# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dongmei Cui' _publ_contact_author_email DMCUI@CIAC.JL.CN _publ_section_title ; Living Catalyzed-Chain-Growth Polymerization and Block Copolymerization of Isoprene by Rare-Earth Metal Allyl Precursors Bearing CGC Ligand ; loop_ _publ_author_name 'Dongmei Cui.' 'Zhaomin Hou.' 'Zhongbao Jian.' 'Xiaofang Li.' # Attachment 'complexes_1_3_and_4.cif' data_complex1 #CCDC 743541 _database_code_depnum_ccdc_archive 'CCDC 743541' #TrackingRef 'complexes_1_3_and_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 N Y' _chemical_formula_weight 411.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7801(6) _cell_length_b 18.6736(13) _cell_length_c 12.9685(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.4000(10) _cell_angle_gamma 90.00 _cell_volume 2103.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 186.5(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 2.777 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6066 _exptl_absorpt_correction_T_max 0.7882 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186.5(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11647 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4122 _reflns_number_gt 3375 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0429P)^2^+0.8676P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4122 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.27315(3) 0.883957(12) 0.823909(17) 0.02352(9) Uani 1 1 d . . . C5 C 0.2018(4) 0.88687(15) 1.0157(2) 0.0443(7) Uani 1 1 d . . . H5 H 0.1044 0.8868 1.0358 0.053 Uiso 1 1 calc R . . N1 N 0.0396(2) 0.79925(10) 0.75859(15) 0.0261(4) Uani 1 1 d . . . C6 C 0.2611(4) 0.95253(15) 0.9964(2) 0.0432(7) Uani 1 1 d . . . H6A H 0.3581 0.9559 0.9760 0.052 Uiso 1 1 calc R . . H6B H 0.2043 0.9938 1.0036 0.052 Uiso 1 1 calc R . . C16 C -0.0160(3) 0.88189(12) 0.60881(19) 0.0262(5) Uani 1 1 d . . . C7 C 0.1118(3) 0.92975(12) 0.65507(17) 0.0246(5) Uani 1 1 d . . . C14 C 0.2948(3) 1.08118(14) 0.8189(2) 0.0373(6) Uani 1 1 d . . . H14A H 0.3935 1.0732 0.8599 0.056 Uiso 1 1 calc R . . H14B H 0.2190 1.0885 0.8642 0.056 Uiso 1 1 calc R . . H14C H 0.2997 1.1228 0.7761 0.056 Uiso 1 1 calc R . . C8 C 0.2626(3) 0.92886(13) 0.62807(18) 0.0280(5) Uani 1 1 d . . . C12 C 0.3141(4) 0.88455(15) 0.5430(2) 0.0418(7) Uani 1 1 d . . . H12A H 0.2958 0.9104 0.4784 0.063 Uiso 1 1 calc R . . H12B H 0.2575 0.8404 0.5362 0.063 Uiso 1 1 calc R . . H12C H 0.4221 0.8744 0.5599 0.063 Uiso 1 1 calc R . . C3 C 0.5708(3) 0.88197(15) 0.8709(2) 0.0436(7) Uani 1 1 d . . . H3A H 0.5274 0.8738 0.9311 0.052 Uiso 1 1 calc R . . H3B H 0.6344 0.9214 0.8669 0.052 Uiso 1 1 calc R . . C21 C -0.0471(3) 0.81753(12) 0.65612(18) 0.0259(5) Uani 1 1 d . . . C9 C 0.3488(3) 0.98287(13) 0.68738(19) 0.0290(5) Uani 1 1 d . . . C17 C -0.1068(3) 0.90040(14) 0.5151(2) 0.0379(6) Uani 1 1 d . . . H17 H -0.0882 0.9433 0.4828 0.045 Uiso 1 1 calc R . . C23 C -0.0674(3) 0.80916(16) 0.8370(2) 0.0406(7) Uani 1 1 d . . . H23A H -0.0952 0.8588 0.8398 0.061 Uiso 1 1 calc R . . H23B H -0.0174 0.7941 0.9044 0.061 Uiso 1 1 calc R . . H23C H -0.1584 0.7809 0.8174 0.061 Uiso 1 1 calc R . . C10 C 0.2511(3) 1.01699(12) 0.75060(18) 0.0272(5) Uani 1 1 d . . . C11 C 0.1031(3) 0.98506(12) 0.72919(18) 0.0260(5) Uani 1 1 d . . . C19 C -0.2524(3) 0.79292(15) 0.5165(2) 0.0396(6) Uani 1 1 d . . . H19 H -0.3308 0.7630 0.4858 0.048 Uiso 1 1 calc R . . C20 C -0.1646(3) 0.77365(14) 0.6093(2) 0.0363(6) Uani 1 1 d . . . H20 H -0.1846 0.7306 0.6409 0.044 Uiso 1 1 calc R . . C22 C 0.0881(3) 0.72289(13) 0.7626(2) 0.0387(6) Uani 1 1 d . . . H22A H -0.0014 0.6927 0.7564 0.058 Uiso 1 1 calc R . . H22B H 0.1520 0.7135 0.8278 0.058 Uiso 1 1 calc R . . H22C H 0.1448 0.7131 0.7063 0.058 Uiso 1 1 calc R . . C4 C 0.2698(4) 0.82071(16) 1.0089(2) 0.0478(8) Uani 1 1 d . . . H4A H 0.3672 0.8174 0.9892 0.057 Uiso 1 1 calc R . . H4B H 0.2182 