Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shu-Mei Chen' _publ_contact_author_address ; National Center for Nanoscience and Nanotechnology Fujian Institute of Research on the Structure of Matter Fuzhou 350002 CHINA ; _publ_contact_author_email CSM@FJIRSM.AC.CN _publ_section_title ; One-pot synthesis of two isomeric zinc complexes with unusual polycatenation motifs ; loop_ _publ_author_name 'Shu-Mei Chen.' Can-Zhong. 'Jian Zhang.' data_a _database_code_depnum_ccdc_archive 'CCDC 629052' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H18 N2 O4 Zn), 3(H2 O)' _chemical_formula_sum 'C42 H42 N4 O11 Zn2' _chemical_formula_weight 909.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.019(6) _cell_length_b 11.483(3) _cell_length_c 19.949(6) _cell_angle_alpha 90.00 _cell_angle_beta 119.920(3) _cell_angle_gamma 90.00 _cell_volume 4173(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4851 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.48 _exptl_crystal_description diamond _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7272 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15875 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4793 _reflns_number_gt 4288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+6.1401P] 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 4793 _refine_ls_number_parameters 286 _refine_ls_number_restraints 1 _refine_ls_R_factor_ref 0.0505 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.021 _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 0.364003(15) 0.13292(2) 0.303795(16) 0.03892(12) Uani 1 1 d . . . O1 O 0.39443(13) 0.2003(2) 0.20149(13) 0.0743(7) Uani 1 1 d . . . O1W O 0.5000 0.3790(4) 0.2500 0.175(4) Uani 1 2 d S . . H1WA H 0.5349 0.3300 0.2702 0.210 Uiso 1 1 d R . . O2 O 0.28971(13) 0.1524(2) 0.19161(12) 0.0613(6) Uani 1 1 d . . . O2W O 0.22707(19) 0.4015(3) 0.3733(2) 0.1089(11) Uani 1 1 d . . . H2WA H 0.2566 0.3772 0.3590 0.131 Uiso 1 1 d RD . . H2WB H 0.2273 0.4659 0.3524 0.131 Uiso 1 1 d RD . . O3 O 0.34279(12) 0.34874(18) 0.34105(13) 0.0639(6) Uani 1 1 d . . . O4 O 0.43880(11) 0.23296(17) 0.38505(12) 0.0547(5) Uani 1 1 d . . . N1 N 0.29519(12) 0.07893(19) 0.34300(12) 0.0431(5) Uani 1 1 d . . . N2 N -0.06978(13) 0.49024(19) 0.32287(13) 0.0459(5) Uani 1 1 d . . . C1 C 0.31222(17) 0.0976(3) 0.41618(17) 0.0534(7) Uani 1 1 d . . . H1A H 0.3589 0.1252 0.4510 0.064 Uiso 1 1 calc R . . C2 C 0.26342(18) 0.0776(3) 0.44218(18) 0.0574(7) Uani 1 1 d . . . H2B H 0.2774 0.0920 0.4936 0.069 Uiso 1 1 calc R . . C3 C 0.19383(17) 0.0362(2) 0.39195(18) 0.0494(7) Uani 1 1 d . B . C4 C 0.17757(17) 0.0138(3) 0.3178(2) 0.0574(7) Uani 1 1 d . . . H4A H 0.1320 -0.0168 0.2825 0.069 Uiso 1 1 calc R . . C5 C 0.22857(16) 0.0365(3) 0.29482(17) 0.0525(7) Uani 1 1 d . . . H5A H 0.2159 0.0215 0.2438 0.063 Uiso 1 1 calc R . . C6 C 0.1387(2) 0.0205(3) 0.4181(2) 0.0676(10) Uani 1 1 d . . . H6A H 0.1619 -0.0158 0.4688 0.081 Uiso 1 1 calc R A 1 H6B H 0.0992 -0.0296 0.3822 0.081 Uiso 1 1 calc R A 1 C7A C 0.1068(4) 0.1448(6) 0.4219(4) 0.053(2) Uani 0.492(9) 1 d P B 1 H7AA H 0.0762 0.1374 0.4454 0.064 Uiso 0.492(9) 1 calc PR B 1 H7AB H 0.1468 0.1976 0.4533 0.064 Uiso 0.492(9) 1 calc PR B 1 C7B C 0.0696(4) 0.0999(5) 0.3737(4) 0.0493(18) Uani 0.508(9) 1 d P B 2 H7BA H 0.0501 0.0943 0.3183 0.059 Uiso 0.508(9) 1 calc PR B 2 H7BB H 0.0316 0.0775 