 H13 O41 0.95 2.46 3.175(6) 131.7 1_455 C98 H98B O43 0.99 2.52 3.107(7) 118.0 3_666 C2 H2 O52 0.95 2.53 3.363(6) 146.1 1_655 C12 H12 O53 0.95 2.49 3.410(7) 162.0 4_576 C7 H7 O62 0.95 2.58 3.502(7) 163.2 2_655 C14 H14 O63 0.95 2.54 3.22(3) 128.5 3_666 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.951 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.100 ####END data_cam35 _database_code_CSD 169193 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 4 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 Lu N6 O10' _chemical_formula_weight 640.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7235(2) _cell_length_b 21.9191(3) _cell_length_c 11.3386(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.649(2) _cell_angle_gamma 90.00 _cell_volume 2167.17(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14776 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 29.27 _exptl_crystal_description Plate _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 4.623 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.6549 _exptl_absorpt_correction_T_max 0.9132 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68870 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker AXS SMART' _diffrn_measurement_method 'omega rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14776 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.27 _reflns_number_total 5825 _reflns_number_gt 5138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'LSCELL (Clegg, 1997)' _computing_data_reduction 'Bruker SAINT version 5.00 (Bruker, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+3.5709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5825 _refine_ls_number_parameters 311 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.075889(15) 0.123544(6) -0.175363(12) 0.02255(7) Uani 1 1 d . . . N1 N 0.2947(3) 0.18757(15) -0.2344(3) 0.0276(6) Uani 1 1 d . . . C1 C 0.4214(5) 0.1625(2) -0.2801(4) 0.0349(8) Uani 1 1 d . . . H1A H 0.4268 0.1193 -0.2872 0.042 Uiso 1 1 calc R . . C2 C 0.5440(5) 0.1972(2) -0.3171(4) 0.0377(9) Uani 1 1 d . . . H2A H 0.6307 0.1782 -0.3501 0.045 Uiso 1 1 calc R . . C3 C 0.5379(4) 0.2598(2) -0.3051(4) 0.0362(9) Uani 1 1 d . . . H3A H 0.6209 0.2845 -0.3291 0.043 Uiso 1 1 calc R . . C4 C 0.4093(5) 0.28617(19) -0.2579(3) 0.0323(8) Uani 1 1 d . . . H4A H 0.4036 0.3292 -0.2484 0.039 Uiso 1 1 calc R . . C5 C 0.2878(4) 0.24905(17) -0.2241(3) 0.0262(7) Uani 1 1 d . . . C6 C 0.1423(4) 0.27426(16) -0.1785(3) 0.0265(7) Uani 1 1 d . . . N2 N 0.0367(3) 0.23334(13) -0.1456(3) 0.0238(6) Uani 1 1 d . . . C7 C 0.1143(6) 0.33702(19) -0.1747(4) 0.0385(9) Uani 1 1 d . . . H7A H 0.1909 0.3654 -0.1960 0.046 Uiso 1 1 calc R . . C8 C -0.0277(6) 0.3568(2) -0.1393(5) 0.0472(11) Uani 1 1 d . . . H8A H -0.0505 0.3992 -0.1385 0.057 Uiso 1 1 calc R . . C9 C -0.1359(5) 0.3153(2) -0.1053(4) 0.0394(9) Uani 1 1 d . . . H9A H -0.2336 0.3285 -0.0807 0.047 Uiso 1 1 calc R . . C10 C -0.0998(4) 0.25368(17) -0.1075(3) 0.0269(7) Uani 1 1 d . . . C11 C -0.2075(4) 0.20647(19) -0.0660(3) 0.0287(7) Uani 1 1 d . . . N3 N -0.1602(4) 0.14786(16) -0.0743(3) 0.0294(6) Uani 1 1 d . . . C12 C -0.3479(4) 0.2218(2) -0.0170(4) 0.0376(9) Uani 1 1 d . . . H12A H -0.3785 0.2632 -0.0110 0.045 Uiso 1 1 calc R . . C13 C -0.4418(5) 0.1752(3) 0.0228(4) 0.0468(12) Uani 1 1 d . . . H13A H -0.5386 0.1845 0.0545 0.056 Uiso 1 1 calc R . . C14 C -0.3931(6) 0.1161(3) 0.0156(5) 0.0487(12) Uani 1 1 d . . . H14A H -0.4550 0.0839 0.0437 0.058 Uiso 1 1 calc R . . C15 C -0.2528(5) 0.1035(2) -0.0330(4) 0.0410(9) Uani 1 1 d . . . H15A H -0.2201 0.0623 -0.0376 0.049 Uiso 1 1 calc R . . O1 O 0.2004(3) 0.14693(13) 0.0052(3) 0.0304(6) Uani 1 1 d . . . N4 N 0.1563(4) 0.10054(16) 0.0645(3) 0.0352(7) Uani 1 1 d . . . O2 O 0.0741(4) 0.06230(14) 0.0087(3) 0.0415(7) Uani 1 1 d . . . O3 O 0.1899(5) 0.09485(18) 0.1694(3) 0.0611(11) Uani 1 1 d . . . O4 O 0.1140(4) 0.11013(19) -0.3865(3) 0.0500(9) Uani 1 1 d . . . N5 N -0.0064(5) 0.13857(19) -0.4168(3) 0.0413(9) Uani 1 1 d . . . O5 O -0.0830(3) 0.16172(15) -0.3330(3) 0.0375(7) Uani 1 1 d . . . O6 O -0.0478(6) 0.1446(2) -0.5199(3) 0.0666(13) Uani 1 1 d . . . O7 O 0.2649(4) 0.05218(14) -0.1865(3) 0.0471(8) Uani 1 1 d . . . N6 N 0.2820(4) -0.00142(17) -0.2265(4) 0.0429(9) Uani 1 1 d . . . O8 O 0.1722(4) -0.03715(15) -0.2341(4) 0.0552(10) Uani 1 1 d . . . O9 O 0.4110(5) -0.0159(2) -0.2537(7) 0.105(2) Uani 1 1 d . . . O10 O -0.0746(3) 0.04109(13) -0.2260(3) 0.0343(6) Uani 1 1 d D . . H10A H -0.024(6) 0.0116(16) -0.216(5) 0.051 Uiso 1 1 d D . . C16 C -0.2262(7) 0.0314(3) -0.2913(5) 0.0559(13) Uani 1 1 d . . . H16A H -0.2781 0.0714 -0.3009 0.067 Uiso 1 1 calc R . . H16B H -0.2920 0.0053 -0.2426 0.067 Uiso 1 1 calc R . . C17 C -0.2122(10) 0.0020(4) -0.4131(7) 0.090(3) Uani 1 1 d . . . H17A H -0.3094 0.0066 -0.4578 0.136 Uiso 1 1 calc R . . H17B H -0.1883 -0.0414 -0.4037 0.136 Uiso 1 1 calc R . . H17C H -0.1300 0.0221 -0.4556 0.136 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01762(9) 0.02159(9) 0.02837(10) -0.00052(5) -0.00031(6) 0.00011(5) N1 0.0222(14) 0.0303(15) 