0.7794 1.0240 0.057 Uiso 1 1 calc R . . C2 C 0.5406(3) 0.83538(15) 0.7872(2) 0.0398(7) Uani 1 1 d . . . H2 H 0.5869 0.8461 0.7290 0.048 Uiso 1 1 calc R . . C15 C -0.0400(3) 1.00889(14) 0.7706(2) 0.0398(7) Uani 1 1 d . . . H15A H -0.0209 1.0096 0.8454 0.060 Uiso 1 1 calc R . . H15B H -0.1224 0.9762 0.7478 0.060 Uiso 1 1 calc R . . H15C H -0.0680 1.0560 0.7450 0.060 Uiso 1 1 calc R . . C1 C 0.4504(3) 0.77545(16) 0.7807(2) 0.0435(7) Uani 1 1 d . . . H1A H 0.4013 0.7622 0.8366 0.052 Uiso 1 1 calc R . . H1B H 0.4381 0.7479 0.7203 0.052 Uiso 1 1 calc R . . C18 C -0.2239(3) 0.85613(15) 0.4695(2) 0.0406(7) Uani 1 1 d . . . H18 H -0.2832 0.8693 0.4070 0.049 Uiso 1 1 calc R . . C13 C 0.5096(3) 1.00668(16) 0.6765(2) 0.0457(7) Uani 1 1 d . . . H13A H 0.5660 0.9671 0.6537 0.069 Uiso 1 1 calc R . . H13B H 0.5605 1.0235 0.7427 0.069 Uiso 1 1 calc R . . H13C H 0.5049 1.0447 0.6263 0.069 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 0.02523(13) 0.02338(13) 0.02164(13) 0.00003(9) 0.00236(9) 0.00379(9) C5 0.067(2) 0.0484(18) 0.0196(13) -0.0024(12) 0.0136(13) -0.0009(15) N1 0.0292(11) 0.0226(10) 0.0266(10) 0.0057(8) 0.0050(8) -0.0004(8) C6 0.0625(19) 0.0394(16) 0.0297(15) -0.0060(12) 0.0130(13) 0.0041(14) C16 0.0258(12) 0.0253(12) 0.0271(12) 0.0004(10) 0.0027(10) -0.0008(10) C7 0.0270(12) 0.0226(12) 0.0233(12) 0.0059(9) 0.0010(10) -0.0018(9) C14 0.0433(16) 0.0251(13) 0.0412(16) -0.0019(11) -0.0015(13) -0.0017(11) C8 0.0326(13) 0.0278(13) 0.0244(12) 0.0039(10) 0.0069(10) -0.0023(10) C12 0.0521(18) 0.0452(17) 0.0323(15) -0.0055(12) 0.0197(13) -0.0068(13) C3 0.0266(14) 0.0454(17) 0.0563(19) -0.0119(14) -0.0024(13) 0.0071(12) C21 0.0239(12) 0.0250(12) 0.0285(13) 0.0009(10) 0.0035(10) 0.0006(9) C9 0.0265(13) 0.0300(13) 0.0306(13) 0.0064(10) 0.0045(10) -0.0045(10) C17 0.0428(16) 0.0329(15) 0.0351(15) 0.0073(11) -0.0041(12) -0.0067(12) C23 0.0382(16) 0.0483(17) 0.0374(16) 0.0038(13) 0.0129(13) -0.0021(13) C10 0.0297(13) 0.0217(12) 0.0289(13) 0.0031(10) 0.0000(10) -0.0005(10) C11 0.0262(13) 0.0217(12) 0.0295(13) 0.0042(10) 0.0022(10) 0.0037(9) C19 0.0328(14) 0.0381(15) 0.0456(16) -0.0071(13) -0.0026(12) -0.0094(12) C20 0.0389(15) 0.0292(14) 0.0402(16) 0.0031(11) 0.0034(12) -0.0083(11) C22 0.0413(16) 0.0264(14) 0.0462(16) 0.0077(12) -0.0004(13) 0.0018(11) C4 0.072(2) 0.0409(17) 0.0300(15) 0.0081(13) 0.0079(14) 0.0036(15) C2 0.0220(13) 0.0491(17) 0.0476(17) -0.0067(14) 0.0026(12) 0.0145(12) C15 0.0318(15) 0.0328(15) 0.0558(18) -0.0040(13) 0.0099(13) 0.0072(11) C1 0.0324(15) 0.0465(17) 0.0496(18) -0.0151(14) -0.0002(13) 0.0130(13) C18 0.0417(16) 0.0419(16) 0.0334(15) 0.0003(12) -0.0101(12) -0.0045(13) C13 0.0330(15) 0.0471(17) 0.0593(19) 0.0056(14) 0.0139(14) -0.0110(13) _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 C7 2.574(2) . ? Y1 C6 2.593(3) . ? Y1 C3 2.596(3) . ? Y1 C11 2.601(2) . ? Y1 C2 2.625(2) . ? Y1 N1 2.630(2) . ? Y1 C5 2.653(3) . ? Y1 C10 2.657(2) . ? Y1 C8 2.663(2) . ? Y1 C1 2.664(3) . ? Y1 C4 2.678(3) . ? Y1 C9 2.708(2) . ? C5 C6 1.370(4) . ? C5 C4 1.381(4) . ? N1 C21 1.472(3) . ? N1 C22 1.487(3) . ? N1 C23 1.494(3) . ? C16 C21 1.394(3) . ? C16 C17 1.396(4) . ? C16 C7 1.490(3) . ? C7 C8 1.419(3) . ? C7 C11 1.421(3) . ? C14 C10 1.506(3) . ? C8 C9 1.418(3) . ? C8 C12 1.501(3) . ? C3 C2 1.386(4) . ? C21 C20 1.387(3) . ? C9 C10 1.421(3) . ? C9 C13 1.507(3) . ? C17 C18 1.384(4) . ? C10 C11 1.420(3) . ? C11 C15 1.504(3) . ? C19 C18 1.368(4) . ? C19 C20 1.379(4) . ? C2 C1 1.367(4) . ? 