data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'J Lewinski' _publ_contact_author_email LEWIN@CH.PW.EDU.PL _publ_section_title ; Oxygenation of Alkylzinc Complexes with Pyrrolylketiminate Ligand: Access to Alkylperoxide versus Oxo-Encapsulated Complexes ; loop_ _publ_author_name 'J Lewinski' 'Michal Galezowski' 'Daniel T Gryko' 'Iwona Justyniak' 'Tomasz Kaczorowski' ; J.Lipkowski ; 'Karolina Suwala' # Attachment 'comp2_CCDC_696853.cif' #====================================================== data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 696853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C24 H36 N4 Zn2' _chemical_formula_weight 511.31 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3637(2) _cell_length_b 8.7342(3) _cell_length_c 9.4312(3) _cell_angle_alpha 105.1357(11) _cell_angle_beta 104.473(2) _cell_angle_gamma 104.829(2) _cell_volume 604.73(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20419 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 2.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_measurement_details ; 453 frames, \w rotation 0.8\% per frame (34s per frame) 130 frames, \w rotation 0.8\% per frame (34s per frame) 68 frames, \w rotation 0.8\% per frame (34s per frame) 36 frames, \w rotation 0.8\% per frame (34s per frame) 32 frames, \w rotation 0.8\% per frame (34s per frame) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5115 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.56 _reflns_number_total 2775 _reflns_number_gt 2631 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _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^)+(0.0000P)^2^+0.7260P] 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 2775 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1008(2) 0.3809(2) 0.7411(2) 0.0156(3) Uani 1 1 d . . . C2 C 1.1856(3) 0.4615(3) 0.6399(3) 0.0264(4) Uani 1 1 d . . . C3 C 1.2403(3) 0.4309(3) 0.9001(3) 0.0278(5) Uani 1 1 d . . . C4 C 0.9557(3) 0.4517(2) 0.7638(3) 0.0214(4) Uani 1 1 d . . . C5 C 0.7598(2) 0.0239(2) 0.2611(2) 0.0165(3) Uani 1 1 d . . . H5 H 0.8334 0.0925 0.2229 0.020 Uiso 1 1 calc R . . C6 C 0.5838(2) -0.0699(2) 0.1804(2) 0.0178(4) Uani 1 1 d . . . H6 H 0.5173 -0.0783 0.0792 0.021 Uiso 1 1 calc R . . C7 C 0.5221(2) -0.1505(2) 0.2777(2) 0.0164(3) Uani 1 1 d . . . H7 H 0.4061 -0.2234 0.2552 0.020 Uiso 1 1 calc R . . C8 C 0.6643(2) -0.1024(2) 0.4124(2) 0.0131(3) Uani 1 1 d . . . C9 C 0.6768(2) -0.1329(2) 0.5563(2) 0.0126(3) Uani 1 1 d . . . C10 C 0.5356(2) -0.2515(2) 0.5874(2) 0.0151(3) Uani 1 1 d . . . H10A H 0.4859 -0.3645 0.5048 0.018 Uiso 1 1 calc R . . H10B H 0.4397 -0.2065 0.5956 0.018 Uiso 1 1 calc R . . C11 C 0.6372(2) -0.2577(2) 0.7448(2) 0.0191(4) Uani 1 1 d . . . H11A H 0.5660 -0.2570 0.8143 0.023 Uiso 1 1 calc R . . H11B H 0.6711 -0.3599 0.7297 0.023 Uiso 1 1 calc R . . C12 C 0.8004(2) -0.0967(2) 0.8123(2) 0.0181(4) Uani 1 1 d . . . H12A H 0.7833 -0.0054 0.8882 0.022 Uiso 1 1 calc R . . H12B H 0.9057 -0.1187 0.8655 0.022 Uiso 1 1 calc R . . N1 N 0.81440(19) 0.00490(18) 0.40368(17) 0.0142(3) Uani 1 1 d . . . N2 N 0.82010(19) -0.04981(18) 0.67620(17) 0.0144(3) Uani 1 1 d . . . Zn1 Zn 0.99511(3) 0.13174(2) 0.63455(2) 0.01422(7) Uani 1 1 d . . . H2A H 1.224(3) 0.587(3) 0.685(3) 0.040(7) Uiso 1 1 d . . . H2B H 1.106(3) 0.427(3) 0.532(3) 0.029(6) Uiso 1 1 d . . . H2C H 1.290(3) 0.430(3) 0.633(3) 0.040(7) Uiso 1 1 d . . . H3A H 1.288(3) 0.555(3) 0.951(3) 0.032(6) Uiso 1 1 d . . . H3B H 1.338(3) 0.394(3) 0.893(3) 0.032(6) Uiso 1 1 d . . . H3C H 1.190(3) 0.380(3) 0.968(3) 0.042(7) Uiso 1 1 d . . . H4A H 1.002(3) 0.572(3) 0.809(3) 0.028(6) Uiso 1 1 d . . . H4B H 0.903(3) 0.413(3) 0.836(3) 0.029(6) Uiso 1 1 d . . . H4C H 0.864(3) 0.425(3) 0.666(3) 0.022(6) Uiso 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 C1 0.0139(8) 0.0115(8) 0.0190(9) 0.0029(7) 0.0057(7) 0.0029(6) C2 0.0276(10) 0.0174(10) 0.0436(13) 0.0152(9) 0.0221(10) 0.0083(8) C3 0.0215(10) 0.0250(11) 0.0235(10) -0.0049(9) -0.0010(8) 0.0085(8) C4 0.0192(9) 0.0172(9) 0.0276(10) 0.0054(8) 0.0098(8) 0.0063(7) C5 0.0218(9) 0.0155(8) 0.0167(9) 0.0083(7) 0.0093(7) 0.0084(7) C6 0.0186(8) 0.0206(9) 0.0153(9) 0.0077(7) 0.0042(7) 0.0084(7) C7 0.0147(8) 0.0167(8) 0.0169(9) 0.0055(7) 0.0040(7) 0.0054(7) C8 0.0133(7) 0.0107(8) 0.0153(8) 0.0037(6) 0.0062(6) 0.0038(6) C9 0.0126(7) 0.0104(8) 0.0146(8) 0.0030(6) 0.0059(6) 0.0038(6) C10 0.0153(8) 0.0138(8) 0.0154(8) 0.0047(7) 0.0066(7) 0.0026(6) C11 0.0184(8) 0.0200(9) 0.0175(9) 0.0086(7) 0.0063(7) 0.0019(7) C12 0.0173(8) 0.0214(9) 0.0134(8) 0.0065(7) 0.0053(7) 0.0028(7) N1 0.0142(7) 0.0131(7) 0.0143(7) 0.0046(6) 0.0056(6) 0.0025(6) N2 0.0154(7) 0.0144(7) 0.0124(7) 0.0043(6) 0.0053(6) 0.0032(6) Zn1 0.01312(10) 0.01133(10) 0.01462(11) 0.00199(8) 0.00508(8) 0.00065(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.525(3) . ? C1 C2 1.530(3) . ? C1 C4 1.531(2) . ? C1 Zn1 1.9893(17) . ? C2 H2A 1.00(3) . ? C2 H2B 0.98(2) . ? C2 H2C 1.00(3) . ? C3 H3A 0.99(3) . ? C3 H3B 0.96(2) . ? C3 H3C 0.99(3) . ? C4 H4A 0.95(2) . ? C4 H4B 0.98(2) . ? C4 H4C 0.97(2) . ? C5 N1 1.376(2) . ? C5 C6 1.384(2) . ? C5 H5 0.9500 . ? C6 C7 1.412(2) . ? C6 H6 0.9500 . ? C7 C8 1.383(2) . ? C7 H7 0.9500 . ? C8 N1 1.397(2) . ? C8 C9 1.434(2) . ? C9 N2 1.300(2) . ? C9 C10 1.503(2) . ? C10 C11 1.538(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.537(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.480(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N1 Zn1 2.1192(15) . ? N1 Zn1 2.2645(14) 2_756 ? N2 Zn1 2.0580(14) . ? Zn1 N1 2.2645(15) 2_756 ? Zn1 Zn1 2.9822(4) 2_756 ? 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 C3 C1 C2 108.46(17) . . ? C3 C1 C4 108.71(16) . . ? C2 C1 C4 108.36(15) . . ? C3 C1 Zn1 112.24(13) . . ? C2 C1 Zn1 109.88(13) . . ? C4 C1 Zn1 109.11(12) . . ? C1 C2 H2A 110.5(15) . . ? C1 C2 H2B 113.3(14) . . ? H2A C2 H2B 107(2) . . ? C1 C2 H2C 111.0(15) . . ? H2A C2 H2C 108(2) . . ? H2B C2 H2C 107(2) . . ? C1 C3 H3A 110.2(14) . . ? C1 C3 H3B 112.8(15) . . ? H3A C3 H3B 107(2) . . ? C1 C3 H3C 110.3(16) . . ? H3A C3 H3C 109(2) . . ? H3B C3 H3C 107(2) . . ? C1 C4 H4A 110.8(14) . . ? C1 C4 H4B 112.5(14) . . ? H4A C4 H4B 105.6(19) . . ? C1 C4 H4C 112.3(13) . . ? H4A C4 H4C 105.8(19) . . ? H4B C4 H4C 109.5(19) . . ? N1 C5 C6 111.26(15) . . ? N1 C5 H5 124.4 . . ? C6 C5 H5 124.4 . . ? C5 C6 C7 106.66(16) . . ? C5 C6 H6 126.7 . . ? C7 C6 H6 126.7 . . ? C8 C7 C6 106.36(15) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 N1 110.82(15) . . ? C7 C8 C9 131.29(16) . . ? N1 C8 C9 117.68(15) . . ? N2 C9 C8 119.38(15) . . ? N2 C9 C10 114.25(15) . . ? C8 C9 C10 126.35(15) . . ? C9 C10 C11 101.95(14) . . ? C9 C10 H10A 111.4 . . ? C11 C10 H10A 111.4 . . ? C9 C10 H10B 111.4 . . ? C11 C10 H10B 111.4 . . ? H10A C10 H10B 109.2 . . ? C12 C11 C10 103.80(14) . . ? C12 C11 H11A 111.0 . . ? C10 C11 H11A 111.0 . . ? C12 C11 H11B 111.0 . . ? C10 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? N2 C12 C11 105.19(14) . . ? N2 C12 H12A 110.7 . . ? C11 C12 H12A 110.7 . . ? N2 C12 H12B 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C5 N1 C8 104.89(14) . . ? C5 N1 Zn1 142.67(12) . . ? C8 N1 Zn1 107.24(11) . . ? C5 N1 Zn1 100.29(10) . 2_756 ? C8 N1 Zn1 110.78(10) . 2_756 ? Zn1 N1 Zn1 85.66(5) . 2_756 ? C9 N2 C12 109.84(14) . . ? C9 N2 Zn1 112.25(11) . . ? C12 N2 Zn1 137.19(11) . . ? C1 Zn1 N2 131.31(6) . . ? C1 Zn1 N1 125.59(7) . . ? N2 Zn1 N1 81.44(6) . . ? C1 Zn1 N1 115.96(6) . 2_756 ? N2 Zn1 N1 98.61(5) . 2_756 ? N1 Zn1 N1 94.34(5) . 2_756 ? C1 Zn1 Zn1 138.24(5) . 2_756 ? N2 Zn1 Zn1 90.45(4) . 2_756 ? N1 Zn1 Zn1 49.22(4) . 2_756 ? N1 Zn1 Zn1 45.12(4) 2_756 2_756 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.409 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.063 # Attachment 'comp3_CCDC_696854.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 696854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H62 N8 O4 Zn3' _chemical_formula_weight 999.