Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal SOciety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Zinc(II) Coordination Architectures with Two Bulky Anthracene-Based Carboxylic Ligands: Crystal Structures, Photoluminescent Properties, and Aromatic Skeleton Effect ; loop_ _publ_author_name 'Xian-He Bu' 'Ze Chang' 'Pei-Quan Chen' 'Cai-Yun Li' 'Zheng-Ming Li' ; Chun-Sen Liu ; 'Jun-Jie Wang' 'Zhe Wang' 'Qiang Wu' 'Li-Fen Yan' 'Xinzheng Zhang' ; Li-Juan Zhao ; #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 617255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C140 H90 N4 O18 Zn5' _chemical_formula_weight 2443.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.013(2) _cell_length_b 15.329(3) _cell_length_c 15.464(3) _cell_angle_alpha 67.147(2) _cell_angle_beta 65.165(2) _cell_angle_gamma 83.999(3) _cell_volume 2771.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5487 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 26.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8039 _exptl_absorpt_correction_T_max 0.8752 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13974 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9665 _reflns_number_gt 7000 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+12.2344P] 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 9665 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.0000 0.5000 0.0304(2) Uani 1 2 d S . . Zn2 Zn 0.70393(5) -0.06388(5) 0.32557(5) 0.03191(19) Uani 1 1 d . . . Zn3 Zn 0.74976(6) 0.02687(5) 0.46913(6) 0.0360(2) Uani 1 1 d . . . C1 C 0.5054(5) -0.0239(4) 0.3055(5) 0.0339(14) Uani 1 1 d . . . C2 C 0.4509(5) -0.0083(5) 0.2352(5) 0.0381(15) Uani 1 1 d . . . C3 C 0.4433(6) -0.0820(5) 0.2056(6) 0.0471(17) Uani 1 1 d . . . C4 C 0.4808(6) -0.1724(6) 0.2410(6) 0.060(2) Uani 1 1 d . . . H4A H 0.5143 -0.1846 0.2848 0.072 Uiso 1 1 calc R . . C5 C 0.4683(8) -0.2420(7) 0.2115(8) 0.084(3) Uani 1 1 d . . . H5A H 0.4915 -0.3017 0.2372 0.101 Uiso 1 1 calc R . . C6 C 0.4206(10) -0.2250(9) 0.1423(10) 0.108(4) Uani 1 1 d . . . H6A H 0.4145 -0.2725 0.1212 0.129 Uiso 1 1 calc R . . C7 C 0.3846(10) -0.1406(8) 0.1077(9) 0.103(4) Uani 1 1 d . . . H7A H 0.3527 -0.1306 0.0629 0.124 Uiso 1 1 calc R . . C8 C 0.3929(7) -0.0642(6) 0.1367(7) 0.066(2) Uani 1 1 d . . . C9 C 0.3569(8) 0.0237(7) 0.1011(7) 0.083(3) Uani 1 1 d . . . H9A H 0.3260 0.0346 0.0554 0.100 Uiso 1 1 calc R . . C10 C 0.3639(7) 0.0953(6) 0.1292(7) 0.064(2) Uani 1 1 d . . . C11 C 0.3278(9) 0.1853(7) 0.0912(8) 0.092(3) Uani 1 1 d . . . H11A H 0.2977 0.1961 0.0449 0.111 Uiso 1 1 calc R . . C12 C 0.3348(10) 0.2571(8) 0.1193(9) 0.102(4) Uani 1 1 d . . . H12A H 0.3086 0.3153 0.0942 0.123 Uiso 1 1 calc R . . C13 C 0.3831(8) 0.2412(6) 0.1877(8) 0.083(3) Uani 1 1 d . . . H13A H 0.3893 0.2902 0.2067 0.100 Uiso 1 1 calc R . . C14 C 0.4202(6) 0.1571(5) 0.2259(6) 0.056(2) Uani 1 1 d . . . H14A H 0.4514 0.1493 0.2707 0.067 Uiso 1 1 calc R . . C15 C 0.4128(5) 0.0803(5) 0.1993(5) 0.0420(16) Uani 1 1 d . . . C16 C 0.7426(6) -0.2513(5) 0.3588(6) 0.0531(19) Uani 1 1 d . . . C17 C 0.7879(6) -0.3408(4) 0.4072(6) 0.0436(16) Uani 1 1 d . . . C18 C 0.7397(5) -0.3882(5) 0.5141(6) 0.0441(17) Uani 1 1 d . . . C19 C 0.6500(6) -0.3564(6) 0.5795(6) 0.0525(19) Uani 1 1 d . . . H19A H 0.6208 -0.3017 0.5502 0.063 Uiso 1 1 calc R . . C20 C 0.6064(7) -0.4031(7) 0.6823(7) 0.068(2) Uani 1 1 d . . . H20A H 0.5471 -0.3810 0.7227 0.082 Uiso 1 1 calc R . . C21 C 0.6497(8) -0.4856(8) 0.7298(7) 0.091(3) Uani 1 1 d . . . H21A H 0.6201 -0.5166 0.8012 0.109 Uiso 1 1 calc R . . C22 C 0.7325(8) -0.5188(7) 0.6724(7) 0.080(3) Uani 1 1 d . . . H22A H 0.7592 -0.5739 0.7047 0.096 Uiso 1 1 calc R . . C23 C 0.7823(6) -0.4729(5) 0.5629(6) 0.057(2) Uani 1 1 d . . . C24 C 0.8685(7) -0.5077(6) 0.5014(7) 0.071(2) Uani 1 1 d . . . H24A H 0.8962 -0.5627 0.5324 0.085 Uiso 1 1 calc R . . C25 C 0.9139(7) -0.4617(5) 0.3945(7) 0.059(2) Uani 1 1 d . . . C26 C 1.0003(8) -0.4981(7) 0.3316(9) 0.082(3) Uani 1 1 d . . . H26A H 1.0259 -0.5548 0.3620 0.099 Uiso 1 1 calc R . . C27 C 1.0456(9) -0.4522(9) 0.2293(10) 0.094(3) Uani 1 1 d . . . H27A H 1.1036 -0.4764 0.1900 0.112 Uiso 1 1 calc R . . C28 C 1.0065(8) -0.3672(8) 0.1797(8) 0.086(3) Uani 1 1 d . . . H28A H 1.0371 -0.3368 0.1083 0.103 Uiso 1 1 calc R . . C29 C 0.9250(7) -0.3312(7) 0.2370(6) 0.065(2) Uani 1 1 d . . . H29A H 0.9010 -0.2743 0.2046 0.078 Uiso 1 1 calc R . . C30 C 0.8741(6) -0.3772(5) 0.3459(6) 0.0486(18) Uani 1 1 d . . . C31 C 0.6333(5) 0.1830(4) 0.3636(5) 0.0326(14) Uani 1 1 d . . . C32 C 0.6442(5) 0.2854(4) 0.2920(5) 0.0358(14) Uani 1 1 d . . . C33 C 0.6638(5) 0.3077(4) 0.1891(5) 0.0390(15) Uani 1 1 d . . . C34 C 0.6783(6) 0.2384(5) 0.1459(5) 0.0501(18) Uani 1 1 d . . . H34A H 0.6774 0.1748 0.1865 0.060 Uiso 1 1 calc R . . C35 C 0.6938(7) 0.2633(7) 0.0453(6) 0.072(3) Uani 1 1 d . . . H35A H 0.7012 0.2164 0.0191 0.087 Uiso 1 1 calc R . . C36 C 0.6984(8) 0.3582(8) -0.0177(7) 0.084(3) Uani 1 1 d . . . H36A H 0.7111 0.3741 -0.0863 0.101 Uiso 1 1 calc R . . C37 C 0.6850(8) 0.4266(7) 0.0186(7) 0.077(3) Uani 1 1 d . . . H37A H 0.6853 0.4891 -0.0246 0.093 Uiso 1 1 calc R . . C38 C 0.6697(6) 0.4065(5) 0.1239(6) 0.056(2) Uani 1 1 d . . . C39 C 0.6606(6) 0.4752(5) 0.1615(7) 0.061(2) Uani 1 1 d . . . H39A H 0.6636 0.5383 0.1185 0.073 Uiso 1 1 calc R . . C40 C 0.6470(6) 0.4544(5) 0.2621(7) 0.055(2) Uani 1 1 d . . . C41 C 0.6409(7) 0.5254(6) 0.3029(10) 0.080(3) Uani 1 1 d . . . H41A H 0.6486 0.5891 0.2598 0.096 Uiso 1 1 calc R . . C42 C 0.6245(8) 0.5030(8) 0.4004(10) 0.086(3) Uani 1 1 d . . . H42A H 0.6241 0.5508 0.4234 0.103 Uiso 1 1 calc R . . C43 C 0.6076(7) 0.4070(7) 0.4697(8) 0.076(3) Uani 1 1 d . . . H43A H 0.5927 0.3922 0.5386 0.091 Uiso 1 1 calc R . . C44 C 0.6133(6) 0.3359(5) 0.4352(6) 0.0536(19) Uani 1 1 d . . . H44A H 0.6022 0.2730 0.4812 0.064 Uiso 1 1 calc R . . C45 C 0.6357(5) 0.3561(4) 0.3309(5) 0.0399(15) Uani 1 1 d . . . C46 C 0.8837(5) 0.0657(4) 0.2490(5) 0.0328(14) Uani 1 1 d . . . C47 C 0.9790(5) 0.1190(5) 0.1535(5) 0.0374(15) Uani 1 1 d . . . C48 C 0.9987(5) 0.2155(5) 0.1272(5) 0.0439(17) Uani 1 1 d . . . C49 C 0.9341(6) 0.2663(5) 0.1880(6) 0.0528(19) Uani 1 1 d . . . H49A H 0.8747 0.2351 0.2473 0.063 Uiso 1 1 calc R . . C50 C 0.9573(7) 0.3598(5) 0.1611(7) 0.067(2) Uani 1 1 d . . . H50A H 0.9145 0.3913 0.2028 0.080 Uiso 1 1 calc R . . C51 C 1.0461(8) 0.4092(6) 0.0702(8) 0.078(3) Uani 1 1 d . . . H51A H 1.0632 0.4723 0.0536 0.094 Uiso 1 1 calc R . . C52 C 1.1058(8) 0.3652(7) 0.0078(8) 0.075(3) Uani 1 1 d . . . H52A H 1.1612 0.3996 -0.0540 0.090 Uiso 1 1 calc R . . C53 C 1.0866(6) 0.2672(6) 0.0336(6) 0.056(2) Uani 1 1 d . . . C54 C 1.1503(6) 0.2187(6) -0.0279(6) 0.059(2) Uani 1 1 d . . . H54A H 1.2064 0.2524 -0.0894 0.071 Uiso 1 1 calc R . . C55 C 1.1336(5) 0.1232(6) -0.0015(5) 0.0493(19) Uani 1 1 d . . . C56 C 1.2022(6) 0.0740(8) -0.0635(6) 0.066(3) Uani 1 1 d . . . H56A H 1.2586 0.1072 -0.1250 0.080 Uiso 1 1 calc R . . C57 C 1.1850(7) -0.0205(8) -0.0329(7) 0.068(2) Uani 1 1 d . . . H57A H 1.2314 -0.0520 -0.0727 0.082 Uiso 1 1 calc R . . C58 C 1.0984(6) -0.0719(6) 0.0580(6) 0.060(2) Uani 1 1 d . . . H58A H 1.0874 -0.1367 0.0768 0.072 Uiso 1 1 calc R . . C59 C 1.0307(6) -0.0279(6) 0.1187(6) 0.0505(18) Uani 1 1 d . . . H59A H 0.9738 -0.0630 0.1785 0.061 Uiso 1 1 calc R . . C60 C 1.0454(5) 0.0709(5) 0.0921(5) 0.0421(16) Uani 1 1 d . . . C61 C 0.7857(6) 0.1716(6) 0.5451(6) 0.058(2) Uani 1 1 d . . . H61A H 0.7530 0.2120 0.5046 0.069 Uiso 1 1 calc R . . C62 C 0.8184(8) 0.2052(7) 0.5995(8) 0.080(3) Uani 1 1 d . . . H62A H 0.8075 0.2671 0.5962 0.095 Uiso 1 1 calc R . . C63 C 0.8664(9) 0.1470(8) 0.6577(9) 0.095(4) Uani 1 1 d . . . H63A H 0.8892 0.1683 0.6951 0.114 Uiso 1 1 calc R . . C64 C 0.8815(8) 0.0556(7) 0.6613(7) 0.078(3) Uani 1 1 d . . . H64A H 0.9150 0.0147 0.7006 0.093 Uiso 1 1 calc R . . C65 C 0.8465(6) 0.0254(5) 0.6065(5) 0.0476(17) Uani 1 1 d . . . C66 C 0.8579(6) -0.0714(5) 0.6050(5) 0.0466(17) Uani 1 1 d . . . C67 C 0.9118(7) -0.1399(6) 0.6545(7) 0.077(3) Uani 1 1 d . . . H67A H 0.9432 -0.1257 0.6903 0.092 Uiso 1 1 calc R . . C68 C 0.9181(9) -0.2260(7) 0.6501(9) 0.097(4) Uani 1 1 d . . . H68A H 0.9517 -0.2723 0.6852 0.116 Uiso 1 1 calc R . . C69 C 0.8748(8) -0.2472(6) 0.5937(8) 0.082(3) Uani 1 1 d . . . H69A H 0.8790 -0.3065 0.5895 0.099 Uiso 1 1 calc R . . C70 C 0.8254(6) -0.1756(5) 0.5445(6) 0.058(2) Uani 1 1 d . . . H70A H 0.7972 -0.1873 0.5050 0.070 Uiso 1 1 calc R . . N1 N 0.8159(4) -0.0906(4) 0.5505(4) 0.0410(13) Uani 1 1 d . . . N2 N 0.7991(4) 0.0835(4) 0.5483(4) 0.0409(13) Uani 1 1 d . . . O1WA O 0.6483(3) -0.0529(3) 0.4622(3) 0.0294(9) Uani 1 1 d . . . O1 O 0.7811(5) -0.1762(4) 0.3481(4) 0.0638(15) Uani 1 1 d . . . O2 O 0.6735(7) -0.2550(5) 0.3321(9) 0.152(4) Uani 1 1 d . . . O3 O 0.8834(3) 0.0477(3) 0.3347(3) 0.0399(10) Uani 1 1 d . . . O4 O 0.8099(3) 0.0425(3) 0.2333(3) 0.0403(11) Uani 1 1 d . . . O5 O 0.6057(3) -0.0292(3) 0.2626(3) 0.0427(11) Uani 1 1 d . . . O6 O 0.4538(3) -0.0308(3) 0.3957(3) 0.0375(10) Uani 1 1 d . . . O7 O 0.5531(3) 0.1333(3) 0.3884(3) 0.0387(10) Uani 1 1 d . . . O8 O 0.7057(3) 0.1546(3) 0.3938(3) 0.0385(10) Uani 1 1 d . . . H1WA H 0.632(5) -0.101(4) 0.510(5) 0.028(18) 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 Zn1 0.0270(5) 0.0303(5) 0.0311(5) -0.0080(4) -0.0129(4) 0.0018(4) Zn2 0.0302(4) 0.0355(4) 0.0365(4) -0.0159(3) -0.0180(3) 0.0036(3) Zn3 0.0433(4) 0.0352(4) 0.0387(4) -0.0103(3) -0.0285(4) 0.0013(3) C1 0.037(4) 0.031(3) 0.033(4) -0.009(3) -0.016(3) 0.000(3) C2 0.031(3) 0.055(4) 0.031(3) -0.015(3) -0.017(3) 0.001(3) C3 0.051(4) 0.057(4) 0.051(4) -0.029(4) -0.030(4) 0.005(3) C4 0.064(5) 0.062(5) 0.074(6) -0.033(4) -0.042(5) 0.009(4) C5 0.106(8) 0.072(6) 0.112(8) -0.053(6) -0.065(7) 0.016(6) C6 0.151(11) 0.107(9) 0.148(11) -0.092(9) -0.101(10) 0.023(8) C7 0.146(11) 0.107(9) 0.134(10) -0.069(8) -0.109(9) 0.023(8) C8 0.079(6) 0.076(6) 0.079(6) -0.037(5) -0.058(5) 0.005(5) C9 0.112(8) 0.094(7) 0.086(7) -0.032(6) -0.082(7) 0.011(6) C10 0.073(6) 0.072(6) 0.071(6) -0.025(5) -0.056(5) 0.012(4) C11 0.118(9) 0.087(7) 0.110(8) -0.028(6) -0.096(8) 0.028(6) C12 0.133(10) 0.071(7) 0.128(10) -0.026(7) -0.097(9) 0.044(7) C13 0.114(8) 0.056(5) 0.103(8) -0.026(5) -0.074(7) 0.021(5) C14 0.060(5) 0.053(5) 0.057(5) -0.012(4) -0.034(4) 0.003(4) C15 0.038(4) 0.056(4) 0.034(4) -0.012(3) -0.021(3) 0.000(3) C16 0.049(5) 0.046(4) 0.056(5) -0.008(4) -0.025(4) 0.003(3) C17 0.051(4) 0.032(3) 0.055(4) -0.014(3) -0.031(4) 0.008(3) C18 0.044(4) 0.038(4) 0.057(4) -0.012(3) -0.030(4) -0.004(3) C19 0.039(4) 0.059(5) 0.066(5) -0.026(4) -0.027(4) 0.006(3) C20 0.046(5) 0.085(6) 0.066(6) -0.027(5) -0.018(4) -0.002(4) C21 0.068(7) 0.120(9) 0.052(6) -0.007(6) -0.014(5) -0.014(6) C22 0.072(6) 0.075(6) 0.063(6) 0.007(5) -0.030(5) 0.002(5) C23 0.055(5) 0.047(4) 0.063(5) -0.013(4) -0.027(4) 0.002(4) C24 0.080(6) 0.044(5) 0.087(7) -0.012(5) -0.048(6) 0.019(4) C25 0.060(5) 0.048(4) 0.076(6) -0.029(4) -0.032(5) 0.015(4) C26 0.084(7) 0.076(6) 0.104(8) -0.055(6) -0.043(7) 0.038(6) C27 0.075(7) 0.118(9) 0.109(9) -0.080(8) -0.027(7) 0.023(7) C28 0.075(7) 0.123(9) 0.072(6) -0.048(7) -0.034(6) 0.020(6) C29 0.059(5) 0.084(6) 0.058(5) -0.028(5) -0.029(4) 0.013(5) C30 0.049(4) 0.044(4) 0.061(5) -0.021(4) -0.031(4) 0.007(3) C31 0.035(3) 0.031(3) 0.030(3) -0.010(3) -0.013(3) 0.000(3) C32 0.029(3) 0.033(3) 0.043(4) -0.008(3) -0.018(3) -0.001(3) C33 0.030(3) 0.037(4) 0.040(4) -0.005(3) -0.015(3) 0.005(3) C34 0.056(5) 0.052(4) 0.044(4) -0.014(3) -0.027(4) 0.010(3) C35 0.087(7) 0.086(7) 0.046(5) -0.023(5) -0.033(5) 0.008(5) C36 0.102(8) 0.095(8) 0.044(5) -0.005(5) -0.039(5) 0.004(6) C37 0.083(7) 0.065(6) 0.051(5) 0.015(5) -0.030(5) 0.001(5) C38 0.045(4) 0.041(4) 0.056(5) 0.005(4) -0.020(4) -0.003(3) C39 0.051(5) 0.029(4) 0.072(6) 0.007(4) -0.020(4) -0.002(3) C40 0.044(4) 0.032(4) 0.089(6) -0.023(4) -0.026(4) 0.002(3) C41 0.062(6) 0.045(5) 0.137(10) -0.040(6) -0.038(6) -0.003(4) C42 0.069(6) 0.079(7) 0.146(11) -0.077(8) -0.049(7) 0.014(5) C43 0.066(6) 0.091(7) 0.093(7) -0.059(6) -0.035(5) 0.018(5) C44 0.056(5) 0.052(4) 0.074(5) -0.037(4) -0.037(4) 0.015(4) C45 0.030(3) 0.037(4) 0.056(4) -0.020(3) -0.020(3) 0.004(3) C46 0.033(3) 0.029(3) 0.037(4) -0.011(3) -0.018(3) 0.006(3) C47 0.032(3) 0.047(4) 0.032(3) -0.007(3) -0.019(3) -0.003(3) C48 0.040(4) 0.048(4) 0.042(4) -0.004(3) -0.026(3) -0.007(3) C49 0.056(5) 0.042(4) 0.065(5) -0.007(4) -0.040(4) -0.001(3) C50 0.070(6) 0.045(5) 0.094(7) -0.016(5) -0.053(5) 0.005(4) C51 0.086(7) 0.044(5) 0.102(8) -0.001(5) -0.057(7) -0.013(5) C52 0.068(6) 0.061(6) 0.072(6) 0.016(5) -0.038(5) -0.025(5) C53 0.052(5) 0.061(5) 0.051(5) 0.002(4) -0.035(4) -0.015(4) C54 0.038(4) 0.086(6) 0.039(4) -0.002(4) -0.018(4) -0.014(4) C55 0.034(4) 0.080(6) 0.033(4) -0.013(4) -0.020(3) 0.001(4) C56 0.039(4) 0.124(8) 0.034(4) -0.029(5) -0.015(4) 0.009(5) C57 0.055(5) 0.112(8) 0.052(5) -0.044(5) -0.029(4) 0.027(5) C58 0.061(5) 0.080(6) 0.060(5) -0.039(5) -0.037(5) 0.020(4) C59 0.043(4) 0.065(5) 0.046(4) -0.024(4) -0.018(3) 0.006(4) C60 0.036(4) 0.061(5) 0.035(4) -0.014(3) -0.023(3) 0.001(3) C61 0.062(5) 0.057(5) 0.075(6) -0.029(4) -0.045(5) 0.006(4) C62 0.094(7) 0.082(6) 0.110(8) -0.059(6) -0.064(7) 0.010(5) C63 0.135(10) 0.099(8) 0.123(9) -0.066(7) -0.101(8) 0.023(7) C64 0.099(7) 0.085(7) 0.092(7) -0.041(6) -0.074(6) 0.016(5) C65 0.048(4) 0.051(4) 0.051(4) -0.014(3) -0.031(4) -0.001(3) C66 0.048(4) 0.050(4) 0.049(4) -0.011(3) -0.034(4) 0.000(3) C67 0.100(7) 0.067(6) 0.104(7) -0.022(5) -0.091(7) 0.016(5) C68 0.131(9) 0.062(6) 0.151(10) -0.027(6) -0.125(9) 0.030(6) C69 0.112(8) 0.051(5) 0.124(8) -0.030(5) -0.093(7) 0.024(5) C70 0.069(5) 0.054(5) 0.072(5) -0.024(4) -0.051(5) 0.010(4) N1 0.047(3) 0.041(3) 0.043(3) -0.011(3) -0.031(3) 0.006(3) N2 0.037(3) 0.046(3) 0.045(3) -0.015(3) -0.021(3) -0.003(2) O1WA 0.030(2) 0.028(2) 0.028(2) -0.006(2) -0.0146(19) 0.0010(18) O1 0.091(4) 0.046(3) 0.087(4) -0.036(3) -0.062(4) 0.027(3) O2 0.146(7) 0.067(5) 0.276(12) 0.001(6) -0.174(9) -0.001(5) O3 0.035(2) 0.053(3) 0.032(2) -0.010(2) -0.019(2) 0.001(2) O4 0.034(2) 0.051(3) 0.039(2) -0.013(2) -0.021(2) -0.004(2) O5 0.033(3) 0.063(3) 0.039(3) -0.021(2) -0.020(2) 0.005(2) O6 0.035(2) 0.051(3) 0.033(2) -0.017(2) -0.019(2) 0.001(2) O7 0.042(3) 0.032(2) 0.040(2) -0.0008(19) -0.025(2) -0.0067(19) O8 0.039(3) 0.035(2) 0.045(3) -0.010(2) -0.025(2) 0.0045(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 2.051(4) 2_656 ? Zn1 O7 2.051(4) . ? Zn1 O1WA 2.077(4) 2_656 ? Zn1 O1WA 2.077(4) . ? Zn1 O6 2.186(4) 2_656 ? Zn1 O6 2.186(4) . ? Zn2 O5 1.922(4) . ? Zn2 O1 1.927(5) . ? Zn2 O4 1.955(4) . ? Zn2 O1WA 1.991(4) . ? Zn3 O1WA 2.030(4) . ? Zn3 O8 2.037(4) . ? Zn3 O3 2.066(4) . ? Zn3 N2 2.095(5) . ? Zn3 N1 2.135(5) . ? C1 O6 1.238(7) . ? C1 O5 1.288(7) . ? C1 C2 1.510(8) . ? C2 C15 1.397(9) . ? C2 C3 1.401(9) . ? C3 C4 1.413(10) . ? C3 C8 1.440(10) . ? C4 C5 1.364(11) . ? C4 H4A 0.9300 . ? C5 C6 1.416(14) . ? C5 H5A 0.9300 . ? C6 C7 1.330(14) . ? C6 H6A 0.9300 . ? C7 C8 1.437(12) . ? C7 H7A 0.9300 . ? C8 C9 1.375(12) . ? C9 C10 1.354(12) . ? C9 H9A 0.9300 . ? C10 C11 1.407(12) . ? C10 C15 1.448(9) . ? C11 C12 1.355(14) . ? C11 H11A 0.9300 . ? C12 C13 1.414(13) . ? C12 H12A 0.9300 . ? C13 C14 1.344(11) . ? C13 H13A 0.9300 . ? C14 C15 1.415(10) . ? C14 H14A 0.9300 . ? C16 O2 1.215(10) . ? C16 O1 1.246(9) . ? C16 C17 1.506(9) . ? C17 C18 1.395(10) . ? C17 C30 1.406(10) . ? C18 C19 1.425(10) . ? C18 C23 1.437(10) . ? C19 C20 1.343(11) . ? C19 H19A 0.9300 . ? C20 C21 1.414(13) . ? C20 H20A 0.9300 . ? C21 C22 1.325(13) . ? C21 H21A 0.9300 . ? C22 C23 1.426(12) . ? C22 H22A 0.9300 . ? C23 C24 1.394(12) . ? C24 C25 1.393(12) . ? C24 H24A 0.9300 . ? C25 C30 1.414(10) . ? C25 C26 1.419(12) . ? C26 C27 1.336(14) . ? C26 H26A 0.9300 . ? C27 C28 1.419(14) . ? C27 H27A 0.9300 . ? C28 C29 1.339(12) . ? C28 H28A 0.9300 . ? C29 C30 1.420(11) . ? C29 H29A 0.9300 . ? C31 O7 1.258(7) . ? C31 O8 1.258(7) . ? C31 C32 1.508(8) . ? C32 C33 1.398(9) . ? C32 C45 1.404(9) . ? C33 C34 1.416(10) . ? C33 C38 1.445(9) . ? C34 C35 1.374(10) . ? C34 H34A 0.9300 . ? C35 C36 1.391(13) . ? C35 H35A 0.9300 . ? C36 C37 1.335(13) . ? C36 H36A 0.9300 . ? C37 C38 1.456(12) . ? C37 H37A 0.9300 . ? C38 C39 1.359(11) . ? C39 C40 1.392(12) . ? C39 H39A 0.9300 . ? C40 C41 1.434(12) . ? C40 C45 1.445(10) . ? C41 C42 1.330(14) . ? C41 H41A 0.9300 . ? C42 C43 1.416(14) . ? C42 H42A 0.9300 . ? C43 C44 1.370(11) . ? C43 H43A 0.9300 . ? C44 C45 1.415(10) . ? C44 H44A 0.9300 . ? C46 O3 1.242(7) . ? C46 O4 1.268(7) . ? C46 C47 1.506(8) . ? C47 C48 1.397(9) . ? C47 C60 1.403(9) . ? C48 C49 1.420(11) . ? C48 C53 1.434(10) . ? C49 C50 1.362(10) . ? C49 H49A 0.9300 . ? C50 C51 1.415(13) . ? C50 H50A 0.9300 . ? C51 C52 1.340(13) . ? C51 H51A 0.9300 . ? C52 C53 1.419(12) . ? C52 H52A 0.9300 . ? C53 C54 1.398(12) . ? C54 C55 1.375(11) . ? C54 H54A 0.9300 . ? C55 C56 1.430(11) . ? C55 C60 1.438(9) . ? C56 C57 1.351(12) . ? C56 H56A 0.9300 . ? C57 C58 1.406(12) . ? C57 H57A 0.9300 . ? C58 C59 1.359(10) . ? C58 H58A 0.9300 . ? C59 C60 1.420(10) . ? C59 H59A 0.9300 . ? C61 N2 1.329(9) . ? C61 C62 1.376(11) . ? C61 H61A 0.9300 . ? C62 C63 1.350(13) . ? C62 H62A 0.9300 . ? C63 C64 1.378(13) . ? C63 H63A 0.9300 . ? C64 C65 1.369(10) . ? C64 H64A 0.9300 . ? C65 N2 1.341(8) . ? C65 C66 1.485(10) . ? C66 N1 1.336(8) . ? C66 C67 1.399(10) . ? C67 C68 1.340(12) . ? C67 H67A 0.9300 . ? C68 C69 1.393(12) . ? C68 H68A 0.9300 . ? C69 C70 1.377(10) . ? C69 H69A 0.9300 . ? C70 N1 1.330(9) . ? C70 H70A 0.9300 . ? O1WA H1WA 0.78(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O7 180.0(3) 2_656 . ? O7 Zn1 O1WA 94.47(17) 2_656 2_656 ? O7 Zn1 O1WA 85.53(17) . 