data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Guangming Li' _publ_contact_author_email 'gmli 2000@163.com' _publ_section_title ; Effect of Lanthanide Contraction and Rigid Ligand on the Structure of Salen Type Lanthanide Complexes ; loop_ _publ_author_name 'Peng Chen' 'Han Chen' 'Pengfei Yan' 'Yan Wang' 'Guangming Li' # Attachment '- 1.CIF' data_ca _database_code_depnum_ccdc_archive 'CCDC 822890' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Cl6 N4 O12 Pr2 Zn2' _chemical_formula_weight 1502.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.393(2) _cell_length_b 11.270(2) _cell_length_c 12.065(2) _cell_angle_alpha 105.91(3) _cell_angle_beta 95.95(3) _cell_angle_gamma 96.73(3) _cell_volume 1336.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 3.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.673 _exptl_absorpt_process_details SADABS _exptl_special_details ; Two restraints (dfix) are used to define the distances of O(1)-H(1) and O(2)-H(2) bond lengths in the reasonable distances. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13243 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6057 _reflns_number_gt 5358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART ' _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0189P)^2^+0.6460P] 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 6057 _refine_ls_number_parameters 345 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.478769(14) 0.814823(13) 0.342226(11) 0.02280(5) Uani 1 1 d . . . Zn1 Zn 0.29948(3) 0.67862(3) 0.05336(2) 0.02603(7) Uani 1 1 d . . . Cl1 Cl 0.38633(7) 0.93173(6) 0.56953(6) 0.03378(15) Uani 1 1 d . . . Cl2 Cl 0.65589(7) 0.75848(7) 0.50411(6) 0.03751(16) Uani 1 1 d . . . Cl3 Cl 0.32662(7) 0.47545(6) -0.00796(6) 0.03495(15) Uani 1 1 d . . . O1 O 0.5343(2) 0.60427(19) 0.23912(17) 0.0394(5) Uani 1 1 d D . . H1 H 0.545(4) 0.599(4) 0.1716(19) 0.075(14) Uiso 1 1 d D . . O2 O 0.3277(2) 0.9752(2) 0.31600(18) 0.0382(5) Uani 1 1 d D . . H2 H 0.366(5) 1.045(3) 0.357(4) 0.114(19) Uiso 1 1 d D . . O3 O 0.27675(17) 0.70611(16) 0.22265(14) 0.0260(4) Uani 1 1 d . . . O4 O 0.46732(18) 0.79510(17) 0.13557(15) 0.0296(4) Uani 1 1 d . . . O5 O 0.70191(19) 0.84843(19) 0.24508(17) 0.0359(5) Uani 1 1 d . . . O6 O 0.31576(18) 0.65266(17) 0.41431(15) 0.0302(4) Uani 1 1 d . . . C1 C 0.7889(3) 0.9088(3) 0.0836(3) 0.0417(7) Uani 1 1 d . . . H1A H 0.8742 0.9285 0.1223 0.050 Uiso 1 1 calc R . . C2 C 0.0209(4) 0.7641(3) -0.2987(2) 0.0456(8) Uani 1 1 d . . . H2A H 0.0050 0.7822 -0.3691 0.055 Uiso 1 1 calc R . . C3 C 0.7610(4) 0.9231(3) -0.0277(3) 0.0483(8) Uani 1 1 d . . . H3A H 0.8283 0.9522 -0.0631 0.058 Uiso 1 1 calc R . . C4 C -0.0449(3) 0.5771(3) 0.3521(3) 0.0404(7) Uani 1 1 d . . . H4A H -0.1169 0.5539 0.3854 0.049 Uiso 1 1 calc R . . C5 C 0.8296(3) 0.8868(3) 0.3125(3) 0.0482(8) Uani 1 1 d . . . H5A H 0.8913 0.8417 0.2712 0.072 Uiso 1 1 calc R . . H5B H 0.8275 0.8696 0.3860 0.072 Uiso 1 1 calc R . . H5C H 0.8553 0.9747 0.3254 0.072 Uiso 1 1 calc R . . C6 C 0.3428(3) 0.6096(3) 0.5150(2) 0.0409(7) Uani 1 1 d . . . H6A H 0.3111 0.5219 0.4955 0.061 Uiso 1 1 calc R . . H6B H 0.2998 0.6541 0.5767 0.061 Uiso 1 1 calc R . . H6C H 0.4355 0.6243 0.5400 0.061 Uiso 1 1 calc R . . C7 C 0.6372(3) 0.8948(3) -0.0840(3) 0.0433(8) Uani 1 1 d . . . H7A H 0.6208 0.9063 -0.1573 0.052 Uiso 1 1 calc R . . C8 C -0.0632(3) 0.5952(3) 0.2445(2) 0.0352(6) Uani 1 1 d . . . H8A H -0.1474 0.5811 0.2042 0.042 Uiso 1 1 calc R . . C9 C 0.1894(4) 0.9630(3) 0.2994(4) 0.0599(10) Uani 1 1 d . . . H9A H 0.1634 1.0400 0.2926 0.090 Uiso 1 1 calc R . . H9B H 0.1563 0.9436 0.3648 0.090 Uiso 1 1 calc R . . H9C H 0.1547 0.8971 0.2296 0.090 Uiso 1 1 calc R . . C10 C 0.0805(3) 0.5932(3) 0.4121(2) 0.0352(7) Uani 1 1 d . . . H10A H 0.0925 0.5778 0.4841 0.042 Uiso 1 1 calc R . . C11 C -0.0830(4) 0.7192(3) -0.2505(3) 0.0451(8) Uani 1 1 d . . . H11A H -0.1681 0.7077 -0.2884 0.054 Uiso 1 1 calc R . . C12 C 0.4024(3) 0.8261(3) -0.0983(2) 0.0334(6) Uani 1 1 d . . . H12A H 0.3924 0.8570 -0.1622 0.040 Uiso 1 1 calc R . . C13 C 0.1733(3) 0.7543(2) -0.1381(2) 0.0298(6) Uani 1 1 d . . . C14 C 0.0442(3) 0.6352(2) 0.1934(2) 0.0266(5) Uani 1 1 d . . . C15 C 0.1470(4) 0.7820(3) -0.2437(2) 0.0407(7) Uani 1 1 d . . . H15A H 0.2156 0.8128 -0.2768 0.049 Uiso 1 1 calc R . . C16 C 0.1868(3) 0.6320(2) 0.3646(2) 0.0262(5) Uani 1 1 d . . . C17 C 0.5586(3) 0.8340(2) 0.0782(2) 0.0275(6) Uani 1 1 d . . . C18 C 0.6879(3) 0.8652(2) 0.1350(2) 0.0316(6) Uani 1 1 d . . . C19 C 0.5311(3) 0.8480(2) -0.0346(2) 0.0318(6) Uani 1 1 d . . . C20 C -0.0598(3) 0.6916(3) -0.1460(2) 0.0371(7) Uani 1 1 d . . . H20A H -0.1296 0.6610 -0.1141 0.044 Uiso 1 1 calc R . . C21 C 0.0145(3) 0.6574(2) 0.0813(2) 0.0293(6) Uani 1 1 d . . . H21A H -0.0731 0.6513 0.0519 0.035 Uiso 1 1 calc R . . C22 C 0.0673(3) 0.7092(2) -0.0882(2) 0.0293(6) Uani 1 1 d . . . C23 C 0.1706(3) 0.6575(2) 0.2561(2) 0.0238(5) Uani 1 1 d . . . C24 C 0.5190(5) 0.4877(3) 0.2609(3) 0.0643(12) Uani 1 1 d . . . H24A H 0.5922 0.4463 0.2397 0.096 Uiso 1 1 calc R . . H24B H 0.4398 0.4377 0.2158 0.096 Uiso 1 1 calc R . . H24C H 0.5144 0.4994 0.3422 0.096 Uiso 1 1 calc R . . N1 N 0.2992(2) 0.7677(2) -0.07538(18) 0.0288(5) Uani 1 1 d . . . N2 N 0.1014(2) 0.6851(2) 0.01948(17) 0.0267(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02395(8) 0.02218(7) 0.02015(7) 0.00380(6) 0.00076(5) 0.00286(5) Zn1 0.02921(17) 0.02843(16) 0.02033(14) 0.00770(13) 0.00390(12) 0.00197(13) Cl1 0.0360(4) 0.0265(3) 0.0375(3) 0.0057(3) 0.0125(3) 0.0015(3) Cl2 0.0384(4) 0.0349(4) 0.0357(3) 0.0065(3) -0.0059(3) 0.0104(3) Cl3 0.0314(4) 0.0308(3) 0.0383(4) 0.0032(3) 0.0023(3) 0.0061(3) O1 0.0585(15) 0.0321(11) 0.0269(10) 0.0042(9) 0.0053(10) 0.0151(10) O2 0.0396(13) 0.0332(11) 0.0356(11) 0.0019(10) -0.0052(9) 0.0098(10) O3 0.0247(10) 0.0310(9) 0.0211(8) 0.0078(8) 0.0037(7) -0.0010(8) O4 0.0292(11) 0.0352(10) 0.0239(9) 0.0088(8) 0.0085(8) -0.0017(8) O5 0.0292(11) 0.0391(11) 0.0364(10) 0.0061(9) 0.0071(9) 0.0032(9) O6 0.0303(11) 0.0358(10) 0.0253(9) 0.0141(8) -0.0006(8) -0.0008(8) C1 0.0348(18) 0.0335(15) 0.0569(19) 0.0088(15) 0.0196(15) 0.0041(13) C2 0.074(3) 0.0419(17) 0.0223(13) 0.0098(13) -0.0015(15) 0.0189(17) C3 0.051(2) 0.0431(18) 0.057(2) 0.0179(17) 0.0319(17) 0.0046(16) C4 0.0358(17) 0.0489(18) 0.0405(16) 0.0208(15) 0.0131(13) -0.0038(14) C5 0.0266(17) 0.055(2) 0.063(2) 0.0172(18) 0.0060(15) 0.0060(15) C6 0.0451(19) 0.0498(18) 0.0347(15) 0.0266(15) -0.0004(13) 0.0051(15) C7 0.056(2) 0.0400(17) 0.0404(16) 0.0166(15) 0.0246(15) 0.0061(15) C8 0.0265(15) 0.0406(16) 0.0384(15) 0.0147(14) 0.0033(12) -0.0015(12) C9 0.045(2) 0.0402(19) 0.081(3) 0.0008(19) -0.0174(19) 0.0138(16) C10 0.0413(18) 0.0399(16) 0.0270(13) 0.0164(13) 0.0067(12) -0.0008(13) C11 0.055(2) 