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6481(3) _cell_length_b 18.5359(3) _cell_length_c 18.7841(4) _cell_angle_alpha 92.2702(10) _cell_angle_beta 98.1488(10) _cell_angle_gamma 94.0181(10) _cell_volume 5029.93(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27823 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 24.713 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_measurement_details ; 226 frames, \w rotation 1.6\% per frame (50s per frame) 34 frames, \w rotation 1.6\% per frame (50s per frame) 16 frames, \w rotation 1.6\% per frame (50s per frame) 21 frames, \w rotation 1.6\% per frame (50s per frame) 35 frames, \w rotation 1.6\% per frame (50s per frame) 52 frames, \w rotation 1.6\% per frame (50s per frame) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25362 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 22.72 _reflns_number_total 13525 _reflns_number_gt 10061 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _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^)+(0.0654P)^2^+22.8437P] 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 13525 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2369(4) 0.4228(3) 0.1136(3) 0.0443(18) Uani 1 1 d D . . C5 C 0.4508(4) 0.6192(3) 0.3007(4) 0.0358(16) Uani 1 1 d . . . C6 C 0.4771(4) 0.5419(3) 0.2871(4) 0.0407(17) Uani 1 1 d . . . H6A H 0.4795 0.5161 0.3318 0.061 Uiso 1 1 calc R . . H6B H 0.5379 0.5435 0.2709 0.061 Uiso 1 1 calc R . . H6C H 0.4308 0.5167 0.2500 0.061 Uiso 1 1 calc R . . C7 C 0.4419(5) 0.6598(4) 0.2302(4) 0.0461(19) Uani 1 1 d . . . H7A H 0.4013 0.6304 0.1924 0.069 Uiso 1 1 calc R . . H7B H 0.5032 0.6686 0.2156 0.069 Uiso 1 1 calc R . . H7C H 0.4156 0.7062 0.2380 0.069 Uiso 1 1 calc R . . C8 C 0.5164(5) 0.6598(4) 0.3608(4) 0.0470(18) Uani 1 1 d . . . H8A H 0.4931 0.7067 0.3715 0.071 Uiso 1 1 calc R . . H8B H 0.5777 0.6674 0.3460 0.071 Uiso 1 1 calc R . . H8C H 0.5208 0.6314 0.4040 0.071 Uiso 1 1 calc R . . C9 C 0.2686(5) 0.1807(4) 0.1965(4) 0.0464(19) Uani 1 1 d . . . H9 H 0.2110 0.1831 0.1666 0.056 Uiso 1 1 calc R . . C10 C 0.3233(6) 0.1228(4) 0.1966(4) 0.053(2) Uani 1 1 d . . . H10 H 0.3098 0.0791 0.1678 0.063 Uiso 1 1 calc R . . C11 C 0.4023(5) 0.1410(3) 0.2473(4) 0.0445(19) Uani 1 1 d . . . H11 H 0.4530 0.1123 0.2594 0.053 Uiso 1 1 calc R . . C12 C 0.3914(5) 0.2099(3) 0.2764(4) 0.0361(16) Uani 1 1 d . . . C13 C 0.4452(4) 0.2559(3) 0.3326(3) 0.0319(15) Uani 1 1 d . . . C14 C 0.5371(5) 0.2428(4) 0.3733(4) 0.0442(18) Uani 1 1 d . . . H14A H 0.5866 0.2480 0.3427 0.053 Uiso 1 1 calc R . . H14B H 0.5365 0.1941 0.3932 0.053 Uiso 1 1 calc R . . C15 C 0.5492(6) 0.3030(4) 0.4338(4) 0.059(2) Uani 1 1 d . . . H15A H 0.5359 0.2832 0.4797 0.071 Uiso 1 1 calc R . . H15B H 0.6129 0.3263 0.4409 0.071 Uiso 1 1 calc R . . C16 C 0.4792(4) 0.3569(4) 0.4072(4) 0.0382(16) Uani 1 1 d . . . H16A H 0.4470 0.3739 0.4470 0.046 Uiso 1 1 calc R . . H16B H 0.5103 0.3993 0.3877 0.046 Uiso 1 1 calc R . . C17 C 0.1006(5) 0.2750(4) 0.3190(5) 0.062(2) Uani 1 1 d . . . H17A H 0.0609 0.2942 0.2780 0.074 Uiso 1 1 calc R . . H17B H 0.1204 0.2276 0.3035 0.074 Uiso 1 1 calc R . . C18 C 0.0507(5) 0.2677(4) 0.3815(6) 0.074(3) Uani 1 1 d . . . H18A H 0.0591 0.2200 0.4025 0.089 Uiso 1 1 calc R . . H18B H -0.0163 0.2720 0.3669 0.089 Uiso 1 1 calc R . . C19 C 0.0911(5) 0.3285(4) 0.4362(5) 0.061(2) Uani 1 1 d . . . H19A H 0.0472 0.3664 0.4391 0.073 Uiso 1 1 calc R . . H19B H 0.1077 0.3099 0.4847 0.073 Uiso 1 1 calc R . . C20 C 0.1756(4) 0.3570(3) 0.4063(4) 0.0305(15) Uani 1 1 d . . . C21 C 0.2384(4) 0.4140(3) 0.4416(3) 0.0214(13) Uani 1 1 d . . . C22 C 0.2633(5) 0.4288(3) 0.5157(3) 0.0357(16) Uani 1 1 d . . . H22 H 0.2387 0.4042 0.5530 0.043 Uiso 1 1 calc R . . C23 C 0.3306(5) 0.4862(3) 0.5244(3) 0.0356(16) Uani 1 1 d . . . H23 H 0.3620 0.5077 0.5687 0.043 Uiso 1 1 calc R . . C24 C 0.3431(4) 0.5059(3) 0.4563(3) 0.0265(14) Uani 1 1 d . . . H24 H 0.3847 0.5448 0.4467 0.032 Uiso 1 1 calc R . . C25 C 0.0431(5) 0.4494(4) 0.2590(5) 0.060(2) Uani 1 1 d . . . H25 H 0.0548 0.4219 0.2179 0.071 Uiso 1 1 calc R . . C26 C -0.0363(6) 0.4436(4) 0.2851(6) 0.067(2) Uani 1 1 d . . . H26 H -0.0908 0.4149 0.2650 0.080 Uiso 1 1 calc R . . C27 C -0.0240(5) 0.4876(4) 0.3474(5) 0.060(3) Uani 1 1 d . . . H27 H -0.0671 0.4924 0.3803 0.072 Uiso 1 1 calc R . . C28 C 0.0659(4) 0.5245(3) 0.3529(4) 0.0339(15) Uani 1 1 d . . . C29 C 0.1114(5) 0.5800(4) 0.4021(3) 0.0404(18) Uani 1 1 d . . . C30 C 0.1005(7) 0.5828(5) 0.4800(4) 0.075(3) Uani 1 1 d . . . H30A H 0.0344 0.5801 0.4863 0.090 Uiso 1 1 calc R . . H30B H 0.1306 0.5428 0.5051 0.090 Uiso 1 1 calc R . . C31 C 0.1478(7) 0.6543(6) 0.5068(4) 0.089(4) Uani 1 1 d . . . H31A H 0.1852 0.6505 0.5545 0.107 Uiso 1 1 calc R . . H31B H 0.1020 0.6904 0.5112 0.107 Uiso 1 1 calc R . . C32 C 0.2110(6) 0.6766(5) 0.4500(5) 0.070(3) Uani 1 1 d . . . H32A H 0.2097 0.7289 0.4413 0.085 Uiso 1 1 calc R . . H32B H 0.2757 0.6654 0.4655 0.085 Uiso 1 1 calc R . . C33 C -0.0005(5) 0.6108(4) 0.1801(4) 0.0452(18) Uani 1 1 d . . . H33A H -0.0302 0.5865 0.2178 0.054 Uiso 1 1 calc R . . H33B H 0.0173 0.5735 0.1467 0.054 Uiso 1 1 calc R . . C34 C -0.0665(6) 0.6615(5) 0.1393(5) 0.071(3) Uani 1 1 d . . . H34A H -0.0899 0.6410 0.0901 0.085 Uiso 1 1 calc R . . H34B H -0.1197 0.6690 0.1651 0.085 Uiso 1 1 calc R . . C35 C -0.0085(6) 0.7317(5) 0.1367(4) 0.068(3) Uani 1 1 d . . . H35A H 0.0078 0.7382 0.0878 0.082 Uiso 1 1 calc R . . H35B H -0.0417 0.7735 0.1507 0.082 Uiso 1 1 calc R . . C36 C 0.0762(5) 0.7237(4) 0.1900(4) 0.050(2) Uani 1 1 d . . . C37 C 0.1489(5) 0.7767(4) 0.2156(5) 0.060(3) Uani 1 1 d . . . C38 C 0.1644(7) 0.8493(5) 0.2006(6) 0.089(4) Uani 1 1 d . . . H38 H 0.1252 0.8769 0.1695 0.106 Uiso 1 1 calc R . . C39 C 0.2487(8) 0.8726(5) 0.2405(8) 0.117(5) Uani 1 1 d . . . H39 H 0.2794 0.9196 0.2412 0.141 Uiso 1 1 calc R . . C40 C 0.2806(6) 0.8143(4) 0.2798(8) 0.112(5) Uani 1 1 d . . . H40 H 0.3364 0.8159 0.3126 0.134 Uiso 1 1 calc R . . C41 C -0.4428(4) 0.8908(3) 0.2145(3) 0.0298(14) Uani 1 1 d . . . C42 C -0.4322(5) 0.8525(4) 0.2846(4) 0.0421(17) Uani 1 1 d . . . H42A H -0.4065 0.8058 0.2773 0.063 Uiso 1 1 calc R . . H42B H -0.4929 0.8444 0.3005 0.063 Uiso 1 1 calc R . . H42C H -0.3905 0.8825 0.3214 0.063 Uiso 1 1 calc R . . C43 C -0.5114(5) 0.8488(4) 0.1562(4) 0.0415(17) Uani 1 1 d . . . H43A H -0.5124 0.8732 0.1107 0.062 Uiso 1 1 calc R . . H43B H -0.5733 0.8468 0.1705 0.062 Uiso 1 1 calc R . . H43C H -0.4927 0.7996 0.1499 0.062 Uiso 1 1 calc R . . C44 C -0.4695(4) 0.9684(3) 0.2235(4) 0.0355(16) Uani 1 1 d . . . H44A H -0.4228 0.9958 0.2587 0.053 Uiso 1 1 calc R . . H44B H -0.5298 0.9681 0.2404 0.053 Uiso 1 1 calc R . . H44C H -0.4732 0.9913 0.1771 0.053 Uiso 1 1 calc R . . C49 C -0.2695(5) 0.6937(4) 0.2438(5) 0.054(2) Uani 1 1 d . . . H49 H -0.3282 0.6899 0.2145 0.065 Uiso 1 1 calc R . . C50 C -0.2288(6) 0.6367(4) 0.2821(5) 0.059(2) Uani 1 1 d . . . H50 H -0.2544 0.5880 0.2812 0.071 Uiso 1 1 calc R . . C51 C -0.1461(5) 0.6640(4) 0.3206(4) 0.050(2) Uani 1 1 d . . . H51 H -0.1044 0.6394 0.3527 0.060 Uiso 1 1 calc R . . C52 C -0.1368(5) 0.7361(3) 0.3020(4) 0.0391(17) Uani 1 1 d . . . C53 C -0.0654(5) 0.7915(4) 0.3239(3) 0.0369(16) Uani 1 1 d . . . C54 C 0.0220(5) 0.7875(4) 0.3761(4) 0.0468(19) Uani 1 1 d . . . H54A H 0.0077 0.7796 0.4253 0.056 Uiso 1 1 calc R . . H54B H 0.0580 0.7477 0.3613 0.056 Uiso 1 1 calc R . . C55 C 0.0736(6) 0.8589(5) 0.3731(6) 0.085(3) Uani 1 1 d . . . H55A H 0.1311 0.8533 0.3522 0.102 Uiso 1 1 calc R . . H55B H 0.0899 0.8824 0.4220 0.102 Uiso 1 1 calc R . . C56 C 0.0088(4) 0.9040(4) 0.3256(4) 0.0402(17) Uani 1 1 d . . . H56A H -0.0097 0.9452 0.3541 0.048 Uiso 1 1 calc R . . H56B H 0.0394 0.9232 0.2858 0.048 Uiso 1 1 calc R . . C57 C -0.2341(5) 0.8085(4) 0.0679(3) 0.0456(19) Uani 1 1 d . . . H57A H -0.2338 0.7588 0.0853 0.055 Uiso 1 1 calc R . . H57B H -0.2989 0.8214 0.0573 0.055 Uiso 1 1 calc R . . C58 C -0.1872(6) 0.8140(4) 0.0028(4) 0.057(2) Uani 1 1 d . . . H58A H -0.2327 0.8085 -0.0417 0.069 Uiso 1 1 calc R . . H58B H -0.1425 0.7765 0.0013 0.069 Uiso 1 1 calc R . . C59 C -0.1382(5) 0.8890(4) 0.0112(4) 0.051(2) Uani 1 1 d . . . H59A H -0.1755 0.9242 -0.0159 0.061 Uiso 1 1 calc R . . H59B H -0.0770 0.8892 -0.0054 0.061 Uiso 1 1 calc R . . C60 C -0.1285(4) 0.9058(3) 0.0919(3) 0.0302(15) Uani 1 1 d . . . C61 C -0.0729(4) 0.9658(3) 0.1301(4) 0.0367(17) Uani 1 1 d . A . C62 C 0.0125(5) 0.9951(4) 0.1165(4) 0.0494(19) Uani 1 1 d . . . H62 H 0.0441 0.9822 0.0776 0.059 Uiso 1 1 calc R . . C63 C 0.0415(5) 1.0463(4) 0.1709(5) 0.054(2) Uani 1 1 d . . . H63 H 0.0992 1.0742 0.1777 0.065 Uiso 1 1 calc R . . C64 C -0.0274(5) 1.0510(3) 0.2148(4) 0.0454(19) Uani 1 1 d . A . H64 H -0.0249 1.0839 0.2552 0.054 Uiso 1 1 calc R . . C65 C -0.3466(4) 0.9925(3) 0.0481(3) 0.0234(13) Uani 1 1 d . A . H65 H -0.3863 0.9549 0.0628 0.028 Uiso 1 1 calc R . . C66 C -0.3427(4) 1.0075(3) -0.0224(3) 0.0309(15) Uani 1 1 d . . . H66 H -0.3792 0.9839 -0.0638 0.037 Uiso 1 1 calc R . . C67 C -0.2743(4) 1.0646(3) -0.0215(3) 0.0312(15) Uani 1 1 d . . . H67 H -0.2536 1.0862 -0.0620 0.037 Uiso 1 1 calc R . . C68 C -0.2426(4) 1.0832(3) 0.0515(3) 0.0238(13) Uani 1 1 d . A . C69 C -0.1750(4) 1.1405(3) 0.0798(3) 0.0275(14) Uani 1 1 d . A . C70 C -0.0980(5) 1.1652(4) 0.0383(4) 0.0478(19) Uani 1 1 d . . . H70A H -0.0606 1.1246 0.0280 0.057 Uiso 1 1 calc R . . H70B H -0.1230 1.1857 -0.0076 0.057 Uiso 1 1 calc R . . C71 C -0.0413(5) 1.2224(4) 0.0885(4) 0.053(2) Uani 1 1 d . . . H71A H -0.0397 1.2696 0.0658 0.063 Uiso 1 1 calc R . . H71B H 0.0230 1.2087 0.1011 0.063 Uiso 1 1 calc R . . C72 C -0.0889(5) 1.2265(4) 0.1555(5) 0.052(2) Uani 1 1 d . A . H72A H -0.0474 1.2126 0.1982 0.062 Uiso 1 1 calc R . . H72B H -0.1063 1.2764 0.1647 0.062 Uiso 1 1 calc R . . C73 C -0.4641(4) 1.1451(3) 0.0854(3) 0.0344(15) Uani 1 1 d . A . H73A H -0.4955 1.1033 0.1056 0.041 Uiso 1 1 calc R . . H73B H -0.4308 1.1272 0.0468 0.041 Uiso 1 1 calc R . . C74 C -0.5334(5) 1.1976(4) 0.0565(4) 0.0478(18) Uani 1 1 d . . . H74A H -0.5970 1.1740 0.0494 0.057 Uiso 1 1 calc R . . H74B H -0.5195 1.2155 0.0100 0.057 Uiso 1 1 calc R . . C75 C -0.5230(5) 1.2600(4) 0.1144(4) 0.0428(17) Uani 1 1 d . . . H75A H -0.5215 1.3078 0.0925 0.051 Uiso 1 1 calc R . . H75B H -0.5737 1.2565 0.1441 0.051 Uiso 1 1 calc R . . C76 C -0.4326(4) 1.2482(3) 0.1573(3) 0.0297(14) Uani 1 1 d . A . C77 C -0.3795(4) 1.2966(3) 0.2118(3) 0.0323(15) Uani 1 1 d . A . C78 C -0.3931(5) 1.3656(4) 0.2392(4) 0.0470(19) Uani 1 1 d . . . H78 H -0.4448 1.3930 0.2260 0.056 Uiso 1 1 calc R . . C79 C -0.3153(6) 1.3865(4) 0.2901(4) 0.055(2) Uani 1 1 d . . . H79 H -0.3036 1.4308 0.3180 0.066 Uiso 1 1 calc R . . C80 C -0.2583(5) 1.3290(4) 0.2915(4) 0.0443(18) Uani 1 1 d . A . H80 H -0.2006 1.3282 0.3216 0.053 Uiso 1 1 calc R . . C81 C 0.2972(6) 0.7331(4) 0.0615(5) 0.066(2) Uani 1 1 d . . . H81A H 0.3508 0.7096 0.0847 0.099 Uiso 1 1 calc R . . H81B H 0.2609 0.7496 0.0982 0.099 Uiso 1 1 calc R . . H81C H 0.3186 0.7747 0.0360 0.099 Uiso 1 1 calc R . . C82 C 0.2391(5) 0.6808(4) 0.0097(4) 0.0470(19) Uani 1 1 d . . . C83 C 0.1636(5) 0.6452(4) 0.0306(4) 0.0513(19) Uani 1 1 d . . . H83 H 0.1491 0.6552 0.0775 0.062 Uiso 1 1 calc R . . C84 C 0.1092(7) 0.5959(5) -0.0140(5) 0.068(2) Uani 1 1 d . . . H84 H 0.0562 0.5729 0.0019 0.081 Uiso 1 1 calc R . . C85 C 0.1283(6) 0.5782(4) -0.0816(6) 0.077(3) Uani 1 1 d . . . H85 H 0.0909 0.5426 -0.1125 0.093 Uiso 1 1 calc R . . C86 C 0.2063(7) 0.6156(5) -0.1028(5) 0.077(3) Uani 1 1 d . . . H86 H 0.2216 0.6051 -0.1494 0.093 Uiso 1 1 calc R . . C87 C 0.2608(5) 0.6668(5) -0.0580(4) 0.056(2) Uani 1 1 d . . . H87 H 0.3126 0.6921 -0.0736 0.068 Uiso 1 1 calc R . . O3 O 0.2898(3) 0.5840(2) 0.2730(2) 0.0291(10) Uani 1 1 d . C . O4 O 0.3646(3) 0.6171(2) 0.3291(2) 0.0330(10) Uani 1 1 d . . . O5 O -0.2817(3) 0.9268(2) 0.2367(2) 0.0305(10) Uani 1 1 d . A . O6 O -0.3583(3) 0.8906(2) 0.1829(2) 0.0279(9) Uani 1 1 d . . . O7 O -0.2456(4) 1.0984(3) 0.2556(2) 0.0668(18) Uani 1 1 d D . . N1 N 0.3093(4) 0.2340(3) 0.2455(3) 0.0357(13) Uani 1 1 d . C . N2 N 0.4136(3) 0.3170(3) 0.3506(3) 0.0285(12) Uani 1 1 d . C . N3 N 0.1819(3) 0.3263(3) 0.3442(3) 0.0319(12) Uani 1 1 d . C . N4 N 0.2885(3) 0.4626(2) 0.4044(2) 0.0183(10) Uani 1 1 d . . . N5 N 0.1058(3) 0.4986(2) 0.2971(3) 0.0293(12) Uani 1 1 d . . . N6 N 0.1690(4) 0.6319(3) 0.3856(3) 0.0325(13) Uani 1 1 d . C . N7 N 0.0804(4) 0.6577(3) 0.2124(3) 0.0365(13) Uani 1 1 d . C . N8 N 0.2203(4) 0.7555(3) 0.2641(4) 0.060(2) Uani 1 1 d . C . N9 N -0.2115(4) 0.7541(3) 0.2557(3) 0.0401(14) Uani 1 1 d . A . N10 N -0.0718(3) 0.8547(3) 0.2974(3) 0.0321(12) Uani 1 1 d . A . N11 N -0.1788(3) 0.8612(3) 0.1221(2) 0.0260(11) Uani 1 1 d . A . N12 N -0.0993(3) 1.0006(3) 0.1905(3) 0.0302(12) Uani 1 1 d . . . N13 N -0.2870(3) 1.0378(2) 0.0943(2) 0.0200(10) Uani 1 1 d . . . N14 N -0.1730(3) 1.1751(2) 0.1406(3) 0.0312(12) Uani 1 1 d . . . N15 N -0.4005(3) 1.1867(2) 0.1414(3) 0.0277(12) Uani 1 1 d . . . N16 N -0.2966(4) 1.2743(3) 0.2439(3) 0.0359(13) Uani 1 1 d . . . Zn1 Zn 0.29059(5) 0.32937(4) 0.29149(4) 0.0296(2) Uani 1 1 d D . . Zn2 Zn 0.24205(4) 0.49049(3) 0.30521(3) 0.01958(18) Uani 1 1 d . C . Zn3 Zn -0.23360(4) 1.01459(3) 0.19330(3) 0.02061(18) Uani 1 1 d . A . Zn5 Zn -0.19062(5) 0.85506(4) 0.22579(4) 0.0272(2) Uani 1 1 d . . . Zn22 Zn -0.27582(5) 1.17843(4) 0.20071(4) 0.0291(2) Uani 1 1 d . A . Zn23 Zn 0.19543(5) 0.65170(4) 0.28523(4) 0.0295(2) Uani 1 1 d . . . C45 C -0.2303(4) 1.0904(3) 0.3834(3) 0.0490(19) Uani 1 1 d D . . O8 O -0.2972(4) 1.0885(3) 0.3177(3) 0.0494(18) Uani 0.70 1 d PD A 1 C46 C -0.1613(9) 1.0329(6) 0.3826(6) 0.074(4) Uani 0.70 1 d PD A 1 H46A H -0.1946 0.9855 0.3696 0.110 Uiso 0.70 1 calc PR A 1 H46B H -0.1248 1.0320 0.4304 0.110 Uiso 0.70 1 calc PR A 1 H46C H -0.1200 1.0443 0.3471 0.110 Uiso 0.70 1 calc PR A 1 C47 C -0.1979(8) 1.1693(3) 0.4027(6) 0.064(3) Uani 0.70 1 d PD A 1 H47A H -0.2517 1.1981 0.4015 0.096 Uiso 0.70 1 calc PR A 1 H47B H -0.1589 1.1872 0.3679 0.096 Uiso 0.70 1 calc PR A 1 H47C H -0.1622 1.1736 0.4511 0.096 Uiso 0.70 1 calc PR A 1 C48 C -0.3044(7) 1.0672(7) 0.4287(6) 0.070(4) Uani 0.70 1 d PD A 1 H48A H -0.3484 1.1046 0.4291 0.105 Uiso 0.70 1 calc PR A 1 H48B H -0.2753 1.0606 0.4781 0.105 Uiso 0.70 1 calc PR A 1 H48C H -0.3370 1.0215 0.4082 0.105 Uiso 0.70 1 calc PR A 1 O8A O -0.1797(6) 1.1051(7) 0.3240(3) 0.037(3) Uiso 0.30 1 d PD A 2 C47A C -0.2513(14) 1.0088(3) 0.3824(12) 0.048(6) Uiso 0.30 1 d PD A 2 H47D H -0.2013 0.9845 0.3643 0.071 Uiso 0.30 1 calc PR A 2 H47E H -0.3097 0.9952 0.3509 0.071 Uiso 0.30 1 calc PR A 2 H47F H -0.2565 0.9942 0.4313 0.071 Uiso 0.30 1 calc PR A 2 C48A C -0.1352(8) 1.1110(12) 0.4260(13) 0.082(9) Uiso 0.30 1 d PD A 2 H48D H -0.0889 1.0843 0.4053 0.123 Uiso 0.30 1 calc PR A 2 H48E H -0.1353 1.0988 0.4763 0.123 Uiso 0.30 1 calc PR A 2 H48F H -0.1202 1.1631 0.4238 0.123 Uiso 0.30 1 calc PR A 2 C46A C -0.3050(11) 1.1333(11) 0.4093(14) 0.077(9) Uiso 0.30 1 d PD A 2 H46D H -0.2877 1.1852 0.4080 0.115 Uiso 0.30 1 calc PR A 2 H46E H -0.3116 1.1213 0.4588 0.115 Uiso 0.30 1 calc PR A 2 H46F H -0.3638 1.1210 0.3779 0.115 Uiso 0.30 1 calc PR A 2 C89 C 0.2354(4) 0.1766(3) 0.4959(3) 0.037(3) Uiso 0.675(10) 1 d PG B 1 C90 C 0.1603(5) 0.1321(4) 0.5100(3) 0.051(3) Uiso 0.675(10) 1 d PGD B 1 H90 H 0.1404 0.1353 0.5559 0.061 Uiso 0.675(10) 1 calc PR B 1 C91 C 0.1142(5) 0.0831(4) 0.4568(4) 0.067(4) Uiso 0.675(10) 1 d PG B 1 H91 H 0.0629 0.0527 0.4664 0.080 Uiso 0.675(10) 1 calc PR B 1 C92 C 0.1433(5) 0.0785(4) 0.3895(4) 0.077(4) Uiso 0.675(10) 1 d PG B 1 H92 H 0.1118 0.0449 0.3532 0.093 Uiso 0.675(10) 1 calc PR B 1 C93 C 0.2184(5) 0.1229(4) 0.3755(3) 0.067(4) Uiso 0.675(10) 1 d PG B 1 H93 H 0.2382 0.1198 0.3296 0.080 Uiso 0.675(10) 1 calc PR B 1 C94 C 0.2645(4) 0.1720(3) 0.4287(3) 0.028(4) Uiso 0.675(10) 1 d PGD B 1 H94 H 0.3158 0.2024 0.4191 0.033 Uiso 0.675(10) 1 calc PR B 1 C88 C 0.2903(7) 0.2276(6) 0.5549(5) 0.054(3) Uiso 0.675(10) 1 d PD B 1 H88A H 0.3404 0.2545 0.5354 0.082 Uiso 0.675(10) 1 calc PR B 1 H88B H 0.3165 0.1994 0.5948 0.082 Uiso 0.675(10) 1 calc PR B 1 H88C H 0.2493 0.2617 0.5723 0.082 Uiso 0.675(10) 1 calc PR B 1 C89A C 0.2158(9) 0.1157(6) 0.4256(5) 0.019(4) Uiso 0.325(10) 1 d PG B 2 C90A C 0.1714(8) 0.0999(5) 0.4844(6) 0.039(5) Uiso 0.325(10) 1 d PG B 2 H90A H 0.1299 0.0579 0.4825 0.046 Uiso 0.325(10) 1 calc PR B 2 C91A C 0.1876(8) 0.1456(6) 0.5460(5) 0.023(5) Uiso 0.325(10) 1 d PG B 2 H91A H 0.1573 0.1349 0.5862 0.028 Uiso 0.325(10) 1 calc PR B 2 C92A C 0.2483(9) 0.2071(6) 0.5489(5) 0.032(5) Uiso 0.325(10) 1 d PG B 2 H92A H 0.2594 0.2384 0.5910 0.038 Uiso 0.325(10) 1 calc PR B 2 C93A C 0.2927(9) 0.2229(6) 0.4901(7) 0.036(5) Uiso 0.325(10) 1 d PG B 2 H93A H 0.3342 0.2649 0.4920 0.044 Uiso 0.325(10) 1 calc PR B 2 C94A C 0.2765(10) 0.1772(7) 0.4284(6) 0.097(18) Uiso 0.325(10) 1 d PG B 2 H94A H 0.3068 0.1879 0.3882 0.116 Uiso 0.325(10) 1 calc PR B 2 C88A C 0.1983(16) 0.0658(12) 0.3574(12) 0.050(6) Uiso 0.325(10) 1 d P B 2 H88D H 0.2335 0.0859 0.3211 0.075 Uiso 0.325(10) 