2_656 ? O7 Zn1 O1WA 85.53(17) 2_656 . ? O7 Zn1 O1WA 94.47(17) . . ? O1WA Zn1 O1WA 180.000(1) 2_656 . ? O7 Zn1 O6 87.89(16) 2_656 2_656 ? O7 Zn1 O6 92.11(16) . 2_656 ? O1WA Zn1 O6 98.91(16) 2_656 2_656 ? O1WA Zn1 O6 81.09(16) . 2_656 ? O7 Zn1 O6 92.11(16) 2_656 . ? O7 Zn1 O6 87.89(16) . . ? O1WA Zn1 O6 81.09(16) 2_656 . ? O1WA Zn1 O6 98.91(16) . . ? O6 Zn1 O6 180.0(2) 2_656 . ? O5 Zn2 O1 129.4(2) . . ? O5 Zn2 O4 99.74(18) . . ? O1 Zn2 O4 106.0(2) . . ? O5 Zn2 O1WA 112.97(18) . . ? O1 Zn2 O1WA 101.8(2) . . ? O4 Zn2 O1WA 104.49(18) . . ? O1WA Zn3 O8 95.66(17) . . ? O1WA Zn3 O3 103.58(17) . . ? O8 Zn3 O3 87.93(17) . . ? O1WA Zn3 N2 152.46(19) . . ? O8 Zn3 N2 92.52(19) . . ? O3 Zn3 N2 102.95(19) . . ? O1WA Zn3 N1 95.50(19) . . ? O8 Zn3 N1 168.83(19) . . ? O3 Zn3 N1 89.83(19) . . ? N2 Zn3 N1 77.3(2) . . ? O6 C1 O5 125.9(6) . . ? O6 C1 C2 120.3(5) . . ? O5 C1 C2 113.9(5) . . ? C15 C2 C3 122.3(6) . . ? C15 C2 C1 118.6(6) . . ? C3 C2 C1 119.0(6) . . ? C2 C3 C4 123.5(6) . . ? C2 C3 C8 117.7(7) . . ? C4 C3 C8 118.8(7) . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 121.2(9) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C7 C6 C5 119.6(9) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C8 122.6(9) . . ? C6 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? C9 C8 C7 123.5(8) . . ? C9 C8 C3 119.3(7) . . ? C7 C8 C3 117.2(8) . . ? C10 C9 C8 123.4(7) . . ? C10 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? C9 C10 C11 122.8(8) . . ? C9 C10 C15 119.2(7) . . ? C11 C10 C15 118.0(8) . . ? C12 C11 C10 122.8(9) . . ? C12 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? C11 C12 C13 118.4(9) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C14 C13 C12 121.6(9) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 121.4(8) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C2 C15 C14 124.3(6) . . ? C2 C15 C10 118.0(7) . . ? C14 C15 C10 117.7(7) . . ? O2 C16 O1 124.0(7) . . ? O2 C16 C17 120.3(7) . . ? O1 C16 C17 115.7(7) . . ? C18 C17 C30 121.1(6) . . ? C18 C17 C16 118.2(6) . . ? C30 C17 C16 120.7(6) . . ? C17 C18 C19 123.4(6) . . ? C17 C18 C23 119.5(7) . . ? C19 C18 C23 117.0(7) . . ? C20 C19 C18 121.9(8) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 120.7(9) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C22 C21 C20 119.8(9) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 122.3(9) . . ? C21 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C24 C23 C22 123.0(8) . . ? C24 C23 C18 118.8(7) . . ? C22 C23 C18 118.2(8) . . ? C25 C24 C23 121.3(7) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C30 120.4(7) . . ? C24 C25 C26 121.4(8) . . ? C30 C25 C26 118.3(8) . . ? C27 C26 C25 121.2(9) . . ? C27 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? C26 C27 C28 121.0(10) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C29 C28 C27 119.2(10) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 121.9(9) . . ? C28 C29 H29A 119.1 . . ? C30 C29 H29A 119.1 . . ? C17 C30 C25 118.9(7) . . ? C17 C30 C29 122.7(7) . . ? C25 C30 C29 118.4(7) . . ? O7 C31 O8 125.5(5) . . ? O7 C31 C32 117.6(5) . . ? O8 C31 C32 116.9(5) . . ? C33 C32 C45 121.8(6) . . ? C33 C32 C31 119.7(6) . . ? C45 C32 C31 118.5(6) . . ? C32 C33 C34 123.3(6) . . ? C32 C33 C38 118.0(7) . . ? C34 C33 C38 118.7(7) . . ? C35 C34 C33 121.3(7) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? C34 C35 C36 120.4(9) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C37 C36 C35 121.0(9) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 122.1(8) . . ? C36 C37 H37A 119.0 . . ? C38 C37 H37A 119.0 . . ? C39 C38 C33 120.3(7) . . ? C39 C38 C37 123.3(7) . . ? C33 C38 C37 116.4(8) . . ? C38 C39 C40 122.3(7) . . ? C38 C39 H39A 118.8 . . ? C40 C39 H39A 118.8 . . ? C39 C40 C41 123.6(8) . . ? C39 C40 C45 118.8(7) . . ? C41 C40 C45 117.6(9) . . ? C42 C41 C40 122.0(9) . . ? C42 C41 H41A 119.0 . . ? C40 C41 H41A 119.0 . . ? C41 C42 C43 120.7(9) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C42 119.9(9) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 121.3(8) . . ? C43 C44 H44A 119.3 . . ? C45 C44 H44A 119.3 . . ? C32 C45 C44 123.1(6) . . ? C32 C45 C40 118.6(7) . . ? C44 C45 C40 118.3(7) . . ? O3 C46 O4 125.8(6) . . ? O3 C46 C47 118.9(5) . . ? O4 C46 C47 115.4(5) . . ? C48 C47 C60 121.5(6) . . ? C48 C47 C46 119.3(6) . . ? C60 C47 C46 119.2(6) . . ? C47 C48 C49 123.1(6) . . ? C47 C48 C53 119.3(7) . . ? C49 C48 C53 117.6(7) . . ? C50 C49 C48 121.4(8) . . ? C50 C49 H49A 119.3 . . ? C48 C49 H49A 119.3 . . ? C49 C50 C51 120.3(9) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C52 C51 C50 120.2(8) . . ? C52 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? C51 C52 C53 121.6(9) . . ? C51 C52 H52A 119.2 . . ? C53 C52 H52A 119.2 . . ? C54 C53 C52 122.8(8) . . ? C54 C53 C48 118.4(7) . . ? C52 C53 C48 118.8(9) . . ? C55 C54 C53 122.9(7) . . ? C55 C54 H54A 118.6 . . ? C53 C54 H54A 118.6 . . ? C54 C55 C56 122.0(7) . . ? C54 C55 C60 118.9(7) . . ? C56 C55 C60 119.0(8) . . ? C57 C56 C55 120.1(8) . . ? C57 C56 H56A 119.9 . . ? C55 C56 H56A 119.9 . . ? C56 C57 C58 121.2(8) . . ? C56 C57 H57A 119.4 . . ? C58 C57 H57A 119.4 . . ? C59 C58 C57 120.6(8) . . ? C59 C58 H58A 119.7 . . ? C57 C58 H58A 119.7 . . ? C58 C59 C60 121.0(7) . . ? C58 C59 H59A 119.5 . . ? C60 C59 H59A 119.5 . . ? C47 C60 C59 123.1(6) . . ? C47 C60 C55 119.0(7) . . ? C59 C60 C55 118.0(7) . . ? N2 C61 C62 122.3(8) . . ? N2 C61 H61A 118.8 . . ? C62 C61 H61A 118.8 . . ? C63 C62 C61 119.0(9) . . ? C63 C62 H62A 120.5 . . ? C61 C62 H62A 120.5 . . ? C62 C63 C64 119.3(8) . . ? C62 C63 H63A 120.3 . . ? C64 C63 H63A 120.3 . . ? C65 C64 C63 119.3(8) . . ? C65 C64 H64A 120.4 . . ? C63 C64 H64A 120.4 . . ? N2 C65 C64 121.3(7) . . ? N2 C65 C66 114.6(6) . . ? C64 C65 C66 124.0(7) . . ? N1 C66 C67 120.2(7) . . ? N1 C66 C65 116.6(6) . . ? C67 C66 C65 123.2(7) . . ? C68 C67 C66 119.7(7) . . ? C68 C67 H67A 120.2 . . ? C66 C67 H67A 120.2 . . ? C67 C68 C69 120.8(8) . . ? C67 C68 H68A 119.6 . . ? C69 C68 H68A 119.6 . . ? C70 C69 C68 116.4(8) . . ? C70 C69 H69A 121.8 . . ? C68 C69 H69A 121.8 . . ? N1 C70 C69 123.5(7) . . ? N1 C70 H70A 118.2 . . ? C69 C70 H70A 118.2 . . ? C70 N1 C66 119.4(6) . . ? C70 N1 Zn3 125.9(5) . . ? C66 N1 Zn3 114.5(5) . . ? C61 N2 C65 118.7(6) . . ? C61 N2 Zn3 124.5(5) . . ? C65 N2 Zn3 116.8(5) . . ? Zn2 O1WA Zn3 111.6(2) . . ? Zn2 O1WA Zn1 112.08(18) . . ? Zn3 O1WA Zn1 110.52(19) . . ? Zn2 O1WA H1WA 115(5) . . ? Zn3 O1WA H1WA 111(5) . . ? Zn1 O1WA H1WA 96(5) . . ? C16 O1 Zn2 118.7(5) . . ? C46 O3 Zn3 125.0(4) . . ? C46 O4 Zn2 126.9(4) . . ? C1 O5 Zn2 128.5(4) . . ? C1 O6 Zn1 130.8(4) . . ? C31 O7 Zn1 128.5(4) . . ? C31 O8 Zn3 136.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C1 C2 C15 72.0(8) . . . . ? O5 C1 C2 C15 -108.2(7) . . . . ? O6 C1 C2 C3 -110.0(7) . . . . ? O5 C1 C2 C3 69.8(8) . . . . ? C15 C2 C3 C4 -179.8(7) . . . . ? C1 C2 C3 C4 2.3(11) . . . . ? C15 C2 C3 C8 -0.7(11) . . . . ? C1 C2 C3 C8 -178.7(7) . . . . ? C2 C3 C4 C5 178.2(8) . . . . ? C8 C3 C4 C5 -0.9(13) . . . . ? C3 C4 C5 C6 2.0(16) . . . . ? C4 C5 C6 C7 -2.0(19) . . . . ? C5 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C9 179.5(12) . . . . ? C6 C7 C8 C3 0.4(18) . . . . ? C2 C3 C8 C9 1.5(13) . . . . ? C4 C3 C8 C9 -179.5(9) . . . . ? C2 C3 C8 C7 -179.4(9) . . . . ? C4 C3 C8 C7 -0.3(13) . . . . ? C7 C8 C9 C10 179.4(11) . . . . ? C3 C8 C9 C10 -1.5(16) . . . . ? C8 C9 C10 C11 179.3(10) . . . . ? C8 C9 C10 C15 0.8(16) . . . . ? C9 C10 C11 C12 180.0(12) . . . . ? C15 C10 C11 C12 -1.5(17) . . . . ? C10 C11 C12 C13 1.6(19) . . . . ? C11 C12 C13 C14 -0.9(18) . . . . ? C12 C13 C14 C15 0.1(15) . . . . ? C3 C2 C15 C14 -179.0(7) . . . . ? C1 C2 C15 C14 -1.1(10) . . . . ? C3 C2 C15 C10 0.0(10) . . . . ? C1 C2 C15 C10 178.0(6) . . . . ? C13 C14 C15 C2 179.2(8) . . . . ? C13 C14 C15 C10 0.1(12) . . . . ? C9 C10 C15 C2 0.0(12) . . . . ? C11 C10 C15 C2 -178.6(8) . . . . ? C9 C10 C15 C14 179.1(8) . . . . ? C11 C10 C15 C14 0.5(12) . . . . ? O2 C16 C17 C18 -89.1(11) . . . . ? O1 C16 C17 C18 91.4(9) . . . . ? O2 C16 C17 C30 88.7(11) . . . . ? O1 C16 C17 C30 -90.8(9) . . . . ? C30 C17 C18 C19 -177.7(6) . . . . ? C16 C17 C18 C19 0.1(10) . . . . ? C30 C17 C18 C23 3.4(10) . . . . ? C16 C17 C18 C23 -178.8(7) . . . . ? C17 C18 C19 C20 -179.2(7) . . . . ? C23 C18 C19 C20 -0.2(11) . . . . ? C18 C19 C20 C21 1.1(13) . . . . ? C19 C20 C21 C22 -1.7(15) . . . . ? C20 C21 C22 C23 1.4(16) . . . . ? C21 C22 C23 C24 -179.0(10) . . . . ? C21 C22 C23 C18 -0.5(14) . . . . ? C17 C18 C23 C24 -2.6(11) . . . . ? C19 C18 C23 C24 178.4(7) . . . . ? C17 C18 C23 C22 178.9(7) . . . . ? C19 C18 C23 C22 -0.1(11) . . . . ? C22 C23 C24 C25 178.9(9) . . . . ? C18 C23 C24 C25 0.5(13) . . . . ? C23 C24 C25 C30 1.0(13) . . . . ? C23 C24 C25 C26 -178.7(9) . . . . ? C24 C25 C26 C27 -178.0(10) . . . . ? C30 C25 C26 C27 2.3(14) . . . . ? C25 C26 C27 C28 -2.2(17) . . . . ? C26 C27 C28 C29 2.1(17) . . . . ? C27 C28 C29 C30 -2.1(15) . . . . ? C18 C17 C30 C25 -2.0(10) . . . . ? C16 C17 C30 C25 -179.7(7) . . . . ? C18 C17 C30 C29 179.9(7) . . . . ? C16 C17 C30 C29 2.1(11) . . . . ? C24 C25 C30 C17 -0.2(11) . . . . ? C26 C25 C30 C17 179.5(8) . . . . ? C24 C25 C30 C29 178.0(8) . . . . ? C26 C25 C30 C29 -2.3(12) . . . . ? C28 C29 C30 C17 -179.5(8) . . . . ? C28 C29 C30 C25 2.3(13) . . . . ? O7 C31 C32 C33 -69.2(8) . . . . ? O8 C31 C32 C33 111.0(7) . . . . ? O7 C31 C32 C45 111.7(7) . . . . ? O8 C31 C32 C45 -68.1(8) . . . . ? C45 C32 C33 C34 176.6(6) . . . . ? C31 C32 C33 C34 -2.5(9) . . . . ? C45 C32 C33 C38 -3.3(9) . . . . ? C31 C32 C33 C38 177.7(6) . . . . ? C32 C33 C34 C35 177.7(7) . . . . ? C38 C33 C34 C35 -2.5(11) . . . . ? C33 C34 C35 C36 1.8(13) . . . . ? C34 C35 C36 C37 -1.9(16) . . . . ? C35 C36 C37 C38 2.9(16) . . . . ? C32 C33 C38 C39 2.6(10) . . . . ? C34 C33 C38 C39 -177.2(7) . . . . ? C32 C33 C38 C37 -177.0(7) . . . . ? C34 C33 C38 C37 3.1(10) . . . . ? C36 C37 C38 C39 176.9(9) . . . . ? C36 C37 C38 C33 -3.4(13) . . . . ? C33 C38 C39 C40 0.9(12) . . . . ? C37 C38 C39 C40 -179.4(8) . . . . ? C38 C39 C40 C41 177.7(8) . . . . ? C38 C39 C40 C45 -3.8(11) . . . . ? C39 C40 C41 C42 177.9(9) . . . . ? C45 C40 C41 C42 -0.6(13) . . . . ? C40 C41 C42 C43 -2.8(15) . . . . ? C41 C42 C43 C44 3.3(14) . . . . ? C42 C43 C44 C45 -0.1(13) . . . . ? C33 C32 C45 C44 178.4(6) . . . . ? C31 C32 C45 C44 -2.6(9) . . . . ? C33 C32 C45 C40 0.5(9) . . . . ? C31 C32 C45 C40 179.5(6) . . . . ? C43 C44 C45 C32 178.8(7) . . . . ? C43 C44 C45 C40 -3.3(11) . . . . ? C39 C40 C45 C32 3.1(10) . . . . ? C41 C40 C45 C32 -178.3(7) . . . . ? C39 C40 C45 C44 -174.9(7) . . . . ? C41 C40 C45 C44 3.6(10) . . . . ? O3 C46 C47 C48 -71.9(8) . . . . ? O4 C46 C47 C48 108.6(7) . . . . ? O3 C46 C47 C60 109.0(7) . . . . ? O4 C46 C47 C60 -70.6(7) . . . . ? C60 C47 C48 C49 -179.2(6) . . . . ? C46 C47 C48 C49 1.6(9) . . . . ? C60 C47 C48 C53 2.1(9) . . . . ? C46 C47 C48 C53 -177.0(6) . . . . ? C47 C48 C49 C50 178.4(7) . . . . ? C53 C48 C49 C50 -3.0(10) . . . . ? C48 C49 C50 C51 1.1(11) . . . . ? C49 C50 C51 C52 2.5(13) . . . . ? C50 C51 C52 C53 -4.2(14) . . . . ? C51 C52 C53 C54 -177.2(8) . . . . ? C51 C52 C53 C48 2.2(12) . . . . ? C47 C48 C53 C54 -0.5(9) . . . . ? C49 C48 C53 C54 -179.2(6) . . . . ? C47 C48 C53 C52 -180.0(6) . . . . ? C49 C48 C53 C52 1.3(10) . . . . ? C52 C53 C54 C55 178.0(7) . . . . ? C48 C53 C54 C55 -1.4(10) . . . . ? C53 C54 C55 C56 -177.5(7) . . . . ? C53 C54 C55 C60 1.6(10) . . . . ? C54 C55 C56 C57 177.7(7) . . . . ? C60 C55 C56 C57 -1.5(10) . . . . ? C55 C56 C57 C58 2.0(12) . . . . ? C56 C57 C58 C59 -1.3(12) . . . . ? C57 C58 C59 C60 -0.1(11) . . . . ? C48 C47 C60 C59 177.1(6) . . . . ? C46 C47 C60 C59 -3.8(9) . . . . ? C48 C47 C60 C55 -1.9(9) . . . . ? C46 C47 C60 C55 177.3(5) . . . . ? C58 C59 C60 C47 -178.4(6) . . . . ? C58 C59 C60 C55 0.6(10) . . . . ? C54 C55 C60 C47 0.0(9) . . . . ? C56 C55 C60 C47 179.2(6) . . . . ? C54 C55 C60 C59 -179.0(6) . . . . ? C56 C55 C60 C59 0.2(9) . . . . ? N2 C61 C62 C63 0.4(15) . . . . ? C61 C62 C63 C64 0.0(17) . . . . ? C62 C63 C64 C65 -0.6(17) . . . . ? C63 C64 C65 N2 0.8(14) . . . . ? C63 C64 C65 C66 -179.7(9) . . . . ? N2 C65 C66 N1 -2.9(10) . . . . ? C64 C65 C66 N1 177.6(8) . . . . ? N2 C65 C66 C67 175.2(8) . . . . ? C64 C65 C66 C67 -4.3(13) . . . . ? N1 C66 C67 C68 -2.3(14) . . . . ? C65 C66 C67 C68 179.6(9) . . . . ? C66 C67 C68 C69 2.3(18) . . . . ? C67 C68 C69 C70 -0.5(18) . . . . ? C68 C69 C70 N1 -1.4(15) . . . . ? C69 C70 N1 C66 1.5(13) . . . . ? C69 C70 N1 Zn3 175.7(7) . . . . ? C67 C66 N1 C70 0.5(11) . . . . ? C65 C66 N1 C70 178.7(7) . . . . ? C67 C66 N1 Zn3 -174.5(6) . . . . ? C65 C66 N1 Zn3 3.7(8) . . . . ? O1WA Zn3 N1 C70 29.8(6) . . . . ? O8 Zn3 N1 C70 -152.2(9) . . . . ? O3 Zn3 N1 C70 -73.8(6) . . . . ? N2 Zn3 N1 C70 -177.1(7) . . . . ? O1WA Zn3 N1 C66 -155.7(5) . . . . ? O8 Zn3 N1 C66 22.3(13) . . . . ? O3 Zn3 N1 C66 100.7(5) . . . . ? N2 Zn3 N1 C66 -2.6(5) . . . . ? C62 C61 N2 C65 -0.2(12) . . . . ? C62 C61 N2 Zn3 179.2(7) . . . . ? C64 C65 N2 C61 -0.5(11) . . . . ? C66 C65 N2 C61 -180.0(6) . . . . ? C64 C65 N2 Zn3 -179.9(7) . . . . ? C66 C65 N2 Zn3 0.6(8) . . . . ? O1WA Zn3 N2 C61 -101.1(7) . . . . ? O8 Zn3 N2 C61 6.3(6) . . . . ? O3 Zn3 N2 C61 94.8(6) . . . . ? N1 Zn3 N2 C61 -178.4(6) . . . . ? O1WA Zn3 N2 C65 78.4(7) . . . . ? O8 Zn3 N2 C65 -174.3(5) . . . . ? O3 Zn3 N2 C65 -85.8(5) . . . . ? N1 Zn3 N2 C65 1.0(5) . . . . ? O5 Zn2 O1WA Zn3 -127.4(2) . . . . ? O1 Zn2 O1WA Zn3 90.1(3) . . . . ? O4 Zn2 O1WA Zn3 -20.0(2) . . . . ? O5 Zn2 O1WA Zn1 -2.9(3) . . . . ? O1 Zn2 O1WA Zn1 -145.3(2) . . . . ? O4 Zn2 O1WA Zn1 104.5(2) . . . . ? O8 Zn3 O1WA Zn2 80.7(2) . . . . ? O3 Zn3 O1WA Zn2 -8.5(2) . . . . ? N2 Zn3 O1WA Zn2 -172.7(3) . . . . ? N1 Zn3 O1WA Zn2 -99.7(2) . . . . ? O8 Zn3 O1WA Zn1 -44.7(2) . . . . ? O3 Zn3 O1WA Zn1 -133.96(19) . . . . ? N2 Zn3 O1WA Zn1 61.9(5) . . . . ? N1 Zn3 O1WA Zn1 134.9(2) . . . . ? O7 Zn1 O1WA Zn2 111.2(2) 2_656 . . . ? O7 Zn1 O1WA Zn2 -68.8(2) . . . . ? O1WA Zn1 O1WA Zn2 16(100) 2_656 . . . ? O6 Zn1 O1WA Zn2 -160.2(2) 2_656 . . . ? O6 Zn1 O1WA Zn2 19.8(2) . . . . ? O7 Zn1 O1WA Zn3 -123.6(2) 2_656 . . . ? O7 Zn1 O1WA Zn3 56.4(2) . . . . ? O1WA Zn1 O1WA Zn3 141(100) 2_656 . . . ? O6 Zn1 O1WA Zn3 -35.06(19) 2_656 . . . ? O6 Zn1 O1WA Zn3 144.94(19) . . . . ? O2 C16 O1 Zn2 18.5(13) . . . . ? C17 C16 O1 Zn2 -162.1(5) . . . . ? O5 Zn2 O1 C16 -28.1(7) . . . . ? O4 Zn2 O1 C16 -145.7(6) . . . . ? O1WA Zn2 O1 C16 105.3(6) . . . . ? O4 C46 O3 Zn3 -26.6(9) . . . . ? C47 C46 O3 Zn3 153.9(4) . . . . ? O1WA Zn3 O3 C46 41.5(5) . . . . ? O8 Zn3 O3 C46 -53.9(5) . . . . ? N2 Zn3 O3 C46 -146.0(5) . . . . ? N1 Zn3 O3 C46 137.1(5) . . . . ? O3 C46 O4 Zn2 -25.5(9) . . . . ? C47 C46 O4 Zn2 154.0(4) . . . . ? O5 Zn2 O4 C46 166.0(5) . . . . ? O1 Zn2 O4 C46 -58.0(5) . . . . ? O1WA Zn2 O4 C46 49.0(5) . . . . ? O6 C1 O5 Zn2 8.3(9) . . . . ? C2 C1 O5 Zn2 -171.5(4) . . . . ? O1 Zn2 O5 C1 110.4(6) . . . . ? O4 Zn2 O5 C1 -129.4(5) . . . . ? O1WA Zn2 O5 C1 -19.0(6) . . . . ? O5 C1 O6 Zn1 26.6(9) . . . . ? C2 C1 O6 Zn1 -153.6(4) . . . . ? O7 Zn1 O6 C1 -125.7(5) 2_656 . . . ? O7 Zn1 O6 C1 54.3(5) . . . . ? O1WA Zn1 O6 C1 140.1(5) 2_656 . . . ? O1WA Zn1 O6 C1 -39.9(5) . . . . ? O6 Zn1 O6 C1 123(100) 2_656 . . . ? O8 C31 O7 Zn1 10.5(9) . . . . ? C32 C31 O7 Zn1 -169.3(4) . . . . ? O7 Zn1 O7 C31 -140(100) 2_656 . . . ? O1WA Zn1 O7 C31 136.4(5) 2_656 . . . ? O1WA Zn1 O7 C31 -43.6(5) . . . . ? O6 Zn1 O7 C31 37.6(5) 2_656 . . . ? O6 Zn1 O7 C31 -142.4(5) . . . . ? O7 C31 O8 Zn3 11.5(10) . . . . ? C32 C31 O8 Zn3 -168.7(4) . . . . ? O1WA Zn3 O8 C31 9.4(6) . . . . ? O3 Zn3 O8 C31 112.8(6) . . . . ? N2 Zn3 O8 C31 -144.3(6) . . . . ? N1 Zn3 O8 C31 -168.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.860 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.090 data_1 _database_code_depnum_ccdc_archive 'CCDC 623311' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 O7 Zn' _chemical_formula_weight 561.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9951(2) _cell_length_b 7.70390(10) _cell_length_c 23.5124(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.7870(10) _cell_angle_gamma 90.00 _cell_volume 2522.