Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Youngmee Kim' _publ_contact_author_address ; Division of Nano Sciences Ewha Womans University 11-1 Daehyn-dong, Seodaemun-gu Seoul 120-750 SOUTH KOREA ; _publ_contact_author_email YMEEKIM@EWHA.AC.KR _publ_section_title ; Construction of interpenetrated 3-D network by [2 + 2] cycloaddition of Zn(ClO4)2 and 1,2-trans-(4-pyridyl)ethene: Counteranion Effects ; loop_ _publ_author_name 'Youngmee Kim' 'Sung Jin Hong' 'Cheal Kim' 'Jun Yong Lee' data_[{Zn(H2O)3(bpe)2}2(bpe)](NO3)4(4bpe)(14H2O) _database_code_depnum_ccdc_archive 'CCDC 260338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H130 N22 O32 Zn2' _chemical_formula_weight 2379.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4958(15) _cell_length_b 15.296(2) _cell_length_c 19.225(3) _cell_angle_alpha 104.723(2) _cell_angle_beta 92.725(2) _cell_angle_gamma 98.389(2) _cell_volume 2941.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5155 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.07 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17817 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.05 _reflns_number_total 12420 _reflns_number_gt 7361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12420 _refine_ls_number_parameters 760 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 1.729 _refine_ls_shift/su_mean 0.002 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 0.19874(3) 0.49563(2) 0.307713(19) 0.04383(14) Uani 1 1 d . . . O1 O 0.1009(2) 0.4731(2) 0.39781(14) 0.0646(6) Uani 1 1 d D . . H1 H 0.143(3) 0.463(3) 0.4321(14) 0.077 Uiso 1 1 d D . . H2 H 0.0239(12) 0.479(3) 0.405(2) 0.077 Uiso 1 1 d D . . O2 O 0.0201(2) 0.53059(16) 0.27837(13) 0.0566(6) Uani 1 1 d D . . H3 H -0.012(3) 0.522(2) 0.2359(7) 0.068 Uiso 1 1 d D . . H4 H 0.009(3) 0.5771(15) 0.3103(14) 0.068 Uiso 1 1 d D . . O3 O 0.3668(2) 0.46670(16) 0.35640(15) 0.0598(6) Uani 1 1 d D . . H5 H 0.4400(15) 0.499(2) 0.361(2) 0.072 Uiso 1 1 d D . . H6 H 0.358(4) 0.435(2) 0.3860(15) 0.072 Uiso 1 1 d D . . N1 N 0.2825(3) 0.51071(17) 0.20946(14) 0.0491(6) Uani 1 1 d . . . C11 C 0.4053(3) 0.5498(2) 0.2092(2) 0.0582(9) Uani 1 1 d . . . H11 H 0.4526 0.5805 0.2530 0.070 Uiso 1 1 calc R . . C12 C 0.4649(4) 0.5457(3) 0.1445(3) 0.0795(14) Uani 1 1 d . . . H12 H 0.5505 0.5731 0.1463 0.095 Uiso 1 1 calc R . . C13 C 0.3961(4) 0.5007(3) 0.0775(2) 0.0656(10) Uiso 1 1 d D . . C14 C 0.2731(4) 0.4633(3) 0.0806(2) 0.0705(10) Uiso 1 1 d . . . H14 H 0.2234 0.4325 0.0376 0.085 Uiso 1 1 calc R . . C15 C 0.2183(4) 0.4686(2) 0.14404(18) 0.0583(9) Uani 1 1 d . . . H15 H 0.1323 0.4420 0.1423 0.070 Uiso 1 1 calc R . . C16 C 0.4454(5) 0.4889(4) 0.0090(2) 0.1042(16) Uiso 1 1 d D . . H16 H 0.3845 0.4589 -0.0296 0.125 Uiso 1 1 calc R . . N21 N 0.2633(2) 0.63718(16) 0.36255(13) 0.0430(6) Uani 1 1 d . . . C21 C 0.2968(3) 0.6660(2) 0.43446(17) 0.0468(7) Uani 1 1 d . . . H21 H 0.3062 0.6222 0.4593 0.056 Uiso 1 1 calc R . . C22 C 0.3175(3) 0.7560(2) 0.47248(17) 0.0493(8) Uani 1 1 d . . . H22 H 0.3375 0.7722 0.5222 0.059 Uiso 1 1 calc R . . C23 C 0.3085(3) 0.8237(2) 0.43637(17) 0.0429(7) Uani 1 1 d . . . C24 C 0.2780(3) 0.7944(2) 0.36273(17) 0.0456(7) Uani 1 1 d . . . H24 H 0.2726 0.8370 0.3362 0.055 Uiso 1 1 calc R . . C25 C 0.2557(3) 0.7026(2) 0.32853(17) 0.0462(7) Uani 1 1 d . . . H25 H 0.2341 0.6848 0.2789 0.055 Uiso 1 1 calc R . . C26 C 0.3257(3) 0.9224(2) 0.47239(18) 0.0503(8) Uani 1 1 d . . . H26 H 0.3218 0.9607 0.4419 0.060 Uiso 1 1 calc R . . C27 C 0.3457(3) 0.9639(2) 0.54165(18) 0.0499(8) Uani 1 1 d . . . H27 H 0.3516 0.9273 0.5733 0.060 Uiso 1 1 calc R . . C28 C 0.3593(3) 1.0624(2) 0.57304(17) 0.0444(7) Uani 1 1 d . . . C29 C 0.3838(3) 1.0998(2) 0.64751(18) 0.0527(8) Uani 1 1 d . . . H29 H 0.3914 1.0618 0.6778 0.063 Uiso 1 1 calc R . . C210 C 0.3965(3) 1.1935(2) 0.6762(2) 0.0585(9) Uani 1 1 d . . . H210 H 0.4113 1.2165 0.7261 0.070 Uiso 1 1 calc R . . N22 N 0.3888(3) 1.25294(18) 0.63652(17) 0.0558(7) Uani 1 1 d . . . C211 C 0.3638(3) 1.2165(2) 0.5653(2) 0.0555(8) Uani 1 1 d . . . H211 H 0.3556 1.2561 0.5364 0.067 Uiso 1 1 calc R . . C212 C 0.3495(3) 1.1246(2) 0.53221(18) 0.0523(8) Uani 1 1 d . . . H212 H 0.3331 1.1038 0.4823 0.063 Uiso 1 1 calc R . . N31 N 0.1446(2) 0.35155(17) 0.25270(14) 0.0495(6) Uani 1 1 d . . . C31 C 0.2334(3) 0.3025(2) 0.22306(18) 0.0528(8) Uani 1 1 d . . . H31 H 0.3189 0.3313 0.2277 0.063 Uiso 1 1 calc R . . C32 C 0.2039(3) 0.2112(2) 0.18598(18) 0.0550(8) Uani 1 1 d . . . H32 H 0.2687 0.1800 0.1660 0.066 Uiso 1 1 calc R . . C33 C 0.0778(3) 0.1658(2) 0.17842(18) 0.0549(8) Uani 1 1 d . . . C34 C -0.0129(3) 0.2163(2) 0.20922(19) 0.0591(9) Uani 1 1 d . . . H34 H -0.0988 0.1888 0.2058 0.071 Uiso 1 1 calc R . . C35 C 0.0228(3) 0.3067(2) 0.24479(19) 0.0568(9) Uani 1 1 d . . . H35 H -0.0410 0.3390 0.2647 0.068 Uiso 1 1 calc R . . C36 C 0.0354(4) 0.0696(3) 0.1366(2) 0.0658(10) Uani 1 1 d . . . H36 H -0.0490 0.0432 0.1400 0.079 Uiso 1 1 calc R . . C37 C 0.1059(4) 0.0186(3) 0.0955(2) 0.0675(10) Uani 1 1 d . . . H37 H 0.1914 0.0446 0.0946 0.081 Uiso 1 1 calc R . . C38 C 0.0650(4) -0.0761(2) 0.05010(19) 0.0571(9) Uani 1 1 d . . . C39 C 0.1524(4) -0.1207(3) 0.0103(2) 0.0691(10) Uani 1 1 d . . . H39 H 0.2369 -0.0913 0.0115 0.083 Uiso 1 1 calc R . . C310 C 0.1149(5) -0.2082(3) -0.0312(2) 0.0789(12) Uani 1 1 d . . . H310 H 0.1764 -0.2365 -0.0576 0.095 Uiso 1 1 calc R . . N32 N -0.0022(4) -0.2555(2) -0.03654(19) 0.0788(10) Uani 1 1 d . . . C311 C -0.0870(4) -0.2120(3) 0.0002(2) 0.0721(11) Uani 1 1 d . . . H311 H -0.1711 -0.2430 -0.0035 0.087 Uiso 1 1 calc R . . C312 C -0.0594(4) -0.1229(2) 0.0443(2) 0.0643(10) Uani 1 1 d . . . H312 H -0.1233 -0.0955 0.0692 0.077 Uiso 1 1 calc R . . N41 N 0.2168(4) 0.6916(2) 0.10157(19) 0.0760(9) Uani 1 1 d . . . C41 C 0.3377(4) 0.7372(3) 0.1119(2) 0.0738(11) Uani 1 1 d . . . H41 H 0.4015 0.7082 0.0883 0.089 Uiso 1 1 calc R . . C42 C 0.3722(4) 0.8234(3) 0.1548(2) 0.0685(10) Uani 1 1 d . . . H42 H 0.4576 0.8523 0.1590 0.082 Uiso 1 1 calc R . . C43 C 0.2824(4) 0.8690(2) 0.1924(2) 0.0610(9) Uani 1 1 d . . . C44 C 0.1564(4) 0.8217(3) 0.1832(2) 0.0668(10) Uani 1 1 d . . . H44 H 0.0914 0.8486 0.2072 0.080 Uiso 1 1 calc R . . C45 C 0.1295(4) 0.7347(3) 0.1379(2) 0.0736(11) Uani 1 1 d . . . H45 H 0.0449 0.7040 0.1323 0.088 Uiso 1 1 calc R . . C46 C 0.3246(4) 0.9635(3) 0.2395(2) 0.0692(10) Uani 1 1 d . . . H46 H 0.4109 0.9890 0.2403 0.083 Uiso 1 1 calc R . . C47 C 0.2523(4) 1.0137(3) 0.2796(2) 0.0723(11) Uani 1 1 d . . . H47 H 0.1681 0.9862 0.2820 0.087 Uiso 1 1 calc R . . C48 C 0.2897(4) 1.1088(2) 0.3213(2) 0.0611(9) Uani 1 1 d . . . C49 C 0.4158(4) 1.1561(3) 0.3308(2) 0.0685(10) Uani 1 1 d . . . H49 H 0.4832 1.1263 0.3128 0.082 Uiso 1 1 calc R . . C410 C 0.4393(4) 1.2478(3) 0.3672(2) 0.0769(11) Uani 1 1 d . . . H410 H 0.5240 1.2784 0.3731 0.092 Uiso 1 1 calc R . . N42 N 0.3474(3) 1.2958(2) 0.39481(19) 0.0756(9) Uani 1 1 d . . . C411 C 0.2300(4) 1.2481(3) 0.3878(2) 0.0672(10) Uani 1 1 d . . . H411 H 0.1651 1.2788 0.4083 0.081 Uiso 1 1 calc R . . C412 C 0.1963(4) 1.1581(3) 0.3530(2) 0.0619(9) Uani 1 1 d . . . H412 H 0.1111 1.1293 0.3502 0.074 Uiso 1 1 calc R . . N5 N 0.5560(3) 0.2939(2) 0.1588(2) 0.0775(10) Uani 1 1 d . . . C51 C 0.5853(4) 0.2177(3) 0.1730(2) 0.0718(11) Uani 1 1 d . . . H51 H 0.6239 0.2221 0.2186 0.086 Uiso 1 1 calc R . . C52 C 0.5614(4) 0.1335(3) 0.1241(2) 0.0674(10) Uani 1 1 d . . . H52 H 0.5827 0.0825 0.1369 0.081 Uiso 1 1 calc R . . C53 C 0.5054(3) 0.1246(2) 0.05520(19) 0.0550(8) Uani 1 1 d . . . C54 C 0.4739(4) 0.2029(3) 0.0405(2) 0.0702(10) Uani 1 1 d . . . H54 H 0.4342 0.2009 -0.0043 0.084 Uiso 1 1 calc R . . C55 C 0.5024(5) 0.2841(3) 0.0936(3) 0.0829(13) Uani 1 1 d . . . H55 H 0.4819 0.3363 0.0824 0.099 Uiso 1 1 calc R . . C56 C 0.4811(3) 0.0384(2) -0.0018(2) 0.0610(9) Uani 1 1 d . . . H57 H 0.4348 0.0382 -0.0443 0.073 Uiso 1 1 calc R . . N6 N 0.0459(3) 0.30779(19) 0.63768(16) 0.0571(7) Uani 1 1 d . . . C61 C 0.0659(3) 0.2467(2) 