# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Michael Drew' 'Clement Hill' 'Michael J Hudson' 'Peter B. Iveson' 'Charles Madic' 'Ludovic Vaillant' 'Tristan G. A. Youngs' _publ_contact_author_name 'Prof Michael Drew' _publ_contact_author_address ; Department of Chemistry University of Reading Whiteknights Reading Berks RG6 6AD UNITED KINGDOM ; _publ_contact_author_email M.G.B.DREW@READING.AC.UK _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Separation of lanthanides and actinides using tridentate benzimidazole, benzoxazole and benzothiazole ligands ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_La-1 _database_code_depnum_ccdc_archive 'CCDC 193084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 La N6 O14.50' _chemical_formula_weight 700.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 33.77(4) _cell_length_b 8.900(14) _cell_length_c 21.83(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.805(10) _cell_angle_gamma 90.00 _cell_volume 5113(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2756 _exptl_absorpt_coefficient_mu 1.755 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.192 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2 intervals, counting time 2 min.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6052 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.11 _reflns_number_total 3612 _reflns_number_gt 2251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+23.4505P] 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 3612 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2361 _refine_ls_wR_factor_gt 0.2119 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.283 _refine_ls_shift/su_mean 0.027 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.18890(3) 0.65945(8) 0.29080(5) 0.0628(4) Uani 1 d . . . N43 N 0.1540(6) 0.6640(13) 0.3959(8) 0.080(3) Uani 1 d . . . O41 O 0.1267(4) 0.7019(12) 0.3256(7) 0.089(3) Uani 1 d . . . O44 O 0.1358(5) 0.6484(12) 0.4291(8) 0.103(4) Uani 1 d . . . O42 O 0.2004(4) 0.6335(11) 0.4277(7) 0.086(3) Uani 1 d . . . N53 N 0.1750(4) 0.5294(14) 0.1488(7) 0.067(3) Uani 1 d . . . O51 O 0.1608(4) 0.6614(10) 0.1466(6) 0.073(3) Uani 1 d . . . O52 O 0.1903(4) 0.4483(10) 0.2108(6) 0.076(3) Uani 1 d . . . O54 O 0.1726(4) 0.4755(11) 0.0952(6) 0.080(3) Uani 1 d . . . N63 N 0.1516(4) 0.9720(13) 0.2111(7) 0.065(3) Uani 1 d . . . O62 O 0.1977(4) 0.9374(10) 0.2427(6) 0.076(3) Uani 1 d . . . O64 O 0.1372(4) 1.0960(13) 0.1808(7) 0.092(3) Uani 1 d . . . O61 O 0.1285(3) 0.8870(9) 0.2215(5) 0.065(2) Uani 1 d . . . N11 N 0.1570(4) 0.3851(12) 0.3025(7) 0.064(3) Uani 1 d . . . C12 C 0.1048(6) 0.3502(14) 0.2548(9) 0.068(4) Uani 1 d . . . C13 C 0.0868(5) 0.2177(15) 0.2606(9) 0.074(4) Uani 1 d . . . H13 H 0.0521 0.1968 0.2268 0.088 Uiso 1 calc R . . C14 C 0.1224(6) 0.1120(16) 0.3200(9) 0.077(4) Uani 1 d . . . H14 H 0.1119 0.0225 0.3277 0.092 Uiso 1 calc R . . C15 C 0.1735(6) 0.1505(16) 0.3654(10) 0.085(5) Uani 1 d . . . H15 H 0.1974 0.0839 0.4043 0.101 Uiso 1 calc R . . C16 C 0.1905(5) 0.2799(15) 0.3561(8) 0.063(3) Uani 1 d . . . N21 N 0.2613(4) 0.4486(11) 0.3959(6) 0.063(3) Uani 1 d . . . O23 O 0.2800(4) 0.2212(11) 0.4522(6) 0.077(3) Uani 1 d . . . C22 C 0.2427(5) 0.3161(15) 0.4012(8) 0.067(4) Uani 1 d . . . C24 C 0.3240(5) 0.2948(15) 0.4823(7) 0.061(3) Uani 1 d . . . C25 C 0.3740(6) 0.2361(18) 0.5380(8) 0.078(4) Uani 1 d . . . H25 H 0.3795 0.1386 0.5572 0.093 Uiso 1 calc R . . C26 C 0.4127(6) 0.3280(18) 0.5616(12) 0.098(6) Uani 1 d . . . H26 H 0.4458 0.2941 0.5993 0.117 Uiso 1 calc R . . C27 C 0.4044(6) 0.480(2) 0.5299(9) 0.092(5) Uani 1 d . . . H27 H 0.4319 0.5420 0.5474 0.110 Uiso 1 calc R . . C28 C 0.3537(5) 0.5312(16) 0.4717(9) 0.073(4) Uani 1 d . . . H28 H 0.3472 0.6269 0.4501 0.088 Uiso 1 calc R . . N31 N 0.0892(4) 0.5702(12) 0.1757(7) 0.065(3) Uani 1 d . . . C29 C 0.3144(5) 0.4338(15) 0.4484(9) 0.068(4) Uani 1 d . . . C34 C 0.0029(5) 0.5490(14) 0.0884(8) 0.064(3) Uani 1 d . . . C35 C -0.0484(6) 0.5694(16) 0.0242(9) 0.080(4) Uani 1 d . . . H35 H -0.0744 0.5087 0.0139 0.096 Uiso 1 calc R . . C36 C -0.0565(5) 0.6940(16) -0.0239(9) 0.075(4) Uani 1 d . . . H36 H -0.0893 0.7197 -0.0676 0.090 Uiso 1 calc R . . C37 C -0.0151(5) 0.7765(15) -0.0049(9) 0.069(4) Uani 1 d . . . H37 H -0.0210 0.8540 -0.0384 0.083 Uiso 1 calc R . . C38 C 0.0319(5) 0.7503(16) 0.0577(9) 0.075(4) Uani 1 d . . . H38 H 0.0576 0.8129 0.0683 0.090 Uiso 1 calc R . . C39 C 0.0443(5) 0.6342(15) 0.1080(8) 0.064(3) Uani 1 d . . . C32 C 0.0740(5) 0.4529(15) 0.1923(8) 0.063(3) Uani 1 d . . . O33 O 0.0213(4) 0.4330(11) 0.1426(6) 0.084(3) Uani 1 d . . . O100 O 0.2526(4) 0.8363(10) 0.4062(6) 0.084(3) Uani 1 d . . . O200 O 0.2646(3) 0.6795(9) 0.2931(6) 0.073(3) Uani 1 d . . . O300 O 0.0000 -0.004(4) 0.2500 0.198(11) Uiso 1 d S . . O400 O 0.0000 -0.132(4) 0.2500 0.217(13) Uiso 1 d S . . O500 O 0.0000 0.690(4) 0.2500 0.225(13) Uiso 1 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0718(6) 0.0499(6) 0.0766(6) 0.0009(4) 0.0513(5) 0.0007(4) N43 0.093(10) 0.075(9) 0.081(9) 0.014(7) 0.059(8) 0.011(7) O41 0.100(8) 0.085(7) 0.100(8) 0.006(6) 0.072(7) 0.020(6) O44 0.115(9) 0.106(9) 0.118(10) 0.000(7) 0.089(8) -0.004(6) O42 0.093(8) 0.086(7) 0.091(7) 0.009(6) 0.063(6) 0.007(6) N53 0.078(8) 0.062(9) 0.069(8) -0.017(7) 0.050(6) -0.009(6) O51 0.084(7) 0.050(6) 0.093(7) 0.004(5) 0.060(6) 0.004(4) O52 0.080(6) 0.079(7) 0.080(7) 0.001(5) 0.055(5) 0.006(5) O54 0.093(7) 0.083(7) 0.073(6) -0.006(5) 0.058(5) 0.010(5) N63 0.064(7) 0.047(7) 0.083(8) -0.007(6) 0.044(6) -0.019(6) O62 0.068(6) 0.074(7) 0.088(7) 0.000(5) 0.050(5) -0.007(5) O64 0.107(8) 0.066(7) 0.127(9) 0.023(7) 0.085(7) 0.019(6) O61 0.084(6) 0.048(5) 0.081(6) 0.001(4) 0.060(5) -0.007(4) N11 0.065(7) 0.061(7) 0.083(7) -0.004(6) 0.055(6) -0.007(5) C12 0.088(10) 0.046(9) 0.086(10) -0.002(7) 0.063(8) 0.000(7) C13 0.078(9) 0.042(8) 0.103(11) 0.000(7) 0.058(8) 0.004(7) C14 0.087(11) 0.055(9) 0.091(11) 0.002(8) 0.058(9) -0.006(7) C15 0.097(12) 0.072(11) 0.100(11) 0.030(8) 0.069(10) 0.022(8) C16 0.086(10) 0.046(8) 0.072(9) 0.011(7) 0.056(8) 0.011(7) N21 0.080(8) 0.045(7) 0.069(7) -0.008(5) 0.049(6) 0.001(5) O23 0.075(7) 0.074(6) 0.080(6) 0.007(5) 0.047(5) 0.012(5) C22 0.065(9) 0.053(9) 0.080(9) -0.001(7) 0.044(7) 0.003(7) C24 0.055(8) 0.057(9) 0.064(8) -0.021(7) 0.034(6) -0.006(6) C25 0.100(12) 0.080(11) 0.063(8) 0.014(8) 0.056(8) 0.013(9) C26 0.062(9) 0.086(12) 0.149(16) 0.011(11) 0.068(10) 0.018(8) C27 0.078(11) 0.100(13) 0.086(11) 0.013(9) 0.046(9) -0.004(9) C28 0.067(9) 0.066(9) 0.081(9) -0.005(7) 0.044(8) -0.003(7) N31 0.074(7) 0.054(7) 0.079(8) 0.001(6) 0.055(6) -0.004(5) C29 0.068(9) 0.050(9) 0.096(11) 0.001(7) 0.057(8) 0.003(6) C34 0.078(10) 0.048(8) 0.071(9) 0.002(7) 0.050(8) 0.006(6) C35 0.090(11) 0.058(10) 0.085(10) -0.002(8) 0.051(9) 0.002(7) C36 0.052(8) 0.079(10) 0.082(10) 0.004(8) 0.036(7) 0.008(7) C37 0.086(11) 0.045(8) 0.088(10) 0.016(7) 0.059(9) 0.008(7) C38 0.063(9) 0.063(10) 0.090(10) 0.008(8) 0.043(8) -0.008(7) C39 0.051(7) 0.068(9) 0.072(9) -0.002(7) 0.037(7) -0.006(6) C32 0.056(8) 0.066(9) 0.070(9) -0.015(7) 0.041(7) -0.010(6) O33 0.082(7) 0.079(7) 0.094(7) -0.004(6) 0.056(6) -0.010(5) O100 0.086(7) 0.077(7) 0.096(7) -0.017(5) 0.060(6) -0.007(5) O200 0.077(6) 0.060(6) 0.095(7) -0.013(5) 0.061(5) -0.006(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 La1 O200 2.533(9) . ? La1 O100 2.581(10) . ? La1 O61 2.585(9) . ? La1 O52 2.587(10) . ? La1 O51 2.658(11) . ? La1 O41 2.670(11) . ? La1 N11 2.744(11) . ? La1 O42 2.771(11) . ? La1 N31 2.770(11) . ? La1 O62 2.775(10) . ? La1 N21 2.781(11) . ? N43 O41 1.243(16) . ? N43 O44 1.217(16) . ? N43 O42 1.284(16) . ? N53 O54 1.217(14) . ? N53 O51 1.260(13) . ? N53 O52 1.320(14) . ? N63 O64 1.220(13) . ? N63 O61 1.205(12) . ? N63 O62 1.284(13) . ? N11 C16 1.366(16) . ? N11 C12 1.410(17) . ? C12 C13 1.370(18) . ? C12 C32 1.414(18) . ? C13 C14 1.43(2) . ? C14 C15 1.39(2) . ? C15 C16 1.358(18) . ? C16 C22 1.416(18) . ? N21 C22 1.376(16) . ? N21 C29 1.402(16) . ? O23 C22 1.335(15) . ? O23 C24 1.358(14) . ? C24 C29 1.373(18) . ? C24 C25 1.423(19) . ? C25 C26 1.34(2) . ? C26 C27 1.47(2) . ? C27 C28 1.424(19) . ? C28 C29 1.389(18) . ? N31 C32 1.311(16) . ? N31 C39 1.414(16) . ? C34 C35 1.398(19) . ? C34 C39 1.403(17) . ? C34 O33 1.388(15) . ? C35 C36 1.43(2) . ? C36 C37 1.393(18) . ? C37 C38 1.312(17) . ? C38 C39 1.369(19) . ? C32 O33 1.399(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 O200 La1 O100 74.0(3) . . ? O200 La1 O61 111.9(3) . . ? O100 La1 O61 87.9(3) . . ? O200 La1 O52 67.6(3) . . ? O100 La1 O52 138.2(3) . . ? O61 La1 O52 121.0(3) . . ? O200 La1 O51 68.3(3) . . ? O100 La1 O51 127.8(3) . . ? O61 La1 O51 74.7(3) . . ? O52 La1 O51 49.4(3) . . ? O200 La1 O41 161.6(3) . . ? O100 La1 O41 87.6(4) . . ? O61 La1 O41 65.4(3) . . ? O52 La1 O41 130.2(3) . . ? O51 La1 O41 125.1(3) . . ? O200 La1 N11 120.7(3) . . ? O100 La1 N11 126.0(4) . . ? O61 La1 N11 122.7(3) . . ? O52 La1 N11 65.8(3) . . ? O51 La1 N11 104.2(3) . . ? O41 La1 N11 71.1(3) . . ? O200 La1 O42 121.8(3) . . ? O100 La1 O42 62.0(3) . . ? O61 La1 O42 102.9(3) . . ? O52 La1 O42 128.2(3) . . ? O51 La1 O42 169.2(3) . . ? O41 La1 O42 46.3(3) . . ? N11 La1 O42 67.9(3) . . ? O200 La1 N31 132.6(3) . . ? O100 La1 N31 148.9(3) . . ? O61 La1 N31 68.3(3) . . ? O52 La1 N31 72.9(3) . . ? O51 La1 N31 66.3(3) . . ? O41 La1 N31 64.7(4) . . ? N11 