0.3852 0.059 Uiso 0.508(9) 1 calc PR B 2 C8B C 0.0633(5) 0.1912(7) 0.3428(5) 0.080(3) Uani 0.492(9) 1 d P B 1 H8BA H 0.0254 0.1367 0.3092 0.096 Uiso 0.492(9) 1 calc PR B 1 H8BB H 0.0941 0.2093 0.3208 0.096 Uiso 0.492(9) 1 calc PR B 1 C8A C 0.0959(3) 0.2222(6) 0.4017(4) 0.0566(19) Uani 0.508(9) 1 d P B 2 H8AA H 0.1352 0.2429 0.3917 0.068 Uiso 0.508(9) 1 calc PR B 2 H8AB H 0.1145 0.2275 0.4569 0.068 Uiso 0.508(9) 1 calc PR B 2 C9 C -0.0899(2) 0.3804(3) 0.3240(3) 0.0679(9) Uani 1 1 d . . . H9A H -0.1374 0.3659 0.3139 0.081 Uiso 1 1 calc R . . C10 C -0.0433(3) 0.2880(3) 0.3394(3) 0.0980(16) Uani 1 1 d . B . H10A H -0.0597 0.2124 0.3383 0.118 Uiso 1 1 calc R . . C11 C 0.0281(3) 0.3076(4) 0.3564(3) 0.1029(18) Uani 1 1 d . . . C12 C 0.0484(2) 0.4198(3) 0.3539(3) 0.0743(10) Uani 1 1 d . B . H12A H 0.0956 0.4361 0.3637 0.089 Uiso 1 1 calc R . . C13 C -0.00118(16) 0.5081(3) 0.33703(19) 0.0553(7) Uani 1 1 d . . . H13A H 0.0135 0.5840 0.3353 0.066 Uiso 1 1 calc R B . C14 C 0.21215(16) 0.2452(3) 0.03970(16) 0.0504(6) Uani 1 1 d . . . H14A H 0.1865 0.2422 0.0665 0.060 Uiso 1 1 calc R . . C15 C 0.28646(15) 0.2204(2) 0.07776(14) 0.0432(6) Uani 1 1 d . . . C16 C 0.32423(16) 0.2256(3) 0.03799(17) 0.0524(7) Uani 1 1 d . . . H16A H 0.3743 0.2095 0.0633 0.063 Uiso 1 1 calc R . . C17 C 0.32695(17) 0.1893(2) 0.16260(16) 0.0500(6) Uani 1 1 d . . . C18 C 0.52921(14) 0.3936(2) 0.49765(16) 0.0415(5) Uani 1 1 d . . . H18A H 0.5490 0.3218 0.4962 0.050 Uiso 1 1 calc R . . C19 C 0.45657(14) 0.4182(2) 0.44447(14) 0.0371(5) Uani 1 1 d . . . C20 C 0.42764(14) 0.5254(2) 0.44726(15) 0.0416(5) Uani 1 1 d . . . H20A H 0.3789 0.5428 0.4118 0.050 Uiso 1 1 calc R . . C21 C 0.40832(15) 0.3289(2) 0.38523(15) 0.0433(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03954(18) 0.03756(18) 0.03498(17) -0.00389(11) 0.01505(13) -0.00012(11) O1 0.0571(14) 0.0864(17) 0.0493(12) 0.0104(12) 0.0040(10) -0.0079(12) O1W 0.080(4) 0.077(3) 0.300(11) 0.000 0.043(5) 0.000 O2 0.0687(14) 0.0722(14) 0.0407(10) 0.0040(10) 0.0256(10) -0.0083(11) O2W 0.112(3) 0.109(2) 0.125(3) 0.034(2) 0.073(2) 0.029(2) O3 0.0557(13) 0.0498(11) 0.0547(12) -0.0073(9) 0.0039(10) -0.0052(9) O4 0.0562(12) 0.0430(10) 0.0599(12) -0.0199(9) 0.0252(10) -0.0065(8) N1 0.0470(12) 0.0425(11) 0.0420(11) -0.0037(9) 0.0237(10) 0.0001(9) N2 0.0511(13) 0.0361(11) 0.0514(13) 0.0004(9) 0.0261(11) 0.0050(9) C1 0.0524(16) 0.0636(17) 0.0422(14) -0.0016(13) 0.0220(13) -0.0007(13) C2 0.071(2) 0.0637(18) 0.0469(15) 0.0068(14) 0.0364(15) 0.0103(15) C3 0.0615(17) 0.0345(12) 0.0681(18) 0.0152(12) 0.0444(15) 0.0148(11) C4 0.0517(17) 0.0557(17) 0.0662(19) -0.0039(14) 0.0305(15) -0.0069(13) C5 0.0544(16) 0.0597(17) 0.0465(14) -0.0117(13) 0.0274(13) -0.0104(13) C6 0.077(2) 0.0560(17) 0.097(3) 0.0340(18) 0.064(2) 0.0248(16) C7A 0.073(5) 0.048(4) 0.057(4) 0.014(3) 0.046(4) 0.015(3) C7B 0.054(4) 0.038(3) 0.065(4) 0.006(3) 0.037(3) 0.008(2) C8B 0.106(6) 0.073(5) 0.063(5) 0.010(4) 0.044(5) 0.048(5) C8A 0.049(3) 0.044(4) 0.070(5) -0.001(3) 0.024(3) 0.005(2) C9 0.073(2) 0.0438(16) 0.106(3) 0.0077(16) 0.059(2) 0.0040(14) C10 0.124(4) 0.0432(18) 0.170(5) 0.032(2) 0.106(4) 0.024(2) C11 0.115(4) 0.065(2) 0.180(5) 0.056(3) 0.112(4) 0.048(2) C12 0.061(2) 0.073(2) 0.101(3) 0.029(2) 0.049(2) 0.0236(17) C13 0.0493(16) 0.0489(15) 0.0664(18) 0.0045(14) 0.0279(14) 0.0052(12) C14 0.0503(15) 0.0576(16) 