# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Dongwhan Lee.' 'Xuan Jiang.' 'Byung Gyu Park.' 'Maren Pink' 'Justin Riddle' 'Bong June Zhang.' _publ_contact_author_name 'Prof Dongwhan Lee' _publ_contact_author_email DONGWHAN@INDIANA.EDU _publ_section_title ; Torsionally Restricted Tetradentate Fluorophore: A Cross-Conjugated Platform for Ratiometric Sensing of Metal Ions ; # Attachment '4.cif' data_07117 _database_code_depnum_ccdc_archive 'CCDC 695503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 N4' _chemical_formula_sum 'C48 H38 N4' _chemical_formula_weight 670.82 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 19.8857(13) _cell_length_b 6.7009(4) _cell_length_c 27.6711(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3687.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 26.5 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9894 _exptl_absorpt_correction_T_max 0.9979 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 60 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART APEXII' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56364 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.40 _reflns_number_total 4268 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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^)+(0.0961P)^2^+0.2477P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 2(4) _refine_ls_number_reflns 4268 _refine_ls_number_parameters 501 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.061 _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 N1 N 0.19102(12) -0.7332(4) 0.26523(10) 0.0416(6) Uani 1 1 d . . . N2 N 0.30941(13) -0.5616(4) 0.17405(9) 0.0369(6) Uani 1 1 d . . . N3 N 0.45070(13) 1.0709(4) 0.44054(10) 0.0428(6) Uani 1 1 d . . . N4 N 0.57206(14) 1.2380(4) 0.34976(11) 0.0490(7) Uani 1 1 d . . . C1 C 0.14828(17) -0.8859(6) 0.27203(13) 0.0475(8) Uani 1 1 d . . . H1A H 0.1215 -0.8869 0.3005 0.057 Uiso 1 1 calc R . . C2 C 0.14121(15) -1.0425(5) 0.23951(13) 0.0409(7) Uani 1 1 d . . . H2A H 0.1100 -1.1471 0.2452 0.049 Uiso 1 1 calc R . . C3 C 0.18093(17) -1.0411(5) 0.19877(13) 0.0428(8) Uani 1 1 d . . . H3A H 0.1778 -1.1471 0.1761 0.051 Uiso 1 1 calc R . . C4 C 0.22513(15) -0.8867(4) 0.19084(11) 0.0348(6) Uani 1 1 d . . . H4A H 0.2527 -0.8844 0.1628 0.042 Uiso 1 1 calc R . . C5 C 0.22863(12) -0.7357(4) 0.22439(10) 0.0272(6) Uani 1 1 d . . . C6 C 0.27516(12) -0.5646(4) 0.21640(10) 0.0295(6) Uani 1 1 d . . . C7 C 0.28300(14) -0.4193(4) 0.25102(11) 0.0327(6) Uani 1 1 d . . . H7A H 0.2586 -0.4262 0.2805 0.039 Uiso 1 1 calc R . . C8 C 0.32692(15) -0.2626(5) 0.24242(11) 0.0375(7) Uani 1 1 d . . . H8A H 0.3330 -0.1612 0.2660 0.045 Uiso 1 1 calc R . . C9 C 0.36233(14) -0.2551(4) 0.19850(11) 0.0326(6) Uani 1 1 d . . . C10 C 0.35217(15) -0.4099(5) 0.16593(11) 0.0373(7) Uani 1 1 d . . . H10A H 0.3767 -0.4085 0.1364 0.045 Uiso 1 1 calc R . . C11 C 0.40709(14) -0.0933(4) 0.18844(10) 0.0323(6) Uani 1 1 d . . . C12 C 0.44330(14) 0.0480(4) 0.18169(10) 0.0306(6) Uani 1 1 d . . . C13 C 0.48278(12) 0.2248(4) 0.17909(10) 0.0263(5) Uani 1 1 d . . . C14 C 0.51865(13) 0.2777(4) 0.13755(10) 0.0274(5) Uani 1 1 d . . . H14A H 0.5181 0.1902 0.1105 0.033 Uiso 1 1 calc R . . C15 C 0.55537(13) 0.4561(4) 0.13458(10) 0.0289(6) Uani 1 1 d . A . C16 C 0.55747(14) 0.5776(4) 0.17542(11) 0.0325(6) Uani 1 1 d . . . H16A H 0.5833 0.6968 0.1748 0.039 Uiso 1 1 calc R . . C17 C 0.52239(13) 0.5270(4) 0.21700(10) 0.0317(6) Uani 1 1 d . . . H17A H 0.5249 0.6124 0.2443 0.038 Uiso 1 1 calc R . . C18 C 0.48362(12) 0.3547(4) 0.21970(9) 0.0278(6) Uani 1 1 d . . . C19 C 0.44250(13) 0.3088(4) 0.26024(10) 0.0304(6) Uani 1 1 d . . . C20 C 0.40262(13) 0.2647(4) 0.29143(10) 0.0305(6) Uani 1 1 d . . . C21 C 0.35696(13) 0.2177(4) 0.32665(10) 0.0301(6) Uani 1 1 d . . . C22 C 0.31668(14) 0.1764(4) 0.35800(10) 0.0308(6) Uani 1 1 d . . . C23 C 0.27441(12) 0.1474(4) 0.39913(9) 0.0264(6) Uani 1 1 d . . . C24 C 0.23300(13) -0.0199(5) 0.40458(10) 0.0322(6) Uani 1 1 d . . . H24A H 0.2306 -0.1161 0.3794 0.039 Uiso 1 1 calc R . . C25 C 0.19557(13) -0.0467(4) 0.44610(10) 0.0317(6) Uani 1 1 d . . . H25A H 0.1680 -0.1620 0.4489 0.038 Uiso 1 1 calc R . . C26 C 0.19704(12) 0.0908(4) 0.48408(9) 0.0284(6) Uani 1 1 d . B . C27 C 0.23690(12) 0.2598(4) 0.47843(10) 0.0283(6) Uani 1 1 d . . . H27A H 0.2379 0.3570 0.5034 0.034 Uiso 1 1 calc R . . C28 C 0.27569(12) 0.2903(4) 0.43672(9) 0.0260(5) Uani 1 1 d . . . C29 C 0.31744(13) 0.4626(4) 0.43169(11) 0.0306(6) Uani 1 1 d . . . C30 C 0.35436(14) 0.6009(4) 0.42485(10) 0.0329(6) Uani 1 1 d . . . C31 C 0.39975(14) 0.7628(4) 0.41578(12) 0.0334(6) Uani 1 1 d . . . C32 C 0.40734(16) 0.9199(4) 0.44824(12) 0.0389(7) Uani 1 1 d . . . H32A H 0.3810 0.9206 0.4769 0.047 Uiso 1 1 calc R . . C33 C 0.43835(15) 0.7672(5) 0.37306(13) 0.0410(7) Uani 1 1 d . . . H33A H 0.4343 0.6634 0.3498 0.049 Uiso 1 1 calc R . . C34 C 0.48165(14) 0.9224(4) 0.36540(12) 0.0350(7) Uani 1 1 d . . . H34A H 0.5080 0.9269 0.3368 0.042 Uiso 1 1 calc R . . C35 C 0.48707(13) 1.0715(4) 0.39904(11) 0.0318(6) Uani 1 1 d . . . C36 C 0.53432(13) 1.2409(4) 0.39110(11) 0.0304(6) Uani 1 1 d . . . C37 C 0.53870(15) 1.3893(4) 0.42494(12) 0.0355(7) Uani 1 1 d . . . H37A H 0.5118 1.3864 0.4533 0.043 Uiso 1 1 calc R . . C38 C 0.58308(17) 1.5424(5) 0.41674(14) 0.0473(8) Uani 1 1 d . . . H38A H 0.5870 1.6473 0.4397 0.057 Uiso 1 1 calc R . . C39 C 0.62213(16) 1.5454(5) 0.37549(14) 0.0491(9) Uani 1 1 d . . . H39A H 0.6533 1.6503 0.3698 0.059 Uiso 1 1 calc R . . C40 C 0.61477(17) 1.3928(6) 0.34289(14) 0.0530(9) Uani 1 1 d . . . H40A H 0.6409 1.3958 0.3141 0.064 Uiso 1 1 calc R . . C41 C 0.59068(14) 0.5134(4) 0.08682(10) 0.0326(6) Uani 1 1 d D . . C42 C 0.6114(3) 0.7321(6) 0.08466(17) 0.0665(15) Uani 0.856(5) 1 d PD A 1 H42A H 0.6486 0.7556 0.1072 0.100 Uiso 0.856(5) 1 calc PR A 1 H42B H 0.5731 0.8163 0.0936 0.100 Uiso 0.856(5) 1 calc PR A 1 H42C H 0.6260 0.7651 0.0518 0.100 Uiso 0.856(5) 1 calc PR A 1 C43 C 0.6528(2) 0.3802(8) 0.08000(17) 0.0608(15) Uani 0.856(5) 1 d PD A 1 H43A H 0.6744 0.4121 0.0491 0.091 Uiso 0.856(5) 1 calc PR A 1 H43B H 0.6390 0.2398 0.0801 0.091 Uiso 0.856(5) 1 calc PR A 1 H43C H 0.6846 0.4038 0.1064 0.091 Uiso 0.856(5) 1 calc PR A 1 C44 C 0.5433(2) 0.4798(7) 0.04381(13) 0.0463(10) Uani 0.856(5) 1 d PD A 1 H44A H 0.5674 0.5063 0.0136 0.069 Uiso 0.856(5) 1 calc PR A 1 H44B H 0.5047 0.5704 0.0464 0.069 Uiso 0.856(5) 1 calc PR A 1 H44C H 0.5274 0.3414 0.0440 0.069 Uiso 0.856(5) 1 calc PR A 1 C42D C 0.5658(12) 0.723(3) 0.0780(10) 0.0608(15) Uani 0.144(5) 1 d PD A 2 H42D H 0.5875 0.8144 0.1007 0.091 Uiso 0.144(5) 1 calc PR A 2 H42E H 0.5169 0.7273 0.0826 0.091 Uiso 0.144(5) 1 calc PR A 2 H42F H 0.5767 0.7627 0.0448 0.091 Uiso 0.144(5) 1 calc PR A 2 C43D C 0.6662(7) 0.511(4) 0.0992(8) 0.0463(10) Uani 0.144(5) 1 d PD A 2 H43D H 0.6754 0.4028 0.1221 0.069 Uiso 