# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wenbin Lin' _publ_contact_author_email wlin@email.unc.edu loop_ _publ_author_name 'Wenbin Lin' 'Liang Wen' 'Peng Cheng' data_f _database_code_depnum_ccdc_archive 'CCDC 854460' #TrackingRef '1-cc-wl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.25 H15 N1.50 O4.50 Zn0.50' _chemical_formula_weight 360.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.3366(7) _cell_length_b 36.0309(18) _cell_length_c 7.0730(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3653.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8094 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 14408 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 50.37 _reflns_number_total 3340 _reflns_number_gt 2722 _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^)+(0.1000P)^2^+0.1490P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.96(8) _refine_ls_number_reflns 3340 _refine_ls_number_parameters 406 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 0.784 _refine_ls_restrained_S_all 0.787 _refine_ls_shift/su_max 0.129 _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 C22A C 0.0583(6) 0.4748(2) -0.424(6) 0.074(3) Uani 1 1 d . . . Zn1 Zn 0.50399(9) 0.28888(3) 0.435(5) 0.0953(17) Uani 1 1 d . . . C1A C 0.7710(6) 0.4055(2) 0.951(6) 0.085(3) Uani 1 1 d . . . C2A C 0.6981(6) 0.3839(3) 1.032(6) 0.084(3) Uani 1 1 d . . . H2A H 0.6838 0.3859 1.1601 0.101 Uiso 1 1 calc R . . C4A C 0.6676(6) 0.3566(2) 0.725(6) 0.077(3) Uani 1 1 d . . . C3A C 0.6479(6) 0.3595(2) 0.913(6) 0.086(3) Uani 1 1 d . . . H3A H 0.6004 0.3451 0.9643 0.103 Uiso 1 1 calc R . . C5A C 0.7378(6) 0.3782(2) 0.649(6) 0.086(3) Uani 1 1 d . . . H5A H 0.7498 0.3770 0.5197 0.103 Uiso 1 1 calc R . . C6A C 0.7911(7) 0.4019(3) 0.762(6) 0.087(3) Uani 1 1 d . . . H6A H 0.8402 0.4151 0.7095 0.105 Uiso 1 1 calc R . . C10A C 0.3421(6) 0.3575(3) 0.141(6) 0.094(4) Uani 1 1 d . . . C9A C 0.3465(6) 0.3558(3) -0.054(6) 0.088(3) Uani 1 1 d . . . H9A H 0.3851 0.3387 -0.1141 0.105 Uiso 1 1 calc R . . C8A C 0.2926(6) 0.3799(3) -0.156(6) 0.087(3) Uani 1 1 d . . . H8A H 0.2957 0.3783 -0.2868 0.105 Uiso 1 1 calc R . . C11A C 0.2872(7) 0.3851(3) 0.225(6) 0.104(4) Uani 1 1 d . . . H11A H 0.2855 0.3871 0.3564 0.125 Uiso 1 1 calc R . . C12A C 0.2360(6) 0.4092(3) 0.117(6) 0.093(3) Uani 1 1 d . . . H12A H 0.2018 0.4280 0.1753 0.111 Uiso 1 1 calc R . . C7A C 0.2349(6) 0.4059(3) -0.081(6) 0.080(3) Uani 1 1 d . . . C16A C 0.9349(6) 0.4767(2) 1.316(6) 0.073(3) Uani 1 1 d . . . C2B C 0.6124(7) 0.3307(3) 0.606(6) 0.094(4) Uani 1 1 d . . . C13A C 0.8267(6) 0.4300(2) 1.076(6) 0.078(3) Uani 1 1 d . . . C18A C 0.7875(6) 0.4500(2) 1.224(5) 0.082(3) Uani 1 1 d . . . H18A H 0.7237 0.4480 1.2463 0.098 Uiso 1 1 calc R . . C14A C 0.9220(6) 0.4349(2) 1.047(6) 0.075(3) Uani 1 1 d . . . H14A H 0.9507 0.4226 0.9469 0.091 Uiso 1 1 calc R . . C17A C 0.8407(5) 0.4729(2) 1.341(6) 0.077(3) Uani 1 1 d . . . H17A H 0.8116 0.4859 1.4386 0.092 Uiso 1 1 calc