Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Marinella Mazzanti' 'Frank A. Dunand' 'Christelle Gateau' 'Lothar Helm' 'Jacques Pecaut' _publ_contact_author_name 'Dr Marinella Mazzanti' _publ_contact_author_address ; Departement de Recherche Fondamentale sur la Matiere Condensee CEA-Grenoble Laboratoire de Reconnaissance Ioniq Grenoble 38054 FRANCE ; _publ_contact_author_email MAZZANTI@DRFMC.CENG.CEA.FR _publ_section_title ; Solid-State and Solution Properties of The Lanthanide Complexes of a New Nonadentate Tripodal Ligand Derived from 1,4,7-triazacyclononane ; data_complexNd(tpatcn)_(1) _database_code_CSD 206375 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 N6 Nd O9' _chemical_formula_weight 729.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.042(4) _cell_length_b 11.948(7) _cell_length_c 14.985(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.400(10) _cell_angle_gamma 90.00 _cell_volume 1416.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 1.898 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8804 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.74 _reflns_number_total 4841 _reflns_number_gt 3584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0437P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(19) _refine_ls_number_reflns 4841 _refine_ls_number_parameters 388 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.114 _refine_ls_shift/su_mean 0.010 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 Nd Nd 0.31436(4) 0.27816(3) 0.82121(4) 0.02440(11) Uani 1 1 d . . . O11 O 0.5480(8) 0.3641(6) 0.9226(4) 0.0440(17) Uani 1 1 d . . . O12 O 0.6589(10) 0.4290(7) 1.0600(5) 0.073(3) Uani 1 1 d . . . O21 O 0.4587(8) 0.3322(7) 0.7010(5) 0.0506(19) Uani 1 1 d . . . O22 O 0.5611(9) 0.4574(8) 0.6153(5) 0.078(3) Uani 1 1 d . . . O31 O 0.4898(8) 0.1107(5) 0.8362(4) 0.0415(16) Uani 1 1 d . . . O32 O 0.5907(8) -0.0454(5) 0.7858(4) 0.0451(17) Uani 1 1 d . . . N1 N 0.0598(8) 0.1687(6) 0.8834(5) 0.0334(17) Uani 1 1 d . . . N2 N 0.0837(9) 0.4131(6) 0.8799(5) 0.0315(18) Uani 1 1 d . . . N3 N 0.0127(9) 0.2818(7) 0.7089(4) 0.0324(16) Uani 1 1 d . . . N11 N 0.3634(8) 0.2139(7) 0.9904(4) 0.0308(16) Uani 1 1 d . . . N21 N 0.3306(10) 0.4906(7) 0.7932(5) 0.039(2) Uani 1 1 d . . . N31 N 0.2579(8) 0.1315(7) 0.6905(5) 0.0318(17) Uani 1 1 d . . . C1 C -0.0491(11) 0.2373(8) 0.9322(7) 0.044(3) Uani 1 1 d . . . H1A H -0.0632 0.1986 0.9873 0.052 Uiso 1 1 calc R . . H1B H -0.1598 0.2451 0.8945 0.052 Uiso 1 1 calc R . . C2 C 0.0238(12) 0.3533(10) 0.9569(6) 0.046(3) Uani 1 1 d . . . H2A H -0.0620 0.3987 0.9774 0.056 Uiso 1 1 calc R . . H2B H 0.1180 0.3463 1.0071 0.056 Uiso 1 1 calc R . . C3 C -0.0620(11) 0.4389(8) 0.8058(6) 0.041(2) Uani 1 1 d . . . H3A H -0.0791 0.5192 0.8035 0.050 Uiso 1 1 calc R . . H3B H -0.1630 0.4051 0.8210 0.050 Uiso 1 1 calc R . . C4 C -0.0421(12) 0.3985(8) 0.7117(6) 0.037(2) Uani 1 1 d . . . H4A H -0.1494 0.4072 0.6707 0.044 Uiso 1 1 calc R . . H4B H 0.0397 0.4460 0.6897 0.044 Uiso 1 1 calc R . . C5 C -0.1153(10) 0.2005(8) 0.7322(6) 0.038(2) Uani 1 1 d . . . H5A H -0.2047 0.2422 0.7528 0.045 Uiso 1 1 calc R . . H5B H -0.1655 0.1606 0.6776 0.045 Uiso 1 1 calc R . . C6 C -0.0464(11) 0.1171(7) 0.8032(6) 0.034(2) Uani 1 1 d . . . H6A H -0.1396 0.0779 0.8222 0.041 Uiso 1 1 calc R . . H6B H 0.0204 0.0625 0.7773 0.041 Uiso 1 1 calc R . . C11 C 0.1450(12) 0.0815(8) 0.9458(6) 0.036(2) Uani 1 1 d . . . H11A H 0.2028 0.0291 0.9125 0.043 Uiso 1 1 calc R . . H11B H 0.0619 0.0404 0.9722 0.043 Uiso 1 1 calc R . . C12 C 0.2697(11) 0.1359(8) 1.0193(6) 0.035(2) Uani 1 1 d . . . C13 C 0.2883(13) 0.1104(9) 1.1106(7) 0.049(3) Uani 1 1 d . . . H13 H 0.2236 0.0536 1.1295 0.058 Uiso 1 1 calc R . . C14 C 0.3991(15) 0.1669(11) 1.1719(7) 0.062(3) Uani 1 1 d . . . H14 H 0.4121 0.1491 1.2332 0.074 Uiso 1 1 calc R . . C15 C 0.4930(13) 0.2512(10) 1.1434(7) 0.060(4) Uani 1 1 d . . . H15 H 0.5670 0.2935 1.1851 0.072 Uiso 1 1 calc R . . C16 C 0.4750(11) 0.2724(9) 1.0492(6) 0.034(2) Uani 1 1 d . . . C17 C 0.5686(12) 0.3633(9) 1.0082(7) 0.042(2) Uani 1 1 d . . . C21 C 0.173(2) 0.5157(12) 0.9138(11) 0.038(4) Uani 1 1 d . . . H21A H 0.2467 0.4999 0.9710 0.045 Uiso 1 1 calc R . . H21B H 0.0907 0.5711 0.9251 0.045 Uiso 1 1 calc R . . C22 C 0.2790(14) 0.5649(9) 0.8465(7) 0.046(3) Uani 1 1 d . . . C23 C 0.3146(17) 0.6797(9) 0.8482(6) 0.053(3) Uani 1 1 d . . . H23 H 0.2668 0.7281 0.8851 0.063 Uiso 1 1 calc R . . C24 C 0.4250(18) 0.7194(13) 0.7925(9) 0.080(4) Uani 1 1 d . . . H24 H 0.4600 0.7937 0.7938 0.096 Uiso 1 1 calc R . . C25 C 0.4789(13) 0.6400(11) 0.7349(8) 0.068(4) Uani 1 1 d . . . H25 H 0.5478 0.6628 0.6947 0.082 Uiso 1 1 calc R . . C26 C 0.4324(17) 0.5287(15) 0.7363(10) 0.041(4) Uani 1 1 d . . . C27 C 0.4884(11) 0.4308(11) 0.6787(7) 0.044(3) Uani 1 1 d . . . C31 C 0.0457(12) 0.2563(8) 0.6169(6) 0.039(3) Uani 1 1 d . . . H31A H 0.1112 0.3165 0.5970 0.047 Uiso 1 1 calc R . . H31B H -0.0609 0.2516 0.5748 0.047 Uiso 1 1 calc R . . C32 C 0.1388(11) 0.1495(8) 0.6154(6) 0.030(2) Uani 1 1 d . . . C33 C 0.1146(12) 0.0745(9) 0.5441(6) 0.041(2) Uani 1 1 d . . . H33 H 0.0333 0.0880 0.4926 0.050 Uiso 1 1 calc R . . C34 C 0.2109(12) -0.0187(9) 0.5504(6) 0.044(3) Uani 1 1 d . . . H34 H 0.1946 -0.0708 0.5035 0.053 Uiso 1 1 calc R . . C35 C 0.3331(11) -0.0370(8) 0.6258(6) 0.036(2) Uani 1 1 d . . . H35 H 0.4010 -0.1005 0.6301 0.043 Uiso 1 1 calc R . . C36 C 0.3529(11) 0.0412(7) 0.6955(6) 0.032(2) Uani 1 1 d . . . C37 C 0.4906(11) 0.0330(8) 0.7793(6) 0.029(2) Uani 1 1 d . . . O1 O 0.6002(12) 0.1860(9) 0.5454(7) 0.112(4) Uani 1 1 d . . . O2 O 0.2685(12) 0.3854(7) 0.4606(6) 0.089(3) Uani 1 1 d . . . O3 O 0.3462(10) 0.1793(7) 0.3903(5) 0.073(2) 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 Nd 0.01995(16) 0.0309(2) 0.02251(18) -0.0002(5) 0.00441(12) -0.0004(6) O11 0.037(4) 0.062(5) 0.031(4) 0.002(3) 0.001(3) -0.020(4) O12 0.056(5) 0.096(7) 0.065(6) -0.030(5) 0.006(4) -0.036(5) O21 0.052(4) 0.059(5) 0.048(4) 0.005(4) 0.029(4) -0.008(4) O22 0.043(4) 0.147(8) 0.051(5) 0.051(5) 0.026(4) 0.008(5) O31 0.039(4) 0.053(4) 0.028(4) -0.012(3) -0.006(3) 