0.0441(18) 0.0334(15) 0.0089(14) -0.0094(15) 0.0175(16) C12 0.0499(19) 0.0300(14) 0.0258(13) 0.0129(12) 0.0127(13) 0.0098(13) C13 0.0439(17) 0.0238(13) 0.0217(12) 0.0058(11) 0.0026(11) 0.0089(12) C14 0.0296(15) 0.0253(13) 0.0233(12) 0.0061(11) 0.0036(10) 0.0003(11) C15 0.064(2) 0.0335(15) 0.0281(14) 0.0120(13) 0.0095(14) 0.0111(15) C16 0.0318(15) 0.0221(12) 0.0234(12) 0.0062(11) 0.0029(11) 0.0006(11) C17 0.0317(15) 0.0191(12) 0.0316(13) 0.0043(11) 0.0122(11) 0.0032(11) C18 0.0338(16) 0.0213(12) 0.0393(15) 0.0040(12) 0.0147(12) 0.0062(11) C19 0.0422(17) 0.0222(13) 0.0345(14) 0.0090(12) 0.0166(13) 0.0066(12) C20 0.0416(18) 0.0387(16) 0.0291(14) 0.0072(13) -0.0004(12) 0.0100(13) C21 0.0279(15) 0.0291(13) 0.0275(13) 0.0058(12) -0.0017(11) 0.0012(11) C22 0.0394(16) 0.0266(13) 0.0208(12) 0.0048(11) 0.0015(11) 0.0086(11) C23 0.0291(14) 0.0192(11) 0.0218(12) 0.0047(10) 0.0046(10) 0.0008(10) C24 0.118(4) 0.0373(18) 0.046(2) 0.0186(17) 0.016(2) 0.030(2) N1 0.0383(14) 0.0258(11) 0.0230(10) 0.0074(10) 0.0068(10) 0.0052(10) N2 0.0307(13) 0.0276(11) 0.0212(10) 0.0063(9) 0.0018(9) 0.0057(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O3 2.406(2) . ? Pr1 O4 2.4308(17) . ? Pr1 O1 2.522(2) . ? Pr1 O2 2.590(2) . ? Pr1 O6 2.7235(19) . ? Pr1 O5 2.738(2) . ? Pr1 Cl2 2.7955(10) . ? Pr1 Cl1 2.8883(12) 2_676 ? Pr1 Cl1 3.0070(11) . ? Pr1 Zn1 3.6090(14) . ? Zn1 O3 2.0233(17) . ? Zn1 O4 2.035(2) . ? Zn1 N1 2.068(2) . ? Zn1 N2 2.071(2) . ? Zn1 Cl3 2.2661(9) . ? Cl1 Pr1 2.8883(12) 2_676 ? O1 C24 1.403(4) . ? O1 H1 0.821(18) . ? O2 C9 1.416(4) . ? O2 H2 0.834(19) . ? O3 C23 1.324(3) . ? O4 C17 1.332(3) . ? O5 C18 1.387(3) . ? O5 C5 1.434(4) . ? O6 C16 1.376(3) . ? O6 C6 1.440(3) . ? C1 C18 1.382(4) . ? C1 C3 1.400(5) . ? C1 H1A 0.9300 . ? C2 C15 1.372(5) . ? C2 C11 1.387(5) . ? C2 H2A 0.9300 . ? C3 C7 1.350(5) . ? C3 H3A 0.9300 . ? C4 C8 1.365(4) . ? C4 C10 1.390(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C19 1.421(4) . ? C7 H7A 0.9300 . ? C8 C14 1.417(4) . ? C8 H8A 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C16 1.377(4) . ? C10 H10A 0.9300 . ? C11 C20 1.384(4) . ? C11 H11A 0.9300 . ? C12 N1 1.288(4) . ? C12 C19 1.430(4) . ? C12 H12A 0.9300 . ? C13 C15 1.401(4) . ? C13 N1 1.412(4) . ? C13 C22 1.417(4) . ? C14 C23 1.405(4) . ? C14 C21 1.450(3) . ? C15 H15A 0.9300 . ? C16 C23 1.413(3) . ? C17 C18 1.402(4) . ? C17 C19 1.417(4) . ? C20 C22 1.393(4) . ? C20 H20A 0.9300 . ? C21 N2 1.292(3) . ? C21 H21A 0.9300 . ? C22 N2 1.417(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 O3 Pr1 O4 64.03(6) . . ? O3 Pr1 O1 76.19(7) . . ? O4 Pr1 O1 71.17(7) . . ? O3 Pr1 O2 70.67(7) . . ? O4 Pr1 O2 77.48(7) . . ? O1 Pr1 O2 141.79(7) . . ? O3 Pr1 O6 59.22(6) . . ? O4 Pr1 O6 119.43(6) . . ? O1 Pr1 O6 76.52(7) . . ? O2 Pr1 O6 101.44(7) . . ? O3 Pr1 O5 120.75(6) . . ? O4 Pr1 O5 59.28(6) . . ? O1 Pr1 O5 70.96(7) . . ? O2 Pr1 O5 110.72(7) . . ? O6 Pr1 O5 145.71(6) . . ? O3 Pr1 Cl2 134.22(5) . . ? O4 Pr1 Cl2 134.04(5) . . ? O1 Pr1 Cl2 74.63(6) . . ? O2 Pr1 Cl2 143.33(5) . . ? O6 Pr1 Cl2 80.05(5) . . ? O5 Pr1 Cl2 81.15(5) . . ? O3 Pr1 Cl1 137.77(5) . 2_676 ? O4 Pr1 Cl1 98.08(5) . 2_676 ? O1 Pr1 Cl1 136.82(6) . 2_676 ? O2 Pr1 Cl1 68.08(5) . 2_676 ? O6 Pr1 Cl1 138.47(5) . 2_676 ? O5 Pr1 Cl1 67.95(5) . 2_676 ? Cl2 Pr1 Cl1 86.42(4) . 2_676 ? O3 Pr1 Cl1 101.74(5) . . ? O4 Pr1 Cl1 147.58(5) . . ? O1 Pr1 Cl1 136.52(5) . . ? O2 Pr1 Cl1 70.20(5) . . ? O6 Pr1 Cl1 66.32(5) . . ? O5 Pr1 Cl1 135.74(5) . . ? Cl2 Pr1 Cl1 77.37(3) . . ? Cl1 Pr1 Cl1 72.46(4) 2_676 . ? O3 Pr1 Zn1 32.05(4) . . ? O4 Pr1 Zn1 32.53(4) . . ? O1 Pr1 Zn1 66.25(5) . . ? O2 Pr1 Zn1 75.56(5) . . ? O6 Pr1 Zn1 87.65(5) . . ? O5 Pr1 Zn1 89.06(5) . . ? Cl2 Pr1 Zn1 140.74(2) . . ? Cl1 Pr1 Zn1 124.75(3) 2_676 . ? Cl1 Pr1 Zn1 130.72(2) . . ? O3 Zn1 O4 78.38(7) . . ? O3 Zn1 N1 142.08(8) . . ? O4 Zn1 N1 88.17(8) . . ? O3 Zn1 N2 87.66(8) . . ? O4 Zn1 N2 139.14(8) . . ? N1 Zn1 N2 79.66(9) . . ? O3 Zn1 Cl3 103.80(6) . . ? O4 Zn1 Cl3 113.37(7) . . ? N1 Zn1 Cl3 114.07(7) . . ? N2 Zn1 Cl3 107.19(7) . . ? O3 Zn1 Pr1 39.14(5) . . ? O4 Zn1 Pr1 39.97(5) . . ? N1 Zn1 Pr1 123.34(6) . . ? N2 Zn1 Pr1 121.18(6) . . ? Cl3 Zn1 Pr1 108.38(4) . . ? Pr1 Cl1 Pr1 107.54(4) 2_676 . ? C24 O1 Pr1 133.3(2) . . ? C24 O1 H1 113(3) . . ? Pr1 O1 H1 112(3) . . ? C9 O2 Pr1 130.03(19) . . ? C9 O2 H2 115(4) . . ? Pr1 O2 H2 107(4) . . ? C23 O3 Zn1 122.95(15) . . ? C23 O3 Pr1 127.82(14) . . ? Zn1 O3 Pr1 108.81(8) . . ? C17 O4 Zn1 122.73(16) . . ? C17 O4 Pr1 129.02(16) . . ? Zn1 O4 Pr1 107.51(8) . . ? C18 O5 C5 117.0(2) . . ? C18 O5 Pr1 117.37(16) . . ? C5 O5 Pr1 122.85(17) . . ? C16 O6 C6 116.2(2) . . ? C16 O6 Pr1 115.48(13) . . ? C6 O6 Pr1 126.68(16) . . ? C18 C1 C3 119.1(3) . . ? C18 C1 H1A 120.5 . . ? C3 C1 H1A 120.5 . . ? C15 C2 C11 120.7(3) . . ? C15 C2 H2A 119.6 . . ? C11 C2 H2A 119.6 . . ? C7 C3 C1 120.6(3) . . ? C7 C3 H3A 119.7 . . ? C1 C3 H3A 119.7 . . ? C8 C4 C10 120.5(3) . . ? C8 C4 H4A 119.8 . . ? C10 C4 H4A 119.8 . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O6 C6 H6A 109.5 . . ? O6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 C19 122.0(3) . . ? C3 C7 H7A 119.0 . . ? C19 C7 H7A 119.0 . . ? C4 C8 C14 121.0(3) . . ? C4 C8 H8A 119.5 . . ? C14 C8 H8A 119.5 . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C10 C4 119.8(2) . . ? C16 C10 H10A 120.1 . . ? C4 C10 H10A 120.1 . . ? C20 C11 C2 119.9(3) . . ? C20 C11 H11A 120.0 . . ? C2 C11 H11A 120.0 . . ? N1 C12 C19 126.1(2) . . ? N1 C12 H12A 117.0 . . ? C19 C12 H12A 117.0 . . ? C15 C13 N1 125.0(3) . . ? C15 C13 C22 118.9(3) . . ? N1 C13 C22 116.1(2) . . ? C23 C14 C8 118.7(2) . . ? C23 C14 C21 124.2(2) . . ? C8 C14 C21 117.0(2) . . ? C2 C15 C13 120.5(3) . . ? C2 C15 H15A 119.7 . . ? C13 C15 H15A 119.7 . . ? O6 C16 C10 126.1(2) . . ? O6 C16 C23 112.8(2) . . ? C10 C16 C23 121.1(3) . . ? O4 C17 C18 117.4(2) . . ? O4 C17 C19 123.6(3) . . ? C18 C17 C19 119.0(2) . . ? C1 C18 O5 124.9(3) . . ? C1 C18 C17 121.7(3) . . ? O5 C18 C17 113.4(2) . . ? C17 C19 C7 117.7(3) . . ? C17 C19 C12 124.1(2) . . ? C7 C19 C12 118.1(3) . . ? C11 C20 C22 120.5(3) . . ? C11 C20 H20A 119.7 . . ? C22 C20 H20A 119.7 . . ? N2 C21 C14 124.5(3) . . ? N2 C21 H21A 117.8 . . ? C14 C21 H21A 117.8 . . ? C20 C22 N2 125.0(3) . . ? C20 C22 C13 119.4(2) . . ? N2 C22 C13 115.6(2) . . ? O3 C23 C14 124.2(2) . . ? O3 C23 C16 116.9(2) . . ? C14 C23 C16 118.8(2) . . ? O1 C24 H24A 109.5 . . ? O1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 N1 C13 123.5(2) . . ? C12 N1 Zn1 124.0(2) . . ? C13 N1 Zn1 112.46(16) . . ? C21 N2 C22 122.3(2) . . ? C21 N2 Zn1 125.02(18) . . ? C22 N2 Zn1 112.30(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 Cl3 0.821(18) 2.50(3) 3.231(2) 148(4) 2_665 O1 H1 Cl3 0.821(18) 2.90(4) 3.348(3) 117(3) . O2 H2 Cl2 0.834(19) 2.43(3) 3.159(2) 146(5) 2_676 O2 H2 Cl1 0.834(19) 2.59(5) 3.077(3) 118(4) 2_676 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.457 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.086 # Attachment '- 2.CIF' data_cb _database_code_depnum_ccdc_archive 'CCDC 822891' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H25 Cl2 N2 O7 Tb Zn' _chemical_formula_weight 760.66 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0110(16) _cell_length_b 13.379(3) _cell_length_c 13.674(3) _cell_angle_alpha 74.93(3) _cell_angle_beta 83.71(3) _cell_angle_gamma 86.61(3) _cell_volume 1406.