# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Richard Jones' _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Heteronuclear Trimetallic and 1-D Polymeric 3d-4f Schiff-base Complexes with OCN- and SCN- Ligands ; loop_ _publ_author_name 'Richard Jones' 'An-Xin Hou' 'Xingqiang Lu' 'Wai-Yeung Wong' 'Wai-Kwok Wong' 'Xiaoping Yang' 'Shunsheng Zhao' # Attachment '2b.cif' data_wy1771 _database_code_depnum_ccdc_archive 'CCDC 700787' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 N5 Nd O12 Zn' _chemical_formula_sum 'C19 H20 N5 Nd O12 Zn' _chemical_formula_weight 720.01 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 '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 12.1674(5) _cell_length_b 7.9501(3) _cell_length_c 25.4391(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.5860(10) _cell_angle_gamma 90.00 _cell_volume 2410.64(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14593 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 28.33 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 3.199 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4275 _exptl_absorpt_correction_T_max 0.5140 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11512 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4239 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0272P)^2^+1.0593P] 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 4239 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0430 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.6460(3) 0.0853(5) -0.02036(14) 0.0613(10) Uani 1 1 d U . . H1A H 0.6333 0.1320 -0.0559 0.092 Uiso 1 1 calc R . . H1B H 0.5754 0.0704 -0.0096 0.092 Uiso 1 1 calc R . . H1C H 0.6829 -0.0216 -0.0202 0.092 Uiso 1 1 calc R . . C2 C 0.8237(2) 0.2196(3) 0.00815(10) 0.0304(6) Uani 1 1 d U . . C3 C 0.8645(2) 0.1459(4) -0.03304(11) 0.0400(7) Uani 1 1 d U . . H3A H 0.8178 0.0808 -0.0586 0.048 Uiso 1 1 calc R . . C4 C 0.9757(3) 0.1695(4) -0.03608(12) 0.0451(7) Uani 1 1 d U . . H4A H 1.0038 0.1212 -0.0639 0.054 Uiso 1 1 calc R . . C5 C 1.0437(2) 0.2633(4) 0.00166(12) 0.0402(7) Uani 1 1 d U . . H5A H 1.1187 0.2760 -0.0004 0.048 Uiso 1 1 calc R . . C6 C 1.0043(2) 0.3418(3) 0.04371(11) 0.0314(6) Uani 1 1 d U . . C7 C 0.8901(2) 0.3229(3) 0.04673(10) 0.0278(6) Uani 1 1 d U . . C8 C 1.0852(2) 0.4359(4) 0.08237(12) 0.0393(7) Uani 1 1 d U . . H8A H 1.1596 0.4328 0.0786 0.047 Uiso 1 1 calc R . . C9 C 1.1508(2) 0.6045(4) 0.15989(14) 0.0530(8) Uani 1 1 d U . . H9A H 1.1434 0.7257 0.1563 0.064 Uiso 1 1 calc R . . H9B H 1.2243 0.5727 0.1538 0.064 Uiso 1 1 calc R . . C10 C 1.1383(2) 0.5506(4) 0.21538(14) 0.0535(9) Uani 1 1 d U . . H10A H 1.1722 0.4409 0.2237 0.064 Uiso 1 1 calc R . . H10B H 1.1763 0.6302 0.2418 0.064 Uiso 1 1 calc R . . C11 C 0.9859(3) 0.5623(4) 0.26116(12) 0.0473(8) Uani 1 1 d U . . H11A H 1.0404 0.5868 0.2914 0.057 Uiso 1 1 calc R . . C12 C 0.8713(3) 0.5490(4) 0.26818(11) 0.0415(7) Uani 1 1 d U . . C13 C 0.7809(2) 0.4940(3) 0.22802(10) 0.0337(6) Uani 1 1 d U . . C14 C 0.6727(2) 0.4978(3) 0.23944(11) 0.0374(6) Uani 1 1 d U . . C15 C 0.6547(3) 0.5491(4) 0.28860(12) 0.0521(8) Uani 1 1 d U . . H15A H 0.5823 0.5504 0.2953 0.062 Uiso 1 1 calc R . . C16 C 0.7447(3) 0.5988(4) 0.32835(12) 0.0595(9) Uani 1 1 d U . . H16A H 0.7326 0.6322 0.3618 0.071 Uiso 1 1 calc R . . C17 C 0.8494(3) 0.5987(4) 0.31849(12) 0.0532(9) Uani 1 1 d U . . H17A H 0.9088 0.6321 0.3454 0.064 Uiso 1 1 calc R . . C18 C 0.4769(3) 0.4733(5) 0.20419(15) 0.0638(10) Uani 1 1 d U . . H18A H 0.4675 0.5883 0.2139 0.096 Uiso 1 1 calc R . . H18B H 0.4625 0.4006 0.2322 0.096 Uiso 1 1 calc R . . H18C H 0.4253 0.4479 0.1714 0.096 Uiso 1 1 calc R . . C19 C 0.8371(2) 0.9212(3) 0.12929(10) 0.0302(6) Uani 1 1 d U . . N1 N 1.06310(18) 0.5214(3) 0.12068(10) 0.0390(6) Uani 1 1 d U . . N2 N 1.01831(19) 0.5435(3) 0.21739(10) 0.0427(6) Uani 1 1 d U . . N3 N 0.8568(2) 0.7806(3) 0.13235(11) 0.0452(6) Uani 1 1 d U . . N4 N 0.5913(2) -0.0277(3) 0.14480(10) 0.0413(6) Uani 1 1 d U . . N5 N 0.4270(2) 0.3274(3) 0.05014(10) 0.0431(6) Uani 1 1 d U . . Nd1 Nd 0.669935(10) 0.296852(16) 0.108410(5) 0.02502(5) Uani 1 1 d U . . O1 O 0.71520(15) 0.1972(2) 0.01626(7) 0.0347(4) Uani 1 1 d U . . O2 O 0.84045(13) 0.3932(2) 0.08336(7) 0.0286(4) Uani 1 1 d U . . O3 O 0.79312(15) 0.4362(2) 0.18001(7) 0.0321(4) Uani 1 1 d U . . O4 O 0.58988(16) 0.4479(2) 0.19692(7) 0.0416(5) Uani 1 1 d U . . O5 O 0.62035(18) 0.0933(2) 0.17680(8) 0.0447(5) Uani 1 1 d U . . O6 O 0.58956(16) -0.0027(2) 0.09582(8) 0.0410(5) Uani 1 1 d U . . O7 O 0.5663(3) -0.1643(3) 0.16092(11) 0.0735(8) Uani 1 1 d U . . O8 O 0.45245(18) 0.2991(3) 0.09943(9) 0.0448(6) Uani 1 1 d U . . O9 O 0.50521(16) 0.3179(2) 0.02458(8) 0.0409(5) Uani 1 1 d U . . O10 O 0.33214(19) 0.3604(4) 0.02690(11) 0.0789(8) Uani 1 1 d U . . O12 O 0.61358(18) 0.5863(2) 0.08632(8) 0.0479(5) Uani 1 1 d U . . H12A H 0.6018 0.6137 0.0555 0.072 Uiso 1 1 d R . . H12B H 0.6013 0.6503 0.1055 0.072 Uiso 1 1 d R . . Zn1 Zn 0.91134(2) 0.54783(4) 0.142782(12) 0.03028(8) Uani 1 1 d U . . O11 O 0.82020(16) 1.0712(2) 0.12697(8) 0.0444(5) Uani 1 1 d U . . 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 C1 0.0480(19) 0.076(2) 0.061(2) -0.0387(19) 0.0129(16) -0.0227(17) C2 0.0308(14) 0.0303(14) 0.0312(14) 0.0014(11) 0.0087(11) 0.0018(11) C3 0.0461(17) 0.0397(16) 0.0358(15) -0.0044(12) 0.0118(13) 0.0018(13) C4 0.0531(18) 0.0440(18) 0.0452(17) 0.0002(14) 0.0270(15) 0.0069(14) C5 0.0352(15) 0.0373(16) 0.0537(18) 0.0085(14) 0.0227(14) 0.0071(12) C6 0.0286(13) 0.0246(13) 0.0430(15) 0.0075(11) 0.0119(12) 0.0038(11) C7 0.0302(13) 0.0224(13) 0.0322(14) 0.0052(10) 0.0093(11) 0.0034(10) C8 0.0255(14) 0.0324(16) 0.0610(19) 0.0070(14) 0.0110(13) -0.0001(12) C9 0.0315(16) 0.0444(19) 0.078(2) -0.0106(17) -0.0019(15) -0.0054(14) C10 0.0343(16) 0.0484(19) 0.067(2) -0.0111(16) -0.0157(15) -0.0004(14) C11 0.055(2) 0.0370(17) 0.0381(17) -0.0044(13) -0.0188(14) 0.0045(14) C12 0.0595(19) 0.0312(15) 0.0283(14) -0.0015(12) -0.0041(13) 0.0050(14) C13 0.0525(17) 0.0208(13) 0.0265(14) 0.0009(10) 0.0047(12) 0.0023(12) C14 0.0545(18) 0.0274(15) 0.0303(14) 0.0011(11) 0.0091(13) 0.0002(13) C15 0.075(2) 0.0465(19) 0.0392(17) -0.0003(14) 0.0219(16) 0.0053(17) C16 0.097(3) 0.054(2) 0.0278(16) -0.0050(14) 0.0123(17) 0.0084(19) C17 0.082(2) 0.0437(19) 0.0270(15) -0.0057(13) -0.0048(16) 0.0059(17) C18 0.0497(19) 0.081(3) 0.067(2) -0.022(2) 0.0266(17) -0.0092(18) C19 0.0252(13) 0.0320(17) 0.0320(14) 0.0002(11) 0.0022(10) -0.0016(11) N1 0.0249(11) 0.0310(13) 0.0581(15) -0.0018(12) 0.0012(10) -0.0037(10) N2 0.0393(13) 0.0361(14) 0.0452(15) -0.0048(11) -0.0099(11) 0.0004(11) N3 0.0463(15) 0.0270(14) 0.0633(17) 0.0028(12) 0.0133(13) 0.0052(11) N4 0.0477(14) 0.0308(13) 0.0509(15) 0.0028(12) 0.0226(12) -0.0013(11) N5 0.0332(13) 0.0458(15) 0.0472(15) -0.0033(12) 0.0009(12) -0.0007(11) Nd1 0.02437(8) 0.02326(8) 0.02671(8) -0.00002(5) 0.00339(5) -0.00106(5) O1 0.0305(10) 0.0402(11) 0.0338(10) -0.0116(8) 0.0075(8) -0.0067(8) O2 0.0265(9) 0.0270(9) 0.0329(9) -0.0064(8) 0.0076(7) -0.0026(7) O3 0.0394(10) 0.0299(10) 0.0264(9) -0.0043(7) 0.0054(8) -0.0029(8) O4 0.0453(11) 0.0434(12) 0.0391(11) -0.0078(9) 0.0155(9) -0.0065(9) O5 0.0667(14) 0.0339(11) 0.0358(11) -0.0020(9) 0.0154(10) -0.0039(10) O6 0.0465(11) 0.0392(12) 0.0363(11) -0.0030(9) 0.0060(9) -0.0099(9) O7 0.123(2) 0.0320(13) 0.0823(18) 0.0029(12) 0.0600(17) -0.0113(13) O8 0.0435(12) 0.0487(17) 0.0440(13) 0.0012(11) 0.0131(10) -0.0001(11) O9 0.0390(11) 0.0465(13) 0.0368(11) -0.0017(9) 0.0064(9) 0.0008(9) O10 0.0324(13) 0.105(2) 0.0896(19) 0.0062(17) -0.0096(12) 0.0098(13) O12 0.0718(14) 0.0297(11) 0.0385(11) -0.0001(9) 0.0021(10) 0.0086(10) Zn1 0.02677(16) 0.02410(16) 0.03725(17) -0.00288(13) -0.00012(12) 0.00006(12) O11 0.0433(11) 0.0259(11) 0.0591(13) 0.0011(9) -0.0017(10) 0.0071(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 C1 O1 1.433(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.377(4) . ? C2 O1 1.388(3) . ? C2 C7 1.404(4) . ? C3 C4 1.383(4) . ? C3 H3A 0.9300 . ? C4 C5 1.358(4) . ? C4 H4A 0.9300 . ? C5 C6 1.404(4) . ? C5 H5A 0.9300 . ? C6 C7 1.414(3) . ? C6 C8 1.451(4) . ? C7 O2 1.331(3) . ? C8 N1 1.261(4) . ? C8 H8A 0.9300 . ? C9 N1 1.464(4) . ? C9 C10 1.512(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.472(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.263(4) . ? C11 C12 1.444(4) . ? C11 H11A 0.9300 . ? C12 C13 1.412(4) . ? C12 C17 1.415(4) . ? C13 O3 1.341(3) . ? C13 C14 1.405(4) . ? C14 C15 1.374(4) . ? C14 O4 1.380(3) . ? C15 C16 1.390(5) . ? C15 H15A 0.9300 . ? C16 C17 1.347(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 O4 1.437(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.143(3) . ? C19 O11 1.209(3) . ? N1 Zn1 2.046(2) . ? N2 Zn1 2.075(2) . ? N3 Zn1 1.966(2) . ? N4 O7 1.221(3) . ? N4 O6 1.258(3) . ? N4 O5 1.264(3) . ? N4 Nd1 2.964(2) . ? N5 O10 1.215(3) . ? N5 O8 1.250(3) . ? N5 O9 1.258(3) . ? Nd1 O3 2.3862(17) . ? Nd1 O2 2.4141(16) . ? Nd1 O12 2.4346(19) . ? Nd1 O5 2.5359(19) . ? Nd1 O11 2.5373(19) 1_545 ? Nd1 O6 2.5701(19) . ? Nd1 O8 2.610(2) . ? Nd1 O9 2.6222(19) . ? Nd1 O1 2.6353(17) . ? Nd1 O4 2.8883(18) . ? Nd1 Zn1 3.5130(3) . ? O2 Zn1 2.0042(16) . ? O3 Zn1 2.0738(18) . ? O12 H12A 0.7986 . ? O12 H12B 0.7408 . ? O11 Nd1 2.5373(18) 1_565 ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 123.9(2) . . ? C3 C2 C7 122.4(2) . . ? O1 C2 C7 113.7(2) . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 122.0(3) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 C8 117.2(2) . . ? C7 C6 C8 123.9(2) . . ? O2 C7 C2 117.1(2) . . ? O2 C7 C6 125.6(2) . . ? C2 C7 C6 117.2(2) . . ? N1 C8 C6 125.5(2) . . ? N1 C8 H8A 117.2 . . ? C6 C8 H8A 117.3 . . ? N1 C9 C10 108.2(3) . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C9 109.3(2) . . ? N2 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C12 125.5(3) . . ? N2 C11 H11A 117.3 . . ? C12 C11 H11A 117.3 . . ? C13 C12 C17 118.7(3) . . ? C13 C12 C11 124.4(3) . . ? C17 C12 C11 117.0(3) . . ? O3 C13 C14 118.4(2) . . ? O3 C13 C12 123.5(3) . . ? C14 C13 C12 118.1(2) . . ? C15 C14 O4 125.0(3) . . ? C15 C14 C13 121.5(3) . . ? O4 C14 C13 113.5(2) . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C12 121.7(3) . . ? C16 C17 H17A 119.1 . . ? C12 C17 H17A 119.1 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 O11 177.6(3) . . ? C8 N1 C9 122.0(2) . . ? C8 N1 Zn1 127.74(19) . . ? C9 N1 Zn1 110.0(2) . . ? C11 N2 C10 120.9(3) . . ? C11 N2 Zn1 123.7(2) . . ? C10 N2 Zn1 114.3(2) . . ? C19 N3 Zn1 172.1(2) . . ? O7 N4 O6 121.2(3) . . ? O7 N4 O5 121.1(3) . . ? O6 N4 O5 117.7(2) . . ? O7 N4 Nd1 175.7(2) . . ? O6 N4 Nd1 59.69(13) . . ? O5 N4 Nd1 58.16(13) . . ? O10 N5 O8 123.1(3) . . ? O10 N5 O9 120.3(3) . . ? O8 N5 O9 116.6(2) . . ? O3 Nd1 O2 67.22(6) . . ? O3 Nd1 O12 80.91(6) . . ? O2 Nd1 O12 81.74(7) . . ? O3 Nd1 O5 88.40(6) . . ? O2 Nd1 O5 135.97(6) . . ? O12 Nd1 O5 131.82(7) . . ? O3 Nd1 O11 82.39(6) . 1_545 ? O2 Nd1 O11 69.39(6) . 1_545 ? O12 Nd1 O11 150.50(7) . 1_545 ? O5 Nd1 O11 71.52(7) . 1_545 ? O3 Nd1 O6 133.65(6) . . ? O2 Nd1 O6 125.93(6) . . ? O12 Nd1 O6 139.88(7) . . ? O5 Nd1 O6 50.00(6) . . ? O11 Nd1 O6 67.04(6) 1_545 . ? O3 Nd1 O8 122.27(7) . . ? O2 Nd1 O8 152.21(6) . . ? O12 Nd1 O8 74.91(7) . . ? O5 Nd1 O8 71.81(7) . . ? O11 Nd1 O8 134.52(7) 1_545 . ? O6 Nd1 O8 69.01(7) . . ? O3 Nd1 O9 148.37(6) . . ? O2 Nd1 O9 108.79(6) . . ? O12 Nd1 O9 67.55(6) . . ? O5 Nd1 O9 110.51(6) . . ? O11 Nd1 O9 126.94(6) 1_545 . ? O6 Nd1 O9 75.42(6) . . ? O8 Nd1 O9 48.12(7) . . ? O3 Nd1 O1 127.38(6) . . ? O2 Nd1 O1 61.08(5) . . ? O12 Nd1 O1 100.27(6) . . ? O5 Nd1 O1 122.65(6) . . ? O11 Nd1 O1 71.42(6) 1_545 . ? O6 Nd1 O1 75.69(6) . . ? O8 Nd1 O1 108.27(6) . . ? O9 Nd1 O1 63.76(6) . . ? O3 Nd1 O4 58.02(6) . . ? O2 Nd1 O4 121.07(5) . . ? O12 Nd1 O4 70.33(6) . . ? O5 Nd1 O4 64.32(6) . . ? O11 Nd1 O4 119.49(6) 1_545 . ? O6 Nd1 O4 107.64(6) . . ? O8 Nd1 O4 64.57(6) . . ? O9 Nd1 O4 106.56(6) . . ? O1 Nd1 O4 169.09(6) . . ? O3 Nd1 N4 111.00(7) . . ? O2 Nd1 N4 134.99(6) . . ? O12 Nd1 N4 143.26(7) . . ? O5 Nd1 N4 25.05(6) . . ? O11 Nd1 N4 65.92(7) 1_545 . ? O6 Nd1 N4 24.99(6) . . ? O8 Nd1 N4 69.40(7) . . ? O9 Nd1 N4 93.88(7) . . ? O1 Nd1 N4 98.88(6) . . ? O4 Nd1 N4 86.45(6) . . ? O3 Nd1 Zn1 34.99(4) . . ? O2 Nd1 Zn1 33.45(4) . . ? O12 Nd1 Zn1 72.73(5) . . ? O5 Nd1 Zn1 119.60(5) . . ? O11 Nd1 Zn1 79.63(4) 1_545 . ? O6 Nd1 Zn1 146.67(4) . . ? O8 Nd1 Zn1 143.15(5) . . ? O9 Nd1 Zn1 129.08(4) . . ? O1 Nd1 Zn1 94.50(4) . . ? O4 Nd1 Zn1 88.04(4) . . ? N4 Nd1 Zn1 136.29(5) . . ? C2 O1 C1 115.8(2) . . ? C2 O1 Nd1 117.95(14) . . ? C1 O1 Nd1 124.36(17) . . ? C7 O2 Zn1 126.74(15) . . ? C7 O2 Nd1 125.93(15) . . ? Zn1 O2 Nd1 104.95(7) . . ? C13 O3 Zn1 118.87(16) . . ? C13 O3 Nd1 133.40(16) . . ? Zn1 O3 Nd1 103.72(7) . . ? C14 O4 C18 115.2(2) . . ? C14 O4 Nd1 115.03(16) . . ? C18 O4 Nd1 129.75(17) . . ? N4 O5 Nd1 96.79(15) . . ? N4 O6 Nd1 95.32(15) . . ? N5 O8 Nd1 97.55(16) . . ? N5 O9 Nd1 96.74(15) . . ? Nd1 O12 H12A 118.1 . . ? Nd1 O12 H12B 125.6 . . ? H12A O12 H12B 116.0 . . ? N3 Zn1 O2 113.15(9) . . ? N3 Zn1 N1 111.00(10) . . ? O2 Zn1 N1 90.30(8) . . ? N3 Zn1 O3 102.60(9) . . ? O2 Zn1 O3 81.31(7) . . ? N1 Zn1 O3 145.95(8) . . ? N3 Zn1 N2 105.78(10) . . ? O2 Zn1 N2 140.85(8) . . ? N1 Zn1 N2 79.32(10) . . ? O3 Zn1 N2 86.58(9) . . ? N3 Zn1 Nd1 104.97(8) . . ? O2 Zn1 Nd1 41.60(5) . . ? N1 Zn1 Nd1 128.96(7) . . ? O3 Zn1 Nd1 41.29(5) . . ? N2 Zn1 Nd1 123.90(7) . . ? C19 O11 Nd1 144.61(18) . 