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 C7 Y1 C6 118.88(9) . . ? C7 Y1 C3 127.93(9) . . ? C6 Y1 C3 88.34(10) . . ? C7 Y1 C11 31.86(7) . . ? C6 Y1 C11 87.47(9) . . ? C3 Y1 C11 127.59(9) . . ? C7 Y1 C2 110.88(8) . . ? C6 Y1 C2 118.52(10) . . ? C3 Y1 C2 30.79(9) . . ? C11 Y1 C2 129.21(8) . . ? C7 Y1 N1 67.63(7) . . ? C6 Y1 N1 116.53(8) . . ? C3 Y1 N1 141.07(7) . . ? C11 Y1 N1 85.29(7) . . ? C2 Y1 N1 114.19(8) . . ? C7 Y1 C5 127.93(9) . . ? C6 Y1 C5 30.24(9) . . ? C3 Y1 C5 98.49(10) . . ? C11 Y1 C5 103.30(9) . . ? C2 Y1 C5 121.14(10) . . ? N1 Y1 C5 91.98(8) . . ? C7 Y1 C10 51.89(7) . . ? C6 Y1 C10 80.61(8) . . ? C3 Y1 C10 96.64(9) . . ? C11 Y1 C10 31.31(7) . . ? C2 Y1 C10 106.17(9) . . ? N1 Y1 C10 115.76(7) . . ? C5 Y1 C10 107.55(8) . . ? C7 Y1 C8 31.37(7) . . ? C6 Y1 C8 131.84(8) . . ? C3 Y1 C8 97.00(9) . . ? C11 Y1 C8 51.95(7) . . ? C2 Y1 C8 80.98(8) . . ? N1 Y1 C8 88.02(7) . . ? C5 Y1 C8 155.18(9) . . ? C10 Y1 C8 51.23(7) . . ? C7 Y1 C1 109.84(8) . . ? C6 Y1 C1 131.00(9) . . ? C3 Y1 C1 55.91(9) . . ? C11 Y1 C1 139.93(8) . . ? C2 Y1 C1 29.94(9) . . ? N1 Y1 C1 85.79(8) . . ? C5 Y1 C1 115.99(10) . . ? C10 Y1 C1 130.54(9) . . ? C8 Y1 C1 88.77(9) . . ? C7 Y1 C4 146.28(9) . . ? C6 Y1 C4 55.80(9) . . ? C3 Y1 C4 85.74(10) . . ? C11 Y1 C4 131.49(9) . . ? C2 Y1 C4 97.89(10) . . ? N1 Y1 C4 85.02(8) . . ? C5 Y1 C4 30.01(8) . . ? C10 Y1 C4 136.32(8) . . ? C8 Y1 C4 171.77(8) . . ? C1 Y1 C4 86.35(10) . . ? C7 Y1 C9 51.26(7) . . ? C6 Y1 C9 105.79(8) . . ? C3 Y1 C9 80.13(9) . . ? C11 Y1 C9 51.30(8) . . ? C2 Y1 C9 78.80(9) . . ? N1 Y1 C9 116.99(7) . . ? C5 Y1 C9 135.50(8) . . ? C10 Y1 C9 30.70(7) . . ? C8 Y1 C9 30.60(7) . . ? C1 Y1 C9 100.05(9) . . ? C4 Y1 C9 157.30(9) . . ? C6 C5 C4 127.6(3) . . ? C6 C5 Y1 72.45(15) . . ? C4 C5 Y1 75.99(16) . . ? C21 N1 C22 111.21(19) . . ? C21 N1 C23 107.00(18) . . ? C22 N1 C23 107.4(2) . . ? C21 N1 Y1 115.30(13) . . ? C22 N1 Y1 111.10(15) . . ? C23 N1 Y1 104.15(15) . . ? C5 C6 Y1 77.31(16) . . ? C21 C16 C17 118.2(2) . . ? C21 C16 C7 121.6(2) . . ? C17 C16 C7 120.2(2) . . ? C8 C7 C11 108.6(2) . . ? C8 C7 C16 124.7(2) . . ? C11 C7 C16 126.6(2) . . ? C8 C7 Y1 77.78(13) . . ? C11 C7 Y1 75.12(13) . . ? C16 C7 Y1 115.58(15) . . ? C9 C8 C7 107.5(2) . . ? C9 C8 C12 126.6(2) . . ? C7 C8 C12 125.5(2) . . ? C9 C8 Y1 76.43(13) . . ? C7 C8 Y1 70.85(12) . . ? C12 C8 Y1 123.73(17) . . ? C2 C3 Y1 75.78(15) . . ? C20 C21 C16 119.8(2) . . ? C20 C21 N1 120.8(2) . . ? C16 C21 N1 119.2(2) . . ? C8 C9 C10 108.2(2) . . ? C8 C9 C13 126.3(2) . . ? C10 C9 C13 125.1(2) . . ? C8 C9 Y1 72.97(13) . . ? C10 C9 Y1 72.67(13) . . ? C13 C9 Y1 125.82(18) . . ? C18 C17 C16 121.3(2) . . ? C11 C10 C9 108.1(2) . . ? C11 C10 C14 126.6(2) . . ? C9 C10 C14 125.0(2) . . ? C11 C10 Y1 72.19(13) . . ? C9 C10 Y1 76.63(13) . . ? C14 C10 Y1 122.33(16) . . ? C10 C11 C7 107.4(2) . . ? C10 C11 C15 126.5(2) . . ? C7 C11 C15 125.9(2) . . ? C10 C11 Y1 76.50(13) . . ? C7 C11 Y1 73.02(13) . . ? C15 C11 Y1 119.87(16) . . ? C18 C19 C20 119.9(2) . . ? C19 C20 C21 120.9(2) . . ? C5 C4 Y1 74.00(15) . . ? C1 C2 C3 127.3(3) . . ? C1 C2 Y1 76.62(15) . . ? C3 C2 Y1 73.43(15) . . ? C2 C1 Y1 73.45(15) . . ? C19 C18 C17 119.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.356 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.062 #===========END============= data_complex3 #CCDC 743542 _database_code_depnum_ccdc_archive 'CCDC 743542' #TrackingRef 'complexes_1_3_and_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Gd N' _chemical_formula_weight 479.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7876(6) _cell_length_b 18.6815(12) _cell_length_c 13.0273(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.3860(10) _cell_angle_gamma 90.00 _cell_volume 2115.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 186.5(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 3.139 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6174 _exptl_absorpt_correction_T_max 0.7045 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186.5(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11706 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4145 _reflns_number_gt 3707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0290P)^2^+2.9177P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4145 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C4 