# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Ma, Shengming' _publ_contact_author_email masm@sioc.ac.cn _publ_section_title ; An Unexpected Assembly of Oxazolidine-2,4-diones via the Regioselectivity Control by the Aryl Group in Simple Fixation of CO2 with 3-Aryl-2-alkynamides ; loop_ _publ_author_name 'Chunling Fu' 'Guofei Chen' 'Shengming Ma' data_z _database_code_depnum_ccdc_archive 'CCDC 779363' #TrackingRef 'Z.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H13 N O3' _chemical_formula_weight 279.28 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.4285(4) _cell_length_b 31.4664(18) _cell_length_c 7.0702(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.517(2) _cell_angle_gamma 90.00 _cell_volume 1371.16(14) _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 needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.505 _exptl_crystal_size_mid 0.121 _exptl_crystal_size_min 0.077 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795411 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15862 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2426 _reflns_number_gt 2086 _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^)+(0.0416P)^2^+0.6758P] 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 2426 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.059 _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 N1 N 0.2001(2) 0.10956(4) 0.17480(19) 0.0300(3) Uani 1 1 d . . . O1 O -0.1567(2) 0.13115(4) 0.05164(19) 0.0451(3) Uani 1 1 d . . . O2 O 0.49464(19) 0.06670(4) 0.31777(18) 0.0395(3) Uani 1 1 d . . . O3 O -0.07127(18) 0.06384(4) 0.15223(16) 0.0340(3) Uani 1 1 d . . . C1 C 0.0385(3) -0.07197(5) 0.3451(2) 0.0329(4) Uani 1 1 d . . . H1A H 0.1888 -0.0781 0.3957 0.039 Uiso 1 1 calc R . . C2 C -0.1124(3) -0.10362(6) 0.3351(3) 0.0375(4) Uani 1 1 d . . . H2A H -0.0651 -0.1314 0.3794 0.045 Uiso 1 1 calc R . . C3 C -0.3295(3) -0.09543(6) 0.2620(2) 0.0368(4) Uani 1 1 d . . . H3A H -0.4323 -0.1175 0.2561 0.044 Uiso 1 1 calc R . . C4 C -0.3985(3) -0.05528(6) 0.1973(2) 0.0360(4) Uani 1 1 d . . . H4A H -0.5493 -0.0498 0.1450 0.043 Uiso 1 1 calc R . . C5 C -0.2515(3) -0.02289(5) 0.2073(2) 0.0327(4) Uani 1 1 d . . . H5A H -0.3014 0.0048 0.1640 0.039 Uiso 1 1 calc R . . C6 C -0.0285(3) -0.03074(5) 0.2811(2) 0.0292(4) Uani 1 1 d U . . C7 C 0.1368(3) 0.00169(5) 0.2945(2) 0.0304(4) Uani 1 1 d U . . H7A H 0.2810 -0.0077 0.3541 0.036 Uiso 1 1 calc R . . C8 C 0.1214(3) 0.04235(5) 0.2377(2) 0.0301(4) Uani 1 1 d . . . C9 C 0.3014(3) 0.07201(5) 0.2536(2) 0.0307(4) Uani 1 1 d . . . C10 C -0.0212(3) 0.10496(5) 0.1188(2) 0.0326(4) Uani 1 1 d . . . C11 C 0.3135(3) 0.14893(6) 0.1559(2) 0.0357(4) Uani 1 1 d . . . H11A H 0.2186 0.1667 0.0505 0.043 Uiso 1 1 calc R . . H11B H 0.4457 0.1420 0.1167 0.043 Uiso 1 1 calc R . . C12 C 0.3764(3) 0.17383(5) 0.3459(2) 0.0342(4) Uani 1 1 d . . . C13 C 0.5893(3) 0.17374(6) 0.4630(3) 0.0434(5) Uani 1 1 d . . . H13A H 0.6968 0.1587 0.4217 0.052 Uiso 1 1 calc R . . C14 C 0.6458(4) 0.19568(6) 0.6411(3) 0.0557(6) Uani 1 1 d . . . H14A H 0.7919 0.1955 0.7216 0.067 Uiso 1 1 calc R . . C15 C 0.4907(4) 0.21772(6) 0.7012(3) 0.0587(6) Uani 1 1 d . . . H15A H 0.5297 0.2326 0.8231 0.070 Uiso 1 1 calc R . . C16 C 0.2798(4) 0.21811(6) 0.5848(3) 0.0556(6) Uani 1 1 d . . . H16A H 0.1730 0.2335 0.6260 0.067 Uiso 1 1 calc R . . C17 C 0.2218(3) 0.19625(6) 0.4075(3) 0.0425(5) Uani 1 1 d . . . H17A H 0.0754 0.1966 0.3278 0.051 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 N1 0.0336(8) 0.0295(7) 0.0271(7) -0.0010(6) 0.0087(6) -0.0013(6) O1 0.0393(7) 0.0405(7) 0.0521(8) 0.0073(6) 0.0074(6) 0.0065(6) O2 0.0327(7) 0.0438(7) 0.0395(7) -0.0059(6) 0.0064(5) 0.0019(5) O3 0.0342(7) 0.0341(6) 0.0328(6) 0.0007(5) 0.0080(5) -0.0012(5) C1 0.0324(9) 0.0387(9) 0.0265(8) 0.0006(7) 0.0067(7) 0.0058(7) C2 0.0505(11) 0.0292(9) 0.0334(9) 0.0034(7) 0.0131(8) 0.0008(8) C3 0.0419(10) 0.0414(10) 0.0293(9) -0.0055(8) 0.0137(8) -0.0101(8) C4 0.0306(9) 0.0498(11) 0.0275(9) -0.0047(8) 0.0081(7) -0.0003(8) C5 0.0409(10) 0.0327(9) 0.0250(8) 0.0019(7) 0.0104(7) 0.0085(7) C6 0.0389(9) 0.0319(8) 0.0189(7) -0.0044(6) 0.0119(7) -0.0027(6) C7 0.0303(8) 0.0375(9) 0.0235(8) -0.0040(7) 0.0079(6) 0.0017(6) C8 0.0396(10) 0.0311(9) 0.0206(8) -0.0037(6) 0.0101(7) -0.0004(7) C9 0.0352(10) 0.0365(9) 0.0207(8) -0.0042(7) 0.0082(7) 0.0051(7) C10 0.0369(10) 0.0337(9) 0.0277(8) -0.0009(7) 0.0102(7) -0.0006(8) C11 0.0427(10) 0.0347(9) 0.0316(9) 0.0022(7) 0.0137(8) -0.0049(8) C12 0.0462(11) 0.0241(8) 0.0334(9) 0.0033(7) 0.0134(8) -0.0039(7) C13 0.0522(12) 0.0322(10) 0.0422(11) 0.0002(8) 0.0077(9) 0.0014(8) C14 0.0709(15) 0.0392(11) 0.0442(11) -0.0002(9) -0.0042(10) -0.0050(10) C15 0.0975(19) 0.0358(11) 0.0418(12) -0.0105(9) 0.0184(12) -0.0119(11) C16 0.0837(17) 0.0320(10) 0.0637(14) -0.0104(9) 0.0413(13) -0.0061(10) C17 0.0512(11) 0.0299(9) 0.0503(11) 0.0006(8) 0.0206(9) -0.0043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.371(2) . ? N1 C9 1.387(2) . ? N1 C11 1.463(2) . ? O1 C10 1.195(2) . ? O2 C9 1.207(2) . ? O3 C10 1.370(2) . ? O3 C8 1.390(2) . ? C1 C2 1.378(2) . ? C1 C6 1.401(2) . ? C1 H1A 0.9500 . ? C2 C3 1.368(3) . ? C2 H2A 0.9500 . ? C3 C4 1.374(3) . ? C3 H3A 0.9500 . ? C4 C5 1.378(2) . ? C4 H4A 0.9500 . ? C5 C6 1.400(2) . ? C5 H5A 0.9500 . ? C6 C7 1.457(2) . ? C7 C8 1.336(2) . ? C7 H7A 0.9500 . ? C8 C9 1.466(2) . ? C11 C12 1.508(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.383(3) . ? C12 C17 1.386(3) . ? C13 C14 1.391(3) . ? C13 H13A 0.9500 . ? C14 C15 1.377(3) . ? C14 H14A 0.9500 . ? C15 C16 1.372(3) . ? C15 H15A 0.9500 . ? C16 C17 1.385(3) . ? C16 H16A 0.9500 . ? C17 H17A 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 C10 N1 C9 110.87(14) . . ? C10 N1 C11 124.49(14) . . ? C9 N1 C11 124.64(14) . . ? C10 O3 C8 108.08(13) . . ? C2 C1 C6 120.34(16) . . ? C2 C1 H1A 119.8 . . ? C6 C1 H1A 119.8 . . ? C3 C2 C1 120.73(16) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 119.82(16) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 120.76(16) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C4 C5 C6 120.19(16) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 118.16(15) . . ? C5 C6 C7 123.44(15) . . ? C1 C6 C7 118.40(15) . . ? C8 C7 C6 131.36(16) . . ? C8 C7 H7A 114.3 . . ? C6 C7 H7A 114.3 . . ? C7 C8 O3 125.25(15) . . ? C7 C8 C9 126.68(16) . . ? O3 C8 C9 108.07(13) . . ? O2 C9 N1 125.79(16) . . ? O2 C9 C8 130.26(16) . . ? N1 C9 C8 103.95(14) . . ? O1 C10 O3 122.64(16) . . ? O1 C10 N1 128.38(16) . . ? O3 C10 N1 108.99(14) . . ? N1 C11 C12 111.89(13) . . ? N1 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C17 119.26(17) . . ? C13 C12 C11 120.06(16) . . ? C17 C12 C11 120.66(17) . . ? C12 C13 C14 119.99(19) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 119.90(19) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 120.3(2) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C16 C17 C12 120.3(2) . . ? C16 C17 H17A 119.8 . . ? C12 C17 H17A 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.3(2) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C2 C3 C4 C5 -0.8(2) . . . . ? C3 C4 C5 C6 1.0(2) . . . . ? C4 C5 C6 C1 -0.6(2) . . . . ? C4 C5 C6 C7 179.35(14) . . . . ? C2 C1 C6 C5 0.0(2) . . . . ? C2 C1 C6 C7 -179.98(14) . . . . ? C5 C6 C7 C8 -3.2(3) . . . . ? C1 C6 C7 C8 176.69(16) . . . . ? C6 C7 C8 O3 1.9(3) . . . . ? C6 C7 C8 C9 -178.06(15) . . . . ? C10 O3 C8 C7 178.74(15) . . . . ? C10 O3 C8 C9 -1.33(16) . . . . ? C10 N1 C9 O2 -178.88(15) . . . . ? C11 N1 C9 O2 0.5(2) . . . . ? C10 N1 C9 C8 1.36(16) . . . . ? C11 N1 C9 C8 -179.25(13) . . . . ? C7 C8 C9 O2 0.2(3) . . . . ? O3 C8 C9 O2 -179.75(15) . . . . ? C7 C8 C9 N1 179.93(15) . . . . ? O3 C8 C9 N1 0.00(16) . . . . ? C8 O3 C10 O1 -177.60(15) . . . . ? C8 O3 C10 N1 2.18(16) . . . . ? C9 N1 C10 O1 177.51(17) . . . . ? C11 N1 C10 O1 -1.9(3) . . . . ? C9 N1 C10 O3 -2.26(17) . . . . ? C11 N1 C10 O3 178.35(13) . . . . ? C10 N1 C11 C12 97.09(18) . . . . ? C9 N1 C11 C12 -82.22(19) . . . . ? N1 C11 C12 C13 103.75(18) . . . . ? N1 C11 C12 C17 -74.8(2) . . . . ? C17 C12 C13 C14 0.6(3) . . . . ? C11 C12 C13 C14 -178.07(17) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 0.3(3) . . . . ? C15 C16 C17 C12 -0.1(3) . . . . ? C13 C12 C17 C16 -0.3(3) . . . . ? C11 C12 C17 C16 178.27(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.382 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.034 # Attachment '- Complex 1.CIF' data_w05240 _database_code_depnum_ccdc_archive 'CCDC 780297' #TrackingRef '- Complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 N2 Nd O10 Zn' _chemical_formula_weight 1065.49 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 Monoclinic _symmetry_space_group_name_H-M Cc 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 23.576(3) _cell_length_b 16.388(2) _cell_length_c 24.599(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.441(2) _cell_angle_gamma 90.00 _cell_volume 9501(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4312 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8527 _exptl_absorpt_correction_T_max 0.8527 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27342 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.92 _reflns_number_total 16046 _reflns_number_gt 11460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material 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^)+(0.0703P)^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 0.190(17) _refine_ls_number_reflns 16046 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.013 _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 0.98547(2) 0.64074(3) 0.10263(2) 0.03450(15) Uani 1 1 d . . . Nd2 Nd 1.03271(2) 0.89310(3) 0.05844(2) 0.03471(15) Uani 1 1 d . . . Zn1 Zn 1.09293(7) 1.13005(8) 0.06029(6) 0.0414(4) Uani 1 1 d . . . Zn2 Zn 0.92581(6) 0.40771(8) 0.09021(6) 0.0405(4) Uani 1 1 d . . . N1 N 1.1155(4) 1.2515(5) 0.0494(3) 0.040(2) Uani 1 1 d . . . N2 N 1.1815(5) 1.1357(6) 0.0953(4) 0.040(3) Uani 1 1 d . . . N3 N 0.9030(4) 0.2829(5) 0.1032(4) 0.039(2) Uani 1 1 d . . . N4 N 0.8391(5) 0.4035(6) 0.0582(4) 0.046(3) Uani 1 1 d . . . O1 O 0.9518(4) 0.4160(6) 0.0110(4) 0.059(3) Uani 1 1 d . . . O2 O 0.9424(4) 0.5427(5) 0.0381(3) 0.054(2) Uani 1 1 d . . . O3 O 1.0644(4) 0.6977(6) 0.1543(3) 0.061(3) Uani 1 1 d . . . O4 O 1.0933(4) 0.8114(5) 0.1144(3) 0.059(2) Uani 1 1 d . . . O5 O 1.1272(4) 1.0890(5) -0.0087(3) 0.058(2) Uani 1 1 d . . . O6 O 1.0974(4) 0.9624(5) 0.0026(3) 0.052(2) Uani 1 1 d . . . O7 O 1.0644(4) 1.1219(5) 0.1358(3) 0.052(2) Uani 1 1 d . . . O8 O 1.0696(4) 0.9885(5) 0.1284(3) 0.062(3) Uani 1 1 d . . . O9 O 0.9685(4) 0.8570(5) 0.1237(3) 0.057(2) Uani 1 1 d . . . O10 O 0.9444(4) 0.7406(5) 0.1636(3) 0.062(3) Uani 1 1 d . . . O11 O 1.0717(4) 0.7946(5) -0.0043(3) 0.062(3) Uani 1 1 d . . . O12 O 1.0493(4) 0.6776(5) 0.0349(3) 0.054(2) Uani 1 1 d . . . O13 O 0.9285(4) 0.7241(5) 0.0453(4) 0.065(3) Uani 1 1 d . . . O14 O 0.9518(4) 0.8414(6) 0.0072(3) 0.062(3) Uani 1 1 d . . . O15 O 0.9822(4) 1.0163(5) 0.0386(4) 0.064(3) Uani 1 1 d . . . O16 O 1.0160(4) 1.1418(5) 0.0252(4) 0.055(2) Uani 1 1 d . . . O17 O 0.8937(4) 0.4446(5) 0.1610(3) 0.050(2) Uani 1 1 d . . . O18 O 0.9231(4) 0.5698(5) 0.1587(4) 0.059(3) Uani 1 1 d . . . O19 O 1.0053(4) 0.3950(5) 0.1232(4) 0.052(2) Uani 1 1 d . . . O20 O 1.0394(4) 0.5207(5) 0.1195(4) 0.061(2) Uani 1 1 d . . . C1 C 1.2572(7) 0.7409(8) 0.2381(5) 0.066(4) Uani 1 1 d . . . C2 C 1.2428(6) 0.8106(9) 0.2106(6) 0.069(4) Uani 1 1 d . . . H2A H 1.2679 0.8543 0.2106 0.083 Uiso 1 1 calc R . . C3 C 1.1923(7) 0.8170(7) 0.1833(6) 0.064(4) Uani 1 1 d . . . H3A H 1.1829 0.8653 0.1653 0.077 Uiso 1 1 calc R . . C4 C 1.1534(5) 0.7500(7) 0.1819(4) 0.042(3) Uani 1 1 d . . . C5 C 1.1710(6) 0.6808(8) 0.2107(5) 0.055(3) Uani 1 1 d . . . H5A H 1.1475 0.6353 0.2108 0.066 Uiso 1 1 calc R . . C6 C 1.2210(6) 0.6779(9) 0.2384(5) 0.066(4) Uani 1 1 d . . . H6A H 1.2305 0.6312 0.2581 0.080 Uiso 1 1 calc R . . C7 C 1.3132(7) 0.7328(10) 0.2655(7) 0.100(6) Uani 1 1 d . . . H7A H 1.3163 0.6799 0.2822 0.150 Uiso 1 1 calc R . . H7B H 1.3175 0.7742 0.2929 0.150 Uiso 1 1 calc R . . H7C H 1.3425 0.7388 0.2393 0.150 Uiso 1 1 calc R . . C8 C 1.0993(6) 0.7533(8) 0.1472(5) 0.050(3) Uani 1 1 d . . . C9 C 1.1788(6) 0.9623(9) -0.1846(5) 0.059(4) Uani 1 1 d . . . C10 C 1.1745(6) 1.0418(8) -0.1669(5) 0.058(3) Uani 1 1 d . . . H10A H 1.1833 1.0844 -0.1902 0.069 Uiso 1 1 calc R . . C11 C 1.1574(6) 1.0586(8) -0.1159(5) 0.060(4) Uani 1 1 d . . . H11A H 1.1569 1.1126 -0.1042 0.072 Uiso 1 1 calc R . . C12 C 1.1410(5) 0.9986(7) -0.0810(5) 0.044(3) Uani 1 1 d . . . C13 C 1.1445(5) 0.9180(8) -0.0971(5) 0.053(3) Uani 1 1 d . . . H13A H 1.1344 0.8760 -0.0738 0.063 Uiso 1 1 calc R . . C14 C 1.1636(6) 0.9015(9) -0.1493(6) 0.064(4) Uani 1 1 d . . . H14A H 1.1660 0.8475 -0.1606 0.077 Uiso 1 1 calc R . . C15 C 1.1980(6) 0.9408(9) -0.2420(5) 0.074(4) Uani 1 1 d . . . H15A H 1.2066 0.9900 -0.2613 0.112 Uiso 1 1 calc R . . H15B H 1.1682 0.9119 -0.2611 0.112 Uiso 