# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Timothy Boyle' _publ_contact_author_address ; Nanomaterials and Inorganic chemistry Sandia National Laboratories Advanced Materials Laboratory 1001 University Blvd Albuquerque NM 87106 UNITED STATES OF AMERICA ; _publ_contact_author_email TJBOYLE@SANDIA.GOV loop_ _publ_author_name 'Timothy J. Boyle' 'Daniel M. Boye' 'Ping Lu.' 'Leigh Anna Ottley' 'Rebecca Raymond' data_6sp182s _database_code_depnum_ccdc_archive 'CCDC 753900' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 O8 Zn2' _chemical_formula_weight 479.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.120(2) _cell_length_b 12.827(3) _cell_length_c 9.273(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.729(4) _cell_angle_gamma 90.00 _cell_volume 1084.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 157(2) _cell_measurement_reflns_used 3746 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 24.81 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 2.247 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.354 _exptl_absorpt_correction_T_max 0.510 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 157(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7707 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.41 _reflns_number_total 3904 _reflns_number_gt 3425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.2201P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.0(1) _refine_ls_number_reflns 3904 _refine_ls_number_parameters 233 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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 Zn1 Zn 0.19659(7) 0.41581(4) -0.09627(8) 0.0535(2) Uani 1 1 d . . . Zn2 Zn -0.02805(8) 0.59410(5) 0.00152(8) 0.0562(2) Uani 1 1 d . . . O1 O -0.1573(7) 0.5077(5) -0.1180(8) 0.0893(18) Uani 1 1 d . . . O2 O 0.0085(7) 0.4021(5) -0.1995(7) 0.0867(17) Uani 1 1 d . . . O3 O 0.1287(7) 0.6629(4) -0.0947(8) 0.0794(18) Uani 1 1 d . . . O4 O 0.2845(6) 0.5442(4) -0.1721(7) 0.0751(15) Uani 1 1 d . . . O5 O 0.2067(5) 0.4172(5) 0.1130(6) 0.0709(12) Uani 1 1 d . . . O6 O 0.0281(7) 0.5214(5) 0.1777(6) 0.0749(15) Uani 1 1 d . . . O7 O -0.1487(6) 0.7109(3) 0.0629(6) 0.0643(13) Uani 1 1 d . . . O8 O 0.3143(6) 0.2999(4) -0.1689(7) 0.0716(15) Uani 1 1 d . . . C1 C -0.1175(9) 0.4317(6) -0.1918(10) 0.079(2) Uani 1 1 d . . . C2 C -0.2300(15) 0.3766(10) -0.283(2) 0.151(7) Uani 1 1 d . . . H2 H -0.1878 0.3973 -0.3773 0.181 Uiso 1 1 calc R . . C3 C -0.2064(10) 0.2655(8) -0.3016(12) 0.093(3) Uani 1 1 d . . . H3A H -0.2499 0.2276 -0.2218 0.139 Uiso 1 1 calc R . . H3B H -0.1008 0.2512 -0.3024 0.139 Uiso 1 1 calc R . . H3C H -0.2524 0.2427 -0.3931 0.139 Uiso 1 1 calc R . . C4 C -0.3649(12) 0.4222(10) -0.3101(16) 0.114(4) Uani 1 1 d . . . H4A H -0.4242 0.4167 -0.2240 0.171 Uiso 1 1 calc R . . H4B H -0.4150 0.3865 -0.3909 0.171 Uiso 1 1 calc R . . H4C H -0.3515 0.4959 -0.3345 0.171 Uiso 1 1 calc R . . C5 C 0.2348(11) 0.6354(7) -0.1643(10) 0.077(2) Uani 1 1 d . . . C6 C 0.3016(19) 0.7195(8) -0.2575(19) 0.138(6) Uani 1 1 d . . . H6 H 0.2267 0.7328 -0.3363 0.166 Uiso 1 1 calc R . . C7 C 0.314(2) 0.8181(9) -0.179(2) 0.168(9) Uani 1 1 d . . . H7A H 0.3741 0.8078 -0.0904 0.252 Uiso 1 1 calc R . . H7B H 0.2164 0.8423 -0.1538 0.252 Uiso 1 1 calc R . . H7C H 0.3608 0.8703 -0.2396 0.252 Uiso 1 1 calc R . . C8 C 0.4306(17) 0.6860(10) -0.3300(15) 0.117(4) Uani 1 1 d . . . H8A H 0.4677 0.7435 -0.3881 0.175 Uiso 1 1 calc R . . H8B H 0.4058 0.6267 -0.3928 0.175 Uiso 1 1 calc R . . H8C H 0.5060 0.6649 -0.2583 0.175 Uiso 1 1 calc R . . C9 C 0.1256(9) 0.4560(7) 0.2036(9) 0.0731(19) Uani 1 1 d . . . C10 C 0.1376(15) 0.4200(12) 0.3608(11) 0.110(3) Uani 1 1 d . . . H10 H 0.0554 0.4529 0.4134 0.132 Uiso 1 1 calc R . . C11 C 0.123(3) 0.303(2) 0.376(2) 0.203(9) Uiso 1 1 d . . . H11A H 0.1717 0.2810 0.4671 0.304 Uiso 1 1 calc R . . H11B H 0.1696 0.2688 0.2953 0.304 Uiso 1 1 calc R . . H11C H 0.0192 0.2843 0.3772 0.304 Uiso 1 1 calc R . . C12 C 0.266(3) 0.451(3) 0.427(3) 0.219(11) Uiso 1 1 d . . . H12A H 0.2913 0.4025 0.5055 0.329 Uiso 1 1 calc R . . H12B H 0.2537 0.5212 0.4662 0.329 Uiso 1 1 calc R . . H12C H 0.3438 0.4512 0.3568 0.329 Uiso 1 1 calc R . . C13 C -0.2577(7) 0.7146(5) 0.1376(9) 0.0613(19) Uani 1 1 d . . . C14 C -0.3285(9) 0.6162(6) 0.1902(11) 0.071(2) Uani 1 1 d . . . H14 H -0.2596 0.5570 0.1744 0.085 Uiso 1 1 calc R . . C15 C -0.4727(10) 0.5937(9) 0.1053(14) 0.111(4) Uani 1 1 d . . . H15A H -0.5278 0.6587 0.0918 0.167 Uiso 1 1 calc R . . H15B H -0.5314 0.5439 0.1591 0.167 Uiso 1 1 calc R . . H15C H -0.4505 0.5642 0.0110 0.167 Uiso 1 1 calc R . . C16 C -0.356(2) 0.6234(14) 0.3503(15) 0.145(6) Uani 1 1 d . . . H16A H -0.2629 0.6139 0.4048 0.217 Uiso 1 1 calc R . . H16B H -0.4250 0.5689 0.3774 0.217 Uiso 1 1 calc R . . H16C H -0.3967 0.6920 0.3723 0.217 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0507(3) 0.0290(3) 0.0813(5) -0.0019(3) 0.0106(3) 0.0011(3) Zn2 0.0603(4) 0.0310(4) 0.0780(5) -0.0015(3) 0.0169(3) 0.0038(3) O1 0.077(3) 0.064(4) 0.126(5) -0.025(3) -0.018(3) 0.004(3) O2 0.084(4) 0.057(3) 0.116(4) -0.026(3) -0.035(3) 0.012(3) O3 0.101(4) 0.029(3) 0.111(5) 0.007(2) 0.051(3) 0.001(2) O4 0.082(4) 0.038(3) 0.107(4) 0.001(3) 0.038(3) -0.002(2) O5 0.066(3) 0.059(3) 0.088(3) 0.004(3) -0.005(2) 0.013(3) O6 0.084(4) 0.064(3) 0.077(3) 0.012(3) 0.020(3) 0.011(3) O7 0.065(3) 0.026(2) 0.103(4) -0.001(2) 0.024(3) 0.0020(19) O8 0.062(3) 0.038(3) 0.117(4) -0.003(3) 0.036(3) -0.005(2) C1 0.077(5) 0.049(5) 0.109(6) -0.009(4) -0.027(4) 0.020(4) C2 0.115(9) 0.092(8) 0.239(16) -0.063(9) -0.105(11) 0.036(7) C3 0.075(5) 0.080(6) 0.122(7) -0.019(6) -0.016(5) -0.001(4) C4 0.083(6) 0.065(6) 0.191(11) -0.008(7) -0.037(7) 0.012(5) C5 0.099(6) 0.045(4) 0.090(6) 0.011(4) 0.046(5) -0.002(4) C6 0.187(13) 0.047(5) 0.188(13) 0.010(6) 0.127(11) 0.004(6) C7 0.246(18) 0.046(6) 0.223(16) -0.013(7) 0.163(15) -0.033(8) C8 0.153(11) 0.085(7) 0.116(9) 0.011(7) 0.056(8) -0.016(7) C9 0.069(4) 0.069(5) 0.081(5) 0.002(4) 0.002(4) 0.007(4) C10 0.131(9) 0.114(9) 0.085(6) 0.004(7) -0.009(6) 0.024(8) C13 0.052(3) 0.023(3) 0.110(6) 0.000(3) 0.021(3) -0.001(2) C14 0.059(4) 0.032(4) 0.123(6) 0.004(3) 0.024(4) -0.010(3) C15 0.075(5) 0.068(5) 0.190(11) 0.005(8) -0.006(6) -0.035(5) C16 0.202(15) 0.120(12) 0.113(9) 0.011(8) 0.018(9) -0.069(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 Zn1 O5 1.940(5) . ? Zn1 O2 1.947(5) . ? Zn1 O8 1.965(5) . ? Zn1 O4 1.970(5) . ? Zn2 O3 1.923(5) . ? Zn2 O6 1.937(6) . ? Zn2 O1 1.941(6) . ? Zn2 O7 1.954(5) . ? O1 C1 1.251(10) . ? O2 C1 1.215(10) . ? O3 C5 1.231(10) . ? O4 C5 1.258(10) . ? O5 C9 1.241(10) . ? O6 C9 1.240(10) . ? O7 C13 1.230(9) . ? O8 C13 1.247(8) 2_545 ? C1 C2 1.489(13) . ? C2 C4 1.379(15) . ? C2 C3 1.453(16) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.521(12) . ? C6 C8 1.438(18) . ? C6 C7 1.462(18) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.530(13) . ? C10 C12 1.36(3) . ? C10 C11 1.51(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O8 1.247(8) 2 ? C13 C14 1.505(9) . ? C14 C16 1.515(17) . ? C14 C15 1.539(13) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 O5 Zn1 O2 120.5(3) . . ? O5 Zn1 O8 109.9(3) . . ? O2 Zn1 O8 104.2(3) . . ? O5 Zn1 O4 110.0(3) . . ? O2 Zn1 O4 105.2(3) . . ? O8 Zn1 O4 106.1(2) . . ? O3 Zn2 O6 115.6(3) . . ? O3 Zn2 O1 116.4(3) . . ? O6 Zn2 O1 110.3(3) . . ? O3 Zn2 O7 102.5(2) . . ? O6 Zn2 O7 105.1(2) . . ? O1 Zn2 O7 105.4(2) . . ? C1 O1 Zn2 125.2(5) . . ? C1 O2 Zn1 139.8(6) . . ? C5 O3 Zn2 136.0(5) . . ? C5 O4 Zn1 127.3(5) . . ? C9 O5 Zn1 132.0(5) . . ? C9 O6 Zn2 131.2(5) . . ? C13 O7 Zn2 131.8(4) . . ? C13 O8 Zn1 110.4(4) 2_545 . ? O2 C1 O1 124.5(7) . . ? O2 C1 C2 117.1(9) . . ? O1 C1 C2 118.4(8) . . ? C4 C2 C3 122.0(11) . . ? C4 C2 C1 119.9(10) . . ? C3 C2 C1 115.5(8) . . ? C4 C2 H2 95.4 . . ? C3 C2 H2 95.4 . . ? C1 C2 H2 95.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 O4 125.9(7) . . ? O3 C5 C6 115.4(8) . . ? O4 C5 C6 118.5(8) . . ? C8 C6 C7 116.0(14) . . ? C8 C6 C5 113.6(10) . . ? C7 C6 C5 110.9(10) . . ? C8 C6 H6 105.0 . . ? C7 C6 H6 105.0 . . ? C5 C6 H6 105.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O6 C9 O5 125.4(8) . . ? O6 C9 C10 114.8(8) . . ? O5 C9 C10 119.8(8) . . ? C12 C10 C11 108.7(19) . . ? C12 C10 C9 112.1(16) . . ? C11 C10 C9 112.8(13) . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C9 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 O8 120.8(6) . 2 ? O7 C13 C14 120.8(6) . . ? O8 C13 C14 118.4(6) 2 . ? C13 C14 C16 110.6(8) . . ? C13 C14 C15 111.1(8) . . ? C16 C14 C15 110.5(10) . . ? C13 C14 H14 108.2 . . ? C16 C14 H14 108.2 . . ? C15 C14 H14 108.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.002 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.128 # start Validation Reply Form _vrf_PLAT241_6sp182s ; PROBLEM: Check High Ueq as Compared to Neighbors for C2 RESPONSE: some disorder was found on the methyl carbons attached to these methylene C atoms. The C-atoms were fixed using AFIX and they were left isotropic to allow for structure convergence ; _vrf_PLAT242_6sp182s ; PROBLEM: Check Low Ueq as Compared to Neighbors for C10 RESPONSE: see above ; # end Validation Reply Form #===END data_6my172ss _database_code_depnum_ccdc_archive 'CCDC 753901' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnONc _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 O8 Zn2' _chemical_formula_weight 591.33 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 11.5433(6) _cell_length_b 11.5433(6) _cell_length_c 22.9224(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3054.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7904 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 24.99 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.274 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.087 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.609 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22354 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5561 _reflns_number_gt 5235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(9) _refine_ls_number_reflns 5561 _refine_ls_number_parameters 319 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.004 _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 Zn1 Zn 0.81310(3) 0.73973(2) 0.113269(11) 0.02616(8) Uani 1 1 d . . . Zn2 Zn 0.73497(3) 0.95453(3) 0.031930(14) 0.03182(9) Uani 1 1 d . . . O1 O 0.70400(18) 0.83731(18) 0.15541(9) 0.0379(5) Uani 1 1 d . . . O2 O 0.6837(2) 1.00460(17) 0.10835(9) 0.0458(5) Uani 1 1 d . . . O3 O 0.95910(16) 0.80850(18) 0.09035(9) 0.0371(5) Uani 1 1 d . . . O4 O 0.90075(17) 0.93773(17) 0.02437(9) 0.0392(5) Uani 1 1 d . . . O5 O 0.73927(18) 0.67562(17) 0.04343(8) 0.0407(5) Uani 1 1 d . . . O6 O 0.6433(2) 0.82371(18) 0.00474(10) 0.0436(5) Uani 1 1 d . . . O7 O 0.83602(18) 0.59862(16) 0.15763(8) 0.0349(5) Uani 1 1 d . . . O8 O 0.70230(16) 1.07082(16) -0.02747(8) 0.0319(4) Uani 1 1 d . . . C1 C 0.6708(3) 0.9400(3) 0.15212(12) 0.0350(7) Uani 1 1 d . . . C2 C 0.6075(3) 0.9915(3) 0.20409(13) 0.0440(8) Uani 1 1 d . . . H19A H 0.5274 0.9609 0.2041 0.053 Uiso 1 1 calc R . . H19B H 0.6022 1.0763 0.1982 0.053 Uiso 1 1 calc R . . C3 C 0.6593(3) 0.9701(3) 0.26425(12) 0.0364(7) Uani 1 1 d . . . C4 C 0.5949(3) 1.0480(3) 0.30741(14) 0.0528(9) Uani 1 1 d . . . H23A H 0.5124 1.0279 0.3074 0.079 Uiso 1 1 calc R . . H23B H 0.6042 1.1292 0.2959 0.079 Uiso 1 1 calc R . . H23C H 0.6267 1.0367 0.3466 0.079 Uiso 1 1 calc R . . C5 C 0.7863(3) 1.0025(5) 0.2643(2) 0.0883(17) Uani 1 1 d . . . H20A H 0.8182 0.9921 0.3036 0.132 Uiso 1 1 calc R . . H20B H 0.7949 1.0837 0.2525 0.132 Uiso 1 1 calc R . . H20C H 0.8283 0.9527 0.2368 0.132 Uiso 1 1 calc R . . C6 C 0.6452(5) 0.8458(3) 0.28338(18) 0.0862(15) Uani 1 1 d . . . H22A H 0.6904 0.7953 0.2577 0.129 Uiso 1 1 calc R . . H22B H 0.5632 0.8242 0.2813 0.129 Uiso 1 1 calc R . . H22C H 0.6727 0.8373 0.3236 0.129 Uiso 1 1 calc R . . C7 C 0.9776(2) 0.8795(2) 0.05000(12) 0.0293(6) Uani 1 1 d . . . C8 C 1.1005(2) 0.8947(2) 0.03023(13) 0.0337(6) Uani 1 1 d . . . H9A H 1.1531 0.8624 0.0602 0.040 Uiso 1 1 calc R . . H9B H 1.1174 0.9785 0.0266 0.040 Uiso 1 1 calc R . . C9 C 1.1251(3) 0.8348(2) -0.02892(12) 0.0327(7) Uani 1 1 d . . . C10 C 1.0845(3) 0.7094(3) -0.02671(15) 0.0512(9) Uani 1 1 d . . . H15A H 0.9997 0.7073 -0.0245 0.077 Uiso 1 1 calc R . . H15B H 1.1174 0.6714 0.0077 0.077 Uiso 1 1 calc R . . H15C H 1.1102 0.6689 -0.0620 0.077 Uiso 1 1 calc R . . C11 C 1.0666(4) 0.8977(3) -0.07873(15) 0.0594(10) Uani 1 1 d . . . H11A H 1.0819 0.8566 -0.1153 0.089 Uiso 1 1 calc R . . H11B H 1.0971 0.9767 -0.0814 0.089 Uiso 1 1 calc R . . H11C H 0.9829 0.9005 -0.0717 0.089 Uiso 1 1 calc R . . C12 C 1.2560(3) 0.8355(4) -0.03870(17) 0.0608(10) Uani 1 1 d . . . H14A H 1.2940 0.7917 -0.0075 0.091 Uiso 1 1 calc R . . H14B H 1.2842 0.9156 -0.0384 0.091 Uiso 1 1 calc R . . H14C H 1.2737 0.7998 -0.0764 0.091 Uiso 1 1 calc R . . C13 C 0.6648(3) 0.7174(3) 0.00962(12) 0.0351(7) Uani 1 1 d . . . C14 C 0.5979(3) 0.6339(3) -0.02817(14) 0.0464(8) Uani 1 1 d . . . H6A H 0.5143 0.6510 -0.0238 0.056 Uiso 1 1 calc R . . H6B H 0.6111 0.5545 -0.0133 0.056 Uiso 1 1 calc R . . C15 C 0.6279(3) 0.6360(3) -0.09334(13) 0.0393(7) Uani 1 1 d . . . C16 C 0.7563(3) 0.6250(5) -0.10241(19) 0.0771(13) Uani 1 1 d . . . H27A H 0.7730 0.6206 -0.1443 0.116 Uiso 1 1 calc R . . H27B H 0.7843 0.5545 -0.0832 0.116 Uiso 1 1 calc R . . H27C H 0.7955 0.6926 -0.0857 0.116 Uiso 1 1 calc R . . C17 C 0.5849(5) 0.7458(4) -0.12156(18) 0.0976(18) Uani 1 1 d . . . H16A H 0.6264 0.8123 -0.1052 0.146 Uiso 1 1 calc R . . H16B H 0.5017 0.7544 -0.1141 0.146 Uiso 1 1 calc R . . H16C H 0.5985 0.7421 -0.1637 0.146 Uiso 1 1 calc R . . C18 C 0.5699(5) 0.5302(5) -0.12170(19) 0.1025(19) Uani 1 1 d . . . H24A H 0.5836 0.5316 -0.1639 0.154 Uiso 1 1 calc R . . H24B H 0.4863 0.5324 -0.1142 0.154 Uiso 1 1 calc R . . H24C H 0.6026 0.4591 -0.1051 0.154 Uiso 1 1 calc R . . C19 C 0.8916(2) 0.6071(3) 0.20496(12) 0.0308(6) Uani 1 1 d . . . C20 C 0.9099(3) 0.4978(3) 0.23952(15) 0.0457(8) Uani 1 1 d . . . H12A H 0.9581 0.5165 0.2740 0.055 Uiso 1 1 calc R . . H12B H 0.9543 0.4426 0.2152 0.055 Uiso 1 1 calc R . . C21 C 0.7999(3) 0.4375(3) 0.26054(15) 0.0503(9) Uani 1 1 d . . . C22 C 0.7413(5) 0.3760(5) 0.2117(2) 0.123(3) Uani 1 1 d . . . H25A H 0.6625 0.3546 0.2235 0.185 Uiso 1 1 calc R . . H25B H 0.7850 0.3060 0.2018 0.185 Uiso 1 1 calc R . . H25C H 0.7377 0.4271 0.1776 0.185 Uiso 1 1 calc R . . C23 C 0.7235(6) 0.5263(5) 0.2885(4) 0.159(4) Uani 1 1 d . . . H26A H 0.7191 0.5950 0.2635 0.239 Uiso 1 1 calc R . . H26B H 0.7557 0.5481 0.3265 0.239 Uiso 1 1 calc R . . H26C H 0.6457 0.4941 0.2939 0.239 Uiso 1 1 calc R . . C24 C 0.8340(4) 0.3473(3) 0.30640(17) 0.0763(13) Uani 1 1 d . . . H17A H 0.7643 0.3084 0.3209 0.114 Uiso 1 1 calc R . . H17B H 0.8737 0.3859 0.3389 0.114 Uiso 1 1 calc R . . H17C H 0.8860 0.2901 0.2888 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03293(17) 0.02783(16) 0.01771(14) 0.00091(13) 0.00085(13) 0.00125(13) Zn2 0.03763(19) 0.03093(18) 0.02690(16) 0.00495(14) 0.00144(14) 0.00423(14) O1 0.0451(13) 0.0402(12) 0.0283(11) -0.0003(9) 0.0098(9) 0.0093(10) O2 0.0627(14) 0.0448(12) 0.0300(12) 0.0002(10) 0.0077(11) 0.0117(11) O3 0.0326(11) 0.0507(12) 0.0278(10) 0.0088(9) 0.0029(8) -0.0030(9) O4 0.0382(11) 0.0379(11) 0.0414(12) 0.0068(10) 0.0032(10) 0.0022(9) O5 0.0613(14) 0.0368(11) 0.0241(11) -0.0033(9) -0.0151(10) 0.0014(10) O6 0.0501(13) 0.0353(12) 0.0452(13) 0.0072(10) -0.0134(10) -0.0032(10) O7 0.0476(12) 0.0296(11) 0.0276(11) 0.0049(8) -0.0122(9) -0.0010(9) O8 0.0319(11) 0.0364(11) 0.0272(10) 0.0090(8) 0.0031(8) 0.0043(8) C1 0.0316(16) 0.0443(19) 0.0292(16) -0.0066(13) 0.0010(12) 0.0047(13) C2 0.0439(18) 0.053(2) 0.0351(17) -0.0079(15) 0.0067(15) 0.0122(15) C3 0.0343(16) 0.0457(18) 0.0293(15) -0.0124(13) -0.0038(12) 0.0061(13) C4 0.050(2) 0.070(2) 0.0383(19) -0.0219(17) 0.0038(15) 0.0119(18) C5 0.042(2) 0.139(4) 0.084(3) -0.069(3) -0.005(2) 0.007(2) C6 0.158(5) 0.062(3) 0.038(2) 0.007(2) 0.034(3) 0.026(3) C7 0.0348(15) 0.0287(15) 0.0244(14) -0.0058(11) 0.0018(12) -0.0023(12) C8 0.0381(16) 0.0363(15) 0.0266(14) -0.0037(13) 0.0007(13) -0.0078(12) C9 0.0379(17) 0.0351(16) 0.0251(14) -0.0030(12) 0.0047(12) -0.0057(12) C10 0.071(2) 0.0368(18) 0.046(2) -0.0107(15) 0.0192(18) -0.0087(16) C11 0.082(3) 0.065(2) 0.0311(19) 0.0083(17) 0.0033(18) 0.018(2) C12 0.042(2) 0.087(3) 0.054(2) -0.019(2) 0.0181(17) -0.0124(19) C13 0.0439(18) 0.0403(18) 0.0210(14) 0.0030(12) 0.0004(13) -0.0079(14) C14 0.057(2) 0.052(2) 0.0304(17) 0.0034(15) -0.0102(15) -0.0158(16) C15 0.0428(18) 0.0498(19) 0.0254(15) -0.0006(14) -0.0080(13) 0.0062(14) C16 0.063(3) 0.114(4) 0.054(3) -0.021(3) 0.001(2) 0.024(3) C17 0.143(5) 0.113(4) 0.036(2) 0.025(2) 0.003(3) 0.069(3) C18 0.126(4) 0.135(5) 0.047(3) -0.027(3) -0.011(3) -0.049(4) C19 0.0288(14) 0.0360(16) 0.0275(16) 0.0041(12) -0.0023(12) 0.0006(12) C20 0.054(2) 0.0369(18) 0.0463(19) 0.0109(15) -0.0188(16) 0.0009(15) C21 0.059(2) 0.0425(19) 0.049(2) 0.0203(16) 0.0051(17) 0.0041(16) C22 0.152(5) 0.112(4) 0.106(4) 0.068(4) -0.079(4) -0.092(4) C23 0.172(6) 0.104(4) 0.201(8) 0.077(5) 0.142(6) 0.059(4) C24 0.121(4) 0.055(2) 0.053(3) 0.027(2) -0.014(2) -0.012(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 Zn1 O3 1.9356(19) . ? Zn1 O7 1.9384(18) . ? Zn1 O1 1.9463(19) . ? Zn1 O5 1.9587(19) . ? Zn2 O4 1.931(2) . ? Zn2 O2 1.937(2) . ? Zn2 O6 1.947(2) . ? Zn2 O8 1.9489(19) . ? O1 C1 1.248(4) . ? O2 C1 1.259(4) . ? O3 C7 1.254(3) . ? O4 C7 1.259(3) . ? O5 C13 1.253(3) . ? O6 C13 1.257(4) . ? O7 C19 1.264(3) . ? O8 C19 1.248(3) 4_574 ? C1 C2 1.519(4) . ? C2 C3 1.523(4) . ? C2 H19A 0.9900 . ? C2 H19B 0.9900 . ? C3 C6 1.509(5) . ? C3 C5 1.513(5) . ? C3 C4 1.530(4) . ? C4 H23A 0.9800 . ? C4 H23B 0.9800 . ? C4 H23C 0.9800 . ? C5 H20A 0.9800 . ? C5 H20B 0.9800 . ? C5 H20C 0.9800 . ? C6 H22A 0.9800 . ? C6 H22B 0.9800 . ? C6 H22C 0.9800 . ? C7 C8 1.499(4) . ? C8 C9 1.549(4) . ? C8 H9A 0.9900 . ? C8 H9B 0.9900 . ? C9 C11 1.512(4) . ? C9 C10 1.522(4) . ? C9 C12 1.527(4) . ? C10 H15A 0.9800 . ? C10 H15B 0.9800 . ? C10 H15C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H14A 0.9800 . ? C12 H14B 0.9800 . ? C12 H14C 0.9800 . ? C13 C14 1.509(4) . ? C14 C15 1.534(4) . ? C14 H6A 0.9900 . ? C14 H6B 0.9900 . ? C15 C16 1.502(5) . ? C15 C17 1.507(5) . ? C15 C18 1.538(5) . ? C16 H27A 0.9800 . ? C16 H27B 0.9800 . ? C16 H27C 0.9800 . ? C17 H16A 0.9800 . ? C17 H16B 0.9800 . ? C17 H16C 0.9800 . ? C18 H24A 0.9800 . ? C18 H24B 0.9800 . ? C18 H24C 0.9800 . ? C19 O8 1.248(3) 3_755 ? C19 C20 1.505(4) . ? C20 C21 1.527(5) . ? C20 H12A 0.9900 . ? C20 H12B 0.9900 . ? C21 C22 1.488(6) . ? C21 C23 1.497(6) . ? C21 C24 1.531(5) . ? C22 H25A 0.9800 . ? C22 H25B 0.9800 . ? C22 H25C 0.9800 . ? C23 H26A 0.9800 . ? C23 H26B 0.9800 . ? C23 H26C 0.9800 . ? C24 H17A 0.9800 . ? C24 H17B 0.9800 . ? C24 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O7 111.61(9) . . ? O3 Zn1 O1 117.44(9) . . ? O7 Zn1 O1 108.32(9) . . ? O3 Zn1 O5 108.18(9) . . ? O7 Zn1 O5 99.83(8) . . ? O1 Zn1 O5 110.04(9) . . ? O4 Zn2 O2 114.46(9) . . ? O4 Zn2 O6 115.60(10) . . ? O2 Zn2 O6 110.78(10) . . ? O4 Zn2 O8 101.43(8) . . ? O2 Zn2 O8 111.53(8) . . ? O6 Zn2 O8 101.85(9) . . ? C1 O1 Zn1 135.9(2) . . ? C1 O2 Zn2 125.47(19) . . ? C7 O3 Zn1 128.07(18) . . ? C7 O4 Zn2 135.26(19) . . ? C13 O5 Zn1 131.16(19) . . ? C13 O6 Zn2 128.4(2) . . ? C19 O7 Zn1 117.03(18) . . ? C19 O8 Zn2 129.44(18) 4_574 . ? O1 C1 O2 125.0(3) . . ? O1 C1 C2 118.2(3) . . ? O2 C1 C2 116.8(3) . . ? C1 C2 C3 117.2(3) . . ? C1 C2 H19A 108.0 . . ? C3 C2 H19A 108.0 . . ? C1 C2 H19B 108.0 . . ? C3 C2 H19B 108.0 . . ? H19A C2 H19B 107.2 . . ? C6 C3 C5 109.9(4) . . ? C6 C3 C2 112.0(3) . . ? C5 C3 C2 109.9(3) . . ? C6 C3 C4 108.5(3) . . ? C5 C3 C4 109.0(3) . . ? C2 C3 C4 107.4(2) . . ? C3 C4 H23A 109.5 . . ? C3 C4 H23B 109.5 . . ? H23A C4 H23B 109.5 . . ? C3 C4 H23C 109.5 . . ? H23A C4 H23C 109.5 . . ? H23B C4 H23C 109.5 . . ? C3 C5 H20A 109.5 . . ? C3 C5 H20B 109.5 . . ? H20A C5 H20B 109.5 . . ? C3 C5 H20C 109.5 . . ? H20A C5 H20C 109.5 . . ? H20B C5 H20C 109.5 . . ? C3 C6 H22A 109.5 . . ? C3 C6 H22B 109.5 . . ? H22A C6 H22B 109.5 . . ? C3 C6 H22C 109.5 . . ? H22A C6 H22C 109.5 . . ? H22B C6 H22C 109.5 . . ? O3 C7 O4 125.0(3) . . ? O3 C7 C8 117.4(3) . . ? O4 C7 C8 117.6(3) . . ? C7 C8 C9 112.7(2) . . ? C7 C8 H9A 109.0 . . ? C9 C8 H9A 109.0 . . ? C7 C8 H9B 109.0 . . ? C9 C8 H9B 109.0 . . ? H9A C8 H9B 107.8 . . ? C11 C9 C10 110.1(3) . . ? C11 C9 C12 109.2(3) . . ? C10 C9 C12 108.4(3) . . ? C11 C9 C8 111.4(3) . . ? C10 C9 C8 109.8(2) . . ? C12 C9 C8 107.9(2) . . ? C9 C10 H15A 109.5 . . ? C9 C10 H15B 109.5 . . ? H15A C10 H15B 109.5 . . ? C9 C10 H15C 109.5 . . ? H15A C10 H15C 109.5 . . ? H15B C10 H15C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H14A 109.5 . . ? C9 C12 H14B 109.5 . . ? H14A C12 H14B 109.5 . . ? C9 C12 H14C 109.5 . . ? H14A C12 H14C 109.5 . . ? H14B C12 H14C 109.5 . . ? O5 C13 O6 124.5(3) . . ? O5 C13 C14 117.4(3) . . ? O6 C13 C14 118.1(3) . . ? C13 C14 C15 115.7(3) . . ? C13 C14 H6A 108.4 . . ? C15 C14 H6A 108.4 . . ? C13 C14 H6B 108.4 . . ? C15 C14 H6B 108.4 . . ? H6A C14 H6B 107.4 . . ? C16 C15 C17 109.7(4) . . ? C16 C15 C14 110.9(3) . . ? C17 C15 C14 110.9(3) . . ? C16 C15 C18 107.7(3) . . ? C17 C15 C18 110.0(4) . . ? C14 C15 C18 107.5(3) . . ? C15 C16 H27A 109.5 . . ? C15 C16 H27B 109.5 . . ? H27A C16 H27B 109.5 . . ? C15 C16 H27C 109.5 . . ? H27A C16 H27C 109.5 . . ? H27B C16 H27C 109.5 . . ? C15 C17 H16A 109.5 . . ? C15 C17 H16B 109.5 . . ? H16A C17 H16B 109.5 . . ? C15 C17 H16C 109.5 . . ? H16A C17 H16C 109.5 . . ? H16B C17 H16C 109.5 . . ? C15 C18 H24A 109.5 . . ? C15 C18 H24B 109.5 . . ? H24A C18 H24B 109.5 . . ? C15 C18 H24C 109.5 . . ? H24A C18 H24C 109.5 . . ? H24B C18 H24C 109.5 . . ? O8 C19 O7 121.4(3) 3_755 . ? O8 C19 C20 121.3(3) 3_755 . ? O7 C19 C20 117.3(3) . . ? C19 C20 C21 115.6(3) . . ? C19 C20 H12A 108.4 . . ? C21 C20 H12A 108.4 . . ? C19 C20 H12B 108.4 . . ? C21 C20 H12B 108.4 . . ? H12A C20 H12B 107.5 . . ? C22 C21 C23 112.4(5) . . ? C22 C21 C20 111.0(4) . . ? C23 C21 C20 108.2(4) . . ? C22 C21 C24 108.1(3) . . ? C23 C21 C24 108.9(4) . . ? C20 C21 C24 108.2(3) . . ? C21 C22 H25A 109.5 . . ? C21 C22 H25B 109.5 . . ? H25A C22 H25B 109.5 . . ? C21 C22 H25C 109.5 . . ? H25A C22 H25C 109.5 . . ? H25B C22 H25C 109.5 . . ? C21 C23 H26A 109.5 . . ? C21 C23 H26B 109.5 . . ? H26A C23 H26B 109.5 . . ? C21 C23 H26C 109.5 . . ? H26A C23 H26C 109.5 . . ? H26B C23 H26C 109.5 . . ? C21 C24 H17A 109.5 . . ? C21 C24 H17B 109.5 . . ? H17A C24 H17B 109.5 . . ? C21 C24 H17C 109.5 . . ? H17A C24 H17C 109.5 . . ? H17B C24 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.051 # start Validation Reply Form _vrf_PLAT220_6my172ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.43 Ratio RESPONSE: slight disorder in the OPc ligands results in large thermo parameters. Splitting ocupancy with neighboring atom sites did not improve the refinement of these values and was abandoned. ; _vrf_PLAT222_6my172ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.97 Ratio RESPONSE:see above ; _vrf_PLAT242_6my172ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C21 RESPONSE: see above ; # end Validation Reply Form #===END data_7fb072ss _database_code_depnum_ccdc_archive 'CCDC 753902' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H51 N3 O8 Zn2' _chemical_formula_weight 772.563 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5570(9) _cell_length_b 11.8053(9) _cell_length_c 15.0066(11) _cell_angle_alpha 79.674(1) _cell_angle_beta 69.581(1) _cell_angle_gamma 88.035(1) _cell_volume 1886.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6000 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.34 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.266 _exptl_crystal_size_mid 0.244 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13826 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.38 _reflns_number_total 6820 _reflns_number_gt 5818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.6296P] 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 6820 _refine_ls_number_parameters 431 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.094 _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 C9 C 0.6782(10) 0.7338(7) 0.6622(7) 0.068(3) Uani 0.50 1 d PD . . C10 C 0.4654(8) 0.6713(10) 0.7772(6) 0.079(3) Uani 0.50 1 d PD . . C8' C 0.7155(10) 0.5774(12) 0.6926(10) 0.113(5) Uani 0.50 1 d PD . . Zn1 Zn 0.49922(3) 0.61856(2) 0.45091(2) 0.03026(11) Uani 1 1 d . . . Zn2 Zn 0.92150(3) -0.01542(3) 0.10045(2) 0.03004(11) Uani 1 1 d . . . N1 N 0.4733(2) 0.76449(18) 0.36441(16) 0.0304(5) Uani 1 1 d . . . N2 N 0.8180(2) -0.01276(18) 0.24105(15) 0.0284(5) Uani 1 1 d . . . O1 O 0.32142(19) 0.58780(18) 0.54087(16) 0.0468(5) Uani 1 1 d . . . O2 O 0.68294(19) 0.59621(17) 0.38957(16) 0.0452(5) Uani 1 1 d . . . O3 O 0.5347(2) 0.67652(17) 0.56009(14) 0.0439(5) Uani 1 1 d . . . O4 O 0.4678(2) 0.50651(17) 0.37106(16) 0.0479(5) Uani 1 1 d . . . O5 O 1.0311(2) 0.12706(18) 0.07573(15) 0.0489(6) Uani 1 1 d . . . O6 O 0.8439(2) -0.15598(19) 0.07713(16) 0.0473(5) Uani 1 1 d . . . O7 O 0.8132(2) 0.0841(2) 0.03875(15) 0.0496(6) Uani 1 1 d . . . O8 O 1.06315(19) -0.11445(19) 0.11491(15) 0.0439(5) Uani 1 1 d . . . C1 C 0.2669(3) 0.4970(3) 0.5946(2) 0.0366(6) Uani 1 1 d . . . C2 C 0.1269(3) 0.4999(3) 0.6434(3) 0.0526(9) Uani 1 1 d . . . C3 C 0.0800(4) 0.6178(4) 0.6249(5) 0.118(2) Uani 1 1 d . . . H3A H -0.0105 0.6150 0.6520 0.177 Uiso 1 1 calc R . . H3B H 0.1071 0.6463 0.5551 0.177 Uiso 1 1 calc R . . H3C H 0.1125 0.6695 0.6554 0.177 Uiso 1 1 calc R . . C4 C 0.0681(4) 0.4162(4) 0.6010(4) 0.0801(13) Uani 1 1 d . . . H4A H 0.0980 0.3385 0.6138 0.120 Uiso 1 1 calc R . . H4B H 0.0912 0.4422 0.5311 0.120 Uiso 1 1 calc R . . H4C H -0.0220 0.4153 0.6314 0.120 Uiso 1 1 calc R . . C5 C 0.0918(4) 0.4496(4) 0.7515(3) 0.0829(14) Uani 1 1 d . . . H5A H 0.1319 0.4959 0.7811 0.124 Uiso 1 1 calc R . . H5B H 0.1192 0.3701 0.7592 0.124 Uiso 1 1 calc R . . H5C H 0.0020 0.4506 0.7831 0.124 Uiso 1 1 calc R . . C6 C 0.5478(3) 0.5979(2) 0.6252(2) 0.0348(6) Uani 1 1 d . . . C7 C 0.5863(3) 0.6331(2) 0.7043(2) 0.0404(7) Uani 1 1 d D . . C8 C 0.6346(12) 0.5321(7) 0.7568(8) 0.076(3) Uani 0.50 1 d PD . . C9' C 0.6032(15) 0.7627(7) 0.6925(11) 0.122(7) Uani 0.50 1 d PD . . C10' C 0.4980(15) 0.5758(15) 0.8019(6) 0.169(9) Uani 0.50 1 d PD . . C11 C 1.1173(3) 0.1804(2) 0.0055(2) 0.0366(6) Uani 1 1 d . . . C12 C 1.1772(3) 0.2825(3) 0.0245(3) 0.0588(10) Uani 1 1 d D . . C13 C 1.2632(12) 0.2099(11) 0.0821(10) 0.112(5) Uani 0.50 1 d PD . . C14' C 1.0724(8) 0.3802(7) 0.0272(7) 0.070(2) Uani 0.50 1 d PD . . C15 C 1.2815(5) 0.3386(5) -0.0613(3) 0.0985(18) Uani 1 1 d . . . H15A H 1.2495 0.3775 -0.1109 0.148 Uiso 1 1 calc R . . H15B H 1.3395 0.2800 -0.0872 0.148 Uiso 1 1 calc R . . H15C H 1.3242 0.3951 -0.0422 0.148 Uiso 1 1 calc R . . C16 C 0.8394(3) 0.1284(2) -0.0488(2) 0.0341(6) Uani 1 1 d . . . C17 C 0.7419(3) 0.2059(3) -0.0747(2) 0.0412(7) Uani 1 1 d . . . C18 C 0.7516(4) 0.3207(3) -0.0428(3) 0.0738(12) Uani 1 1 d . . . H18A H 0.8306 0.3600 -0.0837 0.111 Uiso 1 1 calc R . . H18B H 0.7470 0.3060 0.0247 0.111 Uiso 1 1 calc R . . H18C H 0.6835 0.3694 -0.0492 0.111 Uiso 1 1 calc R . . C19 C 0.6143(3) 0.1488(4) -0.0194(3) 0.0869(16) Uani 1 1 d . . . H19A H 0.5518 0.1958 -0.0377 0.130 Uiso 1 1 calc R . . H19B H 0.5964 0.1420 0.0502 0.130 Uiso 1 1 calc R . . H19C H 0.6126 0.0720 -0.0352 0.130 Uiso 1 1 calc R . . C20 C 0.7665(4) 0.2266(3) -0.1826(3) 0.0594(9) Uani 1 1 d . . . H20A H 0.7692 0.1525 -0.2039 0.089 Uiso 1 1 calc R . . H20B H 0.8459 0.2684 -0.2170 0.089 Uiso 1 1 calc R . . H20C H 0.7004 0.2723 -0.1965 0.089 Uiso 1 1 calc R . . C21 C 0.5569(3) 0.8004(2) 0.2766(2) 0.0347(6) Uani 1 1 d . . . H21 H 0.6273 0.7552 0.2546 0.042 Uiso 1 1 calc R . . C22 C 0.5459(3) 0.9001(3) 0.2166(2) 0.0416(7) Uani 1 1 d . . . H22 H 0.6071 0.9233 0.1547 0.050 Uiso 1 1 calc R . . C23 C 0.4430(3) 0.9649(3) 0.2494(2) 0.0436(7) Uani 1 1 d . . . H23 H 0.4330 1.0346 0.2104 0.052 Uiso 1 1 calc R . . C24 C 0.3551(3) 0.9282(3) 0.3389(2) 0.0423(7) Uani 1 1 d . . . H24 H 0.2833 0.9714 0.3619 0.051 Uiso 1 1 calc R . . C25 C 0.3729(3) 0.8279(2) 0.3945(2) 0.0343(6) Uani 1 1 d . . . H25 H 0.3122 0.8025 0.4563 0.041 Uiso 1 1 calc R . . C26 C 0.7648(3) 0.0838(3) 0.2693(2) 0.0425(7) Uani 1 1 d . . . H26 H 0.7794 0.1530 0.2230 0.051 Uiso 1 1 calc R . . C27 C 0.6898(4) 0.0857(3) 0.3632(2) 0.0590(10) Uani 1 1 d . . . H27 H 0.6538 0.1554 0.3816 0.071 Uiso 1 1 calc R . . C28 C 0.6677(3) -0.0152(4) 0.4301(2) 0.0549(9) Uani 1 1 d . . . H28 H 0.6154 -0.0162 0.4952 0.066 Uiso 1 1 calc R . . C29 C 0.7223(3) -0.1140(3) 0.4016(2) 0.0505(8) Uani 1 1 d . . . H29 H 0.7093 -0.1843 0.4465 0.061 Uiso 1 1 calc R . . C30 C 0.7957(3) -0.1092(3) 0.3072(2) 0.0423(7) Uani 1 1 d . . . H30 H 0.8327 -0.1779 0.2876 0.051 Uiso 1 1 calc R . . C14 C 1.0899(10) 0.3414(10) 0.1017(11) 0.106(4) Uani 0.50 1 d PD . . C13' C 1.2007(17) 0.2639(12) 0.1162(7) 0.137(8) Uani 0.50 1 d PD . . 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 C9 0.107(8) 0.045(5) 0.066(5) 0.004(4) -0.049(6) -0.036(5) C10 0.076(6) 0.120(9) 0.042(5) -0.043(5) -0.010(4) 0.026(6) C8' 0.104(9) 0.171(13) 0.133(11) -0.092(10) -0.100(9) 0.067(9) Zn1 0.03332(19) 0.02358(17) 0.03175(18) -0.00120(12) -0.01071(14) 0.00275(13) Zn2 0.02900(18) 0.03523(19) 0.02427(17) -0.00764(13) -0.00620(13) 0.00184(13) N1 0.0326(12) 0.0261(11) 0.0324(12) -0.0040(9) -0.0116(10) 0.0013(9) N2 0.0269(11) 0.0301(11) 0.0275(11) -0.0070(9) -0.0076(9) 0.0013(9) O1 0.0341(11) 0.0443(12) 0.0490(12) 0.0082(10) -0.0067(10) 0.0032(9) O2 0.0344(11) 0.0333(11) 0.0593(13) -0.0072(10) -0.0067(10) 0.0059(9) O3 0.0608(14) 0.0370(11) 0.0365(11) -0.0030(9) -0.0214(10) -0.0051(10) O4 0.0698(15) 0.0285(11) 0.0573(14) -0.0112(10) -0.0353(12) 0.0031(10) O5 0.0534(14) 0.0436(12) 0.0446(12) -0.0112(10) -0.0077(11) -0.0139(10) O6 0.0479(13) 0.0512(13) 0.0452(12) -0.0213(10) -0.0123(10) -0.0060(10) O7 0.0456(13) 0.0630(15) 0.0367(12) -0.0011(10) -0.0150(10) 0.0158(11) O8 0.0356(11) 0.0514(13) 0.0398(11) -0.0052(10) -0.0094(9) 0.0122(10) C1 0.0321(15) 0.0403(16) 0.0346(15) -0.0072(13) -0.0081(12) 0.0033(13) C2 0.0372(17) 0.0442(18) 0.059(2) 0.0027(15) -0.0009(15) 0.0083(14) C3 0.047(2) 0.060(3) 0.189(6) 0.021(3) 0.006(3) 0.019(2) C4 0.054(2) 0.087(3) 0.100(3) -0.001(3) -0.034(2) -0.007(2) C5 0.069(3) 0.090(3) 0.059(2) -0.004(2) 0.011(2) 0.014(2) C6 0.0337(15) 0.0353(16) 0.0349(15) -0.0098(12) -0.0096(12) 0.0025(12) C7 0.0542(19) 0.0328(15) 0.0366(15) -0.0072(12) -0.0183(14) 0.0028(13) C8 0.122(9) 0.058(5) 0.072(6) -0.007(4) -0.068(6) 0.023(6) C9' 0.221(18) 0.045(5) 0.187(16) -0.055(7) -0.166(15) 0.042(8) C10' 0.22(2) 0.231(18) 0.034(5) -0.023(8) -0.008(8) -0.150(17) C11 0.0363(16) 0.0359(15) 0.0411(16) -0.0131(13) -0.0149(13) 0.0022(12) C12 0.059(2) 0.060(2) 0.051(2) -0.0266(17) -0.0004(17) -0.0252(18) C13 0.125(11) 0.148(12) 0.107(10) -0.048(8) -0.077(9) -0.042(9) C14' 0.084(6) 0.048(4) 0.068(5) -0.035(4) -0.001(5) -0.004(4) C15 0.123(4) 0.094(4) 0.071(3) -0.015(3) -0.019(3) -0.063(3) C16 0.0328(15) 0.0330(15) 0.0385(15) -0.0056(12) -0.0151(13) -0.0007(12) C17 0.0353(16) 0.0424(17) 0.0420(16) 0.0007(13) -0.0129(13) 0.0057(13) C18 0.095(3) 0.054(2) 0.076(3) -0.019(2) -0.032(2) 0.030(2) C19 0.035(2) 0.110(4) 0.095(3) 0.038(3) -0.024(2) -0.007(2) C20 0.062(2) 0.068(2) 0.053(2) -0.0030(17) -0.0307(18) 0.0145(19) C21 0.0334(15) 0.0363(15) 0.0341(14) -0.0052(12) -0.0118(12) 0.0026(12) C22 0.0426(17) 0.0455(17) 0.0331(15) 0.0043(13) -0.0138(13) -0.0042(14) C23 0.0545(19) 0.0311(15) 0.0480(18) 0.0052(13) -0.0272(16) -0.0012(14) C24 0.0404(17) 0.0344(15) 0.0533(18) -0.0087(13) -0.0184(15) 0.0109(13) C25 0.0341(15) 0.0309(14) 0.0359(14) -0.0057(11) -0.0099(12) 0.0018(11) C26 0.0504(18) 0.0414(17) 0.0360(15) -0.0095(13) -0.0151(14) 0.0103(14) C27 0.064(2) 0.072(2) 0.0474(19) -0.0311(18) -0.0194(17) 0.0293(19) C28 0.0405(18) 0.089(3) 0.0306(16) -0.0169(17) -0.0033(14) -0.0035(18) C29 0.059(2) 0.053(2) 0.0332(16) -0.0008(14) -0.0099(15) -0.0193(16) C30 0.0550(19) 0.0365(16) 0.0332(15) -0.0061(12) -0.0123(14) -0.0036(14) C14 0.096(8) 0.082(8) 0.131(10) -0.085(8) 0.005(8) -0.005(6) C13' 0.25(2) 0.132(12) 0.039(5) -0.003(6) -0.053(9) -0.126(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 C9 C7 1.513(7) . ? C10 C7 1.556(7) . ? C8' C7 1.575(8) . ? Zn1 O2 2.027(2) . ? Zn1 O1 2.029(2) . ? Zn1 N1 2.044(2) . ? Zn1 O3 2.052(2) . ? Zn1 O4 2.055(2) . ? Zn1 Zn1 2.9229(6) 2_666 ? Zn2 O8 2.030(2) . ? Zn2 O7 2.030(2) . ? Zn2 N2 2.036(2) . ? Zn2 O5 2.041(2) . ? Zn2 O6 2.052(2) . ? Zn2 Zn2 2.8894(6) 2_755 ? N1 C21 1.338(3) . ? N1 C25 1.344(4) . ? N2 C30 1.335(4) . ? N2 C26 1.341(4) . ? O1 C1 1.256(4) . ? O2 C1 1.249(3) 2_666 ? O3 C6 1.268(3) . ? O4 C6 1.241(3) 2_666 ? O5 C11 1.254(3) . ? O6 C11 1.247(3) 2_755 ? O7 C16 1.257(3) . ? O8 C16 1.244(3) 2_755 ? C1 O2 1.249(3) 2_666 ? C1 C2 1.528(4) . ? C2 C3 1.491(5) . ? C2 C5 1.537(5) . ? C2 C4 1.554(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O4 1.241(3) 2_666 ? C6 C7 1.529(4) . ? C7 C8 1.509(7) . ? C7 C10' 1.515(8) . ? C7 C9' 1.520(8) . ? C11 O6 1.247(3) 2_755 ? C11 C12 1.527(4) . ? C12 C13' 1.471(9) . ? C12 C15 1.488(5) . ? C12 C14 1.507(8) . ? C12 C14' 1.639(9) . ? C12 C13 1.657(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O8 1.244(3) 2_755 ? C16 C17 1.537(4) . ? C17 C20 1.517(4) . ? C17 C19 1.527(5) . ? C17 C18 1.536(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.376(4) . ? C23 H23 0.9500 . ? C24 C25 1.375(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.377(4) . ? C26 H26 0.9500 . ? C27 C28 1.381(5) . ? C27 H27 0.9500 . ? C28 C29 1.372(5) . ? C28 H28 0.9500 . ? C29 C30 1.366(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 159.85(8) . . ? O2 Zn1 N1 101.93(9) . . ? O1 Zn1 N1 98.16(8) . . ? O2 Zn1 O3 88.36(9) . . ? O1 Zn1 O3 88.00(9) . . ? N1 Zn1 O3 104.70(8) . . ? O2 Zn1 O4 88.75(9) . . ? O1 Zn1 O4 87.89(10) . . ? N1 Zn1 O4 95.39(9) . . ? O3 Zn1 O4 159.88(8) . . ? O2 Zn1 Zn1 83.27(6) . 2_666 ? O1 Zn1 Zn1 76.90(6) . 2_666 ? N1 Zn1 Zn1 164.85(7) . 2_666 ? O3 Zn1 Zn1 89.56(6) . 2_666 ? O4 Zn1 Zn1 70.33(6) . 2_666 ? O8 Zn2 O7 160.79(9) . . ? O8 Zn2 N2 101.34(8) . . ? O7 Zn2 N2 97.87(9) . . ? O8 Zn2 O5 88.65(9) . . ? O7 Zn2 O5 88.51(10) . . ? N2 Zn2 O5 98.17(8) . . ? O8 Zn2 O6 88.90(9) . . ? O7 Zn2 O6 87.57(10) . . ? N2 Zn2 O6 100.97(8) . . ? O5 Zn2 O6 160.81(9) . . ? O8 Zn2 Zn2 81.18(6) . 2_755 ? O7 Zn2 Zn2 79.79(6) . 2_755 ? N2 Zn2 Zn2 171.58(6) . 2_755 ? O5 Zn2 Zn2 73.76(6) . 2_755 ? O6 Zn2 Zn2 87.05(6) . 2_755 ? C21 N1 C25 118.2(2) . . ? C21 N1 Zn1 120.76(18) . . ? C25 N1 Zn1 121.07(18) . . ? C30 N2 C26 117.9(2) . . ? C30 N2 Zn2 120.63(19) . . ? C26 N2 Zn2 121.36(19) . . ? C1 O1 Zn1 130.89(19) . . ? C1 O2 Zn1 122.92(19) 2_666 . ? C6 O3 Zn1 114.83(18) . . ? C6 O4 Zn1 140.7(2) 2_666 . ? C11 O5 Zn2 136.1(2) . . ? C11 O6 Zn2 118.3(2) 2_755 . ? C16 O7 Zn2 127.56(19) . . ? C16 O8 Zn2 126.12(19) 2_755 . ? O2 C1 O1 125.7(3) 2_666 . ? O2 C1 C2 117.1(3) 2_666 . ? O1 C1 C2 117.3(3) . . ? C3 C2 C1 111.7(3) . . ? C3 C2 C5 113.1(4) . . ? C1 C2 C5 109.1(3) . . ? C3 C2 C4 109.3(4) . . ? C1 C2 C4 107.3(3) . . ? C5 C2 C4 106.0(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 124.3(3) 2_666 . ? O4 C6 C7 117.3(2) 2_666 . ? O3 C6 C7 118.4(2) . . ? C8 C7 C9 112.5(6) . . ? C8 C7 C10' 63.6(8) . . ? C9 C7 C10' 138.8(6) . . ? C8 C7 C9' 132.9(6) . . ? C9 C7 C9' 35.1(6) . . ? C10' C7 C9' 114.8(8) . . ? C8 C7 C6 111.3(4) . . ? C9 C7 C6 110.1(4) . . ? C10' C7 C6 108.9(5) . . ? C9' C7 C6 112.9(5) . . ? C8 C7 C10 108.2(6) . . ? C9 C7 C10 109.5(6) . . ? C10' C7 C10 46.5(8) . . ? C9' C7 C10 75.3(7) . . ? C6 C7 C10 105.0(4) . . ? C8 C7 C8' 43.5(6) . . ? C9 C7 C8' 75.6(7) . . ? C10' C7 C8' 106.4(9) . . ? C9' C7 C8' 108.0(7) . . ? C6 C7 C8' 105.2(4) . . ? C10 C7 C8' 145.1(6) . . ? O6 C11 O5 124.7(3) 2_755 . ? O6 C11 C12 118.8(3) 2_755 . ? O5 C11 C12 116.5(3) . . ? C13' C12 C15 114.9(7) . . ? C13' C12 C14 65.1(8) . . ? C15 C12 C14 126.2(6) . . ? C13' C12 C11 115.5(5) . . ? C15 C12 C11 113.2(3) . . ? C14 C12 C11 113.3(5) . . ? C13' C12 C14' 109.4(8) . . ? C15 C12 C14' 100.1(5) . . ? C14 C12 C14' 45.1(6) . . ? C11 C12 C14' 101.5(4) . . ? C13' C12 C13 37.1(7) . . ? C15 C12 C13 96.4(6) . . ? C14 C12 C13 102.0(7) . . ? C11 C12 C13 98.5(5) . . ? C14' C12 C13 146.4(6) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 125.2(3) 2_755 . ? O8 C16 C17 118.3(3) 2_755 . ? O7 C16 C17 116.5(3) . . ? C20 C17 C19 110.2(3) . . ? C20 C17 C18 109.7(3) . . ? C19 C17 C18 110.5(3) . . ? C20 C17 C16 111.3(3) . . ? C19 C17 C16 108.9(3) . . ? C18 C17 C16 106.2(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 123.1(3) . . ? N1 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 117.8(3) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 118.9(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N1 C25 C24 122.2(3) . . ? N1 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N2 C26 C27 122.1(3) . . ? N2 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C26 C27 C28 118.9(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 118.5(3) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? N2 C30 C29 123.4(3) . . ? N2 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.580 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.073 # start Validation Reply Form _vrf_PLAT043_7fb072ss ; PROBLEM: Check Reported Molecular Weight ................ 772.56 RESPONSE: This MW accounts for the 1 disordered py molecule squeezed out using PLATON ; _vrf_CHEMW01_7fb072ss ; PROBLEM: The ratio of given/expected molecular weight as calculated RESPONSE: 1 disordered py molecule was squeezed using PLATON(284.9A^3) ; _vrf_DENSD01_7fb072ss ; PROBLEM: The ratio of the submitted crystal density and that RESPONSE: see above ; _vrf_PLAT046_7fb072ss ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.36 RESPONSE: see above ; _vrf_PLAT242_7fb072ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C7 RESPONSE: This carbon is attached to the disorderd OBc ligand that was modeled for this disorder ; _vrf_CHEMW03_7fb072ss ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE:see above ; # end Validation Reply Form #===END data_7no281s _database_code_depnum_ccdc_archive 'CCDC 753903' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnONCpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 N2 O8 Zn2' _chemical_formula_weight 749.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.880(3) _cell_length_b 18.289(5) _cell_length_c 21.322(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.485(4) _cell_angle_gamma 90.00 _cell_volume 3828.