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6013 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.74 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8216 _exptl_absorpt_correction_T_max 0.8617 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25201 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6218 _reflns_number_gt 4554 _reflns_threshold_expression i>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6218 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.509836(13) 0.95109(3) 0.779157(8) 0.02995(7) Uani 1 1 d . . . C1 C 0.47521(11) 0.5904(2) 0.82272(7) 0.0275(4) Uani 1 1 d . . . C2 C 0.48458(12) 0.6457(2) 0.88393(7) 0.0300(4) Uani 1 1 d . . . C3 C 0.40783(13) 0.7388(2) 0.90432(8) 0.0364(4) Uani 1 1 d . . . C4 C 0.32055(13) 0.7739(3) 0.87042(9) 0.0435(5) Uani 1 1 d . . . H4A H 0.3123 0.7350 0.8328 0.052 Uiso 1 1 calc R . . C5 C 0.24855(16) 0.8636(3) 0.89194(11) 0.0629(6) Uani 1 1 d . . . H5A H 0.1918 0.8860 0.8691 0.075 Uiso 1 1 calc R . . C6 C 0.2602(2) 0.9225(3) 0.94891(13) 0.0765(8) Uani 1 1 d . . . H6A H 0.2110 0.9852 0.9631 0.092 Uiso 1 1 calc R . . C7 C 0.3402(2) 0.8903(3) 0.98300(11) 0.0669(7) Uani 1 1 d . . . H7A H 0.3456 0.9298 1.0206 0.080 Uiso 1 1 calc R . . C8 C 0.41809(16) 0.7958(3) 0.96271(9) 0.0478(5) Uani 1 1 d . . . C9 C 0.50114(17) 0.7586(3) 0.99707(9) 0.0537(6) Uani 1 1 d . . . H9A H 0.5073 0.7975 1.0347 0.064 Uiso 1 1 calc R . . C10 C 0.57587(15) 0.6652(3) 0.97756(8) 0.0457(5) Uani 1 1 d . . . C11 C 0.66067(19) 0.6237(3) 1.01381(9) 0.0623(6) Uani 1 1 d . . . H11A H 0.6662 0.6604 1.0517 0.075 Uiso 1 1 calc R . . C12 C 0.7320(2) 0.5338(4) 0.99476(11) 0.0709(8) Uani 1 1 d . . . H12A H 0.7859 0.5064 1.0196 0.085 Uiso 1 1 calc R . . C13 C 0.72667(17) 0.4795(3) 0.93700(11) 0.0633(6) Uani 1 1 d . . . H13A H 0.7778 0.4192 0.9240 0.076 Uiso 1 1 calc R . . C14 C 0.64758(15) 0.5146(3) 0.90042(9) 0.0454(5) Uani 1 1 d . . . H14A H 0.6451 0.4779 0.8626 0.054 Uiso 1 1 calc R . . C15 C 0.56840(13) 0.6068(2) 0.91925(7) 0.0350(4) Uani 1 1 d . . . C16 C 0.72560(12) 0.9362(2) 0.81341(8) 0.0350(4) Uani 1 1 d . . . C17 C 0.82074(11) 0.8453(2) 0.80984(8) 0.0337(4) Uani 1 1 d . . . C18 C 0.84976(12) 0.8005(2) 0.75624(8) 0.0347(4) Uani 1 1 d . . . C19 C 0.79561(14) 0.8432(3) 0.70310(8) 0.0445(5) Uani 1 1 d . . . H19A H 0.7370 0.8998 0.7033 0.053 Uiso 1 1 calc R . . C20 C 0.82861(16) 0.8022(3) 0.65283(9) 0.0580(6) Uani 1 1 d . . . H20A H 0.7922 0.8318 0.6189 0.070 Uiso 1 1 calc R . . C21 C 0.91708(16) 0.7156(3) 0.65035(9) 0.0580(6) Uani 1 1 d . . . H21A H 0.9384 0.6894 0.6151 0.070 Uiso 1 1 calc R . . C22 C 0.97056(15) 0.6709(3) 0.69902(9) 0.0487(5) Uani 1 1 d . . . H22A H 1.0282 0.6119 0.6972 0.058 Uiso 1 1 calc R . . C23 C 0.93963(12) 0.7132(2) 0.75321(8) 0.0373(4) Uani 1 1 d . . . C24 C 0.99509(13) 0.6711(3) 0.80376(8) 0.0438(5) Uani 1 1 d . . . H24A H 1.0522 0.6107 0.8019 0.053 Uiso 1 1 calc R . . C25 C 0.96784(12) 0.7165(3) 0.85689(8) 0.0392(4) Uani 1 1 d . . . C26 C 1.02657(15) 0.6742(3) 0.90827(9) 0.0549(6) Uani 1 1 d . . . H26A H 1.0827 0.6111 0.9061 0.066 Uiso 1 1 calc R . . C27 C 1.00237(16) 0.7237(3) 0.95940(9) 0.0660(7) Uani 1 1 d . . . H27A H 1.0418 0.6960 0.9924 0.079 Uiso 1 1 calc R . . C28 C 0.91723(17) 0.8175(4) 0.96318(9) 0.0691(7) Uani 1 1 d . . . H28A H 0.9016 0.8535 0.9988 0.083 Uiso 1 1 calc R . . C29 C 0.85752(14) 0.8567(3) 0.91615(9) 0.0532(6) Uani 1 1 d . . . H29A H 0.8007 0.9161 0.9201 0.064 Uiso 1 1 calc R . . C30 C 0.88018(12) 0.8086(2) 0.86054(7) 0.0356(4) Uani 1 1 d . . . O1 O 0.47908(9) 0.43286(15) 0.80984(5) 0.0352(3) Uani 1 1 d . . . O1WA O 0.21057(17) 0.8537(3) 0.72895(13) 0.0930(8) Uani 1 1 d . . . O2 O 0.46366(8) 0.70274(14) 0.78301(5) 0.0305(3) Uani 1 1 d . . . O3 O 0.72500(10) 1.08138(18) 0.83654(7) 0.0549(4) Uani 1 1 d . . . O4 O 0.65085(8) 0.85561(16) 0.79295(5) 0.0377(3) Uani 1 1 d . . . O5 O 0.37091(10) 1.0440(2) 0.76593(7) 0.0444(4) Uani 1 1 d . . . H5B H 0.3622(16) 1.134(3) 0.7504(10) 0.064(8) Uiso 1 1 d . . . H5C H 0.3296(19) 0.984(3) 0.7564(11) 0.064(9) Uiso 1 1 d . . . O6 O 0.53654(13) 1.1041(2) 0.84882(6) 0.0406(3) Uani 1 1 d . . . H6B H 0.5145(16) 1.185(3) 0.8477(9) 0.049(8) Uiso 1 1 d . . . H6C H 0.5937(17) 1.111(3) 0.8521(10) 0.057(8) Uiso 1 1 d . . . H1WA H 0.170(3) 0.886(5) 0.7155(17) 0.126(18) Uiso 1 1 d . . . H2WA H 0.219(2) 0.768(5) 0.7056(14) 0.117(14) 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 Zn1 0.02989(11) 0.02711(12) 0.03251(12) 0.00104(8) 0.00138(8) 0.00317(8) C1 0.0213(8) 0.0282(9) 0.0328(9) 0.0003(7) 0.0016(6) 0.0009(7) C2 0.0386(9) 0.0209(9) 0.0307(8) -0.0002(7) 0.0046(7) -0.0038(7) C3 0.0456(10) 0.0256(9) 0.0399(10) -0.0011(8) 0.0144(8) -0.0036(8) C4 0.0412(10) 0.0371(11) 0.0542(12) 0.0015(9) 0.0151(9) 0.0037(9) C5 0.0517(13) 0.0557(15) 0.0849(17) 0.0049(13) 0.0248(12) 0.0138(11) C6 0.0771(19) 0.0624(18) 0.097(2) -0.0116(15) 0.0458(17) 0.0182(14) C7 0.0889(19) 0.0530(14) 0.0654(15) -0.0192(12) 0.0403(15) -0.0030(14) C8 0.0658(14) 0.0356(11) 0.0449(12) -0.0072(9) 0.0209(10) -0.0064(10) C9 0.0773(16) 0.0499(13) 0.0349(11) -0.0094(9) 0.0110(11) -0.0133(12) C10 0.0597(13) 0.0425(12) 0.0332(10) 0.0032(9) -0.0037(9) -0.0140(10) C11 0.0745(17) 0.0658(16) 0.0421(12) 0.0064(11) -0.0157(12) -0.0184(14) C12 0.0677(17) 0.0751(19) 0.0622(16) 0.0142(13) -0.0314(13) -0.0038(14) C13 0.0480(13) 0.0701(17) 0.0685(16) 0.0074(13) -0.0111(12) 0.0065(11) C14 0.0449(11) 0.0463(12) 0.0428(11) 0.0029(9) -0.0061(9) 0.0013(9) C15 0.0406(10) 0.0307(9) 0.0327(9) 0.0034(7) -0.0018(8) -0.0059(8) C16 0.0295(9) 0.0309(10) 0.0429(10) 0.0010(8) -0.0043(7) 0.0006(8) C17 0.0245(8) 0.0283(10) 0.0474(10) 0.0002(8) 0.0001(7) -0.0028(7) C18 0.0293(9) 0.0311(10) 0.0426(10) 0.0019(8) -0.0020(8) -0.0061(7) C19 0.0354(10) 0.0483(13) 0.0478(12) 0.0082(9) -0.0056(8) -0.0053(9) C20 0.0552(13) 0.0742(17) 0.0414(12) 0.0063(11) -0.0103(10) -0.0156(12) C21 0.0609(14) 0.0706(17) 0.0428(12) -0.0081(11) 0.0072(11) -0.0122(12) C22 0.0464(11) 0.0519(13) 0.0485(12) -0.0085(10) 0.0086(9) -0.0038(10) C23 0.0351(10) 0.0355(11) 0.0415(10) -0.0012(8) 0.0046(8) -0.0017(8) C24 0.0313(9) 0.0482(12) 0.0514(12) -0.0001(9) 0.0021(8) 0.0112(9) C25 0.0311(9) 0.0427(11) 0.0428(11) 0.0022(8) -0.0011(8) 0.0051(8) C26 0.0415(11) 0.0700(16) 0.0511(13) 0.0044(11) -0.0053(10) 0.0168(11) C27 0.0577(14) 0.094(2) 0.0437(13) 0.0068(12) -0.0080(11) 0.0189(13) C28 0.0629(15) 0.105(2) 0.0388(12) -0.0065(12) 0.0028(11) 0.0193(14) C29 0.0397(11) 0.0708(16) 0.0490(12) -0.0059(11) 0.0045(9) 0.0120(11) C30 0.0288(9) 0.0375(11) 0.0396(10) 0.0011(8) 0.0000(7) 0.0004(8) O1 0.0436(7) 0.0246(7) 0.0371(7) -0.0030(5) 0.0032(5) 0.0009(5) O1WA 0.0542(12) 0.0662(14) 0.155(2) -0.0269(15) -0.0100(14) -0.0018(11) O2 0.0308(6) 0.0283(7) 0.0322(6) 0.0047(5) 0.0020(5) -0.0008(5) O3 0.0381(8) 0.0341(8) 0.0897(11) -0.0181(7) -0.0070(7) 0.0027(6) O4 0.0252(6) 0.0323(7) 0.0542(8) -0.0074(6) -0.0026(5) 0.0024(5) O5 0.0310(7) 0.0337(8) 0.0686(10) 0.0154(8) 0.0060(7) 0.0023(7) O6 0.0461(10) 0.0335(8) 0.0413(8) -0.0021(6) -0.0005(7) 0.0088(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 Zn1 O6 2.0222(15) . ? Zn1 O2 2.0244(11) . ? Zn1 O5 2.0657(14) . ? Zn1 O4 2.1004(11) . ? Zn1 O1 2.1186(12) 2_656 ? Zn1 O2 2.4783(12) 2_656 ? C1 O1 1.2537(19) . ? C1 O2 1.2713(19) . ? C1 C2 1.494(2) . ? C2 C15 1.400(2) . ? C2 C3 1.415(2) . ? C3 C4 1.416(3) . ? C3 C8 1.435(3) . ? C4 C5 1.361(3) . ? C4 H4A 0.9300 . ? C5 C6 1.408(4) . ? C5 H5A 0.9300 . ? C6 C7 1.333(4) . ? C6 H6A 0.9300 . ? C7 C8 1.431(3) . ? C7 H7A 0.9300 . ? C8 C9 1.377(3) . ? C9 C10 1.385(3) . ? C9 H9A 0.9300 . ? C10 C11 1.426(3) . ? C10 C15 1.437(3) . ? C11 C12 1.329(3) . ? C11 H11A 0.9300 . ? C12 C13 1.416(3) . ? C12 H12A 0.9300 . ? C13 C14 1.359(3) . ? C13 H13A 0.9300 . ? C14 C15 1.424(3) . ? C14 H14A 0.9300 . ? C16 O3 1.244(2) . ? C16 O4 1.269(2) . ? C16 C17 1.514(2) . ? C17 C18 1.406(2) . ? C17 C30 1.412(2) . ? C18 C19 1.433(2) . ? C18 C23 1.434(2) . ? C19 C20 1.349(3) . ? C19 H19A 0.9300 . ? C20 C21 1.413(3) . ? C20 H20A 0.9300 . ? C21 C22 1.347(3) . ? C21 H21A 0.9300 . ? C22 C23 1.424(3) . ? C22 H22A 0.9300 . ? C23 C24 1.391(3) . ? C24 C25 1.387(3) . ? C24 H24A 0.9300 . ? C25 C30 1.427(2) . ? C25 C26 1.429(3) . ? C26 C27 1.337(3) . ? C26 H26A 0.9300 . ? C27 C28 1.404(3) . ? C27 H27A 0.9300 . ? C28 C29 1.351(3) . ? C28 H28A 0.9300 . ? C29 C30 1.425(3) . ? C29 H29A 0.9300 . ? O1 Zn1 2.1186(12) 2_646 ? O1WA H1WA 0.67(4) . ? O1WA H2WA 0.87(3) . ? O2 Zn1 2.4783(11) 2_646 ? O5 H5B 0.79(3) . ? O5 H5C 0.76(3) . ? O6 H6B 0.69(2) . ? O6 H6C 0.80(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 O6 Zn1 O2 123.27(5) . . ? O6 Zn1 O5 90.81(7) . . ? O2 Zn1 O5 91.96(6) . . ? O6 Zn1 O4 89.15(6) . . ? O2 Zn1 O4 87.79(5) . . ? O5 Zn1 O4 179.67(6) . . ? O6 Zn1 O1 144.37(6) . 2_656 ? O2 Zn1 O1 92.12(4) . 2_656 ? O5 Zn1 O1 92.05(6) . 2_656 ? O4 Zn1 O1 88.17(5) . 2_656 ? O6 Zn1 O2 89.72(5) . 2_656 ? O2 Zn1 O2 146.42(2) . 2_656 ? O5 Zn1 O2 80.49(5) . 2_656 ? O4 Zn1 O2 99.83(4) . 2_656 ? O1 Zn1 O2 55.88(4) 2_656 2_656 ? O1 C1 O2 119.14(15) . . ? O1 C1 C2 120.47(15) . . ? O2 C1 C2 120.39(15) . . ? C15 C2 C3 121.81(16) . . ? C15 C2 C1 119.82(15) . . ? C3 C2 C1 118.36(15) . . ? C2 C3 C4 123.20(16) . . ? C2 C3 C8 118.25(17) . . ? C4 C3 C8 118.53(17) . . ? C5 C4 C3 121.1(2) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C7 C6 C5 121.4(2) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 121.1(2) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C9 C8 C7 122.4(2) . . ? C9 C8 C3 119.63(18) . . ? C7 C8 C3 117.9(2) . . ? C8 C9 C10 122.33(18) . . ? C8 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C9 C10 C11 121.9(2) . . ? C9 C10 C15 119.61(19) . . ? C11 C10 C15 118.4(2) . . ? C12 C11 C10 121.6(2) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C2 C15 C14 123.67(16) . . ? C2 C15 C10 118.36(17) . . ? C14 C15 C10 117.97(17) . . ? O3 C16 O4 124.34(16) . . ? O3 C16 C17 118.99(15) . . ? O4 C16 C17 116.66(15) . . ? C18 C17 C30 120.59(16) . . ? C18 C17 C16 119.90(16) . . ? C30 C17 C16 119.51(16) . . ? C17 C18 C19 123.38(17) . . ? C17 C18 C23 119.59(16) . . ? C19 C18 C23 116.99(17) . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C19 C20 C21 121.7(2) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.5(2) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C24 C23 C22 121.16(17) . . ? C24 C23 C18 118.91(17) . . ? C22 C23 C18 119.92(17) . . ? C25 C24 C23 122.04(17) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C24 C25 C30 119.70(16) . . ? C24 C25 C26 121.14(17) . . ? C30 C25 C26 119.16(17) . . ? C27 C26 C25 121.3(2) . . ? C27 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? C26 C27 C28 119.8(2) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C29 C28 C27 121.5(2) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C30 121.07(19) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C17 C30 C29 123.76(16) . . ? C17 C30 C25 119.06(16) . . ? C29 C30 C25 117.18(16) . . ? C1 O1 Zn1 100.58(10) . 2_646 ? H1WA O1WA H2WA 98(4) . . ? C1 O2 Zn1 131.18(11) . . ? C1 O2 Zn1 83.42(9) . 2_646 ? Zn1 O2 Zn1 130.20(5) . 2_646 ? C16 O4 Zn1 127.81(11) . . ? Zn1 O5 H5B 118.3(17) . . ? Zn1 O5 H5C 121(2) . . ? H5B O5 H5C 109(3) . . ? Zn1 O6 H6B 116.7(19) . . ? Zn1 O6 H6C 102.6(17) . . ? H6B O6 H6C 112(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C15 60.3(2) . . . . ? O2 C1 C2 C15 -119.37(18) . . . . ? O1 C1 C2 C3 -120.46(17) . . . . ? O2 C1 C2 C3 59.9(2) . . . . ? C15 C2 C3 C4 -177.24(17) . . . . ? C1 C2 C3 C4 3.5(3) . . . . ? C15 C2 C3 C8 0.9(3) . . . . ? C1 C2 C3 C8 -178.35(16) . . . . ? C2 C3 C4 C5 179.83(19) . . . . ? C8 C3 C4 C5 1.7(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C6 C7 C8 C9 -179.1(2) . . . . ? C6 C7 C8 C3 0.8(3) . . . . ? C2 C3 C8 C9 -0.2(3) . . . . ? C4 C3 C8 C9 178.00(18) . . . . ? C2 C3 C8 C7 179.85(18) . . . . ? C4 C3 C8 C7 -1.9(3) . . . . ? C7 C8 C9 C10 179.1(2) . . . . ? C3 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 -178.5(2) . . . . ? C8 C9 C10 C15 1.1(3) . . . . ? C9 C10 C11 C12 179.9(2) . . . . ? C15 C10 C11 C12 0.3(3) . . . . ? C10 C11 C12 C13 1.4(4) . . . . ? C11 C12 C13 C14 -1.6(4) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C3 C2 C15 C14 -179.55(17) . . . . ? C1 C2 C15 C14 -0.3(3) . . . . ? C3 C2 C15 C10 -0.6(3) . . . . ? C1 C2 C15 C10 178.67(16) . . . . ? C13 C14 C15 C2 -179.4(2) . . . . ? C13 C14 C15 C10 1.6(3) . . . . ? C9 C10 C15 C2 -0.5(3) . . . . ? C11 C10 C15 C2 179.21(18) . . . . ? C9 C10 C15 C14 178.60(18) . . . . ? C11 C10 C15 C14 -1.7(3) . . . . ? O3 C16 C17 C18 -120.7(2) . . . . ? O4 C16 C17 C18 60.4(2) . . . . ? O3 C16 C17 C30 58.5(2) . . . . ? O4 C16 C17 C30 -120.43(19) . . . . ? C30 C17 C18 C19 -176.19(17) . . . . ? C16 C17 C18 C19 2.9(3) . . . . ? C30 C17 C18 C23 1.4(3) . . . . ? C16 C17 C18 C23 -179.51(16) . . . . ? C17 C18 C19 C20 177.62(18) . . . . ? C23 C18 C19 C20 0.0(3) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C22 0.4(4) . . . . ? C20 C21 C22 C23 -1.2(4) . . . . ? C21 C22 C23 C24 -178.6(2) . . . . ? C21 C22 C23 C18 1.5(3) . . . . ? C17 C18 C23 C24 1.5(3) . . . . ? C19 C18 C23 C24 179.24(18) . . . . ? C17 C18 C23 C22 -178.56(17) . . . . ? C19 C18 C23 C22 -0.8(3) . . . . ? C22 C23 C24 C25 177.73(18) . . . . ? C18 C23 C24 C25 -2.4(3) . . . . ? C23 C24 C25 C30 0.3(3) . . . . ? C23 C24 C25 C26 -179.09(19) . . . . ? C24 C25 C26 C27 177.3(2) . . . . ? C30 C25 C26 C27 -2.0(4) . . . . ? C25 C26 C27 C28 0.7(4) . . . . ? C26 C27 C28 C29 1.3(4) . . . . ? C27 C28 C29 C30 -1.9(4) . . . . ? C18 C17 C30 C29 177.20(18) . . . . ? C16 C17 C30 C29 -1.9(3) . . . . ? C18 C17 C30 C25 -3.4(3) . . . . ? C16 C17 C30 C25 177.44(16) . . . . ? C28 C29 C30 C17 179.9(2) . . . . ? C28 C29 C30 C25 0.5(3) . . . . ? C24 C25 C30 C17 2.6(3) . . . . ? C26 C25 C30 C17 -177.99(18) . . . . ? C24 C25 C30 C29 -178.0(2) . . . . ? C26 C25 C30 C29 1.4(3) . . . . ? O2 C1 O1 Zn1 10.74(16) . . . 2_646 ? C2 C1 O1 Zn1 -168.93(12) . . . 2_646 ? O1 C1 O2 Zn1 -148.75(11) . . . . ? C2 C1 O2 Zn1 30.9(2) . . . . ? O1 C1 O2 Zn1 -9.07(13) . . . 2_646 ? C2 C1 O2 Zn1 170.60(14) . . . 2_646 ? O6 Zn1 O2 C1 -27.36(16) . . . . ? O5 Zn1 O2 C1 -119.63(14) . . . . ? O4 Zn1 O2 C1 60.16(14) . . . . ? O1 Zn1 O2 C1 148.25(14) 2_656 . . . ? O2 Zn1 O2 C1 164.69(13) 2_656 . . . ? O6 Zn1 O2 Zn1 -150.05(8) . . . 2_646 ? O5 Zn1 O2 Zn1 117.69(7) . . . 2_646 ? O4 Zn1 O2 Zn1 -62.52(7) . . . 2_646 ? O1 Zn1 O2 Zn1 25.57(7) 2_656 . . 2_646 ? O2 Zn1 O2 Zn1 42.01(7) 2_656 . . 2_646 ? O3 C16 O4 Zn1 10.8(3) . . . . ? C17 C16 O4 Zn1 -170.36(11) . . . . ? O6 Zn1 O4 C16 -33.17(15) . . . . ? O2 Zn1 O4 C16 -156.51(15) . . . . ? O5 Zn1 O4 C16 -116(16) . . . . ? O1 Zn1 O4 C16 111.30(15) 2_656 . . . ? O2 Zn1 O4 C16 56.40(15) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.291 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.050 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 623312' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H54 N4 O9 Zn2' _chemical_formula_weight 1394.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.62(2) _cell_length_b 17.580(15) _cell_length_c 18.070(17) _cell_angle_alpha 90.00 _cell_angle_beta 115.734(13) _cell_angle_gamma 90.00 _cell_volume 6474(10) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8473 _cell_measurement_theta_min 1.5297 _cell_measurement_theta_max 27.9564 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.431 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8550 _exptl_absorpt_correction_T_max 0.9235 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23800 _diffrn_reflns_av_R_equivalents 0.1404 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5688 _reflns_number_gt 4214 _reflns_threshold_expression I>2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. In the data, there are 135 restrains including 63 operations of DFIX and 72 operations of ISOR, which are used to refine the disordered anthracene ring. ; _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^+149.8739P] 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 SHELXL _refine_ls_extinction_coef 0.00136(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5688 _refine_ls_number_parameters 579 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.2341 _refine_ls_wR_factor_gt 0.2180 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.07115(4) 0.32019(5) 0.31859(6) 0.0193(3) Uani 1 1 d . . . N1 N 0.0867(3) 0.3615(4) 0.4365(4) 0.0253(17) Uani 1 1 d . . . N2 N 0.1347(3) 0.2356(4) 0.3948(4) 0.0226(16) Uani 1 1 d . . . O1 O 0.1439(3) 0.3895(3) 0.3155(3) 0.0243(14) Uani 1 1 d . . . O2 O 0.0872(3) 0.4722(5) 0.2148(5) 0.061(3) Uani 1 1 d . . . O3 O 0.0293(3) 0.2736(3) 0.2022(3) 0.0188(12) Uani 1 1 d . . . O4 O 0.1225(3) 0.2455(4) 0.1924(4) 0.0268(14) Uani 1 1 d . A . O1W O 0.0000 0.4081(5) 0.2500 0.0227(19) Uani 1 2 d SD . . C1 C 0.1397(5) 0.4452(5) 0.2686(6) 0.035(2) Uani 1 1 d . . . C2 C 0.2033(4) 0.4846(5) 0.2830(5) 0.026(2) Uani 1 1 d . . . C3 C 0.2401(4) 0.4572(5) 0.2417(5) 0.028(2) Uani 1 1 d . . . C4 C 0.2230(6) 0.3898(6) 0.1936(6) 0.043(3) Uani 1 1 d . . . H4 H 0.1847 0.3623 0.1860 0.052 Uiso 1 1 calc R . . C5 C 0.2619(8) 0.3646(7) 0.1582(8) 0.074(5) Uani 1 1 d . . . H5 H 0.2508 0.3188 0.1273 0.089 Uiso 1 1 calc R . . C6 C 0.3193(7) 0.4060(7) 0.1669(8) 0.069(4) Uani 1 1 d . . . H6 H 0.3450 0.3881 0.1408 0.083 Uiso 1 1 calc R . . C7 C 0.3368(5) 0.4710(6) 0.2128(6) 0.041(3) Uani 1 1 d . . . H7 H 0.3752 0.4978 0.2190 0.049 Uiso 1 1 calc R . . C8 C 0.2980(4) 0.4985(5) 0.2511(5) 0.027(2) Uani 1 1 d . . . C9 C 0.3177(4) 0.5622(5) 0.3027(5) 0.0231(19) Uani 1 1 d . . . H9 H 0.3556 0.5894 0.3077 0.028 Uiso 1 1 calc R . . C10 C 0.2839(4) 0.5875(5) 0.3474(6) 0.027(2) Uani 1 1 d . . . C11 C 0.3065(5) 0.6484(5) 0.4051(6) 0.039(2) Uani 1 1 d . . . H11 H 0.3448 0.6754 0.4116 0.046 Uiso 1 1 calc R . . C12 C 0.2755(7) 0.6687(7) 0.4506(8) 0.061(4) Uani 1 1 d . . . H12 H 0.2929 0.7078 0.4906 0.073 Uiso 1 1 calc R . . C13 C 0.2143(7) 0.6300(7) 0.4381(9) 0.071(4) Uani 1 1 d . . . H13 H 0.1904 0.6465 0.4673 0.085 Uiso 1 1 calc R . . C14 C 0.1924(6) 0.5720(6) 0.3859(8) 0.053(3) Uani 1 1 d . . . H14 H 0.1541 0.5459 0.3810 0.063 Uiso 1 1 calc R . . C15 C 0.2245(4) 0.5474(5) 0.3369(6) 0.028(2) Uani 1 1 d . . . C16 C 0.0625(4) 0.2478(4) 0.1629(5) 0.0178(17) Uani 1 1 d . . . C17 C 0.0176(15) 0.2046(11) 0.0820(7) 0.022(5) Uani 0.491(12) 1 d PD A 1 C18 C -0.0102(9) 0.1346(7) 0.0827(8) 0.018(5) Uani 0.491(12) 1 d PDU A 1 C19 C -0.0021(8) 0.0999(7) 0.1560(7) 0.010(4) Uani 0.491(12) 1 d PDU A 1 H19A H 0.0206 0.1261 0.2065 0.011 Uiso 0.491(12) 1 calc PR A 1 C20 C -0.0267(9) 0.0276(7) 0.1560(8) 0.033(5) Uani 0.491(12) 1 d PD A 1 H20A H -0.0187 0.0034 0.2064 0.040 Uiso 0.491(12) 1 calc PR A 1 C21 C -0.0633(8) -0.0096(7) 0.0816(8) 0.035(5) Uani 0.491(12) 1 d PDU A 1 H21A H -0.0802 -0.0591 0.0813 0.042 Uiso 0.491(12) 1 calc PR A 1 C22 C -0.075(2) 0.0263(15) 0.0080(8) 0.053(12) Uani 0.491(12) 1 d PD A 1 H22A H -0.0998 0.0012 -0.0426 0.064 Uiso 0.491(12) 1 calc PR A 1 C23 C -0.0498(7) 0.0986(6) 0.0078(7) 0.022(4) Uani 0.491(12) 1 d PD A 1 C24 C -0.0601(9) 0.1328(8) -0.0661(8) 0.029(6) Uani 0.491(12) 1 d PDU A 1 H24A H -0.0871 0.1083 -0.1164 0.035 Uiso 0.491(12) 1 calc PR A 1 C25 C -0.0314(12) 0.2022(9) -0.0677(8) 0.028(6) Uani 0.491(12) 1 d PD A 1 C26 C -0.0419(8) 0.2359(8) -0.1419(6) 0.042(6) Uani 0.491(12) 1 d PD A 1 H26A H -0.0712 0.2131 -0.1921 0.050 Uiso 0.491(12) 1 calc PR A 1 C27 C -0.0096(15) 0.3031(12) -0.1432(7) 0.040(9) Uani 0.491(12) 1 d