0.0453(14) -0.0021(12) 0.0254(13) -0.0106(12) C15 0.0482(14) 0.0337(12) 0.0361(12) 0.0013(9) 0.0123(11) -0.0092(10) C16 0.0411(14) 0.0584(17) 0.0482(15) 0.0046(13) 0.0152(12) -0.0023(12) C17 0.0597(17) 0.0390(13) 0.0427(14) -0.0025(11) 0.0191(13) -0.0055(12) C18 0.0438(13) 0.0329(11) 0.0490(14) -0.0043(10) 0.0239(12) 0.0007(10) C19 0.0439(13) 0.0322(11) 0.0372(11) -0.0043(9) 0.0217(10) -0.0055(9) C20 0.0382(12) 0.0377(12) 0.0433(13) -0.0022(10) 0.0161(11) -0.0001(10) C21 0.0524(15) 0.0394(13) 0.0364(12) -0.0032(10) 0.0208(12) -0.0065(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.9690(19) . ? Zn1 O2 2.003(2) . ? Zn1 N1 2.053(2) . ? Zn1 N2 2.059(2) 3_545 ? Zn1 O1 2.545(3) . ? Zn1 C17 2.602(3) . ? O1 C17 1.238(4) . ? O1W H1WA 0.8501 . ? O2 C17 1.257(4) . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8499 . ? O3 C21 1.231(3) . ? O4 C21 1.275(3) . ? N1 C5 1.334(3) . ? N1 C1 1.336(4) . ? N2 C9 1.334(4) . ? N2 C13 1.340(4) . ? N2 Zn1 2.059(2) 3_455 ? C1 C2 1.380(4) . ? C1 H1A 0.9300 . ? C2 C3 1.381(5) . ? C2 H2B 0.9300 . ? C3 C4 1.366(4) . ? C3 C6 1.500(4) . ? C4 C5 1.385(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7B 1.563(6) . ? C6 C7A 1.594(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7A C8B 1.474(11) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C7B C8A 1.510(9) . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C8B C11 1.614(8) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C8A C11 1.590(7) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C9 C10 1.371(5) . ? C9 H9A 0.9300 . ? C10 C11 1.382(6) . ? C10 H10A 0.9300 . ? C11 C12 1.365(6) . ? C12 C13 1.370(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.383(4) . ? C14 C16 1.385(4) 7 ? C14 H14A 0.9300 . ? C15 C16 1.375(4) . ? C15 C17 1.510(4) . ? C16 C14 1.385(4) 7 ? C16 H16A 0.9300 . ? C18 C20 1.379(4) 5_666 ? C18 C19 1.386(4) . ? C18 H18A 0.9300 . ? C19 C20 1.387(3) . ? C19 C21 1.510(3) . ? C20 C18 1.379(4) 5_666 ? C20 H20A 0.9300 . ? 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 O4 Zn1 O2 135.41(9) . . ? O4 Zn1 N1 106.71(9) . . ? O2 Zn1 N1 98.90(9) . . ? O4 Zn1 N2 97.10(9) . 3_545 ? O2 Zn1 N2 111.96(10) . 3_545 ? N1 Zn1 N2 103.24(9) . 3_545 ? O4 Zn1 O1 93.77(9) . . ? O2 Zn1 O1 55.77(9) . . ? N1 Zn1 O1 154.67(8) . . ? N2 Zn1 O1 88.47(9) 3_545 . ? O4 Zn1 C17 115.52(9) . . ? O2 Zn1 C17 28.00(9) . . ? N1 Zn1 C17 126.87(9) . . ? N2 Zn1 C17 102.00(9) 3_545 . ? O1 Zn1 C17 27.80(8) . . ? C17 O1 Zn1 78.69(18) . . ? C17 O2 Zn1 103.58(19) . . ? H2WA O2W H2WB 86.3 . . ? C21 O4 Zn1 108.08(18) . . ? C5 N1 C1 117.3(2) . . ? C5 N1 Zn1 121.44(18) . . ? C1 N1 Zn1 120.8(2) . . ? C9 N2 C13 117.2(3) . . ? C9 N2 Zn1 124.4(2) . 3_455 ? C13 N2 Zn1 118.32(19) . 3_455 ? N1 C1 C2 122.7(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2B 120.0 . . ? C3 C2 H2B 120.0 . . ? C4 C3 C2 116.9(3) . . ? C4 C3 C6 122.3(3) . . ? C2 C3 C6 120.7(3) . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N1 C5 C4 122.5(3) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? C3 C6 C7B 113.1(3) . . ? C3 C6 C7A 109.0(3) . . ? C7B C6 C7A 37.9(3) . . ? C3 C6 H6A 109.9 . . ? C7B C6 H6A 133.1 . . ? C7A C6 H6A 109.9 . . ? C3 C6 H6B 109.9 . . ? C7B C6 H6B 73.5 . . ? C7A C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8B C7A C6 108.9(6) . . ? C8B C7A H7AA 109.9 . . ? C6 C7A H7AA 109.9 . . ? C8B C7A H7AB 109.9 . . ? C6 C7A H7AB 109.9 . . ? H7AA C7A H7AB 108.3 . . ? C8A C7B C6 105.5(5) . . ? C8A C7B H7BA 110.6 . . ? C6 C7B H7BA 110.6 . . ? C8A C7B H7BB 110.6 . . ? C6 C7B H7BB 110.6 . . ? H7BA C7B H7BB 108.8 . . ? C7A C8B C11 102.2(6) . . ? C7A C8B H8BA 111.3 . . ? C11 C8B H8BA 111.3 . . ? C7A C8B H8BB 111.3 . . ? C11 C8B H8BB 111.3 . . ? H8BA C8B H8BB 109.2 . . ? C7B C8A C11 107.7(5) . . ? C7B C8A H8AA 110.2 . . ? C11 C8A H8AA 110.2 . . ? C7B C8A H8AB 110.2 . . ? C11 C8A H8AB 110.2 . . ? H8AA C8A H8AB 108.5 . . ? N2 C9 C10 122.6(3) . . ? N2 C9 H9A 118.7 . . ? C10 C9 H9A 118.7 . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 117.7(3) . . ? C12 C11 C8A 113.3(4) . . ? C10 C11 C8A 126.5(4) . . ? C12 C11 C8B 126.7(5) . . ? C10 C11 C8B 110.8(5) . . ? C8A C11 C8B 39.5(4) . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? N2 C13 C12 123.0(3) . . ? N2 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C15 C14 C16 120.4(3) . 7 ? C15 C14 H14A 119.8 . . ? C16 C14 H14A 119.8 7 . ? C16 C15 C14 119.5(2) . . ? C16 C15 C17 119.5(3) . . ? C14 C15 C17 121.0(3) . . ? C15 C16 C14 120.0(3) . 7 ? C15 C16 H16A 120.0 . . ? C14 C16 H16A 120.0 7 . ? O1 C17 O2 121.9(3) . . ? O1 C17 C15 120.5(3) . . ? O2 C17 C15 117.6(3) . . ? O1 C17 Zn1 73.52(17) . . ? O2 C17 Zn1 48.42(14) . . ? C15 C17 Zn1 165.8(2) . . ? C20 C18 C19 120.5(2) 5_666 . ? C20 C18 H18A 119.7 5_666 . ? C19 C18 H18A 119.7 . . ? C18 C19 C20 119.2(2) . . ? C18 C19 C21 120.9(2) . . ? C20 C19 C21 119.8(2) . . ? C18 C20 C19 120.2(2) 5_666 . ? C18 C20 H20A 119.9 5_666 . ? C19 C20 H20A 119.9 . . ? O3 C21 O4 122.8(2) . . ? O3 C21 C19 120.6(2) . . ? O4 C21 C19 116.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.517 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.061 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # Attachment '2.cif' data_a2 _database_code_depnum_ccdc_archive 'CCDC 629053' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H44 N4 O16 Zn4' _chemical_formula_weight 1314.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.497(3) _cell_length_b 14.594(4) _cell_length_c 19.106(5) _cell_angle_alpha 89.927(8) _cell_angle_beta 83.212(7) _cell_angle_gamma 73.564(4) _cell_volume 2786.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4767 _cell_measurement_theta_min 2.4180 _cell_measurement_theta_max 27.4526 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1700 _exptl_crystal_size_mid 0.0600 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.775 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8758 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 21993 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12508 _reflns_number_gt 7204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^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 12508 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.58194(5) 0.63865(4) -0.15078(3) 0.03173(15) Uani 1 1 d . . . Zn2 Zn 0.64107(5) 0.86196(4) -0.11579(3) 0.03343(15) Uani 1 1 d . . . Zn3 Zn 0.07910(5) 0.62742(4) 0.34419(3) 0.03479(16) Uani 1 1 d . . . Zn4 Zn 0.15273(6) 0.84026(4) 0.38631(3) 0.03707(16) Uani 1 1 d . . . O1 O 0.5627(3) 0.8098(3) -0.03291(16) 0.0445(9) Uani 1 1 d . . . O2 O 0.4462(3) 0.7253(3) -0.08275(15) 0.0385(8) Uani 1 1 d . . . O3 O 0.1322(3) 0.6724(3) 0.25222(16) 0.0449(9) Uani 1 1 d . . . O4 O 0.7206(4) 0.8009(3) -0.20741(16) 0.0457(9) Uani 1 1 d . . . O5 