C 0.2762(7) 0.3217(3) 1.0119(3) 0.0489(13) Uani 1 1 d . . . H4A H 0.2114 0.2797 1.0130 0.059 Uiso 1 1 calc R . . H4B H 0.3761 0.3162 1.0539 0.059 Uiso 1 1 calc R . . C3 C 0.5739(5) 0.3821(3) 0.8690(4) 0.0430(12) Uani 1 1 d . . . H3A H 0.6257 0.4261 0.8551 0.052 Uiso 1 1 calc R . . H3B H 0.6150 0.3610 0.9353 0.052 Uiso 1 1 calc R . . C1 C 0.4542(5) 0.2739(3) 0.7830(4) 0.0448(13) Uani 1 1 d . . . H1A H 0.4814 0.2395 0.8385 0.054 Uiso 1 1 calc R . . H1B H 0.4275 0.2517 0.7155 0.054 Uiso 1 1 calc R . . C6 C 0.2633(6) 0.4528(3) 0.9975(3) 0.0429(12) Uani 1 1 d . . . H6A H 0.3620 0.4648 1.0373 0.052 Uiso 1 1 calc R . . H6B H 0.1910 0.4923 0.9928 0.052 Uiso 1 1 calc R . . Gd1 Gd 0.27539(2) 0.383964(10) 0.825217(14) 0.02283(7) Uani 1 1 d . . . N1 N 0.0428(4) 0.29832(18) 0.7572(3) 0.0268(7) Uani 1 1 d . . . C2 C 0.5451(5) 0.3346(3) 0.7863(4) 0.0425(12) Uani 1 1 d . . . H2 H 0.5910 0.3446 0.7279 0.051 Uiso 1 1 calc R . . C5 C 0.2046(7) 0.3869(3) 1.0190(3) 0.0465(13) Uani 1 1 d . . . H5 H 0.1081 0.3864 1.0403 0.056 Uiso 1 1 calc R . . C7 C 0.1125(4) 0.4298(2) 0.6547(3) 0.0241(8) Uani 1 1 d . . . C8 C 0.2632(5) 0.4295(2) 0.6276(3) 0.0273(9) Uani 1 1 d . . . C9 C 0.3488(5) 0.4836(2) 0.6866(3) 0.0292(9) Uani 1 1 d . . . C10 C 0.2502(5) 0.5173(2) 0.7489(3) 0.0270(9) Uani 1 1 d . . . C11 C 0.1032(4) 0.4854(2) 0.7282(3) 0.0253(9) Uani 1 1 d . . . C12 C 0.3148(6) 0.3845(2) 0.5429(4) 0.0432(12) Uani 1 1 d . . . H12A H 0.2547 0.3415 0.5343 0.065 Uiso 1 1 calc R . . H12B H 0.4215 0.3725 0.5615 0.065 Uiso 1 1 calc R . . H12C H 0.3012 0.4110 0.4791 0.065 Uiso 1 1 calc R . . C13 C 0.5098(5) 0.5078(3) 0.6754(4) 0.0442(12) Uani 1 1 d . . . H13A H 0.5045 0.5462 0.6262 0.066 Uiso 1 1 calc R . . H13B H 0.5657 0.4685 0.6516 0.066 Uiso 1 1 calc R . . H13C H 0.5613 0.5239 0.7414 0.066 Uiso 1 1 calc R . . C14 C 0.2937(5) 0.5816(2) 0.8169(3) 0.0373(10) Uani 1 1 d . . . H14A H 0.2958 0.6234 0.7743 0.056 Uiso 1 1 calc R . . H14B H 0.3936 0.5742 0.8563 0.056 Uiso 1 1 calc R . . H14C H 0.2194 0.5880 0.8633 0.056 Uiso 1 1 calc R . . C15 C -0.0399(5) 0.5090(2) 0.7690(4) 0.0398(11) Uani 1 1 d . . . H15A H -0.0180 0.5150 0.8429 0.060 Uiso 1 1 calc R . . H15B H -0.1187 0.4735 0.7529 0.060 Uiso 1 1 calc R . . H15C H -0.0747 0.5537 0.7375 0.060 Uiso 1 1 calc R . . C16 C -0.0149(4) 0.3817(2) 0.6088(3) 0.0266(9) Uani 1 1 d . . . C17 C -0.1061(5) 0.4001(2) 0.5159(3) 0.0367(11) Uani 1 1 d . . . H17 H -0.0884 0.4432 0.4840 0.044 Uiso 1 1 calc R . . C18 C -0.2222(5) 0.3556(3) 0.4700(4) 0.0416(11) Uani 1 1 d . . . H18 H -0.2817 0.3687 0.4079 0.050 Uiso 1 1 calc R . . C19 C -0.2489(5) 0.2919(3) 0.5168(4) 0.0407(11) Uani 1 1 d . . . H19 H -0.3269 0.2618 0.4864 0.049 Uiso 1 1 calc R . . C20 C -0.1606(5) 0.2727(2) 0.6085(3) 0.0372(11) Uani 1 1 d . . . H20 H -0.1794 0.2294 0.6395 0.045 Uiso 1 1 calc R . . C21 C -0.0440(4) 0.3167(2) 0.6556(3) 0.0258(9) Uani 1 1 d . . . C22 C 0.0903(5) 0.2219(2) 0.7625(4) 0.0375(11) Uani 1 1 d . . . H22A H 0.0006 0.1920 0.7569 0.056 Uiso 1 1 calc R . . H22B H 0.1542 0.2129 0.8275 0.056 Uiso 1 1 calc R . . H22C H 0.1468 0.2114 0.7066 0.056 Uiso 1 1 calc R . . C23 C -0.0623(5) 0.3093(3) 0.8358(3) 0.0401(11) Uani 1 1 d . . . H23A H -0.0894 0.3590 0.8378 0.060 Uiso 1 1 calc R . . H23B H -0.0115 0.2947 0.9028 0.060 Uiso 1 1 calc R . . H23C H -0.1537 0.2812 0.8174 0.060 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 C4 0.076(4) 0.041(3) 0.028(2) 0.007(2) 0.001(2) 0.001(3) C3 0.031(2) 0.040(3) 0.054(3) -0.006(2) -0.007(2) 0.007(2) C1 0.034(2) 0.039(3) 0.057(3) -0.018(2) -0.011(2) 0.017(2) C6 0.066(3) 0.040(3) 0.023(2) -0.004(2) 0.007(2) 0.002(2) Gd1 0.02523(11) 0.02202(12) 0.02082(11) 0.00027(8) 0.00193(7) 0.00361(8) N1 0.0295(17) 0.0224(18) 0.0286(18) 0.0054(14) 0.0042(14) -0.0012(14) C2 0.023(2) 0.052(3) 0.051(3) -0.010(2) -0.0003(19) 0.018(2) C5 0.074(4) 0.046(3) 0.022(2) 0.000(2) 0.014(2) -0.001(3) C7 