# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Arjan Kleij' _publ_contact_author_email AKLEIJ@ICIQ.ES _publ_section_title ; Isolation and Characterization of a New Type of Biomimetic 'mu'-Hydroxy-bis-Zn(salphen) Sandwich Structure ; loop_ _publ_author_name 'Arjan Kleij' 'Daniele Anselmo' 'Jordi Benet-Buchholz' 'Eduardo Escudero-Adan' # Attachment 'AWK408_0m.cif' data_awk408_0m _database_code_depnum_ccdc_archive 'CCDC 760569' #TrackingRef 'AWK408_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H57 N3 O2 Zn' _chemical_formula_weight 677.26 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.1860(9) _cell_length_b 19.0560(10) _cell_length_c 22.1544(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7255.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9812 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 28.01 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 93066 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.06 _reflns_number_total 17462 _reflns_number_gt 15951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0309P)^2^+4.5928P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(7) _refine_ls_number_reflns 17462 _refine_ls_number_parameters 847 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 C1A C 0.06503(13) 0.11422(13) 0.87974(11) 0.0172(5) Uani 1 1 d . . . C1AS C 0.20318(13) 0.15582(13) 0.72493(11) 0.0190(5) Uani 1 1 d . . . H1A1 H 0.2500 0.1521 0.7507 0.023 Uiso 1 1 calc R . . H1A2 H 0.2207 0.1535 0.6824 0.023 Uiso 1 1 calc R . . N1A N 0.22417(11) 0.17837(11) 0.87170(9) 0.0170(4) Uani 1 1 d . . . N1AS N 0.16722(11) 0.22618(11) 0.73533(9) 0.0173(4) Uani 1 1 d . . . O1A O 0.06108(9) 0.17835(10) 0.86001(8) 0.0188(4) Uani 1 1 d . . . Zn1A Zn 0.140894(13) 0.243558(13) 0.830397(12) 0.01471(6) Uani 1 1 d . . . C2A C -0.00556(13) 0.07331(14) 0.88494(11) 0.0198(5) Uani 1 1 d . . . C2AS C 0.15182(14) 0.09254(14) 0.73718(12) 0.0205(5) Uani 1 1 d . . . H2A1 H 0.1158 0.0853 0.7028 0.025 Uiso 1 1 calc R . . H2A2 H 0.1203 0.1009 0.7739 0.025 Uiso 1 1 calc R . . N2A N 0.22493(11) 0.31520(11) 0.85984(9) 0.0168(4) Uani 1 1 d . . . O2A O 0.06554(9) 0.32216(9) 0.82739(9) 0.0189(3) Uani 1 1 d . . . C3A C 0.00075(15) 0.00453(14) 0.90406(12) 0.0235(5) Uani 1 1 d . . . H3A H -0.0453 -0.0229 0.9061 0.028 Uiso 1 1 calc R . . C3AS C 0.20212(14) 0.02706(13) 0.74595(12) 0.0236(5) Uani 1 1 d . . . H3A1 H 0.2358 0.0209 0.7101 0.028 Uiso 1 1 calc R . . H3A2 H 0.2363 0.0341 0.7814 0.028 Uiso 1 1 calc R . . C4A C 0.07163(15) -0.02715(14) 0.92075(12) 0.0241(5) Uani 1 1 d . . . H4A H 0.0730 -0.0746 0.9337 0.029 Uiso 1 1 calc R . . C4AS C 0.15442(16) -0.03910(15) 0.75523(14) 0.0290(6) Uani 1 1 d . . . H4A1 H 0.1179 -0.0320 0.7886 0.044 Uiso 1 1 calc R . . H4A2 H 0.1892 -0.0783 0.7648 0.044 Uiso 1 1 calc R . . H4A3 H 0.1254 -0.0497 0.7183 0.044 Uiso 1 1 calc R . . C5A C 0.13848(14) 0.01190(14) 0.91787(12) 0.0205(5) Uani 1 1 d . . . H5A H 0.1864 -0.0085 0.9302 0.025 Uiso 1 1 calc R . . C5AS C 0.09097(13) 0.23475(14) 0.70342(11) 0.0173(5) Uani 1 1 d . . . H5A1 H 0.0697 0.2815 0.7137 0.021 Uiso 1 1 calc R . . H5A2 H 0.0544 0.1992 0.7195 0.021 Uiso 1 1 calc R . . C6A C 0.13741(13) 0.08207(13) 0.89688(11) 0.0171(5) Uani 1 1 d . . . C6AS C 0.09271(14) 0.22800(15) 0.63486(11) 0.0217(5) Uani 1 1 d . . . H6A1 H 0.1280 0.2639 0.6178 0.026 Uiso 1 1 calc R . . H6A2 H 0.1131 0.1812 0.6236 0.026 Uiso 1 1 calc R . . C7A C 0.21047(13) 0.11756(13) 0.89588(11) 0.0181(5) Uani 1 1 d . . . H7A H 0.2531 0.0945 0.9147 0.022 Uiso 1 1 calc R . . C7AS C 0.01147(16) 0.23746(17) 0.60863(13) 0.0286(6) Uani 1 1 d . . . H7A1 H -0.0105 0.2824 0.6231 0.034 Uiso 1 1 calc R . . H7A2 H -0.0225 0.1991 0.6233 0.034 Uiso 1 1 calc R . . C8A C -0.08471(14) 0.10798(14) 0.87189(12) 0.0231(5) Uani 1 1 d . . . C8AS C 0.01191(18) 0.2373(2) 0.53956(14) 0.0391(8) Uani 1 1 d . . . H8A1 H 0.0343 0.1931 0.5250 0.059 Uiso 1 1 calc R . . H8A2 H 0.0432 0.2767 0.5249 0.059 Uiso 1 1 calc R . . H8A3 H -0.0415 0.2419 0.5246 0.059 Uiso 1 1 calc R . . C9A C -0.15109(16) 0.05447(18) 0.87575(17) 0.0434(9) Uani 1 1 d . . . H9A1 H -0.1439 0.0185 0.8447 0.065 Uiso 1 1 calc R . . H9A2 H -0.2009 0.0784 0.8694 0.065 Uiso 1 1 calc R . . H9A3 H -0.1509 0.0324 0.9157 0.065 Uiso 1 1 calc R . . C9AS C 0.22643(13) 0.27831(14) 0.71440(12) 0.0193(5) Uani 1 1 d . . . H9A4 H 0.2431 0.2650 0.6732 0.023 Uiso 1 1 calc R . . H9A5 H 0.2725 0.2746 0.7410 0.023 Uiso 1 1 calc R . . C10A C -0.09973(15) 0.16445(16) 0.91998(13) 0.0294(6) Uani 1 1 d . . . H10A H -0.1065 0.1420 0.9594 0.044 Uiso 1 1 calc R . . H10B H -0.1469 0.1907 0.9096 0.044 Uiso 1 1 calc R . . H10C H -0.0554 0.1967 0.9216 0.044 Uiso 1 1 calc R . . C10S C 0.20081(13) 0.35422(13) 0.71312(11) 0.0192(5) Uani 1 1 d . . . H10D H 0.1716 0.3651 0.7505 0.023 Uiso 1 1 calc R . . H10E H 0.1656 0.3618 0.6784 0.023 Uiso 1 1 calc R . . C11A C -0.08730(15) 0.14202(15) 0.80860(12) 0.0261(6) Uani 1 1 d . . . H11A H -0.0513 0.1818 0.8073 0.039 Uiso 1 1 calc R . . H11B H -0.1402 0.1585 0.8002 0.039 Uiso 1 1 calc R . . H11C H -0.0721 0.1073 0.7782 0.039 Uiso 1 1 calc R . . C11S C 0.27071(14) 0.40325(14) 0.70793(13) 0.0273(6) Uani 1 1 d . . . H11D H 0.3049 0.3964 0.7434 0.033 Uiso 1 1 calc R . . H11E H 0.3009 0.3907 0.6715 0.033 Uiso 1 1 calc R . . C12S C 0.24773(16) 0.47993(14) 0.70418(14) 0.0313(6) Uani 1 1 d . . . H12A H 0.2172 0.4878 0.6675 0.047 Uiso 1 1 calc R . . H12B H 0.2947 0.5091 0.7031 0.047 Uiso 1 1 calc R . . H12C H 0.2165 0.4924 0.7396 0.047 Uiso 1 1 calc R . . C13A C 0.36858(13) 0.17418(14) 0.88263(11) 0.0217(5) Uani 1 1 d . . . H13A H 0.3689 0.1244 0.8847 0.026 Uiso 1 1 calc R . . C13S C 0.29836(13) 0.21030(14) 0.87550(11) 0.0181(5) Uani 1 1 d . . . C14A C 0.43796(13) 0.21141(15) 0.88669(12) 0.0236(5) Uani 1 1 d . . . H14A H 0.4856 0.1869 0.8921 0.028 Uiso 1 1 calc R . . C15A C 0.43803(13) 0.28375(15) 0.88294(11) 0.0231(5) Uani 1 1 d . . . H15A H 0.4856 0.3088 0.8866 0.028 Uiso 1 1 calc R . . C16A C 0.36910(13) 0.32020(15) 0.87385(11) 0.0208(5) Uani 1 1 d . . . H16A H 0.3698 0.3698 0.8699 0.025 Uiso 1 1 calc R . . C17A C 0.29844(13) 0.28376(15) 0.87050(11) 0.0185(5) Uani 1 1 d . . . C18A C 0.21254(13) 0.38129(13) 0.87205(11) 0.0180(5) Uani 1 1 d . . . H18A H 0.2549 0.4068 0.8887 0.022 Uiso 1 1 calc R . . C19A C 0.14186(13) 0.41927(14) 0.86297(11) 0.0182(5) Uani 1 1 d . . . C20A C 0.14495(14) 0.49216(14) 0.87559(12) 0.0216(5) Uani 1 1 d . . . H20A H 0.1924 0.5125 0.8889 0.026 Uiso 1 1 calc R . . C21A C 0.08079(15) 0.53332(13) 0.86882(13) 0.0251(5) Uani 1 1 d . . . H21A H 0.0840 0.5826 0.8751 0.030 Uiso 1 1 calc R . . C22A C 0.00988(15) 0.50214(14) 0.85251(12) 0.0243(5) Uani 1 1 d . . . H22A H -0.0347 0.5314 0.8491 0.029 Uiso 1 1 calc R . . C23A C 0.00126(13) 0.43106(13) 0.84111(11) 0.0192(5) Uani 1 1 d . . . C24A C 0.06998(13) 0.38765(13) 0.84292(10) 0.0164(5) Uani 1 1 d . . . C25A C -0.07928(13) 0.39876(13) 0.82856(13) 0.0217(5) Uani 1 1 d . . . C26A C -0.14466(14) 0.45296(15) 0.83518(16) 0.0336(6) Uani 1 1 d . . . H26A H -0.1443 0.4719 0.8763 0.050 Uiso 1 1 calc R . . H26B H -0.1949 0.4304 0.8272 0.050 Uiso 1 1 calc R . . H26C H -0.1365 0.4912 0.8063 0.050 Uiso 1 1 calc R . . C27A C -0.09540(15) 0.33926(16) 0.87379(13) 0.0271(6) Uani 1 1 d . . . H27A H -0.0540 0.3041 0.8710 0.041 Uiso 1 1 calc R . . H27B H -0.1455 0.3173 0.8643 0.041 Uiso 1 1 calc R . . H27C H -0.0970 0.3585 0.9148 0.041 Uiso 1 1 calc R . . C28A C -0.08379(14) 0.36803(15) 0.76414(12) 0.0248(5) Uani 1 1 d . . . H28A H -0.0768 0.4058 0.7346 0.037 Uiso 1 1 calc R . . H28B H -0.1347 0.3459 0.7581 0.037 Uiso 1 1 calc R . . H28C H -0.0427 0.3329 0.7589 0.037 Uiso 1 1 calc R . . C1B C 0.62258(13) 0.11230(13) 0.57560(11) 0.0181(4) Uani 1 1 d . . . C1SB C 0.48700(13) 0.34420(13) 0.68771(11) 0.0197(5) Uani 1 1 d . . . H1S1 H 0.4676 0.3459 0.7298 0.024 Uiso 1 1 calc R . . H1S2 H 0.4413 0.3487 0.6608 0.024 Uiso 1 1 calc R . . N1B N 0.46768(11) 0.18167(12) 0.55412(9) 0.0184(4) Uani 1 1 d . . . N1BS N 0.52262(11) 0.27391(11) 0.67741(9) 0.0160(4) Uani 1 1 d . . . O1B O 0.62686(9) 0.17912(9) 0.58661(8) 0.0186(3) Uani 1 1 d . . . Zn1B Zn 0.550417(13) 0.256256(14) 0.582173(12) 0.01516(6) Uani 1 1 d . . . C2B C 0.69238(12) 0.06999(12) 0.57763(11) 0.0171(4) Uani 1 1 d . . . C2SB C 0.53910(14) 0.40736(14) 0.67762(12) 0.0206(5) Uani 1 1 d . . . H2S1 H 0.5727 0.3992 0.6420 0.025 Uiso 1 1 calc R . . H2S2 H 0.5731 0.4143 0.7132 0.025 Uiso 1 1 calc R . . N2B N 0.46742(11) 0.31973(12) 0.53837(9) 0.0190(4) Uani 1 1 d . . . O2B O 0.62961(9) 0.32410(9) 0.55479(8) 0.0182(4) Uani 1 1 d . . . C3B C 0.68556(14) -0.00139(14) 0.56920(11) 0.0222(5) Uani 1 1 d . . . H3B H 0.7312 -0.0294 0.5720 0.027 Uiso 1 1 calc R . . C3SB C 0.48935(14) 0.47266(14) 0.66755(13) 0.0254(5) Uani 1 1 d . . . H3S1 H 0.4573 0.4661 0.6308 0.030 Uiso 1 1 calc R . . H3S2 H 0.4536 0.4787 0.7022 0.030 Uiso 1 1 calc R . . C4B C 0.61435(16) -0.03493(14) 0.55659(13) 0.0267(5) Uani 1 1 d . . . H4B H 0.6119 -0.0845 0.5525 0.032 Uiso 1 1 calc R . . C4SB C 0.53849(16) 0.53868(16) 0.66046(15) 0.0312(6) Uani 1 1 d . . . H4S1 H 0.5642 0.5495 0.6989 0.047 Uiso 1 1 calc R . . H4S2 H 0.5050 0.5780 0.6488 0.047 Uiso 1 1 calc R . . H4S3 H 0.5779 0.5310 0.6292 0.047 Uiso 1 1 calc R . . C5B C 0.54907(14) 0.00498(15) 0.55040(12) 0.0228(5) Uani 1 1 d . . . H5B H 0.5013 -0.0171 0.5401 0.027 Uiso 1 1 calc R . . C5SB C 0.59862(13) 0.26553(14) 0.70958(11) 0.0185(5) Uani 1 1 d . . . H5S1 H 0.6347 0.3021 0.6945 0.022 Uiso 1 1 calc R . . H5S2 H 0.6208 0.2194 0.6983 0.022 Uiso 1 1 calc R . . C6B C 0.55079(13) 0.07861(14) 0.55902(11) 0.0185(5) Uani 1 1 d . . . C6SB C 0.59673(14) 0.27004(15) 0.77803(11) 0.0222(5) Uani 1 1 d . . . H6S1 H 0.5594 0.2351 0.7940 0.027 Uiso 1 1 calc R . . H6S2 H 0.5786 0.3172 0.7903 0.027 Uiso 1 1 calc R . . C7B C 0.47979(13) 0.11523(14) 0.54659(11) 0.0193(5) Uani 1 1 d . . . H7B H 0.4377 0.0882 0.5314 0.023 Uiso 1 1 calc R . . C7SB C 0.67749(16) 0.25633(17) 0.80528(14) 0.0319(7) Uani 1 1 d . . . H7S1 H 0.7023 0.2169 0.7835 0.038 Uiso 1 1 calc R . . H7S2 H 0.7104 0.2984 0.7995 0.038 Uiso 1 1 calc R . . C8B C 0.77213(12) 0.10538(13) 0.58616(12) 0.0200(5) Uani 1 1 d . . . C8SB C 0.67392(19) 0.2391(2) 0.87148(15) 0.0408(8) Uani 1 1 d . . . H8S1 H 0.6465 0.2767 0.8929 0.061 Uiso 1 1 calc R . . H8S2 H 0.7269 0.2348 0.8875 0.061 Uiso 1 1 calc R . . H8S3 H 0.6461 0.1947 0.8772 0.061 Uiso 1 1 calc R . . C9B C 0.83878(14) 0.05187(15) 0.58477(14) 0.0272(5) Uani 1 1 d . . . H9B1 H 0.8886 0.0764 0.5892 0.041 Uiso 1 1 calc R . . H9B2 H 0.8380 0.0266 0.5462 0.041 Uiso 1 1 calc R . . H9B3 H 0.8324 0.0184 0.6180 0.041 Uiso 1 1 calc R . . C9SB C 0.46316(13) 0.22199(14) 0.69809(11) 0.0186(5) Uani 1 1 d . . . H9S1 H 0.4181 0.2246 0.6703 0.022 Uiso 1 1 calc R . . H9S2 H 0.4447 0.2366 0.7385 0.022 Uiso 1 1 calc R . . C10B C 0.78544(15) 0.15701(16) 0.53358(13) 0.0266(6) Uani 1 1 d . . . H10F H 0.8366 0.1792 0.5380 0.040 Uiso 1 1 calc R . . H10G H 0.7449 0.1932 0.5341 0.040 Uiso 1 1 calc R . . H10H H 0.7833 0.1315 0.4952 0.040 Uiso 1 1 calc R . . C11B C 0.77755(14) 0.14462(15) 0.64682(12) 0.0251(5) Uani 1 1 d . . . H11F H 0.7703 0.1113 0.6800 0.038 Uiso 1 1 calc R . . H11G H 0.7370 0.1807 0.6486 0.038 Uiso 1 1 calc R . . H11H H 0.8288 0.1668 0.6504 0.038 Uiso 1 1 calc R . . C12B C 0.39430(13) 0.21206(14) 0.54072(11) 0.0176(5) Uani 1 1 d . . . C13B C 0.32408(14) 0.17593(15) 0.53812(11) 0.0216(5) Uani 1 1 d . . . H13B H 0.3235 0.1265 0.5436 0.026 Uiso 1 1 calc R . . C14B C 0.25486(14) 0.21123(16) 0.52770(12) 0.0256(6) Uani 1 1 d . . . H14B H 0.2074 0.1857 0.5253 0.031 Uiso 1 1 calc R . . C14S C 0.48899(13) 0.14593(13) 0.70192(11) 0.0190(5) Uani 1 1 d . . . H14C H 0.5188 0.1334 0.6652 0.023 Uiso 1 1 calc R . . H14D H 0.5235 0.1397 0.7373 0.023 Uiso 1 1 calc R . . C15B C 0.25445(14) 0.28368(16) 0.52075(12) 0.0266(6) Uani 1 1 d . . . H15B H 0.2069 0.3077 0.5139 0.032 Uiso 1 1 calc R . . C15S C 0.41898(14) 0.09787(15) 0.70778(13) 0.0261(6) Uani 1 1 d . . . H15C H 0.3871 0.1015 0.6707 0.031 Uiso 1 1 calc R . . H15D H 0.3866 0.1139 0.7421 0.031 Uiso 1 1 calc R . . C16B C 0.32366(14) 0.32069(15) 0.52385(12) 0.0241(5) Uani 1 1 d . . . H16B H 0.3231 0.3703 0.5197 0.029 Uiso 1 1 calc R . . C16S C 0.44110(17) 0.02161(15) 0.71765(14) 0.0334(6) Uani 1 1 d . . . H16C H 0.4739 0.0056 0.6842 0.050 Uiso 1 1 calc R . . H16D H 0.3939 -0.0071 0.7194 0.050 Uiso 1 1 calc R . . H16E H 0.4698 0.0171 0.7557 0.050 Uiso 1 1 calc R . . C17B C 0.39415(13) 0.28603(14) 0.53303(11) 0.0196(5) Uani 1 1 d . . . C18B C 0.47977(14) 0.38124(14) 0.51580(11) 0.0204(5) Uani 1 1 d . . . H18B H 0.4376 0.4029 0.4952 0.025 Uiso 1 1 calc R . . C19B C 0.55162(13) 0.41987(15) 0.51904(12) 0.0203(5) Uani 1 1 d . . . C20B C 0.54866(14) 0.49045(16) 0.50008(12) 0.0244(6) Uani 1 1 d . . . H20B H 0.5006 0.5099 0.4871 0.029 Uiso 1 1 calc R . . C21B C 0.61385(16) 0.53097(15) 0.50010(12) 0.0271(6) Uani 1 1 d . . . H21B H 0.6113 0.5789 0.4885 0.033 Uiso 1 1 calc R . . C22B C 0.68515(15) 0.50091(15) 0.51761(12) 0.0237(5) Uani 1 1 d . . . H22B H 0.7303 0.5297 0.5175 0.028 Uiso 1 1 calc R . . C23B C 0.69291(14) 0.43166(13) 0.53499(11) 0.0190(5) Uani 1 1 d . . . C24B C 0.62415(14) 0.38890(14) 0.53754(11) 0.0182(5) Uani 1 1 d . . . C25B C 0.77300(13) 0.39931(14) 0.54769(12) 0.0207(5) Uani 1 1 d . . . C26B C 0.79173(14) 0.34884(15) 0.49573(13) 0.0256(5) Uani 1 1 d . . . H26D H 0.8417 0.3257 0.5035 0.038 Uiso 1 1 calc R . . H26E H 0.7949 0.3752 0.4578 0.038 Uiso 1 1 calc R . . H26F H 0.7506 0.3134 0.4926 0.038 Uiso 1 1 calc R . . C27B C 0.83727(15) 0.45540(16) 0.54963(14) 0.0298(6) Uani 1 1 d . . . H27D H 0.8267 0.4884 0.5826 0.045 Uiso 1 1 calc R . . H27E H 0.8384 0.4808 0.5112 0.045 Uiso 1 1 calc R . . H27F H 0.8877 0.4327 0.5564 0.045 Uiso 1 1 calc R . . C28B C 0.77627(15) 0.35944(15) 0.60826(12) 0.0246(5) Uani 1 1 d . . . H28D H 0.7550 0.3892 0.6404 0.037 Uiso 1 1 calc R . . H28E H 0.8304 0.3475 0.6177 0.037 Uiso 1 1 calc R . . H28F H 0.7455 0.3163 0.6052 0.037 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 C1A 0.0158(10) 0.0190(12) 0.0166(11) -0.0014(9) 0.0016(8) -0.0006(9) C1AS 0.0161(10) 0.0199(12) 0.0209(12) -0.0025(10) 0.0016(8) 0.0024(9) N1A 0.0131(9) 0.0211(10) 0.0167(9) -0.0010(8) 0.0001(7) -0.0012(8) N1AS 0.0133(9) 0.0193(10) 0.0192(10) -0.0014(8) -0.0005(7) 0.0003(8) O1A 0.0128(7) 0.0188(9) 0.0248(9) 0.0019(8) 0.0010(6) -0.0010(6) Zn1A 0.01070(11) 0.01616(12) 0.01726(12) -0.00047(14) 0.00013(9) -0.00038(9) C2A 0.0167(11) 0.0237(12) 0.0190(11) 0.0024(9) 0.0007(8) -0.0036(9) C2AS 0.0183(11) 0.0213(13) 0.0217(12) -0.0043(10) 0.0012(9) 0.0015(10) N2A 0.0123(9) 0.0179(10) 0.0201(10) 0.0000(8) 0.0004(7) 0.0007(7) O2A 0.0143(7) 0.0166(8) 0.0259(9) -0.0028(8) -0.0013(7) 0.0006(6) C3A 0.0213(12) 0.0229(13) 0.0264(13) 0.0019(10) 0.0007(9) -0.0078(10) C3AS 0.0216(12) 0.0207(12) 0.0285(14) -0.0025(11) 0.0009(10) 0.0004(10) C4A 0.0273(12) 0.0172(12) 0.0279(13) 0.0033(10) 0.0028(10) -0.0024(10) C4AS 0.0294(13) 0.0206(14) 0.0372(16) -0.0035(12) 0.0052(12) -0.0008(11) C5A 0.0221(12) 0.0191(13) 0.0204(12) -0.0015(10) 0.0017(9) 0.0025(9) C5AS 0.0127(10) 0.0212(12) 0.0179(11) -0.0011(10) 0.0007(9) 0.0004(9) C6A 0.0178(11) 0.0154(12) 0.0182(12) 0.0005(10) 0.0016(8) 0.0003(8) C6AS 0.0162(11) 0.0296(14) 0.0193(12) -0.0033(11) -0.0011(9) 0.0027(10) C7A 0.0143(10) 0.0191(12) 0.0209(11) -0.0014(10) 0.0005(8) 0.0037(9) C7AS 0.0203(12) 0.0429(17) 0.0225(13) 0.0006(12) -0.0024(10) -0.0012(12) C8A 0.0145(11) 0.0252(13) 0.0297(13) 0.0108(11) -0.0035(9) -0.0032(9) C8AS 0.0247(14) 0.068(2) 0.0246(14) 0.0016(15) -0.0074(11) 0.0044(15) C9A 0.0190(13) 0.0464(19) 0.065(2) 0.0257(17) -0.0105(13) -0.0138(12) C9AS 0.0126(10) 0.0236(13) 0.0218(12) -0.0007(10) 0.0011(8) -0.0001(9) C10A 0.0183(12) 0.0419(17) 0.0279(14) 0.0131(12) 0.0044(10) 0.0075(11) C10S 0.0148(10) 0.0209(12) 0.0219(12) 0.0030(10) 0.0002(8) -0.0004(9) C11A 0.0266(13) 0.0286(14) 0.0231(12) 0.0042(11) -0.0077(10) -0.0048(11) C11S 0.0197(11) 0.0289(14) 0.0332(14) 0.0066(12) -0.0017(10) -0.0047(11) C12S 0.0299(13) 0.0243(14) 0.0397(16) 0.0096(12) -0.0080(12) -0.0086(11) C13A 0.0169(11) 0.0264(13) 0.0220(12) 0.0023(10) 0.0000(9) 0.0023(10) C13S 0.0125(10) 0.0267(13) 0.0152(11) -0.0018(9) 0.0009(8) 0.0007(9) C14A 0.0126(10) 0.0340(15) 0.0242(13) 0.0039(11) -0.0001(9) 0.0030(10) C15A 0.0123(10) 0.0344(15) 0.0226(12) 0.0008(11) -0.0003(9) -0.0033(10) C16A 0.0153(11) 0.0274(13) 0.0198(11) -0.0008(10) -0.0001(9) -0.0036(10) C17A 0.0124(10) 0.0280(14) 0.0151(11) -0.0006(10) 0.0001(8) 0.0000(10) C18A 0.0140(10) 0.0201(12) 0.0199(11) -0.0010(10) 0.0012(8) -0.0040(9) C19A 0.0169(11) 0.0169(12) 0.0208(12) -0.0028(9) 0.0037(8) -0.0029(9) C20A 0.0197(11) 0.0186(12) 0.0265(13) -0.0044(10) 0.0043(9) -0.0031(9) C21A 0.0251(12) 0.0145(12) 0.0356(14) -0.0041(10) 0.0050(10) -0.0004(10) C22A 0.0202(12) 0.0193(12) 0.0335(13) -0.0026(10) 0.0031(10) 0.0045(10) C23A 0.0162(10) 0.0202(12) 0.0213(12) -0.0019(9) 0.0020(8) 0.0019(9) C24A 0.0159(10) 0.0156(11) 0.0178(11) -0.0004(9) 0.0037(8) 0.0004(9) C25A 0.0144(10) 0.0234(12) 0.0272(12) -0.0066(12) -0.0003(9) 0.0028(9) C26A 0.0167(11) 0.0365(15) 0.0476(17) -0.0140(15) -0.0021(11) 0.0065(11) C27A 0.0182(12) 0.0377(16) 0.0254(13) -0.0013(12) 0.0023(10) -0.0065(11) C28A 0.0190(11) 0.0287(14) 0.0268(13) -0.0048(11) 0.0005(9) 0.0004(10) C1B 0.0141(9) 0.0245(12) 0.0156(11) 0.0004(10) 0.0022(8) -0.0001(9) C1SB 0.0146(10) 0.0222(13) 0.0223(12) -0.0039(10) 0.0007(8) 0.0028(9) N1B 0.0112(9) 0.0258(11) 0.0183(10) -0.0018(8) 0.0003(7) -0.0016(8) N1BS 0.0108(8) 0.0175(10) 0.0197(10) 0.0000(8) -0.0004(7) 0.0013(7) O1B 0.0132(7) 0.0187(8) 0.0240(9) -0.0015(8) -0.0001(7) 