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 181(2) _cell_measurement_reflns_used 5124 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.30 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.288 _exptl_crystal_size_mid 0.201 _exptl_crystal_size_min 0.088 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 181(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26026 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6935 _reflns_number_gt 5742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+59.8796P] 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 6935 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.2596 _refine_ls_wR_factor_gt 0.2554 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 Zn1 Zn 0.92866(10) 0.64641(5) 0.77932(5) 0.0269(3) Uani 1 1 d . . . Zn2A Zn 1.03408(10) 0.53599(5) 0.69975(5) 0.0273(3) Uani 1 1 d . . . N1 N 1.1078(7) 0.4549(4) 0.6467(4) 0.0303(16) Uani 1 1 d . . . N2 N 0.8559(7) 0.7289(3) 0.8309(3) 0.0275(15) Uani 1 1 d . . . O1 O 0.7499(7) 0.5939(3) 0.7472(3) 0.0350(14) Uani 1 1 d . . . O2 O 0.8312(6) 0.5147(3) 0.6808(3) 0.0369(15) Uani 1 1 d . . . O3 O 0.9731(7) 0.5684(3) 0.8455(3) 0.0376(15) Uani 1 1 d . . . O4 O 1.0384(7) 0.4794(3) 0.7830(3) 0.0377(15) Uani 1 1 d . . . O5 O 1.1301(6) 0.6771(3) 0.7940(3) 0.0361(15) Uani 1 1 d . . . O6 O 1.2067(6) 0.5873(3) 0.7367(3) 0.0341(14) Uani 1 1 d . . . O7 O 0.9186(6) 0.6950(3) 0.6927(3) 0.0368(15) Uani 1 1 d . . . O8 O 1.0108(7) 0.6156(3) 0.6304(3) 0.0382(15) Uani 1 1 d . . . C1 C 0.7352(8) 0.5473(4) 0.7039(4) 0.0269(18) Uani 1 1 d . . . C2 C 0.5912(9) 0.5289(5) 0.6773(4) 0.034(2) Uani 1 1 d . . . H2A H 0.5286 0.5396 0.7093 0.041 Uiso 1 1 calc R . . H2B H 0.5848 0.4760 0.6675 0.041 Uiso 1 1 calc R . . C3 C 0.5466(9) 0.5739(5) 0.6159(4) 0.033(2) Uani 1 1 d . . . C4 C 0.5622(10) 0.6556(5) 0.6285(5) 0.042(2) Uani 1 1 d . . . H4A H 0.6592 0.6682 0.6346 0.063 Uiso 1 1 calc R . . H4B H 0.5201 0.6682 0.6665 0.063 Uiso 1 1 calc R . . H4C H 0.5173 0.6828 0.5924 0.063 Uiso 1 1 calc R . . C5 C 0.3948(9) 0.5557(6) 0.5962(5) 0.042(2) Uani 1 1 d . . . H5A H 0.3407 0.5708 0.6298 0.062 Uiso 1 1 calc R . . H5B H 0.3847 0.5029 0.5893 0.062 Uiso 1 1 calc R . . H5C H 0.3630 0.5817 0.5572 0.062 Uiso 1 1 calc R . . C6 C 0.6288(10) 0.5510(7) 0.5621(5) 0.048(3) Uani 1 1 d . . . H6A H 0.6013 0.5810 0.5247 0.072 Uiso 1 1 calc R . . H6B H 0.6113 0.4994 0.5520 0.072 Uiso 1 1 calc R . . H6C H 0.7262 0.5580 0.5754 0.072 Uiso 1 1 calc R . . C7 C 1.0127(9) 0.5034(5) 0.8356(4) 0.0292(19) Uani 1 1 d . . . C8 C 1.0308(9) 0.4523(5) 0.8915(4) 0.0316(19) Uani 1 1 d . . . H8A H 1.0617 0.4810 0.9298 0.038 Uiso 1 1 calc R . . H8B H 1.1034 0.4166 0.8851 0.038 Uiso 1 1 calc R . . C9 C 0.9020(10) 0.4103(5) 0.9029(4) 0.034(2) Uani 1 1 d . . . C10 C 0.8549(12) 0.3641(6) 0.8447(5) 0.053(3) Uani 1 1 d . . . H10A H 0.8355 0.3961 0.8080 0.080 Uiso 1 1 calc R . . H10B H 0.7723 0.3372 0.8519 0.080 Uiso 1 1 calc R . . H10C H 0.9269 0.3294 0.8371 0.080 Uiso 1 1 calc R . . C11 C 0.9359(12) 0.3612(6) 0.9606(5) 0.051(3) Uani 1 1 d . . . H11A H 0.8560 0.3316 0.9672 0.076 Uiso 1 1 calc R . . H11B H 0.9613 0.3917 0.9979 0.076 Uiso 1 1 calc R . . H11C H 1.0120 0.3290 0.9537 0.076 Uiso 1 1 calc R . . C12 C 0.7871(11) 0.4626(7) 0.9159(6) 0.057(3) Uani 1 1 d . . . H12A H 0.7677 0.4962 0.8801 0.086 Uiso 1 1 calc R . . H12B H 0.8151 0.4907 0.9543 0.086 Uiso 1 1 calc R . . H12C H 0.7050 0.4344 0.9215 0.086 Uiso 1 1 calc R . . C13 C 1.2243(9) 0.6395(5) 0.7749(4) 0.032(2) Uani 1 1 d . . . C14 C 1.3693(9) 0.6562(5) 0.8017(4) 0.0309(19) Uani 1 1 d . . . H14A H 1.3767 0.7092 0.8111 0.037 Uiso 1 1 calc R . . H14B H 1.4303 0.6453 0.7692 0.037 Uiso 1 1 calc R . . C15 C 1.4192(9) 0.6134(5) 0.8620(4) 0.0297(19) Uani 1 1 d . . . C16 C 1.4169(11) 0.5314(5) 0.8492(5) 0.045(2) Uani 1 1 d . . . H16A H 1.4822 0.5198 0.8193 0.067 Uiso 1 1 calc R . . H16B H 1.3252 0.5168 0.8313 0.067 Uiso 1 1 calc R . . H16C H 1.4419 0.5050 0.8888 0.067 Uiso 1 1 calc R . . C17 C 1.5664(10) 0.6364(6) 0.8826(5) 0.042(2) Uani 1 1 d . . . H17A H 1.5696 0.6890 0.8913 0.063 Uiso 1 1 calc R . . H17B H 1.6228 0.6253 0.8489 0.063 Uiso 1 1 calc R . . H17C H 1.6011 0.6096 0.9209 0.063 Uiso 1 1 calc R . . C18 C 1.3302(10) 0.6288(6) 0.9148(5) 0.043(2) Uani 1 1 d . . . H18A H 1.3660 0.6020 0.9529 0.064 Uiso 1 1 calc R . . H18B H 1.2366 0.6130 0.9015 0.064 Uiso 1 1 calc R . . H18C H 1.3310 0.6814 0.9239 0.064 Uiso 1 1 calc R . . C19 C 0.9677(8) 0.6776(5) 0.6424(4) 0.0279(18) Uani 1 1 d . . . C20 C 0.9770(9) 0.7380(5) 0.5945(4) 0.0293(19) Uani 1 1 d . . . H20A H 0.8926 0.7676 0.5915 0.035 Uiso 1 1 calc R . . H20B H 0.9838 0.7159 0.5526 0.035 Uiso 1 1 calc R . . C21 C 1.2338(11) 0.7441(7) 0.6177(7) 0.067(4) Uani 1 1 d . . . H21A H 1.3122 0.7773 0.6234 0.100 Uiso 1 1 calc R . . H21B H 1.2377 0.7151 0.5793 0.100 Uiso 1 1 calc R . . H21C H 1.2359 0.7114 0.6542 0.100 Uiso 1 1 calc R . . C22 C 1.1014(9) 0.7890(5) 0.6118(4) 0.0311(19) Uani 1 1 d . . . C23 C 1.0907(13) 0.8324(5) 0.6713(5) 0.054(3) Uani 1 1 d . . . H23A H 1.1625 0.8696 0.6760 0.080 Uiso 1 1 calc R . . H23B H 1.1012 0.7995 0.7078 0.080 Uiso 1 1 calc R . . H23C H 1.0014 0.8562 0.6686 0.080 Uiso 1 1 calc R . . C24 C 1.1037(11) 0.8430(5) 0.5569(5) 0.043(2) Uani 1 1 d . . . H24A H 1.0208 0.8729 0.5533 0.064 Uiso 1 1 calc R . . H24B H 1.1081 0.8159 0.5175 0.064 Uiso 1 1 calc R . . H24C H 1.1836 0.8749 0.5647 0.064 Uiso 1 1 calc R . . C25 C 1.1959(10) 0.4052(5) 0.6725(5) 0.040(2) Uani 1 1 d . . . H25 H 1.2246 0.4078 0.7165 0.048 Uiso 1 1 calc R . . C26 C 1.2474(13) 0.3497(6) 0.6375(6) 0.056(3) Uani 1 1 d . . . H26 H 1.3081 0.3141 0.6572 0.067 Uiso 1 1 calc R . . C27 C 1.2086(13) 0.3475(6) 0.5742(6) 0.056(3) Uani 1 1 d . . . H27 H 1.2436 0.3104 0.5493 0.068 Uiso 1 1 calc R . . C28 C 1.1190(12) 0.3987(5) 0.5461(5) 0.048(3) Uani 1 1 d . . . H28 H 1.0915 0.3980 0.5020 0.058 Uiso 1 1 calc R . . C29 C 1.0705(10) 0.4513(5) 0.5850(5) 0.038(2) Uani 1 1 d . . . H29 H 1.0075 0.4865 0.5665 0.046 Uiso 1 1 calc R . . C30 C 0.8951(10) 0.7348(6) 0.8908(5) 0.044(2) Uani 1 1 d . . . H30 H 0.9568 0.6996 0.9104 0.053 Uiso 1 1 calc R . . C31 C 0.8493(13) 0.7915(7) 0.9277(6) 0.062(3) Uani 1 1 d . . . H31 H 0.8792 0.7948 0.9715 0.075 Uiso 1 1 calc R . . C32 C 0.7612(13) 0.8413(6) 0.8988(7) 0.063(4) Uani 1 1 d . . . H32 H 0.7285 0.8803 0.9224 0.075 Uiso 1 1 calc R . . C33 C 0.7198(14) 0.8353(6) 0.8358(7) 0.062(4) Uani 1 1 d . . . H33 H 0.6594 0.8703 0.8149 0.075 Uiso 1 1 calc R . . C34 C 0.7670(12) 0.7777(5) 0.8030(5) 0.048(3) Uani 1 1 d . . . H34 H 0.7360 0.7722 0.7595 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0291(5) 0.0155(5) 0.0375(6) -0.0011(4) 0.0098(4) 0.0013(4) Zn2A 0.0299(5) 0.0161(5) 0.0372(6) -0.0014(4) 0.0100(4) 0.0003(4) N1 0.030(4) 0.020(3) 0.042(4) 0.000(3) 0.010(3) 0.001(3) N2 0.029(4) 0.014(3) 0.040(4) 0.001(3) 0.008(3) 0.000(3) O1 0.036(3) 0.031(3) 0.038(3) -0.005(3) 0.009(3) -0.009(3) O2 0.031(3) 0.024(3) 0.057(4) -0.001(3) 0.007(3) -0.004(3) O3 0.050(4) 0.022(3) 0.041(4) 0.003(3) 0.004(3) 0.001(3) O4 0.047(4) 0.030(3) 0.039(4) 0.010(3) 0.014(3) 0.003(3) O5 0.026(3) 0.029(3) 0.052(4) 0.001(3) 0.004(3) -0.002(3) O6 0.034(3) 0.033(3) 0.034(3) -0.004(3) 0.000(3) -0.007(3) O7 0.035(4) 0.034(3) 0.044(4) 0.009(3) 0.016(3) 0.001(3) O8 0.043(4) 0.023(3) 0.049(4) 0.005(3) 0.006(3) -0.002(3) C1 0.027(4) 0.019(4) 0.036(5) 0.007(3) 0.009(4) -0.001(3) C2 0.034(5) 0.022(4) 0.047(5) -0.009(4) 0.011(4) -0.005(4) C3 0.026(5) 0.036(5) 0.037(5) 0.000(4) 0.008(4) 0.001(4) C4 0.041(6) 0.027(5) 0.057(6) 0.003(4) -0.003(5) -0.002(4) C5 0.031(5) 0.041(6) 0.053(6) -0.006(5) 0.006(4) -0.005(4) C6 0.036(5) 0.075(8) 0.034(5) -0.006(5) 0.005(4) -0.002(5) C7 0.028(4) 0.023(4) 0.036(5) 0.010(4) 0.000(4) -0.002(3) C8 0.035(5) 0.026(4) 0.033(5) 0.005(4) 0.002(4) 0.001(4) C9 0.035(5) 0.027(4) 0.042(5) 0.006(4) 0.010(4) 0.000(4) C10 0.059(7) 0.047(6) 0.054(7) -0.001(5) 0.007(5) -0.027(5) C11 0.067(7) 0.033(5) 0.057(7) 0.010(5) 0.024(6) 0.002(5) C12 0.042(6) 0.062(7) 0.072(8) 0.010(6) 0.022(6) 0.003(6) C13 0.031(5) 0.029(5) 0.039(5) 0.009(4) 0.010(4) 0.001(4) C14 0.031(5) 0.025(4) 0.040(5) -0.004(4) 0.015(4) -0.010(4) C15 0.025(4) 0.031(5) 0.034(5) -0.002(4) 0.009(4) -0.004(4) C16 0.049(6) 0.031(5) 0.054(6) 0.007(4) 0.004(5) 0.005(4) C17 0.033(5) 0.042(6) 0.054(6) -0.008(5) 0.015(4) 0.000(4) C18 0.035(5) 0.053(6) 0.042(6) 0.003(5) 0.013(4) 0.008(5) C19 0.023(4) 0.025(4) 0.035(5) 0.003(4) 0.002(4) -0.008(3) C20 0.031(5) 0.026(4) 0.030(4) 0.002(3) -0.002(4) -0.005(4) C21 0.031(6) 0.056(7) 0.115(11) 0.041(7) 0.021(6) 0.007(5) C22 0.026(4) 0.030(5) 0.036(5) 0.006(4) 0.002(4) -0.003(4) C23 0.084(9) 0.027(5) 0.048(6) 0.004(4) -0.004(6) -0.022(5) C24 0.044(6) 0.033(5) 0.050(6) 0.017(4) 0.003(5) -0.004(4) C25 0.040(5) 0.035(5) 0.045(6) 0.002(4) 0.007(4) 0.011(4) C26 0.067(8) 0.029(5) 0.077(9) 0.004(5) 0.027(6) 0.015(5) C27 0.084(9) 0.027(5) 0.064(8) -0.009(5) 0.036(7) 0.001(5) C28 0.071(8) 0.032(5) 0.045(6) -0.007(4) 0.024(5) -0.006(5) C29 0.048(6) 0.026(5) 0.042(6) -0.002(4) 0.012(4) -0.004(4) C30 0.037(5) 0.046(6) 0.048(6) -0.007(5) -0.002(5) 0.010(4) C31 0.066(8) 0.073(9) 0.048(7) -0.031(6) 0.010(6) -0.001(7) C32 0.063(8) 0.030(6) 0.100(11) -0.028(6) 0.035(7) 0.000(5) C33 0.080(9) 0.027(5) 0.086(9) 0.008(6) 0.035(7) 0.027(6) C34 0.070(8) 0.027(5) 0.049(6) 0.013(4) 0.020(5) 0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.020(6) . ? Zn1 O7 2.041(6) . ? Zn1 N2 2.045(7) . ? Zn1 O5 2.057(6) . ? Zn1 O1 2.058(6) . ? Zn2A O6 2.027(6) . ? Zn2A O2 2.038(6) . ? Zn2A N1 2.049(7) . ? Zn2A O4 2.051(6) . ? Zn2A O8 2.069(6) . ? N1 C29 1.326(12) . ? N1 C25 1.334(12) . ? N2 C30 1.295(12) . ? N2 C34 1.342(12) . ? O1 C1 1.252(10) . ? O2 C1 1.266(10) . ? O3 C7 1.276(10) . ? O4 C7 1.256(11) . ? O5 C13 1.261(11) . ? O6 C13 1.254(11) . ? O7 C19 1.267(10) . ? O8 C19 1.250(11) . ? C1 C2 1.510(12) . ? C2 C3 1.567(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(13) . ? C3 C6 1.537(13) . ? C3 C5 1.547(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.510(11) . ? C8 C9 1.528(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(14) . ? C9 C11 1.530(13) . ? C9 C12 1.534(14) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.513(12) . ? C14 C15 1.538(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(13) . ? C15 C17 1.529(13) . ? C15 C18 1.531(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.514(11) . ? C20 C22 1.553(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.537(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.510(14) . ? C22 C24 1.534(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.390(14) . ? C25 H25 0.9500 . ? C26 C27 1.361(17) . ? C26 H26 0.9500 . ? C27 C28 1.378(16) . ? C27 H27 0.9500 . ? C28 C29 1.391(13) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.407(15) . ? C30 H30 0.9500 . ? C31 C32 1.359(18) . ? C31 H31 0.9500 . ? C32 C33 1.363(18) . ? C32 H32 0.9500 . ? C33 C34 1.375(14) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O7 157.5(3) . . ? O3 Zn1 N2 102.0(3) . . ? O7 Zn1 N2 100.4(3) . . ? O3 Zn1 O5 87.5(3) . . ? O7 Zn1 O5 88.0(3) . . ? N2 Zn1 O5 96.3(3) . . ? O3 Zn1 O1 90.8(3) . . ? O7 Zn1 O1 87.1(3) . . ? N2 Zn1 O1 100.5(3) . . ? O5 Zn1 O1 163.1(3) . . ? O6 Zn2A O2 158.7(3) . . ? O6 Zn2A N1 102.4(3) . . ? O2 Zn2A N1 98.9(3) . . ? O6 Zn2A O4 87.9(3) . . ? O2 Zn2A O4 90.0(3) . . ? N1 Zn2A O4 98.0(3) . . ? O6 Zn2A O8 88.4(3) . . ? O2 Zn2A O8 88.0(3) . . ? N1 Zn2A O8 97.6(3) . . ? O4 Zn2A O8 164.4(3) . . ? C29 N1 C25 118.1(8) . . ? C29 N1 Zn2A 120.5(6) . . ? C25 N1 Zn2A 121.4(7) . . ? C30 N2 C34 119.3(8) . . ? C30 N2 Zn1 120.5(6) . . ? C34 N2 Zn1 120.3(7) . . ? C1 O1 Zn1 125.9(6) . . ? C1 O2 Zn2A 126.5(6) . . ? C7 O3 Zn1 126.1(6) . . ? C7 O4 Zn2A 127.6(6) . . ? C13 O5 Zn1 122.6(6) . . ? C13 O6 Zn2A 130.8(6) . . ? C19 O7 Zn1 132.3(6) . . ? C19 O8 Zn2A 120.3(6) . . ? O1 C1 O2 125.3(8) . . ? O1 C1 C2 117.1(7) . . ? O2 C1 C2 117.6(8) . . ? C1 C2 C3 111.1(7) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C6 110.4(8) . . ? C4 C3 C5 109.6(8) . . ? C6 C3 C5 108.4(8) . . ? C4 C3 C2 110.8(8) . . ? C6 C3 C2 110.9(8) . . ? C5 C3 C2 106.6(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 O3 124.7(8) . . ? O4 C7 C8 118.1(8) . . ? O3 C7 C8 117.2(8) . . ? C7 C8 C9 114.2(7) . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 109.4(8) . . ? C10 C9 C11 110.3(8) . . ? C8 C9 C11 108.2(8) . . ? C10 C9 C12 109.1(9) . . ? C8 C9 C12 111.2(8) . . ? C11 C9 C12 108.6(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 O5 124.9(9) . . ? O6 C13 C14 117.1(8) . . ? O5 C13 C14 118.0(8) . . ? C13 C14 C15 114.5(7) . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C17 108.5(8) . . ? C16 C15 C18 108.4(8) . . ? C17 C15 C18 110.2(8) . . ? C16 C15 C14 110.8(7) . . ? C17 C15 C14 107.7(7) . . ? C18 C15 C14 111.3(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 C19 O7 125.0(8) . . ? O8 C19 C20 118.4(8) . . ? O7 C19 C20 116.5(8) . . ? C19 C20 C22 112.6(7) . . ? C19 C20 H20A 109.1 . . ? C22 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C22 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 108.1(8) . . ? C23 C22 C21 110.6(9) . . ? C24 C22 C21 108.7(8) . . ? C23 C22 C20 112.7(8) . . ? C24 C22 C20 106.6(7) . . ? C21 C22 C20 110.0(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 122.4(10) . . ? N1 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 118.4(10) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C26 C27 C28 120.4(10) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 117.3(10) . . ? C27 C28 H28 121.3 . . ? C29 C28 H28 121.3 . . ? N1 C29 C28 123.3(10) . . ? N1 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? N2 C30 C31 122.2(10) . . ? N2 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C32 C31 C30 118.1(11) . . ? C32 C31 H31 121.0 . . ? C30 C31 H31 121.0 . . ? C31 C32 C33 119.9(10) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 118.7(11) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? N2 C34 C33 121.8(11) . . ? N2 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.148 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.159 #===END data_7ap303ss _database_code_depnum_ccdc_archive 'CCDC 753904' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnOPcpy _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 N2 O4 Zn' _chemical_formula_sum 'C18 H24 N2 O4 Zn' _chemical_formula_weight 397.76 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 11.6387(16) _cell_length_b 13.2354(16) _cell_length_c 25.080(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3863.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5539 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 25.37 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.317 _exptl_crystal_size_mid 0.244 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13572 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.37 _reflns_number_total 1864 _reflns_number_gt 1705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+13.3314P] 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 1864 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Zn1 Zn 0.5000 0.15312(3) 0.381813(19) 0.0304(2) Uani 1 2 d S . . N1 N 0.3564(2) 0.06482(19) 0.37844(9) 0.0306(6) Uani 1 1 d . . . O1 O 0.5000 0.2450(2) 0.32105(13) 0.0440(8) Uani 1 2 d S . . O2 O 0.5000 0.1235(4) 0.26173(14) 0.0706(13) Uani 1 2 d S . . O3 O 0.5000 0.2587(2) 0.43696(14) 0.0509(9) Uani 1 2 d S . . O4 O 0.5000 0.1228(3) 0.48722(14) 0.0608(11) Uani 1 2 d S . . C1 C 0.5000 0.2152(4) 0.48282(19) 0.0476(13) Uani 1 2 d S . . C2 C 0.5000 0.2142(5) 0.2739(2) 0.0552(14) Uani 1 2 d S . . C3 C 0.3358(3) -0.0086(2) 0.41381(13) 0.0411(7) Uani 1 1 d . . . H3 H 0.3870 -0.0176 0.4429 0.049 Uiso 1 1 calc R . . C4 C 0.5000 0.2814(8) 0.5317(3) 0.110(4) Uani 1 2 d S . . H4 H 0.5000 0.2272 0.5595 0.132 Uiso 1 2 calc SR . . C5 C 0.1861(3) 0.0168(3) 0.33171(16) 0.0545(10) Uani 1 1 d . . . H5 H 0.1342 0.0285 0.3031 0.065 Uiso 1 1 calc R . . C6 C 0.1667(3) -0.0595(3) 0.36722(18) 0.0598(11) Uani 1 1 d . . . H6 H 0.1026 -0.1033 0.3631 0.072 Uiso 1 1 calc R . . C7 C 0.2818(3) 0.0765(3) 0.33798(13) 0.0430(8) Uani 1 1 d . . . H7 H 0.2958 0.1283 0.3126 0.052 Uiso 1 1 calc R . . C8 C 0.2418(4) -0.0718(3) 0.40911(18) 0.0564(10) Uani 1 1 d . . . H8 H 0.2292 -0.1235 0.4347 0.068 Uiso 1 1 calc R . . C9 C 0.5000 0.2949(9) 0.2304(4) 0.128(4) Uani 1 2 d S . . H9 H 0.5000 0.3540 0.2552 0.153 Uiso 1 2 calc SR . . C10 C 0.6043(7) 0.3140(6) 0.2090(3) 0.170(4) Uani 1 1 d . . . H10A H 0.6629 0.3108 0.2370 0.256 Uiso 1 1 calc R . . H10B H 0.6043 0.3815 0.1930 0.256 Uiso 1 1 calc R . . H10C H 0.6213 0.2635 0.1815 0.256 Uiso 1 1 calc R . . C11 C 0.3927(6) 0.3255(5) 0.5436(3) 0.117(2) Uani 1 1 d . . . H11A H 0.3817 0.3858 0.5215 0.176 Uiso 1 1 calc R . . H11B H 0.3905 0.3445 0.5813 0.176 Uiso 1 1 calc R . . H11C H 0.3313 0.2768 0.5362 0.176 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0315(3) 0.0238(3) 0.0359(3) -0.00326(18) 0.000 0.000 N1 0.0299(13) 0.0308(13) 0.0311(12) -0.0035(9) 0.0033(10) -0.0019(10) O1 0.049(2) 0.0351(17) 0.048(2) 0.0123(15) 0.000 0.000 O2 0.070(3) 0.110(4) 0.033(2) -0.015(2) 0.000 0.000 O3 0.071(2) 0.0301(16) 0.052(2) -0.0109(16) 0.000 0.000 O4 0.079(3) 0.065(3) 0.039(2) 0.0010(18) 0.000 0.000 C1 0.046(3) 0.060(3) 0.036(3) -0.020(2) 0.000 0.000 C2 0.048(3) 0.078(4) 0.040(3) 0.020(3) 0.000 0.000 C3 0.0415(18) 0.0404(17) 0.0416(17) 0.0041(14) 0.0070(14) -0.0001(15) C4 0.090(6) 0.161(9) 0.079(5) -0.088(6) 0.000 0.000 C5 0.0383(19) 0.067(2) 0.058(2) -0.0155(19) -0.0062(17) -0.0044(18) C6 0.0357(19) 0.049(2) 0.095(3) -0.017(2) 0.008(2) -0.0106(17) C7 0.0370(18) 0.053(2) 0.0392(17) -0.0014(15) -0.0005(14) -0.0043(15) C8 0.055(2) 0.0392(18) 0.075(3) 0.0087(18) 0.022(2) -0.0076(17) C9 0.094(6) 0.191(11) 0.098(6) 0.107(7) 0.000 0.000 C10 0.115(6) 0.179(7) 0.217(9) 0.144(7) 0.057(6) 0.001(6) C11 0.117(5) 0.131(5) 0.104(5) -0.066(4) 0.010(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.949(3) . ? Zn1 O3 1.967(3) . ? Zn1 N1 2.041(3) . ? Zn1 N1 2.041(3) 12_655 ? N1 C3 1.338(4) . ? N1 C7 1.345(4) . ? O1 C2 1.251(7) . ? O2 C2 1.238(8) . ? O3 C1 1.287(6) . ? O4 C1 1.227(7) . ? C1 C4 1.508(7) . ? C2 C9 1.529(8) . ? C3 C8 1.381(5) . ? C3 H3 0.9500 . ? C4 C11 1.410(7) . ? C4 C11 1.410(7) 12_655 ? C4 H4 1.0000 . ? C5 C6 1.365(6) . ? C5 C7 1.375(5) . ? C5 H5 0.9500 . ? C6 C8 1.377(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.350(7) 12_655 ? C9 C10 1.350(7) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 Zn1 O3 96.11(15) . . ? O1 Zn1 N1 108.95(9) . . ? O3 Zn1 N1 115.87(8) . . ? O1 Zn1 N1 108.95(9) . 12_655 ? O3 Zn1 N1 115.86(8) . 12_655 ? N1 Zn1 N1 109.92(14) . 12_655 ? C3 N1 C7 117.9(3) . . ? C3 N1 Zn1 122.4(2) . . ? C7 N1 Zn1 119.6(2) . . ? C2 O1 Zn1 122.4(4) . . ? C1 O3 Zn1 108.1(3) . . ? O4 C1 O3 121.8(4) . . ? O4 C1 C4 120.4(6) . . ? O3 C1 C4 117.8(6) . . ? O2 C2 O1 123.3(5) . . ? O2 C2 C9 120.1(7) . . ? O1 C2 C9 116.6(7) . . ? N1 C3 C8 121.7(3) . . ? N1 C3 H3 119.2 . . ? C8 C3 H3 119.2 . . ? C11 C4 C11 124.7(8) . 12_655 ? C11 C4 C1 114.3(4) . . ? C11 C4 C1 114.3(4) 12_655 . ? C11 C4 H4 98.6 . . ? C11 C4 H4 98.6 12_655 . ? C1 C4 H4 98.6 . . ? C6 C5 C7 119.0(4) . . ? C6 C5 H5 120.5 . . ? C7 C5 H5 120.5 . . ? C5 C6 C8 118.7(3) . . ? C5 C6 H6 120.7 . . ? C8 C6 H6 120.7 . . ? N1 C7 C5 123.0(3) . . ? N1 C7 H7 118.5 . . ? C5 C7 H7 118.5 . . ? C6 C8 C3 119.8(4) . . ? C6 C8 H8 120.1 . . ? C3 C8 H8 120.1 . . ? C10 C9 C10 128.0(9) 12_655 . ? C10 C9 C2 114.5(5) 12_655 . ? C10 C9 C2 114.5(5) . . ? C10 C9 H9 95.8 12_655 . ? C10 C9 H9 95.8 . . ? C2 C9 H9 95.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.998 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.082 # start Validation Reply Form _vrf_PLAT222_7ap303ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.22 Ratio RESPONSE: Error due to butyl group of isobutyrate (OPc) ligand ; # end Validation Reply Form #===END data_7ja111aa _database_code_depnum_ccdc_archive 'CCDC 753905' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZNONcH2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 O6 Zn' _chemical_formula_weight 331.70 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.073(8) _cell_length_b 5.5883(14) _cell_length_c 10.729(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.501(6) _cell_angle_gamma 90.00 _cell_volume 1632.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 3256 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.27 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5580 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.42 _reflns_number_total 1511 _reflns_number_gt 1405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.2341P] 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 1511 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Zn1 Zn 0.5000 0.56599(4) 0.7500 0.03557(13) Uani 1 2 d S . . O1 O 0.54798(5) 0.6690(2) 0.93843(12) 0.0451(3) Uani 1 1 d . . . O2 O 0.55487(5) 0.8671(2) 0.77149(12) 0.0471(3) Uani 1 1 d . . . O3 O 0.46513(6) 0.3214(2) 0.82136(14) 0.0594(4) Uani 1 1 d . . . H3A H 0.4648 0.1929 0.7842 0.089 Uiso 1 1 calc R . . H3B H 0.4620 0.3264 0.8761 0.089 Uiso 1 1 d R . . C1 C 0.56823(6) 0.8336(3) 0.89470(17) 0.0382(4) Uani 1 1 d . . . C2 C 0.60872(7) 0.9821(3) 0.9894(2) 0.0440(4) Uani 1 1 d . . . H2A H 0.5979 1.0411 1.0596 0.053 Uiso 1 1 calc R . . H2B H 0.6146 1.1196 0.9418 0.053 Uiso 1 1 calc R . . C3 C 0.65755(7) 0.8451(3) 1.05315(17) 0.0428(4) Uani 1 1 d . . . C4 C 0.69833(9) 1.0279(5) 1.1134(3) 0.0727(7) Uani 1 1 d . . . H4A H 0.7282 0.9461 1.1629 0.109 Uiso 1 1 calc R . . H4B H 0.6892 1.1327 1.1718 0.109 Uiso 1 1 calc R . . H4C H 0.7032 1.1198 1.0435 0.109 Uiso 1 1 calc R . . C5 C 0.66964(9) 0.6979(5) 0.9487(2) 0.0707(6) Uani 1 1 d . . . H5A H 0.7013 0.6248 0.9886 0.106 Uiso 1 1 calc R . . H5B H 0.6700 0.8006 0.8773 0.106 Uiso 1 1 calc R . . H5C H 0.6452 0.5758 0.9145 0.106 Uiso 1 1 calc R . . C6 C 0.65439(8) 0.6788(5) 1.1630(2) 0.0643(6) Uani 1 1 d . . . H6A H 0.6295 0.5601 1.1252 0.096 Uiso 1 1 calc R . . H6B H 0.6461 0.7703 1.2280 0.096 Uiso 1 1 calc R . . H6C H 0.6855 0.6015 1.2049 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.04130(19) 0.03325(19) 0.03153(18) 0.000 0.01197(13) 0.000 O1 0.0543(7) 0.0418(7) 0.0378(6) 0.0001(6) 0.0144(6) -0.0110(6) O2 0.0558(8) 0.0454(7) 0.0362(7) 0.0053(6) 0.0115(6) 0.0008(6) O3 0.0940(11) 0.0477(8) 0.0548(9) -0.0177(7) 0.0488(8) -0.0278(8) C1 0.0425(9) 0.0325(8) 0.0380(9) 0.0007(7) 0.0124(7) 0.0029(7) C2 0.0528(11) 0.0311(8) 0.0452(10) -0.0015(8) 0.0135(9) -0.0045(8) C3 0.0445(10) 0.0416(9) 0.0417(10) -0.0042(8) 0.0145(8) -0.0044(8) C4 0.0540(14) 0.0674(15) 0.088(2) -0.0141(14) 0.0142(13) -0.0178(12) C5 0.0717(15) 0.0741(15) 0.0768(16) -0.0123(13) 0.0390(13) 0.0059(13) C6 0.0609(13) 0.0693(14) 0.0569(13) 0.0179(12) 0.0133(10) 0.0080(12) _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 Zn1 O3 2.0065(13) 2_656 ? Zn1 O3 2.0065(13) . ? Zn1 O1 2.0950(13) . ? Zn1 O1 2.0950(13) 2_656 ? Zn1 O2 2.2744(15) . ? Zn1 O2 2.2744(15) 2_656 ? Zn1 C1 2.5347(18) 2_656 ? O1 C1 1.268(2) . ? O2 C1 1.255(2) . ? O3 H3A 0.8200 . ? O3 H3B 0.6265 . ? C1 C2 1.506(3) . ? C2 C3 1.546(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.527(3) . ? C3 C5 1.527(3) . ? C3 C6 1.529(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O3 94.13(8) 2_656 . ? O3 Zn1 O1 107.50(6) 2_656 . ? O3 Zn1 O1 94.22(5) . . ? O3 Zn1 O1 94.22(5) 2_656 2_656 ? O3 Zn1 O1 107.50(6) . 2_656 ? O1 Zn1 O1 148.12(7) . 2_656 ? O3 Zn1 O2 96.46(6) 2_656 . ? O3 Zn1 O2 153.59(5) . . ? O1 Zn1 O2 59.51(5) . . ? O1 Zn1 O2 95.79(5) 2_656 . ? O3 Zn1 O2 153.59(5) 2_656 2_656 ? O3 Zn1 O2 96.46(6) . 2_656 ? O1 Zn1 O2 95.79(5) . 2_656 ? O1 Zn1 O2 59.51(5) 2_656 2_656 ? O2 Zn1 O2 84.55(7) . 2_656 ? O3 Zn1 C1 124.05(6) 2_656 2_656 ? O3 Zn1 C1 104.12(7) . 2_656 ? O1 Zn1 C1 122.88(5) . 2_656 ? O1 Zn1 C1 29.90(5) 2_656 2_656 ? O2 Zn1 C1 89.79(5) . 2_656 ? O2 Zn1 C1 29.61(5) 2_656 2_656 ? C1 O1 Zn1 94.63(10) . . ? C1 O2 Zn1 86.77(10) . . ? Zn1 O3 H3A 109.5 . . ? Zn1 O3 H3B 126.0 . . ? H3A O3 H3B 121.0 . . ? O2 C1 O1 119.07(16) . . ? O2 C1 C2 120.58(16) . . ? O1 C1 C2 120.33(16) . . ? C1 C2 C3 113.91(16) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C5 109.08(18) . . ? C4 C3 C6 109.13(19) . . ? C5 C3 C6 109.27(18) . . ? C4 C3 C2 108.22(18) . . ? C5 C3 C2 110.71(17) . . ? C6 C3 C2 110.41(16) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.483 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.074 #===END data_7jn052aa _database_code_depnum_ccdc_archive 'CCDC 753906' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PrZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H73 N2 O14 Pr Zn2' _chemical_formula_weight 1137.70 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' 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' Pr Pr -0.2180 2.8214 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.105(2) _cell_length_b 15.219(2) _cell_length_c 19.231(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5591.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4072 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.765 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39666 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.46 _reflns_number_total 10304 _reflns_number_gt 7504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.0(1) _refine_ls_number_reflns 10304 _refine_ls_number_parameters 597 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.243838(16) 0.012980(18) 0.24500(3) 0.04216(9) Uani 1 1 d . . . Zn1 Zn 0.31482(4) -0.10140(5) 0.42061(4) 0.0574(2) Uani 1 1 d . . . Zn2 Zn 0.34604(4) 0.12943(5) 0.08408(4) 0.0569(2) Uani 1 1 d . . . O1 O 0.2437(3) -0.0275(4) 0.4605(3) 0.0754(17) Uani 1 1 d . . . O2 O 0.1993(3) 0.0214(4) 0.3628(3) 0.0739(17) Uani 1 1 d . . . O3 O 0.3974(3) -0.0302(3) 0.4000(3) 0.0684(14) Uani 1 1 d . . . O4 O 0.3398(3) 0.0517(4) 0.3252(3) 0.0786(17) Uani 1 1 d . . . O5 O 0.2848(3) -0.2068(3) 0.3721(3) 0.0788(16) Uani 1 1 d . . . O6 O 0.2746(3) -0.1365(3) 0.2748(2) 0.0638(14) Uani 1 1 d . . . O7 O 0.1339(2) -0.0716(3) 0.2409(3) 0.0715(13) Uani 1 1 d . . . O8 O 0.1215(2) 0.0696(3) 0.2225(2) 0.0620(14) Uani 1 1 d . . . O9 O 0.2249(4) -0.0012(4) 0.1206(3) 0.0816(19) Uani 1 1 d . . . O10 O 0.2759(3) 0.0663(4) 0.0323(3) 0.0700(15) Uani 1 1 d . . . O11 O 0.3563(3) -0.0067(3) 0.1857(3) 0.0831(18) Uani 1 1 d . . . O12 O 0.4212(3) 0.0454(3) 0.1030(3) 0.0687(15) Uani 1 1 d . . . O13 O 0.2604(2) 0.1657(3) 0.2197(2) 0.0631(14) Uani 1 1 d . . . O14 O 0.3213(3) 0.2307(3) 0.1378(3) 0.0716(15) Uani 1 1 d . . . N1 N 0.3546(3) -0.1664(3) 0.5049(3) 0.0530(15) Uani 1 1 d . . . N2 N 0.3958(3) 0.1963(4) 0.0042(3) 0.0626(17) Uani 1 1 d . . . C1 C 0.2047(4) 0.0255(5) 0.4264(5) 0.058(2) Uani 1 1 d . . . C2 C 0.1654(5) 0.0937(5) 0.4654(4) 0.071(2) Uani 1 1 d . . . C3 C 0.1186(12) 0.0569(10) 0.5120(12) 0.352(18) Uani 1 1 d . . . H3A H 0.1397 0.0047 0.5333 0.528 Uiso 1 1 calc R . . H3B H 0.0757 0.0401 0.4874 0.528 Uiso 1 1 calc R . . H3C H 0.1074 0.0999 0.5483 0.528 Uiso 1 1 calc R . . C4 C 0.2123(12) 0.1406(15) 0.5062(16) 0.371(19) Uani 1 1 d . . . H4A H 0.1891 0.1588 0.5494 0.557 Uiso 1 1 calc . . . H4B H 0.2282 0.1927 0.4808 0.557 Uiso 1 1 calc . . . H4C H 0.2526 0.1033 0.5173 0.557 Uiso 1 1 calc . . . C5 C 0.1307(12) 0.1547(11) 0.4223(7) 0.311(14) Uani 1 1 d . . . H5A H 0.0890 0.1271 0.4021 0.466 Uiso 1 1 calc R . . H5B H 0.1622 0.1735 0.3849 0.466 Uiso 1 1 calc R . . H5C H 0.1167 0.2059 0.4499 0.466 Uiso 1 1 calc R . . C6 C 0.3921(4) 0.0367(5) 0.3602(4) 0.0533(19) Uani 1 1 d . . . C7 C 0.4505(4) 0.1046(5) 0.3632(4) 0.060(2) Uani 1 1 d . . . C8 C 0.4264(5) 0.1773(5) 0.4119(5) 0.103(3) Uani 1 1 d . . . H8A H 0.4129 0.1517 0.4567 0.154 Uiso 1 1 calc R . . H8B H 0.3862 0.2077 0.3915 0.154 Uiso 1 1 calc R . . H8C H 0.4647 0.2192 0.4190 0.154 Uiso 1 1 calc R . . C9 C 0.5191(4) 0.0662(6) 0.3912(5) 0.097(3) Uani 1 1 d . . . H9A H 0.5131 0.0499 0.4402 0.145 Uiso 1 1 calc R . . H9B H 0.5564 0.1101 0.3872 0.145 Uiso 1 1 calc R . . H9C H 0.5317 0.0139 0.3642 0.145 Uiso 1 1 calc R . . C10 C 0.4630(5) 0.1438(6) 0.2901(4) 0.095(3) Uani 1 1 d . . . H10A H 0.4933 0.1955 0.2939 0.143 Uiso 1 1 calc R . . H10B H 0.4180 0.1610 0.2697 0.143 Uiso 1 1 calc R . . H10C H 0.4854 0.0997 0.2605 0.143 Uiso 1 1 calc R . . C11 C 0.2688(3) -0.2034(4) 0.3083(4) 0.0498(18) Uani 1 1 d . . . C12 C 0.2473(5) -0.2900(6) 0.2750(5) 0.070(3) Uani 1 1 d . . . C13 C 0.3061(7) -0.3453(7) 0.2697(9) 0.214(10) Uani 1 1 d . . . H13A H 0.2949 -0.3954 0.2398 0.320 Uiso 1 1 calc R . . H13B H 0.3191 -0.3665 0.3161 0.320 Uiso 1 1 calc R . . H13C H 0.3453 -0.3124 0.2497 0.320 Uiso 1 1 calc R . . C14 C 0.1947(9) -0.3328(10) 0.3151(8) 0.287(13) Uani 1 1 d . . . H14A H 0.1560 -0.2919 0.3237 0.431 Uiso 1 1 calc R . . H14B H 0.2146 -0.3518 0.3595 0.431 Uiso 1 1 calc R . . H14C H 0.1773 -0.3840 0.2896 0.431 Uiso 1 1 calc R . . C15 C 0.2201(8) -0.2749(8) 0.2051(6) 0.187(7) Uani 1 1 d . . . H15A H 0.1777 -0.2389 0.2077 0.281 Uiso 1 1 calc R . . H15B H 0.2089 -0.3315 0.1833 0.281 Uiso 1 1 calc R . . H15C H 0.2555 -0.2444 0.1772 0.281 Uiso 1 1 calc R . . C16 C 0.0956(4) -0.0075(5) 0.2291(3) 0.060(2) Uani 1 1 d . . . C17 C 0.0180(4) -0.0202(6) 0.2178(5) 0.081(3) Uani 1 1 d . . . C18 C 0.0025(5) -0.1127(6) 0.1942(6) 0.123(4) Uani 1 1 d . . . H18A H -0.0481 -0.1199 0.1881 0.184 Uiso 1 1 calc R . . H18B H 0.0193 -0.1544 0.2292 0.184 Uiso 1 1 calc R . . H18C H 0.0262 -0.1239 0.1499 0.184 Uiso 1 1 calc R . . C19 C -0.0173(5) -0.0035(6) 0.2886(6) 0.120(4) Uani 1 1 d . . . H19A H -0.0075 0.0567 0.3038 0.181 Uiso 1 1 calc R . . H19B H 0.0011 -0.0450 0.3230 0.181 Uiso 1 1 calc R . . H19C H -0.0680 -0.0116 0.2841 0.181 Uiso 1 1 calc R . . C20 C -0.0115(5) 0.0448(7) 0.1672(6) 0.119(4) Uani 1 1 d . . . H20A H -0.0075 0.1042 0.1866 0.179 Uiso 1 1 calc R . . H20B H -0.0609 0.0313 0.1586 0.179 Uiso 1 1 calc R . . H20C H 0.0146 0.0415 0.1234 0.179 Uiso 1 1 calc R . . C21 C 0.2359(5) 0.0097(5) 0.0565(4) 0.056(2) Uani 1 1 d . . . C22 C 0.1977(6) -0.0524(6) 0.0065(4) 0.086(3) Uani 1 1 d . . . C23 C 0.1696(8) -0.1331(8) 0.0445(5) 0.181(7) Uani 1 1 d . . . H23A H 0.2066 -0.1581 0.0738 0.272 Uiso 1 1 calc R . . H23B H 0.1543 -0.1771 0.0105 0.272 Uiso 1 1 calc R . . H23C H 0.1298 -0.1160 0.0737 0.272 Uiso 1 1 calc R . . C24 C 0.1426(8) -0.0022(7) -0.0300(8) 0.192(8) Uani 1 1 d . . . H24A H 0.1075 0.0176 0.0037 0.288 Uiso 1 1 calc R . . H24B H 0.1203 -0.0398 -0.0649 0.288 Uiso 1 1 calc R . . H24C H 0.1636 0.0489 -0.0529 0.288 Uiso 1 1 calc R . . C25 C 0.2512(6) -0.0837(8) -0.0464(6) 0.158(6) Uani 1 1 d . . . H25A H 0.2502 -0.0450 -0.0871 0.237 Uiso 1 1 calc R . . H25B H 0.2400 -0.1439 -0.0607 0.237 Uiso 1 1 calc R . . H25C H 0.2980 -0.0824 -0.0255 0.237 Uiso 1 1 calc R . . C26 C 0.4065(4) -0.0130(4) 0.1473(4) 0.0535(18) Uani 1 1 d . . . C27 C 0.4549(4) -0.0940(4) 0.1521(4) 0.0578(19) Uani 1 1 d . . . C28 C 0.4180(5) -0.1632(5) 0.1057(5) 0.102(3) Uani 1 1 d . . . H28A H 0.3695 -0.1705 0.1211 0.153 Uiso 1 1 calc R . . H28B H 0.4427 -0.2194 0.1094 0.153 Uiso 1 1 calc R . . H28C H 0.4186 -0.1433 0.0572 0.153 Uiso 1 1 calc R . . C29 C 0.5272(4) -0.0766(6) 0.1253(6) 0.112(4) Uani 1 1 d . . . H29A H 0.5251 -0.0629 0.0756 0.168 Uiso 1 1 calc R . . H29B H 0.5564 -0.1289 0.1324 0.168 Uiso 1 1 calc R . . H29C H 0.5476 -0.0268 0.1505 0.168 Uiso 1 1 calc R . . C30 C 0.4568(4) -0.1260(5) 0.2257(4) 0.086(3) Uani 1 1 d . . . H30A H 0.4771 -0.0804 0.2555 0.130 Uiso 1 1 calc R . . H30B H 0.4855 -0.1793 0.2283 0.130 Uiso 1 1 calc R . . H30C H 0.4092 -0.1392 0.2413 0.130 Uiso 1 1 calc R . . C31 C 0.2827(4) 0.2326(4) 0.1914(4) 0.0490(17) Uani 1 1 d . . . C32 C 0.2670(4) 0.3237(4) 0.2238(4) 0.060(2) Uani 1 1 d . . . C33 C 0.3292(5) 0.3456(6) 0.2712(5) 0.108(3) Uani 1 1 d . . . H33A H 0.3728 0.3413 0.2446 0.161 Uiso 1 1 calc R . . H33B H 0.3305 0.3039 0.3101 0.161 Uiso 1 1 calc R . . H33C H 0.3239 0.4054 0.2893 0.161 Uiso 1 1 calc R . . C34 C 0.2006(5) 0.3206(5) 0.2660(5) 0.096(3) Uani 1 1 d . . . H34A H 0.1928 0.3778 0.2881 0.144 Uiso 1 1 calc R . . H34B H 0.2048 0.2752 0.3019 0.144 Uiso 1 1 calc R . . H34C H 0.1611 0.3067 0.2355 0.144 Uiso 1 1 calc R . . C35 C 0.2632(5) 0.3930(5) 0.1672(4) 0.098(3) Uani 1 1 d . . . H35A H 0.2425 0.4468 0.1861 0.147 Uiso 1 1 calc R . . H35B H 0.2342 0.3713 0.1288 0.147 Uiso 1 1 calc R . . H35C H 0.3105 0.4055 0.1500 0.147 Uiso 1 1 calc R . . C36 C 0.4048(4) -0.1296(5) 0.5448(4) 0.070(2) Uani 1 1 d . . . H36 H 0.4210 -0.0727 0.5324 0.084 Uiso 1 1 calc R . . C37 C 0.4334(4) -0.1685(5) 0.6013(4) 0.071(2) Uani 1 1 d . . . H37 H 0.4686 -0.1396 0.6277 0.085 Uiso 1 1 calc R . . C38 C 0.4104(4) -0.2506(5) 0.6192(4) 0.071(2) Uani 1 1 d . . . H38 H 0.4301 -0.2800 0.6581 0.085 Uiso 1 1 calc R . . C39 C 0.3587(4) -0.2904(5) 0.5810(4) 0.069(2) Uani 1 1 d . . . H39 H 0.3406 -0.3462 0.5938 0.082 Uiso 1 1 calc R . . C40 C 0.3341(4) -0.2469(5) 0.5237(4) 0.065(2) Uani 1 1 d . . . H40 H 0.3003 -0.2758 0.4956 0.078 Uiso 1 1 calc R . . C41 C 0.4383(5) 0.1566(5) -0.0353(4) 0.074(2) Uani 1 1 d . . . H41 H 0.4429 0.0951 -0.0284 0.089 Uiso 1 1 calc R . . C42 C 0.4793(5) 0.1934(6) -0.0880(5) 0.092(3) Uani 1 1 d . . . H42 H 0.5119 0.1596 -0.1141 0.110 Uiso 1 1 calc R . . C43 C 0.4698(8) 0.2785(8) -0.0991(7) 0.191(7) Uani 1 1 d . . . H43 H 0.4957 0.3087 -0.1338 0.229 Uiso 1 1 calc R . . C44 C 0.3871(8) 0.2779(7) -0.0049(6) 0.193(8) Uani 1 1 d . . . H44 H 0.3570 0.3103 0.0249 0.231 Uiso 1 1 calc R . . C45 C 0.4227(11) 0.3203(7) -0.0602(8) 0.281(13) Uani 1 1 d . . . H45 H 0.4128 0.3802 -0.0697 0.338 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.05526(19) 0.03376(15) 0.03746(16) 0.0016(3) -0.0009(3) -0.00069(16) Zn1 0.0779(6) 0.0467(5) 0.0477(5) 0.0081(4) 0.0002(5) -0.0039(4) Zn2 0.0744(5) 0.0425(4) 0.0538(5) 0.0075(4) 0.0095(5) 0.0068(4) O1 0.107(5) 0.061(4) 0.058(4) 0.010(3) 0.005(3) 0.015(3) O2 0.080(4) 0.094(4) 0.048(4) -0.003(3) 0.008(3) 0.007(3) O3 0.081(4) 0.061(3) 0.063(4) 0.017(3) 0.001(3) -0.002(3) O4 0.084(4) 0.082(4) 0.069(4) 0.019(3) -0.027(3) -0.023(3) O5 0.122(5) 0.064(4) 0.050(3) 0.007(3) -0.011(3) -0.018(3) O6 0.086(4) 0.041(3) 0.065(3) 0.008(2) -0.001(3) 0.002(2) O7 0.074(3) 0.045(3) 0.096(4) 0.009(4) -0.010(4) -0.006(2) O8 0.056(3) 0.046(3) 0.084(4) 0.012(2) -0.009(3) -0.003(2) O9 0.113(5) 0.091(5) 0.041(3) -0.012(3) -0.005(3) -0.010(3) O10 0.086(4) 0.066(4) 0.058(3) 0.008(3) 0.004(3) -0.005(3) O11 0.084(4) 0.069(4) 0.096(4) 0.020(3) 0.032(4) 0.026(3) O12 0.079(4) 0.057(3) 0.071(4) 0.030(3) 0.010(3) 0.007(3) O13 0.093(4) 0.035(2) 0.062(4) 0.006(2) 0.002(3) -0.002(2) O14 0.096(4) 0.054(3) 0.065(4) 0.001(3) 0.019(3) -0.006(3) N1 0.067(4) 0.041(3) 0.051(4) 0.007(3) -0.001(3) -0.012(3) N2 0.080(5) 0.040(4) 0.067(4) 0.007(3) 0.023(4) 0.010(3) C1 0.075(6) 0.055(5) 0.044(5) 0.002(4) 0.008(5) -0.012(4) C2 0.103(7) 0.057(5) 0.053(5) -0.016(4) 0.015(5) 0.004(5) C3 0.46(3) 0.109(12) 0.49(3) 0.028(17) 0.40(3) 0.071(17) C4 0.29(2) 0.27(3) 0.56(4) -0.34(3) -0.07(3) 0.07(2) C5 0.54(3) 0.28(2) 0.110(10) -0.013(14) -0.031(18) 0.32(2) C6 0.069(6) 0.045(5) 0.046(5) -0.003(4) -0.004(4) -0.009(4) C7 0.056(5) 0.056(5) 0.066(5) 0.015(4) -0.001(4) -0.009(4) C8 0.134(8) 0.068(6) 0.106(7) -0.011(6) -0.012(7) -0.026(5) C9 0.088(6) 0.094(7) 0.109(8) 0.017(6) -0.027(6) -0.011(5) C10 0.105(7) 0.100(7) 0.081(6) 0.025(5) -0.014(5) -0.037(6) C11 0.060(5) 0.045(4) 0.045(5) 0.006(3) 0.009(4) 0.002(3) C12 0.103(7) 0.044(5) 0.064(5) -0.013(4) 0.005(5) -0.015(5) C13 0.183(12) 0.082(8) 0.38(3) -0.115(12) -0.122(15) 0.057(8) C14 0.37(2) 0.30(2) 0.194(16) -0.136(15) 0.148(17) -0.28(2) C15 0.36(2) 0.091(10) 0.113(11) -0.026(8) -0.100(13) -0.022(12) C16 0.057(4) 0.073(5) 0.049(6) 0.002(4) -0.001(3) -0.010(4) C17 0.054(6) 0.080(6) 0.107(8) 0.013(5) 0.006(5) -0.021(4) C18 0.090(7) 0.100(8) 0.178(10) -0.027(7) -0.019(7) -0.045(6) C19 0.082(8) 0.148(11) 0.131(10) 0.005(8) 0.001(7) 0.008(7) C20 0.070(7) 0.137(9) 0.151(11) 0.042(8) -0.028(7) -0.016(6) C21 0.078(6) 0.047(5) 0.042(5) -0.011(4) -0.014(4) 0.018(4) C22 0.130(9) 0.072(6) 0.055(5) -0.021(5) -0.010(6) -0.018(6) C23 0.303(18) 0.151(12) 0.089(9) -0.029(8) -0.037(10) -0.133(12) C24 0.218(15) 0.135(12) 0.223(16) -0.040(10) -0.165(14) 0.026(10) C25 0.204(14) 0.185(13) 0.084(8) -0.081(9) 0.013(8) 0.013(10) C26 0.061(5) 0.047(4) 0.052(5) 0.004(4) 0.003(4) 0.006(4) C27 0.071(5) 0.043(4) 0.059(5) 0.005(4) 0.011(4) 0.013(4) C28 0.138(8) 0.055(5) 0.113(8) -0.012(5) -0.009(7) 0.005(5) C29 0.067(6) 0.095(7) 0.173(10) 0.041(7) 0.026(6) 0.021(5) C30 0.113(7) 0.071(5) 0.075(7) 0.020(4) 0.002(5) 0.027(5) C31 0.058(5) 0.041(4) 0.049(5) 0.004(3) -0.004(4) 0.001(3) C32 0.088(6) 0.041(4) 0.050(6) -0.008(3) 0.007(4) 0.000(4) C33 0.133(8) 0.090(7) 0.099(7) -0.036(5) -0.034(6) -0.017(6) C34 0.116(7) 0.079(6) 0.092(8) -0.025(5) 0.031(6) 0.008(5) C35 0.175(10) 0.030(4) 0.089(7) 0.006(4) 0.000(6) 0.006(5) C36 0.099(6) 0.054(5) 0.057(5) 0.001(4) 0.001(5) -0.025(5) C37 0.087(6) 0.066(5) 0.060(5) 0.009(4) -0.019(4) -0.010(4) C38 0.088(6) 0.063(5) 0.062(5) 0.025(4) -0.014(5) 0.013(5) C39 0.096(6) 0.046(4) 0.063(5) 0.016(4) -0.014(5) -0.003(4) C40 0.082(6) 0.054(5) 0.060(5) 0.007(4) -0.008(4) -0.024(4) C41 0.100(7) 0.050(5) 0.073(6) 0.006(4) 0.010(5) 0.019(5) C42 0.111(7) 0.097(7) 0.066(6) 0.015(6) 0.024(6) 0.029(6) C43 0.292(17) 0.105(9) 0.176(14) 0.033(9) 0.180(14) 0.015(10) C44 0.326(19) 0.072(8) 0.180(12) 0.038(8) 0.192(14) 0.055(10) C45 0.54(3) 0.062(7) 0.240(17) 0.049(9) 0.28(2) 0.024(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O13 2.396(4) . ? Pr1 O6 2.418(5) . ? Pr1 O2 2.423(6) . ? Pr1 O9 2.429(6) . ? Pr1 O11 2.450(6) . ? Pr1 O7 2.465(4) . ? Pr1 O4 2.467(5) . ? Pr1 O8 2.529(4) . ? Zn1 O1 1.924(5) . ? Zn1 O5 1.941(5) . ? Zn1 O3 1.954(5) . ? Zn1 N1 2.046(5) . ? Zn2 O14 1.915(5) . ? Zn2 O10 1.927(5) . ? Zn2 O12 1.957(5) . ? Zn2 N2 2.073(6) . ? O1 C1 1.278(9) . ? O2 C1 1.229(9) . ? O3 C6 1.277(8) . ? O4 C6 1.227(8) . ? O5 C11 1.265(8) . ? O6 C11 1.211(7) . ? O7 C16 1.241(7) . ? O8 C16 1.279(8) . ? O9 C21 1.262(10) . ? O10 C21 1.241(9) . ? O11 C26 1.214(8) . ? O12 C26 1.263(8) . ? O13 C31 1.230(7) . ? O14 C31 1.268(8) . ? N1 C40 1.336(8) . ? N1 C36 1.350(9) . ? N2 C44 1.265(10) . ? N2 C41 1.266(9) . ? C1 C2 1.484(10) . ? C2 C3 1.384(15) . ? C2 C4 1.389(19) . ? C2 C5 1.410(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9799 . ? C4 H4B 0.9801 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.523(9) . ? C7 C8 1.521(11) . ? C7 C9 1.534(10) . ? C7 C10 1.544(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.522(10) . ? C12 C13 1.409(13) . ? C12 C14 1.423(13) . ? C12 C15 1.460(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.511(10) . ? C17 C20 1.497(11) . ? C17 C18 1.509(11) . ? C17 C19 1.541(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.534(11) . ? C22 C24 1.477(13) . ? C22 C25 1.518(13) . ? C22 C23 1.527(13) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.543(9) . ? C27 C30 1.497(9) . ? C27 C29 1.498(10) . ? C27 C28 1.549(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.550(9) . ? C32 C34 1.507(10) . ? C32 C35 1.516(10) . ? C32 C33 1.534(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.352(9) . ? C36 H36 0.9500 . ? C37 C38 1.369(9) . ? C37 H37 0.9500 . ? C38 C39 1.372(10) . ? C38 H38 0.9500 . ? C39 C40 1.367(10) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.397(11) . ? C41 H41 0.9500 . ? C42 C43 1.325(13) . ? C42 H42 0.9500 . ? C43 C45 1.332(16) . ? C43 H43 0.9500 . ? C44 C45 1.418(14) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 O13 Pr1 O6 158.23(16) . . ? O13 Pr1 O2 100.65(17) . . ? O6 Pr1 O2 85.03(18) . . ? O13 Pr1 O9 84.61(17) . . ? O6 Pr1 O9 100.73(17) . . ? O2 Pr1 O9 150.8(2) . . ? O13 Pr1 O11 84.75(16) . . ? O6 Pr1 O11 77.42(16) . . ? O2 Pr1 O11 138.5(2) . . ? O9 Pr1 O11 70.2(2) . . ? O13 Pr1 O7 127.80(16) . . ? O6 Pr1 O7 73.93(16) . . ? O2 Pr1 O7 76.0(2) . . ? O9 Pr1 O7 78.2(2) . . ? O11 Pr1 O7 131.96(18) . . ? O13 Pr1 O4 78.28(17) . . ? O6 Pr1 O4 84.03(17) . . ? O2 Pr1 O4 70.37(18) . . ? O9 Pr1 O4 138.4(2) . . ? O11 Pr1 O4 70.64(19) . . ? O7 Pr1 O4 141.06(19) . . ? O13 Pr1 O8 75.94(15) . . ? O6 Pr1 O8 125.84(15) . . ? O2 Pr1 O8 79.47(17) . . ? O9 Pr1 O8 73.96(19) . . ? O11 Pr1 O8 140.59(17) . . ? O7 Pr1 O8 52.02(14) . . ? O4 Pr1 O8 135.45(18) . . ? O1 Zn1 O5 117.8(2) . . ? O1 Zn1 O3 109.1(2) . . ? O5 Zn1 O3 126.8(2) . . ? O1 Zn1 N1 103.3(2) . . ? O5 Zn1 N1 95.2(2) . . ? O3 Zn1 N1 97.4(2) . . ? O14 Zn2 O10 120.6(2) . . ? O14 Zn2 O12 127.3(2) . . ? O10 Zn2 O12 106.3(2) . . ? O14 Zn2 N2 96.8(2) . . ? O10 Zn2 N2 100.4(2) . . ? O12 Zn2 N2 97.0(2) . . ? C1 O1 Zn1 125.1(5) . . ? C1 O2 Pr1 154.6(6) . . ? C6 O3 Zn1 119.9(5) . . ? C6 O4 Pr1 154.7(5) . . ? C11 O5 Zn1 120.3(5) . . ? C11 O6 Pr1 153.6(5) . . ? C16 O7 Pr1 95.6(4) . . ? C16 O8 Pr1 91.6(4) . . ? C21 O9 Pr1 157.8(6) . . ? C21 O10 Zn2 125.5(5) . . ? C26 O11 Pr1 170.1(6) . . ? C26 O12 Zn2 115.0(5) . . ? C31 O13 Pr1 159.7(5) . . ? C31 O14 Zn2 126.9(4) . . ? C40 N1 C36 115.8(6) . . ? C40 N1 Zn1 123.3(5) . . ? C36 N1 Zn1 120.9(5) . . ? C44 N2 C41 118.0(7) . . ? C44 N2 Zn2 121.6(6) . . ? C41 N2 Zn2 120.4(5) . . ? O2 C1 O1 121.9(8) . . ? O2 C1 C2 119.7(8) . . ? O1 C1 C2 118.5(8) . . ? C3 C2 C4 104.9(16) . . ? C3 C2 C5 110.0(14) . . ? C4 C2 C5 107.3(14) . . ? C3 C2 C1 111.8(8) . . ? C4 C2 C1 108.6(10) . . ? C5 C2 C1 113.7(8) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 122.8(7) . . ? O4 C6 C7 119.4(7) . . ? O3 C6 C7 117.5(7) . . ? C8 C7 C6 107.2(6) . . ? C8 C7 C9 108.6(7) . . ? C6 C7 C9 112.4(6) . . ? C8 C7 C10 109.1(7) . . ? C6 C7 C10 110.0(7) . . ? C9 C7 C10 109.6(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 121.9(7) . . ? O6 C11 C12 121.9(7) . . ? O5 C11 C12 116.0(7) . . ? C13 C12 C14 109.2(13) . . ? C13 C12 C15 108.1(10) . . ? C14 C12 C15 108.6(11) . . ? C13 C12 C11 109.4(8) . . ? C14 C12 C11 111.0(8) . . ? C15 C12 C11 110.4(9) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 120.8(6) . . ? O7 C16 C17 120.3(7) . . ? O8 C16 C17 118.8(7) . . ? C20 C17 C18 110.3(9) . . ? C20 C17 C16 112.2(7) . . ? C18 C17 C16 110.8(8) . . ? C20 C17 C19 107.5(8) . . ? C18 C17 C19 109.5(8) . . ? C16 C17 C19 106.3(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 O9 124.1(8) . . ? O10 C21 C22 119.1(8) . . ? O9 C21 C22 116.9(8) . . ? C24 C22 C25 108.9(10) . . ? C24 C22 C23 113.2(11) . . ? C25 C22 C23 107.8(10) . . ? C24 C22 C21 108.5(8) . . ? C25 C22 C21 107.0(9) . . ? C23 C22 C21 111.3(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 122.0(7) . . ? O11 C26 C27 120.0(7) . . ? O12 C26 C27 117.9(7) . . ? C30 C27 C29 111.0(7) . . ? C30 C27 C26 109.3(6) . . ? C29 C27 C26 113.1(6) . . ? C30 C27 C28 109.5(6) . . ? C29 C27 C28 110.0(7) . . ? C26 C27 C28 103.7(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O13 C31 O14 122.8(6) . . ? O13 C31 C32 119.7(7) . . ? O14 C31 C32 117.4(6) . . ? C34 C32 C35 111.6(7) . . ? C34 C32 C33 109.8(6) . . ? C35 C32 C33 108.3(7) . . ? C34 C32 C31 110.5(6) . . ? C35 C32 C31 110.0(6) . . ? C33 C32 C31 106.5(6) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N1 C36 C37 124.2(7) . . ? N1 C36 H36 117.9 . . ? C37 C36 H36 117.9 . . ? C36 C37 C38 118.1(7) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C37 C38 C39 119.9(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 117.7(7) . . ? C40 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? N1 C40 C39 124.1(7) . . ? N1 C40 H40 118.0 . . ? C39 C40 H40 118.0 . . ? N2 C41 C42 127.2(8) . . ? N2 C41 H41 116.4 . . ? C42 C41 H41 116.4 . . ? C43 C42 C41 115.5(9) . . ? C43 C42 H42 122.2 . . ? C41 C42 H42 122.2 . . ? C42 C43 C45 118.0(10) . . ? C42 C43 H43 121.0 . . ? C45 C43 H43 121.0 . . ? N2 C44 C45 119.1(10) . . ? N2 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C43 C45 C44 121.9(11) . . ? C43 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.676 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.073 # start Validation Reply Form _vrf_PLAT220_7jn052aa ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.61 Ratio RESPONSE: silght disorder is present as seen from the large thermo parameters however no large Q-peaks were found near the ligand carbon atoms only located near the heaviest atoms (Zn and Ln). Therefore split occupancy modeling could not be done for the C-atoms ; _vrf_PLAT222_7jn052aa ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.14 Ratio RESPONSE: see above ; _vrf_PLAT241_7jn052aa ; PROBLEM: Check High Ueq as Compared to Neighbors for C45 RESPONSE: see above ; _vrf_PLAT242_7jn052aa ; PROBLEM: Check Low Ueq as Compared to Neighbors for C2 RESPONSE: see above ; # end Validation Reply Form #===END data_7ag031ss _database_code_depnum_ccdc_archive 'CCDC 753907' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NdZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H73 N2 Nd O14 Zn2' _chemical_formula_weight 1141.03 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' 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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.846(2) _cell_length_b 15.125(2) _cell_length_c 19.045(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5428.