# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Bis(hydroxylaminato)-mono(pentamethylcyclopentadienyl) Rare Earth Metal Complexes ; loop_ _publ_author_name 'Norbert Mitzel' 'Tania Pape' 'Ajay Venugopal' 'Alexander Willner' # Attachment 'Compound_1.cif' data_ajay12 _database_code_depnum_ccdc_archive 'CCDC 716018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 N4 O4 Y2' _chemical_formula_weight 800.78 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1441(14) _cell_length_b 13.0349(14) _cell_length_c 21.666(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3994.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'beautiful plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.931 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59452 _diffrn_reflns_av_R_equivalents 0.1453 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.65 _diffrn_reflns_theta_max 26.94 _reflns_number_total 4174 _reflns_number_gt 3144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+5.8062P] 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 4174 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.00758(2) 0.52222(2) 0.083720(14) 0.01404(11) Uani 1 1 d . . . O1 O -0.09057(17) 0.53698(18) -0.00104(10) 0.0168(5) Uani 1 1 d . . . O2 O 0.07985(18) 0.66657(18) 0.08915(12) 0.0227(6) Uani 1 1 d . . . N1 N -0.1545(2) 0.5048(2) 0.04751(13) 0.0157(6) Uani 1 1 d . . . N2 N -0.0131(2) 0.7029(2) 0.10631(14) 0.0183(6) Uani 1 1 d . . . C1 C 0.0995(3) 0.4812(3) 0.19074(16) 0.0232(8) Uani 1 1 d . . . C2 C 0.0027(3) 0.4759(3) 0.20668(17) 0.0244(8) Uani 1 1 d . . . C3 C -0.0368(3) 0.3898(3) 0.17678(16) 0.0214(8) Uani 1 1 d . . . C4 C 0.0357(3) 0.3425(3) 0.14179(16) 0.0220(8) Uani 1 1 d . . . C5 C 0.1198(3) 0.3989(3) 0.15085(17) 0.0230(8) Uani 1 1 d . . . C6 C 0.1712(3) 0.5553(3) 0.2154(2) 0.0338(10) Uani 1 1 d . . . H6A H 0.2214(18) 0.5208(10) 0.2293(14) 0.051 Uiso 1 1 calc R . . H6B H 0.1457(10) 0.591(2) 0.2462(13) 0.051 Uiso 1 1 calc R . . H6C H 0.1891(17) 0.598(2) 0.1853(10) 0.051 Uiso 1 1 calc R . . C7 C -0.0457(4) 0.5356(3) 0.25649(19) 0.0363(11) Uani 1 1 d . . . H7A H -0.064(2) 0.4947(13) 0.2851(12) 0.054 Uiso 1 1 calc R . . H7B H -0.094(2) 0.566(2) 0.2414(6) 0.054 Uiso 1 1 calc R . . H7C H -0.0074(14) 0.580(2) 0.2714(12) 0.054 Uiso 1 1 calc R . . C8 C -0.1337(3) 0.3482(3) 0.18859(19) 0.0309(9) Uani 1 1 d . . . H8A H -0.1338(6) 0.312(2) 0.2251(12) 0.046 Uiso 1 1 calc R . . H8B H -0.1509(10) 0.305(2) 0.1567(11) 0.046 Uiso 1 1 calc R . . H8C H -0.1761(12) 0.4017(14) 0.1912(13) 0.046 Uiso 1 1 calc R . . C9 C 0.0272(3) 0.2415(3) 0.10891(19) 0.0319(10) Uani 1 1 d . . . H9A H 0.026(2) 0.1865(15) 0.1388(8) 0.048 Uiso 1 1 calc R . . H9B H 0.0805(18) 0.2326(11) 0.0816(13) 0.048 Uiso 1 1 calc R . . H9C H -0.0307(19) 0.2404(9) 0.0852(13) 0.048 Uiso 1 1 calc R . . C10 C 0.2161(3) 0.3672(3) 0.1281(2) 0.0355(10) Uani 1 1 d . . . H10A H 0.2383(12) 0.309(2) 0.1519(12) 0.053 Uiso 1 1 calc R . . H10B H 0.2597(13) 0.4237(17) 0.1328(13) 0.053 Uiso 1 1 calc R . . H10C H 0.2122(5) 0.348(2) 0.0851(12) 0.053 Uiso 1 1 calc R . . C11 C -0.2269(3) 0.5855(3) 0.05387(17) 0.0221(8) Uani 1 1 d . . . H11A H -0.2648 0.5893 0.0155 0.027 Uiso 1 1 calc R . . H11B H -0.1956 0.6526 0.0600 0.027 Uiso 1 1 calc R . . C12 C -0.2915(3) 0.5635(4) 0.1080(2) 0.0413(11) Uani 1 1 d . . . H12A H -0.331(2) 0.619(2) 0.1145(11) 0.062 Uiso 1 1 calc R . . H12B H -0.2555(11) 0.552(3) 0.1431(11) 0.062 Uiso 1 1 calc R . . H12C H -0.328(2) 0.506(2) 0.0996(7) 0.062 Uiso 1 1 calc R . . C13 C -0.1942(3) 0.4039(3) 0.03141(17) 0.0219(8) Uani 1 1 d . . . H13A H -0.2300 0.3780 0.0675 0.026 Uiso 1 1 calc R . . H13B H -0.1412 0.3559 0.0241 0.026 Uiso 1 1 calc R . . C14 C -0.2589(3) 0.4009(3) -0.0245(2) 0.0311(9) Uani 1 1 d . . . H14A H -0.2719(18) 0.3300(19) -0.0355(9) 0.047 Uiso 1 1 calc R . . H14B H -0.2284(12) 0.435(2) -0.0590(10) 0.047 Uiso 1 1 calc R . . H14C H -0.3179(18) 0.436(2) -0.0149(5) 0.047 Uiso 1 1 calc R . . C21 C -0.0062(3) 0.7513(3) 0.16734(17) 0.0261(8) Uani 1 1 d . . . H21A H 0.0364 0.8114 0.1647 0.031 Uiso 1 1 calc R . . H21B H 0.0220 0.7019 0.1968 0.031 Uiso 1 1 calc R . . C22 C -0.1012(3) 0.7854(3) 0.1913(2) 0.0375(11) Uani 1 1 d . . . H22A H -0.0963(6) 0.801(2) 0.2335(12) 0.056 Uiso 1 1 calc R . . H22B H -0.1454(14) 0.7326(17) 0.1857(13) 0.056 Uiso 1 1 calc R . . H22C H -0.1209(12) 0.844(2) 0.1696(12) 0.056 Uiso 1 1 calc R . . C23 C -0.0429(3) 0.7768(3) 0.05840(17) 0.0232(8) Uani 1 1 d . . . H23A H -0.1059 0.8041 0.0697 0.028 Uiso 1 1 calc R . . H23B H -0.0499 0.7396 0.0188 0.028 Uiso 1 1 calc R . . C24 C 0.0241(4) 0.8672(3) 0.0483(2) 0.0368(10) Uani 1 1 d . . . H24A H 0.0067(15) 0.9029(18) 0.0108(14) 0.055 Uiso 1 1 calc R . . H24B H 0.088(2) 0.8421(8) 0.0448(15) 0.055 Uiso 1 1 calc R . . H24C H 0.0196(17) 0.9139(19) 0.0831(12) 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01425(18) 0.01279(17) 