# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Cheal Kim' _publ_contact_author_email chealkim@snut.ac.kr loop_ _publ_author_name 'Cheal Kim' 'Sung-Jin Kim' 'Youngmee Kim' data_1 _database_code_depnum_ccdc_archive 'CCDC 756680' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 N4 O11 Zn2' _chemical_formula_weight 837.48 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 8.9211(12) _cell_length_b 9.6889(13) _cell_length_c 11.3220(15) _cell_angle_alpha 113.677(2) _cell_angle_beta 100.094(2) _cell_angle_gamma 91.366(2) _cell_volume 877.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2165 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.36 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.435 _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 4915 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3360 _reflns_number_gt 2691 _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. The positions of H atoms of a water ligand were refined isotropically with O-H restraints (0.93 \%A). ; _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^)+(0.0288P)^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 3360 _refine_ls_number_parameters 247 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 0.23164(3) 0.18267(3) 0.49677(2) 0.02980(10) Uani 1 1 d . . . O1 O 0.01961(19) 0.09510(19) 0.36870(16) 0.0360(4) Uani 1 1 d D . . H1A H 0.050(3) 0.015(2) 0.3014(19) 0.072(10) Uiso 1 1 d D . . H1B H -0.0670(18) 0.055(3) 0.384(2) 0.058(9) Uiso 1 1 d D . . O11 O 0.23599(18) 0.03833(18) 0.59784(14) 0.0335(4) Uani 1 1 d . . . O12 O 0.43151(18) 0.21027(17) 0.66181(15) 0.0347(4) Uani 1 1 d . . . O13 O 0.65262(18) -0.06041(17) 0.64489(14) 0.0346(4) Uani 1 1 d . . . O14 O 0.8414(2) 0.0967(2) 0.80013(18) 0.0626(6) Uani 1 1 d . . . N21 N 0.2726(2) 0.3830(2) 0.46716(17) 0.0279(4) Uani 1 1 d . . . N22 N 0.1247(2) 0.3517(2) 0.64002(17) 0.0313(5) Uani 1 1 d . . . C11 C 0.3633(3) 0.1052(2) 0.6745(2) 0.0273(5) Uani 1 1 d . . . C12 C 0.4228(3) 0.0545(3) 0.7835(2) 0.0298(5) Uani 1 1 d . . . H12 H 0.4089 -0.0565 0.7446 0.036 Uiso 1 1 calc R . . C13 C 0.5924(3) 0.1035(3) 0.8487(2) 0.0309(5) Uani 1 1 d . . . H13 H 0.6129 0.0541 0.9094 0.037 Uiso 1 1 calc R . . C14 C 0.6261(3) 0.2727(3) 0.9369(2) 0.0407(6) Uani 1 1 d . . . H14A H 0.7331 0.2950 0.9807 0.049 Uiso 1 1 calc R . . H14B H 0.6077 0.3298 0.8833 0.049 Uiso 1 1 calc R . . C15 C 0.5262(3) 0.3213(3) 1.0397(2) 0.0563(8) Uani 1 1 d . . . H15A H 0.5529 0.2730 1.0997 0.068 Uiso 1 1 calc R . . H15B H 0.5447 0.4301 1.0904 0.068 Uiso 1 1 calc R . . C16 C 0.3576(3) 0.2782(3) 0.9747(3) 0.0568(8) Uani 1 1 d . . . H16A H 0.2965 0.3060 1.0422 0.068 Uiso 1 1 calc R . . H16B H 0.3287 0.3341 0.9213 0.068 Uiso 1 1 calc R . . C17 C 0.3244(3) 0.1103(3) 0.8893(2) 0.0463(7) Uani 1 1 d . . . H17A H 0.2171 0.0879 0.8464 0.056 Uiso 1 1 calc R . . H17B H 0.3428 0.0552 0.9446 0.056 Uiso 1 1 calc R . . C18 C 0.7037(3) 0.0437(3) 0.7562(2) 0.0328(6) Uani 1 1 d . . . C21 C 0.3460(3) 0.3914(3) 0.3753(2) 0.0336(6) Uani 1 1 d . . . H21 H 0.3797 0.3037 0.3189 0.040 Uiso 1 1 calc R . . C22 C 0.3731(3) 0.5235(3) 0.3615(2) 0.0372(6) Uani 1 1 d . . . H22 H 0.4253 0.5253 0.2978 0.045 Uiso 1 1 calc R . . C23 C 0.3218(3) 0.6531(3) 0.4434(2) 0.0415(6) Uani 1 1 d . . . H23 H 0.3387 0.7441 0.4361 0.050 Uiso 1 1 calc R . . C24 C 0.2447(3) 0.6461(3) 0.5370(2) 0.0359(6) Uani 1 1 d . . . H24 H 0.2085 0.7326 0.5929 0.043 Uiso 1 1 calc R . . C25 C 0.2215(2) 0.5095(2) 0.5471(2) 0.0281(5) Uani 1 1 d . . . C26 C 0.1399(3) 0.4923(3) 0.6445(2) 0.0291(5) Uani 1 1 d . . . C27 C 0.0797(3) 0.6107(3) 0.7342(2) 0.0400(6) Uani 1 1 d . . . H27 H 0.0905 0.7075 0.7365 0.048 Uiso 1 1 calc R . . C28 C 0.0033(3) 0.5834(3) 0.8204(2) 0.0449(7) Uani 1 1 d . . . H28 H -0.0362 0.6621 0.8820 0.054 Uiso 1 1 calc R . . C29 C -0.0135(3) 0.4398(3) 0.8142(2) 0.0447(7) Uani 1 1 d . . . H29 H -0.0657 0.4187 0.8703 0.054 Uiso 1 1 calc R . . C210 C 0.0489(3) 0.3274(3) 0.7227(2) 0.0408(6) Uani 1 1 d . . . H210 H 0.0377 0.2296 0.7183 0.049 Uiso 1 1 calc R . . O1W O 0.9863(10) 0.9423(7) 0.9646(7) 0.147(3) Uiso 0.50 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 0.03198(17) 0.02907(16) 0.03319(16) 0.01586(12) 0.01065(12) 0.00773(12) O1 0.0275(10) 0.0363(10) 0.0446(10) 0.0160(8) 0.0100(8) 0.0033(8) O11 0.0265(9) 0.0407(10) 0.0360(9) 0.0191(8) 0.0055(8) 0.0025(8) O12 0.0343(10) 0.0384(10) 0.0403(9) 0.0245(8) 0.0099(8) 0.0020(8) O13 0.0325(10) 0.0355(9) 0.0317(9) 0.0087(8) 0.0084(8) 0.0071(8) O14 0.0342(12) 0.0733(14) 0.0544(12) -0.0030(10) 0.0172(10) 0.0005(10) N21 0.0250(11) 0.0299(10) 0.0317(10) 0.0151(9) 0.0071(9) 0.0046(9) N22 0.0291(11) 0.0362(11) 0.0335(10) 0.0170(9) 0.0114(9) 0.0079(9) C11 0.0262(13) 0.0313(13) 0.0283(12) 0.0126(10) 0.0134(11) 0.0087(11) C12 0.0306(14) 0.0324(13) 0.0320(12) 0.0183(11) 0.0084(11) 0.0032(11) C13 0.0299(14) 0.0400(14) 0.0293(12) 0.0193(11) 0.0087(11) 0.0071(11) C14 0.0325(14) 0.0458(15) 0.0318(13) 0.0034(12) 0.0074(12) 0.0042(12) C15 0.0507(19) 0.067(2) 0.0358(15) 0.0043(14) 0.0117(14) 0.0130(16) C16 0.0434(18) 0.083(2) 0.0399(15) 0.0152(15) 0.0219(14) 0.0186(16) C17 0.0366(16) 0.076(2) 0.0410(14) 0.0357(15) 0.0160(13) 0.0057(15) C18 0.0328(15) 0.0343(14) 0.0358(14) 0.0172(12) 0.0109(12) 0.0081(12) C21 0.0319(14) 0.0356(14) 0.0344(13) 0.0151(11) 0.0075(11) 0.0052(11) C22 0.0362(15) 0.0443(15) 0.0392(13) 0.0243(12) 0.0110(12) 0.0014(12) C23 0.0385(16) 0.0367(15) 0.0565(16) 0.0282(13) 0.0059(14) 0.0004(12) C24 0.0322(14) 0.0288(13) 0.0473(14) 0.0158(11) 0.0090(12) 0.0067(11) C25 0.0210(12) 0.0283(12) 0.0326(12) 0.0113(10) 0.0026(10) 0.0035(10) C26 0.0239(13) 0.0312(13) 0.0297(12) 0.0110(10) 0.0022(10) 0.0057(10) C27 0.0384(16) 0.0345(14) 0.0425(14) 0.0094(12) 0.0119(13) 0.0095(12) C28 0.0379(16) 0.0494(17) 0.0394(14) 0.0069(13) 0.0148(13) 0.0108(13) C29 0.0365(16) 0.0649(19) 0.0391(14) 0.0244(14) 0.0162(13) 0.0089(14) C210 0.0421(16) 0.0429(15) 0.0465(15) 0.0238(13) 0.0179(13) 0.0097(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 O13 2.0383(15) 2_656 ? Zn1 O1 2.0915(17) . ? Zn1 O11 2.1305(16) . ? Zn1 N21 2.1320(18) . ? Zn1 N22 2.1693(18) . ? Zn1 O12 2.2694(16) . ? Zn1 C11 2.534(2) . ? O1 H1A 0.93(2) . ? O1 H1B 0.93(2) . ? O11 C11 1.277(3) . ? O12 C11 1.243(2) . ? O13 C18 1.252(3) . ? O13 Zn1 2.0383(15) 2_656 ? O14 C18 1.253(3) . ? N21 C25 1.345(3) . ? N21 C21 1.350(3) . ? N22 C210 1.334(3) . ? N22 C26 1.346(3) . ? C11 C12 1.522(3) . ? C12 C13 1.533(3) . ? C12 C17 1.539(3) . ? C12 H12 0.9800 . ? C13 C18 1.525(3) . ? C13 C14 1.527(3) . ? C13 H13 0.9800 . ? C14 C15 1.522(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.521(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.511(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C21 C22 1.371(3) . ? C21 H21 0.9300 . ? C22 C23 1.374(3) . ? C22 H22 0.9300 . ? C23 C24 1.382(3) . ? C23 H23 0.9300 . ? C24 C25 1.388(3) . ? C24 H24 0.9300 . ? C25 C26 1.481(3) . ? C26 C27 1.386(3) . ? C27 C28 1.385(3) . ? C27 H27 0.9300 . ? C28 C29 1.368(4) . ? C28 H28 0.9300 . ? C29 C210 1.377(3) . ? C29 H29 0.9300 . ? C210 H210 0.9300 . ? O1W O1W 1.073(11) 2_777 ? 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 O13 Zn1 O1 92.16(6) 2_656 . ? O13 Zn1 O11 98.68(6) 2_656 . ? O1 Zn1 O11 98.30(6) . . ? O13 Zn1 N21 92.21(7) 2_656 . ? O1 Zn1 N21 99.80(7) . . ? O11 Zn1 N21 158.46(6) . . ? O13 Zn1 N22 168.24(7) 2_656 . ? O1 Zn1 N22 91.02(7) . . ? O11 Zn1 N22 92.06(6) . . ? N21 Zn1 N22 76.08(7) . . ? O13 Zn1 O12 92.53(6) 2_656 . ? O1 Zn1 O12 157.84(6) . . ? O11 Zn1 O12 59.57(6) . . ? N21 Zn1 O12 101.64(6) . . ? N22 Zn1 O12 88.76(6) . . ? O13 Zn1 C11 97.05(6) 2_656 . ? O1 Zn1 C11 128.51(7) . . ? O11 Zn1 C11 30.24(6) . . ? N21 Zn1 C11 130.10(7) . . ? N22 Zn1 C11 89.80(7) . . ? O12 Zn1 C11 29.34(6) . . ? Zn1 O1 H1A 99.8(18) . . ? Zn1 O1 H1B 128.2(16) . . ? H1A O1 H1B 105(2) . . ? C11 O11 Zn1 92.63(13) . . ? C11 O12 Zn1 87.20(13) . . ? C18 O13 Zn1 129.03(16) . 2_656 ? C25 N21 C21 118.4(2) . . ? C25 N21 Zn1 116.81(14) . . ? C21 N21 Zn1 124.78(15) . . ? C210 N22 C26 118.9(2) . . ? C210 N22 Zn1 125.61(17) . . ? C26 N22 Zn1 115.53(15) . . ? O12 C11 O11 120.5(2) . . ? O12 C11 C12 122.3(2) . . ? O11 C11 C12 117.1(2) . . ? O12 C11 Zn1 63.46(12) . . ? O11 C11 Zn1 57.13(11) . . ? C12 C11 Zn1 172.96(16) . . ? C11 C12 C13 115.56(18) . . ? C11 C12 C17 109.35(19) . . ? C13 C12 C17 109.58(18) . . ? C11 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C17 C12 H12 107.3 . . ? C18 C13 C14 113.5(2) . . ? C18 C13 C12 114.92(18) . . ? C14 C13 C12 113.36(19) . . ? C18 C13 H13 104.5 . . ? C14 C13 H13 104.5 . . ? C12 C13 H13 104.5 . . ? C15 C14 C13 111.1(2) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 110.8(2) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 111.4(2) . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C12 112.8(2) . . ? C16 C17 H17A 109.0 . . ? C12 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C12 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? O13 C18 O14 124.9(2) . . ? O13 C18 C13 117.7(2) . . ? O14 C18 C13 117.3(2) . . ? N21 C21 C22 122.9(2) . . ? N21 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C21 C22 C23 118.8(2) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C24 119.0(2) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 119.7(2) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N21 C25 C24 121.1(2) . . ? N21 C25 C26 115.8(2) . . ? C24 C25 C26 123.1(2) . . ? N22 C26 C27 120.8(2) . . ? N22 C26 C25 115.7(2) . . ? C27 C26 C25 123.4(2) . . ? C28 C27 C26 119.4(2) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 119.5(2) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C210 118.2(2) . . ? C28 C29 H29 120.9 . . ? C210 C29 H29 120.9 . . ? N22 C210 C29 123.2(2) . . ? N22 C210 H210 118.4 . . ? C29 C210 H210 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Zn1 O11 C11 89.12(12) 2_656 . . . ? O1 Zn1 O11 C11 -177.39(12) . . . . ? N21 Zn1 O11 C11 -30.4(2) . . . . ? N22 Zn1 O11 C11 -86.06(12) . . . . ? O12 Zn1 O11 C11 1.29(11) . . . . ? O13 Zn1 O12 C11 -99.91(12) 2_656 . . . ? O1 Zn1 O12 C11 2.1(2) . . . . ? O11 Zn1 O12 C11 -1.33(11) . . . . ? N21 Zn1 O12 C11 167.30(12) . . . . ? N22 Zn1 O12 C11 91.79(12) . . . . ? O13 Zn1 N21 C25 -176.92(15) 2_656 . . . ? O1 Zn1 N21 C25 90.51(15) . . . . ? O11 Zn1 N21 C25 -56.3(2) . . . . ? N22 Zn1 N21 C25 1.89(14) . . . . ? O12 Zn1 N21 C25 -83.88(15) . . . . ? C11 Zn1 N21 C25 -75.78(17) . . . . ? O13 Zn1 N21 C21 2.71(18) 2_656 . . . ? O1 Zn1 N21 C21 -89.86(18) . . . . ? O11 Zn1 N21 C21 123.3(2) . . . . ? N22 Zn1 N21 C21 -178.47(19) . . . . ? O12 Zn1 N21 C21 95.76(18) . . . . ? C11 Zn1 N21 C21 103.85(18) . . . . ? O13 Zn1 N22 C210 -175.7(3) 2_656 . . . ? O1 Zn1 N22 C210 78.7(2) . . . . ? O11 Zn1 N22 C210 -19.7(2) . . . . ? N21 Zn1 N22 C210 178.5(2) . . . . ? O12 Zn1 N22 C210 -79.18(19) . . . . ? C11 Zn1 N22 C210 -49.9(2) . . . . ? O13 Zn1 N22 C26 3.4(4) 2_656 . . . ? O1 Zn1 N22 C26 -102.25(16) . . . . ? O11 Zn1 N22 C26 