1_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.376 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.061 # Attachment '3b.cif' data_wy1751 _database_code_depnum_ccdc_archive 'CCDC 700788' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 N7 Nd O11 S2 Zn2, C2 H3 N' _chemical_formula_sum 'C40 H39 N8 Nd O11 S2 Zn2' _chemical_formula_weight 1146.89 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' S S 0.1246 0.1234 '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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2378(6) _cell_length_b 12.5947(6) _cell_length_c 16.5103(8) _cell_angle_alpha 87.8249(10) _cell_angle_beta 69.1710(09) _cell_angle_gamma 70.7700(10) _cell_volume 2236.69(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14021 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 2.368 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5369 _exptl_absorpt_correction_T_max 0.7031 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11182 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7712 _reflns_number_gt 6395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0455P)^2^+1.1272P] 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 7712 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.045 _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 C1 C -0.1197(5) 0.9568(4) 0.9741(3) 0.0529(12) Uani 1 1 d U . . H1A H -0.1093 0.9179 1.0234 0.079 Uiso 1 1 calc R . . H1B H -0.2066 0.9886 0.9835 0.079 Uiso 1 1 calc R . . H1C H -0.0848 1.0162 0.9666 0.079 Uiso 1 1 calc R . . C2 C -0.0910(4) 0.7838(4) 0.8987(3) 0.0403(10) Uani 1 1 d U . . C3 C -0.1971(5) 0.7701(4) 0.9578(3) 0.0536(12) Uani 1 1 d U . . H3A H -0.2512 0.8257 1.0028 0.064 Uiso 1 1 calc R . . C4 C -0.2223(5) 0.6715(5) 0.9492(4) 0.0665(15) Uani 1 1 d U . . H4A H -0.2932 0.6609 0.9890 0.080 Uiso 1 1 calc R . . C5 C -0.1425(5) 0.5902(5) 0.8820(4) 0.0586(14) Uani 1 1 d U . . H5A H -0.1619 0.5263 0.8759 0.070 Uiso 1 1 calc R . . C6 C -0.0325(5) 0.6012(4) 0.8224(3) 0.0443(11) Uani 1 1 d U . . C7 C -0.0051(4) 0.7007(3) 0.8305(3) 0.0376(10) Uani 1 1 d U . . C8 C 0.0423(5) 0.5121(4) 0.7522(3) 0.0482(12) Uani 1 1 d U . . H8A H 0.0121 0.4540 0.7499 0.058 Uiso 1 1 calc R . . C9 C 0.2083(5) 0.4159(4) 0.6217(3) 0.0576(14) Uani 1 1 d U . . H9A H 0.1611 0.4270 0.5839 0.069 Uiso 1 1 calc R . . H9B H 0.2134 0.3432 0.6449 0.069 Uiso 1 1 calc R . . C10 C 0.3385(5) 0.4182(4) 0.5704(4) 0.0587(14) Uani 1 1 d U . . H10A H 0.3939 0.3835 0.6011 0.070 Uiso 1 1 calc R . . H10B H 0.3712 0.3770 0.5136 0.070 Uiso 1 1 calc R . . C11 C 0.3452(5) 0.5767(4) 0.4874(3) 0.0492(12) Uani 1 1 d U . . H11A H 0.3798 0.5251 0.4386 0.059 Uiso 1 1 calc R . . C12 C 0.3149(4) 0.6957(4) 0.4727(3) 0.0429(11) Uani 1 1 d U . . C13 C 0.3408(5) 0.7230(5) 0.3863(3) 0.0571(13) Uani 1 1 d U . . H13A H 0.3836 0.6653 0.3415 0.069 Uiso 1 1 calc R . . C14 C 0.3048(5) 0.8318(5) 0.3666(3) 0.0645(15) Uani 1 1 d U . . H14A H 0.3260 0.8479 0.3088 0.077 Uiso 1 1 calc R . . C15 C 0.2371(5) 0.9184(5) 0.4320(3) 0.0602(14) Uani 1 1 d U . . H15A H 0.2103 0.9926 0.4186 0.072 Uiso 1 1 calc R . . C16 C 0.2095(5) 0.8939(4) 0.5174(3) 0.0453(11) Uani 1 1 d U . . C17 C 0.2501(4) 0.7842(4) 0.5410(3) 0.0389(10) Uani 1 1 d U . . C18 C 0.0929(7) 1.0891(5) 0.5709(4) 0.091(2) Uani 1 1 d U . . H18A H 0.0757 1.0920 0.5183 0.137 Uiso 1 1 calc R . . H18B H 0.1549 1.1230 0.5641 0.137 Uiso 1 1 calc R . . H18C H 0.0182 1.1294 0.6183 0.137 Uiso 1 1 calc R . . C19 C 0.4112(6) 0.9456(6) 0.6135(4) 0.088(2) Uani 1 1 d U . . H19A H 0.4318 0.9951 0.5693 0.132 Uiso 1 1 calc R . . H19B H 0.4093 0.8795 0.5877 0.132 Uiso 1 1 calc R . . H19C H 0.4726 0.9239 0.6400 0.132 Uiso 1 1 calc R . . C20 C 0.2806(4) 1.0980(4) 0.7245(3) 0.0456(11) Uani 1 1 d U . . C21 C 0.3753(5) 1.1386(4) 0.7157(4) 0.0580(13) Uani 1 1 d U . . H21A H 0.4545 1.1028 0.6751 0.070 Uiso 1 1 calc R . . C22 C 0.3519(5) 1.2333(5) 0.7677(4) 0.0619(14) Uani 1 1 d U . . H22A H 0.4155 1.2615 0.7616 0.074 Uiso 1 1 calc R . . C23 C 0.2374(5) 1.2850(4) 0.8273(3) 0.0525(12) Uani 1 1 d U . . H23A H 0.2239 1.3479 0.8621 0.063 Uiso 1 1 calc R . . C24 C 0.1373(4) 1.2461(3) 0.8382(3) 0.0410(10) Uani 1 1 d U . . C25 C 0.1601(4) 1.1501(3) 0.7844(3) 0.0384(10) Uani 1 1 d U . . C26 C 0.0187(5) 1.3003(3) 0.9074(3) 0.0445(11) Uani 1 1 d U . . H26A H 0.0163 1.3498 0.9489 0.053 Uiso 1 1 calc R . . C27 C -0.1948(5) 1.3304(4) 0.9919(3) 0.0523(12) Uani 1 1 d U . . H27A H -0.2008 1.4039 1.0126 0.063 Uiso 1 1 calc R . . H27B H -0.1921 1.2806 1.0379 0.063 Uiso 1 1 calc R . . C28 C -0.3075(5) 1.3411(4) 0.9689(3) 0.0545(13) Uani 1 1 d U . . H28A H -0.3781 1.3456 1.0214 0.065 Uiso 1 1 calc R . . H28B H -0.3286 1.4094 0.9402 0.065 Uiso 1 1 calc R . . C29 C -0.3535(5) 1.1891(4) 0.9210(3) 0.0489(12) Uani 1 1 d U . . H29A H -0.4299 1.2160 0.9665 0.059 Uiso 1 1 calc R . . C30 C -0.3300(4) 1.0892(4) 0.8666(3) 0.0459(11) Uani 1 1 d U . . C31 C -0.4297(5) 1.0503(5) 0.8808(4) 0.0654(15) Uani 1 1 d U . . H31A H -0.5063 1.0882 0.9234 0.078 Uiso 1 1 calc R . . C32 C -0.4161(6) 0.9574(5) 0.8328(4) 0.0718(16) Uani 1 1 d U . . H32A H -0.4841 0.9347 0.8413 0.086 Uiso 1 1 calc R . . C33 C -0.3025(5) 0.8979(5) 0.7723(4) 0.0620(14) Uani 1 1 d U . . H33A H -0.2938 0.8345 0.7402 0.074 Uiso 1 1 calc R . . C34 C -0.2018(5) 0.9309(4) 0.7585(3) 0.0434(11) Uani 1 1 d U . . C35 C -0.2127(4) 1.0287(4) 0.8043(3) 0.0395(10) Uani 1 1 d U . . C36 C -0.0631(5) 0.7822(4) 0.6443(3) 0.0570(13) Uani 1 1 d U . . H36A H -0.1403 0.7879 0.6389 0.086 Uiso 1 1 calc R . . H36B H -0.0328 0.7128 0.6682 0.086 Uiso 1 1 calc R . . H36C H -0.0034 0.7834 0.5880 0.086 Uiso 1 1 calc R . . C37 C 0.4064(5) 0.4999(4) 0.7897(3) 0.0475(11) Uani 1 1 d U . . C38 C -0.0982(5) 1.3528(4) 0.6622(3) 0.0601(12) Uani 1 1 d U . . C39 C 0.6851(8) 0.7435(7) 0.5897(6) 0.114(3) Uani 1 1 d DU . . H39A H 0.6183 0.7678 0.5682 0.171 Uiso 1 1 calc R . . H39B H 0.7595 0.6979 0.5445 0.171 Uiso 1 1 calc R . . H39C H 0.6983 0.8083 0.6079 0.171 Uiso 1 1 calc R . . C40 C 0.6553(9) 0.6810(8) 0.6595(7) 0.125(3) Uani 1 1 d DU . . N1 N 0.1457(4) 0.5068(3) 0.6937(3) 0.0469(9) Uani 1 1 d U . . N2 N 0.3284(4) 0.5372(3) 0.5609(2) 0.0463(9) Uani 1 1 d U . . N3 N -0.0821(4) 1.2852(3) 0.9154(2) 0.0427(9) Uani 1 1 d U . . N4 N -0.2784(4) 1.2422(3) 0.9111(2) 0.0432(9) Uani 1 1 d U . . N5 N 0.3595(4) 0.5472(4) 0.7428(3) 0.0493(11) Uani 1 1 d U . . N6 N -0.1108(4) 1.3094(3) 0.7260(3) 0.0564(11) Uani 1 1 d U . . N7 N 0.2904(4) 0.8396(3) 0.8288(3) 0.0481(10) Uani 1 1 d U . . N8 N 0.6352(11) 0.6227(10) 0.7308(8) 0.202(5) Uani 1 1 d U . . Nd1 Nd 0.09868(2) 0.913418(18) 0.745441(14) 0.03328(8) Uani 1 1 d U . . O1 O -0.0572(3) 0.8784(2) 0.89705(19) 0.0452(7) Uani 1 1 d U . . O2 O 0.0921(3) 0.7244(2) 0.77714(18) 0.0382(7) Uani 1 1 d U . . O3 O 0.2224(3) 0.7696(2) 0.62490(17) 0.0414(7) Uani 1 1 d U . . O4 O 0.1373(3) 0.9740(3) 0.5888(2) 0.0563(9) Uani 1 1 d U . . O5 O 0.2915(3) 1.0029(3) 0.6783(2) 0.0547(9) Uani 1 1 d U . . O6 O 0.0747(3) 1.1054(2) 0.7873(2) 0.0417(7) Uani 1 1 d U . . O7 O -0.1097(3) 1.0542(2) 0.78644(19) 0.0381(7) Uani 1 1 d U . . O8 O -0.0822(3) 0.8764(3) 0.7013(2) 0.0487(8) Uani 1 1 d U . . O9 O 0.3165(3) 0.7962(3) 0.7536(2) 0.0463(9) Uani 1 1 d U . . O10 O 0.1812(4) 0.9050(3) 0.8660(2) 0.0503(9) Uani 1 1 d U . . O11 O 0.3674(4) 0.8183(4) 0.8639(3) 0.0768(12) Uani 1 1 d U . . S1 S 0.47471(16) 0.43197(13) 0.85268(10) 0.0714(4) Uani 1 1 d U . . S2 S -0.07720(18) 1.41392(17) 0.57291(11) 0.0865(5) Uani 1 1 d U . . Zn1 Zn 0.24225(5) 0.61897(4) 0.68321(3) 0.03997(13) Uani 1 1 d U . . Zn2 Zn -0.10608(5) 1.20604(4) 0.81751(3) 0.03864(13) Uani 1 1 d U . . 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 C1 0.063(3) 0.047(3) 0.035(2) -0.004(2) -0.011(2) -0.008(2) C2 0.044(3) 0.040(2) 0.037(2) 0.0108(19) -0.016(2) -0.013(2) C3 0.049(3) 0.058(3) 0.045(3) 0.009(2) -0.008(2) -0.016(2) C4 0.055(3) 0.074(4) 0.068(4) 0.022(3) -0.011(3) -0.034(3) C5 0.062(3) 0.057(3) 0.065(3) 0.020(3) -0.021(3) -0.034(3) C6 0.052(3) 0.039(2) 0.048(3) 0.013(2) -0.020(2) -0.021(2) C7 0.042(3) 0.038(2) 0.034(2) 0.0115(18) -0.0140(19) -0.0152(19) C8 0.058(3) 0.036(2) 0.062(3) 0.012(2) -0.029(3) -0.023(2) C9 0.071(4) 0.041(3) 0.065(3) -0.007(2) -0.030(3) -0.016(2) C10 0.068(4) 0.038(3) 0.062(3) -0.009(2) -0.022(3) -0.008(2) C11 0.045(3) 0.052(3) 0.040(3) -0.012(2) -0.010(2) -0.007(2) C12 0.042(3) 0.049(3) 0.035(2) -0.001(2) -0.013(2) -0.012(2) C13 0.057(3) 0.067(3) 0.035(3) -0.006(2) -0.011(2) -0.012(3) C14 0.070(4) 0.073(4) 0.035(3) 0.011(2) -0.014(3) -0.011(3) C15 0.071(4) 0.059(3) 0.037(3) 0.013(2) -0.018(2) -0.008(3) C16 0.050(3) 0.046(3) 0.032(2) 0.002(2) -0.013(2) -0.009(2) C17 0.039(2) 0.043(2) 0.032(2) 0.0018(18) -0.0108(19) -0.0129(19) C18 0.130(6) 0.048(3) 0.055(3) 0.009(3) -0.018(4) 0.002(3) C19 0.069(4) 0.088(4) 0.084(4) -0.017(3) 0.008(3) -0.034(3) C20 0.048(3) 0.038(2) 0.052(3) 0.010(2) -0.015(2) -0.019(2) C21 0.049(3) 0.059(3) 0.066(3) 0.007(3) -0.016(3) -0.024(3) C22 0.056(3) 0.064(3) 0.079(4) 0.014(3) -0.028(3) -0.033(3) C23 0.064(3) 0.045(3) 0.064(3) 0.010(2) -0.034(3) -0.027(2) C24 0.050(3) 0.033(2) 0.047(3) 0.0131(19) -0.024(2) -0.018(2) C25 0.040(3) 0.035(2) 0.046(3) 0.0138(19) -0.019(2) -0.0174(19) C26 0.064(3) 0.030(2) 0.048(3) 0.0050(19) -0.029(2) -0.017(2) C27 0.060(3) 0.046(3) 0.043(3) -0.001(2) -0.013(2) -0.013(2) C28 0.053(3) 0.044(3) 0.052(3) -0.003(2) -0.009(2) -0.008(2) C29 0.038(3) 0.051(3) 0.048(3) 0.008(2) -0.011(2) -0.008(2) C30 0.042(3) 0.054(3) 0.046(3) 0.012(2) -0.019(2) -0.019(2) C31 0.042(3) 0.081(4) 0.072(4) 0.006(3) -0.015(3) -0.026(3) C32 0.054(4) 0.087(4) 0.087(4) 0.005(3) -0.025(3) -0.041(3) C33 0.064(4) 0.066(3) 0.073(4) 0.003(3) -0.032(3) -0.036(3) C34 0.050(3) 0.046(2) 0.044(3) 0.010(2) -0.023(2) -0.021(2) C35 0.042(3) 0.039(2) 0.045(2) 0.0147(19) -0.022(2) -0.017(2) C36 0.073(4) 0.050(3) 0.060(3) -0.002(2) -0.038(3) -0.021(3) C37 0.048(3) 0.043(3) 0.050(3) -0.006(2) -0.020(2) -0.010(2) C38 0.061(3) 0.056(3) 0.066(3) 0.012(2) -0.024(2) -0.016(2) C39 0.089(5) 0.121(6) 0.129(6) -0.058(5) -0.060(5) -0.001(4) C40 0.105(6) 0.110(6) 0.153(7) -0.070(5) -0.059(6) -0.008(5) N1 0.057(3) 0.035(2) 0.054(2) 0.0018(17) -0.027(2) -0.0151(18) N2 0.050(2) 0.041(2) 0.043(2) -0.0037(17) -0.0161(19) -0.0093(18) N3 0.050(2) 0.0355(19) 0.040(2) 0.0015(16) -0.0134(18) -0.0131(17) N4 0.040(2) 0.038(2) 0.044(2) 0.0017(16) -0.0119(17) -0.0055(17) N5 0.053(3) 0.041(2) 0.063(3) 0.008(2) -0.040(2) -0.013(2) N6 0.070(3) 0.048(2) 0.054(3) 0.016(2) -0.024(2) -0.024(2) N7 0.051(3) 0.049(2) 0.053(2) 0.012(2) -0.023(2) -0.025(2) N8 0.188(8) 0.190(8) 0.208(8) 0.029(7) -0.030(6) -0.085(7) Nd1 0.04084(15) 0.02824(12) 0.02884(13) 0.00133(9) -0.01042(10) -0.01158(10) O1 0.055(2) 0.0393(17) 0.0341(16) 0.0001(13) -0.0076(14) -0.0156(15) O2 0.0415(18) 0.0324(15) 0.0351(16) 0.0023(12) -0.0064(13) -0.0134(13) O3 0.054(2) 0.0382(16) 0.0268(15) 0.0011(12) -0.0109(14) -0.0123(14) O4 0.079(3) 0.0392(17) 0.0342(17) 0.0083(14) -0.0137(17) -0.0078(16) O5 0.043(2) 0.0485(19) 0.059(2) -0.0082(16) 0.0002(16) -0.0176(15) O6 0.0403(18) 0.0324(15) 0.0512(18) 0.0003(13) -0.0121(14) -0.0152(13) O7 0.0352(17) 0.0357(15) 0.0438(17) 0.0045(13) -0.0128(13) -0.0141(13) O8 0.055(2) 0.0428(17) 0.056(2) -0.0006(15) -0.0267(17) -0.0190(16) O9 0.047(2) 0.050(2) 0.041(2) -0.0043(17) -0.0180(17) -0.0196(17) O10 0.050(2) 0.059(2) 0.035(2) -0.0063(17) -0.0222(18) -0.0091(19) O11 0.070(3) 0.103(3) 0.078(3) 0.021(2) -0.047(2) -0.035(2) S1 0.0839(11) 0.0677(9) 0.0657(9) 0.0050(7) -0.0456(9) -0.0093(8) S2 0.0882(13) 0.1102(13) 0.0734(11) 0.0534(10) -0.0386(10) -0.0441(11) Zn1 0.0445(3) 0.0338(3) 0.0402(3) 0.0006(2) -0.0170(2) -0.0095(2) Zn2 0.0429(3) 0.0323(3) 0.0386(3) 0.0041(2) -0.0126(2) -0.0126(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 C1 O1 1.443(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.379(6) . ? C2 O1 1.381(5) . ? C2 C7 1.411(6) . ? C3 C4 1.398(7) . ? C3 H3A 0.9300 . ? C4 C5 1.375(8) . ? C4 H4A 0.9300 . ? C5 C6 1.403(7) . ? C5 H5A 0.9300 . ? C6 C7 1.423(6) . ? C6 C8 1.451(7) . ? C7 O2 1.322(5) . ? C8 N1 1.272(6) . ? C8 H8A 0.9300 . ? C9 N1 1.479(6) . ? C9 C10 1.525(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.470(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.268(6) . ? C11 C12 1.453(7) . ? C11 H11A 0.9300 . ? C12 C13 1.401(6) . ? C12 C17 1.421(6) . ? C13 C14 1.360(7) . ? C13 H13A 0.9300 . ? C14 C15 1.378(7) . ? C14 H14A 0.9300 . ? C15 C16 1.376(6) . ? C15 H15A 0.9300 . ? C16 O4 1.396(5) . ? C16 C17 1.397(6) . ? C17 O3 1.325(5) . ? C18 O4 1.431(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.435(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.375(7) . ? C20 O5 1.388(5) . ? C20 C25 1.399(6) . ? C21 C22 1.386(7) . ? C21 H21A 0.9300 . ? C22 C23 1.350(7) . ? C22 H22A 0.9300 . ? C23 C24 1.416(6) . ? C23 H23A 0.9300 . ? C24 C25 1.418(6) . ? C24 C26 1.451(7) . ? C25 O6 1.327(5) . ? C26 N3 1.269(6) . ? C26 H26A 0.9300 . ? C27 N3 1.455(6) . ? C27 C28 1.519(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N4 1.464(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.269(6) . ? C29 C30 1.460(7) . ? C29 H29A 0.9300 . ? C30 C31 1.403(7) . ? C30 C35 1.410(6) . ? C31 C32 1.368(8) . ? C31 H31A 0.9300 . ? C32 C33 1.369(8) . ? C32 H32A 0.9300 . ? C33 C34 1.369(7) . ? C33 H33A 0.9300 . ? C34 O8 1.382(6) . ? C34 C35 1.414(6) . ? C35 O7 1.332(5) . ? C36 O8 1.447(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N5 1.157(6) . ? C37 S1 1.610(5) . ? C38 N6 1.152(6) . ? C38 S2 1.615(5) . ? C39 C40 1.379(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N8 1.354(13) . ? N1 Zn1 2.088(4) . ? N2 Zn1 2.044(4) . ? N3 Zn2 2.085(4) . ? N4 Zn2 2.036(4) . ? N5 Zn1 1.982(4) . ? N6 Zn2 1.961(4) . ? N7 O11 1.227(5) . ? N7 O10 1.253(5) . ? N7 O9 1.264(5) . ? N7 Nd1 3.004(4) . ? Nd1 O3 2.420(3) . ? Nd1 O6 2.434(3) . ? Nd1 O2 2.439(3) . ? Nd1 O7 2.448(3) . ? Nd1 O10 2.517(3) . ? Nd1 O4 2.591(3) . ? Nd1 O9 2.637(4) . ? Nd1 O1 2.678(3) . ? Nd1 O8 2.739(3) . ? Nd1 O5 2.805(3) . ? Nd1 Zn1 3.5509(5) . ? O2 Zn1 2.017(3) . ? O3 Zn1 2.076(3) . ? O6 Zn2 2.042(3) . ? O7 Zn2 2.016(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 125.4(4) . . ? C3 C2 C7 122.4(4) . . ? O1 C2 C7 112.2(4) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.8(5) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C7 118.9(4) . . ? C5 C6 C8 116.9(4) . . ? C7 C6 C8 124.0(4) . . ? O2 C7 C2 116.8(4) . . ? O2 C7 C6 125.4(4) . . ? C2 C7 C6 117.7(4) . . ? N1 C8 C6 125.5(4) . . ? N1 C8 H8A 117.2 . . ? C6 C8 H8A 117.2 . . ? N1 C9 C10 109.0(4) . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C9 107.3(4) . . ? N2 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? N2 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C12 125.6(4) . . ? N2 C11 H11A 117.2 . . ? C12 C11 H11A 117.2 . . ? C13 C12 C17 119.0(4) . . ? C13 C12 C11 117.3(4) . . ? C17 C12 C11 123.4(4) . . ? C14 C13 C12 121.5(5) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 O4 124.2(4) . . ? C15 C16 C17 122.5(4) . . ? O4 C16 C17 113.2(4) . . ? O3 C17 C16 118.1(4) . . ? O3 C17 C12 124.8(4) . . ? C16 C17 C12 117.1(4) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O5 125.6(5) . . ? C21 C20 C25 121.9(4) . . ? O5 C20 C25 112.5(4) . . ? C20 C21 C22 119.5(5) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 121.8(5) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C23 C24 C25 118.1(4) . . ? C23 C24 C26 119.1(4) . . ? C25 C24 C26 122.6(4) . . ? O6 C25 C20 117.4(4) . . ? O6 C25 C24 124.3(4) . . ? C20 C25 C24 118.3(4) . . ? N3 C26 C24 124.8(4) . . ? N3 C26 H26A 117.6 . . ? C24 C26 H26A 117.6 . . ? N3 C27 C28 109.7(4) . . ? N3 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? N3 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N4 C28 C27 108.8(4) . . ? N4 C28 H28A 109.9 . . ? C27 C28 H28A 109.9 . . ? N4 C28 H28B 109.9 . . ? C27 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? N4 C29 C30 125.4(5) . . ? N4 C29 H29A 117.3 . . ? C30 C29 H29A 117.3 . . ? C31 C30 C35 119.2(5) . . ? C31 C30 C29 117.1(5) . . ? C35 C30 C29 123.6(4) . . ? C32 C31 C30 121.1(5) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C33 120.1(5) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 120.7(5) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 O8 126.1(4) . . ? C33 C34 C35 121.1(5) . . ? O8 C34 C35 112.8(4) . . ? O7 C35 C30 125.4(4) . . ? O7 C35 C34 116.9(4) . . ? C30 C35 C34 117.7(4) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 S1 178.4(5) . . ? N6 C38 S2 178.5(5) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N8 C40 C39 173.6(10) . . ? C8 N1 C9 120.3(4) . . ? C8 N1 Zn1 126.9(3) . . ? C9 N1 Zn1 112.8(3) . . ? C11 N2 C10 121.0(4) . . ? C11 N2 Zn1 130.0(3) . . ? C10 N2 Zn1 106.9(3) . . ? C26 N3 C27 122.4(4) . . ? C26 N3 Zn2 123.5(3) . . ? C27 N3 Zn2 113.9(3) . . ? C29 N4 C28 122.5(4) . . ? C29 N4 Zn2 126.8(3) . . ? C28 N4 Zn2 110.7(3) . . ? C37 N5 Zn1 165.3(5) . . ? C38 N6 Zn2 167.3(4) . . ? O11 N7 O10 121.7(4) . . ? O11 N7 O9 121.9(5) . . ? O10 N7 O9 116.4(4) . . ? O11 N7 Nd1 175.0(3) . . ? O10 N7 Nd1 55.6(2) . . ? O9 N7 Nd1 61.1(2) . . ? O3 Nd1 O6 139.34(10) . . ? O3 Nd1 O2 65.04(9) . . ? O6 Nd1 O2 153.06(10) . . ? O3 Nd1 O7 132.82(10) . . ? O6 Nd1 O7 62.92(10) . . ? O2 Nd1 O7 111.93(9) . . ? O3 Nd1 O10 115.97(11) . . ? O6 Nd1 O10 72.32(11) . . ? O2 Nd1 O10 86.54(11) . . ? O7 Nd1 O10 110.59(11) . . ? O3 Nd1 O4 61.69(9) . . ? O6 Nd1 O4 86.49(10) . . ? O2 Nd1 O4 120.28(10) . . ? O7 Nd1 O4 86.96(10) . . ? O10 Nd1 O4 140.61(13) . . ? O3 Nd1 O9 67.87(10) . . ? O6 Nd1 O9 102.39(10) . . ? O2 Nd1 O9 74.03(10) . . ? O7 Nd1 O9 159.31(10) . . ? O10 Nd1 O9 48.99(11) . . ? O4 Nd1 O9 107.50(11) . . ? O3 Nd1 O1 123.68(9) . . ? O6 Nd1 O1 96.72(9) . . ? O2 Nd1 O1 59.06(9) . . ? O7 Nd1 O1 67.95(10) . . ? O10 Nd1 O1 67.98(11) . . ? O4 Nd1 O1 149.34(11) . . ? O9 Nd1 O1 101.58(10) . . ? O3 Nd1 O8 78.77(10) . . ? O6 Nd1 O8 119.15(10) . . ? O2 Nd1 O8 69.68(10) . . ? O7 Nd1 O8 58.62(9) . . ? O10 Nd1 O8 143.98(11) . . ? O4 Nd1 O8 75.35(11) . . ? O9 Nd1 O8 138.43(10) . . ? O1 Nd1 O8 76.53(10) . . ? O3 Nd1 O5 84.79(10) . . ? O6 Nd1 O5 57.57(10) . . ? O2 Nd1 O5 133.87(10) . . ? O7 Nd1 O5 114.17(9) . . ? O10 Nd1 O5 75.95(12) . . ? O4 Nd1 O5 64.67(11) . . ? O9 Nd1 O5 62.18(11) . . ? O1 Nd1 O5 141.09(10) . . ? O8 Nd1 O5 139.91(10) . . ? O3 Nd1 N7 92.45(11) . . ? O6 Nd1 N7 85.99(10) . . ? O2 Nd1 N7 80.72(10) . . ? O7 Nd1 N7 134.60(11) . . ? O10 Nd1 N7 24.25(11) . . ? O4 Nd1 N7 125.41(12) . . ? O9 Nd1 N7 24.81(10) . . ? O1 Nd1 N7 85.26(11) . . ? O8 Nd1 N7 150.16(10) . . ? O5 Nd1 N7 65.88(10) . . ? O3 Nd1 Zn1 34.55(7) . . ? O6 Nd1 Zn1 159.32(7) . . ? O2 Nd1 Zn1 33.23(7) . . ? O7 Nd1 Zn1 137.64(6) . . ? O10 Nd1 Zn1 93.69(8) . . ? O4 Nd1 Zn1 95.80(7) . . ? O9 Nd1 Zn1 57.30(7) . . ? O1 Nd1 Zn1 91.74(6) . . ? O8 Nd1 Zn1 81.15(7) . . ? O5 Nd1 Zn1 104.94(7) . . ? N7 Nd1 Zn1 75.92(8) . . ? C2 O1 C1 117.2(4) . . ? C2 O1 Nd1 117.2(2) . . ? C1 O1 Nd1 125.2(3) . . ? C7 O2 Zn1 127.2(3) . . ? C7 O2 Nd1 125.6(3) . . ? Zn1 O2 Nd1 105.28(11) . . ? C17 O3 Zn1 128.0(3) . . ? C17 O3 Nd1 126.8(3) . . ? Zn1 O3 Nd1 104.06(11) . . ? C16 O4 C18 117.2(4) . . ? C16 O4 Nd1 120.1(2) . . ? C18 O4 Nd1 122.6(3) . . ? C20 O5 C19 116.5(4) . . ? C20 O5 Nd1 116.7(3) . . ? C19 O5 Nd1 125.2(3) . . ? C25 O6 Zn2 120.2(3) . . ? C25 O6 Nd1 129.9(3) . . ? Zn2 O6 Nd1 109.47(12) . . ? C35 O7 Zn2 124.7(3) . . ? C35 O7 Nd1 123.9(2) . . ? Zn2 O7 Nd1 109.83(12) . . ? C34 O8 C36 117.4(4) . . ? C34 O8 Nd1 114.3(2) . . ? C36 O8 Nd1 125.1(3) . . ? N7 O9 Nd1 94.1(3) . . ? N7 O10 Nd1 100.2(3) . . ? N5 Zn1 O2 104.37(16) . . ? N5 Zn1 N2 103.92(17) . . ? O2 Zn1 N2 151.23(14) . . ? N5 Zn1 O3 127.66(16) . . ? O2 Zn1 O3 79.31(11) . . ? N2 Zn1 O3 87.54(13) . . ? N5 Zn1 N1 103.25(16) . . ? O2 Zn1 N1 89.14(14) . . ? N2 Zn1 N1 79.44(16) . . ? O3 Zn1 N1 129.09(14) . . ? N5 Zn1 Nd1 111.45(12) . . ? O2 Zn1 Nd1 41.50(8) . . ? N2 Zn1 Nd1 128.70(11) . . ? O3 Zn1 Nd1 41.39(8) . . ? N1 Zn1 Nd1 124.34(11) . . ? N6 Zn2 O7 113.51(15) . . ? N6 Zn2 N4 110.25(17) . . ? O7 Zn2 N4 90.14(13) . . ? N6 Zn2 O6 107.18(16) . . ? O7 Zn2 O6 77.78(11) . . ? N4 Zn2 O6 142.43(13) . . ? N6 Zn2 N3 107.38(16) . . ? O7 Zn2 N3 138.80(13) . . ? N4 Zn2 N3 80.22(15) . . ? O6 Zn2 N3 85.85(14) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.802 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.079 # Attachment '2a.cif' data_wy1772 _database_code_depnum_ccdc_archive 'CCDC 729274' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 La N5 O12 Zn' _chemical_formula_sum 'C19 H20 La N5 O12 Zn' _chemical_formula_weight 714.68 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 12.1855(6) _cell_length_b 8.0054(4) _cell_length_c 25.6608(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.7220(10) _cell_angle_gamma 90.00 _cell_volume 2451.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14631 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.32 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.771 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4709 _exptl_absorpt_correction_T_max 0.5938 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11552 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4302 _reflns_number_gt 3886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0260P)^2^+1.2782P] 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 4302 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0431 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6487(3) 0.9177(5) -0.01861(13) 0.0679(10) Uani 1 1 d U . . H1A H 0.6356 0.8730 -0.0541 0.102 Uiso 1 1 calc R . . H1B H 0.6861 1.0235 -0.0179 0.102 Uiso 1 1 calc R . . H1C H 0.5784 0.9327 -0.0078 0.102 Uiso 1 1 calc R . . C2 C 0.8254(2) 0.7814(3) 0.00902(9) 0.0320(5) Uani 1 1 d U . . C3 C 0.8655(2) 0.8538(4) -0.03208(10) 0.0429(6) Uani 1 1 d U . . H3A H 0.8185 0.9189 -0.0572 0.051 Uiso 1 1 calc R . . C4 C 0.9762(2) 0.8291(4) -0.03577(11) 0.0459(7) Uani 1 1 d U . . H4A H 1.0035 0.8767 -0.0637 0.055 Uiso 1 1 calc R . . C5 C 1.0449(2) 0.7355(4) 0.00136(12) 0.0440(7) Uani 1 1 d U . . H5A H 1.1195 0.7219 -0.0012 0.053 Uiso 1 1 calc R . . C6 C 1.0061(2) 0.6584(3) 0.04357(10) 0.0345(6) Uani 1 1 d U . . C7 C 0.89266(19) 0.6786(3) 0.04737(9) 0.0303(5) Uani 1 1 d U . . C8 C 1.0875(2) 0.5644(3) 0.08142(12) 0.0412(6) Uani 1 1 d U . . H8A H 1.1614 0.5663 0.0770 0.049 Uiso 1 1 calc R . . C9 C 1.1544(2) 0.3952(4) 0.15815(13) 0.0557(8) Uani 1 1 d U . . H9A H 1.2274 0.4271 0.1519 0.067 Uiso 1 1 calc R . . H9B H 1.1466 0.2751 0.1540 0.067 Uiso 1 1 calc R . . C10 C 1.1436(2) 0.4457(4) 0.21381(13) 0.0558(8) Uani 1 1 d U . . H10A H 1.1819 0.3651 0.2394 0.067 Uiso 1 1 calc R . . H10B H 1.1781 0.5541 0.2225 0.067 Uiso 1 1 calc R . . C11 C 0.9933(2) 0.4328(4) 0.26006(11) 0.0498(7) Uani 1 1 d U . . H11A H 1.0482 0.4070 0.2898 0.060 Uiso 1 1 calc R . . C12 C 0.8792(2) 0.4462(3) 0.26774(10) 0.0449(7) Uani 1 1 d U . . C13 C 0.8590(3) 0.3968(4) 0.31786(11) 0.0566(8) Uani 1 1 d U . . H13A H 0.9187 0.3613 0.3442 0.068 Uiso 1 1 calc R . . C14 C 0.7540(3) 0.4002(4) 0.32834(11) 0.0615(9) Uani 1 1 d U . . H14A H 0.7424 0.3667 0.3615 0.074 Uiso 1 1 calc R . . C15 C 0.6640(3) 0.4536(4) 0.28951(11) 0.0528(8) Uani 1 1 d U . . H15A H 0.5921 0.4546 0.2966 0.063 Uiso 1 1 calc R . . C16 C 0.6813(2) 0.5050(3) 0.24054(10) 0.0396(6) Uani 1 1 d U . . C17 C 0.7885(2) 0.5049(3) 0.22860(9) 0.0359(6) Uani 1 1 d U . . C18 C 0.4852(3) 0.5442(5) 0.20725(14) 0.0664(10) Uani 1 1 d U . . H18A H 0.4713 0.4307 0.2161 0.100 Uiso 1 1 calc R . . H18B H 0.4337 0.5755 0.1753 0.100 Uiso 1 1 calc R . . H18C H 0.4752 0.6163 0.2358 0.100 Uiso 1 1 calc R . . C19 C 0.8373(2) 0.0851(3) 0.12959(10) 0.0342(6) Uani 1 1 d U . . La1 La 0.668504(10) 0.703797(17) 0.109640(5) 0.02669(5) Uani 1 1 d U . . N1 N 1.06630(17) 0.4795(3) 0.12016(9) 0.0407(5) Uani 1 1 d U . . N2 N 1.02467(18) 0.4531(3) 0.21645(9) 0.0466(6) Uani 1 1 d U . . N3 N 0.8593(2) 0.2238(3) 0.13169(10) 0.0488(6) Uani 1 1 d U . . N4 N 0.42224(18) 0.6693(3) 0.04877(10) 0.0467(6) Uani 1 1 d U . . N5 N 0.5850(2) 1.0334(3) 0.14552(10) 0.0477(6) Uani 1 1 d U . . O1 O 0.71741(14) 0.8041(2) 0.01720(7) 0.0378(4) Uani 1 1 d U . . O2 O 0.84419(12) 0.6105(2) 0.08447(6) 0.0314(4) Uani 1 1 d U . . O3 O 0.79960(14) 0.5628(2) 0.18106(6) 0.0347(4) Uani 1 1 d U . . O4 O 0.59833(15) 0.5593(2) 0.19913(7) 0.0426(4) Uani 1 1 d U . . O5 O 0.81747(16) -0.0635(2) 0.12792(8) 0.0513(5) Uani 1 1 d U . . O6 O 0.44480(17) 0.6962(3) 0.09790(9) 0.0605(6) Uani 1 1 d U . . O7 O 0.50153(15) 0.6839(2) 0.02439(7) 0.0425(4) Uani 1 1 d U . . O8 O 0.32890(18) 0.6317(4) 0.02483(10) 0.0849(8) Uani 1 1 d U . . O9 O 0.61334(18) 0.9133(2) 0.17753(7) 0.0510(5) Uani 1 1 d U . . O10 O 0.58405(16) 1.0087(2) 0.09703(7) 0.0467(5) Uani 1 1 d U . . O11 O 0.5605(3) 1.1699(3) 0.16128(11) 0.0831(8) Uani 1 1 d U . . O12 O 0.60893(18) 0.4105(2) 0.08643(8) 0.0563(5) Uani 1 1 d U . . H12A H 0.5998 0.3366 0.1058 0.084 Uiso 1 1 d R . . H12B H 0.6014 0.3849 0.0565 0.084 Uiso 1 1 d R . . Zn1 Zn 0.91563(2) 0.45415(3) 0.142640(11) 0.03265(8) Uani 1 1 d U . . 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 C1 0.0466(18) 0.085(3) 0.074(2) 0.045(2) 0.0157(16) 0.0231(17) C2 0.0318(12) 0.0320(13) 0.0335(13) 0.0006(10) 0.0098(10) -0.0009(10) C3 0.0492(16) 0.0450(16) 0.0361(14) 0.0046(12) 0.0126(12) -0.0013(13) C4 0.0525(17) 0.0463(17) 0.0456(16) 0.0022(13) 0.0257(14) -0.0060(13) C5 0.0397(14) 0.0410(16) 0.0574(17) -0.0098(13) 0.0244(13) -0.0074(12) C6 0.0315(12) 0.0277(13) 0.0457(15) -0.0080(11) 0.0115(11) -0.0021(10) C7 0.0324(12) 0.0248(12) 0.0348(13) -0.0044(10) 0.0096(10) -0.0030(10) C8 0.0274(13) 0.0337(15) 0.0638(18) -0.0084(13) 0.0124(12) -0.0011(11) C9 0.0335(15) 0.0468(18) 0.081(2) 0.0064(16) -0.0026(14) 0.0078(13) C10 0.0375(15) 0.0480(18) 0.071(2) 0.0108(16) -0.0157(14) 0.0012(13) C11 0.0567(18) 0.0390(16) 0.0419(16) 0.0051(13) -0.0179(14) -0.0014(13) C12 0.0619(18) 0.0333(15) 0.0334(14) 0.0023(11) -0.0050(12) -0.0038(13) C13 0.082(2) 0.0477(18) 0.0314(14) 0.0076(13) -0.0080(15) -0.0060(16) C14 0.098(3) 0.055(2) 0.0308(15) 0.0068(14) 0.0126(16) -0.0066(18) C15 0.077(2) 0.0447(17) 0.0416(16) 0.0018(13) 0.0224(15) -0.0042(15) C16 0.0591(17) 0.0291(14) 0.0311(13) -0.0006(11) 0.0106(12) -0.0015(12) C17 0.0548(16) 0.0229(13) 0.0285(12) 0.0007(10) 0.0049(11) -0.0035(11) C18 0.0544(18) 0.084(3) 0.068(2) 0.0238(19) 0.0305(16) 0.0161(18) C19 0.0292(12) 0.0338(16) 0.0386(14) 0.0004(11) 0.0044(10) -0.0013(11) La1 0.02573(8) 0.02498(8) 0.02871(8) 0.00066(5) 0.00399(5) 0.00065(5) N1 0.0281(11) 0.0315(12) 0.0596(14) 0.0026(11) 0.0020(10) 0.0031(9) N2 0.0415(13) 0.0427(14) 0.0476(14) 0.0040(11) -0.0095(10) 0.0000(10) N3 0.0507(14) 0.0295(14) 0.0673(16) -0.0011(11) 0.0143(12) -0.0056(11) N4 0.0327(12) 0.0536(16) 0.0512(15) 0.0045(12) 0.0025(11) 0.0015(10) N5 0.0593(15) 0.0321(13) 0.0584(16) 0.0003(11) 0.0277(12) 0.0047(11) O1 0.0311(9) 0.0443(11) 0.0384(10) 0.0137(8) 0.0076(7) 0.0073(8) O2 0.0276(8) 0.0307(9) 0.0364(9) 0.0064(7) 0.0082(7) 0.0017(7) O3 0.0407(9) 0.0332(10) 0.0291(9) 0.0053(7) 0.0046(7) 0.0031(7) O4 0.0468(10) 0.0439(11) 0.0403(10) 0.0086(8) 0.0159(8) 0.0070(9) O5 0.0499(11) 0.0293(11) 0.0671(13) 0.0009(9) -0.0059(10) -0.0088(9) O6 0.0430(12) 0.0953(19) 0.0458(13) -0.0015(12) 0.0160(10) 0.0007(11) O7 0.0374(10) 0.0494(12) 0.0399(10) 0.0018(8) 0.0056(8) -0.0013(8) O8 0.0326(12) 0.124(2) 0.0896(18) -0.0046(17) -0.0073(11) -0.0132(13) O9 0.0794(14) 0.0369(11) 0.0411(11) 0.0018(9) 0.0225(10) 0.0052(10) O10 0.0546(12) 0.0438(11) 0.0406(11) 0.0046(9) 0.0074(9) 0.0132(9) O11 0.143(2) 0.0354(13) 0.0905(18) 0.0011(12) 0.0704(18) 0.0161(14) O12 0.0892(16) 0.0328(11) 0.0420(11) -0.0007(9) 0.0016(10) -0.0081(10) Zn1 0.02887(15) 0.02575(15) 0.04051(16) 0.00332(12) 0.00041(12) 0.00006(11) _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 C1 O1 1.435(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(3) . ? C2 O1 1.386(3) . ? C2 C7 1.411(3) . ? C3 C4 1.386(4) . ? C3 H3A 0.9300 . ? C4 C5 1.359(4) . ? C4 H4A 0.9300 . ? C5 C6 1.409(4) . ? C5 H5A 0.9300 . ? C6 C7 1.415(3) . ? C6 C8 1.450(4) . ? C7 O2 1.334(3) . ? C8 N1 1.273(3) . ? C8 H8A 0.9300 . ? C9 N1 1.461(3) . ? C9 C10 1.516(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.466(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.265(4) . ? C11 C12 1.446(4) . ? C11 H11A 0.9300 . ? C12 C13 1.414(4) . ? C12 C17 1.415(4) . ? C13 C14 1.360(5) . ? C13 H13A 0.9300 . ? C14 C15 1.391(4) . ? C14 H14A 0.9300 . ? C15 C16 1.379(4) . ? C15 H15A 0.9300 . ? C16 O4 1.380(3) . ? C16 C17 1.401(4) . ? C17 O3 1.337(3) . ? C18 O4 1.441(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.141(3) . ? C19 O5 1.213(3) . ? La1 O3 2.4483(16) . ? La1 O2 2.4737(15) . ? La1 O12 2.4937(19) . ? La1 O5 2.5769(18) 1_565 ? La1 O9 2.6028(18) . ? La1 O10 2.6430(19) . ? La1 O7 2.6725(18) . ? La1 O6 2.682(2) . ? La1 O1 2.6835(16) . ? La1 O4 2.8533(17) . ? La1 N5 3.038(2) . ? La1 Zn1 3.5697(3) . ? N1 Zn1 2.043(2) . ? N2 Zn1 2.081(2) . ? N3 Zn1 1.968(2) . ? N4 O8 1.216(3) . ? N4 O6 1.253(3) . ? N4 O7 1.259(3) . ? N5 O11 1.223(3) . ? N5 O10 1.258(3) . ? N5 O9 1.266(3) . ? O2 Zn1 2.0063(16) . ? O3 Zn1 2.0723(17) . ? O5 La1 2.5769(18) 1_545 ? O12 H12A 0.7948 . ? O12 H12B 0.7810 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 123.8(2) . . ? C3 C2 C7 122.3(2) . . ? O1 C2 C7 113.9(2) . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.7(2) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C7 119.2(2) . . ? C5 C6 C8 116.9(2) . . ? C7 C6 C8 123.9(2) . . ? O2 C7 C2 117.2(2) . . ? O2 C7 C6 125.7(2) . . ? C2 C7 C6 117.1(2) . . ? N1 C8 C6 125.5(2) . . ? N1 C8 H8A 117.3 . . ? C6 C8 H8A 117.3 . . ? N1 C9 C10 108.2(2) . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C9 109.3(2) . . ? N2 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C12 125.7(2) . . ? N2 C11 H11A 117.2 . . ? C12 C11 H11A 117.2 . . ? C13 C12 C17 118.9(3) . . ? C13 C12 C11 116.9(3) . . ? C17 C12 C11 124.2(2) . . ? C14 C13 C12 121.3(3) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 O4 124.9(3) . . ? C15 C16 C17 121.5(3) . . ? O4 C16 C17 113.7(2) . . ? O3 C17 C16 118.1(2) . . ? O3 C17 C12 123.6(2) . . ? C16 C17 C12 118.3(2) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 O5 178.0(3) . . ? O3 La1 O2 65.71(5) . . ? O3 La1 O12 81.89(6) . . ? O2 La1 O12 83.04(6) . . ? O3 La1 O5 82.45(6) . 1_565 ? O2 La1 O5 69.56(6) . 1_565 ? O12 La1 O5 152.17(7) . 1_565 ? O3 La1 O9 90.80(6) . . ? O2 La1 O9 136.39(6) . . ? O12 La1 O9 131.63(6) . . ? O5 La1 O9 71.37(7) 1_565 . ? O3 La1 O10 134.10(6) . . ? O2 La1 O10 125.65(6) . . ? O12 La1 O10 138.85(7) . . ? O5 La1 O10 66.23(6) 1_565 . ? O9 La1 O10 48.69(6) . . ? O3 La1 O7 149.05(6) . . ? O2 La1 O7 108.88(5) . . ? O12 La1 O7 67.17(6) . . ? O5 La1 O7 125.67(6) 1_565 . ? O9 La1 O7 109.22(6) . . ? O10 La1 O7 75.06(6) . . ? O3 La1 O6 124.56(6) . . ? O2 La1 O6 151.36(6) . . ? O12 La1 O6 73.25(7) . . ? O5 La1 O6 134.37(7) 1_565 . ? O9 La1 O6 72.24(7) . . ? O10 La1 O6 69.25(7) . . ? O7 La1 O6 47.10(6) . . ? O3 La1 O1 124.84(5) . . ? O2 La1 O1 60.01(5) . . ? O12 La1 O1 100.18(6) . . ? O5 La1 O1 70.72(6) 1_565 . ? O9 La1 O1 122.19(6) . . ? O10 La1 O1 76.48(5) . . ? O7 La1 O1 64.10(5) . . ? O6 La1 O1 108.11(6) . . ? O3 La1 O4 57.81(5) . . ? O2 La1 O4 120.30(5) . . ? O12 La1 O4 71.95(6) . . ? O5 La1 O4 117.51(6) 1_565 . ? O9 La1 O4 64.04(6) . . ? O10 La1 O4 107.46(5) . . ? O7 La1 O4 109.37(5) . . ? O6 La1 O4 67.49(6) . . ? O1 La1 O4 171.68(6) . . ? O3 La1 N5 112.42(6) . . ? O2 La1 N5 134.62(6) . . ? O12 La1 N5 142.28(7) . . ? O5 La1 N5 65.41(6) 1_565 . ? O9 La1 N5 24.42(6) . . ? O10 La1 N5 24.33(6) . . ? O7 La1 N5 93.08(6) . . ? O6 La1 N5 70.02(7) . . ? O1 La1 N5 98.99(6) . . ? O4 La1 N5 86.25(6) . . ? O3 La1 Zn1 34.28(4) . . ? O2 La1 Zn1 32.85(4) . . ? O12 La1 Zn1 73.75(5) . . ? O5 La1 Zn1 80.36(4) 1_565 . ? O9 La1 Zn1 121.47(5) . . ? O10 La1 Zn1 146.59(4) . . ? O7 La1 Zn1 128.76(4) . . ? O6 La1 Zn1 143.43(5) . . ? O1 La1 Zn1 92.82(3) . . ? O4 La1 Zn1 87.61(4) . . ? N5 La1 Zn1 137.13(5) . . ? C8 N1 C9 122.0(2) . . ? C8 N1 Zn1 127.58(18) . . ? C9 N1 Zn1 110.26(19) . . ? C11 N2 C10 121.0(2) . . ? C11 N2 Zn1 123.6(2) . . ? C10 N2 Zn1 114.37(19) . . ? C19 N3 Zn1 172.1(2) . . ? O8 N4 O6 122.8(3) . . ? O8 N4 O7 120.4(3) . . ? O6 N4 O7 116.8(2) . . ? O11 N5 O10 120.9(3) . . ? O11 N5 O9 121.1(2) . . ? O10 N5 O9 117.9(2) . . ? O11 N5 La1 174.6(2) . . ? O10 N5 La1 59.97(13) . . ? O9 N5 La1 58.18(12) . . ? C2 O1 C1 115.7(2) . . ? C2 O1 La1 118.88(13) . . ? C1 O1 La1 123.38(16) . . ? C7 O2 Zn1 126.69(14) . . ? C7 O2 La1 126.52(14) . . ? Zn1 O2 La1 105.18(6) . . ? C17 O3 Zn1 119.56(15) . . ? C17 O3 La1 132.16(15) . . ? Zn1 O3 La1 104.00(6) . . ? C16 O4 C18 115.8(2) . . ? C16 O4 La1 117.05(15) . . ? C18 O4 La1 127.05(16) . . ? C19 O5 La1 147.52(17) . 1_545 ? N4 O6 La1 97.30(15) . . ? N4 O7 La1 97.61(14) . . ? N5 O9 La1 97.40(14) . . ? N5 O10 La1 95.70(15) . . ? La1 O12 H12A 128.6 . . ? La1 O12 H12B 116.9 . . ? H12A O12 H12B 114.5 . . ? N3 Zn1 O2 113.10(9) . . ? N3 Zn1 N1 111.13(10) . . ? O2 Zn1 N1 90.39(8) . . ? N3 Zn1 O3 102.08(9) . . ? O2 Zn1 O3 81.78(6) . . ? N1 Zn1 O3 146.26(8) . . ? N3 Zn1 N2 105.42(10) . . ? O2 Zn1 N2 141.27(8) . . ? N1 Zn1 N2 79.23(9) . . ? O3 Zn1 N2 86.56(8) . . ? N3 Zn1 La1 103.74(7) . . ? O2 Zn1 La1 41.98(4) . . ? N1 Zn1 La1 129.82(6) . . ? O3 Zn1 La1 41.72(4) . . ? N2 Zn1 La1 124.76(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.363 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.055 # Attachment '3c.cif' data_wy1855 _database_code_depnum_ccdc_archive 'CCDC 729275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 Er N7 O11 S2 Zn2, 0.5(O2)' _chemical_formula_sum 'C38 H36 Er N7 O12 S2 Zn2' _chemical_formula_weight 1144.86 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 10.8792(6) _cell_length_b 14.3457(8) _cell_length_c 14.9616(8) _cell_angle_alpha 75.8170(10) _cell_angle_beta 72.9120(9) _cell_angle_gamma 73.8340(10) _cell_volume 2109.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13048 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 28.28 _exptl_crystal_description Rod _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 3.268 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4029 _exptl_absorpt_correction_T_max 0.6229 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _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 'smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10307 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7191 _reflns_number_gt 6122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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. Hydrogen atoms of disordered water molecules were not added. ; _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^)+(0.0418P)^2^+1.3127P] 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 7191 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.011 _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 C1 C 0.4616(4) 0.5270(3) 0.1498(3) 0.0439(12) Uani 1 1 d U . . H1A H 0.4776 0.4707 0.1985 0.066 Uiso 1 1 calc R . . H1B H 0.5400 0.5523 0.1227 0.066 Uiso 1 1 calc R . . H1C H 0.4377 0.5078 0.1012 0.066 Uiso 1 1 calc R . . C2 C 0.2374(4) 0.5736(3) 0.2394(3) 0.0294(9) Uani 1 1 d U . . C3 C 0.2039(5) 0.4912(3) 0.2305(3) 0.0394(11) Uani 1 1 d U . . H3A H 0.2609 0.4498 0.1895 0.047 Uiso 1 1 calc R . . C4 C 0.0820(5) 0.4710(4) 0.2848(4) 0.0516(13) Uani 1 1 d U . . H4A H 0.0551 0.4180 0.2770 0.062 Uiso 1 1 calc R . . C5 C 0.0026(5) 0.5290(4) 0.3492(4) 0.0491(13) Uani 1 1 d U . . H5A H -0.0762 0.5130 0.3866 0.059 Uiso 1 1 calc R . . C6 C 0.0369(4) 0.6121(3) 0.3603(3) 0.0390(11) Uani 1 1 d U . . C7 C 0.1542(4) 0.6382(3) 0.2997(3) 0.0281(9) Uani 1 1 d U . . C8 C -0.0386(4) 0.6602(4) 0.4407(3) 0.0460(13) Uani 1 1 d U . . H8A H -0.1049 0.6319 0.4840 0.055 Uiso 1 1 calc R . . C9 C -0.0881(5) 0.7781(4) 0.5431(3) 0.0551(15) Uani 1 1 d U . . H9A H -0.1292 0.7296 0.5912 0.066 Uiso 1 1 calc R . . H9B H -0.1562 0.8363 0.5306 0.066 Uiso 1 1 calc R . . C10 C 0.0142(5) 0.8049(4) 0.5778(3) 0.0621(16) Uani 1 1 d U . . H10A H -0.0298 0.8497 0.6225 0.075 Uiso 1 1 calc R . . H10B H 0.0638 0.7458 0.6101 0.075 Uiso 1 1 calc R . . C11 C 0.1843(5) 0.8959(4) 0.5085(3) 0.0512(14) Uani 1 1 d U . . H11A H 0.1768 0.9022 0.5704 0.061 Uiso 1 1 calc R . . C12 C 0.2861(5) 0.9369(3) 0.4337(3) 0.0417(11) Uani 1 1 d U . . C13 C 0.3493(6) 0.9969(4) 0.4575(4) 0.0527(14) Uani 1 1 d U . . H13A H 0.3221 1.0118 0.5184 0.063 Uiso 1 1 calc R . . C14 C 0.4500(6) 1.0338(3) 0.3931(4) 0.0549(14) Uani 1 1 d U . . H14A H 0.4870 1.0762 0.4099 0.066 Uiso 1 1 calc R . . C15 C 0.4987(5) 1.0090(3) 0.3021(3) 0.0418(11) Uani 1 1 d U . . H15A H 0.5689 1.0327 0.2588 0.050 Uiso 1 1 calc R . . C16 C 0.4390(4) 0.9481(3) 0.2790(3) 0.0312(10) Uani 1 1 d U . . C17 C 0.3300(4) 0.9142(3) 0.3411(3) 0.0309(9) Uani 1 1 d U . . C18 C 0.5542(4) 0.9690(3) 0.1135(3) 0.0334(10) Uani 1 1 d U . . H18A H 0.6344 0.9715 0.1266 0.050 Uiso 1 1 calc R . . H18B H 0.5025 1.0348 0.1010 0.050 Uiso 1 1 calc R . . H18C H 0.5749 0.9384 0.0591 0.050 Uiso 1 1 calc R . . C19 C 0.2931(4) 0.5471(3) 0.4846(3) 0.0426(12) Uani 1 1 d U . . H19A H 0.2539 0.5134 0.4560 0.064 Uiso 1 1 calc R . . H19B H 0.2252 0.5927 0.5197 0.064 Uiso 1 1 calc R . . H19C H 0.3415 0.4999 0.5268 0.064 Uiso 1 1 calc R . . C20 C 0.4439(4) 0.6513(3) 0.4425(3) 0.0304(9) Uani 1 1 d U . . C21 C 0.4281(4) 0.6566(3) 0.5359(3) 0.0407(11) Uani 1 1 d U . . H21A H 0.3681 0.6257 0.5836 0.049 Uiso 1 1 calc R . . C22 C 0.5022(5) 0.7081(4) 0.5588(3) 0.0459(12) Uani 1 1 d U . . H22A H 0.4898 0.7136 0.6216 0.055 Uiso 1 1 calc R . . C23 C 0.5931(4) 0.7508(3) 0.4888(3) 0.0387(11) Uani 1 1 d U . . H23A H 0.6446 0.7830 0.5050 0.046 Uiso 1 1 calc R . . C24 C 0.6106(4) 0.7469(3) 0.3924(3) 0.0289(9) Uani 1 1 d U . . C25 C 0.5298(4) 0.7009(3) 0.3674(3) 0.0257(9) Uani 1 1 d U . . C26 C 0.7163(4) 0.7898(3) 0.3253(3) 0.0310(9) Uani 1 1 d U . . H26A H 0.7495 0.8315 0.3462 0.037 Uiso 1 1 calc R . . C27 C 0.8738(4) 0.8222(3) 0.1800(3) 0.0342(10) Uani 1 1 d U . . H27A H 0.9363 0.8186 0.2162 0.041 Uiso 1 1 calc R . . H27B H 0.8383 0.8912 0.1577 0.041 Uiso 1 1 calc R . . C28 C 0.9430(4) 0.7698(3) 0.0957(3) 0.0364(10) Uani 1 1 d U . . H28A H 0.9949 0.8108 0.0460 0.044 Uiso 1 1 calc R . . H28B H 1.0016 0.7082 0.1151 0.044 Uiso 1 1 calc R . . C29 C 0.8362(4) 0.7784(3) -0.0254(3) 0.0327(10) Uani 1 1 d U . . H29A H 0.9026 0.8075 -0.0675 0.039 Uiso 1 1 calc R . . C30 C 0.7328(4) 0.7673(3) -0.0630(3) 0.0274(9) Uani 1 1 d U . . C31 C 0.7543(4) 0.7789(3) -0.1613(3) 0.0362(10) Uani 1 1 d U . . H31A H 0.8337 0.7928 -0.1998 0.043 Uiso 1 1 calc R . . C32 C 0.6625(4) 0.7706(3) -0.2030(3) 0.0375(11) Uani 1 1 d U . . H32A H 0.6806 0.7772 -0.2687 0.045 Uiso 1 1 calc R . . C33 C 0.5409(4) 0.7521(3) -0.1462(3) 0.0305(9) Uani 1 1 d U . . H33A H 0.4776 0.7463 -0.1737 0.037 Uiso 1 1 calc R . . C34 C 0.5165(4) 0.7426(3) -0.0492(3) 0.0252(9) Uani 1 1 d U . . C35 C 0.6118(4) 0.7485(3) -0.0048(3) 0.0228(8) Uani 1 1 d U . . C36 C 0.3051(4) 0.7061(3) -0.0216(3) 0.0381(11) Uani 1 1 d U . . H36A H 0.3465 0.6545 -0.0584 0.057 Uiso 1 1 calc R . . H36B H 0.2684 0.7646 -0.0611 0.057 Uiso 1 1 calc R . . H36C H 0.2361 0.6856 0.0303 0.057 Uiso 1 1 calc R . . C37 C -0.0861(4) 1.0088(3) 0.2737(3) 0.0312(9) Uani 1 1 d U . . C38 C 0.7897(4) 0.4641(3) 0.2124(3) 0.0320(10) Uani 1 1 d U . . Er1 Er 0.374093(16) 0.771681(12) 0.191119(12) 0.02098(6) Uani 1 1 d U . . N1 N -0.0210(3) 0.7380(3) 0.4563(2) 0.0426(10) Uani 1 1 d U . . N2 N 0.1049(4) 0.8522(3) 0.4961(2) 0.0454(10) Uani 1 1 d U . . N3 N -0.0239(4) 0.9418(3) 0.3133(3) 0.0406(9) Uani 1 1 d U . . N4 N 0.7670(3) 0.7751(2) 0.2404(2) 0.0280(8) Uani 1 1 d U . . N5 N 0.8417(3) 0.7509(2) 0.0610(2) 0.0298(8) Uani 1 1 d U . . N6 N 0.7700(3) 0.5493(2) 0.2027(3) 0.0363(9) Uani 1 1 d U . . N7 N 0.2167(3) 0.9129(3) 0.0756(2) 0.0329(8) Uani 1 1 d U . . O1 O 0.3554(2) 0.60223(18) 0.19039(18) 0.0271(6) Uani 1 1 d U . . O2 O 0.1946(2) 0.71725(19) 0.29765(18) 0.0294(6) Uani 1 1 d U . . O3 O 0.2790(3) 0.85763(19) 0.31041(18) 0.0289(6) Uani 1 1 d U . . O4 O 0.4806(3) 0.91279(18) 0.19430(19) 0.0300(6) Uani 1 1 d U . . O5 O 0.3798(3) 0.5990(2) 0.4128(2) 0.0369(7) Uani 1 1 d U . . O6 O 0.5304(2) 0.70247(17) 0.27757(17) 0.0231(6) Uani 1 1 d U . . O7 O 0.5774(2) 0.73835(18) 0.09055(17) 0.0237(6) Uani 1 1 d U . . O8 O 0.4013(2) 0.72648(19) 0.01491(18) 0.0278(6) Uani 1 1 d U . . O9 O 0.1767(3) 0.8392(2) 0.13311(19) 0.0322(7) Uani 1 1 d U . . O10 O 0.3316(3) 0.9181(2) 0.0748(2) 0.0334(7) Uani 1 1 d U . . O11 O 0.1497(3) 0.9723(3) 0.0268(3) 0.0582(10) Uani 1 1 d U . . S1 S -0.17904(16) 1.10218(9) 0.22317(11) 0.0637(4) Uani 1 1 d U . . S2 S 0.81821(13) 0.34484(8) 0.22364(9) 0.0462(3) Uani 1 1 d U . . Zn1 Zn 0.09837(4) 0.83006(3) 0.36864(3) 0.03128(12) Uani 1 1 d U . . Zn2 Zn 0.70624(4) 0.69200(3) 0.17565(3) 0.02395(11) Uani 1 1 d U . . O1WA O 1.0000 0.5000 0.0000 0.089(5) Uani 0.52 2 d SPU . . O1WB O 1.2000(15) 0.4890(8) 0.0216(7) 0.081(3) Uani 0.37 1 d PU . . O1WC O 1.0871(15) 0.4961(10) 0.0126(9) 0.079(4) Uani 0.37 1 d PU . . 