0.0009(6) Zn1B 0.01022(11) 0.01810(13) 0.01715(12) -0.00047(14) -0.00051(9) 0.00031(9) C2B 0.0172(10) 0.0189(11) 0.0152(10) 0.0008(10) 0.0033(9) 0.0011(8) C2SB 0.0188(11) 0.0209(13) 0.0220(12) -0.0020(10) 0.0005(9) 0.0017(10) N2B 0.0119(9) 0.0251(11) 0.0199(10) -0.0003(9) -0.0006(7) 0.0013(8) O2B 0.0138(7) 0.0172(9) 0.0237(9) 0.0015(7) 0.0000(6) 0.0009(6) C3B 0.0209(11) 0.0208(12) 0.0247(13) 0.0005(10) 0.0001(9) 0.0054(10) C3SB 0.0214(12) 0.0209(13) 0.0338(15) -0.0045(11) 0.0025(10) 0.0019(10) C4B 0.0297(13) 0.0176(12) 0.0328(14) 0.0000(11) 0.0008(10) -0.0003(10) C4SB 0.0294(14) 0.0257(15) 0.0387(16) -0.0002(13) 0.0079(12) -0.0009(12) C5B 0.0227(12) 0.0229(13) 0.0226(12) -0.0009(10) 0.0014(9) -0.0056(10) C5SB 0.0118(9) 0.0244(12) 0.0193(12) -0.0003(10) -0.0018(8) 0.0019(9) C6B 0.0160(11) 0.0215(13) 0.0181(11) 0.0002(9) 0.0028(8) -0.0001(9) C6SB 0.0191(12) 0.0293(14) 0.0183(12) -0.0025(11) -0.0015(9) 0.0000(10) C7B 0.0136(10) 0.0248(13) 0.0194(12) -0.0003(10) 0.0020(8) -0.0039(9) C7SB 0.0188(12) 0.049(2) 0.0281(14) 0.0000(13) -0.0040(10) -0.0033(12) C8B 0.0135(10) 0.0243(12) 0.0223(12) 0.0028(11) 0.0027(9) 0.0027(8) C8SB 0.0311(15) 0.063(2) 0.0284(15) 0.0002(15) -0.0093(12) 0.0055(14) C9B 0.0181(11) 0.0318(14) 0.0317(13) -0.0024(13) 0.0025(10) 0.0090(10) C9SB 0.0127(10) 0.0256(13) 0.0174(11) 0.0018(10) 0.0012(8) 0.0016(9) C10B 0.0177(12) 0.0300(15) 0.0322(14) 0.0069(12) 0.0029(10) -0.0006(10) C11B 0.0162(11) 0.0321(14) 0.0271(13) -0.0049(11) -0.0019(9) 0.0001(10) C12B 0.0130(10) 0.0241(13) 0.0155(11) -0.0035(9) -0.0012(8) 0.0012(9) C13B 0.0171(11) 0.0276(13) 0.0200(11) -0.0037(10) 0.0008(9) -0.0024(10) C14B 0.0120(11) 0.0426(16) 0.0221(13) -0.0047(11) 0.0011(9) -0.0045(11) C14S 0.0160(10) 0.0229(13) 0.0181(11) 0.0009(10) -0.0003(9) -0.0002(9) C15B 0.0144(11) 0.0406(16) 0.0248(13) 0.0024(12) -0.0010(9) 0.0051(11) C15S 0.0195(11) 0.0294(15) 0.0294(14) 0.0061(11) -0.0033(10) -0.0040(10) C16B 0.0172(11) 0.0321(14) 0.0230(12) 0.0020(11) -0.0005(9) 0.0039(10) C16S 0.0294(14) 0.0313(15) 0.0396(16) 0.0098(13) -0.0102(12) -0.0103(12) C17B 0.0127(10) 0.0292(14) 0.0168(11) 0.0018(10) -0.0010(8) -0.0011(9) C18B 0.0148(10) 0.0276(13) 0.0189(11) 0.0004(10) -0.0006(8) 0.0050(10) C19B 0.0185(11) 0.0226(14) 0.0198(12) 0.0019(10) 0.0005(8) 0.0003(9) C20B 0.0227(13) 0.0260(15) 0.0246(13) 0.0071(11) 0.0024(9) 0.0072(10) C21B 0.0307(13) 0.0217(13) 0.0290(14) 0.0076(11) 0.0037(10) 0.0037(11) C22B 0.0225(12) 0.0228(13) 0.0257(12) 0.0039(11) 0.0031(10) -0.0048(10) C23B 0.0193(11) 0.0192(12) 0.0184(11) -0.0004(9) 0.0009(8) 0.0004(9) C24B 0.0180(10) 0.0217(12) 0.0151(11) -0.0011(9) 0.0022(8) -0.0010(10) C25B 0.0163(11) 0.0206(12) 0.0253(13) 0.0020(10) 0.0003(9) -0.0016(9) C26B 0.0184(11) 0.0283(14) 0.0301(14) -0.0005(11) 0.0045(10) 0.0008(10) C27B 0.0194(12) 0.0331(15) 0.0369(15) 0.0025(12) -0.0031(10) -0.0075(11) C28B 0.0202(12) 0.0248(14) 0.0287(13) 0.0021(11) -0.0033(10) -0.0018(10) _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 C1A O1A 1.300(3) . ? C1A C6A 1.438(3) . ? C1A C2A 1.447(3) . ? C1AS N1AS 1.494(3) . ? C1AS C2AS 1.519(3) . ? N1A C7A 1.298(3) . ? N1A C13S 1.415(3) . ? N1A Zn1A 2.105(2) . ? N1AS C9AS 1.496(3) . ? N1AS C5AS 1.498(3) . ? N1AS Zn1A 2.180(2) . ? O1A Zn1A 1.9636(17) . ? Zn1A O2A 1.9811(16) . ? Zn1A N2A 2.092(2) . ? C2A C3A 1.382(4) . ? C2A C8A 1.540(3) . ? C2AS C3AS 1.530(3) . ? N2A C18A 1.306(3) . ? N2A C17A 1.418(3) . ? O2A C24A 1.297(3) . ? C3A C4A 1.409(4) . ? C3AS C4AS 1.518(4) . ? C4A C5A 1.370(4) . ? C5A C6A 1.416(4) . ? C5AS C6AS 1.525(3) . ? C6A C7A 1.426(3) . ? C6AS C7AS 1.523(3) . ? C7AS C8AS 1.530(4) . ? C8A C9A 1.532(4) . ? C8A C10A 1.536(4) . ? C8A C11A 1.545(4) . ? C9AS C10S 1.512(3) . ? C10S C11S 1.526(3) . ? C11S C12S 1.516(4) . ? C13A C14A 1.390(3) . ? C13A C13S 1.398(3) . ? C13S C17A 1.404(4) . ? C14A C15A 1.381(4) . ? C15A C16A 1.388(3) . ? C16A C17A 1.401(3) . ? C18A C19A 1.428(3) . ? C19A C20A 1.418(4) . ? C19A C24A 1.444(3) . ? C20A C21A 1.361(4) . ? C21A C22A 1.403(4) . ? C22A C23A 1.386(4) . ? C23A C24A 1.443(3) . ? C23A C25A 1.540(3) . ? C25A C26A 1.533(3) . ? C25A C27A 1.538(4) . ? C25A C28A 1.544(4) . ? C1B O1B 1.298(3) . ? C1B C6B 1.438(3) . ? C1B C2B 1.446(3) . ? C1SB N1BS 1.490(3) . ? C1SB C2SB 1.517(4) . ? N1B C7B 1.294(3) . ? N1B C12B 1.419(3) . ? N1B Zn1B 2.104(2) . ? N1BS C9SB 1.494(3) . ? N1BS C5SB 1.496(3) . ? N1BS Zn1B 2.189(2) . ? O1B Zn1B 1.9739(16) . ? Zn1B O2B 1.9728(17) . ? Zn1B N2B 2.107(2) . ? C2B C3B 1.378(3) . ? C2B C8B 1.539(3) . ? C2SB C3SB 1.526(4) . ? N2B C18B 1.292(3) . ? N2B C17B 1.418(3) . ? O2B C24B 1.296(3) . ? C3B C4B 1.409(4) . ? C3SB C4SB 1.523(4) . ? C4B C5B 1.362(4) . ? C5B C6B 1.416(4) . ? C5SB C6SB 1.519(3) . ? C6B C7B 1.432(3) . ? C6SB C7SB 1.536(4) . ? C7SB C8SB 1.504(4) . ? C8B C9B 1.534(3) . ? C8B C11B 1.541(4) . ? C8B C10B 1.542(4) . ? C9SB C14S 1.518(3) . ? C12B C13B 1.391(3) . ? C12B C17B 1.420(4) . ? C13B C14B 1.386(4) . ? C14B C15B 1.389(4) . ? C14S C15S 1.518(3) . ? C15B C16B 1.384(4) . ? C15S C16S 1.518(4) . ? C16B C17B 1.395(3) . ? C18B C19B 1.439(3) . ? C19B C20B 1.410(4) . ? C19B C24B 1.439(3) . ? C20B C21B 1.361(4) . ? C21B C22B 1.407(4) . ? C22B C23B 1.381(4) . ? C23B C24B 1.437(3) . ? C23B C25B 1.534(3) . ? C25B C26B 1.534(4) . ? C25B C27B 1.538(3) . ? C25B C28B 1.543(4) . ? 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 O1A C1A C6A 122.3(2) . . ? O1A C1A C2A 119.3(2) . . ? C6A C1A C2A 118.4(2) . . ? N1AS C1AS C2AS 116.38(19) . . ? C7A N1A C13S 121.5(2) . . ? C7A N1A Zn1A 125.66(16) . . ? C13S N1A Zn1A 112.63(16) . . ? C1AS N1AS C9AS 105.47(18) . . ? C1AS N1AS C5AS 112.76(19) . . ? C9AS N1AS C5AS 112.1(2) . . ? C1AS N1AS Zn1A 111.79(15) . . ? C9AS N1AS Zn1A 109.87(15) . . ? C5AS N1AS Zn1A 104.94(14) . . ? C1A O1A Zn1A 132.14(15) . . ? O1A Zn1A O2A 91.89(7) . . ? O1A Zn1A N2A 142.29(8) . . ? O2A Zn1A N2A 88.19(7) . . ? O1A Zn1A N1A 87.49(8) . . ? O2A Zn1A N1A 154.88(8) . . ? N2A Zn1A N1A 77.30(8) . . ? O1A Zn1A N1AS 111.82(8) . . ? O2A Zn1A N1AS 102.59(8) . . ? N2A Zn1A N1AS 104.90(8) . . ? N1A Zn1A N1AS 100.91(8) . . ? C3A C2A C1A 118.0(2) . . ? C3A C2A C8A 122.3(2) . . ? C1A C2A C8A 119.6(2) . . ? C1AS C2AS C3AS 109.98(19) . . ? C18A N2A C17A 121.2(2) . . ? C18A N2A Zn1A 125.57(16) . . ? C17A N2A Zn1A 113.04(16) . . ? C24A O2A Zn1A 132.86(15) . . ? C2A C3A C4A 123.7(2) . . ? C4AS C3AS C2AS 112.9(2) . . ? C5A C4A C3A 118.7(2) . . ? C4A C5A C6A 121.1(2) . . ? N1AS C5AS C6AS 116.35(19) . . ? C5A C6A C7A 116.2(2) . . ? C5A C6A C1A 120.0(2) . . ? C7A C6A C1A 123.7(2) . . ? C7AS C6AS C5AS 110.6(2) . . ? N1A C7A C6A 126.1(2) . . ? C6AS C7AS C8AS 112.1(2) . . ? C9A C8A C10A 107.6(2) . . ? C9A C8A C2A 111.2(2) . . ? C10A C8A C2A 108.6(2) . . ? C9A C8A C11A 108.0(2) . . ? C10A C8A C11A 109.3(2) . . ? C2A C8A C11A 112.1(2) . . ? N1AS C9AS C10S 116.29(19) . . ? C9AS C10S C11S 110.97(19) . . ? C12S C11S C10S 112.9(2) . . ? C14A C13A C13S 119.7(2) . . ? C13A C13S C17A 119.9(2) . . ? C13A C13S N1A 124.9(2) . . ? C17A C13S N1A 115.1(2) . . ? C15A C14A C13A 120.4(2) . . ? C14A C15A C16A 120.5(2) . . ? C15A C16A C17A 120.0(3) . . ? C16A C17A C13S 119.4(2) . . ? C16A C17A N2A 124.9(2) . . ? C13S C17A N2A 115.7(2) . . ? N2A C18A C19A 126.7(2) . . ? C20A C19A C18A 115.9(2) . . ? C20A C19A C24A 120.1(2) . . ? C18A C19A C24A 124.0(2) . . ? C21A C20A C19A 120.8(2) . . ? C20A C21A C22A 119.2(2) . . ? C23A C22A C21A 123.6(2) . . ? C22A C23A C24A 117.9(2) . . ? C22A C23A C25A 121.3(2) . . ? C24A C23A C25A 120.8(2) . . ? O2A C24A C23A 119.8(2) . . ? O2A C24A C19A 122.2(2) . . ? C23A C24A C19A 118.0(2) . . ? C26A C25A C27A 107.6(2) . . ? C26A C25A C23A 111.8(2) . . ? C27A C25A C23A 109.8(2) . . ? C26A C25A C28A 107.9(2) . . ? C27A C25A C28A 108.3(2) . . ? C23A C25A C28A 111.3(2) . . ? O1B C1B C6B 122.3(2) . . ? O1B C1B C2B 119.6(2) . . ? C6B C1B C2B 118.1(2) . . ? N1BS C1SB C2SB 116.62(19) . . ? C7B N1B C12B 121.0(2) . . ? C7B N1B Zn1B 126.17(16) . . ? C12B N1B Zn1B 112.74(16) . . ? C1SB N1BS C9SB 105.50(17) . . ? C1SB N1BS C5SB 112.43(19) . . ? C9SB N1BS C5SB 112.35(19) . . ? C1SB N1BS Zn1B 112.04(15) . . ? C9SB N1BS Zn1B 110.06(14) . . ? C5SB N1BS Zn1B 104.60(13) . . ? C1B O1B Zn1B 133.09(15) . . ? O2B Zn1B O1B 92.53(7) . . ? O2B Zn1B N1B 144.88(8) . . ? O1B Zn1B N1B 87.79(7) . . ? O2B Zn1B N2B 87.09(8) . . ? O1B Zn1B N2B 154.29(8) . . ? N1B Zn1B N2B 78.13(9) . . ? O2B Zn1B N1BS 110.26(8) . . ? O1B Zn1B N1BS 102.22(8) . . ? N1B Zn1B N1BS 103.94(8) . . ? N2B Zn1B N1BS 102.00(8) . . ? C3B C2B C1B 118.4(2) . . ? C3B C2B C8B 121.7(2) . . ? C1B C2B C8B 119.9(2) . . ? C1SB C2SB C3SB 109.7(2) . . ? C18B N2B C17B 121.6(2) . . ? C18B N2B Zn1B 126.01(16) . . ? C17B N2B Zn1B 112.31(16) . . ? C24B O2B Zn1B 131.69(15) . . ? C2B C3B C4B 123.3(2) . . ? C4SB C3SB C2SB 112.2(2) . . ? C5B C4B C3B 