159.40(16) . . . . ? N21 Zn1 N22 C26 -2.40(15) . . . . ? O12 Zn1 N22 C26 99.91(16) . . . . ? C11 Zn1 N22 C26 129.24(16) . . . . ? Zn1 O12 C11 O11 2.22(18) . . . . ? Zn1 O12 C11 C12 -175.39(18) . . . . ? Zn1 O11 C11 O12 -2.4(2) . . . . ? Zn1 O11 C11 C12 175.37(16) . . . . ? O13 Zn1 C11 O12 82.58(12) 2_656 . . . ? O1 Zn1 C11 O12 -178.98(11) . . . . ? O11 Zn1 C11 O12 177.73(19) . . . . ? N21 Zn1 C11 O12 -16.34(15) . . . . ? N22 Zn1 C11 O12 -87.83(12) . . . . ? O13 Zn1 C11 O11 -95.15(12) 2_656 . . . ? O1 Zn1 C11 O11 3.30(15) . . . . ? N21 Zn1 C11 O11 165.93(11) . . . . ? N22 Zn1 C11 O11 94.44(12) . . . . ? O12 Zn1 C11 O11 -177.73(19) . . . . ? O12 C11 C12 C13 -18.5(3) . . . . ? O11 C11 C12 C13 163.84(17) . . . . ? O12 C11 C12 C17 105.7(2) . . . . ? O11 C11 C12 C17 -72.0(2) . . . . ? C11 C12 C13 C18 -61.0(3) . . . . ? C17 C12 C13 C18 175.0(2) . . . . ? C11 C12 C13 C14 71.8(2) . . . . ? C17 C12 C13 C14 -52.2(3) . . . . ? C18 C13 C14 C15 -172.1(2) . . . . ? C12 C13 C14 C15 54.5(3) . . . . ? C13 C14 C15 C16 -55.2(3) . . . . ? C14 C15 C16 C17 56.4(3) . . . . ? C15 C16 C17 C12 -56.1(3) . . . . ? C11 C12 C17 C16 -74.6(3) . . . . ? C13 C12 C17 C16 53.0(3) . . . . ? Zn1 O13 C18 O14 2.6(4) 2_656 . . . ? Zn1 O13 C18 C13 -173.17(14) 2_656 . . . ? C14 C13 C18 O13 -146.1(2) . . . . ? C12 C13 C18 O13 -13.4(3) . . . . ? C14 C13 C18 O14 37.8(3) . . . . ? C12 C13 C18 O14 170.5(2) . . . . ? C25 N21 C21 C22 1.2(3) . . . . ? Zn1 N21 C21 C22 -178.45(17) . . . . ? N21 C21 C22 C23 -0.8(4) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C22 C23 C24 C25 0.5(4) . . . . ? C21 N21 C25 C24 -0.7(3) . . . . ? Zn1 N21 C25 C24 178.97(17) . . . . ? C21 N21 C25 C26 179.16(19) . . . . ? Zn1 N21 C25 C26 -1.2(2) . . . . ? C23 C24 C25 N21 -0.1(3) . . . . ? C23 C24 C25 C26 -179.9(2) . . . . ? C210 N22 C26 C27 0.7(3) . . . . ? Zn1 N22 C26 C27 -178.43(16) . . . . ? C210 N22 C26 C25 -178.3(2) . . . . ? Zn1 N22 C26 C25 2.6(2) . . . . ? N21 C25 C26 N22 -1.0(3) . . . . ? C24 C25 C26 N22 178.9(2) . . . . ? N21 C25 C26 C27 -179.93(19) . . . . ? C24 C25 C26 C27 -0.1(3) . . . . ? N22 C26 C27 C28 0.2(3) . . . . ? C25 C26 C27 C28 179.1(2) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C210 0.9(4) . . . . ? C26 N22 C210 C29 -0.8(4) . . . . ? Zn1 N22 C210 C29 178.24(17) . . . . ? C28 C29 C210 N22 0.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.488 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.067 data_2 _database_code_depnum_ccdc_archive 'CCDC 756681' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H44 N2 O14 Zn2' _chemical_formula_weight 763.4 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 5.8322(6) _cell_length_b 10.6119(10) _cell_length_c 13.5639(13) _cell_angle_alpha 89.324(2) _cell_angle_beta 86.923(2) _cell_angle_gamma 86.978(2) _cell_volume 837.07(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2102 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 1.501 _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 4699 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3206 _reflns_number_gt 2574 _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. The positions of H atoms of a water ligand were refined isotropically with O-H restraints (0.86 \%A) and U~iso~(H) = 1.2U~eq~(O), and the positions of H atoms of water solvent molecules were refined isotropically with O-H restraints (0.93 \%A) and U~iso~(H) = 1.2U~eq~(O). ; _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^)+(0.0529P)^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 3206 _refine_ls_number_parameters 210 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.973 _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 0.69627(6) 0.58755(3) 0.86369(2) 0.03050(13) Uani 1 1 d . . . O1 O 0.3724(4) 0.52538(19) 0.88264(17) 0.0394(5) Uani 1 1 d D . . H1A H 0.355(6) 0.4602(18) 0.9199(19) 0.047 Uiso 1 1 d D . . H1B H 0.260(4) 0.577(2) 0.900(2) 0.047 Uiso 1 1 d D . . O11 O 0.7049(3) 0.67885(18) 0.99317(15) 0.0344(5) Uani 1 1 d . . . O12 O 1.0256(4) 0.71384(19) 0.90682(15) 0.0388(5) Uani 1 1 d . . . O13 O 1.1388(4) 0.57122(18) 1.10518(17) 0.0408(5) Uani 1 1 d . . . O14 O 1.0763(5) 0.5780(2) 1.26516(19) 0.0712(8) Uani 1 1 d . . . N21 N 0.6438(4) 0.7009(2) 0.74605(18) 0.0331(6) Uani 1 1 d . . . C11 C 0.9006(5) 0.7282(2) 0.9841(2) 0.0309(7) Uani 1 1 d . . . C12 C 0.9646(5) 0.8114(3) 1.0673(2) 0.0331(7) Uani 1 1 d . . . H12 H 0.8589 0.8862 1.0655 0.040 Uiso 1 1 calc R . . C13 C 0.9229(5) 0.7514(3) 1.1697(2) 0.0367(7) Uani 1 1 d . . . H13 H 0.7594 0.7341 1.1771 0.044 Uiso 1 1 calc R . . C14 C 0.9701(7) 0.8448(3) 1.2506(3) 0.0609(11) Uani 1 1 d . . . H14A H 0.9540 0.8035 1.3146 0.073 Uiso 1 1 calc R . . H14B H 0.8575 0.9153 1.2495 0.073 Uiso 1 1 calc R . . C15 C 1.2123(8) 0.8938(4) 1.2360(3) 0.0687(12) Uani 1 1 d . . . H15A H 1.2337 0.9561 1.2861 0.082 Uiso 1 1 calc R . . H15B H 1.3251 0.8245 1.2443 0.082 Uiso 1 1 calc R . . C16 C 1.2514(7) 0.9528(3) 1.1346(3) 0.0642(11) Uani 1 1 d . . . H16A H 1.4087 0.9782 1.1264 0.077 Uiso 1 1 calc R . . H16B H 1.1500 1.0276 1.1288 0.077 Uiso 1 1 calc R . . C17 C 1.2062(6) 0.8603(3) 1.0538(3) 0.0450(8) Uani 1 1 d . . . H17A H 1.3186 0.7897 1.0552 0.054 Uiso 1 1 calc R . . H17B H 1.2235 0.9018 0.9900 0.054 Uiso 1 1 calc R . . C18 C 1.0585(5) 0.6261(3) 1.1821(2) 0.0375(7) Uani 1 1 d . . . C21 C 0.4443(5) 0.7690(3) 0.7403(2) 0.0415(8) Uani 1 1 d . . . H21 H 0.3351 0.7655 0.7927 0.050 Uiso 1 1 calc R . . C22 C 0.3955(6) 0.8438(3) 0.6598(3) 0.0482(9) Uani 1 1 d . . . H22 H 0.2555 0.8900 0.6589 0.058 Uiso 1 1 calc R . . C23 C 0.5527(7) 0.8509(3) 0.5804(2) 0.0465(9) Uani 1 1 d . . . C24 C 0.7565(7) 0.7820(3) 0.5876(3) 0.0565(10) Uani 1 1 d . . . H24 H 0.8691 0.7849 0.5365 0.068 Uiso 1 1 calc R . . C25 C 0.7957(6) 0.7085(3) 0.6697(3) 0.0503(9) Uani 1 1 d . . . H25 H 0.9349 0.6619 0.6720 0.060 Uiso 1 1 calc R . . C26 C 0.4999(9) 0.9317(3) 0.4907(3) 0.0670(12) Uani 1 1 d . . . H26A H 0.6131 0.9103 0.4377 0.080 Uiso 1 1 calc R . . H26B H 0.3504 0.9120 0.4689 0.080 Uiso 1 1 calc R . . O1W O 0.7244(8) 0.3500(4) 0.5565(4) 0.1261(14) Uiso 1 1 d D . . H1WA H 0.580(5) 0.381(5) 0.587(4) 0.151 Uiso 1 1 d D . . H1WB H 0.797(9) 0.403(4) 0.508(3) 0.151 Uiso 1 1 d D . . O2W O 0.2815(10) 0.4708(5) 0.5945(4) 0.174(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0345(2) 0.0278(2) 0.0292(2) 0.01001(14) -0.00606(14) 0.00107(13) O1 0.0344(12) 0.0355(13) 0.0481(14) 0.0140(10) -0.0009(10) -0.0033(9) O11 0.0333(11) 0.0329(11) 0.0371(12) 0.0044(9) -0.0046(9) -0.0014(9) O12 0.0442(12) 0.0407(12) 0.0307(12) 0.0058(10) 0.0013(10) 0.0010(10) O13 0.0461(13) 0.0294(11) 0.0460(14) 0.0041(10) -0.0077(11) 0.0097(10) O14 0.108(2) 0.0564(16) 0.0478(16) 0.0214(13) -0.0138(16) 0.0104(15) N21 0.0383(14) 0.0312(13) 0.0299(14) 0.0097(11) -0.0050(11) -0.0024(11) C11 0.0389(17) 0.0203(14) 0.0334(17) 0.0072(12) -0.0077(14) 0.0043(12) C12 0.0401(17) 0.0244(15) 0.0345(17) 0.0028(13) -0.0060(14) 0.0058(12) C13 0.0406(18) 0.0346(17) 0.0344(18) 0.0005(14) -0.0041(14) 0.0057(13) C14 0.094(3) 0.048(2) 0.039(2) -0.0081(17) -0.014(2) 0.018(2) C15 0.093(3) 0.053(2) 0.064(3) -0.009(2) -0.037(2) -0.010(2) C16 0.078(3) 0.041(2) 0.077(3) 0.006(2) -0.031(2) -0.0169(18) C17 0.050(2) 0.0318(17) 0.055(2) 0.0098(16) -0.0125(17) -0.0094(14) C18 0.0417(18) 0.0314(16) 0.0397(19) 0.0085(15) -0.0082(15) -0.0025(14) C21 0.0444(19) 0.0398(18) 0.0392(19) 0.0144(15) 0.0034(15) 0.0017(15) C22 0.057(2) 0.0397(19) 0.047(2) 0.0156(16) -0.0127(18) 0.0084(16) C23 0.081(3) 0.0302(17) 0.0284(17) 0.0077(14) -0.0090(18) -0.0010(17) C24 0.076(3) 0.050(2) 0.040(2) 0.0173(17) 0.0166(19) 0.0053(19) C25 0.049(2) 0.050(2) 0.049(2) 0.0219(17) 0.0085(17) 0.0079(16) C26 0.124(4) 0.043(2) 0.034(2) 0.0152(17) -0.014(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O13 1.9489(19) 2_767 ? Zn1 N21 2.014(2) . ? Zn1 O11 2.020(2) . ? Zn1 O1 2.036(2) . ? O1 H1A 0.86(2) . ? O1 H1B 0.86(2) . ? O11 C11 1.280(3) . ? O12 C11 1.250(4) . ? O13 C18 1.257(4) . ? O13 Zn1 1.9489(19) 2_767 ? O14 C18 1.238(4) . ? N21 C25 1.331(4) . ? N21 C21 1.342(4) . ? C11 C12 1.515(4) . ? C12 C17 1.528(4) . ? C12 C13 1.535(4) . ? C12 H12 0.9800 . ? C13 C18 1.523(4) . ? C13 C14 1.532(5) . ? C13 H13 0.9800 . ? C14 C15 1.533(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.517(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.522(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C21 C22 1.376(4) . ? C21 H21 0.9300 . ? C22 C23 1.380(5) . ? C22 H22 0.9300 . ? C23 C24 1.370(5) . ? C23 C26 1.515(4) . ? C24 C25 1.375(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C26 1.475(7) 2_676 ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? O1W H1WA 0.96(4) . ? O1W H1WB 0.96(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 O13 Zn1 N21 138.92(10) 2_767 . ? O13 Zn1 O11 100.78(9) 2_767 . ? N21 Zn1 O11 114.56(9) . . ? O13 Zn1 O1 97.25(9) 2_767 . ? N21 Zn1 O1 97.87(9) . . ? O11 Zn1 O1 97.96(9) . . ? Zn1 O1 H1A 117(2) . . ? Zn1 O1 H1B 120(2) . . ? H1A O1 H1B 105(3) . . ? C11 O11 Zn1 101.69(18) . . ? C18 O13 Zn1 111.42(19) . 2_767 ? C25 N21 C21 117.0(3) . . ? C25 N21 Zn1 123.0(2) . . ? C21 N21 Zn1 120.0(2) . . ? O12 C11 O11 120.7(3) . . ? O12 C11 C12 122.0(3) . . ? O11 C11 C12 117.1(3) . . ? C11 C12 C17 114.0(3) . . ? C11 C12 C13 113.1(2) . . ? C17 C12 C13 111.6(3) . . ? C11 C12 H12 105.8 . . ? C17 C12 H12 105.8 . . ? C13 C12 H12 105.8 . . ? C18 C13 C14 111.6(3) . . ? C18 C13 C12 113.0(3) . . ? C14 C13 C12 110.4(3) . . ? C18 C13 H13 107.2 . . ? C14 C13 H13 107.2 . . ? C12 C13 H13 107.2 . . ? C13 C14 C15 111.3(3) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.6(3) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.0(3) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C12 111.4(3) . . ? C16 C17 H17A 109.4 . . ? C12 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C12 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O14 C18 O13 122.0(3) . . ? O14 C18 C13 120.3(3) . . ? O13 C18 C13 117.6(3) . . ? N21 C21 C22 122.4(3) . . ? N21 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 116.5(3) . . ? C24 C23 C26 122.4(3) . . ? C22 C23 C26 121.1(3) . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? N21 C25 C24 123.1(3) . . ? N21 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C26 C26 C23 113.5(4) 2_676 . ? C26 C26 H26A 108.9 2_676 . ? C23 C26 H26A 108.9 . . ? C26 C26 H26B 108.9 2_676 . ? C23 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? H1WA O1W H1WB 117(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Zn1 O11 C11 85.03(17) 2_767 . . . ? N21 Zn1 O11 C11 -73.52(18) . . . . ? O1 Zn1 O11 C11 -175.98(16) . . . . ? O13 Zn1 N21 C25 -28.5(3) 2_767 . . . ? O11 Zn1 N21 C25 118.3(3) . . . . ? O1 Zn1 N21 C25 -139.2(3) . . . . ? O13 Zn1 N21 C21 148.5(2) 2_767 . . . ? O11 Zn1 N21 C21 -64.6(3) . . . . ? O1 Zn1 N21 C21 37.9(3) . . . . ? Zn1 O11 C11 O12 1.4(3) . . . . ? Zn1 O11 C11 C12 177.17(18) . . . . ? O12 C11 C12 C17 -7.8(4) . . . . ? O11 C11 C12 C17 176.5(2) . . . . ? O12 C11 C12 C13 -136.6(3) . . . . ? O11 C11 C12 C13 47.7(3) . . . . ? C11 C12 C13 C18 59.4(3) . . . . ? C17 C12 C13 C18 -70.7(3) . . . . ? C11 C12 C13 C14 -174.9(3) . . . . ? C17 C12 C13 C14 55.1(3) . . . . ? C18 C13 C14 C15 71.6(4) . . . . ? C12 C13 C14 C15 -54.9(4) . . . . ? C13 C14 C15 C16 55.8(4) . . . . ? C14 C15 C16 C17 -55.7(4) . . . . ? C15 C16 C17 C12 55.7(4) . . . . ? C11 C12 C17 C16 174.7(2) . . . . ? C13 C12 C17 C16 -55.8(3) . . . . ? Zn1 O13 C18 O14 -3.5(4) 2_767 . . . ? Zn1 O13 C18 C13 -179.5(2) 2_767 . . . ? C14 C13 C18 O14 41.6(4) . . . . ? C12 C13 C18 O14 166.7(3) . . . . ? C14 C13 C18 O13 -142.3(3) . . . . ? C12 C13 C18 O13 -17.2(4) . . . . ? C25 N21 C21 C22 0.0(5) . . . . ? Zn1 N21 C21 C22 -177.2(2) . . . . ? N21 C21 C22 C23 0.4(5) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C21 C22 C23 C26 179.2(3) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? C26 C23 C24 C25 -179.0(3) . . . . ? C21 N21 C25 C24 0.2(5) . . . . ? Zn1 N21 C25 C24 177.3(3) . . . . ? C23 C24 C25 N21 -0.9(6) . . . . ? C24 C23 C26 C26 -108.6(6) . . . 2_676 ? C22 C23 C26 C26 71.2(6) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.748 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.087 data_3 _database_code_depnum_ccdc_archive 'CCDC 756682' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 N2 O10 Zn2' _chemical_formula_weight 691.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 6.167(3) _cell_length_b 12.715(7) _cell_length_c 13.095(7) _cell_angle_alpha 114.959(8) _cell_angle_beta 97.225(9) _cell_angle_gamma 93.347(8) _cell_volume 916.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 21.12 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 1.356 _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 5001 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1968 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3496 _reflns_number_gt 1826 _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. The positions of C and O atoms of methanol solvent molecules were refined isotropically with half occupancies and C-O restraints (1.48 \%A). The position of C13 atom was refined isotropically. ; _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^)+(0.1266P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3496 _refine_ls_number_parameters 210 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2633 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.016 _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 0.53301(17) 0.59375(8) 0.96439(10) 0.0336(4) Uani 1 1 d . . . O11 O 0.6917(10) 0.4729(5) 0.8559(5) 0.0395(16) Uani 1 1 d . . . O12 O 0.6492(10) 0.3312(5) 0.9138(6) 0.0418(17) Uani 1 1 d . . . O13 O 1.2215(10) 0.3979(5) 0.9033(6) 0.0460(17) Uani 1 1 d . . . O14 O 1.2644(10) 0.5299(5) 0.8356(6) 0.0472(17) Uani 1 1 d . . . N21 N 0.6868(12) 0.7404(6) 0.9638(7) 0.038(2) Uani 1 1 d . . . C11 C 0.7129(13) 0.3708(7) 0.8457(8) 0.036(2) Uani 1 1 d . . . C12 C 0.8179(14) 0.2939(7) 0.7486(8) 0.035(2) Uani 1 1 d . . . H12 H 0.7034 0.2655 0.6807 0.041 Uiso 1 1 calc R . . C13 C 1.0077(14) 0.3649(8) 0.7251(8) 0.037(2) Uani 1 1 d U . . H13 H 0.9425 0.4183 0.6973 0.044 Uiso 1 1 calc R . . C14 C 1.1290(19) 0.2821(9) 0.6341(10) 0.064(3) Uani 1 1 d . . . H14A H 1.0354 0.2546 0.5603 0.077 Uiso 1 1 calc R . . H14B H 1.2606 0.3263 0.6320 0.077 Uiso 1 1 calc R . . C15 C 1.1955(17) 0.1770(10) 0.6502(11) 0.066(3) Uani 1 1 d . . . H15A H 1.3032 0.2028 0.7194 0.079 Uiso 1 1 calc R . . H15B H 1.2637 0.1284 0.5864 0.079 Uiso 1 1 calc R . . C16 C 0.9934(17) 0.1038(9) 0.6587(10) 0.062(3) Uani 1 1 d . . . H16A H 0.8870 0.0755 0.5888 0.074 Uiso 1 1 calc R . . H16B H 1.0399 0.0368 0.6689 0.074 Uiso 1 1 calc R . . C17 C 0.8880(17) 0.1803(8) 0.7600(10) 0.054(3) Uani 1 1 d . . . H17A H 0.9917 0.2036 0.8301 0.065 Uiso 1 1 calc R . . H17B H 0.7592 0.1357 0.7641 0.065 Uiso 1 1 calc R . . C18 C 1.1730(14) 0.4336(8) 0.8277(9) 0.039(2) Uani 1 1 d . . . C21 C 0.6313(16) 0.8464(8) 1.0276(10) 0.051(3) Uani 1 1 d . . . H21 H 0.5075 0.8504 1.0623 0.061 Uiso 1 1 calc R . . C22 C 0.7482(16) 0.9487(8) 1.0439(10) 0.053(3) Uani 1 1 d . . . H22 H 0.7035 1.0199 1.0891 0.064 Uiso 1 1 calc R . . C23 C 0.9341(15) 0.9461(7) 0.9930(9) 0.042(3) Uani 1 1 d . . . C24 C 0.9954(17) 0.8345(8) 0.9287(10) 0.057(3) Uani 1 1 d . . . H24 H 1.1214 0.8270 0.8952 0.069 Uiso 1 1 calc R . . C25 C 0.8634(17) 0.7366(8) 0.9166(10) 0.057(3) Uani 1 1 d . . . H25 H 0.9027 0.6635 0.8723 0.069 Uiso 1 1 calc R . . O1S O 0.605(4) 0.178(2) 0.252(2) 0.129(8) Uani 0.50 1 d PDU . . C1S C 0.500(6) 0.139(3) 0.332(3) 0.121(11) Uani 0.50 1 d PDU . . O2S O 0.094(2) 0.6131(14) 0.6551(14) 0.071(4) Uani 0.50 1 d PDU . . H2S H 0.0327 0.5676 0.5907 0.106 Uiso 0.50 1 calc PR . . C2S C 0.328(3) 0.594(3) 0.670(3) 0.110(10) Uani 0.50 1 d PDU . . H2S1 H 0.3639 0.5426 0.5976 0.165 Uiso 0.50 1 calc PR . . H2S2 H 0.3528 0.5599 0.7226 0.165 Uiso 0.50 1 calc PR . . H2S3 H 0.4198 0.6677 0.6994 0.165 Uiso 0.50 1 calc PR . . 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 0.0318(6) 0.0204(5) 0.0534(8) 0.0171(5) 0.0204(5) 0.0008(4) O11 0.038(4) 0.028(3) 0.060(4) 0.022(3) 0.022(3) 0.009(3) O12 0.033(4) 0.034(3) 0.066(5) 0.025(3) 0.026(3) 0.002(3) O13 0.038(4) 0.041(4) 0.058(5) 0.021(4) 0.009(3) 0.002(3) O14 0.042(4) 0.039(4) 0.059(5) 0.018(3) 0.016(3) -0.005(3) N21 0.035(4) 0.024(4) 0.061(6) 0.020(4) 0.020(4) 0.001(3) C11 0.020(5) 0.032(5) 0.050(6) 0.010(5) 0.010(4) 0.003(4) C12 0.025(5) 0.028(5) 0.041(6) 0.006(4) 0.009(4) -0.003(4) C13 0.035(2) 0.037(2) 0.036(2) 0.0143(13) 0.0073(11) 0.0040(10) C14 0.060(7) 0.059(7) 0.064(8) 0.013(6) 0.033(6) -0.003(6) C15 0.040(6) 0.054(7) 0.090(9) 0.013(6) 0.029(6) 0.012(5) C16 0.053(7) 0.033(5) 0.086(9) 0.005(5) 0.036(6) 0.007(5) C17 0.052(6) 0.025(5) 0.076(8) 0.008(5) 0.031(6) 0.007(4) C18 0.028(5) 0.033(5) 0.059(7) 0.015(5) 0.028(5) 0.009(4) C21 0.044(6) 0.030(5) 0.094(9) 0.032(5) 0.042(6) 0.005(4) C22 0.046(6) 0.023(5) 0.091(9) 0.019(5) 0.036(6) 0.004(4) C23 0.043(6) 0.028(5) 0.063(7) 0.023(5) 0.023(5) 0.000(4) C24 0.059(7) 0.025(5) 0.092(9) 0.020(5) 0.048(7) 0.003(4) C25 0.065(7) 0.020(5) 0.090(9) 0.017(5) 0.048(7) 0.002(5) O1S 0.129(8) 0.128(8) 0.129(8) 0.055(4) 0.023(2) 0.016(2) C1S 0.121(12) 0.121(12) 0.122(12) 0.053(5) 0.021(3) 0.015(2) O2S 0.073(5) 0.070(5) 0.071(5) 0.032(3) 0.014(2) 0.008(2) C2S 0.111(11) 0.110(11) 0.110(11) 0.048(5) 0.019(3) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O12 2.002(6) 2_667 ? Zn1 O11 2.006(6) . ? Zn1 N21 2.046(7) . ? Zn1 O14 2.057(7) 1_455 ? Zn1 O13 2.115(7) 2_767 ? Zn1 Zn1 2.929(2) 2_667 ? O11 C11 1.263(10) . ? O12 C11 1.284(11) . ? O12 Zn1 2.002(6) 2_667 ? O13 C18 1.263(12) . ? O13 Zn1 2.115(7) 2_767 ? O14 C18 1.275(10) . ? O14 Zn1 2.057(7) 1_655 ? N21 C25 1.312(11) . ? N21 C21 1.344(11) . ? C11 C12 1.491(12) . ? C12 C13 1.576(12) . ? C12 C17 1.591(13) . ? C12 H12 0.9800 . ? C13 C18 1.472(13) . ? C13 C14 1.532(13) . ? C13 H13 0.9800 . ? C14 C15 1.509(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.555(14) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.526(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C21 C22 1.369(12) . ? C21 H21 0.9300 . ? C22 C23 1.392(13) . ? C22 H22 0.9300 . ? C23 C24 1.414(12) . ? C23 C23 1.481(16) 2_777 ? C24 C25 1.387(12) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O1S C1S 1.528(18) . ? O2S C2S 1.480(2) . ? O2S H2S 0.8200 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? 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 O11 160.3(2) 2_667 . ? O12 Zn1 N21 99.4(3) 2_667 . ? O11 Zn1 N21 99.3(3) . . ? O12 Zn1 O14 93.4(3) 2_667 1_455 ? O11 Zn1 O14 86.5(3) . 1_455 ? N21 Zn1 O14 108.3(3) . 1_455 ? O12 Zn1 O13 86.5(3) 2_667 2_767 ? O11 Zn1 O13 86.9(3) . 2_767 ? N21 Zn1 O13 91.6(3) . 2_767 ? O14 Zn1 O13 159.8(2) 1_455 2_767 ? O12 Zn1 Zn1 80.42(18) 2_667 2_667 ? O11 Zn1 Zn1 79.91(18) . 2_667 ? N21 Zn1 Zn1 157.0(2) . 2_667 ? O14 Zn1 Zn1 94.58(19) 1_455 2_667 ? O13 Zn1 Zn1 65.45(18) 2_767 2_667 ? C11 O11 Zn1 128.4(6) . . ? C11 O12 Zn1 127.2(6) . 2_667 ? C18 O13 Zn1 145.1(6) . 2_767 ? C18 O14 Zn1 110.3(7) . 1_655 ? C25 N21 C21 117.5(7) . . ? C25 N21 Zn1 121.2(6) . . ? C21 N21 Zn1 120.4(6) . . ? O11 C11 O12 123.6(8) . . ? O11 C11 C12 117.2(8) . . ? O12 C11 C12 119.2(8) . . ? C11 C12 C13 111.7(7) . . ? C11 C12 C17 113.0(8) . . ? C13 C12 C17 113.9(7) . . ? C11 C12 H12 105.8 . . ? C13 C12 H12 105.8 . . ? C17 C12 H12 105.8 . . ? C18 C13 C14 107.3(8) . . ? C18 C13 C12 112.8(8) . . ? C14 C13 C12 110.5(7) . . ? C18 C13 H13 108.7 . . ? C14 C13 H13 108.7 . . ? C12 C13 H13 108.7 . . ? C15 C14 C13 115.9(10) . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 111.3(9) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 109.2(8) . . ? C17 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? C17 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? C16 C17 C12 111.3(9) . . ? C16 C17 H17A 109.4 . . ? C12 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C12 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O13 C18 O14 122.1(9) . . ? O13 C18 C13 121.3(8) . . ? O14 C18 C13 116.6(9) . . ? N21 C21 C22 123.2(9) . . ? N21 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 120.0(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 116.5(8) . . ? C22 C23 C23 122.4(10) . 2_777 ? C24 C23 C23 121.0(10) . 2_777 ? C25 C24 C23 118.5(9) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N21 C25 C24 124.2(9) . . ? N21 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Zn1 O11 C11 -3.2(13) 2_667 . . . ? N21 Zn1 O11 C11 158.5(7) . . . . ? O14 Zn1 O11 C11 -93.5(8) 1_455 . . . ? O13 Zn1 O11 C11 67.4(7) 2_767 . . . ? Zn1 Zn1 O11 C11 1.8(7) 2_667 . . . ? O12 Zn1 N21 C25 163.2(8) 2_667 . . . ? O11 Zn1 N21 C25 -10.6(9) . . . . ? O14 Zn1 N21 C25 -100.0(9) 1_455 . . . ? O13 Zn1 N21 C25 76.5(9) 2_767 . . . ? Zn1 Zn1 N21 C25 75.5(11) 2_667 . . . ? O12 Zn1 N21 C21 -5.9(8) 2_667 . . . ? O11 Zn1 N21 C21 -179.7(8) . . . . ? O14 Zn1 N21 C21 90.9(8) 1_455 . . . ? O13 Zn1 N21 C21 -92.6(8) 2_767 . . . ? Zn1 Zn1 N21 C21 -93.6(9) 2_667 . . . ? Zn1 O11 C11 O12 -6.8(13) . . . . ? Zn1 O11 C11 C12 173.1(5) . . . . ? Zn1 O12 C11 O11 9.5(13) 2_667 . . . ? Zn1 O12 C11 C12 -170.5(6) 2_667 . . . ? O11 C11 C12 C13 36.4(11) . . . . ? O12 C11 C12 C13 -143.6(8) . . . . ? O11 C11 C12 C17 166.4(8) . . . . ? O12 C11 C12 C17 -13.7(11) . . . . ? C11 C12 C13 C18 53.7(11) . . . . ? C17 C12 C13 C18 -75.8(10) . . . . ? C11 C12 C13 C14 173.8(8) . . . . ? C17 C12 C13 C14 44.3(11) . . . . ? C18 C13 C14 C15 75.9(11) . . . . ? C12 C13 C14 C15 -47.5(12) . . . . ? C13 C14 C15 C16 56.1(14) . . . . ? C14 C15 C16 C17 -59.6(14) . . . . ? C15 C16 C17 C12 57.3(13) . . . . ? C11 C12 C17 C16 179.7(8) . . . . ? C13 C12 C17 C16 -51.5(11) . . . . ? Zn1 O13 C18 O14 -24.8(16) 2_767 . . . ? Zn1 O13 C18 C13 154.9(7) 2_767 . . . ? Zn1 O14 C18 O13 12.0(10) 1_655 . . . ? Zn1 O14 C18 C13 -167.8(6) 1_655 . . . ? C14 C13 C18 O13 -89.3(10) . . . . ? C12 C13 C18 O13 32.7(12) . . . . ? C14 C13 C18 O14 90.5(10) . . . . ? C12 C13 C18 O14 -147.6(8) . . . . ? C25 N21 C21 C22 0.8(17) . . . . ? Zn1 N21 C21 C22 170.3(9) . . . . ? N21 C21 C22 C23 0.2(18) . . . . ? C21 C22 C23 C24 -2.0(17) . . . . ? C21 C22 C23 C23 179.5(12) . . . 