O 0.7276(4) 0.9539(3) -0.08244(19) 0.0533(10) Uani 1 1 d . . . O6 O 0.2323(4) 0.7712(3) 0.29517(17) 0.0500(10) Uani 1 1 d . . . O7 O 0.9440(4) 0.6954(3) -0.58075(17) 0.0520(10) Uani 1 1 d . . . O8 O 0.9934(4) 0.8281(3) -0.55111(18) 0.0530(10) Uani 1 1 d . . . O9 O 0.6185(3) 0.6964(3) -0.24221(16) 0.0422(9) Uani 1 1 d . . . O10 O 0.7581(3) 0.6049(3) -0.12010(17) 0.0473(10) Uani 1 1 d . . . O11 O 0.8734(5) 0.8152(3) -0.0751(2) 0.0694(12) Uani 1 1 d . . . O12 O 0.2369(4) 0.5561(3) 0.3849(2) 0.0606(11) Uani 1 1 d . . . O13 O 0.2547(4) 0.8915(3) 0.44384(19) 0.0624(12) Uani 1 1 d . . . O14 O 0.2460(5) 0.6929(3) 0.4319(2) 0.0711(13) Uani 1 1 d . . . O15 O 0.3480(5) 0.9431(4) 0.3478(2) 0.0744(14) Uani 1 1 d . . . O16 O 0.6521(4) 0.5403(3) -0.03560(18) 0.0522(10) Uani 1 1 d . . . N1 N 0.4993(4) 1.5389(3) -0.17935(19) 0.0359(9) Uani 1 1 d . . . N2 N 0.4788(4) 0.9625(3) -0.1491(2) 0.0395(10) Uani 1 1 d . . . N3 N -0.0109(4) 0.5286(3) 0.3185(2) 0.0379(10) Uani 1 1 d . . . N4 N 0.0262(4) -0.0489(3) 0.3330(2) 0.0444(11) Uani 1 1 d . . . C1 C 0.4406(7) 0.9309(5) 0.5236(3) 0.0649(18) Uani 1 1 d . . . H1A H 0.4016 0.8838 0.5399 0.078 Uiso 1 1 calc R . . C2 C 1.0374(5) 0.9013(4) -0.0045(3) 0.0431(12) Uani 1 1 d . . . H2A H 1.0626 0.8349 -0.0072 0.052 Uiso 1 1 calc R . . C3 C 0.5177(7) 0.9643(5) 0.5655(3) 0.0684(19) Uani 1 1 d . . . H3A H 0.5287 0.9402 0.6102 0.082 Uiso 1 1 calc R . . C4 C 1.1131(5) 0.9489(4) 0.0275(3) 0.0446(13) Uani 1 1 d . . . H4A H 1.1897 0.9139 0.0459 0.054 Uiso 1 1 calc R . . C14 C 0.4769(5) 0.7632(3) -0.0298(2) 0.0327(11) Uani 1 1 d . . . C15 C 0.4243(5) 0.8043(3) 0.0992(2) 0.0349(11) Uani 1 1 d . . . H15A H 0.4786 0.8449 0.0935 0.042 Uiso 1 1 calc R . . C19 C 0.3591(4) 0.7952(3) 0.1650(2) 0.0325(11) Uani 1 1 d . . . H19A H 0.3695 0.8298 0.2037 0.039 Uiso 1 1 calc R . . C20 C 0.7533(5) 0.5592(4) -0.0629(2) 0.0385(12) Uani 1 1 d . . . C21 C 0.6942(5) 0.7495(4) -0.2530(2) 0.0352(11) Uani 1 1 d . . . C23 C 0.2083(5) 0.7254(4) 0.2456(2) 0.0364(12) Uani 1 1 d . . . C24 C 0.9231(5) 0.9535(4) -0.0325(2) 0.0346(11) Uani 1 1 d . . . C26 C 0.9091(5) 0.4480(4) 0.0095(3) 0.0456(13) Uani 1 1 d . . . H26A H 0.8473 0.4130 0.0161 0.055 Uiso 1 1 calc R . . C28 C 0.3285(5) 0.6915(4) 0.0503(2) 0.0368(11) Uani 1 1 d . . . H28A H 0.3189 0.6560 0.0118 0.044 Uiso 1 1 calc R . . C29 C 0.2782(5) 0.7342(4) 0.1734(2) 0.0338(11) Uani 1 1 d . . . C31 C 0.8826(5) 0.5284(4) -0.0305(2) 0.0350(11) Uani 1 1 d . . . C32 C 0.8383(5) 0.9019(4) -0.0657(3) 0.0409(12) Uani 1 1 d . . . C34 C 0.8750(6) 0.8269(4) -0.4148(2) 0.0488(14) Uani 1 1 d . . . H34A H 0.9132 0.8756 -0.4277 0.059 Uiso 1 1 calc R . . C35 C 0.9432(5) 0.7614(4) -0.5376(2) 0.0391(12) Uani 1 1 d . . . C36 C 0.8176(6) 0.8236(4) -0.3459(2) 0.0480(14) Uani 1 1 d . . . H36A H 0.8197 0.8691 -0.3123 0.058 Uiso 1 1 calc R . . C37 C 0.8754(5) 0.7583(4) -0.4640(2) 0.0385(12) Uani 1 1 d . . . C39 C 0.3715(5) 1.4303(4) -0.1453(3) 0.0446(13) Uani 1 1 d . . . H39A H 0.3249 1.4055 -0.1093 0.054 Uiso 1 1 calc R . . C40 C 0.2622(5) 0.6829(4) 0.1168(2) 0.0381(12) Uani 1 1 d . . . H40A H 0.2076 0.6425 0.1226 0.046 Uiso 1 1 calc R . . C42 C 0.5087(6) 1.5072(4) -0.2455(3) 0.0478(14) Uani 1 1 d . . . H42A H 0.5549 1.5336 -0.2808 0.057 Uiso 1 1 calc R . . C43 C 0.4079(4) 0.7523(3) 0.0415(2) 0.0296(10) Uani 1 1 d . . . C44 C 0.7578(5) 0.7536(4) -0.3272(2) 0.0334(11) Uani 