118.8(3) . . ? C4B C5B C6B 121.5(2) . . ? N1BS C5SB C6SB 116.78(19) . . ? C5B C6B C7B 116.0(2) . . ? C5B C6B C1B 119.6(2) . . ? C7B C6B C1B 124.2(2) . . ? C5SB C6SB C7SB 111.3(2) . . ? N1B C7B C6B 126.1(2) . . ? C8SB C7SB C6SB 112.5(3) . . ? C9B C8B C2B 111.8(2) . . ? C9B C8B C11B 107.2(2) . . ? C2B C8B C11B 111.94(19) . . ? C9B C8B C10B 107.4(2) . . ? C2B C8B C10B 108.6(2) . . ? C11B C8B C10B 109.9(2) . . ? N1BS C9SB C14S 116.69(18) . . ? C13B C12B N1B 125.3(2) . . ? C13B C12B C17B 119.0(2) . . ? N1B C12B C17B 115.6(2) . . ? C14B C13B C12B 120.8(3) . . ? C13B C14B C15B 120.3(2) . . ? C15S C14S C9SB 110.42(19) . . ? C16B C15B C14B 119.8(2) . . ? C14S C15S C16S 113.0(2) . . ? C15B C16B C17B 120.8(3) . . ? C16B C17B N2B 124.7(2) . . ? C16B C17B C12B 119.3(2) . . ? N2B C17B C12B 116.0(2) . . ? N2B C18B C19B 125.8(2) . . ? C20B C19B C24B 120.5(2) . . ? C20B C19B C18B 116.2(2) . . ? C24B C19B C18B 123.2(2) . . ? C21B C20B C19B 120.8(2) . . ? C20B C21B C22B 119.1(3) . . ? C23B C22B C21B 123.4(2) . . ? C22B C23B C24B 118.3(2) . . ? C22B C23B C25B 121.4(2) . . ? C24B C23B C25B 120.2(2) . . ? O2B C24B C23B 119.5(2) . . ? O2B C24B C19B 122.5(2) . . ? C23B C24B C19B 118.0(2) . . ? C23B C25B C26B 107.6(2) . . ? C23B C25B C27B 111.7(2) . . ? C26B C25B C27B 107.8(2) . . ? C23B C25B C28B 112.9(2) . . ? C26B C25B C28B 109.6(2) . . ? C27B C25B C28B 107.0(2) . . ? 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 C2AS C1AS N1AS C9AS -174.6(2) . . . . ? C2AS C1AS N1AS C5AS -51.9(3) . . . . ? C2AS C1AS N1AS Zn1A 66.0(2) . . . . ? C6A C1A O1A Zn1A 15.0(4) . . . . ? C2A C1A O1A Zn1A -165.12(17) . . . . ? C1A O1A Zn1A O2A -172.1(2) . . . . ? C1A O1A Zn1A N2A -82.7(2) . . . . ? C1A O1A Zn1A N1A -17.3(2) . . . . ? C1A O1A Zn1A N1AS 83.5(2) . . . . ? C7A N1A Zn1A O1A 7.9(2) . . . . ? C13S N1A Zn1A O1A -166.95(16) . . . . ? C7A N1A Zn1A O2A 97.1(3) . . . . ? C13S N1A Zn1A O2A -77.8(2) . . . . ? C7A N1A Zn1A N2A 153.2(2) . . . . ? C13S N1A Zn1A N2A -21.70(16) . . . . ? C7A N1A Zn1A N1AS -103.8(2) . . . . ? C13S N1A Zn1A N1AS 81.31(16) . . . . ? C1AS N1AS Zn1A O1A -64.93(15) . . . . ? C9AS N1AS Zn1A O1A 178.34(14) . . . . ? C5AS N1AS Zn1A O1A 57.62(16) . . . . ? C1AS N1AS Zn1A O2A -162.16(14) . . . . ? C9AS N1AS Zn1A O2A 81.10(15) . . . . ? C5AS N1AS Zn1A O2A -39.61(16) . . . . ? C1AS N1AS Zn1A N2A 106.35(15) . . . . ? C9AS N1AS Zn1A N2A -10.38(16) . . . . ? C5AS N1AS Zn1A N2A -131.10(15) . . . . ? C1AS N1AS Zn1A N1A 26.75(16) . . . . ? C9AS N1AS Zn1A N1A -89.99(15) . . . . ? C5AS N1AS Zn1A N1A 149.29(15) . . . . ? O1A C1A C2A C3A 177.8(2) . . . . ? C6A C1A C2A C3A -2.3(4) . . . . ? O1A C1A C2A C8A -4.8(3) . . . . ? C6A C1A C2A C8A 175.1(2) . . . . ? N1AS C1AS C2AS C3AS -160.5(2) . . . . ? O1A Zn1A N2A C18A -86.2(2) . . . . ? O2A Zn1A N2A C18A 4.5(2) . . . . ? N1A Zn1A N2A C18A -154.8(2) . . . . ? N1AS Zn1A N2A C18A 107.1(2) . . . . ? O1A Zn1A N2A C17A 88.95(19) . . . . ? O2A Zn1A N2A C17A 179.70(17) . . . . ? N1A Zn1A N2A C17A 20.35(16) . . . . ? N1AS Zn1A N2A C17A -77.74(17) . . . . ? O1A Zn1A O2A C24A 137.4(2) . . . . ? N2A Zn1A O2A C24A -4.9(2) . . . . ? N1A Zn1A O2A C24A 49.2(3) . . . . ? N1AS Zn1A O2A C24A -109.8(2) . . . . ? C1A C2A C3A C4A 2.3(4) . . . . ? C8A C2A C3A C4A -175.0(2) . . . . ? C1AS C2AS C3AS C4AS -177.0(2) . . . . ? C2A C3A C4A C5A -0.2(4) . . . . ? C3A C4A C5A C6A -1.9(4) . . . . ? C1AS N1AS C5AS C6AS -60.3(3) . . . . ? C9AS N1AS C5AS C6AS 58.5(3) . . . . ? Zn1A N1AS C5AS C6AS 177.76(19) . . . . ? C4A C5A C6A C7A 180.0(2) . . . . ? C4A C5A C6A C1A 1.8(4) . . . . ? O1A C1A C6A C5A -179.7(2) . . . . ? C2A C1A C6A C5A 0.4(4) . . . . ? O1A C1A C6A C7A 2.2(4) . . . . ? C2A C1A C6A C7A -177.7(2) . . . . ? N1AS C5AS C6AS C7AS 179.7(2) . . . . ? C13S N1A C7A C6A 177.3(2) . . . . ? Zn1A N1A C7A C6A 2.8(4) . . . . ? C5A C6A C7A N1A 171.0(2) . . . . ? C1A C6A C7A N1A -10.8(4) . . . . ? C5AS C6AS C7AS C8AS 175.1(3) . . . . ? C3A C2A C8A C9A -6.6(4) . . . . ? C1A C2A C8A C9A 176.1(3) . . . . ? C3A C2A C8A C10A 111.6(3) . . . . ? C1A C2A C8A C10A -65.7(3) . . . . ? C3A C2A C8A C11A -127.6(3) . . . . ? C1A C2A C8A C11A 55.1(3) . . . . ? C1AS N1AS C9AS C10S 173.0(2) . . . . ? C5AS N1AS C9AS C10S 49.9(3) . . . . ? Zn1A N1AS C9AS C10S -66.3(2) . . . . ? N1AS C9AS C10S C11S 164.5(2) . . . . ? C9AS C10S C11S C12S 177.9(2) . . . . ? C14A C13A C13S C17A 2.1(4) . . . . ? C14A C13A C13S N1A -179.1(2) . . . . ? C7A N1A C13S C13A 25.9(4) . . . . ? Zn1A N1A C13S C13A -159.0(2) . . . . ? C7A N1A C13S C17A -155.2(2) . . . . ? Zn1A N1A C13S C17A 19.9(3) . . . . ? C13S C13A C14A C15A -0.9(4) . . . . ? C13A C14A C15A C16A -1.3(4) . . . . ? C14A C15A C16A C17A 2.2(4) . . . . ? C15A C16A C17A C13S -1.0(4) . . . . ? C15A C16A C17A N2A -178.3(2) . . . . ? C13A C13S C17A C16A -1.2(4) . . . . ? N1A C13S C17A C16A 179.9(2) . . . . ? C13A C13S C17A N2A 176.4(2) . . . . ? N1A C13S C17A N2A -2.6(3) . . . . ? C18A N2A C17A C16A -23.4(4) . . . . ? Zn1A N2A C17A C16A 161.2(2) . . . . ? C18A N2A C17A C13S 159.2(2) . . . . ? Zn1A N2A C17A C13S -16.2(3) . . . . ? C17A N2A C18A C19A 179.4(2) . . . . ? Zn1A N2A C18A C19A -5.8(4) . . . . ? N2A C18A C19A C20A -175.3(2) . . . . ? N2A C18A C19A C24A 5.3(4) . . . . ? C18A C19A C20A C21A -179.6(2) . . . . ? C24A C19A C20A C21A -0.3(4) . . . . ? C19A C20A C21A C22A 3.7(4) . . . . ? C20A C21A C22A C23A -1.8(4) . . . . ? C21A C22A C23A C24A -3.5(4) . . . . ? C21A C22A C23A C25A 174.8(3) . . . . ? Zn1A O2A C24A C23A -173.35(17) . . . . ? Zn1A O2A C24A C19A 5.9(4) . . . . ? C22A C23A C24A O2A -174.0(2) . . . . ? C25A C23A C24A O2A 7.6(3) . . . . ? C22A C23A C24A C19A 6.7(3) . . . . ? C25A C23A C24A C19A -171.7(2) . . . . ? C20A C19A C24A O2A 175.8(2) . . . . ? C18A C19A C24A O2A -4.9(4) . . . . ? C20A C19A C24A C23A -5.0(3) . . . . ? C18A C19A C24A C23A 174.3(2) . . . . ? C22A C23A C25A C26A -4.2(4) . . . . ? C24A C23A C25A C26A 174.1(2) . . . . ? C22A C23A C25A C27A -123.6(3) . . . . ? C24A C23A C25A C27A 54.7(3) . . . . ? C22A C23A C25A C28A 116.5(3) . . . . ? C24A C23A C25A C28A -65.1(3) . . . . ? C2SB C1SB N1BS C9SB 172.8(2) . . . . ? C2SB C1SB N1BS C5SB 50.0(3) . . . . ? C2SB C1SB N1BS Zn1B -67.5(2) . . . . ? C6B C1B O1B Zn1B -3.6(4) . . . . ? C2B C1B O1B Zn1B 173.97(17) . . . . ? C1B O1B Zn1B O2B -144.5(2) . . . . ? C1B O1B Zn1B N1B 0.4(2) . . . . ? C1B O1B Zn1B N2B -55.9(3) . . . . ? C1B O1B Zn1B N1BS 104.2(2) . . . . ? C7B N1B Zn1B O2B 91.0(2) . . . . ? C12B N1B Zn1B O2B -86.23(19) . . . . ? C7B N1B Zn1B O1B -0.3(2) . . . . ? C12B N1B Zn1B O1B -177.49(17) . . . . ? C7B N1B Zn1B N2B 158.1(2) . . . . ? C12B N1B Zn1B N2B -19.13(16) . . . . ? C7B N1B Zn1B N1BS -102.3(2) . . . . ? C12B N1B Zn1B N1BS 80.47(17) . . . . ? C1SB N1BS Zn1B O2B 63.47(15) . . . . ? C9SB N1BS Zn1B O2B -179.49(13) . . . . ? C5SB N1BS Zn1B O2B -58.59(16) . . . . ? C1SB N1BS Zn1B O1B 160.83(14) . . . . ? C9SB N1BS Zn1B O1B -82.13(14) . . . . ? C5SB N1BS Zn1B O1B 38.77(16) . . . . ? C1SB N1BS Zn1B N1B -108.42(15) . . . . ? C9SB N1BS Zn1B N1B 8.63(16) . . . . ? C5SB N1BS Zn1B N1B 129.52(15) . . . . ? C1SB N1BS Zn1B N2B -27.86(16) . . . . ? C9SB N1BS Zn1B N2B 89.19(15) . . . . ? C5SB N1BS Zn1B N2B -149.91(15) . . . . ? O1B C1B C2B C3B 176.3(2) . . . . ? C6B C1B C2B C3B -6.0(3) . . . . ? O1B C1B C2B C8B -6.4(4) . . . . ? C6B C1B C2B C8B 171.3(2) . . . . ? N1BS C1SB C2SB C3SB 159.7(2) . . . . ? O2B Zn1B N2B C18B -9.4(2) . . . . ? O1B Zn1B N2B C18B -99.2(3) . . . . ? N1B Zn1B N2B C18B -157.3(2) . . . . ? N1BS Zn1B N2B C18B 100.7(2) . . . . ? O2B Zn1B N2B C17B 167.69(17) . . . . ? O1B Zn1B N2B C17B 77.9(2) . . . . ? N1B Zn1B N2B C17B 19.74(16) . . . . ? N1BS Zn1B N2B C17B -82.21(17) . . . . ? O1B Zn1B O2B C24B 174.9(2) . . . . ? N1B Zn1B O2B C24B 85.1(2) . . . . ? N2B Zn1B O2B C24B 20.6(2) . . . . ? N1BS Zn1B O2B C24B -81.1(2) . . . . ? C1B C2B C3B C4B 2.3(4) . . . . ? C8B C2B C3B C4B -174.9(2) . . . . ? C1SB C2SB C3SB C4SB 177.0(2) . . . . ? C2B C3B C4B C5B 2.2(4) . . . . ? C3B C4B C5B C6B -2.9(4) . . . . ? C1SB N1BS C5SB C6SB 62.2(3) . . . . ? C9SB N1BS C5SB C6SB -56.6(3) . . . . ? Zn1B N1BS C5SB C6SB -175.95(19) . . . . ? C4B C5B C6B C7B 175.3(2) . . . . ? C4B C5B C6B C1B -1.0(4) . . . . ? O1B C1B C6B C5B -177.0(2) . . . . ? C2B C1B C6B C5B 5.4(3) . . . . ? O1B C1B C6B C7B 7.1(4) . . . . ? C2B C1B C6B C7B -170.5(2) . . . . ? N1BS C5SB C6SB C7SB 176.7(2) . . . . ? C12B N1B C7B C6B -179.4(2) . . . . ? Zn1B N1B C7B C6B 3.6(4) . . . . ? C5B C6B C7B N1B 176.6(2) . . . . ? C1B C6B C7B N1B -7.3(4) . . . . ? C5SB C6SB C7SB C8SB -162.9(3) . . . . ? C3B C2B C8B C9B -0.7(3) . . . . ? C1B C2B C8B C9B -177.9(2) . . . . ? C3B C2B C8B C11B -121.0(3) . . . . ? C1B C2B C8B C11B 61.9(3) . . . . ? C3B C2B C8B C10B 117.5(3) . . . . ? C1B C2B C8B C10B -59.7(3) . . . . ? C1SB N1BS C9SB C14S -170.7(2) . . . . ? C5SB N1BS C9SB