2_777 ? C22 C23 C24 C25 2.7(17) . . . . ? C23 C23 C24 C25 -178.8(13) 2_777 . . . ? C21 N21 C25 C24 0.1(18) . . . . ? Zn1 N21 C25 C24 -169.3(9) . . . . ? C23 C24 C25 N21 -1.8(19) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.650 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.203 data_4 _database_code_depnum_ccdc_archive 'CCDC 756683' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 N2 O10 Zn2' _chemical_formula_weight 689.31 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 6.2142(12) _cell_length_b 9.4307(18) _cell_length_c 12.213(3) _cell_angle_alpha 81.975(3) _cell_angle_beta 82.195(3) _cell_angle_gamma 85.397(4) _cell_volume 700.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 752 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 21.11 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 1.773 _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 3955 _diffrn_reflns_av_R_equivalents 0.2034 _diffrn_reflns_av_sigmaI/netI 0.2067 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.98 _reflns_number_total 2686 _reflns_number_gt 1451 _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. The positions of H atoms of water solvent molecules were refined isotropically with O-H restraints (0.93 \%A) and U~iso~(H) = 1.2U~eq~(O). ; _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^)+(0.0505P)^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 2686 _refine_ls_number_parameters 191 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.52937(13) 0.86709(8) 0.57550(6) 0.0283(3) Uani 1 1 d . . . O11 O 0.3380(8) 0.7593(5) 0.4962(3) 0.0355(12) Uani 1 1 d . . . O12 O 0.2858(8) 0.9692(5) 0.3932(3) 0.0383(13) Uani 1 1 d . . . O13 O -0.2727(8) 1.0348(5) 0.3389(3) 0.0390(13) Uani 1 1 d . . . O14 O -0.2292(8) 0.8288(5) 0.4509(3) 0.0361(12) Uani 1 1 d . . . N21 N 0.6339(9) 0.7311(5) 0.7052(4) 0.0294(13) Uani 1 1 d . . . C1 C 0.2682(12) 0.8362(8) 0.4123(5) 0.0325(17) Uani 1 1 d . . . C2 C 0.1720(11) 0.7631(7) 0.3318(5) 0.0318(17) Uani 1 1 d . . . H2 H 0.1094 0.6762 0.3730 0.038 Uiso 1 1 calc R . . C3 C -0.0111(11) 0.8537(7) 0.2766(5) 0.0294(16) Uani 1 1 d . . . H3 H -0.0850 0.7870 0.2418 0.035 Uiso 1 1 calc R . . C4 C 0.0687(12) 0.9699(7) 0.1821(5) 0.0376(18) Uani 1 1 d . . . H4A H -0.0527 1.0101 0.1431 0.045 Uiso 1 1 calc R . . H4B H 0.1236 1.0466 0.2136 0.045 Uiso 1 1 calc R . . C5 C 0.2484(13) 0.9102(9) 0.0990(5) 0.053(2) Uani 1 1 d . . . H5A H 0.1905 0.8398 0.0619 0.063 Uiso 1 1 calc R . . H5B H 0.2999 0.9873 0.0427 0.063 Uiso 1 1 calc R . . C6 C 0.4380(13) 0.8402(8) 0.1592(5) 0.045(2) Uani 1 1 d . . . H6A H 0.5533 0.8055 0.1058 0.055 Uiso 1 1 calc R . . H6B H 0.4961 0.9100 0.1967 0.055 Uiso 1 1 calc R . . C7 C 0.3567(12) 0.7157(8) 0.2439(5) 0.0436(19) Uani 1 1 d . . . H7A H 0.4772 0.6705 0.2816 0.052 Uiso 1 1 calc R . . H7B H 0.3045 0.6449 0.2051 0.052 Uiso 1 1 calc R . . C8 C -0.1789(11) 0.9116(7) 0.3619(5) 0.0285(16) Uani 1 1 d . . . C21 C 0.8382(13) 0.6731(7) 0.6974(5) 0.0402(19) Uani 1 1 d . . . H21 H 0.9192 0.6769 0.6273 0.048 Uiso 1 1 calc R . . C22 C 0.9342(12) 0.6078(8) 0.7885(5) 0.045(2) Uani 1 1 d . . . H22 H 1.0768 0.5689 0.7792 0.054 Uiso 1 1 calc R . . C23 C 0.8164(13) 0.6004(8) 0.8949(5) 0.0397(19) Uani 1 1 d . . . C24 C 0.6066(13) 0.6607(8) 0.9015(5) 0.042(2) Uani 1 1 d . . . H24 H 0.5216 0.6578 0.9705 0.051 Uiso 1 1 calc R . . C25 C 0.5210(12) 0.7250(7) 0.8076(5) 0.0352(17) Uani 1 1 d . . . H25 H 0.3795 0.7659 0.8151 0.042 Uiso 1 1 calc R . . C26 C 0.9052(13) 0.5349(8) 0.9973(6) 0.053(2) Uani 1 1 d . . . H26 H 0.8182 0.5439 1.0645 0.063 Uiso 1 1 calc R . . O1W O 0.2543(13) 0.4770(8) 0.5956(6) 0.0831(19) Uiso 1 1 d D . . H1WA H 0.389(7) 0.511(9) 0.600(6) 0.100 Uiso 1 1 d D . . H1WB H 0.172(12) 0.468(10) 0.539(5) 0.100 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 0.0313(5) 0.0315(5) 0.0192(4) 0.0057(3) -0.0064(3) 0.0056(3) O11 0.042(3) 0.032(3) 0.034(2) -0.001(2) -0.015(2) -0.002(2) O12 0.048(4) 0.033(3) 0.033(2) -0.002(2) -0.008(2) 0.002(2) O13 0.038(3) 0.042(3) 0.032(2) 0.000(2) -0.004(2) 0.017(2) O14 0.043(3) 0.036(3) 0.026(2) 0.001(2) 0.003(2) -0.003(2) N21 0.038(4) 0.020(3) 0.026(3) 0.007(2) -0.003(3) 0.002(3) C1 0.033(4) 0.039(5) 0.023(3) -0.001(3) -0.004(3) 0.014(3) C2 0.030(4) 0.035(4) 0.029(3) 0.002(3) -0.006(3) 0.001(3) C3 0.027(4) 0.039(4) 0.023(3) -0.004(3) -0.007(3) -0.001(3) C4 0.037(5) 0.047(5) 0.026(3) 0.004(3) -0.005(3) 0.004(4) C5 0.047(6) 0.077(6) 0.028(4) 0.002(4) 0.005(4) -0.004(5) C6 0.037(5) 0.064(6) 0.035(4) -0.018(4) 0.004(3) 0.004(4) C7 0.042(5) 0.054(5) 0.037(4) -0.013(4) -0.014(4) 0.011(4) C8 0.021(4) 0.041(4) 0.026(3) -0.008(3) -0.010(3) -0.001(3) C21 0.049(5) 0.043(5) 0.025(3) 0.002(3) -0.005(3) 0.014(4) C22 0.030(5) 0.057(5) 0.045(4) 0.005(4) -0.015(4) 0.018(4) C23 0.041(5) 0.044(5) 0.032(4) 0.010(3) -0.015(3) 0.004(4) C24 0.050(6) 0.051(5) 0.024(3) 0.005(3) -0.010(3) 0.004(4) C25 0.032(4) 0.038(4) 0.032(4) 0.006(3) -0.008(3) 0.007(3) C26 0.063(7) 0.058(6) 0.033(4) 0.006(4) -0.018(4) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O13 2.019(5) 2_576 ? Zn1 O14 2.036(4) 1_655 ? Zn1 N21 2.038(5) . ? Zn1 O11 2.041(4) . ? Zn1 O12 2.102(5) 2_676 ? Zn1 Zn1 2.9265(15) 2_676 ? O11 C1 1.275(7) . ? O12 C1 1.255(7) . ? O12 Zn1 2.102(5) 2_676 ? O13 C8 1.270(7) . ? O13 Zn1 2.019(5) 2_576 ? O14 C8 1.264(7) . ? O14 Zn1 2.036(4) 1_455 ? N21 C21 1.338(9) . ? N21 C25 1.344(8) . ? C1 C2 1.488(9) . ? C2 C3 1.540(8) . ? C2 C7 1.544(9) . ? C2 H2 0.9800 . ? C3 C8 1.498(9) . ? C3 C4 1.536(8) . ? C3 H3 0.9800 . ? C4 C5 1.532(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.529(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.522(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C21 C22 1.380(8) . ? C21 H21 0.9300 . ? C22 C23 1.398(10) . ? C22 H22 0.9300 . ? C23 C24 1.376(10) . ? C23 C26 1.472(9) . ? C24 C25 1.373(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C26 1.308(15) 2_767 ? C26 H26 0.9300 . ? O1W H1WA 0.93(5) . ? O1W H1WB 0.93(7) . ? 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 O13 Zn1 O14 160.28(16) 2_576 1_655 ? O13 Zn1 N21 98.21(19) 2_576 . ? O14 Zn1 N21 100.6(2) 1_655 . ? O13 Zn1 O11 93.4(2) 2_576 . ? O14 Zn1 O11 86.11(18) 1_655 . ? N21 Zn1 O11 108.58(19) . . ? O13 Zn1 O12 86.8(2) 2_576 2_676 ? O14 Zn1 O12 86.91(18) 1_655 2_676 ? N21 Zn1 O12 91.51(19) . 2_676 ? O11 Zn1 O12 159.63(15) . 2_676 ? O13 Zn1 Zn1 79.27(12) 2_576 2_676 ? O14 Zn1 Zn1 81.05(12) 1_655 2_676 ? N21 Zn1 Zn1 158.82(16) . 2_676 ? O11 Zn1 Zn1 92.58(12) . 2_676 ? O12 Zn1 Zn1 67.41(12) 2_676 2_676 ? C1 O11 Zn1 112.7(4) . . ? C1 O12 Zn1 142.4(4) . 2_676 ? C8 O13 Zn1 129.5(4) . 2_576 ? C8 O14 Zn1 126.4(4) . 1_455 ? C21 N21 C25 117.2(5) . . ? C21 N21 Zn1 120.3(4) . . ? C25 N21 Zn1 120.5(5) . . ? O12 C1 O11 122.5(6) . . ? O12 C1 C2 119.2(5) . . ? O11 C1 C2 118.2(6) . . ? C1 C2 C3 114.0(6) . . ? C1 C2 C7 108.6(6) . . ? C3 C2 C7 111.5(5) . . ? C1 C2 H2 107.5 . . ? C3 C2 H2 107.5 . . ? C7 C2 H2 107.5 . . ? C8 C3 C4 112.7(5) . . ? C8 C3 C2 111.3(5) . . ? C4 C3 C2 114.4(5) . . ? C8 C3 H3 105.9 . . ? C4 C3 H3 105.9 . . ? C2 C3 H3 105.9 . . ? C5 C4 C3 111.9(6) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 110.3(5) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 109.0(6) . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 C7 C2 112.7(6) . . ? C6 C7 H7A 109.0 . . ? C2 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O14 C8 O13 123.7(6) . . ? O14 C8 C3 116.8(6) . . ? O13 C8 C3 119.3(5) . . ? N21 C21 C22 123.0(6) . . ? N21 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C21 C22 C23 119.8(7) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 116.4(6) . . ? C24 C23 C26 119.7(6) . . ? C22 C23 C26 123.9(7) . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? N21 C25 C24 122.6(7) . . ? N21 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C26 C26 C23 126.1(9) 2_767 . ? C26 C26 H26 116.9 2_767 . ? C23 C26 H26 116.9 . . ? H1WA O1W H1WB 136(8) . . ? 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 O13 Zn1 O11 C1 81.3(4) 2_576 . . . ? O14 Zn1 O11 C1 -79.0(4) 1_655 . . . ? N21 Zn1 O11 C1 -178.9(4) . . . . ? O12 Zn1 O11 C1 -8.7(8) 2_676 . . . ? Zn1 Zn1 O11 C1 1.9(4) 2_676 . . . ? O13 Zn1 N21 C21 -159.6(5) 2_576 . . . ? O14 Zn1 N21 C21 14.5(6) 1_655 . . . ? O11 Zn1 N21 C21 103.9(5) . . . . ? O12 Zn1 N21 C21 -72.7(5) 2_676 . . . ? Zn1 Zn1 N21 C21 -78.2(7) 2_676 . . . ? O13 Zn1 N21 C25 4.1(5) 2_576 . . . ? O14 Zn1 N21 C25 178.2(5) 1_655 . . . ? O11 Zn1 N21 C25 -92.3(5) . . . . ? O12 Zn1 N21 C25 91.1(5) 2_676 . . . ? Zn1 Zn1 N21 C25 85.6(7) 2_676 . . . ? Zn1 O12 C1 O11 23.9(11) 2_676 . . . ? Zn1 O12 C1 C2 -153.2(5) 2_676 . . . ? Zn1 O11 C1 O12 -11.3(8) . . . . ? Zn1 O11 C1 C2 165.8(5) . . . . ? O12 C1 C2 C3 -35.0(9) . . . . ? O11 C1 C2 C3 147.8(6) . . . . ? O12 C1 C2 C7 89.9(7) . . . . ? O11 C1 C2 C7 -87.3(7) . . . . ? C1 C2 C3 C8 -51.0(8) . . . . ? C7 C2 C3 C8 -174.4(6) . . . . ? C1 C2 C3 C4 78.1(7) . . . . ? C7 C2 C3 C4 -45.3(7) . . . . ? C8 C3 C4 C5 177.1(6) . . . . ? C2 C3 C4 C5 48.7(8) . . . . ? C3 C4 C5 C6 -56.4(8) . . . . ? C4 C5 C6 C7 61.5(8) . . . . ? C5 C6 C7 C2 -59.4(8) . . . . ? C1 C2 C7 C6 -75.3(7) . . . . ? C3 C2 C7 C6 51.1(8) . . . . ? Zn1 O14 C8 O13 1.5(9) 1_455 . . . ? Zn1 O14 C8 C3 -173.5(4) 1_455 . . . ? Zn1 O13 C8 O14 -3.8(10) 2_576 . . . ? Zn1 O13 C8 C3 171.1(4) 2_576 . . . ? C4 C3 C8 O14 -169.5(5) . . . . ? C2 C3 C8 O14 -39.5(8) . . . . ? C4 C3 C8 O13 15.3(9) . . . . ? C2 C3 C8 O13 145.2(6) . . . . ? C25 N21 C21 C22 0.5(10) . . . . ? Zn1 N21 C21 C22 164.8(5) . . . . ? N21 C21 C22 C23 0.0(11) . . . . ? C21 C22 C23 C24 0.0(11) . . . . ? C21 C22 C23 C26 -179.2(7) . . . . ? C22 C23 C24 C25 -0.4(11) . . . . ? C26 C23 C24 C25 178.7(7) . . . . ? C21 N21 C25 C24 -1.0(10) . . . . ? Zn1 N21 C25 C24 -165.2(5) . . . . ? C23 C24 C25 N21 1.0(11) . . . . ? C24 C23 C26 C26 174.8(11) . . . 2_767 ? C22 C23 C26 C26 -6.1(16) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.424 _refine_diff_density_min -1.806 _refine_diff_density_rms 0.171 data_5 _database_code_depnum_ccdc_archive 'CCDC 756684' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H79 N5 O20 Zn4' _chemical_formula_weight 1451.76 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 5.6008(5) _cell_length_b 13.9738(13) _cell_length_c 20.9424(19) _cell_angle_alpha 93.765(2) _cell_angle_beta 96.678(2) _cell_angle_gamma 94.342(2) _cell_volume 1618.