0.6739(2) 0.0579(9) Uani 1 1 d . . . H61 H 0.0861 0.2675 0.7235 0.070 Uiso 1 1 calc R . . C62 C 0.0583(3) 0.1544(2) 0.64192(18) 0.0537(8) Uani 1 1 d . . . H62 H 0.0737 0.1152 0.6701 0.064 Uiso 1 1 calc R . . C63 C 0.0279(3) 0.1195(2) 0.56800(17) 0.0454(7) Uani 1 1 d . . . C64 C 0.0090(3) 0.1834(2) 0.52962(18) 0.0519(8) Uani 1 1 d . . . H64 H -0.0102 0.1647 0.4798 0.062 Uiso 1 1 calc R . . C65 C 0.0189(3) 0.2745(2) 0.5662(2) 0.0567(9) Uani 1 1 d . . . H65 H 0.0059 0.3157 0.5394 0.068 Uiso 1 1 calc R . . C66 C 0.0184(3) 0.0216(2) 0.53471(17) 0.0504(8) Uani 1 1 d . . . H67 H 0.0398 -0.0143 0.5645 0.060 Uiso 1 1 calc R . . N7 N 0.8235(4) 0.1488(4) 0.3369(3) 0.0971(14) Uani 1 1 d . . . O71 O 0.7237(4) 0.1552(4) 0.3069(3) 0.173(2) Uani 1 1 d . . . O72 O 0.8661(4) 0.0772(3) 0.3248(2) 0.1198(13) Uani 1 1 d . . . O73 O 0.8882(4) 0.2181(3) 0.3801(2) 0.1169(12) Uani 1 1 d . . . N8 N 0.2492(3) 0.2538(3) 0.8580(2) 0.0698(9) Uani 1 1 d . . . O81 O 0.1831(3) 0.1872(3) 0.81418(18) 0.1053(10) Uani 1 1 d . . . O82 O 0.2148(4) 0.3278(2) 0.8675(3) 0.1322(15) Uani 1 1 d . . . O83 O 0.3420(3) 0.2429(3) 0.8911(2) 0.1260(14) Uani 1 1 d . . . O1W O 0.9132(4) 0.4348(3) 0.0240(2) 0.1165(12) Uiso 1 1 d D . . H1W H 0.971(4) 0.393(3) 0.033(3) 0.140 Uiso 1 1 d D . . H2W H 0.829(3) 0.453(3) 0.028(3) 0.140 Uiso 1 1 d D . . O2W O 0.8597(3) 0.5197(2) 0.15879(17) 0.0912(9) Uiso 1 1 d D . . H3W H 0.833(4) 0.5799(18) 0.158(2) 0.109 Uiso 1 1 d D . . H4W H 0.874(4) 0.467(2) 0.1192(18) 0.109 Uiso 1 1 d D . . O3W O 0.7095(3) 0.44050(19) 0.25777(17) 0.0843(9) Uani 1 1 d D . . H5W H 0.652(3) 0.3842(19) 0.230(2) 0.101 Uiso 1 1 d D . . H6W H 0.767(4) 0.458(3) 0.2223(19) 0.101 Uiso 1 1 d D . . O4W O 0.6105(3) 0.56245(16) 0.36588(15) 0.0685(7) Uani 1 1 d D . . H7W H 0.635(4) 0.524(2) 0.3204(14) 0.082 Uiso 1 1 d D . . H8W H 0.613(4) 0.6216(17) 0.354(2) 0.082 Uiso 1 1 d D . . O5W O 0.1712(4) 0.6076(3) 0.6253(2) 0.1206(12) Uiso 1 1 d D . . H9W H 0.251(4) 0.662(3) 0.628(3) 0.145 Uiso 1 1 d D . . H10W H 0.225(4) 0.599(3) 0.6716(18) 0.145 Uiso 1 1 d D . . O6W O 0.2303(5) 0.4669(3) 0.5179(3) 0.1573(17) Uiso 1 1 d D . . H12W H 0.285(3) 0.526(2) 0.530(3) 0.189 Uiso 1 1 d D . . O7W O 0.3139(4) 0.0287(3) 0.8185(2) 0.1254(13) Uiso 1 1 d D . . H13W H 0.250(4) 0.037(4) 0.849(2) 0.151 Uiso 1 1 d D . . H14W H 0.288(4) -0.010(3) 0.7721(14) 0.151 Uiso 1 1 d D . . H11W H 0.1501(15) 0.4850(12) 0.5465(10) 0.000(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0458(2) 0.0427(2) 0.0435(2) 0.01253(16) 0.00836(15) 0.00540(15) O1 0.0601(16) 0.0810(17) 0.0537(15) 0.0249(13) 0.0074(13) 0.0017(14) O2 0.0574(14) 0.0557(14) 0.0527(15) 0.0045(12) -0.0018(12) 0.0163(12) O3 0.0494(13) 0.0539(15) 0.0814(18) 0.0313(13) -0.0021(13) 0.0041(11) N1 0.0590(17) 0.0487(15) 0.0420(15) 0.0146(12) 0.0139(13) 0.0093(13) C11 0.057(2) 0.059(2) 0.065(2) 0.0242(18) 0.0178(18) 0.0099(17) C12 0.064(2) 0.065(2) 0.141(4) 0.064(3) 0.056(3) 0.030(2) C15 0.077(2) 0.058(2) 0.0436(19) 0.0154(16) 0.0128(18) 0.0146(18) N21 0.0423(14) 0.0432(14) 0.0443(15) 0.0137(12) 0.0037(11) 0.0058(11) C21 0.0484(18) 0.0455(18) 0.0469(19) 0.0146(15) -0.0001(14) 0.0065(14) C22 0.0530(19) 0.0499(19) 0.0430(18) 0.0082(15) 0.0015(15) 0.0097(15) C23 0.0342(15) 0.0405(16) 0.0523(19) 0.0088(14) 0.0063(13) 0.0061(13) C24 0.0492(18) 0.0438(17) 0.0483(19) 0.0185(15) 0.0077(14) 0.0096(14) C25 0.0468(17) 0.0500(19) 0.0431(17) 0.0142(15) 0.0069(14) 0.0075(14) C26 0.0513(19) 0.0452(18) 0.057(2) 0.0165(16) 0.0086(16) 0.0093(15) C27 0.0484(18) 0.0469(18) 0.055(2) 0.0153(16) 0.0107(15) 0.0057(15) C28 0.0354(15) 0.0440(17) 0.0548(19) 0.0131(15) 0.0098(14) 0.0078(13) C29 0.0533(19) 0.052(2) 0.056(2) 0.0176(16) 0.0077(16) 0.0109(15) C210 0.058(2) 0.057(2) 0.053(2) 0.0007(17) 0.0071(17) 0.0080(17) N22 0.0522(16) 0.0460(16) 0.066(2) 0.0077(14) 0.0085(14) 0.0080(13) C211 0.055(2) 0.0475(19) 0.067(2) 0.0193(17) 0.0076(17) 0.0099(16) C212 0.0527(19) 0.053(2) 0.0497(19) 0.0095(16) 0.0041(15) 0.0093(16) N31 0.0503(16) 0.0455(15) 0.0533(16) 0.0147(13) 0.0092(13) 0.0056(12) C31 0.0501(19) 0.0517(19) 0.057(2) 0.0159(16) 0.0100(16) 0.0065(16) C32 0.063(2) 0.053(2) 0.053(2) 0.0138(16) 0.0124(17) 0.0184(17) C33 0.066(2) 0.052(2) 0.0460(19) 0.0172(16) 0.0019(17) 0.0013(17) C34 0.056(2) 0.061(2) 0.057(2) 0.0178(18) 0.0102(17) -0.0031(17) C35 0.0517(19) 0.058(2) 0.062(2) 0.0173(17) 0.0134(17) 0.0071(17) C36 0.066(2) 0.063(2) 0.069(2) 0.023(2) 0.008(2) 0.0000(19) C37 0.070(2) 0.064(2) 0.067(2) 0.021(2) 0.007(2) -0.001(2) C38 0.073(2) 0.0459(19) 0.054(2) 0.0202(16) -0.0011(18) 0.0051(18) C39 0.073(3) 0.071(3) 0.063(2) 0.017(2) 0.008(2) 0.013(2) C310 0.097(3) 0.073(3) 0.069(3) 0.016(2) 0.018(2) 0.022(3) N32 0.106(3) 0.057(2) 0.068(2) 0.0094(16) 0.011(2) 0.007(2) C311 0.079(3) 0.062(2) 0.072(3) 0.022(2) 0.001(2) -0.005(2) C312 0.079(3) 0.060(2) 0.060(2) 0.0245(19) 0.0119(19) 0.017(2) N41 0.080(2) 0.065(2) 0.080(2) 0.0164(18) 0.0012(19) 0.0070(18) C41 0.071(3) 0.069(3) 0.088(3) 0.025(2) 0.007(2) 0.023(2) C42 0.058(2) 0.071(3) 0.080(3) 0.026(2) 0.002(2) 0.011(2) C43 0.070(2) 0.056(2) 0.060(2) 0.0231(18) 0.0014(19) 0.0058(19) C44 0.073(3) 0.075(3) 0.059(2) 0.025(2) 0.0102(19) 0.020(2) C45 0.064(2) 0.079(3) 0.075(3) 0.027(2) -0.002(2) -0.006(2) C46 0.056(2) 0.082(3) 0.078(3) 0.035(2) 0.006(2) 0.011(2) C47 0.067(2) 0.083(3) 0.077(3) 0.037(2) 0.013(2) 0.014(2) C48 0.073(2) 0.060(2) 0.060(2) 0.0305(18) 0.0098(19) 0.0149(19) C49 0.059(2) 0.075(3) 0.084(3) 0.035(2) 0.011(2) 0.024(2) C410 0.059(2) 0.083(3) 0.092(3) 0.032(2) -0.003(2) 0.008(2) N42 0.073(2) 0.073(2) 0.080(2) 0.0181(18) 0.0034(18) 0.0132(19) C411 0.071(3) 0.070(3) 0.065(2) 0.021(2) 0.014(2) 0.018(2) C412 0.059(2) 0.071(3) 0.066(2) 0.036(2) 0.0119(18) 0.0144(19) N5 0.091(3) 0.059(2) 0.079(2) 0.0084(18) 0.007(2) 0.0181(18) C51 0.082(3) 0.068(3) 0.064(2) 0.012(2) -0.004(2) 0.019(2) C52 0.080(3) 0.060(2) 0.069(3) 0.023(2) 0.008(2) 0.024(2) C53 0.0519(19) 0.055(2) 0.059(2) 0.0156(17) 0.0078(17) 0.0103(16) C54 0.080(3) 0.065(2) 0.068(3) 0.016(2) -0.002(2) 0.024(2) C55 0.108(4) 0.063(3) 0.088(3) 0.027(2) 0.005(3) 0.034(2) C56 0.057(2) 0.063(2) 0.065(2) 0.0196(19) 0.0033(18) 0.0097(17) N6 0.0493(16) 0.0578(17) 0.062(2) 0.0091(15) 0.0088(14) 0.0130(13) C61 0.053(2) 0.063(2) 0.055(2) 0.0077(18) 0.0020(16) 0.0170(17) C62 0.0475(18) 0.060(2) 0.058(2) 0.0194(17) 0.0047(16) 0.0159(16) C63 0.0335(15) 0.0533(19) 0.0502(19) 0.0127(15) 0.0084(13) 0.0105(13) C64 0.0494(18) 0.059(2) 0.0503(19) 0.0157(16) 0.0102(15) 0.0163(16) C65 0.0481(19) 0.061(2) 0.067(2) 0.0236(19) 0.0121(17) 0.0169(16) C66 0.0434(17) 0.060(2) 0.0535(18) 0.0191(16) 0.0087(15) 0.0167(15) N7 0.058(3) 0.163(5) 0.100(3) 0.087(4) 0.017(2) 0.015(3) O71 0.063(2) 0.307(7) 0.205(5) 0.160(5) 0.000(3) 0.045(3) O72 0.090(3) 0.123(3) 0.163(4) 0.074(3) -0.001(2) 0.009(2) O73 0.126(3) 0.147(4) 0.097(3) 0.053(3) 0.013(2) 0.045(3) N8 0.0544(19) 0.088(3) 0.074(2) 0.034(2) 0.0041(17) 0.0115(19) O81 0.112(3) 0.114(3) 0.083(2) 0.023(2) -0.007(2) 0.006(2) O82 0.121(3) 0.083(2) 0.199(4) 0.041(3) -0.010(3) 0.036(2) O83 0.074(2) 0.171(4) 0.147(3) 0.063(3) -0.018(2) 0.035(2) O3W 0.079(2) 0.0701(18) 0.088(2) 0.0006(16) 0.0114(16) -0.0022(15) O4W 0.0724(17) 0.0501(14) 0.0814(19) 0.0163(13) 0.0073(14) 0.0064(13) _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 O2 2.113(2) . ? Zn1 O3 2.113(2) . ? Zn1 O1 2.131(3) . ? Zn1 N21 2.145(2) . ? Zn1 N31 2.166(3) . ? Zn1 N1 2.171(3) . ? O1 H1 0.840(2) . ? O1 H2 0.840(2) . ? O2 H3 0.840(2) . ? O2 H4 0.840(2) . ? O3 H5 0.839(2) . ? O3 H6 0.840(2) . ? N1 C11 1.341(4) . ? N1 C15 1.353(4) . ? C11 C12 1.410(5) . ? C11 H11 0.9300 . ? C12 C13 1.404(6) . ? C12 H12 0.9300 . ? C13 C14 1.345(5) . ? C13 C16 1.416(2) . ? C14 C15 1.363(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C16 1.238(8) 2_665 ? C16 H16 0.9300 . ? N21 C25 1.336(4) . ? N21 C21 1.352(4) . ? C21 C22 1.365(4) . ? C21 H21 0.9300 . ? C22 C23 1.397(4) . ? C22 H22 0.9300 . ? C23 C24 1.378(4) . ? C23 C26 1.473(4) . ? C24 