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 3.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13507 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6251 _reflns_number_gt 5311 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0551P)^2^+6.6641P] 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 6251 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 Tb1 Tb 0.23625(4) 0.75014(3) 0.21538(2) 0.03474(12) Uani 1 1 d . . . Zn1 Zn 0.12201(10) 0.78260(6) 0.45883(6) 0.03409(19) Uani 1 1 d . . . Cl1 Cl 0.3693(2) 0.84790(15) 0.47992(16) 0.0467(4) Uani 1 1 d . . . Cl2 Cl 0.4327(3) 0.75699(19) 0.04558(16) 0.0595(5) Uani 1 1 d . . . C1 C -0.1379(13) 1.1351(6) 0.1908(7) 0.060(2) Uani 1 1 d . . . H1A H -0.1898 1.1983 0.1617 0.072 Uiso 1 1 calc R . . C2 C -0.2717(11) 0.7113(7) 0.8009(6) 0.051(2) Uani 1 1 d . . . H2A H -0.3101 0.6779 0.8674 0.062 Uiso 1 1 calc R . . C3 C -0.1845(12) 1.0844(6) 0.2906(6) 0.052(2) Uani 1 1 d . . . H3A H -0.2673 1.1140 0.3285 0.063 Uiso 1 1 calc R . . C4 C 0.2557(12) 1.0068(7) 0.0291(6) 0.058(2) Uani 1 1 d . . . H4B H 0.3456 0.9673 0.0030 0.088 Uiso 1 1 calc R . . H4C H 0.2985 1.0696 0.0369 0.088 Uiso 1 1 calc R . . H4A H 0.1707 1.0235 -0.0174 0.088 Uiso 1 1 calc R . . C5 C 0.5187(12) 0.5218(7) 0.2258(7) 0.060(2) Uani 1 1 d . . . H5A H 0.6187 0.5006 0.2595 0.090 Uiso 1 1 calc R . . H5B H 0.5473 0.5678 0.1601 0.090 Uiso 1 1 calc R . . H5C H 0.4668 0.4620 0.2176 0.090 Uiso 1 1 calc R . . C6 C -0.0133(12) 1.0921(6) 0.1333(6) 0.052(2) Uani 1 1 d . . . H6A H 0.0186 1.1267 0.0661 0.062 Uiso 1 1 calc R . . C7 C 0.2240(9) 0.4201(5) 0.5799(6) 0.0395(15) Uani 1 1 d . . . H7A H 0.1808 0.3867 0.6455 0.047 Uiso 1 1 calc R . . C8 C -0.1073(10) 0.9871(5) 0.3366(5) 0.0392(15) Uani 1 1 d . . . C9 C -0.3333(11) 0.8099(7) 0.7568(6) 0.053(2) Uani 1 1 d . . . H9A H -0.4127 0.8421 0.7943 0.064 Uiso 1 1 calc R . . C10 C -0.2790(10) 0.8610(6) 0.6582(6) 0.0475(18) Uani 1 1 d . . . H10A H -0.3231 0.9267 0.6297 0.057 Uiso 1 1 calc R . . C11 C 0.0622(10) 0.9983(5) 0.1764(5) 0.0393(15) Uani 1 1 d . . . C12 C -0.0003(10) 0.6728(6) 0.1294(6) 0.0454(17) Uani 1 1 d . . . C13 C 0.3956(9) 0.4148(6) 0.4273(6) 0.0428(17) Uani 1 1 d . . . H13A H 0.4697 0.3783 0.3909 0.051 Uiso 1 1 calc R . . C14 C -0.1667(9) 0.9376(5) 0.4412(5) 0.0385(15) Uani 1 1 d . . . H14A H -0.2656 0.9644 0.4684 0.046 Uiso 1 1 calc R . . C15 C 0.1788(8) 0.5252(5) 0.5381(5) 0.0313(13) Uani 1 1 d . . . C16 C 0.3308(9) 0.3672(6) 0.5245(6) 0.0440(17) Uani 1 1 d . . . H16A H 0.3598 0.2982 0.5529 0.053 Uiso 1 1 calc R . . C17 C -0.1576(8) 0.8145(5) 0.6006(5) 0.0342(14) Uani 1 1 d . . . C18 C 0.0145(9) 0.9434(5) 0.2771(5) 0.0341(14) Uani 1 1 d . . . C19 C 0.2404(8) 0.5736(5) 0.4376(5) 0.0309(13) Uani 1 1 d . . . C20 C -0.1538(10) 0.6630(6) 0.7465(6) 0.0452(17) Uani 1 1 d . . . H20A H -0.1130 0.5966 0.7758 0.054 Uiso 1 1 calc R . . C21 C 0.3513(8) 0.5163(5) 0.3835(5) 0.0342(14) Uani 1 1 d . . . C22 C -0.0949(9) 0.7143(5) 0.6461(5) 0.0343(14) Uani 1 1 d . . . C23 C 0.6312(15) 0.8517(12) 0.2213(9) 0.099(5) Uani 1 1 d . . . H23A H 0.6882 0.8736 0.2700 0.149 Uiso 1 1 calc R . . H23B H 0.6247 0.9078 0.1614 0.149 Uiso 1 1 calc R . . H23C H 0.6920 0.7939 0.2036 0.149 Uiso 1 1 calc R . . C24 C 0.0623(8) 0.5736(5) 0.6014(5) 0.0325(13) Uani 1 1 d . . . H24A H 0.0095 0.5309 0.6601 0.039 Uiso 1 1 calc R . . C25 C -0.0952(15) 0.6324(9) 0.0575(9) 0.081(3) Uani 1 1 d . . . H25A H -0.1944 0.6751 0.0422 0.122 Uiso 1 1 calc R . . H25B H -0.1264 0.5624 0.0893 0.122 Uiso 1 1 calc R . . H25C H -0.0244 0.6344 -0.0043 0.122 Uiso 1 1 calc R . . N1 N -0.0935(7) 0.8594(4) 0.4996(4) 0.0358(12) Uani 1 1 d . . . N2 N 0.0261(7) 0.6710(4) 0.5832(4) 0.0340(12) Uani 1 1 d . . . O1 O 0.0864(8) 0.6103(4) 0.1902(5) 0.0575(15) Uani 1 1 d . . . O2 O -0.0015(8) 0.7675(4) 0.1212(5) 0.0541(14) Uani 1 1 d . . . O3 O 0.1992(6) 0.6699(3) 0.3880(3) 0.0371(11) Uani 1 1 d . . . O4 O 0.0872(6) 0.8494(4) 0.3105(4) 0.0394(11) Uani 1 1 d . . . O5 O 0.1843(7) 0.9469(4) 0.1264(4) 0.0458(12) Uani 1 1 d . . . O6 O 0.4039(6) 0.5742(4) 0.2856(4) 0.0420(11) Uani 1 1 d . . . O7 O 0.4689(7) 0.8223(5) 0.2636(5) 0.0578(15) Uani 1 1 d . . . H7 H 0.4644 0.7856 0.3285 0.087 Uiso 1 1 d 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 Tb1 0.03859(19) 0.03545(19) 0.02666(17) -0.00321(12) 0.00122(12) -0.00238(13) Zn1 0.0396(4) 0.0296(4) 0.0286(4) -0.0017(3) 0.0005(3) 0.0020(3) Cl1 0.0430(9) 0.0487(10) 0.0532(11) -0.0226(8) -0.0042(8) 0.0017(8) Cl2 0.0673(13) 0.0665(13) 0.0393(10) -0.0107(9) 0.0139(9) -0.0057(11) C1 0.094(7) 0.035(4) 0.045(5) 0.003(3) -0.015(4) 0.018(4) C2 0.062(5) 0.063(5) 0.026(4) -0.009(3) 0.007(3) -0.015(4) C3 0.071(5) 0.040(4) 0.043(4) -0.008(3) -0.011(4) 0.017(4) C4 0.068(5) 0.055(5) 0.041(4) 0.006(4) 0.010(4) -0.015(4) C5 0.063(5) 0.057(5) 0.056(5) -0.017(4) 0.016(4) 0.008(4) C6 0.075(6) 0.033(4) 0.039(4) 0.006(3) -0.006(4) -0.001(4) C7 0.044(4) 0.032(3) 0.040(4) -0.003(3) -0.008(3) 0.001(3) C8 0.050(4) 0.031(3) 0.035(4) -0.007(3) -0.009(3) 0.007(3) C9 0.056(5) 0.063(5) 0.044(5) -0.024(4) 0.005(4) -0.001(4) C10 0.051(4) 0.047(4) 0.046(4) -0.018(3) 0.002(3) 0.004(4) C11 0.050(4) 0.032(3) 0.034(4) -0.005(3) -0.004(3) -0.004(3) C12 0.043(4) 0.047(4) 0.042(4) -0.003(3) -0.004(3) -0.006(3) C13 0.038(4) 0.037(4) 0.053(5) -0.013(3) -0.008(3) 0.009(3) C14 0.047(4) 0.033(3) 0.036(4) -0.011(3) -0.002(3) 0.005(3) C15 0.030(3) 0.028(3) 0.033(3) -0.003(2) -0.004(2) -0.001(3) C16 0.043(4) 0.033(3) 0.053(5) -0.007(3) -0.010(3) 0.009(3) C17 0.038(3) 0.036(3) 0.030(3) -0.011(3) -0.002(3) -0.004(3) C18 0.040(3) 0.026(3) 0.033(3) 0.000(2) -0.008(3) 0.000(3) C19 0.029(3) 0.029(3) 0.034(3) -0.006(2) -0.007(2) -0.003(3) C20 0.056(4) 0.042(4) 0.034(4) -0.006(3) 0.002(3) -0.005(3) C21 0.030(3) 0.036(3) 0.037(4) -0.007(3) -0.006(3) -0.001(3) C22 0.041(4) 0.032(3) 0.028(3) -0.006(3) -0.003(3) -0.003(3) C23 0.074(7) 0.166(14) 0.055(7) -0.022(8) 0.011(5) -0.044(8) C24 0.035(3) 0.032(3) 0.028(3) -0.003(2) -0.003(2) -0.003(3) C25 0.084(7) 0.084(8) 0.086(8) -0.026(6) -0.028(6) -0.022(6) N1 0.041(3) 0.030(3) 0.032(3) -0.004(2) 0.000(2) 0.004(2) N2 0.037(3) 0.032(3) 0.029(3) -0.003(2) -0.002(2) 0.003(2) O1 0.074(4) 0.039(3) 0.055(4) 