PD A 1 H27A H -0.0135 0.3234 -0.1938 0.048 Uiso 0.491(12) 1 calc PR A 1 C28 C 0.0285(11) 0.3402(9) -0.0693(8) 0.049(7) Uani 0.491(12) 1 d PD A 1 H28A H 0.0474 0.3884 -0.0698 0.059 Uiso 0.491(12) 1 calc PR A 1 C29 C 0.0389(9) 0.3066(9) 0.0049(7) 0.024(5) Uani 0.491(12) 1 d PDU A 1 H29A H 0.0675 0.3304 0.0550 0.029 Uiso 0.491(12) 1 calc PR A 1 C30 C 0.0079(8) 0.2387(8) 0.0071(6) 0.021(5) Uani 0.491(12) 1 d PD A 1 C31 C 0.0639(5) 0.4243(7) 0.4557(7) 0.047(3) Uani 1 1 d . . . H31 H 0.0351 0.4560 0.4126 0.056 Uiso 1 1 calc R . . C32 C 0.0808(5) 0.4459(9) 0.5376(8) 0.072(5) Uani 1 1 d . . . H32 H 0.0635 0.4913 0.5490 0.086 Uiso 1 1 calc R . . C33 C 0.1226(6) 0.4006(10) 0.6006(8) 0.084(6) Uani 1 1 d . . . H33 H 0.1347 0.4151 0.6559 0.101 Uiso 1 1 calc R . . C34 C 0.1477(4) 0.3325(7) 0.5834(6) 0.045(3) Uani 1 1 d . . . C35 C 0.1931(5) 0.2839(9) 0.6445(7) 0.072(5) Uani 1 1 d . . . H35 H 0.2070 0.2959 0.7008 0.086 Uiso 1 1 calc R . . C36 C 0.2175(5) 0.2197(7) 0.6238(6) 0.046(3) Uani 1 1 d . . . H36 H 0.2474 0.1877 0.6657 0.055 Uiso 1 1 calc R . . C37 C 0.1980(4) 0.2012(6) 0.5395(5) 0.030(2) Uani 1 1 d . . . C38 C 0.2218(4) 0.1370(6) 0.5145(6) 0.035(2) Uani 1 1 d . . . H38 H 0.2513 0.1027 0.5538 0.043 Uiso 1 1 calc R . . C39 C 0.2013(5) 0.1248(5) 0.4317(6) 0.040(3) Uani 1 1 d . . . H39 H 0.2167 0.0814 0.4139 0.048 Uiso 1 1 calc R . . C40 C 0.1582(4) 0.1756(5) 0.3733(5) 0.031(2) Uani 1 1 d . . . H40 H 0.1456 0.1663 0.3167 0.037 Uiso 1 1 calc R . . C41 C 0.1541(4) 0.2493(5) 0.4777(5) 0.0232(19) Uani 1 1 d . . . C42 C 0.1286(4) 0.3178(6) 0.4984(5) 0.031(2) Uani 1 1 d . . . C17' C 0.0251(17) 0.2234(12) 0.0731(8) 0.019(5) Uani 0.509(12) 1 d PDU A 2 C18' C -0.0089(9) 0.1551(8) 0.0562(8) 0.021(5) Uani 0.509(12) 1 d PDU A 2 C19' C -0.0121(9) 0.1108(8) 0.1181(8) 0.022(5) Uani 0.509(12) 1 d PDU A 2 H19B H 0.0095 0.1273 0.1736 0.027 Uiso 0.509(12) 1 calc PR A 2 C20' C -0.0467(8) 0.0427(8) 0.0995(8) 0.040(6) Uani 0.509(12) 1 d PD A 2 H20B H -0.0482 0.0126 0.1423 0.048 Uiso 0.509(12) 1 calc PR A 2 C21' C -0.079(2) 0.0185(15) 0.0180(9) 0.020(7) Uani 0.509(12) 1 d PDU A 2 H21B H -0.1029 -0.0281 0.0052 0.023 Uiso 0.509(12) 1 calc PR A 2 C22' C -0.0771(8) 0.0631(7) -0.0442(8) 0.034(5) Uani 0.509(12) 1 d PD A 2 H22B H -0.1011 0.0479 -0.0998 0.041 Uiso 0.509(12) 1 calc PR A 2 C23' C -0.0402(8) 0.1296(7) -0.0262(8) 0.023(4) Uani 0.509(12) 1 d PD A 2 C24' C -0.0382(12) 0.1732(9) -0.0893(8) 0.030(6) Uani 0.509(12) 1 d PD A 2 H24B H -0.0627 0.1578 -0.1448 0.036 Uiso 0.509(12) 1 calc PR A 2 C25' C -0.0007(7) 0.2395(6) -0.0719(7) 0.020(4) Uani 0.509(12) 1 d PDU A 2 C26' C 0.0018(13) 0.2818(11) -0.1354(7) 0.041(9) Uani 0.509(12) 1 d PDU A 2 H26B H -0.0216 0.2650 -0.1905 0.049 Uiso 0.509(12) 1 calc PR A 2 C27' C 0.0385(9) 0.3487(8) -0.1188(7) 0.034(5) Uani 0.509(12) 1 d PD A 2 H27B H 0.0409 0.3769 -0.1622 0.040 Uiso 0.509(12) 1 calc PR A 2 C28' C 0.0715(7) 0.3734(7) -0.0377(7) 0.030(5) Uani 0.509(12) 1 d PD A 2 H28B H 0.0976 0.4181 -0.0258 0.036 Uiso 0.509(12) 1 calc PR A 2 C29' C 0.0666(8) 0.3339(7) 0.0255(6) 0.019(4) Uani 0.509(12) 1 d PD A 2 H29B H 0.0876 0.3531 0.0800 0.023 Uiso 0.509(12) 1 calc PR A 2 C30' C 0.0305(8) 0.2647(8) 0.0096(6) 0.016(4) Uani 0.509(12) 1 d PDU A 2 H1W H -0.022(5) 0.431(6) 0.272(7) 0.08(5) Uiso 1 1 d 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 Zn1 0.0200(5) 0.0162(5) 0.0253(6) 0.0004(4) 0.0133(4) 0.0003(4) N1 0.019(4) 0.037(5) 0.021(4) -0.008(3) 0.010(3) -0.003(3) N2 0.022(4) 0.021(4) 0.028(4) -0.001(3) 0.013(3) -0.006(3) O1 0.021(3) 0.024(3) 0.028(3) 0.010(3) 0.010(3) 0.003(3) O2 0.022(4) 0.061(5) 0.075(6) 0.055(5) -0.002(4) -0.009(3) O3 0.019(3) 0.020(3) 0.018(3) 0.001(2) 0.009(2) 0.001(2) O4 0.022(3) 0.033(4) 0.027(3) -0.001(3) 0.012(3) 0.003(3) O1W 0.018(4) 0.012(4) 0.035(5) 0.000 0.009(4) 0.000 C1 0.031(5) 0.028(5) 0.048(6) 0.016(5) 0.020(5) 0.002(4) C2 0.013(4) 0.030(5) 0.024(5) 0.017(4) -0.001(4) -0.003(4) C3 0.024(5) 0.034(5) 0.023(5) 0.002(4) 0.009(4) -0.009(4) C4 0.069(7) 0.034(6) 0.033(6) -0.018(5) 0.028(6) -0.035(5) C5 0.143(13) 0.051(8) 0.061(8) -0.031(7) 0.075(9) -0.059(9) C6 0.125(12) 0.047(8) 0.073(9) -0.026(7) 0.079(9) -0.037(8) C7 0.050(6) 0.044(6) 0.044(6) -0.003(5) 0.035(5) -0.012(5) C8 0.023(4) 0.030(5) 0.029(5) 0.010(4) 0.012(4) -0.001(4) C9 0.019(4) 0.019(4) 0.031(5) 0.005(4) 0.010(4) -0.004(3) C10 0.033(5) 0.025(5) 0.033(5) 0.010(4) 0.022(4) 0.000(4) C11 0.062(7) 0.021(5) 0.048(6) -0.007(5) 0.038(6) -0.014(5) C12 0.098(10) 0.037(7) 0.083(9) -0.017(6) 0.073(8) -0.015(7) C13 0.118(12) 0.032(7) 0.120(12) 0.008(7) 0.105(11) 0.009(7) C14 0.066(8) 0.024(6) 0.103(10) 0.001(6) 0.071(8) -0.002(5) C15 0.026(5) 0.020(5) 0.040(6) 0.011(4) 0.017(4) -0.003(4) C16 0.028(5) 0.010(4) 0.020(4) 0.002(3) 0.013(4) 0.003(3) C17 0.023(13) 0.024(15) 0.026(12) 0.012(10) 0.019(10) 0.020(11) C18 0.024(8) 0.014(8) 0.015(8) -0.002(7) 0.009(7) 0.002(6) C19 0.012(7) 0.008(6) 0.009(8) -0.003(6) 0.006(6) 0.002(5) C20 0.037(12) 0.014(10) 0.063(15) 0.010(10) 0.035(12) 0.002(9) C21 0.029(8) 0.030(9) 0.043(9) -0.004(7) 0.013(7) 0.005(7) C22 0.04(2) 0.06(3) 0.07(2) -0.04(2) 0.04(2) -0.003(19) C23 0.022(9) 0.018(10) 0.029(11) -0.008(9) 0.013(9) 0.009(8) C24 0.027(9) 0.033(9) 0.031(9) -0.011(7) 0.015(8) 0.002(7) C25 0.024(12) 0.020(13) 0.024(12) -0.002(10) -0.003(11) 0.000(11) C26 0.033(11) 0.053(14) 0.029(12) 0.020(10) 0.005(9) 0.015(10) C27 0.09(2) 0.017(12) 0.018(11) 0.005(9) 0.028(12) 0.004(15) C28 0.09(2) 0.048(15) 0.027(12) 0.003(10) 0.042(13) -0.009(14) C29 0.023(8) 0.027(9) 0.023(8) -0.010(7) 0.012(6) -0.001(7) C30 0.013(10) 0.027(12) 0.025(11) 0.007(9) 0.010(8) -0.003(8) C31 0.022(5) 0.057(7) 0.066(7) -0.041(6) 0.023(5) -0.012(5) C32 0.031(6) 0.100(11) 0.080(10) -0.058(9) 0.020(7) 0.005(7) C33 0.029(6) 0.158(16) 0.056(8) -0.065(10) 0.012(6) 0.004(8) C34 0.015(4) 0.094(9) 0.021(5) -0.017(6) 0.002(4) 0.010(5) C35 0.026(6) 0.160(16) 0.030(6) -0.011(8) 0.013(5) 0.016(7) C36 0.029(5) 0.091(9) 0.020(5) 0.010(5) 0.013(4) 0.009(6) C37 0.022(4) 0.047(6) 0.025(5) 0.015(4) 0.013(4) -0.004(4) C38 0.022(5) 0.038(6) 0.038(6) 0.025(5) 0.005(4) 0.004(4) C39 0.035(5) 0.017(5) 0.047(6) 0.005(4) -0.001(5) 0.002(4) C40 0.036(5) 0.019(5) 0.026(5) -0.007(4) 0.004(4) -0.003(4) C41 0.018(4) 0.036(5) 0.019(4) 0.000(4) 0.011(4) -0.001(4) C42 0.021(4) 0.049(6) 0.027(5) -0.020(5) 0.015(4) -0.015(4) C17' 0.018(8) 0.014(8) 0.022(9) -0.007(7) 0.006(7) 0.003(7) C18' 0.015(7) 0.014(8) 0.027(8) 0.000(7) 0.004(6) -0.004(6) C19' 0.023(8) 0.033(9) 0.011(8) 0.002(7) 0.008(7) 0.002(6) C20' 0.028(11) 0.017(10) 0.086(19) 0.001(11) 0.035(13) -0.008(9) C21' 0.013(10) 0.015(10) 0.028(10) -0.003(8) 0.007(8) -0.012(7) C22' 0.029(10) 0.024(11) 0.040(12) -0.016(10) 0.007(10) 0.002(8) C23' 0.028(11) 0.021(10) 0.016(11) 0.012(8) 0.007(9) 0.011(8) C24' 0.022(10) 0.037(15) 0.022(11) -0.013(10) 0.000(9) -0.013(12) C25' 0.024(7) 0.019(7) 0.017(7) -0.012(6) 0.010(6) 0.002(6) C26' 0.041(11) 0.042(13) 0.040(12) -0.003(7) 0.017(8) 0.006(9) C27' 0.046(12) 0.045(12) 0.008(9) 0.006(8) 0.008(8) -0.007(10) C28' 0.027(10) 0.028(11) 0.041(12) 0.006(9) 0.020(9) 0.011(8) C29' 0.029(10) 0.007(9) 0.029(10) -0.002(7) 0.020(8) 0.002(7) C30' 0.019(8) 0.011(8) 0.018(7) -0.002(6) 0.009(6) -0.002(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 Zn1 O3 2.065(6) . ? Zn1 O1 2.068(6) . ? Zn1 N2 2.111(7) . ? Zn1 N1 2.130(7) . ? Zn1 O1W 2.187(6) . ? Zn1 O3 2.288(6) 2 ? Zn1 Zn1 3.095(3) 2 ? N1 C31 1.327(12) . ? N1 C42 1.349(12) . ? N2 C40 1.313(11) . ? N2 C41 1.386(10) . ? O1 C1 1.272(10) . ? O2 C1 1.255(11) . ? O3 C16 1.317(9) . ? O3 Zn1 2.288(6) 2 ? O4 C16 1.226(9) . ? O1W Zn1 2.187(6) 2 ? O1W H1W 0.850(10) . ? C1 C2 1.515(12) . ? C2 C15 1.411(13) . ? C2 C3 1.421(13) . ? C3 C4 1.421(13) . ? C3 C8 1.442(12) . ? C4 C5 1.366(16) . ? C4 H4 0.9500 . ? C5 C6 1.435(17) . ? C5 H5 0.9500 . ? C6 C7 1.365(15) . ? C6 H6 0.9500 . ? C7 C8 1.418(13) . ? C7 H7 0.9500 . ? C8 C9 1.401(12) . ? C9 C10 1.403(12) . ? C9 H9 0.9500 . ? C10 C11 1.424(13) . ? C10 C15 1.456(12) . ? C11 C12 1.340(14) . ? C11 H11 0.9500 . ? C12 C13 1.468(17) . ? C12 H12 0.9500 . ? C13 C14 1.330(17) . ? C13 H13 0.9500 . ? C14 C15 1.434(13) . ? C14 H14 0.9500 . ? C16 C17' 1.530(15) . ? C16 C17 1.567(14) . ? C17 C18 1.384(8) . ? C17 C30 1.407(9) . ? C18 C19 1.396(9) . ? C18 C23 1.409(15) . ? C19 C20 1.389(8) . ? C19 H19A 0.9500 . ? C20 C21 1.397(9) . ? C20 H20A 0.9500 . ? C21 C22 1.390(8) . ? C21 H21A 0.9500 . ? C22 C23 1.391(8) . ? C22 H22A 0.9500 . ? C23 C24 1.391(9) . ? C24 C25 1.387(8) . ? C24 H24A 0.9500 . ? C25 C26 1.388(9) . ? C25 C30 1.410(14) . ? C26 C27 1.393(8) . ? C26 H26A 0.9500 . ? C27 C28 1.398(9) . ? C27 H27A 0.9500 . ? C28 C29 1.389(9) . ? C28 H28A 0.9500 . ? C29 C30 1.394(14) . ? C29 H29A 0.9500 . ? C31 C32 1.410(15) . ? C31 H31 0.9500 . ? C32 C33 1.37(2) . ? C32 H32 0.9500 . ? C33 C34 1.415(17) . ? C33 H33 0.9500 . ? C34 C35 1.421(16) . ? C34 C42 1.428(12) . ? C35 C36 1.377(17) . ? C35 H35 0.9500 . ? C36 C37 1.427(13) . ? C36 H36 0.9500 . ? C37 C38 1.409(14) . ? C37 C41 1.410(12) . ? C38 C39 1.377(14) . ? C38 H38 0.9500 . ? C39 C40 1.404(12) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.451(13) . ? C17' C18' 1.387(8) . ? C17' C30' 1.407(9) . ? C18' C19' 1.390(9) . ? C18' C23' 1.416(15) . ? C19' C20' 1.389(8) . ? C19' H19B 0.9500 . ? C20' C21' 1.396(9) . ? C20' H20B 0.9500 . ? C21' C22' 1.389(8) . ? C21' H21B 0.9500 . ? C22' C23' 1.390(8) . ? C22' H22B 0.9500 . ? C23' C24' 1.391(9) . ? C24' C25' 1.395(8) . ? C24' H24B 0.9500 . ? C25' C26' 1.388(8) . ? C25' C30' 1.400(13) . ? C26' C27' 1.395(8) . ? C26' H26B 0.9500 . ? C27' C28' 1.394(8) . ? C27' H27B 0.9500 . ? C28' C29' 1.382(9) . ? C28' H28B 0.9500 . ? C29' C30' 1.424(13) . ? C29' H29B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 103.0(2) . . ? O3 Zn1 N2 105.4(3) . . ? O1 Zn1 N2 96.2(2) . . ? O3 Zn1 N1 163.3(2) . . ? O1 Zn1 N1 92.2(3) . . ? N2 Zn1 N1 79.5(3) . . ? O3 Zn1 O1W 78.7(2) . . ? O1 Zn1 O1W 88.1(2) . . ? N2 Zn1 O1W 173.09(19) . . ? N1 Zn1 O1W 95.0(2) . . ? O3 Zn1 O3 73.0(2) . 2 ? O1 Zn1 O3 162.2(2) . 2 ? N2 Zn1 O3 101.6(2) . 2 ? N1 Zn1 O3 90.4(2) . 2 ? O1W Zn1 O3 74.09(19) . 2 ? O3 Zn1 Zn1 47.67(15) . 2 ? O1 Zn1 Zn1 122.79(16) . 2 ? N2 Zn1 Zn1 134.38(19) . 2 ? N1 Zn1 Zn1 117.64(19) . 2 ? O1W Zn1 Zn1 44.96(16) . 2 ? O3 Zn1 Zn1 41.84(14) 2 2 ? C31 N1 C42 118.0(8) . . ? C31 N1 Zn1 129.1(7) . . ? C42 N1 Zn1 112.7(6) . . ? C40 N2 C41 118.8(8) . . ? C40 N2 Zn1 128.4(6) . . ? C41 N2 Zn1 112.8(6) . . ? C1 O1 Zn1 129.9(6) . . ? C16 O3 Zn1 124.7(5) . . ? C16 O3 Zn1 142.4(5) . 2 ? Zn1 O3 Zn1 90.5(2) . 2 ? Zn1 O1W Zn1 90.1(3) 2 . ? Zn1 O1W H1W 100(9) 2 . ? Zn1 O1W H1W 120(9) . . ? O2 C1 O1 125.3(8) . . ? O2 C1 C2 118.0(8) . . ? O1 C1 C2 116.5(8) . . ? C15 C2 C3 121.8(8) . . ? C15 C2 C1 119.2(8) . . ? C3 C2 C1 119.0(8) . . ? C2 C3 C4 122.5(8) . . ? C2 C3 C8 118.6(8) . . ? C4 C3 C8 118.9(9) . . ? C5 C4 C3 119.8(9) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.3(10) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 120.2(11) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.2(10) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.9(8) . . ? C9 C8 C3 119.3(8) . . ? C7 C8 C3 119.7(9) . . ? C8 C9 C10 122.8(8) . . ? C8 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C11 123.2(8) . . ? C9 C10 C15 118.3(8) . . ? C11 C10 C15 118.4(8) . . ? C12 C11 C10 122.2(10) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 119.5(11) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.0(10) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 122.4(10) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C2 C15 C14 123.4(8) . . ? C2 C15 C10 119.1(8) . . ? C14 C15 C10 117.4(9) . . ? O4 C16 O3 124.0(7) . . ? O4 C16 C17' 116.7(16) . . ? O3 C16 C17' 119.1(16) . . ? O4 C16 C17 122.4(15) . . ? O3 C16 C17 112.4(14) . . ? C17' C16 C17 16.0(6) . . ? C18 C17 C30 120.4(9) . . ? C18 C17 C16 122.3(8) . . ? C30 C17 C16 117.3(8) . . ? C17 C18 C19 121.6(9) . . ? C17 C18 C23 119.5(9) . . ? C19 C18 C23 118.8(7) . . ? C20 C19 C18 120.8(8) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C19 C20 C21 119.9(7) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 120.6(8) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C24 C23 C22 120.0(9) . . ? C24 C23 C18 120.0(8) . . ? C22 C23 C18 119.9(9) . . ? C25 C24 C23 121.1(9) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 120.7(10) . . ? C24 C25 C30 119.1(8) . . ? C26 C25 C30 120.2(7) . . ? C25 C26 C27 120.5(8) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C28 119.4(7) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? C29 C28 C27 120.0(8) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 121.0(9) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C29 C30 C17 121.4(9) . . ? C29 C30 C25 118.6(7) . . ? C17 C30 C25 119.9(8) . . ? N1 C31 C32 122.6(12) . . ? N1 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C33 C32 C31 119.3(12) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.4(11) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 124.2(10) . . ? C33 C34 C42 115.3(10) . . ? C35 C34 C42 120.3(10) . . ? C36 C35 C34 121.5(10) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 120.1(10) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C41 117.6(8) . . ? C38 C37 C36 122.8(9) . . ? C41 C37 C36 119.6(9) . . ? C39 C38 C37 118.6(8) . . ? C39 C38 H38 120.7 . . ? C37 C38 H38 120.7 . . ? C38 C39 C40 120.9(9) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? N2 C40 C39 121.8(9) . . ? N2 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N2 C41 C37 122.3(8) . . ? N2 C41 C42 116.6(8) . . ? C37 C41 C42 121.0(8) . . ? N1 C42 C34 124.3(9) . . ? N1 C42 C41 118.2(7) . . ? C34 C42 C41 117.4(9) . . ? C18' C17' C30' 120.2(9) . . ? C18' C17' C16 118.3(8) . . ? C30' C17' C16 121.1(9) . . ? C19' C18' C17' 121.7(9) . . ? C19' C18' C23' 119.4(7) . . ? C17' C18' C23' 118.8(8) . . ? C18' C19' C20' 120.6(9) . . ? C18' C19' H19B 119.7 . . ? C20' C19' H19B 119.7 . . ? C19' C20' C21' 120.1(7) . . ? C19' C20' H20B 119.9 . . ? C21' C20' H20B 119.9 . . ? C22' C21' C20' 119.5(7) . . ? C22' C21' H21B 120.2 . . ? C20' C21' H21B 120.2 . . ? C21' C22' C23' 121.0(8) . . ? C21' C22' H22B 119.5 . . ? C23' C22' H22B 119.5 . . ? C22' C23' C24' 120.1(9) . . ? C22' C23' C18' 119.2(9) . . ? C24' C23' C18' 120.5(8) . . ? C23' C24' C25' 120.6(9) . . ? C23' C24' H24B 119.7 . . ? C25' C24' H24B 119.7 . . ? C26' C25' C24' 120.0(9) . . ? C26' C25' C30' 121.1(7) . . ? C24' C25' C30' 118.8(7) . . ? C25' C26' C27' 120.5(8) . . ? C25' C26' H26B 119.7 . . ? C27' C26' H26B 119.7 . . ? C28' C27' C26' 119.1(7) . . ? C28' C27' H27B 120.4 . . ? C26' C27' H27B 120.4 . . ? C29' C28' C27' 120.9(8) . . ? C29' C28' H28B 119.5 . . ? C27' C28' H28B 119.5 . . ? C28' C29' C30' 120.5(8) . . ? C28' C29' H29B 119.8 . . ? C30' C29' H29B 119.8 . . ? C25' C30' C17' 120.8(8) . . ? C25' C30' C29' 117.8(7) . . ? C17' C30' C29' 121.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N1 C31 -72.8(13) . . . . ? O1 Zn1 N1 C31 82.4(8) . . . . ? N2 Zn1 N1 C31 178.3(8) . . . . ? O1W Zn1 N1 C31 -5.9(8) . . . . ? O3 Zn1 N1 C31 -80.0(8) 2 . . . ? Zn1 Zn1 N1 C31 -46.8(8) 2 . . . ? O3 Zn1 N1 C42 110.9(9) . . . . ? O1 Zn1 N1 C42 -93.9(6) . . . . ? N2 Zn1 N1 C42 2.0(6) . . . . ? O1W Zn1 N1 C42 177.8(6) . . . . ? O3 Zn1 N1 C42 103.7(6) 2 . . . ? Zn1 Zn1 N1 C42 136.9(5) 2 . . . ? O3 Zn1 N2 C40 17.6(8) . . . . ? O1 Zn1 N2 C40 -87.7(7) . . . . ? N1 Zn1 N2 C40 -178.8(8) . . . . ? O1W Zn1 N2 C40 143.8(18) . . . . ? O3 Zn1 N2 C40 93.0(7) 2 . . . ? Zn1 Zn1 N2 C40 62.6(8) 2 . . . ? O3 Zn1 N2 C41 -164.5(5) . . . . ? O1 Zn1 N2 C41 90.1(5) . . . . ? N1 Zn1 N2 C41 -0.9(5) . . . . ? O1W Zn1 N2 C41 -38(2) . . . . ? O3 Zn1 N2 C41 -89.2(5) 2 . . . ? Zn1 Zn1 N2 C41 -119.5(5) 2 . . . ? O3 Zn1 O1 C1 58.9(8) . . . . ? N2 Zn1 O1 C1 166.4(8) . . . . ? N1 Zn1 O1 C1 -113.9(8) . . . . ? O1W Zn1 O1 C1 -19.0(8) . . . . ? O3 Zn1 O1 C1 -15.7(13) 2 . . . ? Zn1 Zn1 O1 C1 11.3(9) 2 . . . ? O1 Zn1 O3 C16 43.0(6) . . . . ? N2 Zn1 O3 C16 -57.3(6) . . . . ? N1 Zn1 O3 C16 -162.5(9) . . . . ? O1W Zn1 O3 C16 128.4(6) . . . . ? O3 Zn1 O3 C16 -155.0(5) 2 . . . ? Zn1 Zn1 O3 C16 165.8(7) 2 . . . ? O1 Zn1 O3 Zn1 -122.8(2) . . . 2 ? N2 Zn1 O3 Zn1 136.9(2) . . . 2 ? N1 Zn1 O3 Zn1 31.7(10) . . . 2 ? O1W Zn1 O3 Zn1 -37.44(16) . . . 2 ? O3 Zn1 O3 Zn1 39.2(2) 2 . . 2 ? O3 Zn1 O1W Zn1 39.50(15) . . . 2 ? O1 Zn1 O1W Zn1 143.14(18) . . . 2 ? N2 Zn1 O1W Zn1 -88(2) . . . 2 ? N1 Zn1 O1W Zn1 -124.8(2) . . . 2 ? O3 Zn1 O1W Zn1 -35.82(14) 2 . . 