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 2812 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 1.540 _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 170(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 9011 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6178 _reflns_number_gt 4253 _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. The positions of H atoms of a water ligand were refined isotropically with O-H restraints (0.86 \%A) and U~iso~(H) = 1.2U~eq~(O). The positions of O atoms of isolated water solvent molecules were refined isotropically with half occupancies. The positions of C and N atoms of acetonitrile solvent molecules were isotropically with half occupancies and C-N restraints (1.1 \%A) and C-C restraints (1.54 \%A). ; _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^)+(0.0759P)^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 6178 _refine_ls_number_parameters 416 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.003 _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 -0.25945(8) 0.13750(3) 0.04429(2) 0.01877(16) Uani 1 1 d . . . Zn2 Zn 0.65295(9) 0.88386(4) 0.47881(2) 0.02001(16) Uani 1 1 d . . . O1 O -0.6156(5) 0.1166(2) 0.01123(15) 0.0240(7) Uani 1 1 d D . . H1A H -0.655(8) 0.082(3) -0.0244(11) 0.029 Uiso 1 1 d D . . H1B H -0.714(6) 0.110(3) 0.0395(16) 0.029 Uiso 1 1 d D . . O11 O -0.2439(5) 0.0157(2) 0.09095(14) 0.0212(7) Uani 1 1 d . . . O12 O 0.1152(5) 0.0963(2) 0.11182(14) 0.0246(7) Uani 1 1 d . . . O13 O 0.1403(5) -0.1012(2) 0.03665(14) 0.0228(7) Uani 1 1 d . . . O14 O 0.0962(7) -0.2589(2) 0.04364(18) 0.0451(10) Uani 1 1 d . . . O21 O 0.9668(5) 0.8562(2) 0.51819(15) 0.0265(7) Uani 1 1 d . . . O22 O 0.8003(7) 0.7191(3) 0.5427(2) 0.0596(12) Uani 1 1 d . . . O23 O 1.2564(6) 1.0290(2) 0.58669(15) 0.0283(8) Uani 1 1 d . . . O24 O 1.5221(6) 0.9314(2) 0.55650(15) 0.0295(8) Uani 1 1 d . . . N31 N -0.2734(6) 0.2562(3) 0.10283(17) 0.0206(8) Uani 1 1 d . . . N32 N 0.3819(6) 0.7976(3) 0.42799(17) 0.0215(8) Uani 1 1 d . . . C11 C -0.0218(8) 0.0238(3) 0.1179(2) 0.0193(10) Uani 1 1 d . . . C12 C 0.0538(7) -0.0555(3) 0.1611(2) 0.0205(10) Uani 1 1 d . . . H12 H -0.0350 -0.0482 0.1996 0.025 Uiso 1 1 calc R . . C13 C -0.0241(8) -0.1567(3) 0.1297(2) 0.0207(10) Uiso 1 1 d . . . H13 H -0.2037 -0.1613 0.1196 0.025 Uiso 1 1 calc R . . C14 C 0.0363(8) -0.2326(3) 0.1763(2) 0.0286(11) Uiso 1 1 d . . . H14A H -0.0049 -0.2973 0.1538 0.034 Uiso 1 1 calc R . . H14B H -0.0622 -0.2266 0.2124 0.034 Uiso 1 1 calc R . . C15 C 0.3022(9) -0.2222(4) 0.2028(3) 0.0398(13) Uani 1 1 d . . . H15A H 0.4000 -0.2369 0.1676 0.048 Uiso 1 1 calc R . . H15B H 0.3324 -0.2691 0.2357 0.048 Uiso 1 1 calc R . . C16 C 0.3799(9) -0.1205(4) 0.2332(2) 0.0353(12) Uani 1 1 d . . . H16A H 0.2975 -0.1090 0.2720 0.042 Uiso 1 1 calc R . . H16B H 0.5559 -0.1148 0.2470 0.042 Uiso 1 1 calc R . . C17 C 0.3205(8) -0.0445(3) 0.1866(2) 0.0262(11) Uani 1 1 d . . . H17A H 0.4174 -0.0509 0.1501 0.031 Uiso 1 1 calc R . . H17B H 0.3626 0.0203 0.2088 0.031 Uiso 1 1 calc R . . C18 C 0.0787(8) -0.1759(3) 0.0657(2) 0.0245(10) Uani 1 1 d . . . C21 C 0.9681(8) 0.7819(4) 0.5499(2) 0.0272(11) Uani 1 1 d . . . C22 C 1.1898(8) 0.7762(3) 0.5991(2) 0.0227(10) Uani 1 1 d . . . H22 H 1.3231 0.7550 0.5751 0.027 Uiso 1 1 calc R . . C23 C 1.2728(8) 0.8770(3) 0.6330(2) 0.0199(10) Uani 1 1 d . . . H23 H 1.4197 0.8685 0.6634 0.024 Uiso 1 1 calc R . . C24 C 1.0821(9) 0.9103(3) 0.6754(2) 0.0268(11) Uani 1 1 d . . . H24A H 1.1369 0.9745 0.6972 0.032 Uiso 1 1 calc R . . H24B H 0.9279 0.9155 0.6480 0.032 Uiso 1 1 calc R . . C25 C 1.0435(10) 0.8377(4) 0.7262(2) 0.0383(13) Uani 1 1 d . . . H25A H 1.1941 0.8373 0.7560 0.046 Uiso 1 1 calc R . . H25B H 0.9155 0.8579 0.7517 0.046 Uiso 1 1 calc R . . C26 C 0.9718(10) 0.7364(4) 0.6949(3) 0.0388(13) Uani 1 1 d . . . H26A H 0.8095 0.7347 0.6702 0.047 Uiso 1 1 calc R . . H26B H 0.9630 0.6908 0.7289 0.047 Uiso 1 1 calc R . . C27 C 1.1507(9) 0.7043(3) 0.6498(2) 0.0316(12) Uani 1 1 d . . . H27A H 1.0901 0.6408 0.6278 0.038 Uiso 1 1 calc R . . H27B H 1.3072 0.6969 0.6755 0.038 Uiso 1 1 calc R . . C28 C 1.3506(8) 0.9498(3) 0.5878(2) 0.0209(10) Uani 1 1 d . . . C31 C -0.4473(8) 0.2569(3) 0.1419(2) 0.0263(11) Uani 1 1 d . . . H31 H -0.5520 0.2002 0.1421 0.032 Uiso 1 1 calc R . . C32 C -0.4802(8) 0.3355(4) 0.1813(2) 0.0315(12) Uani 1 1 d . . . H32 H -0.6052 0.3323 0.2083 0.038 Uiso 1 1 calc R . . C33 C -0.3312(8) 0.4202(3) 0.1821(2) 0.0292(11) Uani 1 1 d . . . C34 C -0.1505(9) 0.4187(4) 0.1423(2) 0.0356(13) Uani 1 1 d . . . H34 H -0.0419 0.4742 0.1419 0.043 Uiso 1 1 calc R . . C35 C -0.1263(9) 0.3379(3) 0.1036(2) 0.0303(11) Uani 1 1 d . . . H35 H -0.0021 0.3392 0.0763 0.036 Uiso 1 1 calc R . . C36 C -0.3685(9) 0.5074(4) 0.2244(3) 0.0392(14) Uani 1 1 d . . . H36A H -0.4967 0.4899 0.2514 0.047 Uiso 1 1 calc R . . H36B H -0.4272 0.5575 0.1966 0.047 Uiso 1 1 calc R . . C37 C -0.1456(8) 0.5505(3) 0.2686(2) 0.0255(11) Uani 1 1 d . . . H37A H -0.0704 0.4991 0.2920 0.031 Uiso 1 1 calc R . . H37B H -0.0266 0.5793 0.2424 0.031 Uiso 1 1 calc R . . C38 C -0.2118(8) 0.6272(4) 0.3166(2) 0.0339(12) Uani 1 1 d . . . H38A H -0.3147 0.6709 0.2928 0.041 Uiso 1 1 calc R . . H38B H -0.3102 0.5953 0.3467 0.041 Uiso 1 1 calc R . . C39 C -0.0069(8) 0.6864(3) 0.3552(2) 0.0254(11) Uani 1 1 d . . . C310 C 0.0037(8) 0.7858(3) 0.3616(2) 0.0237(10) Uani 1 1 d . . . H310 H -0.1233 0.8182 0.3408 0.028 Uiso 1 1 calc R . . C311 C 0.1978(8) 0.8387(3) 0.3980(2) 0.0239(10) Uani 1 1 d . . . H311 H 0.1996 0.9068 0.4018 0.029 Uiso 1 1 calc R . . C312 C 0.3728(9) 0.7013(3) 0.4238(2) 0.0300(11) Uani 1 1 d . . . H312 H 0.5003 0.6710 0.4462 0.036 Uiso 1 1 calc R . . C313 C 0.1847(9) 0.6441(3) 0.3880(2) 0.0338(12) Uani 1 1 d . . . H313 H 0.1861 0.5760 0.3857 0.041 Uiso 1 1 calc R . . O1W O 0.6814(12) 0.4324(5) 0.9239(3) 0.0349(16) Uani 0.50 1 d PU . . O2W O 0.2560(17) 0.4163(6) 0.9779(4) 0.068(3) Uani 0.50 1 d PU . . N1S N 0.833(2) 0.5231(10) 0.4881(6) 0.094(4) Uani 0.50 1 d PDU . . C1S C 0.710(3) 0.5320(12) 0.5250(7) 0.080(5) Uiso 0.50 1 d PD . . C2S C 0.561(3) 0.5435(14) 0.5820(7) 0.120(7) Uani 0.50 1 d PDU . . H2S1 H 0.4675 0.4825 0.5862 0.179 Uiso 0.50 1 calc PR . . H2S2 H 0.4503 0.5938 0.5742 0.179 Uiso 0.50 1 calc PR . . H2S3 H 0.6693 0.5615 0.6218 0.179 Uiso 0.50 1 calc PR . . 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 0.0161(3) 0.0184(3) 0.0214(3) -0.0021(2) 0.0031(2) 0.0004(2) Zn2 0.0180(3) 0.0195(3) 0.0217(3) -0.0007(2) 0.0010(2) 0.0006(2) O1 0.0154(16) 0.031(2) 0.0240(18) -0.0044(15) 0.0023(14) -0.0004(14) O11 0.0165(16) 0.0256(18) 0.0213(16) 0.0001(13) 0.0018(13) 0.0025(13) O12 0.0252(17) 0.0220(18) 0.0260(17) 0.0001(14) 0.0069(14) -0.0050(14) O13 0.0212(16) 0.0253(18) 0.0226(17) 0.0001(14) 0.0061(13) 0.0026(13) O14 0.066(3) 0.027(2) 0.044(2) -0.0091(17) 0.018(2) 0.0078(19) O21 0.0209(17) 0.033(2) 0.0261(18) 0.0059(15) 0.0031(14) 0.0029(14) O22 0.050(3) 0.045(3) 0.074(3) 0.015(2) -0.026(2) -0.020(2) O23 0.0320(19) 0.0221(18) 0.0323(19) 0.0041(14) 0.0079(15) 0.0051(15) O24 0.0235(17) 0.038(2) 0.0269(18) -0.0038(15) 0.0080(15) -0.0005(15) N31 0.0190(19) 0.019(2) 0.022(2) -0.0059(16) 0.0011(16) -0.0017(16) N32 0.022(2) 0.021(2) 0.021(2) -0.0029(16) 0.0046(16) 0.0009(16) C11 0.021(2) 0.021(2) 0.015(2) -0.0031(18) 0.0058(18) -0.0003(19) C12 0.017(2) 0.026(3) 0.019(2) -0.0016(19) 0.0042(18) 0.0011(19) C15 0.034(3) 0.045(3) 0.042(3) 0.019(3) 0.000(2) 0.010(3) C16 0.027(3) 0.049(4) 0.029(3) 0.012(3) -0.002(2) 0.003(2) C17 0.017(2) 0.035(3) 0.024(3) 0.001(2) -0.0016(19) 0.000(2) C18 0.016(2) 0.028(3) 0.028(3) -0.003(2) -0.0030(19) 0.004(2) C21 0.021(2) 0.028(3) 0.031(3) -0.006(2) 0.004(2) 0.001(2) C22 0.021(2) 0.021(2) 0.026(2) -0.002(2) 0.0014(19) 0.0038(19) C23 0.019(2) 0.021(2) 0.019(2) 0.0013(19) -0.0004(18) 0.0011(19) C24 0.031(3) 0.030(3) 0.021(2) 0.004(2) 0.008(2) 0.003(2) C25 0.045(3) 0.046(3) 0.026(3) 0.005(2) 0.012(2) 0.001(3) C26 0.040(3) 0.037(3) 0.042(3) 0.016(3) 0.011(3) 0.000(2) C27 0.033(3) 0.026(3) 0.036(3) 0.008(2) 0.002(2) 0.003(2) C28 0.018(2) 0.024(3) 0.019(2) -0.0020(19) 0.0004(19) -0.0034(19) C31 0.021(2) 0.024(3) 0.032(3) -0.007(2) 0.006(2) -0.008(2) C32 0.023(3) 0.040(3) 0.030(3) -0.010(2) 0.006(2) 0.000(2) C33 0.024(2) 0.027(3) 0.033(3) -0.009(2) -0.006(2) 0.005(2) C34 0.040(3) 0.023(3) 0.042(3) -0.006(2) 0.007(3) -0.009(2) C35 0.033(3) 0.026(3) 0.031(3) -0.006(2) 0.012(2) -0.007(2) C36 0.033(3) 0.030(3) 0.050(3) -0.017(3) -0.002(3) 0.005(2) C37 0.025(2) 0.024(3) 0.026(3) -0.004(2) 0.001(2) 0.003(2) C38 0.025(3) 0.032(3) 0.040(3) -0.018(2) -0.002(2) 0.003(2) C39 0.022(2) 0.030(3) 0.023(2) -0.007(2) 0.003(2) 0.000(2) C310 0.023(2) 0.025(3) 0.023(2) 0.000(2) 0.004(2) 0.004(2) C311 0.025(2) 0.023(3) 0.023(2) 0.001(2) 0.001(2) 0.002(2) C312 0.028(3) 0.025(3) 0.035(3) -0.002(2) -0.005(2) 0.008(2) C313 0.033(3) 0.018(3) 0.046(3) -0.009(2) -0.003(2) 0.002(2) O1W 0.036(2) 0.032(2) 0.036(2) 0.0043(17) 0.0005(17) 0.0045(17) O2W 0.070(3) 0.063(3) 0.069(3) 0.0008(19) 0.0098(19) 0.0000(19) N1S 0.095(5) 0.092(5) 0.094(5) 0.005(2) 0.011(2) 0.004(2) C2S 0.119(7) 0.117(7) 0.122(7) 0.010(2) 0.012(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O13 1.944(3) 2 ? Zn1 N31 2.009(3) . ? Zn1 O11 2.020(3) . ? Zn1 O1 2.027(3) . ? Zn2 O21 1.930(3) . ? Zn2 O24 1.959(3) 1_455 ? Zn2 O23 1.977(3) 2_776 ? Zn2 N32 2.017(4) . ? O1 H1A 0.86(3) . ? O1 H1B 0.86(3) . ? O11 C11 1.298(5) . ? O12 C11 1.246(5) . ? O13 C18 1.287(5) . ? O13 Zn1 1.944(3) 2 ? O14 C18 1.235(5) . ? O21 C21 1.270(5) . ? O22 C21 1.224(6) . ? O23 C28 1.263(5) . ? O23 Zn2 1.977(3) 2_776 ? O24 C28 1.257(5) . ? O24 Zn2 1.958(3) 1_655 ? N31 C31 1.343(5) . ? N31 C35 1.353(6) . ? N32 C311 1.331(6) . ? N32 C312 1.339(6) . ? C11 C12 1.529(6) . ? C12 C17 1.519(6) . ? C12 C13 1.530(6) . ? C12 H12 1.0000 . ? C13 C14 1.518(6) . ? C13 C18 1.534(6) . ? C13 H13 1.0000 . ? C14 C15 1.521(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.529(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.518(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 C22 1.529(6) . ? C22 C27 1.530(6) . ? C22 C23 1.548(6) . ? C22 H22 1.0000 . ? C23 C28 1.509(6) . ? C23 C24 1.544(6) . ? C23 H23 1.0000 . ? C24 C25 1.539(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.525(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.526(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C31 C32 1.368(6) . ? C31 H31 0.9500 . ? C32 C33 1.395(7) . ? C32 H32 0.9500 . ? C33 C34 1.383(7) . ? C33 C36 1.502(6) . ? C34 C35 1.371(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.523(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.518(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.486(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C310 1.383(6) . ? C39 C313 1.396(7) . ? C310 C311 1.386(6) . ? C310 H310 0.9500 . ? C311 H311 0.9500 . ? C312 C313 1.386(7) . ? C312 H312 0.9500 . ? C313 H313 0.9500 . ? N1S C1S 1.103(2) . ? C1S C2S 1.541(2) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Zn1 N31 138.90(14) 2 . ? O13 Zn1 O11 102.69(12) 2 . ? N31 Zn1 O11 113.64(13) . . ? O13 Zn1 O1 96.80(12) 2 . ? N31 Zn1 O1 97.80(13) . . ? O11 Zn1 O1 96.06(12) . . ? O21 Zn2 O24 98.67(13) . 1_455 ? O21 Zn2 O23 100.95(13) . 