R . . C15A C 0.9753(5) 0.4575(2) 1.163(6) 0.076(3) Uani 1 1 d . . . H15A H 1.0388 0.4600 1.1400 0.092 Uiso 1 1 calc R . . O2A O 0.3938(4) 0.3339(2) 0.440(6) 0.109(3) Uani 1 1 d . . . O1A O 0.4426(5) 0.30596(18) 0.188(6) 0.102(3) Uani 1 1 d . . . O3A O 0.6182(4) 0.33352(18) 0.428(6) 0.098(3) Uani 1 1 d . . . O4A O 0.5629(5) 0.30739(18) 0.685(6) 0.099(3) Uani 1 1 d . . . C1B C 0.3946(6) 0.3318(3) 0.267(6) 0.085(3) Uani 1 1 d . . . C25A C 1.0000 0.5000 1.442(6) 0.075(3) Uani 1 2 d S . . C19A C 0.1752(6) 0.4304(3) -0.196(6) 0.078(3) Uani 1 1 d . . . C20A C 0.1641(5) 0.4675(2) -0.163(6) 0.076(3) Uani 1 1 d . . . H20A H 0.1959 0.4784 -0.0625 0.092 Uiso 1 1 calc R . . O1S O 0.4259(6) 0.2483(2) 0.557(6) 0.124(3) Uani 1 1 d . . . O2S O 0.5873(6) 0.2506(2) 0.310(6) 0.118(3) Uani 1 1 d . . . C21A C 0.1075(6) 0.4889(2) -0.273(6) 0.076(3) Uani 1 1 d . . . H21A H 0.1020 0.5141 -0.2457 0.091 Uiso 1 1 calc R . . C23A C 0.0685(6) 0.4361(2) -0.454(6) 0.084(3) Uani 1 1 d . . . H23A H 0.0367 0.4247 -0.5530 0.100 Uiso 1 1 calc R . . C24A C 0.1246(6) 0.4153(2) -0.339(6) 0.086(3) Uani 1 1 d . . . H24A H 0.1283 0.3899 -0.3600 0.104 Uiso 1 1 calc R . . C4S C 0.6138(10) 0.2557(4) 0.145(7) 0.138(6) Uani 1 1 d . . . H4S H 0.5993 0.2781 0.0867 0.166 Uiso 1 1 calc R . . C1S C 0.4116(8) 0.2478(3) 0.729(6) 0.112(4) Uani 1 1 d . . . H1S H 0.4316 0.2678 0.8020 0.134 Uiso 1 1 calc R . . C6S C 0.6921(11) 0.1953(3) 0.138(6) 0.191(9) Uani 1 1 d . . . H6S1 H 0.7299 0.2008 0.2462 0.286 Uiso 1 1 calc R . . H6S2 H 0.7276 0.1808 0.0494 0.286 Uiso 1 1 calc R . . H6S3 H 0.6381 0.1815 0.1766 0.286 Uiso 1 1 calc R . . C2S C 0.3271(13) 0.1888(4) 0.708(6) 0.198(9) Uani 1 1 d . . . H2S1 H 0.2688 0.1824 0.7668 0.297 Uiso 1 1 calc R . . H2S2 H 0.3684 0.1679 0.7130 0.297 Uiso 1 1 calc R . . H2S3 H 0.3164 0.1957 0.5792 0.297 Uiso 1 1 calc R . . C3S C 0.3510(14) 0.2204(5) 1.014(6) 0.223(11) Uani 1 1 d . . . H3S1 H 0.3884 0.2017 1.0736 0.334 Uiso 1 1 calc R . . H3S2 H 0.2862 0.2152 1.0349 0.334 Uiso 1 1 calc R . . H3S3 H 0.3661 0.2443 1.0659 0.334 Uiso 1 1 calc R . . N1S N 0.3698(8) 0.2205(3) 0.811(6) 0.140(4) Uani 1 1 d . . . N2S N 0.6623(8) 0.2304(4) 0.046(6) 0.154(5) Uani 1 1 d . . . C5S C 0.6874(15) 0.2342(6) -0.163(6) 0.226(11) Uani 1 1 d . . . H5S1 H 0.7150 0.2581 -0.1856 0.339 Uiso 1 1 calc R . . H5S2 H 0.6320 0.2317 -0.2385 0.339 Uiso 1 1 calc R . . H5S3 H 0.7310 0.2151 -0.1975 0.339 Uiso 1 1 calc R . . C7S C 0.507(4) 0.5663(14) 0.333(8) 0.49(3) Uiso 1 1 d DU . . C10S C 0.6227(16) 0.5209(6) 0.494(6) 0.230(9) Uiso 1 1 d . . . C8S C 0.515(5) 0.5382(16) -0.012(9) 0.67(4) Uiso 1 1 d DU . . C9S C 0.610(3) 0.5145(12) 0.257(8) 0.45(2) Uiso 1 1 d DU . . O3S O 0.517(2) 0.5618(9) 0.504(7) 0.427(16) Uiso 1 1 d DU . . N3S N 0.547(3) 0.5444(13) 0.184(7) 0.55(2) Uiso 1 1 d DU . . O10 O 0.4953 0.1542 0.9422 0.686 Uiso 1 1 d . . . O11 O 0.5050 0.1615 0.4517 0.977 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 C22A 0.077(5) 0.067(5) 0.078(7) 0.002(5) -0.001(5) 