0.01508(17) -0.00045(12) -0.00102(12) 0.00077(12) O1 0.0149(13) 0.0163(12) 0.0191(12) 0.0013(9) 0.0020(9) -0.0006(9) O2 0.0152(13) 0.0149(12) 0.0380(15) -0.0037(11) 0.0010(11) -0.0009(9) N1 0.0133(16) 0.0133(14) 0.0204(15) 0.0003(11) 0.0020(11) 0.0012(10) N2 0.0188(17) 0.0144(14) 0.0216(15) -0.0019(11) -0.0012(11) 0.0016(11) C1 0.028(2) 0.0244(19) 0.0172(17) 0.0034(15) -0.0073(14) 0.0013(16) C2 0.029(2) 0.0243(18) 0.0202(17) 0.0016(15) -0.0019(14) 0.0041(17) C3 0.026(2) 0.0195(18) 0.0185(18) 0.0050(14) 0.0013(14) 0.0011(14) C4 0.029(2) 0.0186(18) 0.0188(17) 0.0039(14) 0.0004(14) 0.0058(15) C5 0.025(2) 0.0231(19) 0.0212(19) 0.0056(15) -0.0009(14) 0.0067(15) C6 0.033(3) 0.035(2) 0.034(2) 0.0022(19) -0.0155(18) -0.0012(18) C7 0.054(3) 0.032(2) 0.023(2) -0.0003(18) 0.0074(18) 0.0060(19) C8 0.030(2) 0.031(2) 0.032(2) 0.0098(18) 0.0032(17) -0.0021(17) C9 0.057(3) 0.0160(18) 0.0229(19) 0.0012(15) 0.0016(18) 0.0053(18) C10 0.026(2) 0.038(2) 0.042(3) 0.010(2) 0.0037(18) 0.0142(18) C11 0.021(2) 0.0181(18) 0.0271(19) -0.0017(15) 0.0012(14) 0.0040(14) C12 0.033(3) 0.040(3) 0.051(3) -0.002(2) 0.019(2) 0.010(2) C13 0.024(2) 0.0143(17) 0.027(2) 0.0000(14) 0.0031(15) -0.0024(14) C14 0.024(2) 0.029(2) 0.040(2) -0.0075(18) -0.0011(17) -0.0071(16) C21 0.035(2) 0.0197(17) 0.0232(18) -0.0061(14) -0.0057(17) 0.0028(17) C22 0.045(3) 0.033(2) 0.034(2) -0.0071(19) 0.0027(19) 0.012(2) C23 0.028(2) 0.0159(18) 0.0260(19) -0.0007(15) -0.0033(15) 0.0016(15) C24 0.046(3) 0.0177(19) 0.047(3) 0.0080(18) -0.002(2) -0.0070(18) _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 Y1 O2 2.145(2) . ? Y1 O1 2.276(2) 5_565 ? Y1 O1 2.310(2) . ? Y1 N2 2.423(3) . ? Y1 N1 2.434(3) . ? Y1 C5 2.686(4) . ? Y1 C4 2.688(4) . ? Y1 C1 2.712(3) . ? Y1 C3 2.728(4) . ? Y1 C2 2.733(4) . ? Y1 Y1 3.6800(8) 5_565 ? O1 N1 1.450(4) . ? O1 Y1 2.276(2) 5_565 ? O2 N2 1.446(4) . ? N1 C13 1.472(4) . ? N1 C11 1.474(4) . ? N2 C21 1.468(4) . ? N2 C23 1.478(5) . ? C1 C5 1.407(5) . ? C1 C2 1.414(6) . ? C1 C6 1.498(5) . ? C2 C3 1.411(5) . ? C2 C7 1.497(5) . ? C3 C4 1.416(5) . ? C3 C8 1.496(5) . ? C4 C5 1.412(6) . ? C4 C9 1.502(5) . ? C5 C10 1.507(5) . ? C11 C12 1.515(6) . ? C13 C14 1.519(6) . ? C21 C22 1.508(6) . ? C23 C24 1.527(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Y1 O1 95.44(9) . 5_565 ? O2 Y1 O1 104.89(9) . . ? O1 Y1 O1 73.29(10) 5_565 . ? O2 Y1 N2 36.25(9) . . ? O1 Y1 N2 123.40(9) 5_565 . ? O1 Y1 N2 90.41(9) . . ? O2 Y1 N1 123.28(9) . . ? O1 Y1 N1 101.56(9) 5_565 . ? O1 Y1 N1 35.46(9) . . ? N2 Y1 N1 92.43(10) . . ? O2 Y1 C5 102.34(11) . . ? O1 Y1 C5 85.34(10) 5_565 . ? O1 Y1 C5 146.64(10) . . ? N2 Y1 C5 122.91(11) . . ? N1 Y1 C5 132.45(11) . . ? O2 Y1 C4 131.93(11) . . ? O1 Y1 C4 89.81(10) 5_565 . ? O1 Y1 C4 122.24(10) . . ? N2 Y1 C4 140.37(10) . . ? N1 Y1 C4 102.04(11) . . ? C5 Y1 C4 30.46(12) . . ? O2 Y1 C1 84.11(11) . . ? O1 Y1 C1 111.03(10) 5_565 . ? O1 Y1 C1 169.85(10) . . ? N2 Y1 C1 94.40(11) . . ? N1 Y1 C1 135.15(11) . . ? C5 Y1 C1 30.21(11) . . ? C4 Y1 C1 50.00(12) . . ? O2 Y1 C3 128.64(11) . . ? O1 Y1 C3 119.06(10) 5_565 . ? O1 Y1 C3 120.14(10) . . ? N2 Y1 C3 115.99(11) . . ? N1 Y1 C3 87.85(11) . . ? C5 Y1 C3 49.97(12) . . ? C4 Y1 C3 30.29(11) . . ? C1 Y1 C3 49.72(12) . . ? O2 Y1 C2 98.77(11) . . ? O1 Y1 C2 134.86(10) 5_565 . ? O1 Y1 C2 141.10(10) . . ? N2 Y1 C2 90.86(11) . . ? N1 Y1 C2 105.65(11) . . ? C5 Y1 C2 49.82(11) . . ? C4 Y1 C2 49.82(11) . . ? C1 Y1 C2 30.11(12) . . ? C3 Y1 C2 29.95(11) . . ? O2 Y1 Y1 102.71(7) . 5_565 ? O1 Y1 Y1 36.96(6) 5_565 5_565 ? O1 Y1 Y1 36.33(6) . 5_565 ? N2 Y1 Y1 110.19(7) . 5_565 ? N1 Y1 Y1 67.21(7) . 5_565 ? C5 Y1 Y1 118.30(8) . 5_565 ? C4 Y1 Y1 109.44(8) . 5_565 ? C1 Y1 Y1 147.12(8) . 5_565 ? C3 Y1 Y1 128.00(8) . 5_565 ? C2 Y1 Y1 157.64(8) . 5_565 ? N1 O1 Y1 142.62(18) . 5_565 ? N1 O1 Y1 76.95(15) . . ? Y1 O1 Y1 106.71(10) 5_565 . ? N2 O2 Y1 82.43(16) . . ? O1 N1 C13 109.0(2) . . ? O1 N1 C11 107.1(2) . . ? C13 N1 C11 113.3(3) . . ? O1 N1 Y1 67.59(14) . . ? C13 N1 Y1 121.3(2) . . ? C11 N1 Y1 123.9(2) . . ? O2 N2 C21 108.2(3) . . ? O2 N2 C23 107.0(3) . . ? C21 N2 C23 111.8(3) . . ? O2 N2 Y1 61.31(13) . . ? C21 N2 Y1 126.2(2) . . ? C23 N2 Y1 121.8(2) . . ? C5 C1 C2 108.0(3) . . ? C5 C1 C6 124.9(4) . . ? C2 C1 C6 126.9(4) . . ? C5 C1 Y1 73.9(2) . . ? C2 C1 Y1 75.8(2) . . ? C6 C1 Y1 120.1(3) . . ? C3 C2 C1 108.1(3) . . ? C3 C2 C7 124.3(4) . . ? C1 C2 C7 126.4(4) . . ? C3 C2 Y1 74.8(2) . . ? C1 C2 Y1 74.1(2) . . ? C7 C2 Y1 126.8(3) . . ? C2 C3 C4 107.8(3) . . ? C2 C3 C8 124.9(4) . . ? C4 C3 C8 126.7(4) . . ? C2 C3 Y1 75.2(2) . . ? C4 C3 Y1 73.3(2) . . ? C8 C3 Y1 124.5(2) . . ? C5 C4 C3 108.0(3) . . ? C5 C4 C9 126.2(4) . . ? C3 C4 C9 125.3(4) . . ? C5 C4 Y1 74.7(2) . . ? C3 C4 Y1 76.4(2) . . ? C9 C4 Y1 122.0(2) . . ? C1 C5 C4 108.1(3) . . ? C1 C5 C10 126.4(4) . . ? C4 C5 C10 125.0(4) . . ? C1 C5 Y1 75.9(2) . . ? C4 C5 Y1 74.9(2) . . ? C10 C5 Y1 121.4(3) . . ? N1 C11 C12 110.9(3) . . ? N1 C13 C14 116.2(3) . . ? N2 C21 C22 112.2(3) . . ? N2 C23 C24 115.2(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.95 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.446 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.106 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 716019' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 Ho2 N4 O4' _chemical_formula_weight 952.