0.144(5) 1 calc PR A 2 H43E H 0.6788 0.6390 0.1138 0.069 Uiso 0.144(5) 1 calc PR A 2 H43F H 0.6924 0.4900 0.0697 0.069 Uiso 0.144(5) 1 calc PR A 2 C44D C 0.5758(16) 0.373(3) 0.0464(7) 0.0665(15) Uani 0.144(5) 1 d PD A 2 H44D H 0.6004 0.4148 0.0174 0.100 Uiso 0.144(5) 1 calc PR A 2 H44E H 0.5274 0.3734 0.0397 0.100 Uiso 0.144(5) 1 calc PR A 2 H44F H 0.5899 0.2378 0.0555 0.100 Uiso 0.144(5) 1 calc PR A 2 C45 C 0.15879(13) 0.0533(5) 0.53169(10) 0.0345(7) Uani 1 1 d D . . C46 C 0.1476(3) 0.2511(7) 0.56011(19) 0.0549(13) Uani 0.836(9) 1 d PD B 1 H46A H 0.1262 0.3496 0.5389 0.082 Uiso 0.836(9) 1 calc PR B 1 H46B H 0.1910 0.3026 0.5713 0.082 Uiso 0.836(9) 1 calc PR B 1 H46C H 0.1184 0.2255 0.5880 0.082 Uiso 0.836(9) 1 calc PR B 1 C47 C 0.2029(3) -0.0758(10) 0.56316(19) 0.0639(15) Uani 0.836(9) 1 d PD B 1 H47A H 0.1802 -0.1015 0.5939 0.096 Uiso 0.836(9) 1 calc PR B 1 H47B H 0.2456 -0.0071 0.5692 0.096 Uiso 0.836(9) 1 calc PR B 1 H47C H 0.2117 -0.2027 0.5467 0.096 Uiso 0.836(9) 1 calc PR B 1 C48 C 0.0899(2) -0.0361(11) 0.52346(17) 0.0641(18) Uani 0.836(9) 1 d PD B 1 H48A H 0.0944 -0.1619 0.5057 0.096 Uiso 0.836(9) 1 calc PR B 1 H48B H 0.0624 0.0571 0.5047 0.096 Uiso 0.836(9) 1 calc PR B 1 H48C H 0.0683 -0.0615 0.5547 0.096 Uiso 0.836(9) 1 calc PR B 1 C46D C 0.1143(14) 0.223(3) 0.5451(9) 0.0639(15) Uani 0.164(9) 1 d PD B 2 H46D H 0.0698 0.2038 0.5306 0.096 Uiso 0.164(9) 1 calc PR B 2 H46E H 0.1338 0.3481 0.5331 0.096 Uiso 0.164(9) 1 calc PR B 2 H46F H 0.1099 0.2295 0.5803 0.096 Uiso 0.164(9) 1 calc PR B 2 C47D C 0.2098(10) 0.017(5) 0.5715(8) 0.0641(18) Uani 0.164(9) 1 d PD B 2 H47D H 0.1869 -0.0373 0.6000 0.096 Uiso 0.164(9) 1 calc PR B 2 H47E H 0.2318 0.1428 0.5800 0.096 Uiso 0.164(9) 1 calc PR B 2 H47F H 0.2437 -0.0789 0.5603 0.096 Uiso 0.164(9) 1 calc PR B 2 C48D C 0.1167(14) -0.142(3) 0.5267(8) 0.0549(13) Uani 0.164(9) 1 d PD B 2 H48D H 0.0922 -0.1663 0.5568 0.082 Uiso 0.164(9) 1 calc PR B 2 H48E H 0.1468 -0.2541 0.5201 0.082 Uiso 0.164(9) 1 calc PR B 2 H48F H 0.0846 -0.1271 0.5000 0.082 Uiso 0.164(9) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0373(13) 0.0465(16) 0.0410(14) -0.0055(12) 0.0070(12) -0.0116(11) N2 0.0404(14) 0.0344(15) 0.0359(13) 0.0055(11) -0.0026(11) -0.0057(11) N3 0.0432(14) 0.0368(15) 0.0484(16) 0.0079(12) -0.0096(12) -0.0073(11) N4 0.0457(15) 0.0514(18) 0.0499(16) 0.0029(13) 0.0046(13) -0.0142(13) C1 0.0422(17) 0.054(2) 0.0458(18) -0.0005(15) 0.0067(14) -0.0187(15) C2 0.0358(15) 0.0349(17) 0.0519(18) 0.0082(14) -0.0075(14) -0.0104(13) C3 0.0498(18) 0.0335(17) 0.0451(18) -0.0045(13) -0.0118(15) -0.0121(14) C4 0.0404(16) 0.0288(15) 0.0352(15) -0.0008(11) 0.0029(12) -0.0026(12) C5 0.0239(13) 0.0261(13) 0.0317(14) 0.0017(10) -0.0046(10) 0.0012(10) C6 0.0230(12) 0.0264(14) 0.0390(15) 0.0053(11) -0.0018(11) 0.0027(10) C7 0.0317(13) 0.0266(14) 0.0398(16) 0.0021(12) 0.0064(12) -0.0007(11) C8 0.0396(16) 0.0320(16) 0.0409(17) 0.0029(12) 0.0075(13) -0.0006(12) C9 0.0284(13) 0.0291(15) 0.0402(16) 0.0069(11) -0.0033(12) -0.0014(11) C10 0.0383(15) 0.0371(17) 0.0367(16) 0.0056(12) 0.0014(13) -0.0032(13) C11 0.0342(14) 0.0298(15) 0.0330(15) 0.0032(11) 0.0010(12) 0.0025(12) C12 0.0337(14) 0.0289(14) 0.0293(14) 0.0030(11) 0.0017(11) 0.0048(11) C13 0.0236(12) 0.0268(14) 0.0285(13) 0.0046(10) -0.0002(10) 0.0030(10) C14 0.0289(13) 0.0266(13) 0.0267(12) -0.0007(10) 0.0042(10) 0.0013(10) C15 0.0221(12) 0.0341(14) 0.0304(14) 0.0018(11) -0.0003(10) -0.0020(10) C16 0.0304(14) 0.0322(15) 0.0351(14) -0.0027(12) 0.0004(11) -0.0087(11) C17 0.0333(14) 0.0343(15) 0.0274(14) -0.0041(11) 0.0000(11) -0.0011(12) C18 0.0219(12) 0.0340(15) 0.0276(13) 0.0029(11) 0.0000(10) 0.0020(11) C19 0.0278(13) 0.0372(15) 0.0262(13) 0.0010(11) 0.0005(11) 0.0019(11) C20 0.0279(13) 0.0372(15) 0.0264(13) 0.0000(11) -0.0007(11) 0.0009(11) C21 0.0285(13) 0.0343(15) 0.0275(13) -0.0002(11) 0.0013(11) 0.0017(11) C22 0.0281(13) 0.0343(15) 0.0301(14) 0.0001(12) 0.0007(11) 0.0033(11) C23 0.0232(12) 0.0280(14) 0.0282(13) 0.0039(10) 0.0019(10) 0.0028(10) C24 0.0316(14) 0.0326(15) 0.0325(14) -0.0075(11) 0.0036(12) -0.0047(11) C25 0.0250(13) 0.0326(15) 0.0375(15) 0.0029(12) -0.0009(11) -0.0081(10) C26 0.0212(12) 0.0386(16) 0.0255(13) 0.0032(11) -0.0015(10) -0.0034(11) C27 0.0235(12) 0.0339(14) 0.0274(13) -0.0022(11) -0.0017(10) -0.0022(10) C28 0.0202(12) 0.0277(13) 0.0300(13) 0.0045(11) -0.0011(10) -0.0009(9) C29 0.0299(13) 0.0299(14) 0.0319(14) 0.0000(11) 0.0027(11) -0.0028(11) C30 0.0283(13) 0.0332(15) 0.0373(15) 0.0058(12) 0.0017(11) -0.0029(12) C31 0.0287(13) 0.0239(14) 0.0475(17) 0.0103(12) -0.0005(12) -0.0011(10) C32 0.0407(16) 0.0323(16) 0.0436(17) 0.0058(13) -0.0093(14) -0.0029(13) C33 0.0354(15) 0.0329(16) 0.055(2) 0.0044(14) 0.0096(14) 0.0021(12) C34 0.0276(13) 0.0276(15) 0.0499(17) 0.0085(13) 0.0103(12) -0.0006(11) C35 0.0258(13) 0.0273(15) 0.0423(16) 0.0095(12) -0.0026(12) -0.0010(10) C36 0.0254(13) 0.0276(14) 0.0381(15) 0.0098(11) -0.0068(11) 0.0006(10) C37 0.0364(15) 0.0262(14) 0.0438(17) -0.0016(12) -0.0048(13) -0.0041(12) C38 0.0499(19) 0.0366(17) 0.055(2) -0.0017(15) -0.0144(16) -0.0081(15) C39 0.0396(17) 0.0439(19) 0.064(2) 0.0179(17) -0.0154(16) -0.0185(15) C40 0.0400(17) 0.066(2) 0.053(2) 0.0060(18) 0.0061(15) -0.0234(17) C41 0.0305(13) 0.0395(16) 0.0278(14) 0.0037(12) 0.0040(11) -0.0052(12) C42 0.107(4) 0.049(2) 0.044(2) 0.0079(19) 0.018(3) -0.032(3) C43 0.040(2) 0.089(4) 0.054(3) 0.031(3) 0.0207(19) 0.018(2) C44 0.048(2) 0.064(3) 0.0277(17) 0.0107(17) -0.0033(15) -0.0043(19) C42D 0.040(2) 0.089(4) 0.054(3) 0.031(3) 0.0207(19) 0.018(2) C43D 0.048(2) 0.064(3) 0.0277(17) 0.0107(17) -0.0033(15) -0.0043(19) C44D 0.107(4) 0.049(2) 0.044(2) 0.0079(19) 0.018(3) -0.032(3) C45 0.0277(14) 0.0501(18) 0.0257(13) 0.0041(12) 0.0026(11) -0.0086(12) C46 0.059(3) 0.064(3) 0.042(2) -0.0093(19) 0.026(2) -0.013(2) C47 0.069(3) 0.079(4) 0.043(3) 0.031(2) 0.004(2) 0.010(3) C48 0.041(2) 0.103(5) 0.048(2) -0.027(3) 0.019(2) -0.035(3) C46D 0.069(3) 0.079(4) 0.043(3) 0.031(2) 0.004(2) 0.010(3) C47D 0.041(2) 0.103(5) 0.048(2) -0.027(3) 0.019(2) -0.035(3) C48D 0.059(3) 0.064(3) 0.042(2) -0.0093(19) 0.026(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.343(4) . ? N1 C5 1.355(4) . ? N2 C10 1.344(4) . ? N2 C6 1.356(4) . ? N3 C32 1.346(4) . ? N3 C35 1.357(4) . ? N4 C40 1.354(4) . ? N4 C36 1.368(4) . ? C1 C2 1.389(5) . ? C1 H1A 0.9500 . ? C2 C3 1.377(5) . ? C2 H2A 0.9500 . ? C3 C4 1.376(4) . ? C3 H3A 0.9500 . ? C4 C5 1.375(4) . ? C4 H4A 0.9500 . ? C5 C6 1.490(4) . ? C6 C7 1.375(4) . ? C7 C8 1.386(4) . ? C7 H7A 0.9500 . ? C8 C9 1.406(4) . ? C8 H8A 0.9500 . ? C9 C10 1.389(5) . ? C9 C11 1.430(4) . ? C10 H10A 0.9500 . ? C11 C12 1.204(4) . ? C12 C13 1.423(4) . ? C13 C14 1.398(4) . ? C13 C18 1.422(4) . ? C14 C15 1.403(4) . ? C14 H14A 0.9500 . ? C15 C16 1.393(4) . ? C15 C41 1.545(4) . ? C16 C17 1.387(4) . ? C16 H16A 0.9500 . ? C17 C18 1.390(4) . ? C17 H17A 0.9500 . ? C18 C19 1.422(4) . ? C19 C20 1.209(4) . ? C20 C21 1.369(3) . ? C21 C22 1.213(4) . ? C22 C23 1.428(4) . ? C23 C24 1.399(4) . ? C23 C28 1.414(4) . ? C24 C25 1.381(4) . ? C24 H24A 0.9500 . ? C25 C26 1.398(4) . ? C25 H25A 0.9500 . ? C26 C27 1.391(4) . ? C26 C45 1.542(4) . ? C27 C28 1.403(3) . ? C27 H27A 0.9500 . ? C28 C29 1.429(4) . ? C29 C30 1.198(4) . ? C30 C31 1.433(4) . ? C31 C32 1.392(4) . ? C31 C33 1.410(4) . ? C32 H32A 0.9500 . ? C33 C34 1.367(4) . ? C33 H33A 0.9500 . ? C34 C35 1.370(4) . ? C34 H34A 0.9500 . ? C35 C36 1.490(4) . ? C36 C37 1.369(4) . ? C37 C38 1.372(4) . ? C37 H37A 0.9500 . ? C38 C39 1.380(5) . ? C38 H38A 0.9500 . ? C39 C40 1.371(5) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C44D 1.492(14) . ? C41 C42D 1.508(14) . ? C41 C42 1.524(5) . ? C41 C43 1.535(5) . ? C41 C44 1.535(4) . ? C41 C43D 1.540(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C42D H42D 0.9800 . ? C42D H42E 0.9800 . ? C42D H42F 0.9800 . ? C43D H43D 0.9800 . ? C43D H43E 0.9800 . ? C43D H43F 0.9800 . ? C44D H44D 0.9800 . ? C44D H44E 0.9800 . ? C44D H44F 0.9800 . ? C45 C46D 1.489(14) . ? C45 C47 1.509(5) . ? C45 C48 1.512(5) . ? C45 C47D 1.519(14) . ? C45 C48D 1.558(13) . ? C45 C46 1.557(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C46D H46D 0.9800 . ? C46D H46E 0.9800 . ? C46D H46F 0.9800 . ? C47D H47D 0.9800 . ? C47D H47E 0.9800 . ? C47D H47F 0.9800 . ? C48D H48D 0.9800 . ? C48D H48E 0.9800 . ? C48D H48F 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 C1 N1 C5 117.2(3) . . ? C10 N2 C6 118.3(3) . . ? C32 N3 C35 118.5(3) . . ? C40 N4 C36 116.8(3) . . ? N1 C1 C2 123.3(3) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 117.9(3) . . ? C3 C2 H2A 121.1 . . ? C1 C2 H2A 121.1 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 123.0(2) . . ? N1 C5 C6 117.2(2) . . ? C4 C5 C6 119.8(2) . . ? N2 C6 C7 122.3(2) . . ? N2 C6 C5 116.9(2) . . ? C7 C6 C5 120.8(2) . . ? C6 C7 C8 119.2(3) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C7 C8 C9 119.4(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C10 C9 C8 117.5(3) . . ? C10 C9 C11 122.0(3) . . ? C8 C9 C11 120.5(3) . . ? N2 C10 C9 123.2(3) . . ? N2 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? C12 C11 C9 176.9(3) . . ? C11 C12 C13 172.9(3) . . ? C14 C13 C18 119.3(2) . . ? C14 C13 C12 122.3(2) . . ? C18 C13 C12 118.4(2) . . ? C13 C14 C15 122.0(2) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C16 C15 C14 117.8(2) . . ? C16 C15 C41 122.3(2) . . ? C14 C15 C41 119.9(2) . . ? C17 C16 C15 121.0(3) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 121.7(3) . . ? C16 C17 H17A 119.1 . . ? C18 C17 H17A 119.1 . . ? C17 C18 C13 118.2(2) . . ? C17 C18 C19 122.7(3) . . ? C13 C18 C19 119.0(2) . . ? C20 C19 C18 173.5(3) . . ? C19 C20 C21 179.0(3) . . ? C22 C21 C20 179.7(3) . . ? C21 C22 C23 171.8(3) . . ? C24 C23 C28 118.3(2) . . ? C24 C23 C22 122.8(3) . . ? C28 C23 C22 118.9(2) . . ? C25 C24 C23 120.8(3) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 121.9(2) . . ? C24 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C27 C26 C25 117.7(2) . . ? C27 C26 C45 120.7(2) . . ? C25 C26 C45 121.6(2) . . ? C26 C27 C28 121.6(2) . . ? C26 C27 H27A 119.2 . . ? C28 C27 H27A 119.2 . . ? C27 C28 C23 119.8(2) . . ? C27 C28 C29 121.1(2) . . ? C23 C28 C29 119.1(2) . . ? C30 C29 C28 175.6(3) . . ? C29 C30 C31 178.3(3) . . ? C32 C31 C33 117.8(3) . . ? C32 C31 C30 121.9(3) . . ? C33 C31 C30 120.4(3) . . ? N3 C32 C31 122.4(3) . . ? N3 C32 H32A 118.8 . . ? C31 C32 H32A 118.8 . . ? C34 C33 C31 119.3(3) . . ? C34 C33 H33A 120.4 . . ? C31 C33 H33A 120.4 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? N3 C35 C34 122.1(3) . . ? N3 C35 C36 117.6(3) . . ? C34 C35 C36 120.3(3) . . ? N4 C36 C37 123.2(3) . . ? N4 C36 C35 117.3(3) . . ? C37 C36 C35 119.5(3) . . ? C36 C37 C38 118.1(3) . . ? C36 C37 H37A 120.9 . . ? C38 C37 H37A 120.9 . . ? C37 C38 C39 120.6(3) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C40 C39 C38 118.2(3) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? N4 C40 C39 123.1(3) . . ? N4 C40 H40A 118.5 . . ? C39 C40 H40A 118.5 . . ? C44D C41 C42D 113.6(14) . . ? C44D C41 C42 129.2(10) . . ? C42D C41 C42 35.7(10) . . ? C44D C41 C43 72.5(13) . . ? C42D C41 C43 141.7(10) . . ? C42 C41 C43 109.7(4) . . ? C44D C41 C44 37.3(12) . . ? C42D C41 C44 79.0(11) . . ? C42 C41 C44 106.1(3) . . ? C43 C41 C44 108.3(3) . . ? C44D C41 C43D 110.7(14) . . ? C42D C41 C43D 111.5(13) . . ? C42 C41 C43D 75.8(10) . . ? C43 C41 C43D 40.3(10) . . ? C44 C41 C43D 140.4(9) . . ? C44D C41 C15 113.2(10) . . ? C42D C41 C15 102.8(10) . . ? C42 C41 C15 113.3(3) . . ? C43 C41 C15 109.1(2) . . ? C44 C41 C15 110.3(2) . . ? C43D C41 C15 104.5(9) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? C41 C42D H42D 109.5 . . ? C41 C42D H42E 109.5 . . ? H42D C42D H42E 109.5 . . ? C41 C42D H42F 109.5 . . ? H42D C42D H42F 109.5 . . ? H42E C42D H42F 109.5 . . ? C41 C43D H43D 109.5 . . ? C41 C43D H43E 109.5 . . ? H43D C43D H43E 109.5 . . ? C41 C43D H43F 109.5 . . ? H43D C43D H43F 109.5 . . ? H43E C43D H43F 109.5 . . ? C41 C44D H44D 109.5 . . ? C41 C44D H44E 109.5 . . ? H44D C44D H44E 109.5 . . ? C41 C44D H44F 109.5 . . ? H44D C44D H44F 109.5 . . ? H44E C44D H44F 109.5 . . ? C46D C45 C47 129.8(10) . . ? C46D C45 C48 78.6(12) . . ? C47 C45 C48 112.8(4) . . ? C46D C45 C47D 109.9(12) . . ? C47 C45 C47D 25.8(10) . . ? C48 C45 C47D 130.6(11) . . ? C46D C45 C26 112.4(9) . . ? C47 C45 C26 107.4(3) . . ? C48 C45 C26 112.5(3) . . ? C47D C45 C26 108.5(10) . . ? C46D C45 C48D 110.1(12) . . ? C47 C45 C48D 83.3(11) . . ? C48 C45 C48D 33.6(11) . . ? C47D C45 C48D 106.8(12) . . ? C26 C45 C48D 109.0(9) . . ? C46D C45 C46 30.5(12) . . ? C47 C45 C46 106.2(4) . . ? C48 C45 C46 106.5(3) . . ? C47D C45 C46 82.3(11) . . ? C26 C45 C46 111.3(3) . . ? C48D C45 C46 133.0(10) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? C45 C46D H46D 109.5 . . ? C45 C46D H46E 109.5 . . ? H46D C46D H46E 109.5 . . ? C45 C46D H46F 109.5 . . ? H46D C46D H46F 109.5 . . ? H46E C46D H46F 109.5 . . ? C45 C47D H47D 109.5 . . ? C45 C47D H47E 109.5 . . ? H47D C47D H47E 109.5 . . ? C45 C47D H47F 109.5 . . ? H47D C47D H47F 109.5 . . ? H47E C47D H47F 109.5 . . ? C45 C48D H48D 109.5 . . ? C45 C48D H48E 109.5 . . ? H48D C48D H48E 109.5 . . ? C45 C48D H48F 109.5 . . ? H48D C48D H48F 109.5 . . ? H48E C48D H48F 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 C5 N1 C1 C2 -0.1(5) . . . . ? N1 C1 C2 C3 1.0(5) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C1 N1 C5 C4 -0.8(4) . . . . ? C1 N1 C5 C6 179.0(3) . . . . ? C3 C4 C5 N1 0.8(4) . . . . ? C3 C4 C5 C6 -179.0(3) . . . . ? C10 N2 C6 C7 -0.3(4) . . . . ? C10 N2 C6 C5 -179.5(2) . . . . ? N1 C5 C6 N2 -175.9(2) . . . . ? C4 C5 C6 N2 3.9(4) . . . . ? N1 C5 C6 C7 4.9(4) . . . . ? C4 C5 C6 C7 -175.4(3) . . . . ? N2 C6 C7 C8 0.6(4) . . . . ? C5 C6 C7 C8 179.8(2) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? C7 C8 C9 C10 -1.2(4) . . . . ? C7 C8 C9 C11 179.0(3) . . . . ? C6 N2 C10 C9 -0.8(4) . . . . ? C8 C9 C10 N2 1.6(4) . . . . ? C11 C9 C10 N2 -178.6(3) . . . . ? C10 C9 C11 C12 162(6) . . . . ? C8 C9 C11 C12 -18(6) . . . . ? C9 C11 C12 C13 11(8) . . . . ? C11 C12 C13 C14 -168(2) . . . . ? C11 C12 C13 C18 9(2) . . . . ? C18 C13 C14 C15 -0.3(4) . . . . ? C12 C13 C14 C15 177.5(3) . . . . ? C13 C14 C15 C16 2.6(4) . . . . ? C13 C14 C15 C41 -176.4(2) . . . . ? C14 C15 C16 C17 -2.3(4) . . . . ? C41 C15 C16 C17 176.6(2) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C13 2.6(4) . . . . ? C16 C17 C18 C19 -174.2(3) . . . . ? C14 C13 C18 C17 -2.3(4) . . . . ? C12 C13 C18 C17 179.9(2) . . . . ? C14 C13 C18 C19 174.6(2) . . . . ? C12 C13 C18 C19 -3.2(4) . . . . ? C17 C18 C19 C20 135(3) . . . . ? C13 C18 C19 C20 -41(3) . . . . ? C18 C19 C20 C21 -81(18) . . . . ? C19 C20 C21 C22 -96(100) . . . . ? C20 C21 C22 C23 24(100) . . . . ? C21 C22 C23 C24 -160.9(19) . . . . ? C21 C22 C23 C28 17(2) . . . . ? C28 C23 C24 C25 -1.5(4) . . . . ? C22 C23 C24 C25 176.6(3) . . . . ? C23 C24 C25 C26 0.3(4) . . . . ? C24 C25 C26 C27 1.2(4) . . . . ? C24 C25 C26 C45 -175.9(3) . . . . ? C25 C26 C27 C28 -1.5(4) . . . . ? C45 C26 C27 C28 175.6(2) . . . . ? C26 C27 C28 C23 0.3(4) . . . . ? C26 C27 C28 C29 -178.8(2) . . . . ? C24 C23 C28 C27 1.1(4) . . . . ? C22 C23 C28 C27 -177.0(2) . . . . ? C24 C23 C28 C29 -179.7(2) . . . . ? C22 C23 C28 C29 2.1(4) . . . . ? C27 C28 C29 C30 168(4) . . . . ? C23 C28 C29 C30 -11(4) . . . . ? C28 C29 C30 C31 -17(15) . . . . ? C29 C30 C31 C32 -154(12) . . . . ? C29 C30 C31 C33 26(12) . . . . ? C35 N3 C32 C31 1.5(4) . . . . ? C33 C31 C32 N3 -1.3(4) . . . . ? C30 C31 C32 N3 178.8(3) . . . . ? C32 C31 C33 C34 0.6(4) . . . . ? C30 C31 C33 C34 -179.5(3) . . . . ? C31 C33 C34 C35 -0.1(4) . . . . ? C32 N3 C35 C34 -1.0(4) . . . . ? C32 N3 C35 C36 179.5(2) . . . . ? C33 C34 C35 N3 0.2(4) . . . . ? C33 C34 C35 C36 179.8(3) . . . . ? C40 N4 C36 C37 -0.7(4) . . . . ? C40 N4 C36 C35 179.9(3) . . . . ? N3 C35 C36 N4 178.4(3) . . . . ? C34 C35 C36 N4 -1.1(4) . . . . ? N3 C35 C36 C37 -1.0(4) . . . . ? C34 C35 C36 C37 179.5(3) . . . . ? N4 C36 C37 C38 0.2(4) . . . . ? C35 C36 C37 C38 179.5(3) . . . . ? C36 C37 C38 C39 -0.1(5) . . . . ? C37 C38 C39 C40 0.7(5) . . . . ? C36 N4 C40 C39 1.3(5) . . . . ? C38 C39 C40 N4 -1.3(6) . . . . ? C16 C15 C41 C44D -173.8(14) . . . . ? C14 C15 C41 C44D 5.1(15) . . . . ? C16 C15 C41 C42D -50.9(12) . . . . ? C14 C15 C41 C42D 128.0(12) . . . . ? C16 C15 C41 C42 -14.9(4) . . . . ? C14 C15 C41 C42 164.0(4) . . . . ? C16 C15 C41 C43 107.5(4) . . . . ? C14 C15 C41 C43 -73.6(4) . . . . ? C16 C15 C41 C44 -133.7(3) . . . . ? C14 C15 C41 C44 45.3(4) . . . . ? C16 C15 C41 C43D 65.6(11) . . . . ? C14 C15 C41 C43D -115.5(11) . . . . ? C27 C26 C45 C46D 55.5(14) . . . . ? C25 C26 C45 C46D -127.5(14) . . . . ? C27 C26 C45 C47 -93.3(4) . . . . ? C25 C26 C45 C47 83.7(4) . . . . ? C27 C26 C45 C48 142.0(4) . . . . ? C25 C26 C45 C48 -41.0(5) . . . . ? C27 C26 C45 C47D -66.2(13) . . . . ? C25 C26 C45 C47D 110.8(12) . . . . ? C27 C26 C45 C48D 177.9(13) . . . . ? C25 C26 C45 C48D -5.1(13) . . . . ? C27 C26 C45 C46 22.6(4) . . . . ? C25 C26 C45 C46 -160.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.285 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.049 # start Validation Reply Form #_vrf_STRVA01_07117 #; #PROBLEM: Chirality of atom sites is inverted? #RESPONSE: Light atom structure. Flack is meaningless. #; #_vrf_PLAT032_07117 #; #PROBLEM: Std. Uncertainty in Flack Parameter too High #RESPONSE: Light atom structure. Flack is meaningless. #; #_vrf_PLAT242_07117 #; #PROBLEM: Check Low Ueq as Compared to Neighbors for C41 C45 #RESPONSE: T-butyl groups disordered over two sites with very minor second #sites. #; # Attachment '4_zn.cif' data_07124 _database_code_depnum_ccdc_archive 'CCDC 695504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H37 F6 N4 O6 S2 Zn' _chemical_formula_sum 'C50 H38 F6 N4 O6 S2 Zn' _chemical_formula_weight 1034.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 59.348(3) _cell_length_b 9.9017(6) _cell_length_c 19.2658(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.291(2) _cell_angle_gamma 90.00 _cell_volume 11062.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4317 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 24.1 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8819 _exptl_absorpt_correction_T_max 0.9713 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 60 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35934 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -70 _diffrn_reflns_limit_h_max 70 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.04 _reflns_number_total 9700 _reflns_number_gt 5347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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^)+(0.1249P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9700 _refine_ls_number_parameters 697 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2058 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.963 _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 0.572277(9) 1.01799(6) 0.73099(4) 0.0567(2) Uani 1 1 d D . . N1 N 0.55136(7) 1.0102(4) 0.8053(3) 0.0586(12) Uani 1 1 d . B . N2 N 0.59102(8) 0.8798(5) 0.8097(3) 0.0672(14) Uani 1 1 d . B . N3 N 0.59371(6) 0.9951(4) 0.6575(3) 0.0539(12) Uani 1 1 d . B . N4 N 0.55296(6) 0.8830(4) 0.6544(3) 0.0594(13) Uani 1 1 d . B . C1 C 0.53142(8) 1.0773(5) 0.7998(3) 0.0551(14) Uani 1 1 d . . . H1 H 0.5260 1.1307 0.7587 0.066 Uiso 1 1 calc R B . C2 C 0.51867(8) 1.0720(6) 0.8510(3) 0.0592(15) Uani 1 1 d . B . H2 H 0.5046 1.1203 0.8453 0.071 Uiso 1 1 calc R . . C3 C 0.52647(9) 0.9963(5) 0.9105(3) 0.0575(15) Uani 1 1 d . . . H3 H 0.5179 0.9910 0.9467 0.069 Uiso 1 1 calc R B . C4 C 0.54720(9) 0.9270(5) 0.9173(3) 0.0595(15) Uani 1 1 d . B . H4 H 0.5529 0.8737 0.9582 0.071 Uiso 1 1 calc R . . C5 C 0.55928(9) 0.9367(5) 0.8643(3) 0.0597(15) Uani 1 1 d . . . C6 C 0.58167(9) 0.8680(5) 0.8680(3) 0.0658(17) Uani 1 1 d . B . C7 C 0.59298(10) 0.7969(6) 0.9273(4) 0.0747(19) Uani 1 1 d . . . H7 H 0.5867 0.7925 0.9687 0.090 Uiso 1 1 calc R B . C8 C 0.61368(11) 0.7317(6) 0.9250(4) 0.077(2) Uani 1 1 d . B . H8 H 0.6216 0.6825 0.9652 0.092 Uiso 1 1 calc R . . C9 C 0.62275(10) 0.7383(6) 0.8649(3) 0.0652(17) Uani 1 1 d . . . C10 C 0.61081(9) 0.8162(6) 0.8085(3) 0.0615(16) Uani 1 1 d . B . H10 H 0.6171 0.8245 0.7672 0.074 Uiso 1 1 calc R . . C11 C 0.64281(9) 0.6629(5) 0.8586(3) 0.0546(14) Uani 1 1 d . B . C12 C 0.65786(8) 0.5873(5) 0.8526(3) 0.0449(12) Uani 1 1 d . . . C13 C 0.67386(7) 0.4802(5) 0.8448(2) 0.0399(11) Uani 1 1 d . B . C14 C 0.67032(7) 0.3526(4) 0.8729(2) 