0.001(4) Zn1 0.1037(18) 0.0812(17) 0.1010(19) 0.0035(10) -0.0254(6) -0.0030(7) C1A 0.077(5) 0.083(6) 0.095(10) 0.009(7) -0.010(7) -0.004(4) C2A 0.079(5) 0.090(6) 0.083(7) -0.002(6) -0.001(6) 0.001(5) C4A 0.091(6) 0.074(6) 0.065(8) -0.008(5) -0.017(6) -0.006(5) C3A 0.082(5) 0.077(6) 0.099(10) 0.024(7) -0.013(7) -0.010(4) C5A 0.094(6) 0.095(6) 0.067(7) -0.013(6) -0.009(6) -0.009(5) C6A 0.086(6) 0.097(7) 0.078(8) 0.001(5) -0.002(6) -0.004(5) C10A 0.072(6) 0.090(7) 0.121(11) -0.009(7) -0.004(7) 0.004(5) C9A 0.099(6) 0.095(7) 0.070(8) -0.003(7) -0.016(7) 0.008(5) C8A 0.096(6) 0.095(7) 0.070(7) -0.006(6) -0.007(6) 0.021(5) C11A 0.105(7) 0.120(8) 0.088(8) 0.002(7) 0.004(6) 0.002(7) C12A 0.088(6) 0.104(7) 0.087(9) 0.003(6) -0.005(5) 0.033(5) C7A 0.095(6) 0.090(6) 0.057(8) 0.007(6) -0.006(6) 0.005(5) C16A 0.073(5) 0.085(6) 0.059(6) 0.007(5) -0.001(5) 0.000(5) C2B 0.094(7) 0.079(7) 0.110(12) 0.000(7) -0.010(7) 0.002(6) C13A 0.086(6) 0.078(6) 0.070(7) 0.006(5) -0.005(6) -0.007(5) C18A 0.080(5) 0.082(5) 0.084(7) -0.002(5) 0.004(5) -0.004(4) C14A 0.085(6) 0.075(5) 0.067(5) -0.005(4) -0.001(5) -0.011(4) C17A 0.079(5) 0.081(5) 0.070(6) -0.009(4) 0.005(4) 0.003(4) C15A 0.065(5) 0.086(5) 0.078(6) 0.002(5) 0.005(5) 0.002(4) O2A 0.113(5) 0.114(6) 0.100(7) 0.013(6) -0.021(5) 0.006(4) O1A 0.102(5) 0.084(4) 0.119(7) -0.001(5) -0.029(5) 0.009(4) O3A 0.098(4) 0.106(5) 0.091(7) -0.013(5) -0.006(5) -0.017(3) O4A 0.109(5) 0.086(4) 0.104(6) 0.009(4) -0.020(4) -0.016(4) C1B 0.078(6) 0.089(8) 0.088(10) -0.004(7) -0.017(6) 0.001(5) C25A 0.082(6) 0.071(5) 0.071(6) 0.000 0.000 0.009(7) C19A 0.072(5) 0.089(6) 0.073(7) 0.002(6) -0.005(5) 0.003(5) C20A 0.078(5) 0.087(6) 0.065(5) 0.002(5) -0.004(4) 0.003(4) O1S 0.140(7) 0.108(6) 0.124(7) 0.008(6) -0.016(6) -0.023(5) O2S 0.121(6) 0.097(5) 0.136(8) 0.007(6) -0.008(6) 0.017(4) C21A 0.083(5) 0.076(5) 0.069(6) -0.003(5) 0.004(5) 0.000(4) C23A 0.091(6) 0.093(6) 0.067(6) -0.003(5) -0.008(5) -0.002(5) C24A 0.095(6) 0.078(5) 0.086(7) 0.009(5) 0.000(6) 0.011(5) C4S 0.129(10) 0.100(9) 0.186(18) 0.014(11) 0.004(12) 0.017(8) C1S 0.107(8) 0.087(7) 0.141(13) -0.018(8) 0.007(8) -0.036(6) C6S 0.210(15) 0.126(10) 0.24(2) 0.071(13) 0.053(15) 0.085(10) C2S 0.253(18) 0.184(14) 0.156(15) -0.033(12) 0.058(14) -0.112(14) C3S 0.25(2) 0.27(2) 0.148(16) -0.106(14) 0.069(14) -0.150(18) N1S 0.166(9) 0.126(8) 0.128(10) -0.017(7) 0.017(8) -0.046(8) N2S 0.132(8) 0.160(10) 0.171(12) 0.052(9) 0.029(8) 0.038(8) C5S 0.25(2) 0.26(2) 0.168(18) 0.081(16) 0.084(16) 0.117(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C22A C21A 1.375(12) . ? C22A C23A 1.419(11) . ? C22A C25A 1.558(16) 1_453 ? Zn1 O1S 2.034(10) . ? Zn1 O2S 2.029(10) . ? Zn1 O1A 2.049(7) . ? Zn1 O4A 2.072(7) . ? Zn1 O2A 2.266(7) . ? Zn1 O3A 2.296(6) . ? Zn1 C2B 2.478(12) . ? Zn1 C1B 2.502(11) . ? C1A C6A 1.375(15) . ? C1A C2A 1.423(13) . ? C1A C13A 1.481(13) . ? C2A C3A 1.416(15) . ? C4A C5A 1.381(14) . ? C4A C3A 1.366(15) . ? C4A C2B 1.486(15) . ? C5A C6A 