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1189(16) _cell_length_b 13.0204(15) _cell_length_c 21.678(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3985.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour pink _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 3.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5509 _exptl_absorpt_correction_T_max 0.7412 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.650853 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43594 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.02 _reflns_number_total 5813 _reflns_number_gt 5291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+7.0114P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5813 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.269 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 1.007596(8) 0.521427(10) 0.083765(6) 0.01369(4) Uani 1 1 d . . . C1 C 1.1004(2) 0.4813(3) 0.19075(14) 0.0207(6) Uani 1 1 d . . . C2 C 1.0026(2) 0.4757(2) 0.20637(15) 0.0211(6) Uani 1 1 d . . . C3 C 0.9625(2) 0.3896(2) 0.17632(13) 0.0185(6) Uani 1 1 d . . . C4 C 1.0351(2) 0.3416(2) 0.14159(14) 0.0204(6) Uani 1 1 d . . . C5 C 1.1198(2) 0.3980(3) 0.15050(14) 0.0202(6) Uani 1 1 d . . . C6 C 1.1717(3) 0.5557(3) 0.21520(17) 0.0311(8) Uani 1 1 d . . . H6A H 1.1890 0.6046 0.1827 0.047 Uiso 1 1 calc R . . H6B H 1.2284 0.5184 0.2286 0.047 Uiso 1 1 calc R . . H6C H 1.1447 0.5930 0.2503 0.047 Uiso 1 1 calc R . . C7 C 0.9524(3) 0.5354(3) 0.25668(17) 0.0335(8) Uani 1 1 d . . . H7A H 0.9955 0.5873 0.2736 0.050 Uiso 1 1 calc R . . H7B H 0.9329 0.4882 0.2896 0.050 Uiso 1 1 calc R . . H7C H 0.8964 0.5693 0.2394 0.050 Uiso 1 1 calc R . . C8 C 0.8653(2) 0.3468(3) 0.18871(16) 0.0278(7) Uani 1 1 d . . . H8A H 0.8661 0.3082 0.2275 0.042 Uiso 1 1 calc R . . H8B H 0.8470 0.3010 0.1549 0.042 Uiso 1 1 calc R . . H8C H 0.8197 0.4033 0.1918 0.042 Uiso 1 1 calc R . . C9 C 1.0268(3) 0.2409(3) 0.10870(16) 0.0297(8) Uani 1 1 d . . . H9A H 1.0813 0.2318 0.0813 0.045 Uiso 1 1 calc R . . H9B H 0.9683 0.2400 0.0844 0.045 Uiso 1 1 calc R . . H9C H 1.0253 0.1850 0.1390 0.045 Uiso 1 1 calc R . . C10 C 1.2163(2) 0.3664(3) 0.12791(18) 0.0314(8) Uani 1 1 d . . . H10A H 1.2382 0.3067 0.1515 0.047 Uiso 1 1 calc R . . H10B H 1.2608 0.4234 0.1335 0.047 Uiso 1 1 calc R . . H10C H 1.2127 0.3484 0.0841 0.047 Uiso 1 1 calc R . . C11 C 0.7729(2) 0.5856(3) 0.05465(15) 0.0216(6) Uani 1 1 d . . . H11A H 0.7350 0.5906 0.0164 0.026 Uiso 1 1 calc R . . H11B H 0.8044 0.6526 0.0614 0.026 Uiso 1 1 calc R . . C12 C 0.7079(3) 0.5627(3) 0.10851(18) 0.0356(9) Uani 1 1 d . . . H12A H 0.6701 0.5014 0.0993 0.053 Uiso 1 1 calc R . . H12B H 0.6656 0.6213 0.1154 0.053 Uiso 1 1 calc R . . H12C H 0.7458 0.5506 0.1457 0.053 Uiso 1 1 calc R . . C13 C 0.8057(2) 0.4038(2) 0.03109(15) 0.0210(6) Uani 1 1 d . . . H13A H 0.7703 0.3774 0.0672 0.025 Uiso 1 1 calc R . . H13B H 0.8591 0.3561 0.0235 0.025 Uiso 1 1 calc R . . C14 C 0.7406(2) 0.4008(3) -0.02445(16) 0.0279(7) Uani 1 1 d . . . H14A H 0.6814 0.4364 -0.0146 0.042 Uiso 1 1 calc R . . H14B H 0.7269 0.3292 -0.0352 0.042 Uiso 1 1 calc R . . H14C H 0.7714 0.4348 -0.0594 0.042 Uiso 1 1 calc R . . C21 C 0.9943(2) 0.7506(3) 0.16778(15) 0.0251(7) Uani 1 1 d . . . H21A H 1.0374 0.8104 0.1656 0.030 Uiso 1 1 calc R . . H21B H 1.0218 0.7005 0.1971 0.030 Uiso 1 1 calc R . . C22 C 0.8989(3) 0.7853(3) 0.19151(17) 0.0333(8) Uani 1 1 d . . . H22A H 0.8784 0.8463 0.1686 0.050 Uiso 1 1 calc R . . H22B H 0.9039 0.8021 0.2355 0.050 Uiso 1 1 calc R . . H22C H 0.8525 0.7301 0.1858 0.050 Uiso 1 1 calc R . . C23 C 0.9571(2) 0.7764(2) 0.05838(15) 0.0221(6) Uani 1 1 d . . . H23A H 0.8938 0.8030 0.0697 0.026 Uiso 1 1 calc R . . H23B H 0.9505 0.7394 0.0187 0.026 Uiso 1 1 calc R . . C24 C 1.0235(3) 0.8675(3) 0.04864(19) 0.0334(8) Uani 1 1 d . . . H24A H 1.0202 0.9133 0.0845 0.050 Uiso 1 1 calc R . . H24B H 1.0044 0.9052 0.0115 0.050 Uiso 1 1 calc R . . H24C H 1.0886 0.8426 0.0437 0.050 Uiso 1 1 calc R . . N1 N 0.84531(17) 0.50505(19) 0.04733(11) 0.0152(5) Uani 1 1 d . . . N2 N 0.98730(17) 0.70265(19) 0.10585(12) 0.0166(5) Uani 1 1 d . . . O1 O 0.90896(14) 0.53846(16) -0.00118(9) 0.0159(4) Uani 1 1 d . . . O2 O 1.08023(15) 0.66584(17) 0.08917(11) 0.0211(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01417(6) 0.01467(7) 0.01224(7) -0.00046(5) -0.00075(4) 0.00047(5) C1 0.0247(15) 0.0232(15) 0.0141(14) 0.0020(12) -0.0048(11) 0.0003(13) C2 0.0262(16) 