0.0306(15) 0.0015(12) 0.0032(12) 0.0002(11) C1 0.0288(19) 0.042(2) 0.034(2) -0.0022(16) 0.0068(15) 0.0030(16) C2 0.0208(17) 0.058(3) 0.034(2) 0.0040(18) 0.0026(15) 0.0006(17) C3 0.0228(17) 0.055(3) 0.0309(19) 0.0113(17) -0.0036(14) -0.0083(16) C4 0.0309(19) 0.036(2) 0.0294(18) 0.0058(15) -0.0042(15) -0.0107(15) C5 0.0267(17) 0.0279(17) 0.0239(16) 0.0020(13) -0.0018(13) -0.0033(13) C6 0.0283(17) 0.0237(16) 0.0272(16) 0.0012(12) -0.0032(13) 0.0004(13) N2 0.0225(13) 0.0236(14) 0.0250(13) 0.0002(11) -0.0016(11) 0.0038(11) C7 0.043(2) 0.0232(18) 0.049(2) 0.0029(16) 0.0022(18) -0.0013(16) C8 0.052(3) 0.028(2) 0.062(3) 0.0032(19) 0.005(2) 0.0141(19) C9 0.036(2) 0.038(2) 0.043(2) -0.0011(17) 0.0019(18) 0.0130(17) C10 0.0225(16) 0.0311(18) 0.0267(16) -0.0010(13) -0.0026(13) 0.0046(13) C11 0.0184(15) 0.041(2) 0.0264(16) -0.0037(14) -0.0022(13) 0.0021(14) N3 0.0216(14) 0.0362(17) 0.0306(15) 0.0021(13) 0.0033(12) -0.0029(12) C12 0.0230(18) 0.056(3) 0.033(2) -0.0064(18) -0.0015(15) 0.0101(17) C13 0.0210(18) 0.079(4) 0.041(2) -0.012(2) 0.0053(16) -0.002(2) C14 0.032(2) 0.067(3) 0.047(3) -0.003(2) 0.010(2) -0.017(2) C15 0.035(2) 0.047(2) 0.042(2) 0.0015(19) 0.0101(18) -0.0105(19) O1 0.0286(13) 0.0280(13) 0.0342(14) 0.0025(11) -0.0049(11) -0.0040(10) N4 0.0375(18) 0.0299(17) 0.0377(18) 0.0075(14) -0.0067(15) -0.0013(14) O2 0.0458(17) 0.0312(15) 0.0468(17) 0.0077(12) -0.0129(14) -0.0097(13) O3 0.086(3) 0.052(2) 0.0434(19) 0.0169(16) -0.027(2) -0.013(2) O4 0.0292(16) 0.085(3) 0.0359(17) -0.0160(17) 0.0048(13) -0.0112(16) N5 0.048(2) 0.045(2) 0.0304(17) 0.0034(15) -0.0042(16) -0.0257(18) O5 0.0384(17) 0.0356(16) 0.0376(16) 0.0012(11) -0.0121(13) 0.0000(11) O6 0.089(3) 0.079(3) 0.0304(17) 0.0093(18) -0.0183(19) -0.036(3) O7 0.0335(16) 0.0299(15) 0.078(2) -0.0106(15) -0.0031(16) 0.0081(12) N6 0.0322(18) 0.0303(18) 0.067(3) 0.0013(17) 0.0105(18) 0.0073(14) O8 0.0394(18) 0.0307(16) 0.096(3) 0.0011(17) 0.0125(19) -0.0021(13) O9 0.042(2) 0.065(3) 0.211(7) -0.052(4) 0.050(3) -0.004(2) O10 0.0298(14) 0.0256(13) 0.0470(17) 0.0004(12) -0.0082(12) -0.0003(10) C16 0.057(3) 0.047(3) 0.063(3) 0.007(2) -0.012(3) -0.013(2) C17 0.104(6) 0.097(6) 0.069(4) 0.003(4) -0.010(4) -0.054(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 Lu1 O7 2.279(3) . ? Lu1 O10 2.297(3) . ? Lu1 O1 2.346(3) . ? Lu1 O5 2.382(3) . ? Lu1 O4 2.444(3) . ? Lu1 N3 2.444(3) . ? Lu1 N2 2.455(3) . ? Lu1 N1 2.477(3) . ? Lu1 O2 2.482(3) . ? Lu1 N5 2.829(4) . ? Lu1 N4 2.834(4) . ? N1 C1 1.351(5) . ? N1 C5 1.354(5) . ? C1 C2 1.387(6) . ? C2 C3 1.381(7) . ? C3 C4 1.383(6) . ? C4 C5 1.398(5) . ? C5 C6 1.491(5) . ? C6 N2 1.346(5) . ? C6 C7 1.398(5) . ? N2 C10 1.354(5) . ? C7 C8 1.383(7) . ? C8 C9 1.374(7) . ? C9 C10 1.387(6) . ? C10 C11 1.484(5) . ? C11 N3 1.353(5) . ? C11 C12 1.400(5) . ? N3 C15 1.355(5) . ? C12 C13 1.391(7) . ? C13 C14 1.368(8) . ? C14 C15 1.384(7) . ? O1 N4 1.284(5) . ? N4 O3 1.224(5) . ? N4 O2 1.261(5) . ? O4 N5 1.260(6) . ? N5 O6 1.222(5) . ? N5 O5 1.282(5) . ? O7 N6 1.270(5) . ? N6 O9 1.218(5) . ? N6 O8 1.238(5) . ? O10 C16 1.512(6) . ? C16 C17 1.532(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Lu1 O10 81.69(11) . . ? O7 Lu1 O1 83.15(12) . . ? O10 Lu1 O1 129.55(10) . . ? O7 Lu1 O5 127.31(12) . . ? O10 Lu1 O5 76.87(10) . . ? O1 Lu1 O5 145.35(11) . . ? O7 Lu1 O4 75.18(14) . . ? O10 Lu1 O4 75.73(12) . . ? O1 Lu1 O4 143.93(11) . . ? O5 Lu1 O4 53.13(12) . . ? O7 Lu1 N3 142.78(13) . . ? O10 Lu1 N3 78.77(11) . . ? O1 Lu1 N3 85.33(10) . . ? O5 Lu1 N3 78.17(11) . . ? O4 Lu1 N3 128.72(11) . . ? O7 Lu1 N2 141.63(11) . . ? O10 Lu1 N2 136.45(10) . . ? O1 Lu1 N2 74.27(10) . . ? O5 Lu1 N2 71.24(10) . . ? O4 Lu1 N2 106.01(12) . . ? N3 Lu1 N2 66.40(11) . . ? O7 Lu1 N1 79.01(12) . . ? O10 Lu1 N1 144.85(11) . . ? O1 Lu1 N1 76.77(10) . . ? O5 Lu1 N1 91.97(10) . . ? O4 Lu1 N1 71.08(11) . . ? N3 Lu1 N1 132.03(11) . . ? N2 Lu1 N1 65.99(10) . . ? O7 Lu1 O2 72.37(13) . . ? O10 Lu1 O2 76.54(10) . . ? O1 Lu1 O2 53.01(9) . . ? O5 Lu1 O2 143.46(10) . . ? O4 Lu1 O2 139.71(12) . . ? N3 Lu1 O2 72.43(11) . . ? N2 Lu1 O2 114.24(11) . . ? N1 Lu1 O2 123.87(10) . . ? O7 Lu1 N5 100.97(14) . . ? O10 Lu1 N5 73.90(11) . . ? O1 Lu1 N5 156.48(10) . . ? O5 Lu1 N5 26.77(12) . . ? O4 Lu1 N5 26.38(13) . . ? N3 Lu1 N5 103.56(12) . . ? N2 Lu1 N5 89.21(11) . . ? N1 Lu1 N5 81.28(10) . . ? O2 Lu1 N5 150.35(10) . . ? O7 Lu1 N4 76.79(13) . . ? O10 Lu1 N4 102.92(11) . . ? O1 Lu1 N4 26.63(10) . . ? O5 Lu1 N4 154.84(11) . . ? O4 Lu1 N4 151.83(12) . . ? N3 Lu1 N4 77.15(11) . . ? N2 Lu1 N4 94.26(10) . . ? N1 Lu1 N4 100.89(10) . . ? O2 Lu1 N4 26.39(10) . . ? N5 Lu1 N4 176.43(10) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 Lu1 121.2(3) . . ? C5 N1 Lu1 120.3(2) . . ? N1 C1 C2 122.6(4) . . ? C3 C2 C1 119.0(4) . . ? C2 C3 C4 119.1(4) . . ? C3 C4 C5 119.5(4) . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 122.6(4) . . ? N2 C6 C7 121.7(4) . . ? N2 C6 C5 116.4(3) . . ? C7 C6 C5 121.8(4) . . ? C6 N2 C10 119.0(3) . . ? C6 N2 Lu1 121.1(2) . . ? C10 N2 Lu1 119.6(2) . . ? C8 C7 C6 118.4(4) . . ? C9 C8 C7 120.1(4) . . ? C8 C9 C10 118.8(4) . . ? N2 C10 C9 121.9(4) . . ? N2 C10 C11 116.3(3) . . ? C9 C10 C11 121.8(4) . . ? N3 C11 C12 121.8(4) . . ? N3 C11 C10 116.3(3) . . ? C12 C11 C10 121.9(4) . . ? C11 N3 C15 118.1(4) . . ? C11 N3 Lu1 120.1(2) . . ? C15 N3 Lu1 121.6(3) . . ? C13 C12 C11 118.9(4) . . ? C14 C13 C12 119.3(4) . . ? C13 C14 C15 119.5(5) . . ? N3 C15 C14 122.5(5) . . ? N4 O1 Lu1 98.4(2) . . ? O3 N4 O2 122.5(4) . . ? O3 N4 O1 121.5(4) . . ? O2 N4 O1 116.0(3) . . ? O3 N4 Lu1 175.6(3) . . ? O2 N4 Lu1 61.0(2) . . ? O1 N4 Lu1 54.99(18) . . ? N4 O2 Lu1 92.6(2) . . ? N5 O4 Lu1 94.1(3) . . ? O6 N5 O4 122.4(5) . . ? O6 N5 O5 121.4(5) . . ? O4 N5 O5 116.2(3) . . ? O6 N5 Lu1 177.4(4) . . ? O4 N5 Lu1 59.5(2) . . ? O5 N5 Lu1 56.80(19) . . ? N5 O5 Lu1 96.4(2) . . ? N6 O7 Lu1 138.4(3) . . ? O9 N6 O8 122.4(4) . . ? O9 N6 O7 116.8(4) . . ? O8 N6 O7 120.8(4) . . ? C16 O10 Lu1 135.9(3) . . ? O10 C16 C17 114.1(5) . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 2.232 _refine_diff_density_min -2.177 _refine_diff_density_rms 0.146 ####END data_pr9929 _database_code_CSD 169194 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 5 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H17 N6 O12 Yb' _chemical_formula_weight 646.39 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 8.8970(10) _cell_length_b 10.9810(10) _cell_length_c 20.9500(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.870(10) _cell_angle_gamma 90.00 _cell_volume 2044.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17495 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 4.655 _exptl_absorpt_correction_type 'semi empirical multiple scans' _exptl_absorpt_correction_T_min 0.6050 _exptl_absorpt_correction_T_max 0.9549 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not applicable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5509 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3532 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius HKL Scalepack' _computing_data_reduction 'Nonius HKL Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+9.4525P] 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 'water fixed, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3532 _refine_ls_number_parameters 325 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.79036(3) -0.26588(3) 0.366814(12) 0.01923(13) Uani 1 1 d . . . N1 N 0.5493(6) -0.3277(5) 0.4104(3) 0.0243(13) Uani 1 1 d DU . . C1 C 0.4362(8) -0.3743(7) 0.3739(3) 0.0296(17) Uani 1 1 d DU . . H1 H 0.4479 -0.3773 0.3291 0.035 Uiso 1 1 calc R . . C2 C 0.3027(8) -0.4186(7) 0.3964(4) 0.0309(17) Uani 1 1 d DU . . H2 H 0.2262 -0.4511 0.3681 0.037 Uiso 1 1 calc R . . C3 C 0.2850(8) -0.4137(7) 0.4621(4) 0.0315(17) Uani 1 1 d DU . . H3 H 0.1949 -0.4417 0.4796 0.038 Uiso 1 1 calc R . . C4 C 0.4012(8) -0.3674(7) 0.5013(3) 0.0305(17) Uani 1 1 d DU . . H4 H 0.3929 -0.3662 0.5463 0.037 Uiso 1 1 calc R . . C5 C 0.5291(8) -0.3229(7) 0.4747(3) 0.0227(14) Uani 1 1 d DU . . N2 N 0.7802(6) -0.2406(5) 0.4843(3) 0.0234(13) Uani 1 1 d DU . . C6 C 0.6539(8) -0.2681(6) 0.5138(3) 0.0227(15) Uani 1 1 d DU . . C7 C 0.6430(9) -0.2477(7) 0.5795(3) 0.0358(19) Uani 1 1 d DU . . H7 H 0.5516 -0.2647 0.5994 0.043 Uiso 1 1 calc R . . C8 C 0.7642(8) -0.2033(8) 0.6149(3) 0.0374(19) Uani 1 1 d DU . . H8 H 0.7581 -0.1894 0.6594 0.045 Uiso 1 1 calc R . . C9 C 0.8945(9) -0.1791(7) 0.5851(3) 0.0309(17) Uani 1 1 d DU . . H9 H 0.9807 -0.1508 0.6093 0.037 Uiso 1 1 calc R . . C10 C 0.9008(7) -0.1959(7) 0.5189(3) 0.0230(15) Uani 1 1 d DU . . N3 N 1.0194(6) -0.1765(6) 0.4185(3) 0.0252(13) Uani 1 1 d DU . . C11 C 1.0355(8) -0.1641(6) 0.4839(3) 0.0253(15) Uani 1 1 d DU . . C12 C 1.1654(8) -0.1213(7) 0.5140(4) 0.0308(17) Uani 1 1 d DU . . H12 H 1.1734 -0.1147 0.5593 0.037 Uiso 1 1 calc R . . C13 C 1.2845(9) -0.0880(7) 0.4780(4) 0.0326(18) Uani 1 1 d DU . . H13 H 1.3747 -0.0578 0.4984 0.039 Uiso 1 1 calc R . . C14 C 1.2722(8) -0.0985(7) 0.4126(4) 0.0311(17) Uani 1 1 d DU . . H14 H 1.3533 -0.0756 0.3872 0.037 Uiso 1 1 calc R . . C15 C 1.1385(8) -0.1435(7) 0.3841(3) 0.0280(17) Uani 1 1 d DU . . H15 H 1.1302 -0.1514 0.3389 0.034 Uiso 1 1 calc R . . N4 N 0.7331(7) -0.0129(6) 0.3415(3) 0.0248(14) Uani 1 1 d . . . O41 O 0.6557(6) -0.0795(5) 0.3786(2) 0.0289(12) Uani 1 1 d . . . O42 O 0.8395(6) -0.0679(5) 0.3159(2) 0.0315(12) Uani 1 1 d . . . O43 O 0.7079(6) 0.0947(5) 0.3332(2) 0.0323(12) Uani 1 1 d . . . N5 N 0.8379(7) -0.5212(6) 0.3803(3) 0.0272(14) Uani 1 1 d . . . O51 O 0.7440(5) -0.4773(5) 0.3376(2) 0.0289(12) Uani 1 1 d . . . O52 O 0.9114(6) -0.4419(5) 0.4142(2) 0.0288(12) Uani 1 1 d . . . O53 O 0.8542(7) -0.6299(5) 0.3880(3) 0.0410(14) Uani 1 1 d . . . N6 N 0.3527(7) -0.0793(6) 0.2487(3) 0.0293(15) Uani 1 1 d . . . O61 O 0.3243(6) -0.1876(5) 0.2597(3) 0.0409(14) Uani 1 1 d . . . O62 O 0.4867(6) -0.0498(5) 0.2373(2) 0.0374(14) Uani 1 1 d . . . O63 O 0.2527(6) -0.0004(5) 0.2483(3) 0.0408(15) Uani 1 1 d . . . O1W O 0.6447(6) -0.2680(5) 0.2719(2) 0.0300(13) Uani 1 1 d D . . H1WA H 0.681(8) -0.314(6) 0.241(3) 0.039 Uiso 1 1 d D . . H1WB H 0.586(8) -0.204(5) 0.260(4) 0.039 Uiso 1 1 d D . . O2W O 