C25 1.371(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.313(4) . ? C26 H26 0.9300 . ? C27 C28 1.457(4) . ? C27 H27 0.9300 . ? C28 C212 1.391(5) . ? C28 C29 1.396(4) . ? C29 C210 1.382(4) . ? C29 H29 0.9300 . ? C210 N22 1.335(5) . ? C210 H210 0.9300 . ? N22 C211 1.338(4) . ? C211 C212 1.370(4) . ? C211 H211 0.9300 . ? C212 H212 0.9300 . ? N31 C31 1.340(4) . ? N31 C35 1.341(4) . ? C31 C32 1.379(4) . ? C31 H31 0.9300 . ? C32 C33 1.384(5) . ? C32 H32 0.9300 . ? C33 C34 1.374(5) . ? C33 C36 1.478(5) . ? C34 C35 1.365(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.301(5) . ? C36 H36 0.9300 . ? C37 C38 1.479(5) . ? C37 H37 0.9300 . ? C38 C39 1.370(5) . ? C38 C312 1.379(5) . ? C39 C310 1.362(5) . ? C39 H39 0.9300 . ? C310 N32 1.318(5) . ? C310 H310 0.9300 . ? N32 C311 1.314(5) . ? C311 C312 1.391(5) . ? C311 H311 0.9300 . ? C312 H312 0.9300 . ? N41 C45 1.328(5) . ? N41 C41 1.335(5) . ? C41 C42 1.353(5) . ? C41 H41 0.9300 . ? C42 C43 1.377(5) . ? C42 H42 0.9300 . ? C43 C44 1.392(5) . ? C43 C46 1.489(5) . ? C44 C45 1.374(5) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.298(5) . ? C46 H46 0.9300 . ? C47 C48 1.457(5) . ? C47 H47 0.9300 . ? C48 C412 1.392(5) . ? C48 C49 1.393(5) . ? C49 C410 1.380(5) . ? C49 H49 0.9300 . ? C410 N42 1.344(5) . ? C410 H410 0.9300 . ? N42 C411 1.319(5) . ? C411 C412 1.355(5) . ? C411 H411 0.9300 . ? C412 H412 0.9300 . ? N5 C55 1.312(5) . ? N5 C51 1.336(5) . ? C51 C52 1.369(5) . ? C51 H51 0.9300 . ? C52 C53 1.389(5) . ? C52 H52 0.9300 . ? C53 C54 1.380(5) . ? C53 C56 1.464(5) . ? C54 C55 1.374(5) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C56 1.309(7) 2_655 ? C56 H57 0.9300 . ? N6 C61 1.333(4) . ? N6 C65 1.338(4) . ? C61 C62 1.377(4) . ? C61 H61 0.9300 . ? C62 C63 1.388(4) . ? C62 H62 0.9300 . ? C63 C64 1.396(5) . ? C63 C66 1.458(4) . ? C64 C65 1.378(5) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 C66 1.339(6) 2_556 ? C66 H67 0.9300 . ? N7 O71 1.200(5) . ? N7 O72 1.215(5) . ? N7 O73 1.250(5) . ? N8 O83 1.193(4) . ? N8 O82 1.210(4) . ? N8 O81 1.237(4) . ? O1W H1W 0.981(19) . ? O1W H2W 0.971(19) . ? O2W H3W 1.004(19) . ? O2W H4W 0.993(19) . ? O3W H5W 0.985(19) . ? O3W H6W 0.992(19) . ? O4W H7W 0.990(18) . ? O4W H8W 0.983(18) . ? O5W H9W 1.081(19) . ? O5W H10W 1.080(19) . ? O6W H12W 0.961(19) . ? O6W H11W 1.059(13) . ? O7W H13W 0.916(19) . ? O7W H14W 0.939(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O3 169.53(10) . . ? O2 Zn1 O1 82.45(10) . . ? O3 Zn1 O1 87.94(10) . . ? O2 Zn1 N21 88.58(9) . . ? O3 Zn1 N21 87.54(9) . . ? O1 Zn1 N21 91.52(10) . . ? O2 Zn1 N31 94.46(10) . . ? O3 Zn1 N31 89.60(10) . . ? O1 Zn1 N31 89.69(10) . . ? N21 Zn1 N31 176.85(9) . . ? O2 Zn1 N1 93.99(10) . . ? O3 Zn1 N1 95.89(10) . . ? O1 Zn1 N1 174.57(10) . . ? N21 Zn1 N1 92.50(10) . . ? N31 Zn1 N1 86.48(10) . . ? Zn1 O1 H1 119(3) . . ? Zn1 O1 H2 127(3) . . ? H1 O1 H2 114(4) . . ? Zn1 O2 H3 125(3) . . ? Zn1 O2 H4 107(2) . . ? H3 O2 H4 120(4) . . ? Zn1 O3 H5 124(3) . . ? Zn1 O3 H6 119(3) . . ? H5 O3 H6 113(4) . . ? C11 N1 C15 116.2(3) . . ? C11 N1 Zn1 122.5(2) . . ? C15 N1 Zn1 120.6(2) . . ? N1 C11 C12 121.8(4) . . ? N1 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 115.3(3) . . ? C14 C13 C16 118.3(4) . . ? C12 C13 C16 126.4(4) . . ? C13 C14 C15 122.7(4) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? N1 C15 C14 123.4(4) . . ? N1 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C16 C16 C13 131.8(7) 2_665 . ? C16 C16 H16 114.1 2_665 . ? C13 C16 H16 114.1 . . ? C25 N21 C21 116.3(3) . . ? C25 N21 Zn1 120.8(2) . . ? C21 N21 Zn1 122.4(2) . . ? N21 C21 C22 123.5(3) . . ? N21 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 116.8(3) . . ? C24 C23 C26 119.1(3) . . ? C22 C23 C26 124.1(3) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? N21 C25 C24 123.6(3) . . ? N21 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C27 C26 C23 128.8(3) . . ? C27 C26 H26 115.6 . . ? C23 C26 H26 115.6 . . ? C26 C27 C28 125.4(3) . . ? C26 C27 H27 117.3 . . ? C28 C27 H27 117.3 . . ? C212 C28 C29 115.9(3) . . ? C212 C28 C27 123.3(3) . . ? C29 C28 C27 120.8(3) . . ? C210 C29 C28 119.9(3) . . ? C210 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? N22 C210 C29 123.8(3) . . ? N22 C210 H210 118.1 . . ? C29 C210 H210 118.1 . . ? C210 N22 C211 115.9(3) . . ? N22 C211 C212 124.2(3) . . ? N22 C211 H211 117.9 . . ? C212 C211 H211 117.9 . . ? C211 C212 C28 120.2(3) . . ? C211 C212 H212 119.9 . . ? C28 C212 H212 119.9 . . ? C31 N31 C35 116.2(3) . . ? C31 N31 Zn1 120.5(2) . . ? C35 N31 Zn1 123.3(2) . . ? N31 C31 C32 123.0(3) . . ? N31 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 116.7(3) . . ? C34 C33 C36 119.1(3) . . ? C32 C33 C36 124.1(3) . . ? C35 C34 C33 120.2(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? N31 C35 C34 123.8(3) . . ? N31 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? C37 C36 C33 125.6(4) . . ? C37 C36 H36 117.2 . . ? C33 C36 H36 117.2 . . ? C36 C37 C38 127.1(4) . . ? C36 C37 H37 116.4 . . ? C38 C37 H37 116.4 . . ? C39 C38 C312 117.1(3) . . ? C39 C38 C37 119.6(3) . . ? C312 C38 C37 123.2(3) . . ? C310 C39 C38 119.6(4) . . ? C310 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N32 C310 C39 124.8(4) . . ? N32 C310 H310 117.6 . . ? C39 C310 H310 117.6 . . ? C311 N32 C310 115.6(3) . . ? N32 C311 C312 124.5(4) . . ? N32 C311 H311 117.7 . . ? C312 C311 H311 117.7 . . ? C38 C312 C311 118.3(4) . . ? C38 C312 H312 120.8 . . ? C311 C312 H312 120.8 . . ? C45 N41 C41 116.2(3) . . ? N41 C41 C42 123.4(4) . . ? N41 C41 H41 118.3 . . ? C42 C41 H41 118.3 . . ? C41 C42 C43 120.9(4) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C44 116.3(4) . . ? C42 C43 C46 119.2(4) . . ? C44 C43 C46 124.5(3) . . ? C45 C44 C43 119.0(4) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? N41 C45 C44 124.1(4) . . ? N41 C45 H45 117.9 . . ? C44 C45 H45 117.9 . . ? C47 C46 C43 126.1(4) . . ? C47 C46 H46 116.9 . . ? C43 C46 H46 116.9 . . ? C46 C47 C48 126.6(4) . . ? C46 C47 H47 116.7 . . ? C48 C47 H47 116.7 . . ? C412 C48 C49 116.3(4) . . ? C412 C48 C47 119.9(4) . . ? C49 C48 C47 123.7(4) . . ? C410 C49 C48 119.0(4) . . ? C410 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? N42 C410 C49 124.2(4) . . ? N42 C410 H410 117.9 . . ? C49 C410 H410 117.9 . . ? C411 N42 C410 115.4(3) . . ? N42 C411 C412 125.3(4) . . ? N42 C411 H411 117.4 . . ? C412 C411 H411 117.4 . . ? C411 C412 C48 119.8(4) . . ? C411 C412 H412 120.1 . . ? C48 C412 H412 120.1 . . ? C55 N5 C51 115.9(3) . . ? N5 C51 C52 123.5(4) . . ? N5 C51 H51 118.3 . . ? C52 C51 H51 118.3 . . ? C51 C52 C53 119.8(3) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 116.8(3) . . ? C54 C53 C56 119.3(3) . . ? C52 C53 C56 123.9(3) . . ? C55 C54 C53 118.6(4) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? N5 C55 C54 125.4(4) . . ? N5 C55 H55 117.3 . . ? C54 C55 H55 117.3 . . ? C56 C56 C53 125.8(5) 2_655 . ? C56 C56 H57 117.1 2_655 . ? C53 C56 H57 117.1 . . ? C61 N6 C65 115.7(3) . . ? N6 C61 C62 123.8(3) . . ? N6 C61 H61 118.1 . . ? C62 C61 H61 118.1 . . ? C61 C62 C63 120.5(3) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C62 C63 C64 116.0(3) . . ? C62 C63 C66 120.2(3) . . ? C64 C63 C66 123.8(3) . . ? C65 C64 C63 119.4(3) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? N6 C65 C64 124.6(3) . . ? N6 C65 H65 117.7 . . ? C64 C65 H65 117.7 . . ? C66 C66 C63 126.2(4) 2_556 . ? C66 C66 H67 116.9 2_556 . ? C63 C66 H67 116.9 . . ? O71 N7 O72 121.8(6) . . ? O71 N7 O73 119.5(6) . . ? O72 N7 O73 118.6(5) . . ? O83 N8 O82 122.1(4) . . ? O83 N8 O81 119.4(4) . . ? O82 N8 O81 118.5(4) . . ? H1W O1W H2W 148(5) . . ? H3W O2W H4W 131(4) . . ? H5W O3W H6W 105(4) . . ? H7W O4W H8W 101(3) . . ? H9W O5W H10W 83.7(17) . . ? H12W O6W H11W 99(2) . . ? H13W O7W H14W 116(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 O2 Zn1 N1 C11 139.2(2) . . . . ? O3 Zn1 N1 C11 -37.3(3) . . . . ? O1 Zn1 N1 C11 -171.9(10) . . . . ? N21 Zn1 N1 C11 50.5(3) . . . . ? N31 Zn1 N1 C11 -126.5(3) . . . . ? O2 Zn1 N1 C15 -50.7(2) . . . . ? O3 Zn1 N1 C15 132.8(2) . . . . ? O1 Zn1 N1 C15 -1.8(12) . . . . ? N21 Zn1 N1 C15 -139.4(2) . . . . ? N31 Zn1 N1 C15 43.5(2) . . . . ? C15 N1 C11 C12 -1.2(5) . . . . ? Zn1 N1 C11 C12 169.3(2) . . . . ? N1 C11 C12 C13 0.6(5) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? C11 C12 C13 C16 -177.7(4) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C16 C13 C14 C15 178.0(4) . . . . ? C11 N1 C15 C14 1.4(5) . . . . ? Zn1 N1 C15 C14 -169.3(3) . . . . ? C13 C14 C15 N1 -0.9(6) . . . . ? C14 C13 C16 C16 -175.5(8) . . . 