0.015(3) O32 0.041(4) 0.029(4) 0.063(5) -0.006(3) 0.003(3) 0.009(3) N1 0.026(4) 0.036(4) 0.039(5) -0.001(3) 0.008(3) -0.005(3) N2 0.029(4) 0.038(5) 0.030(4) 0.002(3) 0.013(3) 0.003(3) N3 0.031(4) 0.038(4) 0.027(4) -0.002(4) 0.002(3) 0.000(4) N11 0.032(4) 0.038(4) 0.023(4) 0.001(4) 0.007(3) 0.002(4) N21 0.030(5) 0.048(5) 0.036(6) 0.007(4) 0.002(4) 0.003(4) N31 0.023(4) 0.047(5) 0.027(4) 0.001(3) 0.008(3) -0.001(3) C1 0.032(5) 0.059(7) 0.044(6) 0.010(5) 0.019(4) 0.001(5) C2 0.035(6) 0.081(9) 0.025(5) 0.007(5) 0.012(4) 0.004(6) C3 0.033(5) 0.037(6) 0.055(7) 0.007(5) 0.011(5) 0.004(5) C4 0.029(5) 0.053(7) 0.031(5) 0.005(4) 0.010(4) 0.008(5) C5 0.020(4) 0.052(8) 0.040(5) -0.003(4) 0.002(4) -0.001(4) C6 0.027(5) 0.034(6) 0.041(6) -0.002(4) 0.001(4) -0.005(4) C11 0.039(6) 0.032(6) 0.038(6) 0.010(4) 0.008(4) -0.001(5) C12 0.036(5) 0.037(6) 0.036(5) 0.018(4) 0.014(4) 0.009(4) C13 0.041(6) 0.057(7) 0.050(7) 0.022(5) 0.015(5) 0.014(5) C14 0.063(7) 0.092(10) 0.033(6) 0.017(6) 0.014(6) -0.001(7) C15 0.043(6) 0.106(12) 0.027(5) -0.010(5) -0.004(4) 0.013(6) C16 0.028(4) 0.044(5) 0.025(5) -0.003(5) -0.006(4) 0.006(5) C17 0.039(6) 0.042(7) 0.041(6) -0.007(5) -0.006(5) 0.000(5) C21 0.045(8) 0.027(8) 0.043(8) -0.006(6) 0.013(6) -0.001(6) C22 0.051(7) 0.046(7) 0.037(7) 0.001(5) -0.005(5) -0.003(6) C23 0.071(7) 0.033(6) 0.047(8) 0.010(4) -0.008(8) -0.015(6) C24 0.071(9) 0.081(10) 0.078(10) -0.008(8) -0.016(8) -0.040(9) C25 0.044(6) 0.088(10) 0.064(8) 0.054(7) -0.013(6) -0.030(7) C26 0.025(6) 0.068(11) 0.025(7) 0.017(7) -0.008(5) -0.001(7) C27 0.020(5) 0.077(9) 0.034(6) 0.013(6) 0.000(4) -0.002(5) C31 0.029(5) 0.052(9) 0.035(5) -0.002(4) 0.001(4) -0.004(4) C32 0.029(5) 0.032(6) 0.028(5) 0.003(4) 0.004(4) -0.001(4) C33 0.034(5) 0.061(7) 0.025(5) -0.012(4) -0.004(4) -0.001(5) C34 0.047(6) 0.051(7) 0.034(6) -0.020(5) 0.007(5) -0.006(5) C35 0.037(5) 0.033(6) 0.040(6) -0.015(4) 0.012(4) -0.012(4) C36 0.025(5) 0.030(5) 0.040(6) 0.002(4) 0.006(4) 0.001(4) C37 0.029(5) 0.031(5) 0.032(5) -0.006(4) 0.017(4) -0.002(4) O1 0.073(6) 0.119(10) 0.123(9) -0.033(6) -0.039(6) 0.013(6) O2 0.106(7) 0.083(7) 0.089(7) -0.025(5) 0.045(6) -0.029(5) O3 0.065(5) 0.102(7) 0.051(5) -0.013(4) 0.006(4) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O21 2.401(6) . ? Nd O11 2.422(6) . ? Nd O31 2.436(6) . ? Nd N21 2.580(9) . ? Nd N31 2.606(7) . ? Nd N11 2.611(7) . ? Nd N3 2.692(7) . ? Nd N2 2.720(7) . ? Nd N1 2.731(7) . ? O11 C17 1.263(11) . ? O12 C17 1.242(11) . ? O21 C27 1.259(12) . ? O22 C27 1.244(11) . ? O31 C37 1.260(10) . ? O32 C37 1.227(10) . ? N1 C6 1.478(11) . ? N1 C11 1.483(11) . ? N1 C1 1.485(11) . ? N2 C21 1.464(16) . ? N2 C3 1.494(11) . ? N2 C2 1.508(11) . ? N3 C4 1.466(12) . ? N3 C31 1.482(11) . ? N3 C5 1.502(12) . ? N11 C12 1.319(11) . ? N11 C16 1.336(12) . ? N21 C22 1.311(11) . ? N21 C26 1.362(15) . ? N31 C36 1.316(11) . ? N31 C32 1.358(10) . ? C1 C2 1.524(14) . ? C3 C4 1.526(13) . ? C5 C6 1.489(12) . ? C11 C12 1.497(13) . ? C12 C13 1.383(12) . ? C13 C14 1.342(15) . ? C14 C15 1.373(15) . ? C15 C16 1.417(13) . ? C16 C17 1.513(14) . ? C21 C22 1.550(16) . ? C22 C23 1.400(14) . ? C23 C24 1.407(18) . ? C24 C25 1.403(18) . ? C25 C26 1.38(2) . ? C26 C27 1.567(19) . ? C31 C32 1.482(13) . ? C32 C33 1.381(12) . ? C33 C34 1.350(13) . ? C34 C35 1.374(13) . ? C35 C36 1.389(12) . ? C36 C37 1.521(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Nd O11 86.1(2) . . ? O21 Nd O31 86.5(2) . . ? O11 Nd O31 85.4(2) . . ? O21 Nd N21 64.4(3) . . ? O11 Nd N21 68.2(3) . . ? O31 Nd N21 141.1(2) . . ? O21 Nd N31 70.1(2) . . ? O11 Nd N31 140.1(2) . . ? O31 Nd N31 62.3(2) . . ? N21 Nd N31 123.1(2) . . ? O21 Nd N11 143.1(2) . . ? O11 Nd N11 63.3(2) . . ? O31 Nd N11 71.7(2) . . ? N21 Nd N11 116.4(3) . . ? N31 Nd N11 120.5(3) . . ? O21 Nd N3 91.7(2) . . ? O11 Nd N3 153.5(3) . . ? O31 Nd N3 120.8(2) . . ? N21 Nd N3 87.1(3) . . ? N31 Nd N3 61.7(2) . . ? N11 Nd N3 125.0(2) . . ? O21 Nd N2 122.2(3) . . ? O11 Nd N2 92.5(2) . . ? O31 Nd N2 151.0(2) . . ? N21 Nd N2 61.8(2) . . ? N31 Nd N2 127.2(2) . . ? N11 Nd N2 81.5(2) . . ? N3 Nd N2 66.6(2) . . ? O21 Nd N1 151.5(2) . . ? O11 Nd N1 122.3(2) . . ? O31 Nd N1 91.9(2) . . ? N21 Nd N1 126.1(2) . . ? N31 Nd N1 84.0(2) . . ? N11 Nd N1 61.2(2) . . ? N3 Nd N1 64.8(2) . . ? N2 Nd N1 64.9(2) . . ? C17 O11 Nd 125.3(6) . . ? C27 O21 Nd 126.3(7) . . ? C37 O31 Nd 128.1(6) . . ? C6 N1 C11 110.7(7) . . ? C6 N1 C1 109.0(7) . . ? C11 N1 C1 108.9(7) . . ? C6 N1 Nd 106.3(5) . . ? C11 N1 Nd 105.2(5) . . ? C1 N1 Nd 116.7(5) . . ? C21 N2 C3 110.7(9) . . ? C21 N2 C2 109.6(9) . . ? C3 N2 C2 110.5(7) . . ? C21 N2 Nd 106.8(7) . . ? C3 N2 Nd 111.8(5) . . ? C2 N2 Nd 107.3(5) . . ? C4 N3 C31 109.1(7) . . ? C4 N3 C5 112.8(7) . . ? C31 N3 C5 109.2(7) . . ? C4 N3 Nd 103.8(6) . . ? C31 N3 Nd 106.6(5) . . ? C5 N3 Nd 115.0(5) . . ? C12 N11 C16 120.6(8) . . ? C12 N11 Nd 122.1(6) . . ? C16 N11 Nd 116.8(6) . . ? C22 N21 C26 116.6(11) . . ? C22 N21 Nd 122.4(6) . . ? C26 N21 Nd 119.0(9) . . ? C36 N31 C32 119.5(8) . . ? C36 N31 Nd 119.2(6) . . ? C32 N31 Nd 121.2(6) . . ? N1 C1 C2 112.7(7) . . ? N2 C2 C1 114.0(7) . . ? N2 C3 C4 115.0(7) . . ? N3 C4 C3 114.2(7) . . ? C6 C5 N3 114.6(7) . . ? N1 C6 C5 112.8(8) . . ? N1 C11 C12 109.3(8) . . ? N11 C12 C13 120.9(9) . . ? N11 C12 C11 114.3(7) . . ? C13 C12 C11 124.8(9) . . ? C14 C13 C12 120.5(10) . . ? C13 C14 C15 119.4(10) . . ? C14 C15 C16 118.6(10) . . ? N11 C16 C15 119.9(9) . . ? N11 C16 C17 115.6(8) . . ? C15 C16 C17 124.4(9) . . ? O12 C17 O11 125.7(10) . . ? O12 C17 C16 118.5(9) . . ? O11 C17 C16 115.8(8) . . ? N2 C21 C22 112.6(10) . . ? N21 C22 C23 126.0(10) . . ? N21 C22 C21 114.3(9) . . ? C23 C22 C21 119.6(11) . . ? C22 C23 C24 118.0(12) . . ? C25 C24 C23 115.8(12) . . ? C26 C25 C24 121.8(12) . . ? N21 C26 C25 121.7(14) . . ? N21 C26 C27 111.1(13) . . ? C25 C26 C27 127.2(13) . . ? O22 C27 O21 125.4(12) . . ? O22 C27 C26 116.9(12) . . ? O21 C27 C26 117.7(10) . . ? N3 C31 C32 111.6(7) . . ? N31 C32 C33 121.3(9) . . ? N31 C32 C31 114.0(8) . . ? C33 C32 C31 124.7(8) . . ? C34 C33 C32 118.8(9) . . ? C33 C34 C35 120.3(9) . . ? C34 C35 C36 118.6(9) . . ? N31 C36 C35 121.5(9) . . ? N31 C36 C37 115.3(8) . . ? C35 C36 C37 123.1(8) . . ? O32 C37 O31 126.3(9) . . ? O32 C37 C36 118.9(8) . . ? O31 C37 C36 114.8(8) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.622 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.125 #===END data_complex_Eu(tpatcn)_(2) _database_code_CSD 206376 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Eu N6 O9' _chemical_formula_weight 737.