0.9601(6) -0.3096(5) 0.2928(2) 0.0266(11) Uani 1 1 d D . . H2WA H 0.972(9) -0.256(5) 0.262(3) 0.035 Uiso 1 1 d D . . H2WB H 0.971(9) -0.387(3) 0.282(3) 0.035 Uiso 1 1 d D . . O3W O 0.5050(6) -0.6460(5) 0.2981(2) 0.0320(12) Uani 1 1 d D . . H3WA H 0.590(5) -0.603(7) 0.299(4) 0.042 Uiso 1 1 d D . . H3WB H 0.427(6) -0.599(6) 0.285(4) 0.042 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01959(19) 0.0219(2) 0.01626(18) 0.00006(12) 0.00184(11) 0.00171(14) N1 0.023(3) 0.020(3) 0.029(3) -0.003(3) -0.002(2) 0.010(3) C1 0.030(4) 0.031(5) 0.027(4) -0.004(3) 0.001(3) 0.003(3) C2 0.027(4) 0.028(5) 0.038(4) -0.005(3) 0.002(3) 0.002(3) C3 0.023(4) 0.031(5) 0.042(4) 0.006(3) 0.013(3) -0.001(3) C4 0.034(4) 0.031(5) 0.028(4) 0.008(3) 0.010(3) 0.001(3) C5 0.026(3) 0.018(4) 0.024(3) 0.004(3) 0.004(3) 0.007(3) N2 0.030(3) 0.024(4) 0.017(3) -0.002(2) 0.006(2) 0.012(3) C6 0.030(3) 0.022(4) 0.017(3) 0.003(3) 0.006(3) 0.006(3) C7 0.041(4) 0.045(6) 0.023(4) 0.002(3) 0.007(3) -0.003(4) C8 0.053(5) 0.045(5) 0.014(3) 0.000(3) 0.001(3) 0.008(4) C9 0.038(4) 0.034(5) 0.020(3) -0.002(3) -0.004(3) 0.005(4) C10 0.026(3) 0.021(4) 0.021(3) 0.000(3) -0.003(3) 0.006(3) N3 0.028(3) 0.028(4) 0.021(3) -0.002(3) 0.005(2) 0.009(3) C11 0.033(4) 0.024(4) 0.019(3) 0.000(3) -0.004(3) 0.006(3) C12 0.036(4) 0.026(5) 0.030(4) -0.003(3) -0.004(3) 0.005(3) C13 0.028(4) 0.026(5) 0.043(4) -0.006(3) -0.009(3) -0.002(3) C14 0.023(4) 0.029(5) 0.041(4) 0.003(3) 0.002(3) 0.002(3) C15 0.028(4) 0.029(4) 0.028(4) 0.006(3) 0.007(3) -0.006(3) N4 0.029(4) 0.026(4) 0.019(3) -0.002(3) -0.004(3) -0.001(3) O41 0.034(3) 0.026(3) 0.027(3) 0.005(2) 0.010(2) 0.006(2) O42 0.029(3) 0.035(3) 0.031(3) 0.001(2) 0.008(2) 0.004(3) O43 0.048(3) 0.018(3) 0.030(3) 0.003(2) -0.001(2) 0.002(3) N5 0.023(3) 0.029(4) 0.030(3) 0.003(3) 0.011(3) 0.000(3) O51 0.025(3) 0.028(3) 0.034(3) -0.001(2) 0.003(2) 0.001(2) O52 0.030(3) 0.031(3) 0.025(3) 0.002(2) -0.001(2) 0.007(2) O53 0.053(4) 0.019(3) 0.052(4) 0.007(3) 0.017(3) 0.006(3) N6 0.030(4) 0.040(5) 0.018(3) 0.003(3) 0.004(3) 0.005(3) O61 0.050(4) 0.026(4) 0.048(3) 0.009(3) 0.009(3) -0.005(3) O62 0.024(3) 0.044(4) 0.044(3) 0.005(3) 0.007(2) -0.002(3) O63 0.035(3) 0.040(4) 0.048(3) 0.008(3) 0.008(3) 0.014(3) O1W 0.030(3) 0.041(4) 0.018(3) -0.005(2) -0.004(2) 0.010(3) O2W 0.033(3) 0.022(3) 0.026(3) 0.001(2) 0.008(2) -0.001(3) O3W 0.030(3) 0.035(4) 0.032(3) -0.003(2) 0.011(2) -0.002(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 Yb1 O2W 2.270(5) . ? Yb1 O1W 2.319(5) . ? Yb1 O41 2.390(5) . ? Yb1 O52 2.403(5) . ? Yb1 O51 2.431(5) . ? Yb1 N3 2.464(6) . ? Yb1 N1 2.468(6) . ? Yb1 O42 2.471(5) . ? Yb1 N2 2.483(5) . ? Yb1 N5 2.847(7) . ? Yb1 N4 2.869(6) . ? N1 C1 1.335(9) . ? N1 C5 1.370(9) . ? C1 C2 1.388(10) . ? C2 C3 1.393(11) . ? C3 C4 1.384(11) . ? C4 C5 1.380(10) . ? C5 C6 1.475(10) . ? N2 C6 1.343(8) . ? N2 C10 1.356(8) . ? C6 C7 1.403(9) . ? C7 C8 1.367(10) . ? C8 C9 1.370(9) . ? C9 C10 1.403(9) . ? C10 C11 1.477(10) . ? N3 C15 1.359(9) . ? N3 C11 1.378(8) . ? C11 C12 1.371(10) . ? C12 C13 1.381(11) . ? C13 C14 1.374(11) . ? C14 C15 1.394(10) . ? N4 O43 1.213(8) . ? N4 O42 1.265(7) . ? N4 O41 1.291(7) . ? N5 O53 1.213(8) . ? N5 O52 1.281(8) . ? N5 O51 1.288(8) . ? N6 O61 1.240(8) . ? N6 O63 1.242(8) . ? N6 O62 1.270(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Yb1 O1W 76.93(18) . . ? O2W Yb1 O41 127.27(17) . . ? O1W Yb1 O41 80.53(18) . . ? O2W Yb1 O52 79.19(18) . . ? O1W Yb1 O52 124.46(19) . . ? O41 Yb1 O52 149.62(16) . . ? O2W Yb1 O51 74.69(18) . . ? O1W Yb1 O51 72.17(19) . . ? O41 Yb1 O51 139.81(17) . . ? O52 Yb1 O51 53.33(17) . . ? O2W Yb1 N3 79.66(18) . . ? O1W Yb1 N3 142.68(19) . . ? O41 Yb1 N3 91.23(18) . . ? O52 Yb1 N3 78.19(19) . . ? O51 Yb1 N3 128.14(18) . . ? O2W Yb1 N1 144.57(19) . . ? O1W Yb1 N1 81.72(18) . . ? O41 Yb1 N1 75.41(18) . . ? O52 Yb1 N1 90.32(18) . . ? O51 Yb1 N1 71.99(17) . . ? N3 Yb1 N1 131.48(18) . . ? O2W Yb1 O42 75.68(18) . . ? O1W Yb1 O42 75.02(19) . . ? O41 Yb1 O42 52.53(16) . . ? O52 Yb1 O42 143.22(17) . . ? O51 Yb1 O42 139.72(16) . . ? N3 Yb1 O42 71.25(18) . . ? N1 Yb1 O42 125.30(17) . . ? O2W Yb1 N2 139.43(18) . . ? O1W Yb1 N2 143.60(17) . . ? O41 Yb1 N2 76.05(17) . . ? O52 Yb1 N2 73.64(17) . . ? O51 Yb1 N2 110.03(17) . . ? N3 Yb1 N2 65.81(18) . . ? N1 Yb1 N2 65.71(18) . . ? O42 Yb1 N2 110.24(18) . . ? O2W Yb1 N5 76.05(18) . . ? O1W Yb1 N5 98.59(19) . . ? O41 Yb1 N5 154.89(16) . . ? O52 Yb1 N5 26.56(17) . . ? O51 Yb1 N5 26.78(17) . . ? N3 Yb1 N5 103.49(19) . . ? N1 Yb1 N5 79.62(17) . . ? O42 Yb1 N5 151.73(16) . . ? N2 Yb1 N5 91.38(18) . . ? O2W Yb1 N4 101.33(18) . . ? O1W Yb1 N4 76.38(18) . . ? O41 Yb1 N4 26.47(16) . . ? O52 Yb1 N4 157.98(17) . . ? O51 Yb1 N4 148.40(16) . . ? N3 Yb1 N4 80.25(18) . . ? N1 Yb1 N4 100.68(18) . . ? O42 Yb1 N4 26.07(16) . . ? N2 Yb1 N4 93.45(17) . . ? N5 Yb1 N4 174.82(16) . . ? C1 N1 C5 116.5(6) . . ? C1 N1 Yb1 122.5(5) . . ? C5 N1 Yb1 120.8(4) . . ? N1 C1 C2 125.0(7) . . ? C1 C2 C3 117.6(7) . . ? C4 C3 C2 118.8(7) . . ? C5 C4 C3 119.8(7) . . ? N1 C5 C4 122.3(7) . . ? N1 C5 C6 115.4(6) . . ? C4 C5 C6 122.3(6) . . ? C6 