2_665 ? C12 C13 C16 C16 2.0(12) . . . 2_665 ? O2 Zn1 N21 C25 -52.7(2) . . . . ? O3 Zn1 N21 C25 137.0(2) . . . . ? O1 Zn1 N21 C25 -135.1(2) . . . . ? N31 Zn1 N21 C25 112.2(17) . . . . ? N1 Zn1 N21 C25 41.2(2) . . . . ? O2 Zn1 N21 C21 118.2(2) . . . . ? O3 Zn1 N21 C21 -52.1(2) . . . . ? O1 Zn1 N21 C21 35.8(2) . . . . ? N31 Zn1 N21 C21 -76.8(18) . . . . ? N1 Zn1 N21 C21 -147.8(2) . . . . ? C25 N21 C21 C22 2.5(4) . . . . ? Zn1 N21 C21 C22 -168.8(2) . . . . ? N21 C21 C22 C23 -2.2(5) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C21 C22 C23 C26 178.4(3) . . . . ? C22 C23 C24 C25 1.3(4) . . . . ? C26 C23 C24 C25 -177.0(3) . . . . ? C21 N21 C25 C24 -0.9(4) . . . . ? Zn1 N21 C25 C24 170.6(2) . . . . ? C23 C24 C25 N21 -1.0(5) . . . . ? C24 C23 C26 C27 174.8(3) . . . . ? C22 C23 C26 C27 -3.3(5) . . . . ? C23 C26 C27 C28 -178.8(3) . . . . ? C26 C27 C28 C212 1.6(5) . . . . ? C26 C27 C28 C29 -178.4(3) . . . . ? C212 C28 C29 C210 0.0(4) . . . . ? C27 C28 C29 C210 180.0(3) . . . . ? C28 C29 C210 N22 -1.1(5) . . . . ? C29 C210 N22 C211 1.9(5) . . . . ? C210 N22 C211 C212 -1.7(5) . . . . ? N22 C211 C212 C28 0.8(5) . . . . ? C29 C28 C212 C211 0.1(4) . . . . ? C27 C28 C212 C211 -179.8(3) . . . . ? O2 Zn1 N31 C31 147.5(3) . . . . ? O3 Zn1 N31 C31 -42.1(3) . . . . ? O1 Zn1 N31 C31 -130.1(3) . . . . ? N21 Zn1 N31 C31 -17.4(19) . . . . ? N1 Zn1 N31 C31 53.8(3) . . . . ? O2 Zn1 N31 C35 -31.1(3) . . . . ? O3 Zn1 N31 C35 139.2(3) . . . . ? O1 Zn1 N31 C35 51.3(3) . . . . ? N21 Zn1 N31 C35 163.9(17) . . . . ? N1 Zn1 N31 C35 -124.9(3) . . . . ? C35 N31 C31 C32 0.3(5) . . . . ? Zn1 N31 C31 C32 -178.4(2) . . . . ? N31 C31 C32 C33 -0.5(5) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C31 C32 C33 C36 176.8(3) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C36 C33 C34 C35 -176.5(3) . . . . ? C31 N31 C35 C34 0.2(5) . . . . ? Zn1 N31 C35 C34 178.9(3) . . . . ? C33 C34 C35 N31 -0.5(6) . . . . ? C34 C33 C36 C37 168.6(4) . . . . ? C32 C33 C36 C37 -8.0(6) . . . . ? C33 C36 C37 C38 -176.6(3) . . . . ? C36 C37 C38 C39 -179.4(4) . . . . ? C36 C37 C38 C312 1.8(6) . . . . ? C312 C38 C39 C310 -1.6(6) . . . . ? C37 C38 C39 C310 179.6(3) . . . . ? C38 C39 C310 N32 -0.1(7) . . . . ? C39 C310 N32 C311 1.7(7) . . . . ? C310 N32 C311 C312 -1.7(6) . . . . ? C39 C38 C312 C311 1.5(5) . . . . ? C37 C38 C312 C311 -179.7(3) . . . . ? N32 C311 C312 C38 0.2(6) . . . . ? C45 N41 C41 C42 -1.9(6) . . . . ? N41 C41 C42 C43 1.5(6) . . . . ? C41 C42 C43 C44 -0.4(6) . . . . ? C41 C42 C43 C46 179.5(3) . . . . ? C42 C43 C44 C45 -0.3(5) . . . . ? C46 C43 C44 C45 179.8(3) . . . . ? C41 N41 C45 C44 1.1(6) . . . . ? C43 C44 C45 N41 -0.1(6) . . . . ? C42 C43 C46 C47 -177.9(4) . . . . ? C44 C43 C46 C47 2.0(6) . . . . ? C43 C46 C47 C48 -174.6(3) . . . . ? C46 C47 C48 C412 170.2(4) . . . . ? C46 C47 C48 C49 -8.3(6) . . . . ? C412 C48 C49 C410 -2.8(5) . . . . ? C47 C48 C49 C410 175.7(4) . . . . ? C48 C49 C410 N42 0.0(6) . . . . ? C49 C410 N42 C411 2.9(6) . . . . ? C410 N42 C411 C412 -3.0(6) . . . . ? N42 C411 C412 C48 0.1(6) . . . . ? C49 C48 C412 C411 2.8(5) . . . . ? C47 C48 C412 C411 -175.8(3) . . . . ? C55 N5 C51 C52 -0.4(6) . . . . ? N5 C51 C52 C53 0.9(6) . . . . ? C51 C52 C53 C54 -1.4(6) . . . . ? C51 C52 C53 C56 177.3(4) . . . . ? C52 C53 C54 C55 1.6(6) . . . . ? C56 C53 C54 C55 -177.2(4) . . . . ? C51 N5 C55 C54 0.6(7) . . . . ? C53 C54 C55 N5 -1.2(7) . . . . ? C54 C53 C56 C56 171.9(5) . . . 2_655 ? C52 C53 C56 C56 -6.8(7) . . . 2_655 ? C65 N6 C61 C62 -0.9(5) . . . . ? N6 C61 C62 C63 -0.3(5) . . . . ? C61 C62 C63 C64 1.3(4) . . . . ? C61 C62 C63 C66 -179.2(3) . . . . ? C62 C63 C64 C65 -1.1(4) . . . . ? C66 C63 C64 C65 179.3(3) . . . . ? C61 N6 C65 C64 1.1(5) . . . . ? C63 C64 C65 N6 -0.1(5) . . . . ? C62 C63 C66 C66 175.3(4) . . . 2_556 ? C64 C63 C66 C66 -5.2(6) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 1.389 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.068 data_[Zn(H2O)(bpe)(4pycb)](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 260339' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Cl2 N6 O9 Zn' _chemical_formula_weight 828.95 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.602(3) _cell_length_b 15.129(3) _cell_length_c 18.549(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.599(4) _cell_angle_gamma 90.00 _cell_volume 3513.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4574 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10413 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.09 _reflns_number_total 3902 _reflns_number_gt 3147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3902 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.061 _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 Zn1 Zn 0.5000 0.53745(2) 0.7500 0.02659(14) Uani 1 2 d S . . O1 O 0.5000 0.40855(15) 0.7500 0.0398(6) Uani 1 2 d S . . H1 H 0.488(3) 0.379(2) 0.7133(15) 0.067(10) Uiso 1 1 d . . . N1 N 0.43016(14) 0.59657(13) 0.83126(10) 0.0297(4) Uani 1 1 d . . . C11 C 0.3977(2) 0.68017(17) 0.82670(13) 0.0406(6) Uani 1 1 d . . . H11 H 0.4085 0.7126 0.7856 0.049 Uiso 1 1 calc R . . C12 C 0.3483(2) 0.72074(17) 0.88085(15) 0.0453(6) Uani 1 1 d . . . H12 H 0.3275 0.7796 0.8758 0.054 Uiso 1 1 calc R . . C13 C 0.32984(18) 0.67430(17) 0.94232(13) 0.0352(5) Uani 1 1 d . . . C14 C 0.3653(2) 0.58783(19) 0.94679(14) 0.0447(6) Uani 1 1 d . . . H14 H 0.3562 0.5541 0.9875 0.054 Uiso 1 1 calc R . . C15 C 0.4138(2) 0.55186(16) 0.89130(14) 0.0406(6) Uani 1 1 d . . . H15 H 0.4365 0.4934 0.8955 0.049 Uiso 1 1 calc R . . C16 C 0.2726(2) 0.71105(16) 1.00040(14) 0.0415(6) Uani 1 1 d . . . H16 H 0.2682 0.6759 1.0411 0.050 Uiso 1 1 calc R . . N21 N 0.34172(16) 0.53391(12) 0.68019(11) 0.0326(4) Uani 1 1 d . . . C21 C 0.31780(19) 0.57109(16) 0.61480(13) 0.0361(5) Uani 1 1 d . . . H21 H 0.3661 0.6111 0.5990 0.043 Uiso 1 1 calc R . . C22 C 0.2252(2) 0.55323(16) 0.56942(13) 0.0381(6) Uani 1 1 d . . . H22 H 0.2134 0.5800 0.5241 0.046 Uiso 1 1 calc R . . C23 C 0.15031(18) 0.49571(16) 0.59160(13) 0.0323(5) Uani 1 1 d . . . C24 C 0.1709(2) 0.46210(16) 0.66175(14) 0.0408(6) Uani 1 1 d . . . H24 H 0.1207 0.4267 0.6808 0.049 Uiso 1 1 calc R . . C25 C 0.2664(2) 0.48170(18) 0.70262(14) 0.0436(6) Uani 1 1 d . . . H25 H 0.2792 0.4571 0.7487 0.052 Uiso 1 1 calc R . . C26 C 0.05001(19) 0.46772(15) 0.54572(13) 0.0337(5) Uani 1 1 d . . . H26 H 0.0283 0.4092 0.5613 0.040 Uiso 1 1 calc R . . C27 C -0.04943(19) 0.53158(15) 0.53836(13) 0.0336(5) Uani 1 1 d . . . H27 H -0.1124 0.4999 0.5513 0.040 Uiso 1 1 calc R . . C28 C -0.03889(18) 0.61899(16) 0.57779(13) 0.0381(6) Uani 1 1 d . . . C29 C 0.0179(2) 0.68974(18) 0.55497(15) 0.0461(6) Uani 1 1 d . . . H29 H 0.0543 0.6847 0.5143 0.055 Uiso 1 1 calc R . . C210 C 0.0201(2) 0.76859(19) 0.59373(17) 0.0539(7) Uani 1 1 d . . . H210 H 0.0598 0.8153 0.5783 0.065 Uiso 1 1 calc R . . N22 N -0.0309(2) 0.78084(16) 0.65106(14) 0.0573(7) Uani 1 1 d . . . C211 C -0.0830(3) 0.7116(2) 0.67429(17) 0.0585(8) Uani 1 1 d . . . H211 H -0.1179 0.7185 0.7155 0.070 Uiso 1 1 calc R . . C212 C -0.0881(2) 0.62955(19) 0.64017(14) 0.0465(7) Uani 1 1 d . . . H212 H -0.1238 0.5826 0.6590 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.68191(6) 0.83145(5) 0.85546(4) 0.0527(2) Uani 1 1 d . . . O11 O 0.7375(2) 0.7833(2) 0.80687(15) 0.0971(9) Uani 1 1 d . . . O12 O 0.7533(5) 0.9058(4) 0.8781(4) 0.0363(13) Uiso 0.34 1 d P . . O13 O 0.5853(6) 0.8611(6) 0.8131(4) 0.0610(18) Uiso 0.34 1 d P . . O14 O 0.6566(7) 0.7845(4) 0.9180(4) 0.0544(17) Uiso 0.34 1 d P . . O22 O 0.6113(9) 0.7825(7) 0.8924(7) 0.105(4) Uiso 0.33 1 d P . . O23 O 0.6070(8) 0.9047(7) 0.8217(5) 0.091(3) Uiso 0.33 1 d P . . O24 O 0.7497(8) 0.8825(7) 0.9032(6) 0.088(3) Uiso 0.33 1 d P . . O32 O 0.7146(8) 0.7837(5) 0.9267(5) 0.081(2) Uiso 0.33 1 d P . . O33 O 0.5767(9) 0.8173(9) 0.8351(8) 0.119(4) Uiso 0.33 1 d P . . O34 O 0.7127(9) 0.9191(6) 0.8668(5) 0.085(3) Uiso 0.33 1 d P . . 