1 1 calc R . . H15C H 1.2313 0.9070 -0.2396 0.112 Uiso 1 1 calc R . . C16 C 1.1201(5) 1.0167(8) -0.0251(4) 0.041(3) Uani 1 1 d . . . C17 C 1.0403(7) 0.9757(9) 0.2402(5) 0.069(4) Uani 1 1 d . . . H17A H 1.0485 0.9284 0.2211 0.083 Uiso 1 1 calc R . . C18 C 1.0443(5) 1.0485(8) 0.2121(5) 0.050(3) Uani 1 1 d . . . C19 C 1.0601(5) 1.0510(8) 0.1560(5) 0.043(3) Uani 1 1 d . . . C20 C 1.0253(8) 0.9657(12) 0.2946(7) 0.094(6) Uani 1 1 d . . . H20A H 1.0254 0.9151 0.3118 0.112 Uiso 1 1 calc R . . C21 C 1.0298(7) 1.1171(9) 0.2385(5) 0.071(4) Uani 1 1 d . . . H21A H 1.0305 1.1671 0.2206 0.085 Uiso 1 1 calc R . . C22 C 1.0133(7) 1.1127(11) 0.2943(6) 0.090(5) Uani 1 1 d . . . H22A H 1.0048 1.1608 0.3124 0.108 Uiso 1 1 calc R . . C23 C 1.0097(7) 1.0398(13) 0.3218(6) 0.090(6) Uani 1 1 d . . . C24 C 0.9894(7) 1.0549(19) 0.3832(6) 0.206(16) Uani 1 1 d . . . H24A H 0.9823 1.1120 0.3885 0.309 Uiso 1 1 calc R . . H24B H 1.0186 1.0370 0.4084 0.309 Uiso 1 1 calc R . . H24C H 0.9553 1.0246 0.3892 0.309 Uiso 1 1 calc R . . C25 C 0.9171(5) 0.8626(6) 0.2072(5) 0.037(3) Uani 1 1 d . . . C26 C 0.9025(6) 0.9424(8) 0.1966(5) 0.058(4) Uani 1 1 d . . . H26A H 0.9100 0.9665 0.1633 0.069 Uiso 1 1 calc R . . C27 C 0.8759(7) 0.9860(8) 0.2379(6) 0.068(4) Uani 1 1 d . . . H27A H 0.8634 1.0390 0.2312 0.081 Uiso 1 1 calc R . . C28 C 0.8678(6) 0.9509(8) 0.2895(5) 0.060(4) Uani 1 1 d . . . C29 C 0.8867(6) 0.8724(8) 0.2990(5) 0.051(3) Uani 1 1 d . . . H29A H 0.8843 0.8503 0.3337 0.062 Uiso 1 1 calc R . . C30 C 0.9086(5) 0.8270(7) 0.2586(5) 0.046(3) Uani 1 1 d . . . H30A H 0.9181 0.7726 0.2646 0.055 Uiso 1 1 calc R . . C31 C 0.9461(5) 0.8170(7) 0.1609(5) 0.045(3) Uani 1 1 d . . . C32 C 0.8384(7) 1.0037(9) 0.3315(6) 0.090(5) Uani 1 1 d . . . H32A H 0.8294 1.0559 0.3158 0.135 Uiso 1 1 calc R . . H32B H 0.8633 1.0111 0.3626 0.135 Uiso 1 1 calc R . . H32C H 0.8042 0.9774 0.3424 0.135 Uiso 1 1 calc R . . C33 C 0.7583(6) 0.7806(7) -0.0752(5) 0.053(3) Uani 1 1 d . . . C34 C 0.7940(6) 0.8465(8) -0.0755(5) 0.060(3) Uani 1 1 d . . . H34A H 0.7819 0.8936 -0.0934 0.072 Uiso 1 1 calc R . . C35 C 0.8478(6) 0.8464(8) -0.0500(5) 0.055(3) Uani 1 1 d . . . H35A H 0.8717 0.8912 -0.0535 0.066 Uiso 1 1 calc R . . C36 C 0.8655(5) 0.7801(7) -0.0196(5) 0.043(3) Uani 1 1 d . . . C37 C 0.8308(6) 0.7127(8) -0.0176(5) 0.058(4) Uani 1 1 d . . . H37A H 0.8420 0.6667 0.0021 0.069 Uiso 1 1 calc R . . C38 C 0.7789(6) 0.7144(7) -0.0453(5) 0.061(4) Uani 1 1 d . . . H38A H 0.7563 0.6680 -0.0439 0.073 Uiso 1 1 calc R . . C39 C 0.9185(6) 0.7824(7) 0.0131(5) 0.048(3) Uani 1 1 d . . . C40 C 0.7031(7) 0.7811(9) -0.1054(7) 0.094(6) Uani 1 1 d . . . H40A H 0.6980 0.8327 -0.1233 0.141 Uiso 1 1 calc R . . H40B H 0.6730 0.7726 -0.0805 0.141 Uiso 1 1 calc R . . H40C H 0.7026 0.7383 -0.1320 0.141 Uiso 1 1 calc R . . C41 C 1.1270(7) 0.5422(8) -0.0823(5) 0.070(4) Uani 1 1 d . . . H41A H 1.1353 0.4875 -0.0759 0.083 Uiso 1 1 calc R . . C42 C 1.1064(7) 0.5876(9) -0.0404(5) 0.061(4) Uani 1 1 d . . . H42A H 1.1007 0.5627 -0.0071 0.073 Uiso 1 1 calc R . . C43 C 1.0939(5) 0.6702(7) -0.0466(4) 0.043(3) Uani 1 1 d . . . C44 C 1.1038(5) 0.7023(7) -0.0968(5) 0.050(3) Uani 1 1 d . . . H44A H 1.0965 0.7574 -0.1027 0.060 Uiso 1 1 calc R . . C45 C 1.1246(6) 0.6558(8) -0.1396(5) 0.061(4) Uani 1 1 d . . . H45A H 1.1309 0.6803 -0.1730 0.073 Uiso 1 1 calc R . . C46 C 1.1358(6) 0.5732(9) -0.1325(5) 0.055(3) Uani 1 1 d . . . C47 C 1.1554(8) 0.5201(9) -0.1802(6) 0.090(5) Uani 1 1 d . . . H47A H 1.1597 0.5537 -0.2118 0.135 Uiso 1 1 calc R . . H47B H 1.1276 0.4786 -0.1879 0.135 Uiso 1 1 calc R . . H47C H 1.1911 0.4950 -0.1707 0.135 Uiso 1 1 calc R . . C48 C 1.0703(6) 0.7191(8) -0.0029(4) 0.048(3) Uani 1 1 d . . . C49 C 0.9200(5) 1.1118(7) -0.0030(5) 0.038(3) Uani 1 1 d . . . C50 C 0.9132(5) 1.1897(7) -0.0251(5) 0.052(3) Uani 1 1 d . . . H50A H 0.9432 1.2266 -0.0242 0.062 Uiso 1 1 calc R . . C51 C 0.8625(6) 1.2108(8) -0.0480(5) 0.057(3) Uani 1 1 d . . . H51A H 0.8587 1.2631 -0.0622 0.069 Uiso 1 1 calc R . . C52 C 0.8166(7) 1.1604(10) -0.0515(6) 0.070(4) Uani 1 1 d . . . C53 C 0.8258(7) 1.0820(11) -0.0304(6) 0.073(4) Uani 1 1 d . . . H53A H 0.7967 1.0439 -0.0327 0.087 Uiso 1 1 calc R . . C54 C 0.8781(6) 1.0594(8) -0.0058(5) 0.053(3) Uani 1 1 d . . . H54A H 0.8828 1.0072 0.0084 0.064 Uiso 1 1 calc R . . C55 C 0.9765(6) 1.0881(8) 0.0217(4) 0.045(3) Uani 1 1 d . . . C56 C 0.7602(7) 1.1850(12) -0.0753(7) 0.113(7) Uani 1 1 d . . . H56A H 0.7621 1.2404 -0.0877 0.170 Uiso 1 1 calc R . . H56B H 0.7319 1.1803 -0.0481 0.170 Uiso 1 1 calc R . . H56C H 0.7506 1.1499 -0.1054 0.170 Uiso 1 1 calc R . . C57 C 0.8340(6) 0.5493(9) 0.3420(5) 0.061(4) Uani 1 1 d . . . C58 C 0.8349(6) 0.4747(8) 0.3185(5) 0.063(4) Uani 1 1 d . . . H58A H 0.8213 0.4303 0.3379 0.075 Uiso 1 1 calc R . . C59 C 0.8556(5) 0.4613(6) 0.2658(4) 0.042(3) Uani 1 1 d . . . H59A H 0.8550 0.4092 0.2508 0.051 Uiso 1 1 calc R . . C60 C 0.8764(5) 0.5250(7) 0.2374(4) 0.037(3) Uani 1 1 d . . . C61 C 0.8753(6) 0.6025(8) 0.2607(5) 0.062(4) Uani 1 1 d . . . H61A H 0.8884 0.6474 0.2415 0.075 Uiso 1 1 calc R . . C62 C 0.8550(8) 0.6126(9) 0.3119(6) 0.084(6) Uani 1 1 d . . . H62A H 0.8555 0.6646 0.3270 0.100 Uiso 1 1 calc R . . C63 C 0.8139(7) 0.5576(10) 0.3978(5) 0.084(5) Uani 1 1 d . . . H63A H 0.8017 0.5054 0.4107 0.126 Uiso 1 1 calc R . . H63B H 0.7828 0.5953 0.3982 0.126 Uiso 1 1 calc R . . H63C H 0.8442 0.5776 0.4210 0.126 Uiso 1 1 calc R . . C64 C 0.8993(5) 0.5125(7) 0.1813(5) 0.040(3) Uani 1 1 d . . . C65 C 1.1967(7) 0.3541(9) 0.2053(5) 0.058(4) Uani 1 1 d . . . C66 C 1.1480(6) 0.3031(7) 0.1992(5) 0.055(3) Uani 1 1 d . . . H66A H 1.1497 0.2492 0.2110 0.066 Uiso 1 1 calc R . . C67 C 1.0987(5) 0.3328(7) 0.1760(4) 0.040(3) Uani 1 1 d . . . H67A H 1.0673 0.2988 0.1722 0.048 Uiso 1 1 calc R . . C68 C 1.1459(6) 0.4626(8) 0.1644(5) 0.059(4) Uani 1 1 d . . . H68A H 1.1452 0.5162 0.1520 0.071 Uiso 1 1 calc R . . C69 C 1.0952(5) 0.4127(7) 0.1584(5) 0.044(3) Uani 1 1 d . . . C70 C 1.1939(6) 0.4325(9) 0.1875(5) 0.060(4) Uani 1 1 d . . . H70A H 1.2256 0.4660 0.1913 0.072 Uiso 1 1 calc R . . C71 C 1.2501(7) 0.3199(10) 0.2333(6) 0.086(5) Uani 1 1 d . . . H71A H 1.2791 0.3611 0.2344 0.130 Uiso 1 1 calc R . . H71B H 1.2632 0.2735 0.2134 0.130 Uiso 1 1 calc R . . H71C H 1.2416 0.3037 0.2697 0.130 Uiso 1 1 calc R . . C72 C 1.0424(6) 0.4460(7) 0.1316(5) 0.043(3) Uani 1 1 d . . . C73 C 0.9624(5) 0.5186(8) -0.0550(4) 0.052(3) Uani 1 1 d . . . C74 C 0.9511(5) 0.4919(8) 0.0015(5) 0.044(3) Uani 1 1 d . . . C75 C 1.0820(6) 1.3089(8) 0.0273(5) 0.049(3) Uani 1 1 d . . . H75A H 1.0443 1.2967 0.0191 0.059 Uiso 1 1 calc R . . C76 C 1.1028(7) 1.3885(6) 0.0161(6) 0.056(4) Uani 1 1 d . . . H76A H 1.0796 1.4277 -0.0004 0.067 Uiso 1 1 calc R . . C77 C 1.1593(7) 1.4060(8) 0.0306(6) 0.060(4) Uani 1 1 d . . . H77A H 1.1734 1.4583 0.0252 0.072 Uiso 1 1 calc R . . C78 C 1.1947(6) 1.3461(7) 0.0531(5) 0.051(3) Uani 1 1 d . . . C79 C 1.1713(5) 1.2707(7) 0.0624(4) 0.041(3) Uani 1 1 d . . . C80 C 1.2501(6) 1.3624(9) 0.0674(6) 0.061(4) Uani 1 1 d . . . H80A H 1.2652 1.4136 0.0600 0.073 Uiso 1 1 calc R . . C81 C 1.2593(6) 1.2256(8) 0.1024(5) 0.052(3) Uani 1 1 d . . . C82 C 1.2914(7) 1.1639(10) 0.1273(6) 0.069(4) Uani 1 1 d . . . H82A H 1.3293 1.1719 0.1371 0.083 Uiso 1 1 calc R . . C83 C 1.2649(7) 1.0908(10) 0.1368(6) 0.070(4) Uani 1 1 d . . . H83A H 1.2843 1.0496 0.1555 0.085 Uiso 1 1 calc R . . C84 C 1.2100(6) 1.0781(8) 0.1190(5) 0.054(4) Uani 1 1 d . . . H84A H 1.1932 1.0274 0.1240 0.065 Uiso 1 1 calc R . . C85 C 1.2834(7) 1.3052(10) 0.0922(5) 0.073(5) Uani 1 1 d . . . H85A H 1.3208 1.3168 0.1025 0.088 Uiso 1 1 calc R . . C86 C 1.2051(5) 1.2077(7) 0.0875(4) 0.041(3) Uani 1 1 d . . . C87 C 0.8625(8) 0.1309(8) 0.1275(7) 0.068(5) Uani 1 1 d . . . H87A H 0.8494 0.0796 0.1372 0.082 Uiso 1 1 calc R . . C88 C 0.8056(6) 0.4607(8) 0.0361(5) 0.053(4) Uani 1 1 d . . . H88A H 0.8210 0.5122 0.0306 0.064 Uiso 1 1 calc R . . C89 C 0.7249(6) 0.3748(9) 0.0288(5) 0.054(3) Uani 1 1 d . . . H89A H 0.6872 0.3663 0.0183 0.065 Uiso 1 1 calc R . . C90 C 0.7554(5) 0.3129(8) 0.0521(5) 0.046(3) Uani 1 1 d . . . C91 C 0.8116(7) 0.3282(8) 0.0662(5) 0.054(4) Uani 1 1 d . . . C92 C 0.8485(5) 0.2653(6) 0.0906(4) 0.041(3) Uani 1 1 d . . . C93 C 0.7489(6) 0.4482(10) 0.0208(5) 0.064(4) Uani 1 1 d . . . H93A H 0.7278 0.4904 0.0051 0.077 Uiso 1 1 calc R . . C94 C 0.8242(5) 0.1889(8) 0.1015(5) 0.050(3) Uani 1 1 d . . . C95 C 0.9168(6) 0.1510(9) 0.1374(6) 0.056(4) Uani 1 1 d . . . H95A H 0.9419 0.1129 0.1525 0.067 Uiso 1 1 calc R . . C96 C 0.9346(6) 0.2260(7) 0.1255(5) 0.049(3) Uani 1 1 d . . . H96A H 0.9723 0.2387 0.1337 0.059 Uiso 1 1 calc R . . C97 C 0.7647(6) 0.1767(9) 0.0853(6) 0.065(4) Uani 1 1 d . . . H97A H 0.7479 0.1261 0.0909 0.078 Uiso 1 1 calc R . . C98 C 0.7348(6) 0.2353(8) 0.0633(6) 0.061(4) Uani 1 1 d . . . H98A H 0.6969 0.2245 0.0544 0.073 Uiso 1 1 calc R . . C99 C 0.9910(8) 0.6153(16) -0.2185(6) 0.183(13) Uani 1 1 d . . . H99A H 0.9852 0.6732 -0.2167 0.274 Uiso 1 1 calc R . . H99B H 0.9647 0.5919 -0.2445 0.274 Uiso 1 1 calc R . . H99C H 1.0291 0.6043 -0.2293 0.274 Uiso 1 1 calc R . . C100 C 0.9810(7) 0.5752(16) -0.1589(6) 0.115(8) Uani 1 1 d . . . C101 C 0.9646(7) 0.6314(10) -0.1206(5) 0.080(5) Uani 1 1 d . . . H10B H 0.9593 0.6862 -0.1293 0.096 Uiso 1 1 calc R . . C103 C 0.9773(6) 0.4621(9) -0.0957(5) 0.072(4) Uani 1 1 d . . . H10C H 0.9800 0.4072 -0.0864 0.087 Uiso 1 1 calc R . . C102 C 0.9561(6) 0.6012(9) -0.0673(5) 0.070(4) Uani 1 1 d . . . H10D H 0.9460 0.6373 -0.0401 0.084 Uiso 1 1 calc R . . C104 C 0.9876(8) 0.4836(12) -0.1474(6) 0.091(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0363(3) 0.0322(3) 0.0352(3) 0.0026(2) 0.0067(3) 0.0008(3) Nd2 0.0357(3) 0.0328(3) 0.0359(3) 0.0035(2) 0.0071(3) 0.0011(3) Zn1 0.0423(9) 0.0418(8) 0.0403(8) 0.0007(6) 0.0037(7) 0.0026(6) Zn2 0.0396(9) 0.0409(8) 0.0410(8) -0.0017(6) 0.0023(7) 0.0029(6) N1 0.039(6) 0.042(6) 0.039(5) -0.003(4) 0.001(5) 0.012(4) N2 0.039(7) 0.043(6) 0.037(5) 0.007(4) 0.002(5) 0.015(5) N3 0.037(6) 0.036(5) 0.045(5) -0.007(4) 0.004(5) -0.001(4) N4 0.056(8) 0.048(7) 0.033(5) -0.007(4) 0.000(5) 0.005(5) O1 0.068(7) 0.056(6) 0.054(5) -0.003(4) 0.015(5) -0.006(5) O2 0.063(6) 0.056(5) 0.043(5) -0.015(4) -0.001(4) -0.007(4) O3 0.049(6) 0.085(7) 0.048(5) 0.006(5) -0.003(5) -0.017(5) O4 0.069(7) 0.052(6) 0.058(5) 0.004(4) -0.006(5) 0.011(5) O5 0.078(7) 0.045(5) 0.051(5) 0.000(4) 0.023(5) -0.009(4) O6 0.057(6) 0.050(5) 0.050(5) 0.011(4) 0.022(5) 0.000(4) O7 0.057(6) 0.051(5) 0.049(5) 0.004(4) 0.011(4) -0.003(4) O8 0.073(7) 0.064(6) 0.050(5) -0.009(4) -0.002(5) 0.005(5) O9 0.062(6) 0.063(6) 0.049(5) -0.003(4) 0.031(5) -0.012(5) O10 0.087(8) 0.031(5) 0.069(6) -0.005(4) 0.031(6) 0.001(5) O11 0.085(8) 0.041(5) 0.063(6) -0.015(4) 0.024(5) 0.007(5) O12 0.055(6) 0.060(5) 0.047(5) -0.003(4) 0.016(4) -0.004(4) O13 0.068(7) 0.052(6) 0.073(6) 0.014(5) -0.019(5) 0.017(5) O14 0.060(6) 0.065(6) 0.060(6) -0.010(5) -0.015(5) -0.014(5) O15 0.073(7) 0.049(6) 0.072(6) 0.003(5) 0.004(5) 0.014(5) O16 0.031(5) 0.061(6) 0.073(6) 0.004(4) -0.006(5) -0.003(4) O17 0.061(6) 0.049(5) 0.042(5) -0.008(4) 0.009(4) -0.007(4) O18 0.074(7) 0.041(5) 0.063(6) 0.002(4) 0.027(5) -0.014(4) O19 0.038(6) 0.053(6) 0.066(6) 0.014(4) -0.004(5) 0.002(4) O20 0.042(5) 0.046(5) 0.095(7) 0.008(5) -0.009(5) 0.010(4) C1 0.091(12) 0.041(7) 0.062(8) 0.007(6) -0.039(8) -0.008(7) C2 0.056(9) 0.066(9) 0.083(10) -0.012(7) -0.031(8) -0.013(7) C3 0.094(12) 0.016(6) 0.080(9) 0.012(6) -0.017(9) 0.001(6) C4 0.043(7) 0.043(7) 0.040(6) 0.003(5) -0.002(6) 0.006(5) C5 0.056(9) 0.048(8) 0.061(8) 0.009(6) -0.001(7) -0.012(6) C6 0.069(10) 0.063(9) 0.065(9) 0.014(7) -0.032(8) -0.008(7) C7 0.070(11) 0.089(12) 0.138(15) -0.001(10) -0.063(11) -0.002(9) C8 0.044(8) 0.058(9) 0.049(7) -0.001(6) 0.013(6) 0.013(6) C9 0.050(9) 0.089(11) 0.039(7) -0.005(7) 0.023(6) -0.002(7) C10 0.062(9) 0.068(9) 0.045(7) -0.002(6) 0.023(7) -0.009(7) C11 0.081(10) 0.049(7) 0.048(7) -0.002(6) 0.005(7) -0.014(7) C12 0.040(7) 0.046(7) 0.045(7) -0.002(5) -0.001(6) 0.000(5) C13 0.051(8) 0.043(7) 0.065(8) 0.000(6) 0.016(7) -0.008(6) C14 0.057(10) 0.081(10) 0.056(8) -0.026(7) 0.018(7) -0.007(7) C15 0.062(10) 0.118(12) 0.044(8) -0.016(7) 0.021(7) -0.011(8) C16 0.026(7) 0.057(9) 0.041(6) 0.000(6) 0.004(5) -0.001(5) C17 0.084(12) 0.068(9) 0.054(8) -0.001(7) -0.003(8) -0.006(8) C18 0.037(7) 0.068(8) 0.043(7) 0.002(6) -0.002(6) -0.004(6) C19 0.028(7) 0.053(8) 0.048(7) 0.001(6) 0.005(5) 0.004(5) C20 0.079(13) 0.128(15) 0.073(11) 0.017(10) -0.012(10) -0.038(11) C21 0.086(12) 0.080(10) 0.046(7) -0.013(7) 0.017(8) 0.009(8) C22 0.073(12) 0.125(14) 0.072(10) -0.009(10) 0.007(9) 0.017(10) C23 0.060(11) 0.163(18) 0.047(9) 0.034(10) 0.003(8) -0.011(11) C24 0.047(11) 0.53(5) 0.038(9) 0.076(17) 0.008(8) -0.047(19) C25 0.031(7) 0.031(7) 0.051(7) -0.004(5) 0.017(5) -0.001(5) C26 0.069(10) 0.050(8) 0.054(8) 0.000(6) 0.014(7) 0.015(7) C27 0.088(12) 0.043(8) 0.073(9) 0.001(6) 0.021(8) 0.013(7) C28 0.080(11) 0.048(8) 