2_776 ? O24 Zn2 O23 121.72(13) 1_455 2_776 ? O21 Zn2 N32 131.16(14) . . ? O24 Zn2 N32 105.25(14) 1_455 . ? O23 Zn2 N32 101.50(14) 2_776 . ? Zn1 O1 H1A 117(3) . . ? Zn1 O1 H1B 117(3) . . ? H1A O1 H1B 115(5) . . ? C11 O11 Zn1 101.8(3) . . ? C18 O13 Zn1 111.2(3) . 2 ? C21 O21 Zn2 115.0(3) . . ? C28 O23 Zn2 117.1(3) . 2_776 ? C28 O24 Zn2 152.6(3) . 1_655 ? C31 N31 C35 117.3(4) . . ? C31 N31 Zn1 118.1(3) . . ? C35 N31 Zn1 124.5(3) . . ? C311 N32 C312 117.9(4) . . ? C311 N32 Zn2 118.1(3) . . ? C312 N32 Zn2 124.0(3) . . ? O12 C11 O11 120.8(4) . . ? O12 C11 C12 122.5(4) . . ? O11 C11 C12 116.6(4) . . ? C17 C12 C13 111.6(4) . . ? C17 C12 C11 113.1(4) . . ? C13 C12 C11 112.9(3) . . ? C17 C12 H12 106.2 . . ? C13 C12 H12 106.2 . . ? C11 C12 H12 106.2 . . ? C14 C13 C12 111.0(4) . . ? C14 C13 C18 111.7(4) . . ? C12 C13 C18 112.6(4) . . ? C14 C13 H13 107.0 . . ? C12 C13 H13 107.0 . . ? C18 C13 H13 107.0 . . ? C13 C14 C15 111.5(4) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.3(4) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 111.9(4) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C12 110.5(4) . . ? C16 C17 H17A 109.5 . . ? C12 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O14 C18 O13 122.8(4) . . ? O14 C18 C13 121.0(4) . . ? O13 C18 C13 116.2(4) . . ? O22 C21 O21 122.3(5) . . ? O22 C21 C22 121.7(5) . . ? O21 C21 C22 116.0(4) . . ? C21 C22 C27 113.7(4) . . ? C21 C22 C23 110.2(4) . . ? C27 C22 C23 109.6(4) . . ? C21 C22 H22 107.7 . . ? C27 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C28 C23 C24 114.3(4) . . ? C28 C23 C22 113.6(4) . . ? C24 C23 C22 110.1(4) . . ? C28 C23 H23 106.0 . . ? C24 C23 H23 106.0 . . ? C22 C23 H23 106.0 . . ? C25 C24 C23 109.9(4) . . ? C25 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? C25 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 C24 111.5(4) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 112.0(4) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C22 112.1(4) . . ? C26 C27 H27A 109.2 . . ? C22 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C22 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? O24 C28 O23 122.7(4) . . ? O24 C28 C23 117.7(4) . . ? O23 C28 C23 119.4(4) . . ? N31 C31 C32 122.9(4) . . ? N31 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 116.5(4) . . ? C34 C33 C36 122.9(5) . . ? C32 C33 C36 120.7(4) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? N31 C35 C34 122.3(4) . . ? N31 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C33 C36 C37 115.1(4) . . ? C33 C36 H36A 108.5 . . ? C37 C36 H36A 108.5 . . ? C33 C36 H36B 108.5 . . ? C37 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C36 110.7(4) . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C37 116.1(4) . . ? C39 C38 H38A 108.3 . . ? C37 C38 H38A 108.3 . . ? C39 C38 H38B 108.3 . . ? C37 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? C310 C39 C313 116.3(4) . . ? C310 C39 C38 122.2(4) . . ? C313 C39 C38 121.5(4) . . ? C39 C310 C311 120.6(4) . . ? C39 C310 H310 119.7 . . ? C311 C310 H310 119.7 . . ? N32 C311 C310 122.5(4) . . ? N32 C311 H311 118.7 . . ? C310 C311 H311 118.7 . . ? N32 C312 C313 122.5(4) . . ? N32 C312 H312 118.7 . . ? C313 C312 H312 118.7 . . ? C312 C313 C39 120.1(5) . . ? C312 C313 H313 119.9 . . ? C39 C313 H313 119.9 . . ? N1S C1S C2S 174.0(18) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Zn1 O11 C11 85.2(2) 2 . . . ? N31 Zn1 O11 C11 -75.2(3) . . . . ? O1 Zn1 O11 C11 -176.5(2) . . . . ? O24 Zn2 O21 C21 73.7(3) 1_455 . . . ? O23 Zn2 O21 C21 -161.4(3) 2_776 . . . ? N32 Zn2 O21 C21 -45.4(4) . . . . ? O13 Zn1 N31 C31 155.7(3) 2 . . . ? O11 Zn1 N31 C31 -54.3(4) . . . . ? O1 Zn1 N31 C31 45.9(3) . . . . ? O13 Zn1 N31 C35 -21.0(5) 2 . . . ? O11 Zn1 N31 C35 129.0(4) . . . . ? O1 Zn1 N31 C35 -130.8(4) . . . . ? O21 Zn2 N32 C311 -170.1(3) . . . . ? O24 Zn2 N32 C311 73.5(3) 1_455 . . . ? O23 Zn2 N32 C311 -54.2(3) 2_776 . . . ? O21 Zn2 N32 C312 11.6(4) . . . . ? O24 Zn2 N32 C312 -104.8(4) 1_455 . . . ? O23 Zn2 N32 C312 127.5(4) 2_776 . . . ? Zn1 O11 C11 O12 1.8(4) . . . . ? Zn1 O11 C11 C12 177.1(3) . . . . ? O12 C11 C12 C17 -9.1(6) . . . . ? O11 C11 C12 C17 175.7(3) . . . . ? O12 C11 C12 C13 -137.1(4) . . . . ? O11 C11 C12 C13 47.7(5) . . . . ? C17 C12 C13 C14 55.9(5) . . . . ? C11 C12 C13 C14 -175.3(3) . . . . ? C17 C12 C13 C18 -70.2(5) . . . . ? C11 C12 C13 C18 58.6(5) . . . . ? C12 C13 C14 C15 -54.9(5) . . . . ? C18 C13 C14 C15 71.7(5) . . . . ? C13 C14 C15 C16 54.3(5) . . . . ? C14 C15 C16 C17 -54.7(6) . . . . ? C15 C16 C17 C12 55.2(5) . . . . ? C13 C12 C17 C16 -55.8(5) . . . . ? C11 C12 C17 C16 175.5(4) . . . . ? Zn1 O13 C18 O14 0.1(5) 2 . . . ? Zn1 O13 C18 C13 -178.6(3) 2 . . . ? C14 C13 C18 O14 32.7(6) . . . . ? C12 C13 C18 O14 158.4(4) . . . . ? C14 C13 C18 O13 -148.5(4) . . . . ? C12 C13 C18 O13 -22.8(5) . . . . ? Zn2 O21 C21 O22 18.3(6) . . . . ? Zn2 O21 C21 C22 -160.3(3) . . . . ? O22 C21 C22 C27 -16.6(7) . . . . ? O21 C21 C22 C27 161.9(4) . . . . ? O22 C21 C22 C23 -140.2(5) . . . . ? O21 C21 C22 C23 38.4(5) . . . . ? C21 C22 C23 C28 -62.5(5) . . . . ? C27 C22 C23 C28 171.7(4) . . . . ? C21 C22 C23 C24 67.2(4) . . . . ? C27 C22 C23 C24 -58.6(5) . . . . ? C28 C23 C24 C25 -171.8(4) . . . . ? C22 C23 C24 C25 58.9(5) . . . . ? C23 C24 C25 C26 -56.3(6) . . . . ? C24 C25 C26 C27 53.8(6) . . . . ? C25 C26 C27 C22 -54.1(6) . . . . ? C21 C22 C27 C26 -67.7(5) . . . . ? C23 C22 C27 C26 56.1(5) . . . . ? Zn2 O24 C28 O23 -88.1(8) 1_655 . . . ? Zn2 O24 C28 C23 97.8(7) 1_655 . . . ? Zn2 O23 C28 O24 11.0(6) 2_776 . . . ? Zn2 O23 C28 C23 -175.0(3) 2_776 . . . ? C24 C23 C28 O24 173.2(4) . . . . ? C22 C23 C28 O24 -59.3(5) . . . . ? C24 C23 C28 O23 -1.1(6) . . . . ? C22 C23 C28 O23 126.4(4) . . . . ? C35 N31 C31 C32 0.2(7) . . . . ? Zn1 N31 C31 C32 -176.8(4) . . . . ? N31 C31 C32 C33 0.4(7) . . . . ? C31 C32 C33 C34 -1.2(7) . . . . ? C31 C32 C33 C36 179.0(5) . . . . ? C32 C33 C34 C35 1.5(7) . . . . ? C36 C33 C34 C35 -178.8(5) . . . . ? C31 N31 C35 C34 0.1(7) . . . . ? Zn1 N31 C35 C34 176.8(4) . . . . ? C33 C34 C35 N31 -0.9(8) . . . . ? C34 C33 C36 C37 -52.8(7) . . . . ? C32 C33 C36 C37 127.0(5) . . . . ? C33 C36 C37 C38 -170.7(5) . . . . ? C36 C37 C38 C39 -170.1(4) . . . . ? C37 C38 C39 C310 130.7(5) . . . . ? C37 C38 C39 C313 -50.3(7) . . . . ? C313 C39 C310 C311 0.9(7) . . . . ? C38 C39 C310 C311 180.0(4) . . . . ? C312 N32 C311 C310 -2.0(6) . . . . ? Zn2 N32 C311 C310 179.6(3) . . . . ? C39 C310 C311 N32 0.4(7) . . . . ? C311 N32 C312 C313 2.2(7) . . . . ? Zn2 N32 C312 C313 -179.5(4) . . . . ? N32 C312 C313 C39 -0.9(8) . . . . ? C310 C39 C313 C312 -0.7(7) . . . . ? C38 C39 C313 C312 -179.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.177 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.112 data_6 _database_code_depnum_ccdc_archive 'CCDC 756685' #TrackingRef 'Zn-1-2-chdc--all-revised.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H45 N4 O12.50 S4 Zn2' _chemical_formula_weight 992.75 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3877(11) _cell_length_b 10.6229(12) _cell_length_c 23.554(3) _cell_angle_alpha 96.562(2) _cell_angle_beta 98.759(2) _cell_angle_gamma 113.605(2) _cell_volume 2309.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 1622 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 26.97 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1025 _exptl_absorpt_coefficient_mu 1.279 _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 170(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 12885 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.2368 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8842 _reflns_number_gt 3351 _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. The positions of O atoms of isolated water solvent molecules were refined isotropically with half occupancies except O1W. ; _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^)+(0.0812P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8842 _refine_ls_number_parameters 559 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1458 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1912 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.884 _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 -0.24285(11) 0.09477(10) 0.17777(4) 0.0377(3) Uani 1 1 d . . . Zn2 Zn -0.12133(12) 0.68298(10) 0.32154(4) 0.0460(3) Uani 1 1 d . . . O11 O -0.2104(7) 0.2375(6) 0.1262(2) 0.0549(18) Uani 1 1 d . . . O12 O -0.3237(7) 0.2907(5) 0.1916(2) 0.0459(17) Uani 1 1 d . . . O13 O -0.1256(7) 0.6052(5) 0.2381(2) 0.0480(16) Uani 1 1 d . . . O14 O -0.3223(8) 0.6219(7) 0.2475(2) 0.064(2) Uani 1 1 d . . . O21 O -0.2249(8) 0.0762(7) 0.2633(2) 0.0504(17) Uani 1 1 d . . . O22 O -0.0240(8) 0.2225(6) 0.2460(2) 0.0608(19) Uani 1 1 d . . . O23 O -0.1463(7) -0.1681(6) 0.3725(2) 0.0529(17) Uani 1 1 d . . . O24 O -0.0217(7) -0.0658(6) 0.3094(2) 0.0555(19) Uani 1 1 d . . . N31 N -0.1590(7) -0.0209(6) 0.1324(2) 0.0285(16) Uani 1 1 d . . . N32 N 0.5445(7) -0.0495(7) 0.1456(3) 0.0349(17) Uani 1 1 d . . . N41 N 0.0797(8) 0.7124(7) 0.3697(3) 0.045(2) Uani 1 1 d . . . N42 N 0.2422(8) 0.4892(7) 0.6442(3) 0.0445(19) Uani 1 1 d . . . C11 C -0.2633(10) 0.3162(8) 0.1503(4) 0.041(2) Uani 1 1 d . . . C12 C -0.2430(9) 0.4464(8) 0.1227(3) 0.034(2) Uani 1 1 d . . . H12 H -0.1373 0.5063 0.1293 0.041 Uiso 1 1 calc R . . C13 C -0.3103(9) 0.5330(8) 0.1506(3) 0.030(2) Uani 1 1 d . . . H13 H -0.2822 0.6181 0.1325 0.036 Uiso 1 1 calc R . . C14 C -0.4731(9) 0.4637(8) 0.1350(3) 0.039(2) Uani 1 1 d . . . H14A H -0.5084 0.3788 0.1524 0.046 Uiso 1 1 calc R . . H14B H -0.5104 0.5287 0.1517 0.046 Uiso 1 1 calc R . . C15 C -0.5281(10) 0.4243(9) 0.0703(3) 0.048(2) Uani 1 1 d . . . H15A H -0.4999 0.5101 0.0535 0.057 Uiso 1 1 calc R . . H15B H -0.6345 0.3761 0.0615 0.057 Uiso 1 1 calc R . . C16 C -0.4689(11) 0.3280(9) 0.0419(3) 0.055(3) Uani 1 1 d . . . H16A H -0.5050 0.3053 -0.0011 0.066 Uiso 1 1 calc R . . H16B H -0.5007 0.2395 0.0569 0.066 Uiso 1 1 calc R . . C17 C -0.3039(10) 0.4043(9) 0.0569(3) 0.047(2) Uani 1 1 d . . . H17A H -0.2640 0.3424 0.0395 0.057 Uiso 1 1 calc R . . H17B H -0.2734 0.4892 0.0393 0.057 Uiso 1 1 calc R . . C18 C -0.2527(11) 0.5883(8) 0.2162(4) 0.041(2) Uani 1 1 d . . . C21 C -0.0931(13) 0.1623(9) 0.2813(4) 0.048(3) Uani 1 1 d . . . C22 C -0.0259(10) 0.1963(8) 0.3454(3) 0.040(2) Uani 1 1 d . . . H22 H -0.0489 0.2729 0.3630 0.048 Uiso 1 1 calc R . . C23 C -0.0944(9) 0.0732(8) 0.3757(3) 0.036(2) Uani 1 1 d . . . H23 H -0.1988 0.0518 0.3708 0.043 Uiso 1 1 calc R . . C24 C -0.0268(10) 0.1161(9) 0.4421(3) 0.043(2) Uani 1 1 d . . . H24A H -0.0514 0.1905 0.4597 0.052 Uiso 1 1 calc R . . H24B H -0.0677 0.0344 0.4609 0.052 Uiso 1 1 calc R . . C25 C 0.1304(10) 0.1673(8) 0.4533(3) 0.050(3) Uani 1 1 d . . . H25A H 0.1552 0.0913 0.4378 0.061 Uiso 1 1 calc R . . H25B H 0.1706 0.1949 0.4960 0.061 Uiso 1 1 calc R . . C26 C 0.1978(11) 0.2944(9) 0.4239(4) 0.056(3) Uani 1 1 d . . . H26A