0.0258(19) 0.020(2) 0.026(2) 0.0086(16) 0.0017(15) -0.0011(16) C8 0.033(2) 0.030(2) 0.0190(19) 0.0030(17) 0.0058(16) -0.0032(18) C9 0.027(2) 0.031(2) 0.029(2) 0.0066(18) 0.0041(17) -0.0042(18) C10 0.032(2) 0.018(2) 0.030(2) 0.0027(17) 0.0000(17) 0.0019(17) C11 0.0245(19) 0.022(2) 0.029(2) 0.0049(17) 0.0019(16) 0.0024(16) C12 0.058(3) 0.042(3) 0.032(3) -0.003(2) 0.018(2) -0.008(2) C13 0.034(2) 0.044(3) 0.057(3) 0.005(2) 0.012(2) -0.009(2) C14 0.046(3) 0.024(2) 0.040(3) -0.003(2) 0.000(2) -0.002(2) C15 0.031(2) 0.031(3) 0.057(3) -0.007(2) 0.009(2) 0.006(2) C16 0.0264(19) 0.028(2) 0.025(2) -0.0023(17) 0.0018(16) 0.0001(18) C17 0.042(3) 0.028(3) 0.037(3) 0.0075(19) -0.004(2) -0.007(2) C18 0.043(3) 0.042(3) 0.035(3) 0.003(2) -0.011(2) -0.004(2) C19 0.037(2) 0.038(3) 0.043(3) -0.008(2) -0.005(2) -0.011(2) C20 0.042(3) 0.026(2) 0.041(3) 0.004(2) 0.001(2) -0.008(2) C21 0.0249(19) 0.024(2) 0.029(2) 0.0024(17) 0.0045(16) -0.0010(17) C22 0.040(2) 0.023(2) 0.048(3) 0.006(2) 0.001(2) 0.002(2) C23 0.037(2) 0.052(3) 0.034(2) 0.005(2) 0.012(2) -0.002(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 C4 C5 1.380(7) . ? C4 Gd1 2.695(4) . ? C3 C2 1.389(6) . ? C3 Gd1 2.602(4) . ? C1 C2 1.385(7) . ? C1 Gd1 2.693(4) . ? C6 C5 1.379(6) . ? C6 Gd1 2.602(4) . ? Gd1 C7 2.606(4) . ? Gd1 C11 2.631(4) . ? Gd1 N1 2.645(3) . ? Gd1 C2 2.660(4) . ? Gd1 C10 2.679(4) . ? Gd1 C8 2.699(4) . ? Gd1 C5 2.687(4) . ? Gd1 C9 2.735(4) . ? N1 C21 1.469(5) . ? N1 C23 1.489(5) . ? N1 C22 1.487(5) . ? C7 C8 1.420(5) . ? C7 C11 1.423(6) . ? C7 C16 1.491(5) . ? C8 C9 1.418(6) . ? C8 C12 1.507(6) . ? C9 C10 1.418(6) . ? C9 C13 1.512(5) . ? C10 C11 1.412(5) . ? C10 C14 1.508(6) . ? C11 C15 1.501(5) . ? C16 C17 1.393(6) . ? C16 C21 1.399(5) . ? C17 C18 1.382(6) . ? C18 C19 1.372(7) . ? C19 C20 1.374(6) . ? C20 C21 1.385(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C4 Gd1 74.8(3) . . ? C2 C3 Gd1 77.0(3) . . ? C2 C1 Gd1 73.7(2) . . ? C5 C6 Gd1 78.4(3) . . ? C6 Gd1 C3 89.10(16) . . ? C6 Gd1 C7 119.10(14) . . ? C3 Gd1 C7 127.03(15) . . ? C6 Gd1 C11 88.02(14) . . ? C3 Gd1 C11 127.29(14) . . ? C7 Gd1 C11 31.53(12) . . ? C6 Gd1 N1 117.46(14) . . ? C3 Gd1 N1 140.39(13) . . ? C7 Gd1 N1 67.15(11) . . ? C11 Gd1 N1 84.99(11) . . ? C6 Gd1 C2 119.02(16) . . ? C3 Gd1 C2 30.60(14) . . ? C7 Gd1 C2 110.22(14) . . ? C11 Gd1 C2 128.62(14) . . ? N1 Gd1 C2 113.16(13) . . ? C6 Gd1 C10 81.34(14) . . ? C3 Gd1 C10 96.89(14) . . ? C7 Gd1 C10 51.13(12) . . ? C11 Gd1 C10 30.83(12) . . ? N1 Gd1 C10 114.84(11) . . ? C2 Gd1 C10 106.20(15) . . ? C6 Gd1 C1 130.67(16) . . ? C3 Gd1 C1 55.58(14) . . ? C7 Gd1 C1 109.97(14) . . ? C11 Gd1 C1 139.82(14) . . ? N1 Gd1 C1 85.14(12) . . ? C2 Gd1 C1 29.97(14) . . ? C10 Gd1 C1 130.78(15) . . ? C6 Gd1 C4 55.25(15) . . ? C3 Gd1 C4 85.79(17) . . ? C7 Gd1 C4 147.14(15) . . ? C11 Gd1 C4 132.07(14) . . ? N1 Gd1 C4 86.63(14) . . ? C2 Gd1 C4 97.89(16) . . ? C10 Gd1 C4 136.51(14) . . ? C1 Gd1 C4 85.97(16) . . ? C6 Gd1 C8 131.80(14) . . ? C3 Gd1 C8 96.43(15) . . ? C7 Gd1 C8 30.98(12) . . ? C11 Gd1 C8 51.30(12) . . ? N1 Gd1 C8 87.11(11) . . ? C2 Gd1 C8 80.79(14) . . ? C10 Gd1 C8 50.46(12) . . ? C1 Gd1 C8 89.37(15) . . ? C4 Gd1 C8 172.49(14) . . ? C6 Gd1 C5 30.16(14) . . ? C3 Gd1 C5 99.11(17) . . ? C7 Gd1 C5 128.35(15) . . ? C11 Gd1 C5 103.94(14) . . ? N1 Gd1 C5 93.08(14) . . ? C2 Gd1 C5 121.39(16) . . ? C10 Gd1 C5 108.17(14) . . ? C1 Gd1 C5 115.42(16) . . ? C4 Gd1 C5 29.72(14) . . ? C8 Gd1 C5 155.16(15) . . ? C6 Gd1 C9 106.06(14) . . ? C3 Gd1 C9 80.02(14) . . ? C7 Gd1 C9 50.69(12) . . ? C11 Gd1 C9 50.73(12) . . ? N1 Gd1 C9 115.82(11) . . ? C2 Gd1 C9 78.90(15) . . ? C10 Gd1 C9 30.34(12) . . ? C1 Gd1 C9 100.60(15) . . ? C4 Gd1 C9 156.90(15) . . ? C8 Gd1 C9 30.24(12) . . ? C5 Gd1 C9 135.69(14) . . ? C21 N1 C23 107.2(3) . . ? C21 N1 C22 111.9(3) . . ? C23 N1 C22 107.4(3) . . ? C21 N1 Gd1 115.7(2) . . ? C23 N1 Gd1 102.3(2) . . ? C22 N1 Gd1 