0.053(8) -0.014(6) 0.012(7) 0.008(7) C29 0.064(9) 0.048(8) 0.042(7) -0.005(5) 0.005(7) 0.007(6) C30 0.046(8) 0.041(7) 0.050(7) -0.004(5) 0.004(6) -0.007(5) C31 0.044(7) 0.033(7) 0.059(8) -0.010(5) 0.004(6) 0.002(5) C32 0.122(15) 0.085(11) 0.062(9) -0.026(8) 0.001(10) 0.026(10) C33 0.046(8) 0.048(8) 0.066(8) 0.010(6) 0.001(7) 0.000(6) C34 0.073(10) 0.050(8) 0.056(8) 0.009(6) -0.003(7) -0.002(7) C35 0.067(10) 0.055(8) 0.043(7) 0.016(6) -0.008(7) -0.017(6) C36 0.041(7) 0.040(7) 0.048(7) 0.007(5) -0.004(6) 0.000(5) C37 0.059(9) 0.053(8) 0.060(8) 0.004(6) -0.013(7) 0.008(7) C38 0.079(11) 0.041(7) 0.064(8) -0.002(6) -0.002(8) -0.013(6) C39 0.056(9) 0.042(8) 0.046(7) -0.005(5) -0.002(6) 0.008(6) C40 0.075(12) 0.083(11) 0.122(14) 0.020(10) -0.046(11) -0.020(9) C41 0.101(13) 0.047(8) 0.062(9) -0.006(6) 0.025(9) 0.005(7) C42 0.096(13) 0.054(9) 0.033(7) 0.014(6) 0.016(7) 0.015(8) C43 0.053(8) 0.040(7) 0.036(6) 0.006(5) 0.006(6) -0.005(6) C44 0.063(9) 0.035(7) 0.052(7) -0.001(5) 0.018(6) -0.004(5) C45 0.080(11) 0.053(8) 0.051(8) -0.006(6) 0.018(7) -0.025(7) C46 0.058(9) 0.062(9) 0.045(7) 0.007(6) 0.021(7) -0.004(7) C47 0.129(16) 0.079(10) 0.065(9) -0.018(8) 0.044(10) 0.007(10) C48 0.053(9) 0.059(9) 0.033(6) 0.001(6) 0.022(6) -0.006(6) C49 0.035(7) 0.040(7) 0.039(6) 0.002(5) 0.009(5) 0.005(5) C50 0.041(8) 0.052(8) 0.061(8) 0.002(6) -0.017(6) 0.004(6) C51 0.053(9) 0.065(8) 0.053(8) 0.011(6) -0.013(7) 0.014(7) C52 0.060(10) 0.089(11) 0.062(9) -0.014(8) -0.018(8) 0.015(8) C53 0.059(11) 0.087(11) 0.072(10) -0.017(9) -0.010(9) 0.004(9) C54 0.046(9) 0.062(8) 0.052(8) -0.003(6) 0.003(7) 0.001(6) C55 0.049(8) 0.059(9) 0.028(6) -0.002(5) 0.010(5) 0.019(6) C56 0.065(12) 0.158(17) 0.114(14) -0.013(13) -0.051(11) 0.036(11) C57 0.059(9) 0.081(10) 0.042(7) -0.010(7) 0.015(7) -0.012(7) C58 0.064(10) 0.068(9) 0.056(8) 0.021(7) 0.002(7) -0.010(7) C59 0.056(8) 0.033(6) 0.037(6) -0.001(4) 0.004(6) -0.013(5) C60 0.045(7) 0.043(7) 0.022(5) -0.002(4) 0.008(5) 0.006(5) C61 0.097(12) 0.042(7) 0.048(7) -0.011(6) 0.010(7) -0.026(7) C62 0.142(17) 0.062(9) 0.047(8) -0.015(7) 0.018(10) -0.011(9) C63 0.098(14) 0.104(13) 0.051(8) -0.010(8) 0.013(9) -0.009(10) C64 0.028(7) 0.039(7) 0.054(7) 0.014(5) 0.007(5) 0.004(5) C65 0.047(9) 0.087(11) 0.039(7) -0.011(6) -0.009(6) 0.025(7) C66 0.064(9) 0.048(7) 0.053(7) -0.006(6) 0.000(7) 0.024(6) C67 0.039(7) 0.038(7) 0.041(6) -0.001(5) -0.002(5) 0.002(5) C68 0.059(10) 0.052(8) 0.065(9) -0.004(6) 0.001(8) 0.002(7) C69 0.036(7) 0.053(8) 0.042(6) -0.012(5) -0.005(5) 0.008(5) C70 0.045(9) 0.078(10) 0.055(8) -0.009(7) -0.008(7) 0.003(7) C71 0.075(12) 0.120(13) 0.064(10) -0.011(9) -0.014(9) 0.028(10) C72 0.053(8) 0.034(7) 0.043(7) 0.002(5) 0.006(6) 0.000(6) C73 0.056(8) 0.072(9) 0.028(6) -0.002(6) -0.007(6) -0.017(6) C74 0.043(8) 0.047(7) 0.040(7) 0.007(5) 0.001(6) -0.006(5) C75 0.044(8) 0.057(9) 0.047(7) -0.006(6) 0.006(6) 0.019(6) C76 0.080(12) 0.025(6) 0.063(9) 0.008(5) 0.006(8) 0.004(6) C77 0.056(10) 0.042(8) 0.083(11) -0.017(7) 0.025(9) -0.015(7) C78 0.053(9) 0.042(8) 0.059(8) -0.005(6) 0.020(7) 0.006(6) C79 0.045(8) 0.042(7) 0.036(6) -0.005(5) 0.006(6) 0.007(5) C80 0.057(9) 0.054(8) 0.070(9) 0.003(7) -0.014(8) -0.019(7) C81 0.047(9) 0.064(9) 0.043(7) -0.006(6) 0.000(6) 0.009(7) C82 0.054(10) 0.103(12) 0.052(8) -0.015(8) 0.017(8) 0.007(9) C83 0.051(10) 0.103(13) 0.058(9) 0.020(8) 0.004(8) 0.008(9) C84 0.056(10) 0.058(8) 0.049(8) 0.003(6) 0.029(7) 0.005(7) C85 0.051(10) 0.118(14) 0.052(9) -0.021(8) 0.016(8) -0.020(9) C86 0.031(7) 0.048(8) 0.044(7) -0.002(5) 0.001(5) 0.014(5) C87 0.087(14) 0.042(8) 0.076(11) 0.029(7) 0.016(10) 0.004(7) C88 0.070(10) 0.054(8) 0.035(6) 0.001(5) 0.004(7) 0.028(7) C89 0.035(8) 0.082(10) 0.044(7) -0.001(7) -0.005(6) 0.006(7) C90 0.027(7) 0.065(9) 0.047(7) 0.000(6) 0.007(6) 0.011(6) C91 0.072(11) 0.057(9) 0.033(7) -0.008(6) 0.015(7) 0.013(7) C92 0.042(8) 0.040(7) 0.042(6) -0.008(5) 0.001(6) 0.005(5) C93 0.053(10) 0.098(12) 0.042(7) 0.013(7) -0.004(7) 0.043(8) C94 0.041(8) 0.053(8) 0.055(7) -0.012(6) 0.002(6) -0.008(6) C95 0.025(8) 0.070(10) 0.073(9) 0.014(7) 0.008(7) 0.006(6) C96 0.050(8) 0.033(7) 0.065(8) -0.004(6) -0.002(7) -0.002(6) C97 0.047(9) 0.063(9) 0.086(10) -0.004(8) 0.017(8) -0.008(7) C98 0.030(7) 0.059(9) 0.094(11) -0.010(7) 0.016(8) -0.001(6) C99 0.104(17) 0.40(4) 0.043(9) 0.064(15) -0.005(10) -0.12(2) C100 0.048(10) 0.26(3) 0.032(8) 0.027(12) -0.008(7) -0.071(13) C101 0.101(13) 0.100(11) 0.040(7) 0.017(7) -0.005(8) -0.021(9) C103 0.070(11) 0.089(10) 0.059(9) 0.000(7) 0.020(8) -0.016(8) C102 0.088(11) 0.073(9) 0.048(7) 0.006(6) -0.022(8) -0.025(8) C104 0.087(13) 0.145(17) 0.041(8) 0.000(9) 0.019(8) -0.037(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 Nd1 O18 2.350(8) . ? Nd1 O12 2.353(8) . ? Nd1 O13 2.359(8) . ? Nd1 O20 2.372(8) . ? Nd1 O3 2.415(9) . ? Nd1 O10 2.437(8) . ? Nd1 O2 2.460(8) . ? Nd2 O9 2.311(7) . ? Nd2 O6 2.369(8) . ? Nd2 O4 2.373(9) . ? Nd2 O15 2.388(9) . ? Nd2 O14 2.414(9) . ? Nd2 O11 2.430(8) . ? Nd2 O8 2.466(9) . ? Zn1 O7 1.996(8) . ? Zn1 O16 1.998(9) . ? Zn1 O5 2.013(8) . ? Zn1 N1 2.079(9) . ? Zn1 N2 2.241(11) . ? Zn2 O17 2.009(8) . ? Zn2 O19 2.035(9) . ? Zn2 O1 2.063(9) . ? Zn2 N3 2.141(9) . ? Zn2 N4 2.173(12) . ? N1 C75 1.335(14) . ? N1 C79 1.382(15) . ? N2 C84 1.289(16) . ? N2 C86 1.321(14) . ? N3 C96 1.306(14) . ? N3 C92 1.344(14) . ? N4 C88 1.333(15) . ? N4 C91 1.411(17) . ? O1 C74 1.266(13) . ? O2 C74 1.246(13) . ? O3 C8 1.242(15) . ? O4 C8 1.254(14) . ? O5 C16 1.262(13) . ? O6 C16 1.248(13) . ? O7 C19 1.268(13) . ? O8 C19 1.253(14) . ? O9 C31 1.254(13) . ? O10 C31 1.255(12) . ? O11 C48 1.239(14) . ? O12 C48 1.261(13) . ? O13 C39 1.261(14) . ? O14 C39 1.255(14) . ? O15 C55 1.254(13) . ? O16 C55 1.283(15) . ? O17 C64 1.225(12) . ? O18 C64 1.233(13) . ? O19 C72 1.223(14) . ? O20 C72 1.263(13) . ? C1 C6 1.341(18) . ? C1 C2 1.367(18) . ? C1 C7 1.474(19) . ? C2 C3 1.355(18) . ? C3 C4 1.431(17) . ? C4 C5 1.394(16) . ? C4 C8 1.519(17) . ? C5 C6 1.346(17) . ? C9 C14 1.375(18) . ? C9 C10 1.379(17) . ? C9 C15 1.535(16) . ? C10 C11 1.357(15) . ? C11 C12 1.366(16) . ? C12 C13 1.382(16) . ? C12 C16 1.503(15) . ? C13 C14 1.399(17) . ? C17 C18 1.384(17) . ? C17 C20 1.40(2) . ? C18 C21 1.346(16) . ? C18 C19 1.440(16) . ? C20 C23 1.44(2) . ? C21 C22 1.438(19) . ? C22 C23 1.38(2) . ? C23 C24 1.62(2) . ? C25 C26 1.376(16) . ? C25 C30 1.410(15) . ? C25 C31 1.536(15) . ? C26 C27 1.403(17) . ? C27 C28 1.410(18) . ? C28 C29 1.379(16) . ? C28 C32 1.527(17) . ? C29 C30 1.356(16) . ? C33 C34 1.370(17) . ? C33 C38 1.391(17) . ? C33 C40 1.482(19) . ? C34 C35 1.403(18) . ? C35 C36 1.377(16) . ? C36 C37 1.376(17) . ? C36 C39 1.469(17) . ? C37 C38 1.387(18) . ? C41 C46 1.358(17) . ? C41 C42 1.369(17) . ? C42 C43 1.393(17) . ? C43 C44 1.368(14) . ? C43 C48 1.463(15) . ? C44 C45 1.398(16) . ? C45 C46 1.390(17) . ? C46 C47 1.541(17) . ? C49 C54 1.309(17) . ? C49 C50 1.396(15) . ? C49 C55 1.501(17) . ? C50 C51 1.354(16) . ? C51 C52 1.362(19) . ? C52 C53 1.40(2) . ? C52 C56 1.494(19) . ? C53 C54 1.41(2) . ? C57 C58 1.353(17) . ? C57 C62 1.373(19) . ? C57 C63 1.470(17) . ? C58 C59 1.414(16) . ? C59 C60 1.355(14) . ? C60 C61 1.395(15) . ? C60 C64 1.508(14) . ? C61 C62 1.368(18) . ? C65 C70 1.359(19) . ? C65 C66 1.43(2) . ? C65 C71 1.526(19) . ? C66 C67 1.372(16) . ? C67 C69 1.383(15) . ? C68 C70 1.347(18) . ? C68 C69 1.452(18) . ? C69 C72 1.496(17) . ? C73 C102 1.394(17) . ? C73 C103 1.415(17) . ? C73 C74 1.488(15) . ? C75 C76 1.423(17) . ? C76 C77 1.40(2) . ? C77 C78 1.40(2) . ? C78 C80 1.370(18) . ? C78 C79 1.374(16) . ? C79 C86 1.434(16) . ? C80 C85 1.36(2) . ? C81 C86 1.353(18) . ? C81 C82 1.394(19) . ? C81 C85 1.447(19) . ? C82 C83 1.37(2) . ? C83 C84 1.37(2) . ? C87 C95 1.34(2) . ? C87 C94 1.449(19) . ? C88 C93 1.394(19) . ? C89 C93 1.346(19) . ? C89 C90 1.361(17) . ? C90 C91 1.385(18) . ? C90 C98 1.391(17) . ? C91 C92 1.467(17) . ? C92 C94 1.406(16) . ? C94 C97 1.462(18) . ? C95 C96 1.334(16) . ? C97 C98 1.302(19) . ? C99 C100 1.63(2) . ? C100 C101 1.38(3) . ? C100 C104 1.53(3) . ? C101 C102 1.420(17) . ? C103 C104 1.347(19) . ? 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 O18 Nd1 O12 164.6(3) . . ? O18 Nd1 O13 106.4(3) . . ? O12 Nd1 O13 78.0(3) . . ? O18 Nd1 O20 80.1(3) . . ? O12 Nd1 O20 89.3(3) . . ? O13 Nd1 O20 151.5(3) . . ? O18 Nd1 O3 111.6(3) . . ? O12 Nd1 O3 77.0(3) . . ? O13 Nd1 O3 120.7(3) . . ? O20 Nd1 O3 80.0(3) . . ? O18 Nd1 O10 72.9(3) . . ? O12 Nd1 O10 122.3(3) . . ? O13 Nd1 O10 75.5(3) . . ? O20 Nd1 O10 131.9(3) . . ? O3 Nd1 O10 74.3(3) . . ? O18 Nd1 O2 78.6(3) . . ? O12 Nd1 O2 88.4(3) . . ? O13 Nd1 O2 76.9(3) . . ? O20 Nd1 O2 77.4(3) . . ? O3 Nd1 O2 153.1(3) . . ? O10 Nd1 O2 132.2(3) . . ? O9 Nd2 O6 165.5(3) . . ? O9 Nd2 O4 81.3(3) . . ? O6 Nd2 O4 102.7(3) . . ? O9 Nd2 O15 91.5(3) . . ? O6 Nd2 O15 78.5(3) . . ? O4 Nd2 O15 152.3(3) . . ? O9 Nd2 O14 75.5(3) . . ? O6 Nd2 O14 112.2(3) . . ? O4 Nd2 O14 124.2(3) . . ? O15 Nd2 O14 78.9(3) . . ? O9 Nd2 O11 122.4(3) . . ? O6 Nd2 O11 72.0(3) . . ? O4 Nd2 O11 76.2(3) . . ? O15 Nd2 O11 128.8(3) . . ? O14 Nd2 O11 75.1(3) . . ? O9 Nd2 O8 84.4(3) . . ? O6 Nd2 O8 83.1(3) . . ? O4 Nd2 O8 75.9(3) . . ? O15 Nd2 O8 76.8(3) . . ? O14 Nd2 O8 147.9(3) . . ? O11 Nd2 O8 137.0(3) . . ? O7 Zn1 O16 94.9(4) . . ? O7 Zn1 O5 156.0(3) . . ? O16 Zn1 O5 92.7(4) . . ? O7 Zn1 N1 106.1(3) . . ? O16 Zn1 N1 94.8(4) . . ? O5 Zn1 N1 95.9(3) . . ? O7 Zn1 N2 88.7(4) . . ? O16 Zn1 N2 171.5(3) . . ? O5 Zn1 N2 87.0(4) . . ? N1 Zn1 N2 76.8(4) . . ? O17 Zn2 O19 92.8(4) . . ? O17 Zn2 O1 157.9(4) . . ? O19 Zn2 O1 95.2(4) . . ? O17 Zn2 N3 93.2(3) . . ? O19 Zn2 N3 94.3(3) . . ? O1 Zn2 N3 106.6(4) . . ? O17 Zn2 N4 87.2(4) . . ? O19 Zn2 N4 172.0(3) . . ? O1 Zn2 N4 87.7(4) . . ? N3 Zn2 N4 77.7(4) . . ? C75 N1 C79 118.8(10) . . ? C75 N1 Zn1 125.2(9) . . ? C79 N1 Zn1 115.7(7) . . ? C84 N2 C86 120.2(13) . . ? C84 N2 Zn1 127.8(10) . . ? C86 N2 Zn1 111.9(7) . . ? C96 N3 C92 118.4(10) . . ? C96 N3 Zn2 127.0(9) . . ? C92 N3 Zn2 114.3(7) . . ? C88 N4 C91 113.7(13) . . ? C88 N4 Zn2 131.9(10) . . ? C91 N4 Zn2 114.1(9) . . ? C74 O1 Zn2 103.6(7) . . ? C74 O2 Nd1 146.0(8) . . ? C8 O3 Nd1 135.5(9) . . ? C8 O4 Nd2 149.1(9) . . ? C16 O5 Zn1 122.0(7) . . ? C16 O6 Nd2 161.6(8) . . ? C19 O7 Zn1 117.3(8) . . ? C19 O8 Nd2 146.3(8) . . ? C31 O9 Nd2 159.5(8) . . ? C31 O10 Nd1 128.6(7) . . ? C48 O11 Nd2 129.4(7) . . ? C48 O12 Nd1 158.4(9) . . ? C39 O13 Nd1 155.4(10) . . ? C39 O14 Nd2 134.3(8) . . ? C55 O15 Nd2 155.5(9) . . ? C55 O16 Zn1 127.8(8) . . ? C64 O17 Zn2 126.0(7) . . ? C64 O18 Nd1 160.0(8) . . ? C72 O19 Zn2 130.2(8) . . ? C72 O20 Nd1 150.8(8) . . ? C6 C1 C2 119.7(14) . . ? C6 C1 C7 119.5(13) . . ? C2 C1 C7 120.8(13) . . ? C3 C2 C1 121.0(13) . . ? C2 C3 C4 120.4(11) . . ? C5 C4 C3 115.5(12) . . ? C5 C4 C8 123.3(11) . . ? C3 C4 C8 121.0(11) . . ? C6 C5 C4 122.0(12) . . ? C1 C6 C5 121.3(13) . . ? O3 C8 O4 125.7(14) . . ? O3 C8 C4 116.4(11) . . ? O4 C8 C4 117.9(12) . . ? C14 C9 C10 117.6(11) . . ? C14 C9 C15 120.2(13) . . ? C10 C9 C15 122.2(12) . . ? C11 C10 C9 120.6(12) . . ? C10 C11 C12 122.0(12) . . ? C11 C12 C13 119.2(11) . . ? C11 C12 C16 122.5(11) . . ? C13 C12 C16 118.2(11) . . ? C12 C13 C14 118.0(12) . . ? C9 C14 C13 122.4(13) . . ? O6 C16 O5 123.4(10) . . ? O6 C16 C12 120.9(11) . . ? O5 C16 C12 115.7(10) . . ? C18 C17 C20 126.8(15) . . ? C21 C18 C17 117.3(12) . . ? C21 C18 C19 120.8(12) . . ? C17 C18 C19 121.8(12) . . ? O8 C19 O7 121.3(11) . . ? O8 C19 C18 123.4(12) . . ? O7 C19 C18 115.3(11) . . ? C17 C20 C23 114.7(15) . . ? C18 C21 C22 119.8(14) . . ? C23 C22 C21 122.2(16) . . ? C22 C23 C20 119.0(14) . . ? C22 C23 C24 110(2) . . ? C20 C23 C24 130.4(18) . . ? C26 C25 C30 121.5(11) . . ? C26 C25 C31 115.8(10) . . ? C30 C25 C31 122.6(10) . . ? C25 C26 C27 117.4(12) . . ? C26 C27 C28 121.1(12) . . ? C29 C28 C27 118.9(11) . . ? C29 C28 C32 124.3(12) . . ? C27 C28 C32 116.8(12) . . ? C30 C29 C28 120.9(12) . . ? C29 C30 C25 119.7(11) . . ? O9 C31 O10 125.1(11) . . ? O9 C31 C25 119.4(10) . . ? O10 C31 C25 115.5(10) . . ? C34 C33 C38 114.3(13) . . ? C34 C33 C40 121.6(12) . . ? C38 C33 C40 124.1(12) . . ? C33 C34 C35 123.1(12) . . ? C36 C35 C34 120.1(12) . . ? C37 C36 C35 118.8(12) . . ? C37 C36 C39 119.9(11) . . ? C35 C36 C39 121.2(11) . . ? C36 C37 C38 118.9(12) . . ? C37 C38 C33 124.6(12) . . ? O14 C39 O13 123.3(13) . . ? O14 C39 C36 118.8(11) . . ? O13 C39 C36 117.8(12) . . ? C46 C41 C42 123.1(13) . . ? C41 C42 C43 121.7(11) . . ? C44 C43 C42 115.5(10) . . ? C44 C43 C48 122.0(11) . . ? C42 C43 C48 122.4(10) . . ? C43 C44 C45 122.8(11) . . ? C46 C45 C44 120.4(11) . . ? C41 C46 C45 116.5(12) . . ? C41 C46 C47 122.6(13) . . ? C45 C46 C47 120.9(11) . . ? O11 C48 O12 124.8(11) . . ? O11 C48 C43 121.0(10) . . ? O12 C48 C43 114.2(11) . . ? C54 C49 C50 120.0(12) . . ? C54 C49 C55 120.9(12) . . ? C50 C49 C55 119.0(11) . . ? C51 C50 C49 119.1(12) . . ? C50 C51 C52 124.3(13) . . ? C51 C52 C53 114.7(14) . . ? C51 C52 C56 123.9(16) . . ? C53 C52 C56 121.4(16) . . ? C52 C53 C54 121.8(15) . . ? C49 