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 7.9946(18) _cell_length_b 11.947(3) _cell_length_c 14.884(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.953(15) _cell_angle_gamma 90.00 _cell_volume 1400.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6884 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.99 _reflns_number_total 4604 _reflns_number_gt 4052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(8) _refine_ls_number_reflns 4604 _refine_ls_number_parameters 512 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.009 _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 Eu Eu 0.324204(16) 0.275178(14) 0.818774(14) 0.01616(5) Uani 1 1 d . . . O11 O 0.5618(4) 0.3623(3) 0.9137(2) 0.0272(7) Uani 1 1 d . . . O12 O 0.6752(5) 0.4344(3) 1.0488(2) 0.0470(10) Uani 1 1 d . . . O21 O 0.4702(4) 0.3191(3) 0.6970(2) 0.0317(8) Uani 1 1 d . . . O22 O 0.5745(4) 0.4357(3) 0.6047(2) 0.0424(9) Uani 1 1 d . . . O31 O 0.4948(4) 0.1097(2) 0.83796(19) 0.0274(7) Uani 1 1 d . . . O32 O 0.5981(4) -0.0473(2) 0.7868(2) 0.0318(8) Uani 1 1 d . . . N1 N 0.0711(4) 0.1733(3) 0.8834(2) 0.0221(8) Uani 1 1 d . . . N2 N 0.1034(4) 0.4160(3) 0.8769(2) 0.0219(8) Uani 1 1 d . . . N3 N 0.0278(5) 0.2873(3) 0.7072(2) 0.0221(8) Uani 1 1 d . . . N11 N 0.3753(4) 0.2207(3) 0.9872(2) 0.0212(7) Uani 1 1 d . . . N21 N 0.3505(4) 0.4837(3) 0.7859(2) 0.0242(8) Uani 1 1 d . . . N31 N 0.2647(4) 0.1306(3) 0.6902(2) 0.0217(8) Uani 1 1 d . . . C1 C -0.0322(6) 0.2480(4) 0.9338(3) 0.0269(11) Uani 1 1 d . . . H1A H -0.159(11) 0.256(5) 0.893(6) 0.03(2) Uiso 1 1 d . . . H1B H -0.059(5) 0.211(3) 0.990(3) 0.009(9) Uiso 1 1 d . . . C2 C 0.0435(7) 0.3621(4) 0.9567(3) 0.0267(10) Uani 1 1 d . . . H2A H 0.137(6) 0.367(4) 1.004(3) 0.018(12) Uiso 1 1 d . . . H2B H -0.046(7) 0.399(4) 0.978(3) 0.035(14) Uiso 1 1 d . . . C3 C -0.0433(6) 0.4448(5) 0.8041(3) 0.0287(11) Uani 1 1 d . . . H3A H -0.140(8) 0.417(3) 0.819(5) 0.038(16) Uiso 1 1 d . . . H3B H -0.065(7) 0.525(5) 0.801(4) 0.057(18) Uiso 1 1 d . . . C4 C -0.0263(6) 0.4055(4) 0.7095(3) 0.0239(10) Uani 1 1 d . . . H4A H 0.054(5) 0.450(3) 0.688(2) 0.003(9) Uiso 1 1 d . . . H4B H -0.130(6) 0.416(3) 0.669(3) 0.019(11) Uiso 1 1 d . . . C5 C -0.1059(6) 0.2080(4) 0.7310(3) 0.0278(11) Uani 1 1 d . . . H5A H -0.162(5) 0.170(3) 0.675(3) 0.013(10) Uiso 1 1 d . . . H5B H -0.210(10) 0.249(5) 0.743(6) 0.02(2) Uiso 1 1 d . . . C6 C -0.0380(6) 0.1218(4) 0.8031(3) 0.0264(10) Uani 1 1 d . . . H6A H 0.031(6) 0.071(3) 0.775(3) 0.017(11) Uiso 1 1 d . . . H6B H -0.155(11) 0.080(4) 0.831(5) 0.067(18) Uiso 1 1 d . . . C11 C 0.1552(6) 0.0852(4) 0.9458(3) 0.0250(10) Uani 1 1 d . . . H11A H 0.075(5) 0.039(3) 0.982(3) 0.013(10) Uiso 1 1 d . . . H11B H 0.221(6) 0.027(4) 0.906(3) 0.009(11) Uiso 1 1 d . . . C12 C 0.2837(6) 0.1407(4) 1.0192(3) 0.0250(10) Uani 1 1 d . . . C13 C 0.3053(7) 0.1166(5) 1.1112(3) 0.0360(13) Uani 1 1 d . . . H13 H 0.249(6) 0.067(4) 1.125(3) 0.020(14) Uiso 1 1 d . . . C14 C 0.4194(7) 0.1757(5) 1.1714(3) 0.0441(14) Uani 1 1 d . . . H14 H 0.440(6) 0.152(4) 1.232(3) 0.030(13) Uiso 1 1 d . . . C15 C 0.5148(7) 0.2595(5) 1.1385(3) 0.0383(13) Uani 1 1 d . . . H15 H 0.606(7) 0.290(4) 1.179(4) 0.043(15) Uiso 1 1 d . . . C16 C 0.4885(6) 0.2789(5) 1.0451(3) 0.0259(11) Uani 1 1 d . . . C17 C 0.5842(6) 0.3670(4) 1.0003(3) 0.0274(11) Uani 1 1 d . . . C21 C 0.1995(11) 0.5172(7) 0.9077(6) 0.029(2) Uani 1 1 d . . . H21A H 0.130(7) 0.579(4) 0.930(4) 0.017(16) Uiso 1 1 d . . . H21B H 0.273(6) 0.505(3) 0.964(3) 0.020(12) Uiso 1 1 d . . . C22 C 0.3022(7) 0.5601(4) 0.8403(3) 0.0288(13) Uani 1 1 d . . . C23 C 0.3561(9) 0.6701(4) 0.8381(4) 0.0379(15) Uani 1 1 d . . . H23 H 0.321(8) 0.706(4) 0.870(4) 0.029(17) Uiso 1 1 d . . . C24 C 0.4622(8) 0.7000(4) 0.7778(4) 0.0439(16) Uani 1 1 d . . . H24 H 0.502(7) 0.769(4) 0.777(3) 0.039(15) Uiso 1 1 d . . . C25 C 0.5108(8) 0.6202(6) 0.7223(4) 0.0399(16) Uani 1 1 d . . . H25 H 0.587(9) 0.634(6) 0.690(4) 0.08(2) Uiso 1 1 d . . . C26 C 0.4550(9) 0.5132(7) 0.7259(5) 0.025(2) Uani 1 1 d . . . C27 C 0.5046(6) 0.4156(5) 0.6710(3) 0.0287(12) Uani 1 1 d . . . C31 C 0.0583(7) 0.2604(5) 0.6149(3) 0.0284(11) Uani 1 1 d . . . H31A H -0.049(5) 0.258(3) 0.572(3) 0.009(10) Uiso 1 1 d . . . H31B H 0.117(7) 0.314(5) 0.596(4) 0.025(18) Uiso 1 1 d . . . C32 C 0.1484(6) 0.1504(4) 0.6143(3) 0.0243(10) Uani 1 1 d . . . C33 C 0.1232(6) 0.0747(4) 0.5429(3) 0.0291(11) Uani 1 1 d . . . H33 H 0.048(7) 0.099(4) 0.483(4) 0.049(15) Uiso 1 1 d . . . C34 C 0.2209(6) -0.0209(5) 0.5491(3) 0.0329(12) Uani 1 1 d . . . H34 H 0.202(6) -0.061(4) 0.503(3) 0.028(13) Uiso 1 1 d . . . C35 C 0.3416(6) -0.0398(4) 0.6252(3) 0.0268(10) Uani 1 1 d . . . H35 H 0.409(6) -0.101(4) 0.630(3) 0.021(12) Uiso 1 1 d . . . C36 C 0.3614(6) 0.0393(4) 0.6946(3) 0.0211(10) Uani 1 1 d . . . C37 C 0.4966(6) 0.0315(4) 0.7804(3) 0.0229(10) Uani 1 1 d . . . O1 O 0.6330(7) 0.1844(5) 0.5339(4) 0.125(3) Uani 1 1 d . . . H1O1 H 0.5570 0.1946 0.4924 0.050 Uiso 1 1 d . . . H2O1 H 0.5996 0.1698 0.5704 0.050 Uiso 1 1 d . . . O2 O 0.2957(7) 0.3794(4) 0.4581(3) 0.0540(12) Uani 1 1 d . . . H1O2 H 0.412(16) 0.396(9) 0.507(7) 0.20(5) Uiso 1 1 d . . . H2O2 H 0.244(7) 0.427(5) 0.466(4) 0.03(2) Uiso 1 1 d . . . O3 O 0.3664(5) 0.1727(5) 0.3872(3) 0.0488(11) Uani 1 1 d . . . H1O3 H 0.302(11) 0.230(6) 0.397(5) 0.08(3) Uiso 1 1 d . . . H2O3 H 0.303(7) 0.125(4) 0.366(3) 0.037(17) Uiso 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 Eu 0.01482(8) 0.01813(8) 0.01574(7) -0.0004(2) 0.00326(5) -0.0002(2) O11 0.0207(17) 0.0318(19) 0.0281(17) 0.0044(15) 0.0017(13) -0.0044(15) O12 0.042(2) 0.053(3) 0.045(2) -0.0218(19) 0.0053(18) -0.0227(19) O21 0.036(2) 0.034(2) 0.0299(17) -0.0053(16) 