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8404 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.39 _exptl_crystal_description cube _exptl_crystal_colour blue _exptl_crystal_size_max 0.431 _exptl_crystal_size_mid 0.418 _exptl_crystal_size_min 0.314 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2356 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_correction_T_max 0.555 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38472 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.39 _reflns_number_total 9871 _reflns_number_gt 9665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+2.5402P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.0(1) _refine_ls_number_reflns 9871 _refine_ls_number_parameters 597 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Nd1 Nd 0.244972(7) 0.013843(8) 0.245343(13) 0.02417(5) Uani 1 1 d . . . Zn1 Zn 0.315137(19) -0.10090(2) 0.422870(19) 0.03130(8) Uani 1 1 d . . . Zn2 Zn 0.347914(19) 0.13061(2) 0.081047(19) 0.03106(8) Uani 1 1 d . . . O1 O 0.24368(13) -0.02370(18) 0.46372(16) 0.0409(6) Uani 1 1 d . . . O2 O 0.19661(14) 0.01855(17) 0.36295(13) 0.0419(6) Uani 1 1 d . . . O3 O 0.39980(12) -0.03076(14) 0.40134(12) 0.0377(5) Uani 1 1 d . . . O4 O 0.33886(13) 0.05400(17) 0.32871(13) 0.0429(6) Uani 1 1 d . . . O5 O 0.28176(14) -0.20565(16) 0.37402(11) 0.0429(6) Uani 1 1 d . . . O6 O 0.27738(13) -0.13517(15) 0.27317(12) 0.0382(5) Uani 1 1 d . . . O7 O 0.13524(12) -0.07352(13) 0.24038(15) 0.0415(5) Uani 1 1 d . . . O8 O 0.12210(12) 0.06943(14) 0.22181(12) 0.0372(5) Uani 1 1 d . . . O9 O 0.22645(19) -0.00269(18) 0.11968(13) 0.0481(7) Uani 1 1 d . . . O10 O 0.27472(14) 0.06762(17) 0.02997(12) 0.0416(5) Uani 1 1 d . . . O11 O 0.35931(15) -0.00107(16) 0.18686(15) 0.0476(6) Uani 1 1 d . . . O12 O 0.42412(13) 0.04427(15) 0.09861(12) 0.0393(5) Uani 1 1 d . . . O13 O 0.25962(11) 0.16784(15) 0.22018(12) 0.0350(5) Uani 1 1 d . . . O14 O 0.32282(13) 0.23277(15) 0.13669(12) 0.0401(5) Uani 1 1 d . . . N1 N 0.35507(13) -0.16765(17) 0.50838(13) 0.0295(5) Uani 1 1 d . . . N2 N 0.39688(15) 0.19959(18) 0.00092(15) 0.0371(6) Uani 1 1 d . . . C1 C 0.20453(17) 0.0261(2) 0.42738(17) 0.0307(7) Uani 1 1 d . . . C2 C 0.1639(2) 0.0978(2) 0.46719(19) 0.0433(8) Uani 1 1 d . . . C3 C 0.1098(9) 0.0589(6) 0.5058(9) 0.316(12) Uani 1 1 d . . . H3A H 0.1151 -0.0055 0.5045 0.474 Uiso 1 1 calc R . . H3B H 0.0638 0.0755 0.4857 0.474 Uiso 1 1 calc R . . H3C H 0.1123 0.0794 0.5546 0.474 Uiso 1 1 calc R . . C4 C 0.2101(7) 0.1429(11) 0.5123(11) 0.361(15) Uani 1 1 d . . . H4A H 0.1846 0.1603 0.5549 0.542 Uiso 1 1 calc . . . H4B H 0.2283 0.1959 0.4886 0.542 Uiso 1 1 calc . . . H4C H 0.2499 0.1042 0.5248 0.542 Uiso 1 1 calc . . . C5 C 0.1314(7) 0.1595(7) 0.4208(4) 0.228(7) Uani 1 1 d . . . H5A H 0.0943 0.1298 0.3936 0.343 Uiso 1 1 calc R . . H5B H 0.1673 0.1835 0.3887 0.343 Uiso 1 1 calc R . . H5C H 0.1104 0.2078 0.4480 0.343 Uiso 1 1 calc R . . C6 C 0.39273(17) 0.0388(2) 0.36278(16) 0.0307(7) Uani 1 1 d . . . C7 C 0.45287(18) 0.1068(2) 0.36444(17) 0.0343(7) Uani 1 1 d . . . C8 C 0.4278(2) 0.1811(2) 0.4130(2) 0.0489(9) Uani 1 1 d . . . H8A H 0.4189 0.1571 0.4600 0.073 Uiso 1 1 calc R . . H8B H 0.3840 0.2069 0.3944 0.073 Uiso 1 1 calc R . . H8C H 0.4645 0.2269 0.4158 0.073 Uiso 1 1 calc R . . C9 C 0.52204(19) 0.0684(3) 0.3931(2) 0.0500(9) Uani 1 1 d . . . H9A H 0.5147 0.0481 0.4414 0.075 Uiso 1 1 calc R . . H9B H 0.5589 0.1141 0.3925 0.075 Uiso 1 1 calc R . . H9C H 0.5369 0.0185 0.3638 0.075 Uiso 1 1 calc R . . C10 C 0.4651(2) 0.1428(3) 0.29010(19) 0.0468(9) Uani 1 1 d . . . H10A H 0.4986 0.1922 0.2920 0.070 Uiso 1 1 calc R . . H10B H 0.4199 0.1632 0.2705 0.070 Uiso 1 1 calc R . . H10C H 0.4845 0.0958 0.2603 0.070 Uiso 1 1 calc R . . C11 C 0.26887(16) -0.2032(2) 0.30847(17) 0.0294(6) Uani 1 1 d . . . C12 C 0.24602(17) -0.2903(2) 0.2744(2) 0.0369(8) Uani 1 1 d . . . C13 C 0.3133(3) -0.3421(4) 0.2654(4) 0.108(3) Uani 1 1 d . . . H13A H 0.3034 -0.3959 0.2385 0.163 Uiso 1 1 calc R . . H13B H 0.3322 -0.3582 0.3117 0.163 Uiso 1 1 calc R . . H13C H 0.3483 -0.3061 0.2403 0.163 Uiso 1 1 calc R . . C14 C 0.1940(5) -0.3367(5) 0.3184(4) 0.146(4) Uani 1 1 d . . . H14A H 0.1528 -0.2984 0.3261 0.219 Uiso 1 1 calc R . . H14B H 0.2157 -0.3515 0.3636 0.219 Uiso 1 1 calc R . . H14C H 0.1789 -0.3910 0.2947 0.219 Uiso 1 1 calc R . . C15 C 0.2157(4) -0.2730(3) 0.2019(3) 0.093(2) Uani 1 1 d . . . H15A H 0.1765 -0.2307 0.2055 0.140 Uiso 1 1 calc R . . H15B H 0.1982 -0.3285 0.1819 0.140 Uiso 1 1 calc R . . H15C H 0.2528 -0.2486 0.1715 0.140 Uiso 1 1 calc R . . C16 C 0.09644(18) -0.0078(2) 0.22648(16) 0.0348(7) Uani 1 1 d . . . C17 C 0.0166(2) -0.0217(2) 0.2159(2) 0.0433(8) Uani 1 1 d . . . C18 C 0.0021(2) -0.1163(3) 0.1930(3) 0.0670(13) Uani 1 1 d . . . H18A H -0.0491 -0.1250 0.1873 0.100 Uiso 1 1 calc R . . H18B H 0.0202 -0.1573 0.2286 0.100 Uiso 1 1 calc R . . H18C H 0.0260 -0.1277 0.1481 0.100 Uiso 1 1 calc R . . C19 C -0.0174(2) -0.0028(3) 0.2881(2) 0.0529(10) Uani 1 1 d . . . H19A H -0.0100 0.0594 0.3005 0.079 Uiso 1 1 calc R . . H19B H 0.0046 -0.0406 0.3237 0.079 Uiso 1 1 calc R . . H19C H -0.0684 -0.0152 0.2859 0.079 Uiso 1 1 calc R . . C20 C -0.0132(2) 0.0422(4) 0.1615(2) 0.0665(12) Uani 1 1 d . . . H20A H -0.0107 0.1028 0.1797 0.100 Uiso 1 1 calc R . . H20B H -0.0628 0.0271 0.1516 0.100 Uiso 1 1 calc R . . H20C H 0.0146 0.0380 0.1182 0.100 Uiso 1 1 calc R . . C21 C 0.23641(19) 0.0078(2) 0.0560(2) 0.0320(8) Uani 1 1 d . . . C22 C 0.1969(2) -0.0526(2) 0.00383(18) 0.0433(8) Uani 1 1 d . . . C23 C 0.1642(4) -0.1295(4) 0.0422(3) 0.106(3) Uani 1 1 d . . . H23A H 0.2018 -0.1687 0.0594 0.159 Uiso 1 1 calc R . . H23B H 0.1332 -0.1624 0.0101 0.159 Uiso 1 1 calc R . . H23C H 0.1363 -0.1076 0.0819 0.159 Uiso 1 1 calc R . . C24 C 0.1417(4) 0.0027(4) -0.0342(4) 0.104(2) Uani 1 1 d . . . H24A H 0.1047 0.0208 -0.0010 0.156 Uiso 1 1 calc R . . H24B H 0.1203 -0.0325 -0.0719 0.156 Uiso 1 1 calc R . . H24C H 0.1643 0.0552 -0.0542 0.156 Uiso 1 1 calc R . . C25 C 0.2507(3) -0.0841(5) -0.0499(3) 0.0862(19) Uani 1 1 d . . . H25A H 0.2638 -0.0348 -0.0807 0.129 Uiso 1 1 calc R . . H25B H 0.2299 -0.1318 -0.0780 0.129 Uiso 1 1 calc R . . H25C H 0.2931 -0.1060 -0.0257 0.129 Uiso 1 1 calc R . . C26 C 0.40978(16) -0.01107(19) 0.14660(17) 0.0281(6) Uani 1 1 d . . . C27 C 0.45549(17) -0.09493(19) 0.15214(16) 0.0327(7) Uani 1 1 d . . . C28 C 0.4160(2) -0.1642(2) 0.1085(2) 0.0523(10) Uani 1 1 d . . . H28A H 0.3666 -0.1679 0.1243 0.078 Uiso 1 1 calc R . . H28B H 0.4389 -0.2219 0.1144 0.078 Uiso 1 1 calc R . . H28C H 0.4172 -0.1473 0.0588 0.078 Uiso 1 1 calc R . . C29 C 0.52926(19) -0.0803(3) 0.1216(2) 0.0525(10) Uani 1 1 d . . . H29A H 0.5251 -0.0577 0.0736 0.079 Uiso 1 1 calc R . . H29B H 0.5552 -0.1364 0.1211 0.079 Uiso 1 1 calc R . . H29C H 0.5550 -0.0373 0.1506 0.079 Uiso 1 1 calc R . . C30 C 0.4602(2) -0.1238(2) 0.22847(18) 0.0460(9) Uani 1 1 d . . . H30A H 0.4847 -0.0782 0.2558 0.069 Uiso 1 1 calc R . . H30B H 0.4866 -0.1794 0.2316 0.069 Uiso 1 1 calc R . . H30C H 0.4122 -0.1323 0.2472 0.069 Uiso 1 1 calc R . . C31 C 0.28383(16) 0.23431(19) 0.19111(15) 0.0281(6) Uani 1 1 d . . . C32 C 0.26955(19) 0.3261(2) 0.22302(17) 0.0347(7) Uani 1 1 d . . . C33 C 0.3335(2) 0.3469(3) 0.2690(2) 0.0505(9) Uani 1 1 d . . . H33A H 0.3768 0.3449 0.2405 0.076 Uiso 1 1 calc R . . H33B H 0.3368 0.3032 0.3068 0.076 Uiso 1 1 calc R . . H33C H 0.3281 0.4061 0.2893 0.076 Uiso 1 1 calc R . . C34 C 0.2022(2) 0.3246(3) 0.2682(2) 0.0512(10) Uani 1 1 d . . . H34A H 0.1956 0.3825 0.2903 0.077 Uiso 1 1 calc R . . H34B H 0.2069 0.2792 0.3046 0.077 Uiso 1 1 calc R . . H34C H 0.1612 0.3111 0.2385 0.077 Uiso 1 1 calc R . . C35 C 0.2638(2) 0.3958(2) 0.1648(2) 0.0493(10) Uani 1 1 d . . . H35A H 0.2557 0.4540 0.1859 0.074 Uiso 1 1 calc R . . H35B H 0.2242 0.3810 0.1337 0.074 Uiso 1 1 calc R . . H35C H 0.3080 0.3969 0.1377 0.074 Uiso 1 1 calc R . . C36 C 0.40548(19) -0.1302(2) 0.54854(17) 0.0379(7) Uani 1 1 d . . . H36 H 0.4221 -0.0729 0.5363 0.045 Uiso 1 1 calc R . . C37 C 0.43392(19) -0.1706(2) 0.60614(18) 0.0419(8) Uani 1 1 d . . . H37 H 0.4700 -0.1424 0.6327 0.050 Uiso 1 1 calc R . . C38 C 0.40942(18) -0.2533(2) 0.62521(17) 0.0375(7) Uani 1 1 d . . . H38 H 0.4278 -0.2822 0.6656 0.045 Uiso 1 1 calc R . . C39 C 0.35809(18) -0.2932(2) 0.58485(19) 0.0371(7) Uani 1 1 d . . . H39 H 0.3405 -0.3501 0.5968 0.045 Uiso 1 1 calc R . . C40 C 0.33245(17) -0.2485(2) 0.52620(16) 0.0325(7) Uani 1 1 d . . . H40 H 0.2976 -0.2765 0.4978 0.039 Uiso 1 1 calc R . . C41 C 0.44446(19) 0.1587(2) -0.03816(17) 0.0399(8) Uani 1 1 d . . . H41 H 0.4528 0.0979 -0.0290 0.048 Uiso 1 1 calc R . . C42 C 0.4830(2) 0.1978(3) -0.09141(19) 0.0497(9) Uani 1 1 d . . . H42 H 0.5188 0.1662 -0.1159 0.060 Uiso 1 1 calc R . . C43 C 0.4678(4) 0.2821(4) -0.1072(4) 0.120(3) Uani 1 1 d . . . H43 H 0.4944 0.3128 -0.1419 0.144 Uiso 1 1 calc R . . C44 C 0.3807(3) 0.2816(3) -0.0160(3) 0.091(2) Uani 1 1 d . . . H44 H 0.3463 0.3121 0.0113 0.110 Uiso 1 1 calc R . . C45 C 0.4119(4) 0.3247(3) -0.0717(4) 0.128(3) Uani 1 1 d . . . H45 H 0.3960 0.3816 -0.0859 0.154 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03269(8) 0.01968(7) 0.02013(7) 0.00078(9) -0.00056(7) -0.00096(5) Zn1 0.04110(19) 0.02585(17) 0.02693(16) 0.00425(14) 0.00196(15) -0.00100(14) Zn2 0.03712(18) 0.02557(16) 0.03050(17) 0.00430(14) 0.00345(15) 0.00239(14) O1 0.0538(17) 0.0350(16) 0.0338(15) 0.0037(12) 0.0049(10) 0.0078(10) O2 0.0436(15) 0.0533(16) 0.0288(13) -0.0034(10) 0.0021(11) 0.0016(11) O3 0.0409(12) 0.0337(12) 0.0384(13) 0.0102(10) 0.0055(10) -0.0038(9) O4 0.0452(14) 0.0454(14) 0.0381(13) 0.0074(11) -0.0100(11) -0.0101(11) O5 0.0655(16) 0.0341(13) 0.0291(12) 0.0015(10) -0.0074(11) -0.0078(12) O6 0.0522(14) 0.0248(11) 0.0377(12) 0.0043(9) -0.0013(10) 0.0001(10) O7 0.0479(12) 0.0273(10) 0.0493(13) 0.0077(12) -0.0051(13) -0.0060(9) O8 0.0362(11) 0.0291(11) 0.0462(13) 0.0056(9) -0.0048(9) -0.0045(9) O9 0.0709(19) 0.0490(15) 0.0244(14) -0.0049(10) -0.0030(13) -0.0096(13) O10 0.0500(14) 0.0400(14) 0.0348(12) 0.0007(10) 0.0018(11) -0.0058(11) O11 0.0534(16) 0.0404(14) 0.0491(15) 0.0103(12) 0.0142(13) 0.0122(11) O12 0.0432(13) 0.0325(11) 0.0420(13) 0.0110(10) 0.0037(10) 0.0063(10) O13 0.0432(12) 0.0254(12) 0.0364(12) 0.0019(9) -0.0015(9) -0.0027(9) O14 0.0545(14) 0.0283(12) 0.0377(12) 0.0006(10) 0.0101(11) 0.0008(10) N1 0.0339(13) 0.0261(13) 0.0286(13) 0.0027(10) 0.0007(10) -0.0018(10) N2 0.0438(15) 0.0306(15) 0.0370(14) 0.0078(12) 0.0104(12) 0.0085(12) C1 0.0360(17) 0.0313(15) 0.0248(15) -0.0002(13) 0.0075(13) -0.0057(12) C2 0.056(2) 0.0338(18) 0.0400(19) -0.0056(15) 0.0062(17) 0.0087(15) C3 0.42(2) 0.089(6) 0.44(2) 0.026(9) 0.393(19) 0.062(9) C4 0.196(11) 0.309(18) 0.58(3) -0.38(2) -0.189(17) 0.162(13) C5 0.408(17) 0.207(10) 0.071(4) -0.003(6) 0.002(8) 0.240(12) C6 0.0369(17) 0.0289(16) 0.0264(15) 0.0006(13) 0.0013(13) -0.0039(13) C7 0.0392(17) 0.0318(17) 0.0320(16) 0.0051(13) -0.0026(14) -0.0034(14) C8 0.061(2) 0.0347(18) 0.051(2) -0.0073(16) -0.0058(19) -0.0029(16) C9 0.0403(19) 0.048(2) 0.062(2) 0.0075(18) -0.0102(17) -0.0047(16) C10 0.054(2) 0.045(2) 0.041(2) 0.0125(16) -0.0010(16) -0.0159(17) C11 0.0325(15) 0.0233(15) 0.0323(16) -0.0011(13) 0.0061(13) 0.0036(12) C12 0.0439(19) 0.0254(18) 0.0416(18) -0.0064(15) 0.0042(13) -0.0061(13) C13 0.088(4) 0.055(3) 0.182(7) -0.057(4) -0.039(4) 0.027(3) C14 0.184(8) 0.149(7) 0.105(5) -0.056(5) 0.067(5) -0.133(6) C15 0.158(6) 0.050(3) 0.072(4) -0.025(3) -0.044(4) 0.003(4) C16 0.0359(17) 0.0366(18) 0.0320(19) 0.0034(12) -0.0009(12) -0.0077(13) C17 0.0355(19) 0.042(2) 0.052(2) -0.0019(16) 0.0009(16) -0.0135(15) C18 0.050(2) 0.066(3) 0.085(3) -0.023(2) 0.010(2) -0.029(2) C19 0.049(2) 0.052(2) 0.058(3) 0.0021(19) 0.007(2) 0.0000(18) C20 0.039(2) 0.099(4) 0.061(3) 0.013(3) -0.014(2) -0.014(2) C21 0.0373(18) 0.0321(18) 0.0264(19) -0.0047(13) -0.0041(14) 0.0078(14) C22 0.058(2) 0.041(2) 0.0312(17) -0.0078(15) -0.0047(15) -0.0033(17) C23 0.169(7) 0.094(4) 0.055(3) -0.014(3) -0.005(3) -0.078(5) C24 0.106(5) 0.100(5) 0.107(5) -0.032(4) -0.074(4) 0.013(4) C25 0.109(5) 0.093(5) 0.057(3) -0.044(3) 0.002(2) 0.001(3) C26 0.0279(15) 0.0268(15) 0.0297(15) 0.0012(12) -0.0003(13) 0.0004(11) C27 0.0395(17) 0.0264(15) 0.0323(16) 0.0034(12) 0.0033(13) 0.0050(12) C28 0.066(3) 0.0310(18) 0.060(2) -0.0041(17) -0.0129(19) 0.0025(17) C29 0.039(2) 0.048(2) 0.071(3) 0.0137(19) 0.0078(18) 0.0138(16) C30 0.057(2) 0.0407(19) 0.040(2) 0.0088(14) -0.0036(16) 0.0133(16) C31 0.0339(16) 0.0235(15) 0.0270(14) 0.0020(12) -0.0049(13) -0.0020(12) C32 0.0519(19) 0.0222(15) 0.0301(17) -0.0024(12) -0.0021(13) -0.0008(14) C33 0.062(2) 0.040(2) 0.050(2) -0.0113(16) -0.0142(17) -0.0042(17) C34 0.055(2) 0.047(2) 0.052(2) -0.0159(17) 0.0062(17) -0.0014(17) C35 0.080(3) 0.0215(17) 0.046(2) 0.0017(15) -0.0072(19) 0.0042(16) C36 0.0462(19) 0.0316(17) 0.0358(17) 0.0014(14) 0.0028(14) -0.0100(14) C37 0.0397(18) 0.046(2) 0.0395(18) 0.0005(15) -0.0058(15) -0.0086(15) C38 0.0451(19) 0.0349(17) 0.0324(16) 0.0052(13) -0.0025(14) 0.0058(14) C39 0.0458(18) 0.0279(15) 0.0377(16) 0.0089(14) -0.0017(15) -0.0029(13) C40 0.0376(17) 0.0312(16) 0.0287(15) 0.0036(13) -0.0003(13) -0.0055(13) C41 0.052(2) 0.0350(18) 0.0324(16) 0.0018(14) 0.0032(15) 0.0119(15) C42 0.054(2) 0.056(2) 0.0384(19) 0.0049(17) 0.0145(16) 0.0137(18) C43 0.167(6) 0.064(3) 0.128(5) 0.031(3) 0.114(5) 0.016(4) C44 0.133(5) 0.040(2) 0.100(4) 0.024(3) 0.081(4) 0.026(3) C45 0.189(7) 0.051(3) 0.145(6) 0.047(4) 0.117(6) 0.040(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O13 2.394(2) . ? Nd1 O6 2.395(2) . ? Nd1 O2 2.419(2) . ? Nd1 O9 2.431(3) . ? Nd1 O11 2.436(3) . ? Nd1 O4 2.454(2) . ? Nd1 O7 2.456(2) . ? Nd1 O8 2.504(2) . ? Zn1 O5 1.942(2) . ? Zn1 O1 1.945(2) . ? Zn1 O3 1.959(2) . ? Zn1 N1 2.059(3) . ? Zn2 O14 1.932(2) . ? Zn2 O10 1.938(2) . ? Zn2 O12 1.970(2) . ? Zn2 N2 2.066(3) . ? O1 C1 1.261(4) . ? O2 C1 1.241(4) . ? O3 C6 1.290(4) . ? O4 C6 1.227(4) . ? O5 C11 1.272(4) . ? O6 C11 1.240(4) . ? O7 C16 1.262(4) . ? O8 C16 1.267(4) . ? O9 C21 1.238(5) . ? O10 C21 1.259(4) . ? O11 C26 1.231(4) . ? O12 C26 1.268(4) . ? O13 C31 1.235(4) . ? O14 C31 1.271(4) . ? N1 C40 1.339(4) . ? N1 C36 1.345(4) . ? N2 C44 1.317(5) . ? N2 C41 1.319(4) . ? C1 C2 1.530(5) . ? C2 C3 1.388(9) . ? C2 C4 1.401(11) . ? C2 C5 1.424(8) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(4) . ? C7 C9 1.528(5) . ? C7 C8 1.531(5) . ? C7 C10 1.534(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(5) . ? C12 C14 1.467(6) . ? C12 C13 1.501(6) . ? C12 C15 1.517(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.533(5) . ? C17 C18 1.522(5) . ? C17 C20 1.525(6) . ? C17 C19 1.543(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.541(5) . ? C22 C23 1.506(6) . ? C22 C25 1.517(6) . ? C22 C24 1.519(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.537(4) . ? C27 C30 1.520(4) . ? C27 C29 1.523(5) . ? C27 C28 1.531(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.539(4) . ? C32 C33 1.523(5) . ? C32 C34 1.533(5) . ? C32 C35 1.534(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.366(5) . ? C36 H36 0.9500 . ? C37 C38 1.382(5) . ? C37 H37 0.9500 . ? C38 C39 1.375(5) . ? C38 H38 0.9500 . ? C39 C40 1.392(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.380(5) . ? C41 H41 0.9500 . ? C42 C43 1.342(7) . ? C42 H42 0.9500 . ? C43 C45 1.407(7) . ? C43 H43 0.9500 . ? C44 C45 1.377(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 O13 Nd1 O6 158.54(8) . . ? O13 Nd1 O2 101.55(8) . . ? O6 Nd1 O2 85.34(9) . . ? O13 Nd1 O9 85.39(9) . . ? O6 Nd1 O9 99.07(9) . . ? O2 Nd1 O9 149.35(11) . . ? O13 Nd1 O11 84.06(8) . . ? O6 Nd1 O11 77.79(8) . . ? O2 Nd1 O11 139.40(10) . . ? O9 Nd1 O11 70.58(11) . . ? O13 Nd1 O4 78.79(8) . . ? O6 Nd1 O4 84.60(8) . . ? O2 Nd1 O4 70.44(9) . . ? O9 Nd1 O4 139.99(10) . . ? O11 Nd1 O4 71.39(10) . . ? O13 Nd1 O7 127.80(7) . . ? O6 Nd1 O7 73.55(8) . . ? O2 Nd1 O7 74.59(9) . . ? O9 Nd1 O7 77.64(10) . . ? O11 Nd1 O7 132.64(9) . . ? O4 Nd1 O7 139.93(8) . . ? O13 Nd1 O8 75.18(7) . . ? O6 Nd1 O8 126.26(8) . . ? O2 Nd1 O8 78.90(8) . . ? O9 Nd1 O8 74.07(10) . . ? O11 Nd1 O8 140.11(8) . . ? O4 Nd1 O8 134.39(8) . . ? O7 Nd1 O8 52.77(7) . . ? O5 Zn1 O1 117.21(12) . . ? O5 Zn1 O3 127.24(10) . . ? O1 Zn1 O3 108.81(11) . . ? O5 Zn1 N1 95.59(10) . . ? O1 Zn1 N1 103.36(12) . . ? O3 Zn1 N1 97.67(10) . . ? O14 Zn2 O10 119.61(11) . . ? O14 Zn2 O12 127.98(10) . . ? O10 Zn2 O12 106.16(11) . . ? O14 Zn2 N2 96.35(10) . . ? O10 Zn2 N2 101.27(11) . . ? O12 Zn2 N2 97.73(10) . . ? C1 O1 Zn1 123.0(2) . . ? C1 O2 Nd1 150.8(2) . . ? C6 O3 Zn1 118.5(2) . . ? C6 O4 Nd1 153.2(2) . . ? C11 O5 Zn1 120.6(2) . . ? C11 O6 Nd1 150.3(2) . . ? C16 O7 Nd1 94.13(18) . . ? C16 O8 Nd1 91.77(19) . . ? C21 O9 Nd1 158.4(3) . . ? C21 O10 Zn2 124.3(2) . . ? C26 O11 Nd1 168.4(3) . . ? C26 O12 Zn2 113.9(2) . . ? C31 O13 Nd1 157.6(2) . . ? C31 O14 Zn2 127.1(2) . . ? C40 N1 C36 117.8(3) . . ? C40 N1 Zn1 122.1(2) . . ? C36 N1 Zn1 120.1(2) . . ? C44 N2 C41 117.4(3) . . ? C44 N2 Zn2 123.6(3) . . ? C41 N2 Zn2 118.9(2) . . ? O2 C1 O1 123.9(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 C2 116.4(3) . . ? C3 C2 C4 109.8(12) . . ? C3 C2 C5 107.0(9) . . ? C4 C2 C5 109.2(10) . . ? C3 C2 C1 109.3(4) . . ? C4 C2 C1 109.7(5) . . ? C5 C2 C1 111.9(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 122.7(3) . . ? O4 C6 C7 119.9(3) . . ? O3 C6 C7 117.4(3) . . ? C9 C7 C6 112.6(3) . . ? C9 C7 C8 109.1(3) . . ? C6 C7 C8 106.1(3) . . ? C9 C7 C10 109.7(3) . . ? C6 C7 C10 109.3(3) . . ? C8 C7 C10 110.1(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.1(3) . . ? O6 C11 C12 121.4(3) . . ? O5 C11 C12 116.4(3) . . ? C14 C12 C13 112.3(6) . . ? C14 C12 C15 110.5(5) . . ? C13 C12 C15 107.8(4) . . ? C14 C12 C11 111.0(4) . . ? C13 C12 C11 105.1(3) . . ? C15 C12 C11 110.1(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 121.3(3) . . ? O7 C16 C17 119.2(3) . . ? O8 C16 C17 119.4(3) . . ? C18 C17 C20 109.6(4) . . ? C18 C17 C16 110.0(3) . . ? C20 C17 C16 111.4(3) . . ? C18 C17 C19 110.8(3) . . ? C20 C17 C19 109.6(3) . . ? C16 C17 C19 105.4(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 124.4(3) . . ? O9 C21 C22 118.9(3) . . ? O10 C21 C22 116.7(3) . . ? C23 C22 C25 111.0(5) . . ? C23 C22 C24 112.0(5) . . ? C25 C22 C24 108.0(5) . . ? C23 C22 C21 110.1(3) . . ? C25 C22 C21 107.4(4) . . ? C24 C22 C21 108.2(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 122.2(3) . . ? O11 C26 C27 119.5(3) . . ? O12 C26 C27 118.3(3) . . ? C30 C27 C29 110.7(3) . . ? C30 C27 C28 110.5(3) . . ? C29 C27 C28 109.6(3) . . ? C30 C27 C26 109.6(3) . . ? C29 C27 C26 111.4(3) . . ? C28 C27 C26 104.8(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O13 C31 O14 124.3(3) . . ? O13 C31 C32 119.5(3) . . ? O14 C31 C32 116.1(3) . . ? C33 C32 C34 109.6(3) . . ? C33 C32 C35 109.2(3) . . ? C34 C32 C35 111.0(3) . . ? C33 C32 C31 106.0(3) . . ? C34 C32 C31 110.7(3) . . ? C35 C32 C31 110.3(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N1 C36 C37 123.0(3) . . ? N1 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C36 C37 C38 119.1(3) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C39 C38 C37 119.0(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 118.7(3) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N1 C40 C39 122.4(3) . . ? N1 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? N2 C41 C42 124.8(3) . . ? N2 C41 H41 117.6 . . ? C42 C41 H41 117.6 . . ? C43 C42 C41 117.4(4) . . ? C43 C42 H42 121.3 . . ? C41 C42 H42 121.3 . . ? C42 C43 C45 119.1(4) . . ? C42 C43 H43 120.4 . . ? C45 C43 H43 120.4 . . ? N2 C44 C45 122.4(4) . . ? N2 C44 H44 118.8 . . ? C45 C44 H44 118.8 . . ? C44 C45 C43 118.2(5) . . ? C44 C45 H45 120.9 . . ? C43 C45 H45 120.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.809 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.070 # start Validation Reply Form _vrf_PLAT213_7ag031ss ; PROBLEM: Atom C3 has ADP max/min Ratio ..... 5.70 prola RESPONSE: No high numbered Q-peaks were found near the ligands for possible modeling (Q-peaks were only located near the heaviest atoms Zn and Ln) therefore no split occupancy could be done ; _vrf_PLAT220_7ag031ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT222_7ag031ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT242_7ag031ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C2 RESPONSE: see above ; # end Validation Reply Form #===END data_7jy031ss _database_code_depnum_ccdc_archive 'CCDC 753908' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SmZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H73 N2 O14 Sm Zn2' _chemical_formula_weight 1147.14 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' 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' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.856(2) _cell_length_b 15.096(2) _cell_length_c 18.999(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5407.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.279 _exptl_crystal_size_mid 0.257 _exptl_crystal_size_min 0.236 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2364 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.622 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43539 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.21 _reflns_number_total 12243 _reflns_number_gt 11190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+1.7327P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.00(1) _refine_ls_number_reflns 12243 _refine_ls_number_parameters 597 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Sm1 Sm 0.245091(9) 0.014181(10) 0.245303(16) 0.02298(5) Uani 1 1 d . . . Zn1 Zn 0.31433(3) -0.10083(3) 0.42183(3) 0.03117(11) Uani 1 1 d . . . Zn2 Zn 0.34801(2) 0.13096(3) 0.08216(3) 0.03017(10) Uani 1 1 d . . . O1 O 0.24258(16) -0.0244(2) 0.46190(19) 0.0402(8) Uani 1 1 d . . . O2 O 0.19738(17) 0.0226(2) 0.36141(16) 0.0416(8) Uani 1 1 d . . . O3 O 0.39913(15) -0.03024(18) 0.40031(15) 0.0364(7) Uani 1 1 d . . . O4 O 0.33897(16) 0.0540(2) 0.32646(16) 0.0422(8) Uani 1 1 d . . . O5 O 0.28122(18) -0.2064(2) 0.37327(15) 0.0435(8) Uani 1 1 d . . . O6 O 0.27631(17) -0.13382(19) 0.27332(17) 0.0391(7) Uani 1 1 d . . . O7 O 0.13636(14) -0.07196(17) 0.24223(19) 0.0394(6) Uani 1 1 d . . . O8 O 0.12346(14) 0.07066(18) 0.22178(15) 0.0341(7) Uani 1 1 d . . . O9 O 0.2256(2) -0.0035(2) 0.12095(17) 0.0442(8) Uani 1 1 d . . . O10 O 0.27453(17) 0.0677(2) 0.03179(16) 0.0399(7) Uani 1 1 d . . . O11 O 0.35754(18) -0.0025(2) 0.18660(18) 0.0447(8) Uani 1 1 d . . . O12 O 0.42402(16) 0.04440(19) 0.10011(16) 0.0376(7) Uani 1 1 d . . . O13 O 0.26045(14) 0.16619(19) 0.22039(15) 0.0336(7) Uani 1 1 d . . . O14 O 0.32343(17) 0.23309(19) 0.13736(15) 0.0389(7) Uani 1 1 d . . . N1 N 0.35401(17) -0.1672(2) 0.50745(17) 0.0287(7) Uani 1 1 d . . . N2 N 0.39665(19) 0.1991(2) 0.00154(19) 0.0368(8) Uani 1 1 d . . . C1 C 0.2036(2) 0.0274(3) 0.4262(2) 0.0298(9) Uani 1 1 d . . . C2 C 0.1633(3) 0.0981(3) 0.4672(2) 0.0388(10) Uani 1 1 d . . . C3 C 0.1169(9) 0.0588(7) 0.5145(9) 0.290(12) Uani 1 1 d . . . H3A H 0.1387 0.0052 0.5340 0.436 Uiso 1 1 calc R . . H3B H 0.0728 0.0431 0.4902 0.436 Uiso 1 1 calc R . . H3C H 0.1065 0.1003 0.5527 0.436 Uiso 1 1 calc R . . C4 C 0.2119(7) 0.1479(12) 0.5065(12) 0.333(15) Uani 1 1 d . . . H4A H 0.1914 0.1619 0.5526 0.500 Uiso 1 1 calc . . . H4B H 0.2228 0.2030 0.4815 0.500 Uiso 1 1 calc . . . H4C H 0.2556 0.1137 0.5130 0.500 Uiso 1 1 calc . . . C5 C 0.1234(7) 0.1565(7) 0.4217(5) 0.209(7) Uani 1 1 d . . . H5A H 0.0842 0.1236 0.4001 0.313 Uiso 1 1 calc R . . H5B H 0.1546 0.1796 0.3847 0.313 Uiso 1 1 calc R . . H5C H 0.1044 0.2059 0.4493 0.313 Uiso 1 1 calc R . . C6 C 0.3925(2) 0.0387(3) 0.3615(2) 0.0290(9) Uani 1 1 d . . . C7 C 0.4521(2) 0.1072(3) 0.3634(2) 0.0333(9) Uani 1 1 d . . . C8 C 0.4271(3) 0.1813(3) 0.4125(3) 0.0480(12) Uani 1 1 d . . . H8A H 0.4170 0.1567 0.4592 0.072 Uiso 1 1 calc R . . H8B H 0.3840 0.2084 0.3933 0.072 Uiso 1 1 calc R . . H8C H 0.4643 0.2264 0.4164 0.072 Uiso 1 1 calc R . . C9 C 0.5213(2) 0.0686(3) 0.3925(3) 0.0492(12) Uani 1 1 d . . . H9A H 0.5144 0.0508 0.4416 0.074 Uiso 1 1 calc R . . H9B H 0.5588 0.1134 0.3899 0.074 Uiso 1 1 calc R . . H9C H 0.5351 0.0168 0.3645 0.074 Uiso 1 1 calc R . . C10 C 0.4645(3) 0.1442(3) 0.2896(2) 0.0452(12) Uani 1 1 d . . . H10A H 0.4969 0.1949 0.2923 0.068 Uiso 1 1 calc R . . H10B H 0.4193 0.1634 0.2694 0.068 Uiso 1 1 calc R . . H10C H 0.4855 0.0982 0.2598 0.068 Uiso 1 1 calc R . . C11 C 0.2683(2) -0.2037(3) 0.3071(2) 0.0243(8) Uani 1 1 d . . . C12 C 0.2456(2) -0.2887(3) 0.2716(3) 0.0374(11) Uani 1 1 d . . . C13 C 0.3123(4) -0.3422(4) 0.2640(5) 0.098(3) Uani 1 1 d . . . H13A H 0.3013 -0.3984 0.2405 0.147 Uiso 1 1 calc R . . H13B H 0.3323 -0.3542 0.3106 0.147 Uiso 1 1 calc R . . H13C H 0.3468 -0.3090 0.2358 0.147 Uiso 1 1 calc R . . C14 C 0.1927(5) -0.3354(6) 0.3156(4) 0.131(4) Uani 1 1 d . . . H14A H 0.1522 -0.2962 0.3243 0.197 Uiso 1 1 calc R . . H14B H 0.2143 -0.3520 0.3606 0.197 Uiso 1 1 calc R . . H14C H 0.1765 -0.3888 0.2911 0.197 Uiso 1 1 calc R . . C15 C 0.2161(4) -0.2708(4) 0.1999(3) 0.085(2) Uani 1 1 d . . . H15A H 0.1745 -0.2321 0.2040 0.128 Uiso 1 1 calc R . . H15B H 0.2021 -0.3268 0.1779 0.128 Uiso 1 1 calc R . . H15C H 0.2522 -0.2417 0.1710 0.128 Uiso 1 1 calc R . . C16 C 0.0977(2) -0.0062(3) 0.2277(2) 0.0332(10) Uani 1 1 d . . . C17 C 0.0177(3) -0.0203(3) 0.2175(3) 0.0410(11) Uani 1 1 d . . . C18 C 0.0031(3) -0.1152(4) 0.1950(3) 0.0651(16) Uani 1 1 d . . . H18A H -0.0482 -0.1247 0.1917 0.098 Uiso 1 1 calc R . . H18B H 0.0233 -0.1560 0.2297 0.098 Uiso 1 1 calc R . . H18C H 0.0249 -0.1261 0.1490 0.098 Uiso 1 1 calc R . . C19 C -0.0156(3) -0.0012(3) 0.2899(3) 0.0531(13) Uani 1 1 d . . . H19A H -0.0080 0.0612 0.3022 0.080 Uiso 1 1 calc R . . H19B H 0.0067 -0.0391 0.3255 0.080 Uiso 1 1 calc R . . H19C H -0.0666 -0.0134 0.2881 0.080 Uiso 1 1 calc R . . C20 C -0.0122(3) 0.0441(4) 0.1633(3) 0.0638(16) Uani 1 1 d . . . H20A H -0.0082 0.1048 0.1811 0.096 Uiso 1 1 calc R . . H20B H -0.0622 0.0302 0.1546 0.096 Uiso 1 1 calc R . . H20C H 0.0145 0.0386 0.1193 0.096 Uiso 1 1 calc R . . C21 C 0.2351(2) 0.0083(3) 0.0570(2) 0.0311(10) Uani 1 1 d . . . C22 C 0.1964(3) -0.0512(3) 0.0043(2) 0.0414(11) Uani 1 1 d . . . C23 C 0.1600(5) -0.1265(5) 0.0420(3) 0.110(3) Uani 1 1 d . . . H23A H 0.1958 -0.1650 0.0635 0.165 Uiso 1 1 calc R . . H23B H 0.1318 -0.1607 0.0083 0.165 Uiso 1 1 calc R . . H23C H 0.1289 -0.1026 0.0787 0.165 Uiso 1 1 calc R . . C24 C 0.1437(5) 0.0054(5) -0.0356(5) 0.103(3) Uani 1 1 d . . . H24A H 0.1068 0.0263 -0.0033 0.155 Uiso 1 1 calc R . . H24B H 0.1220 -0.0298 -0.0732 0.155 Uiso 1 1 calc R . . H24C H 0.1683 0.0564 -0.0562 0.155 Uiso 1 1 calc R . . C25 C 0.2512(4) -0.0851(6) -0.0477(4) 0.092(3) Uani 1 1 d . . . H25A H 0.2623 -0.0384 -0.0818 0.138 Uiso 1 1 calc R . . H25B H 0.2322 -0.1369 -0.0725 0.138 Uiso 1 1 calc R . . H25C H 0.2944 -0.1019 -0.0223 0.138 Uiso 1 1 calc R . . C26 C 0.4088(2) -0.0115(3) 0.1470(2) 0.0281(8) Uani 1 1 d . . . C27 C 0.4546(2) -0.0952(3) 0.1525(2) 0.0320(9) Uani 1 1 d . . . C28 C 0.4161(3) -0.1654(3) 0.1086(3) 0.0542(13) Uani 1 1 d . . . H28A H 0.3668 -0.1700 0.1244 0.081 Uiso 1 1 calc R . . H28B H 0.4397 -0.2227 0.1145 0.081 Uiso 1 1 calc R . . H28C H 0.4172 -0.1483 0.0589 0.081 Uiso 1 1 calc R . . C29 C 0.5285(2) -0.0807(3) 0.1231(3) 0.0537(14) Uani 1 1 d . . . H29A H 0.5251 -0.0601 0.0743 0.081 Uiso 1 1 calc R . . H29B H 0.5550 -0.1366 0.1245 0.081 Uiso 1 1 calc R . . H29C H 0.5532 -0.0361 0.1515 0.081 Uiso 1 1 calc R . . C30 C 0.4590(3) -0.1247(3) 0.2292(2) 0.0436(11) Uani 1 1 d . . . H30A H 0.4835 -0.0792 0.2568 0.065 Uiso 1 1 calc R . . H30B H 0.4854 -0.1806 0.2321 0.065 Uiso 1 1 calc R . . H30C H 0.4110 -0.1333 0.2478 0.065 Uiso 1 1 calc R . . C31 C 0.2841(2) 0.2336(3) 0.1916(2) 0.0281(8) Uani 1 1 d . . . C32 C 0.2688(2) 0.3251(3) 0.2243(2) 0.0328(10) Uani 1 1 d . . . C33 C 0.3328(3) 0.3477(3) 0.2699(3) 0.0492(12) Uani 1 1 d . . . H33A H 0.3757 0.3479 0.2408 0.074 Uiso 1 1 calc R . . H33B H 0.3377 0.3035 0.3073 0.074 Uiso 1 1 calc R . . H33C H 0.3262 0.4064 0.2909 0.074 Uiso 1 1 calc R . . C34 C 0.2019(3) 0.3220(4) 0.2699(3) 0.0502(13) Uani 1 1 d . . . H34A H 0.1932 0.3807 0.2902 0.075 Uiso 1 1 calc R . . H34B H 0.2083 0.2788 0.3078 0.075 Uiso 1 1 calc R . . H34C H 0.1613 0.3046 0.2408 0.075 Uiso 1 1 calc R . . C35 C 0.2615(3) 0.3949(3) 0.1666(3) 0.0463(12) Uani 1 1 d . . . H35A H 0.2511 0.4525 0.1880 0.069 Uiso 1 1 calc R . . H35B H 0.2227 0.3782 0.1349 0.069 Uiso 1 1 calc R . . H35C H 0.3059 0.3986 0.1400 0.069 Uiso 1 1 calc R . . C36 C 0.4046(2) -0.1289(3) 0.5475(2) 0.0357(10) Uani 1 1 d . . . H36 H 0.4209 -0.0714 0.5351 0.043 Uiso 1 1 calc R . . C37 C 0.4333(2) -0.1694(3) 0.6051(2) 0.0426(11) Uani 1 1 d . . . H37 H 0.4696 -0.1410 0.6314 0.051 Uiso 1 1 calc R . . C38 C 0.4090(2) -0.2520(3) 0.6246(2) 0.0376(10) Uani 1 1 d . . . H38 H 0.4277 -0.2809 0.6650 0.045 Uiso 1 1 calc R . . C39 C 0.3574(2) -0.2917(3) 0.5845(2) 0.0362(9) Uani 1 1 d . . . H39 H 0.3395 -0.3484 0.5969 0.043 Uiso 1 1 calc R . . C40 C 0.3321(2) -0.2485(3) 0.5264(2) 0.0336(9) Uani 1 1 d . . . H40 H 0.2974 -0.2773 0.4983 0.040 Uiso 1 1 calc R . . C41 C 0.4440(2) 0.1581(3) -0.0373(2) 0.0395(10) Uani 1 1 d . . . H41 H 0.4520 0.0971 -0.0280 0.047 Uiso 1 1 calc R . . C42 C 0.4832(2) 0.1968(3) -0.0908(2) 0.0462(12) Uani 1 1 d . . . H42 H 0.5185 0.1646 -0.1157 0.055 Uiso 1 1 calc R . . C43 C 0.4687(5) 0.2822(5) -0.1061(4) 0.115(3) Uani 1 1 d . . . H43 H 0.4952 0.3125 -0.1412 0.139 Uiso 1 1 calc R . . C44 C 0.3816(4) 0.2820(4) -0.0150(4) 0.099(3) Uani 1 1 d . . . H44 H 0.3469 0.3126 0.0118 0.119 Uiso 1 1 calc R . . C45 C 0.4143(5) 0.3258(4) -0.0698(5) 0.141(5) Uani 1 1 d . . . H45 H 0.4004 0.3841 -0.0825 0.169 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.03139(9) 0.01911(8) 0.01845(8) 0.00059(12) 0.00026(10) -0.00110(7) Zn1 0.0399(3) 0.0269(2) 0.0267(2) 0.0027(2) 0.0013(2) -0.0001(2) Zn2 0.0369(2) 0.0252(2) 0.0284(2) 0.0041(2) 0.0047(2) 0.00263(19) O1 0.052(2) 0.037(2) 0.0319(19) 0.0003(15) 0.0034(14) 0.0064(14) O2 0.0440(19) 0.057(2) 0.0242(16) -0.0030(14) 0.0020(13) 0.0042(16) O3 0.0403(16) 0.0343(16) 0.0346(17) 0.0091(13) 0.0030(13) -0.0036(13) O4 0.0478(19) 0.0418(19) 0.0371(17) 0.0059(14) -0.0124(15) -0.0063(15) O5 0.068(2) 0.0337(18) 0.0285(17) 0.0034(13) -0.0062(15) -0.0091(16) O6 0.0496(18) 0.0225(15) 0.0453(17) 0.0054(13) -0.0012(14) 0.0046(13) O7 0.0454(15) 0.0272(14) 0.0457(16) 0.0096(17) -0.0029(17) -0.0064(11) O8 0.0317(15) 0.0293(15) 0.0415(17) 0.0049(12) -0.0034(11) -0.0044(12) O9 0.063(2) 0.047(2) 0.0226(17) -0.0052(13) -0.0019(16) -0.0072(16) O10 0.0449(17) 0.0431(19) 0.0317(16) 0.0011(14) 0.0014(14) -0.0042(15) O11 0.049(2) 0.0389(18) 0.046(2) 0.0059(15) 0.0143(16) 0.0106(14) O12 0.0409(17) 0.0316(15) 0.0404(18) 0.0114(13) 0.0052(13) 0.0070(13) O13 0.0433(17) 0.0236(15) 0.0340(16) 0.0036(11) -0.0035(12) -0.0028(12) O14 0.0550(19) 0.0283(16) 0.0334(16) 0.0002(13) 0.0103(14) 0.0003(14) N1 0.0316(18) 0.0245(17) 0.0301(18) 0.0023(14) 0.0029(14) -0.0008(14) N2 0.044(2) 0.0276(19) 0.038(2) 0.0078(15) 0.0096(16) 0.0071(16) C1 0.032(2) 0.030(2) 0.027(2) -0.0024(18) 0.0043(18) -0.0046(17) C2 0.050(3) 0.031(2) 0.035(2) -0.0043(18) 0.002(2) 0.006(2) C3 0.42(2) 0.090(7) 0.37(2) 0.056(10) 0.36(2) 0.092(11) C4 0.153(11) 0.299(19) 0.55(3) -0.37(2) -0.145(16) 0.119(13) C5 0.341(16) 0.218(12) 0.067(5) -0.010(7) -0.020(9) 0.228(12) C6 0.039(2) 0.029(2) 0.0190(19) -0.0019(16) 0.0028(17) 0.0016(18) C7 0.039(2) 0.033(2) 0.028(2) 0.0048(17) -0.0020(17) -0.0038(18) C8 0.061(3) 0.033(2) 0.050(3) -0.008(2) -0.005(2) -0.003(2) C9 0.042(3) 0.050(3) 0.056(3) 0.006(2) -0.012(2) -0.002(2) C10 0.049(3) 0.046(3) 0.040(3) 0.012(2) -0.001(2) -0.016(2) C11 0.0270(19) 0.0212(19) 0.025(2) 0.0027(15) 0.0085(15) 0.0041(15) C12 0.045(3) 0.030(2) 0.038(2) -0.0067(18) 0.0051(18) -0.0073(19) C13 0.086(5) 0.051(4) 0.157(8) -0.045(4) -0.031(5) 0.026(3) C14 0.159(8) 0.137(8) 0.097(6) -0.045(6) 0.058(6) -0.107(7) C15 0.143(7) 0.051(4) 0.061(4) -0.021(3) -0.043(4) -0.001(4) C16 0.036(2) 0.035(2) 0.028(3) 0.0032(16) 0.0009(15) -0.0070(17) C17 0.037(3) 0.037(3) 0.048(3) -0.002(2) 0.002(2) -0.013(2) C18 0.045(3) 0.065(4) 0.085(4) -0.025(3) 0.011(3) -0.028(3) C19 0.050(3) 0.056(3) 0.054(3) 0.005(3) 0.007(3) -0.001(3) C20 0.037(3) 0.094(4) 0.061(4) 0.015(3) -0.012(3) -0.010(3) C21 0.032(2) 0.036(2) 0.026(2) -0.0043(18) -0.0033(18) 0.0088(19) C22 0.054(3) 0.043(3) 0.028(2) -0.0101(19) -0.006(2) -0.004(2) C23 0.171(8) 0.114(7) 0.045(4) -0.013(4) -0.001(4) -0.091(6) C24 0.112(6) 0.092(6) 0.105(6) -0.026(4) -0.077(5) 0.011(4) C25 0.112(6) 0.102(6) 0.061(4) -0.053(4) 0.000(4) 0.003(4) C26 0.030(2) 0.025(2) 0.029(2) -0.0007(17) 0.0002(17) 0.0013(16) C27 0.041(2) 0.024(2) 0.031(2) 0.0018(17) 0.0015(18) 0.0070(17) C28 0.069(4) 0.035(3) 0.059(3) -0.005(2) -0.015(3) 0.002(2) C29 0.039(3) 0.049(3) 0.073(4) 0.017(3) 0.010(2) 0.016(2) C30 0.055(3) 0.038(2) 0.038(3) 0.0036(19) -0.003(2) 0.011(2) C31 0.037(2) 0.024(2) 0.0240(19) 0.0024(15) -0.0047(17) -0.0009(17) C32 0.048(2) 0.019(2) 0.031(2) -0.0017(15) -0.0013(17) 0.0008(17) C33 0.061(3) 0.040(3) 0.046(3) -0.010(2) -0.016(2) 0.000(2) C34 0.058(3) 0.047(3) 0.046(3) -0.017(2) 0.010(2) 0.002(2) C35 0.073(3) 0.022(2) 0.044(3) 0.0017(19) -0.007(2) 0.003(2) C36 0.043(2) 0.029(2) 0.035(2) 0.0029(18) 0.0037(18) -0.0088(19) C37 0.041(3) 0.047(3) 0.039(3) 0.002(2) -0.008(2) -0.008(2) C38 0.041(2) 0.035(2) 0.036(2) 0.0061(19) -0.0029(19) 0.0076(19) C39 0.043(2) 0.030(2) 0.035(2) 0.0080(19) 0.001(2) -0.0021(18) C40 0.040(2) 0.032(2) 0.029(2) 0.0025(17) 0.0036(17) -0.0068(18) C41 0.054(3) 0.032(2) 0.032(2) 0.0028(18) 0.003(2) 0.011(2) C42 0.047(3) 0.056(3) 0.035(3) 0.007(2) 0.012(2) 0.017(2) C43 0.165(8) 0.065(4) 0.116(6) 0.025(4) 0.109(6) 0.014(5) C44 0.151(7) 0.038(3) 0.108(6) 0.023(3) 0.093(5) 0.031(4) C45 0.220(10) 0.046(4) 0.155(8) 0.046(4) 0.149(8) 0.046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O13 2.361(3) . ? Sm1 O6 2.371(3) . ? Sm1 O2 2.386(3) . ? Sm1 O9 2.406(3) . ? Sm1 O11 2.409(3) . ? Sm1 O4 2.423(3) . ? Sm1 O7 2.429(3) . ? Sm1 O8 2.487(3) . ? Zn1 O1 1.934(3) . ? Zn1 O5 1.945(3) . ? Zn1 O3 1.965(3) . ? Zn1 N1 2.052(3) . ? Zn2 O14 1.921(3) . ? Zn2 O10 1.936(3) . ? Zn2 O12 1.969(3) . ? Zn2 N2 2.061(3) . ? O1 C1 1.270(5) . ? O2 C1 1.238(5) . ? O3 C6 1.281(5) . ? O4 C6 1.232(5) . ? O5 C11 1.280(5) . ? O6 C11 1.245(5) . ? O7 C16 1.262(5) . ? O8 C16 1.262(5) . ? O9 C21 1.242(6) . ? O10 C21 1.259(5) . ? O11 C26 1.233(5) . ? O12 C26 1.260(5) . ? O13 C31 1.239(5) . ? O14 C31 1.269(5) . ? N1 C40 1.345(5) . ? N1 C36 1.351(5) . ? N2 C41 1.314(5) . ? N2 C44 1.320(6) . ? C1 C2 1.525(6) . ? C2 C3 1.387(10) . ? C2 C4 1.402(12) . ? C2 C5 1.447(9) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.527(6) . ? C7 C10 1.527(6) . ? C7 C8 1.531(6) . ? C7 C9 1.533(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.511(6) . ? C12 C14 1.480(8) . ? C12 C15 1.497(8) . ? C12 C13 1.501(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.536(6) . ? C17 C18 1.520(6) . ? C17 C20 1.524(7) . ? C17 C19 1.538(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.530(6) . ? C22 C23 1.508(8) . ? C22 C24 1.513(8) . ? C22 C25 1.519(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.534(5) . ? C27 C29 1.517(6) . ? C27 C30 1.525(6) . ? C27 C28 1.530(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.541(5) . ? C32 C33 1.525(6) . ? C32 C35 1.527(6) . ? C32 C34 1.531(7) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.365(6) . ? C36 H36 0.9500 . ? C37 C38 1.380(6) . ? C37 H37 0.9500 . ? C38 C39 1.374(6) . ? C38 H38 0.9500 . ? C39 C40 1.367(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.385(6) . ? C41 H41 0.9500 . ? C42 C43 1.350(8) . ? C42 H42 0.9500 . ? C43 C45 1.400(9) . ? C43 H43 0.9500 . ? C44 C45 1.378(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 O13 Sm1 O6 158.51(10) . . ? O13 Sm1 O2 100.36(11) . . ? O6 Sm1 O2 86.34(11) . . ? O13 Sm1 O9 85.98(11) . . ? O6 Sm1 O9 98.84(11) . . ? O2 Sm1 O9 148.88(13) . . ? O13 Sm1 O11 84.30(10) . . ? O6 Sm1 O11 77.71(11) . . ? O2 Sm1 O11 139.96(12) . . ? O9 Sm1 O11 70.64(13) . . ? O13 Sm1 O4 78.29(10) . . ? O6 Sm1 O4 84.80(11) . . ? O2 Sm1 O4 70.97(11) . . ? O9 Sm1 O4 139.84(12) . . ? O11 Sm1 O4 71.18(12) . . ? O13 Sm1 O7 128.25(9) . . ? O6 Sm1 O7 73.17(10) . . ? O2 Sm1 O7 74.48(12) . . ? O9 Sm1 O7 77.74(12) . . ? O11 Sm1 O7 132.54(11) . . ? O4 Sm1 O7 139.88(11) . . ? O13 Sm1 O8 75.16(9) . . ? O6 Sm1 O8 126.31(10) . . ? O2 Sm1 O8 78.47(10) . . ? O9 Sm1 O8 73.77(12) . . ? O11 Sm1 O8 139.84(11) . . ? O4 Sm1 O8 134.67(10) . . ? O7 Sm1 O8 53.18(9) . . ? O1 Zn1 O5 116.81(15) . . ? O1 Zn1 O3 109.13(13) . . ? O5 Zn1 O3 127.39(13) . . ? O1 Zn1 N1 103.54(14) . . ? O5 Zn1 N1 95.35(13) . . ? O3 Zn1 N1 97.64(12) . . ? O14 Zn2 O10 119.54(14) . . ? O14 Zn2 O12 127.84(13) . . ? O10 Zn2 O12 106.20(13) . . ? O14 Zn2 N2 96.44(13) . . ? O10 Zn2 N2 101.40(14) . . ? O12 Zn2 N2 97.83(13) . . ? C1 O1 Zn1 124.2(3) . . ? C1 O2 Sm1 152.4(3) . . ? C6 O3 Zn1 118.8(3) . . ? C6 O4 Sm1 153.7(3) . . ? C11 O5 Zn1 120.0(3) . . ? C11 O6 Sm1 152.2(3) . . ? C16 O7 Sm1 94.1(2) . . ? C16 O8 Sm1 91.4(2) . . ? C21 O9 Sm1 157.4(3) . . ? C21 O10 Zn2 125.9(3) . . ? C26 O11 Sm1 169.9(3) . . ? C26 O12 Zn2 113.7(3) . . ? C31 O13 Sm1 158.7(3) . . ? C31 O14 Zn2 126.1(3) . . ? C40 N1 C36 117.2(4) . . ? C40 N1 Zn1 123.1(3) . . ? C36 N1 Zn1 119.7(3) . . ? C41 N2 C44 117.3(4) . . ? C41 N2 Zn2 119.0(3) . . ? C44 N2 Zn2 123.7(3) . . ? O2 C1 O1 123.4(4) . . ? O2 C1 C2 120.1(4) . . ? O1 C1 C2 116.5(4) . . ? C3 C2 C4 107.3(13) . . ? C3 C2 C5 108.7(9) . . ? C4 C2 C5 109.3(11) . . ? C3 C2 C1 110.3(5) . . ? C4 C2 C1 108.8(6) . . ? C5 C2 C1 112.3(5) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 122.9(4) . . ? O4 C6 C7 119.2(4) . . ? O3 C6 C7 117.7(4) . . ? C6 C7 C10 109.9(3) . . ? C6 C7 C8 106.5(3) . . ? C10 C7 C8 109.8(4) . . ? C6 C7 C9 112.1(4) . . ? C10 C7 C9 109.8(4) . . ? C8 C7 C9 108.7(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 120.7(4) . . ? O6 C11 C12 121.6(4) . . ? O5 C11 C12 117.7(4) . . ? C14 C12 C15 110.4(6) . . ? C14 C12 C13 111.3(7) . . ? C15 C12 C13 108.7(5) . . ? C14 C12 C11 110.0(4) . . ? C15 C12 C11 111.0(5) . . ? C13 C12 C11 105.3(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 121.4(4) . . ? O8 C16 C17 119.6(4) . . ? O7 C16 C17 119.0(4) . . ? C18 C17 C20 110.1(5) . . ? C18 C17 C16 110.1(4) . . ? C20 C17 C16 111.1(4) . . ? C18 C17 C19 110.8(4) . . ? C20 C17 C19 109.5(4) . . ? C16 C17 C19 105.2(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 124.0(4) . . ? O9 C21 C22 119.2(4) . . ? O10 C21 C22 116.8(4) . . ? C23 C22 C24 111.5(6) . . ? C23 C22 C25 111.3(6) . . ? C24 C22 C25 108.1(6) . . ? C23 C22 C21 110.3(4) . . ? C24 C22 C21 108.0(4) . . ? C25 C22 C21 107.4(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 122.4(4) . . ? O11 C26 C27 119.4(4) . . ? O12 C26 C27 118.2(4) . . ? C29 C27 C30 110.1(4) . . ? C29 C27 C28 109.6(4) . . ? C30 C27 C28 110.1(4) . . ? C29 C27 C26 111.9(3) . . ? C30 C27 C26 109.6(3) . . ? C28 C27 C26 105.4(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O13 C31 O14 124.3(4) . . ? O13 C31 C32 119.4(4) . . ? O14 C31 C32 116.3(3) . . ? C33 C32 C35 109.0(4) . . ? C33 C32 C34 109.8(4) . . ? C35 C32 C34 110.6(4) . . ? C33 C32 C31 106.4(3) . . ? C35 C32 C31 110.2(3) . . ? C34 C32 C31 110.8(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N1 C36 C37 122.7(4) . . ? N1 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C36 C37 C38 119.3(4) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 118.7(4) . . ? C39 C38 H38 120.7 . . ? C37 C38 H38 120.7 . . ? C40 C39 C38 119.2(4) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? N1 C40 C39 122.9(4) . . ? N1 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? N2 C41 C42 125.2(4) . . ? N2 C41 H41 117.4 . . ? C42 C41 H41 117.4 . . ? C43 C42 C41 116.9(5) . . ? C43 C42 H42 121.5 . . ? C41 C42 H42 121.5 . . ? C42 C43 C45 119.4(5) . . ? C42 C43 H43 120.3 . . ? C45 C43 H43 120.3 . . ? N2 C44 C45 122.6(5) . . ? N2 C44 H44 118.7 . . ? C45 C44 H44 118.7 . . ? C44 C45 C43 118.3(6) . . ? C44 C45 H45 120.8 . . ? C43 C45 H45 120.8 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.139 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.085 # start Validation Reply Form _vrf_PLAT213_7jy031ss ; PROBLEM: Atom C3 has ADP max/min Ratio ..... 