0.0354(10) Uani 1 1 d . . . H14 H 0.6579 0.3413 0.8966 0.042 Uiso 1 1 calc R B . C15 C 0.68421(7) 0.2439(5) 0.8674(2) 0.0387(10) Uani 1 1 d . A . C16 C 0.70175(8) 0.2628(5) 0.8307(3) 0.0457(12) Uani 1 1 d . . . H16 H 0.7112 0.1885 0.8245 0.055 Uiso 1 1 calc R B . C17 C 0.70572(8) 0.3876(5) 0.8029(3) 0.0450(12) Uani 1 1 d . B . H17 H 0.7180 0.3975 0.7788 0.054 Uiso 1 1 calc R . . C18 C 0.69201(7) 0.4985(5) 0.8097(2) 0.0392(11) Uani 1 1 d . . . C19 C 0.69633(8) 0.6252(5) 0.7803(3) 0.0454(12) Uani 1 1 d . B . C20 C 0.70110(8) 0.7298(5) 0.7549(3) 0.0467(12) Uani 1 1 d . . . C21 C 0.70586(8) 0.8489(5) 0.7239(3) 0.0492(12) Uani 1 1 d . B . C22 C 0.70965(8) 0.9539(5) 0.6970(3) 0.0490(13) Uani 1 1 d . . . C23 C 0.71347(8) 1.0812(5) 0.6670(3) 0.0447(12) Uani 1 1 d . B . C24 C 0.73527(8) 1.1306(5) 0.6670(3) 0.0530(13) Uani 1 1 d . . . H24 H 0.7484 1.0785 0.6881 0.064 Uiso 1 1 calc R B . C25 C 0.73845(8) 1.2549(6) 0.6367(3) 0.0526(13) Uani 1 1 d . B . H25 H 0.7537 1.2855 0.6372 0.063 Uiso 1 1 calc R . . C26 C 0.71961(7) 1.3356(5) 0.6056(3) 0.0463(12) Uani 1 1 d . . . C27 C 0.69771(8) 1.2845(5) 0.6051(3) 0.0484(12) Uani 1 1 d . B . H27 H 0.6846 1.3366 0.5840 0.058 Uiso 1 1 calc R . . C28 C 0.69438(8) 1.1595(5) 0.6347(3) 0.0464(12) Uani 1 1 d . . . C29 C 0.67129(8) 1.1140(5) 0.6314(3) 0.0507(13) Uani 1 1 d . B . C30 C 0.65160(9) 1.0781(5) 0.6260(3) 0.0593(15) Uani 1 1 d . . . C31 C 0.62865(8) 1.0267(5) 0.6151(3) 0.0576(15) Uani 1 1 d . B . C32 C 0.61514(8) 1.0488(5) 0.6653(3) 0.0553(14) Uani 1 1 d . . . H32 H 0.6211 1.1028 0.7059 0.066 Uiso 1 1 calc R B . C33 C 0.61912(10) 0.9539(6) 0.5551(4) 0.0745(19) Uani 1 1 d . . . H33 H 0.6277 0.9400 0.5192 0.089 Uiso 1 1 calc R B . C34 C 0.59714(9) 0.9009(6) 0.5467(4) 0.0736(18) Uani 1 1 d . B . H34 H 0.5904 0.8520 0.5050 0.088 Uiso 1 1 calc R . . C35 C 0.58500(9) 0.9199(5) 0.5998(4) 0.0584(15) Uani 1 1 d . . . C36 C 0.56203(8) 0.8611(5) 0.5958(4) 0.0591(16) Uani 1 1 d . B . C37 C 0.55023(9) 0.7914(5) 0.5378(4) 0.0609(16) Uani 1 1 d . . . H37 H 0.5572 0.7756 0.4985 0.073 Uiso 1 1 calc R B . C38 C 0.52832(9) 0.7443(6) 0.5364(4) 0.0632(16) Uani 1 1 d . B . H38 H 0.5199 0.6973 0.4961 0.076 Uiso 1 1 calc R . . C39 C 0.51879(9) 0.7670(6) 0.5950(4) 0.0661(17) Uani 1 1 d . . . H39 H 0.5037 0.7358 0.5957 0.079 Uiso 1 1 calc R B . C40 C 0.53148(9) 0.8352(5) 0.6521(4) 0.0627(16) Uani 1 1 d . B . H40 H 0.5248 0.8497 0.6921 0.075 Uiso 1 1 calc R . . C41 C 0.67951(7) 0.1056(5) 0.8956(3) 0.0476(12) Uani 1 1 d D . . C42 C 0.7015(3) 0.065(3) 0.9526(12) 0.084(4) Uani 0.295(11) 1 d PD A 1 H42A H 0.7035 0.1285 0.9927 0.126 Uiso 0.295(11) 1 calc PR A 1 H42B H 0.7151 0.0690 0.9313 0.126 Uiso 0.295(11) 1 calc PR A 1 H42C H 0.6997 -0.0265 0.9696 0.126 Uiso 0.295(11) 1 calc PR A 1 C43 C 0.6739(5) -0.005(2) 0.8410(12) 0.075(3) Uani 0.295(11) 1 d PD A 1 H43A H 0.6725 -0.0910 0.8649 0.113 Uiso 0.295(11) 1 calc PR A 1 H43B H 0.6863 -0.0115 0.8147 0.113 Uiso 0.295(11) 1 calc PR A 1 H43C H 0.6594 0.0158 0.8080 0.113 Uiso 0.295(11) 1 calc PR A 1 C44 C 0.6602(3) 0.108(3) 0.9376(12) 0.054(2) Uani 0.295(11) 1 d PD A 1 H44A H 0.6596 0.0206 0.9609 0.082 Uiso 0.295(11) 1 calc PR A 1 H44B H 0.6454 0.1255 0.9050 0.082 Uiso 0.295(11) 1 calc PR A 1 H44C H 0.6633 0.1796 0.9735 0.082 Uiso 0.295(11) 1 calc PR A 1 C42D C 0.70066(15) 0.0133(10) 0.9071(7) 0.084(4) Uani 0.705(11) 1 d PD A 2 H42D H 0.7134 0.0554 0.9410 0.126 Uiso 0.705(11) 1 calc PR A 2 H42E H 0.7053 -0.0007 0.8617 0.126 Uiso 0.705(11) 1 calc PR A 2 H42F H 0.6969 -0.0739 0.9257 0.126 Uiso 0.705(11) 1 calc PR A 2 C43D C 0.66089(19) 0.0388(10) 0.8350(5) 0.075(3) Uani 0.705(11) 1 d PD A 2 H43D H 0.6580 -0.0541 0.8484 0.113 Uiso 0.705(11) 1 calc PR A 2 H43E H 0.6665 0.0382 0.7908 0.113 Uiso 0.705(11) 1 calc PR A 2 H43F H 0.6465 0.0908 0.8282 0.113 Uiso 0.705(11) 1 calc PR A 2 C44D C 0.66984(17) 0.1136(11) 0.9613(4) 0.054(2) Uani 0.705(11) 1 d PD A 2 H44D H 0.6806 0.1634 0.9982 0.082 Uiso 0.705(11) 1 calc PR A 2 H44E H 0.6677 0.0222 0.9782 0.082 Uiso 0.705(11) 1 calc PR A 2 H44F H 0.6550 0.1605 0.9503 0.082 Uiso 0.705(11) 1 calc PR A 2 C45 C 0.72342(9) 1.4713(6) 0.5728(3) 0.0557(14) Uani 1 1 d . B . C46 C 0.70085(11) 1.5476(7) 0.5489(4) 0.088(2) Uani 1 1 d . . . H46A H 0.6904 1.4945 0.5129 0.132 Uiso 1 1 calc R B . H46B H 0.7039 1.6348 0.5287 0.132 Uiso 1 1 calc R . . H46C H 0.6938 1.5625 0.5898 0.132 Uiso 1 1 calc R . . C47 C 0.73457(12) 1.4448(7) 0.5089(3) 0.080(2) Uani 1 1 d . . . H47A H 0.7499 1.4054 0.5256 0.120 Uiso 1 1 calc R B . H47B H 0.7360 1.5301 0.4844 0.120 Uiso 1 1 calc R . . H47C H 0.7249 1.3820 0.4761 0.120 Uiso 1 1 calc R . . C48 C 0.73919(10) 1.5590(6) 0.6278(3) 0.0641(15) Uani 1 1 d . . . H48A H 0.7320 1.5741 0.6684 0.096 Uiso 1 1 calc R B . H48B H 0.7417 1.6460 0.6064 0.096 Uiso 1 1 calc R . . H48C H 0.7540 1.5133 0.6439 0.096 Uiso 1 1 calc R . . S1 S 0.59587(5) 1.2715(3) 0.85206(15) 0.0422(6) Uani 0.532(3) 1 d PD B 1 O1 O 0.59156(9) 1.2059(5) 0.7831(2) 0.0364(13) Uani 0.532(3) 1 d PD B 1 O2 O 0.59142(11) 1.1903(5) 0.9092(3) 0.080(3) Uani 0.532(3) 1 d PD B 1 O3 O 0.61675(7) 1.3493(6) 0.8672(3) 0.065(2) Uani 0.532(3) 1 d PD B 1 C49 C 0.57330(8) 1.3986(5) 0.8408(3) 0.053(3) Uani 0.532(3) 1 d PD B 1 F1 F 0.57417(8) 1.4642(5) 0.9018(2) 0.081(2) Uani 0.532(3) 1 d PD B 1 F2 F 0.57647(9) 1.4916(5) 0.7931(3) 0.0711(14) Uani 0.532(3) 1 d PD B 1 F3 F 0.55257(5) 1.3479(5) 0.8196(3) 0.078(2) Uani 0.532(3) 1 d PD B 1 S1D S 0.59453(5) 1.2341(3) 0.84110(17) 0.0422(6) Uani 0.468(3) 1 d PD B 2 O1D O 0.59356(11) 1.1528(4) 0.7778(3) 0.0364(13) Uani 0.468(3) 1 d PD B 2 O2D O 0.57359(7) 1.2397(5) 0.8667(3) 0.0411(17) Uani 0.468(3) 1 d PD B 2 O3D O 0.61533(8) 1.2159(6) 0.8940(3) 0.067(3) Uani 0.468(3) 1 d PD B 2 C49D C 0.59723(8) 1.4045(5) 0.8087(3) 0.059(3) Uani 0.468(3) 1 d PD B 2 F1D F 0.59755(12) 1.4935(4) 0.8608(3) 0.098(3) Uani 0.468(3) 1 d PD B 2 F2D F 0.57891(9) 1.4355(5) 0.7573(3) 0.0711(14) Uani 0.468(3) 1 d PD B 2 F3D F 0.61583(8) 1.4214(5) 0.7832(3) 0.071(2) Uani 0.468(3) 1 d PD B 2 S2 S 0.54421(2) 1.21387(12) 0.59977(8) 0.0529(4) Uani 1 1 d D . . O4 O 0.55035(5) 1.1784(3) 0.67458(15) 0.0570(9) Uani 1 1 d D B . O5 O 0.52541(5) 1.1389(3) 0.55845(17) 0.0591(10) Uani 1 1 d D B . O6 O 0.56376(5) 1.2335(4) 0.56800(18) 0.0659(11) Uani 1 1 d D B . C50 C 0.53235(7) 1.3827(5) 0.6018(3) 0.079(2) Uani 1 1 d D B . F4 F 0.52507(7) 1.4288(3) 0.5358(2) 0.1200(17) Uani 1 1 d D . . F5 F 0.51384(6) 1.3802(4) 0.6315(3) 0.1262(18) Uani 1 1 d D . . F6 F 0.54717(5) 1.4690(3) 0.63731(19) 0.0828(11) Uani 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 0.0393(3) 0.0443(4) 0.0965(5) 0.0287(3) 0.0367(3) 0.0118(3) N1 0.047(2) 0.035(2) 0.105(4) 0.013(2) 0.042(2) 0.005(2) N2 0.063(3) 0.053(3) 0.105(4) 0.038(3) 0.062(3) 0.022(2) N3 0.033(2) 0.041(3) 0.094(3) 0.028(3) 0.029(2) 0.0062(19) N4 0.038(2) 0.030(2) 0.120(4) 0.015(2) 0.038(2) 