C54 C53 120.1(14) . . ? O15 C55 O16 123.3(12) . . ? O15 C55 C49 117.6(12) . . ? O16 C55 C49 119.1(11) . . ? C58 C57 C62 116.3(12) . . ? C58 C57 C63 119.4(13) . . ? C62 C57 C63 124.2(13) . . ? C57 C58 C59 122.7(11) . . ? C60 C59 C58 119.5(10) . . ? C59 C60 C61 118.5(10) . . ? C59 C60 C64 120.7(10) . . ? C61 C60 C64 120.8(10) . . ? C62 C61 C60 119.9(12) . . ? C61 C62 C57 123.0(13) . . ? O17 C64 O18 123.6(11) . . ? O17 C64 C60 117.3(10) . . ? O18 C64 C60 119.0(11) . . ? C70 C65 C66 119.2(12) . . ? C70 C65 C71 121.8(14) . . ? C66 C65 C71 119.0(13) . . ? C67 C66 C65 120.5(12) . . ? C66 C67 C69 120.7(12) . . ? C70 C68 C69 121.2(13) . . ? C67 C69 C68 117.3(11) . . ? C67 C69 C72 121.7(11) . . ? C68 C69 C72 120.9(11) . . ? C68 C70 C65 121.1(14) . . ? O19 C72 O20 125.9(12) . . ? O19 C72 C69 114.2(11) . . ? O20 C72 C69 119.9(11) . . ? C102 C73 C103 120.5(11) . . ? C102 C73 C74 117.9(11) . . ? C103 C73 C74 121.5(12) . . ? O2 C74 O1 121.7(11) . . ? O2 C74 C73 121.0(11) . . ? O1 C74 C73 117.3(11) . . ? N1 C75 C76 121.5(13) . . ? C77 C76 C75 117.9(13) . . ? C78 C77 C76 121.0(12) . . ? C80 C78 C79 121.2(13) . . ? C80 C78 C77 121.5(13) . . ? C79 C78 C77 117.3(13) . . ? C78 C79 N1 123.4(11) . . ? C78 C79 C86 119.8(12) . . ? N1 C79 C86 116.8(10) . . ? C85 C80 C78 121.1(14) . . ? C86 C81 C82 117.3(13) . . ? C86 C81 C85 121.4(13) . . ? C82 C81 C85 121.3(15) . . ? C83 C82 C81 117.6(16) . . ? C84 C83 C82 120.5(15) . . ? N2 C84 C83 120.7(14) . . ? C80 C85 C81 118.4(15) . . ? N2 C86 C81 123.5(11) . . ? N2 C86 C79 118.3(12) . . ? C81 C86 C79 118.2(12) . . ? C95 C87 C94 120.2(13) . . ? N4 C88 C93 124.2(14) . . ? C93 C89 C90 120.6(14) . . ? C89 C90 C91 117.5(12) . . ? C89 C90 C98 125.6(14) . . ? C91 C90 C98 116.9(12) . . ? C90 C91 N4 124.3(12) . . ? C90 C91 C92 122.0(12) . . ? N4 C91 C92 113.7(13) . . ? N3 C92 C94 122.6(11) . . ? N3 C92 C91 119.8(11) . . ? C94 C92 C91 117.5(12) . . ? C89 C93 C88 119.7(12) . . ? C92 C94 C87 114.5(13) . . ? C92 C94 C97 117.6(12) . . ? C87 C94 C97 127.9(13) . . ? C96 C95 C87 119.4(13) . . ? N3 C96 C95 124.8(13) . . ? C98 C97 C94 121.2(14) . . ? C97 C98 C90 124.6(14) . . ? C101 C100 C104 123.7(13) . . ? C101 C100 C99 113(2) . . ? C104 C100 C99 122.9(19) . . ? C100 C101 C102 116.5(15) . . ? C104 C103 C73 123.4(15) . . ? C73 C102 C101 121.5(13) . . ? C103 C104 C100 114.2(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.454 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.118 data_w05174 _database_code_depnum_ccdc_archive 'CCDC 780298' #TrackingRef '- Complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N2 O11 Tb Zn' _chemical_formula_weight 1110.20 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.028(3) _cell_length_b 13.163(3) _cell_length_c 15.397(3) _cell_angle_alpha 75.58(3) _cell_angle_beta 82.38(3) _cell_angle_gamma 83.32(3) _cell_volume 2525.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8309 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9192 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9192 _reflns_number_gt 7112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material 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^)+(0.0588P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9192 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.127 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.482638(19) 0.030308(18) 0.371372(14) 0.03073(8) Uani 1 1 d . . . Zn1 Zn 0.47339(5) 0.16222(4) 0.11523(4) 0.03854(15) Uani 1 1 d . . . N1 N 0.5552(3) 0.3065(3) 0.0703(3) 0.0442(10) Uani 1 1 d . . . N2 N 0.4628(3) 0.2075(3) -0.0276(3) 0.0409(10) Uani 1 1 d . . . O1 O 0.3712(3) 0.1750(3) 0.3154(2) 0.0566(10) Uani 1 1 d . . . O2 O 0.3510(3) 0.2439(3) 0.1703(2) 0.0483(9) Uani 1 1 d . . . O3 O 0.4018(3) -0.0304(3) 0.2712(2) 0.0494(9) Uani 1 1 d . . . O4 O 0.3969(3) 0.0365(3) 0.1258(2) 0.0503(9) Uani 1 1 d . . . O5 O 0.5768(3) 0.1131(3) 0.2299(2) 0.0412(8) Uani 1 1 d . . . O6 O 0.6297(3) 0.0761(3) 0.1002(2) 0.0558(10) Uani 1 1 d . . . O7 O 0.6117(3) -0.0488(3) 0.4909(2) 0.0396(8) Uani 1 1 d . . . O8 O 0.6415(3) -0.0811(3) 0.3574(2) 0.0432(8) Uani 1 1 d . . . O9 O 0.4324(3) -0.1402(3) 0.4480(2) 0.0466(9) Uani 1 1 d . . . O10 O 0.5612(3) 0.1655(3) 0.4039(2) 0.0491(9) Uani 1 1 d . . . O11 O -0.0846(10) 0.6615(12) 0.0199(8) 0.114(5) Uani 0.50 1 d P . . O12 O -0.1561(11) 0.5518(11) 0.1349(12) 0.138(5) Uani 0.50 1 d P . . H12B H -0.1859 0.6061 0.1463 0.207 Uiso 0.50 1 calc PR . . C1 C 0.3236(4) 0.2346(4) 0.2542(3) 0.0392(12) Uani 1 1 d . . . C2 C 0.2307(4) 0.2997(4) 0.2822(3) 0.0411(12) Uani 1 1 d . . . C3 C 0.1466(5) 0.3270(5) 0.2317(4) 0.0564(15) Uani 1 1 d . . . H3A H 0.156(3) 0.307(4) 0.173(3) 0.033(13) Uiso 1 1 d . . . C4 C 0.0574(6) 0.3818(6) 0.2647(6) 0.073(2) Uani 1 1 d . . . H4A H 0.004(5) 0.391(4) 0.226(4) 0.056(17) Uiso 1 1 d . . . C5 C 0.0535(6) 0.4158(6) 0.3420(5) 0.077(2) Uani 1 1 d . . . C6 C 0.1378(6) 0.3913(6) 0.3890(5) 0.078(2) Uani 1 1 d . . . H6A H 0.1367 0.4149 0.4413 0.094 Uiso 1 1 calc R . . C7 C 0.2250(5) 0.3325(5) 0.3614(4) 0.0651(17) Uani 1 1 d . . . H7A H 0.2803 0.3147 0.3964 0.078 Uiso 1 1 calc R . . C8 C -0.0431(7) 0.4790(8) 0.3744(6) 0.120(3) Uani 1 1 d . . . H8A H -0.0938 0.4896 0.3323 0.180 Uiso 1 1 calc R . . H8B H -0.0248 0.5461 0.3786 0.180 Uiso 1 1 calc R . . H8C H -0.0716 0.4413 0.4326 0.180 Uiso 1 1 calc R . . C9 C 0.3743(4) -0.0301(4) 0.1974(3) 0.0376(11) Uani 1 1 d . . . C10 C 0.3102(4) -0.1135(4) 0.1907(3) 0.0358(11) Uani 1 1 d . . . C11 C 0.2781(4) -0.1896(4) 0.2679(4) 0.0482(13) Uani 1 1 d . . . H11A H 0.2966 -0.1878 0.3237 0.058 Uiso 1 1 calc R . . C12 C 0.2193(5) -0.2668(5) 0.2611(4) 0.0573(16) Uani 1 1 d . . . H12A H 0.190(4) -0.318(4) 0.311(4) 0.056(16) Uiso 1 1 d . . . C13 C 0.1893(5) -0.2720(5) 0.1802(4) 0.0631(17) Uani 1 1 d . . . C14 C 0.2229(5) -0.1983(5) 0.1042(4) 0.0575(15) Uani 1 1 d . . . H14A H 0.2054 -0.2013 0.0483 0.069 Uiso 1 1 calc R . . C15 C 0.2822(4) -0.1200(4) 0.1095(3) 0.0452(13) Uani 1 1 d . . . H15A H 0.3035 -0.0710 0.0573 0.054 Uiso 1 1 calc R . . C16 C 0.1268(6) -0.3583(6) 0.1741(6) 0.097(3) Uani 1 1 d . . . H16A H 0.1108 -0.4021 0.2333 0.146 Uiso 1 1 calc R . . H16B H 0.1662 -0.4000 0.1361 0.146 Uiso 1 1 calc R . . H16C H 0.0634 -0.3281 0.1490 0.146 Uiso 1 1 calc R . . C17 C 0.6499(4) 0.0860(4) 0.1741(3) 0.0379(11) Uani 1 1 d . . . C18 C 0.7599(4) 0.0727(4) 0.1939(3) 0.0418(12) Uani 1 1 d . . . C19 C 0.7904(4) 0.1151(4) 0.2589(3) 0.0457(13) Uani 1 1 d . . . H19A H 0.7410 0.1494 0.2936 0.055 Uiso 1 1 calc R . . C20 C 0.8928(5) 0.1069(6) 0.2727(4) 0.0590(16) Uani 1 1 d . . . H20A H 0.905(4) 0.143(5) 0.314(4) 0.060(18) Uiso 1 1 d . . . C21 C 0.9680(5) 0.0544(5) 0.2253(5) 0.0638(17) Uani 1 1 d . . . C22 C 0.9369(5) 0.0109(6) 0.1614(5) 0.075(2) Uani 1 1 d . . . H22A H 0.9863 -0.0255 0.1283 0.091 Uiso 1 1 calc R . . C23 C 0.8351(5) 0.0202(5) 0.1458(4) 0.0629(17) Uani 1 1 d . . . H23A H 0.8163 -0.0094 0.1019 0.075 Uiso 1 1 calc R . . C24 C 1.0805(5) 0.0415(7) 0.2435(6) 0.096(3) Uani 1 1 d . . . H24A H 1.0878 0.0763 0.2900 0.144 Uiso 1 1 calc R . . H24B H 1.1227 0.0722 0.1894 0.144 Uiso 1 1 calc R . . H24C H 1.1025 -0.0320 0.2627 0.144 Uiso 1 1 calc R . . C25 C 0.6731(4) -0.0818(4) 0.4307(3) 0.0357(11) Uani 1 1 d . . . C26 C 0.7831(4) -0.1129(4) 0.4461(3) 0.0392(12) Uani 1 1 d . . . C27 C 0.8493(4) -0.1615(4) 0.3858(4) 0.0500(14) Uani 1 1 d . . . H27A H 0.813(4) -0.187(4) 0.338(4) 0.064(17) Uiso 1 1 d . . . C28 C 0.9523(5) -0.1889(5) 0.3994(4) 0.0604(16) Uani 1 1 d . . . H28A H 1.005(5) -0.234(5) 0.366(4) 0.072(19) Uiso 1 1 d . . . C29 C 0.9943(5) -0.1690(6) 0.4705(4) 0.0650(17) Uani 1 1 d . . . C30 C 0.9290(5) -0.1174(7) 0.5281(4) 0.079(2) Uani 1 1 d . . . H30A H 0.9554 -0.1001 0.5753 0.095 Uiso 1 1 calc R . . C31 C 0.8248(5) -0.0914(5) 0.5155(4) 0.0609(16) Uani 1 1 d . . . H31A H 0.7821 -0.0585 0.5557 0.073 Uiso 1 1 calc R . . C32 C 1.1067(5) -0.1993(7) 0.4840(5) 0.094(3) Uani 1 1 d . . . H32A H 1.1390 -0.2346 0.4384 0.140 Uiso 1 1 calc R . . H32B H 1.1119 -0.2456 0.5425 0.140 Uiso 1 1 calc R . . H32C H 1.1409 -0.1372 0.4796 0.140 Uiso 1 1 calc R . . C33 C 0.5758(4) 0.1951(4) 0.4724(3) 0.0401(12) Uani 1 1 d . . . C34 C 0.6066(4) 0.3051(4) 0.4572(3) 0.0379(11) Uani 1 1 d . . . C35 C 0.6334(5) 0.3637(4) 0.3712(4) 0.0605(17) Uani 1 1 d . . . H35A H 0.6330 0.3342 0.3222 0.073 Uiso 1 1 calc R . . C36 C 0.6610(6) 0.4658(5) 0.3564(4) 0.0623(17) Uani 1 1 d . . . H36A H 0.633(8) 0.548(9) 0.283(7) 0.19(4) Uiso 1 1 d . . . C37 C 0.6647(4) 0.5117(4) 0.4274(4) 0.0483(13) Uani 1 1 d . . . C38 C 0.6366(5) 0.4524(4) 0.5132(4) 0.0548(15) Uani 1 1 d . . . H38A H 0.6363 0.4817 0.5623 0.066 Uiso 1 1 calc R . . C39 C 0.6090(5) 0.3510(4) 0.5279(4) 0.0473(13) Uani 1 1 d . . . H39A H 0.586(4) 0.313(4) 0.589(4) 0.045(14) Uiso 1 1 d . . . C40 C 0.6940(5) 0.6232(5) 0.4102(5) 0.0702(19) Uani 1 1 d . . . H40A H 0.7105 0.6505 0.3465 0.105 Uiso 1 1 calc R . . H40B H 0.7534 0.6238 0.4408 0.105 Uiso 1 1 calc R . . H40C H 0.6367 0.6662 0.4322 0.105 Uiso 1 1 calc R . . C41 C 0.6010(5) 0.3534(5) 0.1189(4) 0.0559(15) Uani 1 1 d . . . H41A H 0.5986 0.3252 0.1808 0.067 Uiso 1 1 calc R . . C42 C 0.6529(6) 0.4431(6) 0.0815(6) 0.0698(19) Uani 1 1 d . . . H42A H 0.680(4) 0.475(4) 0.117(4) 0.052(17) Uiso 1 1 d . . . C43 C 0.6571(5) 0.4860(5) -0.0081(5) 0.0650(17) Uani 1 1 d . . . H43A H 0.6919 0.5460 -0.0336 0.078 Uiso 1 1 calc R . . C44 C 0.6082(4) 0.4392(4) -0.0621(4) 0.0537(15) Uani 1 1 d . . . C45 C 0.6063(5) 0.4784(5) -0.1563(4) 0.0650(18) Uani 1 1 d . . . H45A H 0.6389 0.5390 -0.1849 0.078 Uiso 1 1 calc R . . C46 C 0.5593(5) 0.4313(5) -0.2052(4) 0.0644(18) Uani 1 1 d . . . H46A H 0.5590 0.4602 -0.2668 0.077 Uiso 1 1 calc R . . C47 C 0.5088(4) 0.3362(4) -0.1647(3) 0.0487(14) Uani 1 1 d . . . C48 C 0.4613(5) 0.2791(5) -0.2126(4) 0.0539(15) Uani 1 1 d . . . H48A H 0.4603 0.3027 -0.2746 0.065 Uiso 1 1 calc R . . C49 C 0.4184(4) 0.1916(5) -0.1687(4) 0.0514(14) Uani 1 1 d . . . H49A H 0.3866 0.1541 -0.2000 0.062 Uiso 1 1 calc R . . C50 C 0.4207(4) 0.1557(4) -0.0753(3) 0.0449(13) Uani 1 1 d . . . H50A H 0.3916 0.0934 -0.0458 0.054 Uiso 1 1 calc R . . C51 C 0.5081(4) 0.2965(4) -0.0714(3) 0.0400(12) Uani 1 1 d . . . C52 C 0.5586(4) 0.3486(4) -0.0196(3) 0.0417(12) Uani 1 1 d . . . C53 C -0.0987(9) 0.5739(13) 0.0626(12) 0.060(4) Uani 0.50 1 d P . . C54 C -0.0430(7) 0.4903(10) 0.0340(7) 0.045(3) Uani 0.50 1 d P . . H54A H 0.0001 0.5150 -0.0212 0.067 Uiso 0.50 1 d PR . . H54B H -0.0002 0.4527 0.0798 0.067 Uiso 0.50 1 d PR . . H54C H -0.0904 0.4444 0.0246 0.067 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03965(14) 0.03193(13) 0.02091(11) -0.00587(8) -0.00454(8) -0.00380(9) Zn1 0.0482(3) 0.0386(3) 0.0287(3) -0.0059(2) -0.0049(2) -0.0073(3) N1 0.050(3) 0.041(2) 0.043(3) -0.011(2) -0.005(2) -0.006(2) N2 0.051(3) 0.042(2) 0.029(2) -0.0061(18) -0.0028(18) -0.006(2) O1 0.069(3) 0.055(2) 0.037(2) -0.0055(17) -0.0107(18) 0.024(2) O2 0.057(2) 0.052(2) 0.0316(19) -0.0056(16) -0.0029(16) 0.0027(19) O3 0.067(2) 0.053(2) 0.033(2) -0.0079(16) -0.0150(17) -0.019(2) O4 0.075(3) 0.047(2) 0.0316(19) -0.0048(16) -0.0076(17) -0.022(2) O5 0.0416(19) 0.046(2) 0.0322(18) -0.0039(15) -0.0023(15) -0.0002(17) O6 0.063(2) 0.071(3) 0.037(2) -0.0146(18) -0.0097(18) -0.012(2) O7 0.0441(19) 0.0423(19) 0.0313(18) -0.0108(15) 0.0006(15) -0.0001(17) O8 0.046(2) 0.051(2) 0.0310(19) -0.0076(15) -0.0060(15) 0.0019(17) O9 0.071(3) 0.0373(19) 0.0317(19) -0.0039(15) -0.0089(17) -0.0122(18) O10 0.077(3) 0.044(2) 0.0291(19) -0.0066(15) -0.0084(17) -0.021(2) O11 0.121(10) 0.141(11) 0.078(8) -0.059(8) -0.030(7) 0.092(9) O12 0.117(11) 0.111(10) 0.217(17) -0.090(11) -0.036(11) -0.002(9) C1 0.041(3) 0.034(3) 0.044(3) -0.011(2) -0.002(2) -0.002(2) C2 0.042(3) 0.038(3) 0.038(3) -0.002(2) 0.000(2) -0.005(2) C3 0.057(4) 0.058(4) 0.055(4) -0.010(3) -0.016(3) -0.004(3) C4 0.056(4) 0.070(5) 0.088(6) -0.010(4) -0.022(4) 0.009(4) C5 0.067(5) 0.066(4) 0.079(5) -0.004(4) 0.017(4) 0.015(4) C6 0.090(5) 0.081(5) 0.057(4) -0.027(4) 0.002(4) 0.032(4) C7 0.076(4) 0.064(4) 0.050(4) -0.015(3) -0.004(3) 0.014(4) C8 0.087(6) 0.111(7) 0.134(8) -0.017(6) 0.019(6) 0.041(5) C9 0.042(3) 0.043(3) 0.029(3) -0.012(2) -0.001(2) -0.003(2) C10 0.034(3) 0.041(3) 0.035(3) -0.013(2) -0.002(2) -0.006(2) C11 0.054(3) 0.050(3) 0.038(3) -0.006(2) 0.001(2) -0.008(3) C12 0.058(4) 0.050(4) 0.060(4) -0.005(3) 0.007(3) -0.023(3) C13 0.064(4) 0.064(4) 0.068(4) -0.026(3) 0.002(3) -0.025(3) C14 0.066(4) 0.064(4) 0.053(4) -0.022(3) -0.011(3) -0.024(3) C15 0.052(3) 0.051(3) 0.034(3) -0.010(2) -0.002(2) -0.013(3) C16 0.083(5) 0.093(6) 0.129(7) -0.038(5) -0.003(5) -0.053(5) C17 0.049(3) 0.033(3) 0.031(3) -0.002(2) -0.004(2) -0.010(2) C18 0.045(3) 0.043(3) 0.034(3) -0.003(2) -0.003(2) -0.005(3) C19 0.041(3) 0.053(3) 0.043(3) -0.013(2) -0.005(2) 0.000(3) C20 0.053(4) 0.073(4) 0.056(4) -0.023(3) -0.008(3) -0.005(3) C21 0.046(4) 0.064(4) 0.078(5) -0.011(3) -0.004(3) -0.003(3) C22 0.058(4) 0.071(5) 0.099(6) -0.039(4) 0.009(4) 0.006(4) C23 0.057(4) 0.074(4) 