5.60 prola RESPONSE: C3 and C2 seem to have large thermo parameters however no Q-peaks could be located near these atoms to split occupancy with. They were left anisotropic. ; _vrf_PLAT220_7jy031ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT222_7jy031ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT242_7jy031ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C2 RESPONSE: see above ; # end Validation Reply Form #===END data_9dc043sss _database_code_depnum_ccdc_archive 'CCDC 753909' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TbZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 N3 O10 Tb Zn' _chemical_formula_weight 967.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5275(17) _cell_length_b 20.399(3) _cell_length_c 20.249(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.302(2) _cell_angle_gamma 90.00 _cell_volume 4652.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8610 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.36 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 2.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33526 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.37 _reflns_number_total 8532 _reflns_number_gt 7463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+3.2377P] 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 8532 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Zn1 Zn 0.79384(3) 0.317428(14) 0.319088(16) 0.03049(8) Uani 1 1 d . . . Tb1 Tb 0.973963(10) 0.186220(6) 0.240687(6) 0.02640(5) Uani 1 1 d . . . N1 N 0.76714(19) 0.13112(11) 0.20553(11) 0.0328(5) Uani 1 1 d . . . N2 N 0.6203(2) 0.27562(11) 0.28189(12) 0.0372(5) Uani 1 1 d . . . N3 N 0.74557(19) 0.39951(10) 0.36849(11) 0.0312(5) Uani 1 1 d . . . O1 O 1.10923(19) 0.20719(13) 0.16823(11) 0.0584(6) Uani 1 1 d . . . O2 O 0.95528(16) 0.14847(10) 0.12414(9) 0.0390(5) Uani 1 1 d . . . O3 O 1.1549(2) 0.14094(11) 0.30885(13) 0.0631(7) Uani 1 1 d . . . O4 O 1.01834(17) 0.07155(10) 0.26231(10) 0.0450(5) Uani 1 1 d . . . O5 O 0.84945(16) 0.27085(9) 0.19502(9) 0.0347(4) Uani 1 1 d . . . O6 O 0.78711(18) 0.36484(9) 0.22851(10) 0.0411(5) Uani 1 1 d . . . O7 O 0.96864(17) 0.34292(11) 0.34788(11) 0.0468(5) Uani 1 1 d . . . O8 O 1.06901(18) 0.27649(10) 0.29433(11) 0.0449(5) Uani 1 1 d . . . O9 O 0.89749(19) 0.18435(9) 0.33691(10) 0.0409(5) Uani 1 1 d . . . O10 O 0.82237(17) 0.25412(10) 0.39961(9) 0.0409(5) Uani 1 1 d . . . C1 C 1.0546(2) 0.17163(13) 0.12106(14) 0.0318(6) Uani 1 1 d . . . C2 C 1.1105(3) 0.15756(17) 0.06042(15) 0.0433(7) Uani 1 1 d . . . C3 C 1.1073(6) 0.2215(3) 0.0208(3) 0.112(2) Uani 1 1 d . . . H3A H 1.0246 0.2351 0.0044 0.167 Uiso 1 1 calc R . . H3B H 1.1450 0.2148 -0.0177 0.167 Uiso 1 1 calc R . . H3C H 1.1502 0.2556 0.0504 0.167 Uiso 1 1 calc R . . C4 C 1.2381(3) 0.1366(3) 0.0861(2) 0.105(2) Uani 1 1 d . . . H4A H 1.2812 0.1711 0.1149 0.158 Uiso 1 1 calc R . . H4B H 1.2757 0.1290 0.0476 0.158 Uiso 1 1 calc R . . H4C H 1.2401 0.0961 0.1123 0.158 Uiso 1 1 calc R . . C5 C 1.0430(3) 0.1054(2) 0.01532(17) 0.0608(10) Uani 1 1 d . . . H5A H 1.0502 0.0635 0.0396 0.091 Uiso 1 1 calc R . . H5B H 1.0757 0.1009 -0.0253 0.091 Uiso 1 1 calc R . . H5C H 0.9590 0.1177 0.0023 0.091 Uiso 1 1 calc R . . C6 C 1.1205(3) 0.08334(14) 0.29696(14) 0.0396(7) Uani 1 1 d . . . C7 C 1.2052(3) 0.02636(16) 0.32225(17) 0.0555(9) Uani 1 1 d . . . C8 C 1.2835(4) 0.0429(2) 0.39059(19) 0.0741(12) Uani 1 1 d . . . H8A H 1.2338 0.0492 0.4238 0.111 Uiso 1 1 calc R . . H8B H 1.3279 0.0832 0.3868 0.111 Uiso 1 1 calc R . . H8C H 1.3392 0.0068 0.4052 0.111 Uiso 1 1 calc R . . C9 C 1.1382(5) -0.0352(2) 0.3276(3) 0.121(2) Uani 1 1 d . . . H9A H 1.0847 -0.0285 0.3586 0.182 Uiso 1 1 calc R . . H9B H 1.1942 -0.0706 0.3447 0.182 Uiso 1 1 calc R . . H9C H 1.0917 -0.0472 0.2828 0.182 Uiso 1 1 calc R . . C10 C 1.2836(5) 0.0206(3) 0.2701(2) 0.116(2) Uani 1 1 d . . . H10A H 1.3463 -0.0117 0.2856 0.175 Uiso 1 1 calc R . . H10B H 1.3195 0.0633 0.2647 0.175 Uiso 1 1 calc R . . H10C H 1.2350 0.0066 0.2266 0.175 Uiso 1 1 calc R . . C11 C 0.8273(2) 0.33108(13) 0.18669(13) 0.0310(6) Uani 1 1 d . . . C12 C 0.8528(3) 0.36441(14) 0.12393(14) 0.0420(7) Uani 1 1 d . . . C13 C 0.7810(5) 0.42764(17) 0.10846(19) 0.0800(14) Uani 1 1 d . . . H13A H 0.6961 0.4175 0.1005 0.120 Uiso 1 1 calc R . . H13B H 0.7988 0.4483 0.0680 0.120 Uiso 1 1 calc R . . H13C H 0.8022 0.4577 0.1469 0.120 Uiso 1 1 calc R . . C14 C 0.8225(4) 0.31826(16) 0.06355(16) 0.0559(9) Uani 1 1 d . . . H14A H 0.8680 0.2776 0.0737 0.084 Uiso 1 1 calc R . . H14B H 0.8426 0.3392 0.0239 0.084 Uiso 1 1 calc R . . H14C H 0.7374 0.3083 0.0542 0.084 Uiso 1 1 calc R . . C15 C 0.9853(4) 0.3791(2) 0.1399(2) 0.0815(14) Uani 1 1 d . . . H15A H 1.0045 0.4077 0.1797 0.122 Uiso 1 1 calc R . . H15B H 1.0067 0.4012 0.1012 0.122 Uiso 1 1 calc R . . H15C H 1.0298 0.3381 0.1492 0.122 Uiso 1 1 calc R . . C16 C 1.0623(2) 0.32015(12) 0.33637(13) 0.0302(6) Uani 1 1 d . . . C17 C 1.1790(2) 0.34694(15) 0.37882(14) 0.0391(6) Uani 1 1 d . . . C18 C 1.1936(5) 0.3137(3) 0.4470(3) 0.118(2) Uani 1 1 d . . . H18A H 1.2147 0.2675 0.4428 0.178 Uiso 1 1 calc R . . H18B H 1.1189 0.3164 0.4626 0.178 Uiso 1 1 calc R . . H18C H 1.2567 0.3355 0.4796 0.178 Uiso 1 1 calc R . . C19 C 1.1676(4) 0.42035(19) 0.3898(2) 0.0765(12) Uani 1 1 d . . . H19A H 1.2399 0.4365 0.4199 0.115 Uiso 1 1 calc R . . H19B H 1.0992 0.4286 0.4102 0.115 Uiso 1 1 calc R . . H19C H 1.1563 0.4431 0.3462 0.115 Uiso 1 1 calc R . . C20 C 1.2801(4) 0.3361(3) 0.3457(3) 0.113(2) Uani 1 1 d . . . H20A H 1.2972 0.2891 0.3449 0.169 Uiso 1 1 calc R . . H20B H 1.3502 0.3593 0.3709 0.169 Uiso 1 1 calc R . . H20C H 1.2598 0.3528 0.2993 0.169 Uiso 1 1 calc R . . C21 C 0.8726(2) 0.20093(14) 0.39192(13) 0.0335(6) Uani 1 1 d . . . C22 C 0.8991(3) 0.15340(16) 0.45176(15) 0.0445(7) Uani 1 1 d . . . C23 C 0.7821(4) 0.1196(2) 0.4546(2) 0.0759(12) Uani 1 1 d . . . H23A H 0.7243 0.1525 0.4623 0.114 Uiso 1 1 calc R . . H23B H 0.7954 0.0877 0.4916 0.114 Uiso 1 1 calc R . . H23C H 0.7514 0.0970 0.4118 0.114 Uiso 1 1 calc R . . C24 C 0.9430(4) 0.19171(18) 0.51704(17) 0.0636(11) Uani 1 1 d . . . H24A H 1.0176 0.2139 0.5151 0.095 Uiso 1 1 calc R . . H24B H 0.9562 0.1615 0.5555 0.095 Uiso 1 1 calc R . . H24C H 0.8833 0.2244 0.5224 0.095 Uiso 1 1 calc R . . C25 C 0.9923(4) 0.1034(2) 0.44250(18) 0.0761(13) Uani 1 1 d . . . H25A H 0.9622 0.0774 0.4017 0.114 Uiso 1 1 calc R . . H25B H 1.0097 0.0743 0.4819 0.114 Uiso 1 1 calc R . . H25C H 1.0650 0.1262 0.4379 0.114 Uiso 1 1 calc R . . C26 C 0.6842(2) 0.15468(14) 0.15510(15) 0.0403(7) Uani 1 1 d . . . H26 H 0.7023 0.1927 0.1322 0.048 Uiso 1 1 calc R . . C27 C 0.5736(3) 0.12688(16) 0.13434(18) 0.0517(8) Uani 1 1 d . . . H27 H 0.5164 0.1461 0.0989 0.062 Uiso 1 1 calc R . . C28 C 0.5475(3) 0.07067(17) 0.16584(19) 0.0560(9) Uani 1 1 d . . . H28 H 0.4719 0.0503 0.1525 0.067 Uiso 1 1 calc R . . C29 C 0.6322(3) 0.04472(17) 0.21658(18) 0.0550(9) Uani 1 1 d . . . H29 H 0.6172 0.0054 0.2385 0.066 Uiso 1 1 calc R . . C30 C 0.7404(3) 0.07631(15) 0.23571(15) 0.0435(7) Uani 1 1 d . . . H30 H 0.7981 0.0584 0.2718 0.052 Uiso 1 1 calc R . . C31 C 0.5477(3) 0.29735(17) 0.22526(16) 0.0481(8) Uani 1 1 d . . . H31 H 0.5766 0.3291 0.1984 0.058 Uiso 1 1 calc R . . C32 C 0.4325(3) 0.2751(2) 0.20463(18) 0.0603(10) Uani 1 1 d . . . H32 H 0.3832 0.2919 0.1646 0.072 Uiso 1 1 calc R . . C33 C 0.3894(3) 0.22884(19) 0.24190(19) 0.0601(10) Uani 1 1 d . . . H33 H 0.3103 0.2131 0.2284 0.072 Uiso 1 1 calc R . . C34 C 0.4632(3) 0.2061(2) 0.2989(2) 0.0668(10) Uani 1 1 d . . . H34 H 0.4366 0.1734 0.3257 0.080 Uiso 1 1 calc R . . C35 C 0.5766(3) 0.23068(17) 0.31749(19) 0.0557(9) Uani 1 1 d . . . H35 H 0.6262 0.2147 0.3579 0.067 Uiso 1 1 calc R . . C36 C 0.8222(2) 0.42250(14) 0.42301(13) 0.0356(6) Uani 1 1 d . . . H36 H 0.8900 0.3969 0.4421 0.043 Uiso 1 1 calc R . . C37 C 0.8061(3) 0.48172(15) 0.45208(15) 0.0450(7) Uani 1 1 d . . . H37 H 0.8617 0.4965 0.4908 0.054 Uiso 1 1 calc R . . C38 C 0.7088(3) 0.51954(14) 0.42473(16) 0.0449(7) Uani 1 1 d . . . H38 H 0.6970 0.5611 0.4435 0.054 Uiso 1 1 calc R . . C39 C 0.6292(3) 0.49581(14) 0.36971(15) 0.0430(7) Uani 1 1 d . . . H39 H 0.5602 0.5202 0.3502 0.052 Uiso 1 1 calc R . . C40 C 0.6509(3) 0.43632(14) 0.34325(14) 0.0384(6) Uani 1 1 d . . . H40 H 0.5956 0.4205 0.3049 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03016(16) 0.03017(17) 0.02938(17) -0.00448(12) 0.00240(13) 0.00436(11) Tb1 0.02800(8) 0.02740(8) 0.02263(8) -0.00526(5) 0.00277(5) 0.00209(5) N1 0.0329(12) 0.0325(12) 0.0340(12) -0.0028(10) 0.0095(10) -0.0001(9) N2 0.0330(12) 0.0391(13) 0.0371(13) -0.0073(11) 0.0021(10) 0.0007(10) N3 0.0378(12) 0.0291(11) 0.0271(11) -0.0009(9) 0.0077(9) 0.0031(9) O1 0.0437(12) 0.0903(17) 0.0445(13) -0.0357(13) 0.0169(10) -0.0294(12) O2 0.0388(11) 0.0489(12) 0.0318(10) -0.0151(9) 0.0129(8) -0.0149(9) O3 0.0454(13) 0.0445(13) 0.0846(18) -0.0014(12) -0.0190(12) 0.0058(10) O4 0.0441(12) 0.0364(11) 0.0468(12) -0.0052(9) -0.0077(10) 0.0064(9) O5 0.0375(10) 0.0281(10) 0.0366(10) 0.0021(8) 0.0034(8) -0.0002(8) O6 0.0501(12) 0.0377(11) 0.0355(11) -0.0030(9) 0.0088(9) 0.0056(9) O7 0.0295(10) 0.0513(12) 0.0574(14) -0.0197(11) 0.0041(9) 0.0005(9) O8 0.0479(12) 0.0412(12) 0.0438(12) -0.0190(10) 0.0060(10) -0.0038(9) O9 0.0521(13) 0.0431(12) 0.0279(11) -0.0007(8) 0.0095(9) 0.0065(9) O10 0.0477(11) 0.0416(11) 0.0317(10) 0.0007(9) 0.0051(9) 0.0134(9) C1 0.0280(13) 0.0377(14) 0.0299(14) -0.0045(11) 0.0067(11) 0.0004(11) C2 0.0349(15) 0.061(2) 0.0359(16) -0.0155(15) 0.0133(12) -0.0067(14) C3 0.186(6) 0.087(4) 0.094(4) 0.006(3) 0.102(4) -0.012(4) C4 0.0346(19) 0.208(6) 0.070(3) -0.072(3) 0.0043(18) 0.016(3) C5 0.0471(19) 0.097(3) 0.0403(18) -0.0326(19) 0.0127(15) -0.0101(18) C6 0.0463(17) 0.0385(16) 0.0317(15) -0.0024(12) 0.0029(13) 0.0130(13) C7 0.062(2) 0.0482(19) 0.0466(19) -0.0047(15) -0.0094(16) 0.0269(16) C8 0.072(3) 0.078(3) 0.058(2) 0.001(2) -0.0174(19) 0.032(2) C9 0.108(4) 0.043(2) 0.176(6) 0.018(3) -0.052(4) 0.011(2) C10 0.133(4) 0.147(5) 0.073(3) 0.008(3) 0.029(3) 0.105(4) C11 0.0303(13) 0.0325(14) 0.0257(13) -0.0010(11) -0.0040(11) -0.0008(11) C12 0.0595(19) 0.0351(15) 0.0291(15) 0.0009(12) 0.0040(13) -0.0065(13) C13 0.150(4) 0.042(2) 0.043(2) 0.0108(16) 0.008(2) 0.017(2) C14 0.083(3) 0.054(2) 0.0284(16) -0.0042(14) 0.0060(17) 0.0023(17) C15 0.078(3) 0.104(3) 0.061(2) 0.016(2) 0.011(2) -0.047(3) C16 0.0327(14) 0.0272(13) 0.0280(14) -0.0034(10) 0.0007(11) -0.0024(10) C17 0.0328(14) 0.0456(17) 0.0344(15) -0.0085(13) -0.0027(12) -0.0062(12) C18 0.101(4) 0.139(5) 0.084(3) 0.060(3) -0.050(3) -0.058(3) C19 0.073(3) 0.066(3) 0.091(3) -0.038(2) 0.017(2) -0.023(2) C20 0.046(2) 0.171(5) 0.125(5) -0.091(4) 0.028(3) -0.030(3) C21 0.0352(14) 0.0409(15) 0.0235(14) -0.0015(11) 0.0042(11) 0.0015(12) C22 0.0601(19) 0.0451(17) 0.0286(15) 0.0070(13) 0.0106(14) 0.0142(15) C23 0.095(3) 0.067(3) 0.069(3) 0.028(2) 0.023(2) -0.004(2) C24 0.083(3) 0.077(3) 0.0265(17) 0.0031(16) 0.0009(17) 0.021(2) C25 0.111(3) 0.073(3) 0.045(2) 0.0161(19) 0.018(2) 0.053(2) C26 0.0370(15) 0.0330(15) 0.0480(18) -0.0021(13) 0.0027(13) -0.0007(12) C27 0.0375(16) 0.0487(19) 0.063(2) -0.0089(16) -0.0018(15) -0.0004(14) C28 0.0370(16) 0.060(2) 0.072(2) -0.0113(18) 0.0132(16) -0.0143(15) C29 0.056(2) 0.054(2) 0.060(2) 0.0024(17) 0.0230(17) -0.0161(16) C30 0.0464(17) 0.0472(17) 0.0381(16) 0.0023(14) 0.0120(13) -0.0033(14) C31 0.0410(17) 0.061(2) 0.0381(17) -0.0088(15) -0.0017(13) 0.0012(14) C32 0.0408(18) 0.089(3) 0.0442(19) -0.0207(19) -0.0073(15) 0.0023(18) C33 0.0387(17) 0.078(3) 0.064(2) -0.033(2) 0.0112(17) -0.0115(17) C34 0.051(2) 0.073(2) 0.078(3) 0.000(2) 0.016(2) -0.0170(19) C35 0.0432(18) 0.059(2) 0.061(2) 0.0085(17) 0.0038(16) -0.0037(15) C36 0.0373(14) 0.0404(15) 0.0294(14) -0.0031(12) 0.0077(11) 0.0038(12) C37 0.0504(18) 0.0500(18) 0.0363(16) -0.0139(14) 0.0128(14) -0.0065(14) C38 0.068(2) 0.0290(15) 0.0440(18) -0.0028(13) 0.0266(16) 0.0026(14) C39 0.0591(19) 0.0351(15) 0.0368(16) 0.0094(13) 0.0148(14) 0.0177(14) C40 0.0439(15) 0.0397(16) 0.0300(14) 0.0018(12) 0.0045(12) 0.0111(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 2.042(2) . ? Zn1 O10 2.0508(19) . ? Zn1 O6 2.060(2) . ? Zn1 N3 2.086(2) . ? Zn1 N2 2.157(2) . ? Tb1 O8 2.2943(19) . ? Tb1 O9 2.304(2) . ? Tb1 O5 2.3087(18) . ? Tb1 O1 2.396(2) . ? Tb1 O4 2.414(2) . ? Tb1 O3 2.425(2) . ? Tb1 O2 2.4479(18) . ? Tb1 N1 2.594(2) . ? N1 C26 1.331(4) . ? N1 C30 1.341(4) . ? N2 C35 1.330(4) . ? N2 C31 1.343(4) . ? N3 C40 1.334(3) . ? N3 C36 1.343(3) . ? O1 C1 1.256(3) . ? O2 C1 1.253(3) . ? O3 C6 1.247(4) . ? O4 C6 1.259(3) . ? O5 C11 1.259(3) . ? O6 C11 1.255(3) . ? O7 C16 1.242(3) . ? O8 C16 1.246(3) . ? O9 C21 1.254(3) . ? O10 C21 1.255(3) . ? C1 C2 1.530(4) . ? C2 C5 1.507(4) . ? C2 C4 1.514(5) . ? C2 C3 1.527(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.534(4) . ? C7 C9 1.491(6) . ? C7 C8 1.520(5) . ? C7 C10 1.534(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.524(4) . ? C12 C15 1.522(5) . ? C12 C14 1.524(4) . ? C12 C13 1.528(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.535(4) . ? C17 C20 1.480(5) . ? C17 C18 1.514(5) . ? C17 C19 1.524(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.531(4) . ? C22 C25 1.522(4) . ? C22 C24 1.526(5) . ? C22 C23 1.527(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.377(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(5) . ? C27 H27 0.9500 . ? C28 C29 1.365(5) . ? C28 H28 0.9500 . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.366(5) . ? C32 H32 0.9500 . ? C33 C34 1.362(5) . ? C33 H33 0.9500 . ? C34 C35 1.375(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.374(4) . ? C36 H36 0.9500 . ? C37 C38 1.377(4) . ? C37 H37 0.9500 . ? C38 C39 1.372(4) . ? C38 H38 0.9500 . ? C39 C40 1.371(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 O7 Zn1 O10 87.25(9) . . ? O7 Zn1 O6 88.99(9) . . ? O10 Zn1 O6 166.56(8) . . ? O7 Zn1 N3 90.37(8) . . ? O10 Zn1 N3 97.94(8) . . ? O6 Zn1 N3 94.98(8) . . ? O7 Zn1 N2 170.23(8) . . ? O10 Zn1 N2 90.48(9) . . ? O6 Zn1 N2 91.06(9) . . ? N3 Zn1 N2 99.35(9) . . ? O8 Tb1 O9 80.97(7) . . ? O8 Tb1 O5 77.46(7) . . ? O9 Tb1 O5 91.94(7) . . ? O8 Tb1 O1 80.75(7) . . ? O9 Tb1 O1 159.56(7) . . ? O5 Tb1 O1 92.94(8) . . ? O8 Tb1 O4 129.07(7) . . ? O9 Tb1 O4 86.27(7) . . ? O5 Tb1 O4 152.46(6) . . ? O1 Tb1 O4 98.26(8) . . ? O8 Tb1 O3 76.71(8) . . ? O9 Tb1 O3 87.14(9) . . ? O5 Tb1 O3 153.98(7) . . ? O1 Tb1 O3 79.83(9) . . ? O4 Tb1 O3 53.45(7) . . ? O8 Tb1 O2 130.09(7) . . ? O9 Tb1 O2 147.06(7) . . ? O5 Tb1 O2 85.96(7) . . ? O1 Tb1 O2 53.20(6) . . ? O4 Tb1 O2 80.90(7) . . ? O3 Tb1 O2 108.49(8) . . ? O8 Tb1 N1 142.73(7) . . ? O9 Tb1 N1 74.34(7) . . ? O5 Tb1 N1 75.96(7) . . ? O1 Tb1 N1 126.10(7) . . ? O4 Tb1 N1 77.11(7) . . ? O3 Tb1 N1 128.30(8) . . ? O2 Tb1 N1 73.27(6) . . ? C26 N1 C30 116.9(2) . . ? C26 N1 Tb1 121.47(18) . . ? C30 N1 Tb1 121.55(18) . . ? C35 N2 C31 116.8(3) . . ? C35 N2 Zn1 120.9(2) . . ? C31 N2 Zn1 122.1(2) . . ? C40 N3 C36 117.4(2) . . ? C40 N3 Zn1 123.25(18) . . ? C36 N3 Zn1 118.57(18) . . ? C1 O1 Tb1 94.39(17) . . ? C1 O2 Tb1 92.05(15) . . ? C6 O3 Tb1 92.81(17) . . ? C6 O4 Tb1 93.04(17) . . ? C11 O5 Tb1 150.97(16) . . ? C11 O6 Zn1 113.21(17) . . ? C16 O7 Zn1 134.05(18) . . ? C16 O8 Tb1 143.53(19) . . ? C21 O9 Tb1 161.38(19) . . ? C21 O10 Zn1 116.47(17) . . ? O2 C1 O1 119.7(2) . . ? O2 C1 C2 121.0(2) . . ? O1 C1 C2 119.3(2) . . ? C5 C2 C4 110.3(3) . . ? C5 C2 C3 109.5(3) . . ? C4 C2 C3 109.6(4) . . ? C5 C2 C1 111.5(2) . . ? C4 C2 C1 108.8(3) . . ? C3 C2 C1 107.1(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 120.6(3) . . ? O3 C6 C7 119.7(3) . . ? O4 C6 C7 119.6(3) . . ? C9 C7 C8 109.7(4) . . ? C9 C7 C10 112.1(4) . . ? C8 C7 C10 108.7(4) . . ? C9 C7 C6 111.1(3) . . ? C8 C7 C6 110.4(3) . . ? C10 C7 C6 104.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.6(3) . . ? O6 C11 C12 118.9(2) . . ? O5 C11 C12 118.5(2) . . ? C15 C12 C14 110.0(3) . . ? C15 C12 C11 105.9(2) . . ? C14 C12 C11 110.0(2) . . ? C15 C12 C13 110.6(3) . . ? C14 C12 C13 109.6(3) . . ? C11 C12 C13 110.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 125.4(2) . . ? O7 C16 C17 117.1(2) . . ? O8 C16 C17 117.5(2) . . ? C20 C17 C18 113.6(4) . . ? C20 C17 C19 108.3(3) . . ? C18 C17 C19 107.7(4) . . ? C20 C17 C16 112.0(3) . . ? C18 C17 C16 105.3(3) . . ? C19 C17 C16 109.8(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 122.8(3) . . ? O9 C21 C22 119.2(2) . . ? O10 C21 C22 117.9(2) . . ? C25 C22 C24 109.7(3) . . ? C25 C22 C23 110.8(3) . . ? C24 C22 C23 109.3(3) . . ? C25 C22 C21 110.7(3) . . ? C24 C22 C21 109.5(3) . . ? C23 C22 C21 106.7(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 123.5(3) . . ? N1 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C28 C27 C26 118.8(3) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 118.7(3) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 119.2(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N1 C30 C29 122.8(3) . . ? N1 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N2 C31 C32 122.3(3) . . ? N2 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 118.0(3) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 119.5(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N2 C35 C34 123.5(3) . . ? N2 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? N3 C36 C37 122.3(3) . . ? N3 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C36 C37 C38 119.6(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 118.4(3) . . ? C39 C38 H38 120.8 . . ? C37 C38 H38 120.8 . . ? C40 C39 C38 118.9(3) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N3 C40 C39 123.4(3) . . ? N3 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.050 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.077 #===END data_7mr212ss _database_code_depnum_ccdc_archive 'CCDC 753910' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DyZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 Dy N3 O10 Zn' _chemical_formula_weight 970.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5129(17) _cell_length_b 20.367(3) _cell_length_c 20.210(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.243(2) _cell_angle_gamma 90.00 _cell_volume 4631.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.138 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_min 0.128 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 2.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.757 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28189 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6676 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+3.2529P] 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 6676 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Zn1 Zn 0.79412(4) 0.317389(19) 0.31871(2) 0.02822(11) Uani 1 1 d . . . Dy1 Dy 0.974797(14) 0.186553(8) 0.240770(8) 0.02402(7) Uani 1 1 d . . . N1 N 0.7686(3) 0.13190(14) 0.20620(14) 0.0291(7) Uani 1 1 d . . . N2 N 0.6209(3) 0.27542(15) 0.28168(15) 0.0345(8) Uani 1 1 d . . . N3 N 0.7461(2) 0.39945(13) 0.36854(14) 0.0271(7) Uani 1 1 d . . . O1 O 1.1098(2) 0.20725(15) 0.16863(13) 0.0506(8) Uani 1 1 d . . . O2 O 0.9553(2) 0.14878(12) 0.12464(12) 0.0348(6) Uani 1 1 d . . . O3 O 1.1547(2) 0.14176(14) 0.30850(16) 0.0569(8) Uani 1 1 d . . . O4 O 1.0187(2) 0.07241(12) 0.26213(13) 0.0413(7) Uani 1 1 d . . . O5 O 0.8512(2) 0.27071(11) 0.19519(12) 0.0316(6) Uani 1 1 d . . . O6 O 0.7871(2) 0.36476(12) 0.22775(13) 0.0376(6) Uani 1 1 d . . . O7 O 0.9694(2) 0.34305(13) 0.34732(14) 0.0429(7) Uani 1 1 d . . . O8 O 1.0697(2) 0.27642(12) 0.29397(13) 0.0408(7) Uani 1 1 d . . . O9 O 0.8993(2) 0.18435(11) 0.33704(12) 0.0369(6) Uani 1 1 d . . . O10 O 0.8227(2) 0.25421(12) 0.39957(12) 0.0361(6) Uani 1 1 d . . . C1 C 1.0546(3) 0.17171(17) 0.12123(18) 0.0288(9) Uani 1 1 d . . . C2 C 1.1106(3) 0.1575(2) 0.06073(19) 0.0376(10) Uani 1 1 d . . . C3 C 1.1073(6) 0.2211(3) 0.0205(3) 0.103(2) Uani 1 1 d . . . H3A H 1.0245 0.2344 0.0035 0.154 Uiso 1 1 calc R . . H3B H 1.1458 0.2141 -0.0178 0.154 Uiso 1 1 calc R . . H3C H 1.1494 0.2556 0.0498 0.154 Uiso 1 1 calc R . . C4 C 1.2393(4) 0.1368(3) 0.0865(3) 0.094(2) Uani 1 1 d . . . H4A H 1.2827 0.1720 0.1142 0.141 Uiso 1 1 calc R . . H4B H 1.2763 0.1280 0.0479 0.141 Uiso 1 1 calc R . . H4C H 1.2419 0.0969 0.1139 0.141 Uiso 1 1 calc R . . C5 C 1.0428(4) 0.1052(2) 0.0158(2) 0.0553(13) Uani 1 1 d . . . H5A H 1.0466 0.0639 0.0411 0.083 Uiso 1 1 calc R . . H5B H 1.0780 0.0990 -0.0238 0.083 Uiso 1 1 calc R . . H5C H 0.9597 0.1188 0.0010 0.083 Uiso 1 1 calc R . . C6 C 1.1207(4) 0.08385(19) 0.29678(19) 0.0361(9) Uani 1 1 d . . . C7 C 1.2055(4) 0.0269(2) 0.3219(2) 0.0480(11) Uani 1 1 d . . . C8 C 1.2835(4) 0.0433(2) 0.3901(2) 0.0685(15) Uani 1 1 d . . . H8A H 1.2340 0.0485 0.4237 0.103 Uiso 1 1 calc R . . H8B H 1.3263 0.0843 0.3867 0.103 Uiso 1 1 calc R . . H8C H 1.3408 0.0078 0.4042 0.103 Uiso 1 1 calc R . . C9 C 1.1374(5) -0.0349(2) 0.3276(3) 0.110(3) Uani 1 1 d . . . H9A H 1.0833 -0.0276 0.3584 0.164 Uiso 1 1 calc R . . H9B H 1.1930 -0.0703 0.3453 0.164 Uiso 1 1 calc R . . H9C H 1.0913 -0.0472 0.2828 0.164 Uiso 1 1 calc R . . C10 C 1.2837(5) 0.0208(3) 0.2695(3) 0.110(3) Uani 1 1 d . . . H10A H 1.3468 -0.0114 0.2853 0.165 Uiso 1 1 calc R . . H10B H 1.3192 0.0635 0.2636 0.165 Uiso 1 1 calc R . . H10C H 1.2350 0.0063 0.2262 0.165 Uiso 1 1 calc R . . C11 C 0.8285(3) 0.33097(17) 0.18602(18) 0.0278(8) Uani 1 1 d . . . C12 C 0.8545(4) 0.36434(18) 0.12344(19) 0.0378(10) Uani 1 1 d . . . C13 C 0.7832(5) 0.4275(2) 0.1077(2) 0.0752(17) Uani 1 1 d . . . H13A H 0.6981 0.4175 0.1001 0.113 Uiso 1 1 calc R . . H13B H 0.8007 0.4478 0.0669 0.113 Uiso 1 1 calc R . . H13C H 0.8047 0.4579 0.1459 0.113 Uiso 1 1 calc R . . C14 C 0.8234(4) 0.3179(2) 0.0630(2) 0.0517(12) Uani 1 1 d . . . H14A H 0.8683 0.2770 0.0733 0.078 Uiso 1 1 calc R . . H14B H 0.8439 0.3387 0.0232 0.078 Uiso 1 1 calc R . . H14C H 0.7381 0.3084 0.0536 0.078 Uiso 1 1 calc R . . C15 C 0.9874(4) 0.3783(3) 0.1395(2) 0.0746(16) Uani 1 1 d . . . H15A H 1.0068 0.4078 0.1786 0.112 Uiso 1 1 calc R . . H15B H 1.0097 0.3991 0.1002 0.112 Uiso 1 1 calc R . . H15C H 1.0312 0.3371 0.1499 0.112 Uiso 1 1 calc R . . C16 C 1.0631(3) 0.32041(16) 0.33593(18) 0.0272(8) Uani 1 1 d . . . C17 C 1.1789(3) 0.34685(19) 0.37863(19) 0.0356(9) Uani 1 1 d . . . C18 C 1.1950(6) 0.3130(3) 0.4462(3) 0.119(3) Uani 1 1 d . . . H18A H 1.2192 0.2673 0.4417 0.178 Uiso 1 1 calc R . . H18B H 1.1199 0.3138 0.4616 0.178 Uiso 1 1 calc R . . H18C H 1.2565 0.3357 0.4792 0.178 Uiso 1 1 calc R . . C19 C 1.1671(4) 0.4201(2) 0.3903(3) 0.0742(16) Uani 1 1 d . . . H19A H 1.2401 0.4364 0.4199 0.111 Uiso 1 1 calc R . . H19B H 1.0996 0.4280 0.4117 0.111 Uiso 1 1 calc R . . H19C H 1.1542 0.4432 0.3468 0.111 Uiso 1 1 calc R . . C20 C 1.2801(4) 0.3377(3) 0.3448(3) 0.106(3) Uani 1 1 d . . . H20A H 1.2973 0.2908 0.3423 0.160 Uiso 1 1 calc R . . H20B H 1.3502 0.3603 0.3708 0.160 Uiso 1 1 calc R . . H20C H 1.2596 0.3560 0.2990 0.160 Uiso 1 1 calc R . . C21 C 0.8740(3) 0.20109(18) 0.39189(18) 0.0302(9) Uani 1 1 d . . . C22 C 0.9001(4) 0.1534(2) 0.45208(19) 0.0420(10) Uani 1 1 d . . . C23 C 0.7822(5) 0.1195(2) 0.4545(3) 0.0695(15) Uani 1 1 d . . . H23A H 0.7240 0.1525 0.4616 0.104 Uiso 1 1 calc R . . H23B H 0.7948 0.0879 0.4919 0.104 Uiso 1 1 calc R . . H23C H 0.7524 0.0965 0.4117 0.104 Uiso 1 1 calc R . . C24 C 0.9442(5) 0.1921(2) 0.5175(2) 0.0612(14) Uani 1 1 d . . . H24A H 1.0173 0.2156 0.5147 0.092 Uiso 1 1 calc R . . H24B H 0.9602 0.1619 0.5560 0.092 Uiso 1 1 calc R . . H24C H 0.8833 0.2238 0.5236 0.092 Uiso 1 1 calc R . . C25 C 0.9931(5) 0.1033(2) 0.4430(2) 0.0704(16) Uani 1 1 d . . . H25A H 0.9630 0.0772 0.4023 0.106 Uiso 1 1 calc R . . H25B H 1.0105 0.0743 0.4826 0.106 Uiso 1 1 calc R . . H25C H 1.0659 0.1261 0.4383 0.106 Uiso 1 1 calc R . . C26 C 0.6852(3) 0.15533(18) 0.15545(19) 0.0358(9) Uani 1 1 d . . . H26 H 0.7029 0.1934 0.1323 0.043 Uiso 1 1 calc R . . C27 C 0.5752(3) 0.1272(2) 0.1351(2) 0.0459(11) Uani 1 1 d . . . H27 H 0.5178 0.1463 0.0996 0.055 Uiso 1 1 calc R . . C28 C 0.5490(4) 0.0715(2) 0.1665(2) 0.0514(12) Uani 1 1 d . . . H28 H 0.4735 0.0512 0.1530 0.062 Uiso 1 1 calc R . . C29 C 0.6339(4) 0.0454(2) 0.2178(2) 0.0506(12) Uani 1 1 d . . . H29 H 0.6189 0.0061 0.2400 0.061 Uiso 1 1 calc R . . C30 C 0.7414(3) 0.07736(19) 0.23648(19) 0.0385(10) Uani 1 1 d . . . H30 H 0.7992 0.0597 0.2728 0.046 Uiso 1 1 calc R . . C31 C 0.5481(4) 0.2970(2) 0.2255(2) 0.0440(10) Uani 1 1 d . . . H31 H 0.5769 0.3288 0.1985 0.053 Uiso 1 1 calc R . . C32 C 0.4327(4) 0.2749(2) 0.2049(2) 0.0558(13) Uani 1 1 d . . . H32 H 0.3834 0.2918 0.1648 0.067 Uiso 1 1 calc R . . C33 C 0.3896(4) 0.2289(2) 0.2419(2) 0.0551(13) Uani 1 1 d . . . H33 H 0.3105 0.2131 0.2284 0.066 Uiso 1 1 calc R . . C34 C 0.4635(4) 0.2061(2) 0.2993(3) 0.0619(13) Uani 1 1 d . . . H34 H 0.4365 0.1738 0.3265 0.074 Uiso 1 1 calc R . . C35 C 0.5773(4) 0.2303(2) 0.3175(2) 0.0513(12) Uani 1 1 d . . . H35 H 0.6275 0.2140 0.3576 0.062 Uiso 1 1 calc R . . C36 C 0.8223(3) 0.42248(18) 0.42257(18) 0.0322(9) Uani 1 1 d . . . H36 H 0.8904 0.3970 0.4415 0.039 Uiso 1 1 calc R . . C37 C 0.8063(4) 0.48183(19) 0.45204(19) 0.0398(10) Uani 1 1 d . . . H37 H 0.8616 0.4965 0.4910 0.048 Uiso 1 1 calc R . . C38 C 0.7093(4) 0.51940(18) 0.4243(2) 0.0401(10) Uani 1 1 d . . . H38 H 0.6977 0.5611 0.4431 0.048 Uiso 1 1 calc R . . C39 C 0.6297(4) 0.49618(18) 0.3695(2) 0.0402(10) Uani 1 1 d . . . H39 H 0.5608 0.5208 0.3501 0.048 Uiso 1 1 calc R . . C40 C 0.6511(3) 0.43643(18) 0.34265(19) 0.0363(9) Uani 1 1 d . . . H40 H 0.5960 0.4207 0.3041 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0269(2) 0.0270(2) 0.0300(2) -0.00483(18) 0.00407(18) 0.00425(18) Dy1 0.02486(11) 0.02378(10) 0.02326(10) -0.00500(7) 0.00476(7) 0.00208(7) N1 0.0300(17) 0.0308(17) 0.0292(17) -0.0033(14) 0.0119(15) 0.0018(14) N2 0.0314(18) 0.0343(19) 0.0363(19) -0.0082(15) 0.0038(16) 0.0020(15) N3 0.0306(17) 0.0246(16) 0.0276(17) 0.0010(13) 0.0097(14) 0.0023(14) O1 0.0351(16) 0.080(2) 0.0408(17) -0.0323(16) 0.0166(14) -0.0263(15) O2 0.0320(15) 0.0431(16) 0.0324(15) -0.0134(12) 0.0138(12) -0.0136(13) O3 0.0423(18) 0.0391(18) 0.077(2) -0.0023(16) -0.0145(16) 0.0063(14) O4 0.0402(16) 0.0295(15) 0.0472(17) -0.0064(12) -0.0064(14) 0.0076(12) O5 0.0332(15) 0.0233(14) 0.0364(15) 0.0041(11) 0.0033(12) 0.0027(11) O6 0.0431(16) 0.0340(15) 0.0369(16) -0.0024(12) 0.0111(13) 0.0061(12) O7 0.0269(15) 0.0447(16) 0.0564(18) -0.0184(14) 0.0072(13) 0.0024(13) O8 0.0396(16) 0.0362(16) 0.0452(17) -0.0203(14) 0.0058(13) -0.0037(13) O9 0.0475(17) 0.0373(15) 0.0276(15) -0.0007(12) 0.0115(13) 0.0047(13) O10 0.0419(16) 0.0345(15) 0.0316(15) -0.0001(12) 0.0075(12) 0.0137(13) C1 0.028(2) 0.031(2) 0.027(2) -0.0024(17) 0.0061(17) 0.0032(17) C2 0.030(2) 0.052(3) 0.034(2) -0.011(2) 0.0145(18) -0.0051(19) C3 0.170(7) 0.080(4) 0.090(4) 0.004(3) 0.100(5) -0.007(4) C4 0.031(3) 0.181(6) 0.069(4) -0.068(4) 0.009(3) 0.011(3) C5 0.043(3) 0.087(4) 0.040(3) -0.028(2) 0.017(2) -0.010(2) C6 0.043(3) 0.033(2) 0.030(2) -0.0023(18) 0.004(2) 0.0153(19) C7 0.052(3) 0.042(3) 0.044(3) -0.004(2) -0.003(2) 0.020(2) C8 0.065(3) 0.068(3) 0.061(3) 0.004(3) -0.011(3) 0.031(3) C9 0.102(5) 0.040(3) 0.154(6) 0.013(3) -0.046(4) 0.012(3) C10 0.122(5) 0.134(6) 0.075(4) 0.005(4) 0.026(4) 0.100(5) C11 0.023(2) 0.028(2) 0.029(2) -0.0049(17) -0.0029(16) -0.0034(16) C12 0.054(3) 0.029(2) 0.029(2) 0.0020(17) 0.0067(19) -0.0046(19) C13 0.144(5) 0.035(3) 0.042(3) 0.009(2) 0.009(3) 0.013(3) C14 0.076(3) 0.050(3) 0.029(2) -0.001(2) 0.011(2) 0.000(2) C15 0.076(4) 0.090(4) 0.058(3) 0.011(3) 0.016(3) -0.043(3) C16 0.031(2) 0.023(2) 0.028(2) 0.0007(16) 0.0061(17) -0.0002(16) C17 0.029(2) 0.039(2) 0.036(2) -0.0068(19) 0.0023(18) -0.0059(18) C18 0.098(5) 0.139(6) 0.086(4) 0.064(4) -0.056(4) -0.061(4) C19 0.069(3) 0.065(3) 0.089(4) -0.041(3) 0.017(3) -0.026(3) C20 0.040(3) 0.158(6) 0.127(6) -0.091(5) 0.031(3) -0.028(4) C21 0.028(2) 0.037(2) 0.026(2) -0.0020(17) 0.0052(17) 0.0009(17) C22 0.054(3) 0.042(2) 0.032(2) 0.0077(19) 0.015(2) 0.015(2) C23 0.085(4) 0.060(3) 0.067(3) 0.025(3) 0.023(3) -0.004(3) C24 0.079(4) 0.075(3) 0.026(2) 0.004(2) 0.005(2) 0.021(3) C25 0.101(4) 0.068(3) 0.045(3) 0.018(2) 0.021(3) 0.047(3) C26 0.033(2) 0.030(2) 0.044(2) -0.0013(19) 0.007(2) 0.0016(18) C27 0.031(2) 0.041(3) 0.061(3) -0.006(2) 0.000(2) 0.0010(19) C28 0.036(3) 0.050(3) 0.071(3) -0.015(2) 0.019(2) -0.017(2) C29 0.053(3) 0.049(3) 0.057(3) 0.004(2) 0.028(2) -0.016(2) C30 0.045(3) 0.042(2) 0.031(2) 0.0033(19) 0.0132(19) -0.004(2) C31 0.039(3) 0.054(3) 0.037(2) -0.007(2) 0.002(2) 0.001(2) C32 0.040(3) 0.077(4) 0.045(3) -0.019(3) -0.002(2) 0.004(2) C33 0.031(2) 0.073(3) 0.060(3) -0.034(3) 0.009(2) -0.007(2) C34 0.047(3) 0.065(3) 0.074(4) 0.000(3) 0.015(3) -0.016(2) C35 0.037(3) 0.053(3) 0.060(3) 0.007(2) 0.003(2) -0.004(2) C36 0.032(2) 0.038(2) 0.028(2) -0.0044(17) 0.0081(18) 0.0039(17) C37 0.044(3) 0.043(3) 0.034(2) -0.0109(19) 0.013(2) -0.005(2) C38 0.064(3) 0.023(2) 0.041(3) -0.0017(18) 0.028(2) 0.002(2) C39 0.054(3) 0.034(2) 0.036(2) 0.0075(19) 0.019(2) 0.014(2) C40 0.041(2) 0.037(2) 0.031(2) -0.0003(18) 0.0078(18) 0.0078(19) _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 Zn1 O7 2.046(3) . ? Zn1 O10 2.051(2) . ? Zn1 O6 2.062(3) . ? Zn1 N3 2.086(3) . ? Zn1 N2 2.153(3) . ? Dy1 O8 2.281(2) . ? Dy1 O5 2.292(2) . ? Dy1 O9 2.293(2) . ? Dy1 O1 2.383(3) . ? Dy1 O4 2.399(2) . ? Dy1 O3 2.407(3) . ? Dy1 O2 2.435(2) . ? Dy1 N1 2.580(3) . ? N1 C26 1.336(4) . ? N1 C30 1.337(4) . ? N2 C35 1.332(5) . ? N2 C31 1.335(5) . ? N3 C36 1.333(4) . ? N3 C40 1.340(4) . ? O1 C1 1.260(4) . ? O2 C1 1.250(4) . ? O3 C6 1.250(4) . ? O4 C6 1.256(4) . ? O5 C11 1.260(4) . ? O6 C11 1.258(4) . ? O7 C16 1.238(4) . ? O8 C16 1.247(4) . ? O9 C21 1.252(4) . ? O10 C21 1.258(4) . ? C1 C2 1.526(5) . ? C2 C5 1.505(5) . ? C2 C4 1.523(6) . ? C2 C3 1.526(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(5) . ? C7 C9 1.500(7) . ? C7 C8 1.515(6) . ? C7 C10 1.534(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.521(5) . ? C12 C15 1.521(6) . ? C12 C13 1.524(6) . ? C12 C14 1.527(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.525(5) . ? C17 C20 1.482(6) . ? C17 C18 1.506(6) . ? C17 C19 1.521(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.536(5) . ? C22 C25 1.518(6) . ? C22 C24 1.531(6) . ? C22 C23 1.532(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.371(5) . ? C26 H26 0.9500 . ? C27 C28 1.363(6) . ? C27 H27 0.9500 . ? C28 C29 1.373(6) . ? C28 H28 0.9500 . ? C29 C30 1.378(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(6) . ? C31 H31 0.9500 . ? C32 C33 1.356(6) . ? C32 H32 0.9500 . ? C33 C34 1.367(6) . ? C33 H33 0.9500 . ? C34 C35 1.375(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.377(5) . ? C36 H36 0.9500 . ? C37 C38 1.371(5) . ? C37 H37 0.9500 . ? C38 C39 1.365(5) . ? C38 H38 0.9500 . ? C39 C40 1.375(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 O7 Zn1 O10 87.30(11) . . ? O7 Zn1 O6 88.98(11) . . ? O10 Zn1 O6 166.65(10) . . ? O7 Zn1 N3 90.32(11) . . ? O10 Zn1 N3 97.60(10) . . ? O6 Zn1 N3 95.24(10) . . ? O7 Zn1 N2 170.15(11) . . ? O10 Zn1 N2 90.48(11) . . ? O6 Zn1 N2 91.01(11) . . ? N3 Zn1 N2 99.49(11) . . ? O8 Dy1 O5 77.52(9) . . ? O8 Dy1 O9 81.12(9) . . ? O5 Dy1 O9 92.35(9) . . ? O8 Dy1 O1 80.62(9) . . ? O5 Dy1 O1 92.96(10) . . ? O9 Dy1 O1 159.40(9) . . ? O8 Dy1 O4 129.15(9) . . ? O5 Dy1 O4 152.38(9) . . ? O9 Dy1 O4 86.08(9) . . ? O1 Dy1 O4 98.15(10) . . ? O8 Dy1 O3 76.56(9) . . ? O5 Dy1 O3 153.87(9) . . ? O9 Dy1 O3 86.87(10) . . ? O1 Dy1 O3 79.68(11) . . ? O4 Dy1 O3 53.66(9) . . ? O8 Dy1 O2 130.17(9) . . ? O5 Dy1 O2 85.79(9) . . ? O9 Dy1 O2 146.89(9) . . ? O1 Dy1 O2 53.48(8) . . ? O4 Dy1 O2 80.80(9) . . ? O3 Dy1 O2 108.70(10) . . ? O8 Dy1 N1 142.66(9) . . ? O5 Dy1 N1 75.92(9) . . ? O9 Dy1 N1 74.27(9) . . ? O1 Dy1 N1 126.33(9) . . ? O4 Dy1 N1 77.13(9) . . ? O3 Dy1 N1 128.45(10) . . ? O2 Dy1 N1 73.22(8) . . ? C26 N1 C30 116.6(3) . . ? C26 N1 Dy1 121.6(2) . . ? C30 N1 Dy1 121.7(2) . . ? C35 N2 C31 116.7(3) . . ? C35 N2 Zn1 120.9(3) . . ? C31 N2 Zn1 122.2(3) . . ? C36 N3 C40 117.6(3) . . ? C36 N3 Zn1 118.8(2) . . ? C40 N3 Zn1 122.7(2) . . ? C1 O1 Dy1 94.3(2) . . ? C1 O2 Dy1 92.1(2) . . ? C6 O3 Dy1 93.0(2) . . ? C6 O4 Dy1 93.3(2) . . ? C11 O5 Dy1 151.5(2) . . ? C11 O6 Zn1 113.1(2) . . ? C16 O7 Zn1 134.3(2) . . ? C16 O8 Dy1 143.6(2) . . ? C21 O9 Dy1 161.3(2) . . ? C21 O10 Zn1 116.2(2) . . ? O2 C1 O1 119.5(3) . . ? O2 C1 C2 121.3(3) . . ? O1 C1 C2 119.2(3) . . ? C5 C2 C4 110.7(4) . . ? C5 C2 C3 109.1(4) . . ? C4 C2 C3 109.3(4) . . ? C5 C2 C1 111.3(3) . . ? C4 C2 C1 108.9(3) . . ? C3 C2 C1 107.4(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 119.9(3) . . ? O3 C6 C7 120.0(4) . . ? O4 C6 C7 120.0(4) . . ? C9 C7 C8 109.6(4) . . ? C9 C7 C6 110.8(4) . . ? C8 C7 C6 110.4(3) . . ? C9 C7 C10 112.2(5) . . ? C8 C7 C10 108.9(4) . . ? C6 C7 C10 105.0(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.0(3) . . ? O6 C11 C12 118.9(3) . . ? O5 C11 C12 119.1(3) . . ? C11 C12 C15 105.9(3) . . ? C11 C12 C13 111.0(3) . . ? C15 C12 C13 111.1(4) . . ? C11 C12 C14 109.6(3) . . ? C15 C12 C14 109.9(4) . . ? C13 C12 C14 109.3(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 125.1(3) . . ? O7 C16 C17 117.0(3) . . ? O8 C16 C17 117.8(3) . . ? C20 C17 C18 113.8(5) . . ? C20 C17 C19 107.4(4) . . ? C18 C17 C19 107.9(4) . . ? C20 C17 C16 111.9(3) . . ? C18 C17 C16 106.0(3) . . ? C19 C17 C16 109.8(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 123.2(3) . . ? O9 C21 C22 119.1(3) . . ? O10 C21 C22 117.7(3) . . ? C25 C22 C24 109.7(4) . . ? C25 C22 C23 110.7(4) . . ? C24 C22 C23 109.8(4) . . ? C25 C22 C21 110.7(3) . . ? C24 C22 C21 109.3(3) . . ? C23 C22 C21 106.5(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 123.3(4) . . ? N1 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C28 C27 C26 119.3(4) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 118.8(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 118.5(4) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? N1 C30 C29 123.5(4) . . ? N1 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N2 C31 C32 122.6(4) . . ? N2 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 117.9(4) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C33 C34 C35 119.4(5) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N2 C35 C34 123.4(4) . . ? N2 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? N3 C36 C37 122.5(4) . . ? N3 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 119.0(4) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 C37 119.1(4) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.8(4) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N3 C40 C39 122.9(4) . . ? N3 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.657 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.069 #===END data_7jy231s _database_code_depnum_ccdc_archive 'CCDC 753911' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ErZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 Er N3 O10 Zn' _chemical_formula_weight 975.54 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5126(17) _cell_length_b 20.340(3) _cell_length_c 20.152(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.118(2) _cell_angle_gamma 90.00 _cell_volume 4613.