1.397(13) . ? C10A C11A 1.401(15) . ? C10A C9A 1.383(17) . ? C10A C1B 1.489(16) . ? C9A C8A 1.368(13) . ? C8A C7A 1.357(13) . ? C11A C12A 1.371(14) . ? C12A C7A 1.408(15) . ? C7A C19A 1.476(12) . ? C16A C17A 1.368(11) . ? C16A C15A 1.409(12) . ? C16A C25A 1.538(16) . ? C2B O4A 1.235(13) . ? C2B O3A 1.267(16) . ? C13A C18A 1.391(12) . ? C13A C14A 1.393(11) . ? C18A C17A 1.396(11) . ? C14A C15A 1.387(12) . ? O2A C1B 1.223(14) . ? O1A C1B 1.284(12) . ? C25A C16A 1.538(16) 2_765 ? C25A C22A 1.558(16) 2_667 ? C25A C22A 1.558(16) 1_657 ? C19A C24A 1.358(13) . ? C19A C20A 1.368(11) . ? C20A C21A 1.366(11) . ? O1S C1S 1.235(16) . ? O2S C4S 1.239(19) . ? C23A C24A 1.365(11) . ? C4S N2S 1.341(18) . ? C1S N1S 1.290(15) . ? C6S N2S 1.484(16) . ? C2S N1S 1.486(17) . ? C3S N1S 1.46(2) . ? N2S C5S 1.53(2) . ? C7S O3S 1.23(2) . ? C7S N3S 1.433(19) . ? C10S C9S 1.70(4) . ? C8S N3S 1.48(2) . ? C9S N3S 1.49(2) . ? 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 C21A C22A C23A 115.4(8) . . ? C21A C22A C25A 122.1(8) . 1_453 ? C23A C22A C25A 122.4(10) . 1_453 ? O1S Zn1 O2S 91.2(3) . . ? O1S Zn1 O1A 109.9(4) . . ? O2S Zn1 O1A 94.9(4) . . ? O1S Zn1 O4A 95.3(4) . . ? O2S Zn1 O4A 110.7(4) . . ? O1A Zn1 O4A 143.7(2) . . ? O1S Zn1 O2A 97.2(3) . . ? O2S Zn1 O2A 154.7(4) . . ? O1A Zn1 O2A 59.8(3) . . ? O4A Zn1 O2A 92.3(3) . . ? O1S Zn1 O3A 155.0(4) . . ? O2S Zn1 O3A 92.7(3) . . ? O1A Zn1 O3A 94.4(3) . . ? O4A Zn1 O3A 60.2(3) . . ? O2A Zn1 O3A 89.7(2) . . ? O1S Zn1 C2B 125.1(5) . . ? O2S Zn1 C2B 104.9(4) . . ? O1A Zn1 C2B 120.1(4) . . ? O4A Zn1 C2B 29.8(4) . . ? O2A Zn1 C2B 89.7(3) . . ? O3A Zn1 C2B 30.5(4) . . ? O1S Zn1 C1B 107.5(3) . . ? O2S Zn1 C1B 125.5(5) . . ? O1A Zn1 C1B 30.8(4) . . ? O4A Zn1 C1B 117.5(3) . . ? O2A Zn1 C1B 29.2(3) . . ? O3A Zn1 C1B 90.2(3) . . ? C2B Zn1 C1B 104.4(3) . . ? C6A C1A C2A 119.5(10) . . ? C6A C1A C13A 121.6(9) . . ? C2A C1A C13A 118.8(12) . . ? C3A C2A C1A 118.4(12) . . ? C5A C4A C3A 119.2(9) . . ? C5A C4A C2B 121.5(12) . . ? C3A C4A C2B 119.3(11) . . ? C4A C3A C2A 121.5(10) . . ? C4A C5A C6A 121.2(11) . . ? C1A C6A C5A 120.2(10) . . ? C11A C10A C9A 118.7(12) . . ? C11A C10A C1B 118.2(14) . . ? C9A C10A C1B 123.1(11) . . ? C8A C9A C10A 118.2(11) . . ? C9A C8A C7A 125.3(12) . . ? C12A C11A C10A 121.0(13) . . ? C11A C12A C7A 120.5(10) . . ? C8A C7A C12A 116.1(10) . . ? C8A C7A C19A 123.5(11) . . ? C12A C7A C19A 120.4(10) . . ? C17A C16A C15A 117.1(8) . . ? C17A C16A C25A 125.3(9) . . ? C15A C16A C25A 117.5(8) . . ? O4A C2B O3A 123.1(11) . . ? O4A C2B C4A 118.4(14) . . ? O3A C2B C4A 118.5(12) . . ? O4A C2B Zn1 56.6(6) . . ? O3A C2B Zn1 66.8(6) . . ? C4A C2B Zn1 172.8(10) . . ? C18A C13A C14A 116.2(8) . . ? C18A C13A C1A 122.7(8) . . ? C14A C13A C1A 121.1(9) . . ? C13A C18A C17A 122.2(8) . . ? C15A C14A C13A 121.8(8) . . ? C16A C17A C18A 121.4(8) . . ? C14A C15A C16A 121.2(7) . . ? C1B O2A Zn1 86.2(7) . . ? C1B O1A Zn1 94.5(8) . . ? C2B O3A Zn1 82.7(7) . . ? C2B O4A Zn1 93.6(8) . . ? O2A C1B O1A 119.0(11) . . ? O2A C1B C10A 123.5(11) . . ? O1A C1B C10A 117.5(13) . . ? O2A C1B Zn1 64.6(6) . . ? O1A C1B Zn1 54.7(5) . . ? C10A C1B Zn1 170.1(9) . . ? C16A C25A C16A 109.4(16) . 