0.0194(15) -0.0052(16) O22 0.0263(18) 0.078(3) 0.0272(17) 0.0185(18) 0.0152(15) -0.0053(18) O31 0.0334(19) 0.0244(17) 0.0211(15) -0.0052(13) -0.0049(14) 0.0089(14) O32 0.0324(19) 0.0205(17) 0.0393(19) -0.0043(14) -0.0029(15) 0.0061(15) N1 0.0190(18) 0.0219(19) 0.0251(18) 0.0002(16) 0.0034(15) -0.0007(16) N2 0.023(2) 0.023(2) 0.0210(18) -0.0022(16) 0.0066(15) -0.0016(16) N3 0.0186(18) 0.028(2) 0.0187(16) 0.0054(17) 0.0007(14) 0.0019(17) N11 0.0181(17) 0.0270(19) 0.0194(16) 0.0000(17) 0.0054(14) 0.0035(17) N21 0.0183(19) 0.031(2) 0.0226(18) 0.0074(17) 0.0010(16) 0.0007(18) N31 0.0208(18) 0.027(2) 0.0174(17) -0.0014(16) 0.0027(14) 0.0021(16) C1 0.023(2) 0.032(3) 0.029(2) 0.0071(19) 0.012(2) 0.0024(19) C2 0.025(3) 0.034(3) 0.024(2) 0.004(2) 0.013(2) 0.004(2) C3 0.024(3) 0.027(3) 0.036(3) 0.006(2) 0.007(2) 0.007(2) C4 0.021(2) 0.026(3) 0.025(2) 0.007(2) 0.005(2) 0.005(2) C5 0.020(2) 0.033(3) 0.029(2) 0.003(2) 0.0000(19) -0.002(2) C6 0.018(2) 0.028(3) 0.032(2) -0.002(2) 0.000(2) -0.005(2) C11 0.030(3) 0.021(3) 0.025(2) 0.009(2) 0.006(2) -0.002(2) C12 0.023(2) 0.024(2) 0.027(2) 0.0055(19) 0.0035(19) 0.0036(19) C13 0.033(3) 0.046(3) 0.031(3) 0.018(2) 0.010(2) 0.005(3) C14 0.041(3) 0.073(4) 0.018(2) 0.012(3) 0.006(2) 0.011(3) C15 0.035(3) 0.056(4) 0.021(2) -0.007(2) -0.003(2) 0.002(3) C16 0.019(2) 0.036(3) 0.023(2) -0.005(2) 0.0041(19) 0.001(3) C17 0.018(2) 0.028(3) 0.034(3) -0.011(2) -0.002(2) 0.003(2) C21 0.039(5) 0.022(4) 0.029(4) -0.008(4) 0.015(4) 0.001(4) C22 0.032(3) 0.020(2) 0.031(3) 0.000(2) -0.005(2) -0.001(2) C23 0.046(5) 0.024(3) 0.040(4) -0.004(3) -0.004(3) -0.002(3) C24 0.048(4) 0.026(3) 0.050(3) 0.012(2) -0.012(3) -0.022(3) C25 0.037(3) 0.049(4) 0.032(3) 0.013(3) -0.002(3) -0.017(3) C26 0.018(4) 0.034(5) 0.020(4) 0.006(4) -0.005(3) -0.005(4) C27 0.014(2) 0.048(4) 0.024(2) 0.005(2) 0.0023(18) -0.003(2) C31 0.028(3) 0.037(3) 0.018(2) 0.003(2) -0.002(2) 0.005(2) C32 0.023(2) 0.031(3) 0.020(2) 0.0024(19) 0.0052(18) 0.000(2) C33 0.027(3) 0.040(3) 0.019(2) -0.002(2) 0.0007(19) -0.006(2) C34 0.032(3) 0.039(3) 0.029(3) -0.014(2) 0.010(2) -0.011(2) C35 0.028(2) 0.024(3) 0.029(2) -0.005(2) 0.007(2) -0.001(2) C36 0.018(2) 0.027(3) 0.018(2) -0.0011(19) 0.0035(19) -0.002(2) C37 0.022(2) 0.020(2) 0.026(2) 0.004(2) 0.004(2) 0.000(2) O1 0.094(4) 0.118(5) 0.128(5) -0.061(4) -0.077(4) 0.050(4) O2 0.061(3) 0.045(3) 0.056(3) -0.011(2) 0.011(2) -0.005(2) O3 0.040(2) 0.067(3) 0.038(2) -0.017(2) 0.0005(18) -0.011(2) _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 Eu O21 2.377(3) . ? Eu O31 2.391(3) . ? Eu O11 2.400(3) . ? Eu N11 2.553(3) . ? Eu N21 2.554(4) . ? Eu N31 2.560(3) . ? Eu N3 2.652(3) . ? Eu N1 2.678(4) . ? Eu N2 2.688(4) . ? O11 C17 1.272(6) . ? O12 C17 1.231(5) . ? O21 C27 1.262(6) . ? O22 C27 1.239(6) . ? O31 C37 1.270(5) . ? O32 C37 1.236(5) . ? N1 C11 1.485(6) . ? N1 C6 1.485(5) . ? N1 C1 1.502(6) . ? N2 C21 1.463(9) . ? N2 C3 1.493(6) . ? N2 C2 1.499(6) . ? N3 C31 1.472(6) . ? N3 C4 1.479(6) . ? N3 C5 1.515(6) . ? N11 C16 1.334(6) . ? N11 C12 1.341(6) . ? N21 C22 1.321(5) . ? N21 C26 1.370(8) . ? N31 C36 1.332(6) . ? N31 C32 1.355(5) . ? C1 C2 1.506(7) . ? C3 C4 1.513(7) . ? C5 C6 1.518(6) . ? C11 C12 1.517(6) . ? C12 C13 1.380(6) . ? C13 C14 1.360(8) . ? C14 C15 1.398(8) . ? C15 C16 1.389(7) . ? C16 C17 1.521(8) . ? C21 C22 1.493(9) . ? C22 C23 1.385(7) . ? C23 C24 1.384(9) . ? C24 C25 1.362(9) . ? C25 C26 1.358(10) . ? C26 C27 1.515(10) . ? C31 C32 1.500(7) . ? C32 C33 1.383(6) . ? C33 C34 1.378(7) . ? C34 C35 1.373(7) . ? C35 C36 1.389(6) . ? C36 C37 1.526(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Eu O31 85.89(11) . . ? O21 Eu O11 84.85(11) . . ? O31 Eu O11 84.89(11) . . ? O21 Eu N11 142.03(11) . . ? O31 Eu N11 71.38(11) . . ? O11 Eu N11 63.68(11) . . ? O21 Eu N21 64.64(12) . . ? O31 Eu N21 139.92(11) . . ? O11 Eu N21 66.85(11) . . ? N11 Eu N21 115.60(12) . . ? O21 Eu N31 68.36(11) . . ? O31 Eu N31 63.89(10) . . ? O11 Eu N31 139.31(11) . . ? N11 Eu N31 122.63(13) . . ? N21 Eu N31 121.71(11) . . ? O21 Eu N3 90.81(11) . . ? O31 Eu N3 123.33(11) . . ? O11 Eu N3 151.13(13) . . ? N11 Eu N3 127.04(11) . . ? N21 Eu N3 85.49(11) . . ? N31 Eu N3 62.52(11) . . ? O21 Eu N1 151.01(11) . . ? O31 Eu N1 91.84(11) . . ? O11 Eu N1 123.78(10) . . ? N11 Eu N1 62.23(11) . . ? N21 Eu N1 127.18(11) . . ? N31 Eu N1 84.69(11) . . ? N3 Eu N1 66.47(11) . . ? O21 Eu N2 122.94(12) . . ? O31 Eu N2 150.70(10) . . ? O11 Eu N2 92.07(11) . . ? N11 Eu N2 81.14(11) . . ? N21 Eu N2 62.07(11) . . ? N31 Eu N2 127.98(11) . . ? N3 Eu N2 66.54(11) . . ? N1 Eu N2 65.79(11) . . ? C17 O11 Eu 125.1(3) . . ? C27 O21 Eu 126.6(3) . . ? C37 O31 Eu 126.9(3) . . ? C11 N1 C6 110.5(3) . . ? C11 N1 C1 109.7(3) . . ? C6 N1 C1 110.5(4) . . ? C11 N1 Eu 105.0(3) . . ? C6 N1 Eu 105.9(3) . . ? C1 N1 Eu 115.1(3) . . ? C21 N2 C3 109.9(5) . . ? C21 N2 C2 109.2(4) . . ? C3 N2 C2 110.8(4) . . ? C21 N2 Eu 106.2(4) . . ? C3 N2 Eu 112.8(3) . . ? C2 N2 Eu 107.7(3) . . ? C31 N3 C4 109.0(3) . . ? C31 N3 C5 108.6(4) . . ? C4 N3 C5 111.8(4) . . ? C31 N3 Eu 107.3(3) . . ? C4 N3 Eu 105.7(3) . . ? C5 N3 Eu 114.2(2) . . ? C16 N11 C12 119.5(4) . . ? C16 N11 Eu 118.5(3) . . ? C12 N11 Eu 121.8(3) . . ? C22 N21 C26 119.8(5) . . ? C22 N21 Eu 121.0(3) . . ? C26 N21 Eu 117.1(4) . . ? C36 N31 C32 119.5(4) . . ? C36 N31 Eu 119.0(3) . . ? C32 N31 Eu 121.2(3) . . ? N1 C1 C2 114.6(4) . . ? N2 C2 C1 112.4(4) . . ? N2 C3 C4 114.7(4) . . ? N3 C4 C3 113.0(4) . . ? N3 C5 C6 114.1(4) . . ? N1 C6 C5 112.2(4) . . ? N1 C11 C12 108.6(4) . . ? N11 C12 C13 121.3(4) . . ? N11 C12 C11 113.5(4) . . ? C13 C12 C11 125.2(4) . . ? C14 C13 C12 120.0(5) . . ? C13 C14 C15 119.0(5) . . ? C16 C15 C14 118.2(5) . . ? N11 C16 C15 121.9(5) . . ? N11 C16 C17 114.5(4) . . ? C15 C16 C17 123.6(5) . . ? O12 C17 O11 126.1(5) . . ? O12 C17 C16 119.1(5) . . ? O11 C17 C16 114.8(4) . . ? N2 C21 C22 113.2(6) . . ? N21 C22 C23 121.1(5) . . ? N21 C22 C21 115.3(5) . . ? C23 C22 C21 123.4(6) . . ? C24 C23 C22 119.2(6) . . ? C25 C24 C23 118.9(5) . . ? C26 C25 C24 120.3(7) . . ? C25 C26 N21 120.7(7) . . ? C25 C26 C27 125.7(7) . . ? N21 C26 C27 113.5(6) . . ? O22 