1 calc PR B 2 H88E H 0.1322 0.0619 0.3385 0.075 Uiso 0.325(10) 1 calc PR B 2 H88F H 0.2182 0.0177 0.3689 0.075 Uiso 0.325(10) 1 calc PR B 2 O1 O 0.2889(4) 0.4206(3) 0.2384(3) 0.0209(12) Uani 0.75 1 d P C 1 O2 O 0.2091(4) 0.4019(3) 0.1797(3) 0.0305(13) Uani 0.75 1 d PD C 1 C2 C 0.3168(5) 0.3822(5) 0.0933(5) 0.044(2) Uani 0.75 1 d PD C 1 H2A H 0.3723 0.3956 0.1282 0.066 Uiso 0.75 1 calc PR C 1 H2B H 0.3285 0.3947 0.0451 0.066 Uiso 0.75 1 calc PR C 1 H2C H 0.3010 0.3299 0.0937 0.066 Uiso 0.75 1 calc PR C 1 C3 C 0.1480(5) 0.4051(6) 0.0616(5) 0.053(3) Uani 0.75 1 d PD C 1 H3A H 0.0989 0.4329 0.0767 0.079 Uiso 0.75 1 calc PR C 1 H3B H 0.1297 0.3532 0.0615 0.079 Uiso 0.75 1 calc PR C 1 H3C H 0.1580 0.4178 0.0130 0.079 Uiso 0.75 1 calc PR C 1 C4 C 0.2593(7) 0.5043(3) 0.1162(5) 0.048(3) Uani 0.75 1 d PD C 1 H4A H 0.2065 0.5289 0.1292 0.072 Uiso 0.75 1 calc PR C 1 H4B H 0.2721 0.5190 0.0688 0.072 Uiso 0.75 1 calc PR C 1 H4C H 0.3138 0.5174 0.1522 0.072 Uiso 0.75 1 calc PR C 1 O1A O 0.2369(13) 0.4058(9) 0.2379(9) 0.041(6) Uiso 0.25 1 d PD C 2 O2A O 0.2986(10) 0.4149(12) 0.1811(7) 0.061(6) Uiso 0.25 1 d PD C 2 C2A C 0.1634(15) 0.4769(12) 0.113(2) 0.103(14) Uiso 0.25 1 d PD C 2 H2A1 H 0.1185 0.4613 0.1440 0.154 Uiso 0.25 1 calc PR C 2 H2A2 H 0.1317 0.4794 0.0633 0.154 Uiso 0.25 1 calc PR C 2 H2A3 H 0.1927 0.5247 0.1298 0.154 Uiso 0.25 1 calc PR C 2 C3A C 0.3104(16) 0.4422(14) 0.0665(15) 0.071(10) Uiso 0.25 1 d PD C 2 H3A1 H 0.3522 0.4032 0.0662 0.107 Uiso 0.25 1 calc PR C 2 H3A2 H 0.3457 0.4873 0.0857 0.107 Uiso 0.25 1 calc PR C 2 H3A3 H 0.2806 0.4485 0.0173 0.107 Uiso 0.25 1 calc PR C 2 C4A C 0.1957(19) 0.3452(6) 0.0984(17) 0.079(11) Uiso 0.25 1 d PD C 2 H4A1 H 0.2457 0.3125 0.1000 0.119 Uiso 0.25 1 calc PR C 2 H4A2 H 0.1585 0.3406 0.0506 0.119 Uiso 0.25 1 calc PR C 2 H4A3 H 0.1565 0.3324 0.1348 0.119 Uiso 0.25 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(5) 0.048(4) 0.026(4) -0.007(3) 0.005(3) 0.013(4) C5 0.023(3) 0.037(4) 0.053(4) 0.018(3) 0.018(3) 0.010(3) C6 0.025(4) 0.043(4) 0.060(5) 0.020(3) 0.015(3) 0.014(3) C7 0.032(4) 0.049(4) 0.065(5) 0.033(4) 0.023(4) 0.012(3) C8 0.033(4) 0.045(4) 0.065(5) 0.015(4) 0.010(4) -0.001(3) C9 0.053(5) 0.049(4) 0.034(4) -0.025(3) 0.001(3) 0.004(4) C10 0.072(6) 0.031(4) 0.054(5) -0.025(3) 0.014(4) -0.001(4) C11 0.060(5) 0.019(3) 0.061(5) -0.007(3) 0.026(4) 0.013(3) C12 0.045(4) 0.029(4) 0.036(4) -0.002(3) 0.009(3) 0.010(3) C13 0.032(4) 0.028(3) 0.038(4) 0.011(3) 0.007(3) 0.011(3) C14 0.038(4) 0.042(4) 0.054(5) 0.013(3) -0.001(3) 0.017(3) C15 0.052(5) 0.069(5) 0.050(5) 0.004(4) -0.020(4) 0.016(4) C16 0.035(4) 0.041(4) 0.034(4) -0.001(3) -0.010(3) 0.006(3) C17 0.027(4) 0.032(4) 0.120(8) 0.001(4) -0.002(5) -0.012(3) C18 0.032(4) 0.029(4) 0.156(10) 0.026(5) -0.001(5) -0.009(3) C19 0.038(4) 0.037(4) 0.120(8) 0.026(5) 0.042(5) 0.011(3) C20 0.022(3) 0.023(3) 0.050(4) 0.012(3) 0.012(3) 0.010(3) C21 0.023(3) 0.018(3) 0.025(3) 0.005(2) 0.007(3) 0.010(2) C22 0.057(4) 0.028(4) 0.029(4) 0.010(3) 0.019(3) 0.018(3) C23 0.056(4) 0.030(4) 0.019(3) -0.001(3) -0.004(3) 0.016(3) C24 0.026(3) 0.022(3) 0.031(4) 0.001(3) -0.002(3) 0.005(3) C25 0.020(4) 0.034(4) 0.119(8) 0.002(4) -0.012(4) 0.004(3) C26 0.054(6) 0.038(5) 0.106(8) -0.004(5) 0.012(5) -0.004(4) C27 0.026(4) 0.071(6) 0.098(7) 0.053(5) 0.037(4) 0.024(4) C28 0.031(4) 0.024(3) 0.050(4) 0.014(3) 0.013(3) 0.008(3) C29 0.047(4) 0.054(5) 0.032(4) 0.027(3) 0.026(3) 0.039(4) C30 0.115(8) 0.086(7) 0.041(5) 0.010(5) 0.035(5) 0.067(6) C31 0.109(8) 0.151(10) 0.014(4) -0.003(5) -0.005(5) 0.083(8) C32 0.057(5) 0.065(5) 0.075(6) -0.036(5) -0.046(5) 0.038(4) C33 0.036(4) 0.070(5) 0.031(4) 0.005(3) 0.002(3) 0.020(4) C34 0.057(6) 0.106(8) 0.051(5) 0.013(5) -0.007(4) 0.039(5) C35 0.061(5) 0.109(7) 0.050(5) 0.045(5) 0.025(4) 0.057(5) C36 0.053(5) 0.068(5) 0.048(5) 0.046(4) 0.038(4) 0.048(4) C37 0.046(5) 0.045(5) 0.107(7) 0.046(5) 0.052(5) 0.024(4) C38 0.076(7) 0.066(6) 0.156(10) 0.078(6) 0.087(7) 0.045(5) C39 0.078(8) 0.039(5) 0.267(17) 0.068(7) 0.106(10) 0.025(5) C40 0.047(5) 0.031(5) 0.270(16) 0.048(7) 0.053(8) 0.014(4) C41 0.027(3) 0.027(3) 0.040(4) 0.011(3) 0.014(3) 0.001(3) C42 0.043(4) 0.043(4) 0.048(4) 0.021(3) 0.026(3) 0.010(3) C43 0.035(4) 0.038(4) 0.054(5) 0.012(3) 0.015(3) -0.001(3) C44 0.023(3) 0.031(3) 0.057(4) 0.012(3) 0.016(3) 0.009(3) C49 0.039(4) 0.040(4) 0.086(6) 0.012(4) 0.014(4) 0.002(4) C50 0.074(6) 0.029(4) 0.081(6) 0.017(4) 0.028(5) 0.005(4) C51 0.049(5) 0.049(5) 0.061(5) 0.020(4) 0.023(4) 0.017(4) C52 0.035(4) 0.035(4) 0.055(5) 0.022(3) 0.021(3) 0.022(3) C53 0.038(4) 0.047(4) 0.034(4) 0.016(3) 0.018(3) 0.025(3) C54 0.046(4) 0.077(5) 0.025(4) 0.018(4) 0.009(3) 0.040(4) C55 0.056(6) 0.101(8) 0.091(7) 0.055(6) -0.026(5) 0.003(5) C56 0.036(4) 0.052(4) 0.030(4) 0.004(3) -0.010(3) 0.015(3) C57 0.052(5) 0.049(4) 0.031(4) -0.017(3) -0.013(3) 0.019(4) C58 0.058(5) 0.067(5) 0.044(5) -0.006(4) -0.009(4) 0.026(4) C59 0.054(5) 0.077(6) 0.029(4) 0.019(4) 0.015(3) 0.035(4) C60 0.037(4) 0.037(4) 0.021(3) 0.005(3) 0.004(3) 0.030(3) C61 0.027(4) 0.040(4) 0.051(4) 0.026(3) 0.020(3) 0.021(3) C62 0.047(5) 0.038(4) 0.067(5) 0.011(4) 0.021(4) 0.006(4) C63 0.015(4) 0.059(5) 0.092(6) 0.032(5) 0.012(4) 0.010(3) C64 0.043(4) 0.023(3) 0.065(5) 0.005(3) -0.012(4) 0.006(3) C65 0.029(3) 0.017(3) 0.024(3) 0.000(2) 0.000(3) 0.004(2) C66 0.046(4) 0.023(3) 0.022(3) -0.002(3) 0.000(3) 0.004(3) C67 0.042(4) 0.031(3) 0.024(3) 0.007(3) 0.008(3) 0.015(3) C68 0.024(3) 0.019(3) 0.032(4) 0.005(3) 0.008(3) 0.010(3) C69 0.021(3) 0.019(3) 0.044(4) 0.008(3) 0.004(3) 0.007(3) C70 0.038(4) 0.035(4) 0.076(6) 0.008(4) 0.029(4) 0.001(3) C71 0.034(4) 0.056(5) 0.071(6) 0.026(4) 0.010(4) -0.003(4) C72 0.033(4) 0.028(4) 0.085(6) -0.011(4) -0.018(4) -0.001(3) C73 0.031(4) 0.032(4) 0.036(4) -0.006(3) -0.009(3) 0.002(3) C74 0.040(4) 0.047(4) 0.051(5) 0.002(4) -0.009(4) 0.003(3) C75 0.039(4) 0.043(4) 0.049(4) 0.016(3) 0.004(3) 0.016(3) C76 0.030(3) 0.028(3) 0.032(4) 0.003(3) 0.007(3) 0.005(3) C77 0.032(4) 0.024(3) 0.040(4) -0.007(3) 0.008(3) 0.002(3) C78 0.058(5) 0.030(4) 0.056(5) -0.008(3) 0.015(4) 0.013(3) C79 0.073(6) 0.034(4) 0.059(5) -0.023(4) 0.019(4) -0.003(4) C80 0.050(4) 0.040(4) 0.040(4) -0.014(3) 0.002(3) 0.000(3) C81 0.079(6) 0.048(5) 0.068(6) 0.014(4) -0.005(5) 0.019(4) C82 0.040(4) 0.040(4) 0.061(5) 0.019(4) 0.001(4) 0.003(3) C83 0.049(5) 0.048(5) 0.057(5) 0.012(4) 0.008(4) 0.004(4) C84 0.075(6) 0.061(6) 0.070(6) 0.030(5) 0.008(5) 0.009(5) C85 0.065(6) 0.036(5) 0.112(9) 0.001(5) -0.046(6) -0.002(4) C86 0.067(6) 0.094(7) 0.068(6) -0.014(5) 0.004(5) 0.008(6) C87 0.044(5) 0.076(6) 0.048(5) 0.001(4) 0.007(4) -0.003(4) O3 0.025(2) 0.038(2) 0.028(2) 0.0144(19) 0.0075(18) 0.0124(19) O4 0.024(2) 0.034(2) 0.044(3) 0.012(2) 0.009(2) 0.0067(18) O5 0.025(2) 0.036(2) 0.034(2) 0.0118(19) 0.0086(19) 0.0124(19) O6 0.023(2) 0.030(2) 0.034(2) 0.0138(18) 0.0098(19) 0.0083(18) O7 0.121(5) 0.059(3) 0.026(3) -0.005(2) 0.004(3) 0.063(3) N1 0.044(3) 0.034(3) 0.028(3) -0.010(2) 0.002(3) 0.009(3) N2 0.027(3) 0.029(3) 0.027(3) 0.000(2) -0.004(2) 0.003(2) N3 0.021(3) 0.025(3) 0.046(4) -0.002(2) -0.003(2) 0.002(2) N4 0.019(2) 0.017(2) 0.019(3) 0.002(2) 0.001(2) 0.0044(19) N5 0.017(3) 0.021(3) 0.047(3) 0.006(2) -0.007(2) 0.006(2) N6 0.034(3) 0.041(3) 0.021(3) -0.009(2) -0.007(2) 0.024(3) N7 0.032(3) 0.054(4) 0.030(3) 0.019(3) 0.016(3) 0.021(3) N8 0.027(3) 0.038(4) 0.127(6) 0.039(4) 0.033(4) 0.017(3) N9 0.030(3) 0.030(3) 0.064(4) 0.018(3) 0.017(3) 0.004(3) N10 0.032(3) 0.039(3) 0.030(3) 0.012(2) 0.009(2) 0.016(2) N11 0.026(3) 0.032(3) 0.020(3) 0.000(2) -0.001(2) 0.013(2) N12 0.026(3) 0.027(3) 0.037(3) 0.007(2) 0.001(2) 0.003(2) N13 0.023(3) 0.016(2) 0.020(3) -0.003(2) -0.001(2) 0.003(2) N14 0.020(3) 0.020(3) 0.050(4) -0.001(2) -0.008(2) 0.000(2) N15 0.026(3) 0.023(3) 0.032(3) -0.002(2) -0.002(2) 0.003(2) N16 0.040(3) 0.031(3) 0.035(3) -0.016(2) 0.002(3) 0.003(2) Zn1 0.0336(4) 0.0257(4) 0.0275(4) -0.0074(3) -0.0044(3) 0.0116(3) Zn2 0.0208(4) 0.0199(3) 0.0181(4) 0.0006(3) 0.0005(3) 0.0065(3) Zn3 0.0218(4) 0.0216(4) 0.0190(4) 0.0016(3) 0.0017(3) 0.0075(3) Zn5 0.0240(4) 0.0267(4) 0.0334(4) 0.0109(3) 0.0064(3) 0.0097(3) Zn22 0.0310(4) 0.0277(4) 0.0259(4) -0.0086(3) -0.0061(3) 0.0106(3) Zn23 0.0226(4) 0.0261(4) 0.0436(5) 0.0154(3) 0.0101(3) 0.0100(3) C45 0.079(6) 0.049(4) 0.016(3) 