La1 N31 60.3(3) . . ? O42 La1 N31 102.9(3) . . ? O200 La1 O62 66.3(3) . . ? O100 La1 O62 66.7(3) . . ? O61 La1 O62 46.6(3) . . ? O52 La1 O62 109.9(3) . . ? O51 La1 O62 65.8(3) . . ? O41 La1 O62 105.7(3) . . ? N11 La1 O62 165.8(3) . . ? O42 La1 O62 120.4(3) . . ? N31 La1 O62 105.7(3) . . ? O200 La1 N21 71.1(3) . . ? O100 La1 N21 80.9(3) . . ? O61 La1 N21 167.1(3) . . ? O52 La1 N21 71.8(3) . . ? O51 La1 N21 117.3(3) . . ? O41 La1 N21 107.6(3) . . ? N11 La1 N21 61.1(3) . . ? O42 La1 N21 66.3(3) . . ? N31 La1 N21 119.7(3) . . ? O62 La1 N21 131.8(3) . . ? O41 N43 O44 120.4(15) . . ? O41 N43 O42 115.8(13) . . ? O44 N43 O42 123.6(14) . . ? N43 O41 La1 101.9(9) . . ? N43 O42 La1 95.7(8) . . ? O54 N53 O51 122.5(13) . . ? O54 N53 O52 121.1(12) . . ? O51 N53 O52 116.3(11) . . ? N53 O51 La1 96.0(8) . . ? N53 O52 La1 97.7(7) . . ? O64 N63 O61 125.8(12) . . ? O64 N63 O62 116.4(10) . . ? O61 N63 O62 117.2(11) . . ? N63 O62 La1 92.0(7) . . ? N63 O61 La1 103.7(8) . . ? C16 N11 C12 117.5(11) . . ? C16 N11 La1 121.8(8) . . ? C12 N11 La1 120.6(8) . . ? C13 C12 C32 123.0(13) . . ? C13 C12 N11 123.0(12) . . ? C32 C12 N11 113.2(11) . . ? C12 C13 C14 118.6(13) . . ? C15 C14 C13 116.5(13) . . ? C16 C15 C14 123.6(14) . . ? N11 C16 C15 120.6(13) . . ? N11 C16 C22 116.2(12) . . ? C15 C16 C22 123.2(13) . . ? C22 N21 C29 105.5(10) . . ? C22 N21 La1 115.8(8) . . ? C29 N21 La1 138.6(8) . . ? C22 O23 C24 105.9(11) . . ? O23 C22 N21 111.7(11) . . ? O23 C22 C16 123.3(12) . . ? N21 C22 C16 124.9(12) . . ? O23 C24 C29 110.8(11) . . ? O23 C24 C25 126.0(13) . . ? C29 C24 C25 123.0(13) . . ? C26 C25 C24 116.9(14) . . ? C25 C26 C27 122.0(15) . . ? C26 C27 C28 118.9(15) . . ? C29 C28 C27 117.9(14) . . ? C32 N31 C39 105.1(11) . . ? C32 N31 La1 116.2(8) . . ? C39 N31 La1 136.9(8) . . ? C28 C29 C24 121.0(13) . . ? C28 C29 N21 132.8(13) . . ? C24 C29 N21 106.0(11) . . ? C35 C34 C39 127.4(14) . . ? C35 C34 O33 124.2(13) . . ? C39 C34 O33 108.3(12) . . ? C34 C35 C36 112.6(13) . . ? C37 C36 C35 119.7(13) . . ? C38 C37 C36 123.3(14) . . ? C37 C38 C39 122.3(13) . . ? C38 C39 C34 114.7(12) . . ? C38 C39 N31 137.1(12) . . ? C34 C39 N31 108.2(12) . . ? N31 C32 C12 127.0(12) . . ? N31 C32 O33 114.5(12) . . ? C12 C32 O33 118.5(11) . . ? C34 O33 C32 103.8(10) . . ? _refine_diff_density_max 1.544 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.128 #===END data_Nd-2 _database_code_depnum_ccdc_archive 'CCDC 193085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 N7 Nd O11' _chemical_formula_weight 684.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.094(13) _cell_length_b 9.561(13) _cell_length_c 15.038(17) _cell_angle_alpha 98.736(10) _cell_angle_beta 100.343(10) _cell_angle_gamma 93.335(10) _cell_volume 1266(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 2.123 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.199 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4581 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.07 _reflns_number_total 4581 _reflns_number_gt 2355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1632P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4581 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1796 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2579 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.67053(9) 0.75014(8) 0.76178(5) 0.0720(4) Uani 1 d . . . N21 N 0.4840(12) 0.6255(10) 0.8488(6) 0.065(3) Uani 1 d . . . C22 C 0.4321(14) 0.4934(14) 0.8166(9) 0.065(3) Uani 1 d . . . O23 O 0.3493(11) 0.4327(9) 0.8706(6) 0.072(2) Uani 1 d . . . C24 C 0.3445(16) 0.5434(13) 0.9405(9) 0.068(3) Uani 1 d . . . C25 C 0.2669(16) 0.5420(15) 1.0083(10) 0.081(4) Uani 1 d . . . H25 H 0.2107 0.4605 1.0139 0.097 Uiso 1 calc R . . C26 C 0.274(2) 0.6694(18) 1.0707(10) 0.094(5) Uani 1 d . . . H26 H 0.2237 0.6738 1.1196 0.113 Uiso 1 calc R . . C27 C 0.3583(19) 0.7892(17) 1.0576(12) 0.091(5) Uani 1 d . . . H27 H 0.3661 0.8731 1.0991 0.110 Uiso 1 calc R . . C28 C 0.4301(18) 0.7846(15) 0.9838(10) 0.084(4) Uani 1 d . . . H28 H 0.4829 0.8653 0.9739 0.100 Uiso 1 calc R . . C29 C 0.4218(14) 0.6599(13) 0.9263(8) 0.063(3) Uani 1 d . . . N11 N 0.5488(11) 0.4812(10) 0.6902(7) 0.062(3) Uani 1 d . . . C12 C 0.4605(15) 0.4079(13) 0.7339(9) 0.068(3) Uani 1 d . . . C13 C 0.4069(15) 0.2689(13) 0.7036(10) 0.073(3) Uani 1 d . . . H13 H 0.3496 0.2212 0.7369 0.087 Uiso 1 calc R . . C14 C 0.4399(17) 0.1999(14) 0.6217(11) 0.084(4) Uani 1 d . . . H14 H 0.4040 0.1056 0.5996 0.101 Uiso 1 calc R . . C15 C 0.5262(15) 0.2725(13) 0.5732(9) 0.068(3) Uani 1 d . . . H15 H 0.5456 0.2301 0.5171 0.081 Uiso 1 calc R . . C16 C 0.5830(14) 0.4115(12) 0.6120(9) 0.065(3) Uani 1 d . . . N31 N 0.7394(12) 0.6269(10) 0.6050(7) 0.067(3) Uani 1 d . . . C34 C 0.8087(16) 0.5493(15) 0.4715(10) 0.074(4) Uani 1 d . . . C35 C 0.8779(18) 0.5417(17) 0.3953(10) 0.083(4) Uani 1 d . . . H35 H 0.8652 0.4626 0.3493 0.099 Uiso 1 calc R . . C36 C 0.9654(19) 0.6614(18) 0.3954(12) 0.092(5) Uani 1 d . . . H36 H 1.0113 0.6667 0.3453 0.111 Uiso 1 calc R . . C37 C 0.9894(18) 0.7740(19) 0.4648(12) 0.094(5) Uani 1 d . . . H37 H 1.0549 0.8508 0.4617 0.113 Uiso 1 calc R . . C38 C 0.9205(17) 0.7790(19) 0.5401(11) 0.090(4) Uani 1 d . . . H38 H 0.9360 0.8576 0.5865 0.108 Uiso 1 calc R . . C39 C 0.8265(16) 0.6594(15) 0.5423(10) 0.072(4) Uani 1 d . . . C32 C 0.6802(14) 0.5003(13) 0.5711(9) 0.068(3) Uani 1 d . . . O33 O 0.7138(10) 0.4439(9) 0.4905(6) 0.073(2) Uani 1 d . . . O51 O 0.6853(15) 0.9338(13) 0.6562(9) 0.105(4) Uani 1 d . . . O52 O 0.7966(12) 1.0026(11) 0.7956(9) 0.092(3) Uani 1 d . . . N53 N 0.7648(17) 1.0294(15) 0.7162(13) 0.094(4) Uani 1 d . . . O54 O 0.8068(18) 1.1439(14) 0.6997(11) 0.141(5) Uani 1 d . . . O41 O 0.4082(11) 0.7617(9) 0.6715(6) 0.083(3) Uani 1 d . . . O42 O 0.4751(11) 0.9211(9) 0.7940(7) 0.080(3) Uani 1 d . . . N43 N 0.3802(15) 0.8718(12) 0.7227(9) 0.077(3) Uani 1 d . . . O44 O 0.2648(14) 0.9305(12) 0.7012(9) 0.100(3) Uani 1 d . . . N71 N 0.7637(14) 0.8285(12) 0.9332(8) 0.084(4) Uani 1 d . . . C72 C 0.824(2) 0.8637(18) 1.0079(13) 0.101(5) Uani 1 d . . . C73 C 0.837(3) 0.918(3) 1.1053(14) 0.155(10) Uani 1 d . . . H73A H 0.8719 1.0175 1.1172 0.186 Uiso 1 calc R . . H73B H 0.9072 0.8672 1.1405 0.186 Uiso 1 calc R . . H73C H 0.7408 0.9068 1.1224 0.186 Uiso 1 calc R . . O61 O 0.8394(13) 0.5628(12) 0.8052(8) 0.094(3) Uani 1 d . . . N63 N 0.9587(14) 0.635(2) 0.7978(7) 0.090(4) Uani 1 d . . . O64 O 1.0775(15) 0.5719(17) 0.8114(9) 0.131(5) Uani 1 d . . . O62 O 0.9605(15) 0.7545(14) 0.7763(13) 0.144(7) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0689(6) 0.0684(5) 0.0771(5) 0.0039(3) 0.0162(3) 0.0070(3) N21 0.074(7) 0.069(6) 0.049(6) 0.007(4) 0.009(5) 0.009(5) C22 0.047(7) 0.077(8) 0.067(8) 0.001(6) 0.003(6) 0.012(6) O23 0.079(6) 0.073(5) 0.073(6) 0.015(4) 0.029(5) 0.017(5) C24 0.077(9) 0.068(8) 0.067(8) 0.011(6) 0.030(7) 0.008(7) C25 0.070(9) 0.076(9) 0.096(11) 0.009(7) 0.014(8) 0.014(7) C26 0.123(14) 0.111(13) 0.059(9) 0.020(8) 0.030(8) 0.047(11) C27 0.093(12) 0.076(10) 0.099(12) -0.001(8) 0.014(9) 0.013(9) C28 0.091(11) 0.076(9) 0.088(10) 0.003(7) 0.034(8) 0.014(8) C29 0.054(8) 0.070(8) 0.069(8) 0.016(6) 0.014(6) 0.022(6) N11 0.054(6) 0.056(5) 0.078(7) 0.010(5) 0.013(5) 0.010(5) C12 0.064(9) 0.066(8) 0.073(8) 0.005(6) 0.012(7) 0.019(7) C13 0.067(9) 0.062(7) 0.089(9) 0.012(6) 0.019(7) -0.001(6) C14 0.077(10) 0.056(7) 0.113(12) 0.002(7) 0.012(8) -0.001(7) C15 0.071(9) 0.065(7) 0.070(8) 0.008(6) 0.021(6) 0.013(7) C16 0.057(8) 0.057(7) 0.082(9) 0.001(6) 0.022(6) 0.013(6) N31 0.061(7) 0.063(6) 0.076(7) 0.004(5) 0.017(5) 0.007(5) C34 0.061(9) 0.078(9) 0.087(10) 0.008(7) 0.021(7) 0.020(7) C35 0.097(12) 0.092(10) 0.072(9) 0.020(7) 0.040(8) 0.021(9) C36 0.087(12) 0.104(12) 0.097(12) 0.012(9) 0.043(9) 0.027(10) C37 0.080(11) 0.106(12) 0.109(13) 0.032(10) 0.044(9) 0.001(9) C38 0.072(10) 0.111(12) 0.091(11) 0.016(9) 0.028(8) 0.011(9) C39 0.064(9) 0.077(8) 0.079(9) 0.011(7) 0.024(7) 0.008(7) C32 0.051(8) 0.071(8) 0.080(9) 0.004(6) 0.012(6) 0.017(6) O33 0.074(6) 0.072(5) 0.073(6) 0.004(4) 0.022(4) 0.002(5) O51 0.125(10) 0.098(8) 0.107(9) 0.021(7) 0.057(7) 0.016(7) O52 0.082(7) 0.087(7) 0.107(8) 0.018(6) 0.023(6) -0.010(6) N53 0.091(10) 0.077(9) 0.129(13) 0.025(9) 0.051(9) 0.014(8) O54 0.154(13) 0.096(9) 0.194(15) 0.052(9) 0.073(11) -0.006(9) O41 0.090(7) 0.066(5) 0.084(6) -0.005(4) 0.007(5) 0.007(5) O42 0.072(6) 0.063(5) 0.098(7) -0.004(5) 0.012(5) 0.008(5) N43 0.079(9) 0.060(6) 0.097(9) 0.009(6) 0.030(7) 0.007(6) O44 0.087(8) 0.090(7) 0.128(9) 0.028(6) 0.020(6) 0.032(6) N71 0.088(9) 0.081(8) 0.067(7) -0.011(5) -0.007(6) -0.002(6) C72 0.094(13) 0.091(11) 0.115(15) 0.013(10) 0.013(10) 0.000(9) C73 0.17(2) 0.18(2) 0.111(17) -0.032(14) 0.073(15) -0.027(17) O61 0.080(8) 0.098(7) 0.105(8) 0.013(6) 0.015(6) 0.031(6) N63 0.042(8) 0.171(15) 0.049(7) -0.016(7) 0.017(5) 0.017(10) O64 0.090(10) 0.196(14) 0.104(10) -0.005(8) 0.022(7) 0.047(9) O62 0.082(9) 0.088(8) 0.235(18) 0.011(10) -0.024(10) -0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O61 2.512(10) . ? Nd1 O41 2.542(10) . ? Nd1 O42 2.544(9) . ? Nd1 N71 2.545(11) . ? Nd1 O52 2.549(10) . ? Nd1 O51 2.553(12) . ? Nd1 O62 2.604(14) . ? Nd1 N21 2.654(11) . ? Nd1 N31 2.667(11) . ? Nd1 N11 2.720(10) . ? N21 C22 1.310(15) . ? N21 C29 1.389(16) . ? C22 O23 1.369(16) . ? C22 C12 1.453(17) . ? O23 C24 1.383(14) . ? C24 C25 