C27 O21 125.0(5) . . ? O22 C27 C26 118.5(5) . . ? O21 C27 C26 116.5(5) . . ? N3 C31 C32 110.8(4) . . ? N31 C32 C33 121.0(4) . . ? N31 C32 C31 114.1(4) . . ? C33 C32 C31 124.9(4) . . ? C34 C33 C32 119.0(4) . . ? C35 C34 C33 120.0(5) . . ? C34 C35 C36 118.4(5) . . ? N31 C36 C35 122.0(4) . . ? N31 C36 C37 114.4(4) . . ? C35 C36 C37 123.6(4) . . ? O32 C37 O31 126.3(4) . . ? O32 C37 C36 118.1(4) . . ? O31 C37 C36 115.5(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 O1 H1O1 O3 0.80 2.00 2.778(6) 163.7 . O1 H1O1 O3 0.80 2.00 2.778(6) 163.7 . O2 H1O2 O22 1.10(12) 1.83(12) 2.916(6) 168(9) . O2 H2O2 O12 0.72(5) 2.20(5) 2.855(6) 153(6) 2_464 O3 H1O3 O2 0.88(8) 2.01(7) 2.782(7) 145(7) . O3 H2O3 O32 0.79(5) 2.07(6) 2.823(5) 161(5) 2_454 _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.553 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.081 #===END data_complex_Gd(tpatcn)_(3) _database_code_CSD 206377 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Gd N6 O9' _chemical_formula_weight 742.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.0251(7) _cell_length_b 11.9508(11) _cell_length_c 14.9011(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.992(2) _cell_angle_gamma 90.00 _cell_volume 1407.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8207 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.85 _reflns_number_total 4120 _reflns_number_gt 3530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(17) _refine_ls_number_reflns 4120 _refine_ls_number_parameters 388 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.32357(4) 0.27580(3) 0.81940(3) 0.02267(10) Uani 1 1 d . . . O11 O 0.5591(8) 0.3611(6) 0.9135(4) 0.0418(16) Uani 1 1 d . . . O12 O 0.6782(9) 0.4298(7) 1.0496(5) 0.067(2) Uani 1 1 d . . . O21 O 0.4693(8) 0.3190(6) 0.6986(4) 0.0433(15) Uani 1 1 d . . . O22 O 0.5749(9) 0.4324(7) 0.6069(5) 0.061(2) Uani 1 1 d . . . O31 O 0.4935(7) 0.1099(5) 0.8382(4) 0.0387(15) Uani 1 1 d . . . O32 O 0.5963(7) -0.0454(5) 0.7879(5) 0.0432(16) Uani 1 1 d . . . N1 N 0.0725(8) 0.1728(6) 0.8829(5) 0.0296(15) Uani 1 1 d . . . N2 N 0.1034(8) 0.4171(6) 0.8783(5) 0.0317(16) Uani 1 1 d . . . N3 N 0.0283(8) 0.2877(6) 0.7079(5) 0.0291(15) Uani 1 1 d . . . N11 N 0.3727(8) 0.2186(6) 0.9866(5) 0.0306(15) Uani 1 1 d . . . N21 N 0.3525(8) 0.4831(6) 0.7870(5) 0.0322(15) Uani 1 1 d . . . N31 N 0.2640(8) 0.1309(6) 0.6909(5) 0.0286(15) Uani 1 1 d . . . C1 C -0.0317(11) 0.2456(7) 0.9333(7) 0.038(2) Uani 1 1 d . . . H1A H -0.0448 0.2084 0.9896 0.046 Uiso 1 1 calc R . . H1B H -0.1434 0.2541 0.8969 0.046 Uiso 1 1 calc R . . C2 C 0.0434(13) 0.3610(8) 0.9560(7) 0.039(2) Uani 1 1 d . . . H2A H -0.0413 0.4079 0.9764 0.046 Uiso 1 1 calc R . . H2B H 0.1378 0.3542 1.0061 0.046 Uiso 1 1 calc R . . C3 C -0.0428(11) 0.4451(8) 0.8051(6) 0.038(2) Uani 1 1 d . . . H3A H -0.0582 0.5256 0.8037 0.046 Uiso 1 1 calc R . . H3B H -0.1442 0.4118 0.8206 0.046 Uiso 1 1 calc R . . C4 C -0.0241(11) 0.4059(8) 0.7100(7) 0.036(2) Uani 1 1 d . . . H4A H -0.1313 0.4156 0.6693 0.044 Uiso 1 1 calc R . . H4B H 0.0591 0.4524 0.6878 0.044 Uiso 1 1 calc R . . C5 C -0.1042(11) 0.2089(8) 0.7309(7) 0.039(2) Uani 1 1 d . . . H5A H -0.1565 0.1706 0.6758 0.047 Uiso 1 1 calc R . . H5B H -0.1914 0.2522 0.7526 0.047 Uiso 1 1 calc R . . C6 C -0.0357(11) 0.1213(8) 0.8031(7) 0.039(2) Uani 1 1 d . . . H6A H -0.1297 0.0831 0.8229 0.046 Uiso 1 1 calc R . . H6B H 0.0295 0.0660 0.7764 0.046 Uiso 1 1 calc R . . C11 C 0.1530(11) 0.0849(7) 0.9450(7) 0.038(2) Uani 1 1 d . . . H11A H 0.2086 0.0309 0.9115 0.045 Uiso 1 1 calc R . . H11B H 0.0683 0.0460 0.9723 0.045 Uiso 1 1 calc R . . C12 C 0.2811(11) 0.1396(7) 1.0182(6) 0.035(2) Uani 1 1 d . . . C13 C 0.3038(13) 0.1125(9) 1.1096(6) 0.048(2) Uani 1 1 d . . . H13A H 0.2408 0.0555 1.1300 0.058 Uiso 1 1 calc R . . C14 C 0.4199(14) 0.1706(11) 1.1693(7) 0.058(3) Uani 1 1 d . . . H14A H 0.4349 0.1542 1.2312 0.069 Uiso 1 1 calc R . . C15 C 0.5154(15) 0.2536(9) 1.1385(7) 0.052(3) Uani 1 1 d . . . H15A H 0.5938 0.2946 1.1789 0.063 Uiso 1 1 calc R . . C16 C 0.4909(13) 0.2745(9) 1.0443(7) 0.038(2) Uani 1 1 d . . . C17 C 0.5845(10) 0.3628(8) 1.0006(7) 0.038(2) Uani 1 1 d . . . C21 C 0.2031(18) 0.5157(11) 0.9097(11) 0.040(4) Uani 1 1 d . . . H21A H 0.2812 0.4970 0.9649 0.047 Uiso 1 1 calc R . . H21B H 0.1281 0.5737 0.9248 0.047 Uiso 1 1 calc R . . C22 C 0.3025(13) 0.5611(8) 0.8399(6) 0.036(2) Uani 1 1 d . . . C23 C 0.3546(15) 0.6726(8) 0.8377(7) 0.050(3) Uani 1 1 d . . . H23A H 0.3191 0.7255 0.8761 0.060 Uiso 1 1 calc R . . C24 C 0.4588(17) 0.7029(9) 0.7778(10) 0.068(4) Uani 1 1 d . . . H24A H 0.4944 0.7766 0.7747 0.081 Uiso 1 1 calc R . . C25 C 0.5101(13) 0.6215(10) 0.7220(8) 0.055(3) Uani 1 1 d . . . H25A H 0.5815 0.6401 0.6814 0.067 Uiso 1 1 calc R . . C26 C 0.4557(17) 0.5150(13) 0.7270(9) 0.037(4) Uani 1 1 d . . . C27 C 0.5036(11) 0.4150(9) 0.6740(6) 0.039(2) Uani 1 1 d . . . C31 C 0.0582(14) 0.2576(8) 0.6153(7) 0.037(2) Uani 1 1 d . . . H31A H -0.0496 0.2526 0.5744 0.044 Uiso 1 1 calc R . . H31B H 0.1238 0.3164 0.5929 0.044 Uiso 1 1 calc R . . C32 C 0.1489(10) 0.1503(8) 0.6146(6) 0.034(2) Uani 1 1 d . . . C33 C 0.1253(12) 0.0759(8) 0.5444(6) 0.040(2) Uani 1 1 d . . . H33A H 0.0443 0.0902 0.4929 0.048 Uiso 1 1 calc R . . C34 C 0.2209(12) -0.0205(8) 0.5491(7) 0.044(2) Uani 1 1 d . . . H34A H 0.2042 -0.0728 0.5022 0.052 Uiso 1 1 calc R . . C35 C 0.3438(11) -0.0372(8) 0.6267(7) 0.040(2) Uani 1 1 d . . . H35A H 0.4136 -0.0998 0.6315 0.047 Uiso 1 1 calc R . . C36 C 0.3597(10) 0.0401(7) 0.6955(6) 0.0309(18) Uani 1 1 d . . . C37 C 0.4954(10) 0.0328(7) 0.7818(6) 0.0298(18) Uani 1 1 d . . . O1 O 0.6264(14) 0.1789(11) 0.5377(10) 0.140(6) Uani 1 1 d . . . O2 O 0.2907(12) 0.3799(7) 0.4579(6) 0.080(3) Uani 1 1 d . . . O3 O 0.3631(10) 0.1706(8) 0.3862(5) 0.068(2) 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 Gd 0.02192(15) 0.02835(15) 0.01762(14) -0.0002(4) 0.00306(10) -0.0003(4) O11 0.035(4) 0.058(4) 0.029(4) 0.005(3) -0.003(3) -0.015(3) O12 0.065(5) 0.082(6) 0.051(5) -0.022(5) -0.003(4) -0.037(4) O21 0.048(4) 0.054(4) 0.033(4) -0.002(3) 0.022(3) -0.006(3) O22 0.048(4) 