0.0056(18) C1 0.034(2) 0.038(3) 0.100(4) -0.001(3) 0.029(3) 0.004(2) C2 0.035(3) 0.039(3) 0.109(5) -0.014(3) 0.026(3) -0.003(2) C3 0.049(3) 0.036(3) 0.099(4) -0.016(3) 0.044(3) -0.005(2) C4 0.057(3) 0.035(3) 0.101(4) 0.003(3) 0.050(3) 0.001(2) C5 0.058(3) 0.030(3) 0.107(4) 0.019(3) 0.053(3) 0.008(2) C6 0.065(3) 0.040(3) 0.110(5) 0.035(3) 0.058(3) 0.018(3) C7 0.083(4) 0.057(4) 0.105(5) 0.040(4) 0.066(4) 0.033(3) C8 0.085(4) 0.054(4) 0.112(5) 0.045(4) 0.066(4) 0.033(3) C9 0.069(3) 0.043(3) 0.100(4) 0.032(3) 0.054(3) 0.025(3) C10 0.061(3) 0.051(3) 0.086(4) 0.034(3) 0.044(3) 0.022(3) C11 0.058(3) 0.039(3) 0.077(4) 0.019(3) 0.038(3) 0.017(3) C12 0.046(3) 0.036(3) 0.057(3) 0.016(2) 0.022(2) 0.004(2) C13 0.040(2) 0.034(3) 0.047(3) 0.003(2) 0.012(2) 0.005(2) C14 0.036(2) 0.030(3) 0.043(3) 0.004(2) 0.016(2) 0.0039(19) C15 0.037(2) 0.030(3) 0.051(3) 0.001(2) 0.015(2) 0.002(2) C16 0.048(3) 0.031(3) 0.063(3) 0.002(2) 0.023(2) 0.005(2) C17 0.039(2) 0.042(3) 0.059(3) 0.005(2) 0.022(2) 0.003(2) C18 0.034(2) 0.033(3) 0.052(3) 0.007(2) 0.013(2) 0.005(2) C19 0.038(2) 0.043(3) 0.058(3) 0.006(2) 0.018(2) 0.006(2) C20 0.050(3) 0.035(3) 0.059(3) 0.011(2) 0.022(2) 0.008(2) C21 0.047(3) 0.044(3) 0.060(3) 0.011(3) 0.019(2) 0.006(2) C22 0.053(3) 0.046(3) 0.053(3) 0.016(2) 0.022(2) 0.012(2) C23 0.043(3) 0.038(3) 0.057(3) 0.012(2) 0.019(2) 0.003(2) C24 0.040(3) 0.051(3) 0.069(3) 0.018(3) 0.013(2) 0.010(2) C25 0.032(2) 0.059(4) 0.065(3) 0.016(3) 0.007(2) -0.007(2) C26 0.036(2) 0.049(3) 0.056(3) 0.017(2) 0.014(2) -0.003(2) C27 0.041(3) 0.041(3) 0.067(3) 0.017(3) 0.019(2) 0.005(2) C28 0.046(3) 0.038(3) 0.063(3) 0.011(2) 0.029(2) 0.001(2) C29 0.041(3) 0.041(3) 0.078(4) 0.015(3) 0.030(3) 0.008(2) C30 0.053(3) 0.039(3) 0.099(4) 0.014(3) 0.045(3) 0.009(2) C31 0.043(3) 0.032(3) 0.110(5) 0.023(3) 0.043(3) 0.007(2) C32 0.042(3) 0.040(3) 0.091(4) 0.026(3) 0.029(3) 0.011(2) C33 0.062(3) 0.035(3) 0.144(6) -0.008(4) 0.061(4) 0.000(3) C34 0.054(3) 0.042(3) 0.139(5) -0.023(4) 0.053(4) -0.005(3) C35 0.044(3) 0.022(3) 0.118(5) 0.010(3) 0.038(3) 0.002(2) C36 0.038(3) 0.027(3) 0.123(5) 0.017(3) 0.042(3) 0.009(2) C37 0.049(3) 0.031(3) 0.111(5) 0.020(3) 0.034(3) 0.005(3) C38 0.049(3) 0.036(3) 0.109(5) 0.019(3) 0.025(3) 0.006(2) C39 0.041(3) 0.034(3) 0.129(5) 0.026(3) 0.033(3) 0.010(3) C40 0.045(3) 0.034(3) 0.118(5) 0.014(3) 0.037(3) -0.001(3) C41 0.042(3) 0.030(3) 0.078(3) 0.006(2) 0.030(2) 0.002(2) C42 0.068(5) 0.047(6) 0.152(11) 0.038(6) 0.054(7) 0.027(4) C43 0.101(8) 0.039(6) 0.094(6) -0.005(5) 0.038(6) -0.022(5) C44 0.061(6) 0.046(4) 0.059(6) 0.018(5) 0.018(5) 0.008(6) C42D 0.068(5) 0.047(6) 0.152(11) 0.038(6) 0.054(7) 0.027(4) C43D 0.101(8) 0.039(6) 0.094(6) -0.005(5) 0.038(6) -0.022(5) C44D 0.061(6) 0.046(4) 0.059(6) 0.018(5) 0.018(5) 0.008(6) C45 0.046(3) 0.051(3) 0.068(3) 0.019(3) 0.007(3) -0.015(3) C46 0.072(4) 0.059(4) 0.125(6) 0.052(4) 0.001(4) -0.006(3) C47 0.104(5) 0.071(5) 0.067(4) 0.018(3) 0.023(4) -0.030(4) C48 0.065(3) 0.049(4) 0.082(4) 0.008(3) 0.022(3) -0.012(3) S1 0.0434(8) 0.0428(15) 0.0423(10) 0.0014(11) 0.0130(7) 0.0001(9) O1 0.044(2) 0.019(4) 0.050(2) -0.005(3) 0.0196(17) 0.005(3) O2 0.146(8) 0.051(5) 0.040(4) 0.008(3) 0.015(5) -0.023(5) O3 0.038(4) 0.070(5) 0.080(5) 0.003(4) -0.005(3) -0.006(3) C49 0.052(6) 0.049(6) 0.063(6) -0.005(5) 0.025(5) -0.002(5) F1 0.093(5) 0.069(5) 0.087(4) -0.037(4) 0.035(4) -0.009(4) F2 0.089(3) 0.051(4) 0.071(4) 0.006(3) 0.013(3) 0.007(3) F3 0.052(3) 0.064(4) 0.122(5) -0.033(4) 0.030(3) -0.015(3) S1D 0.0434(8) 0.0428(15) 0.0423(10) 0.0014(11) 0.0130(7) 0.0001(9) O1D 0.044(2) 0.019(4) 0.050(2) -0.005(3) 0.0196(17) 0.005(3) O2D 0.043(4) 0.049(4) 0.038(4) -0.005(3) 0.022(3) -0.009(3) O3D 0.041(4) 0.112(8) 0.044(4) 0.024(5) 0.002(3) 0.030(5) C49D 0.065(7) 0.066(8) 0.050(7) -0.024(6) 0.024(6) -0.035(7) F1D 0.168(9) 0.051(5) 0.102(6) -0.039(4) 0.085(6) -0.049(5) F2D 0.089(3) 0.051(4) 0.071(4) 0.006(3) 0.013(3) 0.007(3) F3D 0.069(4) 0.081(5) 0.071(4) -0.011(4) 0.032(3) -0.040(4) S2 0.0401(7) 0.0320(7) 0.0875(10) 0.0099(7) 0.0156(6) 0.0003(5) O4 0.054(2) 0.042(2) 0.076(2) 0.0085(18) 0.0156(18) 0.0105(17) O5 0.0472(19) 0.040(2) 0.090(3) 0.0005(19) 0.0145(18) -0.0044(17) O6 0.046(2) 0.063(3) 0.093(3) 0.014(2) 0.0228(19) -0.0035(18) C50 0.053(3) 0.039(4) 0.137(6) 0.015(4) 0.002(4) 0.006(3) F4 0.107(3) 0.047(2) 0.173(4) 0.033(3) -0.045(3) 0.005(2) F5 0.064(2) 0.068(3) 0.260(6) -0.009(3) 0.063(3) 0.016(2) F6 0.073(2) 0.0368(19) 0.133(3) 0.001(2) 0.009(2) -0.0050(17) _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 O1D 1.925(5) . ? Zn1 N1 2.087(4) . ? Zn1 N3 2.107(4) . ? Zn1 N4 2.135(5) . ? Zn1 N2 2.165(4) . ? Zn1 O4 2.190(3) . ? Zn1 O1 2.300(5) . ? N1 C1 1.342(6) . ? N1 C5 1.347(7) . ? N2 C10 1.337(6) . ? N2 C6 1.360(7) . ? N3 C35 1.347(7) . ? N3 C32 1.357(6) . ? N4 C40 1.352(6) . ? N4 C36 1.367(7) . ? C1 C2 1.365(7) . ? C1 H1 0.9500 . ? C2 C3 1.365(8) . ? C2 H2 0.9500 . ? C3 C4 1.390(7) . ? C3 H3 0.9500 . ? C4 C5 1.371(7) . ? C4 H4 0.9500 . ? C5 C6 1.480(7) . ? C6 C7 1.388(8) . ? C7 C8 1.396(7) . ? C7 H7 0.9500 . ? C8 C9 1.378(8) . ? C8 H8 0.9500 . ? C9 C10 1.398(7) . ? C9 C11 1.432(7) . ? C10 H10 0.9500 . ? C11 C12 1.191(6) . ? C12 C13 1.453(6) . ? C13 C18 1.400(6) . ? C13 C14 1.409(6) . ? C14 C15 1.374(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(6) . ? C15 C41 1.521(6) . ? C16 C17 1.387(7) . ? C16 H16 0.9500 . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.422(7) . ? C19 C20 1.204(7) . ? C20 C21 1.378(7) . ? C21 C22 1.204(7) . ? C22 C23 1.425(7) . ? C23 C24 1.384(6) . ? C23 C28 1.404(6) . ? C24 C25 1.392(7) . ? C24 H24 0.9500 . ? C25 C26 1.401(7) . ? C25 H25 0.9500 . ? C26 C27 1.393(6) . ? C26 C45 1.522(7) . ? C27 C28 1.393(6) . ? C27 H27 0.9500 . ? C28 C29 1.431(6) . ? C29 C30 1.205(7) . ? C30 C31 1.427(7) . ? C31 C33 1.379(9) . ? C31 C32 1.398(7) . ? C32 H32 0.9500 . ? C33 C34 1.383(7) . ? C33 H33 0.9500 . ? C34 C35 1.383(8) . ? C34 H34 0.9500 . ? C35 C36 1.469(7) . ? C36 C37 1.373(8) . ? C37 C38 1.376(7) . ? C37 H37 0.9500 . ? C38 C39 1.385(8) . ? C38 H38 0.9500 . ? C39 C40 1.370(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C44D 1.498(8) . ? C41 C43 1.505(13) . ? C41 C42D 1.530(8) . ? C41 C44 1.537(13) . ? C41 C42 1.569(13) . ? C41 C43D 1.572(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C42D H42D 0.9800 . ? C42D H42E 0.9800 . ? C42D H42F 0.9800 . ? C43D H43D 0.9800 . ? C43D H43E 0.9800 . ? C43D H43F 0.9800 . ? C44D H44D 0.9800 . ? C44D H44E 0.9800 . ? C44D H44F 0.9800 . ? C45 C46 1.521(8) . ? C45 C48 1.527(8) . ? C45 C47 1.538(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? S1 O2 1.433(3) . ? S1 O3 1.436(3) . ? S1 O1 1.452(3) . ? S1 C49 1.817(5) . ? C49 F3 1.311(5) . ? C49 F1 1.334(6) . ? C49 F2 1.342(5) . ? S1D O2D 1.432(3) . ? S1D O3D 1.435(3) . ? S1D O1D 1.452(3) . ? S1D C49D 1.818(5) . ? C49D F3D 1.311(5) . ? C49D F1D 1.333(6) . ? C49D F2D 1.342(5) . ? S2 O5 1.432(3) . ? S2 O6 1.435(3) . ? S2 O4 1.453(3) . ? S2 C50 1.817(5) . ? C50 F6 1.311(5) . ? C50 F4 1.333(6) . ? C50 F5 1.342(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1D Zn1 N1 97.5(2) . . ? O1D Zn1 N3 87.7(2) . . ? N1 Zn1 N3 171.67(17) . . ? O1D Zn1 N4 163.79(19) . . ? N1 Zn1 N4 98.08(17) . . ? N3 Zn1 N4 77.34(18) . . ? O1D Zn1 N2 85.5(2) . . ? N1 Zn1 N2 77.78(16) . . ? N3 Zn1 N2 96.24(15) . . ? N4 Zn1 N2 102.02(19) . . ? O1D Zn1 O4 89.47(18) . . ? N1 Zn1 O4 89.42(15) . . ? N3 Zn1 O4 97.15(13) . . ? N4 Zn1 O4 86.36(14) . . ? N2 Zn1 O4 165.50(14) . . ? O1D Zn1 O1 11.1(2) . . ? N1 Zn1 O1 92.53(18) . . ? N3 Zn1 O1 93.69(18) . . ? N4 Zn1 O1 162.21(17) . . ? N2 Zn1 O1 94.13(19) . . ? O4 Zn1 O1 79.49(17) . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Zn1 124.9(4) . . ? C5 N1 Zn1 116.5(3) . . ? C10 N2 C6 119.2(5) . . ? C10 N2 Zn1 127.4(3) . . ? C6 N2 Zn1 113.2(3) . . ? C35 N3 C32 119.6(5) . . ? C35 N3 Zn1 115.7(3) . . ? C32 N3 Zn1 124.7(4) . . ? C40 N4 C36 116.8(5) . . ? C40 N4 Zn1 127.3(4) . . ? C36 N4 Zn1 115.0(3) . . ? N1 C1 C2 122.6(6) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.1(5) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.5(5) . . ? N1 C5 C6 115.9(4) . . ? C4 C5 C6 122.6(5) . . ? N2 C6 C7 120.8(5) . . ? N2 C6 C5 116.1(5) . . ? C7 C6 C5 123.0(5) . . ? C6 C7 C8 118.9(5) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 117.1(5) . . ? C8 C9 C11 121.8(5) . . ? C10 C9 C11 121.0(5) . . ? N2 C10 C9 123.2(5) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C12 C11 C9 172.3(6) . . ? C11 C12 C13 172.0(5) . . ? C18 C13 C14 119.7(4) . . ? C18 C13 C12 122.8(4) . . ? C14 C13 C12 117.4(4) . . ? C15 C14 C13 122.1(4) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 117.5(4) . . ? C14 C15 C41 121.2(4) . . ? C16 C15 C41 121.2(4) . . ? C17 C16 C15 121.6(4) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 118.0(4) . . ? C17 C18 C19 120.1(4) . . ? C13 C18 C19 122.0(4) . . ? C20 C19 C18 176.5(5) . . ? C19 C20 C21 177.9(6) . . ? C22 C21 C20 178.8(5) . . ? C21 C22 C23 177.4(5) . . ? C24 C23 C28 118.1(4) . . ? C24 C23 C22 122.9(4) . . ? C28 C23 C22 119.0(4) . . ? C23 C24 C25 121.5(4) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 121.1(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 117.0(4) . . ? C27 C26 C45 122.6(4) . . ? C25 C26 C45 120.3(4) . . ? C26 C27 C28 122.2(4) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C23 120.0(4) . . ? C27 C28 C29 118.6(4) . . ? C23 C28 C29 121.4(4) . . ? C30 C29 C28 177.4(6) . . ? C29 C30 C31 174.9(6) . . ? C33 C31 C32 118.0(5) . . ? C33 C31 C30 121.2(5) . . ? C32 C31 C30 120.9(6) . . ? N3 C32 C31 121.6(6) . . ? N3 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C31 C33 C34 120.2(6) . . ? C31 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.3(6) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N3 C35 C34 121.1(5) . . ? N3 C35 C36 116.8(5) . . ? C34 C35 C36 122.1(6) . . ? N4 C36 C37 122.0(5) . . ? N4 C36 C35 114.7(6) . . ? C37 C36 C35 123.3(5) . . ? C36 C37 C38 120.2(6) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C39 118.5(6) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 118.9(5) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N4 C40 C39 123.6(6) . . ? N4 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? C44D C41 C43 124.2(11) . . ? C44D C41 C15 112.7(5) . . ? C43 C41 C15 115.8(11) . . ? C44D C41 C42D 111.1(6) . . ? C43 C41 C42D 73.6(11) . . ? C15 C41 C42D 112.4(5) . . ? C44D C41 C44 24.8(8) . . ? C43 C41 C44 107.6(13) . . ? C15 C41 C44 112.8(12) . . ? C42D C41 C44 127.9(11) . . ? C44D C41 C42 80.4(9) . . ? C43 C41 C42 109.3(12) . . ? C15 C41 C42 106.9(10) . . ? C42D C41 C42 38.0(9) . . ? C44 C41 C42 103.8(11) . . ? C44D C41 C43D 108.3(6) . . ? C43 C41 C43D 32.9(10) . . ? C15 C41 C43D 105.5(5) . . ? C42D C41 C43D 106.3(6) . . ? C44 C41 C43D 85.0(10) . . ? C42 C41 C43D 139.7(10) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? C41 C42D H42D 109.5 . . ? C41 C42D H42E 109.5 . . ? H42D C42D H42E 109.5 . . ? C41 C42D H42F 109.5 . . ? H42D C42D H42F 109.5 . . ? H42E C42D H42F 109.5 . . ? C41 C43D H43D 109.5 . . ? C41 C43D H43E 109.5 . . ? H43D C43D H43E 109.5 . . ? C41 C43D H43F 109.5 . . ? H43D C43D H43F 109.5 . . ? H43E C43D H43F 109.5 . . ? C41 C44D H44D 109.5 . . ? C41 C44D H44E 109.5 . . ? H44D C44D H44E 109.5 . . ? C41 C44D H44F 109.5 . . ? H44D C44D H44F 109.5 . . ? H44E C44D H44F 109.5 . . ? C46 C45 C26 111.4(4) . . ? C46 C45 C48 107.3(5) . . ? C26 C45 C48 109.7(4) . . ? C46 C45 C47 110.2(5) . . ? C26 C45 C47 108.0(5) . . ? C48 C45 C47 110.3(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O2 S1 O3 116.0(2) . . ? O2 S1 O1 115.30(19) . . ? O3 S1 O1 113.69(18) . . ? O2 S1 C49 103.21(19) . . ? O3 S1 C49 103.59(19) . . ? O1 S1 C49 102.6(2) . . ? S1 O1 Zn1 137.3(3) . . ? F3 C49 F1 108.6(4) . . ? F3 C49 F2 108.0(4) . . ? F1 C49 F2 106.5(4) . . ? F3 C49 S1 113.0(3) . . ? F1 C49 S1 110.1(4) . . ? F2 C49 S1 110.5(3) . . ? O2D S1D O3D 116.0(2) . . ? O2D S1D O1D 115.37(19) . . ? O3D S1D O1D 113.66(18) . . ? O2D S1D C49D 103.21(19) . . ? O3D S1D C49D 103.58(19) . . ? O1D S1D C49D 102.6(2) . . ? S1D O1D Zn1 133.1(3) . . ? F3D C49D F1D 108.7(4) . . ? F3D C49D F2D 107.9(4) . . ? F1D C49D F2D 106.6(4) . . ? F3D C49D S1D 112.9(3) . . ? F1D C49D S1D 110.1(4) . . ? F2D C49D S1D 110.4(3) . . ? O5 S2 O6 116.0(2) . . ? O5 S2 O4 115.30(17) . . ? O6 S2 O4 113.65(17) . . ? O5 S2 C50 103.22(18) . . ? O6 S2 C50 103.66(18) . . ? O4 S2 C50 102.6(2) . . ? S2 O4 Zn1 131.67(18) . . ? F6 C50 F4 108.6(3) . . ? F6 C50 F5 107.9(4) . . ? F4 C50 F5 106.5(4) . . ? F6 C50 S2 113.0(3) . . ? F4 C50 S2 110.1(4) . . ? F5 C50 S2 110.4(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 O1D Zn1 N1 C1 96.9(5) . . . . ? N3 Zn1 N1 C1 -134.7(12) . . . . ? N4 Zn1 N1 C1 -78.7(4) . . . . ? N2 Zn1 N1 C1 -179.3(5) . . . . ? O4 Zn1 N1 C1 7.5(4) . . . . ? O1 Zn1 N1 C1 87.0(4) . . . . ? O1D Zn1 N1 C5 -79.9(4) . . . . ? N3 Zn1 N1 C5 48.5(14) . . . . ? N4 Zn1 N1 C5 104.5(4) . . . . ? N2 Zn1 N1 C5 3.8(4) . . . . ? O4 Zn1 N1 C5 -169.3(4) . . . . ? O1 Zn1 N1 C5 -89.9(4) . . . . ? O1D Zn1 N2 C10 -82.1(5) . . . . ? N1 Zn1 N2 C10 179.2(6) . . . . ? N3 Zn1 N2 C10 5.1(6) . . . . ? N4 Zn1 N2 C10 83.4(5) . . . . ? O4 Zn1 N2 C10 -152.3(5) . . . . ? O1 Zn1 N2 C10 -89.1(5) . . . . ? O1D Zn1 N2 C6 92.9(4) . . . . ? N1 Zn1 N2 C6 -5.8(4) . . . . ? N3 Zn1 N2 C6 -180.0(4) . . . . ? N4 Zn1 N2 C6 -101.6(4) . . . . ? O4 Zn1 N2 C6 22.7(9) . . . . ? O1 Zn1 N2 C6 85.9(4) . . . . ? O1D Zn1 N3 C35 -169.8(4) . . . . ? N1 Zn1 N3 C35 61.3(14) . . . . ? N4 Zn1 N3 C35 4.0(3) . . . . ? N2 Zn1 N3 C35 105.0(4) . . . . ? O4 Zn1 N3 C35 -80.6(4) . . . . ? O1 Zn1 N3 C35 -160.5(4) . . . . ? O1D Zn1 N3 C32 11.0(4) . . . . ? N1 Zn1 N3 C32 -118.0(13) . . . . ? N4 Zn1 N3 C32 -175.3(4) . . . . ? N2 