0.003(3) -0.003(4) 0.006(4) O8 0.043(4) 0.039(4) 0.066(5) 0.003(3) 0.004(4) 0.004(3) C46 0.113(11) 0.088(9) 0.026(6) 0.014(6) 0.008(7) 0.055(8) C47 0.094(10) 0.054(7) 0.038(7) -0.004(5) -0.015(6) 0.021(7) C48 0.077(9) 0.098(10) 0.038(7) 0.008(6) 0.021(6) 0.001(7) O1 0.019(3) 0.026(3) 0.015(3) -0.003(2) -0.006(2) 0.009(2) O2 0.037(3) 0.033(3) 0.016(3) -0.009(2) -0.012(2) 0.000(3) C2 0.056(6) 0.051(6) 0.032(5) 0.011(4) 0.015(5) 0.024(5) C3 0.057(7) 0.069(7) 0.028(5) -0.008(5) -0.013(5) 0.023(5) C4 0.090(8) 0.037(5) 0.020(5) 0.004(4) 0.006(5) 0.026(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 C1 O2 1.420(6) . ? C1 O2A 1.468(10) . ? C1 C2 1.5195(10) . ? C1 C2A 1.5196(10) . ? C1 C3A 1.5197(11) . ? C1 C4A 1.5201(10) . ? C1 C3 1.5201(10) . ? C1 C4 1.5202(10) . ? C5 O4 1.438(7) . ? C5 C8 1.512(10) . ? C5 C6 1.530(9) . ? C5 C7 1.542(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.367(8) . ? C9 C10 1.383(10) . ? C9 H9 0.9500 . ? C10 C11 1.403(11) . ? C10 H10 0.9500 . ? C11 C12 1.399(9) . ? C11 H11 0.9500 . ? C12 N1 1.371(8) . ? C12 C13 1.436(9) . ? C13 N2 1.304(8) . ? C13 C14 1.491(9) . ? C14 C15 1.543(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.529(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N2 1.466(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.476(13) . ? C17 N3 1.479(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.522(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.502(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N3 1.297(8) . ? C20 C21 1.428(8) . ? C21 N4 1.393(7) . ? C21 C22 1.399(8) . ? C22 C23 1.387(9) . ? C22 H22 0.9500 . ? C23 C24 1.378(9) . ? C23 H23 0.9500 . ? C24 N4 1.365(7) . ? C24 H24 0.9500 . ? C25 C26 1.323(11) . ? C25 N5 1.354(8) . ? C25 H25 0.9500 . ? C26 C27 1.382(12) . ? C26 H26 0.9500 . ? C27 C28 1.428(10) . ? C27 H27 0.9500 . ? C28 N5 1.357(8) . ? C28 C29 1.419(10) . ? C29 N6 1.310(9) . ? C29 C30 1.494(10) . ? C30 C31 1.486(14) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.558(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N6 1.472(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N7 1.462(9) . ? C33 C34 1.543(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.509(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.501(11) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N7 1.312(8) . ? C36 C37 1.414(12) . ? C37 N8 1.375(10) . ? C37 C38 1.396(11) . ? C38 C39 1.382(17) . ? C38 H38 0.9500 . ? C39 C40 1.403(14) . ? C39 H39 0.9500 . ? C40 N8 1.349(11) . ? C40 H40 0.9500 . ? C41 O6 1.448(7) . ? C41 C42 1.515(9) . ? C41 C43 1.525(9) . ? C41 C44 1.526(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C49 N9 1.349(9) . ? C49 C50 1.420(10) . ? C49 H49 0.9500 . ? C50 C51 1.373(11) . ? C50 H50 0.9500 . ? C51 C52 1.396(9) . ? C51 H51 0.9500 . ? C52 N9 1.368(9) . ? C52 C53 1.419(10) . ? C53 N10 1.295(8) . ? C53 C54 1.506(9) . ? C54 C55 1.486(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.524(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 N10 1.465(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.487(11) . ? C57 N11 1.492(8) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.511(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.520(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 N11 1.272(8) . ? C60 C61 1.435(9) . ? C61 C62 1.390(9) . ? C61 N12 1.399(8) . ? C62 C63 1.367(11) . ? C62 H62 0.9500 . ? C63 C64 1.396(10) . ? C63 H63 0.9500 . ? C64 N12 1.371(8) . ? C64 H64 0.9500 . ? C65 N13 1.358(7) . ? C65 C66 1.373(8) . ? C65 H65 0.9500 . ? C66 C67 1.403(9) . ? C66 H66 0.9500 . ? C67 C68 1.406(8) . ? C67 H67 0.9500 . ? C68 N13 1.379(7) . ? C68 C69 1.432(8) . ? C69 N14 1.283(8) . ? C69 C70 1.514(9) . ? C70 C71 1.510(10) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.525(11) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 N14 1.490(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 N15 1.458(7) . ? C73 C74 1.514(9) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.541(10) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.485(9) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 N15 1.303(7) . ? C76 C77 1.435(8) . ? C77 N16 1.376(8) . ? C77 C78 1.398(9) . ? C78 C79 1.400(11) . ? C78 H78 0.9500 . ? C79 C80 1.398(10) . ? C79 H79 0.9500 . ? C80 N16 1.359(8) . ? C80 H80 0.9500 . ? C81 C82 1.479(11) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.362(10) . ? C82 C87 1.373(10) . ? C83 C84 1.348(11) . ? C83 H83 0.9500 . ? C84 C85 1.372(13) . ? C84 H84 0.9500 . ? C85 C86 1.409(13) . ? C85 H85 0.9500 . ? C86 C87 1.374(11) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? O3 O4 1.488(6) . ? O3 Zn23 1.962(4) . ? O3 Zn2 1.973(4) . ? O5 O6 1.499(6) . ? O5 Zn5 1.973(4) . ? O5 Zn3 1.979(4) . ? O7 O8 1.4876(10) . ? O7 O8A 1.4885(11) . ? O7 Zn22 1.883(5) . ? O7 Zn3 1.941(4) . ? N1 Zn1 1.990(5) . ? N2 Zn1 2.011(5) . ? N3 Zn1 1.989(5) . ? N4 Zn2 1.992(4) . ? N5 Zn2 1.997(5) . ? N6 Zn23 2.020(5) . ? N7 Zn23 2.027(5) . ? N8 Zn23 1.999(5) . ? N9 Zn5 1.990(5) . ? N10 Zn5 2.044(5) . ? N11 Zn5 1.987(5) . ? N12 Zn3 2.009(5) . ? N13 Zn3 1.989(4) . ? N14 Zn22 2.010(5) . ? N15 Zn22 2.019(5) . ? N16 Zn22 1.984(5) . ? Zn1 O1A 1.921(9) . ? Zn1 O1 1.998(5) . ? Zn1 Zn2 3.1274(9) . ? Zn2 O1A 1.967(19) . ? Zn2 O1 1.990(5) . ? Zn2 Zn23 3.1367(9) . ? Zn3 Zn5 3.1317(9) . ? Zn3 Zn22 3.1431(9) . ? C45 O8A 1.448(9) . ? C45 O8 1.459(7) . ? C45 C46 1.5190(11) . ? C45 C46A 1.5195(11) . ? C45 C47 1.5201(11) . ? C45 C47A 1.5202(11) . ? C45 C48A 1.5205(11) . ? C45 C48 1.5208(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C89 C90 1.3900 . ? C89 C94 1.3900 . ? C89 C88 1.524(7) . ? C90 C91 1.3900 . ? C90 H90 0.9500 . ? C91 C92 1.3900 . ? C91 H91 0.9500 . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89A C90A 1.3900 . ? C89A C94A 1.3900 . ? C89A C88A 1.53(2) . ? C90A C91A 1.3900 . ? C90A H90A 0.9500 . ? C91A C92A 1.3900 . ? C91A H91A 0.9500 . ? C92A C93A 1.3900 . ? C92A H92A 0.9500 . ? C93A C94A 1.3900 . ? C93A H93A 0.9500 . ? C94A H94A 0.9500 . ? C88A H88D 0.9800 . ? C88A H88E 0.9800 . ? C88A H88F 0.9800 . ? O1 O2 1.500(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O1A O2A 1.5000(11) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O2A 54.0(7) . . ? O2 C1 C2 113.0(5) . . ? O2A C1 C2 73.9(8) . . ? O2 C1 C2A 85.7(13) . . ? O2A C1 C2A 118.7(16) . . ? C2 C1 C2A 161.2(13) . . ? O2 C1 C3A 152.0(13) . . ? O2A C1 C3A 98.1(14) . . ? C2 C1 C3A 48.3(11) . . ? C2A C1 C3A 113.7(7) . . ? O2 C1 C4A 75.3(12) . . ? O2A C1 C4A 100.2(16) . . ? C2 C1 C4A 76.0(11) . . ? C2A C1 C4A 112.6(7) . . ? C3A C1 C4A 112.1(7) . . ? O2 C1 C3 101.4(5) . . ? O2A C1 C3 153.1(9) . . ? C2 C1 C3 112.7(6) . . ? C2A C1 C3 63.1(13) . . ? C3A C1 C3 105.3(13) . . ? C4A C1 C3 58.9(13) . . ? O2 C1 C4 109.9(5) . . ? O2A C1 C4 92.4(9) . . ? C2 C1 C4 111.4(6) . . ? C2A C1 C4 57.0(11) . . ? C3A C1 C4 69.3(11) . . ? C4A C1 C4 166.8(13) . . ? C3 C1 C4 108.0(7) . . ? O4 C5 C8 102.1(5) . . ? O4 C5 C6 109.5(5) . . ? C8 C5 C6 112.2(6) . . ? O4 C5 C7 109.8(5) . . ? C8 C5 C7 112.5(6) . . ? C6 C5 C7 110.5(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 110.3(6) . . ? N1 C9 H9 124.8 . . ? C10 C9 H9 124.8 . . ? C9 C10 C11 107.1(6) . . ? C9 C10 H10 126.5 . . ? C11 C10 H10 126.5 . . ? C12 C11 C10 106.0(6) . . ? C12 C11 H11 127.0 . . ? C10 C11 H11 127.0 . . ? N1 C12 C11 110.1(6) . . ? N1 C12 C13 116.9(5) . . ? C11 C12 C13 133.0(7) . . ? N2 C13 C12 118.5(6) . . ? N2 C13 C14 114.3(6) . . ? C12 C13 C14 127.2(6) . . ? C13 C14 C15 101.9(5) . . ? C13 C14 H14A 111.4 . . ? C15 C14 H14A 111.4 . . ? C13 C14 H14B 111.4 . . ? C15 C14 H14B 111.4 . . ? H14A C14 H14B 109.3 . . ? C16 C15 C14 104.5(5) . . ? C16 C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? C16 C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? N2 C16 C15 105.4(5) . . ? N2 C16 H16A 110.7 . . ? C15 C16 H16A 110.7 . . ? N2 C16 H16B 110.7 . . ? C15 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? C18 C17 N3 105.2(7) . . ? C18 C17 H17A 110.7 . . ? N3 C17 H17A 110.7 . . ? C18 C17 H17B 110.7 . . ? N3 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C17 C18 C19 106.7(6) . . ? C17 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? C17 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C18 102.7(7) . . ? C20 C19 H19A 111.2 . . ? C18 C19 H19A 111.2 . . ? C20 C19 H19B 