111.6(2) . . ? C1 C2 C3 125.8(5) . . ? C1 C2 Gd1 76.3(3) . . ? C3 C2 Gd1 72.4(3) . . ? C4 C5 C6 125.9(5) . . ? C4 C5 Gd1 75.4(3) . . ? C6 C5 Gd1 71.5(3) . . ? C8 C7 C11 108.6(3) . . ? C8 C7 C16 124.8(4) . . ? C11 C7 C16 126.6(3) . . ? C8 C7 Gd1 78.1(2) . . ? C11 C7 Gd1 75.2(2) . . ? C16 C7 Gd1 115.5(2) . . ? C7 C8 C9 107.6(3) . . ? C7 C8 C12 125.2(4) . . ? C9 C8 C12 127.0(4) . . ? C7 C8 Gd1 70.9(2) . . ? C9 C8 Gd1 76.3(2) . . ? C12 C8 Gd1 123.2(3) . . ? C10 C9 C8 107.9(3) . . ? C10 C9 C13 125.5(4) . . ? C8 C9 C13 126.2(4) . . ? C10 C9 Gd1 72.6(2) . . ? C8 C9 Gd1 73.5(2) . . ? C13 C9 Gd1 125.5(3) . . ? C11 C10 C9 108.8(4) . . ? C11 C10 C14 126.4(4) . . ? C9 C10 C14 124.5(4) . . ? C11 C10 Gd1 72.7(2) . . ? C9 C10 Gd1 77.0(2) . . ? C14 C10 Gd1 121.5(3) . . ? C10 C11 C7 107.2(3) . . ? C10 C11 C15 126.8(4) . . ? C7 C11 C15 125.9(4) . . ? C10 C11 Gd1 76.4(2) . . ? C7 C11 Gd1 73.3(2) . . ? C15 C11 Gd1 119.6(3) . . ? C17 C16 C21 118.3(4) . . ? C17 C16 C7 120.2(4) . . ? C21 C16 C7 121.5(4) . . ? C18 C17 C16 121.5(4) . . ? C19 C18 C17 119.5(4) . . ? C18 C19 C20 120.0(4) . . ? C19 C20 C21 121.2(4) . . ? C20 C21 C16 119.5(4) . . ? C20 C21 N1 120.9(4) . . ? C16 C21 N1 119.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.805 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.098 #===========END============= data_complex4 #CCDC 748837 _database_code_depnum_ccdc_archive 'CCDC 748837' #TrackingRef 'complexes_1_3_and_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32 Dy N' _chemical_formula_weight 485.00 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7688(4) _cell_length_b 18.6646(9) _cell_length_c 12.9847(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.3560(10) _cell_angle_gamma 90.00 _cell_volume 2102.60(17) _cell_formula_units_Z 4 _cell_measurement_temperature 186.5(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 3.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5220 _exptl_absorpt_correction_T_max 0.5830 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186.5(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11465 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.05 _reflns_number_total 4140 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0312P)^2^+1.2924P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4140 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Dy1 Dy 0.272910(15) 0.383963(6) 0.824225(9) 0.02127(6) Uani 1 1 d . . . N1 N 0.0406(3) 0.29895(12) 0.75790(18) 0.0244(5) Uani 1 1 d . . . C1 C 0.2603(5) 0.45311(19) 0.9957(3) 0.0439(9) Uani 1 1 d . . . H1A H 0.3576 0.4564 0.9756 0.053 Uiso 1 1 calc R . . H1B H 0.2031 0.4944 1.0023 0.053 Uiso 1 1 calc R . . C2 C 0.2008(5) 0.38713(18) 1.0156(3) 0.0449(9) Uani 1 1 d . . . H2 H 0.1031 0.3869 1.0354 0.054 Uiso 1 1 calc R . . C3 C 0.2704(5) 0.3213(2) 1.0095(3) 0.0486(9) Uani 1 1 d . . . H3A H 0.3682 0.3184 0.9901 0.058 Uiso 1 1 calc R . . H3B H 0.2195 0.2798 1.0248 0.058 Uiso 1 1 calc R . . C4 C 0.5710(4) 0.38215(18) 0.8714(3) 0.0424(9) Uani 1 1 d . . . H4A H 0.5285 0.3739 0.9319 0.051 Uiso 1 1 calc R . . H4B H 0.6341 0.4217 0.8668 0.051 Uiso 1 1 calc R . . C5 C 0.5401(4) 0.33520(19) 0.7876(3) 0.0406(8) Uani 1 1 d . . . H5 H 0.5856 0.3460 0.7290 0.049 Uiso 1 1 calc R . . C6 C 0.4507(4) 0.27524(19) 0.7818(3) 0.0428(8) Uani 1 1 d . . . H6A H 0.4025 0.2620 0.8381 0.051 Uiso 1 1 calc R . . H6B H 0.4379 0.2476 0.7216 0.051 Uiso 1 1 calc R . . C7 C 0.1123(3) 0.42979(14) 0.6551(2) 0.0226(6) Uani 1 1 d . . . C8 C 0.2630(3) 0.42884(15) 0.6281(2) 0.0251(6) Uani 1 1 d . . . C9 C 0.3490(3) 0.48286(16) 0.6875(2) 0.0278(6) Uani 1 1 d . . . C10 C 0.2516(3) 0.51682(14) 0.7504(2) 0.0255(6) Uani 1 1 d . . . C11 C 0.1034(3) 0.48523(14) 0.7288(2) 0.0239(6) Uani 1 1 d . . . C12 C 0.3153(5) 0.38404(17) 0.5439(3) 0.0406(8) Uani 1 1 d . . . H12A H 0.2948 0.4090 0.4788 0.061 Uiso 1 1 calc R . . H12B H 0.2607 0.3393 0.5388 0.061 