1.341(19) . ? C24 C29 1.348(18) . ? C25 C26 1.411(19) . ? C26 C27 1.40(2) . ? C27 C28 1.38(2) . ? C28 C29 1.352(18) . ? N11 C12 1.353(17) . ? N11 C16 1.356(15) . ? C12 C13 1.369(17) . ? C13 C14 1.40(2) . ? C14 C15 1.39(2) . ? C15 C16 1.397(17) . ? C16 C32 1.465(19) . ? N31 C32 1.286(15) . ? N31 C39 1.393(18) . ? C34 C39 1.358(18) . ? C34 O33 1.385(16) . ? C34 C35 1.398(19) . ? C35 C36 1.36(2) . ? C36 C37 1.36(2) . ? C37 C38 1.38(2) . ? C38 C39 1.40(2) . ? C32 O33 1.344(15) . ? O51 N53 1.269(18) . ? O52 N53 1.246(18) . ? N53 O54 1.214(17) . ? O41 N43 1.273(14) . ? O42 N43 1.258(15) . ? N43 O44 1.235(15) . ? N71 C72 1.15(2) . ? C72 C73 1.46(3) . ? O61 N63 1.284(17) . ? N63 O62 1.231(19) . ? N63 O64 1.270(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O61 Nd1 O41 137.9(4) . . ? O61 Nd1 O42 151.8(4) . . ? O41 Nd1 O42 50.6(3) . . ? O61 Nd1 N71 76.6(4) . . ? O41 Nd1 N71 127.3(4) . . ? O42 Nd1 N71 81.0(4) . . ? O61 Nd1 O52 115.0(4) . . ? O41 Nd1 O52 106.5(3) . . ? O42 Nd1 O52 71.5(3) . . ? N71 Nd1 O52 69.1(4) . . ? O61 Nd1 O51 132.1(4) . . ? O41 Nd1 O51 71.9(4) . . ? O42 Nd1 O51 74.1(4) . . ? N71 Nd1 O51 118.3(4) . . ? O52 Nd1 O51 49.7(4) . . ? O61 Nd1 O62 51.5(4) . . ? O41 Nd1 O62 152.2(5) . . ? O42 Nd1 O62 138.7(4) . . ? N71 Nd1 O62 77.7(5) . . ? O52 Nd1 O62 67.9(4) . . ? O51 Nd1 O62 85.6(5) . . ? O61 Nd1 N21 84.6(4) . . ? O41 Nd1 N21 74.0(3) . . ? O42 Nd1 N21 72.2(3) . . ? N71 Nd1 N21 72.1(4) . . ? O52 Nd1 N21 129.9(3) . . ? O51 Nd1 N21 142.4(4) . . ? O62 Nd1 N21 131.4(5) . . ? O61 Nd1 N31 74.8(4) . . ? O41 Nd1 N31 87.0(3) . . ? O42 Nd1 N31 131.5(3) . . ? N71 Nd1 N31 145.6(4) . . ? O52 Nd1 N31 106.7(4) . . ? O51 Nd1 N31 70.4(4) . . ? O62 Nd1 N31 69.7(4) . . ? N21 Nd1 N31 123.2(3) . . ? O61 Nd1 N11 66.7(3) . . ? O41 Nd1 N11 71.2(3) . . ? O42 Nd1 N11 113.0(3) . . ? N71 Nd1 N11 121.9(4) . . ? O52 Nd1 N11 168.0(4) . . ? O51 Nd1 N11 119.7(4) . . ? O62 Nd1 N11 108.3(4) . . ? N21 Nd1 N11 61.4(3) . . ? N31 Nd1 N11 61.8(3) . . ? C22 N21 C29 104.2(11) . . ? C22 N21 Nd1 118.2(9) . . ? C29 N21 Nd1 137.5(8) . . ? N21 C22 O23 114.4(11) . . ? N21 C22 C12 126.3(13) . . ? O23 C22 C12 119.2(11) . . ? C22 O23 C24 103.0(10) . . ? C25 C24 C29 124.0(12) . . ? C25 C24 O23 126.8(12) . . ? C29 C24 O23 109.0(11) . . ? C24 C25 C26 117.2(15) . . ? C27 C26 C25 118.6(14) . . ? C28 C27 C26 121.0(14) . . ? C29 C28 C27 118.3(15) . . ? C24 C29 C28 120.6(13) . . ? C24 C29 N21 109.1(11) . . ? C28 C29 N21 130.2(13) . . ? C12 N11 C16 117.2(10) . . ? C12 N11 Nd1 121.7(8) . . ? C16 N11 Nd1 120.9(8) . . ? N11 C12 C13 123.3(12) . . ? N11 C12 C22 112.1(11) . . ? C13 C12 C22 124.5(14) . . ? C12 C13 C14 118.7(14) . . ? C15 C14 C13 119.8(12) . . ? C14 C15 C16 117.4(12) . . ? N11 C16 C15 123.4(12) . . ? N11 C16 C32 112.5(10) . . ? C15 C16 C32 124.0(12) . . ? C32 N31 C39 103.7(11) . . ? C32 N31 Nd1 117.8(9) . . ? C39 N31 Nd1 138.4(8) . . ? C39 C34 O33 107.4(12) . . ? C39 C34 C35 126.3(15) . . ? O33 C34 C35 126.3(13) . . ? C36 C35 C34 113.0(14) . . ? C35 C36 C37 123.3(15) . . ? C36 C37 C38 122.7(16) . . ? C37 C38 C39 116.2(15) . . ? C34 C39 N31 109.2(13) . . ? C34 C39 C38 118.4(13) . . ? N31 C39 C38 132.3(12) . . ? N31 C32 O33 115.9(13) . . ? N31 C32 C16 126.8(13) . . ? O33 C32 C16 117.3(11) . . ? C32 O33 C34 103.7(10) . . ? N53 O51 Nd1 96.3(10) . . ? N53 O52 Nd1 97.1(9) . . ? O54 N53 O52 120.0(17) . . ? O54 N53 O51 123.1(18) . . ? O52 N53 O51 116.9(14) . . ? N43 O41 Nd1 95.3(8) . . ? N43 O42 Nd1 95.6(8) . . ? O44 N43 O42 121.1(11) . . ? O44 N43 O41 120.5(12) . . ? O42 N43 O41 118.3(12) . . ? C72 N71 Nd1 171.3(14) . . ? N71 C72 C73 157(2) . . ? N63 O61 Nd1 93.7(10) . . ? O62 N63 O64 121.4(16) . . ? O62 N63 O61 124.2(14) . . ? O64 N63 O61 114.4(17) . . ? N63 O62 Nd1 90.7(10) . . ? _refine_diff_density_max 1.586 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.193 data_2-Pr _database_code_depnum_ccdc_archive 'CCDC 193086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 N7 O11 Pr' _chemical_formula_weight 681.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.769(12) _cell_length_b 9.483(12) _cell_length_c 15.525(17) _cell_angle_alpha 99.735(10) _cell_angle_beta 98.239(10) _cell_angle_gamma 93.805(10) _cell_volume 1254(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 2.017 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4377 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.97 _reflns_number_total 4377 _reflns_number_gt 3957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1632P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4377 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.351 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.66466(3) 0.74912(2) 0.758107(16) 0.0340(2) Uani 1 d . . . N21 N 0.4766(5) 0.6207(5) 0.8481(3) 0.0348(9) Uani 1 d . . . C22 C 0.4280(6) 0.4857(6) 0.8197(4) 0.0361(11) Uani 1 d . . . O23 O 0.3432(4) 0.4246(4) 0.8719(3) 0.0405(8) Uani 1 d . . . C24 C 0.3322(6) 0.5353(6) 0.9426(4) 0.0389(12) Uani 1 d . . . C25 C 0.2542(8) 0.5339(7) 1.0116(4) 0.0524(15) Uani 1 d . . . H25 H 0.1981 0.4513 1.0190 0.063 Uiso 1 calc R . . C26 C 0.2625(8) 0.6632(7) 1.0708(4) 0.0543(16) Uani 1 d . . . H26 H 0.2123 0.6671 1.1199 0.065 Uiso 1 calc R . . C27 C 0.3440(9) 0.7857(9) 1.0579(5) 0.0579(18) Uani 1 d . . . H27 H 0.3490 0.8698 1.0992 0.069 Uiso 1 calc R . . C28 C 0.4191(8) 0.7869(7) 0.9844(5) 0.0511(16) Uani 1 d . . . H28 H 0.4700 0.8706 0.9746 0.061 Uiso 1 calc R . . C29 C 0.4142(6) 0.6569(6) 0.9266(3) 0.0369(11) Uani 1 d . . . N11 N 0.5425(5) 0.4751(5) 0.6917(3) 0.0369(10) Uani 1 d . . . C12 C 0.4556(6) 0.4004(6) 0.7367(4) 0.0372(11) Uani 1 d . . . C13 C 0.3956(7) 0.2595(6) 0.7056(4) 0.0482(14) Uani 1 d . . . H13 H 0.3377 0.2108 0.7390 0.058 Uiso 1 calc R . . C14 C 0.4233(8) 0.1924(6) 0.6239(5) 0.0540(16) Uani 1 d . . . H14 H 0.3817 0.0986 0.6008 0.065 Uiso 1 calc R . . C15 C 0.5123(7) 0.2648(6) 0.5774(4) 0.0453(13) Uani 1 d . . . H15 H 0.5335 0.2209 0.5227 0.054 Uiso 1 calc R . . C16 C 0.5711(6) 0.4066(6) 0.6138(4) 0.0364(11) Uani 1 d . . . N31 N 0.7357(5) 0.6208(5) 0.6047(3) 0.0373(10) Uani 1 d . . . C34 C 0.8032(6) 0.5418(6) 0.4718(4) 0.0383(11) Uani 1 d . . . C35 C 0.8723(7) 0.5358(8) 0.3968(4) 0.0443(13) Uani 1 d . . . H35 H 0.8545 0.4574 0.3505 0.053 Uiso 1 calc R . . C36 C 0.9706(8) 0.6566(8) 0.3962(5) 0.0562(16) Uani 1 d . . . H36 H 1.0212 0.6596 0.3478 0.067 Uiso 1 calc R . . C37 C 0.9958(8) 0.7739(8) 0.4662(5) 0.0548(17) Uani 1 d . . . H37 H 1.0615 0.8530 0.4624 0.066 Uiso 1 calc R . . C38 C 0.9264(8) 0.7758(8) 0.5403(5) 0.0578(19) Uani 1 d . . . H38 H 0.9456 0.8532 0.5873 0.069 Uiso 1 calc R . . C39 C 0.8255(7) 0.6556(6) 0.5418(4) 0.0405(12) Uani 1 d . . . C32 C 0.6717(6) 0.4932(6) 0.5713(3) 0.0350(11) Uani 1 d . . . O33 O 0.7037(4) 0.4349(4) 0.4912(3) 0.0413(9) Uani 1 d . . . O51 O 0.6751(7) 0.9310(5) 0.6535(3) 0.0602(13) Uani 1 d . . . O52 O 0.7949(6) 1.0056(6) 0.7861(4) 0.0648(14) Uani 1 d . . . N53 N 0.7573(7) 1.0306(6) 0.7084(4) 0.0549(14) Uani 1 d . . . O54 O 0.7942(9) 1.1430(6) 0.6879(6) 0.103(2) Uani 1 d . . . O41 O 0.3925(5) 0.7565(5) 0.6783(3) 0.0535(11) Uani 1 d . . . O42 O 0.4609(5) 0.9207(4) 0.7939(3) 0.0477(10) Uani 1 d . . . N43 N 0.3609(6) 0.8695(5) 0.7268(4) 0.0422(12) Uani 1 d . . . O44 O 0.2463(6) 0.9293(6) 0.7066(4) 0.0605(14) Uani 1 d . . . N71 N 0.7706(7) 0.8394(6) 0.9296(4) 0.0535(14) Uani 1 d . . . C72 C 0.8091(7) 0.8769(8) 1.0025(4) 0.0527(16) Uani 1 d . . . C73 C 0.8523(12) 0.9301(15) 1.0976(5) 0.099(4) Uani 1 d . . . H73A H 0.9083 1.0233 1.1072 0.119 Uiso 1 calc R . . H73B H 0.9163 0.8650 1.1234 0.119 Uiso 1 calc R . . H73C H 0.7605 0.9369 1.1246 0.119 Uiso 1 calc R . . O61 O 0.8371(6) 0.5631(5) 0.8028(3) 0.0571(11) Uani 1 d . . . N63 N 0.9647(7) 0.6298(10) 0.7959(5) 0.066(2) Uani 1 d . . . O64 O 1.0856(7) 0.5727(10) 0.8084(4) 0.086(2) Uani 1 d . . . O62 O 0.9579(6) 0.7509(7) 0.7758(4) 0.0662(14) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0342(3) 0.0340(3) 0.0318(3) 0.00118(16) 0.00545(14) 0.00117(14) N21 0.038(2) 0.038(2) 0.031(2) 0.0106(19) 0.0070(17) 0.0070(18) C22 0.027(2) 0.039(3) 0.041(3) 0.004(2) 0.005(2) 0.0024(19) O23 0.045(2) 0.0360(17) 0.042(2) 0.0057(17) 0.0129(17) 0.0052(15) C24 0.042(3) 0.039(3) 0.039(3) 0.009(2) 0.012(2) 0.012(2) C25 0.058(4) 0.055(3) 0.053(3) 0.020(3) 0.022(3) 0.016(3) C26 0.063(4) 0.064(4) 0.045(3) 0.019(3) 0.023(3) 0.019(3) C27 0.063(4) 0.066(4) 0.046(4) 0.002(3) 0.015(3) 0.017(3) C28 0.055(4) 0.044(3) 0.055(4) 0.002(3) 0.020(3) 0.002(3) C29 0.040(3) 0.045(3) 0.029(2) 0.014(2) 0.006(2) 0.011(2) N11 0.028(2) 0.034(2) 0.046(3) -0.002(2) 0.0078(19) 0.0042(17) C12 0.033(3) 0.038(3) 0.041(3) 0.007(2) 0.006(2) 0.006(2) C13 0.049(3) 0.034(3) 0.063(4) 0.010(3) 0.011(3) 0.007(2) C14 0.056(4) 0.032(3) 0.070(4) -0.002(3) 0.008(3) -0.003(2) C15 0.048(3) 0.037(3) 0.046(3) -0.005(3) 0.005(3) 0.008(2) C16 0.030(2) 0.038(3) 0.041(3) 0.002(2) 0.008(2) 0.006(2) N31 0.033(2) 0.040(2) 0.037(2) 0.000(2) 0.0068(18) 0.0019(18) C34 0.037(3) 0.047(3) 0.032(2) 0.007(2) 0.008(2) 0.010(2) C35 0.045(3) 0.060(3) 0.033(3) 0.013(3) 0.011(2) 0.015(3) C36 0.048(3) 0.071(4) 0.051(3) 0.006(3) 0.022(3) 0.002(3) C37 0.051(4) 0.058(4) 0.061(4) 0.019(3) 0.021(3) 0.003(3) C38 0.053(4) 0.053(4) 0.065(4) -0.008(3) 0.025(3) -0.005(3) C39 0.038(3) 0.043(3) 0.042(3) 0.008(3) 0.009(2) 0.009(2) C32 0.028(2) 0.044(3) 0.031(2) 0.000(2) 0.0028(19) 0.007(2) O33 0.043(2) 