0.0214(15) 0.0156(14) 0.0018(11) -0.0014(11) 0.0037(13) C3 0.0226(14) 0.0213(15) 0.0117(13) 0.0033(11) -0.0006(11) 0.0021(12) C4 0.0267(15) 0.0200(15) 0.0144(13) 0.0033(11) 0.0021(12) 0.0036(12) C5 0.0234(15) 0.0221(15) 0.0152(14) 0.0061(12) 0.0003(11) 0.0050(12) C6 0.0317(18) 0.0332(19) 0.0283(18) -0.0008(16) -0.0134(14) -0.0031(15) C7 0.052(2) 0.0264(18) 0.0222(17) -0.0019(14) 0.0077(16) 0.0061(16) C8 0.0299(17) 0.0282(18) 0.0254(17) 0.0085(14) 0.0035(14) -0.0024(14) C9 0.053(2) 0.0166(15) 0.0195(15) 0.0005(12) 0.0022(15) 0.0055(15) C10 0.0253(17) 0.036(2) 0.0332(19) 0.0109(16) 0.0046(14) 0.0125(15) C11 0.0176(14) 0.0240(16) 0.0232(16) -0.0006(12) 0.0028(11) 0.0036(12) C12 0.0333(19) 0.038(2) 0.036(2) -0.0011(17) 0.0178(16) 0.0086(16) C13 0.0219(15) 0.0176(14) 0.0236(16) 0.0000(12) 0.0003(12) -0.0039(11) C14 0.0222(16) 0.0312(18) 0.0304(18) -0.0072(15) -0.0039(13) -0.0068(13) C21 0.0312(17) 0.0222(15) 0.0218(16) -0.0067(12) -0.0057(14) 0.0007(14) C22 0.043(2) 0.034(2) 0.0229(17) -0.0106(15) 0.0005(15) 0.0115(16) C23 0.0261(16) 0.0190(15) 0.0211(15) -0.0001(12) -0.0044(12) 0.0001(12) C24 0.044(2) 0.0193(16) 0.037(2) 0.0050(15) -0.0033(17) -0.0036(15) N1 0.0168(11) 0.0150(12) 0.0139(12) 0.0008(9) 0.0033(9) -0.0009(9) N2 0.0174(12) 0.0142(11) 0.0182(12) -0.0009(9) -0.0030(9) 0.0017(9) O1 0.0137(9) 0.0211(10) 0.0129(10) 0.0011(8) 0.0020(7) -0.0002(8) O2 0.0183(10) 0.0182(11) 0.0269(12) -0.0042(9) 0.0012(9) 0.0016(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 Ho1 O2 2.145(2) . ? Ho1 O1 2.281(2) 5_765 ? Ho1 O1 2.319(2) . ? Ho1 N2 2.425(2) . ? Ho1 N1 2.433(2) . ? Ho1 C5 2.681(3) . ? Ho1 C4 2.685(3) . ? Ho1 C1 2.714(3) . ? Ho1 C3 2.716(3) . ? Ho1 C2 2.724(3) . ? Ho1 Ho1 3.6806(5) 5_765 ? C1 C5 1.418(4) . ? C1 C2 1.423(4) . ? C1 C6 1.496(5) . ? C2 C3 1.415(4) . ? C2 C7 1.515(5) . ? C3 C4 1.418(4) . ? C3 C8 1.505(4) . ? C4 C5 1.417(5) . ? C4 C9 1.497(5) . ? C5 C10 1.505(4) . ? C11 N1 1.473(4) . ? C11 C12 1.515(5) . ? C13 N1 1.474(4) . ? C13 C14 1.516(5) . ? C21 N2 1.484(4) . ? C21 C22 1.510(5) . ? C23 N2 1.471(4) . ? C23 C24 1.526(5) . ? N1 O1 1.450(3) . ? N2 O2 1.443(3) . ? O1 Ho1 2.281(2) 5_765 ? 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 O2 Ho1 O1 95.49(8) . 5_765 ? O2 Ho1 O1 104.28(8) . . ? O1 Ho1 O1 73.72(8) 5_765 . ? O2 Ho1 N2 36.16(8) . . ? O1 Ho1 N2 123.29(8) 5_765 . ? O1 Ho1 N2 89.59(8) . . ? O2 Ho1 N1 123.01(8) . . ? O1 Ho1 N1 101.64(8) 5_765 . ? O1 Ho1 N1 35.43(7) . . ? N2 Ho1 N1 92.18(8) . . ? O2 Ho1 C5 102.32(9) . . ? O1 Ho1 C5 85.03(8) 5_765 . ? O1 Ho1 C5 147.21(9) . . ? N2 Ho1 C5 123.14(9) . . ? N1 Ho1 C5 132.79(9) . . ? O2 Ho1 C4 132.07(9) . . ? O1 Ho1 C4 89.63(8) 5_765 . ? O1 Ho1 C4 122.75(9) . . ? N2 Ho1 C4 140.70(9) . . ? N1 Ho1 C4 102.21(9) . . ? C5 Ho1 C4 30.63(10) . . ? O2 Ho1 C1 83.77(9) . . ? O1 Ho1 C1 110.83(9) 5_765 . ? O1 Ho1 C1 170.58(8) . . ? N2 Ho1 C1 94.35(9) . . ? N1 Ho1 C1 135.64(9) . . ? C5 Ho1 C1 30.48(10) . . ? C4 Ho1 C1 50.44(10) . . ? O2 Ho1 C3 128.73(9) . . ? O1 Ho1 C3 119.01(8) 5_765 . ? O1 Ho1 C3 120.41(8) . . ? N2 Ho1 C3 116.19(9) . . ? N1 Ho1 C3 87.92(9) . . ? C5 Ho1 C3 50.29(9) . . ? C4 Ho1 C3 30.43(9) . . ? C1 Ho1 C3 50.22(9) . . ? O2 Ho1 C2 98.66(9) . . ? O1 Ho1 C2 134.79(8) 5_765 . ? O1 Ho1 C2 141.24(8) . . ? N2 Ho1 C2 90.96(9) . . ? N1 Ho1 C2 105.85(9) . . ? C5 Ho1 C2 50.05(9) . . ? C4 Ho1 C2 50.04(9) . . ? C1 Ho1 C2 30.33(9) . . ? C3 Ho1 C2 30.14(9) . . ? O2 Ho1 Ho1 102.40(6) . 5_765 ? O1 Ho1 Ho1 37.22(5) 5_765 5_765 ? O1 Ho1 Ho1 36.50(5) . 5_765 ? N2 Ho1 Ho1 109.60(6) . 5_765 ? N1 Ho1 Ho1 67.14(6) . 5_765 ? C5 Ho1 Ho1 118.43(7) . 5_765 ? C4 Ho1 Ho1 109.69(7) . 5_765 ? C1 Ho1 Ho1 147.35(7) . 5_765 ? C3 Ho1 Ho1 128.28(7) . 5_765 ? C2 Ho1 Ho1 158.11(7) . 5_765 ? C5 C1 C2 107.2(3) . . ? C5 C1 C6 125.6(3) . . ? C2 C1 C6 127.0(3) . . ? C5 C1 Ho1 73.45(17) . . ? C2 C1 Ho1 75.23(18) . . ? C6 C1 Ho1 120.2(2) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 C7 123.4(3) . . ? C1 C2 C7 126.8(3) . . ? C3 C2 Ho1 74.59(17) . . ? C1 C2 Ho1 74.43(18) . . ? C7 C2 Ho1 127.0(2) . . ? C2 C3 C4 107.8(3) . . ? C2 C3 C8 125.2(3) . . ? C4 C3 C8 126.2(3) . . ? C2 C3 Ho1 75.27(18) . . ? C4 C3 Ho1 73.57(17) . . ? C8 C3 Ho1 125.4(2) . . ? C5 C4 C3 108.0(3) . . ? C5 C4 C9 125.8(3) . . ? C3 C4 C9 125.6(3) . . ? C5 C4 Ho1 74.52(17) . . ? C3 C4 Ho1 76.00(17) . . ? C9 C4 Ho1 122.0(2) . . ? C4 C5 C1 108.5(3) . . ? C4 C5 C10 125.3(3) . . ? C1 C5 C10 125.8(3) . . ? C4 C5 Ho1 74.85(17) . . ? C1 C5 Ho1 76.07(17) . . ? C10 C5 Ho1 121.6(2) . . ? N1 C11 C12 111.3(3) . . ? N1 C13 C14 116.3(3) . . ? N2 C21 C22 112.0(3) . . ? N2 C23 C24 115.3(3) . . ? O1 N1 C11 107.1(2) . . ? O1 N1 C13 109.3(2) . . ? C11 N1 C13 113.5(2) . . ? O1 N1 Ho1 68.01(12) . . ? C11 N1 Ho1 123.79(19) . . ? C13 N1 Ho1 120.85(18) . . ? O2 N2 C23 107.7(2) . . ? O2 N2 C21 107.8(2) . . ? C23 N2 C21 112.2(2) . . ? O2 N2 Ho1 61.30(12) . . ? C23 N2 Ho1 122.11(19) . . ? C21 N2 Ho1 125.5(2) . . ? N1 O1 Ho1 141.89(16) . 