111.2 . . ? C18 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? N3 C20 C21 124.7(5) . . ? N3 C20 C19 112.3(6) . . ? C21 C20 C19 122.9(6) . . ? N4 C21 C22 109.4(5) . . ? N4 C21 C20 122.8(5) . . ? C22 C21 C20 127.7(5) . . ? C23 C22 C21 107.1(5) . . ? C23 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? C24 C23 C22 106.7(5) . . ? C24 C23 H23 126.7 . . ? C22 C23 H23 126.7 . . ? N4 C24 C23 111.6(5) . . ? N4 C24 H24 124.2 . . ? C23 C24 H24 124.2 . . ? C26 C25 N5 112.8(8) . . ? C26 C25 H25 123.6 . . ? N5 C25 H25 123.6 . . ? C25 C26 C27 106.3(7) . . ? C25 C26 H26 126.8 . . ? C27 C26 H26 126.8 . . ? C26 C27 C28 107.0(7) . . ? C26 C27 H27 126.5 . . ? C28 C27 H27 126.5 . . ? N5 C28 C29 121.6(5) . . ? N5 C28 C27 107.0(6) . . ? C29 C28 C27 131.4(7) . . ? N6 C29 C28 124.7(6) . . ? N6 C29 C30 113.1(7) . . ? C28 C29 C30 122.2(7) . . ? C31 C30 C29 102.9(7) . . ? C31 C30 H30A 111.2 . . ? C29 C30 H30A 111.2 . . ? C31 C30 H30B 111.2 . . ? C29 C30 H30B 111.2 . . ? H30A C30 H30B 109.1 . . ? C30 C31 C32 105.9(6) . . ? C30 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? N6 C32 C31 102.6(7) . . ? N6 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? N6 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.2 . . ? N7 C33 C34 105.4(6) . . ? N7 C33 H33A 110.7 . . ? C34 C33 H33A 110.7 . . ? N7 C33 H33B 110.7 . . ? C34 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? C35 C34 C33 104.9(7) . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.8 . . ? C36 C35 C34 103.9(6) . . ? C36 C35 H35A 111.0 . . ? C34 C35 H35A 111.0 . . ? C36 C35 H35B 111.0 . . ? C34 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? N7 C36 C37 119.2(7) . . ? N7 C36 C35 112.5(8) . . ? C37 C36 C35 128.2(7) . . ? N8 C37 C38 110.8(9) . . ? N8 C37 C36 117.2(6) . . ? C38 C37 C36 132.1(9) . . ? C39 C38 C37 105.6(8) . . ? C39 C38 H38 127.2 . . ? C37 C38 H38 127.2 . . ? C38 C39 C40 107.4(8) . . ? C38 C39 H39 126.3 . . ? C40 C39 H39 126.3 . . ? N8 C40 C39 110.1(10) . . ? N8 C40 H40 125.0 . . ? C39 C40 H40 125.0 . . ? O6 C41 C42 110.3(5) . . ? O6 C41 C43 101.4(5) . . ? C42 C41 C43 112.0(5) . . ? O6 C41 C44 109.7(4) . . ? C42 C41 C44 112.8(5) . . ? C43 C41 C44 110.1(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N9 C49 C50 109.2(7) . . ? N9 C49 H49 125.4 . . ? C50 C49 H49 125.4 . . ? C51 C50 C49 108.1(7) . . ? C51 C50 H50 126.0 . . ? C49 C50 H50 126.0 . . ? C50 C51 C52 104.7(7) . . ? C50 C51 H51 127.6 . . ? C52 C51 H51 127.6 . . ? N9 C52 C51 112.0(6) . . ? N9 C52 C53 117.0(5) . . ? C51 C52 C53 131.0(7) . . ? N10 C53 C52 119.4(6) . . ? N10 C53 C54 112.5(6) . . ? C52 C53 C54 128.1(6) . . ? C55 C54 C53 104.3(6) . . ? C55 C54 H54A 110.9 . . ? C53 C54 H54A 110.9 . . ? C55 C54 H54B 110.9 . . ? C53 C54 H54B 110.9 . . ? H54A C54 H54B 108.9 . . ? C54 C55 C56 105.9(6) . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55A 110.6 . . ? C54 C55 H55B 110.6 . . ? C56 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? N10 C56 C55 105.6(6) . . ? N10 C56 H56A 110.6 . . ? C55 C56 H56A 110.6 . . ? N10 C56 H56B 110.6 . . ? C55 C56 H56B 110.6 . . ? H56A C56 H56B 108.7 . . ? C58 C57 N11 104.6(6) . . ? C58 C57 H57A 110.8 . . ? N11 C57 H57A 110.8 . . ? C58 C57 H57B 110.8 . . ? N11 C57 H57B 110.8 . . ? H57A C57 H57B 108.9 . . ? C57 C58 C59 104.1(6) . . ? C57 C58 H58A 110.9 . . ? C59 C58 H58A 110.9 . . ? C57 C58 H58B 110.9 . . ? C59 C58 H58B 110.9 . . ? H58A C58 H58B 109.0 . . ? C58 C59 C60 102.6(6) . . ? C58 C59 H59A 111.3 . . ? C60 C59 H59A 111.3 . . ? C58 C59 H59B 111.3 . . ? C60 C59 H59B 111.3 . . ? H59A C59 H59B 109.2 . . ? N11 C60 C61 123.2(5) . . ? N11 C60 C59 111.6(6) . . ? C61 C60 C59 125.2(6) . . ? C62 C61 N12 111.1(6) . . ? C62 C61 C60 127.3(6) . . ? N12 C61 C60 121.6(5) . . ? C63 C62 C61 105.5(7) . . ? C63 C62 H62 127.3 . . ? C61 C62 H62 127.3 . . ? C62 C63 C64 109.1(6) . . ? C62 C63 H63 125.5 . . ? C64 C63 H63 125.5 . . ? N12 C64 C63 109.4(7) . . ? N12 C64 H64 125.3 . . ? C63 C64 H64 125.3 . . ? N13 C65 C66 111.9(5) . . ? N13 C65 H65 124.1 . . ? C66 C65 H65 124.1 . . ? C65 C66 C67 106.5(5) . . ? C65 C66 H66 126.7 . . ? C67 C66 H66 126.7 . . ? C66 C67 C68 105.9(5) . . ? C66 C67 H67 127.0 . . ? C68 C67 H67 127.0 . . ? N13 C68 C67 109.9(5) . . ? N13 C68 C69 123.4(5) . . ? C67 C68 C69 126.7(5) . . ? N14 C69 C68 124.7(5) . . ? N14 C69 C70 114.2(5) . . ? C68 C69 C70 121.2(6) . . ? C71 C70 C69 103.5(6) . . ? C71 C70 H70A 111.1 . . ? C69 C70 H70A 111.1 . . ? C71 C70 H70B 111.1 . . ? C69 C70 H70B 111.1 . . ? H70A C70 H70B 109.0 . . ? C70 C71 C72 105.8(5) . . ? C70 C71 H71A 110.6 . . ? C72 C71 H71A 110.6 . . ? C70 C71 H71B 110.6 . . ? C72 C71 H71B 110.6 . . ? H71A C71 H71B 108.7 . . ? N14 C72 C71 106.2(6) . . ? N14 C72 H72A 110.5 . . ? C71 C72 H72A 110.5 . . ? N14 C72 H72B 110.5 . . ? C71 C72 H72B 110.5 . . ? H72A C72 H72B 108.7 . . ? N15 C73 C74 105.2(5) . . ? N15 C73 H73A 110.7 . . ? C74 C73 H73A 110.7 . . ? N15 C73 H73B 110.7 . . ? C74 C73 H73B 110.7 . . ? H73A C73 H73B 108.8 . . ? C73 C74 C75 105.0(5) . . ? C73 C74 H74A 110.7 . . ? C75 C74 H74A 110.7 . . ? C73 C74 H74B 110.7 . . ? C75 C74 H74B 110.7 . . ? H74A C74 H74B 108.8 . . ? C76 C75 C74 101.8(5) . . ? C76 C75 H75A 111.4 . . ? C74 C75 H75A 111.4 . . ? C76 C75 H75B 111.4 . . ? C74 C75 H75B 111.4 . . ? H75A C75 H75B 109.3 . . ? N15 C76 C77 119.1(6) . . ? N15 C76 C75 113.8(5) . . ? C77 C76 C75 127.0(6) . . ? N16 C77 C78 110.3(6) . . ? N16 C77 C76 116.7(5) . . ? C78 C77 C76 132.9(6) . . ? C77 C78 C79 106.4(6) . . ? C77 C78 H78 126.8 . . ? C79 C78 H78 126.8 . . ? C80 C79 C78 106.3(6) . . ? C80 C79 H79 126.8 . . ? C78 C79 H79 126.8 . . ? N16 C80 C79 110.9(6) . . ? N16 C80 H80 124.6 . . ? C79 C80 H80 124.6 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C87 119.9(7) . . ? C83 C82 C81 118.8(8) . . ? C87 C82 C81 121.4(7) . . ? C84 C83 C82 121.3(8) . . ? C84 C83 H83 119.3 . . ? C82 C83 H83 119.3 . . ? C83 C84 C85 121.7(9) . . ? C83 C84 H84 119.1 . . ? C85 C84 H84 119.1 . . ? C84 C85 C86 116.5(8) . . ? C84 C85 H85 121.8 . . ? C86 C85 H85 121.8 . . ? C87 C86 C85 121.9(9) . . ? C87 C86 H86 119.1 . . ? C85 C86 H86 119.1 . . ? C82 C87 C86 118.7(8) . . ? C82 C87 H87 120.6 . . ? C86 C87 H87 120.6 . . ? O4 O3 Zn23 98.4(3) . . ? O4 O3 Zn2 109.1(3) . . ? Zn23 O3 Zn2 105.70(18) . . ? C5 O4 O3 108.9(4) . . ? O6 O5 Zn5 96.6(2) . . ? O6 O5 Zn3 107.3(3) . . ? Zn5 O5 Zn3 104.83(18) . . ? C41 O6 O5 107.7(4) . . ? O8 O7 O8A 70.3(5) . . ? O8 O7 Zn22 115.0(4) . . ? O8A O7 Zn22 122.6(6) . . ? O8 O7 Zn3 118.6(4) . . ? O8A O7 Zn3 114.8(6) . . ? Zn22 O7 Zn3 110.6(2) . . ? C9 N1 C12 106.5(5) . . ? C9 N1 Zn1 143.6(5) . . ? C12 N1 Zn1 109.8(4) . . ? C13 N2 C16 110.4(5) . . ? C13 N2 Zn1 110.7(4) . . ? C16 N2 Zn1 138.8(4) . . ? C20 N3 C17 111.3(6) . . ? C20 N3 Zn1 128.0(4) . . ? C17 N3 Zn1 119.9(5) . . ? C24 N4 C21 105.3(5) . . ? C24 N4 Zn2 125.9(4) . . ? C21 N4 Zn2 122.5(4) . . ? C25 N5 C28 106.7(6) . . ? C25 N5 Zn2 122.8(4) . . ? C28 N5 Zn2 121.9(4) . . ? C29 N6 C32 111.2(6) . . ? C29 N6 Zn23 125.4(4) . . ? C32 N6 Zn23 123.4(6) . . ? C36 N7 C33 111.4(6) . . ? C36 N7 Zn23 110.1(5) . . ? C33 N7 Zn23 138.4(4) . . ? C40 N8 C37 106.1(7) . . ? C40 N8 Zn23 144.1(7) . . ? C37 N8 Zn23 109.8(5) . . ? C49 N9 C52 105.9(6) . . ? C49 N9 Zn5 143.7(5) . . ? C52 N9 Zn5 110.2(4) . . ? C53 N10 C56 111.3(5) . . ? C53 N10 Zn5 110.0(5) . . ? C56 N10 Zn5 138.6(4) . . ? C60 N11 C57 110.8(5) . . ? C60 N11 Zn5 129.2(4) . . ? C57 N11 Zn5 120.0(4) . . ? C64 N12 C61 104.8(6) . . ? C64 N12 Zn3 125.1(4) . . ? C61 N12 Zn3 119.6(4) . . ? C65 N13 C68 105.7(5) . . ? C65 N13 Zn3 124.8(4) . . ? C68 N13 Zn3 123.9(4) . . ? C69 N14 C72 110.2(6) . . ? C69 N14 Zn22 127.3(4) . . ? C72 N14 Zn22 121.5(4) . . ? C76 N15 C73 111.0(5) . . ? C76 N15 Zn22 110.0(4) . . ? C73 N15 Zn22 139.0(4) . . ? C80 N16 C77 106.1(5) . . ? C80 N16 Zn22 144.1(5) . . ? C77 N16 Zn22 109.7(4) . . ? O1A Zn1 N3 87.7(5) . . ? O1A Zn1 N1 122.5(6) . . ? N3 Zn1 N1 113.1(2) . . ? O1A Zn1 O1 23.2(5) . . ? N3 Zn1 O1 106.8(2) . . ? N1 Zn1 O1 122.7(2) . . ? O1A Zn1 N2 135.3(6) . . ? N3 Zn1 N2 116.2(2) . . ? N1 Zn1 N2 84.1(2) . . ? O1 Zn1 N2 113.2(2) . . ? O1A Zn1 Zn2 36.9(6) . . ? N3 Zn1 Zn2 75.22(14) . . ? N1 Zn1 Zn2 159.20(16) . . ? O1 Zn1 Zn2 38.28(14) . . ? N2 Zn1 Zn2 110.00(14) . . ? O1A Zn2 O3 116.9(4) . . ? O1A Zn2 O1 23.0(5) . . ? O3 Zn2 O1 101.5(2) . . ? O1A Zn2 N4 109.3(3) . . ? O3 