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 0.0333(2) 0.0250(2) 0.0225(2) 0.000 0.00765(14) 0.000 O1 0.0608(17) 0.0228(12) 0.0331(14) 0.000 -0.0064(12) 0.000 N1 0.0302(10) 0.0334(10) 0.0260(9) -0.0028(8) 0.0058(7) 0.0014(8) C11 0.0494(15) 0.0388(13) 0.0361(13) 0.0063(11) 0.0150(11) 0.0111(11) C12 0.0523(16) 0.0336(13) 0.0534(16) -0.0019(12) 0.0210(13) 0.0095(11) C13 0.0318(13) 0.0420(14) 0.0329(12) -0.0108(10) 0.0087(10) -0.0049(10) C14 0.0532(16) 0.0483(16) 0.0358(14) 0.0049(12) 0.0187(11) 0.0012(12) C15 0.0492(15) 0.0345(13) 0.0403(14) 0.0006(11) 0.0146(12) 0.0057(11) C16 0.0411(14) 0.0473(14) 0.0378(13) -0.0089(12) 0.0116(11) -0.0031(11) N21 0.0312(10) 0.0377(11) 0.0280(10) 0.0017(8) -0.0008(8) -0.0010(8) C21 0.0359(13) 0.0355(13) 0.0362(13) 0.0024(10) 0.0012(10) -0.0008(10) C22 0.0442(15) 0.0413(13) 0.0273(12) 0.0030(10) -0.0027(10) 0.0026(11) C23 0.0307(12) 0.0308(11) 0.0347(12) -0.0081(10) 0.0005(10) 0.0046(9) C24 0.0367(14) 0.0469(15) 0.0382(14) 0.0023(11) 0.0019(11) -0.0060(11) C25 0.0387(14) 0.0579(17) 0.0329(13) 0.0081(12) -0.0011(11) -0.0063(12) C26 0.0360(13) 0.0305(12) 0.0339(13) -0.0047(9) 0.0010(10) 0.0007(9) C27 0.0286(12) 0.0372(13) 0.0341(13) -0.0072(10) 0.0003(9) -0.0009(9) C28 0.0283(12) 0.0417(14) 0.0417(14) -0.0131(11) -0.0070(10) 0.0053(10) C29 0.0399(14) 0.0469(15) 0.0501(16) -0.0115(13) 0.0000(12) 0.0039(12) C210 0.0490(17) 0.0445(15) 0.0647(19) -0.0132(14) -0.0080(15) 0.0015(12) N22 0.0590(16) 0.0493(15) 0.0598(16) -0.0255(13) -0.0091(13) 0.0094(12) C211 0.0611(19) 0.066(2) 0.0462(17) -0.0231(15) -0.0030(14) 0.0125(16) C212 0.0477(16) 0.0503(16) 0.0398(14) -0.0114(12) -0.0022(12) 0.0051(12) Cl1 0.0578(5) 0.0564(4) 0.0461(4) -0.0082(3) 0.0155(3) -0.0108(3) O11 0.0955(19) 0.119(2) 0.0811(18) -0.0506(17) 0.0279(15) 0.0013(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 O1 1.950(2) . ? Zn1 N1 2.0376(18) 2_656 ? Zn1 N1 2.0376(18) . ? Zn1 N21 2.251(2) 2_656 ? Zn1 N21 2.251(2) . ? O1 H1 0.82(3) . ? N1 C11 1.329(3) . ? N1 C15 1.339(3) . ? C11 C12 1.384(3) . ? C11 H11 0.9300 . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 C14 1.382(4) . ? C13 C16 1.473(3) . ? C14 C15 1.369(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C16 1.308(5) 7_567 ? C16 H16 0.9300 . ? N21 C25 1.338(3) . ? N21 C21 1.339(3) . ? C21 C22 1.385(3) . ? C21 H21 0.9300 . ? C22 C23 1.381(4) . ? C22 H22 0.9300 . ? C23 C24 1.393(3) . ? C23 C26 1.501(3) . ? C24 C25 1.378(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.559(3) 5_566 ? C26 C27 1.576(3) . ? C26 H26 0.9800 . ? C27 C28 1.510(3) . ? C27 C26 1.559(3) 5_566 ? C27 H27 0.9800 . ? C28 C29 1.381(4) . ? C28 C212 1.383(4) . ? C29 C210 1.391(4) . ? C29 H29 0.9300 . ? C210 N22 1.317(4) . ? C210 H210 0.9300 . ? N22 C211 1.335(4) . ? C211 C212 1.391(4) . ? C211 H211 0.9300 . ? C212 H212 0.9300 . ? Cl1 O33 1.353(12) . ? Cl1 O34 1.391(10) . ? Cl1 O24 1.391(10) . ? Cl1 O22 1.396(11) . ? Cl1 O11 1.407(2) . ? Cl1 O14 1.428(7) . ? Cl1 O13 1.442(7) . ? Cl1 O12 1.471(6) . ? Cl1 O32 1.521(9) . ? Cl1 O23 1.541(10) . ? O12 O34 0.566(10) . ? O12 O24 0.592(11) . ? O13 O23 0.725(10) . ? O13 O33 0.792(13) . ? O14 O22 0.700(11) . ? O14 O32 0.730(9) . ? O14 O33 1.809(15) . ? O22 O33 1.221(14) . ? O22 O32 1.382(14) . ? O23 O33 1.406(16) . ? O23 O34 1.506(13) . ? O24 O34 0.953(12) . ? O24 O32 1.632(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 116.04(5) . 2_656 ? O1 Zn1 N1 116.04(6) . . ? N1 Zn1 N1 127.92(11) 2_656 . ? O1 Zn1 N21 88.64(5) . 2_656 ? N1 Zn1 N21 90.37(7) 2_656 2_656 ? N1 Zn1 N21 90.83(7) . 2_656 ? O1 Zn1 N21 88.64(5) . . ? N1 Zn1 N21 90.83(7) 2_656 . ? N1 Zn1 N21 90.37(7) . . ? N21 Zn1 N21 177.28(10) 2_656 . ? Zn1 O1 H1 124(2) . . ? C11 N1 C15 117.2(2) . . ? C11 N1 Zn1 121.79(16) . . ? C15 N1 Zn1 120.96(16) . . ? N1 C11 C12 122.5(2) . . ? N1 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 116.5(2) . . ? C12 C13 C16 123.7(2) . . ? C14 C13 C16 119.7(2) . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N1 C15 C14 123.3(2) . . ? N1 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C16 C16 C13 125.5(3) 7_567 . ? C16 C16 H16 117.2 7_567 . ? C13 C16 H16 117.2 . . ? C25 N21 C21 115.8(2) . . ? C25 N21 Zn1 116.68(15) . . ? C21 N21 Zn1 127.11(16) . . ? N21 C21 C22 123.7(2) . . ? N21 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 116.6(2) . . ? C22 C23 C26 124.7(2) . . ? C24 C23 C26 118.8(2) . . ? C25 C24 C23 119.5(2) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? N21 C25 C24 124.2(2) . . ? N21 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? C23 C26 C27 118.2(2) . 5_566 ? C23 C26 C27 119.05(18) . . ? C27 C26 C27 89.83(18) 5_566 . ? C23 C26 H26 109.4 . . ? C27 C26 H26 109.4 5_566 . ? C27 C26 H26 109.4 . . ? C28 C27 C26 118.0(2) . 5_566 ? C28 C27 C26 118.06(19) . . ? C26 C27 C26 90.18(18) 5_566 . ? C28 C27 H27 109.7 . . ? C26 C27 H27 109.7 5_566 . ? C26 C27 H27 109.7 . . ? C29 C28 C212 117.7(2) . . ? C29 C28 C27 123.4(2) . . ? C212 C28 C27 118.9(2) . . ? C28 C29 C210 119.1(3) . . ? C28 C29 H29 120.5 . . ? C210 C29 H29 120.5 . . ? N22 C210 C29 123.7(3) . . ? N22 C210 H210 118.1 . . ? C29 C210 H210 118.1 . . ? C210 N22 C211 117.0(3) . . ? N22 C211 C212 123.5(3) . . ? N22 C211 H211 118.2 . . ? C212 C211 H211 118.2 . . ? C28 C212 C211 118.8(3) . . ? C28 C212 H212 120.6 . . ? C211 C212 H212 120.6 . . ? O33 Cl1 O34 116.2(7) . . ? O33 Cl1 O24 140.8(7) . . ? O34 Cl1 O24 40.1(5) . . ? O33 Cl1 O22 52.7(6) . . ? O34 Cl1 O22 127.8(6) . . ? O24 Cl1 O22 111.1(7) . . ? O33 Cl1 O11 106.5(5) . . ? O34 Cl1 O11 116.1(4) . . ? O24 Cl1 O11 112.4(4) . . ? O22 Cl1 O11 115.6(5) . . ? O33 Cl1 O14 81.1(7) . . ? O34 Cl1 O14 115.9(5) . . ? O24 Cl1 O14 86.4(6) . . ? O22 Cl1 O14 28.7(5) . . ? O11 Cl1 O14 115.9(3) . . ? O33 Cl1 O13 32.7(6) . . ? O34 Cl1 O13 89.4(5) . . ? O24 Cl1 O13 126.3(6) . . ? O22 Cl1 O13 83.5(6) . . ? O11 Cl1 O13 105.3(3) . . ? O14 Cl1 O13 110.1(5) . . ? O33 Cl1 O12 138.4(6) . . ? O34 Cl1 O12 22.6(4) . . ? O24 Cl1 O12 23.6(4) . . ? O22 Cl1 O12 132.0(6) . . ? O11 Cl1 O12 104.2(3) . . ? O14 Cl1 O12 109.6(4) . . ? O13 Cl1 O12 111.6(5) . . ? O33 Cl1 O32 109.0(7) . . ? O34 Cl1 O32 106.2(5) . . ? O24 Cl1 O32 68.0(5) . . ? O22 Cl1 O32 56.3(6) . . ? O11 Cl1 O32 101.9(4) . . ? O14 Cl1 O32 28.4(4) . . ? O13 Cl1 O32 138.5(5) . . ? O12 Cl1 O32 91.2(5) . . ? O33 Cl1 O23 57.7(6) . . ? O34 Cl1 O23 61.5(5) . . ? O24 Cl1 O23 99.4(6) . . ? O22 Cl1 O23 100.7(6) . . ? O11 Cl1 O23 116.0(4) . . ? O14 Cl1 O23 120.3(5) . . ? O13 Cl1 O23 27.9(4) . . ? O12 Cl1 O23 83.8(5) . . ? O32 Cl1 O23 141.9(5) . . ? O34 O12 O24 110.8(19) . . ? O34 O12 Cl1 70.7(13) . . ? O24 O12 Cl1 70.6(12) . . ? O23 O13 O33 136.0(19) . . ? O23 O13 Cl1 83.7(11) . . ? O33 O13 Cl1 67.5(11) . . ? O22 O14 O32 150(2) . . ? O22 O14 Cl1 73.2(12) . . ? O32 O14 Cl1 82.9(10) . . ? O22 O14 O33 26.3(12) . . ? O32 O14 O33 129.6(12) . . ? Cl1 O14 O33 47.7(5) . . ? O14 O22 O33 139.0(18) . . ? O14 O22 O32 15.3(10) . . ? O33 O22 O32 128.2(11) . . ? O14 O22 Cl1 78.2(12) . . ? O33 O22 Cl1 61.8(8) . . ? O32 O22 Cl1 66.4(6) . . ? O13 O23 O33 23.1(10) . . ? O13 O23 O34 122.7(14) . . ? O33 O23 O34 106.2(9) . . ? O13 O23 Cl1 68.4(11) . . ? O33 O23 Cl1 54.4(6) . . ? O34 O23 Cl1 54.3(5) . . ? O12 O24 O34 33.7(11) . . ? O12 O24 Cl1 85.8(13) . . ? O34 O24 Cl1 69.9(8) . . ? O12 O24 O32 143.7(16) . . ? O34 O24 O32 126.6(12) . . ? Cl1 O24 O32 59.8(5) . . ? O14 O32 O22 14.6(10) . . ? O14 O32 Cl1 68.7(10) . . ? O22 O32 Cl1 57.3(6) . . ? O14 O32 O24 102.8(12) . . ? O22 O32 O24 99.1(8) . . ? Cl1 O32 O24 52.2(5) . . ? O13 O33 O22 138.8(17) . . ? O13 O33 Cl1 79.8(12) . . ? O22 O33 Cl1 65.5(8) . . ? O13 O33 O23 21.0(9) . . ? O22 O33 O23 118.8(12) . . ? Cl1 O33 O23 67.9(7) . . ? O13 O33 O14 124.9(14) . . ? O22 O33 O14 14.7(6) . . ? Cl1 O33 O14 51.3(5) . . ? O23 O33 O14 105.8(8) . . ? O12 O34 O24 35.5(11) . . ? O12 O34 Cl1 86.7(14) . . ? O24 O34 Cl1 70.0(8) . . ? O12 O34 O23 149.1(17) . . ? O24 O34 O23 129.7(12) . . ? Cl1 O34 O23 64.