2_765 ? C16A C25A C22A 110.2(4) . 2_667 ? C16A C25A C22A 111.1(4) 2_765 2_667 ? C16A C25A C22A 111.1(4) . 1_657 ? C16A C25A C22A 110.2(4) 2_765 1_657 ? C22A C25A C22A 104.8(15) 2_667 1_657 ? C24A C19A C20A 117.3(8) . . ? C24A C19A C7A 118.8(9) . . ? C20A C19A C7A 123.8(9) . . ? C21A C20A C19A 121.5(8) . . ? C1S O1S Zn1 121.3(9) . . ? C4S O2S Zn1 119.4(10) . . ? C20A C21A C22A 122.6(8) . . ? C24A C23A C22A 120.6(8) . . ? C19A C24A C23A 122.6(8) . . ? O2S C4S N2S 123.1(15) . . ? O1S C1S N1S 122.1(13) . . ? C1S N1S C3S 122.0(14) . . ? C1S N1S C2S 123.9(14) . . ? C3S N1S C2S 113.7(13) . . ? C4S N2S C5S 124.4(15) . . ? C4S N2S C6S 120.2(15) . . ? C5S N2S C6S 115.4(15) . . ? O3S C7S N3S 127(3) . . ? C10S C9S N3S 108(3) . . ? C7S N3S C9S 113(3) . . ? C7S N3S C8S 130(3) . . ? C9S N3S C8S 114(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 50.37 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.037 _refine_diff_density_min -0.027 _refine_diff_density_rms 0.006 # Attachment '2-cc-wl.cif' data_p21212f _database_code_depnum_ccdc_archive 'CCDC 854461' #TrackingRef '2-cc-wl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.83 H0 O1.67 Zn0.33' _chemical_formula_weight 154.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 26.9842(8) _cell_length_b 31.2626(7) _cell_length_c 7.2309(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6100.0(3) _cell_formula_units_Z 24 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7759 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 2310 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 35.48 _reflns_number_total 2310 _reflns_number_gt 1931 _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^)+(0.1000P)^2^+1.0359P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _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 0.11(13) _refine_ls_number_reflns 2310 _refine_ls_number_parameters 174 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2466 _refine_ls_wR_factor_gt 0.2399 _refine_ls_goodness_of_fit_ref 1.726 _refine_ls_restrained_S_all 1.709 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0489(5) 0.3444(4) 1.653(2) 0.045(8) Uiso 1 1 d GU . . C2 C 0.0640(5) 0.3385(4) 1.835(2) 0.007(7) Uiso 1 1 d GU . . C6 C 0.1035(6) 0.3620(5) 1.9045(15) 0.011(7) Uiso 1 1 d GU . . C5 C 0.1280(5) 0.3913(4) 1.792(2) 0.018(7) Uiso 1 1 d GU . . C3 C 0.1128(6) 0.3972(4) 1.610(2) 0.015(7) Uiso 1 1 d GU . . C4 C 0.0733(6) 0.3738(5) 1.5406(15) 0.029(7) Uiso 1 1 d GU . . Zn1 Zn 0.03200(12) 0.76214(9) -0.0002(4) 0.0272(13) Uani 1 1 d . . . Zn2 Zn -0.04674(18) 0.76906(12) -0.3073(5) 0.090(2) Uani 1 1 d . . . O6 O -0.0651(8) 0.8204(5) -0.140(3) 0.090(7) Uiso 1 1 d DU . . O10 O -0.0468(7) 0.6935(5) 0.113(2) 0.065(6) Uiso 1 1 d U . . O11 O -0.0408(8) 0.7501(5) -0.573(2) 0.099(8) Uiso 1 1 d . . . O13 