H 0.1770 0.3721 0.4408 0.067 Uiso 1 1 calc R . . H26B H 0.3036 0.3271 0.4317 0.067 Uiso 1 1 calc R . . C27 C 0.1371(10) 0.2546(9) 0.3582(3) 0.049(2) Uani 1 1 d . . . H27A H 0.1766 0.3382 0.3403 0.058 Uiso 1 1 calc R . . H27B H 0.1661 0.1836 0.3407 0.058 Uiso 1 1 calc R . . C28 C -0.0845(11) -0.0616(9) 0.3500(4) 0.049(3) Uani 1 1 d . . . C31 C -0.0827(8) -0.0848(8) 0.1554(3) 0.032(2) Uani 1 1 d . . . H31 H -0.0637 -0.0774 0.1967 0.039 Uiso 1 1 calc R . . C32 C -0.0294(9) -0.1616(8) 0.1226(3) 0.034(2) Uani 1 1 d . . . H32 H 0.0271 -0.2033 0.1409 0.041 Uiso 1 1 calc R . . C33 C -0.0607(8) -0.1759(7) 0.0626(3) 0.0283(19) Uani 1 1 d . . . C34 C -0.1389(9) -0.1097(8) 0.0381(3) 0.038(2) Uani 1 1 d . . . H34 H -0.1606 -0.1162 -0.0031 0.045 Uiso 1 1 calc R . . C35 C -0.1844(9) -0.0348(8) 0.0743(3) 0.033(2) Uani 1 1 d . . . H35 H -0.2379 0.0108 0.0570 0.040 Uiso 1 1 calc R . . C36 C 0.2626(9) -0.2386(8) 0.0931(3) 0.036(2) Uani 1 1 d . . . C37 C 0.3089(9) -0.1043(9) 0.0897(4) 0.046(2) Uani 1 1 d . . . H37 H 0.2472 -0.0713 0.0686 0.055 Uiso 1 1 calc R . . C38 C 0.4456(11) -0.0154(10) 0.1168(4) 0.058(3) Uani 1 1 d . . . H38 H 0.4742 0.0808 0.1152 0.069 Uiso 1 1 calc R . . C39 C 0.4950(11) -0.1818(10) 0.1493(4) 0.056(3) Uani 1 1 d . . . H39 H 0.5593 -0.2116 0.1707 0.067 Uiso 1 1 calc R . . C310 C 0.3582(11) -0.2810(10) 0.1249(4) 0.061(3) Uani 1 1 d . . . H310 H 0.3290 -0.3755 0.1294 0.073 Uiso 1 1 calc R . . C41 C 0.1261(10) 0.7921(8) 0.4237(3) 0.045(2) Uani 1 1 d . . . H41 H 0.0692 0.8356 0.4370 0.054 Uiso 1 1 calc R . . C42 C 0.2506(10) 0.8133(9) 0.4601(3) 0.045(2) Uani 1 1 d . . . H42 H 0.2777 0.8674 0.4986 0.054 Uiso 1 1 calc R . . C43 C 0.3376(10) 0.7553(9) 0.4406(4) 0.044(2) Uani 1 1 d . . . C44 C 0.2955(12) 0.6767(10) 0.3863(4) 0.061(3) Uani 1 1 d . . . H44 H 0.3533 0.6357 0.3720 0.074 Uiso 1 1 calc R . . C45 C 0.1676(12) 0.6573(10) 0.3523(4) 0.063(3) Uani 1 1 d . . . H45 H 0.1386 0.6017 0.3142 0.075 Uiso 1 1 calc R . . C46 C 0.4057(10) 0.7104(8) 0.5948(3) 0.041(2) Uani 1 1 d . . . C47 C 0.3579(12) 0.5746(10) 0.5668(4) 0.068(3) Uani 1 1 d . . . H47 H 0.3798 0.5540 0.5301 0.082 Uiso 1 1 calc R . . C48 C 0.2771(13) 0.4675(10) 0.5927(4) 0.074(4) Uani 1 1 d . . . H48 H 0.2448 0.3736 0.5729 0.089 Uiso 1 1 calc R . . C49 C 0.2910(10) 0.6199(9) 0.6705(3) 0.047(3) Uani 1 1 d . . . H49 H 0.2686 0.6388 0.7073 0.056 Uiso 1 1 calc R . . C410 C 0.3738(11) 0.7322(9) 0.6475(4) 0.051(3) Uani 1 1 d . . . H410 H 0.4082 0.8250 0.6689 0.061 Uiso 1 1 calc R . . S41 S 0.5078(3) 0.7810(3) 0.48366(10) 0.0581(7) Uani 1 1 d . . . S42 S 0.5081(3) 0.8579(3) 0.56708(10) 0.0557(7) Uani 1 1 d . . . S31 S -0.0055(3) -0.2707(2) 0.01270(9) 0.0473(7) Uani 1 1 d . . . S32 S 0.0863(3) -0.3691(2) 0.06291(10) 0.0491(7) Uani 1 1 d . . . O1W O 0.8025(8) 0.8380(7) 0.8885(3) 0.080(2) Uani 1 1 d U . . O2W O 0.5140(11) 0.9081(10) 0.3038(4) 0.035(3) Uani 0.50 1 d PU . . O3W O 0.4354(16) 0.6101(15) 0.2800(6) 0.084(4) Uani 0.50 1 d PU . . O4W O 0.2648(16) 0.9448(14) 0.2734(6) 0.085(5) Uani 0.50 1 d PU . . O5W O 0.1291(17) 0.6910(15) 0.2110(6) 0.088(5) Uani 0.50 1 d PU . . O6W O 0.1614(17) 0.4755(15) 0.2230(6) 0.088(5) Uani 0.50 1 d PU . . O7W O 0.6721(17) 0.8064(15) 0.7779(6) 0.092(5) Uani 0.50 1 d PU . . O8W O 0.1026(18) 0.3773(16) 0.1239(7) 0.099(5) Uani 0.50 1 d PU . . 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 0.0434(7) 0.0513(7) 0.0267(5) 0.0081(5) 0.0032(5) 0.0298(6) Zn2 0.0687(9) 0.0346(6) 0.0261(5) 0.0035(4) 0.0018(5) 0.0169(6) O11 0.077(5) 0.045(4) 0.056(4) 0.004(3) 0.001(4) 0.046(4) O12 0.081(5) 0.033(4) 0.029(3) 0.011(3) 0.005(3) 0.030(4) O13 0.067(5) 0.034(4) 0.028(3) 0.007(3) -0.001(3) 0.011(4) O14 0.109(6) 0.073(5) 0.031(3) 0.004(3) 0.023(4) 0.059(5) O21 0.077(5) 0.054(4) 0.027(3) 0.005(3) -0.005(3) 0.041(4) O22 0.093(6) 0.055(4) 0.030(3) 0.011(3) 0.006(4) 0.029(4) O23 0.070(5) 0.029(4) 0.052(4) 0.015(3) 0.001(3) 0.015(3) O24 0.104(6) 0.044(4) 0.027(3) 0.004(3) 0.003(4) 0.044(4) N31 0.038(4) 0.034(4) 0.019(3) 0.004(3) 0.003(3) 0.022(4) N32 0.034(5) 0.043(5) 0.033(4) 0.009(3) 0.005(3) 0.023(4) N41 0.070(6) 0.037(5) 0.026(4) 0.007(3) 0.000(4) 0.025(4) N42 0.061(6) 0.035(5) 0.028(4) -0.004(3) -0.002(4) 0.017(4) C11 0.057(7) 0.032(5) 0.032(5) -0.004(4) -0.007(5) 0.027(5) C12 0.043(6) 0.040(5) 0.020(4) 0.010(4) 0.006(4) 0.019(5) C13 0.045(6) 0.019(4) 0.029(4) 0.007(3) 0.004(4) 0.016(4) C14 0.055(7) 0.040(5) 0.034(5) 0.022(4) 0.011(5) 0.029(5) C15 0.050(6) 0.056(6) 0.039(5) 0.021(5) 0.001(5) 0.024(5) C16 0.087(9) 0.047(6) 0.028(5) 0.013(4) -0.001(5) 0.029(6) C17 0.069(8) 0.057(6) 0.031(5) 0.010(4) 0.008(5) 0.043(6) C18 0.056(7) 0.020(5) 0.040(5) 0.011(4) -0.003(5) 0.012(5) C21 0.079(8) 0.026(6) 0.041(6) 0.007(5) -0.002(6) 0.031(6) C22 0.061(7) 0.026(5) 0.031(5) -0.005(4) -0.007(4) 0.027(5) C23 0.048(6) 0.033(5) 0.029(4) 0.004(4) -0.003(4) 0.024(5) C24 0.068(7) 0.040(5) 0.026(4) 0.007(4) 0.007(5) 0.029(5) C25 0.077(8) 0.036(6) 0.029(5) -0.003(4) -0.013(5) 0.026(6) C26 0.069(8) 0.045(6) 0.046(6) 0.000(5) -0.011(5) 0.026(6) C27 0.063(7) 0.040(6) 0.039(5) 0.007(4) 0.002(5) 0.021(5) C28 0.068(8) 0.040(6) 0.032(5) -0.003(5) -0.023(5) 0.029(6) C31 0.038(6) 0.034(5) 0.026(4) 0.010(4) 0.010(4) 0.015(5) C32 0.039(6) 0.028(5) 0.038(5) 0.012(4) 0.004(4) 0.015(4) C33 0.032(5) 0.024(5) 0.028(4) 0.004(4) 0.003(4) 0.013(4) C34 0.041(6) 0.034(5) 0.035(5) 0.003(4) 0.005(4) 0.014(5) C35 0.041(6) 0.035(5) 0.031(5) 0.009(4) 0.002(4) 0.025(5) C36 0.036(6) 0.030(5) 0.037(5) -0.005(4) 0.000(4) 0.015(5) C37 0.023(5) 0.041(6) 0.067(6) 0.027(5) -0.009(5) 0.009(5) C38 0.060(8) 0.052(7) 0.068(7) 0.031(5) 0.011(6) 0.026(6) C39 0.044(7) 0.050(7) 0.079(7) 0.010(6) -0.008(6) 0.032(6) C310 0.065(8) 0.046(6) 0.077(7) 0.009(5) -0.005(6) 0.037(6) C41 0.062(7) 0.036(5) 0.032(5) -0.003(4) -0.001(5) 0.021(5) C42 0.061(7) 0.051(6) 0.028(5) 0.008(4) 0.006(5) 0.029(6) C43 0.050(7) 0.045(6) 0.035(5) 0.015(4) 0.006(5) 0.017(5) C44 0.084(9) 0.075(8) 0.044(6) 0.011(5) 0.013(6) 0.053(7) C45 0.099(10) 0.070(7) 0.033(5) 0.001(5) 0.007(6) 0.054(8) C46 0.054(7) 0.032(5) 0.028(5) 0.005(4) -0.006(4) 0.014(5) C47 0.098(9) 0.052(7) 0.043(6) 0.005(5) 0.031(6) 0.016(7) C48 0.125(11) 0.038(6) 0.041(6) 0.005(5) 0.019(7) 0.016(7) C49 0.081(8) 0.035(6) 0.028(5) -0.001(4) 0.008(5) 0.030(6) C410 0.086(8) 0.036(6) 0.040(6) 0.013(4) 0.009(5) 0.036(6) S41 0.0556(18) 0.0744(19) 0.0532(15) 0.0298(14) 0.0134(14) 0.0315(16) S42 0.0616(19) 0.0461(16) 0.0487(15) 0.0194(12) 0.0016(13) 0.0133(14) S31 0.0473(16) 0.0536(16) 0.0412(13) -0.0104(11) -0.0039(12) 0.0316(14) S32 0.0481(17) 0.0374(14) 0.0600(15) -0.0085(12) -0.0004(13) 0.0254(13) O1W 0.080(3) 0.076(3) 0.083(3) 0.0187(18) 0.0183(19) 0.0306(19) O2W 0.036(3) 0.034(3) 0.034(3) 0.0063(19) 0.0084(19) 0.012(2) O3W 0.084(5) 0.085(5) 0.083(5) 0.013(2) 0.023(2) 0.034(3) O4W 0.085(5) 0.085(5) 0.085(5) 0.020(2) 0.019(2) 0.035(3) O5W 0.088(5) 0.089(5) 0.088(5) 0.020(2) 0.018(2) 0.038(3) O6W 0.089(5) 0.085(5) 0.087(5) 0.014(2) 0.024(2) 0.033(3) O7W 0.095(5) 0.089(5) 0.088(5) 0.021(2) 0.017(2) 0.035(3) O8W 0.100(5) 0.099(5) 0.100(5) 0.021(2) 0.021(2) 0.043(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 O11 2.006(6) . ? Zn1 O21 2.034(5) . ? Zn1 N31 2.063(6) . ? Zn1 N32 2.078(7) 1_455 ? Zn1 O22 2.347(6) . ? Zn1 C21 2.536(9) . ? Zn1 C11 2.589(8) . ? Zn2 O23 2.000(6) 1_565 ? Zn2 O13 2.029(5) . ? Zn2 N42 2.093(7) 2_566 ? Zn2 N41 2.102(7) . ? Zn2 O14 2.317(7) . ? Zn2 C18 2.516(8) . ? Zn2 C28 2.576(8) 1_565 ? O11 C11 1.295(9) . ? O12 C11 1.234(9) . ? O13 C18 1.274(10) . ? O14 C18 1.226(10) . ? O21 C21 1.274(11) . ? O22 C21 1.246(11) . ? O23 C28 1.279(10) . ? O23 Zn2 2.000(6) 1_545 ? O24 C28 1.243(10) . ? N31 C31 1.329(9) . ? N31 C35 1.332(8) . ? N32 C39 1.308(10) . ? N32 C38 1.338(10) . ? N32 Zn1 2.078(7) 1_655 ? N41 C41 1.344(9) . ? N41 C45 1.353(11) . ? N42 C49 1.309(9) . ? N42 C48 1.338(10) . ? N42 Zn2 2.093(7) 2_566 ? C11 C12 1.547(10) . ? C12 C13 1.511(10) . ? C12 C17 1.523(10) . ? C12 H12 1.0000 . ? C13 C14 1.512(11) . ? C13 C18 1.524(11) . ? C13 H13 1.0000 . ? C14 C15 1.491(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.532(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.535(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 C22 1.500(11) . ? C22 C27 1.518(12) . ? C22 C23 1.532(10) . ? C22 H22 1.0000 . ? C23 C28 1.538(11) . ? C23 C24 1.547(10) . ? C23 H23 1.0000 . ? C24 C25 1.469(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.548(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.521(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 Zn2 2.575(8) 1_545 ? C31 C32 1.385(10) . ? C31 H31 0.9500 . ? C32 C33 1.377(9) . ? C32 H32 0.9500 . ? C33 C34 1.376(10) . ? C33 S31 1.768(7) . ? C34 C35 1.361(10) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.327(10) . ? C36 C310 1.399(11) . ? C36 S32 1.768(8) . ? C37 C38 1.352(11) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C310 1.369(12) . ? C39 H39 0.9500 . ? C310 H310 0.9500 . ? C41 C42 1.358(11) . ? C41 H41 0.9500 . ? C42 C43 1.384(11) . ? C42 H42 0.9500 . ? C43 C44 1.348(11) . ? C43 S41 1.798(9) . ? C44 C45 1.366(12) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C410 1.350(10) . ? C46 C47 1.369(11) . ? C46 S42 1.768(9) . ? C47 C48 1.386(12) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C410 1.388(11) . ? C49 H49 0.9500 . ? C410 H410 0.9500 . ? S41 S42 2.039(4) . ? S31 S32 2.034(3) . ? 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 O11 Zn1 O21 142.0(2) . . ? O11 Zn1 N31 95.6(2) . . ? O21 Zn1 N31 111.9(2) . . ? O11 Zn1 N32 104.6(3) . 1_455 ? O21 Zn1 N32 99.0(3) . 1_455 ? N31 Zn1 N32 94.5(3) . 1_455 ? O11 Zn1 O22 95.4(2) . . ? O21 Zn1 O22 59.1(2) . . ? N31 Zn1 O22 92.5(2) . . ? N32 Zn1 O22 158.0(2) 1_455 . ? O11 Zn1 C21 120.1(3) . . ? O21 Zn1 C21 29.9(3) . . ? N31 Zn1 C21 103.9(3) . . ? N32 Zn1 C21 128.9(3) 1_455 . ? O22 Zn1 C21 29.2(3) . . ? O11 Zn1 C11 29.4(2) . . ? O21 Zn1 C11 118.0(2) . . ? N31 Zn1 C11 125.0(3) . . ? N32 Zn1 C11 99.1(3) 1_455 . ? O22 Zn1 C11 93.9(2) . . ? C21 Zn1 C11 107.7(3) . . ? O23 Zn2 O13 144.7(2) 1_565 . ? O23 Zn2 N42 98.6(3) 1_565 2_566 ? O13 Zn2 N42 106.0(2) . 2_566 ? O23 Zn2 N41 97.7(3) 1_565 . ? O13 Zn2 N41 104.6(3) . . ? N42 Zn2 N41 95.5(3) 2_566 . ? O23 Zn2 O14 97.5(2) 1_565 . ? O13 Zn2 O14 59.2(2) . . ? N42 Zn2 O14 88.1(3) 2_566 . ? N41 Zn2 O14 163.7(3) . . ? O23 Zn2 C18 122.7(3) 1_565 . ? O13 Zn2 C18 30.2(3) . . ? N42 Zn2 C18 97.5(3) 2_566 . ? N41 Zn2 C18 134.7(3) . . ? O14 Zn2 C18 29.0(2) . . ? O23 Zn2 C28 29.1(3) 1_565 1_565 ? O13 Zn2 C28 119.9(3) . 1_565 ? N42 Zn2 C28 127.6(3) 2_566 1_565 ? N41 Zn2 C28 96.0(3) . 1_565 ? O14 Zn2 C28 94.4(2) . 1_565 ? C18 Zn2 C28 109.4(3) . 1_565 ? C11 O11 Zn1 101.1(5) . . ? C18 O13 Zn2 96.5(6) . . ? C18 O14 Zn2 84.5(6) . . ? C21 O21 Zn1 97.4(6) . . ? C21 O22 Zn1 83.8(6) . . ? C28 O23 Zn2 101.2(6) . 1_545 ? C31 N31 C35 116.4(6) . . ? C31 N31 Zn1 126.2(5) . . ? C35 N31 Zn1 117.4(5) . . ? C39 N32 C38 113.5(8) . . ? C39 N32 Zn1 124.2(6) . 