1 1 d . . . C45 C 0.4834(6) 0.9952(4) -0.2145(3) 0.0476(14) Uani 1 1 d . . . H45A H 0.5551 0.9643 -0.2476 0.057 Uiso 1 1 calc R . . C47 C 0.3972(5) 0.5500(4) 0.4626(3) 0.0426(12) Uani 1 1 d . . . C50 C 0.2854(6) 0.6050(5) 0.4236(3) 0.0480(14) Uani 1 1 d . . . C51 C 0.3386(6) 0.9306(4) 0.4121(3) 0.0507(14) Uani 1 1 d . . . C52 C 0.3797(5) 1.3976(4) -0.2136(3) 0.0409(12) Uani 1 1 d . . . C53 C 0.4308(5) 1.4985(4) -0.1295(3) 0.0431(13) Uani 1 1 d . . . H53A H 0.4240 1.5183 -0.0826 0.052 Uiso 1 1 calc R . . C55 C 0.3859(6) 1.0734(4) -0.2355(3) 0.0551(16) Uani 1 1 d . . . H55A H 0.3938 1.0932 -0.2817 0.066 Uiso 1 1 calc R . . C56 C 0.4364(6) 0.4521(5) 0.4615(3) 0.0622(17) Uani 1 1 d . . . H56A H 0.3941 0.4188 0.4350 0.075 Uiso 1 1 calc R . . C57 C 0.9726(5) 0.5811(4) -0.0399(3) 0.0441(13) Uani 1 1 d . . . H57A H 0.9545 0.6358 -0.0663 0.053 Uiso 1 1 calc R . . C58 C 0.0721(7) -0.0221(5) 0.2702(3) 0.0609(17) Uani 1 1 d . . . H58A H 0.1612 -0.0501 0.2527 0.073 Uiso 1 1 calc R . . C59 C 0.4213(5) 0.9668(4) 0.4580(3) 0.0462(13) Uani 1 1 d . . . C60 C 0.2729(6) 1.0866(5) -0.1213(3) 0.0608(17) Uani 1 1 d . . . H60A H 0.2009 1.1159 -0.0880 0.073 Uiso 1 1 calc R . . C61 C 0.4529(6) 1.4367(4) -0.2645(3) 0.0508(14) Uani 1 1 d . . . H61A H 0.4645 1.4155 -0.3113 0.061 Uiso 1 1 calc R . . C62 C 0.2799(6) 1.1208(4) -0.1891(3) 0.0498(14) Uani 1 1 d . . . C63 C 0.1772(6) 1.2091(4) -0.2081(4) 0.0649(18) Uani 1 1 d . . . H63A H 0.0897 1.2096 -0.1849 0.078 Uiso 1 1 calc R . . H63B H 0.1740 1.2082 -0.2587 0.078 Uiso 1 1 calc R . . C64 C 0.4618(6) 0.5989(4) 0.5009(3) 0.0601(16) Uani 1 1 d . . . H64A H 0.4376 0.6654 0.5017 0.072 Uiso 1 1 calc R . . C70 C -0.1011(7) -0.0048(5) 0.3551(4) 0.073(2) Uani 1 1 d . . . H70A H -0.1363 -0.0201 0.3990 0.088 Uiso 1 1 calc R . . C71 C -0.1044(7) 0.5061(5) 0.3664(3) 0.0669(19) Uani 1 1 d . . . H71A H -0.1307 0.5408 0.4090 0.080 Uiso 1 1 calc R . . C72 C -0.1604(7) 0.4347(5) 0.3540(3) 0.071(2) Uani 1 1 d . . . H72A H -0.2252 0.4233 0.3877 0.085 Uiso 1 1 calc R . . C73 C -0.1855(6) 0.0625(5) 0.3176(4) 0.073(2) Uani 1 1 d . . . H73A H -0.2745 0.0894 0.3358 0.088 Uiso 1 1 calc R . . C74 C -0.0049(7) 0.0443(5) 0.2307(3) 0.069(2) Uani 1 1 d . . . H74A H 0.0328 0.0595 0.1874 0.083 Uiso 1 1 calc R . . C75 C -0.2219(8) 0.1681(5) 0.2137(4) 0.075(2) Uani 1 1 d . . . H75A H -0.3137 0.1855 0.2362 0.090 Uiso 1 1 calc R . . H75B H -0.2209 0.1454 0.1659 0.090 Uiso 1 1 calc R . . C77 C -0.1696(7) 0.2566(4) 0.2118(3) 0.0685(19) Uani 1 1 d . . . H77A H -0.0764 0.2387 0.1916 0.082 Uiso 1 1 calc R . . H77B H -0.2203 0.3040 0.1823 0.082 Uiso 1 1 calc R . . C78 C 0.3723(6) 1.0095(4) -0.1035(3) 0.0556(16) Uani 1 1 d . . . H78A H 0.3657 0.9886 -0.0575 0.067 Uiso 1 1 calc R . . C79 C 0.8201(6) 0.6863(5) -0.4448(3) 0.0572(17) Uani 1 1 d . . . H79A H 0.8230 0.6385 -0.4776 0.069 Uiso 1 1 calc R . . C80 C -0.1828(7) 0.2979(5) 0.2842(3) 0.0663(18) Uani 1 1 d . . . H80A H -0.1417 0.2470 0.3141 0.080 Uiso 1 1 calc R . . H80B H -0.2774 0.3200 0.3017 0.080 Uiso 1 1 calc R . . C81 C 0.2106(6) 1.3000(4) -0.1860(4) 0.0647(18) Uani 1 1 d . . . H81A H 0.1322 1.3545 -0.1865 0.078 Uiso 1 1 calc R . . H81B H 0.2334 1.2941 -0.1381 0.078 Uiso 1 1 calc R . . C82 C -0.0296(6) 0.4024(4) 0.2442(3) 0.0500(14) Uani 1 1 d . . . H82A H -0.0026 0.3686 0.2012 0.060 Uiso 1 1 calc R . . C83 C 0.7592(6) 0.6844(4) -0.3758(3) 