Zn2 N4 118.43(17) . . ? O1 Zn2 N4 106.20(18) . . ? O1A Zn2 N5 96.9(5) . . ? O3 Zn2 N5 103.96(17) . . ? O1 Zn2 N5 118.6(2) . . ? N4 Zn2 N5 108.7(2) . . ? O1A Zn2 Zn1 35.9(3) . . ? O3 Zn2 Zn1 135.88(11) . . ? O1 Zn2 Zn1 38.44(15) . . ? N4 Zn2 Zn1 73.51(12) . . ? N5 Zn2 Zn1 111.90(13) . . ? O1A Zn2 Zn23 133.2(3) . . ? O3 Zn2 Zn23 37.03(11) . . ? O1 Zn2 Zn23 130.17(15) . . ? N4 Zn2 Zn23 117.53(12) . . ? N5 Zn2 Zn23 69.48(13) . . ? Zn1 Zn2 Zn23 168.32(3) . . ? O7 Zn3 O5 108.70(19) . . ? O7 Zn3 N13 106.60(18) . . ? O5 Zn3 N13 119.90(17) . . ? O7 Zn3 N12 110.1(2) . . ? O5 Zn3 N12 104.90(18) . . ? N13 Zn3 N12 106.5(2) . . ? O7 Zn3 Zn5 132.22(13) . . ? O5 Zn3 Zn5 37.52(11) . . ? N13 Zn3 Zn5 119.60(12) . . ? N12 Zn3 Zn5 69.29(14) . . ? O7 Zn3 Zn22 34.11(13) . . ? O5 Zn3 Zn22 133.97(12) . . ? N13 Zn3 Zn22 73.35(12) . . ? N12 Zn3 Zn22 113.08(14) . . ? Zn5 Zn3 Zn22 166.29(3) . . ? O5 Zn5 N11 101.09(18) . . ? O5 Zn5 N9 120.79(19) . . ? N11 Zn5 N9 113.5(2) . . ? O5 Zn5 N10 121.14(19) . . ? N11 Zn5 N10 117.8(2) . . ? N9 Zn5 N10 83.2(2) . . ? O5 Zn5 Zn3 37.66(11) . . ? N11 Zn5 Zn3 76.44(13) . . ? N9 Zn5 Zn3 158.25(15) . . ? N10 Zn5 Zn3 109.97(14) . . ? O7 Zn22 N16 123.3(2) . . ? O7 Zn22 N14 97.0(2) . . ? N16 Zn22 N14 117.1(2) . . ? O7 Zn22 N15 123.8(2) . . ? N16 Zn22 N15 84.4(2) . . ? N14 Zn22 N15 112.9(2) . . ? O7 Zn22 Zn3 35.31(13) . . ? N16 Zn22 Zn3 158.61(16) . . ? N14 Zn22 Zn3 75.38(13) . . ? N15 Zn22 Zn3 107.46(13) . . ? O3 Zn23 N8 118.8(2) . . ? O3 Zn23 N6 101.60(17) . . ? N8 Zn23 N6 116.5(3) . . ? O3 Zn23 N7 123.05(19) . . ? N8 Zn23 N7 83.6(3) . . ? N6 Zn23 N7 114.0(2) . . ? O3 Zn23 Zn2 37.26(11) . . ? N8 Zn23 Zn2 155.87(16) . . ? N6 Zn23 Zn2 75.91(14) . . ? N7 Zn23 Zn2 111.19(16) . . ? O8A C45 O8 72.2(4) . . ? O8A C45 C46 73.5(7) . . ? O8 C45 C46 113.4(6) . . ? O8A C45 C46A 127.9(12) . . ? O8 C45 C46A 79.3(10) . . ? C46 C45 C46A 158.5(11) . . ? O8A C45 C47 80.6(7) . . ? O8 C45 C47 107.2(6) . . ? C46 C45 C47 120.9(8) . . ? C46A C45 C47 67.3(9) . . ? O8A C45 C47A 107.2(10) . . ? O8 C45 C47A 86.3(9) . . ? C46 C45 C47A 53.2(9) . . ? C46A C45 C47A 113.6(7) . . ? C47 C45 C47A 166.1(10) . . ? O8A C45 C48A 81.1(11) . . ? O8 C45 C48A 152.1(11) . . ? C46 C45 C48A 64.7(9) . . ? C46A C45 C48A 112.4(7) . . ? C47 C45 C48A 59.3(9) . . ? C47A C45 C48A 109.7(6) . . ? O8A C45 C48 164.0(7) . . ? O8 C45 C48 92.5(6) . . ? C46 C45 C48 110.0(8) . . ? C46A C45 C48 50.3(10) . . ? C47 C45 C48 109.0(5) . . ? C47A C45 C48 66.3(9) . . ? C48A C45 C48 114.7(12) . . ? C45 O8 O7 108.4(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 O8A O7 108.9(6) . . ? C45 C47A H47D 109.5 . . ? C45 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C45 C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C45 C48A H48D 109.5 . . ? C45 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C45 C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? C45 C46A H46D 109.5 . . ? C45 C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? C45 C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C90 C89 C94 120.0 . . ? C90 C89 C88 120.8(4) . . ? C94 C89 C88 119.1(4) . . ? C91 C90 C89 120.0 . . ? C91 C90 H90 120.0 . . ? C89 C90 H90 120.0 . . ? C90 C91 C92 120.0 . . ? C90 C91 H91 120.0 . . ? C92 C91 H91 120.0 . . ? C93 C92 C91 120.0 . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C89 120.0 . . ? C93 C94 H94 120.0 . . ? C89 C94 H94 120.0 . . ? C89 C88 H88A 109.5 . . ? C89 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C89 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C90A C89A C94A 120.0 . . ? C90A C89A C88A 120.5(12) . . ? C94A C89A C88A 119.5(11) . . ? C89A C90A C91A 120.0 . . ? C89A C90A H90A 120.0 . . ? C91A C90A H90A 120.0 . . ? C92A C91A C90A 120.0 . . ? C92A C91A H91A 120.0 . . ? C90A C91A H91A 120.0 . . ? C91A C92A C93A 120.0 . . ? C91A C92A H92A 120.0 . . ? C93A C92A H92A 120.0 . . ? C94A C93A C92A 120.0 . . ? C94A C93A H93A 120.0 . . ? C92A C93A H93A 120.0 . . ? C93A C94A C89A 120.0 . . ? C93A C94A H94A 120.0 . . ? C89A C94A H94A 120.0 . . ? C89A C88A H88D 109.5 . . ? C89A C88A H88E 109.5 . . ? H88D C88A H88E 109.5 . . ? C89A C88A H88F 109.5 . . ? H88D C88A H88F 109.5 . . ? H88E C88A H88F 109.5 . . ? O2 O1 Zn2 104.9(4) . . ? O2 O1 Zn1 100.9(3) . . ? Zn2 O1 Zn1 103.3(2) . . ? C1 O2 O1 108.0(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2A O1A Zn1 102.0(9) . . ? O2A O1A Zn2 114.2(14) . . ? Zn1 O1A Zn2 107.1(8) . . ? C1 O2A O1A 105.8(11) . . ? C1 C2A H2A1 109.5 . . ? C1 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C1 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C1 C3A H3A1 109.5 . . ? C1 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C1 C4A H4A1 109.5 . . ? C1 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C1 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.72 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.733 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.101 # Attachment 'comp4_CCDC_696855.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 696855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 N12 O Zn4' _chemical_formula_weight 1076.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.1870(13) _cell_length_b 17.1310(12) _cell_length_c 19.3830(12) _cell_angle_alpha 90.00 _cell_angle_beta 122.651(3) _cell_angle_gamma 90.00 _cell_volume 6203.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 68064 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_measurement_details ; 259 frames, \w rotation 0.7\% per frame (184s per frame) 78 frames, \w rotation 0.7\% per frame (184s per frame) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5664 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 21.97 _reflns_number_total 3721 _reflns_number_gt 3093 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _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^)+(0.0561P)^2^+52.2726P] 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 3721 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1044(3) -0.0865(4) 0.7741(4) 0.0327(16) Uani 1 1 d . . . H1 H 0.0662 -0.1115 0.7743 0.039 Uiso 1 1 calc R . . C2 C 0.1684(4) -0.1223(4) 0.7975(4) 0.0390(17) Uani 1 1 d . . . H2 H 0.1817 -0.1747 0.8152 0.047 Uiso 1 1 calc R . . C3 C 0.2096(4) -0.0655(4) 0.7898(4) 0.0361(17) Uani 1 1 d . . . H3 H 0.2570 -0.0718 0.8021 0.043 Uiso 1 1 calc R . . C4 C 0.1693(3) 0.0004(4) 0.7614(4) 0.0308(16) Uani 1 1 d . . . C5 C 0.1781(3) 0.0759(4) 0.7346(4) 0.0299(16) Uani 1 1 d . . . C6 C 0.2435(4) 0.1024(4) 0.7353(4) 0.0407(18) Uani 1 1 d . . . H6A H 0.2504 0.0708 0.6973 0.049 Uiso 1 1 calc R . . H6B H 0.2872 0.0990 0.7910 0.049 Uiso 1 1 calc R . . C7 C 0.2259(4) 0.1871(4) 0.7066(4) 0.0425(18) Uani 1 1 d . . . H7A H 0.2338 0.1971 0.6617 0.051 Uiso 1 1 calc R . . H7B H 0.2560 0.2234 0.7523 0.051 Uiso 1 1 calc R . . C8 C 0.1459(3) 0.1970(4) 0.6760(4) 0.0355(16) Uani 1 1 d . . . H8A H 0.1387 0.2444 0.7000 0.043 Uiso 1 1 calc R . . H8B H 0.1163 0.2014 0.6156 0.043 Uiso 1 1 calc R . . C9 C -0.0628(4) -0.0299(4) 0.5667(4) 0.0441(19) Uani 1 1 d . . . H9A H -0.0957 -0.0434 0.5847 0.053 Uiso 1 1 calc R . . H9B H -0.0206 -0.0647 0.5954 0.053 Uiso 1 1 calc R . . C10 C -0.1002(4) -0.0399(5) 0.4752(4) 0.049(2) Uani 1 1 d . . . H10A H -0.0736 -0.0765 0.4616 0.059 Uiso 1 1 calc R . . H10B H -0.1495 -0.0599 0.4514 0.059 Uiso 1 1 calc R . . C11 C -0.1013(4) 0.0393(4) 0.4444(4) 0.0430(19) Uani 1 1 d . . . H11A H -0.1512 0.0570 0.4065 0.052 Uiso 1 1 calc R . . H11B H -0.0763 0.0398 0.4149 0.052 Uiso 1 1 calc R . . C12 C -0.0643(3) 0.0905(4) 0.5172(4) 0.0330(16) Uani 1 1 d . . . C13 C -0.0543(3) 0.1712(4) 0.5156(4) 0.0339(17) Uani 1 1 d . . . C14 C -0.0549(4) 0.2128(5) 0.4503(4) 0.0404(18) Uani 1 1 d . . . H14 H -0.0674 0.1926 0.3986 0.049 Uiso 1 1 calc R . . C15 C -0.0325(4) 0.2921(5) 0.4807(4) 0.049(2) Uani 1 1 d . . . H15 H -0.0244 0.3335 0.4540 0.059 Uiso 1 1 calc R . . C16 C -0.0250(3) 0.2951(4) 0.5586(4) 0.0391(18) Uani 1 1 d . . . H16 H -0.0131 0.3402 0.5920 0.047 Uiso 1 1 calc R . . C17 C -0.1052(4) 0.3627(4) 0.7125(4) 0.0408(18) Uani 1 1 d . . . H17 H -0.0600 0.3881 0.7422 0.049 Uiso 1 1 calc R . . C18 C -0.1686(4) 0.3928(5) 0.7012(5) 0.050(2) Uani 1 1 d . . . H18 H -0.1744 0.4411 0.7210 0.060 Uiso 1 1 calc R . . C19 C -0.2213(4) 0.3380(5) 0.6554(5) 0.051(2) Uani 1 1 d . . . H19 H -0.2704 0.3419 