C14S -47.8(3) . . . . ? Zn1B N1BS C9SB C14S 68.3(2) . . . . ? C7B N1B C12B C13B 22.1(4) . . . . ? Zn1B N1B C12B C13B -160.5(2) . . . . ? C7B N1B C12B C17B -161.7(2) . . . . ? Zn1B N1B C12B C17B 15.7(3) . . . . ? N1B C12B C13B C14B 176.6(2) . . . . ? C17B C12B C13B C14B 0.5(4) . . . . ? C12B C13B C14B C15B -1.2(4) . . . . ? N1BS C9SB C14S C15S -165.6(2) . . . . ? C13B C14B C15B C16B 0.4(4) . . . . ? C9SB C14S C15S C16S -174.7(2) . . . . ? C14B C15B C16B C17B 0.9(4) . . . . ? C15B C16B C17B N2B -178.3(2) . . . . ? C15B C16B C17B C12B -1.6(4) . . . . ? C18B N2B C17B C16B -23.6(4) . . . . ? Zn1B N2B C17B C16B 159.2(2) . . . . ? C18B N2B C17B C12B 159.6(2) . . . . ? Zn1B N2B C17B C12B -17.7(3) . . . . ? C13B C12B C17B C16B 0.8(3) . . . . ? N1B C12B C17B C16B -175.7(2) . . . . ? C13B C12B C17B N2B 177.8(2) . . . . ? N1B C12B C17B N2B 1.4(3) . . . . ? C17B N2B C18B C19B 179.7(2) . . . . ? Zn1B N2B C18B C19B -3.5(4) . . . . ? N2B C18B C19B C20B -170.0(3) . . . . ? N2B C18B C19B C24B 13.0(4) . . . . ? C24B C19B C20B C21B -1.4(4) . . . . ? C18B C19B C20B C21B -178.5(3) . . . . ? C19B C20B C21B C22B 1.9(4) . . . . ? C20B C21B C22B C23B 0.0(4) . . . . ? C21B C22B C23B C24B -2.5(4) . . . . ? C21B C22B C23B C25B 173.9(2) . . . . ? Zn1B O2B C24B C23B 163.70(17) . . . . ? Zn1B O2B C24B C19B -18.0(4) . . . . ? C22B C23B C24B O2B -178.7(2) . . . . ? C25B C23B C24B O2B 4.9(3) . . . . ? C22B C23B C24B C19B 2.9(3) . . . . ? C25B C23B C24B C19B -173.5(2) . . . . ? C20B C19B C24B O2B -179.4(2) . . . . ? C18B C19B C24B O2B -2.5(4) . . . . ? C20B C19B C24B C23B -1.1(4) . . . . ? C18B C19B C24B C23B 175.8(2) . . . . ? C22B C23B C25B C26B -108.1(3) . . . . ? C24B C23B C25B C26B 68.2(3) . . . . ? C22B C23B C25B C27B 10.1(3) . . . . ? C24B C23B C25B C27B -173.6(2) . . . . ? C22B C23B C25B C28B 130.8(3) . . . . ? C24B C23B C25B C28B -52.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.579 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.055 # Attachment 'da146-4.cif' data_da146-4 _database_code_depnum_ccdc_archive 'CCDC 760570' #TrackingRef 'da146-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H99 Cl2 N5 O5 Zn2' _chemical_formula_weight 1328.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.195(5) _cell_length_b 24.208(5) _cell_length_c 24.371(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13685(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7345 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 28.47 _exptl_crystal_description neddle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5648 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; TWINABS Version 2008/4 Bruker AXS Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 16000 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1912 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 28.47 _reflns_number_total 16000 _reflns_number_gt 6395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0181P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16000 _refine_ls_number_parameters 800 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _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 C1A C 0.83574(19) 0.13881(12) 0.19665(14) 0.0222(9) Uani 1 1 d . . . C1B C 0.8177(2) 0.32819(14) 0.11699(14) 0.0264(9) Uani 1 1 d . . . N1A N 0.92516(15) 0.17605(10) 0.27721(11) 0.0220(7) Uani 1 1 d . . . N1B N 0.83789(16) 0.30617(10) 0.23557(11) 0.0235(8) Uani 1 1 d . . . O1 O 0.94114(13) 0.24799(8) 0.16720(9) 0.0278(7) Uani 1 1 d . . . H1 H 0.9421 0.2488 0.1348 0.033 Uiso 1 1 d R . . O1A O 0.88600(13) 0.13286(9) 0.17592(9) 0.0266(7) Uani 1 1 d . . . O1B O 0.86584(13) 0.34857(9) 0.13305(9) 0.0278(7) Uani 1 1 d . . . Zn1A Zn 0.95534(2) 0.174685(14) 0.196473(15) 0.02161(11) Uani 1 1 d . . . Zn1B Zn 0.91467(2) 0.319462(14) 0.193353(15) 0.02130(11) Uani 1 1 d . . . C2A C 0.7849(2) 0.12862(13) 0.16282(15) 0.0281(10) Uani 1 1 d . . . C2B C 0.7974(2) 0.33773(14) 0.06139(14) 0.0308(10) Uani 1 1 d . . . N2A N 1.03270(16) 0.18524(10) 0.24160(11) 0.0244(8) Uani 1 1 d . . . N2B N 0.93997(16) 0.32761(10) 0.27665(11) 0.0225(7) Uani 1 1 d . . . O2A O 1.00616(12) 0.14040(8) 0.14002(8) 0.0221(6) Uani 1 1 d . . . O2B O 0.98347(13) 0.36632(8) 0.17734(9) 0.0228(6) Uani 1 1 d . . . C3A C 0.7324(2) 0.13086(13) 0.18743(15) 0.0301(10) Uani 1 1 d . . . H3A H 0.6995 0.1235 0.1655 0.036 Uiso 1 1 calc R . . C3B C 0.7450(2) 0.31778(15) 0.04698(15) 0.0359(11) Uani 1 1 d . . . H3B H 0.7321 0.3241 0.0105 0.043 Uiso 1 1 calc R . . C4A C 0.7235(2) 0.14328(13) 0.24299(15) 0.0327(11) Uani 1 1 d . . . H4A H 0.6858 0.1431 0.2582 0.039 Uiso 1 1 calc R . . C4B C 0.7085(2) 0.28846(15) 0.08226(16) 0.0384(11) Uani 1 1 d . . . H4B H 0.6718 0.2759 0.0703 0.046 Uiso 1 1 calc R . . C5A C 0.7703(2) 0.15569(13) 0.27467(15) 0.0283(10) Uani 1 1 d . . . H5A H 0.7650 0.1649 0.3122 0.034 Uiso 1 1 calc R . . C5B C 0.7274(2) 0.27842(14) 0.13479(15) 0.0323(11) Uani 1 1 d . . . H5B H 0.7036 0.2578 0.1590 0.039 Uiso 1 1 calc R . . C6A C 0.8262(2) 0.15502(13) 0.25268(14) 0.0263(10) Uani 1 1 d . . . C6B C 0.77990(19) 0.29741(13) 0.15317(14) 0.0236(9) Uani 1 1 d . . . C7A C 0.8721(2) 0.17048(13) 0.28933(14) 0.0266(10) Uani 1 1 d . . . H7A H 0.8617 0.1772 0.3264 0.032 Uiso 1 1 calc R . . C7B C 0.79250(19) 0.28914(13) 0.20956(14) 0.0250(9) Uani 1 1 d . . . H7B H 0.7649 0.2691 0.2303 0.030 Uiso 1 1 calc R . . C8A C 0.7921(2) 0.11863(15) 0.10100(15) 0.0356(11) Uani 1 1 d . . . C8B C 0.8361(2) 0.36874(15) 0.02061(15) 0.0350(11) Uani 1 1 d . . . C9A C 0.8185(2) 0.17084(15) 0.07471(14) 0.0397(12) Uani 1 1 d . . . H9A1 H 0.8252 0.1642 0.0356 0.060 Uiso 1 1 calc R . . H9A2 H 0.8552 0.1794 0.0927 0.060 Uiso 1 1 calc R . . H9A3 H 0.7920 0.2020 0.0792 0.060 Uiso 1 1 calc R . . C9B C 0.8080(3) 0.37208(18) -0.03630(15) 0.0504(14) Uani 1 1 d . . . H9B1 H 0.8010 0.3347 -0.0502 0.076 Uiso 1 1 calc R . . H9B2 H 0.8338 0.3917 -0.0615 0.076 Uiso 1 1 calc R . . H9B3 H 0.7713 0.3920 -0.0336 0.076 Uiso 1 1 calc R . . C10A C 0.8328(2) 0.06890(15) 0.08933(16) 0.0449(13) Uani 1 1 d . . . H10C H 0.8359 0.0632 0.0496 0.067 Uiso 1 1 calc R . . H10D H 0.8171 0.0355 0.1065 0.067 Uiso 1 1 calc R . . H10E H 0.8711 0.0766 0.1045 0.067 Uiso 1 1 calc R . . C10B C 0.8454(2) 0.42804(15) 0.04076(16) 0.0487(14) Uani 1 1 d . . . H10F H 0.8079 0.4463 0.0451 0.073 Uiso 1 1 calc R . . H10G H 0.8687 0.4483 0.0139 0.073 Uiso 1 1 calc R . . H10H H 0.8654 0.4274 0.0761 0.073 Uiso 1 1 calc R . . C11A C 0.7345(2) 0.10726(19) 0.07277(16) 0.0536(14) Uani 1 1 d . . . H11C H 0.7096 0.1398 0.0762 0.080 Uiso 1 1 calc R . . H11D H 0.7158 0.0755 0.0902 0.080 Uiso 1 1 calc R . . H11E H 0.7412 0.0993 0.0339 0.080 Uiso 1 1 calc R . . C11B C 0.8927(2) 0.33901(18) 0.01383(16) 0.0481(13) Uani 1 1 d . . . H11F H 0.9130 0.3381 0.0491 0.072 Uiso 1 1 calc R . . H11G H 0.9164 0.3585 -0.0133 0.072 Uiso 1 1 calc R . . H11H H 0.8856 0.3012 0.0013 0.072 Uiso 1 1 calc R . . C12A C 0.9673(2) 0.18889(12) 0.31722(14) 0.0250(10) Uani 1 1 d . . . C12B C 0.8415(2) 0.30594(12) 0.29332(13) 0.0238(9) Uani 1 1 d . . . C13A C 0.9561(2) 0.19562(13) 0.37324(14) 0.0313(10) Uani 1 1 d . . . H13A H 0.9178 0.1922 0.3866 0.038 Uiso 1 1 calc R . . C13B C 0.7946(2) 0.29849(14) 0.32808(15) 0.0303(10) Uani 1 1 d . . . H13B H 0.7575 0.2911 0.3133 0.036 Uiso 1 1 calc R . . C14A C 1.0008(2) 0.20732(14) 0.40918(15) 0.0327(11) Uani 1 1 d . . . H14A H 0.9930 0.2123 0.4471 0.039 Uiso 1 1 calc R . . C14B C 0.8022(2) 0.30184(15) 0.38377(16) 0.0387(12) Uani 1 1 d . . . H14B H 0.7704 0.2953 0.4075 0.046 Uiso 1 1 calc R . . C15A C 1.0564(2) 0.21169(13) 0.39017(15) 0.0333(11) Uani 1 1 d . . . H15A H 1.0868 0.2195 0.4151 0.040 Uiso 1 1 calc R . . C15B C 0.8547(2) 0.31448(17) 0.40561(16) 0.0438(12) Uani 1 1 d . . . H15B H 0.8590 0.3177 0.4442 0.053 Uiso 1 1 calc R . . C16A C 1.0685(2) 0.20484(12) 0.33532(14) 0.0264(10) Uani 1 1 d . . . H16A H 1.1071 0.2074 0.3226 0.032 Uiso 1 1 calc R . . C16B C 0.9015(2) 0.32256(15) 0.37182(14) 0.0337(10) Uani 1 1 d . . . H16B H 0.9380 0.3312 0.3871 0.040 Uiso 1 1 calc R . . C17A C 1.0239(2) 0.19416(12) 0.29844(14) 0.0248(10) Uani 1 1 d . . . C17B C 0.89526(19) 0.31813(13) 0.31525(14) 0.0237(9) Uani 1 1 d . . . C18A C 1.07892(19) 0.20034(12) 0.21631(14) 0.0225(9) Uani 1 1 d . . . H18A H 1.1072 0.2192 0.2373 0.027 Uiso 1 1 calc R . . C18B C 0.99308(19) 0.32887(12) 0.29085(13) 0.0224(9) Uani 1 1 d . . . H18B H 1.0017 0.3218 0.3283 0.027 Uiso 1 1 calc R . . C19A C 1.09135(19) 0.19146(12) 0.16025(14) 0.0224(9) Uani 1 1 d . . . C19B C 1.0407(2) 0.34008(12) 0.25484(13) 0.0226(9) Uani 1 1 d . . . C20A C 1.1442(2) 0.21163(13) 0.14099(15) 0.0290(10) Uani 1 1 d . . . H20A H 1.1698 0.2290 0.1660 0.035 Uiso 1 1 calc R . . C20B C 1.0958(2) 0.33557(12) 0.27775(15) 0.0250(9) Uani 1 1 d . . . H20B H 1.0998 0.3264 0.3155 0.030 Uiso 1 1 calc R . . C21A C 