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 2.379 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.343 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28061 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 23.30 _reflns_number_total 6645 _reflns_number_gt 6269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+3.5607P] 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 6645 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Zn1 Zn 0.79461(3) 0.316996(13) 0.318191(15) 0.02853(8) Uani 1 1 d . . . Er1 Er 0.975971(10) 0.186712(5) 0.241171(5) 0.02435(5) Uani 1 1 d . . . N1 N 0.77147(18) 0.13266(10) 0.20701(11) 0.0301(5) Uani 1 1 d . . . N2 N 0.62112(19) 0.27525(11) 0.28142(11) 0.0360(5) Uani 1 1 d . . . N3 N 0.74618(18) 0.39921(10) 0.36810(10) 0.0290(5) Uani 1 1 d . . . O1 O 1.11109(18) 0.20614(12) 0.17027(10) 0.0517(6) Uani 1 1 d . . . O2 O 0.95526(16) 0.14901(9) 0.12534(9) 0.0359(4) Uani 1 1 d . . . O3 O 1.15424(18) 0.14256(10) 0.30968(12) 0.0561(6) Uani 1 1 d . . . O4 O 1.01930(16) 0.07323(9) 0.26143(9) 0.0416(5) Uani 1 1 d . . . O5 O 0.85455(15) 0.27011(8) 0.19554(9) 0.0319(4) Uani 1 1 d . . . O6 O 0.78770(17) 0.36401(9) 0.22704(9) 0.0396(5) Uani 1 1 d . . . O7 O 0.96913(16) 0.34282(10) 0.34658(10) 0.0440(5) Uani 1 1 d . . . O8 O 1.07123(17) 0.27589(9) 0.29375(10) 0.0397(5) Uani 1 1 d . . . O9 O 0.90256(18) 0.18410(8) 0.33695(9) 0.0374(5) Uani 1 1 d . . . O10 O 0.82331(16) 0.25355(9) 0.39881(9) 0.0375(4) Uani 1 1 d . . . C1 C 1.0555(2) 0.17118(13) 0.12239(13) 0.0295(6) Uani 1 1 d . . . C2 C 1.1116(2) 0.15692(15) 0.06174(14) 0.0392(7) Uani 1 1 d . . . C3 C 1.1105(5) 0.2208(2) 0.0219(2) 0.1031(18) Uani 1 1 d . . . H3A H 1.0282 0.2343 0.0039 0.155 Uiso 1 1 calc R . . H3B H 1.1509 0.2140 -0.0158 0.155 Uiso 1 1 calc R . . H3C H 1.1517 0.2552 0.0519 0.155 Uiso 1 1 calc R . . C4 C 1.2386(3) 0.1350(3) 0.0874(2) 0.0922(17) Uani 1 1 d . . . H4A H 1.2821 0.1690 0.1171 0.138 Uiso 1 1 calc R . . H4B H 1.2766 0.1278 0.0488 0.138 Uiso 1 1 calc R . . H4C H 1.2395 0.0939 0.1129 0.138 Uiso 1 1 calc R . . C5 C 1.0435(3) 0.10485(19) 0.01645(16) 0.0572(9) Uani 1 1 d . . . H5A H 1.0487 0.0631 0.0411 0.086 Uiso 1 1 calc R . . H5B H 1.0775 0.0995 -0.0239 0.086 Uiso 1 1 calc R . . H5C H 0.9600 0.1181 0.0027 0.086 Uiso 1 1 calc R . . C6 C 1.1205(3) 0.08439(14) 0.29693(13) 0.0362(6) Uani 1 1 d . . . C7 C 1.2060(3) 0.02800(15) 0.32198(16) 0.0502(8) Uani 1 1 d . . . C8 C 1.2833(3) 0.04397(19) 0.39063(18) 0.0670(11) Uani 1 1 d . . . H8A H 1.2333 0.0488 0.4241 0.101 Uiso 1 1 calc R . . H8B H 1.3262 0.0851 0.3876 0.101 Uiso 1 1 calc R . . H8C H 1.3405 0.0083 0.4046 0.101 Uiso 1 1 calc R . . C9 C 1.1384(4) -0.03450(18) 0.3264(3) 0.1027(18) Uani 1 1 d . . . H9A H 1.0820 -0.0277 0.3560 0.154 Uiso 1 1 calc R . . H9B H 1.1941 -0.0696 0.3451 0.154 Uiso 1 1 calc R . . H9C H 1.0951 -0.0470 0.2810 0.154 Uiso 1 1 calc R . . C10 C 1.2848(4) 0.0225(2) 0.2695(2) 0.1011(18) Uani 1 1 d . . . H10A H 1.3449 -0.0117 0.2837 0.152 Uiso 1 1 calc R . . H10B H 1.3243 0.0647 0.2661 0.152 Uiso 1 1 calc R . . H10C H 1.2357 0.0109 0.2251 0.152 Uiso 1 1 calc R . . C11 C 0.8307(2) 0.33028(13) 0.18594(13) 0.0294(6) Uani 1 1 d . . . C12 C 0.8574(3) 0.36334(13) 0.12310(14) 0.0393(7) Uani 1 1 d . . . C13 C 0.7872(4) 0.42714(16) 0.10729(18) 0.0773(13) Uani 1 1 d . . . H13A H 0.7020 0.4177 0.1000 0.116 Uiso 1 1 calc R . . H13B H 0.8048 0.4471 0.0662 0.116 Uiso 1 1 calc R . . H13C H 0.8097 0.4577 0.1455 0.116 Uiso 1 1 calc R . . C14 C 0.8256(4) 0.31692(15) 0.06255(16) 0.0527(9) Uani 1 1 d . . . H14A H 0.8699 0.2758 0.0728 0.079 Uiso 1 1 calc R . . H14B H 0.8461 0.3375 0.0226 0.079 Uiso 1 1 calc R . . H14C H 0.7401 0.3076 0.0534 0.079 Uiso 1 1 calc R . . C15 C 0.9902(4) 0.3768(2) 0.1389(2) 0.0784(13) Uani 1 1 d . . . H15A H 1.0102 0.4059 0.1783 0.118 Uiso 1 1 calc R . . H15B H 1.0126 0.3978 0.0996 0.118 Uiso 1 1 calc R . . H15C H 1.0334 0.3352 0.1488 0.118 Uiso 1 1 calc R . . C16 C 1.0636(2) 0.32008(11) 0.33543(13) 0.0268(6) Uani 1 1 d . . . C17 C 1.1794(2) 0.34761(14) 0.37802(14) 0.0366(6) Uani 1 1 d . . . C18 C 1.1960(5) 0.3132(3) 0.4456(3) 0.124(3) Uani 1 1 d . . . H18A H 1.2250 0.2684 0.4413 0.187 Uiso 1 1 calc R . . H18B H 1.1199 0.3113 0.4600 0.187 Uiso 1 1 calc R . . H18C H 1.2539 0.3374 0.4794 0.187 Uiso 1 1 calc R . . C19 C 1.1656(4) 0.42088(18) 0.3901(2) 0.0755(12) Uani 1 1 d . . . H19A H 1.2387 0.4378 0.4192 0.113 Uiso 1 1 calc R . . H19B H 1.0988 0.4279 0.4125 0.113 Uiso 1 1 calc R . . H19C H 1.1506 0.4441 0.3466 0.113 Uiso 1 1 calc R . . C20 C 1.2803(4) 0.3394(3) 0.3437(3) 0.110(2) Uani 1 1 d . . . H20A H 1.2983 0.2925 0.3409 0.165 Uiso 1 1 calc R . . H20B H 1.3501 0.3623 0.3696 0.165 Uiso 1 1 calc R . . H20C H 1.2592 0.3579 0.2978 0.165 Uiso 1 1 calc R . . C21 C 0.8755(2) 0.20053(13) 0.39158(13) 0.0307(6) Uani 1 1 d . . . C22 C 0.9014(3) 0.15316(15) 0.45197(14) 0.0414(7) Uani 1 1 d . . . C23 C 0.7840(4) 0.11969(19) 0.4552(2) 0.0723(11) Uani 1 1 d . . . H23A H 0.7257 0.1530 0.4614 0.108 Uiso 1 1 calc R . . H23B H 0.7965 0.0889 0.4934 0.108 Uiso 1 1 calc R . . H23C H 0.7545 0.0957 0.4128 0.108 Uiso 1 1 calc R . . C24 C 0.9454(4) 0.19202(17) 0.51724(16) 0.0607(10) Uani 1 1 d . . . H24A H 1.0195 0.2146 0.5147 0.091 Uiso 1 1 calc R . . H24B H 0.9596 0.1619 0.5561 0.091 Uiso 1 1 calc R . . H24C H 0.8853 0.2245 0.5228 0.091 Uiso 1 1 calc R . . C25 C 0.9939(4) 0.10278(18) 0.44315(17) 0.0713(12) Uani 1 1 d . . . H25A H 0.9636 0.0763 0.4026 0.107 Uiso 1 1 calc R . . H25B H 1.0112 0.0741 0.4831 0.107 Uiso 1 1 calc R . . H25C H 1.0667 0.1254 0.4381 0.107 Uiso 1 1 calc R . . C26 C 0.6886(2) 0.15581(13) 0.15586(14) 0.0359(6) Uani 1 1 d . . . H26 H 0.7068 0.1937 0.1324 0.043 Uiso 1 1 calc R . . C27 C 0.5778(3) 0.12769(15) 0.13534(17) 0.0473(8) Uani 1 1 d . . . H27 H 0.5208 0.1465 0.0994 0.057 Uiso 1 1 calc R . . C28 C 0.5515(3) 0.07225(16) 0.16763(17) 0.0522(8) Uani 1 1 d . . . H28 H 0.4759 0.0518 0.1544 0.063 Uiso 1 1 calc R . . C29 C 0.6360(3) 0.04661(16) 0.21940(17) 0.0522(8) Uani 1 1 d . . . H29 H 0.6205 0.0077 0.2422 0.063 Uiso 1 1 calc R . . C30 C 0.7440(3) 0.07838(14) 0.23776(14) 0.0405(7) Uani 1 1 d . . . H30 H 0.8017 0.0607 0.2741 0.049 Uiso 1 1 calc R . . C31 C 0.5484(3) 0.29650(16) 0.22504(15) 0.0455(7) Uani 1 1 d . . . H31 H 0.5774 0.3281 0.1978 0.055 Uiso 1 1 calc R . . C32 C 0.4333(3) 0.27474(19) 0.20459(17) 0.0573(9) Uani 1 1 d . . . H32 H 0.3842 0.2916 0.1643 0.069 Uiso 1 1 calc R . . C33 C 0.3897(3) 0.22865(18) 0.24252(19) 0.0583(10) Uani 1 1 d . . . H33 H 0.3105 0.2129 0.2292 0.070 Uiso 1 1 calc R . . C34 C 0.4634(3) 0.20616(19) 0.2998(2) 0.0646(10) Uani 1 1 d . . . H34 H 0.4363 0.1740 0.3272 0.078 Uiso 1 1 calc R . . C35 C 0.5774(3) 0.23035(16) 0.31790(18) 0.0537(8) Uani 1 1 d . . . H35 H 0.6274 0.2143 0.3583 0.064 Uiso 1 1 calc R . . C36 C 0.8224(2) 0.42209(13) 0.42231(13) 0.0335(6) Uani 1 1 d . . . H36 H 0.8902 0.3964 0.4413 0.040 Uiso 1 1 calc R . . C37 C 0.8066(3) 0.48165(14) 0.45184(15) 0.0424(7) Uani 1 1 d . . . H37 H 0.8620 0.4964 0.4908 0.051 Uiso 1 1 calc R . . C38 C 0.7094(3) 0.51945(13) 0.42420(15) 0.0410(7) Uani 1 1 d . . . H38 H 0.6977 0.5611 0.4432 0.049 Uiso 1 1 calc R . . C39 C 0.6298(3) 0.49613(13) 0.36883(14) 0.0406(7) Uani 1 1 d . . . H39 H 0.5612 0.5208 0.3492 0.049 Uiso 1 1 calc R . . C40 C 0.6517(2) 0.43616(13) 0.34231(13) 0.0357(6) Uani 1 1 d . . . H40 H 0.5968 0.4203 0.3037 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02844(17) 0.02607(16) 0.03008(17) -0.00472(12) 0.00389(13) 0.00447(12) Er1 0.02667(8) 0.02258(8) 0.02352(8) -0.00489(4) 0.00462(5) 0.00203(4) N1 0.0311(12) 0.0289(12) 0.0319(12) -0.0039(10) 0.0105(10) 0.0018(9) N2 0.0330(12) 0.0353(13) 0.0380(13) -0.0084(11) 0.0036(11) 0.0014(10) N3 0.0333(12) 0.0260(11) 0.0289(12) -0.0001(9) 0.0095(10) 0.0040(9) O1 0.0378(12) 0.0793(15) 0.0418(12) -0.0307(11) 0.0168(10) -0.0254(11) O2 0.0364(11) 0.0411(11) 0.0332(10) -0.0140(8) 0.0143(8) -0.0137(9) O3 0.0420(12) 0.0398(13) 0.0749(16) -0.0011(11) -0.0146(11) 0.0079(10) O4 0.0427(12) 0.0296(11) 0.0454(12) -0.0052(8) -0.0068(10) 0.0074(8) O5 0.0341(10) 0.0238(10) 0.0356(10) 0.0022(8) 0.0026(8) 0.0017(8) O6 0.0493(12) 0.0333(10) 0.0372(11) -0.0025(9) 0.0113(9) 0.0074(9) O7 0.0285(11) 0.0446(12) 0.0581(13) -0.0203(10) 0.0069(9) 0.0002(9) O8 0.0420(11) 0.0341(11) 0.0416(11) -0.0174(9) 0.0053(9) -0.0033(9) O9 0.0499(12) 0.0378(11) 0.0256(10) -0.0017(8) 0.0105(9) 0.0054(8) O10 0.0431(11) 0.0369(11) 0.0325(10) 0.0024(8) 0.0081(9) 0.0125(9) C1 0.0269(14) 0.0309(14) 0.0303(15) -0.0017(12) 0.0051(11) 0.0005(12) C2 0.0321(15) 0.0526(18) 0.0357(16) -0.0127(14) 0.0130(12) -0.0033(13) C3 0.170(5) 0.076(3) 0.094(3) 0.005(3) 0.100(4) -0.007(3) C4 0.0340(19) 0.179(5) 0.063(2) -0.063(3) 0.0070(17) 0.015(2) C5 0.0443(18) 0.088(3) 0.0424(18) -0.0311(18) 0.0163(15) -0.0081(17) C6 0.0449(17) 0.0333(16) 0.0289(14) -0.0030(12) 0.0044(13) 0.0096(13) C7 0.056(2) 0.0428(18) 0.0463(18) -0.0044(14) -0.0018(15) 0.0210(15) C8 0.065(2) 0.068(2) 0.056(2) 0.0002(18) -0.0140(18) 0.0313(19) C9 0.097(3) 0.037(2) 0.148(5) 0.014(2) -0.035(3) 0.014(2) C10 0.114(4) 0.116(4) 0.075(3) 0.004(3) 0.024(3) 0.087(3) C11 0.0272(14) 0.0288(15) 0.0280(14) -0.0026(12) -0.0036(11) -0.0017(11) C12 0.0591(19) 0.0291(15) 0.0277(14) 0.0020(11) 0.0044(13) -0.0061(13) C13 0.148(4) 0.0363(19) 0.042(2) 0.0085(15) 0.008(2) 0.020(2) C14 0.078(3) 0.050(2) 0.0295(17) -0.0023(13) 0.0083(16) 0.0015(16) C15 0.079(3) 0.093(3) 0.062(2) 0.015(2) 0.013(2) -0.048(2) C16 0.0315(15) 0.0225(13) 0.0253(14) 0.0002(11) 0.0031(11) -0.0012(11) C17 0.0327(15) 0.0408(16) 0.0344(15) -0.0063(12) 0.0024(12) -0.0057(12) C18 0.108(4) 0.140(5) 0.090(4) 0.062(3) -0.060(3) -0.067(3) C19 0.071(3) 0.062(2) 0.094(3) -0.042(2) 0.020(2) -0.028(2) C20 0.045(2) 0.158(5) 0.133(4) -0.094(4) 0.031(3) -0.030(3) C21 0.0307(14) 0.0353(15) 0.0255(15) -0.0012(11) 0.0046(11) 0.0012(12) C22 0.0553(18) 0.0410(17) 0.0299(15) 0.0052(13) 0.0132(14) 0.0121(14) C23 0.088(3) 0.062(2) 0.069(2) 0.029(2) 0.024(2) -0.006(2) C24 0.079(3) 0.070(2) 0.0295(17) 0.0047(15) 0.0035(17) 0.0183(19) C25 0.102(3) 0.068(2) 0.046(2) 0.0174(18) 0.022(2) 0.047(2) C26 0.0352(16) 0.0277(14) 0.0437(16) -0.0021(12) 0.0055(13) 0.0008(12) C27 0.0358(17) 0.0427(18) 0.059(2) -0.0063(15) -0.0001(14) -0.0010(14) C28 0.0346(17) 0.057(2) 0.067(2) -0.0111(17) 0.0155(16) -0.0146(15) C29 0.053(2) 0.0489(19) 0.061(2) 0.0022(16) 0.0253(17) -0.0164(16) C30 0.0458(18) 0.0403(16) 0.0380(16) 0.0031(13) 0.0142(13) -0.0037(13) C31 0.0403(17) 0.0551(19) 0.0384(17) -0.0091(14) 0.0024(14) 0.0028(15) C32 0.0376(18) 0.082(3) 0.0458(19) -0.0213(18) -0.0055(15) 0.0055(17) C33 0.0346(18) 0.072(2) 0.068(2) -0.034(2) 0.0114(17) -0.0079(17) C34 0.051(2) 0.064(2) 0.079(3) -0.004(2) 0.017(2) -0.0161(18) C35 0.0406(18) 0.053(2) 0.065(2) 0.0055(17) 0.0049(16) -0.0067(15) C36 0.0349(15) 0.0358(15) 0.0309(14) -0.0031(12) 0.0094(12) 0.0031(12) C37 0.0492(18) 0.0448(17) 0.0363(16) -0.0131(14) 0.0159(14) -0.0068(15) C38 0.064(2) 0.0237(14) 0.0432(17) -0.0006(13) 0.0294(16) 0.0035(14) C39 0.0574(19) 0.0306(15) 0.0370(16) 0.0090(13) 0.0169(14) 0.0164(14) C40 0.0420(16) 0.0349(15) 0.0293(14) 0.0016(12) 0.0057(12) 0.0087(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 2.0389(19) . ? Zn1 O10 2.0465(18) . ? Zn1 O6 2.0574(19) . ? Zn1 N3 2.087(2) . ? Zn1 N2 2.154(2) . ? Er1 O9 2.2643(19) . ? Er1 O8 2.2645(18) . ? Er1 O5 2.2666(17) . ? Er1 O1 2.3560(19) . ? Er1 O4 2.3787(19) . ? Er1 O3 2.395(2) . ? Er1 O2 2.4206(17) . ? Er1 N1 2.558(2) . ? N1 C26 1.335(3) . ? N1 C30 1.336(3) . ? N2 C31 1.334(4) . ? N2 C35 1.335(4) . ? N3 C36 1.333(3) . ? N3 C40 1.334(3) . ? O1 C1 1.260(3) . ? O2 C1 1.252(3) . ? O3 C6 1.255(3) . ? O4 C6 1.254(3) . ? O5 C11 1.260(3) . ? O6 C11 1.255(3) . ? O7 C16 1.245(3) . ? O8 C16 1.246(3) . ? O9 C21 1.251(3) . ? O10 C21 1.258(3) . ? C1 C2 1.525(4) . ? C2 C5 1.506(4) . ? C2 C4 1.513(4) . ? C2 C3 1.527(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.526(4) . ? C7 C9 1.503(5) . ? C7 C8 1.515(4) . ? C7 C10 1.537(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.521(4) . ? C12 C15 1.519(5) . ? C12 C14 1.525(4) . ? C12 C13 1.527(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.532(4) . ? C17 C20 1.482(5) . ? C17 C18 1.506(5) . ? C17 C19 1.524(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.532(4) . ? C22 C25 1.515(4) . ? C22 C23 1.526(5) . ? C22 C24 1.527(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.379(4) . ? C26 H26 0.9500 . ? C27 C28 1.367(4) . ? C27 H27 0.9500 . ? C28 C29 1.371(5) . ? C28 H28 0.9500 . ? C29 C30 1.382(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.376(4) . ? C31 H31 0.9500 . ? C32 C33 1.370(5) . ? C32 H32 0.9500 . ? C33 C34 1.360(5) . ? C33 H33 0.9500 . ? C34 C35 1.378(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.378(4) . ? C36 H36 0.9500 . ? C37 C38 1.375(4) . ? C37 H37 0.9500 . ? C38 C39 1.371(4) . ? C38 H38 0.9500 . ? C39 C40 1.376(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 O7 Zn1 O10 87.38(8) . . ? O7 Zn1 O6 88.96(8) . . ? O10 Zn1 O6 166.23(7) . . ? O7 Zn1 N3 90.32(8) . . ? O10 Zn1 N3 97.91(8) . . ? O6 Zn1 N3 95.37(8) . . ? O7 Zn1 N2 170.47(8) . . ? O10 Zn1 N2 90.46(8) . . ? O6 Zn1 N2 90.97(8) . . ? N3 Zn1 N2 99.18(8) . . ? O9 Er1 O8 81.41(7) . . ? O9 Er1 O5 93.13(7) . . ? O8 Er1 O5 77.71(7) . . ? O9 Er1 O1 158.90(7) . . ? O8 Er1 O1 80.38(7) . . ? O5 Er1 O1 93.32(8) . . ? O9 Er1 O4 86.18(6) . . ? O8 Er1 O4 129.31(7) . . ? O5 Er1 O4 152.27(6) . . ? O1 Er1 O4 97.21(8) . . ? O9 Er1 O3 85.86(8) . . ? O8 Er1 O3 76.02(7) . . ? O5 Er1 O3 153.57(7) . . ? O1 Er1 O3 79.48(8) . . ? O4 Er1 O3 54.10(7) . . ? O9 Er1 O2 146.68(6) . . ? O8 Er1 O2 130.17(6) . . ? O5 Er1 O2 85.32(6) . . ? O1 Er1 O2 54.01(6) . . ? O4 Er1 O2 80.37(6) . . ? O3 Er1 O2 109.64(7) . . ? O9 Er1 N1 74.47(7) . . ? O8 Er1 N1 142.95(7) . . ? O5 Er1 N1 76.00(6) . . ? O1 Er1 N1 126.61(7) . . ? O4 Er1 N1 77.12(7) . . ? O3 Er1 N1 128.52(7) . . ? O2 Er1 N1 72.88(6) . . ? C26 N1 C30 116.7(2) . . ? C26 N1 Er1 121.64(17) . . ? C30 N1 Er1 121.62(18) . . ? C31 N2 C35 116.7(3) . . ? C31 N2 Zn1 122.4(2) . . ? C35 N2 Zn1 120.6(2) . . ? C36 N3 C40 117.7(2) . . ? C36 N3 Zn1 118.56(17) . . ? C40 N3 Zn1 122.82(17) . . ? C1 O1 Er1 94.35(16) . . ? C1 O2 Er1 91.52(15) . . ? C6 O3 Er1 92.57(16) . . ? C6 O4 Er1 93.36(16) . . ? C11 O5 Er1 152.24(16) . . ? C11 O6 Zn1 112.87(16) . . ? C16 O7 Zn1 134.46(17) . . ? C16 O8 Er1 142.91(18) . . ? C21 O9 Er1 161.89(18) . . ? C21 O10 Zn1 116.76(16) . . ? O2 C1 O1 119.5(2) . . ? O2 C1 C2 121.3(2) . . ? O1 C1 C2 119.3(2) . . ? C5 C2 C4 110.0(3) . . ? C5 C2 C1 111.4(2) . . ? C4 C2 C1 108.9(2) . . ? C5 C2 C3 109.5(3) . . ? C4 C2 C3 109.3(3) . . ? C1 C2 C3 107.6(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 119.9(2) . . ? O4 C6 C7 120.7(3) . . ? O3 C6 C7 119.4(3) . . ? C9 C7 C8 109.9(3) . . ? C9 C7 C6 110.5(3) . . ? C8 C7 C6 110.8(2) . . ? C9 C7 C10 111.5(4) . . ? C8 C7 C10 109.0(3) . . ? C6 C7 C10 105.1(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.2(2) . . ? O6 C11 C12 119.0(2) . . ? O5 C11 C12 118.8(2) . . ? C15 C12 C11 106.0(2) . . ? C15 C12 C14 109.9(3) . . ? C11 C12 C14 109.6(2) . . ? C15 C12 C13 110.9(3) . . ? C11 C12 C13 111.0(3) . . ? C14 C12 C13 109.4(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 125.3(2) . . ? O7 C16 C17 117.0(2) . . ? O8 C16 C17 117.7(2) . . ? C20 C17 C18 114.0(4) . . ? C20 C17 C19 107.7(3) . . ? C18 C17 C19 107.9(3) . . ? C20 C17 C16 111.8(3) . . ? C18 C17 C16 105.5(3) . . ? C19 C17 C16 109.9(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 123.0(2) . . ? O9 C21 C22 119.2(2) . . ? O10 C21 C22 117.7(2) . . ? C25 C22 C23 110.7(3) . . ? C25 C22 C24 109.7(3) . . ? C23 C22 C24 109.3(3) . . ? C25 C22 C21 110.9(2) . . ? C23 C22 C21 106.7(3) . . ? C24 C22 C21 109.4(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 123.5(3) . . ? N1 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C28 C27 C26 118.9(3) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 118.9(3) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 118.8(3) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N1 C30 C29 123.3(3) . . ? N1 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N2 C31 C32 122.9(3) . . ? N2 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C33 C32 C31 119.7(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 117.9(3) . . ? C34 C33 H33 121.1 . . ? C32 C33 H33 121.1 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N2 C35 C34 123.2(3) . . ? N2 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N3 C36 C37 122.4(3) . . ? N3 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 119.1(3) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 118.9(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 118.5(3) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? N3 C40 C39 123.3(3) . . ? N3 C40 H40 118.4 . . ? C39 C40 H40 118.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.703 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.056 #===END data_7jy111ss _database_code_depnum_ccdc_archive 'CCDC 753912' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common YZnOBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 N3 O10 Y Zn' _chemical_formula_weight 897.19 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5200(17) _cell_length_b 20.366(3) _cell_length_c 20.187(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.118(2) _cell_angle_gamma 90.00 _cell_volume 4630.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9369 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.24 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.818 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33616 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.39 _reflns_number_total 8512 _reflns_number_gt 6728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+2.0564P] 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 8512 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Zn1 Zn 0.79461(2) 0.317149(13) 0.318625(14) 0.02835(8) Uani 1 1 d . . . Y1 Y 0.975939(19) 0.186584(11) 0.241231(11) 0.02429(7) Uani 1 1 d . . . N1 N 0.77018(17) 0.13214(9) 0.20673(10) 0.0292(5) Uani 1 1 d . . . N2 N 0.62134(18) 0.27523(10) 0.28184(11) 0.0348(5) Uani 1 1 d . . . N3 N 0.74625(18) 0.39924(9) 0.36814(10) 0.0284(5) Uani 1 1 d . . . O1 O 1.11087(17) 0.20661(11) 0.16969(10) 0.0518(6) Uani 1 1 d . . . O2 O 0.95581(15) 0.14870(9) 0.12540(8) 0.0355(4) Uani 1 1 d . . . O3 O 1.15489(18) 0.14225(10) 0.30931(11) 0.0558(6) Uani 1 1 d . . . O4 O 1.01911(16) 0.07290(9) 0.26191(9) 0.0415(5) Uani 1 1 d . . . O5 O 0.85364(15) 0.27014(8) 0.19531(8) 0.0323(4) Uani 1 1 d . . . O6 O 0.78770(16) 0.36385(9) 0.22739(9) 0.0393(4) Uani 1 1 d . . . O7 O 0.96938(15) 0.34317(9) 0.34723(10) 0.0436(5) Uani 1 1 d . . . O8 O 1.07042(16) 0.27609(9) 0.29405(9) 0.0403(4) Uani 1 1 d . . . O9 O 0.90148(17) 0.18429(8) 0.33689(8) 0.0377(4) Uani 1 1 d . . . O10 O 0.82343(15) 0.25372(9) 0.39918(8) 0.0378(4) Uani 1 1 d . . . C1 C 1.0552(2) 0.17135(12) 0.12212(12) 0.0295(5) Uani 1 1 d . . . C2 C 1.1117(2) 0.15701(15) 0.06143(13) 0.0386(6) Uani 1 1 d . . . C3 C 1.1101(5) 0.2210(2) 0.0216(2) 0.1031(17) Uani 1 1 d . . . H3A H 1.0277 0.2345 0.0042 0.155 Uiso 1 1 calc R . . H3B H 1.1496 0.2141 -0.0163 0.155 Uiso 1 1 calc R . . H3C H 1.1518 0.2552 0.0515 0.155 Uiso 1 1 calc R . . C4 C 1.2389(3) 0.1357(3) 0.08711(19) 0.0894(15) Uani 1 1 d . . . H4A H 1.2821 0.1701 0.1162 0.134 Uiso 1 1 calc R . . H4B H 1.2768 0.1282 0.0486 0.134 Uiso 1 1 calc R . . H4C H 1.2404 0.0950 0.1131 0.134 Uiso 1 1 calc R . . C5 C 1.0441(3) 0.10478(18) 0.01633(15) 0.0585(9) Uani 1 1 d . . . H5A H 1.0472 0.0635 0.0416 0.088 Uiso 1 1 calc R . . H5B H 1.0798 0.0983 -0.0232 0.088 Uiso 1 1 calc R . . H5C H 0.9612 0.1185 0.0012 0.088 Uiso 1 1 calc R . . C6 C 1.1208(2) 0.08448(13) 0.29718(13) 0.0367(6) Uani 1 1 d . . . C7 C 1.2055(3) 0.02749(14) 0.32219(15) 0.0498(8) Uani 1 1 d . . . C8 C 1.2833(3) 0.04356(18) 0.39058(16) 0.0680(10) Uani 1 1 d . . . H8A H 1.2340 0.0469 0.4245 0.102 Uiso 1 1 calc R . . H8B H 1.3238 0.0855 0.3878 0.102 Uiso 1 1 calc R . . H8C H 1.3423 0.0087 0.4036 0.102 Uiso 1 1 calc R . . C9 C 1.1385(4) -0.03468(17) 0.3270(3) 0.1061(18) Uani 1 1 d . . . H9A H 1.0834 -0.0280 0.3574 0.159 Uiso 1 1 calc R . . H9B H 1.1945 -0.0698 0.3449 0.159 Uiso 1 1 calc R . . H9C H 1.0938 -0.0469 0.2819 0.159 Uiso 1 1 calc R . . C10 C 1.2842(4) 0.0221(2) 0.2696(2) 0.1050(18) Uani 1 1 d . . . H10A H 1.3417 -0.0135 0.2824 0.157 Uiso 1 1 calc R . . H10B H 1.3267 0.0636 0.2679 0.157 Uiso 1 1 calc R . . H10C H 1.2345 0.0129 0.2249 0.157 Uiso 1 1 calc R . . C11 C 0.8297(2) 0.33024(12) 0.18600(12) 0.0285(5) Uani 1 1 d . . . C12 C 0.8561(3) 0.36352(13) 0.12313(13) 0.0391(7) Uani 1 1 d . . . C13 C 0.7854(4) 0.42689(15) 0.10769(17) 0.0762(12) Uani 1 1 d . . . H13A H 0.7004 0.4172 0.1010 0.114 Uiso 1 1 calc R . . H13B H 0.8020 0.4468 0.0665 0.114 Uiso 1 1 calc R . . H13C H 0.8083 0.4574 0.1457 0.114 Uiso 1 1 calc R . . C14 C 0.8249(3) 0.31716(14) 0.06263(14) 0.0515(8) Uani 1 1 d . . . H14A H 0.8692 0.2761 0.0730 0.077 Uiso 1 1 calc R . . H14B H 0.8459 0.3378 0.0229 0.077 Uiso 1 1 calc R . . H14C H 0.7395 0.3079 0.0532 0.077 Uiso 1 1 calc R . . C15 C 0.9894(3) 0.3772(2) 0.13912(19) 0.0773(12) Uani 1 1 d . . . H15A H 1.0092 0.4059 0.1788 0.116 Uiso 1 1 calc R . . H15B H 1.0117 0.3987 0.1002 0.116 Uiso 1 1 calc R . . H15C H 1.0327 0.3357 0.1486 0.116 Uiso 1 1 calc R . . C16 C 1.0633(2) 0.32035(11) 0.33581(12) 0.0275(5) Uani 1 1 d . . . C17 C 1.1795(2) 0.34761(14) 0.37829(13) 0.0367(6) Uani 1 1 d . . . C18 C 1.1954(4) 0.3136(2) 0.4464(2) 0.121(2) Uani 1 1 d . . . H18A H 1.2220 0.2684 0.4423 0.181 Uiso 1 1 calc R . . H18B H 1.1195 0.3132 0.4611 0.181 Uiso 1 1 calc R . . H18C H 1.2548 0.3372 0.4798 0.181 Uiso 1 1 calc R . . C19 C 1.1664(3) 0.42066(18) 0.3902(2) 0.0749(11) Uani 1 1 d . . . H19A H 1.2395 0.4374 0.4191 0.112 Uiso 1 1 calc R . . H19B H 1.0996 0.4279 0.4125 0.112 Uiso 1 1 calc R . . H19C H 1.1515 0.4438 0.3467 0.112 Uiso 1 1 calc R . . C20 C 1.2802(3) 0.3385(3) 0.3440(2) 0.1075(18) Uani 1 1 d . . . H20A H 1.2971 0.2916 0.3412 0.161 Uiso 1 1 calc R . . H20B H 1.3506 0.3609 0.3700 0.161 Uiso 1 1 calc R . . H20C H 1.2597 0.3571 0.2983 0.161 Uiso 1 1 calc R . . C21 C 0.8749(2) 0.20066(12) 0.39181(12) 0.0295(6) Uani 1 1 d . . . C22 C 0.9004(3) 0.15321(14) 0.45185(13) 0.0407(7) Uani 1 1 d . . . C23 C 0.7839(3) 0.11938(18) 0.45515(19) 0.0711(11) Uani 1 1 d . . . H23A H 0.7257 0.1523 0.4623 0.107 Uiso 1 1 calc R . . H23B H 0.7972 0.0879 0.4927 0.107 Uiso 1 1 calc R . . H23C H 0.7537 0.0961 0.4125 0.107 Uiso 1 1 calc R . . C24 C 0.9447(3) 0.19197(17) 0.51746(14) 0.0619(10) Uani 1 1 d . . . H24A H 1.0192 0.2143 0.5152 0.093 Uiso 1 1 calc R . . H24B H 0.9583 0.1618 0.5561 0.093 Uiso 1 1 calc R . . H24C H 0.8850 0.2246 0.5230 0.093 Uiso 1 1 calc R . . C25 C 0.9934(4) 0.10281(17) 0.44274(16) 0.0704(11) Uani 1 1 d . . . H25A H 0.9626 0.0761 0.4025 0.106 Uiso 1 1 calc R . . H25B H 1.0117 0.0744 0.4828 0.106 Uiso 1 1 calc R . . H25C H 1.0657 0.1255 0.4371 0.106 Uiso 1 1 calc R . . C26 C 0.6874(2) 0.15554(13) 0.15576(14) 0.0365(6) Uani 1 1 d . . . H26 H 0.7056 0.1934 0.1324 0.044 Uiso 1 1 calc R . . C27 C 0.5768(2) 0.12730(14) 0.13535(16) 0.0473(7) Uani 1 1 d . . . H27 H 0.5196 0.1462 0.0996 0.057 Uiso 1 1 calc R . . C28 C 0.5507(3) 0.07154(16) 0.16742(17) 0.0524(8) Uani 1 1 d . . . H28 H 0.4754 0.0510 0.1542 0.063 Uiso 1 1 calc R . . C29 C 0.6352(3) 0.04621(16) 0.21887(16) 0.0515(8) Uani 1 1 d . . . H29 H 0.6199 0.0073 0.2416 0.062 Uiso 1 1 calc R . . C30 C 0.7426(2) 0.07772(13) 0.23731(14) 0.0397(6) Uani 1 1 d . . . H30 H 0.8001 0.0600 0.2736 0.048 Uiso 1 1 calc R . . C31 C 0.5486(2) 0.29667(15) 0.22540(14) 0.0443(7) Uani 1 1 d . . . H31 H 0.5775 0.3284 0.1984 0.053 Uiso 1 1 calc R . . C32 C 0.4332(3) 0.27456(18) 0.20477(16) 0.0580(9) Uani 1 1 d . . . H32 H 0.3842 0.2912 0.1645 0.070 Uiso 1 1 calc R . . C33 C 0.3900(3) 0.22855(18) 0.24274(18) 0.0577(9) Uani 1 1 d . . . H33 H 0.3111 0.2126 0.2294 0.069 Uiso 1 1 calc R . . C34 C 0.4633(3) 0.20649(18) 0.29992(19) 0.0626(9) Uani 1 1 d . . . H34 H 0.4362 0.1746 0.3274 0.075 Uiso 1 1 calc R . . C35 C 0.5770(3) 0.23052(16) 0.31788(17) 0.0539(8) Uani 1 1 d . . . H35 H 0.6267 0.2144 0.3582 0.065 Uiso 1 1 calc R . . C36 C 0.8221(2) 0.42237(13) 0.42240(12) 0.0338(6) Uani 1 1 d . . . H36 H 0.8897 0.3968 0.4416 0.041 Uiso 1 1 calc R . . C37 C 0.8061(3) 0.48195(13) 0.45152(14) 0.0407(7) Uani 1 1 d . . . H37 H 0.8618 0.4969 0.4902 0.049 Uiso 1 1 calc R . . C38 C 0.7088(3) 0.51952(13) 0.42404(14) 0.0420(7) Uani 1 1 d . . . H38 H 0.6970 0.5611 0.4429 0.050 Uiso 1 1 calc R . . C39 C 0.6289(3) 0.49608(13) 0.36897(14) 0.0398(7) Uani 1 1 d . . . H39 H 0.5600 0.5206 0.3495 0.048 Uiso 1 1 calc R . . C40 C 0.6509(2) 0.43606(13) 0.34262(13) 0.0359(6) Uani 1 1 d . . . H40 H 0.5956 0.4199 0.3044 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02639(16) 0.02719(16) 0.03040(16) -0.00466(12) 0.00350(12) 0.00429(12) Y1 0.02454(13) 0.02420(13) 0.02374(13) -0.00483(9) 0.00421(9) 0.00198(9) N1 0.0292(11) 0.0286(11) 0.0315(11) -0.0030(9) 0.0100(9) 0.0007(9) N2 0.0301(12) 0.0358(12) 0.0361(12) -0.0074(10) 0.0017(10) 0.0016(10) N3 0.0310(11) 0.0267(11) 0.0281(11) 0.0005(9) 0.0079(9) 0.0036(9) O1 0.0373(11) 0.0801(15) 0.0418(11) -0.0309(11) 0.0168(9) -0.0253(10) O2 0.0331(10) 0.0426(11) 0.0339(10) -0.0130(8) 0.0141(8) -0.0126(8) O3 0.0421(12) 0.0371(12) 0.0765(15) -0.0016(11) -0.0139(11) 0.0070(9) O4 0.0408(11) 0.0316(10) 0.0452(11) -0.0042(8) -0.0066(9) 0.0078(8) O5 0.0326(10) 0.0259(9) 0.0373(10) 0.0023(7) 0.0050(8) 0.0013(7) O6 0.0470(11) 0.0343(10) 0.0369(10) -0.0028(8) 0.0097(9) 0.0059(9) O7 0.0269(10) 0.0450(11) 0.0576(13) -0.0186(10) 0.0062(9) 0.0021(8) O8 0.0423(11) 0.0355(10) 0.0414(11) -0.0182(9) 0.0053(9) -0.0038(8) O9 0.0488(11) 0.0393(11) 0.0265(9) -0.0009(8) 0.0113(8) 0.0054(9) O10 0.0406(11) 0.0391(11) 0.0327(10) 0.0012(8) 0.0055(8) 0.0126(8) C1 0.0264(13) 0.0332(14) 0.0294(13) -0.0038(11) 0.0065(11) -0.0001(11) C2 0.0284(14) 0.0551(17) 0.0351(15) -0.0119(13) 0.0129(12) -0.0052(12) C3 0.166(5) 0.076(3) 0.098(3) 0.010(2) 0.099(3) -0.002(3) C4 0.0332(18) 0.171(4) 0.064(2) -0.058(3) 0.0089(16) 0.014(2) C5 0.0449(18) 0.091(3) 0.0429(18) -0.0320(17) 0.0157(15) -0.0077(17) C6 0.0408(16) 0.0356(16) 0.0321(14) -0.0031(12) 0.0042(12) 0.0122(12) C7 0.0541(19) 0.0438(17) 0.0456(17) -0.0032(14) -0.0031(14) 0.0238(15) C8 0.067(2) 0.071(2) 0.056(2) -0.0005(18) -0.0126(17) 0.0320(19) C9 0.101(3) 0.037(2) 0.150(4) 0.012(2) -0.041(3) 0.013(2) C10 0.119(4) 0.122(4) 0.076(3) 0.001(3) 0.023(3) 0.091(3) C11 0.0268(13) 0.0289(14) 0.0265(13) -0.0027(10) -0.0024(10) -0.0027(10) C12 0.0580(18) 0.0291(14) 0.0287(14) 0.0015(11) 0.0059(13) -0.0062(13) C13 0.145(4) 0.0360(18) 0.0432(19) 0.0098(15) 0.009(2) 0.018(2) C14 0.077(2) 0.0466(18) 0.0302(15) -0.0001(13) 0.0092(15) 0.0004(16) C15 0.074(3) 0.091(3) 0.066(2) 0.014(2) 0.013(2) -0.044(2) C16 0.0298(13) 0.0244(12) 0.0271(13) -0.0013(10) 0.0035(10) -0.0001(10) C17 0.0289(14) 0.0418(16) 0.0366(15) -0.0081(12) 0.0004(11) -0.0073(12) C18 0.100(3) 0.140(4) 0.088(3) 0.060(3) -0.059(3) -0.062(3) C19 0.070(2) 0.065(2) 0.091(3) -0.043(2) 0.020(2) -0.0274(19) C20 0.042(2) 0.161(5) 0.124(4) -0.086(4) 0.029(2) -0.028(3) C21 0.0270(13) 0.0351(14) 0.0263(13) 0.0003(10) 0.0052(10) 0.0030(11) C22 0.0528(18) 0.0413(16) 0.0291(14) 0.0054(12) 0.0109(13) 0.0145(14) C23 0.083(3) 0.061(2) 0.070(2) 0.0266(19) 0.019(2) -0.007(2) C24 0.081(2) 0.073(2) 0.0292(16) 0.0046(15) 0.0045(16) 0.0206(19) C25 0.101(3) 0.068(2) 0.0448(19) 0.0174(17) 0.0203(19) 0.047(2) C26 0.0322(14) 0.0291(14) 0.0469(16) -0.0025(12) 0.0052(12) -0.0004(11) C27 0.0296(15) 0.0440(17) 0.064(2) -0.0078(15) -0.0006(14) -0.0009(13) C28 0.0351(17) 0.0530(19) 0.072(2) -0.0113(16) 0.0171(16) -0.0158(14) C29 0.0512(19) 0.0523(19) 0.0558(19) 0.0052(15) 0.0219(16) -0.0164(15) C30 0.0418(16) 0.0429(16) 0.0370(15) 0.0041(12) 0.0140(13) -0.0027(13) C31 0.0373(16) 0.0548(18) 0.0380(16) -0.0105(14) 0.0020(13) 0.0014(13) C32 0.0393(18) 0.081(2) 0.0468(19) -0.0212(18) -0.0056(15) 0.0039(17) C33 0.0339(17) 0.071(2) 0.067(2) -0.0340(19) 0.0084(16) -0.0081(16) C34 0.0442(19) 0.068(2) 0.077(3) -0.0039(19) 0.0160(18) -0.0153(17) C35 0.0389(17) 0.057(2) 0.063(2) 0.0077(16) 0.0051(15) -0.0055(15) C36 0.0343(14) 0.0387(15) 0.0293(13) -0.0041(11) 0.0085(11) 0.0021(12) C37 0.0475(17) 0.0415(16) 0.0349(15) -0.0123(12) 0.0130(13) -0.0078(13) C38 0.063(2) 0.0283(14) 0.0425(16) -0.0024(12) 0.0276(15) 0.0014(14) C39 0.0537(18) 0.0305(14) 0.0384(15) 0.0099(12) 0.0168(14) 0.0164(13) C40 0.0387(15) 0.0367(15) 0.0320(14) 0.0021(11) 0.0069(12) 0.0092(12) _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 Zn1 O7 2.0445(18) . ? Zn1 O10 2.0487(17) . ? Zn1 O6 2.0595(18) . ? Zn1 N3 2.0830(19) . ? Zn1 N2 2.155(2) . ? Y1 O8 2.2710(17) . ? Y1 O9 2.2721(17) . ? Y1 O5 2.2786(16) . ? Y1 O1 2.3687(18) . ? Y1 O4 2.3865(18) . ? Y1 O3 2.4009(19) . ? Y1 O2 2.4268(17) . ? Y1 N1 2.577(2) . ? N1 C26 1.335(3) . ? N1 C30 1.339(3) . ? N2 C35 1.333(4) . ? N2 C31 1.338(3) . ? N3 C36 1.335(3) . ? N3 C40 1.341(3) . ? O1 C1 1.261(3) . ? O2 C1 1.249(3) . ? O3 C6 1.248(3) . ? O4 C6 1.259(3) . ? O5 C11 1.260(3) . ? O6 C11 1.253(3) . ? O7 C16 1.243(3) . ? O8 C16 1.248(3) . ? O9 C21 1.256(3) . ? O10 C21 1.256(3) . ? C1 C2 1.531(3) . ? C2 C5 1.507(4) . ? C2 C4 1.512(4) . ? C2 C3 1.528(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.532(4) . ? C7 C9 1.496(5) . ? C7 C8 1.515(4) . ? C7 C10 1.539(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(4) . ? C12 C13 1.523(4) . ? C12 C14 1.526(4) . ? C12 C15 1.527(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.534(3) . ? C17 C20 1.482(4) . ? C17 C18 1.515(5) . ? C17 C19 1.520(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.530(4) . ? C22 C25 1.522(4) . ? C22 C23 1.523(4) . ? C22 C24 1.534(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.372(4) . ? C27 H27 0.9500 . ? C28 C29 1.367(4) . ? C28 H28 0.9500 . ? C29 C30 1.374(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.369(5) . ? C32 H32 0.9500 . ? C33 C34 1.356(5) . ? C33 H33 0.9500 . ? C34 C35 1.373(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.377(4) . ? C36 H36 0.9500 . ? C37 C38 1.375(4) . ? C37 H37 0.9500 . ? C38 C39 1.372(4) . ? C38 H38 0.9500 . ? C39 C40 1.378(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 O7 Zn1 O10 87.33(8) . . ? O7 Zn1 O6 89.07(8) . . ? O10 Zn1 O6 166.05(7) . . ? O7 Zn1 N3 90.18(8) . . ? O10 Zn1 N3 98.07(7) . . ? O6 Zn1 N3 95.42(7) . . ? O7 Zn1 N2 170.48(8) . . ? O10 Zn1 N2 90.44(8) . . ? O6 Zn1 N2 90.90(8) . . ? N3 Zn1 N2 99.31(8) . . ? O8 Y1 O9 81.18(7) . . ? O8 Y1 O5 77.64(6) . . ? O9 Y1 O5 92.85(6) . . ? O8 Y1 O1 80.61(7) . . ? O9 Y1 O1 159.21(6) . . ? O5 Y1 O1 92.99(7) . . ? O8 Y1 O4 129.41(6) . . ? O9 Y1 O4 86.18(6) . . ? O5 Y1 O4 152.14(6) . . ? O1 Y1 O4 97.72(7) . . ? O8 Y1 O3 76.34(7) . . ? O9 Y1 O3 86.43(7) . . ? O5 Y1 O3 153.77(6) . . ? O1 Y1 O3 79.59(8) . . ? O4 Y1 O3 54.03(6) . . ? O8 Y1 O2 130.32(6) . . ? O9 Y1 O2 146.68(6) . . ? O5 Y1 O2 85.39(6) . . ? O1 Y1 O2 53.80(6) . . ? O4 Y1 O2 80.46(6) . . ? O3 Y1 O2 109.20(7) . . ? O8 Y1 N1 142.68(6) . . ? O9 Y1 N1 74.39(6) . . ? O5 Y1 N1 75.89(6) . . ? O1 Y1 N1 126.40(6) . . ? O4 Y1 N1 77.05(6) . . ? O3 Y1 N1 128.57(7) . . ? O2 Y1 N1 72.92(6) . . ? C26 N1 C30 116.8(2) . . ? C26 N1 Y1 121.47(16) . . ? C30 N1 Y1 121.71(17) . . ? C35 N2 C31 116.4(2) . . ? C35 N2 Zn1 121.09(19) . . ? C31 N2 Zn1 122.24(19) . . ? C36 N3 C40 117.4(2) . . ? C36 N3 Zn1 118.80(16) . . ? C40 N3 Zn1 123.00(17) . . ? C1 O1 Y1 94.15(15) . . ? C1 O2 Y1 91.74(14) . . ? C6 O3 Y1 92.59(16) . . ? C6 O4 Y1 92.98(16) . . ? C11 O5 Y1 152.06(15) . . ? C11 O6 Zn1 113.34(16) . . ? C16 O7 Zn1 134.00(16) . . ? C16 O8 Y1 143.48(17) . . ? C21 O9 Y1 161.90(17) . . ? C21 O10 Zn1 116.76(15) . . ? O2 C1 O1 119.7(2) . . ? O2 C1 C2 121.4(2) . . ? O1 C1 C2 119.0(2) . . ? C5 C2 C4 110.2(3) . . ? C5 C2 C3 109.7(3) . . ? C4 C2 C3 109.2(3) . . ? C5 C2 C1 111.4(2) . . ? C4 C2 C1 108.9(2) . . ? C3 C2 C1 107.3(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 120.3(2) . . ? O3 C6 C7 119.8(2) . . ? O4 C6 C7 119.8(2) . . ? C9 C7 C8 109.8(3) . . ? C9 C7 C6 111.2(3) . . ? C8 C7 C6 110.5(2) . . ? C9 C7 C10 111.8(3) . . ? C8 C7 C10 108.8(3) . . ? C6 C7 C10 104.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.3(2) . . ? O6 C11 C12 119.0(2) . . ? O5 C11 C12 118.7(2) . . ? C13 C12 C11 110.8(2) . . ? C13 C12 C14 109.6(2) . . ? C11 C12 C14 109.7(2) . . ? C13 C12 C15 111.1(3) . . ? C11 C12 C15 105.8(2) . . ? C14 C12 C15 109.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 125.3(2) . . ? O7 C16 C17 116.9(2) . . ? O8 C16 C17 117.7(2) . . ? C20 C17 C18 114.1(4) . . ? C20 C17 C19 108.1(3) . . ? C18 C17 C19 107.5(3) . . ? C20 C17 C16 111.8(2) . . ? C18 C17 C16 105.5(2) . . ? C19 C17 C16 109.8(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 122.8(2) . . ? O9 C21 C22 119.3(2) . . ? O10 C21 C22 117.8(2) . . ? C25 C22 C23 110.4(3) . . ? C25 C22 C21 110.7(2) . . ? C23 C22 C21 107.2(2) . . ? C25 C22 C24 109.6(3) . . ? C23 C22 C24 109.4(3) . . ? C21 C22 C24 109.4(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 123.1(3) . . ? N1 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C28 C27 C26 119.0(3) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C29 C28 C27 118.6(3) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N1 C30 C29 123.3(3) . . ? N1 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N2 C31 C32 122.8(3) . . ? N2 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C33 C32 C31 119.6(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C34 C33 C32 118.0(3) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? N2 C35 C34 123.6(3) . . ? N2 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? N3 C36 C37 122.5(2) . . ? N3 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 119.3(3) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 119.0(2) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 118.4(3) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N3 C40 C39 123.4(3) . . ? N3 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.703 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.058 #===END data_7jy091ss _database_code_depnum_ccdc_archive 'CCDC 753913' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 N3 O10 Yb Zn' _chemical_formula_weight 981.32 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' Yb Yb -0.3850 5.5486 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5153(17) _cell_length_b 20.333(3) _cell_length_c 20.118(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.034(2) _cell_angle_gamma 90.00 _cell_volume 4606.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9792 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.38 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 2.591 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.523 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33354 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.38 _reflns_number_total 8453 _reflns_number_gt 7788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.8266P] 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 8453 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.79471(3) 0.316618(12) 0.317757(14) 0.02845(7) Uani 1 1 d . . . Yb1 Yb 0.977199(8) 0.187021(4) 0.241553(5) 0.02400(5) Uani 1 1 d . . . N1 N 0.77397(18) 0.13347(9) 0.20779(10) 0.0305(4) Uani 1 1 d . . . N2 N 0.62152(18) 0.27488(10) 0.28145(11) 0.0361(5) Uani 1 1 d . . . N3 N 0.74642(18) 0.39892(9) 0.36754(10) 0.0287(4) Uani 1 1 d . . . O1 O 1.11220(17) 0.20554(11) 0.17157(10) 0.0511(5) Uani 1 1 d . . . O2 O 0.95552(15) 0.14922(9) 0.12625(8) 0.0356(4) Uani 1 1 d . . . O3 O 1.15430(17) 0.14355(9) 0.31042(11) 0.0539(5) Uani 1 1 d . . . O4 O 1.02009(15) 0.07443(9) 0.26077(9) 0.0412(5) Uani 1 1 d . . . O5 O 0.85754(15) 0.26965(8) 0.19582(9) 0.0319(4) Uani 1 1 d . . . O6 O 0.78795(17) 0.36348(9) 0.22624(9) 0.0401(4) Uani 1 1 d . . . O7 O 0.96916(16) 0.34254(9) 0.34591(10) 0.0435(5) Uani 1 1 d . . . O8 O 1.07179(16) 0.27538(9) 0.29346(9) 0.0389(4) Uani 1 1 d . . . O9 O 0.90511(18) 0.18392(8) 0.33699(9) 0.0380(4) Uani 1 1 d . . . O10 O 0.82366(16) 0.25295(9) 0.39825(9) 0.0374(4) Uani 1 1 d . . . C1 C 1.0563(2) 0.17106(12) 0.12330(12) 0.0302(5) Uani 1 1 d . . . C2 C 1.1124(2) 0.15656(14) 0.06241(13) 0.0388(6) Uani 1 1 d . . . C3 C 1.1125(5) 0.2204(2) 0.0227(2) 0.1019(17) Uani 1 1 d . . . H3A H 1.0305 0.2348 0.0054 0.153 Uiso 1 1 calc R . . H3B H 1.1517 0.2132 -0.0155 0.153 Uiso 1 1 calc R . . H3C H 1.1554 0.2544 0.0527 0.153 Uiso 1 1 calc R . . C4 C 1.2390(3) 0.1338(3) 0.08810(18) 0.0892(16) Uani 1 1 d . . . H4A H 1.2826 0.1670 0.1188 0.134 Uiso 1 1 calc R . . H4B H 1.2776 0.1274 0.0495 0.134 Uiso 1 1 calc R . . H4C H 1.2389 0.0921 0.1126 0.134 Uiso 1 1 calc R . . C5 C 1.0431(3) 0.10469(19) 0.01699(15) 0.0586(9) Uani 1 1 d . . . H5A H 1.0487 0.0627 0.0414 0.088 Uiso 1 1 calc R . . H5B H 1.0759 0.0997 -0.0239 0.088 Uiso 1 1 calc R . . H5C H 0.9597 0.1180 0.0040 0.088 Uiso 1 1 calc R . . C6 C 1.1212(2) 0.08560(13) 0.29704(13) 0.0368(6) Uani 1 1 d . . . C7 C 1.2057(3) 0.02864(14) 0.32173(15) 0.0505(8) Uani 1 1 d . . . C8 C 1.2835(3) 0.04431(18) 0.39092(17) 0.0662(10) Uani 1 1 d . . . H8A H 1.2335 0.0491 0.4245 0.099 Uiso 1 1 calc R . . H8B H 1.3265 0.0854 0.3881 0.099 Uiso 1 1 calc R . . H8C H 1.3404 0.0085 0.4047 0.099 Uiso 1 1 calc R . . C9 C 1.1381(4) -0.03423(17) 0.3257(3) 0.1001(17) Uani 1 1 d . . . H9A H 1.0821 -0.0278 0.3557 0.150 Uiso 1 1 calc R . . H9B H 1.1939 -0.0694 0.3438 0.150 Uiso 1 1 calc R . . H9C H 1.0944 -0.0463 0.2802 0.150 Uiso 1 1 calc R . . C10 C 1.2850(4) 0.0234(2) 0.2692(2) 0.0937(16) Uani 1 1 d . . . H10A H 1.3467 -0.0097 0.2841 0.141 Uiso 1 1 calc R . . H10B H 1.3221 0.0661 0.2648 0.141 Uiso 1 1 calc R . . H10C H 1.2365 0.0105 0.2251 0.141 Uiso 1 1 calc R . . C11 C 0.8324(2) 0.32970(12) 0.18570(12) 0.0283(5) Uani 1 1 d . . . C12 C 0.8597(3) 0.36269(12) 0.12266(13) 0.0392(6) Uani 1 1 d . . . C13 C 0.7900(4) 0.42663(15) 0.10686(17) 0.0756(12) Uani 1 1 d . . . H13A H 0.7048 0.4173 0.0993 0.113 Uiso 1 1 calc R . . H13B H 0.8083 0.4466 0.0659 0.113 Uiso 1 1 calc R . . H13C H 0.8123 0.4570 0.1452 0.113 Uiso 1 1 calc R . . C14 C 0.8273(3) 0.31630(14) 0.06203(15) 0.0513(8) Uani 1 1 d . . . H14A H 0.8725 0.2754 0.0718 0.077 Uiso 1 1 calc R . . H14B H 0.8464 0.3372 0.0217 0.077 Uiso 1 1 calc R . . H14C H 0.7421 0.3065 0.0535 0.077 Uiso 1 1 calc R . . C15 C 0.9931(3) 0.3755(2) 0.13838(19) 0.0762(12) Uani 1 1 d . . . H15A H 1.0137 0.4042 0.1782 0.114 Uiso 1 1 calc R . . H15B H 1.0156 0.3969 0.0993 0.114 Uiso 1 1 calc R . . H15C H 1.0357 0.3337 0.1477 0.114 Uiso 1 1 calc R . . C16 C 1.0638(2) 0.31985(10) 0.33492(12) 0.0275(5) Uani 1 1 d . . . C17 C 1.1792(2) 0.34805(13) 0.37735(13) 0.0363(6) Uani 1 1 d . . . C18 C 1.1968(5) 0.3130(3) 0.4448(3) 0.130(3) Uani 1 1 d . . . H18A H 1.2254 0.2682 0.4399 0.195 Uiso 1 1 calc R . . H18B H 1.1212 0.3110 0.4598 0.195 Uiso 1 1 calc R . . H18C H 1.2553 0.3369 0.4786 0.195 Uiso 1 1 calc R . . C19 C 1.1642(3) 0.42131(18) 0.3901(2) 0.0758(12) Uani 1 1 d . . . H19A H 1.2373 0.4385 0.4188 0.114 Uiso 1 1 calc R . . H19B H 1.0979 0.4276 0.4130 0.114 Uiso 1 1 calc R . . H19C H 1.1479 0.4448 0.3466 0.114 Uiso 1 1 calc R . . C20 C 1.2801(3) 0.3407(3) 0.3422(3) 0.110(2) Uani 1 1 d . . . H20A H 1.2993 0.2940 0.3392 0.164 Uiso 1 1 calc R . . H20B H 1.3496 0.3641 0.3678 0.164 Uiso 1 1 calc R . . H20C H 1.2580 0.3592 0.2963 0.164 Uiso 1 1 calc R . . C21 C 0.8768(2) 0.20024(12) 0.39143(12) 0.0301(5) Uani 1 1 d . . . C22 C 0.9024(3) 0.15295(14) 0.45229(13) 0.0423(6) Uani 1 1 d . . . C23 C 0.7851(3) 0.11972(18) 0.4560(2) 0.0707(10) Uani 1 1 d . . . H23A H 0.7265 0.1533 0.4612 0.106 Uiso 1 1 calc R . . H23B H 0.7973 0.0898 0.4950 0.106 Uiso 1 1 calc R . . H23C H 0.7561 0.0948 0.4142 0.106 Uiso 1 1 calc R . . C24 C 0.9466(4) 0.19229(17) 0.51726(15) 0.0603(9) Uani 1 1 d . . . H24A H 1.0201 0.2153 0.5141 0.090 Uiso 1 1 calc R . . H24B H 0.9620 0.1624 0.5563 0.090 Uiso 1 1 calc R . . H24C H 0.8862 0.2245 0.5230 0.090 Uiso 1 1 calc R . . C25 C 0.9948(4) 0.10225(18) 0.44339(17) 0.0711(11) Uani 1 1 d . . . H25A H 0.9640 0.0754 0.4031 0.107 Uiso 1 1 calc R . . H25B H 1.0126 0.0739 0.4836 0.107 Uiso 1 1 calc R . . H25C H 1.0674 0.1247 0.4377 0.107 Uiso 1 1 calc R . . C26 C 0.6913(2) 0.15618(12) 0.15645(14) 0.0356(6) Uani 1 1 d . . . H26 H 0.7098 0.1938 0.1326 0.043 Uiso 1 1 calc R . . C27 C 0.5804(2) 0.12832(14) 0.13597(16) 0.0472(7) Uani 1 1 d . . . H27 H 0.5236 0.1471 0.0999 0.057 Uiso 1 1 calc R . . C28 C 0.5539(3) 0.07279(15) 0.16894(17) 0.0520(8) Uani 1 1 d . . . H28 H 0.4784 0.0523 0.1559 0.062 Uiso 1 1 calc R . . C29 C 0.6383(3) 0.04761(16) 0.22086(16) 0.0531(8) Uani 1 1 d . . . H29 H 0.6228 0.0089 0.2440 0.064 Uiso 1 1 calc R . . C30 C 0.7465(2) 0.07931(13) 0.23918(14) 0.0400(6) Uani 1 1 d . . . H30 H 0.8040 0.0619 0.2757 0.048 Uiso 1 1 calc R . . C31 C 0.5486(3) 0.29602(16) 0.22463(15) 0.0475(7) Uani 1 1 d . . . H31 H 0.5777 0.3272 0.1970 0.057 Uiso 1 1 calc R . . C32 C 0.4333(3) 0.27438(19) 0.20470(17) 0.0581(9) Uani 1 1 d . . . H32 H 0.3842 0.2912 0.1644 0.070 Uiso 1 1 calc R . . C33 C 0.3894(3) 0.22867(18) 0.24282(18) 0.0598(9) Uani 1 1 d . . . H33 H 0.3102 0.2130 0.2297 0.072 Uiso 1 1 calc R . . C34 C 0.4636(3) 0.20628(19) 0.3006(2) 0.0653(9) Uani 1 1 d . . . H34 H 0.4365 0.1744 0.3284 0.078 Uiso 1 1 calc R . . C35 C 0.5778(3) 0.23028(15) 0.31824(17) 0.0530(8) Uani 1 1 d . . . H35 H 0.6278 0.2143 0.3586 0.064 Uiso 1 1 calc R . . C36 C 0.8225(2) 0.42181(12) 0.42207(12) 0.0335(5) Uani 1 1 d . . . H36 H 0.8899 0.3960 0.4413 0.040 Uiso 1 1 calc R . . C37 C 0.8069(3) 0.48154(13) 0.45150(14) 0.0417(6) Uani 1 1 d . . . H37 H 0.8624 0.4964 0.4904 0.050 Uiso 1 1 calc R . . C38 C 0.7093(3) 0.51944(12) 0.42355(14) 0.0423(7) Uani 1 1 d . . . H38 H 0.6976 0.5611 0.4424 0.051 Uiso 1 1 calc R . . C39 C 0.6299(3) 0.49618(12) 0.36841(13) 0.0401(6) Uani 1 1 d . . . H39 H 0.5612 0.5209 0.3489 0.048 Uiso 1 1 calc R . . C40 C 0.6516(2) 0.43586(12) 0.34172(13) 0.0364(6) Uani 1 1 d . . . H40 H 0.5967 0.4199 0.3032 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02570(15) 0.02827(15) 0.03033(15) -0.00478(10) 0.00343(11) 0.00451(10) Yb1 0.02383(7) 0.02453(6) 0.02334(7) -0.00475(3) 0.00419(4) 0.00207(4) N1 0.0307(11) 0.0302(10) 0.0326(11) -0.0035(8) 0.0110(9) 0.0016(9) N2 0.0284(11) 0.0380(12) 0.0402(12) -0.0090(10) 0.0033(9) 0.0029(9) N3 0.0317(11) 0.0264(10) 0.0289(10) -0.0006(8) 0.0087(8) 0.0042(8) O1 0.0344(11) 0.0797(14) 0.0424(11) -0.0294(11) 0.0151(9) -0.0245(10) O2 0.0314(9) 0.0442(10) 0.0346(9) -0.0130(8) 0.0146(7) -0.0132(8) O3 0.0392(11) 0.0385(11) 0.0733(15) -0.0020(10) -0.0129(10) 0.0066(9) O4 0.0399(11) 0.0333(10) 0.0442(11) -0.0050(7) -0.0056(9) 0.0059(8) O5 0.0321(9) 0.0267(8) 0.0357(9) 0.0021(7) 0.0042(7) 0.0000(7) O6 0.0480(11) 0.0366(9) 0.0371(10) -0.0031(8) 0.0115(8) 0.0076(8) O7 0.0263(10) 0.0456(11) 0.0577(12) -0.0207(9) 0.0065(8) 0.0003(8) O8 0.0389(10) 0.0356(10) 0.0406(10) -0.0154(8) 0.0048(8) -0.0016(8) O9 0.0473(12) 0.0403(10) 0.0274(9) -0.0014(7) 0.0100(8) 0.0043(8) O10 0.0398(10) 0.0390(10) 0.0334(9) 0.0018(7) 0.0075(8) 0.0120(8) C1 0.0277(13) 0.0336(12) 0.0297(13) -0.0043(10) 0.0067(10) 0.0018(11) C2 0.0309(14) 0.0539(17) 0.0343(14) -0.0114(12) 0.0128(11) -0.0036(12) C3 0.165(5) 0.080(3) 0.091(3) 0.008(2) 0.097(3) -0.003(3) C4 0.0322(17) 0.173(5) 0.060(2) -0.060(3) 0.0051(15) 0.015(2) C5 0.0419(17) 0.096(3) 0.0418(17) -0.0318(17) 0.0168(13) -0.0088(17) C6 0.0406(15) 0.0355(14) 0.0324(13) -0.0029(11) 0.0033(11) 0.0121(12) C7 0.0565(19) 0.0455(16) 0.0440(16) -0.0036(13) -0.0019(14) 0.0236(14) C8 0.064(2) 0.069(2) 0.054(2) -0.0012(16) -0.0131(16) 0.0323(18) C9 0.095(3) 0.0395(19) 0.139(4) 0.013(2) -0.036(3) 0.014(2) C10 0.105(3) 0.108(3) 0.070(3) 0.002(2) 0.022(2) 0.075(3) C11 0.0250(12) 0.0294(12) 0.0271(12) -0.0005(10) -0.0023(10) -0.0008(10) C12 0.0574(18) 0.0300(13) 0.0283(13) 0.0023(10) 0.0043(12) -0.0065(12) C13 0.142(4) 0.0383(17) 0.0408(18) 0.0094(14) 0.006(2) 0.020(2) C14 0.074(2) 0.0485(18) 0.0293(15) -0.0031(12) 0.0054(15) 0.0030(15) C15 0.074(3) 0.092(3) 0.062(2) 0.014(2) 0.0115(19) -0.046(2) C16 0.0291(13) 0.0249(11) 0.0270(12) -0.0007(9) 0.0023(10) 0.0003(9) C17 0.0294(13) 0.0406(14) 0.0357(14) -0.0060(11) -0.0004(11) -0.0073(11) C18 0.110(4) 0.148(5) 0.094(4) 0.069(3) -0.066(3) -0.073(3) C19 0.069(2) 0.066(2) 0.095(3) -0.044(2) 0.024(2) -0.0284(19) C20 0.040(2) 0.162(5) 0.134(4) -0.093(4) 0.034(2) -0.032(3) C21 0.0285(13) 0.0373(13) 0.0239(12) -0.0003(10) 0.0044(10) 0.0010(11) C22 0.0532(17) 0.0438(15) 0.0311(14) 0.0083(12) 0.0117(12) 0.0123(13) C23 0.079(3) 0.065(2) 0.071(2) 0.0255(19) 0.024(2) -0.0077(19) C24 0.076(2) 0.074(2) 0.0281(16) 0.0032(14) 0.0029(15) 0.0183(18) C25 0.097(3) 0.072(2) 0.0469(19) 0.0189(16) 0.0210(19) 0.049(2) C26 0.0308(13) 0.0292(12) 0.0457(15) -0.0019(11) 0.0054(11) -0.0005(11) C27 0.0335(15) 0.0459(16) 0.0577(18) -0.0075(14) -0.0004(13) 0.0009(13) C28 0.0347(15) 0.0557(18) 0.068(2) -0.0122(15) 0.0154(14) -0.0152(14) C29 0.0522(19) 0.0544(18) 0.0589(19) 0.0036(15) 0.0258(16) -0.0162(15) C30 0.0417(16) 0.0408(14) 0.0392(14) 0.0027(11) 0.0121(12) -0.0040(12) C31 0.0383(16) 0.0610(18) 0.0395(16) -0.0112(14) -0.0005(12) 0.0037(14) C32 0.0358(16) 0.085(2) 0.0472(18) -0.0236(17) -0.0053(14) 0.0063(17) C33 0.0310(16) 0.077(2) 0.071(2) -0.0371(19) 0.0101(16) -0.0081(16) C34 0.0451(19) 0.069(2) 0.083(3) -0.005(2) 0.0168(18) -0.0178(17) C35 0.0381(16) 0.0552(18) 0.063(2) 0.0055(15) 0.0035(14) -0.0044(14) C36 0.0334(13) 0.0377(13) 0.0300(13) -0.0025(10) 0.0077(10) 0.0032(11) C37 0.0460(16) 0.0459(15) 0.0358(14) -0.0127(12) 0.0146(12) -0.0062(13) C38 0.0630(19) 0.0268(13) 0.0449(16) -0.0011(11) 0.0293(14) 0.0034(13) C39 0.0543(17) 0.0320(13) 0.0365(14) 0.0094(11) 0.0156(13) 0.0159(12) C40 0.0405(15) 0.0368(13) 0.0308(13) 0.0022(11) 0.0050(11) 0.0102(12) _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 Zn1 O7 2.0395(18) . ? Zn1 O10 2.0455(17) . ? Zn1 O6 2.0601(18) . ? Zn1 N3 2.0844(19) . ? Zn1 N2 2.150(2) . ? Yb1 O8 2.2429(17) . ? Yb1 O5 2.2448(16) . ? Yb1 O9 2.2459(19) . ? Yb1 O1 2.3353(19) . ? Yb1 O4 2.3568(19) . ? Yb1 O3 2.3836(19) . ? Yb1 O2 2.4067(16) . ? Yb1 N1 2.542(2) . ? N1 C26 1.333(3) . ? N1 C30 1.340(3) . ? N2 C35 1.334(4) . ? N2 C31 1.340(4) . ? N3 C36 1.337(3) . ? N3 C40 1.337(3) . ? O1 C1 1.260(3) . ? O2 C1 1.255(3) . ? O3 C6 1.250(3) . ? O4 C6 1.259(3) . ? O5 C11 1.262(3) . ? O6 C11 1.254(3) . ? O7 C16 1.245(3) . ? O8 C16 1.246(3) . ? O9 C21 1.251(3) . ? O10 C21 1.256(3) . ? C1 C2 1.528(3) . ? C2 C5 1.510(4) . ? C2 C4 1.515(4) . ? C2 C3 1.525(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.528(4) . ? C7 C9 1.507(5) . ? C7 C8 1.523(4) . ? C7 C10 1.537(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.524(3) . ? C12 C14 1.525(4) . ? C12 C15 1.525(5) . ? C12 C13 1.526(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.533(3) . ? C17 C20 1.489(5) . ? C17 C18 1.509(5) . ? C17 C19 1.527(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.536(3) . ? C22 C25 1.518(4) . ? C22 C24 1.526(4) . ? C22 C23 1.526(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.379(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 H27 0.9500 . ? C28 C29 1.369(5) . ? C28 H28 0.9500 . ? C29 C30 1.382(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.377(4) . ? C31 H31 0.9500 . ? C32 C33 1.367(5) . ? C32 H32 0.9500 . ? C33 C34 1.369(5) . ? C33 H33 0.9500 . ? C34 C35 1.378(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.379(4) . ? C36 H36 0.9500 . ? C37 C38 1.382(4) . ? C37 H37 0.9500 . ? C38 C39 1.367(4) . ? C38 H38 0.9500 . ? C39 C40 1.382(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 O7 Zn1 O10 87.43(8) . . ? O7 Zn1 O6 88.86(8) . . ? O10 Zn1 O6 165.88(7) . . ? O7 Zn1 N3 90.29(7) . . ? O10 Zn1 N3 98.25(7) . . ? O6 Zn1 N3 95.39(7) . . ? O7 Zn1 N2 170.54(7) . . ? O10 Zn1 N2 90.33(8) . . ? O6 Zn1 N2 91.11(8) . . ? N3 Zn1 N2 99.13(8) . . ? O8 Yb1 O5 77.78(7) . . ? O8 Yb1 O9 81.64(7) . . ? O5 Yb1 O9 93.82(6) . . ? O8 Yb1 O1 80.32(7) . . ? O5 Yb1 O1 93.50(8) . . ? O9 Yb1 O1 158.61(7) . . ? O8 Yb1 O4 129.56(6) . . ? O5 Yb1 O4 152.12(6) . . ? O9 Yb1 O4 86.25(6) . . ? O1 Yb1 O4 96.45(7) . . ? O8 Yb1 O3 75.69(7) . . ? O5 Yb1 O3 153.31(6) . . ? O9 Yb1 O3 85.22(8) . . ? O1 Yb1 O3 79.27(8) . . ? O4 Yb1 O3 54.54(6) . . ? O8 Yb1 O2 130.34(6) . . ? O5 Yb1 O2 84.98(6) . . ? O9 Yb1 O2 146.35(6) . . ? O1 Yb1 O2 54.46(6) . . ? O4 Yb1 O2 79.86(6) . . ? O3 Yb1 O2 110.25(7) . . ? O8 Yb1 N1 142.97(6) . . ? O5 Yb1 N1 76.04(6) . . ? O9 Yb1 N1 74.49(7) . . ? O1 Yb1 N1 126.83(6) . . ? O4 Yb1 N1 77.14(6) . . ? O3 Yb1 N1 128.68(7) . . ? O2 Yb1 N1 72.60(6) . . ? C26 N1 C30 116.7(2) . . ? C26 N1 Yb1 121.86(16) . . ? C30 N1 Yb1 121.40(17) . . ? C35 N2 C31 116.7(3) . . ? C35 N2 Zn1 120.70(19) . . ? C31 N2 Zn1 122.3(2) . . ? C36 N3 C40 117.7(2) . . ? C36 N3 Zn1 118.61(16) . . ? C40 N3 Zn1 122.83(17) . . ? C1 O1 Yb1 94.44(15) . . ? C1 O2 Yb1 91.23(14) . . ? C6 O3 Yb1 92.23(15) . . ? C6 O4 Yb1 93.25(15) . . ? C11 O5 Yb1 153.01(15) . . ? C11 O6 Zn1 112.54(15) . . ? C16 O7 Zn1 134.67(16) . . ? C16 O8 Yb1 142.79(17) . . ? C21 O9 Yb1 162.05(17) . . ? C21 O10 Zn1 117.15(15) . . ? O2 C1 O1 119.3(2) . . ? O2 C1 C2 121.3(2) . . ? O1 C1 C2 119.4(2) . . ? C5 C2 C4 110.0(3) . . ? C5 C2 C3 109.6(3) . . ? C4 C2 C3 109.5(3) . . ? C5 C2 C1 111.2(2) . . ? C4 C2 C1 108.9(2) . . ? C3 C2 C1 107.6(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 119.9(2) . . ? O3 C6 C7 120.0(2) . . ? O4 C6 C7 120.1(2) . . ? C9 C7 C8 109.9(3) . . ? C9 C7 C6 111.0(3) . . ? C8 C7 C6 110.6(2) . . ? C9 C7 C10 111.4(3) . . ? C8 C7 C10 108.8(3) . . ? C6 C7 C10 105.