0.0417(19) 0.038(2) -0.0007(17) 0.0120(16) 0.0034(16) O51 0.089(4) 0.054(3) 0.044(2) 0.016(2) 0.019(3) 0.015(3) O52 0.059(3) 0.054(3) 0.074(4) 0.002(3) 0.006(3) -0.015(2) N53 0.054(3) 0.053(3) 0.068(4) 0.025(3) 0.024(3) 0.006(3) O54 0.103(5) 0.070(4) 0.153(7) 0.058(4) 0.039(5) -0.004(3) O41 0.055(3) 0.041(2) 0.051(2) -0.010(2) -0.013(2) 0.0044(18) O42 0.047(2) 0.046(2) 0.046(2) -0.0035(19) 0.0039(18) 0.0089(17) N43 0.039(3) 0.035(2) 0.050(3) 0.004(2) 0.007(2) -0.003(2) O44 0.045(3) 0.060(3) 0.077(4) 0.019(3) -0.001(2) 0.013(2) N71 0.057(3) 0.053(3) 0.043(3) -0.005(3) 0.003(2) -0.004(3) C72 0.042(3) 0.068(4) 0.046(4) 0.002(3) 0.010(3) 0.001(3) C73 0.081(6) 0.153(11) 0.042(4) -0.013(6) -0.002(4) -0.031(7) O61 0.052(3) 0.063(3) 0.058(3) 0.015(2) 0.005(2) 0.015(2) N63 0.035(3) 0.098(6) 0.050(4) -0.028(4) 0.001(2) 0.018(3) O64 0.057(4) 0.151(7) 0.057(3) 0.024(4) 0.001(3) 0.050(4) O62 0.046(3) 0.079(4) 0.065(3) -0.004(3) 0.008(2) -0.014(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 Pr1 O61 2.519(5) . ? Pr1 O41 2.537(5) . ? Pr1 O62 2.545(6) . ? Pr1 O42 2.552(5) . ? Pr1 O52 2.558(6) . ? Pr1 O51 2.568(5) . ? Pr1 N31 2.662(5) . ? Pr1 N71 2.664(6) . ? Pr1 N21 2.669(5) . ? Pr1 N11 2.715(5) . ? N21 C22 1.303(7) . ? N21 C29 1.405(7) . ? C22 O23 1.349(7) . ? C22 C12 1.461(8) . ? O23 C24 1.405(6) . ? C24 C25 1.352(8) . ? C24 C29 1.395(8) . ? C25 C26 1.393(9) . ? C26 C27 1.383(11) . ? C27 C28 1.398(10) . ? C28 C29 1.391(8) . ? N11 C16 1.339(7) . ? N11 C12 1.349(8) . ? C12 C13 1.382(8) . ? C13 C14 1.381(9) . ? C14 C15 1.363(9) . ? C15 C16 1.400(8) . ? C16 C32 1.463(8) . ? N31 C32 1.290(7) . ? N31 C39 1.407(8) . ? C34 C39 1.377(8) . ? C34 C35 1.383(8) . ? C34 O33 1.393(7) . ? C35 C36 1.389(10) . ? C36 C37 1.398(10) . ? C37 C38 1.375(10) . ? C38 C39 1.401(9) . ? C32 O33 1.349(6) . ? O51 N53 1.265(7) . ? O52 N53 1.270(8) . ? N53 O54 1.200(8) . ? O41 N43 1.271(7) . ? O42 N43 1.265(7) . ? N43 O44 1.215(8) . ? N71 C72 1.123(8) . ? C72 C73 1.463(10) . ? O61 N63 1.275(9) . ? N63 O62 1.243(10) . ? N63 O64 1.228(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 Pr1 O41 138.00(16) . . ? O61 Pr1 O62 50.10(19) . . ? O41 Pr1 O62 156.76(19) . . ? O61 Pr1 O42 149.28(16) . . ? O41 Pr1 O42 49.99(14) . . ? O62 Pr1 O42 138.99(17) . . ? O61 Pr1 O52 115.1(2) . . ? O41 Pr1 O52 106.63(17) . . ? O62 Pr1 O52 68.7(2) . . ? O42 Pr1 O52 72.21(19) . . ? O61 Pr1 O51 134.55(18) . . ? O41 Pr1 O51 71.86(19) . . ? O62 Pr1 O51 89.6(2) . . ? O42 Pr1 O51 74.09(17) . . ? O52 Pr1 O51 49.66(19) . . ? O61 Pr1 N31 76.92(16) . . ? O41 Pr1 N31 87.86(16) . . ? O62 Pr1 N31 72.39(15) . . ? O42 Pr1 N31 131.68(14) . . ? O52 Pr1 N31 105.94(17) . . ? O51 Pr1 N31 70.33(17) . . ? O61 Pr1 N71 74.56(18) . . ? O41 Pr1 N71 127.33(17) . . ? O62 Pr1 N71 73.54(18) . . ? O42 Pr1 N71 81.46(17) . . ? O52 Pr1 N71 69.07(19) . . ? O51 Pr1 N71 118.21(19) . . ? N31 Pr1 N71 144.76(17) . . ? O61 Pr1 N21 81.68(17) . . ? O41 Pr1 N21 74.16(18) . . ? O62 Pr1 N21 126.76(18) . . ? O42 Pr1 N21 72.97(16) . . ? O52 Pr1 N21 131.15(16) . . ? O51 Pr1 N21 142.95(17) . . ? N31 Pr1 N21 122.77(15) . . ? N71 Pr1 N21 72.81(17) . . ? O61 Pr1 N11 66.66(17) . . ? O41 Pr1 N11 71.63(14) . . ? O62 Pr1 N11 107.63(17) . . ? O42 Pr1 N11 113.19(15) . . ? O52 Pr1 N11 167.22(18) . . ? O51 Pr1 N11 119.34(18) . . ? N31 Pr1 N11 61.59(14) . . ? N71 Pr1 N11 122.44(17) . . ? N21 Pr1 N11 61.18(15) . . ? C22 N21 C29 104.3(5) . . ? C22 N21 Pr1 118.6(4) . . ? C29 N21 Pr1 137.1(4) . . ? N21 C22 O23 115.5(5) . . ? N21 C22 C12 125.2(5) . . ? O23 C22 C12 119.3(5) . . ? C22 O23 C24 105.1(4) . . ? C25 C24 C29 124.4(5) . . ? C25 C24 O23 129.6(5) . . ? C29 C24 O23 105.9(4) . . ? C24 C25 C26 116.2(6) . . ? C27 C26 C25 121.2(6) . . ? C26 C27 C28 121.9(7) . . ? C29 C28 C27 116.9(6) . . ? C24 C29 C28 119.3(5) . . ? C24 C29 N21 109.2(5) . . ? C28 C29 N21 131.4(5) . . ? C16 N11 C12 117.1(5) . . ? C16 N11 Pr1 121.0(4) . . ? C12 N11 Pr1 121.9(3) . . ? N11 C12 C13 123.1(5) . . ? N11 C12 C22 112.8(5) . . ? C13 C12 C22 124.1(6) . . ? C14 C13 C12 118.7(6) . . ? C15 C14 C13 119.5(5) . . ? C14 C15 C16 118.6(5) . . ? N11 C16 C15 123.0(5) . . ? N11 C16 C32 113.5(5) . . ? C15 C16 C32 123.4(5) . . ? C32 N31 C39 104.3(5) . . ? C32 N31 Pr1 118.2(4) . . ? C39 N31 Pr1 137.4(4) . . ? C39 C34 C35 124.9(6) . . ? C39 C34 O33 108.3(5) . . ? C35 C34 O33 126.8(5) . . ? C34 C35 C36 114.4(6) . . ? C37 C36 C35 122.1(6) . . ? C38 C37 C36 122.0(6) . . ? C37 C38 C39 116.8(6) . . ? C34 C39 N31 107.7(5) . . ? C34 C39 C38 119.8(6) . . ? N31 C39 C38 132.5(6) . . ? N31 C32 O33 116.5(5) . . ? N31 C32 C16 125.5(5) . . ? O33 C32 C16 118.0(4) . . ? C32 O33 C34 103.1(4) . . ? N53 O51 Pr1 96.9(4) . . ? N53 O52 Pr1 97.2(4) . . ? O54 N53 O51 121.2(7) . . ? O54 N53 O52 122.5(7) . . ? O51 N53 O52 116.2(5) . . ? N43 O41 Pr1 97.1(3) . . ? N43 O42 Pr1 96.6(3) . . ? O44 N43 O42 122.1(5) . . ? O44 N43 O41 121.8(6) . . ? O42 N43 O41 116.0(5) . . ? C72 N71 Pr1 177.1(5) . . ? N71 C72 C73 177.0(9) . . ? N63 O61 Pr1 96.7(5) . . ? O62 N63 O64 123.7(9) . . ? O62 N63 O61 116.8(6) . . ? O64 N63 O61 119.6(10) . . ? N63 O62 Pr1 96.4(4) . . ? _refine_diff_density_max 1.601 _refine_diff_density_min -1.929 _refine_diff_density_rms 0.240 #===END data_Er-2 _database_code_depnum_ccdc_archive 'CCDC 193087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Er N7 O11' _chemical_formula_weight 701.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.618(9) _cell_length_b 9.458(12) _cell_length_c 15.445(17) _cell_angle_alpha 100.457(10) _cell_angle_beta 97.727(10) _cell_angle_gamma 94.181(10) _cell_volume 1221(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 3.515 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3936 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3936 _reflns_number_gt 3349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+6.9747P] 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 3936 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.66469(4) 0.73637(4) 0.75829(2) 0.03772(16) Uani 1 d . . . N21 N 0.4824(8) 0.6185(7) 0.8490(4) 0.0385(15) Uani 1 d . . . C22 C 0.4293(9) 0.4835(9) 0.8217(5) 0.0387(18) Uani 1 d . . . O23 O 0.3411(7) 0.4246(6) 0.8752(4) 0.0399(12) Uani 1 d . . . C24 C 0.3319(11) 0.5392(10) 0.9439(6) 0.0439(19) Uani 1 d . . . C25 C 0.2539(12) 0.5396(10) 1.0149(6) 0.050(2) Uani 1 d . . . H25 H 0.1994 0.4564 1.0241 0.060 Uiso 1 calc R . . C26 C 0.2603(12) 0.6710(11) 1.0727(6) 0.054(2) Uani 1 d . . . H26 H 0.2088 0.6772 1.1222 0.065 Uiso 1 calc R . . C27 C 0.3434(13) 0.7943(12) 1.0575(6) 0.057(2) Uani 1 d . . . H27 H 0.3455 0.8811 1.0974 0.068 Uiso 1 calc R . . C28 C 0.4216(12) 0.7917(11) 0.9859(6) 0.052(2) Uani 1 d . . . H28 H 0.4752 0.8750 0.9761 0.062 Uiso 1 calc R . . C29 C 0.4179(10) 0.6601(9) 0.9284(5) 0.0391(17) Uani 1 d . . . N11 N 0.5414(8) 0.4713(7) 0.6918(4) 0.0385(15) Uani 1 d . . . C12 C 0.4564(10) 0.3965(8) 0.7378(5) 0.0366(17) Uani 1 d . . . C13 C 0.3952(12) 0.2533(10) 0.7067(6) 0.049(2) Uani 1 d . . . H13 H 0.3382 0.2041 0.7410 0.059 Uiso 1 calc R . . C14 C 0.4215(12) 0.1862(10) 0.6235(6) 0.049(2) Uani 1 d . . . H14 H 0.3802 0.0912 0.6001 0.059 Uiso 1 calc R . . C15 C 0.5107(11) 0.2628(9) 0.5749(6) 0.045(2) Uani 1 d . . . H15 H 0.5307 0.2204 0.5188 0.054 Uiso 1 calc R . . C16 C 0.5685(10) 0.4037(9) 0.6130(5) 0.0363(17) Uani 1 d . . . N31 N 0.7367(8) 0.6206(7) 0.6089(4) 0.0376(15) Uani 1 d . . . C34 C 0.8070(10) 0.5484(10) 0.4733(5) 0.0412(18) Uani 1 d . . . C35 C 0.8785(11) 0.5473(11) 0.3977(5) 0.047(2) Uani 1 d . . . H35 H 0.8608 0.4699 0.3497 0.056 Uiso 1 calc R . . C36 C 0.9777(13) 0.6696(13) 0.3990(6) 0.060(3) Uani 1 d . . . H36 H 1.0276 0.6766 0.3499 0.072 Uiso 1 calc R . . C37 C 1.0042(12) 0.7837(12) 0.4734(7) 0.057(2) Uani 1 d . . . H37 H 1.0723 0.8640 0.4720 0.068 Uiso 1 calc R . . C38 C 0.9337(13) 0.7819(11) 0.5480(7) 0.053(2) Uani 1 d . . . H38 H 0.9540 0.8576 0.5969 0.064 Uiso 1 calc R . . C39 C 0.8304(10) 0.6609(9) 0.5467(5) 0.0397(18) Uani 1 d . . . C32 C 0.6729(10) 0.4927(9) 0.5717(5) 0.0373(17) Uani 1 d . . . O33 O 0.7063(7) 0.4401(6) 0.4898(3) 0.0417(13) Uani 1 d . . . O51 O 0.6653(10) 0.9122(8) 0.6564(5) 0.066(2) Uani 1 d . . . O52 O 0.7970(9) 0.9845(9) 0.7863(5) 0.0659(19) Uani 1 d . . . N53 N 0.7540(11) 1.0120(10) 0.7104(6) 0.058(2) Uani 1 d . . . O54 O 0.7922(13) 1.1261(10) 0.6911(7) 0.098(3) Uani 1 d . . . O41 O 0.4027(8) 0.7395(7) 0.6819(4) 0.0529(16) Uani 1 d . . . O42 O 0.4756(7) 0.9054(6) 0.7980(4) 0.0433(13) Uani 1 d . . . N43 N 0.3733(9) 0.8538(8) 0.7305(5) 0.0439(17) Uani 1 d . . . O44 O 0.2554(10) 0.9163(9) 0.7145(6) 0.069(2) Uani 1 d . . . N71 N 0.7686(10) 0.8262(9) 0.9215(5) 0.053(2) Uani 1 d . . . C72 C 0.8087(12) 0.8685(12) 0.9959(6) 0.054(2) Uani 1 d . . . C73 C 0.8558(18) 0.9215(18) 1.0913(8) 0.094(5) Uani 1 d . . . H73A H 0.8873 1.0234 1.1022 0.113 Uiso 1 calc R . . H73B H 0.9423 0.8722 1.1125 0.113 Uiso 1 calc R . . H73C H 0.7687 0.9039 1.1220 0.113 Uiso 1 calc R . . O61 O 0.8259(8) 0.5562(8) 0.8010(4) 0.0554(16) Uani 1 d . . . N63 N 0.9536(10) 0.6216(12) 0.7948(5) 0.057(2) Uani 1 d . . . O64 O 1.0783(12) 0.5641(13) 0.8084(6) 0.094(3) Uani 1 d . . . O62 O 0.9534(8) 0.7424(9) 0.7743(4) 0.0592(18) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0396(3) 0.0366(3) 0.0362(2) 0.00590(14) 0.00547(15) 0.00193(16) N21 0.043(4) 0.034(4) 0.039(3) 0.005(3) 0.010(3) 0.005(3) C22 0.029(4) 0.047(5) 0.045(4) 0.019(4) 