5_765 ? N1 O1 Ho1 76.57(13) . . ? Ho1 O1 Ho1 106.28(8) 5_765 . ? N2 O2 Ho1 82.53(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.898 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.125 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 716020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 Er2 N4 O4' _chemical_formula_weight 957.48 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1031(16) _cell_length_b 13.0115(15) _cell_length_c 21.635(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3970.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transaprent prism' _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 4.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4294 _exptl_absorpt_correction_T_max 0.5327 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.771340 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43421 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.05 _reflns_number_total 5807 _reflns_number_gt 4696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+7.1468P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5807 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 1.007627(7) 0.521337(9) 0.083443(6) 0.01251(4) Uani 1 1 d . . . C1 C 1.0998(2) 0.4810(3) 0.19031(14) 0.0202(6) Uani 1 1 d . . . C2 C 1.0020(2) 0.4759(2) 0.20598(14) 0.0202(6) Uani 1 1 d . . . C3 C 0.9621(2) 0.3896(2) 0.17599(14) 0.0189(6) Uani 1 1 d . . . C4 C 1.0344(2) 0.3416(2) 0.14081(13) 0.0189(6) Uani 1 1 d . . . C5 C 1.1190(2) 0.3979(2) 0.14978(14) 0.0189(6) Uani 1 1 d . . . C6 C 1.1716(2) 0.5553(3) 0.21478(17) 0.0298(8) Uani 1 1 d . . . H6A H 1.1885 0.6046 0.1823 0.045 Uiso 1 1 calc R . . H6B H 1.2284 0.5178 0.2278 0.045 Uiso 1 1 calc R . . H6C H 1.1449 0.5922 0.2502 0.045 Uiso 1 1 calc R . . C7 C 0.9525(3) 0.5357(3) 0.25639(16) 0.0322(8) Uani 1 1 d . . . H7A H 0.9967 0.5857 0.2742 0.048 Uiso 1 1 calc R . . H7B H 0.9310 0.4884 0.2887 0.048 Uiso 1 1 calc R . . H7C H 0.8978 0.5719 0.2389 0.048 Uiso 1 1 calc R . . C8 C 0.8649(2) 0.3470(3) 0.18862(16) 0.0257(7) Uani 1 1 d . . . H8A H 0.8652 0.3104 0.2282 0.039 Uiso 1 1 calc R . . H8B H 0.8471 0.2993 0.1555 0.039 Uiso 1 1 calc R . . H8C H 0.8189 0.4034 0.1904 0.039 Uiso 1 1 calc R . . C9 C 1.0261(3) 0.2411(3) 0.10825(16) 0.0283(7) Uani 1 1 d . . . H9A H 1.0824 0.2300 0.0826 0.042 Uiso 1 1 calc R . . H9B H 0.9694 0.2416 0.0820 0.042 Uiso 1 1 calc R . . H9C H 1.0208 0.1857 0.1387 0.042 Uiso 1 1 calc R . . C10 C 1.2159(2) 0.3659(3) 0.12728(17) 0.0298(8) Uani 1 1 d . . . H10A H 1.2381 0.3069 0.1514 0.045 Uiso 1 1 calc R . . H10B H 1.2604 0.4232 0.1323 0.045 Uiso 1 1 calc R . . H10C H 1.2122 0.3470 0.0835 0.045 Uiso 1 1 calc R . . C11 C 0.7733(2) 0.5857(2) 0.05493(15) 0.0203(6) Uani 1 1 d . . . H11A H 0.7350 0.5904 0.0167 0.024 Uiso 1 1 calc R . . H11B H 0.8046 0.6530 0.0615 0.024 Uiso 1 1 calc R . . C12 C 0.7087(2) 0.5630(3) 0.10903(17) 0.0342(8) Uani 1 1 d . . . H12A H 0.6716 0.5011 0.1003 0.051 Uiso 1 1 calc R . . H12B H 0.6658 0.6212 0.1156 0.051 Uiso 1 1 calc R . . H12C H 0.7470 0.5520 0.1463 0.051 Uiso 1 1 calc R . . C13 C 0.8062(2) 0.4040(2) 0.03113(15) 0.0202(6) Uani 1 1 d . . . H13A H 0.7707 0.3777 0.0673 0.024 Uiso 1 1 calc R . . H13B H 0.8595 0.3561 0.0235 0.024 Uiso 1 1 calc R . . C14 C 0.7410(2) 0.4014(3) -0.02462(15) 0.0261(7) Uani 1 1 d . . . H14A H 0.6808 0.4348 -0.0143 0.039 Uiso 1 1 calc R . . H14B H 0.7290 0.3298 -0.0365 0.039 Uiso 1 1 calc R . . H14C H 0.7710 0.4377 -0.0591 0.039 Uiso 1 1 calc R . . C21 C 0.9947(2) 0.7500(2) 0.16778(15) 0.0230(6) Uani 1 1 d . . . H21A H 1.0379 0.8098 0.1654 0.028 Uiso 1 1 calc R . . H21B H 1.0224 0.6999 0.1971 0.028 Uiso 1 1 calc R . . C22 C 0.8992(3) 0.7851(3) 0.19182(16) 0.0310(8) Uani 1 1 d . . . H22A H 0.8791 0.8467 0.1693 0.046 Uiso 1 1 calc R . . H22B H 0.9043 0.8010 0.2360 0.046 Uiso 1 1 calc R . . H22C H 0.8525 0.7303 0.1858 0.046 Uiso 1 1 calc R . . C23 C 0.9571(2) 0.7760(2) 0.05862(15) 0.0200(6) Uani 1 1 d . . . H23A H 0.8939 0.8030 0.0702 0.024 Uiso 1 1 calc R . . H23B H 0.9500 0.7392 0.0188 0.024 Uiso 1 1 calc R . . C24 C 1.0237(3) 0.8668(3) 0.04874(18) 0.0343(8) Uani 1 1 d . . . H24A H 1.0202 0.9130 0.0844 0.051 Uiso 1 1 calc R . . H24B H 1.0050 0.9041 0.0113 0.051 Uiso 1 1 calc R . . H24C H 1.0888 0.8417 0.0441 0.051 Uiso 1 1 calc R . . N1 N 0.84606(16) 0.50551(18) 0.04741(11) 0.0146(5) Uani 1 1 d . . . N2 N 0.98709(16) 0.70184(19) 0.10580(12) 0.0161(5) Uani 1 1 d . . . O1 O 0.90947(13) 0.53897(15) -0.00128(9) 0.0139(4) Uani 1 1 d . . . O2 O 1.08014(14) 0.66516(16) 0.08887(10) 0.0197(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01339(6) 0.01362(6) 0.01050(6) -0.00038(5) -0.00075(4) 0.00051(4) C1 0.0245(14) 0.0228(16) 0.0134(14) 0.0021(13) -0.0051(11) 0.0011(13) C2 0.0261(15) 0.0200(14) 0.0145(13) 0.0017(11) -0.0008(11) 0.0055(13) C3 0.0220(14) 