0.002(3) -0.016(3) -0.008(3) O2 0.060(3) 0.044(3) 0.056(4) -0.003(3) -0.019(3) -0.001(3) O3 0.051(3) 0.027(2) 0.029(2) -0.0029(18) -0.001(2) 0.006(2) O4 0.049(3) 0.035(2) 0.028(2) -0.0008(19) -0.001(2) 0.009(2) O5 0.058(3) 0.040(3) 0.031(3) 0.002(2) 0.007(2) -0.005(2) O6 0.042(3) 0.044(3) 0.035(3) -0.007(2) 0.002(2) 0.007(2) O7 0.044(3) 0.085(4) 0.046(3) -0.021(3) 0.004(2) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.291(5) . ? Tb1 O3 2.319(5) . ? Tb1 O7 2.378(6) . ? Tb1 O2 2.381(6) . ? Tb1 O1 2.398(6) . ? Tb1 O5 2.627(5) . ? Tb1 Cl2 2.643(2) . ? Tb1 O6 2.646(5) . ? Tb1 C12 2.720(8) . ? Tb1 Zn1 3.4850(12) . ? Zn1 O3 2.028(5) . ? Zn1 O4 2.036(5) . ? Zn1 N1 2.055(6) . ? Zn1 N2 2.059(6) . ? Zn1 Cl1 2.288(2) . ? C1 C3 1.378(12) . ? C1 C6 1.393(13) . ? C2 C20 1.374(11) . ? C2 C9 1.386(12) . ? C3 C8 1.428(9) . ? C4 O5 1.440(9) . ? C5 O6 1.437(9) . ? C6 C11 1.375(10) . ? C7 C16 1.369(11) . ? C7 C15 1.415(9) . ? C8 C18 1.401(10) . ? C8 C14 1.451(10) . ? C9 C10 1.378(12) . ? C10 C17 1.403(10) . ? C11 O5 1.384(9) . ? C11 C18 1.405(10) . ? C12 O2 1.242(10) . ? C12 O1 1.253(9) . ? C12 C25 1.524(13) . ? C13 C16 1.375(11) . ? C13 C21 1.377(9) . ? C14 N1 1.293(9) . ? C15 C19 1.407(9) . ? C15 C24 1.444(9) . ? C17 N1 1.409(9) . ? C17 C22 1.410(9) . ? C18 O4 1.342(7) . ? C19 O3 1.332(7) . ? C19 C21 1.412(9) . ? C20 C22 1.409(10) . ? C21 O6 1.394(8) . ? C22 N2 1.424(9) . ? C23 O7 1.399(12) . ? C24 N2 1.282(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O3 66.11(16) . . ? O4 Tb1 O7 82.3(2) . . ? O3 Tb1 O7 82.7(2) . . ? O4 Tb1 O2 87.1(2) . . ? O3 Tb1 O2 117.6(2) . . ? O7 Tb1 O2 150.8(2) . . ? O4 Tb1 O1 115.2(2) . . ? O3 Tb1 O1 86.80(19) . . ? O7 Tb1 O1 153.7(2) . . ? O2 Tb1 O1 54.24(19) . . ? O4 Tb1 O5 62.68(16) . . ? O3 Tb1 O5 127.47(16) . . ? O7 Tb1 O5 79.9(2) . . ? O2 Tb1 O5 71.11(19) . . ? O1 Tb1 O5 125.04(19) . . ? O4 Tb1 Cl2 144.06(13) . . ? O3 Tb1 Cl2 144.05(13) . . ? O7 Tb1 Cl2 83.95(15) . . ? O2 Tb1 Cl2 88.93(17) . . ? O1 Tb1 Cl2 90.69(17) . . ? O5 Tb1 Cl2 82.29(13) . . ? O4 Tb1 O6 126.51(15) . . ? O3 Tb1 O6 61.21(15) . . ? O7 Tb1 O6 82.6(2) . . ? O2 Tb1 O6 124.86(19) . . ? O1 Tb1 O6 71.18(18) . . ? O5 Tb1 O6 158.77(17) . . ? Cl2 Tb1 O6 84.06(12) . . ? O4 Tb1 C12 104.8(2) . . ? O3 Tb1 C12 105.8(2) . . ? O7 Tb1 C12 170.5(2) . . ? O2 Tb1 C12 27.2(2) . . ? O1 Tb1 C12 27.4(2) . . ? O5 Tb1 C12 97.6(2) . . ? Cl2 Tb1 C12 86.63(18) . . ? O6 Tb1 C12 97.7(2) . . ? O4 Tb1 Zn1 33.93(11) . . ? O3 Tb1 Zn1 33.92(11) . . ? O7 Tb1 Zn1 72.95(14) . . ? O2 Tb1 Zn1 111.31(16) . . ? O1 Tb1 Zn1 109.93(16) . . ? O5 Tb1 Zn1 93.56(12) . . ? Cl2 Tb1 Zn1 156.90(6) . . ? O6 Tb1 Zn1 92.65(11) . . ? C12 Tb1 Zn1 116.46(17) . . ? O3 Zn1 O4 76.46(19) . . ? O3 Zn1 N1 140.6(2) . . ? O4 Zn1 N1 88.4(2) . . ? O3 Zn1 N2 89.3(2) . . ? O4 Zn1 N2 141.6(2) . . ? N1 Zn1 N2 80.3(2) . . ? O3 Zn1 Cl1 102.95(16) . . ? O4 Zn1 Cl1 103.78(17) . . ? N1 Zn1 Cl1 115.98(18) . . ? N2 Zn1 Cl1 114.21(17) . . ? O3 Zn1 Tb1 39.65(13) . . ? O4 Zn1 Tb1 38.92(13) . . ? N1 Zn1 Tb1 124.43(17) . . ? N2 Zn1 Tb1 126.07(17) . . ? Cl1 Zn1 Tb1 97.29(6) . . ? C3 C1 C6 120.3(7) . . ? C20 C2 C9 120.0(7) . . ? C1 C3 C8 120.8(8) . . ? C11 C6 C1 119.6(7) . . ? C16 C7 C15 120.4(7) . . ? C18 C8 C3 118.3(7) . . ? C18 C8 C14 124.3(6) . . ? C3 C8 C14 117.3(7) . . ? C10 C9 C2 121.2(7) . . ? C9 C10 C17 120.4(7) . . ? C6 C11 O5 124.9(7) . . ? C6 C11 C18 121.5(7) . . ? O5 C11 C18 113.5(6) . . ? O2 C12 O1 121.7(8) . . ? O2 C12 C25 119.1(8) . . ? O1 C12 C25 119.0(8) . . ? O2 C12 Tb1 61.0(4) . . ? O1 C12 Tb1 61.8(4) . . ? C25 C12 Tb1 164.4(7) . . ? C16 C13 C21 120.3(7) . . ? N1 C14 C8 125.4(6) . . ? C19 C15 C7 119.2(6) . . ? C19 C15 C24 124.4(6) . . ? C7 C15 C24 116.3(6) . . ? C7 C16 C13 120.8(7) . . ? C10 C17 N1 125.1(6) . . ? C10 C17 C22 118.1(6) . . ? N1 C17 C22 116.7(6) . . ? O4 C18 C8 123.3(6) . . ? O4 C18 C11 117.3(6) . . ? C8 C18 C11 119.3(6) . . ? O3 C19 C15 124.7(6) . . ? O3 C19 C21 116.8(6) . . ? C15 C19 C21 118.5(6) . . ? C2 C20 C22 119.8(7) . . ? C13 C21 O6 126.9(6) . . ? C13 C21 C19 120.8(7) . . ? O6 C21 C19 112.3(6) . . ? C20 C22 C17 120.5(6) . . ? C20 C22 N2 124.2(6) . . ? C17 C22 N2 115.3(6) . . ? N2 C24 C15 125.1(6) . . ? C14 N1 C17 122.8(6) . . ? C14 N1 Zn1 125.8(5) . . ? C17 N1 Zn1 111.4(4) . . ? C24 N2 C22 122.8(6) . . ? C24 N2 Zn1 125.7(5) . . ? C22 N2 Zn1 111.4(4) . . ? C12 O1 Tb1 90.7(5) . . ? C12 O2 Tb1 91.8(5) . . ? C19 O3 Zn1 123.3(4) . . ? C19 O3 Tb1 129.7(4) . . ? Zn1 O3 Tb1 106.43(19) . . ? C18 O4 Zn1 124.2(4) . . ? C18 O4 Tb1 127.7(4) . . ? Zn1 O4 Tb1 107.15(19) . . ? C11 O5 C4 115.3(6) . . ? C11 O5 Tb1 115.5(4) . . ? C4 O5 Tb1 129.0(5) . . ? C21 O6 C5 115.8(6) . . ? C21 O6 Tb1 117.1(4) . . ? C5 O6 Tb1 125.7(5) . . ? C23 O7 Tb1 137.1(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 Cl1 0.89 2.46 3.079(6) 127.0 . O7 H7 O3 0.89 2.63 3.103(8) 113.9 . _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.389 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.175 # Attachment '- 3.CIF' data_cc _database_code_depnum_ccdc_archive 'CCDC 822892' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H25 Cl2 Dy N2 O7 Zn' _chemical_formula_weight 764.24 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' Zn Zn 0.2839 1.4301 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.990(3) _cell_length_b 13.377(5) _cell_length_c 13.685(5) _cell_angle_alpha 74.414(6) _cell_angle_beta 83.644(7) _cell_angle_gamma 86.540(7) _cell_volume 1399.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rodlike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 3.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 SMART1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9927 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.74 _reflns_number_total 6799 _reflns_number_gt 4489 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.1860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6799 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2757 _refine_ls_wR_factor_gt 0.2232 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.23654(7) 0.74966(4) 0.21527(3) 0.0382(2) Uani 1 1 d . . . Zn1 Zn 0.12214(17) 0.78260(9) 0.45857(8) 0.0356(3) Uani 1 1 d . . . Cl1 Cl 0.3692(4) 0.8481(2) 0.4800(2) 0.0482(7) Uani 1 1 d . . . Cl2 Cl 0.4332(5) 0.7549(3) 0.0454(2) 0.0595(9) Uani 1 1 d . . . C1 C -0.137(2) 1.1344(11) 0.1897(10) 0.065(4) Uani 1 1 d . . . H1A H -0.1872 1.1985 0.1610 0.079 Uiso 1 1 calc R . . C2 C -0.2710(18) 0.7109(11) 0.7994(9) 0.051(3) Uani 1 1 d . . . H2A H -0.3075 0.6760 0.8661 0.061 Uiso 1 1 calc R . . C3 C -0.186(2) 1.0835(10) 0.2895(10) 0.055(3) Uani 1 1 d . . . H3A H -0.2719 1.1119 0.3266 0.066 Uiso 1 1 calc R . . C4 C 0.257(2) 1.0051(10) 0.0269(9) 0.060(4) Uani 1 1 d . . . H4B H 0.3075 1.0664 0.0330 0.090 Uiso 1 1 calc R . . H4C H 0.1709 