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 C1 0.037(3) 0.032(2) 0.057(3) -0.016(2) -0.002(2) -0.002(2) C2 0.026(2) 0.030(2) 0.029(2) 0.0076(18) -0.0061(17) -0.0138(18) C3 0.044(3) 0.033(2) 0.045(3) 0.003(2) -0.013(2) -0.022(2) C4 0.048(3) 0.046(3) 0.066(3) 0.012(3) -0.019(3) -0.033(2) C5 0.033(3) 0.048(3) 0.057(3) 0.022(2) -0.010(2) -0.025(2) C6 0.022(2) 0.044(3) 0.038(3) 0.013(2) -0.0021(19) -0.0099(19) C7 0.022(2) 0.027(2) 0.030(2) 0.0092(17) -0.0067(17) -0.0076(17) C8 0.020(2) 0.052(3) 0.042(3) 0.019(2) 0.0036(19) -0.004(2) C9 0.034(3) 0.065(3) 0.034(3) 0.005(2) 0.011(2) 0.009(2) C10 0.056(3) 0.077(4) 0.022(2) -0.001(2) 0.006(2) 0.013(3) C11 0.056(3) 0.059(3) 0.025(2) -0.019(2) -0.014(2) 0.024(3) C12 0.045(3) 0.044(3) 0.033(2) -0.016(2) -0.021(2) 0.016(2) C13 0.068(4) 0.048(3) 0.046(3) -0.023(2) -0.035(3) 0.017(3) C14 0.080(4) 0.032(2) 0.071(4) -0.021(2) -0.055(3) 0.007(2) C15 0.053(3) 0.026(2) 0.057(3) -0.007(2) -0.034(2) -0.004(2) C16 0.045(3) 0.0181(19) 0.034(2) -0.0047(17) -0.022(2) 0.0003(18) C17 0.035(2) 0.025(2) 0.033(2) -0.0099(18) -0.0185(19) 0.0074(18) C18 0.034(2) 0.027(2) 0.042(2) -0.0007(19) -0.0093(19) -0.0150(18) C19 0.026(2) 0.048(3) 0.041(3) 0.011(2) -0.0017(19) -0.013(2) C20 0.025(2) 0.031(2) 0.027(2) -0.0004(18) -0.0011(17) -0.0038(17) C21 0.038(3) 0.048(3) 0.024(2) 0.002(2) -0.0012(19) -0.006(2) C22 0.050(3) 0.056(3) 0.025(2) -0.008(2) -0.009(2) 0.000(2) C23 0.041(3) 0.046(3) 0.030(2) -0.010(2) -0.013(2) -0.005(2) C24 0.028(2) 0.028(2) 0.029(2) -0.0066(17) -0.0077(17) -0.0027(17) C25 0.021(2) 0.025(2) 0.025(2) -0.0041(16) -0.0024(16) 0.0004(16) C26 0.031(2) 0.028(2) 0.039(3) -0.0085(19) -0.0153(19) -0.0063(18) C27 0.024(2) 0.038(2) 0.046(3) -0.007(2) -0.0075(19) -0.0151(18) C28 0.022(2) 0.044(2) 0.044(3) -0.011(2) -0.0034(19) -0.0111(19) C29 0.023(2) 0.032(2) 0.035(2) -0.0035(19) 0.0059(18) -0.0089(18) C30 0.024(2) 0.024(2) 0.030(2) -0.0059(17) 0.0019(17) -0.0073(16) C31 0.031(2) 0.039(2) 0.026(2) -0.0004(19) 0.0076(18) -0.0082(19) C32 0.042(3) 0.042(2) 0.017(2) -0.0044(18) 0.0024(19) -0.002(2) C33 0.034(2) 0.031(2) 0.025(2) -0.0069(17) -0.0083(18) -0.0024(18) C34 0.026(2) 0.0231(19) 0.023(2) -0.0063(16) -0.0017(16) -0.0028(16) C35 0.024(2) 0.0205(18) 0.0182(19) -0.0050(15) 0.0027(15) -0.0034(15) C36 0.027(2) 0.054(3) 0.038(2) -0.014(2) -0.0107(19) -0.008(2) C37 0.037(2) 0.030(2) 0.026(2) -0.0075(18) -0.0055(19) -0.0076(19) C38 0.028(2) 0.039(2) 0.026(2) -0.0060(19) -0.0041(17) -0.0049(19) Er1 0.01738(10) 0.02421(10) 0.02039(10) -0.00603(7) 0.00134(7) -0.00760(7) N1 0.025(2) 0.051(2) 0.0248(19) 0.0093(18) 0.0073(15) 0.0062(17) N2 0.040(2) 0.060(3) 0.0222(19) -0.0121(18) -0.0047(17) 0.0129(19) N3 0.041(2) 0.040(2) 0.036(2) -0.0090(18) -0.0135(18) 0.0057(18) N4 0.0233(18) 0.0297(18) 0.032(2) -0.0068(15) -0.0051(15) -0.0084(14) N5 0.0205(17) 0.0343(18) 0.033(2) -0.0051(16) -0.0008(14) -0.0101(14) N6 0.031(2) 0.0278(19) 0.047(2) -0.0073(17) -0.0073(17) -0.0034(16) N7 0.029(2) 0.039(2) 0.030(2) -0.0053(17) -0.0053(16) -0.0094(17) O1 0.0210(14) 0.0259(14) 0.0323(15) -0.0061(12) 0.0011(11) -0.0093(11) O2 0.0209(14) 0.0291(15) 0.0290(15) -0.0017(12) 0.0057(11) -0.0063(12) O3 0.0290(15) 0.0325(15) 0.0237(15) -0.0102(12) -0.0032(12) -0.0034(12) O4 0.0367(16) 0.0262(14) 0.0302(15) -0.0063(12) -0.0065(12) -0.0128(12) O5 0.0333(17) 0.0437(17) 0.0313(16) 0.0034(14) -0.0022(13) -0.0197(14) O6 0.0228(14) 0.0240(13) 0.0202(14) -0.0030(11) -0.0010(11) -0.0068(11) O7 0.0187(13) 0.0309(14) 0.0199(14) -0.0054(11) 0.0006(11) -0.0076(11) O8 0.0224(14) 0.0389(15) 0.0227(14) -0.0060(12) -0.0013(11) -0.0116(12) O9 0.0240(15) 0.0429(16) 0.0304(16) -0.0047(13) -0.0024(12) -0.0144(13) O10 0.0250(16) 0.0377(16) 0.0403(17) 0.0020(13) -0.0122(13) -0.0148(13) O11 0.043(2) 0.067(2) 0.060(2) 0.0163(19) -0.0283(17) -0.0112(18) S1 0.0863(11) 0.0355(7) 0.0701(10) 0.0010(6) -0.0465(8) 0.0053(7) S2 0.0599(8) 0.0273(6) 0.0457(7) -0.0019(5) -0.0097(6) -0.0079(5) Zn1 0.0235(3) 0.0379(3) 0.0205(2) -0.0022(2) -0.00015(19) 0.0039(2) Zn2 0.0190(2) 0.0258(2) 0.0257(2) -0.00521(19) -0.00116(18) -0.00698(18) O1WA 0.070(7) 0.078(7) 0.083(8) -0.008(6) 0.020(7) -0.008(7) O1WB 0.137(8) 0.057(6) 0.044(5) -0.007(5) -0.017(6) -0.022(6) O1WC 0.114(9) 0.075(7) 0.050(6) -0.005(5) -0.027(6) -0.024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.443(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.375(5) . ? C2 O1 1.395(4) . ? C2 C7 1.398(6) . ? C3 C4 1.403(6) . ? C3 H3A 0.9300 . ? C4 C5 1.368(7) . ? C4 H4A 0.9300 . ? C5 C6 1.403(6) . ? C5 H5A 0.9300 . ? C6 C7 1.418(5) . ? C6 C8 1.452(6) . ? C7 O2 1.317(4) . ? C8 N1 1.270(6) . ? C8 H8A 0.9300 . ? C9 N1 1.458(6) . ? C9 C10 1.527(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.478(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.274(6) . ? C11 C12 1.463(7) . ? C11 H11A 0.9300 . ? C12 C13 1.401(7) . ? C12 C17 1.413(6) . ? C13 C14 1.364(7) . ? C13 H13A 0.9300 . ? C14 C15 1.404(7) . ? C14 H14A 0.9300 . ? C15 C16 1.378(6) . ? C15 H15A 0.9300 . ? C16 O4 1.385(5) . ? C16 C17 1.400(6) . ? C17 O3 1.326(5) . ? C18 O4 1.437(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.415(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O5 1.372(5) . ? C20 C21 1.374(6) . ? C20 C25 1.416(5) . ? C21 C22 1.391(6) . ? C21 H21A 0.9300 . ? C22 C23 1.365(6) . ? C22 H22A 0.9300 . ? C23 C24 1.412(6) . ? C23 H23A 0.9300 . ? C24 C25 1.410(5) . ? C24 C26 1.456(5) . ? C25 O6 1.336(4) . ? C26 N4 1.271(5) . ? C26 H26A 0.9300 . ? C27 N4 1.465(5) . ? C27 C28 1.521(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N5 1.460(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N5 1.270(5) . ? C29 C30 1.456(6) . ? C29 H29A 0.9300 . ? C30 C31 1.396(6) . ? C30 C35 1.405(5) . ? C31 C32 1.367(6) . ? C31 H31A 0.9300 . ? C32 C33 1.403(6) . ? C32 H32A 0.9300 . ? C33 C34 1.376(5) . ? C33 H33A 0.9300 . ? C34 O8 1.375(4) . ? C34 C35 1.416(5) . ? C35 O7 1.346(4) . ? C36 O8 1.436(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N3 1.151(5) . ? C37 S1 1.609(4) . ? C38 N6 1.160(5) . ? C38 S2 1.626(4) . ? Er1 O3 2.249(2) . ? Er1 O7 2.279(2) . ? Er1 O6 2.296(3) . ? Er1 O2 2.318(2) . ? Er1 O10 2.407(3) . ? Er1 O9 2.414(3) . ? Er1 O1 2.498(2) . ? Er1 O4 2.613(2) . ? Er1 O8 2.780(3) . ? Er1 N7 2.848(4) . ? Er1 Zn2 3.4287(5) . ? Er1 Zn1 3.4297(5) . ? N1 Zn1 2.062(4) . ? N2 Zn1 2.033(4) . ? N3 Zn1 1.958(4) . ? N4 Zn2 2.044(3) . ? N5 Zn2 2.080(3) . ? N6 Zn2 1.951(3) . ? N7 O11 1.206(4) . ? N7 O10 1.269(4) . ? N7 O9 1.280(4) . ? O2 Zn1 2.022(3) . ? O3 Zn1 2.009(3) . ? O6 Zn2 2.061(2) . ? O7 Zn2 2.036(3) . ? O1WA O1WC 1.003(15) 2_765 ? O1WA O1WC 1.003(15) . ? O1WB O1WC 1.248(16) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.7(4) . . ? C3 C2 C7 122.5(4) . . ? O1 C2 C7 112.8(3) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C7 118.4(4) . . ? C5 C6 C8 118.9(4) . . ? C7 C6 C8 122.1(4) . . ? O2 C7 C2 116.5(3) . . ? O2 C7 C6 125.3(4) . . ? C2 C7 C6 118.2(4) . . ? N1 C8 C6 124.9(4) . . ? N1 C8 H8A 117.5 . . ? C6 C8 H8A 117.5 . . ? N1 C9 C10 108.1(4) . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C9 109.8(4) . . ? N2 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 125.6(4) . . ? N2 C11 H11A 117.2 . . ? C12 C11 H11A 117.2 . . ? C13 C12 C17 118.5(5) . . ? C13 C12 C11 117.7(4) . . ? C17 C12 C11 123.7(4) . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C16 C15 C14 117.7(5) . . ? C16 C15 H15A 121.1 . . ? C14 C15 H15A 121.1 . . ? C15 C16 O4 124.4(4) . . ? C15 C16 C17 122.5(4) . . ? O4 C16 C17 113.1(3) . . ? O3 C17 C16 117.1(4) . . ? O3 C17 C12 124.1(4) . . ? C16 C17 C12 118.6(4) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C21 124.4(4) . . ? O5 C20 C25 113.7(3) . . ? C21 C20 C25 121.9(4) . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 121.3(4) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C25 C24 C23 119.4(4) . . ? C25 C24 C26 124.5(4) . . ? C23 C24 C26 116.0(4) . . ? O6 C25 C24 123.4(3) . . ? O6 C25 C20 119.4(4) . . ? C24 C25 C20 117.2(4) . . ? N4 C26 C24 125.5(4) . . ? N4 C26 H26A 117.2 . . ? C24 C26 H26A 117.2 . . ? N4 C27 C28 109.2(3) . . ? N4 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N4 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? N5 C28 C27 107.8(3) . . ? N5 C28 H28A 110.2 . . ? C27 C28 H28A 110.2 . . ? N5 C28 H28B 110.2 . . ? C27 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? N5 C29 C30 124.3(4) . . ? N5 C29 H29A 117.8 . . ? C30 C29 H29A 117.8 . . ? C31 C30 C35 119.0(4) . . ? C31 C30 C29 118.1(4) . . ? C35 C30 C29 122.9(4) . . ? C32 C31 C30 122.2(4) . . ? C32 C31 H31A 118.9 . . ? C30 C31 H31A 118.9 . . ? C31 C32 C33 119.7(4) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? O8 C34 C33 125.5(4) . . ? O8 C34 C35 112.6(3) . . ? C33 C34 C35 121.9(4) . . ? O7 C35 C30 124.9(4) . . ? O7 C35 C34 117.0(3) . . ? C30 C35 C34 118.1(3) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 S1 177.1(4) . . ? N6 C38 S2 178.9(4) . . ? O3 Er1 O7 136.41(9) . . ? O3 Er1 O6 82.76(9) . . ? O7 Er1 O6 70.41(9) . . ? O3 Er1 O2 66.40(9) . . ? O7 Er1 O2 149.78(9) . . ? O6 Er1 O2 99.67(9) . . ? O3 Er1 O10 91.30(10) . . ? O7 Er1 O10 85.30(9) . . ? O6 Er1 O10 135.71(8) . . ? O2 Er1 O10 117.98(9) . . ? O3 Er1 O9 88.43(10) . . ? O7 Er1 O9 121.75(9) . . ? O6 Er1 O9 167.64(8) . . ? O2 Er1 O9 68.73(9) . . ? O10 Er1 O9 52.80(9) . . ? O3 Er1 O1 126.55(9) . . ? O7 Er1 O1 87.58(8) . . ? O6 Er1 O1 88.91(9) . . ? O2 Er1 O1 63.24(8) . . ? O10 Er1 O1 127.52(9) . . ? O9 Er1 O1 89.41(9) . . ? O3 Er1 O4 62.75(9) . . ? O7 Er1 O4 76.58(8) . . ? O6 Er1 O4 73.01(8) . . ? O2 Er1 O4 129.13(9) . . ? O10 Er1 O4 65.46(9) . . ? O9 Er1 O4 110.51(9) . . ? O1 Er1 O4 159.05(9) . . ? O3 Er1 O8 154.53(9) . . ? O7 Er1 O8 59.71(8) . . ? O6 Er1 O8 122.40(8) . . ? O2 Er1 O8 108.85(9) . . ? O10 Er1 O8 68.32(9) . . ? O9 Er1 O8 67.28(8) . . ? O1 Er1 O8 63.40(8) . . ? O4 Er1 O8 117.43(8) . . ? O3 Er1 N7 89.96(10) . . ? O7 Er1 N7 104.18(9) . . ? O6 Er1 N7 160.80(9) . . ? O2 Er1 N7 93.57(9) . . ? O10 Er1 N7 26.26(9) . . ? O9 Er1 N7 26.54(8) . . ? O1 Er1 N7 109.56(9) . . ? O4 Er1 N7 87.85(9) . . ? O8 Er1 N7 64.95(9) . . ? O3 Er1 Zn2 109.66(7) . . ? O7 Er1 Zn2 34.97(6) . . ? O6 Er1 Zn2 35.73(6) . . ? O2 Er1 Zn2 131.56(7) . . ? O10 Er1 Zn2 110.25(6) . . ? O9 Er1 Zn2 156.58(6) . . ? O1 Er1 Zn2 91.27(6) . . ? O4 Er1 Zn2 67.89(6) . . ? O8 Er1 Zn2 92.23(5) . . ? N7 Er1 Zn2 134.69(7) . . ? O3 Er1 Zn1 34.04(7) . . ? O7 Er1 Zn1 169.48(6) . . ? O6 Er1 Zn1 100.72(6) . . ? O2 Er1 Zn1 34.86(7) . . ? O10 Er1 Zn1 98.05(7) . . ? O9 Er1 Zn1 67.42(6) . . ? O1 Er1 Zn1 98.09(6) . . ? O4 Er1 Zn1 95.66(6) . . ? O8 Er1 Zn1 130.79(5) . . ? N7 Er1 Zn1 82.34(7) . . ? Zn2 Er1 Zn1 135.458(12) . . ? C8 N1 C9 123.4(4) . . ? C8 N1 Zn1 128.3(3) . . ? C9 N1 Zn1 108.2(3) . . ? C11 N2 C10 121.1(4) . . ? C11 N2 Zn1 125.3(3) . . ? C10 N2 Zn1 113.4(4) . . ? C37 N3 Zn1 173.7(4) . . ? C26 N4 C27 120.2(3) . . ? C26 N4 Zn2 124.8(3) . . ? C27 N4 Zn2 114.9(3) . . ? C29 N5 C28 121.9(3) . . ? C29 N5 Zn2 128.6(3) . . ? C28 N5 Zn2 109.1(3) . . ? C38 N6 Zn2 167.8(4) . . ? O11 N7 O10 123.3(3) . . ? O11 N7 O9 122.2(3) . . ? O10 N7 O9 114.5(3) . . ? O11 N7 Er1 179.6(3) . . ? O10 N7 Er1 57.08(19) . . ? O9 N7 Er1 57.45(18) . . ? C2 O1 C1 116.1(3) . . ? C2 O1 Er1 118.6(2) . . ? C1 O1 Er1 125.1(2) . . ? C7 O2 Zn1 128.0(2) . . ? C7 O2 Er1 126.9(2) . . ? Zn1 O2 Er1 104.22(11) . . ? C17 O3 Zn1 124.5(2) . . ? C17 O3 Er1 128.3(2) . . ? Zn1 O3 Er1 107.16(11) . . ? C16 O4 C18 117.3(3) . . ? C16 O4 Er1 115.0(2) . . ? C18 O4 Er1 126.3(2) . . ? C20 O5 C19 116.5(3) . . ? C25 O6 Zn2 119.4(2) . . ? C25 O6 Er1 132.5(2) . . ? Zn2 O6 Er1 103.67(10) . . ? C35 O7 Zn2 125.0(2) . . ? C35 O7 Er1 129.9(2) . . ? Zn2 O7 Er1 105.13(10) . . ? C34 O8 C36 116.9(3) . . ? C34 O8 Er1 113.0(2) . . ? C36 O8 Er1 129.2(2) . . ? N7 O9 Er1 96.0(2) . . ? N7 O10 Er1 96.7(2) . . ? N3 Zn1 O3 106.06(14) . . ? N3 Zn1 O2 119.82(13) . . ? O3 Zn1 O2 76.70(10) . . ? N3 Zn1 N2 109.52(15) . . ? O3 Zn1 N2 90.19(14) . . ? O2 Zn1 N2 130.66(13) . . ? N3 Zn1 N1 104.03(15) . . ? O3 Zn1 N1 149.86(13) . . ? O2 Zn1 N1 87.03(13) . . ? N2 Zn1 N1 81.32(17) . . ? N3 Zn1 Er1 107.76(11) . . ? O3 Zn1 Er1 38.80(7) . . ? O2 Zn1 Er1 40.93(7) . . ? N2 Zn1 Er1 123.43(11) . . ? N1 Zn1 Er1 127.57(11) . . ? N6 Zn2 O7 114.44(13) . . ? N6 Zn2 N4 117.29(14) . . ? O7 Zn2 N4 128.17(12) . . ? N6 Zn2 O6 98.07(12) . . ? O7 Zn2 O6 80.16(10) . . ? N4 Zn2 O6 89.77(11) . . ? N6 Zn2 N5 108.85(14) . . ? O7 Zn2 N5 86.80(12) . . ? N4 Zn2 N5 79.84(13) . . ? O6 Zn2 N5 153.01(12) . . ? N6 Zn2 Er1 115.29(10) . . ? O7 Zn2 Er1 39.91(7) . . ? N4 Zn2 Er1 110.34(9) . . ? O6 Zn2 Er1 40.60(7) . . ? N5 Zn2 Er1 120.75(10) . . ? O1WC O1WA O1WC 180.0(19) 2_765 . ? O1WA O1WC O1WB 175.1(15) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.682 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.089 # Attachment '3d.cif' data_wy1846 _database_code_depnum_ccdc_archive 'CCDC 729276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 N7 O11 S2 Tb Zn2, C2 H3 N' _chemical_formula_sum 'C40 H39 N8 O11 S2 Tb Zn2' _chemical_formula_weight 1161.57 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' S S 0.1246 0.1234 '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' _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 12.2288(5) _cell_length_b 12.4841(5) _cell_length_c 16.4978(7) _cell_angle_alpha 88.3160(10) _cell_angle_beta 69.2430(9) _cell_angle_gamma 70.7320(10) _cell_volume 2212.28(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10815 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 2.819 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5057 _exptl_absorpt_correction_T_max 0.6025 