0.0218(16) 0.0131(14) 0.0039(12) 0.0010(11) 0.0013(12) C4 0.0265(14) 0.0183(15) 0.0118(13) 0.0039(11) 0.0024(11) 0.0024(12) C5 0.0215(14) 0.0215(16) 0.0137(14) 0.0069(12) -0.0011(11) 0.0062(12) C6 0.0292(17) 0.0319(19) 0.0283(19) 0.0008(16) -0.0112(14) -0.0036(14) C7 0.048(2) 0.029(2) 0.0189(17) -0.0018(14) 0.0056(15) 0.0068(15) C8 0.0266(16) 0.0266(18) 0.0239(17) 0.0083(14) 0.0034(13) -0.0040(13) C9 0.050(2) 0.0170(16) 0.0184(16) 0.0018(13) 0.0022(15) 0.0035(15) C10 0.0248(16) 0.034(2) 0.0305(19) 0.0089(16) 0.0042(14) 0.0117(14) C11 0.0169(13) 0.0235(17) 0.0205(15) -0.0010(13) 0.0012(11) 0.0037(11) C12 0.0315(18) 0.036(2) 0.035(2) -0.0005(17) 0.0171(15) 0.0087(16) C13 0.0222(14) 0.0158(15) 0.0225(16) -0.0006(12) 0.0006(12) -0.0026(11) C14 0.0236(15) 0.0292(18) 0.0255(17) -0.0063(14) -0.0020(13) -0.0069(13) C21 0.0311(16) 0.0199(14) 0.0180(14) -0.0054(11) -0.0062(14) -0.0026(14) C22 0.041(2) 0.030(2) 0.0226(18) -0.0069(15) 0.0003(15) 0.0087(15) C23 0.0239(14) 0.0169(15) 0.0193(15) 0.0016(12) -0.0015(12) 0.0009(12) C24 0.043(2) 0.0224(18) 0.038(2) 0.0072(15) -0.0030(16) -0.0032(15) N1 0.0145(10) 0.0156(13) 0.0138(12) 0.0006(9) 0.0026(9) -0.0016(9) N2 0.0173(11) 0.0142(12) 0.0166(12) -0.0021(9) -0.0028(9) 0.0023(9) O1 0.0138(9) 0.0170(10) 0.0110(10) 0.0006(8) 0.0019(7) -0.0004(7) O2 0.0168(9) 0.0175(11) 0.0248(12) -0.0028(9) 0.0023(9) 0.0009(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 Er1 O2 2.136(2) . ? Er1 O1 2.2677(19) 5_765 ? Er1 O1 2.3084(19) . ? Er1 N2 2.415(2) . ? Er1 N1 2.417(2) . ? Er1 C5 2.666(3) . ? Er1 C4 2.674(3) . ? Er1 C1 2.704(3) . ? Er1 C3 2.713(3) . ? Er1 C2 2.717(3) . ? Er1 Er1 3.6593(5) 5_765 ? C1 C5 1.418(4) . ? C1 C2 1.422(4) . ? C1 C6 1.496(4) . ? C2 C3 1.413(4) . ? C2 C7 1.511(4) . ? C3 C4 1.418(4) . ? C3 C8 1.504(4) . ? C4 C5 1.413(4) . ? C4 C9 1.490(4) . ? C5 C10 1.509(4) . ? C11 N1 1.473(4) . ? C11 C12 1.512(4) . ? C13 N1 1.478(4) . ? C13 C14 1.518(4) . ? C21 N2 1.484(4) . ? C21 C22 1.513(4) . ? C23 N2 1.467(4) . ? C23 C24 1.524(5) . ? N1 O1 1.449(3) . ? N2 O2 1.444(3) . ? O1 Er1 2.2677(19) 5_765 ? 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 O2 Er1 O1 95.70(7) . 5_765 ? O2 Er1 O1 104.10(8) . . ? O1 Er1 O1 73.81(8) 5_765 . ? O2 Er1 N2 36.33(7) . . ? O1 Er1 N2 123.73(8) 5_765 . ? O1 Er1 N2 89.45(8) . . ? O2 Er1 N1 122.94(8) . . ? O1 Er1 N1 101.76(7) 5_765 . ? O1 Er1 N1 35.61(7) . . ? N2 Er1 N1 91.97(8) . . ? O2 Er1 C5 102.48(9) . . ? O1 Er1 C5 84.82(8) 5_765 . ? O1 Er1 C5 147.22(9) . . ? N2 Er1 C5 123.28(9) . . ? N1 Er1 C5 132.67(9) . . ? O2 Er1 C4 132.29(9) . . ? O1 Er1 C4 89.33(8) 5_765 . ? O1 Er1 C4 122.70(8) . . ? N2 Er1 C4 140.74(9) . . ? N1 Er1 C4 102.03(9) . . ? C5 Er1 C4 30.68(9) . . ? O2 Er1 C1 83.85(9) . . ? O1 Er1 C1 110.81(8) 5_765 . ? O1 Er1 C1 170.60(8) . . ? N2 Er1 C1 94.31(9) . . ? N1 Er1 C1 135.44(9) . . ? C5 Er1 C1 30.62(9) . . ? C4 Er1 C1 50.61(10) . . ? O2 Er1 C3 128.78(9) . . ? O1 Er1 C3 118.82(8) 5_765 . ? O1 Er1 C3 120.46(8) . . ? N2 Er1 C3 115.99(9) . . ? N1 Er1 C3 87.77(9) . . ? C5 Er1 C3 50.32(9) . . ? C4 Er1 C3 30.51(9) . . ? C1 Er1 C3 50.21(9) . . ? O2 Er1 C2 98.70(9) . . ? O1 Er1 C2 134.79(8) 5_765 . ? O1 Er1 C2 141.14(8) . . ? N2 Er1 C2 90.74(9) . . ? N1 Er1 C2 105.57(8) . . ? C5 Er1 C2 50.27(9) . . ? C4 Er1 C2 50.28(9) . . ? C1 Er1 C2 30.42(9) . . ? C3 Er1 C2 30.16(9) . . ? O2 Er1 Er1 102.43(6) . 5_765 ? O1 Er1 Er1 37.29(5) 5_765 5_765 ? O1 Er1 Er1 36.52(5) . 5_765 ? N2 Er1 Er1 109.76(6) . 5_765 ? N1 Er1 Er1 67.26(6) . 5_765 ? C5 Er1 Er1 118.32(7) . 5_765 ? C4 Er1 Er1 109.49(7) . 5_765 ? C1 Er1 Er1 147.41(7) . 5_765 ? C3 Er1 Er1 128.21(7) . 5_765 ? C2 Er1 Er1 158.09(7) . 5_765 ? C5 C1 C2 107.3(3) . . ? C5 C1 C6 125.6(3) . . ? C2 C1 C6 127.0(3) . . ? C5 C1 Er1 73.21(16) . . ? C2 C1 Er1 75.32(17) . . ? C6 C1 Er1 120.2(2) . . ? C3 C2 C1 108.3(3) . . ? C3 C2 C7 123.9(3) . . ? C1 C2 C7 126.6(3) . . ? C3 C2 Er1 74.73(17) . . ? C1 C2 Er1 74.26(17) . . ? C7 C2 Er1 127.3(2) . . ? C2 C3 C4 108.0(3) . . ? C2 C3 C8 124.9(3) . . ? C4 C3 C8 126.2(3) . . ? C2 C3 Er1 75.10(17) . . ? C4 C3 Er1 73.24(16) . . ? C8 C3 Er1 125.7(2) . . ? C5 C4 C3 107.8(3) . . ? C5 C4 C9 125.9(3) . . ? C3 C4 C9 125.7(3) . . ? C5 C4 Er1 74.33(17) . . ? C3 C4 Er1 76.25(17) . . ? C9 C4 Er1 122.5(2) . . ? C4 C5 C1 108.6(3) . . ? C4 C5 C10 125.3(3) . . ? C1 C5 C10 125.6(3) . . ? C4 C5 Er1 74.98(17) . . ? C1 C5 Er1 76.17(17) . . ? C10 C5 Er1 121.7(2) . . ? N1 C11 C12 111.5(3) . . ? N1 C13 C14 116.1(3) . . ? N2 C21 C22 111.9(2) . . ? N2 C23 C24 115.5(3) . . ? O1 N1 C11 107.3(2) . . ? O1 N1 C13 109.3(2) . . ? C11 N1 C13 113.3(2) . . ? O1 N1 Er1 68.10(11) . . ? C11 N1 Er1 124.12(18) . . ? C13 N1 Er1 120.75(18) . . ? O2 N2 C23 107.6(2) . . ? O2 N2 C21 107.7(2) . . ? C23 N2 C21 111.8(2) . . ? O2 N2 Er1 61.23(12) . . ? C23 N2 Er1 122.36(19) . . ? C21 N2 Er1 125.67(19) . . ? N1 O1 Er1 141.65(15) . 