1.0248 -0.0187 0.090 Uiso 1 1 calc R . . H4A H 0.3421 0.9627 0.0005 0.090 Uiso 1 1 calc R . . C5 C 0.515(2) 0.5224(12) 0.2267(11) 0.065(4) Uani 1 1 d . . . H5A H 0.6153 0.4996 0.2606 0.098 Uiso 1 1 calc R . . H5B H 0.5450 0.5690 0.1611 0.098 Uiso 1 1 calc R . . H5C H 0.4615 0.4634 0.2182 0.098 Uiso 1 1 calc R . . C6 C -0.0191(19) 1.0946(9) 0.1335(9) 0.052(3) Uani 1 1 d . . . H6A H 0.0087 1.1302 0.0658 0.062 Uiso 1 1 calc R . . C7 C 0.2209(17) 0.4207(8) 0.5800(9) 0.044(3) Uani 1 1 d . . . H7A H 0.1783 0.3865 0.6457 0.052 Uiso 1 1 calc R . . C8 C -0.1051(15) 0.9870(8) 0.3356(8) 0.037(2) Uani 1 1 d . . . C9 C -0.3399(17) 0.8123(12) 0.7579(9) 0.055(3) Uani 1 1 d . . . H9A H -0.4203 0.8444 0.7949 0.067 Uiso 1 1 calc R . . C10 C -0.277(2) 0.8606(11) 0.6563(9) 0.057(4) Uani 1 1 d . . . H10A H -0.3172 0.9272 0.6259 0.068 Uiso 1 1 calc R . . C11 C 0.0655(17) 0.9977(9) 0.1756(8) 0.042(3) Uani 1 1 d . . . C12 C -0.0002(15) 0.6761(10) 0.1281(9) 0.045(3) Uani 1 1 d . . . C13 C 0.3958(18) 0.4147(10) 0.4266(9) 0.049(3) Uani 1 1 d . . . H13A H 0.4709 0.3785 0.3906 0.059 Uiso 1 1 calc R . . C14 C -0.1708(18) 0.9383(10) 0.4414(8) 0.047(3) Uani 1 1 d . . . H14A H -0.2713 0.9637 0.4683 0.057 Uiso 1 1 calc R . . C15 C 0.1722(16) 0.5263(9) 0.5406(8) 0.040(3) Uani 1 1 d . . . C16 C 0.327(2) 0.3671(9) 0.5262(10) 0.055(4) Uani 1 1 d . . . H16A H 0.3548 0.2978 0.5558 0.066 Uiso 1 1 calc R . . C17 C -0.1610(16) 0.8138(9) 0.6015(8) 0.041(3) Uani 1 1 d . . . C18 C 0.0150(17) 0.9425(8) 0.2772(8) 0.042(3) Uani 1 1 d . . . C19 C 0.2436(14) 0.5733(8) 0.4358(8) 0.035(2) Uani 1 1 d . . . C20 C -0.1550(17) 0.6634(10) 0.7462(8) 0.045(3) Uani 1 1 d . . . H20A H -0.1145 0.5968 0.7763 0.054 Uiso 1 1 calc R . . C21 C 0.3482(15) 0.5171(8) 0.3835(8) 0.035(2) Uani 1 1 d . . . C22 C -0.0954(14) 0.7140(8) 0.6459(7) 0.035(2) Uani 1 1 d . . . C23 C 0.627(3) 0.856(2) 0.2204(13) 0.117(10) Uani 1 1 d . . . H23A H 0.6835 0.8780 0.2693 0.176 Uiso 1 1 calc R . . H23B H 0.6138 0.9141 0.1623 0.176 Uiso 1 1 calc R . . H23C H 0.6933 0.8019 0.1993 0.176 Uiso 1 1 calc R . . C24 C 0.0618(15) 0.5735(8) 0.6008(7) 0.036(2) Uani 1 1 d . . . H24A H 0.0092 0.5305 0.6599 0.043 Uiso 1 1 calc R . . C25 C -0.090(2) 0.6316(14) 0.0555(13) 0.083(6) Uani 1 1 d . . . H25A H -0.2068 0.6521 0.0593 0.125 Uiso 1 1 calc R . . H25B H -0.0782 0.5572 0.0750 0.125 Uiso 1 1 calc R . . H25C H -0.0392 0.6578 -0.0131 0.125 Uiso 1 1 calc R . . N1 N -0.0897(13) 0.8597(7) 0.4984(6) 0.039(2) Uani 1 1 d . . . N2 N 0.0250(12) 0.6707(7) 0.5831(6) 0.036(2) Uani 1 1 d . . . O1 O 0.0887(15) 0.6104(7) 0.1888(7) 0.063(3) Uani 1 1 d . . . O2 O -0.0032(14) 0.7690(7) 0.1210(7) 0.063(3) Uani 1 1 d . . . O3 O 0.1934(11) 0.6709(6) 0.3890(5) 0.0380(17) Uani 1 1 d . . . O4 O 0.0862(11) 0.8499(6) 0.3100(5) 0.0418(19) Uani 1 1 d . . . O5 O 0.1842(13) 0.9470(6) 0.1266(6) 0.048(2) Uani 1 1 d . . . O6 O 0.4047(11) 0.5736(6) 0.2854(6) 0.0428(18) Uani 1 1 d . . . O7 O 0.4716(11) 0.8199(8) 0.2639(7) 0.055(2) Uani 1 1 d . . . H7 H 0.4671 0.7832 0.3288 0.082 Uiso 1 1 d 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 0.0459(4) 0.0388(3) 0.0260(3) -0.0016(2) 0.0011(2) -0.0114(2) Zn1 0.0462(8) 0.0310(6) 0.0251(6) 0.0000(4) 0.0004(5) -0.0072(5) Cl1 0.0519(18) 0.0493(16) 0.0480(15) -0.0205(13) -0.0018(13) -0.0093(13) Cl2 0.065(2) 0.070(2) 0.0352(14) -0.0086(14) 0.0161(14) -0.0071(17) C1 0.102(13) 0.043(7) 0.041(7) 0.003(5) -0.003(7) 0.006(8) C2 0.064(9) 0.058(8) 0.029(5) -0.012(5) 0.007(5) -0.014(7) C3 0.075(10) 0.049(7) 0.039(6) -0.008(5) -0.004(6) 0.001(7) C4 0.087(11) 0.044(7) 0.037(6) 0.007(5) 0.009(6) -0.015(7) C5 0.083(12) 0.059(9) 0.046(7) -0.007(6) 0.007(7) 0.006(8) C6 0.080(10) 0.030(6) 0.035(6) 0.009(4) -0.007(6) -0.003(6) C7 0.062(8) 0.028(5) 0.039(6) -0.004(4) -0.011(5) -0.006(5) C8 0.050(7) 0.031(5) 0.030(5) -0.004(4) -0.007(5) -0.004(5) C9 0.045(8) 0.080(10) 0.037(6) -0.010(6) 0.009(5) -0.013(7) C10 0.086(11) 0.054(8) 0.028(5) -0.005(5) 0.006(6) -0.018(7) C11 0.063(8) 0.033(5) 0.028(5) -0.002(4) -0.006(5) -0.016(5) C12 0.031(6) 0.052(7) 0.043(6) 0.005(5) -0.007(5) -0.009(5) C13 0.057(8) 0.049(7) 0.043(6) -0.013(5) -0.007(6) -0.010(6) C14 0.058(8) 0.052(7) 0.031(5) -0.007(5) -0.007(5) -0.013(6) C15 0.045(7) 0.039(6) 0.033(5) 0.001(4) -0.011(5) -0.017(5) C16 0.074(10) 0.031(6) 0.054(7) 0.007(5) -0.028(7) -0.007(6) C17 0.053(7) 0.042(6) 0.026(5) -0.004(4) 0.001(5) -0.024(5) C18 0.071(9) 0.026(5) 0.027(5) 0.001(4) -0.014(5) -0.014(5) C19 0.040(6) 0.031(5) 0.031(5) -0.001(4) -0.007(4) -0.012(4) C20 0.059(8) 0.048(7) 0.026(5) -0.006(4) 0.008(5) -0.019(6) C21 0.044(6) 0.033(5) 0.029(5) -0.004(4) -0.009(4) -0.009(5) C22 0.040(6) 0.036(5) 0.027(4) -0.003(4) 0.002(4) -0.018(5) C23 0.115(17) 0.19(2) 0.048(9) -0.018(11) 0.014(10) -0.102(18) C24 0.049(7) 0.031(5) 0.022(4) 0.004(4) -0.004(4) -0.012(5) C25 0.087(14) 0.090(13) 0.070(10) -0.006(9) -0.023(10) -0.025(11) N1 0.060(6) 0.027(4) 0.026(4) 0.001(3) -0.005(4) -0.011(4) N2 0.044(5) 0.037(5) 0.025(4) -0.002(3) 0.000(4) -0.014(4) O1 0.090(8) 0.047(5) 0.048(5) 0.003(4) -0.017(5) -0.029(5) O2 0.081(8) 0.044(5) 0.061(6) 0.005(4) -0.031(5) -0.018(5) O3 0.052(5) 0.032(4) 0.026(3) -0.004(3) 0.002(3) 0.000(3) O4 0.057(5) 0.037(4) 0.024(3) 0.007(3) 0.000(3) -0.012(4) O5 0.075(7) 0.033(4) 0.030(4) 0.005(3) 0.000(4) -0.013(4) O6 0.051(5) 0.043(4) 0.032(4) -0.008(3) 0.004(3) -0.004(4) O7 0.039(5) 0.083(7) 0.045(5) -0.025(5) 0.014(4) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O4 2.306(9) . ? Dy1 O3 2.324(7) . ? Dy1 O7 2.383(9) . ? Dy1 O2 2.389(9) . ? Dy1 O1 2.392(8) . ? Dy1 O5 2.622(8) . ? Dy1 O6 2.639(9) . ? Dy1 Cl2 2.645(3) . ? Dy1 C12 2.706(11) . ? Dy1 Zn1 3.4903(18) . ? Zn1 O3 2.001(8) . ? Zn1 N1 2.028(11) . ? Zn1 O4 2.035(7) . ? Zn1 N2 2.055(8) . ? Zn1 Cl1 2.286(3) . ? C1 C6 1.33(2) . ? C1 C3 1.378(19) . ? C2 C20 1.350(19) . ? C2 C9 1.42(2) . ? C3 C8 1.427(17) . ? C4 O5 1.455(14) . ? C5 O6 1.401(17) . ? C6 C11 1.431(17) . ? C7 C16 1.36(2) . ? C7 C15 1.416(16) . ? C8 C18 1.389(18) . ? C8 C14 1.470(15) . ? C9 C10 1.416(17) . ? C10 C17 1.36(2) . ? C11 O5 1.354(16) . ? C11 C18 1.415(15) . ? C12 O2 1.219(16) . ? C12 O1 1.276(15) . ? C12 C25 1.542(19) . ? C13 C21 1.387(17) . ? C13 C16 1.405(19) . ? C14 N1 1.313(15) . ? C15 C24 1.381(18) . ? C15 C19 1.468(15) . ? C17 C22 1.407(17) . ? C17 N1 1.446(13) . ? C18 O4 1.316(14) . ? C19 O3 1.349(12) . ? C19 C21 1.363(17) . ? C20 C22 1.402(14) . ? C21 O6 1.392(13) . ? C22 N2 1.420(15) . ? C23 O7 1.375(19) . ? C24 N2 1.279(14) . ? 