0.066(4) -0.040(3) 0.004(3) -0.003(3) C24 0.044(4) 0.114(7) 0.123(7) -0.016(5) -0.010(4) 0.001(4) C25 0.046(3) 0.027(2) 0.032(3) -0.0042(19) 0.000(2) -0.004(2) C26 0.044(3) 0.040(3) 0.031(3) -0.004(2) -0.001(2) -0.007(2) C27 0.051(3) 0.049(3) 0.049(3) -0.013(3) -0.003(3) 0.001(3) C28 0.048(4) 0.070(4) 0.058(4) -0.014(3) 0.000(3) 0.004(3) C29 0.043(3) 0.089(5) 0.058(4) -0.011(3) -0.006(3) 0.001(3) C30 0.047(4) 0.141(7) 0.058(4) -0.036(4) -0.013(3) -0.011(4) C31 0.050(3) 0.087(5) 0.048(3) -0.025(3) 0.002(3) -0.003(3) C32 0.052(4) 0.147(8) 0.079(5) -0.021(5) -0.014(4) 0.003(5) C33 0.055(3) 0.035(3) 0.032(3) -0.006(2) -0.006(2) -0.009(2) C34 0.045(3) 0.036(3) 0.033(3) -0.004(2) -0.010(2) -0.008(2) C35 0.111(5) 0.048(3) 0.028(3) -0.010(2) -0.009(3) -0.025(3) C36 0.096(5) 0.042(3) 0.048(4) 0.000(3) -0.009(3) -0.028(3) C37 0.056(3) 0.039(3) 0.053(3) -0.007(2) -0.016(3) -0.011(3) C38 0.083(4) 0.045(3) 0.044(3) -0.018(3) -0.016(3) -0.009(3) C39 0.069(4) 0.042(3) 0.032(3) -0.009(2) -0.004(3) -0.012(3) C40 0.084(5) 0.042(3) 0.088(5) -0.007(3) -0.029(4) -0.017(3) C41 0.064(4) 0.057(4) 0.054(4) -0.021(3) -0.013(3) -0.011(3) C42 0.071(5) 0.061(4) 0.089(6) -0.032(4) -0.014(4) -0.015(4) C43 0.063(4) 0.049(4) 0.084(5) -0.019(3) 0.002(3) -0.015(3) C44 0.054(3) 0.041(3) 0.061(4) -0.011(3) 0.011(3) -0.005(3) C45 0.076(4) 0.044(3) 0.063(4) -0.002(3) 0.017(3) -0.012(3) C46 0.085(5) 0.052(4) 0.043(3) 0.003(3) 0.010(3) -0.002(4) C47 0.056(3) 0.047(3) 0.035(3) -0.004(2) 0.004(2) 0.005(3) C48 0.061(4) 0.065(4) 0.030(3) -0.011(3) -0.006(3) 0.017(3) C49 0.051(3) 0.068(4) 0.040(3) -0.021(3) -0.011(2) 0.005(3) C50 0.053(3) 0.045(3) 0.039(3) -0.013(2) -0.006(2) -0.006(3) C51 0.047(3) 0.037(3) 0.032(3) -0.006(2) 0.002(2) -0.002(2) C52 0.048(3) 0.032(3) 0.041(3) -0.007(2) 0.001(2) 0.001(2) C53 0.021(6) 0.086(11) 0.089(11) -0.054(9) -0.004(6) 0.004(7) C54 0.021(5) 0.083(8) 0.047(6) -0.039(6) -0.010(4) -0.015(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 Tb1 O1 2.314(4) . ? Tb1 O3 2.316(3) . ? Tb1 O10 2.338(3) . ? Tb1 O7 2.359(3) 2_656 ? Tb1 O9 2.383(3) . ? Tb1 O8 2.412(3) . ? Tb1 O5 2.420(3) . ? Tb1 O7 2.599(3) . ? Tb1 C25 2.871(5) . ? Tb1 Tb1 3.9176(10) 2_656 ? Zn1 O4 1.991(4) . ? Zn1 O2 2.028(4) . ? Zn1 N2 2.149(4) . ? Zn1 N1 2.201(4) . ? Zn1 O6 2.226(4) . ? Zn1 O5 2.283(3) . ? Zn1 C17 2.585(5) . ? N1 C41 1.315(7) . ? N1 C52 1.354(6) . ? N2 C50 1.322(6) . ? N2 C51 1.356(6) . ? O1 C1 1.249(6) . ? O2 C1 1.273(6) . ? O3 C9 1.235(6) . ? O4 C9 1.251(6) . ? O5 C17 1.277(6) . ? O6 C17 1.242(6) . ? O7 C25 1.270(5) . ? O7 Tb1 2.359(3) 2_656 ? O8 C25 1.249(6) . ? O9 C33 1.255(5) 2_656 ? O10 C33 1.256(6) . ? O11 C53 1.197(18) . ? O12 C53 1.245(19) . ? C1 C2 1.480(7) . ? C2 C7 1.382(8) . ? C2 C3 1.388(8) . ? C3 C4 1.400(9) . ? C4 C5 1.366(11) . ? C5 C6 1.358(10) . ? C5 C8 1.523(10) . ? C6 C7 1.379(9) . ? C9 C10 1.486(7) . ? C10 C15 1.373(7) . ? C10 C11 1.400(7) . ? C11 C12 1.373(8) . ? C12 C13 1.373(9) . ? C13 C14 1.380(8) . ? C13 C16 1.501(9) . ? C14 C15 1.381(8) . ? C17 C18 1.485(7) . ? C18 C23 1.375(8) . ? C18 C19 1.382(7) . ? C19 C20 1.366(8) . ? C20 C21 1.369(9) . ? C21 C22 1.378(10) . ? C21 C24 1.511(9) . ? C22 C23 1.366(9) . ? C25 C26 1.478(7) . ? C26 C31 1.362(8) . ? C26 C27 1.404(7) . ? C27 C28 1.377(8) . ? C28 C29 1.379(9) . ? C29 C30 1.392(9) . ? C29 C32 1.499(8) . ? C30 C31 1.388(8) . ? C33 O9 1.255(5) 2_656 ? C33 C34 1.501(7) . ? C34 C39 1.376(7) . ? C34 C35 1.379(7) . ? C35 C36 1.389(8) . ? C36 C37 1.382(8) . ? C37 C38 1.383(7) . ? C37 C40 1.511(8) . ? C38 C39 1.379(8) . ? C41 C42 1.388(9) . ? C42 C43 1.350(9) . ? C43 C44 1.402(9) . ? C44 C52 1.395(7) . ? C44 C45 1.416(9) . ? C45 C46 1.330(9) . ? C46 C47 1.444(8) . ? C47 C51 1.399(7) . ? C47 C48 1.413(8) . ? C48 C49 1.325(8) . ? C49 C50 1.401(7) . ? C51 C52 1.434(7) . ? C53 C54 1.379(17) . ? C54 C54 1.429(19) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 78.18(14) . . ? O1 Tb1 O10 78.92(14) . . ? O3 Tb1 O10 149.09(12) . . ? O1 Tb1 O7 81.66(12) . 2_656 ? O3 Tb1 O7 118.95(13) . 2_656 ? O10 Tb1 O7 77.57(12) . 2_656 ? O1 Tb1 O9 125.74(14) . . ? O3 Tb1 O9 73.20(12) . . ? O10 Tb1 O9 137.63(12) . . ? O7 Tb1 O9 73.74(12) 2_656 . ? O1 Tb1 O8 151.23(13) . . ? O3 Tb1 O8 94.90(13) . . ? O10 Tb1 O8 95.24(13) . . ? O7 Tb1 O8 124.97(11) 2_656 . ? O9 Tb1 O8 77.06(13) . . ? O1 Tb1 O5 76.87(12) . . ? O3 Tb1 O5 79.57(12) . . ? O10 Tb1 O5 75.21(12) . . ? O7 Tb1 O5 147.98(12) 2_656 . ? O9 Tb1 O5 138.28(12) . . ? O8 Tb1 O5 74.40(11) . . ? O1 Tb1 O7 144.79(12) . . ? O3 Tb1 O7 136.59(12) . . ? O10 Tb1 O7 70.17(12) . . ? O7 Tb1 O7 75.71(12) 2_656 . ? O9 Tb1 O7 72.95(12) . . ? O8 Tb1 O7 51.36(10) . . ? O5 Tb1 O7 109.85(11) . . ? O1 Tb1 C25 156.95(14) . . ? O3 Tb1 C25 118.19(14) . . ? O10 Tb1 C25 79.55(14) . . ? O7 Tb1 C25 101.64(13) 2_656 . ? O9 Tb1 C25 76.51(13) . . ? O8 Tb1 C25 25.49(12) . . ? O5 Tb1 C25 89.73(12) . . ? O7 Tb1 C25 26.24(11) . . ? O1 Tb1 Tb1 117.05(9) . 2_656 ? O3 Tb1 Tb1 140.66(9) . 2_656 ? O10 Tb1 Tb1 69.23(9) . 2_656 ? O7 Tb1 Tb1 40.01(8) 2_656 2_656 ? O9 Tb1 Tb1 68.71(9) . 2_656 ? O8 Tb1 Tb1 86.03(8) . 2_656 ? O5 Tb1 Tb1 137.37(8) . 2_656 ? O7 Tb1 Tb1 35.69(7) . 2_656 ? C25 Tb1 Tb1 61.73(10) . 2_656 ? O4 Zn1 O2 94.57(16) . . ? O4 Zn1 N2 90.40(15) . . ? O2 Zn1 N2 105.24(15) . . ? O4 Zn1 N1 166.82(15) . . ? O2 Zn1 N1 89.75(15) . . ? N2 Zn1 N1 76.45(16) . . ? O4 Zn1 O6 94.24(16) . . ? O2 Zn1 O6 159.22(14) . . ? N2 Zn1 O6 93.47(15) . . ? N1 Zn1 O6 85.88(15) . . ? O4 Zn1 O5 104.39(14) . . ? O2 Zn1 O5 101.77(13) . . ? N2 Zn1 O5 147.96(14) . . ? N1 Zn1 O5 86.85(14) . . ? O6 Zn1 O5 57.75(12) . . ? O4 Zn1 C17 104.58(16) . . ? O2 Zn1 C17 130.53(15) . . ? N2 Zn1 C17 119.49(16) . . ? N1 Zn1 C17 81.72(16) . . ? O6 Zn1 C17 28.70(14) . . ? O5 Zn1 C17 29.58(13) . . ? C41 N1 C52 118.2(5) . . ? C41 N1 Zn1 128.4(4) . . ? C52 N1 Zn1 113.4(3) . . ? C50 N2 C51 118.5(4) . . ? C50 N2 Zn1 126.7(4) . . ? C51 N2 Zn1 114.8(3) . . ? C1 O1 Tb1 152.9(3) . . ? C1 O2 Zn1 126.0(3) . . ? C9 O3 Tb1 156.1(3) . . ? C9 O4 Zn1 125.3(3) . . ? C17 O5 Zn1 88.4(3) . . ? C17 O5 Tb1 137.2(3) . . ? Zn1 O5 Tb1 112.23(14) . . ? C17 O6 Zn1 91.9(3) . . ? C25 O7 Tb1 164.1(3) . 2_656 ? C25 O7 Tb1 88.9(3) . . ? Tb1 O7 Tb1 104.29(12) 2_656 . ? C25 O8 Tb1 98.3(3) . . ? C33 O9 Tb1 137.3(3) 2_656 . ? C33 O10 Tb1 137.8(3) . . ? O1 C1 O2 124.3(5) . . ? O1 C1 C2 117.1(4) . . ? O2 C1 C2 118.5(4) . . ? C7 C2 C3 118.4(6) . . ? C7 C2 C1 120.0(5) . . ? C3 C2 C1 121.5(5) . . ? C2 C3 C4 119.3(6) . . ? C5 C4 C3 121.7(7) . . ? C6 C5 C4 118.1(7) . . ? C6 C5 C8 121.3(8) . . ? C4 C5 C8 120.6(8) . . ? C5 C6 C7 121.9(7) . . ? C6 C7 C2 120.4(6) . . ? O3 C9 O4 124.5(5) . . ? O3 C9 C10 119.3(4) . . ? O4 C9 C10 116.2(4) . . ? C15 C10 C11 118.0(5) . . ? C15 C10 C9 121.6(4) . . ? C11 C10 C9 120.4(4) . . ? C12 C11 C10 120.0(5) . . ? C11 C12 C13 122.0(6) . . ? C12 C13 C14 117.7(6) . . ? C12 C13 C16 121.1(6) . . ? C14 C13 C16 121.1(6) . . ? C13 C14 C15 121.2(5) . . ? C10 C15 C14 121.1(5) . . ? O6 C17 O5 119.7(5) . . ? O6 C17 C18 119.3(5) . . ? O5 C17 C18 120.8(4) . . ? O6 C17 Zn1 59.4(3) . . ? O5 C17 Zn1 62.0(3) . . ? C18 C17 Zn1 163.5(3) . . ? C23 C18 C19 117.9(5) . . ? C23 C18 C17 120.7(5) . . ? C19 C18 C17 121.3(5) . . ? C20 C19 C18 120.4(5) . . ? C19 C20 C21 121.9(6) . . ? C22 C21 C20 117.5(6) . . ? C22 C21 C24 120.8(7) . . ? C20 C21 C24 121.7(7) . . ? C21 C22 C23 121.2(6) . . ? C22 C23 C18 121.0(6) . . ? O8 C25 O7 119.8(4) . . ? O8 C25 C26 121.1(4) . . ? O7 C25 C26 119.0(4) . . ? O8 C25 Tb1 56.2(2) . . ? O7 C25 Tb1 64.8(2) . . ? C26 C25 Tb1 164.3(3) . . ? C31 C26 C27 118.0(5) . . ? C31 C26 C25 122.0(5) . . ? C27 C26 C25 120.0(5) . . ? C28 C27 C26 120.0(6) . . ? C29 C28 C27 122.1(6) . . ? C28 C29 C30 117.4(6) . . ? C28 C29 C32 121.3(6) . . ? C30 C29 C32 121.2(6) . . ? C29 C30 C31 120.4(6) . . ? C26 C31 C30 121.9(6) . . ? O9 C33 O10 125.5(5) 2_656 . ? O9 C33 C34 117.7(4) 2_656 . ? O10 C33 C34 116.8(4) . . ? C39 C34 C35 117.7(5) . . ? C39 C34 C33 121.5(4) . . ? C35 C34 C33 120.8(4) . . ? C34 C35 C36 121.1(5) . . ? C37 C36 C35 121.2(5) . . ? C38 C37 C36 117.0(5) . . ? C38 C37 C40 122.4(5) . . ? C36 C37 C40 120.6(5) . . ? C39 C38 C37 121.8(5) . . ? C34 C39 C38 121.1(5) . . ? N1 C41 C42 122.6(6) . . ? C43 C42 C41 119.9(7) . . ? C42 C43 C44 119.2(6) . . ? C52 C44 C43 117.3(6) . . ? C52 C44 C45 118.7(6) . . ? C43 C44 C45 124.0(6) . . ? C46 C45 C44 122.1(6) . . ? C45 C46 C47 121.4(6) . . ? C51 C47 C48 117.4(5) . . ? C51 C47 C46 117.8(6) . . ? C48 C47 C46 124.7(5) . . ? C49 C48 C47 119.8(5) . . ? C48 C49 C50 120.0(6) . . ? N2 C50 C49 122.3(5) . . ? N2 C51 C47 122.0(5) . . ? N2 C51 C52 117.9(4) . . ? C47 C51 C52 120.1(5) . . ? N1 C52 C44 122.7(5) . . ? N1 C52 C51 117.4(4) . . ? C44 C52 C51 120.0(5) . . ? O11 C53 O12 124.8(15) . . ? O11 C53 C54 118.6(14) . . ? O12 C53 C54 116.4(17) . . ? C53 C54 C54 119.4(15) . 2_565 ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.554 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.107 data_c70327 _database_code_depnum_ccdc_archive 'CCDC 780299' #TrackingRef '- Complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 Ho N2 O11 Zn' _chemical_formula_weight 1116.21 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' Ho Ho -0.2175 4.6783 '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 13.056(4) _cell_length_b 13.146(4) _cell_length_c 15.367(5) _cell_angle_alpha 75.540(3) _cell_angle_beta 82.406(4) _cell_angle_gamma 83.166(4) _cell_volume 2521.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 2.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5354 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13303 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9394 _reflns_number_gt 7735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material 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^)+(0.0978P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9394 _refine_ls_number_parameters 663 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.983294(19) 0.03033(2) 0.371447(16) 0.02852(11) Uani 1 1 d . . . Zn1 Zn 0.97429(5) 0.16221(6) 0.11544(5) 0.03540(18) Uani 1 1 d . . . N1 N 0.9625(4) 0.2082(4) -0.0275(3) 0.0358(11) Uani 1 1 d . . . N2 N 1.0556(4) 0.3055(5) 0.0704(4) 0.0434(13) Uani 1 1 d . . . O1 O 0.8720(4) 0.1726(4) 0.3168(3) 0.0499(12) Uani 1 1 d . . . O2 O 0.8514(4) 0.2428(4) 0.1705(3) 0.0467(11) Uani 1 1 d . . . O3 O 0.9034(4) -0.0312(4) 0.2735(3) 0.0495(12) Uani 1 1 d . . . O4 O 0.8989(4) 0.0359(4) 0.1260(3) 0.0465(11) Uani 1 1 d . . . O5 O 1.1300(4) 0.0762(4) 0.0999(3) 0.0513(12) Uani 1 1 d . . . O6 O 1.0774(3) 0.1120(3) 0.2309(3) 0.0381(10) Uani 1 1 d . . . O7 O 1.1403(3) -0.0794(4) 0.3576(3) 0.0418(11) Uani 1 1 d . . . O8 O 1.1102(3) -0.0481(3) 0.4931(3) 0.0402(10) Uani 1 1 d . . . O9 O 1.0618(4) 0.1629(4) 0.4029(3) 0.0461(11) Uani 1 1 d . . . O10 O 0.9351(4) -0.1392(3) 0.4474(3) 0.0440(11) Uani 1 1 d . . . O11 O 0.4167(12) 0.6651(15) 0.0202(10) 0.111(6) Uani 0.50 1 d P . . H11A H 0.3793 0.7076 0.0438 0.167 Uiso 0.50 1 calc PR . . O12 O 0.3430(14) 0.5485(14) 0.1389(16) 0.136(7) Uani 0.50 1 d P . . C1 C 0.7259(6) 0.3309(6) 0.3622(5) 0.059(2) Uani 1 1 d . . . H1A H 0.7814 0.3126 0.3970 0.071 Uiso 1 1 calc R . . C2 C 0.6388(7) 0.3896(8) 0.3901(6) 0.075(3) Uani 1 1 d . . . H2A H 0.6371 0.4130 0.4427 0.090 Uiso 1 1 calc R . . C3 C 0.5547(6) 0.4142(7) 0.3413(6) 0.068(2) Uani 1 1 d . . . C4 C 0.5586(6) 0.3811(7) 0.2668(6) 0.067(2) Uani 1 1 d . . . H4A H 0.5005 0.3951 0.2352 0.080 Uiso 1 1 calc R . . C5 C 0.6478(6) 0.3252(6) 0.2332(6) 0.0519(19) Uani 1 1 d . . . H5A H 0.669(4) 0.311(5) 0.185(4) 0.020(16) Uiso 1 1 d . . . C6 C 0.7308(5) 0.2992(5) 0.2823(4) 0.0383(14) Uani 1 1 d . . . C7 C 0.8247(4) 0.2341(5) 0.2554(4) 0.0342(13) Uani 1 1 d . . . C8 C 0.4582(8) 0.4765(11) 0.3756(8) 0.116(4) Uani 1 1 d . . . H8A H 0.4069 0.4879 0.3340 0.174 Uiso 1 1 calc R . . H8B H 0.4764 0.5433 0.3807 0.174 Uiso 1 1 calc R . . H8C H 0.4306 0.4376 0.4338 0.174 Uiso 1 1 calc R . . C9 C 0.7789(5) -0.1879(5) 0.2691(4) 0.0441(16) Uani 1 1 d . . . H9A H 0.7970 -0.1846 0.3248 0.053 Uiso 1 1 calc R . . C10 C 0.7206(6) -0.2665(6) 0.2634(5) 0.0563(19) Uani 1 1 d . . . H10A H 0.708(6) -0.326(7) 0.319(5) 0.07(2) Uiso 1 1 d . . . C11 C 0.6916(6) -0.2718(7) 0.1811(6) 0.060(2) Uani 1 1 d . . . C12 C 0.7247(6) -0.1968(7) 0.1054(5) 0.057(2) Uani 1 1 d . . . H12A H 0.7069 -0.1988 0.0492 0.069 Uiso 1 1 calc R . . C13 C 0.7828(5) -0.1204(6) 0.1115(5) 0.0398(15) Uani 1 1 d . . . H13A H 0.805(4) -0.080(5) 0.074(4) 0.022(17) Uiso 1 1 d . . . C14 C 0.8102(4) -0.1147(5) 0.1924(4) 0.0344(13) Uani 1 1 d . . . C15 C 0.8762(4) -0.0310(5) 0.1986(4) 0.0313(13) Uani 1 1 d . . . C16 C 0.6294(8) -0.3564(9) 0.1733(8) 0.103(4) Uani 1 1 d . . . H16A H 0.6122 -0.4005 0.2322 0.154 Uiso 1 1 calc R . . H16B H 0.6692 -0.3982 0.1354 0.154 Uiso 1 1 calc R . . H16C H 0.5669 -0.3251 0.1473 0.154 Uiso 1 1 calc R . . C17 C 1.3355(6) 0.0216(7) 0.1448(5) 0.059(2) Uani 1 1 d . . . H17A H 1.3170 -0.0037 0.0982 0.071 Uiso 1 1 calc R . . C18 C 1.4364(6) 0.0082(7) 0.1620(6) 