0.0547(16) Uani 1 1 d . . . H83A H 0.7197 0.6363 -0.3630 0.066 Uiso 1 1 calc R . . C84 C -0.1371(7) 0.0890(4) 0.2536(3) 0.0540(15) Uani 1 1 d . . . C85 C -0.1229(6) 0.3796(4) 0.2930(3) 0.0481(14) Uani 1 1 d . . . C86 C 0.3263(6) 1.3176(4) -0.2344(3) 0.0533(15) Uani 1 1 d . . . H86A H 0.3995 1.2590 -0.2385 0.064 Uiso 1 1 calc R . . H86B H 0.2981 1.3300 -0.2809 0.064 Uiso 1 1 calc R . . C87 C 0.0234(6) 0.4756(4) 0.2592(3) 0.0466(13) Uani 1 1 d . . . H87A H 0.0873 0.4884 0.2257 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0317(3) 0.0389(3) 0.0267(3) 0.0035(2) -0.0025(2) -0.0140(2) Zn2 0.0401(3) 0.0431(4) 0.0238(3) 0.0000(2) -0.0007(2) -0.0239(3) Zn3 0.0369(3) 0.0453(4) 0.0258(3) 0.0041(2) -0.0024(2) -0.0183(3) Zn4 0.0436(4) 0.0481(4) 0.0258(3) -0.0028(2) 0.0000(2) -0.0249(3) O1 0.050(2) 0.061(3) 0.0296(17) 0.0059(16) 0.0037(15) -0.0295(19) O2 0.0362(19) 0.052(2) 0.0257(17) 0.0010(15) -0.0010(14) -0.0116(16) O3 0.045(2) 0.064(3) 0.0311(18) 0.0088(17) 0.0004(15) -0.0265(19) O4 0.057(2) 0.058(3) 0.0255(17) -0.0051(16) 0.0041(15) -0.0264(19) O5 0.048(2) 0.064(3) 0.061(2) 0.002(2) -0.0236(19) -0.032(2) O6 0.068(3) 0.054(2) 0.0282(18) -0.0052(16) 0.0099(17) -0.024(2) O7 0.053(2) 0.070(3) 0.0353(19) -0.0133(18) 0.0100(17) -0.028(2) O8 0.065(3) 0.047(2) 0.047(2) 0.0044(18) 0.0147(19) -0.025(2) O9 0.046(2) 0.059(2) 0.0285(17) 0.0105(16) -0.0054(15) -0.0256(18) O10 0.037(2) 0.065(3) 0.0387(19) 0.0157(18) -0.0090(15) -0.0109(18) O11 0.085(3) 0.053(3) 0.086(3) -0.002(2) -0.029(3) -0.036(2) O12 0.056(3) 0.074(3) 0.056(2) 0.002(2) -0.029(2) -0.017(2) O13 0.076(3) 0.079(3) 0.051(2) 0.002(2) -0.016(2) -0.050(3) O14 0.079(3) 0.058(3) 0.074(3) 0.016(2) -0.035(2) -0.006(3) O15 0.080(3) 0.114(4) 0.049(2) -0.001(2) -0.015(2) -0.057(3) O16 0.041(2) 0.066(3) 0.054(2) 0.020(2) -0.0132(17) -0.021(2) N1 0.039(2) 0.039(2) 0.032(2) 0.0036(18) -0.0034(17) -0.0154(19) N2 0.041(2) 0.050(3) 0.034(2) 0.0028(19) -0.0059(18) -0.023(2) N3 0.039(2) 0.042(3) 0.035(2) 0.0031(18) -0.0027(18) -0.016(2) N4 0.047(3) 0.042(3) 0.047(3) 0.007(2) -0.002(2) -0.018(2) C1 0.082(5) 0.078(5) 0.055(4) 0.011(3) -0.018(3) -0.051(4) C2 0.048(3) 0.029(3) 0.057(3) -0.002(2) -0.019(3) -0.013(2) C3 0.090(5) 0.092(5) 0.049(4) 0.015(3) -0.024(3) -0.061(4) C4 0.036(3) 0.039(3) 0.062(3) 0.002(3) -0.020(2) -0.009(2) C14 0.033(3) 0.034(3) 0.028(2) 0.009(2) 0.0033(19) -0.006(2) C15 0.036(3) 0.034(3) 0.036(3) 0.000(2) 0.000(2) -0.013(2) C19 0.036(3) 0.034(3) 0.027(2) -0.0025(19) 0.0018(19) -0.012(2) C20 0.040(3) 0.039(3) 0.036(3) 0.000(2) -0.009(2) -0.008(2) C21 0.036(3) 0.037(3) 0.031(2) 0.004(2) 0.001(2) -0.011(2) C23 0.035(3) 0.037(3) 0.032(3) 0.006(2) 0.001(2) -0.005(2) C24 0.032(3) 0.036(3) 0.041(3) 0.002(2) -0.009(2) -0.016(2) C26 0.045(3) 0.048(3) 0.054(3) 0.014(3) -0.013(3) -0.027(3) C28 0.046(3) 0.043(3) 0.027(2) -0.008(2) 0.001(2) -0.023(2) C29 0.034(3) 0.040(3) 0.026(2) 0.008(2) 0.0007(19) -0.011(2) C31 0.032(3) 0.038(3) 0.036(3) 0.003(2) -0.009(2) -0.010(2) C32 0.047(3) 0.048(3) 0.038(3) 0.005(2) -0.012(2) -0.028(3) C34 0.072(4) 0.050(3) 0.035(3) 0.002(2) 0.007(3) -0.040(3) C35 0.038(3) 0.045(3) 0.032(3) 0.004(2) 0.007(2) -0.014(2) C36 0.076(4) 0.045(3) 0.033(3) -0.010(2) 0.009(3) -0.040(3) C37 0.048(3) 0.041(3) 0.029(2) 0.005(2) 0.003(2) -0.019(2) C39 0.047(3) 0.052(4) 0.042(3) 0.008(2) -0.003(2) -0.025(3) C40 0.037(3) 0.050(3) 