1.1600(2) 0.20700(13) 0.08718(15) 0.0321(10) Uani 1 1 d . . . H21A H 1.1965 0.2197 0.0748 0.038 Uiso 1 1 calc R . . C21B C 1.1440(2) 0.34414(13) 0.24664(14) 0.0294(10) Uani 1 1 d . . . H21B H 1.1813 0.3425 0.2626 0.035 Uiso 1 1 calc R . . C22A C 1.1204(2) 0.18276(14) 0.05070(14) 0.0308(10) Uani 1 1 d . . . H22A H 1.1304 0.1809 0.0130 0.037 Uiso 1 1 calc R . . C22B C 1.1370(2) 0.35544(12) 0.19052(15) 0.0290(10) Uani 1 1 d . . . H22B H 1.1707 0.3600 0.1689 0.035 Uiso 1 1 calc R . . C23A C 1.0688(2) 0.16195(13) 0.06618(14) 0.0256(10) Uani 1 1 d . . . C23B C 1.0848(2) 0.36030(12) 0.16517(14) 0.0256(9) Uani 1 1 d . . . C24A C 1.05278(19) 0.16409(12) 0.12326(14) 0.0225(9) Uani 1 1 d . . . C24B C 1.03373(19) 0.35572(12) 0.19800(14) 0.0223(9) Uani 1 1 d . . . C25A C 1.0253(2) 0.13911(14) 0.02403(14) 0.0293(10) Uani 1 1 d . . . C25B C 1.0801(2) 0.37003(14) 0.10319(14) 0.0316(10) Uani 1 1 d . . . C26A C 1.0116(2) 0.07772(13) 0.03572(15) 0.0382(12) Uani 1 1 d . . . H26A H 1.0470 0.0559 0.0328 0.057 Uiso 1 1 calc R . . H26B H 0.9834 0.0643 0.0090 0.057 Uiso 1 1 calc R . . H26C H 0.9958 0.0741 0.0728 0.057 Uiso 1 1 calc R . . C26B C 1.1379(2) 0.37124(16) 0.07479(15) 0.0422(12) Uani 1 1 d . . . H26D H 1.1607 0.4023 0.0889 0.063 Uiso 1 1 calc R . . H26E H 1.1322 0.3757 0.0352 0.063 Uiso 1 1 calc R . . H26F H 1.1584 0.3366 0.0819 0.063 Uiso 1 1 calc R . . C27A C 1.0491(2) 0.14272(15) -0.03421(14) 0.0406(12) Uani 1 1 d . . . H27A H 1.0594 0.1811 -0.0425 0.061 Uiso 1 1 calc R . . H27B H 1.0197 0.1300 -0.0602 0.061 Uiso 1 1 calc R . . H27C H 1.0834 0.1194 -0.0373 0.061 Uiso 1 1 calc R . . C27B C 1.0485(2) 0.42544(13) 0.09150(15) 0.0374(12) Uani 1 1 d . . . H27D H 1.0697 0.4558 0.1088 0.056 Uiso 1 1 calc R . . H27E H 1.0094 0.4238 0.1065 0.056 Uiso 1 1 calc R . . H27F H 1.0466 0.4316 0.0518 0.056 Uiso 1 1 calc R . . C28A C 0.9697(2) 0.17186(16) 0.02662(15) 0.0379(11) Uani 1 1 d . . . H28A H 0.9524 0.1678 0.0631 0.057 Uiso 1 1 calc R . . H28B H 0.9428 0.1580 -0.0012 0.057 Uiso 1 1 calc R . . H28C H 0.9778 0.2109 0.0196 0.057 Uiso 1 1 calc R . . C28B C 1.0449(2) 0.32258(14) 0.07711(14) 0.0322(10) Uani 1 1 d . . . H28D H 1.0437 0.3275 0.0372 0.048 Uiso 1 1 calc R . . H28E H 1.0056 0.3230 0.0918 0.048 Uiso 1 1 calc R . . H28F H 1.0632 0.2871 0.0858 0.048 Uiso 1 1 calc R . . C1S C 0.88546(19) 0.53756(12) 0.30489(13) 0.0280(10) Uani 1 1 d . . . H1S1 H 0.9112 0.5691 0.3130 0.034 Uiso 1 1 calc R . . H1S2 H 0.8479 0.5529 0.2932 0.034 Uiso 1 1 calc R . . N1S N 0.91095(16) 0.50539(10) 0.25698(11) 0.0257(8) Uani 1 1 d . . . C2S C 0.8763(2) 0.50513(14) 0.35751(13) 0.0342(11) Uani 1 1 d . . . H2S1 H 0.9140 0.4933 0.3725 0.041 Uiso 1 1 calc R . . H2S2 H 0.8531 0.4717 0.3497 0.041 Uiso 1 1 calc R . . C3S C 0.8451(2) 0.54102(15) 0.39952(15) 0.0415(12) Uani 1 1 d . . . H3S1 H 0.8693 0.5736 0.4083 0.050 Uiso 1 1 calc R . . H3S2 H 0.8085 0.5545 0.3835 0.050 Uiso 1 1 calc R . . C4S C 0.8325(3) 0.50945(18) 0.45154(16) 0.0585(16) Uani 1 1 d . . . H4S1 H 0.8049 0.4799 0.4437 0.088 Uiso 1 1 calc R . . H4S2 H 0.8162 0.5346 0.4790 0.088 Uiso 1 1 calc R . . H4S3 H 0.8683 0.4934 0.4657 0.088 Uiso 1 1 calc R . . C5S C 0.8702(2) 0.46003(13) 0.23860(14) 0.0286(10) Uani 1 1 d . . . H5S1 H 0.8905 0.4367 0.2114 0.034 Uiso 1 1 calc R . . H5S2 H 0.8612 0.4365 0.2707 0.034 Uiso 1 1 calc R . . C6S C 0.8142(2) 0.47907(15) 0.21355(16) 0.0351(11) Uani 1 1 d . . . H6S1 H 0.7966 0.5077 0.2372 0.042 Uiso 1 1 calc R . . H6S2 H 0.8218 0.4957 0.1772 0.042 Uiso 1 1 calc R . . C7S C 0.7734(2) 0.43215(16) 0.20731(18) 0.0463(13) Uani 1 1 d . . . H7S1 H 0.7582 0.4220 0.2439 0.056 Uiso 1 1 calc R . . H7S2 H 0.7947 0.3999 0.1927 0.056 Uiso 1 1 calc R . . C8S C 0.7235(2) 0.44478(17) 0.16973(18) 0.0524(14) Uani 1 1 d . . . H8S1 H 0.6983 0.4722 0.1871 0.079 Uiso 1 1 calc R . . H8S2 H 0.7016 0.4109 0.1627 0.079 Uiso 1 1 calc R . . H8S3 H 0.7381 0.4595 0.1350 0.079 Uiso 1 1 calc R . . C9S C 0.96720(19) 0.47849(13) 0.27297(14) 0.0264(10) Uani 1 1 d . . . H9S1 H 0.9810 0.4560 0.2417 0.032 Uiso 1 1 calc R . . H9S2 H 0.9600 0.4531 0.3041 0.032 Uiso 1 1 calc R . . C10S C 1.0143(2) 0.51841(13) 0.28919(14) 0.0292(10) Uani 1 1 d . . . H10A H 1.0003 0.5424 0.3193 0.035 Uiso 1 1 calc R . . H10B H 1.0240 0.5422 0.2575 0.035 Uiso 1 1 calc R . . C11S C 1.0676(2) 0.48770(13) 0.30779(14) 0.0302(10) Uani 1 1 d . . . H11A H 1.0998 0.5143 0.3109 0.036 Uiso 1 1 calc R . . H11B H 1.0781 0.4604 0.2793 0.036 Uiso 1 1 calc R . . C12S C 1.0608(2) 0.45771(15) 0.36259(14) 0.0382(12) Uani 1 1 d . . . H12A H 1.0453 0.4833 0.3900 0.057 Uiso 1 1 calc R . . H12B H 1.0984 0.4440 0.3748 0.057 Uiso 1 1 calc R . . H12C H 1.0342 0.4266 0.3581 0.057 Uiso 1 1 calc R . . C13S C 0.9195(2) 0.54665(12) 0.21085(13) 0.0283(10) Uani 1 1 d . . . H13C H 0.8816 0.5631 0.2016 0.034 Uiso 1 1 calc R . . H13D H 0.9446 0.5768 0.2243 0.034 Uiso 1 1 calc R . . C14S C 0.9457(2) 0.52307(13) 0.15916(14) 0.0325(11) Uani 1 1 d . . . H14C H 0.9221 0.4917 0.1460 0.039 Uiso 1 1 calc R . . H14D H 0.9850 0.5092 0.1670 0.039 Uiso 1 1 calc R . . C15S C 0.9484(2) 0.56754(14) 0.11501(15) 0.0414(13) Uani 1 1 d . . . H15C H 0.9087 0.5805 0.1075 0.050 Uiso 1 1 calc R . . H15D H 0.9704 0.5993 0.1297 0.050 Uiso 1 1 calc R . . C16S C 0.9743(3) 0.55098(17) 0.06378(16) 0.0626(19) Uani 1 1 d . . . H16C H 1.0131 0.5365 0.0707 0.094 Uiso 1 1 calc R . . H16D H 0.9768 0.5829 0.0392 0.094 Uiso 1 1 calc R . . H16E H 0.9507 0.5222 0.0466 0.094 Uiso 1 1 calc R . . C1C C 1.1617(3) 0.5119(2) 0.1983(2) 0.084(2) Uani 1 1 d . . . H1CA H 1.1758 0.5346 0.2293 0.101 Uiso 1 1 calc R . . H1CB H 1.1441 0.4779 0.2136 0.101 Uiso 1 1 calc R . . Cl1C Cl 1.10931(8) 0.54952(5) 0.16046(6) 0.0831(5) Uani 1 1 d . . . Cl2C Cl 1.21938(9) 0.49420(7) 0.15581(6) 0.0942(5) 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 C1A 0.025(3) 0.0193(16) 0.0221(19) 0.0025(15) 0.003(2) -0.0017(15) C1B 0.025(3) 0.0279(19) 0.026(2) -0.0020(16) -0.0027(19) 0.0043(18) N1A 0.022(2) 0.0234(14) 0.0206(16) 0.0004(12) -0.0035(15) -0.0008(14) N1B 0.024(2) 0.0242(15) 0.0219(16) 0.0024(11) -0.0009(15) 0.0005(14) O1 0.042(2) 0.0274(12) 0.0144(11) 0.0006(10) -0.0002(13) 0.0003(11) O1A 0.027(2) 0.0292(13) 0.0232(14) -0.0055(10) 0.0038(13) -0.0016(12) O1B 0.022(2) 0.0367(14) 0.0246(14) 0.0060(10) -0.0058(13) -0.0083(12) Zn1A 0.0229(3) 0.02363(19) 0.0183(2) -0.00100(17) 0.0019(2) -0.00061(18) Zn1B 0.0213(3) 0.02296(19) 0.0197(2) -0.00079(17) -0.0024(2) -0.00017(18) C2A 0.029(3) 0.0256(19) 0.030(2) -0.0028(15) 0.000(2) -0.0052(17) C2B 0.031(3) 0.035(2) 0.027(2) -0.0010(16) -0.005(2) -0.0044(19) N2A 0.029(3) 0.0231(15) 0.0211(16) 0.0001(12) 0.0003(15) 0.0020(14) N2B 0.025(2) 0.0212(14) 0.0214(16) -0.0032(12) 0.0010(15) -0.0021(14) O2A 0.0215(19) 0.0231(12) 0.0217(13) -0.0025(9) 0.0018(12) -0.0026(11) O2B 0.0209(19) 0.0239(12) 0.0234(13) 0.0018(9) -0.0021(12) 0.0015(11) C3A 0.027(3) 0.0309(19) 0.032(2) 0.0008(16) -0.006(2) -0.0056(17) C3B 0.031(3) 0.050(2) 0.027(2) 0.0020(19) -0.009(2) -0.004(2) C4A 0.029(3) 0.031(2) 0.038(2) 0.0061(17) 0.007(2) -0.0045(19) C4B 0.027(3) 0.050(2) 0.038(2) 0.0029(19) -0.008(2) -0.007(2) C5A 0.032(3) 0.0268(19) 0.026(2) 0.0030(15) 0.005(2) 0.0038(18) C5B 0.033(3) 0.032(2) 0.032(2) 0.0030(16) -0.001(2) -0.0054(18) C6A 0.030(3) 0.0235(18) 0.025(2) 0.0019(14) 0.0046(19) -0.0039(17) C6B 0.023(3) 0.0281(18) 0.0199(19) -0.0002(15) -0.0030(18) -0.0027(17) C7A 0.038(3) 0.0218(18) 0.0194(19) 0.0015(14) 0.0071(19) -0.0007(18) C7B 0.023(3) 0.0197(18) 0.033(2) 0.0018(14) 0.0030(19) 0.0015(16) C8A 0.037(4) 0.040(2) 0.029(2) -0.0011(17) -0.002(2) -0.003(2) C8B 0.036(4) 0.045(2) 0.024(2) 0.0085(17) -0.008(2) -0.006(2) C9A 0.041(4) 0.051(2) 0.027(2) 0.0031(18) 0.006(2) 0.002(2) C9B 0.046(4) 0.079(3) 0.027(2) 0.016(2) -0.005(2) -0.013(3) C10A 0.049(4) 0.047(2) 0.039(2) -0.0143(19) -0.003(2) 0.001(2) C10B 0.055(4) 0.053(3) 0.038(3) 0.017(2) -0.006(3) -0.011(2) C11A 0.039(4) 0.088(3) 0.033(3) -0.011(2) -0.010(2) -0.004(3) C11B 0.036(4) 0.078(3) 0.030(2) 0.004(2) 0.001(2) 0.001(3) C12A 0.034(3) 0.0163(17) 0.025(2) 0.0007(13) 0.0015(19) 0.0006(16) C12B 0.029(3) 0.0212(17) 0.021(2) 0.0001(13) 0.0023(18) 0.0019(16) C13A 0.035(3) 0.037(2) 0.022(2) -0.0039(16) 0.003(2) -0.0023(19) C13B 0.024(3) 0.038(2) 0.029(2) -0.0015(16) 0.002(2) 0.0024(18) C14A 0.038(4) 0.041(2) 0.019(2) -0.0026(16) 0.001(2) 0.002(2) C14B 0.034(4) 0.053(2) 0.029(2) -0.0012(18) 0.007(2) 0.002(2) C15A 0.046(4) 0.027(2) 0.026(2) -0.0013(15) -0.010(2) -0.0026(19) C15B 0.043(4) 0.069(3) 0.020(2) -0.0076(19) 0.006(2) 0.003(3) C16A 0.028(3) 0.0233(18) 0.028(2) 0.0007(15) -0.0030(19) -0.0041(16) C16B 0.026(3) 0.054(2) 0.021(2) -0.0042(18) -0.0027(18) 0.001(2) C17A 0.038(3) 0.0167(16) 0.020(2) -0.0008(14) -0.0014(19) 0.0034(16) C17B 0.025(3) 0.0214(17) 0.024(2) -0.0033(14) -0.0001(17) 0.0047(16) C18A 0.024(3) 