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _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 'Smart CCD' _diffrn_measurement_method '\w and\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10815 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7565 _reflns_number_gt 6906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0316P)^2^+1.5803P] 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 7565 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.040 _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 C1 C 1.0608(4) 0.2255(3) 0.3586(2) 0.0539(9) Uani 1 1 d U . . H1A H 1.1377 0.2199 0.3646 0.081 Uiso 1 1 calc R . . H1B H 0.9999 0.2263 0.4148 0.081 Uiso 1 1 calc R . . H1C H 1.0317 0.2946 0.3336 0.081 Uiso 1 1 calc R . . C2 C 1.2003(3) 0.0738(3) 0.2453(2) 0.0429(7) Uani 1 1 d U . . C3 C 1.3007(4) 0.1070(4) 0.2323(3) 0.0634(10) Uani 1 1 d U . . H3A H 1.2919 0.1710 0.2648 0.076 Uiso 1 1 calc R . . C4 C 1.4158(4) 0.0452(4) 0.1706(3) 0.0734(12) Uani 1 1 d U . . H4A H 1.4839 0.0681 0.1616 0.088 Uiso 1 1 calc R . . C5 C 1.4290(3) -0.0487(4) 0.1233(3) 0.0631(10) Uani 1 1 d U . . H5A H 1.5062 -0.0888 0.0815 0.076 Uiso 1 1 calc R . . C6 C 1.3279(3) -0.0864(3) 0.1364(2) 0.0456(7) Uani 1 1 d U . . C7 C 1.2118(3) -0.0250(3) 0.19921(19) 0.0373(6) Uani 1 1 d U . . C8 C 1.3525(3) -0.1870(3) 0.0814(2) 0.0480(8) Uani 1 1 d U . . H8A H 1.4292 -0.2144 0.0359 0.058 Uiso 1 1 calc R . . C9 C 1.3056(3) -0.3392(3) 0.0319(2) 0.0524(8) Uani 1 1 d U . . H9A H 1.3262 -0.4085 0.0600 0.063 Uiso 1 1 calc R . . H9B H 1.3765 -0.3440 -0.0205 0.063 Uiso 1 1 calc R . . C10 C 1.1923(3) -0.3265(3) 0.0088(2) 0.0522(8) Uani 1 1 d U . . H10A H 1.1903 -0.2764 -0.0371 0.063 Uiso 1 1 calc R . . H10B H 1.1971 -0.4003 -0.0122 0.063 Uiso 1 1 calc R . . C11 C 0.9778(3) -0.2936(3) 0.0945(2) 0.0457(8) Uani 1 1 d U . . H11A H 0.9793 -0.3429 0.0526 0.055 Uiso 1 1 calc R . . C12 C 0.8596(3) -0.2385(3) 0.1651(2) 0.0430(7) Uani 1 1 d U . . C13 C 0.8378(3) -0.1438(3) 0.2204(2) 0.0402(7) Uani 1 1 d U . . C14 C 0.7169(3) -0.0906(3) 0.2811(2) 0.0476(8) Uani 1 1 d U . . C15 C 0.6216(3) -0.1318(3) 0.2894(3) 0.0592(9) Uani 1 1 d U . . H15A H 0.5424 -0.0965 0.3309 0.071 Uiso 1 1 calc R . . C16 C 0.6454(4) -0.2262(4) 0.2353(3) 0.0630(10) Uani 1 1 d U . . H16A H 0.5819 -0.2543 0.2407 0.076 Uiso 1 1 calc R . . C17 C 0.7604(4) -0.2779(3) 0.1748(2) 0.0536(9) Uani 1 1 d U . . H17A H 0.7743 -0.3408 0.1388 0.064 Uiso 1 1 calc R . . C18 C 0.5867(4) 0.0646(4) 0.3915(3) 0.0880(15) Uani 1 1 d U . . H18A H 0.5649 0.0179 0.4375 0.132 Uiso 1 1 calc R . . H18B H 0.5260 0.0840 0.3643 0.132 Uiso 1 1 calc R . . H18C H 0.5887 0.1331 0.4150 0.132 Uiso 1 1 calc R . . C19 C 0.9153(5) -0.0910(3) 0.4262(3) 0.0885(16) Uani 1 1 d U . . H19A H 0.9620 -0.0972 0.4633 0.133 Uiso 1 1 calc R . . H19B H 0.9676 -0.1383 0.3726 0.133 Uiso 1 1 calc R . . H19C H 0.8454 -0.1152 0.4549 0.133 Uiso 1 1 calc R . . C20 C 0.7977(3) 0.1046(3) 0.48017(19) 0.0428(7) Uani 1 1 d U . . C21 C 0.7681(3) 0.0805(3) 0.5653(2) 0.0552(9) Uani 1 1 d U . . H21A H 0.7950 0.0057 0.5786 0.066 Uiso 1 1 calc R . . C22 C 0.6978(4) 0.1688(4) 0.6315(2) 0.0629(10) Uani 1 1 d U . . H22A H 0.6765 0.1530 0.6894 0.075 Uiso 1 1 calc R . . C23 C 0.6600(3) 0.2779(3) 0.6122(2) 0.0518(8) Uani 1 1 d U . . H23A H 0.6154 0.3363 0.6573 0.062 Uiso 1 1 calc R . . C24 C 0.6865(3) 0.3047(3) 0.52589(19) 0.0403(7) Uani 1 1 d U . . C25 C 0.7542(3) 0.2161(3) 0.45786(17) 0.0357(6) Uani 1 1 d U . . C26 C 0.6548(3) 0.4251(3) 0.5119(2) 0.0457(8) Uani 1 1 d U . . H26A H 0.6195 0.4774 0.5609 0.055 Uiso 1 1 calc R . . C27 C 0.6598(3) 0.5847(3) 0.4292(2) 0.0526(8) Uani 1 1 d U . . H27A H 0.6268 0.6269 0.4860 0.063 Uiso 1 1 calc R . . H27B H 0.6043 0.6189 0.3984 0.063 Uiso 1 1 calc R . . C28 C 0.7906(3) 0.5863(3) 0.3776(2) 0.0538(9) Uani 1 1 d U . . H28A H 0.7854 0.6595 0.3546 0.065 Uiso 1 1 calc R . . H28B H 0.8377 0.5753 0.4155 0.065 Uiso 1 1 calc R . . C29 C 0.9556(3) 0.4902(3) 0.2472(2) 0.0450(8) Uani 1 1 d U . . H29A H 0.9844 0.5500 0.2491 0.054 Uiso 1 1 calc R . . C30 C 1.0321(3) 0.3989(3) 0.1769(2) 0.0415(7) Uani 1 1 d U . . C31 C 1.0074(3) 0.2975(2) 0.16924(18) 0.0340(6) Uani 1 1 d U . . C32 C 1.0937(3) 0.2136(3) 0.10105(18) 0.0392(7) Uani 1 1 d U . . C33 C 1.1988(3) 0.2285(3) 0.0420(2) 0.0518(8) Uani 1 1 d U . . H33A H 1.2540 0.1718 -0.0029 0.062 Uiso 1 1 calc R . . C34 C 1.2218(4) 0.3282(4) 0.0499(3) 0.0621(10) Uani 1 1 d U . . H34A H 1.2924 0.3390 0.0100 0.075 Uiso 1 1 calc R . . C35 C 1.1411(3) 0.4108(3) 0.1160(2) 0.0563(9) Uani 1 1 d U . . H35A H 1.1585 0.4769 0.1210 0.068 Uiso 1 1 calc R . . C36 C 1.1220(3) 0.0381(3) 0.0269(2) 0.0522(8) Uani 1 1 d U . . H36A H 1.1044 0.0760 -0.0209 0.078 Uiso 1 1 calc R . . H36B H 1.0914 -0.0246 0.0367 0.078 Uiso 1 1 calc R . . H36C H 1.2103 0.0102 0.0134 0.078 Uiso 1 1 calc R . . C37 C 1.1010(3) -0.3570(3) 0.3358(2) 0.0477(8) Uani 1 1 d U . . C38 C 0.5965(3) 0.5015(3) 0.2088(2) 0.0431(7) Uani 1 1 d U . . C39 C 0.3433(7) 0.3137(7) 0.3481(6) 0.114(2) Uani 1 1 d U . . C40 C 0.3676(7) 0.3731(6) 0.2729(6) 0.147(3) Uani 1 1 d U . . H40A H 0.4514 0.3731 0.2539 0.220 Uiso 1 1 calc R . . H40B H 0.3108 0.4503 0.2865 0.220 Uiso 1 1 calc R . . H40C H 0.3569 0.3363 0.2274 0.220 Uiso 1 1 calc R . . N1 N 1.2772(2) -0.2401(2) 0.09088(16) 0.0431(6) Uani 1 1 d U . . N2 N 1.0789(3) -0.2789(2) 0.08634(16) 0.0424(6) Uani 1 1 d U . . N3 N 1.1120(3) -0.3107(2) 0.27347(18) 0.0511(7) Uani 1 1 d U . . N4 N 0.6712(2) 0.4648(2) 0.43835(17) 0.0441(6) Uani 1 1 d U . . N5 N 0.8534(3) 0.4951(2) 0.30586(17) 0.0427(6) Uani 1 1 d U . . N6 N 0.6434(3) 0.4529(3) 0.2549(2) 0.0502(7) Uani 1 1 d U . . N7 N 0.7182(3) 0.1592(2) 0.17295(18) 0.0474(7) Uani 1 1 d U . . N8 N 0.3160(7) 0.2639(7) 0.4092(5) 0.148(3) Uani 1 1 d U . . O1 O 1.0804(2) 0.12917(19) 0.30273(14) 0.0466(5) Uani 1 1 d U . . O2 O 1.10798(18) -0.04985(17) 0.21730(13) 0.0367(4) Uani 1 1 d U . . O3 O 0.92371(18) -0.09887(17) 0.21829(14) 0.0397(5) Uani 1 1 d U . . O4 O 0.7064(2) 0.0034(2) 0.32833(18) 0.0626(7) Uani 1 1 d U . . O5 O 0.8718(2) 0.02566(18) 0.40818(13) 0.0502(6) Uani 1 1 d U . . O6 O 0.78321(19) 0.22960(17) 0.37308(12) 0.0375(5) Uani 1 1 d U . . O7 O 0.91080(18) 0.27288(16) 0.22296(12) 0.0363(4) Uani 1 1 d U . . O8 O 1.0624(2) 0.11671(18) 0.10346(13) 0.0441(5) Uani 1 1 d U . . O9 O 0.8286(2) 0.0952(2) 0.13685(15) 0.0531(6) Uani 1 1 d U . . O10 O 0.6905(2) 0.2017(2) 0.24877(16) 0.0555(7) Uani 1 1 d U . . O11 O 0.6423(3) 0.1782(3) 0.13705(18) 0.0723(8) Uani 1 1 d U . . S1 S 1.08020(12) -0.42074(12) 0.42347(8) 0.0824(4) Uani 1 1 d U . . S2 S 0.52769(10) 0.57155(9) 0.14628(7) 0.0657(3) Uani 1 1 d U . . Tb1 Tb 0.905886(13) 0.088773(11) 0.256188(8) 0.03306(6) Uani 1 1 d U . . Zn1 Zn 1.10475(3) -0.20298(3) 0.18508(2) 0.03600(9) Uani 1 1 d U . . Zn2 Zn 0.75869(3) 0.38112(3) 0.31534(2) 0.03563(9) Uani 1 1 d U . . 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 C1 0.070(2) 0.0416(19) 0.060(2) -0.0005(15) -0.0355(18) -0.0180(17) C2 0.0481(18) 0.0421(18) 0.0477(17) 0.0138(14) -0.0255(15) -0.0190(15) C3 0.066(2) 0.074(3) 0.071(2) 0.006(2) -0.033(2) -0.041(2) C4 0.055(2) 0.088(3) 0.093(3) 0.008(2) -0.029(2) -0.043(2) C5 0.0397(19) 0.080(3) 0.071(2) 0.007(2) -0.0161(17) -0.0260(19) C6 0.0380(17) 0.053(2) 0.0486(18) 0.0122(15) -0.0184(14) -0.0162(15) C7 0.0417(16) 0.0364(16) 0.0421(16) 0.0145(13) -0.0225(13) -0.0170(13) C8 0.0345(16) 0.050(2) 0.0490(18) 0.0082(15) -0.0107(14) -0.0066(15) C9 0.050(2) 0.0425(19) 0.0488(19) -0.0024(15) -0.0091(15) -0.0054(15) C10 0.062(2) 0.051(2) 0.0362(17) -0.0021(14) -0.0118(15) -0.0153(17) C11 0.061(2) 0.0398(18) 0.0479(18) 0.0096(14) -0.0295(16) -0.0209(16) C12 0.0526(19) 0.0380(17) 0.0502(18) 0.0158(14) -0.0279(15) -0.0211(15) C13 0.0405(16) 0.0365(17) 0.0496(17) 0.0155(13) -0.0209(14) -0.0168(13) C14 0.0452(18) 0.0389(18) 0.061(2) 0.0112(15) -0.0195(15) -0.0178(15) C15 0.0429(19) 0.061(2) 0.074(2) 0.0143(19) -0.0170(17) -0.0232(17) C16 0.059(2) 0.069(3) 0.081(3) 0.019(2) -0.032(2) -0.040(2) C17 0.063(2) 0.050(2) 0.067(2) 0.0158(17) -0.0363(19) -0.0311(18) C18 0.060(3) 0.083(3) 0.094(3) -0.019(3) 0.008(2) -0.029(2) C19 0.129(4) 0.043(2) 0.051(2) 0.0083(18) -0.017(2) 0.006(2) C20 0.0446(18) 0.0441(18) 0.0318(15) 0.0047(13) -0.0105(13) -0.0090(14) C21 0.066(2) 0.050(2) 0.0361(17) 0.0139(15) -0.0154(16) -0.0072(17) C22 0.064(2) 0.078(3) 0.0293(16) 0.0098(16) -0.0117(15) -0.009(2) C23 0.051(2) 0.062(2) 0.0301(15) -0.0037(15) -0.0092(14) -0.0092(17) C24 0.0366(16) 0.0450(18) 0.0339(15) -0.0007(13) -0.0109(12) -0.0090(13) C25 0.0346(15) 0.0424(17) 0.0280(14) 0.0040(12) -0.0105(11) -0.0117(13) C26 0.0414(17) 0.0468(19) 0.0397(17) -0.0096(14) -0.0134(14) -0.0039(14) C27 0.061(2) 0.0348(18) 0.055(2) -0.0064(14) -0.0240(17) -0.0039(15) C28 0.064(2) 0.0388(19) 0.062(2) -0.0048(15) -0.0282(18) -0.0151(16) C29 0.057(2) 0.0317(17) 0.058(2) 0.0125(14) -0.0298(17) -0.0207(15) C30 0.0455(17) 0.0371(17) 0.0463(17) 0.0134(13) -0.0202(14) -0.0168(14) C31 0.0379(15) 0.0310(15) 0.0330(14) 0.0117(11) -0.0153(12) -0.0100(12) C32 0.0401(16) 0.0436(18) 0.0332(15) 0.0126(13) -0.0146(13) -0.0128(14) C33 0.0469(19) 0.056(2) 0.0424(18) 0.0119(15) -0.0098(15) -0.0124(16) C34 0.051(2) 0.073(3) 0.061(2) 0.0241(19) -0.0111(17) -0.031(2) C35 0.058(2) 0.057(2) 0.062(2) 0.0210(18) -0.0199(18) -0.0326(19) C36 0.066(2) 0.0427(19) 0.0356(16) -0.0014(14) -0.0150(15) -0.0060(16) C37 0.0480(19) 0.0449(19) 0.054(2) 0.0106(16) -0.0223(15) -0.0166(15) C38 0.0418(17) 0.0373(17) 0.0479(18) -0.0044(14) -0.0185(14) -0.0076(14) C39 0.098(4) 0.095(4) 0.145(6) -0.050(4) -0.046(4) -0.021(3) C40 0.115(5) 0.116(5) 0.183(6) -0.037(5) -0.002(4) -0.058(4) N1 0.0408(14) 0.0372(14) 0.0426(14) 0.0047(11) -0.0103(11) -0.0078(12) N2 0.0509(16) 0.0383(15) 0.0374(13) 0.0039(11) -0.0161(12) -0.0144(12) N3 0.0633(19) 0.0399(16) 0.0512(16) 0.0163(13) -0.0231(14) -0.0176(14) N4 0.0465(15) 0.0351(14) 0.0436(15) -0.0040(11) -0.0160(12) -0.0050(12) N5 0.0482(16) 0.0320(14) 0.0511(15) 0.0027(11) -0.0231(13) -0.0122(12) N6 0.0533(18) 0.0426(17) 0.0624(19) 0.0089(14) -0.0377(16) -0.0120(14) N7 0.0587(18) 0.0492(17) 0.0445(15) 0.0125(13) -0.0221(14) -0.0286(15) N8 0.140(5) 0.148(5) 0.157(5) -0.044(4) -0.086(4) -0.012(4) O1 0.0516(13) 0.0400(12) 0.0561(13) 0.0012(10) -0.0264(11) -0.0179(10) O2 0.0331(10) 0.0347(11) 0.0428(11) 0.0044(9) -0.0134(9) -0.0127(9) O3 0.0352(11) 0.0308(11) 0.0546(12) 0.0040(9) -0.0158(9) -0.0138(9) O4 0.0437(14) 0.0506(15) 0.0799(17) -0.0103(13) -0.0064(12) -0.0155(11) O5 0.0676(15) 0.0343(12) 0.0319(11) 0.0073(9) -0.0115(10) -0.0038(11) O6 0.0483(12) 0.0317(11) 0.0272(10) 0.0040(8) -0.0116(9) -0.0095(9) O7 0.0385(11) 0.0321(11) 0.0336(10) 0.0037(8) -0.0073(8) -0.0125(9) O8 0.0523(13) 0.0365(12) 0.0334(11) 0.0007(9) -0.0076(9) -0.0110(10) O9 0.0545(16) 0.0556(16) 0.0423(13) -0.0024(11) -0.0225(12) -0.0080(13) O10 0.0540(15) 0.0678(18) 0.0440(14) -0.0039(12) -0.0139(12) -0.0270(13) O11 0.0700(18) 0.096(2) 0.0674(17) 0.0188(15) -0.0395(15) -0.0343(16) S1 0.0840(8) 0.1059(10) 0.0717(7) 0.0530(7) -0.0378(6) -0.0441(7) S2 0.0738(7) 0.0650(6) 0.0601(6) 0.0068(5) -0.0407(5) -0.0085(5) Tb1 0.04077(9) 0.02684(8) 0.02767(8) 0.00259(5) -0.00978(6) -0.00962(6) Zn1 0.03982(19) 0.02955(18) 0.03657(18) 0.00554(14) -0.01226(14) -0.01131(15) Zn2 0.03867(19) 0.02984(18) 0.03673(18) 0.00184(14) -0.01587(14) -0.00725(14) _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 C1 O1 1.439(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.368(5) . ? C2 O1 1.382(4) . ? C2 C7 1.409(4) . ? C3 C4 1.387(6) . ? C3 H3A 0.9300 . ? C4 C5 1.360(6) . ? C4 H4A 0.9300 . ? C5 C6 1.409(5) . ? C5 H5A 0.9300 . ? C6 C7 1.401(4) . ? C6 C8 1.454(5) . ? C7 O2 1.335(3) . ? C8 N1 1.267(4) . ? C8 H8A 0.9300 . ? C9 N1 1.464(4) . ? C9 C10 1.523(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.469(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.269(4) . ? C11 C12 1.454(5) . ? C11 H11A 0.9300 . ? C12 C13 1.407(4) . ? C12 C17 1.411(4) . ? C13 O3 1.335(3) . ? C13 C14 1.404(5) . ? C14 O4 1.372(4) . ? C14 C15 1.386(5) . ? C15 C16 1.386(5) . ? C15 H15A 0.9300 . ? C16 C17 1.355(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 O4 1.428(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.438(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.372(4) . ? C20 O5 1.386(4) . ? C20 C25 1.405(4) . ? C21 C22 1.388(5) . ? C21 H21A 0.9300 . ? C22 C23 1.354(5) . ? C22 H22A 0.9300 . ? C23 C24 1.400(4) . ? C23 H23A 0.9300 . ? C24 C25 1.406(4) . ? C24 C26 1.457(5) . ? C25 O6 1.336(3) . ? C26 N4 1.271(4) . ? C26 H26A 0.9300 . ? C27 N4 1.465(4) . ? C27 C28 1.529(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N5 1.464(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N5 1.265(4) . ? C29 C30 1.457(5) . ? C29 H29A 0.9300 . ? C30 C35 1.407(5) . ? C30 C31 1.414(4) . ? C31 O7 1.326(3) . ? C31 C32 1.405(4) . ? C32 C33 1.376(4) . ? C32 O8 1.380(4) . ? C33 C34 1.383(5) . ? C33 H33A 0.9300 . ? C34 C35 1.363(5) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 O8 1.427(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N3 1.152(4) . ? C37 S1 1.611(4) . ? C38 N6 1.152(4) . ? C38 S2 1.616(3) . ? C39 N8 1.172(10) . ? C39 C40 1.418(11) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N1 Zn1 2.038(3) . ? N2 Zn1 2.075(3) . ? N3 Zn1 1.960(3) . ? N4 Zn2 2.050(3) . ? N5 Zn2 2.082(3) . ? N6 Zn2 1.974(3) . ? N7 O11 1.227(4) . ? N7 O9 1.249(4) . ? N7 O10 1.257(3) . ? N7 Tb1 2.959(3) . ? O1 Tb1 2.701(2) . ? O2 Zn1 2.0158(19) . ? O2 Tb1 2.373(2) . ? O3 Zn1 2.043(2) . ? O3 Tb1 2.3619(19) . ? O4 Tb1 2.844(2) . ? O5 Tb1 2.538(2) . ? O6 Zn2 2.0731(19) . ? O6 Tb1 2.3384(19) . ? O7 Zn2 2.0153(19) . ? O7 Tb1 2.3623(19) . ? O8 Tb1 2.665(2) . ? O9 Tb1 2.457(2) . ? O10 Tb1 2.590(3) . ? Tb1 Zn2 3.4844(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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 125.8(3) . . ? C3 C2 C7 121.2(3) . . ? O1 C2 C7 112.9(3) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C7 C6 C5 118.9(3) . . ? C7 C6 C8 124.6(3) . . ? C5 C6 C8 116.5(3) . . ? O2 C7 C6 125.2(3) . . ? O2 C7 C2 116.2(3) . . ? C6 C7 C2 118.5(3) . . ? N1 C8 C6 124.9(3) . . ? N1 C8 H8A 117.6 . . ? C6 C8 H8A 117.6 . . ? N1 C9 C10 108.8(3) . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C9 109.4(3) . . ? N2 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N2 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 124.3(3) . . ? N2 C11 H11A 117.8 . . ? C12 C11 H11A 117.8 . . ? C13 C12 C17 118.8(3) . . ? C13 C12 C11 123.1(3) . . ? C17 C12 C11 118.0(3) . . ? O3 C13 C14 117.0(3) . . ? O3 C13 C12 124.7(3) . . ? C14 C13 C12 118.4(3) . . ? O4 C14 C15 125.8(3) . . ? O4 C14 C13 112.8(3) . . ? C15 C14 C13 121.5(3) . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C12 121.5(3) . . ? C16 C17 H17A 119.3 . . ? C12 C17 H17A 119.3 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O5 125.3(3) . . ? C21 C20 C25 121.7(3) . . ? O5 C20 C25 113.0(2) . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 121.5(3) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 C26 117.1(3) . . ? C25 C24 C26 123.4(3) . . ? O6 C25 C20 117.0(3) . . ? O6 C25 C24 125.2(3) . . ? C20 C25 C24 117.8(3) . . ? N4 C26 C24 125.5(3) . . ? N4 C26 H26A 117.2 . . ? C24 C26 H26A 117.2 . . ? N4 C27 C28 106.7(3) . . ? N4 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? N4 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? N5 C28 C27 109.3(3) . . ? N5 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? N5 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? N5 C29 C30 125.5(3) . . ? N5 C29 H29A 117.2 . . ? C30 C29 H29A 117.2 . . ? C35 C30 C31 118.5(3) . . ? C35 C30 C29 117.1(3) . . ? C31 C30 C29 124.3(3) . . ? O7 C31 C32 116.6(3) . . ? O7 C31 C30 125.4(3) . . ? C32 C31 C30 118.0(3) . . ? C33 C32 O8 125.6(3) . . ? C33 C32 C31 122.0(3) . . ? O8 C32 C31 112.3(2) . . ? C32 C33 C34 119.5(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C30 121.9(3) . . ? C34 C35 H35A 119.1 . . ? C30 C35 H35A 119.1 . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 S1 177.9(3) . . ? N6 C38 S2 178.5(3) . . ? N8 C39 C40 175.1(8) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C8 N1 C9 122.5(3) . . ? C8 N1 Zn1 126.8(2) . . ? C9 N1 Zn1 110.7(2) . . ? C11 N2 C10 122.1(3) . . ? C11 N2 Zn1 123.5(2) . . ? C10 N2 Zn1 114.1(2) . . ? C37 N3 Zn1 167.6(3) . . ? C26 N4 C27 121.3(3) . . ? C26 N4 Zn2 129.8(2) . . ? C27 N4 Zn2 106.8(2) . . ? C29 N5 C28 120.3(3) . . ? C29 N5 Zn2 126.6(2) . . ? C28 N5 Zn2 113.0(2) . . ? C38 N6 Zn2 165.7(3) . . ? O11 N7 O9 122.2(3) . . ? O11 N7 O10 122.5(3) . . ? O9 N7 O10 115.3(3) . . ? O11 N7 Tb1 174.3(2) . . ? O9 N7 Tb1 54.63(16) . . ? O10 N7 Tb1 60.84(17) . . ? C2 O1 C1 117.3(3) . . ? C2 O1 Tb1 113.05(17) . . ? C1 O1 Tb1 126.0(2) . . ? C7 O2 Zn1 124.17(18) . . ? C7 O2 Tb1 124.18(18) . . ? Zn1 O2 Tb1 109.82(8) . . ? C13 O3 Zn1 119.33(18) . . ? C13 O3 Tb1 131.26(19) . . ? Zn1 O3 Tb1 109.29(8) . . ? C14 O4 C18 117.3(3) . . ? C14 O4 Tb1 114.52(19) . . ? C18 O4 Tb1 125.7(2) . . ? C20 O5 C19 115.9(3) . . ? C20 O5 Tb1 119.71(18) . . ? C19 O5 Tb1 124.2(2) . . ? C25 O6 Zn2 127.75(18) . . ? C25 O6 Tb1 127.18(18) . . ? Zn2 O6 Tb1 104.18(7) . . ? C31 O7 Zn2 126.62(17) . . ? C31 O7 Tb1 126.27(17) . . ? Zn2 O7 Tb1 105.22(8) . . ? C32 O8 C36 117.7(2) . . ? C32 O8 Tb1 115.86(16) . . ? C36 O8 Tb1 126.30(19) . . ? N7 O9 Tb1 100.88(18) . . ? N7 O10 Tb1 94.09(19) . . ? O6 Tb1 O3 137.14(7) . . ? O6 Tb1 O7 66.25(6) . . ? O3 Tb1 O7 152.96(7) . . ? O6 Tb1 O2 133.18(7) . . ? O3 Tb1 O2 64.22(7) . . ? O7 Tb1 O2 112.51(7) . . ? O6 Tb1 O9 116.04(8) . . ? O3 Tb1 O9 72.30(8) . . ? O7 Tb1 O9 85.07(8) . . ? O2 Tb1 O9 110.24(8) . . ? O6 Tb1 O5 63.04(7) . . ? O3 Tb1 O5 84.44(7) . . ? O7 Tb1 O5 122.55(7) . . ? O2 Tb1 O5 85.25(7) . . ? O9 Tb1 O5 141.34(9) . . ? O6 Tb1 O10 67.62(7) . . ? O3 Tb1 O10 100.41(7) . . ? O7 Tb1 O10 74.29(8) . . ? O2 Tb1 O10 159.17(7) . . ? O9 Tb1 O10 49.51(8) . . ? O5 Tb1 O10 108.13(8) . . ? O6 Tb1 O8 125.76(6) . . ? O3 Tb1 O8 96.66(7) . . ? O7 Tb1 O8 59.93(6) . . ? O2 Tb1 O8 67.57(7) . . ? O9 Tb1 O8 66.57(8) . . ? O5 Tb1 O8 148.67(8) . . ? O10 Tb1 O8 102.47(7) . . ? O6 Tb1 O1 78.37(7) . . ? O3 Tb1 O1 121.00(7) . . ? O7 Tb1 O1 70.40(7) . . ? O2 Tb1 O1 59.63(7) . . ? O9 Tb1 O1 143.94(8) . . ? O5 Tb1 O1 74.62(8) . . ? O10 Tb1 O1 138.39(7) . . ? O8 Tb1 O1 78.17(7) . . ? O6 Tb1 O4 82.27(7) . . ? O3 Tb1 O4 57.58(7) . . ? O7 Tb1 O4 132.33(7) . . ? O2 Tb1 O4 115.14(7) . . ? O9 Tb1 O4 77.49(9) . . ? O5 Tb1 O4 63.94(8) . . ? O10 Tb1 O4 60.58(8) . . ? O8 Tb1 O4 141.31(7) . . ? O1 Tb1 O4 138.55(8) . . ? O6 Tb1 N7 92.37(8) . . ? O3 Tb1 N7 84.93(7) . . ? O7 Tb1 N7 79.94(7) . . ? O2 Tb1 N7 134.38(7) . . ? O9 Tb1 N7 24.49(8) . . ? O5 Tb1 N7 126.28(8) . . ? O10 Tb1 N7 25.07(7) . . ? O8 Tb1 N7 84.88(7) . . ? O1 Tb1 N7 150.21(7) . . ? O4 Tb1 N7 66.02(8) . . ? O6 Tb1 Zn2 35.23(5) . . ? O3 Tb1 Zn2 156.69(5) . . ? O7 Tb1 Zn2 33.92(5) . . ? O2 Tb1 Zn2 139.00(5) . . ? O9 Tb1 Zn2 92.63(6) . . ? O5 Tb1 Zn2 97.86(5) . . ? O10 Tb1 Zn2 56.73(6) . . ? O8 Tb1 Zn2 93.24(5) . . ? O1 Tb1 Zn2 81.67(5) . . ? O4 Tb1 Zn2 102.52(5) . . ? N7 Tb1 Zn2 74.98(6) . . ? N3 Zn1 O2 114.79(10) . . ? N3 Zn1 N1 109.35(12) . . ? O2 Zn1 N1 90.32(9) . . ? N3 Zn1 O3 107.70(11) . . ? O2 Zn1 O3 76.65(8) . . ? N1 Zn1 O3 142.84(10) . . ? N3 Zn1 N2 107.26(11) . . ? O2 Zn1 N2 137.64(9) . . ? N1 Zn1 N2 80.28(11) . . ? O3 Zn1 N2 86.32(9) . . ? N6 Zn2 O7 105.02(11) . . ? N6 Zn2 N4 104.25(12) . . ? O7 Zn2 N4 150.28(10) . . ? N6 Zn2 O6 129.46(11) . . ? O7 Zn2 O6 77.84(8) . . ? N4 Zn2 O6 87.58(9) . . ? N6 Zn2 N5 102.62(11) . . ? O7 Zn2 N5 89.44(9) . . ? N4 Zn2 N5 79.22(11) . . ? O6 Zn2 N5 127.91(9) . . ? N6 Zn2 Tb1 112.85(9) . . ? O7 Zn2 Tb1 40.86(5) . . ? N4 Zn2 Tb1 127.94(8) . . ? O6 Zn2 Tb1 40.59(5) . . ? N5 Zn2 Tb1 123.74(7) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.848 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.065 # Attachment '3e.cif' data_wy1844 _database_code_depnum_ccdc_archive 'CCDC 729277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 Eu N7 O11 S2 Zn2, C2 H3 N' _chemical_formula_sum 'C40 H39 Eu N8 O11 S2 Zn2' _chemical_formula_weight 1154.61 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' S S 0.1246 0.1234 '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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1075(7) _cell_length_b 12.4960(8) _cell_length_c 16.3917(10) _cell_angle_alpha 87.9649(9) _cell_angle_beta 69.2030(10) _cell_angle_gamma 70.8010(10) _cell_volume 2180.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13554 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 28.28 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 2.677 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4813 _exptl_absorpt_correction_T_max 0.5904 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10697 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7448 _reflns_number_gt 7022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0346P)^2^+1.5952P] 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 7448 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.009 _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 C1 C 0.9161(3) 0.9356(3) 0.1122(2) 0.0496(8) Uani 1 1 d U . . H1A H 0.9396 0.9847 0.0680 0.074 Uiso 1 1 calc R . . H1B H 0.9118 0.8704 0.0858 0.074 Uiso 1 1 calc R . . H1C H 0.9775 0.9111 0.1394 0.074 Uiso 1 1 calc R . . C2 C 0.7867(2) 1.09228(19) 0.22232(16) 0.0259(5) Uani 1 1 d U . . C3 C 0.8836(2) 1.1323(2) 0.21202(18) 0.0332(6) Uani 1 1 d U . . H3A H 0.9633 1.0951 0.1712 0.040 Uiso 1 1 calc R . . C4 C 0.8608(3) 1.2294(2) 0.26365(18) 0.0351(6) Uani 1 1 d U . . H4A H 0.9254 1.2577 0.2566 0.042 Uiso 1 1 calc R . . C5 C 0.7439(2) 1.2830(2) 0.32445(16) 0.0287(5) Uani 1 1 d U . . H5A H 0.7305 1.3467 0.3591 0.034 Uiso 1 1 calc R . . C6 C 0.6431(2) 1.24386(19) 0.33577(15) 0.0240(5) Uani 1 1 d U . . C7 C 0.6639(2) 1.14726(19) 0.28303(15) 0.0228(5) Uani 1 1 d U . . C8 C 0.5236(2) 1.29989(19) 0.40681(15) 0.0245(5) Uani 1 1 d U . . H8A H 0.5220 1.3503 0.4480 0.029 Uiso 1 1 calc R . . C9 C 0.3077(2) 1.3307(2) 0.49400(15) 0.0285(5) Uani 1 1 d U . . H9A H 0.3021 1.4049 0.5143 0.034 Uiso 1 1 calc R . . H9B H 0.3110 1.2810 0.5406 0.034 Uiso 1 1 calc R . . C10 C 0.1923(2) 1.3411(2) 0.47144(16) 0.0296(5) Uani 1 1 d U . . H10A H 0.1213 1.3455 0.5246 0.035 Uiso 1 1 calc R . . H10B H 0.1703 1.4098 0.4426 0.035 Uiso 1 1 calc R . . C11 C 0.1458(2) 1.1873(2) 0.42386(16) 0.0270(5) Uani 1 1 d U . . H11A H 0.0689 1.2143 0.4701 0.032 Uiso 1 1 calc R . . C12 C 0.1701(2) 1.0865(2) 0.36881(16) 0.0260(5) Uani 1 1 d U . . C13 C 0.0691(2) 1.0474(2) 0.38237(18) 0.0355(6) Uani 1 1 d U . . H13A H -0.0085 1.0864 0.4249 0.043 Uiso 1 1 calc R . . C14 C 0.0820(3) 0.9531(3) 0.3345(2) 0.0424(7) Uani 1 1 d U . . H14A H 0.0133 0.9298 0.3439 0.051 Uiso 1 1 calc R . . C15 C 0.1982(3) 0.8927(2) 0.27208(18) 0.0356(6) Uani 1 1 d U . . H15A H 0.2076 0.8287 0.2395 0.043 Uiso 1 1 calc R . . C16 C 0.2994(2) 0.9278(2) 0.25846(15) 0.0258(5) Uani 1 1 d U . . C17 C 0.2884(2) 1.02560(19) 0.30472(15) 0.0223(5) Uani 1 1 d U . . C18 C 0.4385(3) 0.7769(2) 0.14406(17) 0.0313(6) Uani 1 1 d U . . H18A H 0.3601 0.7834 0.1388 0.047 Uiso 1 1 calc R . . H18B H 0.4677 0.7076 0.1692 0.047 Uiso 1 1 calc R . . H18C H 0.4994 0.7762 0.0871 0.047 Uiso 1 1 calc R . . C19 C 0.5952(4) 1.0932(2) 0.07278(19) 0.0545(9) Uani 1 1 d U . . H19A H 0.5651 1.0998 0.0253 0.082 Uiso 1 1 calc R . . H19B H 0.6650 1.1202 0.0570 0.082 Uiso 1 1 calc R . . H19C H 0.5292 1.1380 0.1241 0.082 Uiso 1 1 calc R . . C20 C 0.7050(2) 0.8962(2) 0.01791(15) 0.0260(5) Uani 1 1 d U . . C21 C 0.7305(2) 0.9216(2) -0.06779(16) 0.0338(6) Uani 1 1 d U . . H21A H 0.7028 0.9966 -0.0808 0.041 Uiso 1 1 calc R . . C22 C 0.7982(3) 0.8337(2) -0.13483(16) 0.0357(6) Uani 1 1 d U . . H22A H 0.8177 0.8500 -0.1930 0.043 Uiso 1 1 calc R . . C23 C 0.8362(2) 0.7234(2) -0.11503(15) 0.0310(6) Uani 1 1 d U . . H23A H 0.8785 0.6653 -0.1603 0.037 Uiso 1 1 calc R . . C24 C 0.8130(2) 0.6958(2) -0.02843(15) 0.0238(5) Uani 1 1 d U . . C25 C 0.7483(2) 0.78421(19) 0.04013(14) 0.0215(5) Uani 1 1 d U . . C26 C 0.8455(2) 0.5751(2) -0.01455(16) 0.0272(5) Uani 1 1 d U . . H26A H 0.8797 0.5233 -0.0637 0.033 Uiso 1 1 calc R . . C27 C 0.8421(2) 0.4150(2) 0.06932(17) 0.0309(6) Uani 1 1 d U . . H27A H 0.8986 0.3806 0.1000 0.037 Uiso 1 1 calc R . . H27B H 0.8748 0.3732 0.0122 0.037 Uiso 1 1 calc R . . C28 C 0.7103(2) 0.4128(2) 0.12187(17) 0.0311(6) Uani 1 1 d U . . H28A H 0.6622 0.4233 0.0840 0.037 Uiso 1 1 calc R . . H28B H 0.7157 0.3399 0.1457 0.037 Uiso 1 1 calc R . . C29 C 0.5433(2) 0.50982(19) 0.25270(16) 0.0273(5) Uani 1 1 d U . . H29A H 0.5130 0.4509 0.2507 0.033 Uiso 1 1 calc R . . C30 C 0.4673(2) 0.6011(2) 0.32362(16) 0.0252(5) Uani 1 1 d U . . C31 C 0.3561(2) 0.5903(2) 0.38480(17) 0.0316(6) Uani 1 1 d U . . H31A H 0.3366 0.5255 0.3794 0.038 Uiso 1 1 calc R . . C32 C 0.2755(2) 0.6730(2) 0.45214(18) 0.0353(6) Uani 1 1 d U . . H32A H 0.2039 0.6627 0.4924 0.042 Uiso 1 1 calc R . . C33 C 0.3013(2) 0.7723(2) 0.46019(16) 0.0296(5) Uani 1 1 d U . . H33A H 0.2469 0.8288 0.5053 0.036 Uiso 1 1 calc R . . C34 C 0.4085(2) 0.78526(19) 0.40019(15) 0.0227(5) Uani 1 1 d U . . C35 C 0.4946(2) 0.70111(19) 0.33122(14) 0.0206(5) Uani 1 1 d U . . C36 C 0.3810(2) 0.9601(2) 0.47464(15) 0.0291(5) Uani 1 1 d U . . H36A H 0.3895 0.9209 0.5247 0.044 Uiso 1 1 calc R . . H36B H 0.2936 0.9941 0.4834 0.044 Uiso 1 1 calc R . . H36C H 0.4185 1.0183 0.4672 0.044 Uiso 1 1 calc R . . C37 C 0.4014(2) 1.3547(2) 0.16229(17) 0.0284(5) Uani 1 1 d U . . C38 C 0.9089(2) 0.4956(2) 0.29056(16) 0.0260(5) Uani 1 1 d U . . C39 C 0.1684(3) 0.6833(3) 0.1487(3) 0.0601(10) Uani 1 1 d U . . C40 C 0.1417(4) 0.6213(3) 0.2257(3) 0.0793(13) Uani 1 1 d U . . H40A H 0.1977 0.6205 0.2552 0.119 Uiso 1 1 calc R . . H40B H 0.1534 0.5446 0.2083 0.119 Uiso 1 1 calc R . . H40C H 0.0565 0.6578 0.2644 0.119 Uiso 1 1 calc R . . Eu1 Eu 0.599420(10) 0.912028(9) 0.244682(7) 0.01880(5) Uani 1 1 d U . . N1 N 0.42159(19) 1.28394(16) 0.41575(12) 0.0242(4) Uani 1 1 d U . . N2 N 0.22204(18) 1.24090(16) 0.41320(13) 0.0248(4) Uani 1 1 d U . . N3 N 0.3883(2) 1.31115(17) 0.22717(14) 0.0314(5) Uani 1 1 d U . . N4 N 0.83059(18) 0.53527(16) 0.05976(13) 0.0254(4) Uani 1 1 d U . . N5 N 0.64754(19) 0.50478(16) 0.19358(13) 0.0253(4) Uani 1 1 d U . . N6 N 0.8628(2) 0.54364(18) 0.24270(15) 0.0327(5) Uani 1 1 d U . . N7 N 0.79161(19) 0.83573(17) 0.32712(13) 0.0265(4) Uani 1 1 d U . . N8 N 0.1900(3) 0.7343(3) 0.0896(3) 0.0732(10) Uani 1 1 d U . . O1 O 0.79549(16) 0.99613(14) 0.17715(12) 0.0325(4) Uani 1 1 d U . . O2 O 0.57696(15) 1.10238(13) 0.28659(10) 0.0235(3) Uani 1 1 d U . . O3 O 0.39239(14) 1.05167(13) 0.28588(10) 0.0226(3) Uani 1 1 d U . . O4 O 0.42082(16) 0.87304(13) 0.20015(11) 0.0270(4) Uani 1 1 d U . . O5 O 0.63463(17) 0.97578(14) 0.09060(10) 0.0310(4) Uani 1 1 d U . . O6 O 0.72191(15) 0.77017(13) 0.12519(10) 0.0231(3) Uani 1 1 d U . . O7 O 0.59305(14) 0.72501(12) 0.27722(10) 0.0218(3) Uani 1 1 d U . . O8 O 0.44308(15) 0.88050(13) 0.39762(10) 0.0254(4) Uani 1 1 d U . . O9 O 0.68071(16) 0.90430(15) 0.36421(11) 0.0325(4) Uani 1 1 d U . . O10 O 0.81757(16) 0.79211(14) 0.25149(11) 0.0308(4) Uani 1 1 d U . . O11 O 0.86885(18) 0.81370(17) 0.36304(12) 0.0409(5) Uani 1 1 d U . . S1 S 0.42407(7) 1.41516(7) 0.07175(5) 0.04474(18) Uani 1 1 d U . . S2 S 0.97828(7) 0.42676(6) 0.35479(4) 0.03663(16) Uani 1 1 d U . . Zn1 Zn 0.39480(2) 1.20521(2) 0.318244(17) 0.02107(7) Uani 1 1 d U . . Zn2 Zn 0.74452(2) 0.61790(2) 0.183196(17) 0.02117(7) Uani 1 1 d U . . 