Uiso 1 1 calc R . . H12C H 0.4240 0.3751 0.5604 0.061 Uiso 1 1 calc R . . C13 C 0.5100(4) 0.5067(2) 0.6760(3) 0.0440(8) Uani 1 1 d . . . H13A H 0.5049 0.5454 0.6270 0.066 Uiso 1 1 calc R . . H13B H 0.5654 0.4673 0.6516 0.066 Uiso 1 1 calc R . . H13C H 0.5621 0.5225 0.7423 0.066 Uiso 1 1 calc R . . C14 C 0.2950(4) 0.58109(18) 0.8182(2) 0.0370(8) Uani 1 1 d . . . H14A H 0.3962 0.5743 0.8564 0.056 Uiso 1 1 calc R . . H14B H 0.2221 0.5869 0.8660 0.056 Uiso 1 1 calc R . . H14C H 0.2945 0.6231 0.7755 0.056 Uiso 1 1 calc R . . C15 C -0.0395(4) 0.50872(18) 0.7705(3) 0.0388(8) Uani 1 1 d . . . H15A H -0.0186 0.5118 0.8450 0.058 Uiso 1 1 calc R . . H15B H -0.1203 0.4745 0.7509 0.058 Uiso 1 1 calc R . . H15C H -0.0711 0.5548 0.7422 0.058 Uiso 1 1 calc R . . C16 C -0.0148(3) 0.38191(14) 0.6087(2) 0.0252(6) Uani 1 1 d . . . C17 C -0.1060(4) 0.40079(18) 0.5157(3) 0.0371(8) Uani 1 1 d . . . H17 H -0.0880 0.4440 0.4838 0.045 Uiso 1 1 calc R . . C18 C -0.2234(4) 0.35620(19) 0.4699(3) 0.0401(8) Uani 1 1 d . . . H18 H -0.2833 0.3695 0.4078 0.048 Uiso 1 1 calc R . . C19 C -0.2508(4) 0.29255(18) 0.5163(3) 0.0381(8) Uani 1 1 d . . . H19 H -0.3286 0.2624 0.4852 0.046 Uiso 1 1 calc R . . C20 C -0.1637(4) 0.27320(17) 0.6086(3) 0.0361(7) Uani 1 1 d . . . H20 H -0.1836 0.2301 0.6399 0.043 Uiso 1 1 calc R . . C21 C -0.0462(3) 0.31729(15) 0.6558(2) 0.0246(6) Uani 1 1 d . . . C22 C 0.0884(4) 0.22242(15) 0.7620(3) 0.0362(7) Uani 1 1 d . . . H22A H -0.0012 0.1924 0.7584 0.054 Uiso 1 1 calc R . . H22B H 0.1554 0.2134 0.8260 0.054 Uiso 1 1 calc R . . H22C H 0.1419 0.2120 0.7043 0.054 Uiso 1 1 calc R . . C23 C -0.0665(4) 0.3092(2) 0.8361(3) 0.0404(8) Uani 1 1 d . . . H23A H -0.0925 0.3590 0.8396 0.061 Uiso 1 1 calc R . . H23B H -0.0173 0.2934 0.9031 0.061 Uiso 1 1 calc R . . H23C H -0.1586 0.2818 0.8159 0.061 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 Dy1 0.02586(9) 0.01870(8) 0.01859(8) 0.00010(4) 0.00104(6) 0.00388(5) N1 0.0290(13) 0.0188(12) 0.0255(12) 0.0046(9) 0.0046(10) 0.0013(9) C1 0.066(2) 0.0377(19) 0.0301(17) -0.0066(14) 0.0132(17) 0.0025(17) C2 0.075(3) 0.044(2) 0.0172(16) -0.0008(13) 0.0115(17) -0.0020(17) C3 0.081(3) 0.038(2) 0.0267(17) 0.0076(15) 0.0089(17) 0.0030(19) C4 0.0262(17) 0.043(2) 0.055(2) -0.0099(16) -0.0014(16) 0.0032(14) C5 0.0246(16) 0.047(2) 0.049(2) -0.0058(16) -0.0006(14) 0.0155(14) C6 0.0366(19) 0.0396(19) 0.049(2) -0.0166(16) -0.0041(15) 0.0124(15) C7 0.0282(15) 0.0170(13) 0.0210(13) 0.0056(10) -0.0016(11) -0.0016(11) C8 0.0316(15) 0.0235(14) 0.0206(13) 0.0043(11) 0.0047(11) -0.0020(12) C9 0.0290(15) 0.0272(15) 0.0271(15) 0.0059(12) 0.0036(12) -0.0039(12) C10 0.0299(15) 0.0176(13) 0.0277(14) 0.0031(11) -0.0006(12) -0.0013(11) C11 0.0287(15) 0.0164(13) 0.0258(14) 0.0049(11) 0.0017(12) 0.0040(11) C12 0.051(2) 0.042(2) 0.0322(18) -0.0054(14) 0.0168(16) -0.0076(15) C13 0.0325(18) 0.046(2) 0.055(2) 0.0040(17) 0.0115(16) -0.0121(15) C14 0.045(2) 0.0220(16) 0.0420(19) -0.0043(13) -0.0019(15) -0.0017(13) C15 0.0309(17) 0.0310(17) 0.055(2) -0.0042(15) 0.0081(15) 0.0063(13) C16 0.0254(15) 0.0243(15) 0.0247(15) 0.0001(11) -0.0002(12) -0.0025(11) C17 0.047(2) 0.0270(16) 0.0335(17) 0.0080(13) -0.0087(15) -0.0047(14) C18 0.043(2) 0.0395(19) 0.0321(17) 0.0006(15) -0.0142(15) -0.0037(15) C19 0.0359(18) 0.0338(18) 0.0408(18) -0.0056(14) -0.0071(14) -0.0093(14) C20 0.0410(19) 0.0244(15) 0.0416(18) 0.0025(13) 0.0018(15) -0.0097(13) C21 0.0273(15) 0.0194(13) 0.0265(14) 0.0007(11) 0.0024(12) -0.0010(11) C22 0.0436(19) 0.0183(14) 0.0451(19) 0.0054(13) 0.0007(15) 0.0010(13) C23 0.0408(19) 0.046(2) 0.0357(18) 0.0060(15) 0.0118(15) -0.0020(15) _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 Dy1 C7 2.576(3) . ? Dy1 C1 2.589(3) . ? Dy1 C4 2.597(4) . ? Dy1 C11 2.604(3) . ? Dy1 C5 2.621(3) . ? Dy1 N1 2.627(2) . ? Dy1 C2 2.652(3) . ? Dy1 C10 2.656(3) . ? Dy1 C6 2.665(3) . ? Dy1 C8 2.670(3) . ? Dy1 C3 2.678(3) . ? Dy1 C9 2.711(3) . ? N1 C21 1.470(4) . ? N1 C22 1.488(4) . ? N1 C23 1.492(4) . ? C1 C2 1.377(5) . ? C2 C3 1.379(5) . ? C4 C5 1.393(5) . ? C5 C6 1.362(5) . ? C7 C8 1.416(4) . ? C7 C11 1.419(4) . ? C7 C16 1.487(4) . ? C8 C9 1.418(4) . ? C8 C12 1.500(4) . ? C9 C10 1.414(4) . ? C9 C13 1.508(4) . ? C10 C11 1.417(4) . ? C10 C14 1.504(4) . ? C11 C15 1.501(4) . ? C16 C17 1.393(4) . ? C16 C21 1.397(4) . ? C17 C18 1.389(5) . ? C18 C19 1.369(5) . ? C19 C20 1.373(5) . ? C20 C21 1.390(4) . ? 