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 O4 Dy1 O3 65.1(3) . . ? O4 Dy1 O7 82.7(3) . . ? O3 Dy1 O7 82.9(3) . . ? O4 Dy1 O2 86.6(4) . . ? O3 Dy1 O2 116.6(3) . . ? O7 Dy1 O2 151.0(3) . . ? O4 Dy1 O1 115.9(4) . . ? O3 Dy1 O1 87.6(3) . . ? O7 Dy1 O1 152.9(4) . . ? O2 Dy1 O1 54.6(3) . . ? O4 Dy1 O5 62.1(3) . . ? O3 Dy1 O5 126.0(3) . . ? O7 Dy1 O5 80.3(3) . . ? O2 Dy1 O5 70.9(3) . . ? O1 Dy1 O5 125.0(3) . . ? O4 Dy1 O6 126.9(2) . . ? O3 Dy1 O6 62.8(3) . . ? O7 Dy1 O6 82.0(3) . . ? O2 Dy1 O6 125.3(3) . . ? O1 Dy1 O6 71.2(3) . . ? O5 Dy1 O6 158.7(3) . . ? O4 Dy1 Cl2 144.48(19) . . ? O3 Dy1 Cl2 145.1(2) . . ? O7 Dy1 Cl2 84.3(2) . . ? O2 Dy1 Cl2 89.0(3) . . ? O1 Dy1 Cl2 89.3(3) . . ? O5 Dy1 Cl2 83.2(2) . . ? O6 Dy1 Cl2 83.36(19) . . ? O4 Dy1 C12 104.5(4) . . ? O3 Dy1 C12 106.2(3) . . ? O7 Dy1 C12 170.2(3) . . ? O2 Dy1 C12 26.8(3) . . ? O1 Dy1 C12 28.1(3) . . ? O5 Dy1 C12 96.9(3) . . ? O6 Dy1 C12 98.5(3) . . ? Cl2 Dy1 C12 86.0(3) . . ? O4 Dy1 Zn1 33.90(17) . . ? O3 Dy1 Zn1 33.16(19) . . ? O7 Dy1 Zn1 72.8(2) . . ? O2 Dy1 Zn1 111.0(3) . . ? O1 Dy1 Zn1 111.0(3) . . ? O5 Dy1 Zn1 92.90(19) . . ? O6 Dy1 Zn1 93.11(17) . . ? Cl2 Dy1 Zn1 157.13(9) . . ? C12 Dy1 Zn1 116.9(3) . . ? O3 Zn1 N1 139.9(3) . . ? O3 Zn1 O4 76.2(3) . . ? N1 Zn1 O4 88.2(4) . . ? O3 Zn1 N2 88.9(3) . . ? N1 Zn1 N2 80.5(4) . . ? O4 Zn1 N2 141.1(3) . . ? O3 Zn1 Cl1 104.5(3) . . ? N1 Zn1 Cl1 115.2(3) . . ? O4 Zn1 Cl1 104.2(2) . . ? N2 Zn1 Cl1 114.3(3) . . ? O3 Zn1 Dy1 39.4(2) . . ? N1 Zn1 Dy1 124.6(2) . . ? O4 Zn1 Dy1 39.2(3) . . ? N2 Zn1 Dy1 125.7(3) . . ? Cl1 Zn1 Dy1 97.78(9) . . ? C6 C1 C3 121.9(14) . . ? C20 C2 C9 122.9(11) . . ? C1 C3 C8 119.5(14) . . ? C1 C6 C11 120.9(11) . . ? C16 C7 C15 123.1(11) . . ? C18 C8 C3 119.5(10) . . ? C18 C8 C14 125.4(10) . . ? C3 C8 C14 114.9(12) . . ? C10 C9 C2 115.2(13) . . ? C17 C10 C9 122.7(14) . . ? O5 C11 C18 114.2(11) . . ? O5 C11 C6 127.2(10) . . ? C18 C11 C6 118.5(13) . . ? O2 C12 O1 122.9(11) . . ? O2 C12 C25 121.6(11) . . ? O1 C12 C25 115.2(13) . . ? O2 C12 Dy1 61.9(6) . . ? O1 C12 Dy1 62.1(6) . . ? C25 C12 Dy1 162.8(11) . . ? C21 C13 C16 118.1(13) . . ? N1 C14 C8 121.0(12) . . ? C24 C15 C7 118.7(10) . . ? C24 C15 C19 126.7(10) . . ? C7 C15 C19 114.6(12) . . ? C7 C16 C13 121.0(12) . . ? C10 C17 C22 120.1(10) . . ? C10 C17 N1 125.4(11) . . ? C22 C17 N1 114.4(11) . . ? O4 C18 C8 124.1(9) . . ? O4 C18 C11 116.4(12) . . ? C8 C18 C11 119.5(11) . . ? O3 C19 C21 120.1(9) . . ? O3 C19 C15 118.8(10) . . ? C21 C19 C15 120.9(10) . . ? C2 C20 C22 120.3(13) . . ? C19 C21 C13 122.3(10) . . ? C19 C21 O6 113.4(9) . . ? C13 C21 O6 124.3(11) . . ? C20 C22 C17 118.8(12) . . ? C20 C22 N2 124.8(11) . . ? C17 C22 N2 116.4(9) . . ? N2 C24 C15 126.2(10) . . ? C14 N1 C17 118.8(11) . . ? C14 N1 Zn1 128.4(8) . . ? C17 N1 Zn1 112.7(8) . . ? C24 N2 C22 123.5(9) . . ? C24 N2 Zn1 125.0(8) . . ? C22 N2 Zn1 111.5(7) . . ? C12 O1 Dy1 89.8(7) . . ? C12 O2 Dy1 91.3(7) . . ? C19 O3 Zn1 125.4(6) . . ? C19 O3 Dy1 125.7(7) . . ? Zn1 O3 Dy1 107.4(3) . . ? C18 O4 Zn1 123.9(7) . . ? C18 O4 Dy1 128.1(7) . . ? Zn1 O4 Dy1 106.9(4) . . ? C11 O5 C4 116.7(10) . . ? C11 O5 Dy1 116.0(6) . . ? C4 O5 Dy1 127.1(8) . . ? C21 O6 C5 117.3(10) . . ? C21 O6 Dy1 115.3(7) . . ? C5 O6 Dy1 125.7(7) . . ? C23 O7 Dy1 137.8(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 Cl1 0.89 2.48 3.096(9) 126.3 . O7 H7 O3 0.89 2.66 3.115(12) 113.2 . _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 2.986 _refine_diff_density_min -3.450 _refine_diff_density_rms 0.391 # Attachment '- 4.CIF' data_cd _database_code_depnum_ccdc_archive 'CCDC 822893' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 Cl4 Lu4 N4 O22 Zn' _chemical_formula_weight 1998.09 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' Cl Cl 0.1484 0.1585 '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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.979(6) _cell_length_b 13.200(7) _cell_length_c 13.260(7) _cell_angle_alpha 116.241(7) _cell_angle_beta 91.775(8) _cell_angle_gamma 104.446(8) _cell_volume 1796.9(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 5.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.583 _exptl_absorpt_process_details SADABS _exptl_special_details ; The dfix command has been used to refine the Zn-Cl distances to be in the reasonable distances. And the sadi command has been used, refining the distances between the terminal Cl atoms of the [ZnCl~4~]^2-^ to be equivalent (sadi cl1 cl1_$3 cl1 cl2 cl2 cl3 cl3 cl1).' ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17316 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7932 _reflns_number_gt 5931 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT-plus _computing_data_reduction SAINT-plus _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics SHELXL97 _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^)+(0.0478P)^2^+10.2273P] 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 7932 _refine_ls_number_parameters 410 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.09003(3) 0.40325(3) 0.50032(3) 0.03693(11) Uani 1 1 d . . . Zn1 Zn 0.4881(3) 0.0504(4) 0.5949(4) 0.1042(12) Uani 0.50 1 d PD . . C1 C -0.0544(15) 0.6483(12) 0.1009(11) 0.095(5) Uani 1 1 d . . . H1A H -0.0390 0.6860 0.0557 0.114 Uiso 1 1 calc R . . C2 C -0.1195(14) 0.5284(12) 0.0530(11) 0.090(4) Uani 1 1 d . . . H2A H -0.1533 0.4887 -0.0235 0.108 Uiso 1 1 calc R . . C3 C -0.0141(12) 0.7083(11) 0.2161(11) 0.079(4) Uani 1 1 d . . . H3A H 0.0243 0.7889 0.2503 0.095 Uiso 1 1 calc R . . C4 C -0.4510(10) 0.0094(12) -0.1322(10) 0.075(4) Uani 1 1 d . . . H4A H -0.5105 -0.0075 -0.1892 0.090 Uiso 1 1 calc R . . C5 C 0.0771(11) 0.8256(9) 0.4501(10) 0.074(3) Uani 1 1 d . . . H5A H 0.1445 0.8323 0.4134 0.110 Uiso 1 1 calc R . . H5B H 0.1018 0.8531 0.5297 0.110 Uiso 1 1 calc R . . H5C H 0.0318 0.8727 0.4413 0.110 Uiso 1 1 calc R . . C6 C -0.4288(11) -0.0817(12) -0.1183(10) 0.084(4) Uani 1 1 d . . . H6A H -0.4737 -0.1594 -0.1645 0.101 Uiso 1 1 calc R . . C7 C -0.0906(7) 0.5283(7) 0.2351(7) 0.0408(19) Uani 1 1 d . . . C8 C -0.0304(9) 0.6493(9) 0.2823(9) 0.055(2) Uani 1 1 d . . . C9 C 0.0291(8) 0.1373(8) 0.2935(8) 0.044(2) Uani 1 1 d . . . C10 C -0.1127(9) 0.0252(8) 0.1060(8) 0.052(2) Uani 1 1 d . . . H10A H -0.1330 -0.0443 0.0374 0.063 Uiso 1 1 calc R . . C11 C -0.0131(8) 0.0422(7) 0.1835(8) 0.046(2) Uani 1 1 d . . . C12 C 0.1299(9) 0.1422(8) 0.3539(9) 0.050(2) Uani 1 1 d . . . C13 C -0.1346(9) 0.4679(9) 0.1175(8) 0.052(2) Uani 1 1 d . . . C14 C -0.2966(8) 0.1499(9) 0.0197(8) 0.050(2) Uani 1 1 d . . . C15 C -0.3388(10) -0.0560(9) -0.0345(9) 0.065(3) Uani 1 1 d . . . H15A H -0.3235 -0.1169 -0.0245 0.078 Uiso 1 1 calc R . . C16 C 0.4790(11) 0.5833(14) 0.6575(15) 0.128(8) Uani 1 1 d . . . H16A H 0.5265 0.6496 0.6508 0.192 Uiso 1 1 calc R . . H16B H 0.4918 0.5120 0.6016 0.192 Uiso 1 1 calc R . . H16C H 0.4995 0.5928 0.7324 0.192 Uiso 1 1 calc R . . C17 C 0.0462(10) -0.0460(8) 0.1406(9) 0.053(2) Uani 1 1 d . . . H17A H 0.0174 -0.1104 0.0688 0.063 Uiso 1 1 calc R . . C18 C -0.2007(9) 0.3435(8) 