0.6374 0.061 Uiso 1 1 calc R . . C20 C -0.1891(4) 0.2760(4) 0.6403(4) 0.0375(18) Uani 1 1 d . . . C21 C -0.2151(4) 0.2042(4) 0.5982(4) 0.0368(17) Uani 1 1 d . . . C22 C -0.2911(4) 0.1764(5) 0.5552(4) 0.049(2) Uani 1 1 d . . . H22A H -0.3235 0.2114 0.5091 0.059 Uiso 1 1 calc R . . H22B H -0.3076 0.1730 0.5934 0.059 Uiso 1 1 calc R . . C23 C -0.2874(4) 0.0956(5) 0.5243(4) 0.051(2) Uani 1 1 d . . . H23A H -0.3203 0.0926 0.4640 0.061 Uiso 1 1 calc R . . H23B H -0.3010 0.0549 0.5496 0.061 Uiso 1 1 calc R . . C24 C -0.2098(4) 0.0843(5) 0.5487(4) 0.0424(18) Uani 1 1 d . . . H24A H -0.1888 0.0372 0.5833 0.051 Uiso 1 1 calc R . . H24B H -0.2072 0.0788 0.4996 0.051 Uiso 1 1 calc R . . O1 O 0.0000 0.1426(3) 0.7500 0.0274(14) Uani 1 2 d S . . Zn1 Zn 0.03926(4) 0.08132(4) 0.69794(4) 0.0269(2) Uani 1 1 d . . . Zn2 Zn -0.07098(4) 0.20298(4) 0.65454(4) 0.0279(2) Uani 1 1 d . . . N1 N 0.1024(3) -0.0122(3) 0.7510(3) 0.0282(12) Uani 1 1 d . . . N2 N 0.1268(3) 0.1273(3) 0.7030(3) 0.0284(13) Uani 1 1 d . . . N3 N -0.0411(3) 0.0496(3) 0.5855(3) 0.0294(13) Uani 1 1 d . . . N4 N -0.0381(3) 0.2206(3) 0.5780(3) 0.0287(13) Uani 1 1 d . . . N5 N -0.1171(3) 0.2926(3) 0.6752(3) 0.0329(13) Uani 1 1 d . . . N6 N -0.1713(3) 0.1558(3) 0.5955(3) 0.0335(14) 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 C1 0.032(4) 0.040(4) 0.025(4) 0.005(3) 0.015(3) 0.013(3) C2 0.052(5) 0.030(4) 0.042(4) 0.001(3) 0.030(4) 0.006(4) C3 0.030(4) 0.041(5) 0.030(4) -0.003(3) 0.012(3) 0.005(3) C4 0.033(4) 0.038(4) 0.022(4) -0.003(3) 0.014(3) 0.006(3) C5 0.028(4) 0.052(5) 0.012(3) -0.009(3) 0.011(3) -0.004(3) C6 0.031(4) 0.056(5) 0.040(4) -0.005(4) 0.022(4) 0.003(3) C7 0.045(4) 0.049(5) 0.040(4) -0.011(4) 0.027(4) -0.007(4) C8 0.036(4) 0.041(4) 0.038(4) 0.000(3) 0.026(4) 0.001(3) C9 0.033(4) 0.054(5) 0.034(4) -0.011(4) 0.010(4) 0.007(4) C10 0.036(4) 0.073(6) 0.035(4) -0.012(4) 0.016(4) 0.007(4) C11 0.045(4) 0.053(5) 0.025(4) -0.007(4) 0.016(4) 0.012(4) C12 0.028(4) 0.044(5) 0.026(4) -0.001(3) 0.014(3) 0.005(3) C13 0.025(4) 0.050(5) 0.026(4) 0.007(3) 0.014(3) 0.009(3) C14 0.037(4) 0.067(6) 0.017(4) 0.002(3) 0.014(3) 0.003(4) C15 0.038(4) 0.083(6) 0.033(4) 0.007(4) 0.023(4) 0.001(4) C16 0.033(4) 0.048(5) 0.039(4) 0.015(4) 0.022(4) 0.003(3) C17 0.047(5) 0.039(5) 0.041(4) 0.002(4) 0.026(4) 0.006(4) C18 0.060(5) 0.056(5) 0.044(5) 0.007(4) 0.035(4) 0.024(5) C19 0.046(5) 0.071(6) 0.042(5) 0.021(4) 0.028(4) 0.030(5) C20 0.033(4) 0.053(5) 0.033(4) 0.014(4) 0.022(4) 0.011(4) C21 0.032(4) 0.053(5) 0.025(4) 0.016(4) 0.015(3) 0.011(4) C22 0.037(4) 0.074(6) 0.030(4) 0.016(4) 0.014(4) 0.006(4) C23 0.033(4) 0.080(6) 0.031(4) 0.010(4) 0.011(4) -0.011(4) C24 0.032(4) 0.063(5) 0.023(4) 0.004(4) 0.009(3) -0.011(4) O1 0.032(3) 0.030(3) 0.024(3) 0.000 0.018(3) 0.000 Zn1 0.0248(4) 0.0345(5) 0.0217(4) -0.0016(3) 0.0126(3) 0.0006(3) Zn2 0.0257(4) 0.0371(5) 0.0207(4) 0.0022(3) 0.0124(3) 0.0038(3) N1 0.025(3) 0.040(4) 0.019(3) 0.000(2) 0.012(2) 0.001(3) N2 0.023(3) 0.041(3) 0.024(3) -0.001(3) 0.014(3) 0.000(3) N3 0.030(3) 0.032(3) 0.030(3) -0.004(3) 0.019(3) 0.002(3) N4 0.022(3) 0.041(4) 0.020(3) 0.000(3) 0.009(2) 0.003(2) N5 0.034(3) 0.040(4) 0.024(3) 0.006(3) 0.016(3) 0.009(3) N6 0.028(3) 0.050(4) 0.024(3) 0.010(3) 0.014(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(8) . ? C1 C2 1.380(9) . ? C1 H1 0.9500 . ? C2 C3 1.396(10) . ? C2 H2 0.9500 . ? C3 C4 1.359(9) . ? C3 H3 0.9500 . ? C4 N1 1.401(8) . ? C4 C5 1.447(9) . ? C5 N2 1.302(8) . ? C5 C6 1.513(9) . ? C6 C7 1.526(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.548(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N2 1.455(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N3 1.426(9) . ? C9 C10 1.509(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.477(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.478(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.332(8) . ? C12 C13 1.402(10) . ? C13 N4 1.356(8) . ? C13 C14 1.445(9) . ? C14 C15 1.458(11) . ? C14 H14 0.9500 . ? C15 C16 1.428(10) . ? C15 H15 0.9500 . ? C16 N4 1.404(9) . ? C16 H16 0.9500 . ? C17 N5 1.352(9) . ? C17 C18 1.401(10) . ? C17 H17 0.9500 . ? C18 C19 1.384(11) . ? C18 H18 0.9500 . ? C19 C20 1.396(10) . ? C19 H19 0.9500 . ? C20 N5 1.386(9) . ? C20 C21 1.416(10) . ? C21 N6 1.297(8) . ? C21 C22 1.500(10) . ? C22 C23 1.528(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.532(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N6 1.489(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O1 Zn1 1.956(3) . ? O1 Zn1 1.956(3) 2_556 ? O1 Zn2 1.957(3) 2_556 ? O1 Zn2 1.957(3) . ? Zn1 N3 2.008(5) . ? Zn1 N1 2.008(5) . ? Zn1 N2 2.048(5) . ? Zn1 Zn2 2.9688(10) . ? Zn2 N4 1.999(5) . ? Zn2 N5 2.002(5) . ? Zn2 N6 2.042(5) . ? 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 N1 C1 C2 111.9(6) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C1 C2 C3 105.9(6) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? C4 C3 C2 107.2(6) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 N1 110.2(6) . . ? C3 C4 C5 134.5(6) . . ? N1 C4 C5 115.1(5) . . ? N2 C5 C4 121.3(6) . . ? N2 C5 C6 113.1(6) . . ? C4 C5 C6 125.5(6) . . ? C5 C6 C7 103.1(6) . . ? C5 C6 H6A 111.1 . . ? C7 C6 H6A 111.1 . . ? C5 C6 H6B 111.1 . . ? C7 C6 H6B 111.1 . . ? H6A C6 H6B 109.1 . . ? C6 C7 C8 105.0(6) . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7B 110.8 . . ? C8 C7 H7B 110.8 . . ? H7A C7 H7B 108.8 . . ? N2 C8 C7 105.6(5) . . ? N2 C8 H8A 110.6 . . ? C7 C8 H8A 110.6 . . ? N2 C8 H8B 110.6 . . ? C7 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? N3 C9 C10 107.7(6) . . ? N3 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? N3 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C11 C10 C9 104.5(6) . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C10 C11 C12 106.3(6) . . ? C10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? C10 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N3 C12 C13 124.0(6) . . ? N3 C12 C11 110.7(6) . . ? C13 C12 C11 125.3(6) . . ? N4 C13 C12 124.3(6) . . ? N4 C13 C14 110.2(6) . . ? C12 C13 C14 125.3(6) . . ? C13 C14 C15 105.5(6) . . ? C13 C14 H14 127.3 . . ? C15 C14 H14 127.3 . . ? C16 C15 C14 106.2(7) . . ? C16 C15 H15 126.9 . . ? C14 C15 H15 126.9 . . ? N4 C16 C15 109.1(7) . . ? N4 C16 H16 125.4 . . ? C15 C16 H16 125.4 . . ? N5 C17 C18 110.7(7) . . ? N5 C17 H17 124.6 . . ? C18 C17 H17 124.6 . . ? C19 C18 C17 106.2(7) . . ? C19 C18 H18 126.9 . . ? C17 C18 H18 126.9 . . ? C18 C19 C20 107.5(7) . . ? C18 C19 H19 126.3 . . ? C20 C19 H19 126.3 . . ? N5 C20 C19 109.1(7) . . ? N5 C20 C21 117.6(6) . . ? C19 C20 C21 133.3(7) . . ? N6 C21 C20 119.8(6) . . ? N6 C21 C22 114.6(7) . . ? C20 C21 C22 125.6(6) . . ? C21 C22 C23 102.9(6) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C22 C23 C24 106.5(6) . . ? C22 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? C22 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? N6 C24 C23 105.2(6) . . ? N6 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? N6 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? Zn1 O1 Zn1 115.1(3) . 2_556 ? Zn1 O1 Zn2 114.59(3) . 2_556 ? Zn1 O1 Zn2 98.69(3) 2_556 2_556 ? Zn1 O1 Zn2 98.69(3) . . ? Zn1 O1 Zn2 114.59(3) 2_556 . ? Zn2 O1 Zn2 116.2(3) 2_556 . ? O1 Zn1 N3 108.86(14) . . ? O1 Zn1 N1 123.07(17) . . ? N3 Zn1 N1 107.8(2) . . ? O1 Zn1 N2 116.28(19) . . ? N3 Zn1 N2 114.8(2) . . ? N1 Zn1 N2 84.3(2) . . ? O1 Zn1 Zn2 40.66(8) . . ? N3 Zn1 Zn2 76.64(14) . . ? N1 Zn1 Zn2 161.03(14) . . ? N2 Zn1 Zn2 110.98(15) . . ? O1 Zn2 N4 110.58(15) . . ? O1 Zn2 N5 116.98(18) . . ? N4 Zn2 N5 117.6(2) . . ? O1 Zn2 N6 113.50(19) . . ? N4 Zn2 N6 111.6(2) . . ? N5 Zn2 N6 84.0(2) . . ? O1 Zn2 Zn1 40.65(8) . . ? N4 Zn2 Zn1 74.99(15) . . ? N5 Zn2 Zn1 156.02(15) . . ? N6 Zn2 Zn1 111.34(16) . . ? C1 N1 C4 104.8(5) . . ? C1 N1 Zn1 144.6(4) . . ? C4 N1 Zn1 110.1(4) . . ? C5 N2 C8 111.9(5) . . ? C5 N2 Zn1 109.2(4) . . ? C8 N2 Zn1 138.7(4) . . ? C12 N3 C9 110.7(5) . . ? C12 N3 Zn1 125.2(5) . . ? C9 N3 Zn1 121.0(4) . . ? C13 N4 C16 108.8(5) . . ? C13 N4 Zn2 122.7(4) . . ? C16 N4 Zn2 123.1(4) . . ? C17 N5 C20 106.5(6) . . ? C17 N5 Zn2 144.6(5) . . ? C20 N5 Zn2 108.9(5) . . ? C21 N6 C24 110.8(6) . . ? C21 N6 Zn2 109.7(5) . . ? C24 N6 Zn2 139.4(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.403 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.094