0.069(2) Uani 1 1 d . . . H18A H 1.4846 -0.0311 0.1305 0.083 Uiso 1 1 calc R . . C19 C 1.4683(5) 0.0519(7) 0.2253(6) 0.059(2) Uani 1 1 d . . . C20 C 1.3936(5) 0.1057(6) 0.2735(5) 0.0553(19) Uani 1 1 d . . . H20A H 1.4129 0.1372 0.3159 0.066 Uiso 1 1 calc R . . C21 C 1.2907(5) 0.1131(6) 0.2595(5) 0.0460(17) Uani 1 1 d . . . H21A H 1.253(5) 0.147(5) 0.285(4) 0.034(19) Uiso 1 1 d . . . C22 C 1.2599(5) 0.0720(5) 0.1951(4) 0.0384(14) Uani 1 1 d . . . C23 C 1.1503(5) 0.0845(5) 0.1748(4) 0.0352(13) Uani 1 1 d . . . C24 C 1.5807(6) 0.0392(8) 0.2423(7) 0.088(3) Uani 1 1 d . . . H24A H 1.5888 0.0746 0.2883 0.132 Uiso 1 1 calc R . . H24B H 1.6221 0.0694 0.1875 0.132 Uiso 1 1 calc R . . H24C H 1.6028 -0.0344 0.2619 0.132 Uiso 1 1 calc R . . C25 C 1.3221(5) -0.0915(7) 0.5183(5) 0.0548(19) Uani 1 1 d . . . H25A H 1.2791 -0.0606 0.5596 0.066 Uiso 1 1 calc R . . C26 C 1.4271(6) -0.1169(9) 0.5286(6) 0.077(3) Uani 1 1 d . . . H26A H 1.4549 -0.0992 0.5749 0.092 Uiso 1 1 calc R . . C27 C 1.4906(6) -0.1686(7) 0.4699(5) 0.063(2) Uani 1 1 d . . . C28 C 1.4500(5) -0.1900(6) 0.4002(5) 0.0529(18) Uani 1 1 d . . . H28A H 1.4921 -0.2244 0.3607 0.063 Uiso 1 1 calc R . . C29 C 1.3470(5) -0.1613(6) 0.3873(5) 0.0460(16) Uani 1 1 d . . . H29A H 1.3206 -0.1749 0.3384 0.055 Uiso 1 1 calc R . . C30 C 1.2824(5) -0.1121(5) 0.4471(4) 0.0387(14) Uani 1 1 d . . . C31 C 1.1710(5) -0.0804(5) 0.4318(4) 0.0340(13) Uani 1 1 d . . . C32 C 1.6054(6) -0.1956(9) 0.4860(6) 0.091(3) Uani 1 1 d . . . H32A H 1.6406 -0.2307 0.4412 0.137 Uiso 1 1 calc R . . H32B H 1.6106 -0.2411 0.5450 0.137 Uiso 1 1 calc R . . H32C H 1.6369 -0.1319 0.4817 0.137 Uiso 1 1 calc R . . C33 C 1.1341(7) 0.3628(6) 0.3705(5) 0.060(2) Uani 1 1 d . . . H33A H 1.120(7) 0.344(7) 0.318(6) 0.08(3) Uiso 1 1 d . . . C34 C 1.1632(8) 0.4630(6) 0.3570(6) 0.063(2) Uani 1 1 d . . . H34A H 1.169(6) 0.495(6) 0.305(5) 0.05(2) Uiso 1 1 d . . . C35 C 1.1644(6) 0.5097(5) 0.4268(5) 0.0478(17) Uani 1 1 d . . . C36 C 1.1370(7) 0.4524(6) 0.5124(5) 0.0550(19) Uani 1 1 d . . . H36A H 1.150(5) 0.481(6) 0.578(5) 0.06(2) Uiso 1 1 d . . . C37 C 1.1092(6) 0.3512(5) 0.5272(4) 0.0470(16) Uani 1 1 d . . . H37A H 1.0910 0.3139 0.5861 0.056 Uiso 1 1 calc R . . C38 C 1.1076(5) 0.3036(5) 0.4566(4) 0.0363(14) Uani 1 1 d . . . C39 C 1.0764(5) 0.1930(5) 0.4725(4) 0.0345(13) Uani 1 1 d . . . C40 C 1.1930(7) 0.6213(6) 0.4116(6) 0.067(2) Uani 1 1 d . . . H40A H 1.2090 0.6503 0.3481 0.101 Uiso 1 1 calc R . . H40B H 1.2524 0.6211 0.4424 0.101 Uiso 1 1 calc R . . H40C H 1.1357 0.6635 0.4347 0.101 Uiso 1 1 calc R . . C41 C 0.9207(5) 0.1556(6) -0.0759(5) 0.0431(16) Uani 1 1 d . . . H41A H 0.888(5) 0.102(6) -0.045(5) 0.05(2) Uiso 1 1 d . . . C42 C 0.9190(6) 0.1915(6) -0.1689(4) 0.0493(18) Uani 1 1 d . . . H42A H 0.8880 0.1540 -0.2007 0.059 Uiso 1 1 calc R . . C43 C 0.9619(6) 0.2796(6) -0.2123(5) 0.0541(19) Uani 1 1 d . . . H43A H 0.9604 0.3035 -0.2745 0.065 Uiso 1 1 calc R . . C44 C 1.0095(5) 0.3370(6) -0.1655(5) 0.0487(17) Uani 1 1 d . . . C45 C 1.0594(7) 0.4324(6) -0.2064(5) 0.062(2) Uani 1 1 d . . . H45A H 1.0595 0.4607 -0.2682 0.074 Uiso 1 1 calc R . . C46 C 1.1050(7) 0.4803(6) -0.1580(6) 0.064(2) Uani 1 1 d . . . H46A H 1.1369 0.5412 -0.1867 0.076 Uiso 1 1 calc R . . C47 C 1.1065(5) 0.4410(5) -0.0631(5) 0.0504(18) Uani 1 1 d . . . C48 C 1.1558(6) 0.4867(7) -0.0082(6) 0.064(2) Uani 1 1 d . . . H48A H 1.1907 0.5466 -0.0336 0.077 Uiso 1 1 calc R . . C49 C 1.1527(7) 0.4441(7) 0.0803(7) 0.069(2) Uani 1 1 d . . . H49A H 1.1847 0.4744 0.1170 0.082 Uiso 1 1 calc R . . C50 C 1.1001(6) 0.3521(6) 0.1181(6) 0.0553(19) Uani 1 1 d . . . H50A H 1.0975 0.3240 0.1801 0.066 Uiso 1 1 calc R . . C51 C 1.0575(5) 0.3485(5) -0.0200(4) 0.0406(15) Uani 1 1 d . . . C52 C 1.0087(5) 0.2968(5) -0.0716(4) 0.0379(14) Uani 1 1 d . . . C53 C 0.4003(11) 0.5728(17) 0.0637(14) 0.063(5) Uani 0.50 1 d P . . C54 C 0.4571(9) 0.4845(13) 0.0355(9) 0.051(4) Uani 0.50 1 d P . . H54A H 0.4386 0.4190 0.0753 0.076 Uiso 0.50 1 d PR . . H54B H 0.4422 0.4868 -0.0245 0.076 Uiso 0.50 1 d PR . . H54C H 0.5298 0.4901 0.0350 0.076 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.03632(17) 0.02413(17) 0.02443(16) -0.00671(10) -0.00488(10) 0.00388(11) Zn1 0.0438(4) 0.0301(4) 0.0312(4) -0.0063(3) -0.0050(3) 0.0000(3) N1 0.047(3) 0.029(3) 0.030(3) -0.008(2) -0.004(2) 0.005(2) N2 0.051(3) 0.040(3) 0.042(3) -0.015(3) -0.008(2) -0.003(3) O1 0.057(3) 0.050(3) 0.034(2) -0.009(2) -0.005(2) 0.027(2) O2 0.059(3) 0.042(3) 0.034(2) -0.008(2) -0.003(2) 0.009(2) O3 0.066(3) 0.050(3) 0.036(3) -0.007(2) -0.017(2) -0.014(2) O4 0.066(3) 0.041(3) 0.035(2) -0.003(2) -0.011(2) -0.024(2) O5 0.055(3) 0.063(3) 0.038(3) -0.016(2) -0.009(2) -0.001(2) O6 0.035(2) 0.041(3) 0.033(2) -0.0028(18) -0.0006(17) 0.0027(18) O7 0.044(2) 0.047(3) 0.029(2) -0.0081(19) -0.0039(18) 0.014(2) O8 0.047(2) 0.038(3) 0.033(2) -0.0107(19) 0.0035(18) 0.0067(19) O9 0.063(3) 0.046(3) 0.031(2) -0.006(2) -0.008(2) -0.013(2) O10 0.067(3) 0.030(3) 0.034(2) -0.0024(19) -0.010(2) -0.007(2) O11 0.109(11) 0.141(16) 0.089(10) -0.063(11) -0.039(9) 0.076(11) O12 0.108(13) 0.107(14) 0.22(2) -0.102(15) -0.024(14) 0.010(11) C1 0.068(5) 0.058(5) 0.047(4) -0.014(4) -0.013(4) 0.026(4) C2 0.089(6) 0.074(7) 0.057(5) -0.027(4) -0.006(4) 0.034(5) C3 0.059(5) 0.060(6) 0.073(6) -0.012(4) 0.006(4) 0.018(4) C4 0.048(4) 0.057(5) 0.087(6) -0.006(5) -0.012(4) 0.014(4) C5 0.048(4) 0.049(5) 0.059(5) -0.015(4) -0.013(4) 0.009(3) C6 0.039(3) 0.026(3) 0.044(4) -0.001(3) -0.005(3) 0.005(3) C7 0.037(3) 0.026(3) 0.039(3) -0.011(3) -0.004(2) 0.005(2) C8 0.085(7) 0.111(10) 0.129(10) -0.022(8) 0.010(7) 0.048(7) C9 0.047(4) 0.041(4) 0.041(4) -0.007(3) -0.002(3) -0.002(3) C10 0.059(4) 0.049(5) 0.057(5) -0.007(4) 0.005(4) -0.012(4) C11 0.053(4) 0.059(5) 0.075(5) -0.025(4) -0.001(4) -0.013(4) C12 0.066(5) 0.062(5) 0.054(5) -0.026(4) -0.009(4) -0.016(4) C13 0.044(4) 0.038(4) 0.038(4) -0.011(3) 0.000(3) -0.007(3) C14 0.034(3) 0.031(3) 0.039(3) -0.013(3) -0.003(2) 0.002(2) C15 0.037(3) 0.029(3) 0.030(3) -0.012(2) -0.006(2) 0.005(2) C16 0.096(7) 0.087(8) 0.139(10) -0.037(7) -0.006(7) -0.054(6) C17 0.056(4) 0.071(6) 0.059(5) -0.037(4) -0.001(4) 0.003(4) C18 0.047(4) 0.070(6) 0.094(6) -0.041(5) 0.007(4) 0.011(4) C19 0.042(4) 0.058(5) 0.072(5) -0.010(4) -0.007(4) 0.007(3) C20 0.049(4) 0.064(5) 0.055(4) -0.017(4) -0.015(3) 0.003(4) C21 0.041(4) 0.048(5) 0.048(4) -0.016(3) -0.001(3) 0.007(3) C22 0.045(3) 0.030(4) 0.036(3) -0.007(3) 0.002(3) 0.003(3) C23 0.043(3) 0.023(3) 0.037(3) -0.005(2) -0.002(3) 0.002(2) C24 0.041(4) 0.094(8) 0.129(8) -0.028(7) -0.016(5) 0.002(5) C25 0.039(4) 0.076(6) 0.055(4) -0.029(4) -0.005(3) 0.000(4) C26 0.052(5) 0.127(9) 0.059(5) -0.036(5) -0.011(4) 0.001(5) C27 0.042(4) 0.079(6) 0.061(5) -0.010(4) -0.006(3) 0.010(4) C28 0.046(4) 0.060(5) 0.053(4) -0.022(4) 0.000(3) 0.008(3) C29 0.043(4) 0.042(4) 0.050(4) -0.014(3) -0.001(3) 0.007(3) C30 0.039(3) 0.033(4) 0.039(3) -0.004(3) 0.000(3) 0.003(3) C31 0.039(3) 0.023(3) 0.035(3) -0.002(2) 0.004(2) -0.002(2) C32 0.048(5) 0.139(10) 0.079(6) -0.024(6) -0.012(4) 0.021(5) C33 0.106(7) 0.040(5) 0.035(4) -0.009(3) -0.008(4) -0.014(4) C34 0.106(7) 0.038(5) 0.044(5) 0.000(4) -0.008(4) -0.024(4) C35 0.060(4) 0.028(4) 0.058(4) -0.008(3) -0.019(3) -0.003(3) C36 0.083(5) 0.040(4) 0.046(4) -0.014(3) -0.017(4) -0.002(4) C37 0.070(5) 0.032(4) 0.037(4) -0.006(3) -0.006(3) -0.002(3) C38 0.049(3) 0.028(3) 0.033(3) -0.010(3) -0.009(3) -0.002(3) C39 0.048(3) 0.029(3) 0.028(3) -0.008(2) -0.010(2) 0.002(3) C40 0.090(6) 0.034(4) 0.082(6) -0.005(4) -0.032(5) -0.012(4) C41 0.045(4) 0.041(4) 0.045(4) -0.016(3) -0.009(3) 0.008(3) C42 0.061(4) 0.048(5) 0.037(4) -0.009(3) -0.014(3) 0.012(3) C43 0.068(5) 0.059(5) 0.030(4) -0.011(3) -0.007(3) 0.019(4) C44 0.051(4) 0.043(4) 0.043(4) -0.005(3) 0.004(3) 0.010(3) C45 0.083(6) 0.043(5) 0.044(4) 0.007(4) 0.011(4) 0.001(4) C46 0.078(5) 0.030(4) 0.069(5) 0.002(4) 0.017(4) -0.007(4) C47 0.052(4) 0.031(4) 0.061(4) -0.010(3) 0.014(3) -0.001(3) C48 0.058(5) 0.051(5) 0.086(6) -0.022(4) 0.003(4) -0.015(4) C49 0.073(5) 0.060(6) 0.084(7) -0.034(5) -0.015(5) -0.010(4) C50 0.063(5) 0.048(5) 0.061(5) -0.019(4) -0.012(4) -0.005(4) C51 0.041(3) 0.029(4) 0.047(4) -0.009(3) 0.006(3) 0.003(3) C52 0.044(3) 0.035(4) 0.030(3) -0.004(3) 0.000(2) 0.004(3) C53 0.033(7) 0.088(14) 0.087(13) -0.064(12) 0.005(8) -0.002(8) C54 0.034(6) 0.090(12) 0.044(8) -0.037(8) -0.014(5) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1 2.282(4) . ? Ho1 O3 2.287(4) . ? Ho1 O9 2.301(5) . ? Ho1 O8 2.320(4) 2_756 ? Ho1 O10 2.359(4) . ? Ho1 O7 2.379(4) . ? Ho1 O6 2.404(4) . ? Ho1 O8 2.599(4) . ? Ho1 C31 2.839(6) . ? Ho1 Ho1 3.9033(13) 2_756 ? Zn1 O4 1.991(4) . ? Zn1 O2 2.023(5) . ? Zn1 N1 2.149(5) . ? Zn1 N2 2.188(6) . ? Zn1 O5 2.220(5) . ? Zn1 O6 2.287(4) . ? Zn1 C23 2.586(6) . ? N1 C41 1.336(8) . ? N1 C52 1.357(8) . ? N2 C50 1.292(9) . ? N2 C51 1.361(8) . ? O1 C7 1.256(7) . ? O2 C7 1.286(7) . ? O3 C15 1.248(7) . ? O4 C15 1.261(7) . ? O5 C23 1.248(7) . ? O6 C23 1.279(7) . ? O7 C31 1.255(7) . ? O8 C31 1.273(7) . ? O8 Ho1 2.320(4) 2_756 ? O9 C39 1.274(7) . ? O10 C39 1.256(7) 2_756 ? O11 C53 1.26(2) . ? O12 C53 1.28(3) . ? C1 C2 1.379(10) . ? C1 C6 1.383(10) . ? C2 C3 1.374(12) . ? C3 C4 1.315(12) . ? C3 C8 1.527(12) . ? C4 C5 1.412(11) . ? C5 C6 1.364(9) . ? C6 C7 1.483(8) . ? C9 C14 1.371(9) . ? C9 C10 1.380(10) . ? C10 C11 1.387(11) . ? C11 C12 1.382(11) . ? C11 C16 1.489(11) . ? C12 C13 1.357(10) . ? C13 C14 1.360(9) . ? C14 C15 1.505(8) . ? C17 C18 1.361(10) . ? C17 C22 1.382(9) . ? C18 C19 1.376(12) . ? C19 C20 1.381(11) . ? C19 C24 1.507(10) . ? C20 C21 1.376(9) . ? C21 C22 1.363(10) . ? C22 C23 1.486(8) . ? C25 C30 1.368(9) . ? C25 C26 1.392(10) . ? C26 C27 1.391(12) . ? C27 C28 1.359(11) . ? C27 C32 1.537(10) . ? C28 C29 1.380(9) . ? C29 C30 1.391(9) . ? C30 C31 1.497(8) . ? C33 C34 1.373(11) . ? C33 C38 1.380(9) . ? C34 C35 1.364(11) . ? C35 C36 1.367(10) . ? C35 C40 1.511(10) . ? C36 C37 1.377(10) . ? C37 C38 1.385(9) . ? C38 C39 1.508(9) . ? C39 O10 1.256(7) 2_756 ? C41 C42 1.392(9) . ? C42 C43 1.330(11) . ? C43 C44 1.406(11) . ? C44 C52 1.407(9) . ? C44 C45 1.444(11) . ? C45 C46 1.320(12) . ? C46 C47 1.422(11) . ? C47 C48 1.407(11) . ? C47 C51 1.412(9) . ? C48 C49 1.332(12) . ? C49 C50 1.419(11) . ? C51 C52 1.415(9) . ? C53 C54 1.43(2) . ? C54 C54 1.47(3) 2_665 ? 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 Ho1 O3 78.41(18) . . ? O1 Ho1 O9 79.65(18) . . ? O3 Ho1 O9 149.65(16) . . ? O1 Ho1 O8 81.21(15) . 2_756 ? O3 Ho1 O8 118.26(17) . 2_756 ? O9 Ho1 O8 78.40(16) . 2_756 ? O1 Ho1 O10 125.56(18) . . ? O3 Ho1 O10 72.71(16) . . ? O9 Ho1 O10 137.61(14) . . ? O8 Ho1 O10 73.74(16) 2_756 . ? O1 Ho1 O7 151.57(16) . . ? O3 Ho1 O7 94.87(17) . . ? O9 Ho1 O7 94.51(17) . . ? O8 Ho1 O7 125.20(14) 2_756 . ? O10 Ho1 O7 76.90(16) . . ? O1 Ho1 O6 77.69(15) . . ? O3 Ho1 O6 80.19(16) . . ? O9 Ho1 O6 74.83(15) . . ? O8 Ho1 O6 148.36(16) 2_756 . ? O10 Ho1 O6 137.90(16) . . ? O7 Ho1 O6 73.94(14) . . ? O1 Ho1 O8 144.28(16) . . ? O3 Ho1 O8 136.59(16) . . ? O9 Ho1 O8 69.74(15) . . ? O8 Ho1 O8 75.10(15) 2_756 . ? O10 Ho1 O8 72.59(15) . . ? O7 Ho1 O8 52.19(13) . . ? O6 Ho1 O8 110.22(13) . . ? O1 Ho1 C31 157.30(19) . . ? O3 Ho1 C31 118.38(18) . . ? O9 Ho1 C31 78.83(17) . . ? O8 Ho1 C31 101.40(16) 2_756 . ? O10 Ho1 C31 76.16(16) . . ? O7 Ho1 C31 25.95(16) . . ? O6 Ho1 C31 89.74(15) . . ? O8 Ho1 C31 26.60(15) . . ? O1 Ho1 Ho1 116.72(11) . 2_756 ? O3 Ho1 Ho1 139.92(11) . 2_756 ? O9 Ho1 Ho1 69.51(10) . 2_756 ? O8 Ho1 Ho1 40.05(10) 2_756 2_756 ? O10 Ho1 Ho1 68.56(10) . 2_756 ? O7 Ho1 Ho1 86.24(10) . 2_756 ? O6 Ho1 Ho1 137.40(10) . 2_756 ? O8 Ho1 Ho1 35.05(9) . 2_756 ? C31 Ho1 Ho1 61.45(12) . 2_756 ? O4 Zn1 O2 94.3(2) . . ? O4 Zn1 N1 90.42(19) . . ? O2 Zn1 N1 104.79(18) . . ? O4 Zn1 N2 166.74(19) . . ? O2 Zn1 N2 90.5(2) . . ? N1 Zn1 N2 76.4(2) . . ? O4 Zn1 O5 94.0(2) . . ? O2 Zn1 O5 159.68(17) . . ? N1 Zn1 O5 93.67(18) . . ? N2 Zn1 O5 85.6(2) . . ? O4 Zn1 O6 103.91(17) . . ? O2 Zn1 O6 101.94(16) . . ? N1 Zn1 O6 148.53(17) . . ? N2 Zn1 O6 87.12(18) . . ? O5 Zn1 O6 58.00(16) . . ? O4 Zn1 C23 104.0(2) . . ? O2 Zn1 C23 130.84(19) . . ? N1 Zn1 C23 120.01(19) . . ? N2 Zn1 C23 81.9(2) . . ? O5 Zn1 C23 28.84(18) . . ? O6 Zn1 C23 29.64(16) . . ? C41 N1 C52 118.5(5) . . ? C41 N1 Zn1 126.6(4) . . ? C52 N1 Zn1 114.7(4) . . ? C50 N2 C51 118.1(6) . . ? C50 N2 Zn1 128.5(5) . . ? C51 N2 Zn1 113.4(4) . . ? C7 O1 Ho1 153.4(4) . . ? C7 O2 Zn1 125.9(4) . . ? C15 O3 Ho1 155.4(4) . . ? C15 O4 Zn1 125.1(4) . . ? C23 O5 Zn1 92.1(4) . . ? C23 O6 Zn1 88.2(3) . . ? C23 O6 Ho1 137.4(4) . . ? Zn1 O6 Ho1 112.20(16) . . ? C31 O7 Ho1 98.0(4) . . ? C31 O8 Ho1 165.0(4) . 2_756 ? C31 O8 Ho1 87.3(3) . . ? Ho1 O8 Ho1 104.90(15) 2_756 . ? C39 O9 Ho1 137.5(4) . . ? C39 O10 Ho1 137.5(4) 2_756 . ? C2 C1 C6 119.9(7) . . ? C3 C2 C1 120.9(8) . . ? C4 C3 C2 118.8(8) . . ? C4 C3 C8 121.6(9) . . ? C2 C3 C8 119.6(9) . . ? C3 C4 C5 122.3(8) . . ? C6 C5 C4 118.9(8) . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C7 122.5(6) . . ? C1 C6 C7 118.5(6) . . ? O1 C7 O2 124.1(5) . . ? O1 C7 C6 118.2(5) . . ? O2 C7 C6 117.7(5) . . ? C14 C9 C10 119.9(7) . . ? C9 C10 C11 120.9(7) . . ? C12 C11 C10 117.5(7) . . ? C12 C11 C16 120.6(8) . . ? C10 C11 C16 121.8(8) . . ? C13 C12 C11 121.1(7) . . ? C12 C13 C14 121.2(7) . . ? C13 C14 C9 119.4(6) . . ? C13 C14 C15 120.9(6) . . ? C9 C14 C15 119.7(6) . . ? O3 C15 O4 124.8(6) . . ? O3 C15 C14 119.0(5) . . ? O4 C15 C14 116.2(5) . . ? C18 C17 C22 121.3(7) . . ? C17 C18 C19 121.1(7) . . ? C18 C19 C20 117.6(7) . . ? C18 C19 C24 120.8(8) . . ? C20 C19 C24 121.6(8) . . ? C21 C20 C19 120.8(8) . . ? C22 C21 C20 121.3(7) . . ? C21 C22 C17 117.7(6) . . ? C21 C22 C23 122.4(6) . . ? C17 C22 C23 119.9(6) . . ? O5 C23 O6 119.7(6) . . ? O5 C23 C22 119.8(6) . . ? O6 C23 C22 120.2(5) . . ? O5 C23 Zn1 59.1(3) . . ? O6 C23 Zn1 62.1(3) . . ? C22 C23 Zn1 162.9(4) . . ? C30 C25 C26 119.8(7) . . ? C25 C26 C27 120.4(8) . . ? C28 C27 C26 119.2(7) . . ? C28 C27 C32 123.0(8) . . ? C26 C27 C32 117.7(8) . . ? C27 C28 C29 120.7(7) . . ? C28 C29 C30 120.4(7) . . ? C25 C30 C29 119.4(6) . . ? C25 C30 C31 120.8(6) . . ? C29 C30 C31 119.8(6) . . ? O7 C31 O8 120.9(5) . . ? O7 C31 C30 120.3(5) . . ? O8 C31 C30 118.6(6) . . ? O7 C31 Ho1 56.1(3) . . ? O8 C31 Ho1 66.1(3) . . ? C30 C31 Ho1 164.1(4) . . ? C34 C33 C38 120.7(7) . . ? C35 C34 C33 122.2(7) . . ? C36 C35 C34 117.7(7) . . ? C36 C35 C40 120.2(7) . . ? C34 C35 C40 122.1(7) . . ? C35 C36 C37 120.9(7) . . ? C36 C37 C38 121.5(6) . . ? C33 C38 C37 116.9(6) . . ? C33 C38 C39 121.4(6) . . ? C37 C38 C39 121.7(5) . . ? O10 C39 O9 125.4(6) 2_756 . ? O10 C39 C38 118.1(5) 2_756 . ? O9 C39 C38 116.5(5) . . ? N1 C41 C42 122.0(7) . . ? C43 C42 C41 119.8(7) . . ? C42 C43 C44 120.9(6) . . ? C52 C44 C43 116.7(7) . . ? C52 C44 C45 118.2(7) . . ? C43 C44 C45 125.1(7) . . ? C46 C45 C44 121.5(7) . . ? C45 C46 C47 121.7(7) . . ? C48 C47 C51 116.7(7) . . ? C48 C47 C46 124.4(7) . . ? C51 C47 C46 118.8(7) . . ? C49 C48 C47 120.0(7) . . ? C48 C49 C50 119.4(8) . . ? N2 C50 C49 123.2(8) . . ? N2 C51 C47 122.6(7) . . ? N2 C51 C52 117.7(6) . . ? C47 C51 C52 119.8(6) . . ? N1 C52 C44 122.1(6) . . ? N1 C52 C51 117.9(5) . . ? C44 C52 C51 120.0(6) . . ? O11 C53 O12 125.4(18) . . ? O11 C53 C54 119.9(17) . . ? O12 C53 C54 114(2) . . ? C53 C54 C54 112.6(19) . 2_665 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.869 _refine_diff_density_min -1.501 _refine_diff_density_rms 0.151 data_w04149 _database_code_depnum_ccdc_archive 'CCDC 780300' #TrackingRef '- Complex 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H57 N4 O14 Pr Zn2' _chemical_formula_weight 1425.83 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 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 10.719(2) _cell_length_b 21.494(4) _cell_length_c 26.116(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.83(3) _cell_angle_gamma 90.00 _cell_volume 6017(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8516 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37945 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.60 _reflns_number_total 13757 _reflns_number_gt 8483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material 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^)+(0.0470P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13757 _refine_ls_number_parameters 958 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 Pr1 Pr 0.49586(2) 0.257710(11) 0.097960(9) 0.02867(8) Uani 1 1 d . . . Zn1 Zn 0.64412(5) 0.41211(2) 0.06021(2) 0.03408(14) Uani 1 1 d . . . Zn2 Zn 0.32593(5) 0.11541(2) 0.03249(2) 0.03343(14) Uani 1 1 d . . . N1 N 0.7882(4) 0.43874(18) 0.11592(15) 0.0388(10) Uani 1 1 d . . . N2 N 0.7409(3) 0.48435(17) 0.02221(14) 0.0341(9) Uani 1 1 d . . . N3 N 0.1606(3) 0.14894(18) -0.01001(14) 0.0347(9) Uani 1 1 d . . . N4 N 0.2561(3) 0.03300(17) -0.00137(13) 0.0331(9) Uani 1 1 d . . . O1 O 0.4228(3) 0.31828(15) 0.02450(13) 0.0452(9) Uani 1 1 d . . . O2 O 0.5349(3) 0.39893(15) -0.00218(12) 0.0431(8) Uani 1 1 d . . . O3 O 0.5176(3) 0.44714(15) 0.10954(12) 0.0440(9) Uani 1 1 d . . . O4 O 0.4381(3) 0.35643(15) 0.13365(13) 0.0513(10) Uani 1 1 d . . . O5 O 0.6802(3) 0.32034(13) 0.07533(12) 0.0356(8) Uani 1 1 d . . . O6 O 0.8574(3) 0.33804(17) 0.03587(15) 0.0596(11) Uani 1 1 d . . . O7 O 0.6261(3) 0.27081(17) 0.17953(13) 0.0540(10) Uani 1 1 d . . . O8 O 0.4366(3) 0.24377(16) 0.19309(12) 0.0490(9) Uani 1 1 d . . . O9 O 0.4332(3) 0.14627(17) -0.02681(12) 0.0488(9) Uani 1 1 d . . . O10 O 0.5554(3) 0.20439(15) 0.02235(12) 0.0481(9) Uani 1 1 d . . . O11 O 0.2924(3) 0.21385(16) 0.08679(12) 0.0428(8) Uani 1 1 d . . . O12 O 0.2062(3) 0.12189(15) 0.09653(12) 0.0424(8) Uani 1 1 d . . . O13 O 0.5396(3) 0.15021(15) 0.12059(12) 0.0469(9) Uani 1 1 d . . . O14 O 0.4600(3) 0.07200(15) 0.07381(12) 0.0403(8) Uani 1 1 d . . . C1 C 0.4513(4) 0.3576(2) -0.00805(18) 0.0348(11) Uani 1 1 d . . . C2 C 0.3842(4) 0.3568(2) -0.05880(17) 0.0328(11) Uani 1 1 d . . . C3 C 0.3089(5) 0.3073(3) -0.0723(2) 0.0509(15) Uani 1 1 d . . . H3A H 0.302(4) 0.274(2) -0.0489(17) 0.043(14) Uiso 1 1 d . . . C4 C 0.2406(6) 0.3079(3) -0.1174(2) 0.0588(17) Uani 1 1 d . . . H4A H 0.190(5) 0.276(2) -0.1249(18) 0.045(15) Uiso 1 1 d . . . C5 C 0.2461(5) 0.3570(3) -0.15140(19) 0.0470(13) Uani 1 1 d . . . C6 C 0.3255(5) 0.4052(2) -0.1387(2) 0.0442(13) Uani 1 1 d . . . H6A H 0.334(4) 0.439(2) -0.1616(16) 0.040(13) Uiso 1 1 d . . . C7 C 0.3938(5) 0.4050(2) -0.0931(2) 0.0418(13) Uani 1 1 d . . . H7A H 0.445(4) 0.438(2) -0.0875(16) 0.039(14) Uiso 1 1 d . . . C8 C 0.1689(6) 0.3582(3) -0.2002(2) 0.0690(18) Uani 1 1 d . . . H8A H 0.1847 0.3961 -0.2184 0.104 Uiso 1 1 calc R . . H8B H 0.0820 0.3559 -0.1921 0.104 Uiso 1 1 calc R . . H8C H 0.1909 0.3233 -0.2212 0.104 Uiso 1 1 calc R . . C9 C 0.4508(4) 0.4139(2) 0.13813(18) 0.0350(11) Uani 1 1 d . . . C10 C 0.3822(4) 0.4463(2) 0.17983(18) 0.0369(11) Uani 1 1 d . . . C11 C 0.3202(5) 0.4114(3) 0.2169(2) 0.0503(15) Uani 1 1 d . . . H11A H 0.316(6) 0.370(3) 0.214(2) 0.09(2) Uiso 1 1 d . . . C12 C 0.2587(6) 0.4415(3) 0.2560(2) 0.0588(17) Uani 1 1 d . . . H12A H 0.224(6) 0.412(3) 0.279(2) 0.10(2) Uiso 1 1 d . . . C13 C 0.2571(5) 0.5048(3) 0.2602(2) 0.0566(16) Uani 1 1 d . . . C14 C 0.3183(6) 0.5387(3) 0.2243(3) 0.0606(17) Uani 1 1 d . . . H14A H 0.326(4) 0.583(2) 0.2256(17) 0.045(14) Uiso 1 1 d . . . C15 C 0.3822(5) 0.5104(3) 0.1851(2) 0.0494(14) Uani 1 1 d . . . H15A H 0.420(4) 0.532(2) 0.1591(17) 0.037(14) Uiso 1 1 d . . . C16 C 0.1860(6) 0.5367(4) 0.3021(2) 0.094(3) Uani 1 1 d . . . H16A H 0.1960 0.5809 0.2992 0.141 Uiso 1 1 calc R . . H16B H 0.2176 0.5231 0.3349 0.141 Uiso 1 1 calc R . . H16C H 0.0991 0.5263 0.2991 0.141 Uiso 1 1 calc R . . C17 C 0.7927(5) 0.3047(2) 0.06201(18) 0.0382(12) Uani 1 1 d . . . C18 C 0.8361(5) 0.2426(2) 0.0814(2) 0.0582(15) Uani 1 1 d . . . H18A H 0.9193 0.2349 0.0699 0.087 Uiso 1 1 calc R . . H18B H 0.7813 0.2106 0.0685 0.087 Uiso 1 1 calc R . . H18C H 0.8353 0.2424 0.1181 0.087 Uiso 1 1 calc R . . C19 C 0.5378(4) 0.2640(2) 0.21128(17) 0.0298(10) Uani 1 1 d . . . C20 C 0.5507(4) 0.2766(2) 0.25486(15) 0.0315(11) Uani 1 1 d . . . H20A H 0.5747 0.2401 0.2737 0.047 Uiso 1 1 calc R . . H20B H 0.4736 0.2924 0.2678 0.047 Uiso 1 1 calc R . . H20C H 0.6144 0.3077 0.2586 0.047 Uiso 1 1 calc R . . C21 C 0.5200(4) 0.1839(2) -0.02049(18) 0.0361(11) Uani 1 1 d . . . C22 C 0.5882(4) 0.2072(2) -0.06625(17) 0.0335(11) Uani 1 1 d . . . C23 C 0.5839(5) 0.1773(3) -0.1124(2) 0.0482(14) Uani 1 1 d . . . H23A H 0.528(5) 0.142(2) -0.1123(18) 0.055(16) Uiso 1 1 d . . . C24 C 0.6478(6) 0.2015(3) -0.1538(2) 0.0564(16) Uani 1 1 d . . . H24A H 0.649(5) 0.178(2) -0.184(2) 0.062(17) Uiso 1 1 d . . . C25 C 0.7134(5) 0.2563(3) -0.1511(2) 0.0480(14) Uani 1 1 d . . . C26 C 0.7165(5) 0.2870(3) -0.1042(2) 0.0484(14) Uani 1 1 d . . . H26A H 0.758(4) 0.329(2) -0.1034(17) 0.049(15) Uiso 1 1 d . . . C27 C 0.6563(5) 0.2626(2) -0.0620(2) 0.0416(12) Uani 1 1 d . . . H27A H 0.666(5) 0.282(2) -0.028(2) 0.062(17) Uiso 1 1 d . . . C28 C 0.7807(6) 0.2821(3) -0.1965(2) 0.079(2) Uani 1 1 d . . . H28A H 0.7696 0.2546 -0.2252 0.119 Uiso 1 1 calc R . . H28B H 0.8680 0.2858 -0.1884 0.119 Uiso 1 1 calc R . . H28C H 0.7475 0.3223 -0.2050 0.119 Uiso 1 1 calc R . . C29 C 0.2169(4) 0.1779(2) 0.10957(18) 0.0365(11) Uani 1 1 d . . . C30 C 0.1357(4) 0.2039(2) 0.15028(17) 0.0351(11) Uani 1 1 d . . . C31 C 0.0562(5) 0.1656(3) 0.1772(2) 0.0453(14) Uani 1 1 d . . . H31A H 0.065(4) 0.126(2) 0.1693(18) 0.047(16) Uiso 1 1 d . . . C32 C -0.0206(5) 0.1897(3) 0.2140(2) 0.0514(15) Uani 1 1 d . . . H32A H -0.071(5) 0.161(2) 0.2329(19) 0.065(18) Uiso 1 1 d . . . C33 C -0.0217(5) 0.2527(2) 0.2251(2) 0.0447(13) Uani 1 1 d . . . C34 C 0.0581(5) 0.2910(3) 0.1979(2) 0.0523(15) Uani 1 1 d . . . H34A H 0.060(5) 0.340(2) 0.2049(18) 0.064(16) Uiso 1 1 d . . . C35 C 0.1367(5) 0.2667(3) 0.1609(2) 0.0456(14) Uani 1 1 d . . . H35A H 0.186(4) 0.294(2) 0.1449(16) 0.033(13) Uiso 1 1 d . . . C36 C -0.1103(7) 0.2790(4) 0.2645(3) 0.0671(19) Uani 1 1 d . . . H36A H -0.082(5) 0.319(3) 0.2781(19) 0.056(17) Uiso 1 1 d . . . H36B H -0.097(6) 0.248(3) 0.297(3) 0.10(2) Uiso 1 1 d . . . H36C H -0.199(6) 0.275(3) 0.251(2) 0.08(2) Uiso 1 1 d . . . C37 C 0.5334(4) 0.0942(2) 0.10764(17) 0.0338(11) Uani 1 1 d . . . C38 C 0.6198(4) 0.0489(2) 0.13389(17) 0.0336(11) Uani 1 1 d . . . C39 C 0.7074(5) 0.0696(3) 0.1692(2) 0.0457(14) Uani 1 1 d . . . H39A H 0.707(5) 0.107(3) 0.176(2) 0.07(2) Uiso 1 1 d . . . C40 C 0.7888(6) 0.0284(3) 0.1930(2) 0.0599(16) Uani 1 1 d . . . H40A H 0.857(5) 0.047(3) 0.219(2) 0.077(18) Uiso 1 1 d . . . C41 C 0.7855(5) -0.0348(3) 0.1822(2) 0.0495(14) Uani 1 1 d . . . C42 C 0.6964(5) -0.0550(3) 0.1472(2) 0.0483(14) Uani 1 1 d . . . H42A H 0.693(4) -0.097(2) 0.1402(16) 0.038(14) Uiso 1 1 d . . . C43 C 0.6153(5) -0.0142(2) 0.1237(2) 0.0395(12) Uani 1 1 d . . . H43A H 0.558(4) -0.026(2) 0.0992(16) 0.034(13) Uiso 1 1 d . . . C44 C 0.8751(6) -0.0788(3) 0.2078(2) 0.076(2) Uani 1 1 d . . . H44A H 0.8590 -0.1204 0.1961 0.114 Uiso 1 1 calc R . . H44B H 0.8647 -0.0769 0.2442 0.114 Uiso 1 1 calc R . . H44C H 0.9590 -0.0673 0.1996 0.114 Uiso 1 1 calc R . . C45 C 0.8062(6) 0.4183(3) 0.1636(2) 0.0501(14) Uani 1 1 d . . . H45A H 0.751(4) 0.3903(19) 0.1749(15) 0.024(12) Uiso 1 1 d . . . C46 C 0.8976(6) 0.4417(3) 0.1962(2) 0.0568(16) Uani 1 1 d . . . H46A H 0.902(5) 0.421(2) 0.229(2) 0.061(17) Uiso 1 1 d . . . C47 C 0.9762(6) 0.4859(3) 0.1789(2) 0.0582(16) Uani 1 1 d . . . H47A H 1.049(4) 0.502(2) 0.1957(16) 0.043(14) Uiso 1 1 d . . . C48 C 0.9627(5) 0.5093(2) 0.12881(19) 0.0424(12) Uani 1 1 d . . . C49 C 1.0384(5) 0.5567(3) 0.1074(2) 0.0524(15) Uani 1 1 d . . . H49A H 1.110(4) 0.5710(19) 0.1262(15) 0.030(12) Uiso 1 1 d . . . C50 C 1.0142(5) 0.5792(3) 0.0607(3) 0.0521(16) Uani 1 1 d . . . H50A H 1.057(4) 0.606(2) 0.0462(17) 0.040(15) Uiso 1 1 d . . . C51 C 0.9133(4) 0.5567(2) 0.02949(19) 0.0378(12) Uani 1 1 d . . . C52 C 0.8822(5) 0.5802(2) -0.0190(2) 0.0459(13) Uani 1 1 d . . . H52A H 0.925(4) 0.618(2) -0.0321(17) 0.052(15) Uiso 1 1 d . . . C53 C 0.7825(6) 0.5565(3) -0.0447(2) 0.0487(14) Uani 1 1 d . . . H53A H 0.769(4) 0.5637(19) -0.0753(15) 0.019(12) Uiso 1 1 d . . . C54 C 0.7134(5) 0.5076(2) -0.02349(19) 0.0392(12) Uani 1 1 d . . . H54A H 0.647(4) 0.4851(18) -0.0422(14) 0.020(11) Uiso 1 1 d . . . C55 C 0.8397(4) 0.5085(2) 0.04873(18) 0.0340(11) Uani 1 1 d . . . C56 C 0.8641(4) 0.4844(2) 0.09901(18) 0.0355(11) Uani 1 1 d . . . C57 C 0.1107(5) 0.2052(3) -0.0134(2) 0.0471(15) Uani 1 1 d . . . H57A H 0.146(4) 0.2318(19) -0.0002(15) 0.017(12) Uiso 1 1 d . . . C58 C 0.0059(6) 0.2192(3) -0.0422(3) 0.0587(18) Uani 1 1 d . . . H58A H -0.020(5) 0.253(2) -0.047(2) 0.055(18) Uiso 1 1 d . . . C59 C -0.0509(5) 0.1730(3) -0.0695(2) 0.0559(16) Uani 1 1 d . . . H59A H -0.123(4) 0.182(2) -0.0921(16) 0.037(13) Uiso 1 1 d . . . C60 C -0.0037(4) 0.1125(2) -0.06712(18) 0.0406(12) Uani 1 1 d . . . C61 C -0.0617(5) 0.0605(3) -0.0922(2) 0.0508(15) Uani 1 1 d . . . H61A H -0.128(5) 0.070(2) -0.1137(19) 0.055(16) Uiso 1 1 d . . . C62 C -0.0170(5) 0.0035(3) -0.0864(2) 0.0491(15) Uani 1 1 d . . . H62A H -0.045(4) -0.025(2) -0.1005(16) 0.030(14) Uiso 1 1 d . . . C63 C 0.0913(4) -0.0093(2) -0.05595(18) 0.0366(11) Uani 1 1 d . . . C64 C 0.1420(5) -0.0683(2) -0.0481(2) 0.0450(13) Uani 1 1 d . . . H64A H 0.102(4) -0.105(2) -0.0629(15) 0.030(12) Uiso 1 1 d . . . C65 C 0.2463(5) -0.0755(2) -0.0182(2) 0.0467(14) Uani 1 1 d . . . H65A H 0.277(4) -0.1118(19) -0.0127(15) 0.023(12) Uiso 1 1 d . . . C66 C 0.3008(5) -0.0235(2) 0.0047(2) 0.0405(12) Uani 1 1 d . . . H66A H 0.374(3) -0.0257(16) 0.0256(13) 0.007(9) Uiso 1 1 d . . . C67 C 0.1526(4) 0.0406(2) -0.03140(17) 0.0309(10) Uani 1 1 d . . . C68 C 0.1027(4) 0.1023(2) -0.03639(17) 0.0324(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02943(14) 0.02473(13) 0.03192(14) 0.00018(11) 0.00271(10) -0.00423(11) Zn1 0.0347(3) 0.0293(3) 0.0383(3) 0.0013(2) 0.0038(3) -0.0060(2) Zn2 0.0329(3) 0.0318(3) 