2 ? Zn1 O1 C1 O2 3.6(16) . . . . ? Zn1 O1 C1 C2 179.8(6) . . . . ? O2 C1 C2 C15 85.0(12) . . . . ? O1 C1 C2 C15 -91.5(11) . . . . ? O2 C1 C2 C3 -94.9(12) . . . . ? O1 C1 C2 C3 88.6(11) . . . . ? C15 C2 C3 C4 173.8(9) . . . . ? C1 C2 C3 C4 -6.3(13) . . . . ? C15 C2 C3 C8 -4.4(13) . . . . ? C1 C2 C3 C8 175.4(8) . . . . ? C2 C3 C4 C5 -177.2(11) . . . . ? C8 C3 C4 C5 1.0(16) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C4 C5 C6 C7 1(2) . . . . ? C5 C6 C7 C8 -1(2) . . . . ? C6 C7 C8 C9 175.7(10) . . . . ? C6 C7 C8 C3 0.4(16) . . . . ? C2 C3 C8 C9 2.5(13) . . . . ? C4 C3 C8 C9 -175.8(9) . . . . ? C2 C3 C8 C7 177.9(8) . . . . ? C4 C3 C8 C7 -0.4(14) . . . . ? C7 C8 C9 C10 -174.4(9) . . . . ? C3 C8 C9 C10 0.9(13) . . . . ? C8 C9 C10 C11 174.7(9) . . . . ? C8 C9 C10 C15 -2.4(13) . . . . ? C9 C10 C11 C12 -176.0(11) . . . . ? C15 C10 C11 C12 1.1(16) . . . . ? C10 C11 C12 C13 -3.2(19) . . . . ? C11 C12 C13 C14 4(2) . . . . ? C12 C13 C14 C15 -4(2) . . . . ? C3 C2 C15 C14 -173.5(9) . . . . ? C1 C2 C15 C14 6.6(13) . . . . ? C3 C2 C15 C10 3.0(13) . . . . ? C1 C2 C15 C10 -176.9(8) . . . . ? C13 C14 C15 C2 178.0(11) . . . . ? C13 C14 C15 C10 1.4(17) . . . . ? C9 C10 C15 C2 0.4(12) . . . . ? C11 C10 C15 C2 -176.8(8) . . . . ? C9 C10 C15 C14 177.2(9) . . . . ? C11 C10 C15 C14 -0.1(13) . . . . ? Zn1 O3 C16 O4 3.2(11) . . . . ? Zn1 O3 C16 O4 159.6(6) 2 . . . ? Zn1 O3 C16 C17' -172.8(8) . . . . ? Zn1 O3 C16 C17' -16.4(13) 2 . . . ? Zn1 O3 C16 C17 171.0(7) . . . . ? Zn1 O3 C16 C17 -32.6(12) 2 . . . ? O4 C16 C17 C18 98(3) . . . . ? O3 C16 C17 C18 -70(3) . . . . ? C17' C16 C17 C18 172(13) . . . . ? O4 C16 C17 C30 -80(3) . . . . ? O3 C16 C17 C30 112(2) . . . . ? C17' C16 C17 C30 -6(8) . . . . ? C30 C17 C18 C19 -179(2) . . . . ? C16 C17 C18 C19 3(4) . . . . ? C30 C17 C18 C23 -2(4) . . . . ? C16 C17 C18 C23 -180(2) . . . . ? C17 C18 C19 C20 -176(2) . . . . ? C23 C18 C19 C20 7(3) . . . . ? C18 C19 C20 C21 -4(3) . . . . ? C19 C20 C21 C22 0(4) . . . . ? C20 C21 C22 C23 0(6) . . . . ? C21 C22 C23 C24 178(3) . . . . ? C21 C22 C23 C18 3(6) . . . . ? C17 C18 C23 C24 1(3) . . . . ? C19 C18 C23 C24 178.4(19) . . . . ? C17 C18 C23 C22 176(4) . . . . ? C19 C18 C23 C22 -6(4) . . . . ? C22 C23 C24 C25 -175(3) . . . . ? C18 C23 C24 C25 0(3) . . . . ? C23 C24 C25 C26 180(2) . . . . ? C23 C24 C25 C30 -1(4) . . . . ? C24 C25 C26 C27 -176(3) . . . . ? C30 C25 C26 C27 5(4) . . . . ? C25 C26 C27 C28 -6(4) . . . . ? C26 C27 C28 C29 6(4) . . . . ? C27 C28 C29 C30 -5(4) . . . . ? C28 C29 C30 C17 -179(3) . . . . ? C28 C29 C30 C25 4(3) . . . . ? C18 C17 C30 C29 -176(2) . . . . ? C16 C17 C30 C29 2(4) . . . . ? C18 C17 C30 C25 1(4) . . . . ? C16 C17 C30 C25 179(2) . . . . ? C24 C25 C30 C29 177(2) . . . . ? C26 C25 C30 C29 -4(3) . . . . ? C24 C25 C30 C17 0(4) . . . . ? C26 C25 C30 C17 179(3) . . . . ? C42 N1 C31 C32 -1.1(14) . . . . ? Zn1 N1 C31 C32 -177.3(8) . . . . ? N1 C31 C32 C33 0.0(18) . . . . ? C31 C32 C33 C34 -1(2) . . . . ? C32 C33 C34 C35 177.3(12) . . . . ? C32 C33 C34 C42 2.5(18) . . . . ? C33 C34 C35 C36 -177.7(12) . . . . ? C42 C34 C35 C36 -3.1(18) . . . . ? C34 C35 C36 C37 0.8(18) . . . . ? C35 C36 C37 C38 179.2(10) . . . . ? C35 C36 C37 C41 0.6(15) . . . . ? C41 C37 C38 C39 0.3(13) . . . . ? C36 C37 C38 C39 -178.4(9) . . . . ? C37 C38 C39 C40 0.6(14) . . . . ? C41 N2 C40 C39 1.0(13) . . . . ? Zn1 N2 C40 C39 178.7(7) . . . . ? C38 C39 C40 N2 -1.3(15) . . . . ? C40 N2 C41 C37 -0.1(12) . . . . ? Zn1 N2 C41 C37 -178.1(6) . . . . ? C40 N2 C41 C42 177.9(8) . . . . ? Zn1 N2 C41 C42 -0.2(9) . . . . ? C38 C37 C41 N2 -0.6(12) . . . . ? C36 C37 C41 N2 178.1(8) . . . . ? C38 C37 C41 C42 -178.4(8) . . . . ? C36 C37 C41 C42 0.3(13) . . . . ? C31 N1 C42 C34 3.2(13) . . . . ? Zn1 N1 C42 C34 179.9(8) . . . . ? C31 N1 C42 C41 -179.5(8) . . . . ? Zn1 N1 C42 C41 -2.8(10) . . . . ? C33 C34 C42 N1 -3.8(15) . . . . ? C35 C34 C42 N1 -178.8(10) . . . . ? C33 C34 C42 C41 178.9(10) . . . . ? C35 C34 C42 C41 3.9(15) . . . . ? N2 C41 C42 N1 2.1(11) . . . . ? C37 C41 C42 N1 -180.0(8) . . . . ? N2 C41 C42 C34 179.6(8) . . . . ? C37 C41 C42 C34 -2.5(12) . . . . ? O4 C16 C17' C18' 109(3) . . . . ? O3 C16 C17' C18' -74(3) . . . . ? C17 C16 C17' C18' -6(7) . . . . ? O4 C16 C17' C30' -64(3) . . . . ? O3 C16 C17' C30' 112(3) . . . . ? C17 C16 C17' C30' -179(13) . . . . ? C30' C17' C18' C19' 176(2) . . . . ? C16 C17' C18' C19' 3(5) . . . . ? C30' C17' C18' C23' -3(5) . . . . ? C16 C17' C18' C23' -176(2) . . . . ? C17' C18' C19' C20' 180(3) . . . . ? C23' C18' C19' C20' -1(3) . . . . ? C18' C19' C20' C21' -1(4) . . . . ? C19' C20' C21' C22' 0(5) . . . . ? C20' C21' C22' C23' 3(5) . . . . ? C21' C22' C23' C24' 180(3) . . . . ? C21' C22' C23' C18' -5(4) . . . . ? C19' C18' C23' C22' 4(3) . . . . ? C17' C18' C23' C22' -177(3) . . . . ? C19' C18' C23' C24' 179(2) . . . . ? C17' C18' C23' C24' -2(4) . . . . ? C22' C23' C24' C25' -179(2) . . . . ? C18' C23' C24' C25' 6(3) . . . . ? C23' C24' C25' C26' 179(2) . . . . ? C23' C24' C25' C30' -5(3) . . . . ? C24' C25' C26' C27' 179(2) . . . . ? C30' C25' C26' C27' 3(4) . . . . ? C25' C26' C27' C28' -1(4) . . . . ? C26' C27' C28' C29' -2(3) . . . . ? C27' C28' C29' C30' 3(3) . . . . ? C26' C25' C30' C17' 177(3) . . . . ? C24' C25' C30' C17' 1(3) . . . . ? C26' C25' C30' C29' -2(3) . . . . ? C24' C25' C30' C29' -177.9(18) . . . . ? C18' C17' C30' C25' 3(5) . . . . ? C16 C17' C30' C25' 176(2) . . . . ? C18' C17' C30' C29' -178(3) . . . . ? C16 C17' C30' C29' -5(4) . . . . ? C28' C29' C30' C25' -1(3) . . . . ? C28' C29' C30' C17' 180(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.692 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.125 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 623313' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 N2 O6 Zn' _chemical_formula_weight 728.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.168(3) _cell_length_b 11.5740(15) _cell_length_c 12.0378(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.489(2) _cell_angle_gamma 90.00 _cell_volume 3356.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4115 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.8845 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8309 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2956 _reflns_number_gt 2593 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+2.8650P] 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 2956 _refine_ls_number_parameters 237 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.0000 0.73673(3) 0.2500 0.02577(12) Uani 1 2 d S . . C1 C 0.88593(8) 0.74517(15) 0.33627(16) 0.0276(4) Uani 1 1 d . . . C2 C 0.85396(8) 0.78129(17) 0.43389(16) 0.0275(4) Uani 1 1 d . . . C3 C 0.84458(8) 0.89923(18) 0.45107(16) 0.0317(5) Uani 1 1 d . . . C4 C 0.86154(9) 0.98626(19) 0.37745(19) 0.0422(5) Uani 1 1 d . . . H4A H 0.8803 0.9651 0.3160 0.051 Uiso 1 1 calc R . . C5 C 0.85084(11) 1.0994(2) 0.3952(2) 0.0555(7) Uani 1 1 d . . . H5A H 0.8618 1.1547 0.3453 0.067 Uiso 1 1 calc R . . C6 C 0.82328(11) 1.1339(2) 0.4885(3) 0.0630(8) Uani 1 1 d . . . H6A H 0.8164 1.2119 0.5000 0.076 Uiso 1 1 calc R . . C7 C 0.80689(11) 1.0553(2) 0.5611(2) 0.0554(7) Uani 1 1 d . . . H7A H 0.7892 1.0800 0.6227 0.066 Uiso 1 1 calc R . . C8 C 0.81610(9) 0.9347(2) 0.54560(19) 0.0398(5) Uani 1 1 d . . . C9 C 0.79825(9) 0.8517(2) 0.61710(19) 0.0460(6) Uani 1 1 d . . . H9A H 0.7796 0.8751 0.6779 0.055 Uiso 1 1 calc R . . C10 C 0.80714(9) 0.7345(2) 0.60153(18) 0.0394(5) Uani 1 1 d . . . C11 C 0.78934(10) 0.6484(3) 0.6752(2) 0.0560(7) Uani 1 1 d . . . H11A H 0.7708 0.6708 0.7365 0.067 Uiso 1 1 calc R . . C12 C 0.79866(10) 0.5361(3) 0.6585(2) 0.0595(8) Uani 1 1 d . . . H12A H 0.7874 0.4818 0.7090 0.071 Uiso 1 1 calc R . . C13 C 0.82540(10) 0.4994(2) 0.5648(2) 0.0525(7) Uani 1 1 d . . . H13A H 0.8308 0.4209 0.5531 0.063 Uiso 1 1 calc R . . C14 C 0.84347(9) 0.5771(2) 0.4913(2) 0.0406(5) Uani 1 1 d . . . H14A H 0.8612 0.5513 0.4301 0.049 Uiso 1 1 calc R . . C15 C 0.83546(8) 0.69797(18) 0.50691(16) 0.0309(5) Uani 1 1 d . . . C18 C 1.0000 0.1720(2) 0.2500 0.0282(6) Uani 1 2 d S . . C19 C 1.0000 0.3004(2) 0.2500 0.0251(6) Uani 1 2 d S . . C20 C 1.04854(8) 0.36321(17) 0.27116(17) 0.0309(4) Uani 1 1 d . . . H20A H 1.0821 0.3252 0.2875 0.037 Uiso 1 1 calc R . . C21 C 1.04686(8) 0.48209(17) 0.26795(17) 0.0310(4) Uani 1 1 d . . . H21A H 1.0802 0.5223 0.2789 0.037 Uiso 1 1 calc R . . C22 C 1.05262(10) 0.6781(2) 0.48989(18) 0.0457(6) Uani 1 1 d . . . H22A H 1.0855 0.6896 0.5387 0.069 Uiso 1 1 calc R . . H22B H 1.0470 0.5969 0.4772 0.069 Uiso 1 1 calc R . . H22C H 1.0212 0.7097 0.5234 0.069 Uiso 1 1 calc R . . N1 N 1.0000 0.54265(19) 0.2500 0.0271(5) Uani 1 2 d S . . O1 O 0.93790(6) 0.74124(12) 0.35698(12) 0.0338(3) Uani 1 1 d . . . O2 O 0.86013(6) 0.72390(15) 0.24564(12) 0.0458(4) Uani 1 1 d . . . O3 O 1.05877(6) 0.73417(12) 0.38700(11) 0.0312(3) Uani 1 1 d D . . H3A H 1.0882(6) 0.724(2) 0.361(2) 0.049(8) Uiso 1 1 d D . . C17 C 1.02934(9) 0.10938(18) 0.33337(18) 0.0378(5) Uani 1 1 d . . . H17A H 1.0499 0.1474 0.3908 0.045 Uiso 1 1 calc R . . C16 C 1.02769(9) -0.00970(18) 0.33033(18) 0.0378(5) Uani 1 1 d . . . H16A H 1.0471 -0.0500 0.3878 0.045 Uiso 1 1 calc R . . N2 N 1.0000 -0.07039(19) 0.2500 0.0312(5) Uani 1 2 d S . . 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 0.02637(18) 0.02419(18) 0.02730(18) 0.000 0.00565(12) 0.000 C1 0.0306(11) 0.0236(10) 0.0295(11) 0.0011(8) 0.0084(8) 0.0001(8) C2 0.0212(9) 0.0353(11) 0.0262(10) -0.0028(8) 0.0028(8) 0.0033(8) C3 0.0271(10) 0.0360(11) 0.0317(11) -0.0047(9) 0.0001(8) 0.0026(9) C4 0.0455(13) 0.0379(13) 0.0435(13) -0.0049(10) 0.0042(10) -0.0018(10) C5 0.0628(17) 0.0352(13) 0.0673(17) -0.0026(12) -0.0028(13) -0.0055(12) C6 0.0628(17) 0.0367(14) 0.088(2) -0.0231(15) -0.0034(16) 0.0059(13) C7 0.0488(15) 0.0557(16) 0.0619(17) -0.0292(14) 0.0059(13) 0.0094(13) C8 0.0313(11) 0.0491(13) 0.0386(12) -0.0153(10) 0.0009(9) 0.0077(10) C9 0.0350(12) 0.0719(17) 0.0322(12) -0.0114(11) 0.0099(10) 0.0094(12) C10 0.0256(11) 0.0620(15) 0.0311(11) 0.0044(10) 0.0061(9) 0.0030(10) C11 0.0377(13) 0.090(2) 0.0413(14) 0.0171(14) 0.0133(11) -0.0002(13) C12 0.0386(14) 0.077(2) 0.0640(18) 0.0334(15) 0.0094(13) -0.0062(13) C13 0.0380(13) 0.0476(14) 0.0717(18) 0.0226(13) 0.0034(12) 0.0000(11) C14 0.0311(11) 0.0421(13) 0.0491(14) 0.0070(11) 0.0062(10) 0.0041(10) C15 0.0204(10) 0.0420(12) 0.0303(11) 0.0034(9) 0.0024(8) 0.0048(9) C18 0.0302(15) 0.0217(14) 0.0330(15) 0.000 0.0050(12) 0.000 C19 0.0330(15) 0.0222(13) 0.0203(13) 0.000 0.0032(11) 0.000 C20 0.0277(10) 0.0264(10) 0.0382(11) -0.0029(8) -0.0002(8) 0.0038(8) C21 0.0265(10) 0.0273(10) 0.0392(12) -0.0047(9) 0.0024(8) -0.0024(8) C22 0.0479(14) 0.0585(15) 0.0315(12) 0.0063(11) 0.0080(10) 0.0013(12) N1 0.0265(12) 0.0239(12) 0.0311(13) 0.000 0.0042(10) 0.000 O1 0.0266(8) 0.0435(9) 0.0323(8) -0.0005(6) 0.0087(6) 0.0051(6) O2 0.0356(8) 0.0710(11) 0.0312(9) -0.0137(7) 0.0056(7) -0.0033(8) O3 0.0319(8) 0.0350(8) 0.0272(7) 0.0043(6) 0.0051(6) 0.0015(6) C17 0.0471(13) 0.0269(11) 0.0374(12) -0.0048(9) -0.0089(10) 0.0026(10) C16 0.0469(13) 0.0277(11) 0.0375(12) 0.0004(9) -0.0061(10) 0.0074(10) N2 0.0350(13) 0.0239(12) 0.0350(13) 0.000 0.0045(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.0534(13) 2_755 ? Zn1 O1 2.0534(13) . ? Zn1 O3 2.0909(14) 2_755 ? Zn1 O3 2.0909(14) . ? Zn1 N2 2.232(2) 1_565 ? Zn1 N1 2.246(2) . ? C1 O2 1.238(3) . ? C1 O1 1.262(2) . ? C1 C2 1.515(3) . ? C2 C15 1.401(3) . ? C2 C3 1.402(3) . ? C3 C4 1.423(3) . ? C3 C8 1.435(3) . ? C4 C5 1.355(3) . ? C5 C6 1.408(4) . ? C6 C7 1.342(4) . ? C7 C8 1.428(3) . ? C8 C9 1.382(3) . ? C9 C10 1.388(3) . ? C10 C11 1.422(3) . ? C10 C15 1.437(3) . ? C11 C12 1.338(4) . ? C12 C13 1.408(4) . ? C13 C14 1.357(3) . ? C14 C15 1.427(3) . ? C18 C17 1.387(2) 2_755 ? C18 C17 1.387(2) . ? C18 C19 1.486(4) . ? C19 C20 1.387(2) . ? C19 C20 1.387(2) 2_755 ? C20 C21 1.377(3) . ? C21 N1 1.335(2) . ? C22 O3 1.416(2) . ? N1 C21 1.335(2) 2_755 ? C17 C16 1.379(3) . ? C16 N2 1.332(2) . ? N2 C16 1.332(2) 2_755 ? N2 Zn1 2.232(2) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 177.08(8) 2_755 . ? O1 Zn1 O3 89.45(6) 2_755 2_755 ? O1 Zn1 O3 90.59(6) . 2_755 ? O1 Zn1 O3 90.59(6) 2_755 . ? O1 Zn1 O3 89.45(6) . . ? O3 Zn1 O3 178.37(8) 2_755 . ? O1 Zn1 N2 88.54(4) 2_755 1_565 ? O1 Zn1 N2 88.54(4) . 1_565 ? O3 Zn1 N2 90.81(4) 2_755 1_565 ? O3 Zn1 N2 90.81(4) . 1_565 ? O1 Zn1 N1 91.46(4) 2_755 . ? O1 Zn1 N1 91.46(4) . . ? O3 Zn1 N1 89.19(4) 2_755 . ? O3 Zn1 N1 89.19(4) . . ? N2 Zn1 N1 180.000(1) 1_565 . ? O2 C1 O1 126.27(18) . . ? O2 C1 C2 119.08(18) . . ? O1 C1 C2 114.64(17) . . ? C15 C2 C3 120.96(18) . . ? C15 C2 C1 120.25(17) . . ? C3 C2 C1 118.77(17) . . ? C2 C3 C4 122.66(19) . . ? C2 C3 C8 119.3(2) . . ? C4 C3 C8 118.1(2) . . ? C5 C4 C3 121.2(2) . . ? C4 C5 C6 120.5(3) . . ? C7 C6 C5 120.6(2) . . ? C6 C7 C8 121.4(2) . . ? C9 C8 C7 122.7(2) . . ? C9 C8 C3 119.2(2) . . ? C7 C8 C3 118.2(2) . . ? C8 C9 C10 122.5(2) . . ? C9 C10 C11 122.9(2) . . ? C9 C10 C15 118.8(2) . . ? C11 C10 C15 118.3(2) . . ? C12 C11 C10 121.6(2) . . ? C11 C12 C13 120.4(2) . . ? C14 C13 C12 120.9(3) . . ? C13 C14 C15 120.6(2) . . ? C2 C15 C14 122.60(19) . . ? C2 C15 C10 119.33(19) . . ? C14 C15 C10 118.08(19) . . ? C17 C18 C17 117.0(3) 2_755 . ? C17 C18 C19 121.48(13) 2_755 . ? C17 C18 C19 121.48(13) . . ? C20 C19 C20 116.7(2) . 2_755 ? C20 C19 C18 121.63(12) . . ? C20 C19 C18 121.63(12) 2_755 . ? C21 C20 C19 119.75(19) . . ? N1 C21 C20 123.50(19) . . ? C21 N1 C21 116.7(2) 2_755 . ? C21 N1 Zn1 121.67(11) 2_755 . ? C21 N1 Zn1 121.67(11) . . ? C1 O1 Zn1 129.94(13) . . ? C22 O3 Zn1 125.79(13) . . ? C16 C17 C18 119.38(19) . . ? N2 C16 C17 123.9(2) . . ? C16 N2 C16 116.4(2) . 2_755 ? C16 N2 Zn1 121.82(12) . 1_545 ? C16 N2 Zn1 121.82(12) 2_755 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C15 90.6(2) . . . . ? O1 C1 C2 C15 -90.2(2) . . . . ? O2 C1 C2 C3 -91.0(2) . . . . ? O1 C1 C2 C3 88.2(2) . . . . ? C15 C2 C3 C4 -178.48(19) . . . . ? C1 C2 C3 C4 3.1(3) . . . . ? C15 C2 C3 C8 0.6(3) . . . . ? C1 C2 C3 C8 -177.75(17) . . . . ? C2 C3 C4 C5 178.6(2) . . . . ? C8 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C4 C5 C6 C7 -0.4(4) . . . . ? C5 C6 C7 C8 -0.8(4) . . . . ? C6 C7 C8 C9 -178.1(2) . . . . ? C6 C7 C8 C3 1.3(4) . . . . ? C2 C3 C8 C9 -0.4(3) . . . . ? C4 C3 C8 C9 178.7(2) . . . . ? C2 C3 C8 C7 -179.79(19) . . . . ? C4 C3 C8 C7 -0.6(3) . . . . ? C7 C8 C9 C10 179.8(2) . . . . ? C3 C8 C9 C10 0.4(3) . . . . ? C8 C9 C10 C11 179.5(2) . . . . ? C8 C9 C10 C15 -0.6(3) . . . . ? C9 C10 C11 C12 -179.7(2) . . . . ? C15 C10 C11 C12 0.4(4) . . . . ? C10 C11 C12 C13 -1.7(4) . . . . ? C11 C12 C13 C14 1.7(4) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C3 C2 C15 C14 179.03(19) . . . . ? C1 C2 C15 C14 -2.6(3) . . . . ? C3 C2 C15 C10 -0.8(3) . . . . ? C1 C2 C15 C10 177.52(18) . . . . ? C13 C14 C15 C2 179.3(2) . . . . ? C13 C14 C15 C10 -0.8(3) . . . . ? C9 C10 C15 C2 0.8(3) . . . . ? C11 C10 C15 C2 -179.26(19) . . . . ? C9 C10 C15 C14 -179.05(19) . . . . ? C11 C10 C15 C14 0.9(3) . . . . ? C17 C18 C19 C20 -134.64(15) 2_755 . . . ? C17 C18 C19 C20 45.36(15) . . . . ? C17 C18 C19 C20 45.36(15) 2_755 . . 2_755 ? C17 C18 C19 C20 -134.64(15) . . . 2_755 ? C20 C19 C20 C21 -1.42(14) 2_755 . . . ? C18 C19 C20 C21 178.58(14) . . . . ? C19 C20 C21 N1 3.0(3) . . . . ? C20 C21 N1 C21 -1.54(15) . . . 2_755 ? C20 C21 N1 Zn1 178.46(15) . . . . ? O1 Zn1 N1 C21 -130.36(11) 2_755 . . 2_755 ? O1 Zn1 N1 C21 49.64(11) . . . 2_755 ? O3 Zn1 N1 C21 -40.93(11) 2_755 . . 2_755 ? O3 Zn1 N1 C21 139.07(11) . . . 2_755 ? N2 Zn1 N1 C21 101(100) 1_565 . . 2_755 ? O1 Zn1 N1 C21 49.64(11) 2_755 . . . ? O1 Zn1 N1 C21 -130.36(11) . . . . ? O3 Zn1 N1 C21 139.07(11) 2_755 . . . ? O3 Zn1 N1 C21 -40.93(11) . . . . ? N2 Zn1 N1 C21 -79(100) 1_565 . . . ? O2 C1 O1 Zn1 15.7(3) . . . . ? C2 C1 O1 Zn1 -163.48(13) . . . . ? O1 Zn1 O1 C1 88.53(16) 2_755 . . . ? O3 Zn1 O1 C1 -2.27(16) 2_755 . . . ? O3 Zn1 O1 C1 179.35(16) . . . . ? N2 Zn1 O1 C1 88.53(16) 1_565 . . . ? N1 Zn1 O1 C1 -91.47(16) . . . . ? O1 Zn1 O3 C22 -147.74(16) 2_755 . . . ? O1 Zn1 O3 C22 35.17(17) . . . . ? O3 Zn1 O3 C22 -56.29(17) 2_755 . . . ? N2 Zn1 O3 C22 123.71(16) 1_565 . . . ? N1 Zn1 O3 C22 -56.29(16) . . . . ? C17 C18 C17 C16 -0.56(15) 2_755 . . . ? C19 C18 C17 C16 179.44(15) . . . . ? C18 C17 C16 N2 1.2(3) . . . . ? C17 C16 N2 C16 -0.62(16) . . . 