5_765 ? N1 O1 Er1 76.29(12) . . ? Er1 O1 Er1 106.19(8) 5_765 . ? N2 O2 Er1 82.43(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.884 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.134 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 716021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 Lu2 N4 O4' _chemical_formula_weight 972.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.0760(18) _cell_length_b 13.0027(16) _cell_length_c 21.513(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3937.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 5.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3911 _exptl_absorpt_correction_T_max 0.7199 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.601995 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43008 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5750 _reflns_number_gt 4742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+5.7459P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5750 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 1.006982(7) 0.521448(8) 0.082801(5) 0.01319(4) Uani 1 1 d . . . C1 C 1.0984(2) 0.4818(2) 0.18876(14) 0.0200(6) Uani 1 1 d . . . C2 C 1.00080(19) 0.4772(2) 0.20451(15) 0.0206(6) Uani 1 1 d . . . C3 C 0.9601(2) 0.3913(2) 0.17462(13) 0.0190(6) Uani 1 1 d . . . C4 C 1.0325(2) 0.3426(2) 0.13918(13) 0.0192(6) Uani 1 1 d . . . C5 C 1.1183(2) 0.3984(2) 0.14819(13) 0.0192(6) Uani 1 1 d . . . C6 C 1.1712(2) 0.5552(3) 0.21379(16) 0.0302(7) Uani 1 1 d . . . H6A H 1.1453 0.5907 0.2502 0.045 Uiso 1 1 calc R . . H6B H 1.1874 0.6057 0.1817 0.045 Uiso 1 1 calc R . . H6C H 1.2283 0.5170 0.2258 0.045 Uiso 1 1 calc R . . C7 C 0.9513(3) 0.5358(3) 0.25601(16) 0.0311(7) Uani 1 1 d . . . H7A H 0.8953 0.5709 0.2391 0.047 Uiso 1 1 calc R . . H7B H 0.9950 0.5868 0.2736 0.047 Uiso 1 1 calc R . . H7C H 0.9315 0.4878 0.2886 0.047 Uiso 1 1 calc R . . C8 C 0.8631(2) 0.3477(3) 0.18776(15) 0.0254(7) Uani 1 1 d . . . H8A H 0.8634 0.3136 0.2284 0.038 Uiso 1 1 calc R . . H8B H 0.8464 0.2977 0.1555 0.038 Uiso 1 1 calc R . . H8C H 0.8162 0.4034 0.1880 0.038 Uiso 1 1 calc R . . C9 C 1.0238(3) 0.2411(2) 0.10758(16) 0.0280(7) Uani 1 1 d . . . H9A H 1.0200 0.1864 0.1389 0.042 Uiso 1 1 calc R . . H9B H 1.0795 0.2297 0.0811 0.042 Uiso 1 1 calc R . . H9C H 0.9662 0.2403 0.0820 0.042 Uiso 1 1 calc R . . C10 C 1.2145(2) 0.3655(3) 0.12641(17) 0.0321(8) Uani 1 1 d . . . H10A H 1.2595 0.4224 0.1315 0.048 Uiso 1 1 calc R . . H10B H 1.2113 0.3461 0.0824 0.048 Uiso 1 1 calc R . . H10C H 1.2359 0.3064 0.1510 0.048 Uiso 1 1 calc R . . C11 C 0.7745(2) 0.5862(2) 0.05467(14) 0.0199(6) Uani 1 1 d . . . H11A H 0.7359 0.5907 0.0163 0.024 Uiso 1 1 calc R . . H11B H 0.8058 0.6535 0.0612 0.024 Uiso 1 1 calc R . . C12 C 0.7101(3) 0.5627(3) 0.10959(17) 0.0356(8) Uani 1 1 d . . . H12A H 0.6744 0.4994 0.1013 0.053 Uiso 1 1 calc R . . H12B H 0.6656 0.6198 0.1157 0.053 Uiso 1 1 calc R . . H12C H 0.7487 0.5537 0.1471 0.053 Uiso 1 1 calc R . . C13 C 0.8075(2) 0.4042(2) 0.03061(15) 0.0210(6) Uani 1 1 d . . . H13A H 0.7725 0.3772 0.0670 0.025 Uiso 1 1 calc R . . H13B H 0.8608 0.3566 0.0223 0.025 Uiso 1 1 calc R . . C14 C 0.7412(2) 0.4025(3) -0.02502(15) 0.0273(7) Uani 1 1 d . . . H14A H 0.6816 0.4372 -0.0143 0.041 Uiso 1 1 calc R . . H14B H 0.7280 0.3311 -0.0367 0.041 Uiso 1 1 calc R . . H14C H 0.7713 0.4381 -0.0600 0.041 Uiso 1 1 calc R . . C21 C 0.9958(2) 0.7486(2) 0.16788(15) 0.0239(6) Uani 1 1 d . . . H21A H 1.0404 0.8074 0.1651 0.029 Uiso 1 1 calc R . . H21B H 1.0229 0.6980 0.1974 0.029 Uiso 1 1 calc R . . C22 C 0.9012(3) 0.7861(3) 0.19231(16) 0.0330(8) Uani 1 1 d . . . H22A H 0.8824 0.8484 0.1698 0.049 Uiso 1 1 calc R . . H22B H 0.9069 0.8016 0.2367 0.049 Uiso 1 1 calc R . . H22C H 0.8531 0.7326 0.1862 0.049 Uiso 1 1 calc R . . C23 C 0.9563(2) 0.7754(2) 0.05824(15) 0.0214(6) Uani 1 1 d . . . H23A H 0.8929 0.8022 0.0699 0.026 Uiso 1 1 calc R . . H23B H 0.9493 0.7389 0.0181 0.026 Uiso 1 1 calc R . . C24 C 1.0230(3) 0.8661(3) 0.04888(18) 0.0334(8) Uani 1 1 d . . . H24A H 1.0192 0.9119 0.0850 0.050 Uiso 1 1 calc R . . H24B H 1.0044 0.9039 0.0114 0.050 Uiso 1 1 calc R . . H24C H 1.0882 0.8410 0.0443 0.050 Uiso 1 1 calc R . . N1 N 0.84733(16) 0.50564(18) 0.04730(11) 0.0155(5) Uani 1 1 d . . . N2 N 0.98660(16) 0.70029(19) 0.10589(12) 0.0169(5) Uani 1 1 d . . . O1 O 0.91074(13) 0.53999(15) -0.00181(9) 0.0149(4) Uani 1 1 d . . . O2 O 1.07951(14) 0.66312(16) 0.08754(10) 0.0207(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01396(6) 0.01439(6) 0.01122(7) -0.00047(4) -0.00066(4) 0.00052(4) C1 0.0225(14) 0.0231(15) 0.0145(14) 0.0014(12) -0.0054(11) 0.0014(12) C2 0.0244(15) 0.0217(15) 0.0156(15) 0.0010(11) -0.0016(10) 0.0049(12) C3 0.0227(14) 0.0214(14) 0.0128(13) 0.0041(11) 0.0003(10) 0.0007(11) C4 0.0260(14) 0.0186(14) 0.0129(13) 0.0025(11) 0.0025(11) 0.0018(11) C5 0.0206(13) 0.0230(15) 0.0141(14) 0.0059(12) 0.0003(10) 