1_655 ? C38 N32 Zn1 122.3(6) . 1_655 ? C41 N41 C45 115.9(8) . . ? C41 N41 Zn2 117.4(6) . . ? C45 N41 Zn2 126.7(6) . . ? C49 N42 C48 116.3(8) . . ? C49 N42 Zn2 124.4(6) . 2_566 ? C48 N42 Zn2 119.3(6) . 2_566 ? O12 C11 O11 123.4(8) . . ? O12 C11 C12 122.9(7) . . ? O11 C11 C12 113.7(8) . . ? O12 C11 Zn1 74.1(4) . . ? O11 C11 Zn1 49.5(4) . . ? C12 C11 Zn1 162.7(6) . . ? C13 C12 C17 109.9(6) . . ? C13 C12 C11 112.2(6) . . ? C17 C12 C11 110.9(6) . . ? C13 C12 H12 107.9 . . ? C17 C12 H12 107.9 . . ? C11 C12 H12 107.9 . . ? C12 C13 C14 113.3(6) . . ? C12 C13 C18 115.2(7) . . ? C14 C13 C18 111.6(7) . . ? C12 C13 H13 105.2 . . ? C14 C13 H13 105.2 . . ? C18 C13 H13 105.2 . . ? C15 C14 C13 111.0(7) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.6(7) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 108.2(7) . . ? C15 C16 H16A 110.1 . . ? C17 C16 H16A 110.1 . . ? C15 C16 H16B 110.1 . . ? C17 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C12 C17 C16 112.1(7) . . ? C12 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C12 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? O14 C18 O13 119.7(8) . . ? O14 C18 C13 122.0(9) . . ? O13 C18 C13 118.2(9) . . ? O14 C18 Zn2 66.5(5) . . ? O13 C18 Zn2 53.3(4) . . ? C13 C18 Zn2 171.3(7) . . ? O22 C21 O21 119.7(8) . . ? O22 C21 C22 120.9(10) . . ? O21 C21 C22 119.3(9) . . ? O22 C21 Zn1 67.0(5) . . ? O21 C21 Zn1 52.7(4) . . ? C22 C21 Zn1 171.2(8) . . ? C21 C22 C27 113.3(8) . . ? C21 C22 C23 112.0(7) . . ? C27 C22 C23 112.6(6) . . ? C21 C22 H22 106.1 . . ? C27 C22 H22 106.1 . . ? C23 C22 H22 106.1 . . ? C22 C23 C28 114.1(7) . . ? C22 C23 C24 109.9(7) . . ? C28 C23 C24 110.1(6) . . ? C22 C23 H23 107.5 . . ? C28 C23 H23 107.5 . . ? C24 C23 H23 107.5 . . ? C25 C24 C23 111.3(7) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 110.7(7) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 110.5(7) . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C22 C27 C26 110.3(8) . . ? C22 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? C22 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O24 C28 O23 122.7(8) . . ? O24 C28 C23 121.6(8) . . ? O23 C28 C23 115.7(9) . . ? O24 C28 Zn2 73.2(5) . 1_545 ? O23 C28 Zn2 49.6(4) . 1_545 ? C23 C28 Zn2 164.7(8) . 1_545 ? N31 C31 C32 123.6(7) . . ? N31 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C33 C32 C31 118.1(7) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C34 C33 C32 118.9(7) . . ? C34 C33 S31 115.5(6) . . ? C32 C33 S31 125.5(6) . . ? C35 C34 C33 118.3(7) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? N31 C35 C34 124.6(7) . . ? N31 C35 H35 117.7 . . ? C34 C35 H35 117.7 . . ? C37 C36 C310 118.1(8) . . ? C37 C36 S32 125.3(7) . . ? C310 C36 S32 116.6(7) . . ? C36 C37 C38 118.7(8) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? N32 C38 C37 126.4(9) . . ? N32 C38 H38 116.8 . . ? C37 C38 H38 116.8 . . ? N32 C39 C310 125.4(8) . . ? N32 C39 H39 117.3 . . ? C310 C39 H39 117.3 . . ? C39 C310 C36 117.9(9) . . ? C39 C310 H310 121.1 . . ? C36 C310 H310 121.1 . . ? N41 C41 C42 123.0(8) . . ? N41 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C41 C42 C43 119.2(8) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 119.3(9) . . ? C44 C43 S41 117.3(8) . . ? C42 C43 S41 123.4(7) . . ? C43 C44 C45 118.5(9) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? N41 C45 C44 124.1(8) . . ? N41 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C410 C46 C47 117.5(8) . . ? C410 C46 S42 118.2(7) . . ? C47 C46 S42 124.3(7) . . ? C46 C47 C48 119.0(9) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? N42 C48 C47 123.5(9) . . ? N42 C48 H48 118.2 . . ? C47 C48 H48 118.2 . . ? N42 C49 C410 123.3(8) . . ? N42 C49 H49 118.3 . . ? C410 C49 H49 118.3 . . ? C46 C410 C49 120.4(8) . . ? C46 C410 H410 119.8 . . ? C49 C410 H410 119.8 . . ? C43 S41 S42 105.1(3) . . ? C46 S42 S41 105.4(3) . . ? C33 S31 S32 104.4(3) . . ? C36 S32 S31 103.5(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 O21 Zn1 O11 C11 -44.2(7) . . . . ? N31 Zn1 O11 C11 178.6(5) . . . . ? N32 Zn1 O11 C11 82.4(5) 1_455 . . . ? O22 Zn1 O11 C11 -88.4(5) . . . . ? C21 Zn1 O11 C11 -71.8(6) . . . . ? O23 Zn2 O13 C18 -55.4(7) 1_565 . . . ? N42 Zn2 O13 C18 77.1(5) 2_566 . . . ? N41 Zn2 O13 C18 177.4(5) . . . . ? O14 Zn2 O13 C18 -0.7(5) . . . . ? C28 Zn2 O13 C18 -76.7(6) 1_565 . . . ? O23 Zn2 O14 C18 152.3(5) 1_565 . . . ? O13 Zn2 O14 C18 0.7(5) . . . . ? N42 Zn2 O14 C18 -109.3(5) 2_566 . . . ? N41 Zn2 O14 C18 -6.1(11) . . . . ? C28 Zn2 O14 C18 123.2(5) 1_565 . . . ? O11 Zn1 O21 C21 -53.7(7) . . . . ? N31 Zn1 O21 C21 79.6(5) . . . . ? N32 Zn1 O21 C21 178.2(5) 1_455 . . . ? O22 Zn1 O21 C21 0.3(5) . . . . ? C11 Zn1 O21 C21 -76.5(6) . . . . ? O11 Zn1 O22 C21 149.6(5) . . . . ? O21 Zn1 O22 C21 -0.3(5) . . . . ? N31 Zn1 O22 C21 -114.5(5) . . . . ? N32 Zn1 O22 C21 -6.0(9) 1_455 . . . ? C11 Zn1 O22 C21 120.2(5) . . . . ? O11 Zn1 N31 C31 143.8(7) . . . . ? O21 Zn1 N31 C31 -9.5(7) . . . . ? N32 Zn1 N31 C31 -111.0(7) 1_455 . . . ? O22 Zn1 N31 C31 48.1(7) . . . . ? C21 Zn1 N31 C31 20.9(7) . . . . ? C11 Zn1 N31 C31 144.6(6) . . . . ? O11 Zn1 N31 C35 -37.0(6) . . . . ? O21 Zn1 N31 C35 169.8(6) . . . . ? N32 Zn1 N31 C35 68.2(6) 1_455 . . . ? O22 Zn1 N31 C35 -132.6(6) . . . . ? C21 Zn1 N31 C35 -159.9(6) . . . . ? C11 Zn1 N31 C35 -36.1(7) . . . . ? O23 Zn2 N41 C41 12.9(6) 1_565 . . . ? O13 Zn2 N41 C41 165.3(6) . . . . ? N42 Zn2 N41 C41 -86.6(6) 2_566 . . . ? O14 Zn2 N41 C41 171.3(7) . . . . ? C18 Zn2 N41 C41 167.1(5) . . . . ? C28 Zn2 N41 C41 42.2(7) 1_565 . . . ? O23 Zn2 N41 C45 -168.3(7) 1_565 . . . ? O13 Zn2 N41 C45 -15.9(8) . . . . ? N42 Zn2 N41 C45 92.3(7) 2_566 . . . ? O14 Zn2 N41 C45 -9.9(14) . . . . ? C18 Zn2 N41 C45 -14.0(9) . . . . ? C28 Zn2 N41 C45 -139.0(8) 1_565 . . . ? Zn1 O11 C11 O12 -4.2(9) . . . . ? Zn1 O11 C11 C12 175.3(5) . . . . ? O11 Zn1 C11 O12 176.3(8) . . . . ? O21 Zn1 C11 O12 -32.8(6) . . . . ? N31 Zn1 C11 O12 174.6(4) . . . . ? N32 Zn1 C11 O12 72.6(5) 1_455 . . . ? O22 Zn1 C11 O12 -89.6(5) . . . . ? C21 Zn1 C11 O12 -63.3(6) . . . . ? O21 Zn1 C11 O11 150.9(5) . . . . ? N31 Zn1 C11 O11 -1.7(6) . . . . ? N32 Zn1 C11 O11 -103.8(5) 1_455 . . . ? O22 Zn1 C11 O11 94.0(5) . . . . ? C21 Zn1 C11 O11 120.4(5) . . . . ? O11 Zn1 C11 C12 -14.5(16) . . . . ? O21 Zn1 C11 C12 136.4(18) . . . . ? N31 Zn1 C11 C12 -16.3(19) . . . . ? N32 Zn1 C11 C12 -118.3(18) 1_455 . . . ? O22 Zn1 C11 C12 79.5(18) . . . . ? C21 Zn1 C11 C12 105.8(18) . . . . ? O12 C11 C12 C13 -2.3(11) . . . . ? O11 C11 C12 C13 178.2(7) . . . . ? Zn1 C11 C12 C13 -169.8(15) . . . . ? O12 C11 C12 C17 -125.6(8) . . . . ? O11 C11 C12 C17 54.8(10) . . . . ? Zn1 C11 C12 C17 67(2) . . . . ? C17 C12 C13 C14 52.7(9) . . . . ? C11 C12 C13 C14 -71.2(8) . . . . ? C17 C12 C13 C18 -177.0(7) . . . . ? C11 C12 C13 C18 59.1(9) . . . . ? C12 C13 C14 C15 -54.2(8) . . . . ? C18 C13 C14 C15 173.7(6) . . . . ? C13 C14 C15 C16 56.9(9) . . . . ? C14 C15 C16 C17 -58.3(9) . . . . ? C13 C12 C17 C16 -55.1(9) . . . . ? C11 C12 C17 C16 69.5(9) . . . . ? C15 C16 C17 C12 57.6(8) . . . . ? Zn2 O14 C18 O13 -1.1(7) . . . . ? Zn2 O14 C18 C13 -178.0(7) . . . . ? Zn2 O13 C18 O14 1.3(8) . . . . ? Zn2 O13 C18 C13 178.3(6) . . . . ? C12 C13 C18 O14 -157.5(8) . . . . ? C14 C13 C18 O14 -26.4(10) . . . . ? C12 C13 C18 O13 25.5(11) . . . . ? C14 C13 C18 O13 156.7(7) . . . . ? O23 Zn2 C18 O14 -33.2(6) 1_565 . . . ? O13 Zn2 C18 O14 -178.8(8) . . . . ? N42 Zn2 C18 O14 72.1(5) 2_566 . . . ? N41 Zn2 C18 O14 177.6(4) . . . . ? C28 Zn2 C18 O14 -62.2(6) 1_565 . . . ? O23 Zn2 C18 O13 145.6(4) 1_565 . . . ? N42 Zn2 C18 O13 -109.1(5) 2_566 . . . ? N41 Zn2 C18 O13 -3.6(6) . . . . ? O14 Zn2 C18 O13 178.8(8) . . . . ? C28 Zn2 C18 O13 116.6(5) 1_565 . . . ? Zn1 O22 C21 O21 0.5(8) . . . . ? Zn1 O22 C21 C22 -175.6(7) . . . . ? Zn1 O21 C21 O22 -0.6(9) . . . . ? Zn1 O21 C21 C22 175.6(6) . . . . ? O11 Zn1 C21 O22 -35.6(6) . . . . ? O21 Zn1 C21 O22 179.4(8) . . . . ? N31 Zn1 C21 O22 69.5(5) . . . . ? N32 Zn1 C21 O22 177.1(4) 1_455 . . . ? C11 Zn1 C21 O22 -64.9(6) . . . . ? O11 Zn1 C21 O21 145.0(5) . . . . ? N31 Zn1 C21 O21 -110.0(5) . . . . ? N32 Zn1 C21 O21 -2.3(6) 1_455 . . . ? O22 Zn1 C21 O21 -179.4(8) . . . . ? C11 Zn1 C21 O21 115.7(5) . . . . ? O22 C21 C22 C27 -24.9(11) . . . . ? O21 C21 C22 C27 159.0(7) . . . . ? O22 C21 C22 C23 -153.6(8) . . . . ? O21 C21 C22 C23 30.3(11) . . . . ? C21 C22 C23 C28 58.7(10) . . . . ? C27 C22 C23 C28 -70.4(9) . . . . ? C21 C22 C23 C24 -177.1(7) . . . . ? C27 C22 C23 C24 53.8(9) . . . . ? C22 C23 C24 C25 -55.8(9) . . . . ? C28 C23 C24 C25 70.7(10) . . . . ? C23 C24 C25 C26 58.5(9) . . . . ? C24 C25 C26 C27 -58.9(10) . . . . ? C21 C22 C27 C26 176.7(6) . . . . ? C23 C22 C27 C26 -54.9(9) . . . . ? C25 C26 C27 C22 55.9(10) . . . . ? Zn2 O23 C28 O24 -4.1(9) 1_545 . . . ? Zn2 O23 C28 C23 175.0(6) 1_545 . . . ? C22 C23 C28 O24 2.2(11) . . . . ? C24 C23 C28 O24 -122.0(9) . . . . ? C22 C23 C28 O23 -176.9(7) . . . . ? C24 C23 C28 O23 58.9(10) . . . . ? C22 C23 C28 Zn2 -162.3(17) . . . 1_545 ? C24 C23 C28 Zn2 74(2) . . . 1_545 ? C35 N31 C31 C32 0.5(12) . . . . ? Zn1 N31 C31 C32 179.8(6) . . . . ? N31 C31 C32 C33 -1.9(12) . . . . ? C31 C32 C33 C34 2.2(12) . . . . ? C31 C32 C33 S31 -179.3(6) . . . . ? C32 C33 C34 C35 -1.2(12) . . . . ? S31 C33 C34 C35 -179.9(6) . . . . ? C31 N31 C35 C34 0.6(12) . . . . ? Zn1 N31 C35 C34 -178.7(6) . . . . ? C33 C34 C35 N31 -0.2(13) . . . . ? C310 C36 C37 C38 0.2(13) . . . . ? S32 C36 C37 C38 177.6(7) . . . . ? C39 N32 C38 C37 -4.3(13) . . . . ? Zn1 N32 C38 C37 173.4(7) 1_655 . . . ? C36 C37 C38 N32 3.0(15) . . . . ? C38 N32 C39 C310 2.5(13) . . . . ? Zn1 N32 C39 C310 -175.1(7) 1_655 . . . ? N32 C39 C310 C36 0.2(15) . . . . ? C37 C36 C310 C39 -1.7(13) . . . . ? S32 C36 C310 C39 -179.3(7) . . . . ? C45 N41 C41 C42 -2.3(13) . . . . ? Zn2 N41 C41 C42 176.7(7) . . . . ? N41 C41 C42 C43 2.5(13) . . . . ? C41 C42 C43 C44 -1.3(13) . . . . ? C41 C42 C43 S41 177.7(6) . . . . ? C42 C43 C44 C45 0.1(14) . . . . ? S41 C43 C44 C45 -179.0(7) . . . . ? C41 N41 C45 C44 1.0(14) . . . . ? Zn2 N41 C45 C44 -177.9(7) . . . . ? C43 C44 C45 N41 0.1(16) . . . . ? C410 C46 C47 C48 1.6(15) . . . . ? S42 C46 C47 C48 -179.4(8) . . . . ? C49 N42 C48 C47 -1.2(15) . . . . ? Zn2 N42 C48 C47 -179.3(9) 2_566 . . . ? C46 C47 C48 N42 0.2(17) . . . . ? C48 N42 C49 C410 0.4(13) . . . . ? Zn2 N42 C49 C410 178.5(6) 2_566 . . . ? C47 C46 C410 C49 -2.3(13) . . . . ? S42 C46 C410 C49 178.6(7) . . . . ? N42 C49 C410 C46 1.4(14) . . . . ? C44 C43 S41 S42 -165.7(7) . . . . ? C42 C43 S41 S42 15.3(8) . . . . ? C410 C46 S42 S41 -172.5(6) . . . . ? C47 C46 S42 S41 8.5(9) . . . . ? C43 S41 S42 C46 80.4(4) . . . . ? C34 C33 S31 S32 -174.2(6) . . . . ? C32 C33 S31 S32 7.2(8) . . . . ? C37 C36 S32 S31 9.7(8) . . . . ? C310 C36 S32 S31 -172.9(6) . . . . ? C33 S31 S32 C36 -82.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.871 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.127