2_755 ? C17 C16 N2 Zn1 179.38(16) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.277 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.052 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 623314' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 N2 O10 Zn' _chemical_formula_sum 'C46 H40 N2 O10 Zn' _chemical_formula_weight 846.17 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 16.442(2) _cell_length_b 17.697(3) _cell_length_c 27.528(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8010(2) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 18676 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8125 _exptl_absorpt_correction_T_max 0.9478 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37367 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.90 _reflns_number_total 9534 _reflns_number_gt 7641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0532P)^2^+3.1005P] 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 SHELXL _refine_ls_extinction_coef 0.00031(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9534 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.513871(15) 0.249175(11) 0.384131(8) 0.01461(8) Uani 1 1 d . . . O1 O 0.61604(9) 0.25093(8) 0.34789(5) 0.0227(3) Uani 1 1 d . . . O2 O 0.58926(11) 0.14590(10) 0.30530(7) 0.0412(5) Uani 1 1 d . . . O3 O 0.91503(9) 0.21998(8) 0.15165(5) 0.0215(3) Uani 1 1 d . . . O4 O 0.95249(10) 0.31589(9) 0.19872(6) 0.0327(4) Uani 1 1 d . . . O5 O 0.51520(9) 0.34840(8) 0.41433(5) 0.0214(3) Uani 1 1 d . . . O6 O 0.38590(9) 0.34480(8) 0.43957(5) 0.0263(3) Uani 1 1 d . . . O7 O 0.50873(9) 0.17342(9) 0.43483(6) 0.0281(4) Uani 1 1 d . . . O8 O 0.63531(11) 0.15874(10) 0.46207(7) 0.0515(6) Uani 1 1 d . . . O9 O 0.44662(11) 0.07394(9) 0.32635(6) 0.0317(4) Uani 1 1 d . . . H9A H 0.4988(18) 0.0851(16) 0.3204(11) 0.048 Uiso 1 1 d . . . H9B H 0.4256(18) 0.1172(17) 0.3338(10) 0.048 Uiso 1 1 d . . . O10 O 0.24285(11) 0.41384(9) 0.47466(7) 0.0361(4) Uani 1 1 d . . . H10A H 0.2867(19) 0.3881(17) 0.4665(11) 0.054 Uiso 1 1 d . . . H10B H 0.2184(18) 0.3893(17) 0.4992(10) 0.054 Uiso 1 1 d . . . N1 N 0.62862(12) 0.50402(10) 0.24540(7) 0.0282(4) Uani 1 1 d . . . H1 H 0.6045(17) 0.5354(15) 0.2183(11) 0.050(8) Uiso 1 1 d . . . N2 N 0.25633(10) 0.06254(11) 0.49782(6) 0.0224(4) Uani 1 1 d . . . H2 H 0.2566(16) 0.0101(18) 0.4915(10) 0.049(9) Uiso 1 1 d . . . C1 C 0.62911(13) 0.20348(12) 0.31394(7) 0.0233(4) Uani 1 1 d . . . C2 C 0.70128(13) 0.22083(12) 0.28207(7) 0.0215(4) Uani 1 1 d . . . C3 C 0.77848(13) 0.19826(11) 0.29722(7) 0.0217(4) Uani 1 1 d . . . C4 C 0.79242(14) 0.16391(12) 0.34388(8) 0.0272(5) Uani 1 1 d . . . H4 H 0.7478 0.1546 0.3650 0.033 Uiso 1 1 calc R . . C5 C 0.86853(15) 0.14467(13) 0.35802(8) 0.0320(5) Uani 1 1 d . . . H5 H 0.8768 0.1231 0.3892 0.038 Uiso 1 1 calc R . . C6 C 0.93586(15) 0.15621(13) 0.32693(8) 0.0310(5) Uani 1 1 d . . . H6 H 0.9888 0.1419 0.3373 0.037 Uiso 1 1 calc R . . C7 C 0.92536(14) 0.18770(12) 0.28232(8) 0.0262(5) Uani 1 1 d . . . H7 H 0.9710 0.1942 0.2616 0.031 Uiso 1 1 calc R . . C8 C 0.84707(13) 0.21118(11) 0.26613(7) 0.0211(4) Uani 1 1 d . . . C9 C 0.83470(13) 0.24657(11) 0.22105(7) 0.0193(4) Uani 1 1 d . . . C10 C 0.75778(13) 0.27026(12) 0.20621(7) 0.0207(4) Uani 1 1 d . . . C11 C 0.74471(14) 0.30882(12) 0.16094(7) 0.0258(5) Uani 1 1 d . . . H11 H 0.7890 0.3159 0.1392 0.031 Uiso 1 1 calc R . . C12 C 0.67021(15) 0.33518(14) 0.14880(8) 0.0312(5) Uani 1 1 d . . . H12 H 0.6626 0.3604 0.1187 0.037 Uiso 1 1 calc R . . C13 C 0.60326(15) 0.32547(14) 0.18083(9) 0.0333(5) Uani 1 1 d . . . H13 H 0.5515 0.3453 0.1722 0.040 Uiso 1 1 calc R . . C14 C 0.61237(14) 0.28823(13) 0.22362(8) 0.0280(5) Uani 1 1 d . . . H14 H 0.5668 0.2821 0.2445 0.034 Uiso 1 1 calc R . . C15 C 0.68932(13) 0.25824(11) 0.23770(7) 0.0218(4) Uani 1 1 d . . . C16 C 0.90634(13) 0.26313(12) 0.18899(7) 0.0211(4) Uani 1 1 d . . . C17 C 0.45514(13) 0.37164(11) 0.43938(7) 0.0195(4) Uani 1 1 d . . . C18 C 0.47641(12) 0.43821(11) 0.47122(7) 0.0188(4) Uani 1 1 d . . . C19 C 0.52271(12) 0.42559(11) 0.51311(7) 0.0185(4) Uani 1 1 d . . . C20 C 0.54775(14) 0.35148(11) 0.52757(7) 0.0226(4) Uani 1 1 d . . . H20 H 0.5332 0.3093 0.5081 0.027 Uiso 1 1 calc R . . C21 C 0.59197(14) 0.34025(12) 0.56861(8) 0.0266(5) Uani 1 1 d . . . H21 H 0.6079 0.2905 0.5775 0.032 Uiso 1 1 calc R . . C22 C 0.61447(13) 0.40246(12) 0.59830(8) 0.0243(4) Uani 1 1 d . . . H22 H 0.6446 0.3939 0.6272 0.029 Uiso 1 1 calc R . . C23 C 0.59324(13) 0.47420(11) 0.58568(7) 0.0217(4) Uani 1 1 d . . . H23 H 0.6093 0.5153 0.6057 0.026 Uiso 1 1 calc R . . C24 C 0.54709(12) 0.48844(11) 0.54260(7) 0.0182(4) Uani 1 1 d . . . C25 C 0.56390(14) 0.13908(12) 0.45808(8) 0.0262(5) Uani 1 1 d . . . C26 C 0.53397(13) 0.06655(11) 0.48100(8) 0.0232(4) Uani 1 1 d . . . C27 C 0.49042(13) 0.06957(12) 0.52457(8) 0.0244(5) Uani 1 1 d . . . C28 C 0.47851(15) 0.13879(13) 0.55074(8) 0.0312(5) Uani 1 1 d . . . H28 H 0.5005 0.1844 0.5381 0.037 Uiso 1 1 calc R . . C29 C 0.43671(16) 0.14058(14) 0.59308(9) 0.0376(6) Uani 1 1 d . . . H29 H 0.4290 0.1872 0.6096 0.045 Uiso 1 1 calc R . . C30 C 0.59566(16) -0.07294(15) 0.38711(8) 0.0375(6) Uani 1 1 d . . . H30 H 0.6241 -0.0746 0.3571 0.045 Uiso 1 1 calc R . . C31 C 0.58660(14) -0.00600(14) 0.41049(8) 0.0308(5) Uani 1 1 d . . . H31 H 0.6088 0.0386 0.3966 0.037 Uiso 1 1 calc R . . C32 C 0.54402(13) -0.00145(12) 0.45586(8) 0.0236(4) Uani 1 1 d . . . C33 C 0.48987(15) 0.48332(15) 0.27251(11) 0.0414(6) Uani 1 1 d . . . H33A H 0.4803 0.5372 0.2665 0.062 Uiso 1 1 calc R . . H33B H 0.4622 0.4682 0.3025 0.062 Uiso 1 1 calc R . . H33C H 0.4686 0.4537 0.2453 0.062 Uiso 1 1 calc R . . C34 C 0.57888(15) 0.46950(12) 0.27752(8) 0.0294(5) Uani 1 1 d . . . C35 C 0.61283(16) 0.42235(13) 0.31170(8) 0.0321(5) Uani 1 1 d . . . H35 H 0.5794 0.3977 0.3350 0.038 Uiso 1 1 calc R . . C36 C 0.69614(16) 0.41123(13) 0.31185(8) 0.0341(6) Uani 1 1 d . . . H36 H 0.7200 0.3782 0.3350 0.041 Uiso 1 1 calc R . . C37 C 0.74483(16) 0.44800(14) 0.27840(8) 0.0368(6) Uani 1 1 d . . . H37 H 0.8020 0.4404 0.2785 0.044 Uiso 1 1 calc R . . C38 C 0.70969(15) 0.49564(13) 0.24490(8) 0.0321(5) Uani 1 1 d . . . C39 C 0.75663(16) 0.53850(17) 0.20728(9) 0.0444(7) Uani 1 1 d . . . H39A H 0.7609 0.5080 0.1777 0.067 Uiso 1 1 calc R . . H39B H 0.8113 0.5495 0.2196 0.067 Uiso 1 1 calc R . . H39C H 0.7285 0.5860 0.1999 0.067 Uiso 1 1 calc R . . C40 C 0.33599(15) 0.07580(15) 0.42433(8) 0.0370(6) Uani 1 1 d . . . H40A H 0.3271 0.0210 0.4242 0.055 Uiso 1 1 calc R . . H40B H 0.3945 0.0863 0.4245 0.055 Uiso 1 1 calc R . . H40C H 0.3114 0.0981 0.3952 0.055 Uiso 1 1 calc R . . C41 C 0.29788(13) 0.10923(12) 0.46841(8) 0.0255(5) Uani 1 1 d . . . C42 C 0.30149(15) 0.18506(13) 0.48044(9) 0.0326(5) Uani 1 1 d . . . H42 H 0.3305 0.2196 0.4605 0.039 Uiso 1 1 calc R . . C43 C 0.26236(15) 0.20994(13) 0.52183(9) 0.0354(6) Uani 1 1 d . . . H43 H 0.2655 0.2618 0.5306 0.042 Uiso 1 1 calc R . . C44 C 0.21885(15) 0.16083(13) 0.55063(8) 0.0315(5) Uani 1 1 d . . . H44 H 0.1906 0.1787 0.5785 0.038 Uiso 1 1 calc R . . C45 C 0.21701(13) 0.08524(12) 0.53840(8) 0.0253(5) Uani 1 1 d . . . C46 C 0.17550(15) 0.02527(14) 0.56731(8) 0.0328(5) Uani 1 1 d . . . H46A H 0.1539 -0.0134 0.5453 0.049 Uiso 1 1 calc R . . H46B H 0.1308 0.0477 0.5859 0.049 Uiso 1 1 calc R . . H46C H 0.2146 0.0021 0.5897 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01507(14) 0.01659(13) 0.01217(12) 0.00023(8) -0.00002(8) -0.00016(9) O1 0.0192(8) 0.0319(8) 0.0171(7) -0.0002(6) 0.0037(6) 0.0020(6) O2 0.0338(10) 0.0410(10) 0.0489(11) -0.0133(8) 0.0182(8) -0.0143(8) O3 0.0212(8) 0.0258(7) 0.0176(7) 0.0006(6) 0.0034(6) 0.0017(6) O4 0.0310(9) 0.0377(9) 0.0295(8) -0.0051(7) 0.0068(7) -0.0110(8) O5 0.0215(8) 0.0210(7) 0.0218(7) -0.0068(6) 0.0034(6) -0.0015(6) O6 0.0209(8) 0.0251(7) 0.0328(8) -0.0081(6) 0.0039(6) -0.0062(6) O7 0.0259(9) 0.0291(8) 0.0293(8) 0.0147(6) -0.0024(7) -0.0011(7) O8 0.0364(11) 0.0466(11) 0.0716(14) 0.0356(10) -0.0275(10) -0.0223(9) O9 0.0289(9) 0.0320(9) 0.0343(9) -0.0101(7) 0.0031(7) -0.0040(8) O10 0.0342(10) 0.0272(9) 0.0470(11) 0.0025(7) 0.0138(8) 0.0021(7) N1 0.0308(11) 0.0298(10) 0.0240(9) 0.0056(8) 0.0028(8) 0.0027(8) N2 0.0184(9) 0.0244(9) 0.0245(9) 0.0032(7) -0.0015(7) -0.0002(7) C1 0.0198(11) 0.0280(11) 0.0221(10) 0.0020(8) 0.0031(8) 0.0015(9) C2 0.0208(11) 0.0246(10) 0.0192(9) -0.0029(8) 0.0044(8) -0.0008(9) C3 0.0215(11) 0.0244(10) 0.0193(9) -0.0012(8) 0.0030(8) -0.0001(9) C4 0.0285(13) 0.0323(11) 0.0207(10) 0.0039(9) 0.0029(9) -0.0038(10) C5 0.0360(14) 0.0360(13) 0.0240(11) 0.0082(9) -0.0027(10) -0.0005(11) C6 0.0248(12) 0.0372(12) 0.0309(12) 0.0058(10) -0.0045(10) 0.0021(10) C7 0.0210(11) 0.0320(11) 0.0257(11) 0.0017(9) 0.0018(9) -0.0002(9) C8 0.0197(11) 0.0238(10) 0.0198(9) -0.0011(8) 0.0024(8) -0.0013(9) C9 0.0165(10) 0.0232(10) 0.0182(9) -0.0029(7) 0.0029(8) -0.0005(8) C10 0.0180(11) 0.0258(10) 0.0184(9) -0.0014(8) 0.0018(8) -0.0005(9) C11 0.0247(12) 0.0334(11) 0.0192(10) 0.0009(8) 0.0026(8) 0.0004(10) C12 0.0298(13) 0.0395(13) 0.0242(11) 0.0046(9) -0.0030(10) 0.0022(11) C13 0.0216(12) 0.0437(14) 0.0346(13) 0.0025(10) -0.0022(10) 0.0069(10) C14 0.0195(12) 0.0369(12) 0.0275(11) 0.0003(9) 0.0025(9) -0.0007(10) C15 0.0175(11) 0.0273(11) 0.0204(10) -0.0031(8) 0.0020(8) -0.0005(8) C16 0.0168(11) 0.0286(11) 0.0179(9) 0.0034(8) 0.0008(8) 0.0011(9) C17 0.0241(11) 0.0165(9) 0.0180(9) 0.0000(7) -0.0011(8) 0.0000(8) C18 0.0192(11) 0.0189(9) 0.0182(9) -0.0025(7) 0.0033(8) -0.0028(8) C19 0.0200(11) 0.0174(9) 0.0181(9) 0.0004(7) 0.0012(8) -0.0015(8) C20 0.0274(12) 0.0174(9) 0.0231(10) -0.0014(8) 0.0020(9) -0.0022(9) C21 0.0308(13) 0.0210(10) 0.0279(11) 0.0060(8) -0.0001(9) 0.0009(9) C22 0.0255(12) 0.0289(11) 0.0185(9) 0.0034(8) -0.0012(8) -0.0013(9) C23 0.0221(11) 0.0248(10) 0.0182(9) -0.0017(8) 0.0004(8) -0.0023(9) C24 0.0186(10) 0.0197(9) 0.0162(9) -0.0014(7) 0.0028(8) -0.0011(8) C25 0.0276(13) 0.0242(10) 0.0269(11) 0.0078(8) -0.0078(9) -0.0060(9) C26 0.0209(11) 0.0237(10) 0.0252(10) 0.0088(8) -0.0074(9) -0.0039(9) C27 0.0234(12) 0.0245(10) 0.0251(11) 0.0052(8) -0.0098(9) -0.0013(9) C28 0.0360(14) 0.0254(11) 0.0322(12) 0.0032(9) -0.0111(10) -0.0011(10) C29 0.0431(16) 0.0375(13) 0.0321(13) -0.0056(10) -0.0109(11) 0.0099(12) C30 0.0359(15) 0.0523(16) 0.0244(12) 0.0020(10) 0.0001(10) 0.0087(12) C31 0.0255(12) 0.0389(13) 0.0280(12) 0.0093(10) -0.0045(9) -0.0031(10) C32 0.0205(11) 0.0258(10) 0.0244(10) 0.0066(8) -0.0064(9) 0.0000(9) C33 0.0321(14) 0.0379(14) 0.0541(17) 0.0117(12) 0.0079(12) -0.0024(11) C34 0.0332(13) 0.0267(11) 0.0283(11) 0.0019(9) 0.0062(10) -0.0024(10) C35 0.0392(15) 0.0316(12) 0.0254(11) 0.0045(9) 0.0022(10) -0.0064(11) C36 0.0415(15) 0.0365(13) 0.0245(11) 0.0062(9) -0.0069(10) -0.0004(11) C37 0.0302(14) 0.0499(15) 0.0304(12) 0.0088(11) -0.0017(10) 0.0018(12) C38 0.0293(13) 0.0404(13) 0.0265(11) 0.0062(10) 0.0032(10) 0.0034(11) C39 0.0343(15) 0.0611(18) 0.0377(14) 0.0201(13) 0.0094(12) 0.0031(13) C40 0.0304(14) 0.0513(15) 0.0292(12) 0.0001(11) 0.0044(10) -0.0079(12) C41 0.0179(11) 0.0327(11) 0.0259(11) 0.0065(9) -0.0029(9) -0.0030(9) C42 0.0268(13) 0.0289(11) 0.0421(13) 0.0104(10) -0.0063(10) -0.0050(10) C43 0.0323(14) 0.0276(12) 0.0462(14) -0.0041(10) -0.0097(11) 0.0034(10) C44 0.0277(13) 0.0364(12) 0.0303(12) -0.0049(10) -0.0038(10) 0.0074(10) C45 0.0199(11) 0.0336(11) 0.0224(10) 0.0020(9) -0.0031(8) 0.0023(9) C46 0.0285(13) 0.0424(13) 0.0274(11) 0.0084(10) 0.0010(10) -0.0016(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 1.9371(14) . ? Zn1 O5 1.9430(14) . ? Zn1 O1 1.9540(15) . ? Zn1 O3 1.9693(14) 8_556 ? O1 C1 1.275(2) . ? O2 C1 1.235(3) . ? O3 C16 1.288(2) . ? O3 Zn1 1.9692(14) 8_656 ? O4 C16 1.233(3) . ? O5 C17 1.273(2) . ? O6 C17 1.234(3) . ? O7 C25 1.266(3) . ? O8 C25 1.229(3) . ? O9 H9A 0.90(3) . ? O9 H9B 0.86(3) . ? O10 H10A 0.88(3) . ? O10 H10B 0.90(3) . ? N1 C38 1.341(3) . ? N1 C34 1.351(3) . ? N1 H1 1.01(3) . ? N2 C41 1.344(3) . ? N2 C45 1.352(3) . ? N2 H2 0.94(3) . ? C1 C2 1.507(3) . ? C2 C3 1.395(3) . ? C2 C15 1.403(3) . ? C3 C8 1.434(3) . ? C3 C4 1.439(3) . ? C4 C5 1.354(3) . ? C4 H4 0.9500 . ? C5 C6 1.414(3) . ? C5 H5 0.9500 . ? C6 C7 1.359(3) . ? C6 H6 0.9500 . ? C7 C8 1.424(3) . ? C7 H7 0.9500 . ? C8 C9 1.405(3) . ? C9 C10 1.394(3) . ? C9 C16 1.501(3) . ? C10 C15 1.436(3) . ? C10 C11 1.437(3) . ? C11 C12 1.353(3) . ? C11 H11 0.9500 . ? C12 C13 1.421(3) . ? C12 H12 0.9500 . ? C13 C14 1.358(3) . ? C13 H13 0.9500 . ? C14 C15 1.426(3) . ? C14 H14 0.9500 . ? C17 C18 1.509(3) . ? C18 C19 1.400(3) . ? C18 C24 1.407(3) 5_666 ? C19 C20 1.431(3) . ? C19 C24 1.434(3) . ? C20 C21 1.358(3) . ? C20 H20 0.9500 . ? C21 C22 1.420(3) . ? C21 H21 0.9500 . ? C22 C23 1.362(3) . ? C22 H22 0.9500 . ? C23 C24 1.430(3) . ? C23 H23 0.9500 . ? C24 C18 1.407(3) 5_666 ? C25 C26 1.513(3) . ? C26 C27 1.398(3) . ? C26 C32 1.398(3) . ? C27 C28 1.434(3) . ? C27 C32 1.437(3) 5_656 ? C28 C29 1.354(3) . ? C28 H28 0.9500 . ? C29 C30 1.419(4) 5_656 ? C29 H29 0.9500 . ? C30 C31 1.356(3) . ? C30 C29 1.419(4) 5_656 ? C30 H30 0.9500 . ? C31 C32 1.434(3) . ? C31 H31 0.9500 . ? C32 C27 1.437(3) 5_656 ? C33 C34 1.490(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.376(3) . ? C35 C36 1.384(3) . ? C35 H35 0.9500 . ? C36 C37 1.383(3) . ? C36 H36 0.9500 . ? C37 C38 1.377(3) . ? C37 H37 0.9500 . ? C38 C39 1.498(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.488(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.384(3) . ? C42 C43 1.380(4) . ? C42 H42 0.9500 . ? C43 C44 1.377(3) . ? C43 H43 0.9500 . ? C44 C45 1.380(3) . ? C44 H44 0.9500 . ? C45 C46 1.492(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 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 O7 Zn1 O5 108.52(6) . . ? O7 Zn1 O1 114.61(6) . . ? O5 Zn1 O1 101.21(6) . . ? O7 Zn1 O3 98.21(6) . 8_556 ? O5 Zn1 O3 117.41(6) . 8_556 ? O1 Zn1 O3 117.27(6) . 8_556 ? C1 O1 Zn1 120.59(14) . . ? C16 O3 Zn1 109.58(13) . 8_656 ? C17 O5 Zn1 121.01(13) . . ? C25 O7 Zn1 131.70(15) . . ? H9A O9 H9B 103(3) . . ? H10A O10 H10B 108(3) . . ? C38 N1 C34 124.0(2) . . ? C38 N1 H1 116.3(16) . . ? C34 N1 H1 119.6(16) . . ? C41 N2 C45 123.9(2) . . ? C41 N2 H2 119.4(17) . . ? C45 N2 H2 116.5(17) . . ? O2 C1 O1 126.5(2) . . ? O2 C1 C2 118.29(18) . . ? O1 C1 C2 115.17(18) . . ? C3 C2 C15 121.53(19) . . ? C3 C2 C1 118.97(18) . . ? C15 C2 C1 119.50(19) . . ? C2 C3 C8 119.45(18) . . ? C2 C3 C4 122.18(19) . . ? C8 C3 C4 118.34(19) . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 120.4(2) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 121.1(2) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 122.50(19) . . ? C9 C8 C3 118.98(19) . . ? C7 C8 C3 118.52(18) . . ? C10 C9 C8 121.62(19) . . ? C10 C9 C16 118.76(18) . . ? C8 C9 C16 119.54(19) . . ? C9 C10 C15 119.33(19) . . ? C9 C10 C11 122.19(19) . . ? C15 C10 C11 118.45(19) . . ? C12 C11 C10 120.9(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.9(2) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C2 C15 C14 122.4(2) . . ? C2 C15 C10 119.03(19) . . ? C14 C15 C10 118.45(19) . . ? O4 C16 O3 123.64(19) . . ? O4 C16 C9 120.22(18) . . ? O3 C16 C9 116.13(18) . . ? O6 C17 O5 126.43(18) . . ? O6 C17 C18 120.80(18) . . ? O5 C17 C18 112.77(18) . . ? C19 C18 C24 121.28(18) . 5_666 ? C19 C18 C17 118.68(17) . . ? C24 C18 C17 119.98(18) 5_666 . ? C18 C19 C20 122.13(18) . . ? C18 C19 C24 119.65(18) . . ? C20 C19 C24 118.22(18) . . ? C21 C20 C19 121.29(19) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.32(19) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.6(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.79(19) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C18 C24 C23 122.16(18) 5_666 . ? C18 C24 C19 119.08(18) 5_666 . ? C23 C24 C19 118.75(18) . . ? O8 C25 O7 126.4(2) . . ? O8 C25 C26 120.90(19) . . ? O7 C25 C26 112.65(19) . . ? C27 C26 C32 121.21(19) . . ? C27 C26 C25 119.5(2) . . ? C32 C26 C25 119.0(2) . . ? C26 C27 C28 122.2(2) . . ? C26 C27 C32 119.4(2) . 5_656 ? C28 C27 C32 118.3(2) . 5_656 ? C29 C28 C27 121.4(2) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 120.1(2) . 5_656 ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 5_656 . ? C31 C30 C29 120.9(2) . 5_656 ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 5_656 . ? C30 C31 C32 121.1(2) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C26 C32 C31 122.5(2) . . ? C26 C32 C27 119.3(2) . 5_656 ? C31 C32 C27 118.2(2) . 5_656 ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N1 C34 C35 118.5(2) . . ? N1 C34 C33 117.4(2) . . ? C35 C34 C33 124.1(2) . . ? C34 C35 C36 119.3(2) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 119.4(2) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? N1 C38 C37 118.5(2) . . ? N1 C38 C39 117.6(2) . . ? C37 C38 C39 123.8(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N2 C41 C42 118.3(2) . . ? N2 C41 C40 117.4(2) . . ? C42 C41 C40 124.3(2) . . ? C43 C42 C41 119.1(2) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C42 121.1(2) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 118.9(2) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? N2 C45 C44 118.7(2) . . ? N2 C45 C46 116.6(2) . . ? C44 C45 C46 124.7(2) . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Zn1 O1 C1 80.27(16) . . . . ? O5 Zn1 O1 C1 -163.17(15) . . . . ? O3 Zn1 O1 C1 -34.11(17) 8_556 . . . ? O7 Zn1 O5 C17 -63.37(16) . . . . ? O1 Zn1 O5 C17 175.69(14) . . . . ? O3 Zn1 O5 C17 46.71(16) 8_556 . . . ? O5 Zn1 O7 C25 -89.9(2) . . . . ? O1 Zn1 O7 C25 22.4(2) . . . . ? O3 Zn1 O7 C25 147.5(2) 8_556 . . . ? Zn1 O1 C1 O2 -12.9(3) . . . . ? Zn1 O1 C1 C2 167.55(13) . . . . ? O2 C1 C2 C3 -95.6(3) . . . . ? O1 C1 C2 C3 84.0(2) . . . . ? O2 C1 C2 C15 83.6(3) . . . . ? O1 C1 C2 C15 -96.9(2) . . . . ? C15 C2 C3 C8 -2.1(3) . . . . ? C1 C2 C3 C8 176.98(18) . . . . ? C15 C2 C3 C4 176.21(19) . . . . ? C1 C2 C3 C4 -4.7(3) . . . . ? C2 C3 C4 C5 -178.1(2) . . . . ? C8 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 -1.5(3) . . . . ? C4 C5 C6 C7 0.7(4) . . . . ? C5 C6 C7 C8 1.3(3) . . . . ? C6 C7 C8 C9 177.4(2) . . . . ? C6 C7 C8 C3 -2.4(3) . . . . ? C2 C3 C8 C9 0.2(3) . . . . ? C4 C3 C8 C9 -178.25(18) . . . . ? C2 C3 C8 C7 179.99(19) . . . . ? C4 C3 C8 C7 1.6(3) . . . . ? C7 C8 C9 C10 -178.92(19) . . . . ? C3 C8 C9 C10 0.9(3) . . . . ? C7 C8 C9 C16 -2.2(3) . . . . ? C3 C8 C9 C16 177.65(17) . . . . ? C8 C9 C10 C15 0.0(3) . . . . ? C16 C9 C10 C15 -176.81(18) . . . . ? C8 C9 C10 C11 177.84(19) . . . . ? C16 C9 C10 C11 1.1(3) . . . . ? C9 C10 C11 C12 -176.0(2) . . . . ? C15 C10 C11 C12 1.9(3) . . . . ? C10 C11 C12 C13 0.3(4) . . . . ? C11 C12 C13 C14 -1.4(4) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? C3 C2 C15 C14 -173.8(2) . . . . ? C1 C2 C15 C14 7.1(3) . . . . ? C3 C2 C15 C10 3.0(3) . . . . ? C1 C2 C15 C10 -176.12(18) . . . . ? C13 C14 C15 C2 178.7(2) . . . . ? C13 C14 C15 C10 1.8(3) . . . . ? C9 C10 C15 C2 -1.9(3) . . . . ? C11 C10 C15 C2 -179.84(19) . . . . ? C9 C10 C15 C14 175.05(19) . . . . ? C11 C10 C15 C14 -2.9(3) . . . . ? Zn1 O3 C16 O4 2.4(3) 8_656 . . . ? Zn1 O3 C16 C9 -178.27(14) 8_656 . . . ? C10 C9 C16 O4 101.6(2) . . . . ? C8 C9 C16 O4 -75.2(3) . . . . ? C10 C9 C16 O3 -77.8(2) . . . . ? C8 C9 C16 O3 105.4(2) . . . . ? Zn1 O5 C17 O6 -16.1(3) . . . . ? Zn1 O5 C17 C18 163.32(12) . . . . ? O6 C17 C18 C19 104.7(2) . . . . ? O5 C17 C18 C19 -74.7(2) . . . . ? O6 C17 C18 C24 -78.1(3) . . . 5_666 ? O5 C17 C18 C24 102.4(2) . . . 5_666 ? C24 C18 C19 C20 -179.51(19) 5_666 . . . ? C17 C18 C19 C20 -2.4(3) . . . . ? C24 C18 C19 C24 -0.2(3) 5_666 . . . ? C17 C18 C19 C24 176.90(18) . . . . ? C18 C19 C20 C21 -179.3(2) . . . . ? C24 C19 C20 C21 1.4(3) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C20 C21 C22 C23 -1.1(3) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C18 179.4(2) . . . 5_666 ? C22 C23 C24 C19 0.7(3) . . . . ? C18 C19 C24 C18 0.2(3) . . . 5_666 ? C20 C19 C24 C18 179.53(19) . . . 5_666 ? C18 C19 C24 C23 178.98(18) . . . . ? C20 C19 C24 C23 -1.7(3) . . . . ? Zn1 O7 C25 O8 18.9(4) . . . . ? Zn1 O7 C25 C26 -159.62(15) . . . . ? O8 C25 C26 C27 101.5(3) . . . . ? O7 C25 C26 C27 -79.9(3) . . . . ? O8 C25 C26 C32 -84.3(3) . . . . ? O7 C25 C26 C32 94.3(3) . . . . ? C32 C26 C27 C28 -179.3(2) . . . . ? C25 C26 C27 C28 -5.2(3) . . . . ? C32 C26 C27 C32 0.6(3) . . . 5_656 ? C25 C26 C27 C32 174.65(19) . . . 5_656 ? C26 C27 C28 C29 -179.5(2) . . . . ? C32 C27 C28 C29 0.6(3) 5_656 . . . ? C27 C28 C29 C30 0.8(4) . . . 