0.007(3) 0.012(4) O23 0.040(3) 0.034(3) 0.048(3) 0.012(2) 0.010(2) 0.003(2) C24 0.047(5) 0.045(5) 0.044(4) 0.017(4) 0.007(4) 0.009(4) C25 0.057(6) 0.044(5) 0.054(5) 0.017(4) 0.017(4) 0.003(4) C26 0.056(6) 0.065(6) 0.050(5) 0.014(4) 0.027(4) 0.021(5) C27 0.065(7) 0.055(6) 0.049(5) 0.005(4) 0.010(4) 0.011(5) C28 0.057(6) 0.050(6) 0.045(5) 0.004(4) 0.007(4) 0.003(5) C29 0.030(4) 0.041(5) 0.046(4) 0.011(3) 0.003(3) 0.006(3) N11 0.038(4) 0.032(4) 0.043(3) 0.005(3) 0.002(3) 0.003(3) C12 0.038(4) 0.029(4) 0.044(4) 0.009(3) 0.008(3) 0.006(3) C13 0.056(6) 0.040(5) 0.056(5) 0.015(4) 0.013(4) 0.005(4) C14 0.050(5) 0.030(5) 0.066(5) 0.004(4) 0.008(4) 0.003(4) C15 0.053(5) 0.038(5) 0.043(4) 0.002(3) 0.003(4) 0.015(4) C16 0.038(4) 0.035(4) 0.035(4) 0.009(3) 0.001(3) 0.001(3) N31 0.038(4) 0.038(4) 0.037(3) 0.006(3) 0.006(3) 0.006(3) C34 0.035(4) 0.047(5) 0.044(4) 0.011(4) 0.008(3) 0.012(4) C35 0.041(5) 0.066(6) 0.035(4) 0.013(4) 0.004(3) 0.013(4) C36 0.065(7) 0.076(7) 0.047(5) 0.019(5) 0.024(4) 0.013(6) C37 0.051(6) 0.058(6) 0.065(6) 0.020(5) 0.015(4) 0.001(5) C38 0.061(6) 0.042(5) 0.056(5) 0.005(4) 0.012(4) 0.004(4) C39 0.033(4) 0.045(5) 0.040(4) 0.007(3) 0.003(3) 0.007(4) C32 0.041(4) 0.032(4) 0.039(4) 0.008(3) 0.006(3) 0.003(3) O33 0.044(3) 0.045(3) 0.036(3) 0.007(2) 0.007(2) 0.006(3) O51 0.089(6) 0.061(5) 0.050(4) 0.014(3) 0.019(4) 0.006(4) O52 0.052(4) 0.067(5) 0.080(5) 0.023(4) 0.006(4) 0.001(4) N53 0.058(5) 0.050(5) 0.072(5) 0.025(4) 0.023(4) -0.002(4) O54 0.111(8) 0.069(6) 0.127(8) 0.051(6) 0.033(6) -0.010(5) O41 0.059(4) 0.042(4) 0.049(3) -0.001(3) -0.010(3) 0.005(3) O42 0.040(3) 0.039(3) 0.052(3) 0.006(3) 0.007(3) 0.016(3) N43 0.044(5) 0.037(4) 0.050(4) 0.014(3) -0.001(3) -0.002(3) O44 0.058(5) 0.067(5) 0.084(5) 0.023(4) 0.007(4) 0.014(4) N71 0.064(5) 0.050(5) 0.041(4) 0.003(3) 0.010(3) -0.009(4) C72 0.051(6) 0.061(6) 0.047(5) 0.008(4) 0.007(4) -0.005(5) C73 0.094(10) 0.121(12) 0.053(6) -0.003(7) 0.003(6) -0.021(9) O61 0.050(4) 0.058(4) 0.059(4) 0.016(3) 0.006(3) 0.009(3) N63 0.041(5) 0.088(7) 0.039(4) 0.009(4) -0.004(3) 0.012(5) O64 0.068(6) 0.151(10) 0.060(5) 0.008(5) 0.001(4) 0.038(6) O62 0.046(4) 0.082(5) 0.051(4) 0.015(4) 0.018(3) -0.010(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 Er1 O61 2.403(7) . ? Er1 O62 2.463(7) . ? Er1 O41 2.407(7) . ? Er1 N21 2.564(7) . ? Er1 N11 2.617(7) . ? Er1 N31 2.545(7) . ? Er1 O42 2.425(6) . ? Er1 O52 2.470(8) . ? Er1 N71 2.526(8) . ? Er1 O51 2.488(7) . ? N21 C22 1.298(11) . ? N21 C29 1.418(10) . ? C22 O23 1.358(9) . ? C22 C12 1.460(11) . ? O23 C24 1.386(11) . ? C24 C25 1.360(12) . ? C24 C29 1.392(12) . ? C25 C26 1.385(14) . ? C26 C27 1.396(15) . ? C27 C28 1.369(13) . ? C28 C29 1.387(13) . ? N11 C16 1.327(10) . ? N11 C12 1.338(10) . ? C12 C13 1.391(13) . ? C13 C14 1.383(13) . ? C14 C15 1.396(13) . ? C15 C16 1.382(12) . ? C16 C32 1.472(11) . ? N31 C32 1.289(11) . ? N31 C39 1.419(10) . ? C34 C39 1.388(12) . ? C34 C35 1.391(12) . ? C34 O33 1.375(10) . ? C35 C36 1.383(15) . ? C36 C37 1.407(15) . ? C37 C38 1.376(13) . ? C38 C39 1.393(14) . ? C32 O33 1.349(9) . ? O51 N53 1.268(12) . ? O52 N53 1.259(11) . ? N53 O54 1.206(11) . ? O41 N43 1.262(10) . ? O42 N43 1.268(9) . ? N43 O44 1.231(11) . ? N71 C72 1.144(12) . ? C72 C73 1.459(14) . ? O61 N63 1.246(11) . ? N63 O64 1.249(13) . ? N63 O62 1.240(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 O61 Er1 O62 52.2(3) . . ? O61 Er1 O41 136.5(2) . . ? O62 Er1 O41 156.2(2) . . ? O61 Er1 N21 80.6(2) . . ? O62 Er1 N21 127.0(2) . . ? O41 Er1 N21 74.9(2) . . ? O61 Er1 N11 66.5(2) . . ? O62 Er1 N11 108.8(2) . . ? O41 Er1 N11 70.4(2) . . ? N21 Er1 N11 62.8(2) . . ? O61 Er1 N31 78.8(2) . . ? O62 Er1 N31 72.0(2) . . ? O41 Er1 N31 87.4(2) . . ? N21 Er1 N31 126.2(2) . . ? N11 Er1 N31 63.4(2) . . ? O61 Er1 O42 147.6(2) . . ? O62 Er1 O42 136.4(2) . . ? O41 Er1 O42 52.7(2) . . ? N21 Er1 O42 72.8(2) . . ? N11 Er1 O42 114.6(2) . . ? N31 Er1 O42 132.2(2) . . ? O61 Er1 O52 115.5(3) . . ? O62 Er1 O52 67.2(3) . . ? O41 Er1 O52 107.8(2) . . ? N21 Er1 O52 130.0(2) . . ? N11 Er1 O52 166.8(2) . . ? N31 Er1 O52 103.7(2) . . ? O42 Er1 O52 71.3(2) . . ? O61 Er1 N71 74.6(3) . . ? O62 Er1 N71 73.1(3) . . ? O41 Er1 N71 128.1(3) . . ? N21 Er1 N71 72.0(2) . . ? N11 Er1 N71 123.5(2) . . ? N31 Er1 N71 144.5(3) . . ? O42 Er1 N71 79.7(3) . . ? O52 Er1 N71 68.4(3) . . ? O61 Er1 O51 137.7(3) . . ? O62 Er1 O51 91.1(3) . . ? O41 Er1 O51 69.9(3) . . ? N21 Er1 O51 140.9(3) . . ? N11 Er1 O51 118.0(2) . . ? N31 Er1 O51 69.1(2) . . ? O42 Er1 O51 72.6(2) . . ? O52 Er1 O51 51.0(3) . . ? N71 Er1 O51 118.4(3) . . ? C22 N21 C29 103.9(6) . . ? C22 N21 Er1 118.9(5) . . ? C29 N21 Er1 137.2(5) . . ? N21 C22 O23 116.2(7) . . ? N21 C22 C12 123.7(7) . . ? O23 C22 C12 120.0(7) . . ? C22 O23 C24 103.9(6) . . ? C25 C24 C29 123.9(9) . . ? C25 C24 O23 128.1(8) . . ? C29 C24 O23 107.9(7) . . ? C24 C25 C26 116.2(8) . . ? C27 C26 C25 120.8(8) . . ? C26 C27 C28 122.2(9) . . ? C27 C28 C29 117.4(9) . . ? C24 C29 C28 119.4(8) . . ? C24 C29 N21 107.9(7) . . ? C28 C29 N21 132.6(8) . . ? C16 N11 C12 117.6(7) . . ? C16 N11 Er1 120.9(5) . . ? C12 N11 Er1 121.4(5) . . ? N11 C12 C13 123.2(7) . . ? N11 C12 C22 112.6(7) . . ? C13 C12 C22 124.1(7) . . ? C14 C13 C12 118.2(8) . . ? C15 C14 C13 119.2(8) . . ? C14 C15 C16 117.8(8) . . ? N11 C16 C15 124.0(7) . . ? N11 C16 C32 112.8(7) . . ? C15 C16 C32 123.2(7) . . ? C32 N31 C39 104.1(6) . . ? C32 N31 Er1 118.7(5) . . ? C39 N31 Er1 137.1(5) . . ? C39 C34 C35 124.5(9) . . ? C39 C34 O33 108.6(7) . . ? C35 C34 O33 126.9(8) . . ? C34 C35 C36 115.1(9) . . ? C37 C36 C35 121.0(8) . . ? C38 C37 C36 122.9(10) . . ? C37 C38 C39 116.7(9) . . ? C34 C39 N31 107.1(7) . . ? C34 C39 C38 119.7(8) . . ? N31 C39 C38 133.2(8) . . ? N31 C32 O33 116.5(7) . . ? N31 C32 C16 124.1(7) . . ? O33 C32 C16 119.4(7) . . ? C32 O33 C34 103.7(6) . . ? N53 O51 Er1 96.3(5) . . ? N53 O52 Er1 97.5(6) . . ? O54 N53 O51 122.4(10) . . ? O54 N53 O52 122.3(10) . . ? O51 N53 O52 115.2(8) . . ? N43 O41 Er1 95.9(5) . . ? N43 O42 Er1 94.9(5) . . ? O44 N43 O42 120.2(8) . . ? O44 N43 O41 123.8(8) . . ? O42 N43 O41 116.0(8) . . ? C72 N71 Er1 176.8(8) . . ? N71 C72 C73 178.5(12) . . ? N63 O61 Er1 95.8(6) . . ? O64 N63 O62 121.5(10) . . ? O64 N63 O61 119.7(11) . . ? O62 N63 O61 118.8(9) . . ? O64 N63 Er1 176.8(8) . . ? O62 N63 Er1 60.8(5) . . ? O61 N63 Er1 58.1(5) . . ? N63 O62 Er1 93.1(5) . . ? _refine_diff_density_max 1.913 _refine_diff_density_min -1.680 _refine_diff_density_rms 0.159 #===END data_Eu-3 _database_code_depnum_ccdc_archive 'CCDC 193088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H24 Eu N9 O13' _chemical_formula_weight 978.63 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.533(14) _cell_length_b 10.680(14) _cell_length_c 17.12(2) _cell_angle_alpha 86.069(10) _cell_angle_beta 79.225(10) _cell_angle_gamma 82.233(10) _cell_volume 1873(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2 intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5521 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.83 _reflns_number_total 5521 _reflns_number_gt 3721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1676P)^2^+53.0612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5521 _refine_ls_number_parameters 560 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.1076 _refine_ls_wR_factor_ref 0.3331 _refine_ls_wR_factor_gt 0.3053 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.19579(10) 0.29307(11) 0.18279(6) 0.0382(5) Uani 1 d . . . C22 C -0.0193(19) 0.3440(19) 0.0545(11) 0.037(5) Uani 1 d . . . N21 N -0.0233(17) 0.3502(16) 0.1290(9) 0.038(4) Uani 1 d . . . C29 C -0.154(2) 0.398(2) 0.1605(13) 0.044(5) Uani 1 d . . . C28 C -0.219(2) 0.422(2) 0.2363(12) 0.047(5) Uani 1 d . . . H28 H -0.1787 0.4027 0.2803 0.056 Uiso 1 calc R . . C27 C -0.350(2) 0.476(3) 0.2443(13) 0.059(7) Uani 1 d . . . H27 H -0.3952 0.4970 0.2947 0.071 Uiso 1 calc R . . C26 C -0.414(2) 0.499(2) 0.1800(12) 0.051(6) Uani 1 d . . . H26 H -0.5014 0.5334 0.1883 0.061 Uiso 1 calc R . . C25 C -0.350(2) 0.470(2) 0.1031(13) 0.055(6) Uani 1 d . . . H25 H -0.3919 0.4822 0.0594 0.067 Uiso 1 calc R . . C24 C -0.220(2) 0.4237(19) 0.0967(12) 0.039(5) Uani 1 d . . . O23 O -0.1332(14) 0.3890(14) 0.0281(7) 0.044(4) Uani 1 d . . . N11 N 0.1988(13) 0.2694(14) 0.0288(8) 0.027(3) Uani 1 d . . . C12 C 0.0918(18) 0.299(2) -0.0030(11) 0.036(5) Uani 1 d . . . C13 C 0.094(2) 0.285(2) -0.0854(11) 0.041(5) Uani 1 d . . . H13 H 0.0197 0.3083 -0.1072 0.049 Uiso 1 calc R . . C14 C 0.206(2) 0.237(2) -0.1314(13) 0.050(6) Uani 1 d . . . H14 H 0.2081 0.2273 -0.1852 0.060 Uiso 1 calc R . . C15 C 0.322(2) 0.202(2) -0.0991(12) 0.049(6) Uani 1 d . . . H15 H 0.4008 0.1704 -0.1303 0.059 Uiso 1 calc R . . C16 C 0.3102(17) 0.2167(19) -0.0187(11) 0.034(4) Uani 1 d . . . C32 C 0.4219(19) 0.1824(19) 0.0237(11) 0.035(4) Uani 1 d U . . N31 N 0.4210(16) 0.1858(16) 0.0973(9) 0.039(4) Uani 1 d U . . C39 C 0.555(2) 0.1501(17) 0.1049(12) 0.037(4) Uani 1 d U . . C38 C 0.612(2) 0.132(2) 0.1715(13) 0.049(5) Uani 1 d U . . H38 H 0.5646 0.1403 0.2229 0.059 Uiso 1 calc R . . C37 C 0.749(2) 0.101(2) 0.1553(14) 0.051(5) Uani 1 d U . . H37 H 0.7940 0.0975 0.1973 0.061 Uiso 1 calc R . . C36 C 0.819(3) 0.075(2) 0.0803(14) 0.057(6) Uani 1 d U . . H36 H 0.9081 0.0475 0.0743 0.068 Uiso 1 calc R . . C35 C 0.760(2) 0.091(2) 0.0134(13) 0.049(5) Uani 1 d U . . H35 H 0.8053 