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.4(2) . . ? O6 C11 C12 118.9(2) . . ? O5 C11 C12 118.7(2) . . ? C11 C12 C14 109.6(2) . . ? C11 C12 C15 106.0(2) . . ? C14 C12 C15 109.8(3) . . ? C11 C12 C13 111.0(3) . . ? C14 C12 C13 109.3(2) . . ? C15 C12 C13 111.1(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O7 C16 O8 125.2(2) . . ? O7 C16 C17 116.9(2) . . ? O8 C16 C17 117.9(2) . . ? C20 C17 C18 114.1(4) . . ? C20 C17 C19 107.7(3) . . ? C18 C17 C19 108.0(3) . . ? C20 C17 C16 111.7(2) . . ? C18 C17 C16 105.2(2) . . ? C19 C17 C16 110.1(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 123.0(2) . . ? O9 C21 C22 119.3(2) . . ? O10 C21 C22 117.7(2) . . ? C25 C22 C24 109.9(3) . . ? C25 C22 C23 110.8(3) . . ? C24 C22 C23 109.3(3) . . ? C25 C22 C21 110.7(2) . . ? C24 C22 C21 109.2(2) . . ? C23 C22 C21 106.9(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 123.8(3) . . ? N1 C26 H26 118.1 . . ? C27 C26 H26 118.1 . . ? C28 C27 C26 118.6(3) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C29 C28 C27 118.7(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? N1 C30 C29 123.1(3) . . ? N1 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? N2 C31 C32 122.7(3) . . ? N2 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 117.7(3) . . ? C32 C33 H33 121.2 . . ? C34 C33 H33 121.2 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N2 C35 C34 123.3(3) . . ? N2 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N3 C36 C37 122.5(2) . . ? N3 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C36 C37 C38 119.0(3) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C39 C38 C37 119.2(2) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.5(3) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N3 C40 C39 123.2(2) . . ? N3 C40 H40 118.4 . . ? C39 C40 H40 118.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.854 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.070 #===END data_8jy211ss _database_code_depnum_ccdc_archive 'CCDC 753914' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common LaZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 La N3 O15 Zn2' _chemical_formula_weight 1096.59 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6060(11) _cell_length_b 19.0863(11) _cell_length_c 14.9129(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5011.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6597 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.27 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.395 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.206 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.849 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.683 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34297 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.32 _reflns_number_total 4559 _reflns_number_gt 4029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+4.1996P] 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 4559 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Zn1 Zn 0.590488(15) 0.431821(13) 0.362381(17) 0.02684(8) Uani 1 1 d . . . La1 La 0.504696(10) 0.2500 0.2500 0.02392(7) Uani 1 2 d S . . N1 N 0.63114(11) 0.51615(10) 0.43435(13) 0.0297(4) Uani 1 1 d . . . N2 N 0.3340(2) 0.2500 0.2500 0.0951(19) Uani 1 2 d S . . O1 O 0.61660(13) 0.32365(12) 0.22668(17) 0.0717(8) Uani 1 1 d . . . O2 O 0.67344(10) 0.41702(9) 0.27590(11) 0.0358(4) Uani 1 1 d . . . O3 O 0.52660(13) 0.27935(10) 0.40569(12) 0.0517(5) Uani 1 1 d . . . O4 O 0.57076(11) 0.37527(9) 0.46801(11) 0.0389(4) Uani 1 1 d . . . O5 O 0.46520(14) 0.37299(10) 0.23530(14) 0.0552(6) Uani 1 1 d . . . O6 O 0.50626(9) 0.47144(9) 0.29474(12) 0.0363(4) Uani 1 1 d . . . O7 O 0.37138(13) 0.25838(12) 0.32196(18) 0.0698(7) Uani 1 1 d . . . O8 O 0.2647(3) 0.2500 0.2500 0.200(4) Uani 1 2 d S . . C1 C 0.66740(13) 0.36712(12) 0.22132(16) 0.0282(5) Uani 1 1 d . . . C2 C 0.72303(14) 0.36316(12) 0.14238(16) 0.0315(5) Uani 1 1 d . . . C3 C 0.73529(17) 0.28666(14) 0.1150(2) 0.0482(7) Uani 1 1 d . . . H3A H 0.7667 0.2848 0.0608 0.072 Uiso 1 1 calc R . . H3B H 0.6861 0.2646 0.1031 0.072 Uiso 1 1 calc R . . H3C H 0.7610 0.2616 0.1636 0.072 Uiso 1 1 calc R . . C4 C 0.68422(18) 0.40234(16) 0.06525(18) 0.0508(7) Uani 1 1 d . . . H4A H 0.7162 0.3999 0.0116 0.076 Uiso 1 1 calc R . . H4B H 0.6768 0.4515 0.0822 0.076 Uiso 1 1 calc R . . H4C H 0.6349 0.3807 0.0527 0.076 Uiso 1 1 calc R . . C5 C 0.79928(15) 0.39696(16) 0.1639(2) 0.0469(7) Uani 1 1 d . . . H5A H 0.8240 0.3711 0.2126 0.070 Uiso 1 1 calc R . . H5B H 0.7912 0.4457 0.1824 0.070 Uiso 1 1 calc R . . H5C H 0.8317 0.3959 0.1105 0.070 Uiso 1 1 calc R . . C6 C 0.54348(14) 0.31413(12) 0.47221(15) 0.0295(5) Uani 1 1 d . . . C7 C 0.53253(17) 0.28275(13) 0.56555(16) 0.0370(6) Uani 1 1 d . . . C8 C 0.6101(2) 0.2657(2) 0.6022(2) 0.0833(13) Uani 1 1 d . . . H8A H 0.6049 0.2441 0.6615 0.125 Uiso 1 1 calc R . . H8B H 0.6400 0.3089 0.6073 0.125 Uiso 1 1 calc R . . H8C H 0.6359 0.2331 0.5616 0.125 Uiso 1 1 calc R . . C9 C 0.4930(2) 0.33549(19) 0.6265(2) 0.0655(10) Uani 1 1 d . . . H9A H 0.4419 0.3451 0.6035 0.098 Uiso 1 1 calc R . . H9B H 0.5223 0.3791 0.6280 0.098 Uiso 1 1 calc R . . H9C H 0.4893 0.3162 0.6873 0.098 Uiso 1 1 calc R . . C10 C 0.4842(3) 0.2170(2) 0.5597(3) 0.0811(13) Uani 1 1 d . . . H10A H 0.4766 0.1978 0.6200 0.122 Uiso 1 1 calc R . . H10B H 0.5099 0.1822 0.5222 0.122 Uiso 1 1 calc R . . H10C H 0.4348 0.2286 0.5332 0.122 Uiso 1 1 calc R . . C11 C 0.46732(15) 0.43750(13) 0.23819(16) 0.0313(5) Uani 1 1 d . . . C12 C 0.41911(17) 0.47980(15) 0.17282(19) 0.0453(7) Uani 1 1 d . . . C13 C 0.3661(3) 0.5259(3) 0.2242(4) 0.140(3) Uani 1 1 d . . . H13A H 0.3420 0.5593 0.1832 0.210 Uiso 1 1 calc R . . H13B H 0.3946 0.5516 0.2701 0.210 Uiso 1 1 calc R . . H13C H 0.3270 0.4971 0.2530 0.210 Uiso 1 1 calc R . . C14 C 0.3787(4) 0.4352(2) 0.1100(4) 0.158(3) Uani 1 1 d . . . H14A H 0.3405 0.4076 0.1423 0.237 Uiso 1 1 calc R . . H14B H 0.4147 0.4035 0.0805 0.237 Uiso 1 1 calc R . . H14C H 0.3536 0.4643 0.0647 0.237 Uiso 1 1 calc R . . C15 C 0.4725(3) 0.5296(3) 0.1245(4) 0.163(3) Uani 1 1 d . . . H15A H 0.5024 0.5035 0.0804 0.245 Uiso 1 1 calc R . . H15B H 0.5066 0.5516 0.1681 0.245 Uiso 1 1 calc R . . H15C H 0.4428 0.5658 0.0938 0.245 Uiso 1 1 calc R . . C16 C 0.68486(15) 0.55759(13) 0.39882(18) 0.0370(6) Uani 1 1 d . . . H16 H 0.7028 0.5474 0.3401 0.044 Uiso 1 1 calc R . . C17 C 0.71520(16) 0.61409(14) 0.44343(19) 0.0449(7) Uani 1 1 d . . . H17 H 0.7541 0.6415 0.4167 0.054 Uiso 1 1 calc R . . C18 C 0.68824(16) 0.63025(14) 0.5274(2) 0.0468(7) Uani 1 1 d . . . H18 H 0.7078 0.6693 0.5595 0.056 Uiso 1 1 calc R . . C19 C 0.63259(17) 0.58892(15) 0.56381(19) 0.0472(7) Uani 1 1 d . . . H19 H 0.6122 0.5996 0.6212 0.057 Uiso 1 1 calc R . . C20 C 0.60631(15) 0.53177(13) 0.51665(17) 0.0381(6) Uani 1 1 d . . . H20 H 0.5692 0.5024 0.5436 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03349(16) 0.02533(15) 0.02168(14) -0.00277(11) 0.00138(11) -0.00200(11) La1 0.03235(12) 0.01941(11) 0.02000(11) -0.00300(7) 0.000 0.000 N1 0.0352(11) 0.0263(10) 0.0276(10) -0.0039(8) 0.0047(9) -0.0019(8) N2 0.039(2) 0.096(4) 0.150(5) -0.073(4) 0.000 0.000 O1 0.0672(15) 0.0498(13) 0.0983(18) -0.0353(13) 0.0487(14) -0.0300(12) O2 0.0357(9) 0.0438(11) 0.0278(9) -0.0117(8) 0.0042(7) -0.0040(8) O3 0.0903(15) 0.0410(11) 0.0239(10) -0.0033(8) -0.0057(10) -0.0184(11) O4 0.0595(12) 0.0313(9) 0.0259(9) 0.0019(7) 0.0011(8) -0.0132(8) O5 0.0824(15) 0.0272(10) 0.0561(13) -0.0070(9) -0.0254(11) 0.0155(10) O6 0.0387(10) 0.0336(10) 0.0366(10) -0.0005(8) -0.0059(8) 0.0016(7) O7 0.0529(14) 0.0691(15) 0.0874(18) -0.0460(14) 0.0252(13) -0.0135(12) O8 0.036(2) 0.310(10) 0.255(8) -0.128(7) 0.000 0.000 C1 0.0286(12) 0.0263(12) 0.0297(12) 0.0011(10) 0.0009(10) 0.0014(10) C2 0.0331(13) 0.0323(13) 0.0293(12) -0.0038(10) 0.0036(10) 0.0001(10) C3 0.0546(18) 0.0424(16) 0.0477(17) -0.0113(13) 0.0095(14) 0.0066(13) C4 0.0632(19) 0.0558(18) 0.0336(15) 0.0008(13) -0.0029(14) 0.0036(15) C5 0.0398(15) 0.0547(18) 0.0462(16) -0.0080(14) 0.0085(13) -0.0029(13) C6 0.0351(13) 0.0311(13) 0.0224(12) -0.0003(10) 0.0008(10) 0.0015(10) C7 0.0560(17) 0.0328(14) 0.0223(12) 0.0045(10) 0.0044(11) 0.0010(12) C8 0.076(2) 0.135(4) 0.0390(19) 0.031(2) 0.0014(18) 0.032(2) C9 0.105(3) 0.060(2) 0.0315(16) 0.0034(15) 0.0216(17) 0.0179(19) C10 0.132(4) 0.059(2) 0.053(2) 0.0133(18) 0.016(2) -0.037(2) C11 0.0359(13) 0.0292(13) 0.0287(13) 0.0007(10) 0.0024(10) 0.0069(11) C12 0.0526(17) 0.0402(15) 0.0431(16) 0.0068(13) -0.0132(13) 0.0091(13) C13 0.130(5) 0.179(6) 0.111(4) -0.022(4) -0.046(3) 0.117(5) C14 0.251(7) 0.059(3) 0.164(5) -0.004(3) -0.169(6) 0.013(3) C15 0.116(4) 0.201(7) 0.173(6) 0.156(6) -0.041(4) -0.025(4) C16 0.0460(15) 0.0300(13) 0.0349(14) -0.0048(11) 0.0136(12) -0.0038(11) C17 0.0485(16) 0.0334(14) 0.0527(17) -0.0086(12) 0.0189(13) -0.0095(12) C18 0.0529(17) 0.0366(15) 0.0509(17) -0.0196(13) 0.0110(14) -0.0139(13) C19 0.0600(18) 0.0459(16) 0.0358(15) -0.0160(13) 0.0150(13) -0.0133(14) C20 0.0437(15) 0.0371(14) 0.0336(14) -0.0076(11) 0.0112(12) -0.0122(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 Zn1 O4 1.9408(16) . ? Zn1 O6 1.9464(17) . ? Zn1 O2 1.9687(17) . ? Zn1 N1 2.0627(19) . ? La1 O3 2.4193(18) . ? La1 O3 2.4193(18) 4 ? La1 O1 2.445(2) . ? La1 O1 2.445(2) 4 ? La1 O5 2.4580(19) 4 ? La1 O5 2.4580(19) . ? La1 O7 2.586(2) 4 ? La1 O7 2.586(2) . ? N1 C20 1.336(3) . ? N1 C16 1.342(3) . ? N2 O8 1.220(6) . ? N2 O7 1.269(3) . ? N2 O7 1.269(3) 4 ? O1 C1 1.223(3) . ? O2 C1 1.257(3) . ? O3 C6 1.230(3) . ? O4 C6 1.263(3) . ? O5 C11 1.233(3) . ? O6 C11 1.265(3) . ? C1 C2 1.533(3) . ? C2 C5 1.524(4) . ? C2 C3 1.531(3) . ? C2 C4 1.533(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.528(3) . ? C7 C8 1.507(5) . ? C7 C10 1.519(5) . ? C7 C9 1.525(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.524(3) . ? C12 C14 1.453(5) . ? C12 C13 1.494(5) . ? C12 C15 1.518(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.374(4) . ? C17 H17 0.9500 . ? C18 C19 1.370(4) . ? C18 H18 0.9500 . ? C19 C20 1.378(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 120.03(8) . . ? O4 Zn1 O2 125.77(8) . . ? O6 Zn1 O2 106.34(8) . . ? O4 Zn1 N1 94.23(7) . . ? O6 Zn1 N1 103.35(8) . . ? O2 Zn1 N1 101.27(7) . . ? O3 La1 O3 161.66(11) . 4 ? O3 La1 O1 82.81(8) . . ? O3 La1 O1 82.43(8) 4 . ? O3 La1 O1 82.43(8) . 4 ? O3 La1 O1 82.81(8) 4 4 ? O1 La1 O1 72.63(13) . 4 ? O3 La1 O5 100.41(7) . 4 ? O3 La1 O5 84.81(7) 4 4 ? O1 La1 O5 142.16(8) . 4 ? O1 La1 O5 70.50(8) 4 4 ? O3 La1 O5 84.81(7) . . ? O3 La1 O5 100.41(7) 4 . ? O1 La1 O5 70.50(8) . . ? O1 La1 O5 142.16(8) 4 . ? O5 La1 O5 147.13(12) 4 . ? O3 La1 O7 123.87(8) . 4 ? O3 La1 O7 74.46(8) 4 4 ? O1 La1 O7 135.07(10) . 4 ? O1 La1 O7 139.01(7) 4 4 ? O5 La1 O7 73.81(8) 4 4 ? O5 La1 O7 76.42(7) . 4 ? O3 La1 O7 74.46(8) . . ? O3 La1 O7 123.87(8) 4 . ? O1 La1 O7 139.01(7) . . ? O1 La1 O7 135.07(10) 4 . ? O5 La1 O7 76.42(7) 4 . ? O5 La1 O7 73.81(8) . . ? O7 La1 O7 49.62(12) 4 . ? C20 N1 C16 117.5(2) . . ? C20 N1 Zn1 122.58(16) . . ? C16 N1 Zn1 119.94(16) . . ? O8 N2 O7 121.22(19) . . ? O8 N2 O7 121.22(19) . 4 ? O7 N2 O7 117.6(4) . 4 ? C1 O1 La1 171.47(18) . . ? C1 O2 Zn1 118.04(15) . . ? C6 O3 La1 159.62(17) . . ? C6 O4 Zn1 128.46(15) . . ? C11 O5 La1 160.4(2) . . ? C11 O6 Zn1 124.01(16) . . ? N2 O7 La1 96.4(2) . . ? O1 C1 O2 122.2(2) . . ? O1 C1 C2 119.0(2) . . ? O2 C1 C2 118.7(2) . . ? C5 C2 C3 109.6(2) . . ? C5 C2 C4 110.1(2) . . ? C3 C2 C4 109.1(2) . . ? C5 C2 C1 112.4(2) . . ? C3 C2 C1 110.0(2) . . ? C4 C2 C1 105.5(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.4(2) . . ? O3 C6 C7 119.5(2) . . ? O4 C6 C7 117.1(2) . . ? C8 C7 C10 110.5(3) . . ? C8 C7 C9 109.9(3) . . ? C10 C7 C9 108.9(3) . . ? C8 C7 C6 107.5(2) . . ? C10 C7 C6 110.0(2) . . ? C9 C7 C6 110.0(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.4(2) . . ? O5 C11 C12 119.3(2) . . ? O6 C11 C12 117.2(2) . . ? C14 C12 C13 111.8(4) . . ? C14 C12 C15 111.3(4) . . ? C13 C12 C15 105.1(4) . . ? C14 C12 C11 112.0(3) . . ? C13 C12 C11 109.4(3) . . ? C15 C12 C11 106.9(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.0(2) . . ? N1 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.9(2) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 118.6(2) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 119.6(2) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C20 C19 122.4(2) . . ? N1 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.488 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.062 # start Validation Reply Form _vrf_PLAT220_8jy211ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.78 Ratio RESPONSE: disorder in the Methyl carbons and NO3 moeity cause slighly large thermo parameters ; _vrf_PLAT222_8jy211ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.57 Ratio RESPONSE: see above ; _vrf_PLAT242_8jy211ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8jy151ss _database_code_depnum_ccdc_archive 'CCDC 753915' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CeZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Ce N3 O15 Zn2' _chemical_formula_weight 1097.80 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6253(11) _cell_length_b 19.0310(11) _cell_length_c 14.8985(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4997.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8066 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.28 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 1.910 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34203 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.30 _reflns_number_total 4543 _reflns_number_gt 4290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+6.2479P] 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 4543 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Zn1 Zn 0.590596(17) 0.431624(15) 0.362362(19) 0.02757(9) Uani 1 1 d . . . Ce1 Ce 0.505679(11) 0.2500 0.2500 0.02451(7) Uani 1 2 d S . . N1 N 0.63101(12) 0.51612(11) 0.43440(14) 0.0297(5) Uani 1 1 d . . . N2 N 0.3363(3) 0.2500 0.2500 0.0876(19) Uani 1 2 d S . . O1 O 0.61648(14) 0.32331(12) 0.22699(19) 0.0670(8) Uani 1 1 d . . . O2 O 0.67350(11) 0.41693(10) 0.27609(12) 0.0361(4) Uani 1 1 d . . . O3 O 0.52676(14) 0.27881(11) 0.40437(13) 0.0494(6) Uani 1 1 d . . . O4 O 0.57079(12) 0.37470(10) 0.46785(12) 0.0394(5) Uani 1 1 d . . . O5 O 0.46595(15) 0.37183(11) 0.23537(15) 0.0533(6) Uani 1 1 d . . . O6 O 0.50623(11) 0.47090(10) 0.29471(13) 0.0369(4) Uani 1 1 d . . . O7 O 0.37347(14) 0.25881(13) 0.32199(19) 0.0665(8) Uani 1 1 d . . . O8 O 0.2668(3) 0.2500 0.2500 0.182(4) Uani 1 2 d S . . C1 C 0.66764(14) 0.36680(13) 0.22128(17) 0.0280(5) Uani 1 1 d . . . C2 C 0.72275(15) 0.36289(14) 0.14227(17) 0.0321(6) Uani 1 1 d . . . C3 C 0.73524(19) 0.28629(16) 0.1149(2) 0.0474(8) Uani 1 1 d . . . H3A H 0.7674 0.2845 0.0612 0.071 Uiso 1 1 calc R . . H3B H 0.6862 0.2643 0.1018 0.071 Uiso 1 1 calc R . . H3C H 0.7601 0.2610 0.1640 0.071 Uiso 1 1 calc R . . C4 C 0.6841(2) 0.40241(18) 0.0652(2) 0.0507(8) Uani 1 1 d . . . H4A H 0.7159 0.3996 0.0113 0.076 Uiso 1 1 calc R . . H4B H 0.6772 0.4518 0.0821 0.076 Uiso 1 1 calc R . . H4C H 0.6346 0.3811 0.0529 0.076 Uiso 1 1 calc R . . C5 C 0.79899(17) 0.39680(18) 0.1641(2) 0.0466(7) Uani 1 1 d . . . H5A H 0.8233 0.3711 0.2132 0.070 Uiso 1 1 calc R . . H5B H 0.7910 0.4458 0.1822 0.070 Uiso 1 1 calc R . . H5C H 0.8317 0.3954 0.1109 0.070 Uiso 1 1 calc R . . C6 C 0.54351(15) 0.31339(13) 0.47127(17) 0.0293(5) Uani 1 1 d . . . C7 C 0.53232(18) 0.28163(15) 0.56478(18) 0.0382(6) Uani 1 1 d . . . C8 C 0.6097(2) 0.2649(3) 0.6020(3) 0.0831(14) Uani 1 1 d . . . H8A H 0.6043 0.2426 0.6609 0.125 Uiso 1 1 calc R . . H8B H 0.6391 0.3084 0.6081 0.125 Uiso 1 1 calc R . . H8C H 0.6361 0.2328 0.5611 0.125 Uiso 1 1 calc R . . C9 C 0.4925(2) 0.3346(2) 0.6257(2) 0.0654(11) Uani 1 1 d . . . H9A H 0.4419 0.3448 0.6018 0.098 Uiso 1 1 calc R . . H9B H 0.5223 0.3780 0.6283 0.098 Uiso 1 1 calc R . . H9C H 0.4878 0.3149 0.6862 0.098 Uiso 1 1 calc R . . C10 C 0.4842(3) 0.2156(2) 0.5584(3) 0.0812(14) Uani 1 1 d . . . H10A H 0.4784 0.1949 0.6183 0.122 Uiso 1 1 calc R . . H10B H 0.5092 0.1816 0.5187 0.122 Uiso 1 1 calc R . . H10C H 0.4342 0.2275 0.5341 0.122 Uiso 1 1 calc R . . C11 C 0.46761(16) 0.43665(14) 0.23830(18) 0.0320(6) Uani 1 1 d . . . C12 C 0.41865(19) 0.47878(16) 0.1733(2) 0.0463(8) Uani 1 1 d . . . C13 C 0.3676(4) 0.5265(4) 0.2243(4) 0.148(3) Uani 1 1 d . . . H13A H 0.3425 0.5589 0.1826 0.222 Uiso 1 1 calc R . . H13B H 0.3974 0.5534 0.2680 0.222 Uiso 1 1 calc R . . H13C H 0.3292 0.4986 0.2559 0.222 Uiso 1 1 calc R . . C14 C 0.3764(5) 0.4339(3) 0.1128(5) 0.180(4) Uani 1 1 d . . . H14A H 0.3410 0.4048 0.1473 0.270 Uiso 1 1 calc R . . H14B H 0.4116 0.4036 0.0798 0.270 Uiso 1 1 calc R . . H14C H 0.3479 0.4630 0.0702 0.270 Uiso 1 1 calc R . . C15 C 0.4715(4) 0.5271(4) 0.1230(5) 0.185(4) Uani 1 1 d . . . H15A H 0.5004 0.4999 0.0788 0.278 Uiso 1 1 calc R . . H15B H 0.5066 0.5493 0.1654 0.278 Uiso 1 1 calc R . . H15C H 0.4419 0.5634 0.0922 0.278 Uiso 1 1 calc R . . C16 C 0.68488(17) 0.55745(14) 0.39937(19) 0.0378(7) Uani 1 1 d . . . H16 H 0.7030 0.5472 0.3408 0.045 Uiso 1 1 calc R . . C17 C 0.71518(18) 0.61402(15) 0.4441(2) 0.0452(7) Uani 1 1 d . . . H17 H 0.7542 0.6414 0.4175 0.054 Uiso 1 1 calc R . . C18 C 0.68809(18) 0.63027(16) 0.5279(2) 0.0479(8) Uani 1 1 d . . . H18 H 0.7076 0.6693 0.5601 0.057 Uiso 1 1 calc R . . C19 C 0.63221(19) 0.58893(16) 0.5639(2) 0.0481(8) Uani 1 1 d . . . H19 H 0.6116 0.5997 0.6212 0.058 Uiso 1 1 calc R . . C20 C 0.60620(17) 0.53186(15) 0.51669(19) 0.0391(7) Uani 1 1 d . . . H20 H 0.5691 0.5024 0.5436 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03365(17) 0.02561(16) 0.02345(15) -0.00285(12) 0.00152(12) -0.00194(12) Ce1 0.03222(12) 0.01967(11) 0.02163(11) -0.00318(7) 0.000 0.000 N1 0.0353(12) 0.0253(11) 0.0284(11) -0.0042(9) 0.0056(9) -0.0027(9) N2 0.039(2) 0.085(4) 0.139(5) -0.061(4) 0.000 0.000 O1 0.0632(15) 0.0461(13) 0.0917(19) -0.0293(13) 0.0437(14) -0.0260(12) O2 0.0349(10) 0.0433(11) 0.0300(9) -0.0128(9) 0.0045(8) -0.0036(8) O3 0.0843(16) 0.0391(11) 0.0247(10) -0.0040(9) -0.0049(10) -0.0158(11) O4 0.0597(13) 0.0311(10) 0.0273(9) 0.0016(8) -0.0002(9) -0.0128(9) O5 0.0761(16) 0.0281(11) 0.0559(14) -0.0054(10) -0.0222(12) 0.0136(11) O6 0.0387(11) 0.0339(10) 0.0381(11) -0.0008(9) -0.0070(9) 0.0018(8) O7 0.0518(15) 0.0643(16) 0.0834(19) -0.0405(14) 0.0219(14) -0.0102(12) O8 0.037(3) 0.267(9) 0.243(9) -0.109(7) 0.000 0.000 C1 0.0273(13) 0.0261(13) 0.0306(13) 0.0018(11) -0.0005(10) 0.0023(10) C2 0.0330(14) 0.0327(14) 0.0306(13) -0.0037(11) 0.0034(11) 0.0008(11) C3 0.0517(19) 0.0428(17) 0.0479(18) -0.0111(14) 0.0091(15) 0.0062(14) C4 0.062(2) 0.056(2) 0.0340(16) 0.0027(14) -0.0021(15) 0.0048(16) C5 0.0392(17) 0.0553(19) 0.0452(17) -0.0082(15) 0.0089(14) -0.0055(14) C6 0.0329(14) 0.0293(13) 0.0257(13) 0.0009(11) 0.0001(11) 0.0011(11) C7 0.0556(18) 0.0344(15) 0.0247(13) 0.0046(12) 0.0031(13) -0.0003(13) C8 0.076(3) 0.133(4) 0.040(2) 0.029(2) 0.0000(19) 0.029(3) C9 0.104(3) 0.059(2) 0.0332(17) 0.0013(16) 0.0200(18) 0.015(2) C10 0.133(4) 0.059(2) 0.052(2) 0.014(2) 0.016(2) -0.036(3) C11 0.0360(14) 0.0291(14) 0.0307(14) 0.0025(11) 0.0033(12) 0.0067(11) C12 0.0540(19) 0.0394(17) 0.0456(17) 0.0076(14) -0.0130(15) 0.0108(14) C13 0.145(6) 0.185(7) 0.114(4) -0.030(4) -0.053(4) 0.129(5) C14 0.283(9) 0.062(3) 0.194(7) -0.011(4) -0.200(7) 0.024(4) C15 0.119(5) 0.245(9) 0.192(7) 0.189(7) -0.033(5) -0.016(5) C16 0.0475(17) 0.0293(14) 0.0365(15) -0.0049(12) 0.0154(13) -0.0030(12) C17 0.0482(17) 0.0310(15) 0.0565(19) -0.0078(14) 0.0210(15) -0.0096(13) C18 0.0548(19) 0.0366(16) 0.0524(19) -0.0196(14) 0.0129(16) -0.0146(14) C19 0.061(2) 0.0481(18) 0.0355(16) -0.0167(14) 0.0156(15) -0.0141(15) C20 0.0453(17) 0.0382(15) 0.0338(15) -0.0072(12) 0.0114(13) -0.0118(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.9405(18) . ? Zn1 O6 1.9456(19) . ? Zn1 O2 1.9660(18) . ? Zn1 N1 2.060(2) . ? Ce1 O3 2.3934(19) . ? Ce1 O3 2.3934(19) 4 ? Ce1 O1 2.424(2) . ? Ce1 O1 2.424(2) 4 ? Ce1 O5 2.432(2) . ? Ce1 O5 2.432(2) 4 ? Ce1 O7 2.571(2) 4 ? Ce1 O7 2.571(2) . ? N1 C20 1.336(3) . ? N1 C16 1.339(3) . ? N2 O8 1.226(7) . ? N2 O7 1.268(3) . ? N2 O7 1.268(3) 4 ? O1 C1 1.227(3) . ? O2 C1 1.260(3) . ? O3 C6 1.230(3) . ? O4 C6 1.263(3) . ? O5 C11 1.235(3) . ? O6 C11 1.263(3) . ? C1 C2 1.528(4) . ? C2 C5 1.526(4) . ? C2 C3 1.530(4) . ? C2 C4 1.532(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(4) . ? C7 C8 1.506(5) . ? C7 C10 1.519(5) . ? C7 C9 1.527(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(4) . ? C12 C14 1.448(6) . ? C12 C13 1.487(6) . ? C12 C15 1.508(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.374(4) . ? C16 H16 0.9500 . ? C17 C18 1.371(4) . ? C17 H17 0.9500 . ? C18 C19 1.370(4) . ? C18 H18 0.9500 . ? C19 C20 1.373(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.78(9) . . ? O4 Zn1 O2 125.72(9) . . ? O6 Zn1 O2 106.49(8) . . ? O4 Zn1 N1 94.36(8) . . ? O6 Zn1 N1 103.55(8) . . ? O2 Zn1 N1 101.22(8) . . ? O3 Ce1 O3 162.14(12) . 4 ? O3 Ce1 O1 83.05(8) . . ? O3 Ce1 O1 82.58(8) 4 . ? O3 Ce1 O1 82.58(8) . 4 ? O3 Ce1 O1 83.05(8) 4 4 ? O1 Ce1 O1 72.68(13) . 4 ? O3 Ce1 O5 84.97(7) . . ? O3 Ce1 O5 100.19(7) 4 . ? O1 Ce1 O5 70.77(9) . . ? O1 Ce1 O5 142.49(9) 4 . ? O3 Ce1 O5 100.19(7) . 4 ? O3 Ce1 O5 84.97(7) 4 4 ? O1 Ce1 O5 142.49(9) . 4 ? O1 Ce1 O5 70.77(9) 4 4 ? O5 Ce1 O5 146.53(13) . 4 ? O3 Ce1 O7 123.82(9) . 4 ? O3 Ce1 O7 74.03(9) 4 4 ? O1 Ce1 O7 135.13(10) . 4 ? O1 Ce1 O7 138.73(7) 4 4 ? O5 Ce1 O7 76.34(8) . 4 ? O5 Ce1 O7 73.39(9) 4 4 ? O3 Ce1 O7 74.03(9) . . ? O3 Ce1 O7 123.82(9) 4 . ? O1 Ce1 O7 138.73(7) . . ? O1 Ce1 O7 135.13(10) 4 . ? O5 Ce1 O7 73.39(9) . . ? O5 Ce1 O7 76.34(8) 4 . ? O7 Ce1 O7 49.96(13) 4 . ? C20 N1 C16 117.3(2) . . ? C20 N1 Zn1 122.68(18) . . ? C16 N1 Zn1 120.05(17) . . ? O8 N2 O7 121.1(2) . . ? O8 N2 O7 121.1(2) . 4 ? O7 N2 O7 117.8(4) . 4 ? C1 O1 Ce1 171.9(2) . . ? C1 O2 Zn1 118.06(17) . . ? C6 O3 Ce1 159.76(19) . . ? C6 O4 Zn1 128.09(17) . . ? C11 O5 Ce1 160.5(2) . . ? C11 O6 Zn1 123.95(18) . . ? N2 O7 Ce1 96.1(2) . . ? O1 C1 O2 121.7(2) . . ? O1 C1 C2 119.2(2) . . ? O2 C1 C2 118.9(2) . . ? C5 C2 C1 112.0(2) . . ? C5 C2 C3 109.5(2) . . ? C1 C2 C3 110.1(2) . . ? C5 C2 C4 110.1(2) . . ? C1 C2 C4 105.7(2) . . ? C3 C2 C4 109.4(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.6(2) . . ? O3 C6 C7 119.7(2) . . ? O4 C6 C7 116.8(2) . . ? C8 C7 C10 110.7(3) . . ? C8 C7 C9 109.7(3) . . ? C10 C7 C9 109.1(3) . . ? C8 C7 C6 107.5(3) . . ? C10 C7 C6 110.0(2) . . ? C9 C7 C6 109.9(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.5(3) . . ? O5 C11 C12 119.3(3) . . ? O6 C11 C12 117.1(2) . . ? C14 C12 C13 111.5(5) . . ? C14 C12 C15 111.6(5) . . ? C13 C12 C15 104.8(5) . . ? C14 C12 C11 112.1(3) . . ? C13 C12 C11 109.8(3) . . ? C15 C12 C11 106.6(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.1(3) . . ? N1 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 118.9(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 118.5(3) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 119.6(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C20 C19 122.6(3) . . ? N1 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.643 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.064 # start Validation Reply Form _vrf_PLAT220_8jy151ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.61 Ratio RESPONSE: slight disorder in the methyl carbons and NO3 group cause abnormal thermal parameters ; _vrf_PLAT222_8jy151ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.18 Ratio RESPONSE: see above ; _vrf_PLAT242_8jy151ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8ag291ss _database_code_depnum_ccdc_archive 'CCDC 753916' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PrZNNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 N3 O15 Pr Zn2' _chemical_formula_weight 1098.59 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6348(11) _cell_length_b 19.0271(11) _cell_length_c 14.9022(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5000.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7400 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.35 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.315 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.973 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34557 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.36 _reflns_number_total 4589 _reflns_number_gt 4461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+12.3078P] 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 4589 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _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 Zn1 Zn 0.59064(2) 0.43118(2) 0.36227(3) 0.02439(11) Uani 1 1 d . . . Pr1 Pr 0.506332(15) 0.2500 0.2500 0.02185(9) Uani 1 2 d S . . N1 N 0.63065(17) 0.51563(15) 0.43462(19) 0.0255(6) Uani 1 1 d . . . N2 N 0.3383(3) 0.2500 0.2500 0.077(2) Uani 1 2 d S . . O1 O 0.61632(19) 0.32304(17) 0.2267(2) 0.0590(10) Uani 1 1 d . . . O2 O 0.67383(15) 0.41649(14) 0.27620(17) 0.0321(6) Uani 1 1 d . . . O3 O 0.52730(19) 0.27762(15) 0.40368(18) 0.0444(8) Uani 1 1 d . . . O4 O 0.57031(16) 0.37402(13) 0.46741(17) 0.0356(6) Uani 1 1 d . . . O5 O 0.46631(19) 0.37111(15) 0.2345(2) 0.0478(8) Uani 1 1 d . . . O6 O 0.50635(15) 0.47029(14) 0.29413(18) 0.0334(6) Uani 1 1 d . . . O7 O 0.37542(19) 0.25890(18) 0.3217(3) 0.0596(10) Uani 1 1 d . . . O8 O 0.2685(4) 0.2500 0.2500 0.163(5) Uani 1 2 d S . . C1 C 0.6677(2) 0.36643(18) 0.2213(2) 0.0241(7) Uani 1 1 d . . . C2 C 0.7230(2) 0.36265(19) 0.1424(2) 0.0283(8) Uani 1 1 d . . . C3 C 0.7354(3) 0.2858(2) 0.1151(3) 0.0412(10) Uani 1 1 d . . . H3A H 0.7677 0.2839 0.0616 0.062 Uiso 1 1 calc R . . H3B H 0.6863 0.2639 0.1018 0.062 Uiso 1 1 calc R . . H3C H 0.7600 0.2605 0.1644 0.062 Uiso 1 1 calc R . . C4 C 0.6845(3) 0.4024(2) 0.0651(3) 0.0442(11) Uani 1 1 d . . . H4A H 0.7164 0.3997 0.0114 0.066 Uiso 1 1 calc R . . H4B H 0.6776 0.4518 0.0821 0.066 Uiso 1 1 calc R . . H4C H 0.6350 0.3812 0.0525 0.066 Uiso 1 1 calc R . . C5 C 0.7991(2) 0.3964(2) 0.1645(3) 0.0394(10) Uani 1 1 d . . . H5A H 0.8234 0.3704 0.2135 0.059 Uiso 1 1 calc R . . H5B H 0.7911 0.4453 0.1829 0.059 Uiso 1 1 calc R . . H5C H 0.8318 0.3952 0.1114 0.059 Uiso 1 1 calc R . . C6 C 0.5432(2) 0.31258(19) 0.4709(2) 0.0259(8) Uani 1 1 d . . . C7 C 0.5317(2) 0.2810(2) 0.5646(2) 0.0332(9) Uani 1 1 d . . . C8 C 0.6092(3) 0.2636(4) 0.6021(3) 0.0749(19) Uani 1 1 d . . . H8A H 0.6035 0.2407 0.6606 0.112 Uiso 1 1 calc R . . H8B H 0.6386 0.3069 0.6091 0.112 Uiso 1 1 calc R . . H8C H 0.6357 0.2318 0.5609 0.112 Uiso 1 1 calc R . . C9 C 0.4922(3) 0.3341(3) 0.6253(3) 0.0602(15) Uani 1 1 d . . . H9A H 0.4416 0.3443 0.6015 0.090 Uiso 1 1 calc R . . H9B H 0.5220 0.3775 0.6275 0.090 Uiso 1 1 calc R . . H9C H 0.4876 0.3145 0.6859 0.090 Uiso 1 1 calc R . . C10 C 0.4840(4) 0.2145(3) 0.5580(4) 0.0731(18) Uani 1 1 d . . . H10A H 0.4780 0.1939 0.6179 0.110 Uiso 1 1 calc R . . H10B H 0.5092 0.1807 0.5184 0.110 Uiso 1 1 calc R . . H10C H 0.4340 0.2262 0.5335 0.110 Uiso 1 1 calc R . . C11 C 0.4677(2) 0.43628(19) 0.2378(2) 0.0280(8) Uani 1 1 d . . . C12 C 0.4185(3) 0.4781(2) 0.1729(3) 0.0442(11) Uani 1 1 d . . . C13 C 0.3682(5) 0.5264(5) 0.2237(5) 0.146(5) Uani 1 1 d . . . H13A H 0.3462 0.5611 0.1826 0.220 Uiso 1 1 calc R . . H13B H 0.3978 0.5507 0.2700 0.220 Uiso 1 1 calc R . . H13C H 0.3275 0.4994 0.2521 0.220 Uiso 1 1 calc R . . C14 C 0.3754(6) 0.4337(4) 0.1128(6) 0.165(5) Uani 1 1 d . . . H14A H 0.3401 0.4048 0.1477 0.247 Uiso 1 1 calc R . . H14B H 0.4102 0.4031 0.0795 0.247 Uiso 1 1 calc R . . H14C H 0.3469 0.4630 0.0706 0.247 Uiso 1 1 calc R . . C15 C 0.4713(5) 0.5257(6) 0.1223(7) 0.188(6) Uani 1 1 d . . . H15A H 0.4994 0.4982 0.0777 0.282 Uiso 1 1 calc R . . H15B H 0.5070 0.5474 0.1643 0.282 Uiso 1 1 calc R . . H15C H 0.4419 0.5624 0.0920 0.282 Uiso 1 1 calc R . . C16 C 0.6846(2) 0.55690(19) 0.4000(3) 0.0320(9) Uani 1 1 d . . . H16 H 0.7029 0.5466 0.3415 0.038 Uiso 1 1 calc R . . C17 C 0.7151(2) 0.6136(2) 0.4447(3) 0.0403(10) Uani 1 1 d . . . H17 H 0.7542 0.6409 0.4182 0.048 Uiso 1 1 calc R . . C18 C 0.6878(3) 0.6300(2) 0.5283(3) 0.0434(11) Uani 1 1 d . . . H18 H 0.7073 0.6691 0.5605 0.052 Uiso 1 1 calc R . . C19 C 0.6318(3) 0.5886(2) 0.5644(3) 0.0439(11) Uani 1 1 d . . . H19 H 0.6113 0.5994 0.6217 0.053 Uiso 1 1 calc R . . C20 C 0.6056(2) 0.5316(2) 0.5171(3) 0.0365(9) Uani 1 1 d . . . H20 H 0.5683 0.5023 0.5438 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0299(2) 0.0239(2) 0.0194(2) -0.00265(17) 0.00163(17) -0.00139(17) Pr1 0.02888(16) 0.01877(14) 0.01792(14) -0.00256(10) 0.000 0.000 N1 0.0319(17) 0.0228(15) 0.0218(15) -0.0047(12) 0.0046(13) -0.0011(13) N2 0.034(3) 0.071(5) 0.125(7) -0.052(5) 0.000 0.000 O1 0.058(2) 0.0428(18) 0.076(2) -0.0250(17) 0.0372(18) -0.0214(16) O2 0.0307(14) 0.0405(16) 0.0251(13) -0.0120(12) 0.0031(11) -0.0032(12) O3 0.075(2) 0.0365(16) 0.0213(14) -0.0041(12) -0.0036(14) -0.0140(15) O4 0.0545(18) 0.0290(14) 0.0234(13) 0.0008(11) 0.0013(12) -0.0113(13) O5 0.068(2) 0.0276(15) 0.0481(18) -0.0057(13) -0.0204(16) 0.0135(14) O6 0.0339(15) 0.0317(14) 0.0346(15) -0.0001(12) -0.0052(12) 0.0015(12) O7 0.048(2) 0.058(2) 0.073(2) -0.0359(19) 0.0202(18) -0.0102(17) O8 0.033(3) 0.232(11) 0.222(11) -0.092(9) 0.000 0.000 C1 0.0237(18) 0.0220(17) 0.0265(18) 0.0029(15) -0.0007(14) 0.0017(14) C2 0.031(2) 0.0290(19) 0.0248(18) -0.0045(15) 0.0030(15) 0.0004(16) C3 0.047(3) 0.038(2) 0.038(2) -0.0113(19) 0.010(2) 0.008(2) C4 0.056(3) 0.049(3) 0.028(2) 0.0027(19) -0.002(2) 0.003(2) C5 0.033(2) 0.048(3) 0.037(2) -0.0059(19) 0.0083(18) -0.0035(19) C6 0.0298(19) 0.0276(19) 0.0203(18) 0.0012(15) 0.0014(15) 0.0021(15) C7 0.049(2) 0.031(2) 0.0193(18) 0.0035(16) 0.0043(17) 0.0024(18) C8 0.071(4) 0.123(5) 0.031(3) 0.024(3) 0.000(2) 0.029(4) C9 0.096(4) 0.054(3) 0.031(2) 0.001(2) 0.024(3) 0.016(3) C10 0.119(5) 0.052(3) 0.047(3) 0.014(3) 0.016(3) -0.032(3) C11 0.034(2) 0.0258(19) 0.0241(18) 0.0002(15) 0.0031(16) 0.0058(16) C12 0.048(3) 0.041(2) 0.044(2) 0.009(2) -0.011(2) 0.010(2) C13 0.148(8) 0.187(9) 0.105(6) -0.034(6) -0.054(6) 0.135(8) C14 0.262(12) 0.059(4) 0.174(9) -0.014(5) -0.183(9) 0.024(6) C15 0.108(7) 0.254(13) 0.202(11) 0.202(11) -0.034(7) -0.018(8) C16 0.041(2) 0.0238(19) 0.031(2) -0.0026(16) 0.0129(17) 0.0000(16) C17 0.042(2) 0.030(2) 0.050(3) -0.0057(19) 0.018(2) -0.0072(18) C18 0.051(3) 0.034(2) 0.045(3) -0.0166(19) 0.010(2) -0.013(2) C19 0.055(3) 0.044(2) 0.032(2) -0.0130(19) 0.015(2) -0.013(2) C20 0.041(2) 0.036(2) 0.032(2) -0.0069(18) 0.0110(18) -0.0099(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.941(3) . ? Zn1 O6 1.948(3) . ? Zn1 O2 1.969(3) . ? Zn1 N1 2.060(3) . ? Pr1 O3 2.379(3) . ? Pr1 O3 2.379(3) 4 ? Pr1 O1 2.411(3) 4 ? Pr1 O1 2.411(3) . ? Pr1 O5 2.421(3) 4 ? Pr1 O5 2.421(3) . ? Pr1 O7 2.550(3) 4 ? Pr1 O7 2.550(3) . ? N1 C16 1.337(5) . ? N1 C20 1.340(5) . ? N2 O8 1.230(8) . ? N2 O7 1.265(5) . ? N2 O7 1.265(5) 4 ? O1 C1 1.228(4) . ? O2 C1 1.260(4) . ? O3 C6 1.234(4) . ? O4 C6 1.265(4) . ? O5 C11 1.241(5) . ? O6 C11 1.260(5) . ? C1 C2 1.530(5) . ? C2 C5 1.525(5) . ? C2 C3 1.534(5) . ? C2 C4 1.536(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.533(5) . ? C7 C8 1.513(7) . ? C7 C10 1.522(7) . ? C7 C9 1.525(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(5) . ? C12 C14 1.446(8) . ? C12 C13 1.484(8) . ? C12 C15 1.501(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C17 C18 1.371(6) . ? C17 H17 0.9500 . ? C18 C19 1.373(6) . ? C18 H18 0.9500 . ? C19 C20 1.375(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.60(12) . . ? O4 Zn1 O2 125.74(12) . . ? O6 Zn1 O2 106.45(11) . . ? O4 Zn1 N1 94.46(11) . . ? O6 Zn1 N1 103.66(12) . . ? O2 Zn1 N1 101.34(11) . . ? O3 Pr1 O3 162.11(17) . 4 ? O3 Pr1 O1 82.15(11) . 4 ? O3 Pr1 O1 83.48(11) 4 4 ? O3 Pr1 O1 83.48(11) . . ? O3 Pr1 O1 82.15(11) 4 . ? O1 Pr1 O1 72.90(18) 4 . ? O3 Pr1 O5 99.41(10) . 4 ? O3 Pr1 O5 85.82(10) 4 4 ? O1 Pr1 O5 70.86(12) 4 4 ? O1 Pr1 O5 142.82(12) . 4 ? O3 Pr1 O5 85.82(10) . . ? O3 Pr1 O5 99.41(10) 4 . ? O1 Pr1 O5 142.82(12) 4 . ? O1 Pr1 O5 70.86(12) . . ? O5 Pr1 O5 146.11(17) 4 . ? O3 Pr1 O7 123.99(12) . 4 ? O3 Pr1 O7 73.89(12) 4 4 ? O1 Pr1 O7 138.63(10) 4 4 ? O1 Pr1 O7 134.93(14) . 4 ? O5 Pr1 O7 73.32(12) 4 4 ? O5 Pr1 O7 76.07(11) . 4 ? O3 Pr1 O7 73.89(12) . . ? O3 Pr1 O7 123.99(12) 4 . ? O1 Pr1 O7 134.93(14) 4 . ? O1 Pr1 O7 138.63(10) . . ? O5 Pr1 O7 76.07(11) 4 . ? O5 Pr1 O7 73.32(12) . . ? O7 Pr1 O7 50.23(17) 4 . ? C16 N1 C20 117.1(3) . . ? C16 N1 Zn1 120.0(2) . . ? C20 N1 Zn1 122.9(3) . . ? O8 N2 O7 121.2(3) . . ? O8 N2 O7 121.2(3) . 4 ? O7 N2 O7 117.6(5) . 4 ? C1 O1 Pr1 171.9(3) . . ? C1 O2 Zn1 117.8(2) . . ? C6 O3 Pr1 159.3(3) . . ? C6 O4 Zn1 128.4(2) . . ? C11 O5 Pr1 160.3(3) . . ? C11 O6 Zn1 124.3(2) . . ? N2 O7 Pr1 96.1(3) . . ? O1 C1 O2 121.9(3) . . ? O1 C1 C2 119.3(3) . . ? O2 C1 C2 118.7(3) . . ? C5 C2 C1 112.1(3) . . ? C5 C2 C3 109.5(3) . . ? C1 C2 C3 109.8(3) . . ? C5 C2 C4 110.1(3) . . ? C1 C2 C4 105.7(3) . . ? C3 C2 C4 109.5(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.4(3) . . ? O3 C6 C7 119.8(3) . . ? O4 C6 C7 116.7(3) . . ? C8 C7 C10 110.0(5) . . ? C8 C7 C9 109.8(4) . . ? C10 C7 C9 109.6(4) . . ? C8 C7 C6 107.7(3) . . ? C10 C7 C6 109.9(3) . . ? C9 C7 C6 109.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.4(4) . . ? O5 C11 C12 119.0(4) . . ? O6 C11 C12 117.6(3) . . ? C14 C12 C13 111.4(7) . . ? C14 C12 C15 111.6(7) . . ? C13 C12 C15 104.7(7) . . ? C14 C12 C11 112.7(4) . . ? C13 C12 C11 109.8(4) . . ? C15 C12 C11 106.3(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.4(4) . . ? N1 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C18 C17 C16 118.7(4) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 118.6(4) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C20 C19 122.6(4) . . ? N1 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.769 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.081 # start Validation Reply Form _vrf_PLAT220_8ag291ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.80 Ratio RESPONSE: slight disorder in the NO3 and metyl groups of the OBc ligand cause for abnormal thermal parameters ; _vrf_PLAT222_8ag291ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.42 Ratio RESPONSE: see above ; _vrf_PLAT242_8ag291ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_7ag221ss _database_code_depnum_ccdc_archive 'CCDC 753917' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NdZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 N3 Nd O15 Zn2' _chemical_formula_weight 1101.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6239(11) _cell_length_b 18.9783(11) _cell_length_c 14.8859(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4978.