0.108(6) 0.032(4) 0.028(4) 0.017(3) -0.004(4) O31 0.045(4) 0.036(3) 0.030(3) -0.004(3) -0.005(3) 0.013(3) O32 0.044(4) 0.032(3) 0.049(4) -0.006(3) -0.005(3) 0.010(3) N1 0.030(3) 0.022(3) 0.037(4) 0.004(3) 0.008(3) -0.004(3) N2 0.033(4) 0.034(4) 0.029(4) 0.000(3) 0.009(3) -0.001(3) N3 0.026(3) 0.036(4) 0.024(4) 0.003(3) 0.001(3) 0.004(3) N11 0.029(3) 0.033(4) 0.029(4) 0.003(3) 0.004(3) 0.007(3) N21 0.025(3) 0.043(4) 0.029(4) 0.004(4) 0.005(3) -0.004(3) N31 0.024(3) 0.038(4) 0.022(3) 0.001(3) 0.000(3) -0.002(3) C1 0.027(4) 0.048(6) 0.041(5) 0.005(4) 0.013(4) -0.002(3) C2 0.041(5) 0.046(5) 0.031(5) 0.005(4) 0.013(4) 0.008(4) C3 0.034(5) 0.044(5) 0.038(5) 0.002(4) 0.007(4) 0.010(4) C4 0.032(5) 0.044(5) 0.033(5) 0.009(4) 0.006(4) 0.002(4) C5 0.025(4) 0.056(6) 0.036(5) 0.002(4) 0.003(4) -0.005(4) C6 0.026(4) 0.047(5) 0.042(5) 0.001(4) 0.003(4) -0.009(4) C11 0.036(5) 0.036(5) 0.041(6) 0.012(4) 0.005(4) -0.005(4) C12 0.035(4) 0.037(5) 0.034(5) 0.012(4) 0.009(4) 0.010(4) C13 0.054(6) 0.067(7) 0.024(5) 0.016(5) 0.010(4) 0.011(5) C14 0.068(7) 0.085(8) 0.021(5) 0.015(5) 0.008(5) 0.014(6) C15 0.056(6) 0.073(8) 0.025(5) -0.012(5) -0.002(5) 0.002(5) C16 0.033(5) 0.056(6) 0.023(4) -0.013(5) 0.002(4) 0.001(4) C17 0.026(4) 0.047(5) 0.037(5) -0.012(4) -0.001(4) 0.000(4) C21 0.045(8) 0.024(7) 0.052(10) -0.010(7) 0.016(7) 0.007(6) C22 0.038(6) 0.037(4) 0.030(7) 0.007(4) 0.000(4) 0.001(5) C23 0.074(9) 0.033(4) 0.034(8) 0.001(4) -0.015(6) -0.001(5) C24 0.085(9) 0.043(7) 0.064(9) 0.015(6) -0.017(7) -0.025(6) C25 0.047(6) 0.071(7) 0.042(6) 0.026(6) -0.012(5) -0.025(5) C26 0.029(6) 0.060(10) 0.018(6) 0.015(6) -0.006(5) -0.004(6) C27 0.025(4) 0.069(7) 0.025(5) 0.008(5) 0.006(4) -0.006(5) C31 0.035(5) 0.049(6) 0.026(5) 0.001(4) 0.004(4) 0.007(4) C32 0.027(4) 0.052(6) 0.021(4) 0.002(4) 0.002(3) 0.001(4) C33 0.041(5) 0.055(6) 0.021(4) 0.000(4) 0.000(4) -0.006(4) C34 0.056(6) 0.047(5) 0.027(5) -0.018(4) 0.003(4) -0.007(4) C35 0.044(5) 0.039(5) 0.036(5) -0.007(4) 0.007(4) 0.002(4) C36 0.027(4) 0.038(5) 0.029(5) 0.001(4) 0.007(3) 0.000(4) C37 0.033(4) 0.032(4) 0.024(4) 0.002(4) 0.002(4) -0.003(3) O1 0.103(8) 0.124(8) 0.156(13) -0.071(10) -0.079(8) 0.052(7) O2 0.100(6) 0.084(6) 0.056(6) -0.014(5) 0.015(5) -0.029(5) O3 0.064(5) 0.098(6) 0.037(4) -0.014(5) -0.001(4) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O21 2.367(6) . ? Gd O11 2.379(6) . ? Gd O31 2.395(6) . ? Gd N21 2.542(7) . ? Gd N11 2.547(7) . ? Gd N31 2.564(7) . ? Gd N3 2.651(7) . ? Gd N1 2.670(6) . ? Gd N2 2.699(7) . ? O11 C17 1.279(12) . ? O12 C17 1.245(11) . ? O21 C27 1.250(12) . ? O22 C27 1.252(11) . ? O31 C37 1.248(10) . ? O32 C37 1.230(10) . ? N1 C11 1.473(11) . ? N1 C6 1.479(11) . ? N1 C1 1.496(12) . ? N2 C21 1.455(15) . ? N2 C2 1.487(12) . ? N2 C3 1.495(11) . ? N3 C4 1.476(11) . ? N3 C31 1.486(12) . ? N3 C5 1.504(12) . ? N11 C12 1.332(11) . ? N11 C16 1.343(12) . ? N21 C22 1.327(11) . ? N21 C26 1.374(15) . ? N31 C36 1.324(11) . ? N31 C32 1.356(10) . ? C1 C2 1.520(13) . ? C3 C4 1.523(13) . ? C5 C6 1.533(13) . ? C11 C12 1.511(13) . ? C12 C13 1.381(12) . ? C13 C14 1.362(16) . ? C14 C15 1.381(17) . ? C15 C16 1.405(15) . ? C16 C17 1.508(15) . ? C21 C22 1.517(17) . ? C22 C23 1.399(13) . ? C23 C24 1.37(2) . ? C24 C25 1.388(18) . ? C25 C26 1.351(18) . ? C26 C27 1.519(19) . ? C31 C32 1.475(13) . ? C32 C33 1.361(12) . ? C33 C34 1.380(14) . ? C34 C35 1.397(13) . ? C35 C36 1.370(13) . ? C36 C37 1.536(12) . ? 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 O21 Gd O11 84.7(2) . . ? O21 Gd O31 85.6(2) . . ? O11 Gd O31 84.7(2) . . ? O21 Gd N21 64.5(2) . . ? O11 Gd N21 66.7(2) . . ? O31 Gd N21 139.5(2) . . ? O21 Gd N11 142.1(2) . . ? O11 Gd N11 64.3(2) . . ? O31 Gd N11 71.0(2) . . ? N21 Gd N11 116.3(2) . . ? O21 Gd N31 68.4(2) . . ? O11 Gd N31 139.1(2) . . ? O31 Gd N31 63.7(2) . . ? N21 Gd N31 121.9(2) . . ? N11 Gd N31 121.7(2) . . ? O21 Gd N3 91.0(2) . . ? O11 Gd N3 151.5(3) . . ? O31 Gd N3 123.1(2) . . ? N21 Gd N3 86.0(2) . . ? N11 Gd N3 126.7(2) . . ? N31 Gd N3 62.5(2) . . ? O21 Gd N1 150.7(2) . . ? O11 Gd N1 124.1(2) . . ? O31 Gd N1 91.5(2) . . ? N21 Gd N1 128.0(2) . . ? N11 Gd N1 61.8(2) . . ? N31 Gd N1 84.2(2) . . ? N3 Gd N1 66.4(2) . . ? O21 Gd N2 123.3(2) . . ? O11 Gd N2 92.2(2) . . ? O31 Gd N2 150.6(2) . . ? N21 Gd N2 62.5(2) . . ? N11 Gd N2 81.3(2) . . ? N31 Gd N2 128.2(2) . . ? N3 Gd N2 66.8(2) . . ? N1 Gd N2 66.2(2) . . ? C17 O11 Gd 125.1(6) . . ? C27 O21 Gd 125.9(6) . . ? C37 O31 Gd 127.2(5) . . ? C11 N1 C6 109.9(7) . . ? C11 N1 C1 108.7(7) . . ? C6 N1 C1 110.2(7) . . ? C11 N1 Gd 106.0(5) . . ? C6 N1 Gd 106.3(5) . . ? C1 N1 Gd 115.6(5) . . ? C21 N2 C2 110.4(9) . . ? C21 N2 C3 111.8(9) . . ? C2 N2 C3 110.5(7) . . ? C21 N2 Gd 104.9(7) . . ? C2 N2 Gd 106.8(5) . . ? C3 N2 Gd 112.2(5) . . ? C4 N3 C31 110.1(7) . . ? C4 N3 C5 112.3(7) . . ? C31 N3 C5 107.2(8) . . ? C4 N3 Gd 105.4(5) . . ? C31 N3 Gd 107.4(5) . . ? C5 N3 Gd 114.5(5) . . ? C12 N11 C16 119.9(8) . . ? C12 N11 Gd 122.3(6) . . ? C16 N11 Gd 117.7(6) . . ? C22 N21 C26 118.0(9) . . ? C22 N21 Gd 121.6(5) . . ? C26 N21 Gd 118.7(8) . . ? C36 N31 C32 119.2(8) . . ? C36 N31 Gd 118.9(5) . . ? C32 N31 Gd 121.5(6) . . ? N1 C1 C2 113.9(7) . . ? N2 C2 C1 113.9(8) . . ? N2 C3 C4 114.8(7) . . ? N3 C4 C3 112.8(8) . . ? N3 C5 C6 113.9(7) . . ? N1 C6 C5 111.6(7) . . ? N1 C11 C12 108.3(7) . . ? N11 C12 C13 121.9(9) . . ? N11 C12 C11 113.5(8) . . ? C13 C12 C11 124.6(9) . . ? C14 C13 C12 118.9(10) . . ? C13 C14 C15 120.4(9) . . ? C14 C15 C16 118.0(10) . . ? N11 C16 C15 120.9(10) . . ? N11 C16 C17 114.9(8) . . ? C15 C16 C17 124.2(9) . . ? O12 C17 O11 125.4(10) . . ? O12 C17 C16 119.5(9) . . ? O11 C17 C16 115.1(8) . . ? N2 C21 C22 113.3(11) . . ? N21 C22 C23 122.2(10) . . ? N21 C22 C21 113.9(8) . . ? C23 C22 C21 123.5(10) . . ? C24 C23 C22 119.0(12) . . ? C23 C24 C25 118.8(10) . . ? C26 C25 C24 119.6(12) . . ? C25 C26 N21 122.3(13) . . ? C25 C26 C27 126.8(12) . . ? N21 C26 C27 110.8(11) . . ? O21 C27 O22 122.7(10) . . ? O21 C27 C26 118.8(9) . . ? O22 C27 C26 118.5(10) . . ? C32 C31 N3 112.1(7) . . ? N31 C32 C33 121.1(8) . . ? N31 C32 C31 114.1(8) . . ? C33 C32 C31 124.8(8) . . ? C32 C33 C34 120.3(9) . . ? C33 C34 C35 117.9(8) . . ? C36 C35 C34 119.0(8) . . ? N31 C36 C35 122.4(8) . . ? N31 C36 C37 114.2(7) . . ? C35 C36 C37 123.3(8) . . ? O32 C37 O31 126.6(8) . . ? O32 C37 C36 117.8(8) . . ? O31 C37 C36 115.6(7) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 1.721 _refine_diff_density_min -1.443 _refine_diff_density_rms 0.134 #===END data_complex_Lu(tpatcn)_(4) _database_code_CSD 206378 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Lu N6 O9' _chemical_formula_weight 760.