O 0.0491(7) 0.7412(5) 0.267(2) 0.054(5) Uiso 1 1 d U . . O14 O 0.0789(6) 0.7033(4) 0.051(2) 0.049(6) Uiso 1 1 d U . . O16 O 0.4253(8) 0.2982(6) 0.138(3) 0.083(7) Uiso 1 1 d DU . . O17 O 0.4790(9) 0.3009(6) 0.356(3) 0.091(7) Uiso 1 1 d DU . . O18 O -0.1347(9) 0.7597(7) -0.356(3) 0.161(10) Uiso 1 1 d . . . C35 C -0.0394(10) 0.6932(7) -0.055(3) 0.033(8) Uiso 1 1 d U . . C8 C 0.2016(5) 0.5359(4) 0.9777(18) 0.020(7) Uiso 1 1 d GU . . C9 C 0.1725(5) 0.5171(3) 0.841(2) 0.015(7) Uiso 1 1 d GU . . C10 C 0.1455(5) 0.5427(5) 0.7206(16) 0.012(7) Uiso 1 1 d GU . . C11 C 0.1476(5) 0.5870(4) 0.7361(18) 0.005(6) Uiso 1 1 d GU . . C12 C 0.1767(6) 0.6057(3) 0.872(2) 0.028(7) Uiso 1 1 d GU . . C13 C 0.2037(5) 0.5802(5) 0.9932(17) 0.009(6) Uiso 1 1 d GU . . O1 O -0.0169(6) 0.7249(4) -0.1275(17) 0.024(5) Uiso 1 1 d U . . C14 C 0.1229(5) 0.6173(4) 0.598(2) 0.036(8) Uiso 1 1 d GU . . C15 C 0.1206(6) 0.6085(4) 0.410(3) 0.044(8) Uiso 1 1 d GU . . C16 C 0.1025(6) 0.6390(5) 0.2876(17) 0.052(9) Uiso 1 1 d GU . . C50 C 0.0866(6) 0.6784(4) 0.354(2) 0.027(7) Uiso 1 1 d GU . . C18 C 0.0888(5) 0.6873(4) 0.542(2) 0.042(8) Uiso 1 1 d GU . . C19 C 0.1070(6) 0.6568(5) 0.6640(16) 0.020(7) Uiso 1 1 d GU . . C51 C 0.0714(10) 0.7093(8) 0.215(4) 0.036(8) Uiso 1 1 d U . . C20 C 0.2610(5) 0.4721(5) 0.9733(19) 0.027(7) Uiso 1 1 d GU . . C21 C 0.2646(5) 0.4284(5) 1.0049(18) 0.017(7) Uiso 1 1 d GU . . C22 C 0.2937(6) 0.4031(3) 0.890(2) 0.028(7) Uiso 1 1 d GU . . C40 C 0.3191(5) 0.4216(5) 0.7428(19) 0.023(7) Uiso 1 1 d GU . . C39 C 0.3155(5) 0.4654(5) 0.7112(17) 0.013(7) Uiso 1 1 d GU . . C24 C 0.2864(6) 0.4906(3) 0.826(2) 0.024(7) Uiso 1 1 d GU . . C7 C 0.2298(9) 0.5048(6) 1.099(3) 0.015(7) Uiso 1 1 d U . . C30 C 0.1971(7) 0.4769(4) 1.2378(19) 0.026(7) Uiso 1 1 d GU . . C45 C 0.1460(7) 0.4732(4) 1.2169(17) 0.022(7) Uiso 1 1 d GU . . C32 C 0.1189(4) 0.4480(5) 1.339(2) 0.024 Uiso 1 1 d GU . . C33 C 0.1429(6) 0.4264(4) 1.4810(19) 0.013(6) Uiso 1 1 d GU . . C34 C 0.1939(6) 0.4301(4) 1.5019(16) 0.011(6) Uiso 1 1 d GU . . C31 C 0.2210(4) 0.4554(5) 1.380(2) 0.010(7) Uiso 1 1 d GU . . C61 C 0.4371(13) 0.3110(9) 0.277(5) 0.083(11) Uiso 1 1 d DU . . C25 C 0.2667(6) 0.5298(4) 1.2333(19) 0.004(6) Uiso 1 1 d GU . . C26 C 0.3178(6) 0.5293(4) 1.2085(16) 0.002(6) Uiso 1 1 d GU . . C43 C 0.3482(4) 0.5523(5) 1.328(2) 0.013(7) Uiso 1 1 d GU . . C42 C 0.3275(6) 0.5757(4) 1.4718(18) 0.019(7) Uiso 1 1 d GU . . C44 C 0.2764(6) 0.5762(4) 1.4966(16) 0.026(7) Uiso 1 1 d GU . . C29 C 0.2460(4) 0.5532(5) 1.377(2) 0.002(6) Uiso 1 1 d GU . . O2 O -0.0135(7) 0.8059(5) 0.096(2) 0.049(6) Uiso 1 1 d DU . . C52 C 0.3752(7) 0.6303(5) 1.9124(16) 0.024(8) Uiso 1 1 d GU . . C53 C 0.3454(5) 0.6060(5) 1.796(3) 0.034(8) Uiso 1 1 d GU . . C55 C 0.3595(6) 0.5993(4) 1.613(2) 0.034(8) Uiso 1 1 d GU . . C54 C 0.4033(7) 0.6170(5) 1.5471(16) 0.030(7) Uiso 1 1 d GU . . C38 C 0.4331(5) 0.6413(4) 1.664(3) 0.030(7) Uiso 1 1 d GU . . C65 C 0.4190(6) 0.6480(4) 1.846(2) 0.044(8) Uiso 1 1 d GU . . C75 C -0.0434(11) 0.8232(9) 0.021(4) 0.079(10) Uiso 1 1 d DU . . C56 C 0.4140(6) 0.3383(5) 0.588(3) 0.098(11) Uiso 1 1 d GU . . C57 C 0.3861(9) 0.3663(8) 0.6951(19) 0.104(12) Uiso 1 1 d GU . . C58 C 0.3530(7) 0.3942(5) 0.611(3) 0.067(9) Uiso 1 1 d GU . . C49 C 0.3477(6) 0.3942(5) 0.420(3) 0.046(9) Uiso 1 1 d GU . . C62 C 0.3757(8) 0.3663(7) 0.3126(19) 0.054(9) Uiso 1 1 d GU . . C63 C 0.4088(6) 0.3383(5) 0.397(3) 0.043(8) Uiso 1 1 d GU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.035(3) 0.0230(18) 0.024(2) 0.007(2) 0.006(2) 0.004(2) Zn2 0.128(6) 0.080(3) 0.063(3) -0.012(3) 0.006(3) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 C4 1.3900 . ? C2 C6 1.3900 . ? C2 C35 1.44(2) 2_567 ? C6 C5 1.3900 . ? C5 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C33 1.538(14) . ? Zn1 O16 1.90(2) 3 ? Zn1 O2 1.966(18) . ? Zn1 O1 1.985(14) . ? Zn1 O13 2.088(15) . ? Zn1 O14 2.264(16) . ? Zn1 C51 2.51(2) . ? Zn2 O11 2.014(17) . ? Zn2 O1 2.061(14) . ? Zn2 O6 2.070(18) . ? Zn2 O17 2.11(2) 3 ? Zn2 O18 2.42(3) . ? O6 C75 1.31(3) . ? O10 C35 1.23(2) . ? O13 C51 1.22(2) . ? O14 C51 1.22(2) . ? O16 C61 1.13(3) . ? O16 Zn1 1.90(2) 3_545 ? O17 C61 1.30(3) . ? O17 Zn2 2.11(2) 3_545 ? C35 O1 1.28(2) . ? C35 C2 1.44(12) 2_563 ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C8 C7 1.52(2) . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C11 C14 1.531(14) . ? C12 C13 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C50 1.3900 . ? C50 C18 1.3900 . ? C50 C51 1.45(2) . ? C18 C19 1.3900 . ? C20 C21 1.3900 . ? C20 C24 1.3900 . ? C20 C7 1.61(2) . ? C21 C22 1.3900 . ? C22 C40 1.3900 . ? C40 C39 1.3900 . ? C40 C58 1.573(16) . ? C39 C24 1.3900 . ? C7 C25 1.59(2) . ? C7 C30 1.59(2) . ? C30 C45 1.3900 . ? C30 C31 1.3900 . ? C45 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C31 1.3900 . ? C61 C63 1.44(3) . ? C25 C26 1.3900 . ? C25 C29 1.3900 . ? C26 C43 1.3900 . ? C43 C42 1.3900 . ? C42 C44 1.3900 . ? C42 C55 1.528(15) . ? C44 C29 1.3900 . ? O2 C75 1.11(3) . ? C52 C53 1.3900 . ? C52 C65 1.3900 . ? C53 C55 1.3900 . ? C55 C54 1.3900 . ? C54 C38 1.3900 . ? C38 C65 1.3900 . ? C65 C75 1.66(3) 4_567 ? C75 C65 1.66(13) 4_467 ? C56 C57 1.3900 . ? C56 C63 1.3900 . ? C57 C58 1.3900 . ? C58 C49 1.3900 . ? C49 C62 1.3900 . ? C62 C63 1.3900 . ? 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 C2 C1 C4 120.0 . . ? C1 C2 C6 120.0 . . ? C1 C2 C35 118.9(16) . 2_567 ? C6 C2 C35 121.1(16) . 2_567 ? C2 C6 C5 120.0 . . ? C3 C5 C6 120.0 . . ? C5 C3 C4 120.0 . . ? C5 C3 C33 120.0(13) . . ? C4 C3 C33 119.8(13) . . ? C3 C4 C1 120.0 . . ? O16 Zn1 O2 98.7(8) 3 . ? O16 Zn1 O1 120.6(7) 3 . ? O2 Zn1 O1 99.1(7) . . ? O16 Zn1 O13 122.5(8) 3 . ? O2 Zn1 O13 91.7(7) . . ? O1 Zn1 O13 113.1(6) . . ? O16 Zn1 O14 103.3(8) 3 . ? O2 Zn1 O14 149.0(7) . . ? O1 Zn1 O14 88.3(6) . . ? O13 Zn1 O14 58.1(6) . . ? O16 Zn1 C51 117.5(9) 3 . ? O2 Zn1 C51 120.3(8) . . ? O1 Zn1 C51 100.5(7) . . ? O13 Zn1 C51 29.1(6) . . ? O14 Zn1 C51 29.1(6) . . ? O11 Zn2 O1 111.8(6) . . ? O11 Zn2 O6 143.4(8) . . ? O1 Zn2 O6 104.2(7) . . ? O11 Zn2 O17 84.9(8) . 