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8494 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.33 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34424 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4585 _reflns_number_gt 3856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+3.7237P] 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 4585 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Zn1 Zn 0.590839(17) 0.431196(16) 0.36220(2) 0.02190(9) Uani 1 1 d . . . Nd1 Nd 0.506977(11) 0.2500 0.2500 0.01943(7) Uani 1 2 d S . . N1 N 0.63072(13) 0.51598(11) 0.43475(14) 0.0226(5) Uani 1 1 d . . . N2 N 0.3392(2) 0.2500 0.2500 0.0680(15) Uani 1 2 d S . . O1 O 0.61663(14) 0.32231(12) 0.22690(17) 0.0526(7) Uani 1 1 d . . . O2 O 0.67433(11) 0.41651(10) 0.27625(12) 0.0292(5) Uani 1 1 d . . . O3 O 0.52759(14) 0.27709(11) 0.40319(14) 0.0404(5) Uani 1 1 d . . . O4 O 0.57074(12) 0.37370(10) 0.46727(13) 0.0331(5) Uani 1 1 d . . . O5 O 0.46659(14) 0.37029(11) 0.23379(15) 0.0424(6) Uani 1 1 d . . . O6 O 0.50637(11) 0.46996(10) 0.29424(14) 0.0298(5) Uani 1 1 d . . . O7 O 0.37697(14) 0.25872(12) 0.32177(18) 0.0534(7) Uani 1 1 d . . . O8 O 0.2708(2) 0.2500 0.2500 0.139(3) Uani 1 2 d S . . C1 C 0.66782(15) 0.36648(14) 0.22103(18) 0.0217(6) Uani 1 1 d . . . C2 C 0.72328(15) 0.36245(14) 0.14192(18) 0.0238(6) Uani 1 1 d . . . C3 C 0.73574(18) 0.28583(15) 0.1148(2) 0.0347(7) Uani 1 1 d . . . H3A H 0.7681 0.2840 0.0613 0.052 Uiso 1 1 calc R . . H3B H 0.6867 0.2638 0.1014 0.052 Uiso 1 1 calc R . . H3C H 0.7604 0.2605 0.1641 0.052 Uiso 1 1 calc R . . C4 C 0.68492(19) 0.40208(16) 0.0647(2) 0.0379(7) Uani 1 1 d . . . H4A H 0.7166 0.3989 0.0108 0.057 Uiso 1 1 calc R . . H4B H 0.6784 0.4517 0.0814 0.057 Uiso 1 1 calc R . . H4C H 0.6352 0.3810 0.0525 0.057 Uiso 1 1 calc R . . C5 C 0.79942(16) 0.39666(17) 0.1643(2) 0.0341(7) Uani 1 1 d . . . H5A H 0.8237 0.3708 0.2135 0.051 Uiso 1 1 calc R . . H5B H 0.7912 0.4457 0.1825 0.051 Uiso 1 1 calc R . . H5C H 0.8323 0.3954 0.1112 0.051 Uiso 1 1 calc R . . C6 C 0.54343(15) 0.31209(14) 0.47080(18) 0.0233(6) Uani 1 1 d . . . C7 C 0.53171(17) 0.28055(15) 0.56395(19) 0.0283(6) Uani 1 1 d . . . C8 C 0.6099(2) 0.2635(2) 0.6021(2) 0.0591(11) Uani 1 1 d . . . H8A H 0.6043 0.2419 0.6616 0.089 Uiso 1 1 calc R . . H8B H 0.6396 0.3069 0.6074 0.089 Uiso 1 1 calc R . . H8C H 0.6361 0.2306 0.5620 0.089 Uiso 1 1 calc R . . C9 C 0.4920(2) 0.33348(19) 0.6249(2) 0.0494(10) Uani 1 1 d . . . H9A H 0.4406 0.3422 0.6024 0.074 Uiso 1 1 calc R . . H9B H 0.5206 0.3778 0.6253 0.074 Uiso 1 1 calc R . . H9C H 0.4892 0.3145 0.6860 0.074 Uiso 1 1 calc R . . C10 C 0.4843(3) 0.2137(2) 0.5575(3) 0.0626(12) Uani 1 1 d . . . H10A H 0.4786 0.1930 0.6175 0.094 Uiso 1 1 calc R . . H10B H 0.5097 0.1799 0.5179 0.094 Uiso 1 1 calc R . . H10C H 0.4342 0.2252 0.5331 0.094 Uiso 1 1 calc R . . C11 C 0.46727(16) 0.43551(15) 0.23773(18) 0.0250(6) Uani 1 1 d . . . C12 C 0.41783(19) 0.47771(16) 0.1731(2) 0.0375(8) Uani 1 1 d . . . C13 C 0.3686(4) 0.5269(4) 0.2245(4) 0.145(3) Uani 1 1 d . . . H13A H 0.3432 0.5591 0.1828 0.217 Uiso 1 1 calc R . . H13B H 0.3997 0.5540 0.2667 0.217 Uiso 1 1 calc R . . H13C H 0.3305 0.4999 0.2578 0.217 Uiso 1 1 calc R . . C14 C 0.3739(4) 0.4329(2) 0.1138(4) 0.154(4) Uani 1 1 d . . . H14A H 0.3354 0.4077 0.1487 0.232 Uiso 1 1 calc R . . H14B H 0.4076 0.3988 0.0847 0.232 Uiso 1 1 calc R . . H14C H 0.3491 0.4619 0.0680 0.232 Uiso 1 1 calc R . . C15 C 0.4708(4) 0.5251(4) 0.1216(5) 0.186(5) Uani 1 1 d . . . H15A H 0.4986 0.4972 0.0770 0.279 Uiso 1 1 calc R . . H15B H 0.5068 0.5470 0.1633 0.279 Uiso 1 1 calc R . . H15C H 0.4414 0.5618 0.0911 0.279 Uiso 1 1 calc R . . C16 C 0.68451(16) 0.55729(14) 0.40008(19) 0.0272(6) Uani 1 1 d . . . H16 H 0.7025 0.5472 0.3413 0.033 Uiso 1 1 calc R . . C17 C 0.71527(17) 0.61368(15) 0.4452(2) 0.0340(7) Uani 1 1 d . . . H17 H 0.7545 0.6409 0.4186 0.041 Uiso 1 1 calc R . . C18 C 0.68839(18) 0.63018(15) 0.5294(2) 0.0369(7) Uani 1 1 d . . . H18 H 0.7085 0.6689 0.5620 0.044 Uiso 1 1 calc R . . C19 C 0.63159(19) 0.58902(17) 0.5649(2) 0.0405(8) Uani 1 1 d . . . H19 H 0.6106 0.6001 0.6219 0.049 Uiso 1 1 calc R . . C20 C 0.60525(17) 0.53158(15) 0.51721(19) 0.0322(7) Uani 1 1 d . . . H20 H 0.5678 0.5022 0.5437 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02636(17) 0.02136(16) 0.01797(16) -0.00220(13) 0.00113(13) -0.00121(13) Nd1 0.02588(12) 0.01617(11) 0.01623(11) -0.00187(8) 0.000 0.000 N1 0.0279(12) 0.0204(12) 0.0195(11) -0.0018(9) 0.0033(10) 0.0003(9) N2 0.030(2) 0.062(3) 0.112(5) -0.041(3) 0.000 0.000 O1 0.0503(14) 0.0381(13) 0.0694(17) -0.0202(12) 0.0325(13) -0.0194(11) O2 0.0285(11) 0.0355(12) 0.0234(10) -0.0099(9) 0.0030(8) -0.0029(9) O3 0.0672(16) 0.0339(12) 0.0201(11) -0.0034(9) -0.0033(10) -0.0141(11) O4 0.0498(13) 0.0264(11) 0.0231(11) 0.0012(9) 0.0013(9) -0.0096(9) O5 0.0604(15) 0.0235(12) 0.0432(14) -0.0042(10) -0.0158(11) 0.0106(10) O6 0.0301(11) 0.0284(11) 0.0307(11) -0.0006(9) -0.0059(9) 0.0017(9) O7 0.0431(14) 0.0506(15) 0.0665(18) -0.0310(13) 0.0180(13) -0.0079(12) O8 0.026(2) 0.190(6) 0.201(7) -0.070(5) 0.000 0.000 C1 0.0215(14) 0.0229(14) 0.0208(14) 0.0017(11) -0.0008(11) 0.0019(11) C2 0.0270(15) 0.0244(14) 0.0201(14) -0.0033(11) 0.0026(11) 0.0002(11) C3 0.0411(18) 0.0299(16) 0.0332(17) -0.0087(13) 0.0081(14) 0.0027(14) C4 0.049(2) 0.0394(18) 0.0256(16) 0.0010(14) -0.0013(14) 0.0048(15) C5 0.0291(16) 0.0394(18) 0.0337(17) -0.0054(14) 0.0090(13) -0.0026(14) C6 0.0263(14) 0.0242(15) 0.0193(14) 0.0013(12) -0.0006(11) 0.0017(11) C7 0.0397(17) 0.0269(15) 0.0184(14) 0.0018(12) 0.0027(12) 0.0018(13) C8 0.056(2) 0.092(3) 0.0294(19) 0.0189(19) 0.0000(17) 0.023(2) C9 0.075(3) 0.048(2) 0.0256(18) 0.0029(15) 0.0167(17) 0.0150(18) C10 0.100(3) 0.045(2) 0.043(2) 0.0117(18) 0.014(2) -0.027(2) C11 0.0275(15) 0.0253(15) 0.0221(14) 0.0001(12) 0.0035(12) 0.0046(12) C12 0.0446(19) 0.0329(17) 0.0349(18) 0.0072(14) -0.0113(15) 0.0093(15) C13 0.151(6) 0.184(7) 0.100(4) -0.040(4) -0.061(4) 0.137(6) C14 0.241(8) 0.049(3) 0.173(6) -0.013(3) -0.177(6) 0.022(4) C15 0.105(5) 0.254(9) 0.199(8) 0.203(8) -0.040(5) -0.026(5) C16 0.0342(16) 0.0223(15) 0.0251(15) -0.0002(12) 0.0085(12) 0.0013(12) C17 0.0350(17) 0.0244(15) 0.0425(18) -0.0033(14) 0.0151(14) -0.0064(13) C18 0.0403(18) 0.0282(16) 0.0422(19) -0.0125(14) 0.0070(15) -0.0093(13) C19 0.053(2) 0.0409(19) 0.0282(17) -0.0142(14) 0.0131(15) -0.0118(16) C20 0.0366(17) 0.0323(16) 0.0275(16) -0.0048(13) 0.0084(13) -0.0106(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.9397(19) . ? Zn1 O6 1.9444(19) . ? Zn1 O2 1.9697(19) . ? Zn1 N1 2.061(2) . ? Nd1 O3 2.366(2) 4 ? Nd1 O3 2.366(2) . ? Nd1 O1 2.395(2) . ? Nd1 O1 2.395(2) 4 ? Nd1 O5 2.403(2) 4 ? Nd1 O5 2.403(2) . ? Nd1 O7 2.534(2) 4 ? Nd1 O7 2.534(2) . ? N1 C16 1.334(3) . ? N1 C20 1.340(3) . ? N2 O8 1.206(6) . ? N2 O7 1.269(3) . ? N2 O7 1.269(3) 4 ? O1 C1 1.235(3) . ? O2 C1 1.261(3) . ? O3 C6 1.238(3) . ? O4 C6 1.266(3) . ? O5 C11 1.239(3) . ? O6 C11 1.269(3) . ? C1 C2 1.532(4) . ? C2 C3 1.525(4) . ? C2 C5 1.527(4) . ? C2 C4 1.531(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.524(4) . ? C7 C10 1.522(5) . ? C7 C9 1.524(4) . ? C7 C8 1.526(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(4) . ? C12 C14 1.449(5) . ? C12 C13 1.486(6) . ? C12 C15 1.505(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.376(4) . ? C17 H17 0.9500 . ? C18 C19 1.375(4) . ? C18 H18 0.9500 . ? C19 C20 1.381(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.51(9) . . ? O4 Zn1 O2 125.49(9) . . ? O6 Zn1 O2 106.71(8) . . ? O4 Zn1 N1 94.53(8) . . ? O6 Zn1 N1 103.78(8) . . ? O2 Zn1 N1 101.31(8) . . ? O3 Nd1 O3 162.33(12) 4 . ? O3 Nd1 O1 82.08(8) 4 . ? O3 Nd1 O1 83.68(8) . . ? O3 Nd1 O1 83.68(8) 4 4 ? O3 Nd1 O1 82.08(8) . 4 ? O1 Nd1 O1 72.41(13) . 4 ? O3 Nd1 O5 86.32(7) 4 4 ? O3 Nd1 O5 98.92(7) . 4 ? O1 Nd1 O5 142.90(9) . 4 ? O1 Nd1 O5 71.36(8) 4 4 ? O3 Nd1 O5 98.92(7) 4 . ? O3 Nd1 O5 86.32(7) . . ? O1 Nd1 O5 71.36(8) . . ? O1 Nd1 O5 142.90(9) 4 . ? O5 Nd1 O5 145.54(12) 4 . ? O3 Nd1 O7 73.63(9) 4 4 ? O3 Nd1 O7 124.03(8) . 4 ? O1 Nd1 O7 134.96(10) . 4 ? O1 Nd1 O7 138.84(7) 4 4 ? O5 Nd1 O7 73.29(8) 4 4 ? O5 Nd1 O7 75.63(8) . 4 ? O3 Nd1 O7 124.03(8) 4 . ? O3 Nd1 O7 73.63(9) . . ? O1 Nd1 O7 138.84(7) . . ? O1 Nd1 O7 134.96(10) 4 . ? O5 Nd1 O7 75.63(8) 4 . ? O5 Nd1 O7 73.29(8) . . ? O7 Nd1 O7 50.52(12) 4 . ? C16 N1 C20 117.6(2) . . ? C16 N1 Zn1 119.89(18) . . ? C20 N1 Zn1 122.55(19) . . ? O8 N2 O7 121.6(2) . . ? O8 N2 O7 121.6(2) . 4 ? O7 N2 O7 116.8(4) . 4 ? C1 O1 Nd1 171.4(2) . . ? C1 O2 Zn1 117.52(17) . . ? C6 O3 Nd1 159.23(19) . . ? C6 O4 Zn1 128.51(18) . . ? C11 O5 Nd1 160.2(2) . . ? C11 O6 Zn1 124.45(18) . . ? N2 O7 Nd1 96.3(2) . . ? O1 C1 O2 122.1(3) . . ? O1 C1 C2 119.1(2) . . ? O2 C1 C2 118.7(2) . . ? C3 C2 C5 109.7(2) . . ? C3 C2 C4 109.4(2) . . ? C5 C2 C4 110.1(2) . . ? C3 C2 C1 110.1(2) . . ? C5 C2 C1 111.8(2) . . ? C4 C2 C1 105.7(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.2(3) . . ? O3 C6 C7 119.9(2) . . ? O4 C6 C7 116.9(2) . . ? C10 C7 C9 109.5(3) . . ? C10 C7 C6 110.2(2) . . ? C9 C7 C6 110.2(2) . . ? C10 C7 C8 110.0(3) . . ? C9 C7 C8 109.5(3) . . ? C6 C7 C8 107.5(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.5(3) . . ? O5 C11 C12 119.3(3) . . ? O6 C11 C12 117.3(2) . . ? C14 C12 C13 111.7(5) . . ? C14 C12 C15 111.8(5) . . ? C13 C12 C15 104.4(5) . . ? C14 C12 C11 112.4(3) . . ? C13 C12 C11 109.8(3) . . ? C15 C12 C11 106.3(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.3(3) . . ? N1 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 118.1(3) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N1 C20 C19 122.2(3) . . ? N1 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.645 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.075 # start Validation Reply Form _vrf_PLAT220_7ag221ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.57 Ratio RESPONSE: slight disorder in the metyl group carbons cause large thermo parameters ; _vrf_PLAT222_7ag221ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.45 Ratio RESPONSE: see above ; _vrf_PLAT242_7ag221ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8jy161ss _database_code_depnum_ccdc_archive 'CCDC 753918' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SmZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 N3 O15 Sm Zn2' _chemical_formula_weight 1108.03 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6508(11) _cell_length_b 18.8573(11) _cell_length_c 14.8732(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4950.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8494 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.33 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 2.195 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34089 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.33 _reflns_number_total 4519 _reflns_number_gt 3899 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+4.4684P] 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 4519 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Zn1 Zn 0.590282(18) 0.431128(16) 0.36239(2) 0.02696(9) Uani 1 1 d . . . Sm1 Sm 0.507978(11) 0.2500 0.2500 0.02313(7) Uani 1 2 d S . . N1 N 0.63056(13) 0.51627(12) 0.43494(15) 0.0305(5) Uani 1 1 d . . . N2 N 0.3416(3) 0.2500 0.2500 0.0724(16) Uani 1 2 d S . . O1 O 0.61639(14) 0.32160(12) 0.22605(17) 0.0557(7) Uani 1 1 d . . . O2 O 0.67337(11) 0.41625(11) 0.27661(13) 0.0345(5) Uani 1 1 d . . . O3 O 0.52827(14) 0.27644(12) 0.40158(14) 0.0440(5) Uani 1 1 d . . . O4 O 0.57050(13) 0.37305(10) 0.46733(13) 0.0400(5) Uani 1 1 d . . . O5 O 0.46771(15) 0.36951(11) 0.23370(15) 0.0479(6) Uani 1 1 d . . . O6 O 0.50569(11) 0.46999(11) 0.29501(15) 0.0357(5) Uani 1 1 d . . . O7 O 0.37961(14) 0.25914(13) 0.32184(19) 0.0580(7) Uani 1 1 d . . . O8 O 0.2731(2) 0.2500 0.2500 0.138(3) Uani 1 2 d S . . C1 C 0.66750(15) 0.36591(14) 0.22128(18) 0.0268(6) Uani 1 1 d . . . C2 C 0.72319(16) 0.36230(15) 0.14269(19) 0.0314(6) Uani 1 1 d . . . C3 C 0.7358(2) 0.28529(18) 0.1147(2) 0.0495(9) Uani 1 1 d . . . H3A H 0.7674 0.2839 0.0605 0.074 Uiso 1 1 calc R . . H3B H 0.6869 0.2629 0.1021 0.074 Uiso 1 1 calc R . . H3C H 0.7613 0.2597 0.1634 0.074 Uiso 1 1 calc R . . C4 C 0.6844(2) 0.40261(19) 0.0652(2) 0.0500(9) Uani 1 1 d . . . H4A H 0.7156 0.3991 0.0109 0.075 Uiso 1 1 calc R . . H4B H 0.6784 0.4526 0.0819 0.075 Uiso 1 1 calc R . . H4C H 0.6345 0.3818 0.0536 0.075 Uiso 1 1 calc R . . C5 C 0.79883(18) 0.39669(19) 0.1645(2) 0.0488(9) Uani 1 1 d . . . H5A H 0.8235 0.3705 0.2133 0.073 Uiso 1 1 calc R . . H5B H 0.7905 0.4459 0.1833 0.073 Uiso 1 1 calc R . . H5C H 0.8313 0.3959 0.1110 0.073 Uiso 1 1 calc R . . C6 C 0.54352(16) 0.31098(15) 0.46963(18) 0.0286(6) Uani 1 1 d . . . C7 C 0.53148(19) 0.27845(17) 0.56262(19) 0.0369(7) Uani 1 1 d . . . C8 C 0.6089(2) 0.2621(3) 0.6013(3) 0.0730(13) Uani 1 1 d . . . H8A H 0.6031 0.2401 0.6605 0.109 Uiso 1 1 calc R . . H8B H 0.6379 0.3062 0.6072 0.109 Uiso 1 1 calc R . . H8C H 0.6358 0.2295 0.5611 0.109 Uiso 1 1 calc R . . C9 C 0.4901(2) 0.3312(2) 0.6234(2) 0.0624(11) Uani 1 1 d . . . H9A H 0.4394 0.3402 0.5993 0.094 Uiso 1 1 calc R . . H9B H 0.5186 0.3757 0.6257 0.094 Uiso 1 1 calc R . . H9C H 0.4859 0.3114 0.6841 0.094 Uiso 1 1 calc R . . C10 C 0.4847(3) 0.2109(2) 0.5550(3) 0.0734(13) Uani 1 1 d . . . H10A H 0.4790 0.1895 0.6146 0.110 Uiso 1 1 calc R . . H10B H 0.5104 0.1775 0.5148 0.110 Uiso 1 1 calc R . . H10C H 0.4346 0.2224 0.5306 0.110 Uiso 1 1 calc R . . C11 C 0.46698(17) 0.43497(15) 0.23872(19) 0.0303(6) Uani 1 1 d . . . C12 C 0.4162(2) 0.47684(17) 0.1746(2) 0.0451(8) Uani 1 1 d . . . C13 C 0.3714(4) 0.5307(4) 0.2251(4) 0.154(4) Uani 1 1 d . . . H13A H 0.3430 0.5602 0.1826 0.231 Uiso 1 1 calc R . . H13B H 0.4058 0.5606 0.2603 0.231 Uiso 1 1 calc R . . H13C H 0.3360 0.5066 0.2656 0.231 Uiso 1 1 calc R . . C14 C 0.3674(5) 0.4315(3) 0.1219(5) 0.181(4) Uani 1 1 d . . . H14A H 0.3305 0.4085 0.1615 0.271 Uiso 1 1 calc R . . H14B H 0.3980 0.3953 0.0917 0.271 Uiso 1 1 calc R . . H14C H 0.3407 0.4600 0.0769 0.271 Uiso 1 1 calc R . . C15 C 0.4686(4) 0.5178(6) 0.1153(6) 0.229(6) Uani 1 1 d . . . H15A H 0.4956 0.4850 0.0754 0.343 Uiso 1 1 calc R . . H15B H 0.5053 0.5436 0.1524 0.343 Uiso 1 1 calc R . . H15C H 0.4394 0.5515 0.0792 0.343 Uiso 1 1 calc R . . C16 C 0.68501(18) 0.55747(15) 0.4001(2) 0.0372(7) Uani 1 1 d . . . H16 H 0.7029 0.5473 0.3413 0.045 Uiso 1 1 calc R . . C17 C 0.71617(19) 0.61380(17) 0.4458(2) 0.0463(8) Uani 1 1 d . . . H17 H 0.7559 0.6409 0.4197 0.056 Uiso 1 1 calc R . . C18 C 0.68893(19) 0.63024(17) 0.5295(2) 0.0491(9) Uani 1 1 d . . . H18 H 0.7090 0.6692 0.5623 0.059 Uiso 1 1 calc R . . C19 C 0.6324(2) 0.58947(18) 0.5647(2) 0.0495(9) Uani 1 1 d . . . H19 H 0.6114 0.6006 0.6218 0.059 Uiso 1 1 calc R . . C20 C 0.60599(18) 0.53227(17) 0.5171(2) 0.0401(8) Uani 1 1 d . . . H20 H 0.5686 0.5028 0.5439 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03384(18) 0.02551(17) 0.02153(16) -0.00369(13) 0.00210(13) -0.00250(13) Sm1 0.03120(12) 0.01935(11) 0.01885(11) -0.00328(7) 0.000 0.000 N1 0.0381(14) 0.0268(13) 0.0267(12) -0.0050(10) 0.0072(10) -0.0035(10) N2 0.039(3) 0.060(3) 0.119(5) -0.040(3) 0.000 0.000 O1 0.0553(15) 0.0407(13) 0.0709(17) -0.0191(12) 0.0299(13) -0.0174(12) O2 0.0350(11) 0.0410(12) 0.0276(10) -0.0112(9) 0.0031(9) -0.0035(9) O3 0.0723(16) 0.0376(12) 0.0221(11) -0.0038(10) -0.0012(10) -0.0126(11) O4 0.0622(14) 0.0316(11) 0.0262(11) 0.0004(9) 0.0004(10) -0.0148(10) O5 0.0657(15) 0.0272(12) 0.0508(14) -0.0061(10) -0.0172(12) 0.0122(11) O6 0.0372(12) 0.0325(12) 0.0376(12) -0.0019(10) -0.0049(9) 0.0008(9) O7 0.0496(15) 0.0510(15) 0.0734(19) -0.0311(13) 0.0194(14) -0.0084(12) O8 0.032(2) 0.172(6) 0.209(7) -0.064(5) 0.000 0.000 C1 0.0282(14) 0.0255(15) 0.0266(14) 0.0015(11) -0.0016(11) 0.0021(12) C2 0.0327(15) 0.0325(16) 0.0290(15) -0.0043(12) 0.0042(12) 0.0004(12) C3 0.052(2) 0.047(2) 0.050(2) -0.0103(16) 0.0075(17) 0.0060(17) C4 0.064(2) 0.052(2) 0.0337(18) 0.0030(16) 0.0003(16) 0.0018(18) C5 0.0420(19) 0.057(2) 0.047(2) -0.0075(17) 0.0102(15) -0.0045(17) C6 0.0318(15) 0.0317(16) 0.0222(14) -0.0016(12) 0.0003(11) 0.0017(12) C7 0.0548(19) 0.0336(16) 0.0222(15) 0.0010(13) 0.0023(14) -0.0022(15) C8 0.072(3) 0.109(4) 0.038(2) 0.021(2) 0.000(2) 0.019(2) C9 0.096(3) 0.060(2) 0.0319(19) 0.0029(18) 0.0213(19) 0.011(2) C10 0.109(4) 0.061(3) 0.050(2) 0.011(2) 0.018(2) -0.032(3) C11 0.0334(15) 0.0282(16) 0.0294(15) 0.0006(12) 0.0028(12) 0.0051(12) C12 0.054(2) 0.0366(18) 0.0444(19) 0.0060(15) -0.0126(16) 0.0111(16) C13 0.167(6) 0.173(7) 0.122(5) -0.052(5) -0.077(5) 0.137(6) C14 0.257(9) 0.062(3) 0.223(8) -0.022(4) -0.204(8) 0.037(4) C15 0.108(5) 0.346(13) 0.232(9) 0.255(10) -0.006(6) 0.018(7) C16 0.0475(19) 0.0300(16) 0.0342(16) -0.0052(13) 0.0145(14) -0.0034(14) C17 0.050(2) 0.0328(17) 0.057(2) -0.0119(15) 0.0222(17) -0.0120(15) C18 0.053(2) 0.0396(19) 0.055(2) -0.0218(16) 0.0128(17) -0.0162(16) C19 0.061(2) 0.050(2) 0.0372(18) -0.0185(16) 0.0169(16) -0.0170(17) C20 0.0460(19) 0.0408(18) 0.0335(17) -0.0093(14) 0.0118(14) -0.0146(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.938(2) . ? Zn1 O6 1.942(2) . ? Zn1 O2 1.9640(19) . ? Zn1 N1 2.061(2) . ? Sm1 O3 2.337(2) . ? Sm1 O3 2.337(2) 4 ? Sm1 O1 2.369(2) . ? Sm1 O1 2.369(2) 4 ? Sm1 O5 2.375(2) 4 ? Sm1 O5 2.375(2) . ? Sm1 O7 2.511(2) 4 ? Sm1 O7 2.511(2) . ? N1 C20 1.331(4) . ? N1 C16 1.340(4) . ? N2 O8 1.210(6) . ? N2 O7 1.273(3) . ? N2 O7 1.273(3) 4 ? O1 C1 1.232(3) . ? O2 C1 1.261(3) . ? O3 C6 1.233(3) . ? O4 C6 1.264(3) . ? O5 C11 1.237(4) . ? O6 C11 1.267(4) . ? C1 C2 1.529(4) . ? C2 C5 1.519(4) . ? C2 C3 1.527(4) . ? C2 C4 1.541(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.528(4) . ? C7 C8 1.514(5) . ? C7 C10 1.522(5) . ? C7 C9 1.529(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(4) . ? C12 C14 1.444(6) . ? C12 C13 1.489(6) . ? C12 C15 1.493(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.370(4) . ? C17 H17 0.9500 . ? C18 C19 1.365(4) . ? C18 H18 0.9500 . ? C19 C20 1.372(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.36(9) . . ? O4 Zn1 O2 125.23(9) . . ? O6 Zn1 O2 107.03(9) . . ? O4 Zn1 N1 94.63(9) . . ? O6 Zn1 N1 103.97(9) . . ? O2 Zn1 N1 101.17(9) . . ? O3 Sm1 O3 162.36(12) . 4 ? O3 Sm1 O1 84.24(8) . . ? O3 Sm1 O1 81.53(8) 4 . ? O3 Sm1 O1 81.53(8) . 4 ? O3 Sm1 O1 84.24(8) 4 4 ? O1 Sm1 O1 72.24(13) . 4 ? O3 Sm1 O5 98.62(8) . 4 ? O3 Sm1 O5 86.67(8) 4 4 ? O1 Sm1 O5 142.92(9) . 4 ? O1 Sm1 O5 71.68(9) 4 4 ? O3 Sm1 O5 86.67(8) . . ? O3 Sm1 O5 98.62(8) 4 . ? O1 Sm1 O5 71.68(9) . . ? O1 Sm1 O5 142.92(9) 4 . ? O5 Sm1 O5 145.18(13) 4 . ? O3 Sm1 O7 124.30(9) . 4 ? O3 Sm1 O7 73.33(9) 4 4 ? O1 Sm1 O7 134.75(10) . 4 ? O1 Sm1 O7 138.92(7) 4 4 ? O5 Sm1 O7 73.04(9) 4 4 ? O5 Sm1 O7 75.62(8) . 4 ? O3 Sm1 O7 73.33(9) . . ? O3 Sm1 O7 124.30(9) 4 . ? O1 Sm1 O7 138.92(7) . . ? O1 Sm1 O7 134.75(10) 4 . ? O5 Sm1 O7 75.62(8) 4 . ? O5 Sm1 O7 73.04(9) . . ? O7 Sm1 O7 51.06(13) 4 . ? C20 N1 C16 117.2(2) . . ? C20 N1 Zn1 123.0(2) . . ? C16 N1 Zn1 119.80(19) . . ? O8 N2 O7 121.8(2) . . ? O8 N2 O7 121.8(2) . 4 ? O7 N2 O7 116.4(4) . 4 ? C1 O1 Sm1 170.7(2) . . ? C1 O2 Zn1 118.04(18) . . ? C6 O3 Sm1 159.7(2) . . ? C6 O4 Zn1 127.79(18) . . ? C11 O5 Sm1 160.7(2) . . ? C11 O6 Zn1 124.00(19) . . ? N2 O7 Sm1 96.2(2) . . ? O1 C1 O2 122.2(3) . . ? O1 C1 C2 119.0(2) . . ? O2 C1 C2 118.7(2) . . ? C5 C2 C3 109.6(3) . . ? C5 C2 C1 112.5(2) . . ? C3 C2 C1 110.2(2) . . ? C5 C2 C4 109.9(3) . . ? C3 C2 C4 109.3(3) . . ? C1 C2 C4 105.3(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.3(3) . . ? O3 C6 C7 120.0(3) . . ? O4 C6 C7 116.7(2) . . ? C8 C7 C10 110.4(3) . . ? C8 C7 C6 107.4(3) . . ? C10 C7 C6 110.1(3) . . ? C8 C7 C9 109.8(3) . . ? C10 C7 C9 109.2(3) . . ? C6 C7 C9 109.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.7(3) . . ? O5 C11 C12 119.0(3) . . ? O6 C11 C12 117.3(3) . . ? C14 C12 C13 111.1(5) . . ? C14 C12 C15 110.8(6) . . ? C13 C12 C15 105.9(6) . . ? C14 C12 C11 112.5(3) . . ? C13 C12 C11 110.4(3) . . ? C15 C12 C11 105.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.0(3) . . ? N1 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.9(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 118.6(3) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 119.5(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C20 C19 122.8(3) . . ? N1 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.688 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.074 # start Validation Reply Form _vrf_PLAT220_8jy161ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.55 Ratio RESPONSE: slight disorder is found in the methyl carbons and NO3 group that account for the abnormal thermoparameters ; _vrf_PLAT222_8jy161ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.62 Ratio RESPONSE:see above ; _vrf_PLAT242_8jy161ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8sp092ss _database_code_depnum_ccdc_archive 'CCDC 753919' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common EuZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Eu N3 O15 Zn2' _chemical_formula_weight 1109.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6371(11) _cell_length_b 18.8410(11) _cell_length_c 14.8698(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4941.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6597 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.30 _exptl_crystal_description cube _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 2.280 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.710 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34122 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.40 _reflns_number_total 4552 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+6.2491P] 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 4552 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Zn1 Zn 0.59034(2) 0.430890(18) 0.36231(2) 0.02683(11) Uani 1 1 d . . . Eu1 Eu 0.508557(12) 0.2500 0.2500 0.02286(8) Uani 1 2 d S . . N1 N 0.63040(15) 0.51625(13) 0.43504(17) 0.0306(6) Uani 1 1 d . . . N2 N 0.3428(3) 0.2500 0.2500 0.0681(17) Uani 1 2 d S . . O1 O 0.61650(16) 0.32133(14) 0.2259(2) 0.0548(7) Uani 1 1 d . . . O2 O 0.67350(13) 0.41610(12) 0.27663(15) 0.0347(5) Uani 1 1 d . . . O3 O 0.52877(16) 0.27559(13) 0.40119(15) 0.0437(6) Uani 1 1 d . . . O4 O 0.57061(15) 0.37243(12) 0.46695(15) 0.0408(6) Uani 1 1 d . . . O5 O 0.46822(17) 0.36899(13) 0.23294(18) 0.0471(7) Uani 1 1 d . . . O6 O 0.50553(13) 0.46946(13) 0.29467(17) 0.0355(5) Uani 1 1 d . . . O7 O 0.38095(17) 0.25920(14) 0.3217(2) 0.0576(8) Uani 1 1 d . . . O8 O 0.2748(3) 0.2500 0.2500 0.134(3) Uani 1 2 d S . . C1 C 0.66748(17) 0.36552(16) 0.2212(2) 0.0259(6) Uani 1 1 d . . . C2 C 0.72347(18) 0.36213(17) 0.1427(2) 0.0321(7) Uani 1 1 d . . . C3 C 0.7358(2) 0.2850(2) 0.1145(3) 0.0483(9) Uani 1 1 d . . . H3A H 0.7663 0.2836 0.0595 0.072 Uiso 1 1 calc R . . H3B H 0.6866 0.2624 0.1034 0.072 Uiso 1 1 calc R . . H3C H 0.7624 0.2595 0.1626 0.072 Uiso 1 1 calc R . . C4 C 0.6848(2) 0.4025(2) 0.0654(2) 0.0509(10) Uani 1 1 d . . . H4A H 0.7159 0.3988 0.0110 0.076 Uiso 1 1 calc R . . H4B H 0.6792 0.4526 0.0819 0.076 Uiso 1 1 calc R . . H4C H 0.6347 0.3820 0.0539 0.076 Uiso 1 1 calc R . . C5 C 0.7991(2) 0.3965(2) 0.1650(3) 0.0489(10) Uani 1 1 d . . . H5A H 0.8234 0.3704 0.2142 0.073 Uiso 1 1 calc R . . H5B H 0.7907 0.4458 0.1835 0.073 Uiso 1 1 calc R . . H5C H 0.8318 0.3955 0.1118 0.073 Uiso 1 1 calc R . . C6 C 0.54361(18) 0.31020(16) 0.46915(19) 0.0278(7) Uani 1 1 d . . . C7 C 0.5313(2) 0.27783(19) 0.5621(2) 0.0373(8) Uani 1 1 d . . . C8 C 0.6086(3) 0.2617(3) 0.6014(3) 0.0721(15) Uani 1 1 d . . . H8A H 0.6026 0.2394 0.6605 0.108 Uiso 1 1 calc R . . H8B H 0.6374 0.3060 0.6080 0.108 Uiso 1 1 calc R . . H8C H 0.6360 0.2294 0.5613 0.108 Uiso 1 1 calc R . . C9 C 0.4900(3) 0.3307(3) 0.6227(3) 0.0624(13) Uani 1 1 d . . . H9A H 0.4389 0.3391 0.5991 0.094 Uiso 1 1 calc R . . H9B H 0.5181 0.3755 0.6241 0.094 Uiso 1 1 calc R . . H9C H 0.4865 0.3113 0.6837 0.094 Uiso 1 1 calc R . . C10 C 0.4847(3) 0.2100(3) 0.5543(3) 0.0725(15) Uani 1 1 d . . . H10A H 0.4781 0.1890 0.6140 0.109 Uiso 1 1 calc R . . H10B H 0.5111 0.1762 0.5151 0.109 Uiso 1 1 calc R . . H10C H 0.4349 0.2211 0.5286 0.109 Uiso 1 1 calc R . . C11 C 0.4671(2) 0.43433(17) 0.2383(2) 0.0301(7) Uani 1 1 d . . . C12 C 0.4160(2) 0.47622(19) 0.1750(3) 0.0454(9) Uani 1 1 d . . . C13 C 0.3722(5) 0.5312(5) 0.2247(5) 0.151(4) Uani 1 1 d . . . H13A H 0.3416 0.5587 0.1822 0.227 Uiso 1 1 calc R . . H13B H 0.4073 0.5629 0.2563 0.227 Uiso 1 1 calc R . . H13C H 0.3388 0.5080 0.2685 0.227 Uiso 1 1 calc R . . C14 C 0.3663(6) 0.4312(3) 0.1238(7) 0.193(6) Uani 1 1 d . . . H14A H 0.3268 0.4120 0.1633 0.290 Uiso 1 1 calc R . . H14B H 0.3955 0.3920 0.0977 0.290 Uiso 1 1 calc R . . H14C H 0.3426 0.4588 0.0755 0.290 Uiso 1 1 calc R . . C15 C 0.4678(5) 0.5159(7) 0.1141(7) 0.236(7) Uani 1 1 d . . . H15A H 0.4950 0.4823 0.0755 0.354 Uiso 1 1 calc R . . H15B H 0.5044 0.5429 0.1501 0.354 Uiso 1 1 calc R . . H15C H 0.4383 0.5486 0.0767 0.354 Uiso 1 1 calc R . . C16 C 0.6850(2) 0.55735(17) 0.4003(2) 0.0386(8) Uani 1 1 d . . . H16 H 0.7029 0.5472 0.3414 0.046 Uiso 1 1 calc R . . C17 C 0.7165(2) 0.61378(19) 0.4462(3) 0.0473(10) Uani 1 1 d . . . H17 H 0.7565 0.6407 0.4204 0.057 Uiso 1 1 calc R . . C18 C 0.6889(2) 0.6302(2) 0.5301(3) 0.0506(10) Uani 1 1 d . . . H18 H 0.7089 0.6691 0.5631 0.061 Uiso 1 1 calc R . . C19 C 0.6322(2) 0.5894(2) 0.5650(3) 0.0499(10) Uani 1 1 d . . . H19 H 0.6111 0.6007 0.6220 0.060 Uiso 1 1 calc R . . C20 C 0.6057(2) 0.53186(19) 0.5175(2) 0.0404(8) Uani 1 1 d . . . H20 H 0.5685 0.5022 0.5444 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0351(2) 0.02545(19) 0.01991(18) -0.00393(14) 0.00228(14) -0.00258(14) Eu1 0.03239(13) 0.01919(13) 0.01699(13) -0.00314(8) 0.000 0.000 N1 0.0388(15) 0.0273(14) 0.0258(13) -0.0069(11) 0.0055(11) -0.0040(11) N2 0.037(3) 0.056(3) 0.111(5) -0.038(3) 0.000 0.000 O1 0.0566(17) 0.0406(15) 0.0672(18) -0.0164(13) 0.0272(14) -0.0164(13) O2 0.0352(12) 0.0412(13) 0.0276(11) -0.0114(10) 0.0046(10) -0.0024(10) O3 0.0726(17) 0.0388(13) 0.0196(12) -0.0050(11) -0.0034(12) -0.0124(13) O4 0.0650(16) 0.0332(13) 0.0243(12) 0.0013(10) 0.0007(11) -0.0149(11) O5 0.0664(17) 0.0266(13) 0.0484(15) -0.0052(11) -0.0165(13) 0.0106(12) O6 0.0389(13) 0.0327(13) 0.0350(14) -0.0023(11) -0.0048(10) 0.0004(10) O7 0.0512(17) 0.0501(17) 0.071(2) -0.0296(15) 0.0181(16) -0.0076(13) O8 0.037(3) 0.166(7) 0.201(8) -0.061(5) 0.000 0.000 C1 0.0280(16) 0.0264(16) 0.0232(15) 0.0025(12) 0.0000(12) 0.0014(12) C2 0.0343(17) 0.0348(17) 0.0271(16) -0.0045(13) 0.0049(13) -0.0004(14) C3 0.054(2) 0.047(2) 0.044(2) -0.0122(18) 0.0087(18) 0.0050(18) C4 0.066(3) 0.057(2) 0.0299(19) 0.0040(17) 0.0009(18) 0.003(2) C5 0.040(2) 0.059(2) 0.047(2) -0.0082(19) 0.0117(17) -0.0052(18) C6 0.0341(16) 0.0314(17) 0.0177(15) -0.0013(13) -0.0001(12) 0.0019(13) C7 0.055(2) 0.0348(18) 0.0224(17) 0.0015(14) 0.0036(15) -0.0041(17) C8 0.073(3) 0.108(4) 0.036(2) 0.022(2) -0.002(2) 0.018(3) C9 0.097(4) 0.061(3) 0.029(2) 0.002(2) 0.019(2) 0.016(2) C10 0.110(4) 0.056(3) 0.051(3) 0.009(2) 0.017(3) -0.031(3) C11 0.0362(17) 0.0267(17) 0.0275(16) 0.0009(13) 0.0020(14) 0.0047(14) C12 0.058(2) 0.037(2) 0.041(2) 0.0045(16) -0.0144(18) 0.0126(17) C13 0.160(7) 0.178(8) 0.117(5) -0.045(5) -0.068(5) 0.132(7) C14 0.271(11) 0.064(4) 0.244(10) -0.021(5) -0.223(10) 0.033(5) C15 0.114(6) 0.355(16) 0.239(11) 0.265(12) -0.008(7) 0.021(8) C16 0.048(2) 0.0313(18) 0.0365(19) -0.0060(15) 0.0141(16) -0.0047(15) C17 0.049(2) 0.0349(19) 0.058(2) -0.0105(17) 0.0215(19) -0.0117(16) C18 0.057(2) 0.042(2) 0.053(2) -0.0217(18) 0.013(2) -0.0150(18) C19 0.062(3) 0.053(2) 0.035(2) -0.0196(17) 0.0165(18) -0.0188(19) C20 0.048(2) 0.0402(19) 0.0326(18) -0.0112(15) 0.0112(16) -0.0142(16) _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 Zn1 O4 1.938(2) . ? Zn1 O6 1.943(2) . ? Zn1 O2 1.963(2) . ? Zn1 N1 2.063(2) . ? Eu1 O3 2.327(2) 4 ? Eu1 O3 2.327(2) . ? Eu1 O1 2.358(3) . ? Eu1 O1 2.358(3) 4 ? Eu1 O5 2.366(2) 4 ? Eu1 O5 2.366(2) . ? Eu1 O7 2.496(3) 4 ? Eu1 O7 2.496(3) . ? N1 C20 1.335(4) . ? N1 C16 1.339(4) . ? N2 O8 1.199(7) . ? N2 O7 1.273(4) 4 ? N2 O7 1.273(4) . ? O1 C1 1.228(4) . ? O2 C1 1.265(4) . ? O3 C6 1.231(4) . ? O4 C6 1.266(4) . ? O5 C11 1.234(4) . ? O6 C11 1.266(4) . ? C1 C2 1.530(4) . ? C2 C5 1.519(5) . ? C2 C3 1.528(5) . ? C2 C4 1.539(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.527(4) . ? C7 C8 1.515(6) . ? C7 C10 1.524(6) . ? C7 C9 1.527(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.524(5) . ? C12 C14 1.438(7) . ? C12 C15 1.488(8) . ? C12 C13 1.489(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.380(5) . ? C16 H16 0.9500 . ? C17 C18 1.374(5) . ? C17 H17 0.9500 . ? C18 C19 1.363(5) . ? C18 H18 0.9500 . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.33(11) . . ? O4 Zn1 O2 125.08(11) . . ? O6 Zn1 O2 107.00(10) . . ? O4 Zn1 N1 94.80(10) . . ? O6 Zn1 N1 104.09(10) . . ? O2 Zn1 N1 101.25(10) . . ? O3 Eu1 O3 162.38(14) 4 . ? O3 Eu1 O1 81.22(10) 4 . ? O3 Eu1 O1 84.56(10) . . ? O3 Eu1 O1 84.56(10) 4 4 ? O3 Eu1 O1 81.22(10) . 4 ? O1 Eu1 O1 72.31(15) . 4 ? O3 Eu1 O5 87.32(9) 4 4 ? O3 Eu1 O5 97.98(9) . 4 ? O1 Eu1 O5 143.06(10) . 4 ? O1 Eu1 O5 71.72(10) 4 4 ? O3 Eu1 O5 97.98(9) 4 . ? O3 Eu1 O5 87.32(9) . . ? O1 Eu1 O5 71.72(10) . . ? O1 Eu1 O5 143.06(10) 4 . ? O5 Eu1 O5 145.00(15) 4 . ? O3 Eu1 O7 73.21(10) 4 4 ? O3 Eu1 O7 124.41(10) . 4 ? O1 Eu1 O7 134.63(11) . 4 ? O1 Eu1 O7 138.88(9) 4 4 ? O5 Eu1 O7 73.07(10) 4 4 ? O5 Eu1 O7 75.46(9) . 4 ? O3 Eu1 O7 124.41(10) 4 . ? O3 Eu1 O7 73.21(10) . . ? O1 Eu1 O7 138.88(9) . . ? O1 Eu1 O7 134.63(11) 4 . ? O5 Eu1 O7 75.46(9) 4 . ? O5 Eu1 O7 73.07(10) . . ? O7 Eu1 O7 51.27(15) 4 . ? C20 N1 C16 117.5(3) . . ? C20 N1 Zn1 122.8(2) . . ? C16 N1 Zn1 119.7(2) . . ? O8 N2 O7 121.9(2) . 4 ? O8 N2 O7 121.9(2) . . ? O7 N2 O7 116.1(5) 4 . ? C1 O1 Eu1 170.7(2) . . ? C1 O2 Zn1 117.9(2) . . ? C6 O3 Eu1 159.3(2) . . ? C6 O4 Zn1 127.9(2) . . ? C11 O5 Eu1 160.7(3) . . ? C11 O6 Zn1 124.0(2) . . ? N2 O7 Eu1 96.3(3) . . ? O1 C1 O2 122.4(3) . . ? O1 C1 C2 119.2(3) . . ? O2 C1 C2 118.3(3) . . ? C5 C2 C3 109.9(3) . . ? C5 C2 C1 112.5(3) . . ? C3 C2 C1 109.9(3) . . ? C5 C2 C4 110.0(3) . . ? C3 C2 C4 109.2(3) . . ? C1 C2 C4 105.3(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.3(3) . . ? O3 C6 C7 120.1(3) . . ? O4 C6 C7 116.5(3) . . ? C8 C7 C10 110.3(4) . . ? C8 C7 C6 107.5(3) . . ? C10 C7 C6 110.0(3) . . ? C8 C7 C9 109.4(4) . . ? C10 C7 C9 109.6(4) . . ? C6 C7 C9 110.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.7(3) . . ? O5 C11 C12 119.1(3) . . ? O6 C11 C12 117.1(3) . . ? C14 C12 C15 110.5(7) . . ? C14 C12 C13 110.9(6) . . ? C15 C12 C13 105.8(7) . . ? C14 C12 C11 112.4(4) . . ? C15 C12 C11 105.8(4) . . ? C13 C12 C11 111.1(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.0(3) . . ? N1 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.6(3) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19 C18 C17 118.6(3) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N1 C20 C19 122.3(3) . . ? N1 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.546 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.095 # start Validation Reply Form _vrf_PLAT213_8sp092ss ; PROBLEM: Atom C15 has ADP max/min Ratio ..... 5.10 prola RESPONSE: disorder in the metyl carbons of the OBc ligand causes large thermo parameters. modeling this disorder did not improve the refinement value therefore was forgone ; _vrf_PLAT220_8sp092ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.11 Ratio RESPONSE: see above ; _vrf_PLAT222_8sp092ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.70 Ratio RESPONSE: see above ; _vrf_PLAT242_8sp092ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_7ag292ss _database_code_depnum_ccdc_archive 'CCDC 753920' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common GdZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Gd N3 O15 Zn2' _chemical_formula_weight 1114.93 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6518(11) _cell_length_b 18.8458(11) _cell_length_c 14.8744(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4948.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9144 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.37 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2276 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.754 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34327 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0118 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4553 _reflns_number_gt 4231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+5.1312P] 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 4553 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Zn1 Zn 0.590695(14) 0.430664(12) 0.362226(16) 0.02261(7) Uani 1 1 d . . . Gd1 Gd 0.508865(8) 0.2500 0.2500 0.01943(6) Uani 1 2 d S . . N1 N 0.63031(10) 0.51599(9) 0.43535(12) 0.0244(4) Uani 1 1 d . . . N2 N 0.3440(2) 0.2500 0.2500 0.0589(11) Uani 1 2 d S . . O1 O 0.61625(11) 0.32124(10) 0.22660(14) 0.0453(5) Uani 1 1 d . . . O2 O 0.67434(9) 0.41602(9) 0.27699(10) 0.0296(4) Uani 1 1 d . . . O3 O 0.52900(11) 0.27479(9) 0.40066(11) 0.0374(4) Uani 1 1 d . . . O4 O 0.57037(10) 0.37212(8) 0.46665(10) 0.0337(4) Uani 1 1 d . . . O5 O 0.46825(12) 0.36815(9) 0.23219(12) 0.0399(4) Uani 1 1 d . . . O6 O 0.50596(9) 0.46879(9) 0.29418(11) 0.0301(4) Uani 1 1 d . . . O7 O 0.38184(11) 0.25931(10) 0.32150(15) 0.0482(5) Uani 1 1 d . . . O8 O 0.2755(2) 0.2500 0.2500 0.1126(19) Uani 1 2 d S . . C1 C 0.66768(12) 0.36553(11) 0.22121(14) 0.0229(4) Uani 1 1 d . . . C2 C 0.72322(12) 0.36188(11) 0.14249(14) 0.0251(5) Uani 1 1 d . . . C3 C 0.73588(15) 0.28444(13) 0.11489(17) 0.0363(6) Uani 1 1 d . . . H3A H 0.7673 0.2828 0.0606 0.054 Uiso 1 1 calc R . . H3B H 0.6869 0.2619 0.1028 0.054 Uiso 1 1 calc R . . H3C H 0.7616 0.2591 0.1637 0.054 Uiso 1 1 calc R . . C4 C 0.68486(15) 0.40224(14) 0.06528(16) 0.0372(6) Uani 1 1 d . . . H4A H 0.7169 0.3998 0.0115 0.056 Uiso 1 1 calc R . . H4B H 0.6777 0.4520 0.0826 0.056 Uiso 1 1 calc R . . H4C H 0.6355 0.3807 0.0524 0.056 Uiso 1 1 calc R . . C5 C 0.79917(13) 0.39619(14) 0.16509(17) 0.0352(5) Uani 1 1 d . . . H5A H 0.8235 0.3697 0.2139 0.053 Uiso 1 1 calc R . . H5B H 0.7909 0.4454 0.1841 0.053 Uiso 1 1 calc R . . H5C H 0.8318 0.3955 0.1118 0.053 Uiso 1 1 calc R . . C6 C 0.54339(12) 0.30984(11) 0.46900(14) 0.0243(4) Uani 1 1 d . . . C7 C 0.53079(14) 0.27768(13) 0.56234(15) 0.0302(5) Uani 1 1 d . . . C8 C 0.60864(19) 0.26105(19) 0.60172(19) 0.0561(8) Uani 1 1 d . . . H8A H 0.6025 0.2385 0.6607 0.084 Uiso 1 1 calc R . . H8B H 0.6375 0.3051 0.6084 0.084 Uiso 1 1 calc R . . H8C H 0.6358 0.2288 0.5613 0.084 Uiso 1 1 calc R . . C9 C 0.48992(18) 0.33075(16) 0.62247(18) 0.0481(7) Uani 1 1 d . . . H9A H 0.4393 0.3401 0.5982 0.072 Uiso 1 1 calc R . . H9B H 0.5188 0.3751 0.6246 0.072 Uiso 1 1 calc R . . H9C H 0.4854 0.3112 0.6833 0.072 Uiso 1 1 calc R . . C10 C 0.4840(2) 0.21010(17) 0.5544(2) 0.0601(9) Uani 1 1 d . . . H10A H 0.4774 0.1890 0.6141 0.090 Uiso 1 1 calc R . . H10B H 0.5101 0.1763 0.5151 0.090 Uiso 1 1 calc R . . H10C H 0.4342 0.2215 0.5289 0.090 Uiso 1 1 calc R . . C11 C 0.46718(13) 0.43374(12) 0.23769(15) 0.0256(5) Uani 1 1 d . . . C12 C 0.41662(15) 0.47640(13) 0.17413(18) 0.0387(6) Uani 1 1 d . . . C13 C 0.3728(3) 0.5305(3) 0.2244(3) 0.147(3) Uani 1 1 d . . . H13A H 0.3451 0.5606 0.1819 0.220 Uiso 1 1 calc R . . H13B H 0.4075 0.5598 0.2599 0.220 Uiso 1 1 calc R . . H13C H 0.3368 0.5068 0.2646 0.220 Uiso 1 1 calc R . . C14 C 0.3674(4) 0.4308(2) 0.1211(4) 0.167(4) Uani 1 1 d . . . H14A H 0.3294 0.4090 0.1604 0.251 Uiso 1 1 calc R . . H14B H 0.3977 0.3936 0.0924 0.251 Uiso 1 1 calc R . . H14C H 0.3420 0.4592 0.0748 0.251 Uiso 1 1 calc R . . C15 C 0.4685(3) 0.5173(5) 0.1151(5) 0.221(5) Uani 1 1 d . . . H15A H 0.4902 0.4857 0.0696 0.332 Uiso 1 1 calc R . . H15B H 0.5093 0.5378 0.1514 0.332 Uiso 1 1 calc R . . H15C H 0.4402 0.5555 0.0855 0.332 Uiso 1 1 calc R . . C16 C 0.68477(13) 0.55713(11) 0.40100(16) 0.0287(5) Uani 1 1 d . . . H16 H 0.7027 0.5471 0.3422 0.034 Uiso 1 1 calc R . . C17 C 0.71605(14) 0.61338(12) 0.44691(17) 0.0349(6) Uani 1 1 d . . . H17 H 0.7559 0.6403 0.4209 0.042 Uiso 1 1 calc R . . C18 C 0.68873(15) 0.62999(13) 0.53102(18) 0.0393(6) Uani 1 1 d . . . H18 H 0.7090 0.6688 0.5640 0.047 Uiso 1 1 calc R . . C19 C 0.63138(16) 0.58907(14) 0.56608(17) 0.0419(6) Uani 1 1 d . . . H19 H 0.6103 0.6001 0.6232 0.050 Uiso 1 1 calc R . . C20 C 0.60466(14) 0.53171(13) 0.51750(16) 0.0338(5) Uani 1 1 d . . . H20 H 0.5667 0.5024 0.5435 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02613(13) 0.02204(13) 0.01965(13) -0.00236(9) 0.00136(10) -0.00116(10) Gd1 0.02500(9) 0.01629(9) 0.01700(9) -0.00177(5) 0.000 0.000 N1 0.0282(10) 0.0217(9) 0.0232(9) -0.0027(7) 0.0036(7) -0.0006(7) N2 0.0310(18) 0.048(2) 0.098(3) -0.030(2) 0.000 0.000 O1 0.0436(10) 0.0332(10) 0.0591(12) -0.0120(9) 0.0219(9) -0.0140(8) O2 0.0273(8) 0.0359(9) 0.0255(8) -0.0084(7) 0.0028(7) -0.0011(7) O3 0.0588(11) 0.0330(9) 0.0205(8) -0.0035(7) -0.0024(8) -0.0091(9) O4 0.0494(10) 0.0282(8) 0.0235(8) 0.0016(7) 0.0012(7) -0.0118(7) O5 0.0513(11) 0.0231(9) 0.0454(10) -0.0022(7) -0.0128(9) 0.0091(8) O6 0.0308(8) 0.0277(8) 0.0320(9) -0.0011(7) -0.0053(7) 0.0010(7) O7 0.0396(11) 0.0436(11) 0.0615(13) -0.0228(9) 0.0162(10) -0.0058(8) O8 0.0270(18) 0.139(4) 0.171(5) -0.045(3) 0.000 0.000 C1 0.0228(11) 0.0216(11) 0.0242(11) 0.0029(9) -0.0005(9) 0.0032(8) C2 0.0265(11) 0.0258(11) 0.0230(11) -0.0030(9) 0.0024(9) 0.0002(9) C3 0.0398(14) 0.0306(13) 0.0385(14) -0.0096(11) 0.0065(11) 0.0036(11) C4 0.0478(15) 0.0384(14) 0.0254(12) 0.0032(10) -0.0005(11) 0.0013(12) C5 0.0280(12) 0.0407(14) 0.0369(13) -0.0056(11) 0.0077(10) -0.0042(10) C6 0.0256(11) 0.0263(11) 0.0210(11) 0.0001(9) 0.0000(9) 0.0021(9) C7 0.0424(13) 0.0288(12) 0.0195(11) 0.0018(9) 0.0028(10) 0.0012(11) C8 0.0559(18) 0.085(2) 0.0277(14) 0.0144(14) -0.0011(13) 0.0199(16) C9 0.071(2) 0.0481(17) 0.0252(13) 0.0035(12) 0.0148(13) 0.0134(14) C10 0.092(3) 0.0461(18) 0.0419(17) 0.0102(14) 0.0139(16) -0.0255(17) C11 0.0263(11) 0.0245(11) 0.0260(11) 0.0018(9) 0.0030(9) 0.0037(9) C12 0.0450(15) 0.0326(13) 0.0386(14) 0.0056(11) -0.0121(12) 0.0092(11) C13 0.162(5) 0.172(6) 0.106(4) -0.051(4) -0.070(4) 0.139(5) C14 0.233(7) 0.056(2) 0.213(6) -0.027(3) -0.193(6) 0.036(3) C15 0.101(4) 0.329(11) 0.233(8) 0.255(8) -0.022(5) -0.001(5) C16 0.0345(12) 0.0230(11) 0.0287(12) -0.0012(9) 0.0106(10) 0.0002(9) C17 0.0353(13) 0.0243(11) 0.0452(14) -0.0032(10) 0.0142(11) -0.0057(10) C18 0.0419(14) 0.0307(13) 0.0453(15) -0.0145(11) 0.0086(12) -0.0114(11) C19 0.0508(16) 0.0442(15) 0.0308(13) -0.0146(11) 0.0150(12) -0.0151(12) C20 0.0362(13) 0.0344(13) 0.0307(13) -0.0068(10) 0.0110(10) -0.0110(10) _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 Zn1 O4 1.9387(15) . ? Zn1 O6 1.9437(16) . ? Zn1 O2 1.9656(16) . ? Zn1 N1 2.0635(17) . ? Gd1 O3 2.3166(16) . ? Gd1 O3 2.3166(16) 4 ? Gd1 O1 2.3489(17) . ? Gd1 O1 2.3489(17) 4 ? Gd1 O5 2.3542(17) . ? Gd1 O5 2.3542(17) 4 ? Gd1 O7 2.4878(19) 4 ? Gd1 O7 2.4878(19) . ? N1 C20 1.336(3) . ? N1 C16 1.337(3) . ? N2 O8 1.210(5) . ? N2 O7 1.268(3) . ? N2 O7 1.268(3) 4 ? O1 C1 1.236(3) . ? O2 C1 1.268(3) . ? O3 C6 1.239(3) . ? O4 C6 1.267(3) . ? O5 C11 1.239(3) . ? O6 C11 1.269(3) . ? C1 C2 1.529(3) . ? C2 C5 1.526(3) . ? C2 C3 1.532(3) . ? C2 C4 1.535(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(3) . ? C7 C10 1.523(4) . ? C7 C9 1.523(3) . ? C7 C8 1.526(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(3) . ? C12 C14 1.453(5) . ? C12 C13 1.483(5) . ? C12 C15 1.484(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.376(3) . ? C16 H16 0.9500 . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 C19 1.375(4) . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 119.02(7) . . ? O4 Zn1 O2 125.16(7) . . ? O6 Zn1 O2 107.10(7) . . ? O4 Zn1 N1 94.81(7) . . ? O6 Zn1 N1 104.31(7) . . ? O2 Zn1 N1 101.24(7) . . ? O3 Gd1 O3 162.34(10) . 4 ? O3 Gd1 O1 84.50(7) . . ? O3 Gd1 O1 81.26(7) 4 . ? O3 Gd1 O1 81.26(7) . 4 ? O3 Gd1 O1 84.50(7) 4 4 ? O1 Gd1 O1 72.39(10) . 4 ? O3 Gd1 O5 87.98(6) . . ? O3 Gd1 O5 97.39(6) 4 . ? O1 Gd1 O5 71.85(7) . . ? O1 Gd1 O5 143.43(7) 4 . ? O3 Gd1 O5 97.39(6) . 4 ? O3 Gd1 O5 87.98(6) 4 4 ? O1 Gd1 O5 143.43(7) . 4 ? O1 Gd1 O5 71.85(7) 4 4 ? O5 Gd1 O5 144.54(10) . 4 ? O3 Gd1 O7 124.48(7) . 4 ? O3 Gd1 O7 73.17(7) 4 4 ? O1 Gd1 O7 134.78(8) . 4 ? O1 Gd1 O7 138.62(6) 4 4 ? O5 Gd1 O7 75.18(6) . 4 ? O5 Gd1 O7 72.96(7) 4 4 ? O3 Gd1 O7 73.17(7) . . ? O3 Gd1 O7 124.48(7) 4 . ? O1 Gd1 O7 138.62(6) . . ? O1 Gd1 O7 134.78(8) 4 . ? O5 Gd1 O7 72.96(7) . . ? O5 Gd1 O7 75.18(6) 4 . ? O7 Gd1 O7 51.35(10) 4 . ? C20 N1 C16 117.69(19) . . ? C20 N1 Zn1 122.67(15) . . ? C16 N1 Zn1 119.63(14) . . ? O8 N2 O7 121.76(16) . . ? O8 N2 O7 121.76(16) . 4 ? O7 N2 O7 116.5(3) . 4 ? C1 O1 Gd1 171.30(16) . . ? C1 O2 Zn1 117.24(14) . . ? C6 O3 Gd1 158.90(16) . . ? C6 O4 Zn1 128.23(14) . . ? C11 O5 Gd1 160.20(18) . . ? C11 O6 Zn1 124.56(15) . . ? N2 O7 Gd1 96.08(18) . . ? O1 C1 O2 122.2(2) . . ? O1 C1 C2 119.36(19) . . ? O2 C1 C2 118.39(19) . . ? C5 C2 C1 112.07(18) . . ? C5 C2 C3 109.54(19) . . ? C1 C2 C3 109.98(18) . . ? C5 C2 C4 110.0(2) . . ? C1 C2 C4 105.54(18) . . ? C3 C2 C4 109.62(19) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.3(2) . . ? O3 C6 C7 120.2(2) . . ? O4 C6 C7 116.50(19) . . ? C10 C7 C9 109.7(2) . . ? C10 C7 C8 110.3(3) . . ? C9 C7 C8 109.6(2) . . ? C10 C7 C6 109.86(19) . . ? C9 C7 C6 110.0(2) . . ? C8 C7 C6 107.4(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.7(2) . . ? O5 C11 C12 119.5(2) . . ? O6 C11 C12 116.8(2) . . ? C14 C12 C13 111.6(4) . . ? C14 C12 C15 110.8(5) . . ? C13 C12 C15 105.2(5) . . ? C14 C12 C11 111.9(2) . . ? C13 C12 C11 110.8(3) . . ? C15 C12 C11 106.2(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.1(2) . . ? N1 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C16 C17 C18 119.0(2) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 118.3(2) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 119.4(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N1 C20 C19 122.4(2) . . ? N1 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.666 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.066 # start Validation Reply Form _vrf_PLAT213_7ag292ss ; PROBLEM: Atom C15 has ADP max/min Ratio ..... 5.60 prola RESPONSE: slight disorder in the methyl groups of the OBc ligands cause large thermo parameters however modeling this disorder did not prove to improve structure and was forgone ; _vrf_PLAT220_7ag292ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.65 Ratio RESPONSE: see above ; _vrf_PLAT222_7ag292ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.77 Ratio RESPONSE: see above ; _vrf_PLAT242_7ag292ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8sp021s _database_code_depnum_ccdc_archive 'CCDC 753921' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TbZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H74 N5 O15 Tb Zn2' _chemical_formula_weight 1274.844 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 13.447(3) _cell_length_b 15.763(4) _cell_length_c 16.151(4) _cell_angle_alpha 76.244(4) _cell_angle_beta 71.392(4) _cell_angle_gamma 72.483(4) _cell_volume 3055.