0.0157(16) 0.028(2) -0.0003(13) -0.0024(19) 0.0001(16) C18B 0.028(3) 0.0181(17) 0.0210(19) -0.0063(13) -0.0018(17) 0.0020(16) C19A 0.026(3) 0.0162(16) 0.0247(19) 0.0036(13) 0.0033(19) 0.0008(15) C19B 0.026(3) 0.0187(16) 0.0225(19) -0.0030(13) -0.0051(18) -0.0009(16) C20A 0.027(3) 0.0249(19) 0.035(2) -0.0048(15) 0.001(2) -0.0014(17) C20B 0.026(3) 0.0237(18) 0.025(2) 0.0001(14) -0.0060(19) 0.0020(16) C21A 0.027(3) 0.031(2) 0.038(2) 0.0000(17) 0.010(2) -0.0043(18) C21B 0.027(3) 0.0275(19) 0.034(2) -0.0025(15) -0.006(2) 0.0011(18) C22A 0.038(3) 0.030(2) 0.024(2) 0.0000(16) 0.009(2) 0.0040(19) C22B 0.027(3) 0.0246(18) 0.035(2) -0.0022(16) 0.004(2) -0.0061(16) C23A 0.031(3) 0.0216(18) 0.024(2) 0.0017(14) 0.0051(19) 0.0065(17) C23B 0.030(3) 0.0181(17) 0.029(2) -0.0009(14) -0.001(2) -0.0010(17) C24A 0.021(3) 0.0194(17) 0.027(2) 0.0006(14) 0.0026(18) 0.0038(15) C24B 0.024(3) 0.0187(16) 0.0240(19) -0.0025(15) 0.0001(19) -0.0026(15) C25A 0.032(3) 0.032(2) 0.023(2) -0.0008(16) 0.0055(19) 0.0026(18) C25B 0.030(3) 0.036(2) 0.028(2) 0.0040(16) 0.004(2) -0.0010(19) C26A 0.048(4) 0.035(2) 0.031(2) -0.0071(16) -0.002(2) -0.008(2) C26B 0.040(4) 0.058(3) 0.028(2) 0.0049(19) 0.001(2) -0.006(2) C27A 0.047(4) 0.048(2) 0.027(2) -0.0021(17) 0.000(2) 0.004(2) C27B 0.051(4) 0.030(2) 0.032(2) 0.0075(16) 0.003(2) 0.001(2) C28A 0.033(3) 0.054(2) 0.026(2) 0.0002(18) -0.001(2) 0.004(2) C28B 0.032(3) 0.038(2) 0.027(2) -0.0014(16) -0.0023(19) 0.004(2) C1S 0.034(3) 0.0197(16) 0.030(2) -0.0015(15) 0.001(2) 0.0030(16) N1S 0.027(2) 0.0204(14) 0.0299(17) 0.0030(12) -0.0013(16) -0.0021(14) C2S 0.040(4) 0.034(2) 0.029(2) 0.0018(16) 0.005(2) -0.0007(19) C3S 0.044(4) 0.043(2) 0.037(2) 0.0002(18) 0.007(2) -0.004(2) C4S 0.064(5) 0.073(3) 0.039(3) 0.004(2) 0.016(3) -0.019(3) C5S 0.032(3) 0.0247(18) 0.029(2) 0.0045(15) -0.0055(19) -0.0058(18) C6S 0.030(3) 0.035(2) 0.040(2) -0.0062(16) -0.002(2) -0.0014(19) C7S 0.042(4) 0.038(2) 0.059(3) 0.0085(19) -0.007(2) 0.003(2) C8S 0.043(4) 0.051(3) 0.063(3) 0.010(2) -0.014(3) -0.001(2) C9S 0.029(3) 0.0241(18) 0.026(2) 0.0040(15) -0.0015(19) 0.0031(17) C10S 0.034(3) 0.0239(18) 0.030(2) 0.0032(14) -0.0014(19) -0.0050(17) C11S 0.031(3) 0.0260(18) 0.033(2) -0.0040(16) -0.003(2) -0.0034(17) C12S 0.041(4) 0.041(2) 0.032(2) 0.0047(17) -0.005(2) 0.000(2) C13S 0.039(3) 0.0160(16) 0.030(2) 0.0055(14) -0.0033(19) -0.0010(17) C14S 0.037(3) 0.032(2) 0.028(2) -0.0003(16) -0.001(2) -0.0035(19) C15S 0.056(4) 0.036(2) 0.033(2) 0.0058(17) 0.002(2) -0.006(2) C16S 0.103(6) 0.049(3) 0.036(3) 0.006(2) -0.001(3) -0.011(3) C1C 0.109(8) 0.080(4) 0.063(4) 0.011(3) 0.026(4) 0.015(4) Cl1C 0.0765(15) 0.0677(8) 0.1051(11) -0.0321(8) 0.0099(10) -0.0184(8) Cl2C 0.0614(16) 0.1338(13) 0.0873(11) -0.0017(9) 0.0125(10) -0.0208(10) _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 C1A O1A 1.279(5) . ? C1A C6A 1.438(5) . ? C1A C2A 1.459(6) . ? C1B O1B 1.281(5) . ? C1B C6B 1.450(5) . ? C1B C2B 1.453(5) . ? N1A C7A 1.274(5) . ? N1A C12A 1.416(5) . ? N1A Zn1A 2.089(3) . ? N1B C7B 1.296(5) . ? N1B C12B 1.410(4) . ? N1B Zn1B 2.082(4) . ? O1 Zn1A 1.941(2) . ? O1 Zn1B 1.943(2) . ? O1A Zn1A 1.965(3) . ? O1B Zn1B 1.985(3) . ? Zn1A O2A 1.993(2) . ? Zn1A N2A 2.120(3) . ? Zn1B O2B 1.996(3) . ? Zn1B N2B 2.122(3) . ? C2A C3A 1.359(6) . ? C2A C8A 1.535(5) . ? C2B C3B 1.356(6) . ? C2B C8B 1.534(6) . ? N2A C18A 1.290(5) . ? N2A C17A 1.417(4) . ? N2B C18B 1.280(5) . ? N2B C17B 1.419(5) . ? O2A C24A 1.291(4) . ? O2B C24B 1.295(5) . ? C3A C4A 1.402(5) . ? C3B C4B 1.399(6) . ? C4A C5A 1.366(6) . ? C4B C5B 1.375(5) . ? C5A C6A 1.403(6) . ? C5B C6B 1.376(6) . ? C6A C7A 1.438(6) . ? C6B C7B 1.419(5) . ? C8A C11A 1.528(7) . ? C8A C9A 1.544(5) . ? C8A C10A 1.557(6) . ? C8B C11B 1.507(7) . ? C8B C10B 1.532(5) . ? C8B C9B 1.534(5) . ? C12A C17A 1.396(6) . ? C12A C13A 1.400(4) . ? C12B C13B 1.389(6) . ? C12B C17B 1.389(6) . ? C13A C14A 1.387(6) . ? C13B C14B 1.371(5) . ? C14A C15A 1.375(6) . ? C14B C15B 1.364(7) . ? C15A C16A 1.376(5) . ? C15B C16B 1.376(6) . ? C16A C17A 1.393(5) . ? C16B C17B 1.390(4) . ? C18A C19A 1.413(5) . ? C18B C19B 1.436(5) . ? C19A C20A 1.401(6) . ? C19A C24A 1.432(5) . ? C19B C20B 1.400(6) . ? C19B C24B 1.445(5) . ? C20A C21A 1.366(5) . ? C20B C21B 1.366(6) . ? C21A C22A 1.407(6) . ? C21B C22B 1.404(5) . ? C22A C23A 1.351(6) . ? C22B C23B 1.364(6) . ? C23A C24A 1.441(5) . ? C23A C25A 1.542(6) . ? C23B C24B 1.434(6) . ? C23B C25B 1.533(5) . ? C25A C28A 1.516(6) . ? C25A C27A 1.525(5) . ? C25A C26A 1.546(5) . ? C25B C26B 1.510(6) . ? C25B C28B 1.546(5) . ? C25B C27B 1.555(5) . ? C1S C2S 1.519(4) . ? C1S N1S 1.523(4) . ? N1S C9S 1.510(5) . ? N1S C5S 1.516(5) . ? N1S C13S 1.517(4) . ? C2S C3S 1.525(5) . ? C3S C4S 1.509(5) . ? C5S C6S 1.509(6) . ? C6S C7S 1.485(6) . ? C7S C8S 1.508(6) . ? C9S C10S 1.511(5) . ? C10S C11S 1.513(6) . ? C11S C12S 1.529(4) . ? C13S C14S 1.511(5) . ? C14S C15S 1.524(4) . ? C15S C16S 1.442(5) . ? C1C Cl2C 1.745(6) . ? C1C Cl1C 1.778(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 O1A C1A C6A 123.1(4) . . ? O1A C1A C2A 119.6(3) . . ? C6A C1A C2A 117.3(4) . . ? O1B C1B C6B 122.6(3) . . ? O1B C1B C2B 120.4(3) . . ? C6B C1B C2B 116.9(4) . . ? C7A N1A C12A 122.1(3) . . ? C7A N1A Zn1A 122.7(3) . . ? C12A N1A Zn1A 114.9(3) . . ? C7B N1B C12B 122.3(3) . . ? C7B N1B Zn1B 120.1(2) . . ? C12B N1B Zn1B 116.3(3) . . ? Zn1A O1 Zn1B 138.34(12) . . ? C1A O1A Zn1A 126.0(2) . . ? C1B O1B Zn1B 125.9(2) . . ? O1 Zn1A O1A 103.79(11) . . ? O1 Zn1A O2A 103.15(9) . . ? O1A Zn1A O2A 95.36(10) . . ? O1 Zn1A N1A 105.96(10) . . ? O1A Zn1A N1A 88.50(12) . . ? O2A Zn1A N1A 148.79(10) . . ? O1 Zn1A N2A 102.96(11) . . ? O1A Zn1A N2A 152.49(10) . . ? O2A Zn1A N2A 84.71(11) . . ? N1A Zn1A N2A 78.06(13) . . ? O1 Zn1B O1B 104.69(10) . . ? O1 Zn1B O2B 100.91(11) . . ? O1B Zn1B O2B 96.30(10) . . ? O1 Zn1B N1B 107.14(11) . . ? O1B Zn1B N1B 86.14(12) . . ? O2B Zn1B N1B 150.26(10) . . ? O1 Zn1B N2B 108.01(10) . . ? O1B Zn1B N2B 146.41(11) . . ? O2B Zn1B N2B 85.02(11) . . ? N1B Zn1B N2B 77.18(13) . . ? C3A C2A C1A 117.9(4) . . ? C3A C2A C8A 122.4(4) . . ? C1A C2A C8A 119.6(4) . . ? C3B C2B C1B 118.4(4) . . ? C3B C2B C8B 122.1(3) . . ? C1B C2B C8B 119.5(4) . . ? C18A N2A C17A 122.9(3) . . ? C18A N2A Zn1A 119.3(2) . . ? C17A N2A Zn1A 113.8(3) . . ? C18B N2B C17B 121.9(3) . . ? C18B N2B Zn1B 121.8(3) . . ? C17B N2B Zn1B 114.7(3) . . ? C24A O2A Zn1A 121.94(19) . . ? C24B O2B Zn1B 122.1(2) . . ? C2A C3A C4A 124.5(4) . . ? C2B C3B C4B 124.3(4) . . ? C5A C4A C3A 118.4(4) . . ? C5B C4B C3B 118.0(4) . . ? C4A C5A C6A 121.1(4) . . ? C4B C5B C6B 121.8(4) . . ? C5A C6A C1A 120.5(4) . . ? C5A C6A C7A 116.3(3) . . ? C1A C6A C7A 123.2(4) . . ? C5B C6B C7B 116.8(4) . . ? C5B C6B C1B 120.6(3) . . ? C7B C6B C1B 122.5(4) . . ? N1A C7A C6A 126.8(3) . . ? N1B C7B C6B 126.6(4) . . ? C11A C8A C2A 112.1(4) . . ? C11A C8A C9A 107.9(3) . . ? C2A C8A C9A 108.7(3) . . ? C11A C8A C10A 108.0(3) . . ? C2A C8A C10A 111.5(3) . . ? C9A C8A C10A 108.4(4) . . ? C11B C8B C10B 111.1(4) . . ? C11B C8B C9B 107.2(4) . . ? C10B C8B C9B 107.5(3) . . ? C11B C8B C2B 110.3(3) . . ? C10B C8B C2B 109.4(3) . . ? C9B C8B C2B 111.3(4) . . ? C17A C12A C13A 119.0(4) . . ? C17A C12A N1A 116.4(3) . . ? C13A C12A N1A 124.7(4) . . ? C13B C12B C17B 119.7(3) . . ? C13B C12B N1B 124.3(4) . . ? C17B C12B N1B 115.8(4) . . ? C14A C13A C12A 120.0(4) . . ? C14B C13B C12B 119.7(4) . . ? C15A C14A C13A 120.3(4) . . ? C15B C14B C13B 120.9(4) . . ? C14A C15A C16A 120.6(4) . . ? C14B C15B C16B 120.1(4) . . ? C15A C16A C17A 119.9(4) . . ? C15B C16B C17B 120.1(4) . . ? C16A C17A C12A 120.2(3) . . ? C16A C17A N2A 123.5(4) . . ? C12A C17A N2A 116.2(4) . . ? C12B C17B C16B 119.4(4) . . ? C12B C17B N2B 115.8(3) . . ? C16B C17B N2B 124.7(4) . . ? N2A C18A C19A 126.1(4) . . ? N2B C18B C19B 125.4(3) . . ? C20A C19A C18A 116.7(3) . . ? C20A C19A C24A 119.8(3) . . ? C18A C19A C24A 123.5(4) . . ? C20B C19B C18B 116.4(3) . . ? C20B C19B C24B 120.3(4) . . ? C18B C19B C24B 123.3(4) . . ? C21A C20A C19A 121.8(4) . . ? C21B C20B C19B 120.9(4) . . ? C20A C21A C22A 117.8(4) . . ? C20B C21B C22B 118.4(4) . . ? C23A C22A C21A 123.9(3) . . ? C23B C22B C21B 124.1(4) . . ? C22A C23A C24A 119.0(4) . . ? C22A C23A C25A 121.8(3) . . ? C24A C23A C25A 119.2(4) . . ? C22B C23B C24B 118.3(3) . . ? C22B C23B C25B 121.6(4) . . ? C24B C23B C25B 120.2(4) . . ? O2A C24A C19A 122.0(3) . . ? O2A C24A C23A 120.4(3) . . ? C19A C24A C23A 117.6(4) . . ? O2B C24B C23B 120.8(3) . . ? O2B C24B C19B 121.7(4) . . ? C23B C24B C19B 117.6(4) . . ? C28A C25A C27A 108.5(3) . . ? C28A C25A C23A 110.0(3) . . ? C27A C25A C23A 111.3(4) . . ? C28A C25A C26A 108.7(4) . . ? C27A C25A C26A 107.5(3) . . ? C23A C25A C26A 110.9(3) . . ? C26B C25B C23B 113.0(4) . . ? C26B C25B C28B 107.2(3) . . ? C23B C25B C28B 109.2(3) . . ? C26B C25B C27B 