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 C7 Dy1 C1 118.74(10) . . ? C7 Dy1 C4 127.74(11) . . ? C1 Dy1 C4 88.35(13) . . ? C7 Dy1 C11 31.80(9) . . ? C1 Dy1 C11 87.39(11) . . ? C4 Dy1 C11 127.38(10) . . ? C7 Dy1 C5 110.66(10) . . ? C1 Dy1 C5 118.70(12) . . ? C4 Dy1 C5 30.96(11) . . ? C11 Dy1 C5 128.99(10) . . ? C7 Dy1 N1 67.62(8) . . ? C1 Dy1 N1 117.06(10) . . ? C4 Dy1 N1 140.86(9) . . ? C11 Dy1 N1 85.44(8) . . ? C5 Dy1 N1 113.70(9) . . ? C7 Dy1 C2 128.02(11) . . ? C1 Dy1 C2 30.42(11) . . ? C4 Dy1 C2 98.52(14) . . ? C11 Dy1 C2 103.43(11) . . ? C5 Dy1 C2 121.26(13) . . ? N1 Dy1 C2 92.38(10) . . ? C7 Dy1 C10 51.76(8) . . ? C1 Dy1 C10 80.54(10) . . ? C4 Dy1 C10 96.48(10) . . ? C11 Dy1 C10 31.25(9) . . ? C5 Dy1 C10 106.05(10) . . ? N1 Dy1 C10 115.79(8) . . ? C2 Dy1 C10 107.69(10) . . ? C7 Dy1 C6 109.91(10) . . ? C1 Dy1 C6 131.03(12) . . ? C4 Dy1 C6 55.92(10) . . ? C11 Dy1 C6 139.92(10) . . ? C5 Dy1 C6 29.85(11) . . ? N1 Dy1 C6 85.50(9) . . ? C2 Dy1 C6 115.90(12) . . ? C10 Dy1 C6 130.47(11) . . ? C7 Dy1 C8 31.24(9) . . ? C1 Dy1 C8 131.61(10) . . ? C4 Dy1 C8 96.96(11) . . ? C11 Dy1 C8 51.79(9) . . ? C5 Dy1 C8 80.90(10) . . ? N1 Dy1 C8 87.74(8) . . ? C2 Dy1 C8 155.15(10) . . ? C10 Dy1 C8 51.08(9) . . ? C6 Dy1 C8 88.90(11) . . ? C7 Dy1 C3 146.69(12) . . ? C1 Dy1 C3 55.83(12) . . ? C4 Dy1 C3 85.53(13) . . ? C11 Dy1 C3 131.73(11) . . ? C5 Dy1 C3 97.81(12) . . ? N1 Dy1 C3 85.61(10) . . ? C2 Dy1 C3 29.98(11) . . ? C10 Dy1 C3 136.30(10) . . ? C6 Dy1 C3 86.25(12) . . ? C8 Dy1 C3 172.05(10) . . ? C7 Dy1 C9 51.08(9) . . ? C1 Dy1 C9 105.61(10) . . ? C4 Dy1 C9 80.11(11) . . ? C11 Dy1 C9 51.10(9) . . ? C5 Dy1 C9 78.81(11) . . ? N1 Dy1 C9 116.71(8) . . ? C2 Dy1 C9 135.50(10) . . ? C10 Dy1 C9 30.54(9) . . ? C6 Dy1 C9 100.14(11) . . ? C8 Dy1 C9 30.55(9) . . ? C3 Dy1 C9 157.03(11) . . ? C21 N1 C22 111.2(2) . . ? C21 N1 C23 106.9(2) . . ? C22 N1 C23 107.5(2) . . ? C21 N1 Dy1 115.47(16) . . ? C22 N1 Dy1 111.53(18) . . ? C23 N1 Dy1 103.56(18) . . ? C2 C1 Dy1 77.3(2) . . ? C1 C2 C3 127.1(4) . . ? C1 C2 Dy1 72.26(19) . . ? C3 C2 Dy1 76.0(2) . . ? C2 C3 Dy1 74.00(19) . . ? C5 C4 Dy1 75.5(2) . . ? C6 C5 C4 127.2(4) . . ? C6 C5 Dy1 76.85(19) . . ? C4 C5 Dy1 73.6(2) . . ? C5 C6 Dy1 73.29(18) . . ? C8 C7 C11 108.7(2) . . ? C8 C7 C16 124.3(3) . . ? C11 C7 C16 126.9(3) . . ? C8 C7 Dy1 78.05(15) . . ? C11 C7 Dy1 75.18(15) . . ? C16 C7 Dy1 115.53(17) . . ? C7 C8 C9 107.3(2) . . ? C7 C8 C12 125.7(3) . . ? C9 C8 C12 126.7(3) . . ? C7 C8 Dy1 70.71(14) . . ? C9 C8 Dy1 76.31(16) . . ? C12 C8 Dy1 123.3(2) . . ? C10 C9 C8 108.3(3) . . ? C10 C9 C13 125.3(3) . . ? C8 C9 C13 126.0(3) . . ? C10 C9 Dy1 72.56(15) . . ? C8 C9 Dy1 73.14(16) . . ? C13 C9 Dy1 126.0(2) . . ? C9 C10 C11 108.2(2) . . ? C9 C10 C14 124.9(3) . . ? C11 C10 C14 126.4(3) . . ? C9 C10 Dy1 76.90(16) . . ? C11 C10 Dy1 72.37(15) . . ? C14 C10 Dy1 122.31(19) . . ? C10 C11 C7 107.3(2) . . ? C10 C11 C15 126.7(3) . . ? C7 C11 C15 125.9(3) . . ? C10 C11 Dy1 76.38(15) . . ? C7 C11 Dy1 73.02(15) . . ? C15 C11 Dy1 119.3(2) . . ? C17 C16 C21 118.2(3) . . ? C17 C16 C7 120.1(3) . . ? C21 C16 C7 121.7(3) . . ? C18 C17 C16 121.1(3) . . ? C19 C18 C17 119.9(3) . . ? C18 C19 C20 120.1(3) . . ? C19 C20 C21 120.8(3) . . ? C20 C21 C16 119.9(3) . . ? C20 C21 N1 120.9(3) . . ? C16 C21 N1 119.1(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.654 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.110