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.0084(6) _cell_length_b 11.8544(9) _cell_length_c 14.8334(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.6940(10) _cell_angle_gamma 90.00 _cell_volume 1388.10(19) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 3.622 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7054 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.85 _reflns_number_total 5165 _reflns_number_gt 4406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(12) _refine_ls_number_reflns 5165 _refine_ls_number_parameters 388 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.007 _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 Lu Lu 0.68294(4) 0.72385(2) 0.17968(3) 0.02099(8) Uani 1 1 d . . . O11 O 0.4463(7) 0.6422(6) 0.0919(4) 0.0341(14) Uani 1 1 d . . . O12 O 0.3224(8) 0.5685(6) -0.0406(5) 0.059(2) Uani 1 1 d . . . O21 O 0.5350(7) 0.6929(5) 0.2970(4) 0.0364(14) Uani 1 1 d . . . O22 O 0.4256(7) 0.5848(5) 0.3937(4) 0.0447(16) Uani 1 1 d . . . O31 O 0.5191(7) 0.8852(4) 0.1586(4) 0.0318(13) Uani 1 1 d . . . O32 O 0.4129(7) 1.0434(5) 0.2048(4) 0.0441(15) Uani 1 1 d . . . N1 N 0.9299(7) 0.8238(6) 0.1168(4) 0.0271(14) Uani 1 1 d . . . N2 N 0.8894(8) 0.5805(6) 0.1196(4) 0.0278(15) Uani 1 1 d . . . N3 N 0.9712(9) 0.7070(6) 0.2900(5) 0.0298(16) Uani 1 1 d . . . N11 N 0.6312(8) 0.7795(6) 0.0155(4) 0.0286(14) Uani 1 1 d . . . N21 N 0.6476(8) 0.5202(6) 0.2147(4) 0.0309(15) Uani 1 1 d . . . N31 N 0.7442(8) 0.8668(5) 0.3046(4) 0.0263(14) Uani 1 1 d . . . C1 C 1.0299(11) 0.7493(6) 0.0651(6) 0.035(2) Uani 1 1 d . . . H1A H 1.1413 0.7383 0.1014 0.042 Uiso 1 1 calc R . . H1B H 1.0450 0.7875 0.0093 0.042 Uiso 1 1 calc R . . C2 C 0.9526(12) 0.6352(8) 0.0404(6) 0.034(2) Uani 1 1 d . . . H2A H 0.8591 0.6435 -0.0100 0.041 Uiso 1 1 calc R . . H2B H 1.0366 0.5867 0.0202 0.041 Uiso 1 1 calc R . . C3 C 1.0363(10) 0.5462(8) 0.1915(6) 0.038(2) Uani 1 1 d . . . H3A H 1.1398 0.5764 0.1752 0.046 Uiso 1 1 calc R . . H3B H 1.0454 0.4646 0.1918 0.046 Uiso 1 1 calc R . . C4 C 1.0219(10) 0.5860(7) 0.2877(6) 0.0311(18) Uani 1 1 d . . . H4A H 0.9389 0.5399 0.3112 0.037 Uiso 1 1 calc R . . H4B H 1.1301 0.5755 0.3274 0.037 Uiso 1 1 calc R . . C5 C 1.1077(10) 0.7843(7) 0.2667(6) 0.037(2) Uani 1 1 d . . . H5A H 1.1929 0.7390 0.2444 0.044 Uiso 1 1 calc R . . H5B H 1.1618 0.8216 0.3222 0.044 Uiso 1 1 calc R . . C6 C 1.0442(10) 0.8738(7) 0.1955(5) 0.0328(19) Uani 1 1 d . . . H6A H 0.9841 0.9319 0.2232 0.039 Uiso 1 1 calc R . . H6B H 1.1400 0.9087 0.1743 0.039 Uiso 1 1 calc R . . C11 C 0.8512(11) 0.9121(7) 0.0541(6) 0.034(2) Uani 1 1 d . . . H11A H 0.9367 0.9493 0.0255 0.040 Uiso 1 1 calc R . . H11B H 0.7983 0.9682 0.0877 0.040 Uiso 1 1 calc R . . C12 C 0.7207(10) 0.8586(7) -0.0175(5) 0.0305(18) Uani 1 1 d . . . C13 C 0.6947(11) 0.8862(8) -0.1099(6) 0.042(2) Uani 1 1 d . . . H13A H 0.7565 0.9440 -0.1310 0.051 Uiso 1 1 calc R . . C14 C 0.5792(13) 0.8283(10) -0.1685(6) 0.054(3) Uani 1 1 d . . . H14A H 0.5633 0.8436 -0.2309 0.065 Uiso 1 1 calc R . . C15 C 0.4837(13) 0.7452(8) -0.1347(6) 0.048(3) Uani 1 1 d . . . H15A H 0.4030 0.7045 -0.1741 0.057 Uiso 1 1 calc R . . C16 C 0.5108(12) 0.7237(8) -0.0405(6) 0.0324(18) Uani 1 1 d . . . C17 C 0.4196(10) 0.6376(7) 0.0058(6) 0.0326(19) Uani 1 1 d . . . C21 C 0.7881(16) 0.4799(11) 0.0874(9) 0.034(3) Uani 1 1 d . . . H21A H 0.8629 0.4201 0.0741 0.041 Uiso 1 1 calc R . . H21B H 0.7116 0.4980 0.0314 0.041 Uiso 1 1 calc R . . C22 C 0.6854(14) 0.4386(7) 0.1595(5) 0.030(2) Uani 1 1 d . . . C23 C 0.6325(11) 0.3281(7) 0.1641(7) 0.043(2) Uani 1 1 d . . . H23A H 0.6665 0.2727 0.1267 0.051 Uiso 1 1 calc R . . C24 C 0.5260(13) 0.3022(7) 0.2270(7) 0.048(3) Uani 1 1 d . . . H24A H 0.4849 0.2294 0.2314 0.058 Uiso 1 1 calc R . . C25 C 0.4832(12) 0.3883(8) 0.2828(6) 0.041(2) Uani 1 1 d . . . H25A H 0.4143 0.3729 0.3259 0.050 Uiso 1 1 calc R . . C26 C 0.5434(15) 0.4978(12) 0.2743(8) 0.030(3) Uani 1 1 d . . . C27 C 0.4980(11) 0.5995(9) 0.3260(6) 0.032(2) Uani 1 1 d . . . C31 C 0.9419(13) 0.7364(8) 0.3820(6) 0.035(2) Uani 1 1 d . . . H31A H 0.8740 0.6781 0.4041 0.041 Uiso 1 1 calc R . . H31B H 1.0497 0.7400 0.4232 0.041 Uiso 1 1 calc R . . C32 C 0.8546(10) 0.8458(7) 0.3825(6) 0.0314(19) Uani 1 1 d . . . C33 C 0.8748(11) 0.9182(7) 0.4543(5) 0.035(2) Uani 1 1 d . . . H33A H 0.9520 0.9022 0.5069 0.042 Uiso 1 1 calc R . . C34 C 0.7804(12) 1.0154(8) 0.4486(6) 0.044(2) Uani 1 1 d . . . H34A H 0.7957 1.0669 0.4966 0.053 Uiso 1 1 calc R . . C35 C 0.6620(11) 1.0363(7) 0.3708(6) 0.038(2) Uani 1 1 d . . . H35A H 0.5946 1.1006 0.3664 0.046 Uiso 1 1 calc R . . C36 C 0.6465(10) 0.9592(6) 0.2995(5) 0.0288(18) Uani 1 1 d . . . C37 C 0.5164(10) 0.9658(7) 0.2147(5) 0.0294(18) Uani 1 1 d . . . O1 O 0.3574(13) 0.8211(9) 0.4748(8) 0.127(5) Uani 1 1 d . . . O2 O 0.7058(10) 0.6268(6) 0.5420(5) 0.065(2) Uani 1 1 d . . . O3 O 0.6364(8) 0.8384(7) 0.6166(4) 0.0612(19) 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 Lu 0.02017(12) 0.02224(12) 0.02060(12) 0.0004(4) 0.00355(9) 0.0002(4) O11 0.029(3) 0.046(4) 0.025(3) 0.003(3) -0.002(3) -0.008(3) O12 0.047(4) 0.070(5) 0.056(5) -0.015(4) -0.003(4) -0.027(4) O21 0.043(3) 0.035(4) 0.034(3) -0.003(3) 0.016(3) -0.004(3) O22 0.039(4) 0.063(4) 0.035(3) 0.012(3) 0.018(3) 0.000(3) O31 0.036(3) 0.032(3) 0.023(3) 0.001(2) -0.007(2) 0.012(2) O32 0.045(4) 0.022(3) 0.058(4) -0.005(3) -0.011(3) 0.014(3) N1 0.021(3) 0.026(3) 0.036(4) 0.002(3) 0.007(3) -0.002(3) N2 0.027(4) 0.031(4) 0.026(4) -0.002(3) 0.007(3) -0.005(3) N3 0.029(4) 0.031(4) 0.029(4) -0.001(3) 0.002(3) -0.004(3) N11 0.028(3) 