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 N1 C11 -160.60(17) . . . . ? N1 Zn1 N1 C11 19.40(17) 2_656 . . . ? N21 Zn1 N1 C11 110.51(19) 2_656 . . . ? N21 Zn1 N1 C11 -71.94(19) . . . . ? O1 Zn1 N1 C15 18.4(2) . . . . ? N1 Zn1 N1 C15 -161.6(2) 2_656 . . . ? N21 Zn1 N1 C15 -70.46(19) 2_656 . . . ? N21 Zn1 N1 C15 107.09(19) . . . . ? C15 N1 C11 C12 -0.3(4) . . . . ? Zn1 N1 C11 C12 178.8(2) . . . . ? N1 C11 C12 C13 -0.7(4) . . . . ? C11 C12 C13 C14 1.5(4) . . . . ? C11 C12 C13 C16 -176.5(2) . . . . ? C12 C13 C14 C15 -1.4(4) . . . . ? C16 C13 C14 C15 176.7(2) . . . . ? C11 N1 C15 C14 0.4(4) . . . . ? Zn1 N1 C15 C14 -178.6(2) . . . . ? C13 C14 C15 N1 0.4(4) . . . . ? C12 C13 C16 C16 4.0(5) . . . 7_567 ? C14 C13 C16 C16 -173.9(3) . . . 7_567 ? O1 Zn1 N21 C25 49.53(18) . . . . ? N1 Zn1 N21 C25 165.56(19) 2_656 . . . ? N1 Zn1 N21 C25 -66.51(19) . . . . ? N21 Zn1 N21 C25 49.55(18) 2_656 . . . ? O1 Zn1 N21 C21 -123.0(2) . . . . ? N1 Zn1 N21 C21 -7.0(2) 2_656 . . . ? N1 Zn1 N21 C21 121.0(2) . . . . ? N21 Zn1 N21 C21 -123.0(2) 2_656 . . . ? C25 N21 C21 C22 -4.6(4) . . . . ? Zn1 N21 C21 C22 167.99(18) . . . . ? N21 C21 C22 C23 1.5(4) . . . . ? C21 C22 C23 C24 3.4(4) . . . . ? C21 C22 C23 C26 -176.6(2) . . . . ? C22 C23 C24 C25 -4.9(4) . . . . ? C26 C23 C24 C25 175.1(2) . . . . ? C21 N21 C25 C24 2.9(4) . . . . ? Zn1 N21 C25 C24 -170.5(2) . . . . ? C23 C24 C25 N21 1.9(4) . . . . ? C22 C23 C26 C27 27.0(3) . . . 5_566 ? C24 C23 C26 C27 -153.0(2) . . . 5_566 ? C22 C23 C26 C27 -80.0(3) . . . . ? C24 C23 C26 C27 99.9(3) . . . . ? C23 C26 C27 C28 0.4(3) . . . . ? C27 C26 C27 C28 -122.2(3) 5_566 . . . ? C23 C26 C27 C26 122.6(3) . . . 5_566 ? C27 C26 C27 C26 0.0 5_566 . . 5_566 ? C26 C27 C28 C29 -31.8(3) 5_566 . . . ? C26 C27 C28 C29 74.9(3) . . . . ? C26 C27 C28 C212 148.4(2) 5_566 . . . ? C26 C27 C28 C212 -104.9(3) . . . . ? C212 C28 C29 C210 -2.3(4) . . . . ? C27 C28 C29 C210 177.9(2) . . . . ? C28 C29 C210 N22 -1.2(4) . . . . ? C29 C210 N22 C211 3.2(4) . . . . ? C210 N22 C211 C212 -1.7(4) . . . . ? C29 C28 C212 C211 3.5(4) . . . . ? C27 C28 C212 C211 -176.6(2) . . . . ? N22 C211 C212 C28 -1.6(4) . . . . ? O33 Cl1 O12 O34 -11.6(19) . . . . ? O24 Cl1 O12 O34 -121(2) . . . . ? O22 Cl1 O12 O34 -89.2(17) . . . . ? O11 Cl1 O12 O34 124.9(14) . . . . ? O14 Cl1 O12 O34 -110.4(15) . . . . ? O13 Cl1 O12 O34 11.8(15) . . . . ? O32 Cl1 O12 O34 -132.6(15) . . . . ? O23 Cl1 O12 O34 9.6(15) . . . . ? O33 Cl1 O12 O24 109.8(17) . . . . ? O34 Cl1 O12 O24 121(2) . . . . ? O22 Cl1 O12 O24 32.3(17) . . . . ? O11 Cl1 O12 O24 -113.6(13) . . . . ? O14 Cl1 O12 O24 11.0(15) . . . . ? O13 Cl1 O12 O24 133.3(14) . . . . ? O32 Cl1 O12 O24 -11.1(14) . . . . ? O23 Cl1 O12 O24 131.0(14) . . . . ? O33 Cl1 O13 O23 146.0(18) . . . . ? O34 Cl1 O13 O23 -0.3(12) . . . . ? O24 Cl1 O13 O23 16.4(14) . . . . ? O22 Cl1 O13 O23 127.9(12) . . . . ? O11 Cl1 O13 O23 -117.2(11) . . . . ? O14 Cl1 O13 O23 117.2(11) . . . . ? O12 Cl1 O13 O23 -4.8(12) . . . . ? O32 Cl1 O13 O23 113.8(12) . . . . ? O34 Cl1 O13 O33 -146.2(13) . . . . ? O24 Cl1 O13 O33 -129.5(13) . . . . ? O22 Cl1 O13 O33 -18.0(13) . . . . ? O11 Cl1 O13 O33 96.8(12) . . . . ? O14 Cl1 O13 O33 -28.8(13) . . . . ? O12 Cl1 O13 O33 -150.7(12) . . . . ? O32 Cl1 O13 O33 -32.1(15) . . . . ? O23 Cl1 O13 O33 -146.0(18) . . . . ? O33 Cl1 O14 O22 7.5(13) . . . . ? O34 Cl1 O14 O22 122.3(13) . . . . ? O24 Cl1 O14 O22 150.3(13) . . . . ? O11 Cl1 O14 O22 -96.6(12) . . . . ? O13 Cl1 O14 O22 22.8(13) . . . . ? O12 Cl1 O14 O22 145.9(12) . . . . ? O32 Cl1 O14 O22 -161.9(19) . . . . ? O23 Cl1 O14 O22 51.6(13) . . . . ? O33 Cl1 O14 O32 169.4(11) . . . . ? O34 Cl1 O14 O32 -75.8(11) . . . . ? O24 Cl1 O14 O32 -47.8(10) . . . . ? O22 Cl1 O14 O32 161.9(19) . . . . ? O11 Cl1 O14 O32 65.3(11) . . . . ? O13 Cl1 O14 O32 -175.3(10) . . . . ? O12 Cl1 O14 O32 -52.2(11) . . . . ? O23 Cl1 O14 O32 -146.5(10) . . . . ? O34 Cl1 O14 O33 114.8(7) . . . . ? O24 Cl1 O14 O33 142.8(7) . . . . ? O22 Cl1 O14 O33 -7.5(13) . . . . ? O11 Cl1 O14 O33 -104.0(6) . . . . ? O13 Cl1 O14 O33 15.3(6) . . . . ? O12 Cl1 O14 O33 138.4(6) . . . . ? O32 Cl1 O14 O33 -169.4(11) . . . . ? O23 Cl1 O14 O33 44.1(7) . . . . ? O32 O14 O22 O33 -51(5) . . . . ? Cl1 O14 O22 O33 -13(2) . . . . ? Cl1 O14 O22 O32 38(4) . . . . ? O33 O14 O22 O32 51(5) . . . . ? O32 O14 O22 Cl1 -38(4) . . . . ? O33 O14 O22 Cl1 13(2) . . . . ? O33 Cl1 O22 O14 -170.7(17) . . . . ? O34 Cl1 O22 O14 -74.4(14) . . . . ? O24 Cl1 O22 O14 -32.0(13) . . . . ? O11 Cl1 O22 O14 97.6(12) . . . . ? O13 Cl1 O22 O14 -158.5(12) . . . . ? O12 Cl1 O22 O14 -45.3(15) . . . . ? O32 Cl1 O22 O14 10.2(11) . . . . ? O23 Cl1 O22 O14 -136.5(12) . . . . ? O34 Cl1 O22 O33 96.3(10) . . . . ? O24 Cl1 O22 O33 138.7(9) . . . . ? O11 Cl1 O22 O33 -91.7(8) . . . . ? O14 Cl1 O22 O33 170.7(17) . . . . ? O13 Cl1 O22 O33 12.1(8) . . . . ? O12 Cl1 O22 O33 125.4(9) . . . . ? O32 Cl1 O22 O33 -179.1(10) . . . . ? O23 Cl1 O22 O33 34.2(9) . . . . ? O33 Cl1 O22 O32 179.1(10) . . . . ? O34 Cl1 O22 O32 -84.6(8) . . . . ? O24 Cl1 O22 O32 -42.3(7) . . . . ? O11 Cl1 O22 O32 87.4(6) . . . . ? O14 Cl1 O22 O32 -10.2(11) . . . . ? O13 Cl1 O22 O32 -168.8(6) . . . . ? O12 Cl1 O22 O32 -55.5(8) . . . . ? O23 Cl1 O22 O32 -146.8(6) . . . . ? Cl1 O13 O23 O33 -48(2) . . . . ? O33 O13 O23 O34 48(3) . . . . ? Cl1 O13 O23 O34 0.3(13) . . . . ? O33 O13 O23 Cl1 48(2) . . . . ? O33 Cl1 O23 O13 -21.0(12) . . . . ? O34 Cl1 O23 O13 179.7(13) . . . . ? O24 Cl1 O23 O13 -166.6(11) . . . . ? O22 Cl1 O23 O13 -52.9(12) . . . . ? O11 Cl1 O23 O13 72.7(11) . . . . ? O14 Cl1 O23 O13 -75.4(12) . . . . ? O12 Cl1 O23 O13 175.5(11) . . . . ? O32 Cl1 O23 O13 -100.6(13) . . . . ? O34 Cl1 O23 O33 -159.3(9) . . . . ? O24 Cl1 O23 O33 -145.7(8) . . . . ? O22 Cl1 O23 O33 -31.9(8) . . . . ? O11 Cl1 O23 O33 93.7(7) . . . . ? O14 Cl1 O23 O33 -54.4(8) . . . . ? O13 Cl1 O23 O33 21.0(12) . . . . ? O12 Cl1 O23 O33 -163.5(8) . . . . ? O32 Cl1 O23 O33 -79.6(11) . . . . ? O33 Cl1 O23 O34 159.3(9) . . . . ? O24 Cl1 O23 O34 13.7(8) . . . . ? O22 Cl1 O23 O34 127.4(7) . . . . ? O11 Cl1 O23 O34 -107.0(6) . . . . ? O14 Cl1 O23 O34 104.9(6) . . . . ? O13 Cl1 O23 O34 -179.7(13) . . . . ? O12 Cl1 O23 O34 -4.2(6) . . . . ? O32 Cl1 O23 O34 79.8(9) . . . . ? Cl1 O12 O24 O34 -59.4(18) . . . . ? O34 O12 O24 Cl1 59.4(18) . . . . ? O34 O12 O24 O32 77(3) . . . . ? Cl1 O12 O24 O32 18(2) . . . . ? O33 Cl1 O24 O12 -98.5(18) . . . . ? O34 Cl1 O24 O12 -30.6(11) . . . . ? O22 Cl1 O24 O12 -154.8(13) . . . . ? O11 Cl1 O24 O12 73.8(14) . . . . ? O14 Cl1 O24 O12 -169.6(14) . . . . ? O13 Cl1 O24 O12 -57.2(16) . . . . ? O32 Cl1 O24 O12 168.0(15) . . . . ? O23 Cl1 O24 O12 -49.5(14) . . . . ? O33 Cl1 O24 O34 -67.9(16) . . . . ? O22 Cl1 O24 O34 -124.2(11) . . . . ? O11 Cl1 O24 O34 104.4(9) . . . . ? O14 Cl1 O24 O34 -139.0(10) . . . . ? O13 Cl1 O24 O34 -26.6(13) . . . . ? O12 Cl1 O24 O34 30.6(11) . . . . ? O32 Cl1 O24 O34 -161.4(11) . . . . ? O23 Cl1 O24 O34 -18.8(11) . . . . ? O33 Cl1 O24 O32 93.5(12) . . . . ? O34 Cl1 O24 O32 161.4(11) . . . . ? O22 Cl1 O24 O32 37.2(7) . . . . ? O11 Cl1 O24 O32 -94.2(5) . . . . ? O14 Cl1 O24 O32 22.4(5) . . . . ? O13 Cl1 O24 O32 134.8(6) . . . . ? O12 Cl1 O24 O32 -168.0(15) . . . . ? O23 Cl1 O24 O32 142.5(5) . . . . ? Cl1 O14 O32 O22 -37(4) . . . . ? O33 O14 O32 O22 -26(3) . . . . ? O22 O14 O32 Cl1 37(4) . . . . ? O33 O14 O32 Cl1 10.2(11) . . . . ? O22 O14 O32 O24 77(4) . . . . ? Cl1 O14 O32 O24 40.3(7) . . . . ? O33 O14 O32 O24 50.5(16) . . . . ? O33 