N2 C10 119.6(6) . . ? C6 N2 Yb1 120.2(4) . . ? C10 N2 Yb1 120.2(4) . . ? N2 C6 C7 121.1(7) . . ? N2 C6 C5 117.4(6) . . ? C7 C6 C5 121.5(6) . . ? C8 C7 C6 119.8(7) . . ? C7 C8 C9 119.0(7) . . ? C8 C9 C10 120.1(7) . . ? N2 C10 C9 120.4(6) . . ? N2 C10 C11 117.4(6) . . ? C9 C10 C11 122.2(6) . . ? C15 N3 C11 117.1(6) . . ? C15 N3 Yb1 121.5(4) . . ? C11 N3 Yb1 121.3(5) . . ? C12 C11 N3 122.3(7) . . ? C12 C11 C10 122.6(6) . . ? N3 C11 C10 115.0(6) . . ? C11 C12 C13 119.5(7) . . ? C14 C13 C12 119.9(7) . . ? C13 C14 C15 118.6(7) . . ? N3 C15 C14 122.6(7) . . ? O43 N4 O42 122.7(6) . . ? O43 N4 O41 122.5(6) . . ? O42 N4 O41 114.8(6) . . ? O43 N4 Yb1 177.5(5) . . ? O42 N4 Yb1 59.1(3) . . ? O41 N4 Yb1 55.6(3) . . ? N4 O41 Yb1 97.9(4) . . ? N4 O42 Yb1 94.8(4) . . ? O53 N5 O52 122.7(6) . . ? O53 N5 O51 122.0(7) . . ? O52 N5 O51 115.2(6) . . ? O53 N5 Yb1 177.4(5) . . ? O52 N5 Yb1 57.0(3) . . ? O51 N5 Yb1 58.3(3) . . ? N5 O51 Yb1 94.9(4) . . ? N5 O52 Yb1 96.5(4) . . ? O61 N6 O63 121.2(6) . . ? O61 N6 O62 118.8(6) . . ? O63 N6 O62 120.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2W Yb1 N1 C1 -34.6(7) . . . . ? O1W Yb1 N1 C1 18.7(5) . . . . ? O41 Yb1 N1 C1 101.0(5) . . . . ? O52 Yb1 N1 C1 -106.2(5) . . . . ? O51 Yb1 N1 C1 -55.2(5) . . . . ? N3 Yb1 N1 C1 179.4(5) . . . . ? O42 Yb1 N1 C1 83.6(5) . . . . ? N2 Yb1 N1 C1 -178.0(6) . . . . ? N5 Yb1 N1 C1 -81.7(5) . . . . ? N4 Yb1 N1 C1 93.0(5) . . . . ? O2W Yb1 N1 C5 141.2(5) . . . . ? O1W Yb1 N1 C5 -165.6(5) . . . . ? O41 Yb1 N1 C5 -83.3(5) . . . . ? O52 Yb1 N1 C5 69.6(5) . . . . ? O51 Yb1 N1 C5 120.5(5) . . . . ? N3 Yb1 N1 C5 -4.9(6) . . . . ? O42 Yb1 N1 C5 -100.6(5) . . . . ? N2 Yb1 N1 C5 -2.3(5) . . . . ? N5 Yb1 N1 C5 94.0(5) . . . . ? N4 Yb1 N1 C5 -91.3(5) . . . . ? C5 N1 C1 C2 -0.8(9) . . . . ? Yb1 N1 C1 C2 175.1(5) . . . . ? N1 C1 C2 C3 0.3(10) . . . . ? C1 C2 C3 C4 -1.1(11) . . . . ? C2 C3 C4 C5 2.4(12) . . . . ? C1 N1 C5 C4 2.2(10) . . . . ? Yb1 N1 C5 C4 -173.8(5) . . . . ? C1 N1 C5 C6 -178.4(6) . . . . ? Yb1 N1 C5 C6 5.6(8) . . . . ? C3 C4 C5 N1 -3.1(11) . . . . ? C3 C4 C5 C6 177.6(7) . . . . ? O2W Yb1 N2 C6 -149.6(4) . . . . ? O1W Yb1 N2 C6 26.9(6) . . . . ? O41 Yb1 N2 C6 78.4(5) . . . . ? O52 Yb1 N2 C6 -99.7(5) . . . . ? O51 Yb1 N2 C6 -60.0(5) . . . . ? N3 Yb1 N2 C6 176.2(5) . . . . ? N1 Yb1 N2 C6 -1.7(4) . . . . ? O42 Yb1 N2 C6 118.9(5) . . . . ? N5 Yb1 N2 C6 -79.6(5) . . . . ? N4 Yb1 N2 C6 98.5(5) . . . . ? O2W Yb1 N2 C10 32.1(6) . . . . ? O1W Yb1 N2 C10 -151.4(5) . . . . ? O41 Yb1 N2 C10 -99.9(5) . . . . ? O52 Yb1 N2 C10 82.1(5) . . . . ? O51 Yb1 N2 C10 121.8(5) . . . . ? N3 Yb1 N2 C10 -2.1(5) . . . . ? N1 Yb1 N2 C10 -179.9(6) . . . . ? O42 Yb1 N2 C10 -59.3(5) . . . . ? N5 Yb1 N2 C10 102.1(5) . . . . ? N4 Yb1 N2 C10 -79.8(5) . . . . ? C10 N2 C6 C7 2.0(9) . . . . ? Yb1 N2 C6 C7 -176.2(5) . . . . ? C10 N2 C6 C5 -176.6(6) . . . . ? Yb1 N2 C6 C5 5.1(8) . . . . ? N1 C5 C6 N2 -6.9(9) . . . . ? C4 C5 C6 N2 172.4(6) . . . . ? N1 C5 C6 C7 174.4(6) . . . . ? C4 C5 C6 C7 -6.2(10) . . . . ? N2 C6 C7 C8 -2.4(10) . . . . ? C5 C6 C7 C8 176.2(7) . . . . ? C6 C7 C8 C9 0.2(12) . . . . ? C7 C8 C9 C10 2.2(12) . . . . ? C6 N2 C10 C9 0.4(10) . . . . ? Yb1 N2 C10 C9 178.6(5) . . . . ? C6 N2 C10 C11 -178.4(6) . . . . ? Yb1 N2 C10 C11 -0.1(8) . . . . ? C8 C9 C10 N2 -2.5(12) . . . . ? C8 C9 C10 C11 176.2(7) . . . . ? O2W Yb1 N3 C15 22.6(5) . . . . ? O1W Yb1 N3 C15 -29.3(7) . . . . ? O41 Yb1 N3 C15 -105.2(5) . . . . ? O52 Yb1 N3 C15 103.5(5) . . . . ? O51 Yb1 N3 C15 83.6(6) . . . . ? N1 Yb1 N3 C15 -176.7(5) . . . . ? O42 Yb1 N3 C15 -55.7(5) . . . . ? N2 Yb1 N3 C15 -179.3(6) . . . . ? N5 Yb1 N3 C15 95.4(5) . . . . ? N4 Yb1 N3 C15 -81.0(5) . . . . ? O2W Yb1 N3 C11 -153.8(5) . . . . ? O1W Yb1 N3 C11 154.4(4) . . . . ? O41 Yb1 N3 C11 78.5(5) . . . . ? O52 Yb1 N3 C11 -72.8(5) . . . . ? O51 Yb1 N3 C11 -92.8(5) . . . . ? N1 Yb1 N3 C11 7.0(6) . . . . ? O42 Yb1 N3 C11 127.9(5) . . . . ? N2 Yb1 N3 C11 4.4(5) . . . . ? N5 Yb1 N3 C11 -81.0(5) . . . . ? N4 Yb1 N3 C11 102.7(5) . . . . ? C15 N3 C11 C12 -0.5(9) . . . . ? Yb1 N3 C11 C12 176.0(5) . . . . ? C15 N3 C11 C10 177.4(6) . . . . ? Yb1 N3 C11 C10 -6.1(8) . . . . ? N2 C10 C11 C12 -178.2(6) . . . . ? C9 C10 C11 C12 3.1(11) . . . . ? N2 C10 C11 N3 4.0(9) . . . . ? C9 C10 C11 N3 -174.8(7) . . . . ? N3 C11 C12 C13 0.7(10) . . . . ? C10 C11 C12 C13 -177.0(7) . . . . ? C11 C12 C13 C14 -0.4(11) . . . . ? C12 C13 C14 C15 -0.2(12) . . . . ? C11 N3 C15 C14 -0.1(11) . . . . ? Yb1 N3 C15 C14 -176.6(6) . . . . ? C13 C14 C15 N3 0.5(12) . . . . ? O2W Yb1 N4 O43 -149(11) . . . . ? O1W Yb1 N4 O43 138(11) . . . . ? O41 Yb1 N4 O43 42(11) . . . . ? O52 Yb1 N4 O43 -60(11) . . . . ? O51 Yb1 N4 O43 132(11) . . . . ? N3 Yb1 N4 O43 -71(11) . . . . ? N1 Yb1 N4 O43 59(11) . . . . ? O42 Yb1 N4 O43 -138(11) . . . . ? N2 Yb1 N4 O43 -7(11) . . . . ? N5 Yb1 N4 O43 152(10) . . . . ? O2W Yb1 N4 O42 -10.3(4) . . . . ? O1W Yb1 N4 O42 -83.7(4) . . . . ? O41 Yb1 N4 O42 -179.8(6) . . . . ? O52 Yb1 N4 O42 78.9(6) . . . . ? O51 Yb1 N4 O42 -89.5(5) . . . . ? N3 Yb1 N4 O42 67.0(4) . . . . ? N1 Yb1 N4 O42 -162.4(4) . . . . ? N2 