0.034(4) 0.023(3) 0.004(3) 0.005(3) -0.002(3) N21 0.031(4) 0.033(4) 0.028(4) 0.001(3) 0.002(3) 0.006(3) N31 0.024(3) 0.032(4) 0.023(3) 0.001(3) 0.004(3) -0.002(3) C1 0.034(5) 0.038(6) 0.037(5) 0.006(4) 0.017(4) 0.003(3) C2 0.034(5) 0.046(6) 0.027(5) 0.004(4) 0.016(4) 0.009(4) C3 0.029(5) 0.042(5) 0.046(6) -0.001(4) 0.013(4) 0.005(4) C4 0.023(4) 0.039(5) 0.030(4) 0.005(4) 0.001(3) 0.006(4) C5 0.028(4) 0.034(5) 0.048(5) -0.003(4) 0.007(4) -0.011(4) C6 0.027(4) 0.036(5) 0.035(5) 0.004(4) 0.005(4) -0.004(4) C11 0.033(5) 0.036(5) 0.031(5) 0.011(4) 0.004(4) 0.004(4) C12 0.032(4) 0.033(5) 0.027(4) 0.007(3) 0.006(4) 0.005(4) C13 0.042(5) 0.050(6) 0.034(5) 0.009(4) 0.005(4) 0.006(4) C14 0.068(7) 0.075(7) 0.020(5) 0.009(5) 0.013(5) 0.001(6) C15 0.053(6) 0.069(8) 0.016(4) -0.011(4) -0.009(4) 0.010(5) C16 0.032(5) 0.036(5) 0.026(4) -0.007(4) -0.006(4) 0.001(5) C17 0.026(4) 0.036(5) 0.032(5) -0.007(4) -0.006(4) 0.002(4) C21 0.039(7) 0.025(5) 0.040(7) -0.011(5) 0.012(5) 0.002(5) C22 0.031(4) 0.030(4) 0.026(6) 0.005(3) -0.008(5) 0.003(4) C23 0.060(8) 0.024(4) 0.039(6) 0.007(4) -0.006(5) -0.002(4) C24 0.062(6) 0.029(5) 0.045(6) 0.008(4) -0.016(5) -0.020(4) C25 0.048(6) 0.044(5) 0.029(5) 0.013(4) -0.005(4) -0.013(4) C26 0.022(5) 0.045(7) 0.018(5) 0.001(5) -0.009(4) -0.006(5) C27 0.025(5) 0.046(6) 0.026(5) 0.003(4) 0.005(4) -0.001(4) C31 0.028(5) 0.044(6) 0.031(5) 0.002(4) 0.003(4) -0.001(4) C32 0.029(4) 0.031(5) 0.034(5) 0.002(4) 0.004(4) -0.002(4) C33 0.039(5) 0.045(6) 0.020(4) -0.007(4) 0.003(4) -0.009(4) C34 0.056(6) 0.047(6) 0.029(5) -0.019(4) 0.003(4) -0.002(5) C35 0.049(5) 0.029(5) 0.037(5) -0.010(4) 0.007(4) 0.003(4) C36 0.034(5) 0.023(4) 0.030(4) -0.001(3) 0.004(4) -0.003(4) C37 0.039(5) 0.021(4) 0.028(4) 0.004(3) 0.004(4) 0.002(4) O1 0.091(7) 0.106(7) 0.153(10) -0.070(7) -0.067(7) 0.038(6) O2 0.076(5) 0.061(5) 0.056(5) -0.010(4) 0.011(4) -0.018(4) O3 0.048(4) 0.091(6) 0.042(4) -0.011(4) 0.000(3) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu O21 2.293(5) . ? Lu O31 2.311(5) . ? Lu O11 2.322(6) . ? Lu N11 2.490(6) . ? Lu N21 2.495(7) . ? Lu N31 2.498(6) . ? Lu N3 2.603(7) . ? Lu N1 2.609(6) . ? Lu N2 2.628(6) . ? O11 C17 1.261(10) . ? O12 C17 1.253(10) . ? O21 C27 1.242(11) . ? O22 C27 1.253(10) . ? O31 C37 1.270(9) . ? O32 C37 1.229(9) . ? N1 C11 1.470(10) . ? N1 C6 1.481(10) . ? N1 C1 1.489(10) . ? N2 C21 1.476(13) . ? N2 C2 1.502(10) . ? N2 C3 1.505(10) . ? N3 C4 1.493(10) . ? N3 C31 1.466(11) . ? N3 C5 1.510(10) . ? N11 C12 1.323(10) . ? N11 C16 1.337(11) . ? N21 C22 1.335(9) . ? N21 C26 1.341(13) . ? N31 C36 1.340(10) . ? N31 C32 1.355(10) . ? C1 C2 1.507(13) . ? C3 C4 1.525(11) . ? C5 C6 1.522(11) . ? C11 C12 1.501(12) . ? C12 C13 1.390(11) . ? C13 C14 1.346(13) . ? C14 C15 1.391(14) . ? C15 C16 1.401(12) . ? C16 C17 1.488(13) . ? C21 C22 1.534(15) . ? C22 C23 1.383(12) . ? C23 C24 1.400(14) . ? C24 C25 1.393(13) . ? C25 C26 1.398(16) . ? C26 C27 1.505(16) . ? C31 C32 1.474(13) . ? C32 C33 1.356(11) . ? C33 C34 1.373(12) . ? C34 C35 1.387(12) . ? C35 C36 1.387(11) . ? C36 C37 1.494(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Lu O31 83.2(2) . . ? O21 Lu O11 83.2(2) . . ? O31 Lu O11 83.0(2) . . ? O21 Lu N11 139.7(2) . . ? O31 Lu N11 69.6(2) . . ? O11 Lu N11 64.9(2) . . ? O21 Lu N21 66.2(2) . . ? O31 Lu N21 138.3(2) . . ? O11 Lu N21 66.6(2) . . ? N11 Lu N21 117.0(2) . . ? O21 Lu N31 66.9(2) . . ? O31 Lu N31 64.84(19) . . ? O11 Lu N31 137.6(2) . . ? N11 Lu N31 121.7(2) . . ? N21 Lu N31 121.1(2) . . ? O21 Lu N3 91.6(2) . . ? O31 Lu N3 124.9(2) . . ? O11 Lu N3 151.0(3) . . ? N11 Lu N3 128.3(2) . . ? N21 Lu N3 85.1(2) . . ? N31 Lu N3 62.8(2) . . ? O21 Lu N1 149.7(2) . . ? O31 Lu N1 91.3(2) . . ? O11 Lu N1 125.8(2) . . ? N11 Lu N1 62.7(2) . . ? N21 Lu N1 129.3(2) . . ? N31 Lu N1 83.7(2) . . ? N3 Lu N1 67.3(2) . . ? O21 Lu N2 126.0(2) . . ? O31 Lu N2 149.82(19) . . ? O11 Lu N2 92.4(2) . . ? N11 Lu N2 81.4(2) . . ? N21 Lu N2 62.9(2) . . ? N31 Lu N2 129.3(2) . . ? N3 Lu N2 67.8(2) . . ? N1 Lu N2 67.3(2) . . ? C17 O11 Lu 124.7(5) . . ? C27 O21 Lu 126.1(6) . . ? C37 O31 Lu 127.3(5) . . ? C11 N1 C6 110.9(6) . . ? C11 N1 C1 107.9(6) . . ? C6 N1 C1 109.2(6) . . ? C11 N1 Lu 106.2(4) . . ? C6 N1 Lu 107.8(4) . . ? C1 N1 Lu 114.8(5) . . ? C21 N2 C2 109.5(8) . . ? C21 N2 C3 109.4(8) . . ? C2 N2 C3 110.2(6) . . ? C21 N2 Lu 106.8(6) . . ? C2 N2 Lu 107.5(5) . . ? C3 N2 Lu 113.4(4) . . ? C4 N3 C31 109.7(6) . . ? C4 N3 C5 111.6(6) . . ? C31 N3 C5 107.7(7) . . ? C4 N3 Lu 106.0(5) . . ? C31 N3 Lu 107.6(5) . . ? C5 N3 Lu 114.1(5) . . ? C12 N11 C16 120.0(7) . . ? C12 N11 Lu 122.6(5) . . ? C16 N11 Lu 117.4(6) . . ? C22 N21 C26 119.5(8) . . ? C22 N21 Lu 121.9(5) . . ? C26 N21 Lu 115.7(7) . . ? C36 N31 C32 119.3(7) . . ? C36 N31 Lu 118.2(5) . . ? C32 N31 Lu 121.8(5) . . ? N1 C1 C2 115.1(7) . . ? N2 C2 C1 112.0(7) . . ? N2 C3 C4 113.9(6) . . ? N3 C4 C3 112.5(7) . . ? N3 C5 C6 114.3(7) . . ? N1 C6 C5 111.0(7) . . ? N1 C11 C12 108.7(7) . . ? N11 C12 C13 122.1(8) . . ? N11 C12 C11 113.2(7) . . ? C13 C12 C11 124.7(8) . . ? C14 C13 C12 119.3(9) . . ? C13 C14 C15 119.2(8) . . ? C16 C15 C14 119.1(9) . . ? N11 C16 C15 120.2(9) . . ? N11 C16 C17 114.3(7) . . ? C15 C16 C17 125.4(8) . . ? O12 C17 O11 124.6(9) . . ? O12 C17 C16 120.2(8) . . ? O11 C17 C16 115.1(7) . . ? N2 C21 C22 111.2(9) . . ? N21 C22 C23 123.6(9) . . ? N21 C22 C21 113.6(8) . . ? C23 C22 C21 122.8(9) . . ? C22 C23 C24 117.8(9) . . ? C25 C24 C23 118.3(8) . . ? C26 C25 C24 120.3(9) . . ? N21 C26 C25 120.4(11) . . ? N21 C26 C27 114.1(11) . . ? C25 C26 C27 125.5(10) . . ? O22 C27 O21 124.9(9) . . ? O22 C27 C26 118.7(9) . . ? O21 C27 C26 116.4(8) . . ? C32 C31 N3 111.4(7) . . ? N31 C32 C33 121.9(8) . . ? N31 C32 C31 113.6(7) . . ? C33 C32 C31 124.5(8) . . ? C32 C33 C34 119.4(8) . . ? C33 C34 C35 119.5(8) . . ? C34 C35 C36 118.5(8) . . ? N31 C36 C35 121.3(8) . . ? N31 C36 C37 114.1(7) . . ? C35 C36 C37 124.5(8) . . ? O32 C37 O31 124.7(8) . . ? O32 C37 C36 120.0(7) . . ? O31 C37 C36 115.2(7) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.979 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.125 #===END