0.0046(11) C6 0.0324(17) 0.0300(17) 0.0284(18) 0.0020(15) -0.0131(14) -0.0026(14) C7 0.045(2) 0.0260(17) 0.0225(17) -0.0020(14) 0.0085(15) 0.0059(13) C8 0.0260(15) 0.0262(17) 0.0238(17) 0.0080(13) 0.0042(12) -0.0029(12) C9 0.0465(19) 0.0194(15) 0.0183(16) 0.0025(13) 0.0027(14) 0.0028(14) C10 0.0271(16) 0.037(2) 0.0323(19) 0.0108(16) 0.0040(14) 0.0128(14) C11 0.0181(13) 0.0233(15) 0.0182(15) 0.0001(12) 0.0014(11) 0.0039(10) C12 0.0358(19) 0.039(2) 0.033(2) 0.0001(17) 0.0161(15) 0.0113(16) C13 0.0217(14) 0.0192(14) 0.0220(16) -0.0011(12) 0.0015(11) -0.0038(11) C14 0.0253(15) 0.0303(17) 0.0262(17) -0.0046(14) -0.0035(13) -0.0077(13) C21 0.0310(16) 0.0212(15) 0.0196(15) -0.0060(12) -0.0063(13) 0.0002(13) C22 0.042(2) 0.0309(19) 0.0261(19) -0.0096(15) 0.0018(15) 0.0105(15) C23 0.0271(15) 0.0167(14) 0.0203(15) 0.0004(12) -0.0045(12) 0.0000(11) C24 0.0412(19) 0.0225(16) 0.037(2) 0.0075(15) -0.0062(16) -0.0066(14) N1 0.0153(11) 0.0168(12) 0.0143(12) -0.0008(9) 0.0026(8) -0.0004(8) N2 0.0168(11) 0.0165(11) 0.0175(12) -0.0021(9) -0.0031(9) 0.0023(9) O1 0.0147(9) 0.0182(9) 0.0119(10) 0.0019(8) 0.0032(7) -0.0004(7) O2 0.0175(9) 0.0192(10) 0.0252(12) -0.0039(9) 0.0016(8) 0.0002(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 Lu1 O2 2.109(2) . ? Lu1 O1 2.2394(18) 5_765 ? Lu1 O1 2.2819(19) . ? Lu1 N1 2.382(2) . ? Lu1 N2 2.395(2) . ? Lu1 C5 2.644(3) . ? Lu1 C4 2.648(3) . ? Lu1 C1 2.668(3) . ? Lu1 C2 2.682(3) . ? Lu1 C3 2.684(3) . ? Lu1 Lu1 3.6114(5) 5_765 ? C1 C2 1.417(4) . ? C1 C5 1.420(4) . ? C1 C6 1.499(4) . ? C2 C3 1.410(4) . ? C2 C7 1.515(4) . ? C3 C4 1.421(4) . ? C3 C8 1.505(4) . ? C4 C5 1.423(4) . ? C4 C9 1.490(4) . ? C5 C10 1.496(4) . ? C11 N1 1.474(3) . ? C11 C12 1.520(4) . ? C13 N1 1.477(4) . ? C13 C14 1.517(4) . ? C21 N2 1.480(4) . ? C21 C22 1.512(4) . ? C23 N2 1.479(4) . ? C23 C24 1.521(4) . ? N1 O1 1.453(3) . ? N2 O2 1.449(3) . ? O1 Lu1 2.2394(18) 5_765 ? 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 O2 Lu1 O1 95.67(7) . 5_765 ? O2 Lu1 O1 103.51(7) . . ? O1 Lu1 O1 73.98(8) 5_765 . ? O2 Lu1 N1 123.20(8) . . ? O1 Lu1 N1 101.98(8) 5_765 . ? O1 Lu1 N1 36.23(7) . . ? O2 Lu1 N2 36.85(7) . . ? O1 Lu1 N2 124.72(8) 5_765 . ? O1 Lu1 N2 89.53(8) . . ? N1 Lu1 N2 92.14(8) . . ? O2 Lu1 C5 102.47(9) . . ? O1 Lu1 C5 83.78(8) 5_765 . ? O1 Lu1 C5 147.14(8) . . ? N1 Lu1 C5 132.63(9) . . ? N2 Lu1 C5 123.23(9) . . ? O2 Lu1 C4 132.83(9) . . ? O1 Lu1 C4 88.45(8) 5_765 . ? O1 Lu1 C4 122.59(8) . . ? N1 Lu1 C4 101.47(9) . . ? N2 Lu1 C4 140.73(9) . . ? C5 Lu1 C4 31.20(9) . . ? O2 Lu1 C1 83.91(9) . . ? O1 Lu1 C1 110.26(8) 5_765 . ? O1 Lu1 C1 171.26(8) . . ? N1 Lu1 C1 135.42(9) . . ? N2 Lu1 C1 93.91(9) . . ? C5 Lu1 C1 31.00(9) . . ? C4 Lu1 C1 51.22(9) . . ? O2 Lu1 C2 98.98(9) . . ? O1 Lu1 C2 134.40(8) 5_765 . ? O1 Lu1 C2 141.46(7) . . ? N1 Lu1 C2 105.30(8) . . ? N2 Lu1 C2 90.12(9) . . ? C5 Lu1 C2 50.95(9) . . ? C4 Lu1 C2 50.85(9) . . ? C1 Lu1 C2 30.71(8) . . ? O2 Lu1 C3 129.38(9) . . ? O1 Lu1 C3 118.35(8) 5_765 . ? O1 Lu1 C3 120.52(8) . . ? N1 Lu1 C3 87.11(8) . . ? N2 Lu1 C3 115.48(9) . . ? C5 Lu1 C3 51.14(9) . . ? C4 Lu1 C3 30.91(9) . . ? C1 Lu1 C3 50.80(9) . . ? C2 Lu1 C3 30.47(9) . . ? O2 Lu1 Lu1 102.06(6) . 5_765 ? O1 Lu1 Lu1 37.40(5) 5_765 5_765 ? O1 Lu1 Lu1 36.59(5) . 5_765 ? N1 Lu1 Lu1 67.61(6) . 5_765 ? N2 Lu1 Lu1 110.36(6) . 5_765 ? C5 Lu1 Lu1 117.62(7) . 5_765 ? C4 Lu1 Lu1 108.88(6) . 5_765 ? C1 Lu1 Lu1 147.06(7) . 5_765 ? C2 Lu1 Lu1 158.13(7) . 5_765 ? C3 Lu1 Lu1 127.98(6) . 5_765 ? C2 C1 C5 107.8(3) . . ? C2 C1 C6 127.1(3) . . ? C5 C1 C6 124.9(3) . . ? C2 C1 Lu1 75.20(17) . . ? C5 C1 Lu1 73.58(16) . . ? C6 C1 Lu1 120.9(2) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 C7 123.0(3) . . ? C1 C2 C7 126.8(3) . . ? C3 C2 Lu1 74.82(18) . . ? C1 C2 Lu1 74.09(17) . . ? C7 C2 Lu1 128.4(2) . . ? C2 C3 C4 107.9(3) . . ? C2 C3 C8 125.5(3) . . ? C4 C3 C8 125.7(3) . . ? C2 C3 Lu1 74.71(18) . . ? C4 C3 Lu1 73.14(16) . . ? C8 C3 Lu1 126.8(2) . . ? C3 C4 C5 107.9(3) . . ? C3 C4 C9 125.5(3) . . ? C5 C4 C9 125.7(3) . . ? C3 C4 Lu1 75.95(16) . . ? C5 C4 Lu1 74.28(16) . . ? C9 C4 Lu1 123.9(2) . . ? C1 C5 C4 107.8(3) . . ? C1 C5 C10 126.1(3) . . ? C4 C5 C10 125.4(3) . . ? C1 C5 Lu1 75.42(16) . . ? C4 C5 Lu1 74.53(16) . . ? C10 C5 Lu1 122.9(2) . . ? N1 C11 C12 110.8(3) . . ? N1 C13 C14 116.0(3) . . ? N2 C21 C22 111.9(2) . . ? N2 C23 C24 115.2(3) . . ? O1 N1 C11 106.7(2) . . ? O1 N1 C13 109.3(2) . . ? C11 N1 C13 113.3(2) . . ? O1 N1 Lu1 68.11(12) . . ? C11 N1 Lu1 124.07(18) . . ? C13 N1 Lu1 120.88(18) . . ? O2 N2 C23 107.0(2) . . ? O2 N2 C21 107.9(2) . . ? C23 N2 C21 111.7(2) . . ? O2 N2 Lu1 60.76(11) . . ? C23 N2 Lu1 122.15(18) . . ? C21 N2 Lu1 126.05(19) . . ? N1 O1 Lu1 140.67(15) . 5_765 ? N1 O1 Lu1 75.65(12) . . ? Lu1 O1 Lu1 106.02(8) 5_765 . ? N2 O2 Lu1 82.39(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.498 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.152