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 C1 0.0357(16) 0.0465(17) 0.0485(18) -0.0150(14) 0.0097(13) -0.0162(14) C2 0.0281(12) 0.0211(11) 0.0302(13) 0.0059(10) -0.0107(10) -0.0107(10) C3 0.0252(13) 0.0342(14) 0.0377(14) 0.0065(11) -0.0068(11) -0.0123(11) C4 0.0330(14) 0.0368(15) 0.0461(16) 0.0104(12) -0.0183(12) -0.0215(12) C5 0.0352(14) 0.0257(12) 0.0331(13) 0.0053(10) -0.0178(11) -0.0149(11) C6 0.0282(12) 0.0209(11) 0.0275(12) 0.0090(9) -0.0145(10) -0.0099(10) C7 0.0235(12) 0.0203(11) 0.0275(12) 0.0083(9) -0.0109(10) -0.0099(9) C8 0.0334(13) 0.0183(11) 0.0257(12) 0.0038(9) -0.0153(10) -0.0087(10) C9 0.0314(13) 0.0272(12) 0.0228(12) -0.0007(10) -0.0070(10) -0.0075(10) C10 0.0291(13) 0.0246(12) 0.0274(13) -0.0014(10) -0.0060(10) -0.0037(10) C11 0.0207(12) 0.0294(13) 0.0258(12) 0.0040(10) -0.0071(10) -0.0037(10) C12 0.0234(12) 0.0293(13) 0.0279(12) 0.0079(10) -0.0122(10) -0.0097(10) C13 0.0235(13) 0.0451(16) 0.0388(15) 0.0040(12) -0.0101(11) -0.0140(12) C14 0.0328(15) 0.0514(17) 0.0531(18) 0.0049(14) -0.0171(13) -0.0252(13) C15 0.0381(15) 0.0374(15) 0.0417(15) 0.0023(12) -0.0198(12) -0.0202(12) C16 0.0272(12) 0.0281(12) 0.0259(12) 0.0062(10) -0.0134(10) -0.0104(10) C17 0.0242(12) 0.0243(12) 0.0240(12) 0.0088(9) -0.0135(10) -0.0108(10) C18 0.0379(14) 0.0260(13) 0.0348(14) -0.0036(10) -0.0194(12) -0.0096(11) C19 0.084(2) 0.0223(14) 0.0299(15) 0.0033(11) -0.0080(15) 0.0020(14) C20 0.0264(12) 0.0263(12) 0.0193(11) 0.0001(9) -0.0051(10) -0.0047(10) C21 0.0375(14) 0.0317(14) 0.0239(13) 0.0091(10) -0.0095(11) -0.0037(11) C22 0.0396(15) 0.0419(15) 0.0169(12) 0.0046(11) -0.0076(11) -0.0060(12) C23 0.0293(13) 0.0383(14) 0.0170(11) -0.0046(10) -0.0045(10) -0.0043(11) C24 0.0210(11) 0.0280(12) 0.0206(11) -0.0005(9) -0.0064(9) -0.0070(10) C25 0.0196(11) 0.0280(12) 0.0167(11) 0.0012(9) -0.0059(9) -0.0086(9) C26 0.0227(12) 0.0298(13) 0.0234(12) -0.0069(10) -0.0061(10) -0.0033(10) C27 0.0336(14) 0.0211(12) 0.0338(14) -0.0037(10) -0.0132(11) -0.0025(10) C28 0.0384(14) 0.0215(12) 0.0372(14) -0.0018(10) -0.0178(12) -0.0102(11) C29 0.0316(13) 0.0199(12) 0.0365(14) 0.0073(10) -0.0177(11) -0.0114(10) C30 0.0279(12) 0.0229(12) 0.0280(12) 0.0075(10) -0.0126(10) -0.0106(10) C31 0.0337(14) 0.0311(13) 0.0366(14) 0.0117(11) -0.0142(11) -0.0184(11) C32 0.0274(13) 0.0429(15) 0.0354(14) 0.0121(12) -0.0068(11) -0.0173(12) C33 0.0255(12) 0.0334(13) 0.0245(12) 0.0046(10) -0.0062(10) -0.0064(10) C34 0.0239(12) 0.0232(11) 0.0226(11) 0.0077(9) -0.0109(10) -0.0078(9) C35 0.0215(11) 0.0218(11) 0.0194(11) 0.0063(9) -0.0092(9) -0.0069(9) C36 0.0335(13) 0.0258(12) 0.0203(12) -0.0029(10) -0.0070(10) -0.0030(10) C37 0.0262(12) 0.0259(12) 0.0343(14) 0.0040(11) -0.0121(11) -0.0091(10) C38 0.0252(12) 0.0240(12) 0.0283(12) -0.0043(10) -0.0086(10) -0.0083(10) C39 0.0429(19) 0.058(2) 0.077(3) -0.031(2) -0.0205(19) -0.0115(17) C40 0.054(2) 0.064(2) 0.100(3) -0.024(2) 0.005(2) -0.0268(19) Eu1 0.02240(7) 0.01607(7) 0.01643(7) 0.00072(4) -0.00546(5) -0.00627(5) N1 0.0290(11) 0.0202(10) 0.0216(10) 0.0025(8) -0.0074(8) -0.0079(8) N2 0.0233(10) 0.0213(10) 0.0254(10) 0.0019(8) -0.0069(8) -0.0043(8) N3 0.0369(12) 0.0265(11) 0.0309(12) 0.0079(9) -0.0126(10) -0.0109(9) N4 0.0257(10) 0.0218(10) 0.0265(11) -0.0014(8) -0.0101(8) -0.0043(8) N5 0.0275(11) 0.0194(10) 0.0307(11) 0.0008(8) -0.0134(9) -0.0067(8) N6 0.0350(12) 0.0280(11) 0.0401(13) 0.0038(10) -0.0226(10) -0.0071(9) N7 0.0295(11) 0.0277(11) 0.0277(11) 0.0078(9) -0.0126(9) -0.0146(9) N8 0.065(2) 0.072(2) 0.080(2) -0.0240(19) -0.0373(19) -0.0046(17) O1 0.0258(9) 0.0279(9) 0.0370(10) -0.0037(8) -0.0016(8) -0.0105(7) O2 0.0222(8) 0.0174(8) 0.0305(9) 0.0002(6) -0.0078(7) -0.0078(6) O3 0.0211(8) 0.0213(8) 0.0260(8) 0.0019(6) -0.0075(7) -0.0090(7) O4 0.0295(9) 0.0242(8) 0.0298(9) -0.0017(7) -0.0131(7) -0.0094(7) O5 0.0419(10) 0.0210(8) 0.0195(8) 0.0026(7) -0.0062(7) -0.0027(7) O6 0.0297(9) 0.0214(8) 0.0161(8) 0.0022(6) -0.0077(7) -0.0071(7) O7 0.0231(8) 0.0188(8) 0.0203(8) 0.0013(6) -0.0035(6) -0.0079(6) O8 0.0287(9) 0.0227(8) 0.0204(8) -0.0008(6) -0.0042(7) -0.0079(7) O9 0.0316(10) 0.0354(10) 0.0264(9) -0.0024(7) -0.0112(8) -0.0051(8) O10 0.0307(9) 0.0321(9) 0.0281(9) -0.0027(7) -0.0085(7) -0.0105(8) O11 0.0394(11) 0.0543(12) 0.0393(11) 0.0120(9) -0.0234(9) -0.0196(9) S1 0.0443(4) 0.0567(5) 0.0386(4) 0.0252(3) -0.0183(3) -0.0225(4) S2 0.0413(4) 0.0363(4) 0.0342(4) 0.0041(3) -0.0224(3) -0.0062(3) Zn1 0.02254(14) 0.01831(13) 0.02128(14) 0.00214(10) -0.00667(11) -0.00702(11) Zn2 0.02266(14) 0.01851(13) 0.02177(14) 0.00058(10) -0.00902(11) -0.00511(11) _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 C1 O1 1.437(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(3) . ? C2 O1 1.388(3) . ? C2 C7 1.414(3) . ? C3 C4 1.397(4) . ? C3 H3A 0.9300 . ? C4 C5 1.367(4) . ? C4 H4A 0.9300 . ? C5 C6 1.409(3) . ? C5 H5A 0.9300 . ? C6 C7 1.410(3) . ? C6 C8 1.461(3) . ? C7 O2 1.329(3) . ? C8 N1 1.272(3) . ? C8 H8A 0.9300 . ? C9 N1 1.468(3) . ? C9 C10 1.533(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.467(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.271(3) . ? C11 C12 1.461(3) . ? C11 H11A 0.9300 . ? C12 C13 1.406(3) . ? C12 C17 1.416(3) . ? C13 C14 1.373(4) . ? C13 H13A 0.9300 . ? C14 C15 1.389(4) . ? C14 H14A 0.9300 . ? C15 C16 1.376(4) . ? C15 H15A 0.9300 . ? C16 O4 1.389(3) . ? C16 C17 1.405(3) . ? C17 O3 1.332(3) . ? C18 O4 1.450(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.441(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.376(3) . ? C20 O5 1.393(3) . ? C20 C25 1.409(3) . ? C21 C22 1.393(4) . ? C21 H21A 0.9300 . ? C22 C23 1.369(4) . ? C22 H22A 0.9300 . ? C23 C24 1.400(3) . ? C23 H23A 0.9300 . ? C24 C25 1.411(3) . ? C24 C26 1.459(3) . ? C25 O6 1.334(3) . ? C26 N4 1.274(3) . ? C26 H26A 0.9300 . ? C27 N4 1.471(3) . ? C27 C28 1.530(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N5 1.472(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N5 1.273(3) . ? C29 C30 1.464(3) . ? C29 H29A 0.9300 . ? C30 C31 1.410(3) . ? C30 C35 1.414(3) . ? C31 C32 1.375(4) . ? C31 H31A 0.9300 . ? C32 C33 1.397(4) . ? C32 H32A 0.9300 . ? C33 C34 1.378(3) . ? C33 H33A 0.9300 . ? C34 O8 1.380(3) . ? C34 C35 1.413(3) . ? C35 O7 1.326(3) . ? C36 O8 1.439(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N3 1.161(3) . ? C37 S1 1.618(3) . ? C38 N6 1.159(3) . ? C38 S2 1.626(3) . ? C39 N8 1.139(5) . ? C39 C40 1.450(6) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? Eu1 O6 2.3734(15) . ? Eu1 O7 2.3984(15) . ? Eu1 O2 2.4003(15) . ? Eu1 O3 2.4061(15) . ? Eu1 O9 2.4718(17) . ? Eu1 O5 2.5517(16) . ? Eu1 O10 2.6131(18) . ? Eu1 O8 2.6596(15) . ? Eu1 O4 2.6991(16) . ? Eu1 O1 2.7672(17) . ? Eu1 N7 2.972(2) . ? Eu1 Zn2 3.5170(3) . ? N1 Zn1 2.078(2) . ? N2 Zn1 2.0300(19) . ? N3 Zn1 1.965(2) . ? N4 Zn2 2.0468(19) . ? N5 Zn2 2.083(2) . ? N6 Zn2 1.979(2) . ? N7 O11 1.228(3) . ? N7 O10 1.262(3) . ? N7 O9 1.268(3) . ? O2 Zn1 2.0384(16) . ? O3 Zn1 2.0208(15) . ? O6 Zn2 2.0769(15) . ? O7 Zn2 2.0137(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 125.8(2) . . ? C3 C2 C7 122.0(2) . . ? O1 C2 C7 112.2(2) . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C7 119.1(2) . . ? C5 C6 C8 118.3(2) . . ? C7 C6 C8 122.5(2) . . ? O2 C7 C6 125.1(2) . . ? O2 C7 C2 117.0(2) . . ? C6 C7 C2 118.0(2) . . ? N1 C8 C6 124.0(2) . . ? N1 C8 H8A 118.0 . . ? C6 C8 H8A 118.0 . . ? N1 C9 C10 109.32(19) . . ? N1 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? N1 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C9 108.55(19) . . ? N2 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? N2 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C12 124.8(2) . . ? N2 C11 H11A 117.6 . . ? C12 C11 H11A 117.6 . . ? C13 C12 C17 118.6(2) . . ? C13 C12 C11 117.1(2) . . ? C17 C12 C11 124.3(2) . . ? C14 C13 C12 121.8(3) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 O4 125.5(2) . . ? C15 C16 C17 121.8(2) . . ? O4 C16 C17 112.7(2) . . ? O3 C17 C16 116.6(2) . . ? O3 C17 C12 125.2(2) . . ? C16 C17 C12 118.2(2) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O5 124.6(2) . . ? C21 C20 C25 122.1(2) . . ? O5 C20 C25 113.28(19) . . ? C20 C21 C22 119.2(2) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 121.8(2) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C23 C24 C25 119.0(2) . . ? C23 C24 C26 116.9(2) . . ? C25 C24 C26 123.8(2) . . ? O6 C25 C20 116.87(19) . . ? O6 C25 C24 125.2(2) . . ? C20 C25 C24 117.9(2) . . ? N4 C26 C24 125.1(2) . . ? N4 C26 H26A 117.5 . . ? C24 C26 H26A 117.5 . . ? N4 C27 C28 106.76(19) . . ? N4 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? N4 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? N5 C28 C27 108.97(19) . . ? N5 C28 H28A 109.9 . . ? C27 C28 H28A 109.9 . . ? N5 C28 H28B 109.9 . . ? C27 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? N5 C29 C30 125.1(2) . . ? N5 C29 H29A 117.5 . . ? C30 C29 H29A 117.5 . . ? C31 C30 C35 118.6(2) . . ? C31 C30 C29 117.0(2) . . ? C35 C30 C29 124.2(2) . . ? C32 C31 C30 121.8(2) . . ? C32 C31 H31A 119.1 . . ? C30 C31 H31A 119.1 . . ? C31 C32 C33 120.1(2) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 119.0(2) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 O8 125.4(2) . . ? C33 C34 C35 122.5(2) . . ? O8 C34 C35 112.11(19) . . ? O7 C35 C34 116.44(19) . . ? O7 C35 C30 125.6(2) . . ? C34 C35 C30 118.0(2) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 S1 178.1(2) . . ? N6 C38 S2 178.0(2) . . ? N8 C39 C40 177.9(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O6 Eu1 O7 65.60(5) . . ? O6 Eu1 O2 139.07(5) . . ? O7 Eu1 O2 152.46(5) . . ? O6 Eu1 O3 132.88(5) . . ? O7 Eu1 O3 111.97(5) . . ? O2 Eu1 O3 63.22(5) . . ? O6 Eu1 O9 116.27(6) . . ? O7 Eu1 O9 86.04(6) . . ? O2 Eu1 O9 71.92(6) . . ? O3 Eu1 O9 110.23(5) . . ? O6 Eu1 O5 62.63(5) . . ? O7 Eu1 O5 121.69(5) . . ? O2 Eu1 O5 85.69(5) . . ? O3 Eu1 O5 86.11(5) . . ? O9 Eu1 O5 140.73(6) . . ? O6 Eu1 O10 67.20(5) . . ? O7 Eu1 O10 73.07(5) . . ? O2 Eu1 O10 102.89(5) . . ? O3 Eu1 O10 159.90(5) . . ? O9 Eu1 O10 49.84(5) . . ? O5 Eu1 O10 108.19(6) . . ? O6 Eu1 O8 124.79(5) . . ? O7 Eu1 O8 59.62(5) . . ? O2 Eu1 O8 95.82(5) . . ? O3 Eu1 O8 67.49(5) . . ? O9 Eu1 O8 67.25(6) . . ? O5 Eu1 O8 149.05(6) . . ? O10 Eu1 O8 101.60(5) . . ? O6 Eu1 O4 78.21(5) . . ? O7 Eu1 O4 69.64(5) . . ? O2 Eu1 O4 120.11(5) . . ? O3 Eu1 O4 59.33(5) . . ? O9 Eu1 O4 143.91(5) . . ? O5 Eu1 O4 75.28(6) . . ? O10 Eu1 O4 136.95(5) . . ? O8 Eu1 O4 77.36(5) . . ? O6 Eu1 O1 83.73(5) . . ? O7 Eu1 O1 132.56(5) . . ? O2 Eu1 O1 58.46(5) . . ? O3 Eu1 O1 115.41(5) . . ? O9 Eu1 O1 75.85(6) . . ? O5 Eu1 O1 64.93(6) . . ? O10 Eu1 O1 61.65(5) . . ? O8 Eu1 O1 140.49(5) . . ? O4 Eu1 O1 140.20(5) . . ? O6 Eu1 N7 92.05(6) . . ? O7 Eu1 N7 79.66(5) . . ? O2 Eu1 N7 86.30(5) . . ? O3 Eu1 N7 134.89(5) . . ? O9 Eu1 N7 24.82(5) . . ? O5 Eu1 N7 126.05(6) . . ? O10 Eu1 N7 25.07(5) . . ? O8 Eu1 N7 84.84(5) . . ? O4 Eu1 N7 149.17(5) . . ? O1 Eu1 N7 65.59(5) . . ? O6 Eu1 Zn2 34.92(4) . . ? O7 Eu1 Zn2 33.51(4) . . ? O2 Eu1 Zn2 158.57(4) . . ? O3 Eu1 Zn2 138.04(4) . . ? O9 Eu1 Zn2 93.42(4) . . ? O5 Eu1 Zn2 97.14(4) . . ? O10 Eu1 Zn2 55.99(4) . . ? O8 Eu1 Zn2 92.55(3) . . ? O4 Eu1 Zn2 80.96(3) . . ? O1 Eu1 Zn2 103.50(4) . . ? N7 Eu1 Zn2 74.83(4) . . ? C8 N1 C9 121.9(2) . . ? C8 N1 Zn1 123.88(16) . . ? C9 N1 Zn1 113.91(15) . . ? C11 N2 C10 122.1(2) . . ? C11 N2 Zn1 127.09(17) . . ? C10 N2 Zn1 110.84(15) . . ? C37 N3 Zn1 166.3(2) . . ? C26 N4 C27 120.9(2) . . ? C26 N4 Zn2 129.98(17) . . ? C27 N4 Zn2 106.94(15) . . ? C29 N5 C28 119.8(2) . . ? C29 N5 Zn2 126.91(17) . . ? C28 N5 Zn2 113.27(15) . . ? C38 N6 Zn2 164.8(2) . . ? O11 N7 O10 122.3(2) . . ? O11 N7 O9 121.6(2) . . ? O10 N7 O9 116.11(19) . . ? O11 N7 Eu1 174.61(17) . . ? O10 N7 Eu1 61.35(11) . . ? O9 N7 Eu1 54.93(11) . . ? C2 O1 C1 116.5(2) . . ? C2 O1 Eu1 116.90(13) . . ? C1 O1 Eu1 125.02(15) . . ? C7 O2 Zn1 119.76(14) . . ? C7 O2 Eu1 130.01(14) . . ? Zn1 O2 Eu1 109.83(7) . . ? C17 O3 Zn1 124.25(14) . . ? C17 O3 Eu1 123.68(13) . . ? Zn1 O3 Eu1 110.24(7) . . ? C16 O4 C18 116.42(19) . . ? C16 O4 Eu1 113.76(13) . . ? C18 O4 Eu1 126.17(14) . . ? C20 O5 C19 116.29(19) . . ? C20 O5 Eu1 119.97(13) . . ? C19 O5 Eu1 123.49(15) . . ? C25 O6 Zn2 127.42(14) . . ? C25 O6 Eu1 127.16(13) . . ? Zn2 O6 Eu1 104.23(6) . . ? C35 O7 Zn2 126.88(14) . . ? C35 O7 Eu1 125.70(13) . . ? Zn2 O7 Eu1 105.38(6) . . ? C34 O8 C36 117.24(18) . . ? C34 O8 Eu1 116.78(13) . . ? C36 O8 Eu1 125.59(14) . . ? N7 O9 Eu1 100.25(13) . . ? N7 O10 Eu1 93.59(13) . . ? N3 Zn1 O3 113.79(8) . . ? N3 Zn1 N2 110.19(8) . . ? O3 Zn1 N2 90.58(7) . . ? N3 Zn1 O2 107.68(8) . . ? O3 Zn1 O2 76.72(6) . . ? N2 Zn1 O2 142.02(7) . . ? N3 Zn1 N1 106.90(8) . . ? O3 Zn1 N1 138.90(7) . . ? N2 Zn1 N1 80.58(8) . . ? O2 Zn1 N1 85.95(7) . . ? N3 Zn1 Eu1 116.71(6) . . ? O3 Zn1 Eu1 38.35(4) . . ? N2 Zn1 Eu1 120.66(5) . . ? O2 Zn1 Eu1 38.36(4) . . ? N1 Zn1 Eu1 115.88(5) . . ? N6 Zn2 O7 104.99(8) . . ? N6 Zn2 N4 103.77(9) . . ? O7 Zn2 N4 150.72(7) . . ? N6 Zn2 O6 129.00(8) . . ? O7 Zn2 O6 78.36(6) . . ? N4 Zn2 O6 87.82(7) . . ? N6 Zn2 N5 102.40(8) . . ? O7 Zn2 N5 89.50(7) . . ? N4 Zn2 N5 79.08(8) . . ? O6 Zn2 N5 128.60(7) . . ? N6 Zn2 Eu1 112.63(6) . . ? O7 Zn2 Eu1 41.11(4) . . ? N4 Zn2 Eu1 128.43(6) . . ? O6 Zn2 Eu1 40.85(4) . . ? N5 Zn2 Eu1 124.21(5) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.824 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.063