3 ? O1 Zn2 O17 94.8(7) . 3 ? O6 Zn2 O17 86.5(8) . 3 ? O11 Zn2 O18 84.5(9) . . ? O1 Zn2 O18 113.3(7) . . ? O6 Zn2 O18 86.8(8) . . ? O17 Zn2 O18 152.0(8) 3 . ? C75 O6 Zn2 117.6(19) . . ? C51 O13 Zn1 94.7(16) . . ? C51 O14 Zn1 86.6(16) . . ? C61 O16 Zn1 120(3) . 3_545 ? C61 O17 Zn2 142(2) . 3_545 ? O10 C35 O1 119(2) . . ? O10 C35 C2 119(6) . 2_563 ? O1 C35 C2 122(6) . 2_563 ? C9 C8 C13 120.0 . . ? C9 C8 C7 115.2(13) . . ? C13 C8 C7 124.8(13) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 C14 116.6(12) . . ? C10 C11 C14 123.2(12) . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C35 O1 Zn1 125.5(14) . . ? C35 O1 Zn2 126.4(16) . . ? Zn1 O1 Zn2 99.1(6) . . ? C15 C14 C19 120.0 . . ? C15 C14 C11 122.3(13) . . ? C19 C14 C11 117.4(13) . . ? C16 C15 C14 120.0 . . ? C15 C16 C50 120.0 . . ? C16 C50 C18 120.0 . . ? C16 C50 C51 116.0(16) . . ? C18 C50 C51 123.9(16) . . ? C19 C18 C50 120.0 . . ? C18 C19 C14 120.0 . . ? O14 C51 O13 120(2) . . ? O14 C51 C50 122(2) . . ? O13 C51 C50 118(2) . . ? O14 C51 Zn1 64.3(14) . . ? O13 C51 Zn1 56.1(13) . . ? C50 C51 Zn1 170.9(18) . . ? C21 C20 C24 120.0 . . ? C21 C20 C7 124.7(13) . . ? C24 C20 C7 115.3(13) . . ? C22 C21 C20 120.0 . . ? C21 C22 C40 120.0 . . ? C39 C40 C22 120.0 . . ? C39 C40 C58 118.5(14) . . ? C22 C40 C58 121.5(14) . . ? C40 C39 C24 120.0 . . ? C39 C24 C20 120.0 . . ? C8 C7 C25 110.6(14) . . ? C8 C7 C30 115.9(18) . . ? C25 C7 C30 103.5(14) . . ? C8 C7 C20 109.9(15) . . ? C25 C7 C20 109.3(17) . . ? C30 C7 C20 107.4(13) . . ? C45 C30 C31 120.0 . . ? C45 C30 C7 121.8(16) . . ? C31 C30 C7 118.2(16) . . ? C30 C45 C32 120.0 . . ? C33 C32 C45 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 C3 119.6(14) . . ? C34 C33 C3 120.4(14) . . ? C33 C34 C31 120.0 . . ? C34 C31 C30 120.0 . . ? O16 C61 O17 123(3) . . ? O16 C61 C63 127(4) . . ? O17 C61 C63 110(3) . . ? C26 C25 C29 120.0 . . ? C26 C25 C7 122.4(15) . . ? C29 C25 C7 117.6(16) . . ? C43 C26 C25 120.0 . . ? C42 C43 C26 120.0 . . ? C43 C42 C44 120.0 . . ? C43 C42 C55 122.0(15) . . ? C44 C42 C55 117.9(14) . . ? C29 C44 C42 120.0 . . ? C44 C29 C25 120.0 . . ? C75 O2 Zn1 128(2) . . ? C53 C52 C65 120.0 . . ? C55 C53 C52 120.0 . . ? C53 C55 C54 120.0 . . ? C53 C55 C42 123.7(15) . . ? C54 C55 C42 116.2(15) . . ? C38 C54 C55 120.0 . . ? C54 C38 C65 120.0 . . ? C38 C65 C52 120.0 . . ? C38 C65 C75 117.6(18) . 4_567 ? C52 C65 C75 122.4(18) . 4_567 ? O2 C75 O6 137(3) . . ? O2 C75 C65 115(7) . 4_467 ? O6 C75 C65 106(7) . 4_467 ? C57 C56 C63 120.0 . . ? C56 C57 C58 120.0 . . ? C49 C58 C57 120.0 . . ? C49 C58 C40 123.0(19) . . ? C57 C58 C40 116.8(19) . . ? C58 C49 C62 120.0 . . ? C63 C62 C49 120.0 . . ? C62 C63 C56 120.0 . . ? C62 C63 C61 117(2) . . ? C56 C63 C61 123(2) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 35.48 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 1.197 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.095