Yb1 N4 O42 131.7(4) . . . . ? N5 Yb1 N4 O42 -69.5(18) . . . . ? O2W Yb1 N4 O41 169.5(4) . . . . ? O1W Yb1 N4 O41 96.1(4) . . . . ? O52 Yb1 N4 O41 -101.3(5) . . . . ? O51 Yb1 N4 O41 90.4(5) . . . . ? N3 Yb1 N4 O41 -113.2(4) . . . . ? N1 Yb1 N4 O41 17.5(4) . . . . ? O42 Yb1 N4 O41 179.8(6) . . . . ? N2 Yb1 N4 O41 -48.5(4) . . . . ? N5 Yb1 N4 O41 110.3(17) . . . . ? O43 N4 O41 Yb1 -178.0(5) . . . . ? O42 N4 O41 Yb1 0.2(6) . . . . ? O2W Yb1 O41 N4 -13.0(4) . . . . ? O1W Yb1 O41 N4 -78.4(4) . . . . ? O52 Yb1 O41 N4 133.4(4) . . . . ? O51 Yb1 O41 N4 -125.7(4) . . . . ? N3 Yb1 O41 N4 65.0(4) . . . . ? N1 Yb1 O41 N4 -162.3(4) . . . . ? O42 Yb1 O41 N4 -0.1(3) . . . . ? N2 Yb1 O41 N4 129.7(4) . . . . ? N5 Yb1 O41 N4 -168.5(4) . . . . ? O43 N4 O42 Yb1 178.0(5) . . . . ? O41 N4 O42 Yb1 -0.2(5) . . . . ? O2W Yb1 O42 N4 169.6(4) . . . . ? O1W Yb1 O42 N4 89.6(4) . . . . ? O41 Yb1 O42 N4 0.1(3) . . . . ? O52 Yb1 O42 N4 -142.1(4) . . . . ? O51 Yb1 O42 N4 125.9(4) . . . . ? N3 Yb1 O42 N4 -106.7(4) . . . . ? N1 Yb1 O42 N4 21.4(4) . . . . ? N2 Yb1 O42 N4 -52.6(4) . . . . ? N5 Yb1 O42 N4 169.7(4) . . . . ? O2W Yb1 N5 O53 179(100) . . . . ? O1W Yb1 N5 O53 -107(12) . . . . ? O41 Yb1 N5 O53 -21(13) . . . . ? O52 Yb1 N5 O53 85(12) . . . . ? O51 Yb1 N5 O53 -98(12) . . . . ? N3 Yb1 N5 O53 103(12) . . . . ? N1 Yb1 N5 O53 -27(12) . . . . ? O42 Yb1 N5 O53 179(100) . . . . ? N2 Yb1 N5 O53 38(12) . . . . ? N4 Yb1 N5 O53 -121(12) . . . . ? O2W Yb1 N5 O52 93.7(4) . . . . ? O1W Yb1 N5 O52 167.8(4) . . . . ? O41 Yb1 N5 O52 -106.2(5) . . . . ? O51 Yb1 N5 O52 177.3(6) . . . . ? N3 Yb1 N5 O52 18.2(4) . . . . ? N1 Yb1 N5 O52 -112.3(4) . . . . ? O42 Yb1 N5 O52 93.6(5) . . . . ? N2 Yb1 N5 O52 -47.3(4) . . . . ? N4 Yb1 N5 O52 153.9(16) . . . . ? O2W Yb1 N5 O51 -83.6(4) . . . . ? O1W Yb1 N5 O51 -9.4(4) . . . . ? O41 Yb1 N5 O51 76.6(5) . . . . ? O52 Yb1 N5 O51 -177.3(6) . . . . ? N3 Yb1 N5 O51 -159.1(3) . . . . ? N1 Yb1 N5 O51 70.4(4) . . . . ? O42 Yb1 N5 O51 -83.7(5) . . . . ? N2 Yb1 N5 O51 135.4(4) . . . . ? N4 Yb1 N5 O51 -23.3(19) . . . . ? O53 N5 O51 Yb1 176.9(5) . . . . ? O52 N5 O51 Yb1 -2.5(5) . . . . ? O2W Yb1 O51 N5 89.3(4) . . . . ? O1W Yb1 O51 N5 170.2(4) . . . . ? O41 Yb1 O51 N5 -140.2(3) . . . . ? O52 Yb1 O51 N5 1.5(3) . . . . ? N3 Yb1 O51 N5 26.1(4) . . . . ? N1 Yb1 O51 N5 -102.9(4) . . . . ? O42 Yb1 O51 N5 133.3(3) . . . . ? N2 Yb1 O51 N5 -48.3(4) . . . . ? N4 Yb1 O51 N5 176.1(3) . . . . ? O53 N5 O52 Yb1 -176.9(5) . . . . ? O51 N5 O52 Yb1 2.6(5) . . . . ? O2W Yb1 O52 N5 -80.4(4) . . . . ? O1W Yb1 O52 N5 -14.6(4) . . . . ? O41 Yb1 O52 N5 126.3(4) . . . . ? O51 Yb1 O52 N5 -1.5(3) . . . . ? N3 Yb1 O52 N5 -162.0(4) . . . . ? N1 Yb1 O52 N5 65.5(4) . . . . ? O42 Yb1 O52 N5 -127.9(4) . . . . ? N2 Yb1 O52 N5 130.0(4) . . . . ? N4 Yb1 O52 N5 -173.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O43 0.89(2) 2.14(2) 3.022(7) 172(8) 2_645 O1W H1WB O62 0.90(2) 1.96(3) 2.853(8) 171(8) . O1W H1WB O61 0.90(2) 2.34(7) 2.983(8) 129(7) . O2W H2WA O3W 0.89(2) 1.76(2) 2.646(7) 178(8) 2_655 O2W H2WB O62 0.89(2) 1.87(2) 2.758(8) 174(8) 2_645 O3W H3WA O51 0.89(2) 2.08(4) 2.909(7) 153(7) . O3W H3WB O63 0.90(2) 2.03(2) 2.921(8) 177(8) 2_545 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.050 _refine_diff_density_min -2.964 _refine_diff_density_rms 0.160 ####END data_cam36 _database_code_CSD 169195 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ahrens, Birte' 'Cotton, S.' 'Noy, Oliver E.' 'Raithby, P.' 'Teat, Simon J.' _publ_contact_author_name 'Prof P Raithby' _publ_contact_author_address ; Prof P Raithby Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_section_title ; Structural variety in nitrate complexes of the heavy lanthanides with 2,2':6',2''-terpyridine, and stereoselective placement of nitrate. ; _audit_creation_date 2002-02-18T18:07:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C19 H25 Lu N6 O12' _chemical_formula_weight 704.42 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 8.862(7) _cell_length_b 12.260(11) _cell_length_c 13.482(10) _cell_angle_alpha 66.13(5) _cell_angle_beta 82.96(6) _cell_angle_gamma 69.99(6) _cell_volume 1258.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9612 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 29.43 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.996 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9611 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6887 _diffrn_radiation_type Synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART' _diffrn_measurement_method 'omega rotation with narrow frames' _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_unetI/netI 0.1226 _diffrn_reflns_number 9612 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.43 _diffrn_reflns_theta_full 29.43 _diffrn_measured_fraction_theta_full 0.86 _diffrn_measured_fraction_theta_max 0.86 _reflns_number_total 6585 _reflns_number_gt 4910 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'LSCELL (Clegg, 1997)' _computing_data_reduction 'Bruker SAINT version 5.00 (Bruker, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6585 