O22 O32 O14 140(4) . . . . ? Cl1 O22 O32 O14 139(4) . . . . ? O14 O22 O32 Cl1 -139(4) . . . . ? O33 O22 O32 Cl1 1.0(12) . . . . ? O14 O22 O32 O24 -106(4) . . . . ? O33 O22 O32 O24 33.8(15) . . . . ? Cl1 O22 O32 O24 32.8(6) . . . . ? O33 Cl1 O32 O14 -11.1(12) . . . . ? O34 Cl1 O32 O14 114.7(10) . . . . ? O24 Cl1 O32 O14 127.1(11) . . . . ? O22 Cl1 O32 O14 -10.3(11) . . . . ? O11 Cl1 O32 O14 -123.4(9) . . . . ? O13 Cl1 O32 O14 6.6(14) . . . . ? O12 Cl1 O32 O14 131.9(10) . . . . ? O23 Cl1 O32 O14 50.5(14) . . . . ? O33 Cl1 O32 O22 -0.8(9) . . . . ? O34 Cl1 O32 O22 125.1(7) . . . . ? O24 Cl1 O32 O22 137.4(8) . . . . ? O11 Cl1 O32 O22 -113.0(6) . . . . ? O14 Cl1 O32 O22 10.3(11) . . . . ? O13 Cl1 O32 O22 16.9(9) . . . . ? O12 Cl1 O32 O22 142.2(6) . . . . ? O23 Cl1 O32 O22 60.8(10) . . . . ? O33 Cl1 O32 O24 -138.2(7) . . . . ? O34 Cl1 O32 O24 -12.4(7) . . . . ? O22 Cl1 O32 O24 -137.4(8) . . . . ? O11 Cl1 O32 O24 109.6(5) . . . . ? O14 Cl1 O32 O24 -127.1(11) . . . . ? O13 Cl1 O32 O24 -120.5(8) . . . . ? O12 Cl1 O32 O24 4.8(6) . . . . ? O23 Cl1 O32 O24 -76.6(9) . . . . ? O12 O24 O32 O14 -70(3) . . . . ? O34 O24 O32 O14 -28(2) . . . . ? Cl1 O24 O32 O14 -49.7(11) . . . . ? O12 O24 O32 O22 -56(3) . . . . ? O34 O24 O32 O22 -13.3(16) . . . . ? Cl1 O24 O32 O22 -35.2(6) . . . . ? O12 O24 O32 Cl1 -20(3) . . . . ? O34 O24 O32 Cl1 21.9(12) . . . . ? O23 O13 O33 O22 -21(4) . . . . ? Cl1 O13 O33 O22 32(2) . . . . ? O23 O13 O33 Cl1 -53(3) . . . . ? Cl1 O13 O33 O23 53(3) . . . . ? O23 O13 O33 O14 -27(3) . . . . ? Cl1 O13 O33 O14 25.8(10) . . . . ? O14 O22 O33 O13 -21(4) . . . . ? O32 O22 O33 O13 -36(3) . . . . ? Cl1 O22 O33 O13 -35(2) . . . . ? O14 O22 O33 Cl1 14(3) . . . . ? O32 O22 O33 Cl1 -1.1(12) . . . . ? O14 O22 O33 O23 -30(3) . . . . ? O32 O22 O33 O23 -44.7(19) . . . . ? Cl1 O22 O33 O23 -43.6(10) . . . . ? O32 O22 O33 O14 -15.1(18) . . . . ? Cl1 O22 O33 O14 -14(3) . . . . ? O34 Cl1 O33 O13 38.3(14) . . . . ? O24 Cl1 O33 O13 79.9(17) . . . . ? O22 Cl1 O33 O13 157.3(16) . . . . ? O11 Cl1 O33 O13 -92.7(11) . . . . ? O14 Cl1 O33 O13 152.8(12) . . . . ? O12 Cl1 O33 O13 43.2(17) . . . . ? O32 Cl1 O33 O13 158.1(10) . . . . ? O23 Cl1 O33 O13 18.0(10) . . . . ? O34 Cl1 O33 O22 -119.0(9) . . . . ? O24 Cl1 O33 O22 -77.4(14) . . . . ? O11 Cl1 O33 O22 110.0(7) . . . . ? O14 Cl1 O33 O22 -4.5(8) . . . . ? O13 Cl1 O33 O22 -157.3(16) . . . . ? O12 Cl1 O33 O22 -114.1(10) . . . . ? O32 Cl1 O33 O22 0.8(9) . . . . ? O23 Cl1 O33 O22 -139.2(10) . . . . ? O34 Cl1 O33 O23 20.2(9) . . . . ? O24 Cl1 O33 O23 61.9(14) . . . . ? O22 Cl1 O33 O23 139.2(10) . . . . ? O11 Cl1 O33 O23 -110.8(5) . . . . ? O14 Cl1 O33 O23 134.7(6) . . . . ? O13 Cl1 O33 O23 -18.0(10) . . . . ? O12 Cl1 O33 O23 25.2(12) . . . . ? O32 Cl1 O33 O23 140.1(7) . . . . ? O34 Cl1 O33 O14 -114.5(6) . . . . ? O24 Cl1 O33 O14 -72.9(12) . . . . ? O22 Cl1 O33 O14 4.5(8) . . . . ? O11 Cl1 O33 O14 114.5(4) . . . . ? O13 Cl1 O33 O14 -152.8(12) . . . . ? O12 Cl1 O33 O14 -109.6(9) . . . . ? O32 Cl1 O33 O14 5.3(6) . . . . ? O23 Cl1 O33 O14 -134.7(6) . . . . ? O34 O23 O33 O13 -139(3) . . . . ? Cl1 O23 O33 O13 -122(3) . . . . ? O13 O23 O33 O22 164(3) . . . . ? O34 O23 O33 O22 25.3(15) . . . . ? Cl1 O23 O33 O22 42.7(10) . . . . ? O13 O23 O33 Cl1 122(3) . . . . ? O34 O23 O33 Cl1 -17.4(8) . . . . ? O13 O23 O33 O14 157(3) . . . . ? O34 O23 O33 O14 17.8(10) . . . . ? Cl1 O23 O33 O14 35.2(4) . . . . ? O22 O14 O33 O13 163(4) . . . . ? O32 O14 O33 O13 -47(2) . . . . ? Cl1 O14 O33 O13 -33.3(14) . . . . ? O32 O14 O33 O22 150(3) . . . . ? Cl1 O14 O33 O22 164(3) . . . . ? O22 O14 O33 Cl1 -164(3) . . . . ? O32 O14 O33 Cl1 -13.7(15) . . . . ? O22 O14 O33 O23 153(3) . . . . ? O32 O14 O33 O23 -56.9(17) . . . . ? Cl1 O14 O33 O23 -43.2(6) . . . . ? Cl1 O12 O34 O24 59.4(18) . . . . ? O24 O12 O34 Cl1 -59.4(18) . . . . ? O24 O12 O34 O23 -79(4) . . . . ? Cl1 O12 O34 O23 -19(3) . . . . ? Cl1 O24 O34 O12 -114(2) . . . . ? O32 O24 O34 O12 -134(2) . . . . ? O12 O24 O34 Cl1 114(2) . . . . ? O32 O24 O34 Cl1 -20.1(11) . . . . ? O12 O24 O34 O23 139(3) . . . . ? Cl1 O24 O34 O23 25.1(13) . . . . ? O32 O24 O34 O23 5(2) . . . . ? O33 Cl1 O34 O12 171.4(14) . . . . ? O24 Cl1 O34 O12 32.1(12) . . . . ? O22 Cl1 O34 O12 109.7(16) . . . . ? O11 Cl1 O34 O12 -62.3(15) . . . . ? O14 Cl1 O34 O12 78.8(15) . . . . ? O13 Cl1 O34 O12 -169.0(14) . . . . ? O32 Cl1 O34 O12 50.1(15) . . . . ? O23 Cl1 O34 O12 -169.1(17) . . . . ? O33 Cl1 O34 O24 139.3(11) . . . . ? O22 Cl1 O34 O24 77.6(13) . . . . ? O11 Cl1 O34 O24 -94.4(10) . . . . ? O14 Cl1 O34 O24 46.7(12) . . . . ? O13 Cl1 O34 O24 158.9(10) . . . . ? O12 Cl1 O34 O24 -32.1(12) . . . . ? O32 Cl1 O34 O24 18.0(11) . . . . ? O23 Cl1 O34 O24 158.7(12) . . . . ? O33 Cl1 O34 O23 -19.4(9) . . . . ? O24 Cl1 O34 O23 -158.7(12) . . . . ? O22 Cl1 O34 O23 -81.1(9) . . . . ? O11 Cl1 O34 O23 106.9(5) . . . . ? O14 Cl1 O34 O23 -112.0(6) . . . . ? O13 Cl1 O34 O23 0.1(6) . . . . ? O12 Cl1 O34 O23 169.1(17) . . . . ? O32 Cl1 O34 O23 -140.8(6) . . . . ? O13 O23 O34 O12 21(4) . . . . ? O33 O23 O34 O12 39(4) . . . . ? Cl1 O23 O34 O12 21(3) . . . . ? O13 O23 O34 O24 -27(2) . . . . ? O33 O23 O34 O24 -8.9(19) . . . . ? Cl1 O23 O34 O24 -26.3(13) . . . . ? O13 O23 O34 Cl1 -0.3(15) . . . . ? O33 O23 O34 Cl1 17.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.714 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.087 data_[Zn(H2O)2(bpe)](SO4)(4H2O) _database_code_depnum_ccdc_archive 'CCDC 267590' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 N2 O10 S Zn' _chemical_formula_weight 451.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.424(3) _cell_length_b 9.7274(13) _cell_length_c 7.6253(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.731(2) _cell_angle_gamma 90.00 _cell_volume 1876.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2475 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5747 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.12 _reflns_number_total 3892 _reflns_number_gt 3336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(15) _refine_ls_number_reflns 3892 _refine_ls_number_parameters 262 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.228739(16) 0.44322(7) 0.76496(6) 0.02475(13) Uani 1 1 d . . . S1 S 0.27623(4) 0.11335(11) 0.83215(13) 0.0260(2) Uani 1 1 d . . . O11 O 0.26174(11) 0.2554(3) 0.8793(4) 0.0314(7) Uani 1 1 d . . . O12 O 0.28359(14) 0.0327(4) 0.9920(4) 0.0464(9) Uani 1 1 d . . . O13 O 0.32461(12) 0.1144(4) 0.7427(4) 0.0385(7) Uani 1 1 d . . . O14 O 0.23358(12) 0.0545(4) 0.7108(4) 0.0409(8) Uani 1 1 d . . . O2 O 0.20271(13) 0.6309(3) 0.6198(4) 0.0364(8) Uani 1 1 d D . . H2A H 0.1846(16) 0.625(5) 0.522(3) 0.055 Uiso 1 1 d D . . H2B H 0.1873(17) 0.695(4) 0.667(5) 0.055 Uiso 1 1 d D . . O3 O 0.23345(14) 0.3612(3) 0.5113(5) 0.0381(8) Uani 1 1 d D . . H3A H 0.242(2) 0.284(3) 0.475(7) 0.057 Uiso 1 1 d D . . H3B H 0.2448(19) 0.428(4) 0.456(6) 0.057 Uiso 1 1 d D . . N11 N 0.14943(14) 0.3806(4) 0.7578(5) 0.0296(8) Uani 1 1 d . . . C11 C 0.11148(19) 0.4663(6) 0.8062(7) 0.0482(15) Uani 1 1 d . . . H11 H 0.1204 0.5560 0.8393 0.058 Uiso 1 1 calc R . . C12 C 0.0597(2) 0.4232(9) 0.8075(8) 0.0614(17) Uani 1 1 d . . . H12 H 0.0354 0.4846 0.8466 0.074 Uiso 1 1 calc R . . C13 C 0.04270(17) 0.2982(9) 0.7555(8) 0.070(2) Uani 1 1 d D . . C14 C 0.0818(2) 0.2090(7) 0.7060(8) 0.067(2) Uani 1 1 d . . . H14 H 0.0730 0.1191 0.6735 0.080 Uiso 1 1 calc R . . C15 C 0.13470(19) 0.2543(6) 0.7049(7) 0.0435(12) Uani 1 1 d . . . H15 H 0.1598 0.1947 0.6665 0.052 Uiso 1 1 calc R . . C16 C -0.01149(18) 0.2764(9) 0.7674(10) 0.086(2) Uiso 1 1 d D . . H16 H -0.0312 0.3539 0.7895 0.104 Uiso 1 1 calc R . . N21 N 0.30648(14) 0.5261(4) 0.7756(5) 0.0322(9) Uani 1 1 d . . . C21 C 0.3179(2) 0.6553(5) 0.8171(7) 0.0449(13) Uani 1 1 d . . . H21 H 0.2911 0.7113 0.8513 0.054 Uiso 1 1 calc R . . C22 C 0.3677(3) 0.7118(7) 0.8123(8) 0.067(2) Uani 1 1 d . . . H22 H 0.3734 0.8038 0.8417 0.080 Uiso 1 1 calc R . . C23 C 0.4107(2) 0.6294(8) 0.7622(8) 