0.0788 -0.0380 0.059 Uiso 1 calc R . . C34 C 0.6257(18) 0.1253(19) 0.0306(11) 0.035(4) Uani 1 d U . . O33 O 0.5394(13) 0.1510(13) -0.0232(8) 0.040(3) Uani 1 d U . . N43 N 0.254(2) 0.5459(19) 0.1180(10) 0.047(5) Uani 1 d . . . O44 O 0.2875(18) 0.6530(17) 0.0937(10) 0.066(5) Uani 1 d . . . O41 O 0.1559(14) 0.5223(15) 0.1660(8) 0.050(4) Uani 1 d . . . O42 O 0.3293(13) 0.4474(16) 0.0946(8) 0.044(4) Uani 1 d . . . N53 N 0.074(2) 0.054(2) 0.2106(12) 0.056(5) Uani 1 d . . . O52 C 0.1663(15) 0.0739(17) 0.1520(10) 0.024(4) Uani 1 d . . . O54 O 0.0227(18) -0.0412(18) 0.2185(12) 0.074(5) Uani 1 d . . . O51 O 0.0358(19) 0.1460(15) 0.2538(10) 0.065(5) Uani 1 d . . . N63 N 0.3607(19) 0.265(2) 0.3036(11) 0.053(5) Uani 1 d . . . O61 O 0.3511(13) 0.3601(15) 0.2574(8) 0.047(4) Uani 1 d . . . O62 O 0.3105(16) 0.1729(15) 0.2850(9) 0.053(4) Uani 1 d . . . O64 O 0.4212(18) 0.255(2) 0.3547(11) 0.080(6) Uani 1 d . . . C72 C 1.205(3) 0.439(2) 0.4952(12) 0.060(7) Uani 1 d . . . N71 N 1.118(2) 0.3748(19) 0.4746(9) 0.053(5) Uani 1 d . . . C73 C 1.250(3) 0.420(3) 0.5675(17) 0.077(8) Uani 1 d . . . H73 H 1.3146 0.4634 0.5781 0.093 Uiso 1 calc R . . C74 C 1.196(3) 0.335(3) 0.6217(15) 0.070(8) Uani 1 d . . . H74 H 1.2208 0.3242 0.6714 0.083 Uiso 1 calc R . . C75 C 1.104(2) 0.265(3) 0.6042(15) 0.071(8) Uani 1 d . . . H75 H 1.0671 0.2050 0.6403 0.086 Uiso 1 calc R . . C76 C 1.072(2) 0.289(2) 0.5286(12) 0.055(6) Uani 1 d . . . C82 C 0.976(2) 0.220(2) 0.5023(12) 0.053(6) Uani 1 d . . . O83 O 0.9214(17) 0.1288(18) 0.5527(9) 0.068(5) Uani 1 d . . . C84 C 0.834(3) 0.084(2) 0.5146(13) 0.059(7) Uani 1 d . . . C85 C 0.754(3) -0.007(2) 0.5384(17) 0.067(8) Uani 1 d . . . H85 H 0.7552 -0.0531 0.5866 0.081 Uiso 1 calc R . . C86 C 0.673(3) -0.029(3) 0.4879(17) 0.074(8) Uani 1 d . . . H86 H 0.6163 -0.0896 0.5041 0.089 Uiso 1 calc R . . C87 C 0.669(3) 0.033(3) 0.416(2) 0.078(8) Uani 1 d . . . H87 H 0.6154 0.0110 0.3828 0.094 Uiso 1 calc R . . C88 C 0.749(3) 0.132(3) 0.3920(16) 0.076(8) Uani 1 d . . . H88 H 0.7454 0.1801 0.3448 0.091 Uiso 1 calc R . . C89 C 0.833(2) 0.154(2) 0.4417(13) 0.056(6) Uani 1 d . . . N81 N 0.925(2) 0.2384(19) 0.4355(10) 0.055(5) Uani 1 d . . . C92 C 1.259(2) 0.535(2) 0.4336(15) 0.054(6) Uani 1 d . . . O93 O 1.3569(19) 0.5926(17) 0.4467(10) 0.068(5) Uani 1 d . . . C94 C 1.373(3) 0.681(3) 0.3810(15) 0.064(7) Uani 1 d . . . C95 C 1.459(2) 0.772(3) 0.3692(18) 0.070(8) Uani 1 d . . . H95 H 1.5138 0.7828 0.4041 0.084 Uiso 1 calc R . . C96 C 1.452(3) 0.844(3) 0.2988(19) 0.088(9) Uani 1 d . . . H96 H 1.5123 0.9009 0.2828 0.105 Uiso 1 calc R . . C97 C 1.365(3) 0.834(3) 0.2532(18) 0.073(8) Uani 1 d . . . H97 H 1.3650 0.8881 0.2081 0.088 Uiso 1 calc R . . C98 C 1.269(3) 0.747(3) 0.2688(16) 0.074(8) Uani 1 d . . . H98 H 1.2076 0.7418 0.2371 0.088 Uiso 1 calc R . . C99 C 1.280(3) 0.670(2) 0.3364(16) 0.059(6) Uani 1 d . . . N91 N 1.2081(18) 0.571(2) 0.3713(11) 0.056(5) Uani 1 d . . . O100 O 0.0649(14) 0.3846(15) 0.3044(7) 0.050(4) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0428(7) 0.0372(8) 0.0343(6) 0.0005(4) -0.0066(4) -0.0051(4) C22 0.033(11) 0.038(14) 0.045(11) -0.005(9) -0.006(8) -0.023(9) N21 0.050(11) 0.037(11) 0.032(8) 0.004(7) -0.012(7) -0.016(8) C29 0.042(13) 0.028(14) 0.062(13) 0.003(10) -0.008(9) -0.009(9) C28 0.050(14) 0.057(17) 0.036(10) -0.005(10) -0.010(9) -0.009(11) C27 0.043(14) 0.09(2) 0.050(13) -0.007(12) -0.006(10) -0.026(13) C26 0.037(12) 0.065(18) 0.046(12) 0.004(11) -0.008(9) 0.008(11) C25 0.054(15) 0.070(19) 0.045(12) 0.003(11) -0.012(10) -0.015(12) C24 0.049(13) 0.022(13) 0.048(11) 0.004(9) -0.010(9) -0.009(9) O23 0.052(9) 0.047(10) 0.035(7) 0.004(6) -0.018(6) -0.003(7) N11 0.026(8) 0.019(9) 0.038(8) 0.000(6) -0.020(6) 0.010(6) C12 0.030(11) 0.041(14) 0.039(10) 0.004(9) -0.006(7) -0.013(9) C13 0.038(12) 0.044(15) 0.044(11) -0.005(9) -0.018(9) -0.003(9) C14 0.060(15) 0.032(15) 0.054(13) -0.004(10) -0.008(10) 0.004(11) C15 0.029(11) 0.066(18) 0.049(12) -0.006(11) -0.007(8) 0.005(10) C16 0.021(10) 0.037(13) 0.047(11) 0.000(9) -0.010(7) -0.009(8) C32 0.036(10) 0.024(12) 0.043(10) 0.002(8) -0.008(8) 0.007(8) N31 0.044(9) 0.030(10) 0.035(8) -0.002(7) 0.002(7) 0.013(7) C39 0.046(11) 0.003(10) 0.063(11) 0.003(8) -0.007(8) -0.006(8) C38 0.068(14) 0.025(13) 0.053(11) -0.002(9) -0.015(10) 0.006(10) C37 0.040(11) 0.040(14) 0.069(13) -0.003(10) -0.011(9) 0.005(10) C36 0.056(14) 0.049(15) 0.067(13) -0.007(11) -0.012(10) -0.013(11) C35 0.039(11) 0.045(14) 0.056(12) -0.003(10) 0.007(9) 0.001(9) C34 0.028(9) 0.028(11) 0.048(10) -0.006(8) -0.002(7) -0.008(8) O33 0.034(7) 0.035(9) 0.048(7) -0.006(6) -0.002(6) 0.001(6) N43 0.082(15) 0.031(13) 0.039(9) -0.004(8) -0.030(9) -0.017(11) O44 0.083(13) 0.049(13) 0.076(11) 0.020(9) -0.032(9) -0.033(10) O41 0.046(9) 0.069(12) 0.038(7) 0.002(7) -0.005(6) -0.027(8) O42 0.029(8) 0.054(12) 0.051(8) 0.005(7) -0.011(6) -0.014(7) N53 0.072(15) 0.041(15) 0.061(12) 0.003(11) -0.028(10) -0.004(11) O52 0.015(8) 0.022(11) 0.037(9) -0.014(7) -0.001(6) 0.000(7) O54 0.069(13) 0.045(13) 0.109(15) 0.004(10) -0.014(10) -0.016(10) O51 0.101(14) 0.025(11) 0.061(10) -0.014(8) 0.006(9) -0.007(9) N63 0.057(13) 0.055(15) 0.050(11) -0.004(10) -0.018(9) -0.006(10) O61 0.033(8) 0.054(11) 0.054(9) 0.004(8) -0.007(6) -0.014(7) O62 0.061(11) 0.036(10) 0.063(9) 0.002(7) -0.013(7) -0.006(8) O64 0.065(12) 0.112(17) 0.070(12) 0.005(11) -0.032(9) -0.009(11) C72 0.10(2) 0.048(17) 0.028(10) -0.018(10) -0.018(11) 0.012(14) N71 0.073(14) 0.059(14) 0.028(9) -0.011(8) -0.008(8) -0.004(10) C73 0.064(19) 0.10(3) 0.076(19) -0.019(17) -0.019(14) -0.005(16) C74 0.09(2) 0.05(2) 0.055(15) -0.015(13) -0.022(14) 0.027(16) C75 0.040(14) 0.11(3) 0.064(16) -0.016(15) -0.012(11) 0.002(14) C76 0.068(16) 0.064(18) 0.032(11) -0.013(11) -0.006(10) -0.002(13) C82 0.068(16) 0.043(16) 0.043(12) -0.008(10) -0.004(10) 0.002(12) O83 0.067(12) 0.073(13) 0.048(9) 0.013(8) 0.010(8) 0.005(9) C84 0.065(17) 0.062(19) 0.046(12) -0.008(11) 0.013(11) -0.026(13) C85 0.068(18) 0.027(16) 0.10(2) 0.035(13) -0.016(15) -0.001(12) C86 0.054(17) 0.08(2) 0.077(18) -0.010(16) 0.021(13) -0.007(14) C87 0.08(2) 0.05(2) 0.11(2) -0.011(16) -0.012(16) -0.023(15) C88 0.10(2) 0.07(2) 0.068(17) 0.006(14) -0.032(15) -0.027(17) C89 0.068(17) 0.049(17) 0.044(12) 0.001(11) 0.002(10) 0.000(12) N81 0.070(14) 0.054(14) 0.045(10) -0.004(9) -0.010(9) -0.022(10) C92 0.065(16) 0.022(15) 0.074(16) -0.030(11) -0.012(12) 0.012(11) O93 0.083(13) 0.056(12) 0.071(11) -0.015(9) -0.027(9) -0.003(10) C94 0.061(17) 0.06(2) 0.067(16) -0.021(14) -0.007(12) 0.001(13) C95 0.042(15) 0.08(2) 0.10(2) -0.023(16) -0.012(12) -0.024(13) C96 0.09(2) 0.10(3) 0.08(2) -0.009(18) -0.001(17) -0.031(19) C97 0.08(2) 0.047(19) 0.079(19) -0.018(14) 0.008(15) 0.005(15) C98 0.09(2) 0.06(2) 0.068(17) -0.015(14) -0.009(14) 0.009(16) C99 0.061(16) 0.026(16) 0.091(19) -0.019(12) -0.012(13) -0.003(11) N91 0.047(12) 0.065(15) 0.060(11) -0.010(10) -0.026(9) 0.007(10) O100 0.053(9) 0.066(11) 0.026(6) -0.006(6) 0.003(6) -0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O41 2.433(17) . ? Eu1 O100 2.456(13) . ? Eu1 O61 2.459(14) . ? Eu1 O62 2.496(15) . ? Eu1 O52 2.506(17) . ? Eu1 O42 2.542(14) . ? Eu1 O51 2.544(17) . ? Eu1 N21 2.623(16) . ? Eu1 N11 2.659(14) . ? Eu1 N31 2.698(15) . ? C22 N21 1.27(2) . ? C22 O23 1.38(2) . ? C22 C12 1.43(3) . ? N21 C29 1.42(3) . ? C29 C28 1.37(3) . ? C29 C24 1.39(3) . ? C28 C27 1.40(3) . ? C27 C26 1.39(3) . ? C26 C25 1.40(3) . ? C25 C24 1.38(3) . ? C24 O23 1.39(2) . ? N11 C12 1.33(2) . ? N11 C16 1.37(2) . ? C12 C13 1.42(3) . ? C13 C14 1.35(3) . ? C14 C15 1.43(3) . ? C15 C16 1.38(3) . ? C16 C32 1.49(2) . ? C32 N31 1.26(2) . ? C32 O33 1.36(2) . ? N31 C39 1.44(3) . ? C39 C34 1.37(3) . ? C39 C38 1.38(3) . ? C38 C37 1.41(3) . ? C37 C36 1.38(3) . ? C36 C35 1.40(3) . ? C35 C34 1.39(3) . ? C34 O33 1.40(2) . ? N43 O41 1.24(2) . ? N43 O44 1.26(2) . ? N43 O42 1.27(2) . ? N53 O54 1.20(2) . ? N53 O51 1.25(2) . ? N53 O52 1.29(3) . ? N63 O64 1.17(2) . ? N63 O61 1.25(2) . ? N63 O62 1.26(2) . ? C72 N71 1.34(3) . ? C72 C73 1.40(3) . ? C72 C92 1.50(4) . ? N71 C76 1.33(3) . ? C73 C74 1.35(4) . ? C74 C75 1.39(4) . ? C75 C76 1.40(3) . ? C76 C82 1.48(3) . ? C82 N81 1.34(3) . ? C82 O83 1.37(3) . ? O83 C84 1.38(3) . ? C84 C85 1.36(3) . ? C84 C89 1.41(3) . ? C85 C86 1.38(4) . ? C86 C87 1.36(4) . ? C87 C88 1.44(4) . ? C88 C89 1.39(4) . ? C89 N81 1.39(3) . ? C92 N91 1.29(3) . ? C92 O93 1.33(3) . ? O93 C94 1.42(3) . ? C94 C99 1.37(3) . ? C94 C95 1.39(4) . ? C95 C96 1.39(4) . ? C96 C97 1.34(4) . ? C97 C98 1.44(4) . ? C98 C99 1.38(4) . ? C99 N91 1.42(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 O41 Eu1 O100 69.4(5) . . ? O41 Eu1 O61 78.3(5) . . ? O100 Eu1 O61 73.8(5) . . ? O41 Eu1 O62 125.9(5) . . ? O100 Eu1 O62 79.9(5) . . ? O61 Eu1 O62 50.3(5) . . ? O41 Eu1 O52 152.4(5) . . ? O100 Eu1 O52 118.3(5) . . ? O61 Eu1 O52 128.9(5) . . ? O62 Eu1 O52 81.5(5) . . ? O41 Eu1 O42 49.7(5) . . ? O100 Eu1 O42 113.8(5) . . ? O61 Eu1 O42 71.4(4) . . ? O62 Eu1 O42 114.0(5) . . ? O52 Eu1 O42 127.5(5) . . ? O41 Eu1 O51 127.0(5) . . ? O100 Eu1 O51 68.6(5) . . ? O61 Eu1 O51 118.1(5) . . ? O62 Eu1 O51 75.7(6) . . ? O52 Eu1 O51 49.8(5) . . ? O42 Eu1 O51 170.1(5) . . ? O41 Eu1 N21 72.1(5) . . ? O100 Eu1 N21 82.8(5) . . ? O61 Eu1 N21 147.3(5) . . ? O62 Eu1 N21 147.0(5) . . ? O52 Eu1 N21 82.3(5) . . ? O42 Eu1 N21 98.7(4) . . ? O51 Eu1 N21 