Zn1 N3 C32 -74.3(4) . . . . ? O4 Zn1 N3 C32 100.1(4) . . . . ? O1 Zn1 N3 C32 20.3(4) . . . . ? O1D Zn1 N4 C40 -152.2(7) . . . . ? N1 Zn1 N4 C40 12.1(4) . . . . ? N3 Zn1 N4 C40 -175.0(5) . . . . ? N2 Zn1 N4 C40 91.2(4) . . . . ? O4 Zn1 N4 C40 -76.8(4) . . . . ? O1 Zn1 N4 C40 -114.0(6) . . . . ? O1D Zn1 N4 C36 16.4(9) . . . . ? N1 Zn1 N4 C36 -179.3(3) . . . . ? N3 Zn1 N4 C36 -6.3(3) . . . . ? N2 Zn1 N4 C36 -100.1(3) . . . . ? O4 Zn1 N4 C36 91.8(3) . . . . ? O1 Zn1 N4 C36 54.7(7) . . . . ? C5 N1 C1 C2 -1.2(8) . . . . ? Zn1 N1 C1 C2 -178.0(4) . . . . ? N1 C1 C2 C3 0.5(8) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? C2 C3 C4 C5 0.1(8) . . . . ? C1 N1 C5 C4 1.5(8) . . . . ? Zn1 N1 C5 C4 178.5(4) . . . . ? C1 N1 C5 C6 -178.4(5) . . . . ? Zn1 N1 C5 C6 -1.4(7) . . . . ? C3 C4 C5 N1 -0.9(8) . . . . ? C3 C4 C5 C6 178.9(5) . . . . ? C10 N2 C6 C7 3.3(9) . . . . ? Zn1 N2 C6 C7 -172.1(5) . . . . ? C10 N2 C6 C5 -177.6(5) . . . . ? Zn1 N2 C6 C5 7.0(7) . . . . ? N1 C5 C6 N2 -4.0(8) . . . . ? C4 C5 C6 N2 176.2(6) . . . . ? N1 C5 C6 C7 175.1(6) . . . . ? C4 C5 C6 C7 -4.8(9) . . . . ? N2 C6 C7 C8 -3.1(10) . . . . ? C5 C6 C7 C8 177.9(6) . . . . ? C6 C7 C8 C9 0.2(10) . . . . ? C7 C8 C9 C10 2.3(10) . . . . ? C7 C8 C9 C11 -174.4(6) . . . . ? C6 N2 C10 C9 -0.7(9) . . . . ? Zn1 N2 C10 C9 173.9(5) . . . . ? C8 C9 C10 N2 -2.1(10) . . . . ? C11 C9 C10 N2 174.6(6) . . . . ? C8 C9 C11 C12 73(5) . . . . ? C10 C9 C11 C12 -104(4) . . . . ? C9 C11 C12 C13 -3(8) . . . . ? C11 C12 C13 C18 149(4) . . . . ? C11 C12 C13 C14 -30(4) . . . . ? C18 C13 C14 C15 0.1(7) . . . . ? C12 C13 C14 C15 178.9(4) . . . . ? C13 C14 C15 C16 -1.9(7) . . . . ? C13 C14 C15 C41 -177.6(4) . . . . ? C14 C15 C16 C17 2.4(7) . . . . ? C41 C15 C16 C17 178.0(5) . . . . ? C15 C16 C17 C18 -1.1(8) . . . . ? C16 C17 C18 C13 -0.7(7) . . . . ? C16 C17 C18 C19 -179.6(5) . . . . ? C14 C13 C18 C17 1.2(7) . . . . ? C12 C13 C18 C17 -177.5(5) . . . . ? C14 C13 C18 C19 -180.0(5) . . . . ? C12 C13 C18 C19 1.3(7) . . . . ? C17 C18 C19 C20 -13(10) . . . . ? C13 C18 C19 C20 168(10) . . . . ? C18 C19 C20 C21 118(17) . . . . ? C19 C20 C21 C22 67(52) . . . . ? C20 C21 C22 C23 21(56) . . . . ? C21 C22 C23 C24 130(15) . . . . ? C21 C22 C23 C28 -52(16) . . . . ? C28 C23 C24 C25 0.7(8) . . . . ? C22 C23 C24 C25 179.5(5) . . . . ? C23 C24 C25 C26 0.7(8) . . . . ? C24 C25 C26 C27 -1.3(8) . . . . ? C24 C25 C26 C45 180.0(5) . . . . ? C25 C26 C27 C28 0.6(8) . . . . ? C45 C26 C27 C28 179.3(5) . . . . ? C26 C27 C28 C23 0.7(8) . . . . ? C26 C27 C28 C29 -179.4(5) . . . . ? C24 C23 C28 C27 -1.3(7) . . . . ? C22 C23 C28 C27 179.8(5) . . . . ? C24 C23 C28 C29 178.8(5) . . . . ? C22 C23 C28 C29 -0.1(7) . . . . ? C27 C28 C29 C30 36(13) . . . . ? C23 C28 C29 C30 -144(13) . . . . ? C28 C29 C30 C31 74(15) . . . . ? C29 C30 C31 C33 -20(7) . . . . ? C29 C30 C31 C32 160(6) . . . . ? C35 N3 C32 C31 -0.8(7) . . . . ? Zn1 N3 C32 C31 178.4(3) . . . . ? C33 C31 C32 N3 3.3(7) . . . . ? C30 C31 C32 N3 -176.7(5) . . . . ? C32 C31 C33 C34 -2.3(8) . . . . ? C30 C31 C33 C34 177.7(5) . . . . ? C31 C33 C34 C35 -1.1(9) . . . . ? C32 N3 C35 C34 -2.7(8) . . . . ? Zn1 N3 C35 C34 178.0(4) . . . . ? C32 N3 C35 C36 178.0(4) . . . . ? Zn1 N3 C35 C36 -1.3(6) . . . . ? C33 C34 C35 N3 3.6(9) . . . . ? C33 C34 C35 C36 -177.1(5) . . . . ? C40 N4 C36 C37 -1.4(7) . . . . ? Zn1 N4 C36 C37 -171.3(4) . . . . ? C40 N4 C36 C35 177.5(4) . . . . ? Zn1 N4 C36 C35 7.6(5) . . . . ? N3 C35 C36 N4 -4.3(7) . . . . ? C34 C35 C36 N4 176.4(5) . . . . ? N3 C35 C36 C37 174.7(5) . . . . ? C34 C35 C36 C37 -4.6(8) . . . . ? N4 C36 C37 C38 1.9(8) . . . . ? C35 C36 C37 C38 -177.0(5) . . . . ? C36 C37 C38 C39 -1.1(7) . . . . ? C37 C38 C39 C40 0.0(7) . . . . ? C36 N4 C40 C39 0.3(7) . . . . ? Zn1 N4 C40 C39 168.8(4) . . . . ? C38 C39 C40 N4 0.4(8) . . . . ? C14 C15 C41 C44D -34.2(7) . . . . ? C16 C15 C41 C44D 150.3(6) . . . . ? C14 C15 C41 C43 117.3(13) . . . . ? C16 C15 C41 C43 -58.2(13) . . . . ? C14 C15 C41 C42D -160.8(7) . . . . ? C16 C15 C41 C42D 23.7(8) . . . . ? C14 C15 C41 C44 -7.2(12) . . . . ? C16 C15 C41 C44 177.2(11) . . . . ? C14 C15 C41 C42 -120.7(11) . . . . ? C16 C15 C41 C42 63.8(12) . . . . ? C14 C15 C41 C43D 83.8(7) . . . . ? C16 C15 C41 C43D -91.7(6) . . . . ? C27 C26 C45 C46 7.1(8) . . . . ? C25 C26 C45 C46 -174.3(5) . . . . ? C27 C26 C45 C48 125.7(5) . . . . ? C25 C26 C45 C48 -55.7(7) . . . . ? C27 C26 C45 C47 -114.0(6) . . . . ? C25 C26 C45 C47 64.6(6) . . . . ? O2 S1 O1 Zn1 16.0(5) . . . . ? O3 S1 O1 Zn1 153.4(4) . . . . ? C49 S1 O1 Zn1 -95.4(4) . . . . ? O1D Zn1 O1 S1 -95.5(12) . . . . ? N1 Zn1 O1 S1 21.7(4) . . . . ? N3 Zn1 O1 S1 -152.8(4) . . . . ? N4 Zn1 O1 S1 148.4(4) . . . . ? N2 Zn1 O1 S1 -56.3(4) . . . . ? O4 Zn1 O1 S1 110.6(4) . . . . ? O2 S1 C49 F3 -65.0(5) . . . . ? O3 S1 C49 F3 173.7(4) . . . . ? O1 S1 C49 F3 55.2(4) . . . . ? O2 S1 C49 F1 56.6(4) . . . . ? O3 S1 C49 F1 -64.7(4) . . . . ? O1 S1 C49 F1 176.8(4) . . . . ? O2 S1 C49 F2 173.9(4) . . . . ? O3 S1 C49 F2 52.7(5) . . . . ? O1 S1 C49 F2 -65.9(4) . . . . ? O2D S1D O1D Zn1 -15.9(5) . . . . ? O3D S1D O1D Zn1 121.6(4) . . . . ? C49D S1D O1D Zn1 -127.2(4) . . . . ? N1 Zn1 O1D S1D -4.5(4) . . . . ? N3 Zn1 O1D S1D -178.0(4) . . . . ? N4 Zn1 O1D S1D 159.8(5) . . . . ? N2 Zn1 O1D S1D -81.5(4) . . . . ? O4 Zn1 O1D S1D 84.8(4) . . . . ? O1 Zn1 O1D S1D 59.2(10) . . . . ? O2D S1D C49D F3D 179.3(4) . . . . ? O3D S1D C49D F3D 58.0(5) . . . . ? O1D S1D C49D F3D -60.5(4) . . . . ? O2D S1D C49D F1D 57.7(4) . . . . ? O3D S1D C49D F1D -63.7(4) . . . . ? O1D S1D C49D F1D 177.9(4) . . . . ? O2D S1D C49D F2D -59.7(5) . . . . ? O3D S1D C49D F2D 178.9(4) . . . . ? O1D S1D C49D F2D 60.5(4) . . . . ? O5 S2 O4 Zn1 83.7(3) . . . . ? O6 S2 O4 Zn1 -53.7(3) . . . . ? C50 S2 O4 Zn1 -164.9(2) . . . . ? O1D Zn1 O4 S2 114.1(3) . . . . ? N1 Zn1 O4 S2 -148.4(3) . . . . ? N3 Zn1 O4 S2 26.5(3) . . . . ? N4 Zn1 O4 S2 -50.3(3) . . . . ? N2 Zn1 O4 S2 -176.3(5) . . . . ? O1 Zn1 O4 S2 118.9(3) . . . . ? O5 S2 C50 F6 -179.5(3) . . . . ? O6 S2 C50 F6 -58.2(4) . . . . ? O4 S2 C50 F6 60.3(4) . . . . ? O5 S2 C50 F4 -57.8(3) . . . . ? O6 S2 C50 F4 63.5(3) . . . . ? O4 S2 C50 F4 -178.0(3) . . . . ? O5 S2 C50 F5 59.5(4) . . . . ? O6 S2 C50 F5 -179.2(4) . . . . ? O4 S2 C50 F5 -60.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.895 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.093 # start Validation Reply Form #_vrf_PLAT601_07124 #; #PROBLEM: Structure Contains Solvent Accessible VOIDS #RESPONSE: Structure contains large voids with various partial #solvent molecules superimposed. Solvent models refined with #a strong set of restraints and constraints did not converge #and yield chemically reasonable connectivity. The data were #modified using PLATON (SQUEEZE): total potential solvent #accessible void volume is 1892.8 Ang^3 with an electron count per #cell of 143. #;