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18348 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 23.23 _reflns_number_total 8667 _reflns_number_gt 6540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8667 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.36952(7) 0.38975(5) 0.00076(5) 0.0334(2) Uani 1 1 d . . . Zn2 Zn -0.01088(7) 0.13405(5) 0.33991(6) 0.0376(2) Uani 1 1 d . . . Tb1 Tb 0.23375(3) 0.25255(2) 0.22865(2) 0.02834(13) Uani 1 1 d . . . N1 N 0.4346(5) 0.4588(4) -0.1212(4) 0.0326(14) Uani 1 1 d . . . N2 N -0.1425(5) 0.0779(4) 0.3965(4) 0.0384(15) Uani 1 1 d . . . N3 N 0.3576(5) 0.2228(5) 0.3577(4) 0.0484(18) Uani 1 1 d . . . O1 O 0.4972(4) 0.3077(3) 0.0322(3) 0.0423(13) Uani 1 1 d . . . O2 O 0.4163(4) 0.2304(3) 0.1547(3) 0.0464(14) Uani 1 1 d . . . O3 O 0.2493(5) 0.2371(4) 0.0848(3) 0.0551(16) Uani 1 1 d . . . O4 O 0.2888(4) 0.3323(4) -0.0380(3) 0.0491(14) Uani 1 1 d . . . O5 O 0.3024(4) 0.4929(3) 0.0625(3) 0.0488(14) Uani 1 1 d . . . O6 O 0.2289(4) 0.4014(3) 0.1760(3) 0.0445(13) Uani 1 1 d . . . O7 O 0.3229(4) 0.3015(4) 0.3192(3) 0.0464(14) Uani 1 1 d . . . O8 O 0.3371(4) 0.1596(4) 0.3386(3) 0.0489(14) Uani 1 1 d . . . O9 O 0.4103(5) 0.2106(5) 0.4124(4) 0.077(2) Uani 1 1 d . . . O10 O 0.1158(4) 0.2614(4) 0.3697(4) 0.0599(16) Uani 1 1 d . . . O11 O -0.0080(4) 0.1840(4) 0.4379(3) 0.0518(15) Uani 1 1 d . . . O12 O 0.2107(4) 0.1100(3) 0.2538(3) 0.0450(14) Uani 1 1 d . . . O13 O 0.0975(4) 0.0221(3) 0.3131(4) 0.0551(16) Uani 1 1 d . . . O14 O 0.0600(4) 0.3025(4) 0.2118(4) 0.0606(17) Uani 1 1 d . . . O15 O -0.0701(4) 0.2306(3) 0.2576(4) 0.0510(15) Uani 1 1 d . . . C1 C 0.4991(5) 0.2430(5) 0.0950(4) 0.0291(16) Uani 1 1 d . . . C2 C 0.6082(6) 0.1769(5) 0.0991(5) 0.050(2) Uani 1 1 d . . . C3 C 0.6141(8) 0.1492(10) 0.1939(7) 0.134(6) Uani 1 1 d . . . H3A H 0.6895 0.1217 0.1951 0.202 Uiso 1 1 calc R . . H3B H 0.5704 0.1054 0.2243 0.202 Uiso 1 1 calc R . . H3C H 0.5862 0.2023 0.2236 0.202 Uiso 1 1 calc R . . C4 C 0.6101(9) 0.0976(7) 0.0602(9) 0.110(5) Uani 1 1 d . . . H4A H 0.6083 0.1175 -0.0017 0.165 Uiso 1 1 calc R . . H4B H 0.5468 0.0737 0.0937 0.165 Uiso 1 1 calc R . . H4C H 0.6763 0.0505 0.0634 0.165 Uiso 1 1 calc R . . C5 C 0.6993(7) 0.2168(7) 0.0429(7) 0.079(3) Uani 1 1 d . . . H5A H 0.6933 0.2730 0.0624 0.118 Uiso 1 1 calc R . . H5B H 0.6968 0.2295 -0.0189 0.118 Uiso 1 1 calc R . . H5C H 0.7681 0.1744 0.0482 0.118 Uiso 1 1 calc R . . C6 C 0.2541(6) 0.2644(5) 0.0049(5) 0.0364(18) Uani 1 1 d . . . C7 C 0.2260(6) 0.2101(6) -0.0476(5) 0.045(2) Uani 1 1 d . . . C8 C 0.3303(7) 0.1545(6) -0.0968(6) 0.068(3) Uani 1 1 d . . . H8A H 0.3719 0.1943 -0.1410 0.102 Uiso 1 1 calc R . . H8B H 0.3148 0.1143 -0.1264 0.102 Uiso 1 1 calc R . . H8C H 0.3722 0.1187 -0.0551 0.102 Uiso 1 1 calc R . . C9 C 0.1666(9) 0.2764(7) -0.1133(7) 0.089(4) Uani 1 1 d . . . H9A H 0.2067 0.3224 -0.1449 0.134 Uiso 1 1 calc R . . H9B H 0.0936 0.3054 -0.0810 0.134 Uiso 1 1 calc R . . H9C H 0.1616 0.2437 -0.1558 0.134 Uiso 1 1 calc R . . C10 C 0.1556(10) 0.1488(8) 0.0157(7) 0.110(5) Uani 1 1 d . . . H10A H 0.1320 0.1185 -0.0184 0.165 Uiso 1 1 calc R . . H10B H 0.0921 0.1850 0.0531 0.165 Uiso 1 1 calc R . . H10C H 0.1976 0.1037 0.0530 0.165 Uiso 1 1 calc R . . C11 C 0.2408(6) 0.4787(5) 0.1395(5) 0.0344(18) Uani 1 1 d . . . C12 C 0.1786(6) 0.5579(5) 0.1890(5) 0.043(2) Uani 1 1 d . . . C13 C 0.1023(9) 0.6172(7) 0.1343(8) 0.094(4) Uani 1 1 d . . . H13A H 0.0462 0.5870 0.1393 0.141 Uiso 1 1 calc R . . H13B H 0.1432 0.6278 0.0722 0.141 Uiso 1 1 calc R . . H13C H 0.0684 0.6749 0.1562 0.141 Uiso 1 1 calc R . . C14 C 0.2552(7) 0.6106(6) 0.1912(7) 0.069(3) Uani 1 1 d . . . H14A H 0.2133 0.6655 0.2164 0.103 Uiso 1 1 calc R . . H14B H 0.2983 0.6268 0.1309 0.103 Uiso 1 1 calc R . . H14C H 0.3034 0.5735 0.2276 0.103 Uiso 1 1 calc R . . C15 C 0.1178(12) 0.5277(8) 0.2796(8) 0.151(7) Uani 1 1 d . . . H15A H 0.1621 0.4723 0.3052 0.227 Uiso 1 1 calc R . . H15B H 0.0510 0.5159 0.2777 0.227 Uiso 1 1 calc R . . H15C H 0.0997 0.5746 0.3160 0.227 Uiso 1 1 calc R . . C16 C 0.4650(6) 0.5336(5) -0.1245(5) 0.0398(19) Uani 1 1 d . . . H16 H 0.4580 0.5533 -0.0713 0.048 Uiso 1 1 calc R . . C17 C 0.5069(7) 0.5825(5) -0.2063(6) 0.055(2) Uani 1 1 d . . . H17 H 0.5275 0.6359 -0.2087 0.065 Uiso 1 1 calc R . . C18 C 0.5180(8) 0.5533(6) -0.2820(6) 0.064(3) Uani 1 1 d . . . H18 H 0.5487 0.5849 -0.3377 0.077 Uiso 1 1 calc R . . C19 C 0.4850(7) 0.4786(6) -0.2780(5) 0.060(3) Uani 1 1 d . . . H19 H 0.4904 0.4586 -0.3307 0.072 Uiso 1 1 calc R . . C20 C 0.4438(7) 0.4327(6) -0.1969(5) 0.051(2) Uani 1 1 d . . . H20 H 0.4210 0.3804 -0.1942 0.061 Uiso 1 1 calc R . . C21 C 0.0407(6) 0.2446(5) 0.4328(5) 0.0405(19) Uani 1 1 d . . . C22 C 0.0012(7) 0.2983(5) 0.5088(5) 0.053(2) Uani 1 1 d . . . C23 C -0.0785(13) 0.3797(9) 0.4856(8) 0.155(7) Uani 1 1 d . . . H23A H -0.1417 0.3632 0.4825 0.233 Uiso 1 1 calc R . . H23B H -0.0463 0.4119 0.4280 0.233 Uiso 1 1 calc R . . H23C H -0.1009 0.4187 0.5307 0.233 Uiso 1 1 calc R . . C24 C 0.0979(10) 0.3249(10) 0.5177(8) 0.130(6) Uani 1 1 d . . . H24A H 0.1237 0.3665 0.4649 0.195 Uiso 1 1 calc R . . H24B H 0.1564 0.2709 0.5239 0.195 Uiso 1 1 calc R . . H24C H 0.0753 0.3544 0.5701 0.195 Uiso 1 1 calc R . . C25 C -0.0389(11) 0.2434(7) 0.5940(6) 0.108(5) Uani 1 1 d . . . H25A H -0.0550 0.2772 0.6423 0.162 Uiso 1 1 calc R . . H25B H 0.0164 0.1875 0.6023 0.162 Uiso 1 1 calc R . . H25C H -0.1049 0.2289 0.5941 0.162 Uiso 1 1 calc R . . C26 C 0.1930(7) 0.0335(5) 0.2737(5) 0.042(2) Uani 1 1 d . . . C27 C 0.2846(7) -0.0476(5) 0.2541(6) 0.054(2) Uani 1 1 d . . . C28 C 0.3811(11) -0.0236(10) 0.2040(19) 0.33(2) Uani 1 1 d . . . H28A H 0.4388 -0.0782 0.1922 0.489 Uiso 1 1 calc R . . H28B H 0.4010 0.0106 0.2370 0.489 Uiso 1 1 calc R . . H28C H 0.3711 0.0134 0.1479 0.489 Uiso 1 1 calc R . . C29 C 0.2529(11) -0.1072(11) 0.2134(12) 0.171(8) Uani 1 1 d . . . H29A H 0.2132 -0.0705 0.1705 0.256 Uiso 1 1 calc R . . H29B H 0.2066 -0.1421 0.2597 0.256 Uiso 1 1 calc R . . H29C H 0.3180 -0.1484 0.1833 0.256 Uiso 1 1 calc R . . C30 C 0.3027(16) -0.1054(13) 0.3362(12) 0.239(13) Uani 1 1 d . . . H30A H 0.3251 -0.1686 0.3278 0.358 Uiso 1 1 calc R . . H30B H 0.2356 -0.0956 0.3838 0.358 Uiso 1 1 calc R . . H30C H 0.3595 -0.0906 0.3518 0.358 Uiso 1 1 calc R . . C31 C -0.0304(6) 0.2973(5) 0.2166(5) 0.0383(19) Uani 1 1 d . . . C32 C -0.1079(6) 0.3783(5) 0.1755(5) 0.041(2) Uani 1 1 d . . . C33 C -0.1811(8) 0.3475(7) 0.1444(8) 0.094(4) Uani 1 1 d . . . H33A H -0.2342 0.3243 0.1954 0.141 Uiso 1 1 calc R . . H33B H -0.1389 0.2996 0.1089 0.141 Uiso 1 1 calc R . . H33C H -0.2188 0.3981 0.1081 0.141 Uiso 1 1 calc R . . C34 C -0.1684(10) 0.4358(7) 0.2459(8) 0.109(4) Uani 1 1 d . . . H34A H -0.2199 0.4878 0.2233 0.164 Uiso 1 1 calc R . . H34B H -0.1173 0.4569 0.2629 0.164 Uiso 1 1 calc R . . H34C H -0.2078 0.4006 0.2975 0.164 Uiso 1 1 calc R . . C35 C -0.0405(8) 0.4316(6) 0.0988(7) 0.084(3) Uani 1 1 d . . . H35A H 0.0029 0.3932 0.0538 0.126 Uiso 1 1 calc R . . H35B H 0.0075 0.4519 0.1202 0.126 Uiso 1 1 calc R . . H35C H -0.0885 0.4839 0.0729 0.126 Uiso 1 1 calc R . . C36 C -0.2402(7) 0.1206(6) 0.3838(5) 0.051(2) Uani 1 1 d . . . H36 H -0.2479 0.1776 0.3469 0.061 Uiso 1 1 calc R . . C37 C -0.3301(7) 0.0860(6) 0.4214(6) 0.062(3) Uani 1 1 d . . . H37 H -0.3980 0.1177 0.4103 0.075 Uiso 1 1 calc R . . C38 C -0.3179(7) 0.0037(6) 0.4758(6) 0.059(2) Uani 1 1 d . . . H38 H -0.3778 -0.0226 0.5029 0.070 Uiso 1 1 calc R . . C39 C -0.2200(7) -0.0393(6) 0.4902(6) 0.059(3) Uani 1 1 d . . . H39 H -0.2107 -0.0957 0.5280 0.071 Uiso 1 1 calc R . . C40 C -0.1343(6) -0.0007(5) 0.4498(5) 0.042(2) Uani 1 1 d . . . H40 H -0.0660 -0.0316 0.4605 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0396(5) 0.0284(5) 0.0298(5) 0.0030(4) -0.0048(4) -0.0158(4) Zn2 0.0371(5) 0.0269(5) 0.0438(5) 0.0066(4) -0.0066(4) -0.0146(4) Tb1 0.0304(2) 0.0235(2) 0.0282(2) 0.00234(14) -0.00137(15) -0.01416(15) N1 0.038(4) 0.030(3) 0.028(3) 0.000(3) -0.004(3) -0.016(3) N2 0.040(4) 0.031(4) 0.046(4) 0.008(3) -0.013(3) -0.020(3) N3 0.042(4) 0.062(5) 0.041(4) -0.002(4) 0.000(3) -0.027(4) O1 0.039(3) 0.037(3) 0.043(3) 0.009(3) -0.005(3) -0.016(2) O2 0.038(3) 0.046(3) 0.039(3) 0.011(3) -0.001(3) -0.012(3) O3 0.086(5) 0.054(4) 0.035(3) -0.006(3) -0.010(3) -0.038(3) O4 0.065(4) 0.050(3) 0.043(3) 0.002(3) -0.010(3) -0.041(3) O5 0.059(4) 0.040(3) 0.040(3) -0.004(3) 0.004(3) -0.021(3) O6 0.057(4) 0.023(3) 0.047(3) 0.002(2) -0.008(3) -0.014(3) O7 0.051(3) 0.056(4) 0.041(3) 0.000(3) -0.003(3) -0.042(3) O8 0.051(4) 0.051(4) 0.048(3) 0.010(3) -0.015(3) -0.031(3) O9 0.058(4) 0.124(6) 0.065(4) -0.025(4) -0.036(4) -0.014(4) O10 0.054(4) 0.072(4) 0.053(4) -0.029(3) 0.017(3) -0.032(3) O11 0.061(4) 0.051(4) 0.040(3) 0.002(3) 0.001(3) -0.032(3) O12 0.064(4) 0.028(3) 0.040(3) 0.008(2) -0.010(3) -0.022(3) O13 0.044(3) 0.032(3) 0.080(4) 0.007(3) -0.005(3) -0.020(3) O14 0.038(3) 0.055(4) 0.088(5) 0.017(3) -0.024(3) -0.024(3) O15 0.049(3) 0.039(3) 0.064(4) 0.023(3) -0.025(3) -0.022(3) C1 0.029(4) 0.029(4) 0.027(4) -0.005(3) 0.001(3) -0.014(3) C2 0.041(5) 0.042(5) 0.044(5) 0.007(4) -0.004(4) 0.003(4) C3 0.052(7) 0.200(15) 0.063(8) 0.043(8) 0.001(6) 0.028(8) C4 0.081(8) 0.044(6) 0.174(13) -0.023(8) -0.006(8) 0.004(6) C5 0.043(6) 0.077(7) 0.091(8) 0.015(6) -0.006(5) -0.011(5) C6 0.029(4) 0.043(5) 0.038(5) -0.013(4) -0.001(4) -0.014(4) C7 0.049(5) 0.057(5) 0.040(5) -0.008(4) -0.018(4) -0.021(4) C8 0.069(7) 0.053(6) 0.083(7) -0.032(5) -0.008(6) -0.013(5) C9 0.109(9) 0.084(8) 0.106(9) -0.036(7) -0.070(8) -0.007(7) C10 0.157(12) 0.144(11) 0.070(7) -0.024(7) 0.004(7) -0.125(10) C11 0.050(5) 0.029(4) 0.030(4) 0.002(3) -0.015(4) -0.019(4) C12 0.042(5) 0.031(4) 0.052(5) -0.004(4) -0.007(4) -0.013(4) C13 0.088(8) 0.066(7) 0.147(11) -0.037(7) -0.063(8) 0.005(6) C14 0.069(7) 0.048(6) 0.095(8) -0.034(5) -0.018(6) -0.007(5) C15 0.219(17) 0.091(9) 0.093(10) -0.046(8) 0.090(10) -0.079(11) C16 0.040(5) 0.040(5) 0.038(5) 0.001(4) -0.004(4) -0.021(4) C17 0.059(6) 0.039(5) 0.062(6) 0.016(4) -0.010(5) -0.031(4) C18 0.084(7) 0.080(7) 0.032(5) 0.012(5) -0.005(5) -0.051(6) C19 0.077(7) 0.079(7) 0.030(5) 0.000(5) -0.007(5) -0.044(6) C20 0.065(6) 0.061(6) 0.037(5) -0.006(4) -0.001(4) -0.045(5) C21 0.046(5) 0.031(4) 0.035(5) 0.000(4) 0.003(4) -0.015(4) C22 0.066(6) 0.039(5) 0.040(5) -0.008(4) 0.016(4) -0.024(4) C23 0.213(17) 0.107(11) 0.091(10) -0.059(9) -0.036(10) 0.071(11) C24 0.128(12) 0.182(14) 0.109(10) -0.095(10) 0.022(9) -0.081(11) C25 0.197(14) 0.086(8) 0.031(6) -0.012(5) 0.008(7) -0.057(9) C26 0.053(5) 0.036(5) 0.035(5) 0.006(4) -0.009(4) -0.020(4) C27 0.044(5) 0.032(5) 0.080(7) -0.013(5) -0.010(5) -0.007(4) C28 0.077(11) 0.083(11) 0.66(5) -0.12(2) 0.155(19) -0.011(9) C29 0.095(11) 0.171(15) 0.28(2) -0.166(16) -0.038(12) 0.012(10) C30 0.26(2) 0.186(19) 0.170(18) -0.029(15) -0.104(18) 0.138(18) C31 0.041(5) 0.030(4) 0.031(4) 0.002(3) -0.001(4) -0.005(4) C32 0.040(5) 0.038(5) 0.048(5) 0.008(4) -0.026(4) -0.010(4) C33 0.077(8) 0.074(7) 0.133(10) 0.035(7) -0.062(8) -0.027(6) C34 0.109(10) 0.057(7) 0.129(11) -0.018(7) -0.029(8) 0.027(7) C35 0.092(8) 0.062(7) 0.082(8) 0.037(6) -0.027(6) -0.032(6) C36 0.051(6) 0.046(5) 0.045(5) 0.017(4) -0.008(4) -0.022(4) C37 0.040(5) 0.074(7) 0.071(6) 0.017(5) -0.021(5) -0.026(5) C38 0.048(6) 0.078(7) 0.056(6) 0.008(5) -0.010(5) -0.041(5) C39 0.061(6) 0.045(5) 0.068(6) 0.010(5) -0.007(5) -0.033(5) C40 0.033(4) 0.042(5) 0.047(5) 0.013(4) -0.010(4) -0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.918(5) . ? Zn1 O5 1.940(5) . ? Zn1 O1 1.946(5) . ? Zn1 N1 2.069(5) . ? Zn2 O15 1.924(5) . ? Zn2 O11 1.944(5) . ? Zn2 O13 1.960(5) . ? Zn2 N2 2.067(6) . ? Tb1 O12 2.283(5) . ? Tb1 O6 2.286(5) . ? Tb1 O14 2.312(5) . ? Tb1 O2 2.320(5) . ? Tb1 O3 2.330(5) . ? Tb1 O10 2.331(5) . ? Tb1 O8 2.518(5) . ? Tb1 O7 2.526(5) . ? Tb1 N3 2.935(8) . ? N1 C20 1.339(9) . ? N1 C16 1.344(9) . ? N2 C40 1.326(9) . ? N2 C36 1.341(9) . ? N3 O8 1.236(8) . ? N3 O9 1.248(8) . ? N3 O7 1.270(8) . ? O1 C1 1.257(8) . ? O2 C1 1.251(8) . ? O3 C6 1.247(8) . ? O4 C6 1.260(8) . ? O5 C11 1.267(8) . ? O6 C11 1.255(8) . ? O10 C21 1.228(8) . ? O11 C21 1.284(9) . ? O12 C26 1.247(8) . ? O13 C26 1.285(9) . ? O14 C31 1.220(9) . ? O15 C31 1.269(8) . ? C1 C2 1.534(10) . ? C2 C5 1.484(11) . ? C2 C3 1.509(12) . ? C2 C4 1.518(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.530(10) . ? C7 C8 1.498(11) . ? C7 C10 1.529(12) . ? C7 C9 1.538(12) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.522(10) . ? C12 C15 1.475(12) . ? C12 C14 1.517(11) . ? C12 C13 1.522(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.400(10) . ? C16 H16 0.9500 . ? C17 C18 1.357(12) . ? C17 H17 0.9500 . ? C18 C19 1.359(12) . ? C18 H18 0.9500 . ? C19 C20 1.369(10) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.521(11) . ? C22 C23 1.462(14) . ? C22 C25 1.475(11) . ? C22 C24 1.538(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.499(11) . ? C27 C28 1.400(15) . ? C27 C30 1.465(17) . ? C27 C29 1.487(14) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.548(10) . ? C32 C33 1.476(12) . ? C32 C34 1.493(13) . ? C32 C35 1.519(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.377(11) . ? C36 H36 0.9500 . ? C37 C38 1.380(11) . ? C37 H37 0.9500 . ? C38 C39 1.353(11) . ? C38 H38 0.9500 . ? C39 C40 1.370(10) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O5 122.9(2) . . ? O4 Zn1 O1 113.5(2) . . ? O5 Zn1 O1 116.2(2) . . ? O4 Zn1 N1 97.6(2) . . ? O5 Zn1 N1 97.3(2) . . ? O1 Zn1 N1 102.7(2) . . ? O15 Zn2 O11 108.8(2) . . ? O15 Zn2 O13 127.3(2) . . ? O11 Zn2 O13 116.7(2) . . ? O15 Zn2 N2 99.0(2) . . ? O11 Zn2 N2 101.4(2) . . ? O13 Zn2 N2 96.8(2) . . ? O12 Tb1 O6 163.86(18) . . ? O12 Tb1 O14 86.79(19) . . ? O6 Tb1 O14 80.25(19) . . ? O12 Tb1 O2 101.40(18) . . ? O6 Tb1 O2 84.17(18) . . ? O14 Tb1 O2 144.7(2) . . ? O12 Tb1 O3 80.35(18) . . ? O6 Tb1 O3 86.86(18) . . ? O14 Tb1 O3 74.2(2) . . ? O2 Tb1 O3 73.51(19) . . ? O12 Tb1 O10 84.31(19) . . ? O6 Tb1 O10 100.85(19) . . ? O14 Tb1 O10 73.0(2) . . ? O2 Tb1 O10 141.5(2) . . ? O3 Tb1 O10 144.4(2) . . ? O12 Tb1 O8 72.86(18) . . ? O6 Tb1 O8 123.25(18) . . ? O14 Tb1 O8 141.23(18) . . ? O2 Tb1 O8 73.05(17) . . ? O3 Tb1 O8 131.4(2) . . ? O10 Tb1 O8 72.5(2) . . ? O12 Tb1 O7 122.36(18) . . ? O6 Tb1 O7 73.71(19) . . ? O14 Tb1 O7 130.8(2) . . ? O2 Tb1 O7 72.97(18) . . ? O3 Tb1 O7 142.60(17) . . ? O10 Tb1 O7 72.01(18) . . ? O8 Tb1 O7 50.22(18) . . ? O12 Tb1 N3 97.2(2) . . ? O6 Tb1 N3 98.9(2) . . ? O14 Tb1 N3 142.4(2) . . ? O2 Tb1 N3 71.17(18) . . ? O3 Tb1 N3 143.35(19) . . ? O10 Tb1 N3 70.32(19) . . ? O8 Tb1 N3 24.71(17) . . ? O7 Tb1 N3 25.50(17) . . ? C20 N1 C16 119.1(6) . . ? C20 N1 Zn1 121.7(5) . . ? C16 N1 Zn1 119.1(5) . . ? C40 N2 C36 117.2(6) . . ? C40 N2 Zn2 121.1(5) . . ? C36 N2 Zn2 121.7(5) . . ? O8 N3 O9 121.9(8) . . ? O8 N3 O7 117.3(7) . . ? O9 N3 O7 120.8(8) . . ? O8 N3 Tb1 58.4(4) . . ? O9 N3 Tb1 179.7(6) . . ? O7 N3 Tb1 58.9(4) . . ? C1 O1 Zn1 126.8(4) . . ? C1 O2 Tb1 157.9(5) . . ? C6 O3 Tb1 155.1(5) . . ? C6 O4 Zn1 124.9(5) . . ? C11 O5 Zn1 116.2(5) . . ? C11 O6 Tb1 171.0(5) . . ? N3 O7 Tb1 95.6(4) . . ? N3 O8 Tb1 96.9(5) . . ? C21 O10 Tb1 155.9(5) . . ? C21 O11 Zn2 126.6(5) . . ? C26 O12 Tb1 175.2(5) . . ? C26 O13 Zn2 113.4(5) . . ? C31 O14 Tb1 156.8(5) . . ? C31 O15 Zn2 125.5(5) . . ? O2 C1 O1 123.1(6) . . ? O2 C1 C2 118.5(6) . . ? O1 C1 C2 118.4(6) . . ? C5 C2 C3 111.4(9) . . ? C5 C2 C4 108.6(8) . . ? C3 C2 C4 111.5(9) . . ? C5 C2 C1 110.9(7) . . ? C3 C2 C1 109.9(7) . . ? C4 C2 C1 104.4(7) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.1(7) . . ? O3 C6 C7 120.0(7) . . ? O4 C6 C7 116.7(7) . . ? C8 C7 C10 110.0(8) . . ? C8 C7 C6 107.4(6) . . ? C10 C7 C6 109.7(7) . . ? C8 C7 C9 110.1(7) . . ? C10 C7 C9 111.1(8) . . ? C6 C7 C9 108.4(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 121.9(7) . . ? O6 C11 C12 119.0(6) . . ? O5 C11 C12 119.1(6) . . ? C15 C12 C14 110.5(9) . . ? C15 C12 C13 111.0(10) . . ? C14 C12 C13 108.9(7) . . ? C15 C12 C11 111.3(7) . . ? C14 C12 C11 110.3(6) . . ? C13 C12 C11 104.7(7) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 120.1(7) . . ? N1 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 119.5(8) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.9(8) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 118.9(8) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N1 C20 C19 122.4(7) . . ? N1 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? O10 C21 O11 123.3(7) . . ? O10 C21 C22 119.1(7) . . ? O11 C21 C22 117.7(6) . . ? C23 C22 C25 114.3(10) . . ? C23 C22 C21 107.3(8) . . ? C25 C22 C21 111.5(7) . . ? C23 C22 C24 109.2(10) . . ? C25 C22 C24 105.9(9) . . ? C21 C22 C24 108.6(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O12 C26 O13 121.3(7) . . ? O12 C26 C27 120.0(7) . . ? O13 C26 C27 118.7(7) . . ? C28 C27 C30 108.4(15) . . ? C28 C27 C29 113.6(14) . . ? C30 C27 C29 102.0(13) . . ? C28 C27 C26 111.9(8) . . ? C30 C27 C26 110.7(9) . . ? C29 C27 C26 109.8(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O14 C31 O15 124.7(7) . . ? O14 C31 C32 119.8(7) . . ? O15 C31 C32 115.3(7) . . ? C33 C32 C34 112.1(9) . . ? C33 C32 C35 110.1(8) . . ? C34 C32 C35 108.8(8) . . ? C33 C32 C31 110.9(7) . . ? C34 C32 C31 106.3(7) . . ? C35 C32 C31 108.5(7) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N2 C36 C37 123.4(7) . . ? N2 C36 H36 118.3 . . ? C37 C36 H36 118.3 . . ? C36 C37 C38 117.5(8) . . ? C36 C37 H37 121.2 . . ? C38 C37 H37 121.2 . . ? C39 C38 C37 119.6(8) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 119.3(8) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N2 C40 C39 123.0(7) . . ? N2 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.369 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.112 # start Validation Reply Form _vrf_PLAT213_8sp021s ; PROBLEM: Atom C28 has ADP max/min Ratio ..... 6.30 prola RESPONSE: disorder in the methyl carbons and NO3 moeity cause large thermo parameters. modeling of these ligands did not improve the overall structure and was abandoned. ; _vrf_PLAT220_8sp021s ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT222_8sp021s ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT242_8sp021s ; PROBLEM: Check Low Ueq as Compared to Neighbors for C22 RESPONSE: see above ; _vrf_PLAT602_8sp021s ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: disordered pyridene solvent was removed using PLATON. 949A^3 removed. see the the squeeze file in the supplimental for more information ; _vrf_CHEMW03_8sp021s ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: see above ; _vrf_DENSD01_8sp021s ; PROBLEM: The ratio of the submitted crystal density and that RESPONSE: see above ; _vrf_PLAT043_8sp021s ; PROBLEM: Check Reported Molecular Weight ................ 1274.84 RESPONSE:this MW includes the two py squezzed out with PLATON ; _vrf_PLAT046_8sp021s ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.39 RESPONSE: see above ; # end Validation Reply Form #===END data_7ag241ss _database_code_depnum_ccdc_archive 'CCDC 753922' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DyZnNO3Obcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Dy N3 O15 Zn2' _chemical_formula_weight 1120.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6784(11) _cell_length_b 18.7747(11) _cell_length_c 14.8566(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4931.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6675 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.37 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.287 _exptl_crystal_size_mid 0.147 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34146 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.37 _reflns_number_total 4533 _reflns_number_gt 4042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+4.7485P] 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 4533 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.015 _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 Zn1 Zn 0.590622(16) 0.430568(14) 0.362175(18) 0.02191(8) Uani 1 1 d . . . Dy1 Dy 0.509776(9) 0.2500 0.2500 0.01888(6) Uani 1 2 d S . . N1 N 0.63013(11) 0.51598(10) 0.43556(13) 0.0231(4) Uani 1 1 d . . . N2 N 0.3463(2) 0.2500 0.2500 0.0544(12) Uani 1 2 d S . . O1 O 0.61611(12) 0.32065(10) 0.22643(14) 0.0413(5) Uani 1 1 d . . . O2 O 0.67430(10) 0.41573(10) 0.27730(12) 0.0287(4) Uani 1 1 d . . . O3 O 0.52933(12) 0.27402(10) 0.39928(12) 0.0351(4) Uani 1 1 d . . . O4 O 0.57014(11) 0.37154(9) 0.46639(12) 0.0335(4) Uani 1 1 d . . . O5 O 0.46924(12) 0.36716(10) 0.23142(13) 0.0374(5) Uani 1 1 d . . . O6 O 0.50589(10) 0.46844(10) 0.29419(13) 0.0295(4) Uani 1 1 d . . . O7 O 0.38434(12) 0.25956(11) 0.32154(16) 0.0455(6) Uani 1 1 d . . . O8 O 0.2780(2) 0.2500 0.2500 0.1027(18) Uani 1 2 d S . . C1 C 0.66763(14) 0.36513(13) 0.22140(16) 0.0219(5) Uani 1 1 d . . . C2 C 0.72319(14) 0.36160(13) 0.14272(16) 0.0242(5) Uani 1 1 d . . . C3 C 0.73577(16) 0.28391(14) 0.11478(19) 0.0345(6) Uani 1 1 d . . . H3A H 0.7673 0.2824 0.0606 0.052 Uiso 1 1 calc R . . H3B H 0.6869 0.2614 0.1022 0.052 Uiso 1 1 calc R . . H3C H 0.7612 0.2583 0.1637 0.052 Uiso 1 1 calc R . . C4 C 0.68479(17) 0.40227(15) 0.06564(18) 0.0363(7) Uani 1 1 d . . . H4A H 0.7165 0.3997 0.0116 0.054 Uiso 1 1 calc R . . H4B H 0.6780 0.4522 0.0831 0.054 Uiso 1 1 calc R . . H4C H 0.6353 0.3809 0.0530 0.054 Uiso 1 1 calc R . . C5 C 0.79896(15) 0.39586(15) 0.16548(19) 0.0335(6) Uani 1 1 d . . . H5A H 0.8232 0.3692 0.2143 0.050 Uiso 1 1 calc R . . H5B H 0.7908 0.4452 0.1846 0.050 Uiso 1 1 calc R . . H5C H 0.8316 0.3952 0.1122 0.050 Uiso 1 1 calc R . . C6 C 0.54333(14) 0.30891(13) 0.46795(16) 0.0230(5) Uani 1 1 d . . . C7 C 0.53009(16) 0.27616(15) 0.56085(17) 0.0294(6) Uani 1 1 d . . . C8 C 0.6078(2) 0.2600(2) 0.6013(2) 0.0535(9) Uani 1 1 d . . . H8A H 0.6013 0.2369 0.6600 0.080 Uiso 1 1 calc R . . H8B H 0.6359 0.3046 0.6090 0.080 Uiso 1 1 calc R . . H8C H 0.6358 0.2283 0.5610 0.080 Uiso 1 1 calc R . . C9 C 0.4885(2) 0.32908(18) 0.6210(2) 0.0469(8) Uani 1 1 d . . . H9A H 0.4375 0.3373 0.5972 0.070 Uiso 1 1 calc R . . H9B H 0.5163 0.3742 0.6224 0.070 Uiso 1 1 calc R . . H9C H 0.4849 0.3098 0.6821 0.070 Uiso 1 1 calc R . . C10 C 0.4842(2) 0.20799(18) 0.5522(2) 0.0568(10) Uani 1 1 d . . . H10A H 0.4779 0.1863 0.6117 0.085 Uiso 1 1 calc R . . H10B H 0.5107 0.1747 0.5124 0.085 Uiso 1 1 calc R . . H10C H 0.4344 0.2191 0.5268 0.085 Uiso 1 1 calc R . . C11 C 0.46733(15) 0.43294(14) 0.23790(16) 0.0242(5) Uani 1 1 d . . . C12 C 0.41568(17) 0.47525(15) 0.1749(2) 0.0371(7) Uani 1 1 d . . . C13 C 0.3755(4) 0.5329(3) 0.2246(4) 0.136(3) Uani 1 1 d . . . H13A H 0.3467 0.5620 0.1819 0.205 Uiso 1 1 calc R . . H13B H 0.4126 0.5628 0.2558 0.205 Uiso 1 1 calc R . . H13C H 0.3409 0.5117 0.2686 0.205 Uiso 1 1 calc R . . C14 C 0.3626(4) 0.4291(2) 0.1272(5) 0.162(4) Uani 1 1 d . . . H14A H 0.3311 0.4036 0.1710 0.243 Uiso 1 1 calc R . . H14B H 0.3907 0.3947 0.0907 0.243 Uiso 1 1 calc R . . H14C H 0.3302 0.4581 0.0881 0.243 Uiso 1 1 calc R . . C15 C 0.4670(4) 0.5118(5) 0.1104(6) 0.224(6) Uani 1 1 d . . . H15A H 0.4948 0.4762 0.0753 0.336 Uiso 1 1 calc R . . H15B H 0.5030 0.5416 0.1436 0.336 Uiso 1 1 calc R . . H15C H 0.4372 0.5417 0.0697 0.336 Uiso 1 1 calc R . . C16 C 0.68493(15) 0.55702(13) 0.40137(18) 0.0274(6) Uani 1 1 d . . . H16 H 0.7029 0.5470 0.3425 0.033 Uiso 1 1 calc R . . C17 C 0.71646(16) 0.61319(14) 0.44785(19) 0.0327(6) Uani 1 1 d . . . H17 H 0.7564 0.6402 0.4221 0.039 Uiso 1 1 calc R . . C18 C 0.68929(17) 0.62965(15) 0.5320(2) 0.0386(7) Uani 1 1 d . . . H18 H 0.7098 0.6682 0.5654 0.046 Uiso 1 1 calc R . . C19 C 0.63159(18) 0.58889(16) 0.56668(19) 0.0410(7) Uani 1 1 d . . . H19 H 0.6105 0.6000 0.6238 0.049 Uiso 1 1 calc R . . C20 C 0.60452(16) 0.53186(14) 0.51794(18) 0.0330(6) Uani 1 1 d . . . H20 H 0.5663 0.5028 0.5438 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02527(16) 0.02194(15) 0.01851(14) -0.00231(11) 0.00138(11) -0.00101(11) Dy1 0.02435(10) 0.01640(9) 0.01590(9) -0.00164(6) 0.000 0.000 N1 0.0250(11) 0.0216(11) 0.0227(11) -0.0009(8) 0.0040(9) -0.0011(8) N2 0.031(2) 0.042(2) 0.090(4) -0.024(2) 0.000 0.000 O1 0.0390(12) 0.0323(11) 0.0525(13) -0.0094(9) 0.0187(10) -0.0116(9) O2 0.0269(10) 0.0353(10) 0.0240(9) -0.0087(8) 0.0030(7) -0.0015(8) O3 0.0531(12) 0.0322(10) 0.0199(10) -0.0033(8) -0.0013(9) -0.0083(9) O4 0.0503(12) 0.0267(10) 0.0234(9) 0.0016(8) 0.0010(9) -0.0108(9) O5 0.0459(12) 0.0237(10) 0.0425(12) -0.0025(8) -0.0116(9) 0.0072(9) O6 0.0283(10) 0.0298(10) 0.0304(10) -0.0013(8) -0.0050(8) 0.0013(8) O7 0.0392(12) 0.0406(12) 0.0568(14) -0.0191(10) 0.0148(11) -0.0048(9) O8 0.0226(19) 0.126(4) 0.160(5) -0.036(3) 0.000 0.000 C1 0.0232(13) 0.0203(12) 0.0222(12) 0.0023(10) -0.0014(10) 0.0039(10) C2 0.0266(13) 0.0240(13) 0.0220(12) -0.0023(10) 0.0029(10) 0.0006(10) C3 0.0385(16) 0.0315(15) 0.0337(15) -0.0095(12) 0.0051(12) 0.0040(13) C4 0.0459(17) 0.0394(16) 0.0237(14) 0.0017(12) -0.0001(12) 0.0012(14) C5 0.0273(14) 0.0398(16) 0.0335(15) -0.0053(12) 0.0066(12) -0.0032(12) C6 0.0237(13) 0.0258(13) 0.0195(12) 0.0004(10) 0.0021(10) 0.0025(10) C7 0.0401(16) 0.0283(13) 0.0196(13) 0.0018(11) 0.0031(11) 0.0003(12) C8 0.056(2) 0.079(3) 0.0254(16) 0.0136(16) -0.0003(15) 0.0191(18) C9 0.067(2) 0.0486(19) 0.0248(15) 0.0032(14) 0.0132(14) 0.0143(16) C10 0.088(3) 0.044(2) 0.0378(19) 0.0092(16) 0.0125(18) -0.0234(19) C11 0.0253(13) 0.0240(14) 0.0233(13) 0.0013(10) 0.0037(10) 0.0037(11) C12 0.0438(17) 0.0312(15) 0.0362(16) 0.0053(12) -0.0126(13) 0.0087(13) C13 0.155(6) 0.151(6) 0.103(4) -0.048(4) -0.070(4) 0.124(5) C14 0.216(7) 0.056(3) 0.215(7) -0.026(4) -0.186(6) 0.038(4) C15 0.099(5) 0.348(12) 0.226(8) 0.259(9) -0.005(5) 0.024(6) C16 0.0314(14) 0.0230(13) 0.0279(14) -0.0020(11) 0.0090(11) 0.0016(11) C17 0.0318(15) 0.0241(13) 0.0423(16) -0.0027(12) 0.0136(12) -0.0057(11) C18 0.0419(17) 0.0303(15) 0.0436(17) -0.0138(13) 0.0078(14) -0.0117(13) C19 0.0504(19) 0.0443(17) 0.0282(15) -0.0153(13) 0.0163(13) -0.0155(14) C20 0.0360(16) 0.0339(15) 0.0292(14) -0.0071(12) 0.0107(12) -0.0120(12) _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 Zn1 O4 1.9381(17) . ? Zn1 O6 1.9415(18) . ? Zn1 O2 1.9637(17) . ? Zn1 N1 2.061(2) . ? Dy1 O3 2.2894(18) . ? Dy1 O3 2.2894(18) 4 ? Dy1 O1 2.3271(19) . ? Dy1 O1 2.3271(19) 4 ? Dy1 O5 2.3299(19) . ? Dy1 O5 2.3299(19) 4 ? Dy1 O7 2.466(2) 4 ? Dy1 O7 2.466(2) . ? N1 C20 1.339(3) . ? N1 C16 1.338(3) . ? N2 O8 1.209(5) . ? N2 O7 1.270(3) . ? N2 O7 1.270(3) 4 ? O1 C1 1.238(3) . ? O2 C1 1.267(3) . ? O3 C6 1.237(3) . ? O4 C6 1.268(3) . ? O5 C11 1.239(3) . ? O6 C11 1.268(3) . ? C1 C2 1.528(3) . ? C2 C5 1.524(4) . ? C2 C3 1.533(3) . ? C2 C4 1.535(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.529(3) . ? C7 C10 1.521(4) . ? C7 C9 1.525(4) . ? C7 C8 1.529(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.530(4) . ? C12 C14 1.461(5) . ? C12 C15 1.488(6) . ? C12 C13 1.490(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.378(4) . ? C16 H16 0.9500 . ? C17 C18 1.374(4) . ? C17 H17 0.9500 . ? C18 C19 1.375(4) . ? C18 H18 0.9500 . ? C19 C20 1.378(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 118.74(8) . . ? O4 Zn1 O2 124.93(8) . . ? O6 Zn1 O2 107.40(8) . . ? O4 Zn1 N1 94.91(8) . . ? O6 Zn1 N1 104.58(8) . . ? O2 Zn1 N1 101.23(8) . . ? O3 Dy1 O3 162.63(11) . 4 ? O3 Dy1 O1 84.93(7) . . ? O3 Dy1 O1 81.06(7) 4 . ? O3 Dy1 O1 81.06(7) . 4 ? O3 Dy1 O1 84.93(7) 4 4 ? O1 Dy1 O1 72.24(11) . 4 ? O3 Dy1 O5 88.58(7) . . ? O3 Dy1 O5 96.76(7) 4 . ? O1 Dy1 O5 72.09(8) . . ? O1 Dy1 O5 143.55(8) 4 . ? O3 Dy1 O5 96.76(7) . 4 ? O3 Dy1 O5 88.58(7) 4 4 ? O1 Dy1 O5 143.55(8) . 4 ? O1 Dy1 O5 72.09(8) 4 4 ? O5 Dy1 O5 144.18(11) . 4 ? O3 Dy1 O7 124.59(8) . 4 ? O3 Dy1 O7 72.78(8) 4 4 ? O1 Dy1 O7 134.68(8) . 4 ? O1 Dy1 O7 138.58(7) 4 4 ? O5 Dy1 O7 74.99(7) . 4 ? O5 Dy1 O7 72.89(7) 4 4 ? O3 Dy1 O7 72.78(8) . . ? O3 Dy1 O7 124.59(8) 4 . ? O1 Dy1 O7 138.58(7) . . ? O1 Dy1 O7 134.68(8) 4 . ? O5 Dy1 O7 72.89(7) . . ? O5 Dy1 O7 74.99(7) 4 . ? O7 Dy1 O7 51.84(11) 4 . ? C20 N1 C16 117.6(2) . . ? C20 N1 Zn1 122.84(17) . . ? C16 N1 Zn1 119.51(16) . . ? O8 N2 O7 121.94(18) . . ? O8 N2 O7 121.94(18) . 4 ? O7 N2 O7 116.1(4) . 4 ? C1 O1 Dy1 171.07(18) . . ? C1 O2 Zn1 117.19(16) . . ? C6 O3 Dy1 158.93(18) . . ? C6 O4 Zn1 127.92(16) . . ? C11 O5 Dy1 160.1(2) . . ? C11 O6 Zn1 124.42(17) . . ? N2 O7 Dy1 96.02(19) . . ? O1 C1 O2 122.3(2) . . ? O1 C1 C2 119.3(2) . . ? O2 C1 C2 118.3(2) . . ? C5 C2 C1 112.1(2) . . ? C5 C2 C3 109.5(2) . . ? C1 C2 C3 110.0(2) . . ? C5 C2 C4 110.1(2) . . ? C1 C2 C4 105.4(2) . . ? C3 C2 C4 109.6(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.4(2) . . ? O3 C6 C7 120.0(2) . . ? O4 C6 C7 116.5(2) . . ? C10 C7 C9 109.9(3) . . ? C10 C7 C6 110.1(2) . . ? C9 C7 C6 109.9(2) . . ? C10 C7 C8 110.2(3) . . ? C9 C7 C8 109.3(3) . . ? C6 C7 C8 107.3(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 124.1(2) . . ? O5 C11 C12 119.1(2) . . ? O6 C11 C12 116.8(2) . . ? C14 C12 C15 110.7(6) . . ? C14 C12 C13 111.4(4) . . ? C15 C12 C13 106.0(5) . . ? C14 C12 C11 111.9(3) . . ? C15 C12 C11 105.6(3) . . ? C13 C12 C11 111.0(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 122.9(2) . . ? N1 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 119.1(2) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 118.4(3) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C18 C19 C20 119.5(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C20 C19 122.4(2) . . ? N1 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.717 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.074 # start Validation Reply Form _vrf_PLAT213_7ag241ss ; PROBLEM: Atom C15 has ADP max/min Ratio ..... 5.90 prola RESPONSE: slight disorder in the methyl carbons of the OBc ligand cause large thermo parameters. ; _vrf_PLAT220_7ag241ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE:see above ; _vrf_PLAT222_7ag241ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: see above ; _vrf_PLAT242_7ag241ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END data_8ag112ss _database_code_depnum_ccdc_archive 'CCDC 753923' #TrackingRef 'Boyle_revised_final_cif_DT_C002492A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ErZnNO3OBcpy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Er N3 O15 Zn2' _chemical_formula_weight 1124.94 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 17.6682(11) _cell_length_b 18.6448(11) _cell_length_c 14.8314(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4885.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5300 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 2.740 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 0.578 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33758 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.40 _reflns_number_total 4492 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+5.4564P] 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 4492 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Zn1 Zn 0.59024(3) 0.43053(3) 0.36207(3) 0.03004(14) Uani 1 1 d . . . Er1 Er 0.510883(15) 0.2500 0.2500 0.02467(9) Uani 1 2 d S . . N1 N 0.6304(2) 0.51630(19) 0.4348(2) 0.0353(9) Uani 1 1 d . . . N2 N 0.3483(4) 0.2500 0.2500 0.0630(19) Uani 1 2 d S . . O1 O 0.6165(2) 0.31967(18) 0.2246(2) 0.0512(10) Uani 1 1 d . . . O2 O 0.67307(17) 0.41544(17) 0.2772(2) 0.0367(8) Uani 1 1 d . . . O3 O 0.5300(2) 0.27419(18) 0.3976(2) 0.0443(9) Uani 1 1 d . . . O4 O 0.5704(2) 0.37123(16) 0.4666(2) 0.0447(9) Uani 1 1 d . . . O5 O 0.4707(2) 0.36642(17) 0.2306(2) 0.0461(9) Uani 1 1 d . . . O6 O 0.50482(17) 0.46816(17) 0.2952(2) 0.0384(8) Uani 1 1 d . . . O7 O 0.3869(2) 0.26002(18) 0.3217(3) 0.0539(10) Uani 1 1 d . . . O8 O 0.2797(3) 0.2500 0.2500 0.120(3) Uani 1 2 d S . . C1 C 0.6669(2) 0.3644(2) 0.2207(3) 0.0280(10) Uani 1 1 d . . . C2 C 0.7231(3) 0.3615(2) 0.1429(3) 0.0361(11) Uani 1 1 d . . . C3 C 0.7355(3) 0.2843(3) 0.1138(4) 0.0593(15) Uani 1 1 d . . . H3A H 0.7655 0.2835 0.0582 0.089 Uiso 1 1 calc R . . H3B H 0.6865 0.2614 0.1029 0.089 Uiso 1 1 calc R . . H3C H 0.7626 0.2584 0.1613 0.089 Uiso 1 1 calc R . . C4 C 0.6850(3) 0.4031(3) 0.0651(4) 0.0609(16) Uani 1 1 d . . . H4A H 0.7167 0.3999 0.0110 0.091 Uiso 1 1 calc R . . H4B H 0.6790 0.4535 0.0823 0.091 Uiso 1 1 calc R . . H4C H 0.6352 0.3822 0.0525 0.091 Uiso 1 1 calc R . . C5 C 0.7988(3) 0.3959(3) 0.1660(4) 0.0615(16) Uani 1 1 d . . . H5A H 0.8222 0.3699 0.2162 0.092 Uiso 1 1 calc R . . H5B H 0.7907 0.4461 0.1834 0.092 Uiso 1 1 calc R . . H5C H 0.8322 0.3940 0.1133 0.092 Uiso 1 1 calc R . . C6 C 0.5441(3) 0.3080(2) 0.4671(3) 0.0320(10) Uani 1 1 d . . . C7 C 0.5312(3) 0.2743(3) 0.5599(3) 0.0412(12) Uani 1 1 d . . . C8 C 0.6081(4) 0.2595(4) 0.6008(4) 0.077(2) Uani 1 1 d . . . H8A H 0.6016 0.2366 0.6597 0.115 Uiso 1 1 calc R . . H8B H 0.6355 0.3048 0.6082 0.115 Uiso 1 1 calc R . . H8C H 0.6368 0.2277 0.5609 0.115 Uiso 1 1 calc R . . C9 C 0.4875(4) 0.3267(3) 0.6199(4) 0.0723(19) Uani 1 1 d . . . H9A H 0.4377 0.3360 0.5933 0.108 Uiso 1 1 calc R . . H9B H 0.5157 0.3718 0.6247 0.108 Uiso 1 1 calc R . . H9C H 0.4811 0.3058 0.6800 0.108 Uiso 1 1 calc R . . C10 C 0.4861(4) 0.2053(3) 0.5505(4) 0.075(2) Uani 1 1 d . . . H10A H 0.4763 0.1852 0.6104 0.112 Uiso 1 1 calc R . . H10B H 0.5149 0.1707 0.5145 0.112 Uiso 1 1 calc R . . H10C H 0.4378 0.2155 0.5206 0.112 Uiso 1 1 calc R . . C11 C 0.4670(3) 0.4325(2) 0.2379(3) 0.0330(10) Uani 1 1 d . . . C12 C 0.4138(3) 0.4742(3) 0.1762(4) 0.0503(14) Uani 1 1 d . . . C13 C 0.3761(5) 0.5345(5) 0.2258(6) 0.139(4) Uani 1 1 d . . . H13A H 0.3454 0.5626 0.1835 0.208 Uiso 1 1 calc R . . H13B H 0.4147 0.5655 0.2529 0.208 Uiso 1 1 calc R . . H13C H 0.3435 0.5150 0.2733 0.208 Uiso 1 1 calc R . . C14 C 0.3584(6) 0.4280(4) 0.1329(7) 0.172(6) Uani 1 1 d . . . H14A H 0.3266 0.4054 0.1789 0.258 Uiso 1 1 calc R . . H14B H 0.3846 0.3909 0.0981 0.258 Uiso 1 1 calc R . . H14C H 0.3267 0.4567 0.0923 0.258 Uiso 1 1 calc R . . C15 C 0.4641(6) 0.5047(8) 0.1040(7) 0.221(8) Uani 1 1 d . . . H15A H 0.5003 0.4680 0.0843 0.332 Uiso 1 1 calc R . . H15B H 0.4917 0.5461 0.1280 0.332 Uiso 1 1 calc R . . H15C H 0.4332 0.5198 0.0526 0.332 Uiso 1 1 calc R . . C16 C 0.6852(3) 0.5577(3) 0.4012(3) 0.0484(13) Uani 1 1 d . . . H16 H 0.7030 0.5479 0.3420 0.058 Uiso 1 1 calc R . . C17 C 0.7171(3) 0.6139(3) 0.4483(4) 0.0597(17) Uani 1 1 d . . . H17 H 0.7574 0.6410 0.4229 0.072 Uiso 1 1 calc R . . C18 C 0.6899(3) 0.6297(3) 0.5314(4) 0.0609(17) Uani 1 1 d . . . H18 H 0.7105 0.6683 0.5651 0.073 Uiso 1 1 calc R . . C19 C 0.6331(3) 0.5898(3) 0.5654(4) 0.0589(16) Uani 1 1 d . . . H19 H 0.6118 0.6014 0.6224 0.071 Uiso 1 1 calc R . . C20 C 0.6061(3) 0.5324(3) 0.5176(3) 0.0449(13) Uani 1 1 d . . . H20 H 0.5685 0.5029 0.5445 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0371(3) 0.0284(3) 0.0246(2) -0.0062(2) 0.0039(2) -0.0046(2) Er1 0.03223(16) 0.02072(14) 0.02105(14) -0.00457(12) 0.000 0.000 N1 0.039(2) 0.035(2) 0.031(2) -0.0091(17) 0.0132(17) -0.0090(17) N2 0.041(4) 0.046(4) 0.102(6) -0.022(4) 0.000 0.000 O1 0.049(2) 0.040(2) 0.064(2) -0.0125(17) 0.0236(18) -0.0147(17) O2 0.0354(18) 0.0439(19) 0.0309(17) -0.0135(14) 0.0034(13) -0.0036(15) O3 0.068(2) 0.0410(19) 0.0239(17) -0.0074(14) 0.0008(16) -0.0083(17) O4 0.070(2) 0.0378(19) 0.0260(17) -0.0014(14) 0.0012(16) -0.0196(17) O5 0.059(2) 0.0258(18) 0.054(2) -0.0035(15) -0.0152(17) 0.0068(15) O6 0.0388(19) 0.0355(18) 0.0409(19) -0.0066(16) -0.0029(15) -0.0006(14) O7 0.049(2) 0.047(2) 0.065(2) -0.0242(18) 0.015(2) -0.0050(17) O8 0.032(4) 0.121(6) 0.206(10) -0.040(6) 0.000 0.000 C1 0.030(2) 0.030(2) 0.024(2) 0.0012(18) -0.0017(17) 0.0034(19) C2 0.036(3) 0.039(3) 0.034(3) -0.007(2) 0.007(2) -0.001(2) C3 0.059(4) 0.067(4) 0.052(4) -0.009(3) 0.009(3) 0.009(3) C4 0.072(4) 0.072(4) 0.039(3) 0.004(3) 0.003(3) 0.000(3) C5 0.050(4) 0.075(4) 0.060(4) -0.013(3) 0.010(3) -0.002(3) C6 0.037(3) 0.035(3) 0.025(2) -0.0014(19) 0.000(2) -0.003(2) C7 0.060(3) 0.038(3) 0.025(2) 0.002(2) 0.003(2) -0.008(2) C8 0.078(4) 0.107(6) 0.046(3) 0.024(4) -0.005(3) 0.003(4) C9 0.112(5) 0.068(4) 0.037(3) 0.004(3) 0.029(3) 0.009(4) C10 0.110(6) 0.062(4) 0.053(4) 0.012(3) 0.017(4) -0.026(4) C11 0.036(3) 0.030(2) 0.033(3) -0.001(2) 0.003(2) 0.0038(19) C12 0.060(3) 0.037(3) 0.054(3) 0.005(2) -0.014(3) 0.015(3) C13 0.158(9) 0.129(8) 0.129(8) -0.049(6) -0.072(7) 0.099(7) C14 0.213(11) 0.067(5) 0.237(12) -0.021(6) -0.188(10) 0.030(6) C15 0.139(9) 0.325(17) 0.200(12) 0.222(13) 0.020(8) 0.070(10) C16 0.059(3) 0.041(3) 0.045(3) -0.013(2) 0.023(3) -0.011(3) C17 0.056(4) 0.049(3) 0.074(4) -0.025(3) 0.032(3) -0.024(3) C18 0.057(4) 0.056(4) 0.069(4) -0.036(3) 0.022(3) -0.023(3) C19 0.066(4) 0.064(4) 0.047(3) -0.029(3) 0.020(3) -0.027(3) C20 0.049(3) 0.046(3) 0.040(3) -0.014(2) 0.013(2) -0.019(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 Zn1 O4 1.936(3) . ? Zn1 O6 1.938(3) . ? Zn1 O2 1.951(3) . ? Zn1 N1 2.055(4) . ? Er1 O3 2.260(3) 4 ? Er1 O3 2.260(3) . ? Er1 O5 2.302(3) . ? Er1 O5 2.302(3) 4 ? Er1 O1 2.305(3) . ? Er1 O1 2.305(3) 4 ? Er1 O7 2.443(3) 4 ? Er1 O7 2.443(3) . ? N1 C16 1.335(6) . ? N1 C20 1.335(6) . ? N2 O8 1.213(8) . ? N2 O7 1.277(5) . ? N2 O7 1.277(5) 4 ? O1 C1 1.221(5) . ? O2 C1 1.272(5) . ? O3 C6 1.234(5) . ? O4 C6 1.267(5) . ? O5 C11 1.238(5) . ? O6 C11 1.268(5) . ? C1 C2 1.523(6) . ? C2 C3 1.518(7) . ? C2 C5 1.523(7) . ? C2 C4 1.545(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.530(6) . ? C7 C8 1.512(8) . ? C7 C10 1.520(8) . ? C7 C9 1.531(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(6) . ? C12 C14 1.453(9) . ? C12 C13 1.500(8) . ? C12 C15 1.504(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.381(7) . ? C16 H16 0.9500 . ? C17 C18 1.355(7) . ? C17 H17 0.9500 . ? C18 C19 1.348(7) . ? C18 H18 0.9500 . ? C19 C20 1.368(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O6 118.41(15) . . ? O4 Zn1 O2 124.77(14) . . ? O6 Zn1 O2 107.82(14) . . ? O4 Zn1 N1 94.96(13) . . ? O6 Zn1 N1 104.82(14) . . ? O2 Zn1 N1 101.08(13) . . ? O3 Er1 O3 162.79(19) 4 . ? O3 Er1 O5 96.50(12) 4 . ? O3 Er1 O5 88.80(12) . . ? O3 Er1 O5 88.80(12) 4 4 ? O3 Er1 O5 96.50(12) . 4 ? O5 Er1 O5 144.08(18) . 4 ? O3 Er1 O1 80.38(12) 4 . ? O3 Er1 O1 85.69(12) . . ? O5 Er1 O1 72.41(13) . . ? O5 Er1 O1 143.28(13) 4 . ? O3 Er1 O1 85.69(12) 4 4 ? O3 Er1 O1 80.38(12) . 4 ? O5 Er1 O1 143.28(13) . 4 ? O5 Er1 O1 72.41(13) 4 4 ? O1 Er1 O1 71.86(18) . 4 ? O3 Er1 O7 72.38(13) 4 4 ? O3 Er1 O7 124.83(13) . 4 ? O5 Er1 O7 74.99(12) . 4 ? O5 Er1 O7 72.89(12) 4 4 ? O1 Er1 O7 134.28(14) . 4 ? O1 Er1 O7 138.97(11) 4 4 ? O3 Er1 O7 124.83(13) 4 . ? O3 Er1 O7 72.38(13) . . ? O5 Er1 O7 72.89(12) . . ? O5 Er1 O7 74.99(12) 4 . ? O1 Er1 O7 138.97(11) . . ? O1 Er1 O7 134.28(14) 4 . ? O7 Er1 O7 52.47(18) 4 . ? C16 N1 C20 116.5(4) . . ? C16 N1 Zn1 120.2(3) . . ? C20 N1 Zn1 123.2(3) . . ? O8 N2 O7 122.2(3) . . ? O8 N2 O7 122.2(3) . 4 ? O7 N2 O7 115.5(6) . 4 ? C1 O1 Er1 169.4(3) . . ? C1 O2 Zn1 117.9(3) . . ? C6 O3 Er1 160.3(3) . . ? C6 O4 Zn1 127.0(3) . . ? C11 O5 Er1 160.6(3) . . ? C11 O6 Zn1 124.3(3) . . ? N2 O7 Er1 96.0(3) . . ? O1 C1 O2 122.8(4) . . ? O1 C1 C2 119.1(4) . . ? O2 C1 C2 118.0(4) . . ? C3 C2 C1 110.1(4) . . ? C3 C2 C5 109.6(4) . . ? C1 C2 C5 112.8(4) . . ? C3 C2 C4 109.0(4) . . ? C1 C2 C4 105.4(4) . . ? C5 C2 C4 109.8(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 123.0(4) . . ? O3 C6 C7 120.7(4) . . ? O4 C6 C7 116.2(4) . . ? C8 C7 C10 110.7(5) . . ? C8 C7 C6 107.6(4) . . ? C10 C7 C6 110.1(4) . . ? C8 C7 C9 109.6(5) . . ? C10 C7 C9 109.1(5) . . ? C6 C7 C9 109.6(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 123.6(4) . . ? O5 C11 C12 119.1(4) . . ? O6 C11 C12 117.3(4) . . ? C14 C12 C13 111.2(7) . . ? C14 C12 C15 107.8(8) . . ? C13 C12 C15 109.1(8) . . ? C14 C12 C11 112.3(5) . . ? C13 C12 C11 111.3(5) . . ? C15 C12 C11 104.8(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.1(5) . . ? N1 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 118.7(5) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.8(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N1 C20 C19 122.7(5) . . ? N1 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.488 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.098 # start Validation Reply Form _vrf_PLAT220_8ag112ss ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.89 Ratio RESPONSE: slight disorder in the methyl groups of the OBc ligand cause abnormal thermo parameters ; _vrf_PLAT222_8ag112ss ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.15 Ratio RESPONSE: see above ; _vrf_PLAT242_8ag112ss ; PROBLEM: Check Low Ueq as Compared to Neighbors for C12 RESPONSE: see above ; # end Validation Reply Form #===END