0.0554(7) 0.051(2) Uani 1 1 d . . . H18A H -0.2290 0.3151 -0.0212 0.061 Uiso 1 1 calc R . . C19 C -0.2714(8) 0.0592(8) 0.0344(8) 0.050(2) Uani 1 1 d . . . C20 C -0.3867(8) 0.1245(10) -0.0634(9) 0.060(3) Uani 1 1 d . . . H20A H -0.4036 0.1852 -0.0726 0.071 Uiso 1 1 calc R . . C21 C 0.1434(11) -0.0382(9) 0.2017(10) 0.062(3) Uani 1 1 d . . . H21A H 0.1813 -0.0961 0.1713 0.075 Uiso 1 1 calc R . . C22 C 0.1867(9) 0.0569(9) 0.3105(9) 0.057(3) Uani 1 1 d . . . H22A H 0.2532 0.0625 0.3531 0.068 Uiso 1 1 calc R . . C23 C 0.2488(12) 0.2388(12) 0.5402(11) 0.086(4) Uani 1 1 d . . . H23A H 0.2211 0.1674 0.5464 0.129 Uiso 1 1 calc R . . H23B H 0.2579 0.3057 0.6134 0.129 Uiso 1 1 calc R . . H23C H 0.3228 0.2423 0.5139 0.129 Uiso 1 1 calc R . . C24 C 0.3522(8) 0.5765(10) 0.6384(9) 0.059(3) Uani 1 1 d . . . C25 C 0.2149(10) 0.3561(14) 0.1658(10) 0.090(5) Uani 1 1 d . . . H25A H 0.1822 0.3143 0.0863 0.134 Uiso 1 1 calc R . . H25B H 0.2653 0.3168 0.1816 0.134 Uiso 1 1 calc R . . H25C H 0.2591 0.4354 0.1850 0.134 Uiso 1 1 calc R . . C26 C 0.1162(8) 0.3589(8) 0.2371(8) 0.048(2) Uani 1 1 d . . . N1 N -0.2240(6) 0.2692(7) 0.0941(6) 0.0455(18) Uani 1 1 d . . . N2 N -0.1753(7) 0.0945(6) 0.1211(6) 0.0449(17) Uani 1 1 d . . . O1 O 0.0964(5) 0.5910(4) 0.5356(5) 0.0341(12) Uani 1 1 d . . . H1B H 0.1490 0.6189 0.4921 0.041 Uiso 1 1 calc R . . O2 O 0.0155(5) 0.3120(6) 0.1869(6) 0.0499(15) Uani 1 1 d . . . O9 O 0.1472(6) 0.4108(6) 0.3442(5) 0.0539(17) Uani 1 1 d . . . O4 O -0.1017(5) 0.4816(5) 0.3059(5) 0.0409(13) Uani 1 1 d . . . O7 O 0.2831(5) 0.4808(6) 0.5613(6) 0.0558(18) Uani 1 1 d . . . O10 O 0.3242(5) 0.6671(5) 0.6974(6) 0.0495(16) Uani 1 1 d . . . O5 O 0.0069(6) 0.7036(5) 0.3987(6) 0.0535(16) Uani 1 1 d . . . O3 O -0.0199(5) 0.2247(5) 0.3436(5) 0.0401(13) Uani 1 1 d . . . O6 O 0.1656(6) 0.2405(5) 0.4600(6) 0.0564(18) Uani 1 1 d . . . Cl1 Cl 0.5104(5) -0.1069(8) 0.5588(5) 0.309(7) Uani 1 1 d D . . Cl2 Cl 0.6541(7) 0.2001(9) 0.7123(8) 0.131(4) Uani 0.50 1 d PD . . Cl3 Cl 0.3253(6) 0.0742(6) 0.6726(8) 0.095(2) Uani 0.50 1 d PD . . O1W O 0.2808(12) 0.6533(10) 0.4212(11) 0.131(4) Uani 1 1 d . . . Lu2 Lu -0.14955(3) 0.28948(3) 0.27297(3) 0.03670(11) Uani 1 1 d . . . O8 O -0.2730(6) 0.1625(6) 0.3266(6) 0.0575(17) Uani 1 1 d . . . H8A H -0.3287 0.1881 0.3543 0.069 Uiso 1 1 d R . . H8B H -0.2800 0.0901 0.3048 0.069 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.0385(2) 0.03207(18) 0.0290(2) 0.00680(15) -0.00752(14) 0.00772(15) Zn1 0.0710(19) 0.158(4) 0.107(3) 0.084(3) 0.018(2) 0.030(2) C1 0.162(15) 0.065(8) 0.056(8) 0.037(7) -0.011(8) 0.016(9) C2 0.131(12) 0.077(9) 0.050(7) 0.034(7) -0.020(7) 0.008(8) C3 0.107(10) 0.058(7) 0.066(8) 0.037(6) -0.013(7) 0.000(7) C4 0.054(6) 0.085(9) 0.039(6) 0.006(6) -0.015(5) -0.008(6) C5 0.095(9) 0.044(6) 0.060(7) 0.020(5) -0.012(6) -0.006(6) C6 0.065(7) 0.071(8) 0.049(7) -0.009(6) -0.019(6) -0.019(6) C7 0.044(5) 0.037(4) 0.035(5) 0.017(4) -0.009(4) 0.001(4) C8 0.069(6) 0.051(5) 0.040(5) 0.021(5) -0.005(5) 0.013(5) C9 0.046(5) 0.041(5) 0.041(5) 0.016(4) 0.007(4) 0.009(4) C10 0.062(6) 0.035(4) 0.035(5) 0.003(4) 0.004(4) 0.001(4) C11 0.053(5) 0.033(4) 0.042(5) 0.010(4) 0.005(4) 0.009(4) C12 0.057(6) 0.038(5) 0.052(6) 0.018(4) 0.006(5) 0.017(4) C13 0.067(6) 0.050(5) 0.031(5) 0.017(4) -0.011(4) 0.008(5) C14 0.045(5) 0.050(5) 0.031(5) 0.008(4) -0.006(4) -0.001(4) C15 0.068(7) 0.046(5) 0.050(6) 0.005(5) 0.004(5) 0.000(5) C16 0.049(7) 0.099(11) 0.145(15) -0.025(10) -0.035(8) 0.033(7) C17 0.079(7) 0.031(4) 0.044(6) 0.012(4) 0.015(5) 0.019(5) C18 0.066(6) 0.049(5) 0.023(4) 0.013(4) -0.011(4) 0.004(5) C19 0.047(5) 0.046(5) 0.031(5) 0.002(4) -0.006(4) 0.001(4) C20 0.048(5) 0.064(6) 0.043(6) 0.017(5) -0.014(4) -0.003(5) C21 0.083(8) 0.054(6) 0.066(7) 0.029(6) 0.033(6) 0.041(6) C22 0.057(6) 0.053(6) 0.060(7) 0.025(5) 0.005(5) 0.019(5) C23 0.107(10) 0.082(9) 0.069(8) 0.022(7) -0.015(7) 0.056(8) C24 0.042(5) 0.064(6) 0.050(6) 0.007(5) -0.010(4) 0.020(5) C25 0.055(6) 0.137(13) 0.041(6) 0.022(7) -0.002(5) 0.008(7) C26 0.046(5) 0.045(5) 0.039(5) 0.012(4) 0.002(4) 0.005(4) N1 0.044(4) 0.048(4) 0.026(4) 0.007(3) -0.009(3) 0.005(3) N2 0.047(4) 0.037(4) 0.033(4) 0.007(3) -0.002(3) 0.004(3) O1 0.038(3) 0.028(3) 0.028(3) 0.008(2) -0.003(2) 0.007(2) O2 0.040(3) 0.059(4) 0.047(4) 0.021(3) 0.003(3) 0.014(3) O9 0.060(4) 0.046(4) 0.031(3) 0.006(3) 0.003(3) 0.000(3) O4 0.047(3) 0.038(3) 0.028(3) 0.011(3) -0.008(2) 0.006(3) O7 0.040(3) 0.054(4) 0.046(4) 0.002(3) -0.009(3) 0.011(3) O10 0.041(3) 0.042(3) 0.049(4) 0.010(3) 0.000(3) 0.008(3) O5 0.066(4) 0.038(3) 0.039(4) 0.014(3) -0.009(3) -0.005(3) O3 0.046(3) 0.030(3) 0.033(3) 0.006(2) -0.005(3) 0.010(3) O6 0.058(4) 0.040(3) 0.058(4) 0.008(3) -0.015(3) 0.024(3) Cl1 0.135(5) 0.64(2) 0.112(5) 0.087(8) 0.023(4) 0.224(9) Cl2 0.090(5) 0.210(11) 0.155(9) 0.149(9) 0.017(6) 0.023(6) Cl3 0.083(4) 0.089(5) 0.154(8) 0.086(5) 0.026(5) 0.038(4) O1W 0.159(11) 0.108(9) 0.136(11) 0.067(8) 0.068(9) 0.030(8) Lu2 0.03685(19) 0.03204(18) 0.02698(19) 0.00567(14) -0.00695(14) 0.00361(15) O8 0.056(4) 0.049(4) 0.058(5) 0.021(3) 0.005(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O9 2.237(7) . ? Lu1 O7 2.241(6) . ? Lu1 O1 2.290(5) . ? Lu1 O1 2.296(5) 2_566 ? Lu1 O4 2.313(6) 2_566 ? Lu1 O3 2.358(5) . ? Lu1 O6 2.389(6) . ? Lu1 O5 2.465(7) 2_566 ? Lu1 Lu2 3.5903(15) . ? Lu1 Lu2 3.6930(17) 2_566 ? Lu1 Lu1 3.7341(15) 2_566 ? Zn1 Cl1 2.005(9) . ? Zn1 Cl3 2.259(8) . ? Zn1 Cl2 2.326(10) . ? Zn1 Zn1 2.337(9) 2_656 ? Zn1 Cl1 2.459(8) 2_656 ? C1 C3 1.374(17) . ? C1 C2 1.407(18) . ? C1 H1A 0.9300 . ? C2 C13 1.395(15) . ? C2 H2A 0.9300 . ? C3 C8 1.400(15) . ? C3 H3A 0.9300 . ? C4 C20 1.372(15) . ? C4 C6 1.380(19) . ? C4 H4A 0.9300 . ? C5 O5 1.444(11) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C15 1.387(17) . ? C6 H6A 0.9300 . ? C7 O4 1.326(10) . ? C7 C8 1.405(13) . ? C7 C13 1.408(12) . ? C8 O5 1.383(11) . ? C9 O3 1.343(10) . ? C9 C12 1.400(13) . ? C9 C11 1.406(12) . ? C10 N2 1.277(12) . ? C10 C11 1.455(14) . ? C10 H10A 0.9300 . ? C11 C17 1.426(12) . ? C12 C22 1.377(13) . ? C12 O6 1.385(11) . ? C13 C18 1.455(13) . ? C14 C20 1.382(13) . ? C14 C19 1.394(14) . ? C14 N1 1.449(11) . ? C15 C19 1.382(13) . ? C15 H15A 0.9300 . ? C16 C24 1.505(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C21 1.352(15) . ? C17 H17A 0.9300 . ? C18 N1 1.273(12) . ? C18 H18A 0.9300 . ? C19 N2 1.429(12) . ? C20 H20A 0.9300 . ? C21 C22 1.398(15) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 O6 1.445(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O10 1.243(11) . ? C24 O7 1.269(11) . ? C25 C26 1.534(14) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O2 1.223(11) . ? C26 O9 1.267(11) . ? N1 Lu2 2.383(7) . ? N2 Lu2 2.400(7) . ? O1 Lu2 2.279(5) 2_566 ? O1 Lu1 2.296(5) 2_566 ? O1 H1B 0.9800 . ? O2 Lu2 2.333(6) . ? O4 Lu2 2.287(6) . ? O4 Lu1 2.313(6) 2_566 ? O10 Lu2 2.304(6) 2_566 ? O5 Lu1 2.465(7) 2_566 ? O3 Lu2 2.302(6) . ? Cl1 Zn1 2.459(8) 2_656 ? Lu2 O1 2.279(5) 2_566 ? Lu2 O10 2.304(6) 2_566 ? Lu2 O8 2.321(7) . ? Lu2 Lu1 3.6930(17) 2_566 ? O8 H8A 0.8434 . ? O8 H8B 0.8469 . ? 