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.934 _refine_diff_density_min -2.255 _refine_diff_density_rms 0.198 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.472 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.92791(3) 0.42623(3) 0.25965(2) 0.02016(9) Uani 1 1 d . . . N1 N 0.6506(7) 0.5565(6) 0.1973(5) 0.0274(13) Uani 1 1 d . . . C1 C 0.6190(10) 0.6485(8) 0.0985(6) 0.0382(18) Uani 1 1 d . . . H1A H 0.7044 0.6548 0.0487 0.046 Uiso 1 1 calc R . . C2 C 0.4668(9) 0.7356(7) 0.0652(6) 0.0379(18) Uani 1 1 d . . . H2A H 0.4484 0.7985 -0.0063 0.045 Uiso 1 1 calc R . . C3 C 0.3452(10) 0.7293(8) 0.1364(7) 0.0412(19) Uani 1 1 d . . . H3A H 0.2409 0.7888 0.1157 0.049 Uiso 1 1 calc R . . C4 C 0.3742(8) 0.6355(7) 0.2393(6) 0.0325(16) Uani 1 1 d . . . H4A H 0.2902 0.6305 0.2904 0.039 Uiso 1 1 calc R . . C5 C 0.5279(8) 0.5481(7) 0.2676(5) 0.0246(14) Uani 1 1 d . . . C6 C 0.5671(8) 0.4390(7) 0.3732(6) 0.0256(14) Uani 1 1 d . . . C7 C 0.4466(8) 0.4102(8) 0.4469(6) 0.0319(16) Uani 1 1 d . . . H7A H 0.338 0.4632 0.432 0.038 Uiso 1 1 calc R . . C8 C 0.4874(9) 0.3054(8) 0.5399(6) 0.0347(17) Uani 1 1 d . . . H8A H 0.407 0.2844 0.5904 0.042 Uiso 1 1 calc R . . C9 C 0.6473(9) 0.2284(8) 0.5615(6) 0.0341(17) Uani 1 1 d . . . H9A H 0.6776 0.1543 0.6258 0.041 Uiso 1 1 calc R . . N2 N 0.7228(6) 0.3676(5) 0.3923(4) 0.0225(11) Uani 1 1 d . . . C10 C 0.7619(8) 0.2641(7) 0.4847(5) 0.0256(14) Uani 1 1 d . . . C11 C 0.9359(8) 0.1888(7) 0.5036(6) 0.0274(14) Uani 1 1 d . . . C12 C 0.9912(9) 0.0802(7) 0.5935(6) 0.0340(17) Uani 1 1 d . . . H12A H 0.9177 0.0469 0.644 0.041 Uiso 1 1 calc R . . C13 C 1.1547(9) 0.0194(8) 0.6102(7) 0.0421(19) Uani 1 1 d . . . H13A H 1.1959 -0.0562 0.6718 0.05 Uiso 1 1 calc R . . C14 C 1.2559(10) 0.0717(9) 0.5350(8) 0.055(3) Uani 1 1 d . . . H14A H 1.3691 0.0339 0.545 0.066 Uiso 1 1 calc R . . C15 C 1.1919(9) 0.1793(9) 0.4451(7) 0.052(2) Uani 1 1 d . . . H15A H 1.2637 0.213 0.3932 0.062 Uiso 1 1 calc R . . N3 N 1.0355(7) 0.2385(6) 0.4270(5) 0.0306(13) Uani 1 1 d . . . N4 N 0.9878(7) 0.5658(6) 0.3640(5) 0.0301(14) Uani 1 1 d . . . O1 O 1.0984(5) 0.4789(5) 0.3446(4) 0.0303(11) Uani 1 1 d . . . O2 O 0.8441(5) 0.5824(5) 0.3373(4) 0.0291(11) Uani 1 1 d . . . O3 O 1.0128(7) 0.6310(6) 0.4040(5) 0.0420(14) Uani 1 1 d . . . N5 N 0.8732(8) 0.3049(6) 0.1316(5) 0.0337(14) Uani 1 1 d . . . O4 O 0.8835(6) 0.2580(5) 0.2359(4) 0.0342(12) Uani 1 1 d . . . O5 O 0.8947(6) 0.4129(5) 0.0848(4) 0.0298(11) Uani 1 1 d . . . O6 O 0.8402(8) 0.2515(7) 0.0825(5) 0.0525(16) Uani 1 1 d . . . N6 N 1.2426(9) 0.0794(7) 0.1655(6) 0.0487(18) Uani 1 1 d . . . O7 O 1.2115(8) 0.1917(6) 0.1001(5) 0.0561(16) Uani 1 1 d . . . O8 O 1.2160(12) -0.0005(8) 0.1426(8) 0.092(3) Uani 1 1 d . . . O9 O 1.2938(9) 0.0521(7) 0.2564(6) 0.076(2) Uani 1 1 d . . . O10 O 1.1833(6) 0.3385(5) 0.2078(4) 0.0328(11) Uani 1 1 d D . . O11 O 0.9769(6) 0.5998(5) 0.1236(4) 0.0308(11) Uani 1 1 d . . . H11B H 1.007 0.5945 0.0575 0.046 Uiso 1 1 d . . . H11C H 1.0757 0.5669 0.1594 0.046 Uiso 1 1 d . . . C16 C 1.3151(9) 0.3890(10) 0.1712(8) 0.048(2) Uani 1 1 d . . . H16A H 1.2975 0.4589 0.1949 0.058 Uiso 1 1 calc R . . H16B H 1.3153 0.4241 0.0909 0.058 Uiso 1 1 calc R . . C17 C 1.4750(10) 0.2935(11) 0.2128(9) 0.062(3) Uani 1 1 d . . . H17A H 1.559 0.3329 0.1848 0.093 Uiso 1 1 calc R . . H17B H 1.4941 0.2244 0.1888 0.093 Uiso 1 1 calc R . . H17C H 1.4771 0.2603 0.2923 0.093 Uiso 1 1 calc R . . O12 O 0.9281(8) 0.8418(6) 0.0819(6) 0.0585(17) Uani 1 1 d . . . H12B H 0.926 0.7676 0.1134 0.088 Uiso 1 1 calc R . . C18 C 0.6749(13) 0.9143(11) 0.1640(10) 0.072(3) Uani 1 1 d . . . H18A H 0.6269 0.9531 0.2162 0.107 Uiso 1 1 calc R . . H18B H 0.673 0.8275 0.1932 0.107 Uiso 1 1 calc R . . H18C H 0.6134 0.9625 0.0955 0.107 Uiso 1 1 calc R . . C19 C 0.8426(13) 0.9141(10) 0.1448(9) 0.062(3) Uani 1 1 d . . . H19A H 0.8431 1.002 0.1063 0.074 Uiso 1 1 calc R . . H19B H 0.8991 0.8788 0.2154 0.074 Uiso 1 1 calc R . . H10A H 1.197(14) 0.282(9) 0.176(9) 0.093 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.02007(12) 0.02408(15) 0.01855(12) -0.00994(10) 0.00286(8) -0.00860(9) N1 0.029(3) 0.035(4) 0.027(3) -0.016(3) 0.001(2) -0.014(3) C1 0.045(4) 0.040(5) 0.028(4) -0.012(4) -0.005(3) -0.011(4) C2 0.041(4) 0.030(4) 0.030(4) -0.003(3) -0.007(3) -0.004(3) C3 0.041(4) 0.042(5) 0.043(5) -0.022(4) -0.007(4) -0.007(4) C4 0.029(3) 0.032(4) 0.037(4) -0.013(3) -0.004(3) -0.009(3) C5 0.024(3) 0.032(4) 0.025(3) -0.015(3) 0.003(2) -0.013(3) C6 0.031(3) 0.029(4) 0.025(3) -0.015(3) 0.002(3) -0.014(3) C7 0.021(3) 0.048(5) 0.031(4) -0.020(4) 0.001(3) -0.011(3) C8 0.031(4) 0.048(5) 0.031(4) -0.019(4) 0.013(3) -0.019(4) C9 0.042(4) 0.040(5) 0.023(3) -0.010(3) 0.007(3) -0.021(4) N2 0.019(2) 0.028(3) 0.025(3) -0.015(3) 0.002(2) -0.008(2) C10 0.027(3) 0.033(4) 0.026(3) -0.015(3) 0.005(3) -0.018(3) C11 0.029(3) 0.028(4) 0.031(4) -0.017(3) 0.003(3) -0.011(3) C12 0.036(4) 0.031(4) 0.028(4) -0.001(3) 0.007(3) -0.017(3) C13 0.039(4) 0.035(5) 0.042(5) -0.008(4) -0.007(4) -0.005(4) C14 0.031(4) 0.054(6) 0.047(5) -0.001(4) 0.003(4) 0.003(4) C15 