71.9(5) . . ? O41 Eu1 N11 90.7(4) . . ? O100 Eu1 N11 143.5(4) . . ? O61 Eu1 N11 133.5(5) . . ? O62 Eu1 N11 134.8(5) . . ? O52 Eu1 N11 67.5(5) . . ? O42 Eu1 N11 67.4(5) . . ? O51 Eu1 N11 104.6(5) . . ? N21 Eu1 N11 61.6(5) . . ? O41 Eu1 N31 114.9(5) . . ? O100 Eu1 N31 152.4(5) . . ? O61 Eu1 N31 80.4(5) . . ? O62 Eu1 N31 76.2(5) . . ? O52 Eu1 N31 71.5(5) . . ? O42 Eu1 N31 65.3(5) . . ? O51 Eu1 N31 117.4(5) . . ? N21 Eu1 N31 124.8(5) . . ? N11 Eu1 N31 63.6(4) . . ? N21 C22 O23 115.4(17) . . ? N21 C22 C12 126.4(18) . . ? O23 C22 C12 118.2(16) . . ? C22 N21 C29 105.3(16) . . ? C22 N21 Eu1 117.7(13) . . ? C29 N21 Eu1 136.8(12) . . ? C28 C29 C24 120(2) . . ? C28 C29 N21 132.9(19) . . ? C24 C29 N21 107.5(18) . . ? C29 C28 C27 116.7(19) . . ? C26 C27 C28 123(2) . . ? C27 C26 C25 121(2) . . ? C24 C25 C26 115(2) . . ? C25 C24 O23 127.4(18) . . ? C25 C24 C29 125(2) . . ? O23 C24 C29 107.6(18) . . ? C22 O23 C24 104.2(14) . . ? C12 N11 C16 118.2(15) . . ? C12 N11 Eu1 121.8(12) . . ? C16 N11 Eu1 119.8(10) . . ? N11 C12 C13 121.3(17) . . ? N11 C12 C22 112.3(16) . . ? C13 C12 C22 126.4(17) . . ? C14 C13 C12 119.2(18) . . ? C13 C14 C15 121(2) . . ? C16 C15 C14 115.6(18) . . ? N11 C16 C15 124.3(15) . . ? N11 C16 C32 113.8(15) . . ? C15 C16 C32 121.8(17) . . ? N31 C32 O33 116.6(16) . . ? N31 C32 C16 127.5(17) . . ? O33 C32 C16 115.8(16) . . ? C32 N31 C39 104.1(15) . . ? C32 N31 Eu1 115.0(12) . . ? C39 N31 Eu1 139.5(12) . . ? C34 C39 C38 122(2) . . ? C34 C39 N31 108.0(17) . . ? C38 C39 N31 130(2) . . ? C39 C38 C37 114(2) . . ? C36 C37 C38 124(2) . . ? C37 C36 C35 121(2) . . ? C34 C35 C36 114(2) . . ? C39 C34 C35 125.0(19) . . ? C39 C34 O33 107.1(16) . . ? C35 C34 O33 127.7(17) . . ? C32 O33 C34 104.1(14) . . ? O41 N43 O44 128(2) . . ? O41 N43 O42 113.1(17) . . ? O44 N43 O42 119(2) . . ? N43 O41 Eu1 101.7(13) . . ? N43 O42 Eu1 95.4(11) . . ? O54 N53 O51 124(2) . . ? O54 N53 O52 122(2) . . ? O51 N53 O52 114(2) . . ? N53 O52 Eu1 98.4(13) . . ? N53 O51 Eu1 97.9(14) . . ? O64 N63 O61 124(2) . . ? O64 N63 O62 121(2) . . ? O61 N63 O62 113.9(17) . . ? N63 O61 Eu1 98.4(12) . . ? N63 O62 Eu1 96.1(12) . . ? N71 C72 C73 124(3) . . ? N71 C72 C92 115.4(18) . . ? C73 C72 C92 121(3) . . ? C76 N71 C72 115.4(19) . . ? C74 C73 C72 118(3) . . ? C73 C74 C75 121(3) . . ? C74 C75 C76 116(3) . . ? N71 C76 C75 126(2) . . ? N71 C76 C82 113.0(19) . . ? C75 C76 C82 121(2) . . ? N81 C82 O83 112(2) . . ? N81 C82 C76 129(2) . . ? O83 C82 C76 119(2) . . ? C82 O83 C84 106.2(17) . . ? C85 C84 O83 130(2) . . ? C85 C84 C89 122(2) . . ? O83 C84 C89 108(2) . . ? C84 C85 C86 117(2) . . ? C87 C86 C85 124(3) . . ? C86 C87 C88 119(3) . . ? C89 C88 C87 118(3) . . ? C88 C89 N81 132(2) . . ? C88 C89 C84 120(2) . . ? N81 C89 C84 107(2) . . ? C82 N81 C89 106.4(19) . . ? N91 C92 O93 118(2) . . ? N91 C92 C72 123(2) . . ? O93 C92 C72 118(2) . . ? C92 O93 C94 102.3(19) . . ? C99 C94 C95 126(3) . . ? C99 C94 O93 108(2) . . ? C95 C94 O93 126(2) . . ? C96 C95 C94 112(3) . . ? C97 C96 C95 123(3) . . ? C96 C97 C98 125(3) . . ? C99 C98 C97 112(3) . . ? C94 C99 C98 122(3) . . ? C94 C99 N91 108(2) . . ? C98 C99 N91 130(2) . . ? C92 N91 C99 103(2) . . ? _refine_diff_density_max 2.953 _refine_diff_density_min -1.894 _refine_diff_density_rms 0.264 #===END data_Gd-3 _database_code_depnum_ccdc_archive 'CCDC 193089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H24 Gd N9 O13' _chemical_formula_weight 983.92 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.527(14) _cell_length_b 10.643(14) _cell_length_c 17.09(2) _cell_angle_alpha 86.191(10) _cell_angle_beta 79.141(10) _cell_angle_gamma 82.187(10) _cell_volume 1861(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6246 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.96 _reflns_number_total 6246 _reflns_number_gt 4746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6246 _refine_ls_number_parameters 560 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2218 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.549 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.19569(4) 0.29342(4) 0.18224(2) 0.0430(2) Uani 1 d . . . C22 C -0.0186(9) 0.3470(8) 0.0541(5) 0.0410(18) Uani 1 d . . . N21 N -0.0212(7) 0.3513(8) 0.1302(4) 0.0467(17) Uani 1 d . . . C29 C -0.1533(9) 0.4032(8) 0.1599(5) 0.0437(18) Uani 1 d . . . C28 C -0.2172(10) 0.4286(10) 0.2377(6) 0.057(2) Uani 1 d . . . H28 H -0.1739 0.4165 0.2808 0.068 Uiso 1 calc R . . C27 C -0.3477(10) 0.4723(11) 0.2467(6) 0.062(3) Uani 1 d . . . H27 H -0.3947 0.4848 0.2979 0.074 Uiso 1 calc R . . C26 C -0.4136(9) 0.4989(10) 0.1821(6) 0.055(2) Uani 1 d . . . H26 H -0.5003 0.5352 0.1910 0.066 Uiso 1 calc R . . C25 C -0.3497(9) 0.4712(10) 0.1044(6) 0.054(2) Uani 1 d . . . H25 H -0.3917 0.4835 0.0608 0.065 Uiso 1 calc R . . C24 C -0.2194(9) 0.4242(9) 0.0977(5) 0.0449(19) Uani 1 d . . . O23 O -0.1335(6) 0.3883(6) 0.0277(3) 0.0493(14) Uani 1 d . . . N11 N 0.2014(7) 0.2659(7) 0.0289(4) 0.0435(16) Uani 1 d . . . C12 C 0.0936(9) 0.2975(8) -0.0041(5) 0.0443(19) Uani 1 d . . . C13 C 0.0897(10) 0.2875(10) -0.0833(6) 0.054(2) Uani 1 d . . . H13 H 0.0138 0.3120 -0.1037 0.064 Uiso 1 calc R . . C14 C 0.2070(10) 0.2382(10) -0.1321(5) 0.052(2) Uani 1 d . . . H14 H 0.2090 0.2272 -0.1859 0.062 Uiso 1 calc R . . C15 C 0.3174(10) 0.2065(9) -0.1008(5) 0.053(2) Uani 1 d . . . H15 H 0.3959 0.1765 -0.1328 0.064 Uiso 1 calc R . . C16 C 0.3093(8) 0.2203(8) -0.0194(5) 0.0416(18) Uani 1 d . . . C32 C 0.4230(9) 0.1858(8) 0.0223(5) 0.0420(18) Uani 1 d U . . N31 N 0.4213(7) 0.1864(7) 0.0978(4) 0.0489(17) Uani 1 d U . . C39 C 0.5536(8) 0.1490(8) 0.1048(5) 0.0419(18) Uani 1 d U . . C38 C 0.6159(10) 0.1340(10) 0.1717(6) 0.057(2) Uani 1 d U . . H38 H 0.5693 0.1468 0.2231 0.068 Uiso 1 calc R . . C37 C 0.7469(10) 0.1000(10) 0.1575(7) 0.059(2) Uani 1 d U . . H37 H 0.7910 0.0911 0.2002 0.071 Uiso 1 calc R . . C36 C 0.8194(9) 0.0775(9) 0.0795(6) 0.054(2) Uani 1 d U . . H36 H 0.9088 0.0524 0.0726 0.065 Uiso 1 calc R . . C35 C 0.7585(9) 0.0925(9) 0.0133(6) 0.053(2) Uani 1 d U . . H35 H 0.8041 0.0792 -0.0382 0.063 Uiso 1 calc R . . C34 C 0.6250(9) 0.1288(8) 0.0298(5) 0.0447(18) Uani 1 d U . . O33 O 0.5402(6) 0.1475(6) -0.0244(3) 0.0458(13) Uani 1 d U . . N43 N 0.2587(8) 0.5444(8) 0.1167(4) 0.0512(19) Uani 1 d . . . O44 O 0.2869(9) 0.6535(7) 0.0932(4) 0.072(2) Uani 1 d . . . O41 O 0.1526(7) 0.5314(7) 0.1638(4) 0.0594(17) Uani 1 d . . . O42 O 0.3314(7) 0.4449(7) 0.0939(4) 0.0572(17) Uani 1 d . . . N53 N 0.0748(9) 0.0583(8) 0.2091(5) 0.056(2) Uani 1 d . . . O52 C 0.1674(7) 0.0747(7) 0.1534(4) 0.0336(15) Uani 1 d . . . O54 O 0.0256(8) -0.0413(7) 0.2173(6) 0.081(2) Uani 1 d . . . O51 O 0.0332(8) 0.1482(7) 0.2546(4) 0.0656(19) Uani 1 d . . . N63 N 0.3595(9) 0.2653(10) 0.3014(4) 0.061(2) Uani 1 d . . . O61 O 0.3496(7) 0.3646(7) 0.2560(4) 0.0585(16) Uani 1 d . . . O62 O 0.3031(7) 0.1732(6) 0.2850(4) 0.0591(17) Uani 1 d . . . O64 O 0.4184(9) 0.2581(10) 0.3575(5) 0.084(3) Uani 1 d . . . C72 C 1.2095(10) 0.4381(10) 0.4942(6) 0.058(2) Uani 1 d . . . N71 N 1.1183(9) 0.3748(8) 0.4741(5) 0.057(2) Uani 1 d . . . C73 C 1.2443(15) 0.4212(13) 0.5686(7) 0.083(4) Uani 1 d . . . H73 H 1.3038 0.4691 0.5823 0.099 Uiso 1 calc R . . C74 C 1.1896(14) 0.3322(14) 0.6221(7) 0.082(4) Uani 1 d . . . H74 H 1.2137 0.3191 0.6720 0.099 Uiso 1 calc R . . C75 C 1.1006(13) 0.2634(14) 0.6031(7) 0.076(3) Uani 1 d . . . H75 H 1.0638 0.2025 0.6386 0.091 Uiso 1 calc R . . C76 C 1.0670(11) 0.2884(11) 0.5275(6) 0.061(3) Uani 1 d . . . C82 C 0.9690(10) 0.2206(11) 0.5014(6) 0.060(3) Uani 1 d . . . O83 O 0.9213(8) 0.1280(7) 0.5525(4) 0.067(2) Uani 1 d . . . C84 C 0.8342(11) 0.0842(11) 0.5128(6) 0.062(3) Uani 1 d . . . C85 C 0.7550(13) -0.0117(12) 0.5389(8) 0.080(4) Uani 1 d . . . H85 H 0.7566 -0.0568 0.5873 0.096 Uiso 1 calc R . . C86 C 0.6758(15) -0.0340(12) 0.4884(9) 0.084(4) Uani 1 d . . . H86 H 0.6228 -0.0981 0.5019 0.101 Uiso 1 calc R . . C87 C 0.6715(13) 0.0401(13) 0.4134(9) 0.084(4) Uani 1 d . . . H87 H 0.6144 0.0244 0.3809 0.101 Uiso 1 calc R . . C88 C 0.7515(12) 0.1323(13) 0.3912(8) 0.077(3) Uani 1 d . . . H88 H 0.7494 0.1798 0.3437 0.093 Uiso 1 calc R . . C89 C 0.8343(11) 0.1533(10) 0.4400(6) 0.060(2) Uani 1 d . . . N81 N 0.9233(9) 0.2419(9) 0.4354(5) 0.061(2) Uani 1 d . . . C92 C 1.2566(11) 0.5351(11) 0.4344(6) 0.062(3) Uani 1 d . . . O93 O 1.3581(8) 0.5932(8) 0.4458(5) 0.076(2) Uani 1 d . . . C94 C 1.3758(11) 0.6802(10) 0.3821(6) 0.058(2) Uani 1 d . . . C95 C 1.4626(11) 0.7695(13) 0.3643(9) 0.080(4) Uani 1 d . . . H95 H 1.5246 0.7765 0.3955 0.096 Uiso 1 calc R . . C96 C 1.4514(13) 0.8461(13) 0.2988(9) 0.077(3) Uani 1 d . . . H96 H 1.5079 0.9073 0.2849 0.092 Uiso 1 calc R . . C97 C 1.3622(13) 0.8378(12) 0.2524(8) 0.074(3) Uani 1 d . . . H97 H 1.3600 0.8932 0.2081 0.089 Uiso 1 calc R . . C98 C 1.2729(13) 0.7488(12) 0.2685(7) 0.074(3) Uani 1 d . . . H98 H 1.2111 0.7443 0.2368 0.088 Uiso 1 calc R . . C99 C 1.2824(10) 0.6679(10) 0.3351(7) 0.057(2) Uani 1 d . . . N91 N 1.2077(8) 0.5731(9) 0.3711(5) 0.057(2) Uani 1 d . . . O100 O 0.0682(6) 0.3843(6) 0.3024(3) 0.0500(15) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0464(3) 0.0452(3) 0.0376(3) -0.00001(17) -0.00764(17) -0.0071(2) C22 0.051(4) 0.031(4) 0.044(4) 0.002(3) -0.011(3) -0.013(4) N21 0.046(4) 0.055(5) 0.042(4) 0.000(3) -0.009(3) -0.015(3) C29 0.046(4) 0.043(5) 0.042(4) -0.003(3) -0.007(3) -0.007(4) C28 0.059(5) 