5_656 ? C29 C30 C31 C32 -0.1(4) 5_656 . . . ? C27 C26 C32 C31 178.4(2) . . . . ? C25 C26 C32 C31 4.3(3) . . . . ? C27 C26 C32 C27 -0.6(3) . . . 5_656 ? C25 C26 C32 C27 -174.68(19) . . . 5_656 ? C30 C31 C32 C26 179.7(2) . . . . ? C30 C31 C32 C27 -1.3(3) . . . 5_656 ? C38 N1 C34 C35 -0.5(3) . . . . ? C38 N1 C34 C33 -178.6(2) . . . . ? N1 C34 C35 C36 -0.6(3) . . . . ? C33 C34 C35 C36 177.4(2) . . . . ? C34 C35 C36 C37 0.9(4) . . . . ? C35 C36 C37 C38 -0.1(4) . . . . ? C34 N1 C38 C37 1.3(4) . . . . ? C34 N1 C38 C39 -179.3(2) . . . . ? C36 C37 C38 N1 -0.9(4) . . . . ? C36 C37 C38 C39 179.7(2) . . . . ? C45 N2 C41 C42 0.6(3) . . . . ? C45 N2 C41 C40 -178.3(2) . . . . ? N2 C41 C42 C43 -0.2(3) . . . . ? C40 C41 C42 C43 178.7(2) . . . . ? C41 C42 C43 C44 -1.2(4) . . . . ? C42 C43 C44 C45 2.1(4) . . . . ? C41 N2 C45 C44 0.3(3) . . . . ? C41 N2 C45 C46 -178.7(2) . . . . ? C43 C44 C45 N2 -1.7(3) . . . . ? C43 C44 C45 C46 177.2(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O2 0.90(3) 1.88(3) 2.731(2) 157(3) . O9 H9B O3 0.86(3) 1.87(3) 2.705(2) 162(3) 8_556 O10 H10A O6 0.88(3) 1.95(3) 2.821(2) 170(3) . O10 H10B O8 0.90(3) 1.93(3) 2.795(2) 161(3) 6_566 N1 H1 O9 1.01(3) 1.64(3) 2.639(2) 170(3) 7_666 N2 H2 O10 0.94(3) 1.77(3) 2.708(3) 175(3) 2_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.509 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.066 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 623315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H29 N4 O6 Zn' _chemical_formula_weight 775.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6712(2) _cell_length_b 26.8053(4) _cell_length_c 13.5499(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.7680(10) _cell_angle_gamma 90.00 _cell_volume 3508.57(10) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8415 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8569 _exptl_absorpt_correction_T_max 0.9212 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27997 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6173 _reflns_number_gt 5067 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.1740P] 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 6173 _refine_ls_number_parameters 500 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.53235(2) 0.489481(9) 0.828072(17) 0.03002(9) Uani 1 1 d . . . C1 C 0.4071(3) 0.53187(10) 0.62270(18) 0.0485(6) Uani 1 1 d . . . H1A H 0.4469 0.5620 0.6427 0.058 Uiso 1 1 calc R . . C2 C 0.3312(3) 0.53005(12) 0.5338(2) 0.0618(7) Uani 1 1 d . . . H2A H 0.3183 0.5585 0.4952 0.074 Uiso 1 1 calc R . . C3 C 0.2753(3) 0.48533(12) 0.5037(2) 0.0643(8) Uani 1 1 d . . . H3A H 0.2239 0.4831 0.4440 0.077 Uiso 1 1 calc R . . C4 C 0.2954(3) 0.44356(10) 0.56183(17) 0.0506(6) Uani 1 1 d . . . H4A H 0.2596 0.4128 0.5416 0.061 Uiso 1 1 calc R . . C5 C 0.3702(2) 0.44834(8) 0.65138(15) 0.0341(5) Uani 1 1 d . . . C6 C 0.3917(2) 0.40599(8) 0.72144(15) 0.0323(5) Uani 1 1 d . . . C7 C 0.3262(2) 0.36008(9) 0.70827(18) 0.0445(6) Uani 1 1 d . . . H7A H 0.2674 0.3544 0.6531 0.053 Uiso 1 1 calc R . . C8 C 0.3494(2) 0.32338(9) 0.7776(2) 0.0480(6) Uani 1 1 d . . . H8A H 0.3049 0.2927 0.7704 0.058 Uiso 1 1 calc R . . C9 C 0.4383(2) 0.33200(8) 0.85753(18) 0.0409(5) Uani 1 1 d . . . H9A H 0.4564 0.3074 0.9047 0.049 Uiso 1 1 calc R . . C10 C 0.4996(2) 0.37777(8) 0.86605(16) 0.0355(5) Uani 1 1 d . . . H10A H 0.5605 0.3837 0.9201 0.043 Uiso 1 1 calc R . . C11 C 0.8051(3) 0.44235(9) 0.74393(18) 0.0476(6) Uani 1 1 d . . . H11A H 0.7554 0.4126 0.7409 0.057 Uiso 1 1 calc R . . C12 C 0.9431(3) 0.44108(11) 0.7251(2) 0.0582(7) Uani 1 1 d . . . H12A H 0.9859 0.4113 0.7090 0.070 Uiso 1 1 calc R . . C13 C 1.0165(3) 0.48482(12) 0.7305(2) 0.0622(8) Uani 1 1 d . . . H13A H 1.1106 0.4850 0.7195 0.075 Uiso 1 1 calc R . . C14 C 0.9496(2) 0.52862(11) 0.75243(18) 0.0507(6) Uani 1 1 d . . . H14A H 0.9977 0.5587 0.7555 0.061 Uiso 1 1 calc R . . C15 C 0.8097(2) 0.52714(9) 0.76974(15) 0.0346(5) Uani 1 1 d . . . C16 C 0.7295(2) 0.57213(8) 0.79691(15) 0.0342(5) Uani 1 1 d . . . C17 C 0.7796(3) 0.62002(9) 0.7889(2) 0.0553(7) Uani 1 1 d . . . H17A H 0.8649 0.6257 0.7622 0.066 Uiso 1 1 calc R . . C18 C 0.7016(3) 0.65965(10) 0.8210(2) 0.0602(7) Uani 1 1 d . . . H18A H 0.7347 0.6921 0.8167 0.072 Uiso 1 1 calc R . . C19 C 0.5753(3) 0.65067(9) 0.85930(19) 0.0455(6) Uani 1 1 d . . . H19A H 0.5222 0.6766 0.8829 0.055 Uiso 1 1 calc R . . C20 C 0.5297(2) 0.60223(8) 0.86177(17) 0.0398(5) Uani 1 1 d . . . H20A H 0.4429 0.5961 0.8858 0.048 Uiso 1 1 calc R . . C21 C 0.29589(19) 0.51226(7) 0.96358(14) 0.0251(4) Uani 1 1 d . . . C22 C 0.1424(2) 0.50547(7) 0.98198(14) 0.0262(4) Uani 1 1 d . . . C23 C 0.08177(19) 0.45784(7) 0.97896(14) 0.0264(4) Uani 1 1 d . . . C24 C 0.1589(2) 0.41378(8) 0.95849(16) 0.0349(5) Uani 1 1 d . . . H24A H 0.2516 0.4167 0.9441 0.042 Uiso 1 1 calc R . . C25 C 0.0622(2) 0.54786(7) 1.00151(14) 0.0263(4) Uani 1 1 d . . . C26 C 0.1182(2) 0.59722(8) 0.99967(15) 0.0310(5) Uani 1 1 d . . . H26A H 0.2106 0.6015 0.9855 0.037 Uiso 1 1 calc R . . C27 C 0.0409(2) 0.63784(8) 1.01789(16) 0.0358(5) Uani 1 1 d . . . H27A H 0.0799 0.6695 1.0157 0.043 Uiso 1 1 calc R . . C28 C -0.1000(2) 0.63208(8) 1.04036(17) 0.0392(5) Uani 1 1 d . . . H28A H -0.1525 0.6600 1.0544 0.047 Uiso 1 1 calc R . . C29 C 1.1448(2) 0.27081(8) 0.50314(15) 0.0316(5) Uani 1 1 d . . . C30 C 0.99366(19) 0.28670(7) 0.50174(14) 0.0272(4) Uani 1 1 d . . . C31 C 0.92515(19) 0.28937(7) 0.59053(14) 0.0275(4) Uani 1 1 d . . . C32 C 0.9949(2) 0.27953(8) 0.68383(15) 0.0344(5) Uani 1 1 d . . . H32A H 1.0881 0.2709 0.6860 0.041 Uiso 1 1 calc R . . C33 C 0.9283(2) 0.28254(9) 0.76922(16) 0.0403(5) Uani 1 1 d . . . H33A H 0.9759 0.2761 0.8291 0.048 Uiso 1 1 calc R . . C34 C 0.7862(2) 0.29551(8) 0.76756(17) 0.0414(6) Uani 1 1 d . . . H34A H 0.7413 0.2979 0.8266 0.050 Uiso 1 1 calc R . . C35 C 0.7154(2) 0.30445(8) 0.68097(16) 0.0377(5) Uani 1 1 d . . . H35A H 0.6219 0.3125 0.6814 0.045 Uiso 1 1 calc R . . C36 C 0.7810(2) 0.30172(7) 0.58872(15) 0.0301(5) Uani 1 1 d . . . C37 C 0.7100(2) 0.31103(8) 0.49783(16) 0.0317(5) Uani 1 1 d . . . C38 C 0.5529(2) 0.32216(8) 0.49477(16) 0.0354(5) Uani 1 1 d . . . C39 C 0.7790(2) 0.30968(8) 0.40899(15) 0.0306(5) Uani 1 1 d . . . C40 C 0.7109(2) 0.31953(9) 0.31501(17) 0.0402(5) Uani 1 1 d . . . H40A H 0.6175 0.3279 0.3120 0.048 Uiso 1 1 calc R . . C41 C 0.7791(2) 0.31694(9) 0.23039(17) 0.0431(6) Uani 1 1 d . . . H41A H 0.7324 0.3237 0.1703 0.052 Uiso 1 1 calc R . . C42 C 0.9209(2) 0.30402(9) 0.23259(16) 0.0411(5) Uani 1 1 d . . . H42A H 0.9665 0.3018 0.1739 0.049 Uiso 1 1 calc R . . C43 C 0.9905(2) 0.29490(8) 0.31994(15) 0.0344(5) Uani 1 1 d . . . H43A H 1.0840 0.2867 0.3203 0.041 Uiso 1 1 calc R . . C44 C 0.9236(2) 0.29752(7) 0.41133(15) 0.0289(4) Uani 1 1 d . . . N1 N 0.47677(17) 0.41445(6) 0.80088(12) 0.0310(4) Uani 1 1 d . . . N2 N 0.42583(18) 0.49195(7) 0.68117(13) 0.0349(4) Uani 1 1 d . . . N3 N 0.60335(17) 0.56343(6) 0.83144(12) 0.0323(4) Uani 1 1 d . . . N4 N 0.73839(18) 0.48433(7) 0.76652(13) 0.0349(4) Uani 1 1 d . . . O1 O 0.33313(14) 0.50173(6) 0.87884(11) 0.0353(3) Uani 1 1 d . . . O2 O 0.37366(13) 0.52972(5) 1.03178(10) 0.0331(3) Uani 1 1 d . . . O3 O 1.23039(15) 0.30600(6) 0.49902(14) 0.0533(5) Uani 1 1 d . . . O4 O 1.17131(16) 0.22593(6) 0.50735(12) 0.0474(4) Uani 1 1 d . . . O5 O 0.51510(19) 0.36384(8) 0.4896(2) 0.0984(9) Uani 1 1 d . . . O6 O 0.48064(16) 0.28385(7) 0.50032(15) 0.0577(5) Uani 1 1 d D . . H6 H 0.3981(16) 0.2932(13) 0.495(3) 0.116(14) Uiso 1 1 d 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 Zn1 0.02573(14) 0.03052(14) 0.03415(15) -0.00244(10) 0.00496(10) -0.00403(10) C1 0.0541(16) 0.0469(15) 0.0446(15) 0.0077(12) 0.0033(12) -0.0022(12) C2 0.0712(19) 0.0669(19) 0.0468(16) 0.0196(14) -0.0034(14) 0.0028(16) C3 0.071(2) 0.081(2) 0.0391(15) 0.0065(14) -0.0118(14) 0.0033(16) C4 0.0528(16) 0.0601(16) 0.0382(14) -0.0066(12) -0.0058(12) 0.0030(12) C5 0.0302(11) 0.0438(13) 0.0285(11) -0.0057(9) 0.0039(9) 0.0037(9) C6 0.0249(10) 0.0378(12) 0.0343(12) -0.0103(9) 0.0032(9) 0.0024(9) C7 0.0374(13) 0.0415(14) 0.0535(15) -0.0125(11) -0.0104(11) -0.0020(10) C8 0.0399(13) 0.0311(13) 0.0722(18) -0.0074(12) -0.0053(12) -0.0030(10) C9 0.0365(13) 0.0328(12) 0.0535(14) 0.0001(10) 0.0018(11) 0.0027(10) C10 0.0346(12) 0.0360(12) 0.0355(12) -0.0018(10) -0.0027(10) 0.0014(9) C11 0.0483(15) 0.0466(14) 0.0487(15) -0.0043(11) 0.0105(12) 0.0061(12) C12 0.0464(16) 0.0695(19) 0.0597(17) -0.0083(14) 0.0121(13) 0.0199(14) C13 0.0304(13) 0.096(2) 0.0613(18) -0.0075(16) 0.0119(13) 0.0114(15) C14 0.0314(13) 0.0719(18) 0.0494(15) -0.0052(13) 0.0083(11) -0.0068(12) C15 0.0285(11) 0.0471(13) 0.0283(11) 0.0018(9) 0.0040(9) -0.0041(10) C16 0.0299(11) 0.0390(12) 0.0337(12) 0.0044(9) 0.0032(9) -0.0064(9) C17 0.0417(14) 0.0468(16) 0.0787(19) 0.0086(13) 0.0166(13) -0.0138(12) C18 0.0564(17) 0.0331(14) 0.091(2) 0.0088(13) 0.0063(15) -0.0114(12) C19 0.0453(14) 0.0331(13) 0.0580(15) 0.0027(11) -0.0001(12) 0.0018(10) C20 0.0340(12) 0.0368(13) 0.0489(14) 0.0011(10) 0.0058(10) 0.0005(10) C21 0.0202(10) 0.0257(10) 0.0294(11) 0.0014(8) 0.0018(8) -0.0008(8) C22 0.0214(10) 0.0331(11) 0.0242(10) -0.0010(8) 0.0026(8) -0.0016(8) C23 0.0229(10) 0.0308(11) 0.0255(10) -0.0010(8) 0.0016(8) -0.0009(8) C24 0.0259(11) 0.0355(12) 0.0437(13) -0.0028(10) 0.0070(9) 0.0017(9) C25 0.0238(10) 0.0329(11) 0.0224(10) -0.0012(8) 0.0018(8) -0.0021(8) C26 0.0240(10) 0.0365(12) 0.0330(11) -0.0012(9) 0.0053(9) -0.0042(9) C27 0.0374(12) 0.0300(12) 0.0403(13) -0.0002(9) 0.0048(10) -0.0042(10) C28 0.0367(13) 0.0306(12) 0.0508(14) -0.0044(10) 0.0073(11) 0.0064(9) C29 0.0225(10) 0.0452(14) 0.0270(11) -0.0069(9) 0.0012(8) 0.0009(9) C30 0.0185(10) 0.0293(11) 0.0336(11) -0.0035(8) 0.0008(8) -0.0022(8) C31 0.0222(10) 0.0292(11) 0.0313(11) -0.0035(8) 0.0028(8) -0.0017(8) C32 0.0283(11) 0.0404(13) 0.0341(12) -0.0040(9) -0.0012(9) -0.0004(9) C33 0.0433(14) 0.0461(14) 0.0313(12) -0.0029(10) -0.0006(10) -0.0018(11) C34 0.0441(14) 0.0466(14) 0.0345(13) -0.0060(10) 0.0135(11) -0.0037(11) C35 0.0280(11) 0.0435(13) 0.0427(13) -0.0046(10) 0.0121(10) -0.0001(9) C36 0.0232(10) 0.0305(11) 0.0370(12) -0.0021(9) 0.0062(9) -0.0017(8) C37 0.0186(10) 0.0330(11) 0.0437(13) 0.0005(9) 0.0028(9) -0.0011(8) C38 0.0327(12) 0.0338(12) 0.0402(13) 0.0012(10) 0.0077(10) 0.0041(10) C39 0.0216(10) 0.0329(11) 0.0372(12) 0.0006(9) -0.0002(9) -0.0019(8) C40 0.0251(11) 0.0492(14) 0.0455(14) 0.0054(11) -0.0063(10) -0.0008(10) C41 0.0398(13) 0.0512(15) 0.0374(13) 0.0099(11) -0.0076(11) -0.0062(11) C42 0.0401(13) 0.0508(14) 0.0327(12) 0.0035(10) 0.0058(10) -0.0078(11) C43 0.0246(11) 0.0430(13) 0.0359(12) 0.0012(9) 0.0055(9) -0.0028(9) C44 0.0221(10) 0.0319(11) 0.0327(11) -0.0008(9) 0.0016(9) -0.0049(8) N1 0.0280(9) 0.0318(9) 0.0331(10) -0.0039(8) 0.0001(7) -0.0004(7) N2 0.0314(10) 0.0410(10) 0.0326(10) 0.0014(8) 0.0056(8) -0.0003(8) N3 0.0266(9) 0.0332(10) 0.0375(10) 0.0025(8) 0.0056(8) -0.0029(7) N4 0.0308(10) 0.0393(11) 0.0349(10) -0.0009(8) 0.0050(8) 0.0021(8) O1 0.0219(7) 0.0511(10) 0.0334(8) -0.0058(7) 0.0058(6) -0.0042(6) O2 0.0245(7) 0.0389(8) 0.0354(8) -0.0027(6) -0.0029(6) -0.0025(6) O3 0.0192(8) 0.0584(11) 0.0824(13) -0.0131(9) 0.0033(8) -0.0046(7) O4 0.0347(9) 0.0513(11) 0.0562(10) 0.0012(8) 0.0038(8) 0.0114(8) O5 0.0342(11) 0.0573(14) 0.206(3) 0.0215(15) 0.0264(15) 0.0116(9) O6 0.0203(9) 0.0589(12) 0.0941(15) -0.0108(10) 0.0039(9) 0.0017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 2.0976(17) . ? Zn1 O1 2.1027(14) . ? Zn1 N1 2.1097(17) . ? Zn1 O2 2.1285(14) 3_667 ? Zn1 N2 2.1977(18) . ? Zn1 N4 2.2013(18) . ? C1 N2 1.338(3) . ? C1 C2 1.381(3) . ? C2 C3 1.369(4) . ? C3 C4 1.378(4) . ? C4 C5 1.388(3) . ? C5 N2 1.341(3) . ? C5 C6 1.488(3) . ? C6 N1 1.342(3) . ? C6 C7 1.391(3) . ? C7 C8 1.371(3) . ? C8 C9 1.369(3) . ? C9 C10 1.365(3) . ? C10 N1 1.333(3) . ? C11 N4 1.340(3) . ? C11 C12 1.372(4) . ? C12 C13 1.370(4) . ? C13 C14 1.380(4) . ? C14 C15 1.385(3) . ? C15 N4 1.339(3) . ? C15 C16 1.490(3) . ? C16 N3 1.348(3) . ? C16 C17 1.378(3) . ? C17 C18 1.385(4) . ? C18 C19 1.371(4) . ? C19 C20 1.372(3) . ? C20 N3 1.336(3) . ? C21 O1 1.252(2) . ? C21 O2 1.254(2) . ? C21 C22 1.528(3) . ? C22 C23 1.405(3) . ? C22 C25 1.409(3) . ? C23 C24 1.431(3) . ? C23 C25 1.438(3) 3_567 ? C24 C28 1.355(3) 3_567 ? C25 C26 1.430(3) . ? C25 C23 1.438(3) 3_567 ? C26 C27 1.350(3) . ? C27 C28 1.419(3) . ? C28 C24 1.355(3) 3_567 ? C29 O4 1.231(3) . ? C29 O3 1.258(3) . ? C29 C30 1.521(3) . ? C30 C44 1.401(3) . ? C30 C31 1.403(3) . ? C31 C32 1.428(3) . ? C31 C36 1.432(3) . ? C32 C33 1.354(3) . ? C33 C34 1.416(3) . ? C34 C35 1.351(3) . ? C35 C36 1.431(3) . ? C36 C37 1.403(3) . ? C37 C39 1.405(3) . ? C37 C38 1.547(3) . ? C38 O5 1.177(3) . ? C38 O6 1.247(3) . ? C39 C40 1.430(3) . ? C39 C44 1.435(3) . ? C40 C41 1.352(3) . ? C41 C42 1.413(3) . ? C42 C43 1.355(3) . ? C43 C44 1.426(3) . ? O2 Zn1 2.1285(14) 3_667 ? 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 N3 Zn1 O1 98.60(6) . . ? N3 Zn1 N1 170.10(7) . . ? O1 Zn1 N1 88.64(6) . . ? N3 Zn1 O2 94.81(6) . 3_667 ? O1 Zn1 O2 96.00(5) . 3_667 ? N1 Zn1 O2 91.12(6) . 3_667 ? N3 Zn1 N2 97.46(7) . . ? O1 Zn1 N2 83.96(6) . . ? N1 Zn1 N2 76.48(7) . . ? O2 Zn1 N2 167.60(6) 3_667 . ? N3 Zn1 N4 76.47(7) . . ? O1 Zn1 N4 173.86(6) . . ? N1 Zn1 N4 95.84(7) . . ? O2 Zn1 N4 88.13(6) 3_667 . ? N2 Zn1 N4 92.98(7) . . ? N2 C1 C2 122.6(2) . . ? C3 C2 C1 118.5(3) . . ? C2 C3 C4 119.9(3) . . ? C3 C4 C5 118.6(2) . . ? N2 C5 C4 121.9(2) . . ? N2 C5 C6 115.56(18) . . ? C4 C5 C6 122.6(2) . . ? N1 C6 C7 120.7(2) . . ? N1 C6 C5 116.37(18) . . ? C7 C6 C5 122.96(19) . . ? C8 C7 C6 119.2(2) . . ? C9 C8 C7 119.7(2) . . ? C10 C9 C8 118.2(2) . . ? N1 C10 C9 123.3(2) . . ? N4 C11 C12 123.1(2) . . ? C13 C12 C11 118.3(2) . . ? C12 C13 C14 119.5(2) . . ? C13 C14 C15 118.9(3) . . ? N4 C15 C14 121.7(2) . . ? N4 C15 C16 115.33(18) . . ? C14 C15 C16 122.9(2) . . ? N3 C16 C17 121.1(2) . . ? N3 C16 C15 115.91(18) . . ? C17 C16 C15 123.0(2) . . ? C16 C17 C18 119.4(2) . . ? C19 C18 C17 119.5(2) . . ? C18 C19 C20 117.9(2) . . ? N3 C20 C19 123.5(2) . . ? O1 C21 O2 124.84(17) . . ? O1 C21 C22 116.59(17) . . ? O2 C21 C22 118.50(17) . . ? C23 C22 C25 120.36(18) . . ? C23 C22 C21 120.75(17) . . ? C25 C22 C21 118.89(17) . . ? C22 C23 C24 122.32(18) . . ? C22 C23 C25 119.87(18) . 3_567 ? C24 C23 C25 117.79(18) . 3_567 ? C28 C24 C23 121.5(2) 3_567 . ? C22 C25 C26 122.02(18) . . ? C22 C25 C23 119.75(18) . 3_567 ? C26 C25 C23 118.20(18) . 3_567 ? C27 C26 C25 121.94(19) . . ? C26 C27 C28 119.8(2) . . ? C24 C28 C27 120.6(2) 3_567 . ? O4 C29 O3 126.8(2) . . ? O4 C29 C30 118.18(19) . . ? O3 C29 C30 115.06(19) . . ? C44 C30 C31 120.70(17) . . ? C44 C30 C29 119.50(17) . . ? C31 C30 C29 119.78(17) . . ? C30 C31 C32 121.83(17) . . ? C30 C31 C36 119.79(18) . . ? C32 C31 C36 118.38(18) . . ? C33 C32 C31 121.5(2) . . ? C32 C33 C34 120.2(2) . . ? C35 C34 C33 120.5(2) . . ? C34 C35 C36 121.5(2) . . ? C37 C36 C35 122.63(18) . . ? C37 C36 C31 119.38(18) . . ? C35 C36 C31 117.99(19) . . ? C36 C37 C39 121.03(17) . . ? C36 C37 C38 119.73(18) . . ? C39 C37 C38 119.24(18) . . ? O5 C38 O6 127.8(2) . . ? O5 C38 C37 119.1(2) . . ? O6 C38 C37 113.10(19) . . ? C37 C39 C40 122.76(18) . . ? C37 C39 C44 119.31(18) . . ? C40 C39 C44 117.92(19) . . ? C41 C40 C39 121.5(2) . . ? C40 C41 C42 120.5(2) . . ? C43 C42 C41 120.2(2) . . ? C42 C43 C44 121.5(2) . . ? C30 C44 C43 121.88(18) . . ? C30 C44 C39 119.73(18) . . ? C43 C44 C39 118.34(18) . . ? C10 N1 C6 118.85(18) . . ? C10 N1 Zn1 123.69(14) . . ? C6 N1 Zn1 116.25(14) . . ? C1 N2 C5 118.6(2) . . ? C1 N2 Zn1 127.17(16) . . ? C5 N2 Zn1 114.21(14) . . ? C20 N3 C16 118.48(18) . . ? C20 N3 Zn1 124.29(14) . . ? C16 N3 Zn1 117.18(14) . . ? C15 N4 C11 118.3(2) . . ? C15 N4 Zn1 114.12(14) . . ? C11 N4 Zn1 126.42(16) . . ? C21 O1 Zn1 130.09(13) . . ? C21 O2 Zn1 141.49(13) . 3_667 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -1.3(4) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 N2 -1.7(4) . . . . ? C3 C4 C5 C6 177.1(2) . . . . ? N2 C5 C6 N1 -7.2(3) . . . . ? C4 C5 C6 N1 173.9(2) . . . . ? N2 C5 C6 C7 171.4(2) . . . . ? C4 C5 C6 C7 -7.4(3) . . . . ? N1 C6 C7 C8 0.1(3) . . . . ? C5 C6 C7 C8 -178.5(2) . . . . ? C6 C7 C8 C9 -1.3(4) . . . . ? C7 C8 C9 C10 1.1(4) . . . . ? C8 C9 C10 N1 0.4(3) . . . . ? N4 C11 C12 C13 0.6(4) . . . . ? C11 C12 C13 C14 -1.4(4) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 N4 0.6(4) . . . . ? C13 C14 C15 C16 178.1(2) . . . . ? N4 C15 C16 N3 11.1(3) . . . . ? C14 C15 C16 N3 -166.6(2) . . . . ? N4 C15 C16 C17 -169.6(2) . . . . ? C14 C15 C16 C17 12.7(3) . . . . ? N3 C16 C17 C18 2.9(4) . . . . ? C15 C16 C17 C18 -176.3(2) . . . . ? C16 C17 C18 C19 -0.7(4) . . . . ? C17 C18 C19 C20 -1.6(4) . . . . ? C18 C19 C20 N3 1.9(4) . . . . ? O1 C21 C22 C23 65.2(2) . . . . ? O2 C21 C22 C23 -117.7(2) . . . . ? O1 C21 C22 C25 -114.4(2) . . . . ? O2 C21 C22 C25 62.6(2) . . . . ? C25 C22 C23 C24 179.40(18) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C25 C22 C23 C25 -1.7(3) . . . 3_567 ? C21 C22 C23 C25 178.72(17) . . . 3_567 ? C22 C23 C24 C28 177.4(2) . . . 3_567 ? C25 C23 C24 C28 -1.6(3) 3_567 . . 3_567 ? C23 C22 C25 C26 -176.38(17) . . . . ? C21 C22 C25 C26 3.2(3) . . . . ? C23 C22 C25 C23 1.7(3) . . . 3_567 ? C21 C22 C25 C23 -178.71(17) . . . 3_567 ? C22 C25 C26 C27 179.64(19) . . . . ? C23 C25 C26 C27 1.6(3) 3_567 . . . ? C25 C26 C27 C28 0.5(3) . . . . ? C26 C27 C28 C24 -1.5(3) . . . 