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 O9 Lu1 O7 80.7(3) . . ? O9 Lu1 O1 77.1(2) . . ? O7 Lu1 O1 84.3(2) . . ? O9 Lu1 O1 96.0(2) . 2_566 ? O7 Lu1 O1 155.1(2) . 2_566 ? O1 Lu1 O1 71.0(2) . 2_566 ? O9 Lu1 O4 142.5(2) . 2_566 ? O7 Lu1 O4 77.2(2) . 2_566 ? O1 Lu1 O4 71.0(2) . 2_566 ? O1 Lu1 O4 91.8(2) 2_566 2_566 ? O9 Lu1 O3 73.5(2) . . ? O7 Lu1 O3 131.2(2) . . ? O1 Lu1 O3 127.21(19) . . ? O1 Lu1 O3 69.72(19) 2_566 . ? O4 Lu1 O3 142.7(2) 2_566 . ? O9 Lu1 O6 90.2(3) . . ? O7 Lu1 O6 73.8(2) . . ? O1 Lu1 O6 156.2(2) . . ? O1 Lu1 O6 131.1(2) 2_566 . ? O4 Lu1 O6 111.8(2) 2_566 . ? O3 Lu1 O6 65.8(2) . . ? O9 Lu1 O5 152.5(2) . 2_566 ? O7 Lu1 O5 112.4(3) . 2_566 ? O1 Lu1 O5 126.7(2) . 2_566 ? O1 Lu1 O5 81.7(2) 2_566 2_566 ? O4 Lu1 O5 65.0(2) 2_566 2_566 ? O3 Lu1 O5 80.1(2) . 2_566 ? O6 Lu1 O5 71.8(3) . 2_566 ? O9 Lu1 Lu2 67.35(18) . . ? O7 Lu1 Lu2 148.01(19) . . ? O1 Lu1 Lu2 89.21(13) . . ? O1 Lu1 Lu2 38.13(13) 2_566 . ? O4 Lu1 Lu2 129.81(15) 2_566 . ? O3 Lu1 Lu2 39.03(13) . . ? O6 Lu1 Lu2 104.46(16) . . ? O5 Lu1 Lu2 96.56(16) 2_566 . ? O9 Lu1 Lu2 107.48(17) . 2_566 ? O7 Lu1 Lu2 71.22(16) . 2_566 ? O1 Lu1 Lu2 35.97(14) . 2_566 ? O1 Lu1 Lu2 86.61(13) 2_566 2_566 ? O4 Lu1 Lu2 36.36(14) 2_566 2_566 ? O3 Lu1 Lu2 156.17(13) . 2_566 ? O6 Lu1 Lu2 137.15(16) . 2_566 ? O5 Lu1 Lu2 99.77(15) 2_566 2_566 ? Lu2 Lu1 Lu2 118.33(2) . 2_566 ? O9 Lu1 Lu1 85.80(18) . 2_566 ? O7 Lu1 Lu1 119.80(18) . 2_566 ? O1 Lu1 Lu1 35.54(13) . 2_566 ? O1 Lu1 Lu1 35.44(13) 2_566 2_566 ? O4 Lu1 Lu1 79.58(14) 2_566 2_566 ? O3 Lu1 Lu1 99.08(14) . 2_566 ? O6 Lu1 Lu1 164.82(16) . 2_566 ? O5 Lu1 Lu1 106.12(17) 2_566 2_566 ? Lu2 Lu1 Lu1 60.52(3) . 2_566 ? Lu2 Lu1 Lu1 57.81(3) 2_566 2_566 ? Cl1 Zn1 Cl3 112.4(3) . . ? Cl1 Zn1 Cl2 109.5(3) . . ? Cl3 Zn1 Cl2 111.6(4) . . ? Cl1 Zn1 Zn1 68.5(3) . 2_656 ? Cl3 Zn1 Zn1 130.7(3) . 2_656 ? Cl2 Zn1 Zn1 113.9(3) . 2_656 ? Cl1 Zn1 Cl1 117.9(3) . 2_656 ? Cl3 Zn1 Cl1 108.0(3) . 2_656 ? Cl2 Zn1 Cl1 96.5(3) . 2_656 ? Zn1 Zn1 Cl1 49.3(2) 2_656 2_656 ? C3 C1 C2 118.3(12) . . ? C3 C1 H1A 120.8 . . ? C2 C1 H1A 120.8 . . ? C13 C2 C1 121.5(11) . . ? C13 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C1 C3 C8 120.6(11) . . ? C1 C3 H3A 119.7 . . ? C8 C3 H3A 119.7 . . ? C20 C4 C6 121.0(11) . . ? C20 C4 H4A 119.5 . . ? C6 C4 H4A 119.5 . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C15 119.2(11) . . ? C4 C6 H6A 120.4 . . ? C15 C6 H6A 120.4 . . ? O4 C7 C8 116.7(8) . . ? O4 C7 C13 125.9(8) . . ? C8 C7 C13 117.4(8) . . ? O5 C8 C3 124.0(9) . . ? O5 C8 C7 114.2(8) . . ? C3 C8 C7 121.8(10) . . ? O3 C9 C12 117.9(8) . . ? O3 C9 C11 124.3(8) . . ? C12 C9 C11 117.9(8) . . ? N2 C10 C11 127.6(8) . . ? N2 C10 H10A 116.2 . . ? C11 C10 H10A 116.2 . . ? C9 C11 C17 118.7(9) . . ? C9 C11 C10 125.8(8) . . ? C17 C11 C10 115.5(9) . . ? C22 C12 O6 124.2(9) . . ? C22 C12 C9 122.5(9) . . ? O6 C12 C9 113.3(7) . . ? C2 C13 C7 120.2(9) . . ? C2 C13 C18 115.2(9) . . ? C7 C13 C18 124.6(9) . . ? C20 C14 C19 120.3(9) . . ? C20 C14 N1 122.7(10) . . ? C19 C14 N1 117.0(8) . . ? C19 C15 C6 120.8(12) . . ? C19 C15 H15A 119.6 . . ? C6 C15 H15A 119.6 . . ? C24 C16 H16A 109.5 . . ? C24 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C24 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C21 C17 C11 121.6(9) . . ? C21 C17 H17A 119.2 . . ? C11 C17 H17A 119.2 . . ? N1 C18 C13 127.3(8) . . ? N1 C18 H18A 116.4 . . ? C13 C18 H18A 116.4 . . ? C15 C19 C14 119.0(10) . . ? C15 C19 N2 125.0(10) . . ? C14 C19 N2 116.0(8) . . ? C4 C20 C14 119.7(11) . . ? C4 C20 H20A 120.1 . . ? C14 C20 H20A 120.1 . . ? C17 C21 C22 119.9(9) . . ? C17 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C12 C22 C21 119.3(10) . . ? C12 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? O6 C23 H23A 109.5 . . ? O6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O10 C24 O7 125.0(8) . . ? O10 C24 C16 117.0(10) . . ? O7 C24 C16 118.0(9) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 O9 125.6(9) . . ? O2 C26 C25 118.1(9) . . ? O9 C26 C25 116.2(9) . . ? C18 N1 C14 119.0(8) . . ? C18 N1 Lu2 129.2(6) . . ? C14 N1 Lu2 111.6(6) . . ? C10 N2 C19 118.5(8) . . ? C10 N2 Lu2 129.3(6) . . ? C19 N2 Lu2 112.1(6) . . ? Lu2 O1 Lu1 107.8(2) 2_566 . ? Lu2 O1 Lu1 103.4(2) 2_566 2_566 ? Lu1 O1 Lu1 109.0(2) . 2_566 ? Lu2 O1 H1B 112.0 2_566 . ? Lu1 O1 H1B 112.0 . . ? Lu1 O1 H1B 112.0 2_566 . ? C26 O2 Lu2 125.1(6) . . ? C26 O9 Lu1 140.5(6) . . ? C7 O4 Lu2 131.4(5) . . ? C7 O4 Lu1 121.6(5) . 2_566 ? Lu2 O4 Lu1 106.8(2) . 2_566 ? C24 O7 Lu1 137.2(6) . . ? C24 O10 Lu2 134.8(6) . 2_566 ? C8 O5 C5 116.4(8) . . ? C8 O5 Lu1 115.6(6) . 2_566 ? C5 O5 Lu1 126.4(6) . 2_566 ? C9 O3 Lu2 132.6(5) . . ? C9 O3 Lu1 119.3(5) . . ? Lu2 O3 Lu1 100.8(2) . . ? C12 O6 C23 117.4(7) . . ? C12 O6 Lu1 119.0(5) . . ? C23 O6 Lu1 123.6(6) . . ? Zn1 Cl1 Zn1 62.1(3) . 2_656 ? O1 Lu2 O4 71.6(2) 2_566 . ? O1 Lu2 O3 71.01(19) 2_566 . ? O4 Lu2 O3 120.2(2) . . ? O1 Lu2 O10 84.1(2) 2_566 2_566 ? O4 Lu2 O10 77.5(2) . 2_566 ? O3 Lu2 O10 140.4(2) . 2_566 ? O1 Lu2 O8 84.0(2) 2_566 . ? O4 Lu2 O8 140.2(2) . . ? O3 Lu2 O8 78.0(2) . . ? O10 Lu2 O8 68.9(2) 2_566 . ? O1 Lu2 O2 108.2(2) 2_566 . ? O4 Lu2 O2 75.8(2) . . ? O3 Lu2 O2 73.8(2) . . ? O10 Lu2 O2 145.0(2) 2_566 . ? O8 Lu2 O2 143.1(2) . . ? O1 Lu2 N1 146.8(2) 2_566 . ? O4 Lu2 N1 77.9(2) . . ? O3 Lu2 N1 138.5(2) . . ? O10 Lu2 N1 76.6(2) 2_566 . ? O8 Lu2 N1 112.9(3) . . ? O2 Lu2 N1 75.9(2) . . ? O1 Lu2 N2 145.0(2) 2_566 . ? O4 Lu2 N2 140.4(2) . . ? O3 Lu2 N2 77.7(2) . . ? O10 Lu2 N2 112.2(2) 2_566 . ? O8 Lu2 N2 74.5(3) . . ? O2 Lu2 N2 76.6(2) . . ? N1 Lu2 N2 68.1(3) . . ? O1 Lu2 Lu1 38.47(13) 2_566 . ? O4 Lu2 Lu1 83.17(14) . . ? O3 Lu2 Lu1 40.17(14) . . ? O10 Lu2 Lu1 122.53(16) 2_566 . ? O8 Lu2 Lu1 97.07(18) . . ? O2 Lu2 Lu1 76.16(16) . . ? N1 Lu2 Lu1 149.34(19) . . ? N2 Lu2 Lu1 116.84(19) . . ? O1 Lu2 Lu1 36.18(13) 2_566 2_566 ? O4 Lu2 Lu1 36.83(14) . 2_566 ? O3 Lu2 Lu1 101.34(14) . 2_566 ? O10 Lu2 Lu1 71.15(15) 2_566 2_566 ? O8 Lu2 Lu1 109.39(18) . 2_566 ? O2 Lu2 Lu1 99.20(16) . 2_566 ? N1 Lu2 Lu1 111.02(19) . 2_566 ? N2 Lu2 Lu1 175.83(18) . 2_566 ? Lu1 Lu2 Lu1 61.67(2) . 2_566 ? Lu2 O8 H8A 111.7 . . ? Lu2 O8 H8B 127.8 . . ? H8A O8 H8B 117.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O1W 0.98 1.92 2.875(12) 163.2 . O8 H8A O1W 0.84 2.71 3.170(14) 115.6 2_566 O8 H8A Cl1 0.84 2.70 3.339(9) 133.5 2_556 O8 H8B Cl3 0.85 2.26 3.034(9) 152.9 2_556 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.414 _refine_diff_density_min -1.610 _refine_diff_density_rms 0.172