0.059(6) 0.055(5) -0.001(4) -0.019(4) -0.011(5) C27 0.054(5) 0.073(7) 0.055(6) -0.012(5) 0.003(4) -0.008(5) C26 0.038(4) 0.064(6) 0.064(6) -0.003(5) -0.009(4) -0.008(4) C25 0.049(5) 0.062(6) 0.053(5) 0.003(4) -0.010(4) -0.015(5) C24 0.048(5) 0.047(5) 0.043(4) 0.004(4) -0.016(3) -0.012(4) O23 0.053(3) 0.061(4) 0.037(3) 0.006(3) -0.015(2) -0.010(3) N11 0.051(4) 0.043(4) 0.037(3) -0.006(3) -0.003(3) -0.012(3) C12 0.054(5) 0.040(5) 0.040(4) -0.004(3) -0.005(4) -0.016(4) C13 0.060(5) 0.053(6) 0.048(5) -0.004(4) -0.020(4) 0.008(5) C14 0.066(6) 0.056(6) 0.034(4) -0.003(4) -0.010(4) -0.004(5) C15 0.069(6) 0.053(5) 0.033(4) -0.004(4) 0.003(4) -0.010(5) C16 0.045(4) 0.034(4) 0.048(4) 0.001(3) -0.010(3) -0.011(4) C32 0.048(4) 0.035(4) 0.042(4) -0.001(3) -0.003(3) -0.010(4) N31 0.053(4) 0.053(4) 0.042(4) -0.008(3) -0.005(3) -0.013(4) C39 0.038(4) 0.038(4) 0.050(5) -0.004(3) -0.006(3) -0.004(4) C38 0.059(6) 0.057(6) 0.051(5) -0.004(4) -0.005(4) -0.006(5) C37 0.056(5) 0.044(5) 0.078(7) -0.003(5) -0.015(5) -0.002(5) C36 0.045(5) 0.053(6) 0.064(6) -0.003(4) -0.009(4) -0.007(4) C35 0.045(4) 0.038(5) 0.073(6) -0.001(4) -0.007(4) -0.006(4) C34 0.049(4) 0.035(4) 0.049(5) 0.002(3) -0.007(4) -0.006(4) O33 0.048(3) 0.047(3) 0.042(3) -0.003(2) -0.008(2) -0.006(3) N43 0.064(5) 0.054(5) 0.041(4) 0.006(3) -0.016(3) -0.024(4) O44 0.107(6) 0.052(4) 0.064(4) 0.011(3) -0.022(4) -0.033(4) O41 0.055(4) 0.056(4) 0.064(4) 0.002(3) -0.013(3) 0.005(3) O42 0.067(4) 0.046(4) 0.056(4) 0.001(3) -0.002(3) -0.008(3) N53 0.065(5) 0.038(4) 0.070(5) 0.006(4) -0.025(4) -0.008(4) O52 0.042(4) 0.033(4) 0.027(3) -0.010(3) 0.004(3) -0.016(3) O54 0.078(5) 0.043(4) 0.124(7) 0.011(4) -0.020(5) -0.022(4) O51 0.071(5) 0.059(4) 0.060(4) -0.006(3) 0.010(3) -0.013(4) N63 0.060(5) 0.085(7) 0.032(4) -0.005(4) 0.001(3) -0.003(5) O61 0.062(4) 0.062(4) 0.057(4) 0.003(3) -0.018(3) -0.018(3) O62 0.075(5) 0.046(4) 0.056(4) 0.002(3) -0.018(3) 0.003(4) O64 0.085(5) 0.118(7) 0.057(5) 0.001(4) -0.043(4) -0.005(5) C72 0.065(6) 0.061(6) 0.049(5) -0.015(4) -0.015(4) -0.003(5) N71 0.073(5) 0.053(5) 0.043(4) -0.009(3) -0.011(4) -0.001(4) C73 0.115(10) 0.082(8) 0.069(7) -0.005(6) -0.045(7) -0.032(8) C74 0.099(9) 0.101(10) 0.052(6) -0.003(6) -0.029(6) -0.008(8) C75 0.082(8) 0.093(9) 0.050(6) -0.002(6) -0.012(5) 0.002(7) C76 0.064(6) 0.069(7) 0.045(5) -0.010(5) -0.005(4) 0.002(5) C82 0.055(5) 0.064(6) 0.056(6) -0.004(5) -0.004(4) 0.011(5) O83 0.076(5) 0.072(5) 0.044(4) 0.004(3) 0.003(3) -0.001(4) C84 0.072(6) 0.065(6) 0.043(5) -0.004(4) 0.009(4) -0.015(5) C85 0.088(9) 0.065(7) 0.070(7) 0.003(6) 0.030(7) -0.011(7) C86 0.094(9) 0.059(7) 0.097(9) -0.007(6) 0.008(8) -0.036(7) C87 0.075(8) 0.072(8) 0.105(10) -0.010(7) -0.007(7) -0.022(7) C88 0.077(8) 0.084(9) 0.072(7) 0.008(6) -0.013(6) -0.020(7) C89 0.063(6) 0.055(6) 0.057(6) 0.004(4) 0.001(5) -0.008(5) N81 0.071(5) 0.067(6) 0.046(4) 0.003(4) -0.009(4) -0.012(5) C92 0.064(6) 0.067(7) 0.057(6) -0.022(5) -0.012(5) -0.007(5) O93 0.080(5) 0.071(5) 0.084(5) -0.012(4) -0.033(4) -0.009(4) C94 0.066(6) 0.045(5) 0.063(6) -0.009(4) -0.017(5) 0.000(5) C95 0.055(6) 0.071(8) 0.120(11) -0.030(7) -0.028(7) 0.002(6) C96 0.070(7) 0.069(8) 0.097(10) -0.008(7) -0.018(7) -0.019(6) C97 0.085(8) 0.058(7) 0.071(7) -0.008(5) 0.002(6) 0.000(6) C98 0.077(7) 0.069(7) 0.070(7) -0.014(6) -0.007(6) 0.005(6) C99 0.053(5) 0.049(5) 0.067(6) -0.016(4) -0.010(4) 0.003(5) N91 0.058(5) 0.063(5) 0.048(4) -0.013(4) -0.011(4) 0.006(4) O100 0.052(3) 0.065(4) 0.033(3) -0.012(3) -0.002(2) -0.011(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 Gd1 O41 2.521(8) . ? Gd1 O100 2.413(6) . ? Gd1 O61 2.453(7) . ? Gd1 O52 2.480(8) . ? Gd1 O62 2.460(7) . ? Gd1 O42 2.532(7) . ? Gd1 O51 2.552(7) . ? Gd1 N21 2.587(8) . ? Gd1 N11 2.645(7) . ? Gd1 N31 2.686(8) . ? C22 N21 1.298(11) . ? C22 O23 1.376(11) . ? C22 C12 1.457(12) . ? N21 C29 1.435(12) . ? C29 C28 1.398(13) . ? C29 C24 1.367(12) . ? C28 C27 1.372(15) . ? C27 C26 1.405(15) . ? C26 C25 1.401(14) . ? C25 C24 1.381(13) . ? C24 O23 1.398(11) . ? N11 C12 1.353(12) . ? N11 C16 1.325(11) . ? C12 C13 1.374(13) . ? C13 C14 1.411(13) . ? C14 C15 1.362(14) . ? C15 C16 1.394(12) . ? C16 C32 1.498(12) . ? C32 N31 1.287(11) . ? C32 O33 1.364(10) . ? N31 C39 1.421(12) . ? C39 C34 1.373(12) . ? C39 C38 1.411(14) . ? C38 C37 1.358(15) . ? C37 C36 1.423(15) . ? C36 C35 1.391(14) . ? C35 C34 1.386(13) . ? C34 O33 1.391(11) . ? N43 O41 1.266(10) . ? N43 O44 1.258(10) . ? N43 O42 1.258(11) . ? N53 O54 1.230(10) . ? N53 O51 1.253(11) . ? N53 O52 1.249(11) . ? N63 O64 1.230(11) . ? N63 O61 1.273(11) . ? N63 O62 1.285(12) . ? C72 N71 1.350(13) . ? C72 C73 1.381(15) . ? C72 C92 1.472(16) . ? N71 C76 1.345(14) . ? C73 C74 1.379(19) . ? C74 C75 1.362(18) . ? C75 C76 1.401(15) . ? C76 C82 1.484(16) . ? C82 N81 1.302(14) . ? C82 O83 1.357(13) . ? O83 C84 1.382(14) . ? C84 C85 1.402(16) . ? C84 C89 1.403(14) . ? C85 C86 1.36(2) . ? C86 C87 1.46(2) . ? C87 C88 1.368(17) . ? C88 C89 1.363(17) . ? C89 N81 1.406(14) . ? C92 N91 1.300(14) . ? C92 O93 1.355(13) . ? O93 C94 1.384(13) . ? C94 C99 1.406(15) . ? C94 C95 1.386(17) . ? C95 C96 1.355(19) . ? C96 C97 1.353(19) . ? C97 C98 1.402(18) . ? C98 C99 1.390(16) . ? C99 N91 1.403(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 O41 Gd1 O100 69.6(2) . . ? O41 Gd1 O61 78.0(2) . . ? O100 Gd1 O61 73.2(2) . . ? O41 Gd1 O52 152.4(3) . . ? O100 Gd1 O52 118.1(2) . . ? O61 Gd1 O52 129.3(3) . . ? O41 Gd1 O62 127.0(2) . . ? O100 Gd1 O62 78.7(2) . . ? O61 Gd1 O62 52.2(2) . . ? O52 Gd1 O62 80.2(3) . . ? O41 Gd1 O42 50.5(2) . . ? O100 Gd1 O42 114.2(2) . . ? O61 Gd1 O42 70.5(2) . . ? O52 Gd1 O42 127.5(2) . . ? O62 Gd1 O42 115.0(3) . . ? O41 Gd1 O51 126.1(2) . . ? O100 Gd1 O51 68.2(2) . . ? O61 Gd1 O51 118.6(3) . . ? O52 Gd1 O51 50.2(2) . . ? O62 Gd1 O51 74.4(3) . . ? O42 Gd1 O51 170.4(3) . . ? O41 Gd1 N21 71.2(2) . . ? O100 Gd1 N21 82.7(2) . . ? O61 Gd1 N21 146.0(3) . . ? O52 Gd1 N21 83.2(3) . . ? O62 Gd1 N21 145.4(2) . . ? O42 Gd1 N21 99.2(2) . . ? O51 Gd1 N21 71.6(3) . . ? O41 Gd1 N11 91.0(2) . . ? O100 Gd1 N11 144.7(2) . . ? O61 Gd1 N11 133.0(2) . . ? O52 Gd1 N11 67.5(2) . . ? O62 Gd1 N11 134.5(2) . . ? O42 Gd1 N11 67.6(2) . . ? O51 Gd1 N11 104.9(2) . . ? N21 Gd1 N11 62.7(2) . . ? O41 Gd1 N31 114.9(2) . . ? O100 Gd1 N31 151.5(2) . . ? O61 Gd1 N31 80.2(3) . . ? O52 Gd1 N31 71.9(2) . . ? O62 Gd1 N31 77.0(3) . . ? O42 Gd1 N31 64.5(2) . . ? O51 Gd1 N31 118.3(2) . . ? N21 Gd1 N31 125.7(2) . . ? N11 Gd1 N31 63.3(2) . . ? N21 C22 O23 116.6(8) . . ? N21 C22 C12 125.4(8) . . ? O23 C22 C12 118.0(7) . . ? C22 N21 C29 103.0(7) . . ? C22 N21 Gd1 118.2(6) . . ? C29 N21 Gd1 138.4(6) . . ? C28 C29 C24 120.5(9) . . ? C28 C29 N21 130.6(8) . . ? C24 C29 N21 108.9(8) . . ? C29 C28 C27 116.0(9) . . ? C26 C27 C28 123.2(9) . . ? C27 C26 C25 120.5(9) . . ? C24 C25 C26 114.7(9) . . ? C25 C24 O23 126.5(8) . . ? C25 C24 C29 125.0(9) . . ? O23 C24 C29 108.5(8) . . ? C22 O23 C24 102.9(6) . . ? C12 N11 C16 116.6(7) . . ? C12 N11 Gd1 121.4(5) . . ? C16 N11 Gd1 122.0(6) . . ? N11 C12 C13 124.6(8) . . ? N11 C12 C22 112.0(7) . . ? C13 C12 C22 123.4(9) . . ? C14 C13 C12 116.5(9) . . ? C13 C14 C15 120.2(8) . . ? C16 C15 C14 118.0(9) . . ? N11 C16 C15 123.9(8) . . ? N11 C16 C32 113.0(7) . . ? C15 C16 C32 123.1(8) . . ? N31 C32 O33 116.5(8) . . ? N31 C32 C16 126.8(8) . . ? O33 C32 C16 116.6(7) . . ? C32 N31 C39 103.8(7) . . ? C32 N31 Gd1 114.3(6) . . ? C39 N31 Gd1 140.6(6) . . ? C34 C39 C38 120.2(8) . . ? C34 C39 N31 108.2(8) . . ? C38 C39 N31 131.6(8) . . ? C39 C38 C37 116.8(10) . . ? C36 C37 C38 122.4(10) . . ? C37 C36 C35 121.0(9) . . ? C34 C35 C36 115.1(9) . . ? C39 C34 C35 124.5(9) . . ? C39 C34 O33 108.4(7) . . ? C35 C34 O33 127.1(8) . . ? C32 O33 C34 103.0(7) . . ? O41 N43 O44 120.2(9) . . ? O41 N43 O42 117.3(7) . . ? O44 N43 O42 122.4(8) . . ? N43 O41 Gd1 96.1(5) . . ? N43 O42 Gd1 95.8(5) . . ? O54 N53 O51 122.0(9) . . ? O54 N53 O52 120.9(9) . . ? O51 N53 O52 117.1(8) . . ? N53 O52 Gd1 98.2(5) . . ? N53 O51 Gd1 94.5(5) . . ? O64 N63 O61 122.4(10) . . ? O64 N63 O62 122.1(9) . . ? O61 N63 O62 115.5(8) . . ? N63 O61 Gd1 96.2(6) . . ? N63 O62 Gd1 95.5(5) . . ? N71 C72 C73 121.8(11) . . ? N71 C72 C92 114.5(9) . . ? C73 C72 C92 123.3(10) . . ? C76 N71 C72 117.7(9) . . ? C74 C73 C72 119.0(12) . . ? C73 C74 C75 120.9(11) . . ? C74 C75 C76 116.9(12) . . ? N71 C76 C75 123.6(11) . . ? N71 C76 C82 115.1(9) . . ? C75 C76 C82 121.3(11) . . ? N81 C82 O83 117.1(10) . . ? N81 C82 C76 126.8(10) . . ? O83 C82 C76 116.1(9) . . ? C82 O83 C84 102.7(8) . . ? C85 C84 O83 127.5(11) . . ? C85 C84 C89 123.6(12) . . ? O83 C84 C89 108.9(9) . . ? C84 C85 C86 115.2(12) . . ? C87 C86 C85 121.9(11) . . ? C86 C87 C88 120.1(13) . . ? C89 C88 C87 118.7(12) . . ? C88 C89 N81 132.2(10) . . ? C88 C89 C84 120.4(10) . . ? N81 C89 C84 107.3(10) . . ? C82 N81 C89 104.0(9) . . ? N91 C92 O93 116.0(10) . . ? N91 C92 C72 125.8(10) . . ? O93 C92 C72 118.2(10) . . ? C92 O93 C94 104.3(9) . . ? C99 C94 C95 122.7(11) . . ? C99 C94 O93 107.2(10) . . ? C95 C94 O93 130.0(11) . . ? C96 C95 C94 115.9(11) . . ? C97 C96 C95 123.2(13) . . ? C96 C97 C98 122.5(13) . . ? C99 C98 C97 115.8(12) . . ? C94 C99 C98 119.9(11) . . ? C94 C99 N91 108.1(10) . . ? C98 C99 N91 131.9(10) . . ? C92 N91 C99 104.4(9) . . ? _refine_diff_density_max 2.932 _refine_diff_density_min -2.046 _refine_diff_density_rms 0.173 #===END