3_567 ? O4 C29 C30 C44 -97.6(2) . . . . ? O3 C29 C30 C44 81.9(2) . . . . ? O4 C29 C30 C31 81.1(2) . . . . ? O3 C29 C30 C31 -99.4(2) . . . . ? C44 C30 C31 C32 -178.70(19) . . . . ? C29 C30 C31 C32 2.6(3) . . . . ? C44 C30 C31 C36 2.0(3) . . . . ? C29 C30 C31 C36 -176.65(18) . . . . ? C30 C31 C32 C33 179.5(2) . . . . ? C36 C31 C32 C33 -1.2(3) . . . . ? C31 C32 C33 C34 0.2(3) . . . . ? C32 C33 C34 C35 0.8(3) . . . . ? C33 C34 C35 C36 -0.7(3) . . . . ? C34 C35 C36 C37 -179.7(2) . . . . ? C34 C35 C36 C31 -0.3(3) . . . . ? C30 C31 C36 C37 0.0(3) . . . . ? C32 C31 C36 C37 -179.34(18) . . . . ? C30 C31 C36 C35 -179.50(19) . . . . ? C32 C31 C36 C35 1.2(3) . . . . ? C35 C36 C37 C39 177.79(19) . . . . ? C31 C36 C37 C39 -1.6(3) . . . . ? C35 C36 C37 C38 -3.2(3) . . . . ? C31 C36 C37 C38 177.38(18) . . . . ? C36 C37 C38 O5 98.9(3) . . . . ? C39 C37 C38 O5 -82.1(3) . . . . ? C36 C37 C38 O6 -79.7(3) . . . . ? C39 C37 C38 O6 99.3(2) . . . . ? C36 C37 C39 C40 -179.2(2) . . . . ? C38 C37 C39 C40 1.7(3) . . . . ? C36 C37 C39 C44 1.3(3) . . . . ? C38 C37 C39 C44 -177.69(18) . . . . ? C37 C39 C40 C41 -178.6(2) . . . . ? C44 C39 C40 C41 0.9(3) . . . . ? C39 C40 C41 C42 0.3(4) . . . . ? C40 C41 C42 C43 -1.1(4) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? C31 C30 C44 C43 -179.73(19) . . . . ? C29 C30 C44 C43 -1.1(3) . . . . ? C31 C30 C44 C39 -2.3(3) . . . . ? C29 C30 C44 C39 176.36(18) . . . . ? C42 C43 C44 C30 178.1(2) . . . . ? C42 C43 C44 C39 0.6(3) . . . . ? C37 C39 C44 C30 0.6(3) . . . . ? C40 C39 C44 C30 -178.82(19) . . . . ? C37 C39 C44 C43 178.14(19) . . . . ? C40 C39 C44 C43 -1.3(3) . . . . ? C9 C10 N1 C6 -1.6(3) . . . . ? C9 C10 N1 Zn1 165.40(17) . . . . ? C7 C6 N1 C10 1.3(3) . . . . ? C5 C6 N1 C10 179.97(18) . . . . ? C7 C6 N1 Zn1 -166.59(16) . . . . ? C5 C6 N1 Zn1 12.1(2) . . . . ? N3 Zn1 N1 C10 130.3(4) . . . . ? O1 Zn1 N1 C10 -92.55(17) . . . . ? O2 Zn1 N1 C10 3.42(17) 3_667 . . . ? N2 Zn1 N1 C10 -176.66(18) . . . . ? N4 Zn1 N1 C10 91.66(17) . . . . ? N3 Zn1 N1 C6 -62.5(4) . . . . ? O1 Zn1 N1 C6 74.71(14) . . . . ? O2 Zn1 N1 C6 170.68(14) 3_667 . . . ? N2 Zn1 N1 C6 -9.41(14) . . . . ? N4 Zn1 N1 C6 -101.08(14) . . . . ? C2 C1 N2 C5 1.0(4) . . . . ? C2 C1 N2 Zn1 -176.02(19) . . . . ? C4 C5 N2 C1 0.5(3) . . . . ? C6 C5 N2 C1 -178.29(19) . . . . ? C4 C5 N2 Zn1 177.93(17) . . . . ? C6 C5 N2 Zn1 -0.9(2) . . . . ? N3 Zn1 N2 C1 -5.5(2) . . . . ? O1 Zn1 N2 C1 92.4(2) . . . . ? N1 Zn1 N2 C1 -177.6(2) . . . . ? O2 Zn1 N2 C1 -177.2(2) 3_667 . . . ? N4 Zn1 N2 C1 -82.3(2) . . . . ? N3 Zn1 N2 C5 177.33(15) . . . . ? O1 Zn1 N2 C5 -84.75(15) . . . . ? N1 Zn1 N2 C5 5.30(14) . . . . ? O2 Zn1 N2 C5 5.7(4) 3_667 . . . ? N4 Zn1 N2 C5 100.59(15) . . . . ? C19 C20 N3 C16 0.3(3) . . . . ? C19 C20 N3 Zn1 -176.94(18) . . . . ? C17 C16 N3 C20 -2.7(3) . . . . ? C15 C16 N3 C20 176.58(18) . . . . ? C17 C16 N3 Zn1 174.70(18) . . . . ? C15 C16 N3 Zn1 -6.0(2) . . . . ? O1 Zn1 N3 C20 1.42(18) . . . . ? N1 Zn1 N3 C20 138.0(3) . . . . ? O2 Zn1 N3 C20 -95.40(17) 3_667 . . . ? N2 Zn1 N3 C20 86.40(17) . . . . ? N4 Zn1 N3 C20 177.69(18) . . . . ? O1 Zn1 N3 C16 -175.86(15) . . . . ? N1 Zn1 N3 C16 -39.3(4) . . . . ? O2 Zn1 N3 C16 87.32(15) 3_667 . . . ? N2 Zn1 N3 C16 -90.88(15) . . . . ? N4 Zn1 N3 C16 0.41(15) . . . . ? C14 C15 N4 C11 -1.3(3) . . . . ? C16 C15 N4 C11 -179.06(19) . . . . ? C14 C15 N4 Zn1 167.22(17) . . . . ? C16 C15 N4 Zn1 -10.5(2) . . . . ? C12 C11 N4 C15 0.8(4) . . . . ? C12 C11 N4 Zn1 -166.25(19) . . . . ? N3 Zn1 N4 C15 5.76(14) . . . . ? O1 Zn1 N4 C15 42.8(6) . . . . ? N1 Zn1 N4 C15 179.43(14) . . . . ? O2 Zn1 N4 C15 -89.64(15) 3_667 . . . ? N2 Zn1 N4 C15 102.73(15) . . . . ? N3 Zn1 N4 C11 173.2(2) . . . . ? O1 Zn1 N4 C11 -149.7(5) . . . . ? N1 Zn1 N4 C11 -13.09(19) . . . . ? O2 Zn1 N4 C11 77.84(19) 3_667 . . . ? N2 Zn1 N4 C11 -89.79(19) . . . . ? O2 C21 O1 Zn1 18.7(3) . . . . ? C22 C21 O1 Zn1 -164.53(13) . . . . ? N3 Zn1 O1 C21 -73.02(17) . . . . ? N1 Zn1 O1 C21 113.77(17) . . . . ? O2 Zn1 O1 C21 22.78(17) 3_667 . . . ? N2 Zn1 O1 C21 -169.69(18) . . . . ? N4 Zn1 O1 C21 -109.3(6) . . . . ? O1 C21 O2 Zn1 -111.5(2) . . . 3_667 ? C22 C21 O2 Zn1 71.7(3) . . . 3_667 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.416 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.045 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 623316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 N6 O2 Zn' _chemical_formula_weight 486.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5311(19) _cell_length_b 10.770(2) _cell_length_c 12.445(2) _cell_angle_alpha 112.048(3) _cell_angle_beta 95.725(3) _cell_angle_gamma 110.766(3) _cell_volume 1066.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2515 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7557 _exptl_absorpt_correction_T_max 0.8805 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5334 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3706 _reflns_number_gt 2952 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+1.0116P] 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 3706 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.62384(5) 0.70043(5) 0.63591(4) 0.03659(17) Uani 1 1 d . . . C1 C 0.1763(5) 0.4582(4) 0.4031(4) 0.0448(10) Uani 1 1 d . . . C2 C 0.1630(6) 0.5880(5) 0.4632(5) 0.0673(14) Uani 1 1 d . . . H2A H 0.0786 0.6093 0.4491 0.081 Uiso 1 1 calc R . . C3 C 0.3038(6) 0.6793(5) 0.5493(5) 0.0652(14) Uani 1 1 d . . . H3A H 0.3302 0.7756 0.6057 0.078 Uiso 1 1 calc R . . C9 C 0.6030(5) 1.1163(5) 0.8313(4) 0.0544(11) Uani 1 1 d . . . H9A H 0.5785 1.1815 0.8914 0.065 Uiso 1 1 calc R . . C10 C 0.6525(6) 1.1351(5) 0.7354(4) 0.0583(12) Uani 1 1 d . . . H10A H 0.6677 1.2146 0.7175 0.070 Uiso 1 1 calc R . . C11 C 0.6746(5) 1.0089(4) 0.6711(4) 0.0434(9) Uani 1 1 d . . . C12 C 0.7205(5) 0.9567(5) 0.5593(4) 0.0483(10) Uani 1 1 d . . . C13 C 0.7731(8) 1.0442(6) 0.5020(5) 0.0806(17) Uani 1 1 d . . . H13A H 0.7833 1.1411 0.5341 0.097 Uiso 1 1 calc R . . C14 C 0.8105(9) 0.9849(7) 0.3957(6) 0.100(2) Uani 1 1 d . . . H14A H 0.8472 1.0419 0.3554 0.120 Uiso 1 1 calc R . . C15 C 0.7934(8) 0.8430(7) 0.3506(5) 0.0888(19) Uani 1 1 d . . . H15A H 0.8160 0.8009 0.2782 0.107 Uiso 1 1 calc R . . C16 C 0.7428(7) 0.7630(6) 0.4125(4) 0.0698(14) Uani 1 1 d . . . H16A H 0.7322 0.6660 0.3812 0.084 Uiso 1 1 calc R . . C17 C 0.5386(4) 0.6829(4) 0.8706(3) 0.0339(8) Uani 1 1 d . . . C18 C 0.5188(4) 0.5864(4) 0.9362(3) 0.0294(7) Uani 1 1 d . . . C19 C 0.6500(4) 0.5806(4) 0.9930(3) 0.0293(7) Uani 1 1 d . . . C20 C 0.8041(4) 0.6600(4) 0.9894(4) 0.0418(9) Uani 1 1 d . . . H20A H 0.8185 0.7146 0.9453 0.050 Uiso 1 1 calc R . . C21 C 0.9288(5) 0.6576(5) 1.0482(4) 0.0516(11) Uani 1 1 d . . . H21A H 1.0279 0.7110 1.0450 0.062 Uiso 1 1 calc R . . C22 C 0.3705(4) 0.5065(4) 0.9421(3) 0.0296(7) Uani 1 1 d . . . C23 C 0.2339(4) 0.5059(4) 0.8820(3) 0.0416(9) Uani 1 1 d . . . H23A H 0.2442 0.5622 0.8396 0.050 Uiso 1 1 calc R . . C24 C 0.0898(5) 0.4251(5) 0.8855(4) 0.0523(11) Uani 1 1 d . . . H24A H 0.0027 0.4245 0.8438 0.063 Uiso 1 1 calc R . . N1 N 0.3960(4) 0.6107(3) 0.5406(3) 0.0386(7) Uani 1 1 d . . . N2 N 0.3175(4) 0.4728(3) 0.4494(3) 0.0386(7) Uani 1 1 d . . . N4 N 0.5973(4) 0.9864(4) 0.8209(3) 0.0461(8) Uani 1 1 d . . . H4B H 0.5695 0.9507 0.8706 0.055 Uiso 1 1 calc R . . N5 N 0.6395(4) 0.9185(3) 0.7252(3) 0.0391(7) Uani 1 1 d . . . N6 N 0.7075(4) 0.8178(4) 0.5167(3) 0.0483(8) Uani 1 1 d . . . O1 O 0.5676(4) 0.6365(3) 0.7723(2) 0.0513(7) Uani 1 1 d . . . O2 O 0.5246(4) 0.8005(3) 0.9222(3) 0.0520(7) Uani 1 1 d . . . C4 C 0.0272(5) 0.0827(5) 0.1748(4) 0.0538(11) Uani 1 1 d . . . H4A H 0.0626 0.0091 0.1493 0.065 Uiso 1 1 calc R . . C5 C -0.1213(5) 0.0512(5) 0.1168(4) 0.0628(13) Uani 1 1 d . . . H5A H -0.1840 -0.0411 0.0533 0.075 Uiso 1 1 calc R . . C6 C -0.1732(6) 0.1574(6) 0.1543(4) 0.0636(13) Uani 1 1 d . . . H6A H -0.2728 0.1388 0.1170 0.076 Uiso 1 1 calc R . . C7 C -0.0781(5) 0.2931(5) 0.2479(4) 0.0572(12) Uani 1 1 d . . . H7A H -0.1122 0.3676 0.2743 0.069 Uiso 1 1 calc R . . C8 C 0.0670(5) 0.3170(4) 0.3014(3) 0.0403(9) Uani 1 1 d . . . N3 N 0.1220(4) 0.2137(4) 0.2654(3) 0.0406(8) 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 Zn1 0.0452(3) 0.0312(3) 0.0318(2) 0.01317(19) 0.01006(18) 0.0154(2) C1 0.050(2) 0.040(2) 0.048(2) 0.0219(19) 0.0092(19) 0.0210(19) C2 0.054(3) 0.044(3) 0.092(4) 0.015(3) 0.003(3) 0.027(2) C3 0.058(3) 0.037(2) 0.085(4) 0.009(2) 0.009(3) 0.026(2) C9 0.071(3) 0.039(2) 0.055(3) 0.017(2) 0.024(2) 0.028(2) C10 0.081(3) 0.041(2) 0.067(3) 0.030(2) 0.029(3) 0.031(2) C11 0.053(2) 0.034(2) 0.044(2) 0.0199(18) 0.0138(19) 0.0160(19) C12 0.060(3) 0.042(2) 0.048(2) 0.027(2) 0.019(2) 0.019(2) C13 0.129(5) 0.060(3) 0.074(4) 0.046(3) 0.051(4) 0.040(3) C14 0.165(7) 0.083(4) 0.082(4) 0.058(4) 0.071(4) 0.052(5) C15 0.145(6) 0.078(4) 0.065(3) 0.041(3) 0.063(4) 0.051(4) C16 0.106(4) 0.059(3) 0.054(3) 0.026(3) 0.039(3) 0.039(3) C17 0.0329(19) 0.037(2) 0.0327(19) 0.0211(17) 0.0069(15) 0.0110(16) C18 0.040(2) 0.0278(18) 0.0224(16) 0.0125(14) 0.0096(14) 0.0152(16) C19 0.0342(19) 0.0301(18) 0.0266(17) 0.0132(15) 0.0120(14) 0.0152(15) C20 0.040(2) 0.041(2) 0.051(2) 0.0268(19) 0.0182(18) 0.0165(18) C21 0.035(2) 0.056(3) 0.069(3) 0.034(2) 0.021(2) 0.016(2) C22 0.0335(19) 0.0292(18) 0.0272(17) 0.0123(15) 0.0081(14) 0.0148(15) C23 0.043(2) 0.043(2) 0.045(2) 0.0230(19) 0.0090(18) 0.0221(19) C24 0.038(2) 0.059(3) 0.064(3) 0.030(2) 0.007(2) 0.024(2) N1 0.0426(18) 0.0252(16) 0.0384(17) 0.0068(14) 0.0055(14) 0.0135(14) N2 0.0443(19) 0.0363(18) 0.0371(17) 0.0181(15) 0.0114(14) 0.0170(15) N4 0.059(2) 0.0409(19) 0.0400(18) 0.0188(16) 0.0180(16) 0.0200(17) N5 0.0500(19) 0.0323(17) 0.0355(17) 0.0158(14) 0.0152(15) 0.0163(15) N6 0.064(2) 0.041(2) 0.0449(19) 0.0236(17) 0.0207(17) 0.0216(17) O1 0.078(2) 0.0539(18) 0.0378(15) 0.0298(14) 0.0254(15) 0.0325(16) O2 0.080(2) 0.0421(17) 0.0500(17) 0.0285(14) 0.0255(15) 0.0319(16) C4 0.058(3) 0.043(3) 0.046(2) 0.011(2) 0.009(2) 0.017(2) C5 0.052(3) 0.055(3) 0.048(3) 0.004(2) -0.002(2) 0.012(2) C6 0.047(3) 0.072(3) 0.059(3) 0.024(3) 0.000(2) 0.021(2) C7 0.054(3) 0.061(3) 0.057(3) 0.025(2) 0.003(2) 0.029(2) C8 0.046(2) 0.040(2) 0.041(2) 0.0231(18) 0.0135(18) 0.0191(19) N3 0.0424(18) 0.0385(18) 0.0367(17) 0.0149(15) 0.0103(14) 0.0144(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.048(3) . ? Zn1 N2 2.072(3) 2_666 ? Zn1 O1 2.107(3) . ? Zn1 N5 2.129(3) . ? Zn1 N3 2.279(3) 2_666 ? Zn1 N6 2.316(3) . ? C1 N2 1.340(5) . ? C1 C2 1.374(6) . ? C1 C8 1.472(6) . ? C2 C3 1.380(7) . ? C2 H2A 0.9300 . ? C3 N1 1.322(5) . ? C3 H3A 0.9300 . ? C9 N4 1.337(5) . ? C9 C10 1.384(6) . ? C9 H9A 0.9300 . ? C10 C11 1.397(6) . ? C10 H10A 0.9300 . ? C11 N5 1.348(5) . ? C11 C12 1.466(6) . ? C12 N6 1.340(5) . ? C12 C13 1.374(6) . ? C13 C14 1.381(8) . ? C13 H13A 0.9300 . ? C14 C15 1.356(8) . ? C14 H14A 0.9300 . ? C15 C16 1.358(7) . ? C15 H15A 0.9300 . ? C16 N6 1.341(5) . ? C16 H16A 0.9300 . ? C17 O1 1.237(4) . ? C17 O2 1.249(4) . ? C17 C18 1.520(5) . ? C18 C22 1.396(5) . ? C18 C19 1.407(5) . ? C19 C20 1.428(5) . ? C19 C22 1.429(5) 2_667 ? C20 C21 1.347(6) . ? C20 H20A 0.9300 . ? C21 C24 1.405(6) 2_667 ? C21 H21A 0.9300 . ? C22 C19 1.429(5) 2_667 ? C22 C23 1.432(5) . ? C23 C24 1.356(6) . ? C23 H23A 0.9300 . ? C24 C21 1.405(6) 2_667 ? C24 H24A 0.9300 . ? N1 N2 1.353(4) . ? N2 Zn1 2.072(3) 2_666 ? N4 N5 1.329(4) . ? N4 H4B 0.8600 . ? C4 N3 1.333(5) . ? C4 C5 1.383(6) . ? C4 H4A 0.9300 . ? C5 C6 1.347(7) . ? C5 H5A 0.9300 . ? C6 C7 1.374(6) . ? C6 H6A 0.9300 . ? C7 C8 1.363(6) . ? C7 H7A 0.9300 . ? C8 N3 1.342(5) . ? N3 Zn1 2.279(3) 2_666 ? 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 Zn1 N2 100.56(12) . 2_666 ? N1 Zn1 O1 93.79(13) . . ? N2 Zn1 O1 93.59(12) 2_666 . ? N1 Zn1 N5 94.54(12) . . ? N2 Zn1 N5 161.26(12) 2_666 . ? O1 Zn1 N5 96.44(11) . . ? N1 Zn1 N3 176.32(11) . 2_666 ? N2 Zn1 N3 75.77(12) 2_666 2_666 ? O1 Zn1 N3 86.42(12) . 2_666 ? N5 Zn1 N3 89.08(12) . 2_666 ? N1 Zn1 N6 91.81(13) . . ? N2 Zn1 N6 95.12(12) 2_666 . ? O1 Zn1 N6 168.61(12) . . ? N5 Zn1 N6 73.22(12) . . ? N3 Zn1 N6 88.63(12) 2_666 . ? N2 C1 C2 109.6(4) . . ? N2 C1 C8 118.9(3) . . ? C2 C1 C8 131.5(4) . . ? C1 C2 C3 104.1(4) . . ? C1 C2 H2A 128.0 . . ? C3 C2 H2A 128.0 . . ? N1 C3 C2 110.5(4) . . ? N1 C3 H3A 124.7 . . ? C2 C3 H3A 124.7 . . ? N4 C9 C10 106.8(4) . . ? N4 C9 H9A 126.6 . . ? C10 C9 H9A 126.6 . . ? C9 C10 C11 105.1(4) . . ? C9 C10 H10A 127.4 . . ? C11 C10 H10A 127.4 . . ? N5 C11 C10 109.8(4) . . ? N5 C11 C12 116.9(3) . . ? C10 C11 C12 133.3(4) . . ? N6 C12 C13 122.2(4) . . ? N6 C12 C11 115.4(3) . . ? C13 C12 C11 122.3(4) . . ? C12 C13 C14 118.5(5) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? C15 C14 C13 119.5(5) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 119.2(5) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? N6 C16 C15 122.9(5) . . ? N6 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? O1 C17 O2 127.2(3) . . ? O1 C17 C18 116.3(3) . . ? O2 C17 C18 116.4(3) . . ? C22 C18 C19 120.4(3) . . ? C22 C18 C17 119.6(3) . . ? C19 C18 C17 120.0(3) . . ? C18 C19 C20 122.5(3) . . ? C18 C19 C22 119.1(3) . 2_667 ? C20 C19 C22 118.5(3) . 2_667 ? C21 C20 C19 121.5(4) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C24 120.4(4) . 2_667 ? C20 C21 H21A 119.8 . . ? C24 C21 H21A 119.8 2_667 . ? C18 C22 C19 120.6(3) . 2_667 ? C18 C22 C23 121.9(3) . . ? C19 C22 C23 117.6(3) 2_667 . ? C24 C23 C22 121.6(4) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C21 120.4(4) . 2_667 ? C23 C24 H24A 119.8 . . ? C21 C24 H24A 119.8 2_667 . ? C3 N1 N2 107.8(3) . . ? C3 N1 Zn1 126.8(3) . . ? N2 N1 Zn1 125.2(2) . . ? C1 N2 N1 108.0(3) . . ? C1 N2 Zn1 117.5(3) . 2_666 ? N1 N2 Zn1 134.2(2) . 2_666 ? N5 N4 C9 112.4(3) . . ? N5 N4 H4B 123.8 . . ? C9 N4 H4B 123.8 . . ? N4 N5 C11 105.9(3) . . ? N4 N5 Zn1 133.5(2) . . ? C11 N5 Zn1 119.6(3) . . ? C12 N6 C16 117.8(4) . . ? C12 N6 Zn1 114.4(3) . . ? C16 N6 Zn1 127.8(3) . . ? C17 O1 Zn1 140.8(3) . . ? N3 C4 C5 123.0(4) . . ? N3 C4 H4A 118.5 . . ? C5 C4 H4A 118.5 . . ? C6 C5 C4 118.5(4) . . ? C6 C5 H5A 120.7 . . ? C4 C5 H5A 120.7 . . ? C5 C6 C7 119.6(4) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? N3 C8 C7 122.7(4) . . ? N3 C8 C1 114.5(3) . . ? C7 C8 C1 122.8(4) . . ? C4 N3 C8 117.2(4) . . ? C4 N3 Zn1 129.8(3) . 2_666 ? C8 N3 Zn1 112.8(2) . 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -1.1(6) . . . . ? C8 C1 C2 C3 -179.9(5) . . . . ? C1 C2 C3 N1 1.0(6) . . . . ? N4 C9 C10 C11 -0.2(5) . . . . ? C9 C10 C11 N5 0.3(5) . . . . ? C9 C10 C11 C12 177.6(5) . . . . ? N5 C11 C12 N6 6.3(6) . . . . ? C10 C11 C12 N6 -170.8(5) . . . . ? N5 C11 C12 C13 -173.7(5) . . . . ? C10 C11 C12 C13 9.2(8) . . . . ? N6 C12 C13 C14 1.4(9) . . . . ? C11 C12 C13 C14 -178.6(6) . . . . ? C12 C13 C14 C15 0.5(11) . . . . ? C13 C14 C15 C16 -1.4(11) . . . . ? C14 C15 C16 N6 0.5(10) . . . . ? O1 C17 C18 C22 -107.1(4) . . . . ? O2 C17 C18 C22 73.4(4) . . . . ? O1 C17 C18 C19 74.4(4) . . . . ? O2 C17 C18 C19 -105.2(4) . . . . ? C22 C18 C19 C20 179.9(3) . . . . ? C17 C18 C19 C20 -1.6(5) . . . . ? C22 C18 C19 C22 -0.8(5) . . . 2_667 ? C17 C18 C19 C22 177.7(3) . . . 2_667 ? C18 C19 C20 C21 177.4(4) . . . . ? C22 C19 C20 C21 -1.9(6) 2_667 . . . ? C19 C20 C21 C24 0.6(7) . . . 2_667 ? C19 C18 C22 C19 0.8(5) . . . 2_667 ? C17 C18 C22 C19 -177.7(3) . . . 2_667 ? C19 C18 C22 C23 -177.8(3) . . . . ? C17 C18 C22 C23 3.6(5) . . . . ? C18 C22 C23 C24 178.3(4) . . . . ? C19 C22 C23 C24 -0.4(5) 2_667 . . . ? C22 C23 C24 C21 1.8(6) . . . 2_667 ? C2 C3 N1 N2 -0.5(6) . . . . ? C2 C3 N1 Zn1 174.2(3) . . . . ? N2 Zn1 N1 C3 -172.9(4) 2_666 . . . ? O1 Zn1 N1 C3 92.7(4) . . . . ? N5 Zn1 N1 C3 -4.1(4) . . . . ? N3 Zn1 N1 C3 -174.2(17) 2_666 . . . ? N6 Zn1 N1 C3 -77.4(4) . . . . ? N2 Zn1 N1 N2 0.9(4) 2_666 . . . ? O1 Zn1 N1 N2 -93.4(3) . . . . ? N5 Zn1 N1 N2 169.8(3) . . . . ? N3 Zn1 N1 N2 0(2) 2_666 . . . ? N6 Zn1 N1 N2 96.5(3) . . . . ? C2 C1 N2 N1 0.8(5) . . . . ? C8 C1 N2 N1 179.8(3) . . . . ? C2 C1 N2 Zn1 -174.2(3) . . . 2_666 ? C8 C1 N2 Zn1 4.9(5) . . . 2_666 ? C3 N1 N2 C1 -0.2(5) . . . . ? Zn1 N1 N2 C1 -175.0(3) . . . . ? C3 N1 N2 Zn1 173.6(3) . . . 2_666 ? Zn1 N1 N2 Zn1 -1.3(5) . . . 2_666 ? C10 C9 N4 N5 0.0(5) . . . . ? C9 N4 N5 C11 0.2(5) . . . . ? C9 N4 N5 Zn1 -168.0(3) . . . . ? C10 C11 N5 N4 -0.3(5) . . . . ? C12 C11 N5 N4 -178.1(3) . . . . ? C10 C11 N5 Zn1 169.9(3) . . . . ? C12 C11 N5 Zn1 -7.9(5) . . . . ? N1 Zn1 N5 N4 81.4(4) . . . . ? N2 Zn1 N5 N4 -134.9(4) 2_666 . . . ? O1 Zn1 N5 N4 -13.0(4) . . . . ? N3 Zn1 N5 N4 -99.3(4) 2_666 . . . ? N6 Zn1 N5 N4 171.9(4) . . . . ? N1 Zn1 N5 C11 -85.5(3) . . . . ? N2 Zn1 N5 C11 58.2(5) 2_666 . . . ? O1 Zn1 N5 C11 -179.9(3) . . . . ? N3 Zn1 N5 C11 93.8(3) 2_666 . . . ? N6 Zn1 N5 C11 5.0(3) . . . . ? C13 C12 N6 C16 -2.3(7) . . . . ? C11 C12 N6 C16 177.7(4) . . . . ? C13 C12 N6 Zn1 178.0(4) . . . . ? C11 C12 N6 Zn1 -2.0(5) . . . . ? C15 C16 N6 C12 1.3(8) . . . . ? C15 C16 N6 Zn1 -179.0(5) . . . . ? N1 Zn1 N6 C12 92.9(3) . . . . ? N2 Zn1 N6 C12 -166.4(3) 2_666 . . . ? O1 Zn1 N6 C12 -26.6(8) . . . . ? N5 Zn1 N6 C12 -1.3(3) . . . . ? N3 Zn1 N6 C12 -90.8(3) 2_666 . . . ? N1 Zn1 N6 C16 -86.9(4) . . . . ? N2 Zn1 N6 C16 13.9(4) 2_666 . . . ? O1 Zn1 N6 C16 153.7(6) . . . . ? N5 Zn1 N6 C16 178.9(4) . . . . ? N3 Zn1 N6 C16 89.5(4) 2_666 . . . ? O2 C17 O1 Zn1 4.8(7) . . . . ? C18 C17 O1 Zn1 -174.7(3) . . . . ? N1 Zn1 O1 C17 -90.5(4) . . . . ? N2 Zn1 O1 C17 168.6(4) 2_666 . . . ? N5 Zn1 O1 C17 4.5(4) . . . . ? N3 Zn1 O1 C17 93.2(4) 2_666 . . . ? N6 Zn1 O1 C17 28.8(9) . . . . ? N3 C4 C5 C6 -0.6(8) . . . . ? C4 C5 C6 C7 0.3(8) . . . . ? C5 C6 C7 C8 -0.4(8) . . . . ? C6 C7 C8 N3 0.8(7) . . . . ? C6 C7 C8 C1 -179.3(4) . . . . ? N2 C1 C8 N3 0.6(5) . . . . ? C2 C1 C8 N3 179.4(5) . . . . ? N2 C1 C8 C7 -179.2(4) . . . . ? C2 C1 C8 C7 -0.5(8) . . . . ? C5 C4 N3 C8 1.0(6) . . . . ? C5 C4 N3 Zn1 -174.0(3) . . . 2_666 ? C7 C8 N3 C4 -1.1(6) . . . . ? C1 C8 N3 C4 179.0(4) . . . . ? C7 C8 N3 Zn1 174.7(3) . . . 2_666 ? C1 C8 N3 Zn1 -5.1(4) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.461 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.073 #===END #===end