0.067(2) Uani 1 1 d D . . C24 C 0.3964(2) 0.5003(9) 0.7259(9) 0.079(3) Uani 1 1 d . . . H24 H 0.4226 0.4395 0.6981 0.095 Uiso 1 1 calc R . . C25 C 0.34581(17) 0.4499(8) 0.7263(7) 0.0518(13) Uani 1 1 d . . . H25 H 0.3389 0.3596 0.6909 0.062 Uiso 1 1 calc R . . C26 C 0.4637(2) 0.6664(9) 0.7521(11) 0.095(3) Uiso 1 1 d D . . H26 H 0.4849 0.5921 0.7289 0.114 Uiso 1 1 calc R . . O4 O 0.16958(14) 0.8454(4) 0.8199(5) 0.0436(8) Uani 1 1 d D . . H41 H 0.1882(18) 0.815(4) 0.935(4) 0.065 Uiso 1 1 d D . . H42 H 0.1975(15) 0.918(4) 0.834(6) 0.065 Uiso 1 1 d D . . O5 O 1.0000 0.7566(11) 0.0000 0.109(3) Uani 1 2 d SD . . H5 H 1.022(3) 0.830(6) 0.064(12) 0.163 Uiso 1 1 d D . . O6 O 1.0000 0.6985(9) 0.5000 0.113(3) Uani 1 2 d SD . . H6 H 0.979(3) 0.784(5) 0.472(17) 0.170 Uiso 1 1 d D . . O7 O 0.93667(17) 0.6101(6) 0.7587(9) 0.0929(17) Uani 1 1 d D . . H71 H 0.9029(19) 0.572(9) 0.699(10) 0.139 Uiso 1 1 d D . . H72 H 0.916(3) 0.639(9) 0.858(8) 0.139 Uiso 1 1 d D . . O8 O 0.9431(2) 0.8621(6) 0.2550(10) 0.1029(19) Uani 1 1 d D . . H81 H 0.9045(9) 0.859(10) 0.271(12) 0.154 Uiso 1 1 d D . . H82 H 0.930(3) 0.815(10) 0.142(7) 0.154 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0193(2) 0.0267(2) 0.0286(2) -0.0008(2) 0.00417(15) -0.0038(3) S1 0.0248(6) 0.0272(5) 0.0264(5) 0.0008(4) 0.0050(4) 0.0000(4) O11 0.0322(16) 0.0284(15) 0.0339(17) 0.0007(13) 0.0040(13) -0.0011(14) O12 0.061(2) 0.0406(18) 0.0389(19) 0.0148(16) 0.0127(17) 0.0110(18) O13 0.0279(17) 0.0488(19) 0.0404(18) -0.0002(16) 0.0113(14) -0.0003(15) O14 0.0294(18) 0.0469(19) 0.0460(18) -0.0152(17) 0.0015(15) -0.0040(15) O2 0.043(2) 0.0343(18) 0.0322(17) -0.0023(15) 0.0033(15) 0.0041(15) O3 0.052(2) 0.0295(18) 0.0353(19) 0.0014(15) 0.0156(16) 0.0017(16) N11 0.0161(18) 0.037(2) 0.036(2) 0.0029(17) 0.0027(16) -0.0006(15) C11 0.032(2) 0.056(4) 0.058(3) 0.004(3) 0.015(2) 0.015(3) C12 0.026(2) 0.088(5) 0.071(4) 0.001(4) 0.007(2) 0.011(4) C13 0.016(3) 0.147(7) 0.049(4) 0.025(4) 0.003(2) -0.015(4) C14 0.051(4) 0.090(5) 0.057(4) 0.008(3) -0.012(3) -0.050(4) C15 0.033(3) 0.045(3) 0.053(3) 0.001(3) 0.006(2) -0.010(2) N21 0.0224(19) 0.037(2) 0.037(2) 0.0038(18) 0.0024(16) -0.0083(17) C21 0.042(3) 0.052(3) 0.040(3) -0.001(2) 0.003(2) -0.022(3) C22 0.078(5) 0.076(4) 0.045(3) -0.003(3) 0.001(3) -0.060(4) C23 0.040(3) 0.109(6) 0.051(3) 0.018(4) 0.000(3) -0.040(4) C24 0.024(3) 0.130(8) 0.086(5) 0.021(4) 0.014(3) -0.011(3) C25 0.026(2) 0.052(3) 0.080(4) 0.017(4) 0.016(2) 0.001(3) O4 0.044(2) 0.046(2) 0.041(2) -0.0034(16) 0.0009(17) -0.0012(16) O5 0.072(5) 0.126(7) 0.125(7) 0.000 -0.003(5) 0.000 O6 0.073(5) 0.130(8) 0.134(8) 0.000 -0.003(5) 0.000 O7 0.039(3) 0.091(4) 0.148(5) -0.004(4) 0.008(3) 0.007(3) O8 0.054(3) 0.087(4) 0.166(6) 0.002(4) 0.006(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O12 2.099(3) 4_557 ? Zn1 N11 2.102(3) . ? Zn1 O3 2.107(3) . ? Zn1 N21 2.128(4) . ? Zn1 O11 2.158(3) . ? Zn1 O2 2.203(3) . ? S1 O12 1.446(3) . ? S1 O13 1.465(3) . ? S1 O14 1.469(3) . ? S1 O11 1.483(3) . ? O12 Zn1 2.099(3) 4_547 ? O2 H2A 0.840(2) . ? O2 H2B 0.840(2) . ? O3 H3A 0.840(2) . ? O3 H3B 0.840(2) . ? N11 C15 1.335(6) . ? N11 C11 1.354(6) . ? C11 C12 1.382(8) . ? C11 H11 0.9300 . ? C12 C13 1.338(11) . ? C12 H12 0.9300 . ? C13 C14 1.400(10) . ? C13 C16 1.406(2) . ? C14 C15 1.415(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C26 1.241(9) 3_445 ? C16 H16 0.9300 . ? N21 C21 1.322(6) . ? N21 C25 1.328(7) . ? C21 C22 1.384(7) . ? C21 H21 0.9300 . ? C22 C23 1.437(10) . ? C22 H22 0.9300 . ? C23 C24 1.328(10) . ? C23 C26 1.405(2) . ? C24 C25 1.378(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C16 1.241(9) 3 ? C26 H26 0.9300 . ? O4 H41 1.000(2) . ? O4 H42 1.000(2) . ? O5 H5 1.000(2) . ? O6 H6 1.000(2) . ? O7 H71 1.000(2) . ? O7 H72 1.000(2) . ? O8 H81 1.000(2) . ? O8 H82 1.000(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Zn1 N11 85.16(14) 4_557 . ? O12 Zn1 O3 174.14(15) 4_557 . ? N11 Zn1 O3 90.50(14) . . ? O12 Zn1 N21 91.69(15) 4_557 . ? N11 Zn1 N21 174.54(16) . . ? O3 Zn1 N21 92.33(15) . . ? O12 Zn1 O11 94.65(13) 4_557 . ? N11 Zn1 O11 95.66(12) . . ? O3 Zn1 O11 89.69(12) . . ? N21 Zn1 O11 89.03(13) . . ? O12 Zn1 O2 92.06(13) 4_557 . ? N11 Zn1 O2 89.29(13) . . ? O3 Zn1 O2 83.93(13) . . ? N21 Zn1 O2 86.36(14) . . ? O11 Zn1 O2 171.97(12) . . ? O12 S1 O13 110.6(2) . . ? O12 S1 O14 110.2(2) . . ? O13 S1 O14 108.09(19) . . ? O12 S1 O11 108.4(2) . . ? O13 S1 O11 110.30(19) . . ? O14 S1 O11 109.26(19) . . ? S1 O11 Zn1 141.89(19) . . ? S1 O12 Zn1 162.0(2) . 4_547 ? Zn1 O2 H2A 120(3) . . ? Zn1 O2 H2B 122(3) . . ? H2A O2 H2B 101.4(3) . . ? Zn1 O3 H3A 133(4) . . ? Zn1 O3 H3B 103(4) . . ? H3A O3 H3B 114(6) . . ? C15 N11 C11 117.6(4) . . ? C15 N11 Zn1 120.9(3) . . ? C11 N11 Zn1 121.5(3) . . ? N11 C11 C12 121.3(6) . . ? N11 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 123.6(6) . . ? C13 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C12 C13 C14 115.2(4) . . ? C12 C13 C16 114.1(7) . . ? C14 C13 C16 130.6(8) . . ? C13 C14 C15 120.6(6) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N11 C15 C14 121.5(6) . . ? N11 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C26 C16 C13 128.0(8) 3_445 . ? C26 C16 H16 116.0 3_445 . ? C13 C16 H16 116.0 . . ? C21 N21 C25 116.4(5) . . ? C21 N21 Zn1 123.4(4) . . ? C25 N21 Zn1 120.0(4) . . ? N21 C21 C22 123.5(6) . . ? N21 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C21 C22 C23 120.5(6) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C26 118.2(8) . . ? C24 C23 C22 112.6(5) . . ? C26 C23 C22 129.1(7) . . ? C23 C24 C25 124.8(7) . . ? C23 C24 H24 117.6 . . ? C25 C24 H24 117.6 . . ? N21 C25 C24 122.1(7) . . ? N21 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C16 C26 C23 134.2(8) 3 . ? C16 C26 H26 112.9 3 . ? C23 C26 H26 112.9 . . ? H41 O4 H42 81.1(2) . . ? H71 O7 H72 88(6) . . ? H81 O8 H82 81.1(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 O12 S1 O11 Zn1 -164.4(3) . . . . ? O13 S1 O11 Zn1 74.4(3) . . . . ? O14 S1 O11 Zn1 -44.3(3) . . . . ? O12 Zn1 O11 S1 166.9(3) 4_557 . . . ? N11 Zn1 O11 S1 81.3(3) . . . . ? O3 Zn1 O11 S1 -9.2(3) . . . . ? N21 Zn1 O11 S1 -101.5(3) . . . . ? O2 Zn1 O11 S1 -46.5(11) . . . . ? O13 S1 O12 Zn1 170.7(8) . . . 4_547 ? O14 S1 O12 Zn1 -69.9(8) . . . 4_547 ? O11 S1 O12 Zn1 49.6(9) . . . 4_547 ? O12 Zn1 N11 C15 -137.4(4) 4_557 . . . ? O3 Zn1 N11 C15 46.5(4) . . . . ? N21 Zn1 N11 C15 167.7(15) . . . . ? O11 Zn1 N11 C15 -43.2(4) . . . . ? O2 Zn1 N11 C15 130.4(4) . . . . ? O12 Zn1 N11 C11 42.6(4) 4_557 . . . ? O3 Zn1 N11 C11 -133.5(4) . . . . ? N21 Zn1 N11 C11 -12.3(18) . . . . ? O11 Zn1 N11 C11 136.8(4) . . . . ? O2 Zn1 N11 C11 -49.5(4) . . . . ? C15 N11 C11 C12 2.4(7) . . . . ? Zn1 N11 C11 C12 -177.6(4) . . . . ? N11 C11 C12 C13 -2.7(9) . . . . ? C11 C12 C13 C14 2.8(9) . . . . ? C11 C12 C13 C16 -179.9(6) . . . . ? C12 C13 C14 C15 -2.9(9) . . . . ? C16 C13 C14 C15 -179.6(7) . . . . ? C11 N11 C15 C14 -2.5(7) . . . . ? Zn1 N11 C15 C14 177.5(4) . . . . ? C13 C14 C15 N11 2.9(8) . . . . ? C12 C13 C16 C26 -169.1(8) . . . 3_445 ? C14 C13 C16 C26 7.7(14) . . . 3_445 ? O12 Zn1 N21 C21 -46.6(4) 4_557 . . . ? N11 Zn1 N21 C21 8.1(19) . . . . ? O3 Zn1 N21 C21 129.1(4) . . . . ? O11 Zn1 N21 C21 -141.2(4) . . . . ? O2 Zn1 N21 C21 45.4(4) . . . . ? O12 Zn1 N21 C25 138.6(4) 4_557 . . . ? N11 Zn1 N21 C25 -166.7(15) . . . . ? O3 Zn1 N21 C25 -45.7(4) . . . . ? O11 Zn1 N21 C25 44.0(4) . . . . ? O2 Zn1 N21 C25 -129.4(4) . . . . ? C25 N21 C21 C22 -0.4(8) . . . . ? Zn1 N21 C21 C22 -175.4(4) . . . . ? N21 C21 C22 C23 -0.7(9) . . . . ? C21 C22 C23 C24 -0.6(9) . . . . ? C21 C22 C23 C26 -178.8(7) . . . . ? C26 C23 C24 C25 -178.5(7) . . . . ? C22 C23 C24 C25 3.2(10) . . . . ? C21 N21 C25 C24 2.9(8) . . . . ? Zn1 N21 C25 C24 178.0(4) . . . . ? C23 C24 C25 N21 -4.6(10) . . . . ? C24 C23 C26 C16 175.2(10) . . . 3 ? C22 C23 C26 C16 -6.7(16) . . . 3 ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.997 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.169