0.024(4) 0.051(6) 0.042(5) 0.000(4) 0.001(3) 0.010(4) N3 0.026(3) 0.031(3) 0.028(3) -0.010(3) 0.004(2) -0.003(3) N4 0.029(3) 0.042(4) 0.024(3) -0.017(3) 0.004(2) -0.013(3) O1 0.026(2) 0.037(3) 0.034(3) -0.020(2) -0.001(2) -0.009(2) O2 0.023(2) 0.033(3) 0.036(3) -0.020(2) 0.004(2) -0.009(2) O3 0.057(3) 0.048(4) 0.041(3) -0.030(3) 0.005(3) -0.028(3) N5 0.041(3) 0.039(4) 0.027(3) -0.014(3) 0.003(3) -0.020(3) O4 0.047(3) 0.035(3) 0.026(3) -0.014(2) 0.005(2) -0.019(3) O5 0.037(3) 0.028(3) 0.025(2) -0.010(2) -0.001(2) -0.010(2) O6 0.071(4) 0.067(4) 0.041(3) -0.033(3) 0.010(3) -0.035(4) N6 0.054(4) 0.039(5) 0.042(4) -0.008(4) 0.012(4) -0.014(4) O7 0.064(4) 0.051(4) 0.045(4) -0.006(3) -0.002(3) -0.022(3) O8 0.136(8) 0.059(5) 0.107(7) -0.052(5) 0.014(6) -0.042(5) O9 0.086(5) 0.073(5) 0.048(4) 0.000(4) -0.015(4) -0.024(4) O10 0.028(2) 0.042(3) 0.034(3) -0.025(3) 0.011(2) -0.009(2) O11 0.032(2) 0.038(3) 0.023(2) -0.011(2) 0.0061(19) -0.015(2) C16 0.027(4) 0.076(7) 0.057(6) -0.042(5) 0.012(4) -0.018(4) C17 0.036(5) 0.088(8) 0.074(7) -0.049(7) 0.001(5) -0.012(5) O12 0.077(4) 0.043(4) 0.055(4) -0.025(3) 0.003(3) -0.013(3) C18 0.073(7) 0.068(8) 0.062(7) -0.024(6) 0.008(6) -0.012(6) C19 0.079(7) 0.045(6) 0.055(6) -0.020(5) -0.015(5) -0.007(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O10 2.307(5) . ? Lu1 O11 2.315(5) . ? Lu1 O4 2.373(5) . ? Lu1 O1 2.388(5) . ? Lu1 O2 2.403(5) . ? Lu1 N1 2.456(6) . ? Lu1 N2 2.465(6) . ? Lu1 N3 2.474(7) . ? Lu1 O5 2.487(5) . ? Lu1 N4 2.817(6) . ? Lu1 N5 2.864(6) . ? N1 C1 1.336(10) . ? N1 C5 1.355(8) . ? C1 C2 1.391(11) . ? C2 C3 1.353(11) . ? C3 C4 1.381(12) . ? C4 C5 1.395(10) . ? C5 C6 1.483(10) . ? C6 N2 1.346(9) . ? C6 C7 1.403(9) . ? C7 C8 1.357(11) . ? C8 C9 1.395(11) . ? C9 C10 1.405(9) . ? N2 C10 1.344(9) . ? C10 C11 1.493(9) . ? C11 N3 1.361(9) . ? C11 C12 1.369(11) . ? C12 C13 1.383(11) . ? C13 C14 1.374(12) . ? C14 C15 1.376(12) . ? C15 N3 1.326(9) . ? N4 O3 1.216(7) . ? N4 O1 1.270(7) . ? N4 O2 1.291(7) . ? N5 O6 1.218(8) . ? N5 O5 1.286(8) . ? N5 O4 1.287(8) . ? N6 O9 1.234(10) . ? N6 O8 1.238(10) . ? N6 O7 1.251(10) . ? O10 C16 1.447(9) . ? C16 C17 1.491(13) . ? O12 C19 1.438(11) . ? C18 C19 1.477(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Lu1 O11 77.9(2) . . ? O10 Lu1 O4 81.98(19) . . ? O11 Lu1 O4 126.11(18) . . ? O10 Lu1 O1 75.53(18) . . ? O11 Lu1 O1 75.85(19) . . ? O4 Lu1 O1 144.28(18) . . ? O10 Lu1 O2 127.29(17) . . ? O11 Lu1 O2 76.72(18) . . ? O4 Lu1 O2 148.64(17) . . ? O1 Lu1 O2 53.78(16) . . ? O10 Lu1 N1 145.33(19) . . ? O11 Lu1 N1 80.7(2) . . ? O4 Lu1 N1 89.1(2) . . ? O1 Lu1 N1 124.75(18) . . ? O2 Lu1 N1 72.51(18) . . ? O10 Lu1 N2 140.7(2) . . ? O11 Lu1 N2 141.27(18) . . ? O4 Lu1 N2 74.22(18) . . ? O1 Lu1 N2 107.04(18) . . ? O2 Lu1 N2 75.10(18) . . ? N1 Lu1 N2 65.9(2) . . ? O10 Lu1 N3 78.5(2) . . ? O11 Lu1 N3 145.39(19) . . ? O4 Lu1 N3 74.7(2) . . ? O1 Lu1 N3 73.9(2) . . ? O2 Lu1 N3 98.2(2) . . ? N1 Lu1 N3 131.1(2) . . ? N2 Lu1 N3 65.41(19) . . ? O10 Lu1 O5 73.99(18) . . ? O11 Lu1 O5 73.42(17) . . ? O4 Lu1 O5 53.00(17) . . ? O1 Lu1 O5 140.30(17) . . ? O2 Lu1 O5 137.89(17) . . ? N1 Lu1 O5 73.91(18) . . ? N2 Lu1 O5 112.66(17) . . ? N3 Lu1 O5 123.05(19) . . ? O10 Lu1 N4 101.02(18) . . ? O11 Lu1 N4 73.73(18) . . ? O4 Lu1 N4 159.85(18) . . ? O1 Lu1 N4 26.63(16) . . ? O2 Lu1 N4 27.18(16) . . ? N1 Lu1 N4 98.76(19) . . ? N2 Lu1 N4 91.99(18) . . ? N3 Lu1 N4 86.3(2) . . ? O5 Lu1 N4 147.08(18) . . ? O10 Lu1 N5 77.16(18) . . ? O11 Lu1 N5 99.96(19) . . ? O4 Lu1 N5 26.38(18) . . ? O1 Lu1 N5 152.64(18) . . ? O2 Lu1 N5 152.56(18) . . ? N1 Lu1 N5 80.06(19) . . ? N2 Lu1 N5 93.15(18) . . ? N3 Lu1 N5 99.1(2) . . ? O5 Lu1 N5 26.63(17) . . ? N4 Lu1 N5 173.69(18) . . ? C1 N1 C5 118.1(6) . . ? C1 N1 Lu1 121.1(5) . . ? C5 N1 Lu1 120.3(4) . . ? N1 C1 C2 123.0(8) . . ? C3 C2 C1 119.0(8) . . ? C2 C3 C4 119.5(7) . . ? C3 C4 C5 119.3(7) . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C6 115.8(6) . . ? C4 C5 C6 123.1(6) . . ? N2 C6 C7 122.3(7) . . ? N2 C6 C5 116.4(6) . . ? C7 C6 C5 121.2(6) . . ? C8 C7 C6 119.0(7) . . ? C7 C8 C9 120.2(7) . . ? C8 C9 C10 117.7(7) . . ? C10 N2 C6 118.2(6) . . ? C10 N2 Lu1 121.5(4) . . ? C6 N2 Lu1 120.3(5) . . ? N2 C10 C9 122.7(6) . . ? N2 C10 C11 116.5(6) . . ? C9 C10 C11 120.9(7) . . ? N3 C11 C12 122.7(6) . . ? N3 C11 C10 115.0(6) . . ? C12 C11 C10 122.2(6) . . ? C11 C12 C13 119.5(7) . . ? C14 C13 C12 118.0(8) . . ? C13 C14 C15 119.4(8) . . ? N3 C15 C14 123.6(8) . . ? C15 N3 C11 116.8(7) . . ? C15 N3 Lu1 122.0(5) . . ? C11 N3 Lu1 121.2(4) . . ? O3 N4 O1 123.3(6) . . ? O3 N4 O2 121.1(6) . . ? O1 N4 O2 115.6(5) . . ? O3 N4 Lu1 176.8(5) . . ? O1 N4 Lu1 57.4(3) . . ? O2 N4 Lu1 58.2(3) . . ? N4 O1 Lu1 95.9(4) . . ? N4 O2 Lu1 94.6(4) . . ? O6 N5 O5 123.3(6) . . ? O6 N5 O4 121.6(6) . . ? O5 N5 O4 115.1(6) . . ? O6 N5 Lu1 174.9(5) . . ? O5 N5 Lu1 60.1(3) . . ? O4 N5 Lu1 55.0(3) . . ? N5 O4 Lu1 98.6(4) . . ? N5 O5 Lu1 93.3(4) . . ? O9 N6 O8 120.6(9) . . ? O9 N6 O7 117.4(8) . . ? O8 N6 O7 121.9(9) . . ? C16 O10 Lu1 130.7(5) . . ? O10 C16 C17 113.3(9) . . ? O12 C19 C18 112.5(9) . . ? ####END