0.0355(3) -0.0003(2) -0.0013(2) -0.0016(2) N1 0.042(2) 0.032(2) 0.041(2) 0.0032(19) 0.003(2) -0.0024(19) N2 0.033(2) 0.029(2) 0.040(2) 0.0001(18) 0.0044(19) -0.0046(17) N3 0.031(2) 0.033(2) 0.040(2) 0.0013(18) 0.0016(18) -0.0015(18) N4 0.034(2) 0.030(2) 0.036(2) -0.0003(18) 0.0013(18) 0.0017(17) O1 0.041(2) 0.044(2) 0.051(2) 0.0182(18) -0.0014(17) -0.0044(16) O2 0.046(2) 0.037(2) 0.046(2) 0.0044(16) -0.0051(17) -0.0111(16) O3 0.045(2) 0.041(2) 0.046(2) -0.0024(17) 0.0127(17) -0.0051(17) O4 0.070(3) 0.029(2) 0.055(2) -0.0046(17) 0.018(2) -0.0024(17) O5 0.0255(17) 0.0303(18) 0.051(2) 0.0014(15) 0.0048(15) -0.0034(14) O6 0.049(2) 0.053(2) 0.077(3) 0.007(2) 0.023(2) -0.0122(19) O7 0.044(2) 0.071(3) 0.047(2) -0.0002(19) -0.0080(18) -0.0123(19) O8 0.054(2) 0.052(2) 0.041(2) 0.0079(17) 0.0094(18) -0.0087(18) O9 0.044(2) 0.057(2) 0.046(2) 0.0073(18) -0.0007(17) -0.0102(19) O10 0.064(3) 0.043(2) 0.038(2) -0.0064(17) 0.0094(18) -0.0037(18) O11 0.0285(18) 0.057(2) 0.043(2) 0.0056(17) 0.0053(16) -0.0098(16) O12 0.043(2) 0.041(2) 0.043(2) -0.0049(16) 0.0083(17) -0.0029(16) O13 0.063(2) 0.029(2) 0.048(2) 0.0036(16) -0.0013(18) 0.0065(17) O14 0.0369(19) 0.040(2) 0.044(2) 0.0043(16) -0.0074(16) 0.0018(15) C1 0.029(3) 0.034(3) 0.042(3) 0.000(2) 0.000(2) 0.006(2) C2 0.031(3) 0.029(3) 0.039(3) 0.002(2) 0.003(2) 0.003(2) C3 0.059(4) 0.043(3) 0.051(3) 0.014(3) -0.011(3) -0.016(3) C4 0.057(4) 0.052(4) 0.067(4) 0.001(3) -0.015(3) -0.023(3) C5 0.049(3) 0.051(3) 0.041(3) -0.004(3) 0.000(3) 0.008(3) C6 0.059(4) 0.034(3) 0.040(3) 0.008(3) 0.004(3) 0.003(3) C7 0.048(3) 0.032(3) 0.045(3) 0.001(2) 0.001(3) -0.002(2) C8 0.078(5) 0.072(5) 0.056(4) -0.005(3) -0.016(3) 0.008(4) C9 0.035(3) 0.033(3) 0.037(3) -0.005(2) -0.001(2) 0.003(2) C10 0.030(3) 0.038(3) 0.043(3) -0.003(2) -0.001(2) 0.003(2) C11 0.050(4) 0.050(4) 0.051(4) -0.005(3) 0.006(3) -0.010(3) C12 0.053(4) 0.075(5) 0.048(4) -0.014(3) 0.015(3) -0.011(3) C13 0.040(3) 0.084(5) 0.046(4) -0.026(3) 0.005(3) -0.008(3) C14 0.066(4) 0.043(4) 0.073(4) -0.027(3) 0.012(3) 0.001(3) C15 0.057(4) 0.038(3) 0.054(4) -0.005(3) 0.011(3) -0.005(3) C16 0.071(5) 0.129(7) 0.082(5) -0.058(5) 0.017(4) 0.003(5) C17 0.034(3) 0.039(3) 0.041(3) -0.007(2) -0.003(2) -0.002(2) C18 0.048(3) 0.045(3) 0.081(4) -0.001(3) -0.001(3) 0.013(3) C19 0.030(3) 0.029(2) 0.030(3) 0.006(2) 0.001(2) -0.006(2) C20 0.039(3) 0.042(3) 0.014(2) -0.0048(19) -0.0009(19) -0.008(2) C21 0.035(3) 0.037(3) 0.037(3) 0.001(2) -0.001(2) 0.005(2) C22 0.034(3) 0.039(3) 0.028(3) 0.004(2) 0.005(2) 0.003(2) C23 0.050(4) 0.047(3) 0.047(3) 0.003(3) -0.002(3) -0.010(3) C24 0.065(4) 0.066(4) 0.039(3) -0.006(3) 0.003(3) 0.000(3) C25 0.038(3) 0.061(4) 0.045(3) 0.012(3) 0.004(3) 0.002(3) C26 0.050(4) 0.041(3) 0.055(4) 0.004(3) 0.013(3) -0.001(3) C27 0.044(3) 0.041(3) 0.040(3) -0.002(3) 0.009(2) 0.001(2) C28 0.076(5) 0.098(6) 0.065(4) 0.017(4) 0.023(4) -0.006(4) C29 0.025(3) 0.044(3) 0.041(3) 0.004(2) -0.003(2) -0.005(2) C30 0.027(3) 0.041(3) 0.037(3) -0.006(2) 0.000(2) 0.000(2) C31 0.044(3) 0.037(3) 0.055(4) -0.004(3) 0.016(3) -0.011(3) C32 0.045(3) 0.054(4) 0.056(4) -0.004(3) 0.016(3) -0.012(3) C33 0.034(3) 0.052(4) 0.049(3) -0.007(3) 0.000(2) 0.000(3) C34 0.048(4) 0.042(3) 0.067(4) -0.011(3) 0.001(3) -0.003(3) C35 0.035(3) 0.044(3) 0.059(4) -0.004(3) 0.009(3) -0.012(3) C36 0.050(4) 0.079(5) 0.072(5) -0.029(4) 0.016(4) -0.001(4) C37 0.041(3) 0.028(3) 0.032(3) 0.005(2) 0.009(2) -0.003(2) C38 0.038(3) 0.031(3) 0.031(3) 0.004(2) 0.002(2) 0.002(2) C39 0.053(4) 0.040(3) 0.044(3) -0.004(3) -0.013(3) -0.002(3) C40 0.053(4) 0.075(5) 0.051(4) 0.004(3) -0.013(3) -0.003(3) C41 0.047(3) 0.058(4) 0.043(3) 0.017(3) 0.005(3) 0.007(3) C42 0.058(4) 0.029(3) 0.058(4) 0.013(3) 0.004(3) 0.002(3) C43 0.036(3) 0.035(3) 0.047(3) 0.005(2) -0.001(3) -0.003(2) C44 0.068(4) 0.084(5) 0.076(4) 0.025(4) -0.010(4) 0.031(4) C45 0.054(4) 0.049(4) 0.047(3) 0.002(3) 0.004(3) -0.009(3) C46 0.068(4) 0.061(4) 0.041(3) 0.004(3) -0.010(3) 0.003(3) C47 0.047(4) 0.058(4) 0.069(4) -0.003(3) -0.020(3) -0.001(3) C48 0.040(3) 0.038(3) 0.049(3) -0.001(2) -0.006(3) 0.000(2) C49 0.039(3) 0.050(4) 0.068(4) -0.006(3) -0.008(3) -0.010(3) C50 0.037(3) 0.041(3) 0.079(5) 0.005(3) 0.005(3) -0.014(3) C51 0.027(3) 0.036(3) 0.051(3) -0.001(2) 0.009(2) -0.006(2) C52 0.045(3) 0.032(3) 0.061(4) 0.011(3) 0.010(3) -0.002(2) C53 0.057(4) 0.048(3) 0.042(3) 0.013(3) 0.002(3) -0.008(3) C54 0.038(3) 0.038(3) 0.042(3) 0.000(2) 0.000(2) -0.005(2) C55 0.032(3) 0.030(3) 0.040(3) -0.004(2) 0.005(2) 0.000(2) C56 0.031(3) 0.030(3) 0.045(3) -0.002(2) 0.004(2) 0.001(2) C57 0.049(4) 0.030(3) 0.062(4) -0.005(3) -0.007(3) -0.001(3) C58 0.061(4) 0.036(3) 0.080(5) 0.008(3) -0.010(3) 0.014(3) C59 0.044(4) 0.061(4) 0.063(4) 0.008(3) -0.010(3) 0.012(3) C60 0.032(3) 0.051(3) 0.039(3) 0.009(2) -0.004(2) 0.000(2) C61 0.037(3) 0.061(4) 0.053(4) 0.000(3) -0.011(3) 0.002(3) C62 0.047(4) 0.053(4) 0.048(3) -0.014(3) 0.002(3) -0.014(3) C63 0.034(3) 0.034(3) 0.041(3) -0.002(2) 0.006(2) -0.008(2) C64 0.053(4) 0.036(3) 0.047(3) -0.008(3) 0.011(3) -0.014(3) C65 0.053(4) 0.025(3) 0.062(4) 0.000(3) 0.002(3) 0.006(3) C66 0.038(3) 0.036(3) 0.047(3) 0.004(2) 0.002(3) 0.002(2) C67 0.026(2) 0.034(3) 0.033(3) 0.000(2) 0.006(2) -0.002(2) C68 0.026(2) 0.034(3) 0.037(3) 0.003(2) 0.007(2) -0.001(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 Pr1 O10 2.379(3) . ? Pr1 O11 2.390(3) . ? Pr1 O4 2.402(3) . ? Pr1 O13 2.429(3) . ? Pr1 O1 2.438(3) . ? Pr1 O5 2.470(3) . ? Pr1 O7 2.546(3) . ? Pr1 O8 2.591(3) . ? Pr1 C19 2.990(5) . ? Zn1 O2 2.012(3) . ? Zn1 O3 2.029(3) . ? Zn1 O5 2.047(3) . ? Zn1 N2 2.122(4) . ? Zn1 N1 2.183(4) . ? Zn2 O14 2.014(3) . ? Zn2 O9 2.052(3) . ? Zn2 N4 2.112(4) . ? Zn2 O12 2.128(3) . ? Zn2 N3 2.199(4) . ? N1 C45 1.332(6) . ? N1 C56 1.352(6) . ? N2 C54 1.323(6) . ? N2 C55 1.361(6) . ? N3 C57 1.325(6) . ? N3 C68 1.362(6) . ? N4 C66 1.315(6) . ? N4 C67 1.359(5) . ? O1 C1 1.241(5) . ? O2 C1 1.269(5) . ? O3 C9 1.263(5) . ? O4 C9 1.249(5) . ? O5 C17 1.305(5) . ? O6 C17 1.215(6) . ? O7 C19 1.276(5) . ? O8 C19 1.256(5) . ? O9 C21 1.242(5) . ? O10 C21 1.256(5) . ? O11 C29 1.272(5) . ? O12 C29 1.256(5) . ? O13 C37 1.253(5) . ? O14 C37 1.268(5) . ? C1 C2 1.499(6) . ? C2 C7 1.375(6) . ? C2 C3 1.378(7) . ? C3 C4 1.378(7) . ? C4 C5 1.381(7) . ? C5 C6 1.379(7) . ? C5 C8 1.511(7) . ? C6 C7 1.388(7) . ? C9 C10 1.495(6) . ? C10 C15 1.384(7) . ? C10 C11 1.400(7) . ? C11 C12 1.385(8) . ? C12 C13 1.364(8) . ? C13 C14 1.364(8) . ? C13 C16 1.509(7) . ? C14 C15 1.382(7) . ? C17 C18 1.499(7) . ? C19 C20 1.176(5) . ? C21 C22 1.497(6) . ? C22 C23 1.364(7) . ? C22 C27 1.401(7) . ? C23 C24 1.390(7) . ? C24 C25 1.374(8) . ? C25 C26 1.391(7) . ? C25 C28 1.504(7) . ? C26 C27 1.387(7) . ? C29 C30 1.492(6) . ? C30 C35 1.378(7) . ? C30 C31 1.383(7) . ? C31 C32 1.377(7) . ? C32 C33 1.386(7) . ? C33 C34 1.391(7) . ? C33 C36 1.519(8) . ? C34 C35 1.392(7) . ? C37 C38 1.503(6) . ? C38 C39 1.381(7) . ? C38 C43 1.382(6) . ? C39 C40 1.383(8) . ? C40 C41 1.389(8) . ? C41 C42 1.381(8) . ? C41 C44 1.499(7) . ? C42 C43 1.373(7) . ? C45 C46 1.383(8) . ? C46 C47 1.352(8) . ? C47 C48 1.406(7) . ? C48 C56 1.410(6) . ? C48 C49 1.422(7) . ? C49 C50 1.332(8) . ? C50 C51 1.429(7) . ? C51 C52 1.400(7) . ? C51 C55 1.400(6) . ? C52 C53 1.352(7) . ? C53 C54 1.403(7) . ? C55 C56 1.432(6) . ? C57 C58 1.375(8) . ? C58 C59 1.362(8) . ? C59 C60 1.398(7) . ? C60 C68 1.403(6) . ? C60 C61 1.432(7) . ? C61 C62 1.324(8) . ? C62 C63 1.424(7) . ? C63 C64 1.395(7) . ? C63 C67 1.408(6) . ? C64 C65 1.364(7) . ? C65 C66 1.392(7) . ? C67 C68 1.434(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Pr1 O11 87.94(12) . . ? O10 Pr1 O4 145.24(12) . . ? O11 Pr1 O4 98.97(12) . . ? O10 Pr1 O13 71.97(11) . . ? O11 Pr1 O13 80.03(12) . . ? O4 Pr1 O13 142.72(11) . . ? O10 Pr1 O1 72.00(12) . . ? O11 Pr1 O1 80.36(11) . . ? O4 Pr1 O1 75.65(12) . . ? O13 Pr1 O1 139.29(11) . . ? O10 Pr1 O5 80.72(11) . . ? O11 Pr1 O5 156.58(11) . . ? O4 Pr1 O5 79.80(11) . . ? O13 Pr1 O5 115.13(11) . . ? O1 Pr1 O5 76.68(11) . . ? O10 Pr1 O7 126.70(12) . . ? O11 Pr1 O7 129.36(11) . . ? O4 Pr1 O7 73.67(12) . . ? O13 Pr1 O7 78.47(12) . . ? O1 Pr1 O7 139.94(11) . . ? O5 Pr1 O7 73.09(11) . . ? O10 Pr1 O8 144.39(11) . . ? O11 Pr1 O8 80.52(11) . . ? O4 Pr1 O8 70.24(11) . . ? O13 Pr1 O8 72.89(11) . . ? O1 Pr1 O8 137.38(12) . . ? O5 Pr1 O8 120.05(11) . . ? O7 Pr1 O8 49.41(12) . . ? O10 Pr1 C19 143.62(12) . . ? O11 Pr1 C19 105.21(12) . . ? O4 Pr1 C19 67.18(12) . . ? O13 Pr1 C19 77.06(11) . . ? O1 Pr1 C19 142.83(12) . . ? O5 Pr1 C19 95.91(12) . . ? O7 Pr1 C19 25.03(11) . . ? O8 Pr1 C19 24.70(11) . . ? O2 Zn1 O3 100.38(14) . . ? O2 Zn1 O5 97.26(13) . . ? O3 Zn1 O5 111.17(13) . . ? O2 Zn1 N2 90.39(14) . . ? O3 Zn1 N2 111.17(14) . . ? O5 Zn1 N2 134.68(13) . . ? O2 Zn1 N1 166.95(14) . . ? O3 Zn1 N1 87.27(14) . . ? O5 Zn1 N1 89.67(13) . . ? N2 Zn1 N1 76.94(15) . . ? O14 Zn2 O9 98.69(13) . . ? O14 Zn2 N4 94.67(14) . . ? O9 Zn2 N4 98.87(14) . . ? O14 Zn2 O12 92.46(13) . . ? O9 Zn2 O12 157.37(14) . . ? N4 Zn2 O12 99.78(13) . . ? O14 Zn2 N3 170.40(13) . . ? O9 Zn2 N3 88.24(14) . . ? N4 Zn2 N3 77.61(14) . . ? O12 Zn2 N3 83.36(13) . . ? C45 N1 C56 117.7(5) . . ? C45 N1 Zn1 128.9(4) . . ? C56 N1 Zn1 113.3(3) . . ? C54 N2 C55 118.4(4) . . ? C54 N2 Zn1 126.5(3) . . ? C55 N2 Zn1 115.1(3) . . ? C57 N3 C68 117.3(4) . . ? C57 N3 Zn2 130.9(4) . . ? C68 N3 Zn2 111.8(3) . . ? C66 N4 C67 118.3(4) . . ? C66 N4 Zn2 126.7(3) . . ? C67 N4 Zn2 114.9(3) . . ? C1 O1 Pr1 145.5(3) . . ? C1 O2 Zn1 126.7(3) . . ? C9 O3 Zn1 123.8(3) . . ? C9 O4 Pr1 151.9(3) . . ? C17 O5 Zn1 111.7(3) . . ? C17 O5 Pr1 132.0(3) . . ? Zn1 O5 Pr1 114.96(13) . . ? C19 O7 Pr1 97.4(3) . . ? C19 O8 Pr1 95.8(3) . . ? C21 O9 Zn2 122.5(3) . . ? C21 O10 Pr1 145.8(3) . . ? C29 O11 Pr1 140.1(3) . . ? C29 O12 Zn2 102.8(3) . . ? C37 O13 Pr1 147.1(3) . . ? C37 O14 Zn2 129.1(3) . . ? O1 C1 O2 125.1(4) . . ? O1 C1 C2 118.6(4) . . ? O2 C1 C2 116.4(4) . . ? C7 C2 C3 117.6(5) . . ? C7 C2 C1 121.8(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 121.0(5) . . ? C3 C4 C5 121.8(5) . . ? C6 C5 C4 116.9(5) . . ? C6 C5 C8 121.3(5) . . ? C4 C5 C8 121.8(5) . . ? C5 C6 C7 121.3(5) . . ? C2 C7 C6 121.2(5) . . ? O4 C9 O3 124.5(4) . . ? O4 C9 C10 118.4(4) . . ? O3 C9 C10 117.2(4) . . ? C15 C10 C11 117.6(5) . . ? C15 C10 C9 122.4(5) . . ? C11 C10 C9 119.8(5) . . ? C12 C11 C10 119.7(6) . . ? C13 C12 C11 122.1(6) . . ? C14 C13 C12 118.2(5) . . ? C14 C13 C16 120.6(6) . . ? C12 C13 C16 121.2(6) . . ? C13 C14 C15 121.4(6) . . ? C14 C15 C10 120.9(6) . . ? O6 C17 O5 122.4(5) . . ? O6 C17 C18 122.6(5) . . ? O5 C17 C18 115.1(4) . . ? C20 C19 O8 122.3(5) . . ? C20 C19 O7 121.6(5) . . ? O8 C19 O7 116.0(4) . . ? C20 C19 Pr1 169.1(4) . . ? O8 C19 Pr1 59.5(2) . . ? O7 C19 Pr1 57.6(2) . . ? O9 C21 O10 124.3(5) . . ? O9 C21 C22 119.1(4) . . ? O10 C21 C22 116.7(4) . . ? C23 C22 C27 118.7(5) . . ? C23 C22 C21 122.5(5) . . ? C27 C22 C21 118.8(4) . . ? C22 C23 C24 120.1(5) . . ? C25 C24 C23 122.5(5) . . ? C24 C25 C26 117.3(5) . . ? C24 C25 C28 121.7(5) . . ? C26 C25 C28 121.0(5) . . ? C27 C26 C25 120.9(5) . . ? C26 C27 C22 120.5(5) . . ? O12 C29 O11 120.8(5) . . ? O12 C29 C30 120.0(4) . . ? O11 C29 C30 119.2(5) . . ? C35 C30 C31 118.9(5) . . ? C35 C30 C29 120.5(4) . . ? C31 C30 C29 120.6(5) . . ? C32 C31 C30 120.7(5) . . ? C31 C32 C33 121.4(5) . . ? C32 C33 C34 117.7(5) . . ? C32 C33 C36 120.8(5) . . ? C34 C33 C36 121.5(6) . . ? C33 C34 C35 121.0(5) . . ? C30 C35 C34 120.4(5) . . ? O13 C37 O14 125.4(4) . . ? O13 C37 C38 118.1(4) . . ? O14 C37 C38 116.5(4) . . ? C39 C38 C43 117.8(5) . . ? C39 C38 C37 120.3(4) . . ? C43 C38 C37 121.9(4) . . ? C38 C39 C40 120.8(6) . . ? C39 C40 C41 121.4(6) . . ? C42 C41 C40 117.2(5) . . ? C42 C41 C44 122.0(6) . . ? C40 C41 C44 120.8(6) . . ? C43 C42 C41 121.5(5) . . ? C42 C43 C38 121.3(5) . . ? N1 C45 C46 123.2(6) . . ? C47 C46 C45 119.2(6) . . ? C46 C47 C48 120.4(5) . . ? C47 C48 C56 116.3(5) . . ? C47 C48 C49 124.8(5) . . ? C56 C48 C49 118.9(5) . . ? C50 C49 C48 121.0(5) . . ? C49 C50 C51 122.4(5) . . ? C52 C51 C55 117.6(5) . . ? C52 C51 C50 124.3(5) . . ? C55 C51 C50 118.1(5) . . ? C53 C52 C51 119.2(5) . . ? C52 C53 C54 120.3(5) . . ? N2 C54 C53 121.7(5) . . ? N2 C55 C51 122.6(4) . . ? N2 C55 C56 117.3(4) . . ? C51 C55 C56 120.1(4) . . ? N1 C56 C48 123.0(4) . . ? N1 C56 C55 117.4(4) . . ? C48 C56 C55 119.6(4) . . ? N3 C57 C58 124.2(6) . . ? C59 C58 C57 118.9(6) . . ? C58 C59 C60 119.8(5) . . ? C59 C60 C68 117.5(5) . . ? C59 C60 C61 123.5(5) . . ? C68 C60 C61 118.9(5) . . ? C62 C61 C60 121.0(5) . . ? C61 C62 C63 122.2(5) . . ? C64 C63 C67 116.6(5) . . ? C64 C63 C62 124.7(5) . . ? C67 C63 C62 118.7(5) . . ? C65 C64 C63 120.1(5) . . ? C64 C65 C66 119.5(5) . . ? N4 C66 C65 122.6(5) . . ? N4 C67 C63 122.9(4) . . ? N4 C67 C68 117.7(4) . . ? C63 C67 C68 119.4(4) . . ? N3 C68 C60 122.4(4) . . ? N3 C68 C67 117.9(4) . . ? C60 C68 C67 119.7(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.748 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.104