108.5(3) . . ? C23B C25B C27B 110.3(3) . . ? C28B C25B C27B 108.5(4) . . ? C2S C1S N1S 115.9(3) . . ? C9S N1S C5S 107.6(3) . . ? C9S N1S C13S 111.3(3) . . ? C5S N1S C13S 109.8(3) . . ? C9S N1S C1S 111.0(3) . . ? C5S N1S C1S 110.8(3) . . ? C13S N1S C1S 106.4(2) . . ? C1S C2S C3S 109.8(3) . . ? C4S C3S C2S 111.6(3) . . ? C6S C5S N1S 115.8(3) . . ? C7S C6S C5S 110.9(3) . . ? C6S C7S C8S 113.3(3) . . ? N1S C9S C10S 114.6(3) . . ? C9S C10S C11S 110.8(3) . . ? C10S C11S C12S 114.2(4) . . ? C14S C13S N1S 114.9(3) . . ? C13S C14S C15S 109.8(3) . . ? C16S C15S C14S 115.6(3) . . ? Cl2C C1C Cl1C 110.0(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 C6A C1A O1A Zn1A -31.6(4) . . . . ? C2A C1A O1A Zn1A 148.8(2) . . . . ? C6B C1B O1B Zn1B 27.8(5) . . . . ? C2B C1B O1B Zn1B -155.4(3) . . . . ? Zn1B O1 Zn1A O1A 99.4(2) . . . . ? Zn1B O1 Zn1A O2A -161.6(2) . . . . ? Zn1B O1 Zn1A N1A 7.0(3) . . . . ? Zn1B O1 Zn1A N2A -74.1(3) . . . . ? C1A O1A Zn1A O1 -71.3(3) . . . . ? C1A O1A Zn1A O2A -176.2(3) . . . . ? C1A O1A Zn1A N1A 34.8(3) . . . . ? C1A O1A Zn1A N2A 94.9(3) . . . . ? C7A N1A Zn1A O1 80.7(3) . . . . ? C12A N1A Zn1A O1 -93.6(2) . . . . ? C7A N1A Zn1A O1A -23.2(3) . . . . ? C12A N1A Zn1A O1A 162.5(2) . . . . ? C7A N1A Zn1A O2A -121.1(3) . . . . ? C12A N1A Zn1A O2A 64.6(3) . . . . ? C7A N1A Zn1A N2A -179.1(3) . . . . ? C12A N1A Zn1A N2A 6.7(2) . . . . ? Zn1A O1 Zn1B O1B -141.7(2) . . . . ? Zn1A O1 Zn1B O2B 118.8(2) . . . . ? Zn1A O1 Zn1B N1B -51.2(3) . . . . ? Zn1A O1 Zn1B N2B 30.5(3) . . . . ? C1B O1B Zn1B O1 66.2(3) . . . . ? C1B O1B Zn1B O2B 169.2(3) . . . . ? C1B O1B Zn1B N1B -40.5(3) . . . . ? C1B O1B Zn1B N2B -100.3(3) . . . . ? C7B N1B Zn1B O1 -66.1(3) . . . . ? C12B N1B Zn1B O1 101.8(2) . . . . ? C7B N1B Zn1B O1B 38.1(3) . . . . ? C12B N1B Zn1B O1B -154.1(2) . . . . ? C7B N1B Zn1B O2B 134.0(3) . . . . ? C12B N1B Zn1B O2B -58.1(3) . . . . ? C7B N1B Zn1B N2B -171.2(3) . . . . ? C12B N1B Zn1B N2B -3.4(2) . . . . ? O1A C1A C2A C3A 174.6(3) . . . . ? C6A C1A C2A C3A -5.0(5) . . . . ? O1A C1A C2A C8A -8.3(5) . . . . ? C6A C1A C2A C8A 172.1(3) . . . . ? O1B C1B C2B C3B -176.7(4) . . . . ? C6B C1B C2B C3B 0.3(5) . . . . ? O1B C1B C2B C8B 4.5(5) . . . . ? C6B C1B C2B C8B -178.4(3) . . . . ? O1 Zn1A N2A C18A -61.7(3) . . . . ? O1A Zn1A N2A C18A 132.1(3) . . . . ? O2A Zn1A N2A C18A 40.7(2) . . . . ? N1A Zn1A N2A C18A -165.5(3) . . . . ? O1 Zn1A N2A C17A 96.8(2) . . . . ? O1A Zn1A N2A C17A -69.5(3) . . . . ? O2A Zn1A N2A C17A -160.9(2) . . . . ? N1A Zn1A N2A C17A -7.09(19) . . . . ? O1 Zn1B N2B C18B 63.8(3) . . . . ? O1B Zn1B N2B C18B -130.0(3) . . . . ? O2B Zn1B N2B C18B -36.1(3) . . . . ? N1B Zn1B N2B C18B 167.9(3) . . . . ? O1 Zn1B N2B C17B -101.7(2) . . . . ? O1B Zn1B N2B C17B 64.5(3) . . . . ? O2B Zn1B N2B C17B 158.4(2) . . . . ? N1B Zn1B N2B C17B 2.4(2) . . . . ? O1 Zn1A O2A C24A 52.7(3) . . . . ? O1A Zn1A O2A C24A 158.2(3) . . . . ? N1A Zn1A O2A C24A -105.8(3) . . . . ? N2A Zn1A O2A C24A -49.4(3) . . . . ? O1 Zn1B O2B C24B -58.6(3) . . . . ? O1B Zn1B O2B C24B -164.9(2) . . . . ? N1B Zn1B O2B C24B 101.8(3) . . . . ? N2B Zn1B O2B C24B 48.8(2) . . . . ? C1A C2A C3A C4A 1.2(5) . . . . ? C8A C2A C3A C4A -175.8(3) . . . . ? C1B C2B C3B C4B 0.2(6) . . . . ? C8B C2B C3B C4B 178.9(4) . . . . ? C2A C3A C4A C5A 2.1(5) . . . . ? C2B C3B C4B C5B -1.1(7) . . . . ? C3A C4A C5A C6A -1.3(5) . . . . ? C3B C4B C5B C6B 1.5(6) . . . . ? C4A C5A C6A C1A -2.8(5) . . . . ? C4A C5A C6A C7A 178.1(3) . . . . ? O1A C1A C6A C5A -173.8(3) . . . . ? C2A C1A C6A C5A 5.9(5) . . . . ? O1A C1A C6A C7A 5.3(5) . . . . ? C2A C1A C6A C7A -175.0(3) . . . . ? C4B C5B C6B C7B 174.2(3) . . . . ? C4B C5B C6B C1B -1.0(6) . . . . ? O1B C1B C6B C5B 177.1(4) . . . . ? C2B C1B C6B C5B 0.1(5) . . . . ? O1B C1B C6B C7B 2.1(6) . . . . ? C2B C1B C6B C7B -174.8(3) . . . . ? C12A N1A C7A C6A -176.9(3) . . . . ? Zn1A N1A C7A C6A 9.3(5) . . . . ? C5A C6A C7A N1A -175.3(3) . . . . ? C1A C6A C7A N1A 5.6(5) . . . . ? C12B N1B C7B C6B 166.8(3) . . . . ? Zn1B N1B C7B C6B -26.1(5) . . . . ? C5B C6B C7B N1B -176.3(4) . . . . ? C1B C6B C7B N1B -1.3(6) . . . . ? C3A C2A C8A C11A -4.5(5) . . . . ? C1A C2A C8A C11A 178.5(3) . . . . ? C3A C2A C8A C9A 114.7(4) . . . . ? C1A C2A C8A C9A -62.2(5) . . . . ? C3A C2A C8A C10A -125.8(4) . . . . ? C1A C2A C8A C10A 57.3(4) . . . . ? C3B C2B C8B C11B -120.2(5) . . . . ? C1B C2B C8B C11B 58.5(5) . . . . ? C3B C2B C8B C10B 117.3(4) . . . . ? C1B C2B C8B C10B -64.0(5) . . . . ? C3B C2B C8B C9B -1.3(6) . . . . ? C1B C2B C8B C9B 177.3(4) . . . . ? C7A N1A C12A C17A -179.7(3) . . . . ? Zn1A N1A C12A C17A -5.4(3) . . . . ? C7A N1A C12A C13A 1.4(5) . . . . ? Zn1A N1A C12A C13A 175.6(2) . . . . ? C7B N1B C12B C13B -13.4(5) . . . . ? Zn1B N1B C12B C13B 179.1(3) . . . . ? C7B N1B C12B C17B 171.5(3) . . . . ? Zn1B N1B C12B C17B 3.9(4) . . . . ? C17A C12A C13A C14A 0.0(5) . . . . ? N1A C12A C13A C14A 178.9(3) . . . . ? C17B C12B C13B C14B -1.7(5) . . . . ? N1B C12B C13B C14B -176.6(3) . . . . ? C12A C13A C14A C15A -0.8(5) . . . . ? C12B C13B C14B C15B 2.5(6) . . . . ? C13A C14A C15A C16A 0.4(5) . . . . ? C13B C14B C15B C16B -1.8(6) . . . . ? C14A C15A C16A C17A 0.9(5) . . . . ? C14B C15B C16B C17B 0.3(6) . . . . ? C15A C16A C17A C12A -1.8(5) . . . . ? C15A C16A C17A N2A -178.4(3) . . . . ? C13A C12A C17A C16A 1.3(5) . . . . ? N1A C12A C17A C16A -177.8(3) . . . . ? C13A C12A C17A N2A 178.2(3) . . . . ? N1A C12A C17A N2A -0.9(4) . . . . ? C18A N2A C17A C16A -19.1(5) . . . . ? Zn1A N2A C17A C16A -176.7(2) . . . . ? C18A N2A C17A C12A 164.1(3) . . . . ? Zn1A N2A C17A C12A 6.6(3) . . . . ? C13B C12B C17B C16B 0.2(5) . . . . ? N1B C12B C17B C16B 175.5(3) . . . . ? C13B C12B C17B N2B -177.2(3) . . . . ? N1B C12B C17B N2B -1.8(4) . . . . ? C15B C16B C17B C12B 0.5(5) . . . . ? C15B C16B C17B N2B 177.6(3) . . . . ? C18B N2B C17B C12B -166.6(3) . . . . ? Zn1B N2B C17B C12B -1.1(4) . . . . ? C18B N2B C17B C16B 16.2(5) . . . . ? Zn1B N2B C17B C16B -178.3(3) . . . . ? C17A N2A C18A C19A 178.1(3) . . . . ? Zn1A N2A C18A C19A -25.5(4) . . . . ? C17B N2B C18B C19B -177.7(3) . . . . ? Zn1B N2B C18B C19B 17.8(4) . . . . ? N2A C18A C19A C20A 179.6(3) . . . . ? N2A C18A C19A C24A 0.5(5) . . . . ? N2B C18B C19B C20B -175.5(3) . . . . ? N2B C18B C19B C24B 5.0(5) . . . . ? C18A C19A C20A C21A -177.8(3) . . . . ? C24A C19A C20A C21A 1.4(5) . . . . ? C18B C19B C20B C21B 178.5(3) . . . . ? C24B C19B C20B C21B -2.0(5) . . . . ? C19A C20A C21A C22A 2.1(5) . . . . ? C19B C20B C21B C22B -2.5(5) . . . . ? C20A C21A C22A C23A -2.7(6) . . . . ? C20B C21B C22B C23B 2.3(5) . . . . ? C21A C22A C23A C24A -0.3(6) . . . . ? C21A C22A C23A C25A 176.1(3) . . . . ? C21B C22B C23B C24B 2.5(5) . . . . ? C21B C22B C23B C25B -177.1(3) . . . . ? Zn1A O2A C24A C19A 41.6(4) . . . . ? Zn1A O2A C24A C23A -140.7(2) . . . . ? C20A C19A C24A O2A 173.5(3) . . . . ? C18A C19A C24A O2A -7.4(5) . . . . ? C20A C19A C24A C23A -4.3(5) . . . . ? C18A C19A C24A C23A 174.9(3) . . . . ? C22A C23A C24A O2A -174.1(3) . . . . ? C25A C23A C24A O2A 9.4(5) . . . . ? C22A C23A C24A C19A 3.7(5) . . . . ? C25A C23A C24A C19A -172.8(3) . . . . ? Zn1B O2B C24B C23B 138.1(2) . . . . ? Zn1B O2B C24B C19B -43.2(4) . . . . ? C22B C23B C24B O2B 172.0(3) . . . . ? C25B C23B C24B O2B -8.5(5) . . . . ? C22B C23B C24B C19B -6.8(4) . . . . ? C25B C23B C24B C19B 172.8(3) . . . . ? C20B C19B C24B O2B -172.0(3) . . . . ? C18B C19B C24B O2B 7.4(5) . . . . ? C20B C19B C24B C23B 6.7(4) . . . . ? C18B C19B C24B C23B -173.9(3) . . . . ? C22A C23A C25A C28A -119.2(4) . . . . ? C24A C23A C25A C28A 57.2(4) . . . . ? C22A C23A C25A C27A 1.0(5) . . . . ? C24A C23A C25A C27A 177.4(3) . . . . ? C22A C23A C25A C26A 120.6(4) . . . . ? C24A C23A C25A C26A -63.0(4) . . . . ? C22B C23B C25B C26B 2.1(5) . . . . ? C24B C23B C25B C26B -177.4(3) . . . . ? C22B C23B C25B C28B 121.3(4) . . . . ? C24B C23B C25B C28B -58.3(4) . . . . ? C22B C23B C25B C27B -119.5(4) . . . . ? C24B C23B C25B C27B 60.9(4) . . . . ? C2S C1S N1S C9S -55.4(4) . . . . ? C2S C1S N1S C5S 64.1(4) . . . . ? C2S C1S N1S C13S -176.6(4) . . . . ? N1S C1S C2S C3S -174.3(4) . . . . ? C1S C2S C3S C4S 177.2(4) . . . . ? C9S N1S C5S C6S -172.0(3) . . . . ? C13S N1S C5S C6S -50.7(4) . . . . ? C1S N1S C5S C6S 66.5(4) . . . . ? N1S C5S C6S C7S -168.9(3) . . . . ? C5S C6S C7S C8S -165.0(4) . . . . ? C5S N1S C9S C10S 176.4(3) . . . . ? C13S N1S C9S C10S 56.1(4) . . . . ? C1S N1S C9S C10S -62.2(4) . . . . ? N1S C9S C10S C11S 176.5(3) . . . . ? C9S C10S C11S C12S -69.7(4) . . . . ? C9S N1S C13S C14S 58.0(4) . . . . ? C5S N1S C13S C14S -61.1(5) . . . . ? C1S N1S C13S C14S 179.0(4) . . . . ? N1S C13S C14S C15S 176.4(4) . . . . ? C13S C14S C15S C16S 178.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.879 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.086