0.035(3) -0.002(2) 0.002(2) -0.028(2) C42 0.062(4) 0.058(4) 0.029(3) 0.002(2) -0.001(2) -0.027(3) C43 0.033(2) 0.029(3) 0.026(2) 0.0029(18) 0.0014(18) -0.009(2) C44 0.039(3) 0.038(3) 0.025(2) -0.0010(19) 0.0008(19) -0.016(2) C45 0.058(4) 0.050(4) 0.038(3) 0.002(2) -0.008(2) -0.019(3) C47 0.042(3) 0.046(3) 0.043(3) 0.004(2) -0.017(2) -0.014(3) C50 0.046(3) 0.055(4) 0.044(3) 0.010(3) -0.010(2) -0.015(3) C51 0.049(3) 0.061(4) 0.051(3) -0.001(3) -0.008(3) -0.028(3) C52 0.041(3) 0.036(3) 0.047(3) 0.005(2) -0.012(2) -0.011(2) C53 0.050(3) 0.048(3) 0.037(3) 0.003(2) -0.006(2) -0.023(3) C55 0.074(4) 0.054(4) 0.045(3) 0.010(3) -0.022(3) -0.025(3) C56 0.069(4) 0.064(4) 0.067(4) 0.002(3) -0.038(3) -0.030(4) C57 0.042(3) 0.042(3) 0.052(3) 0.013(2) -0.019(2) -0.014(2) C58 0.078(4) 0.060(4) 0.042(3) 0.008(3) 0.002(3) -0.018(3) C59 0.043(3) 0.061(4) 0.045(3) 0.002(3) -0.010(2) -0.030(3) C60 0.041(3) 0.063(4) 0.074(4) 0.015(3) 0.009(3) -0.013(3) C61 0.064(4) 0.059(4) 0.038(3) -0.007(3) -0.003(3) -0.030(3) C62 0.043(3) 0.046(3) 0.072(4) 0.011(3) -0.018(3) -0.026(3) C63 0.046(3) 0.051(4) 0.109(5) 0.020(4) -0.027(3) -0.025(3) C64 0.068(4) 0.040(3) 0.076(4) 0.007(3) -0.027(3) -0.014(3) C70 0.062(4) 0.072(5) 0.075(4) 0.033(4) 0.007(3) -0.009(4) C71 0.092(5) 0.079(5) 0.044(3) -0.016(3) 0.015(3) -0.055(4) C72 0.087(5) 0.075(5) 0.060(4) -0.008(3) 0.018(3) -0.052(4) C73 0.044(4) 0.073(5) 0.099(5) 0.017(4) 0.002(3) -0.014(3) C74 0.096(6) 0.065(5) 0.045(3) 0.014(3) -0.001(3) -0.022(4) C75 0.096(6) 0.053(4) 0.095(5) 0.019(4) -0.054(4) -0.036(4) C77 0.090(5) 0.048(4) 0.080(5) 0.013(3) -0.043(4) -0.026(4) C78 0.054(4) 0.061(4) 0.050(3) 0.014(3) 0.004(3) -0.017(3) C79 0.083(4) 0.078(5) 0.028(3) -0.009(3) 0.012(3) -0.058(4) C80 0.077(5) 0.054(4) 0.076(5) 0.005(3) -0.014(4) -0.030(4) C81 0.050(4) 0.047(4) 0.102(5) 0.015(3) -0.013(3) -0.020(3) C82 0.064(4) 0.046(3) 0.045(3) -0.004(2) -0.006(3) -0.023(3) C83 0.088(5) 0.059(4) 0.033(3) -0.003(2) 0.010(3) -0.054(3) C84 0.067(4) 0.046(4) 0.063(4) 0.009(3) -0.027(3) -0.030(3) C85 0.047(3) 0.041(3) 0.058(4) 0.007(3) -0.011(3) -0.014(3) C86 0.058(4) 0.051(4) 0.060(4) 0.006(3) -0.021(3) -0.025(3) C87 0.051(3) 0.050(4) 0.036(3) -0.002(2) 0.001(2) -0.013(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 O10 1.936(3) . ? Zn1 O2 1.966(3) . ? Zn1 O9 1.982(3) . ? Zn1 N1 1.999(4) 1_545 ? Zn2 O4 1.948(3) . ? Zn2 O1 1.951(3) . ? Zn2 O5 1.964(4) . ? Zn2 N2 2.073(4) . ? Zn2 O11 2.554(5) . ? Zn2 C32 2.588(5) . ? Zn3 O12 1.939(4) . ? Zn3 O7 1.943(4) 1_456 ? Zn3 O3 1.950(3) . ? Zn3 N3 2.024(4) . ? Zn4 O13 1.910(4) . ? Zn4 O6 1.982(3) . ? Zn4 O8 1.988(3) 1_456 ? Zn4 N4 2.126(4) 1_565 ? Zn4 O14 2.313(4) . ? O1 C14 1.269(6) . ? O2 C14 1.270(6) . ? O3 C23 1.257(6) . ? O4 C21 1.254(6) . ? O5 C32 1.272(6) . ? O6 C23 1.248(6) . ? O7 C35 1.266(6) . ? O7 Zn3 1.943(4) 1_654 ? O8 C35 1.245(6) . ? O8 Zn4 1.988(3) 1_654 ? O9 C21 1.259(6) . ? O10 C20 1.283(5) . ? O11 C32 1.220(7) . ? O12 C50 1.269(7) . ? O13 C51 1.274(6) . ? O14 C50 1.235(7) . ? O15 C51 1.238(6) . ? O16 C20 1.230(6) . ? N1 C42 1.330(6) . ? N1 C53 1.359(6) . ? N1 Zn1 1.999(4) 1_565 ? N2 C45 1.337(6) . ? N2 C78 1.348(7) . ? N3 C87 1.325(6) . ? N3 C71 1.370(6) . ? N4 C70 1.326(7) . ? N4 C58 1.339(6) . ? N4 Zn4 2.126(4) 1_545 ? C1 C59 1.372(7) . ? C1 C3 1.383(8) . ? C1 H1A 0.9300 . ? C2 C4 1.383(7) . ? C2 C24 1.393(6) . ? C2 H2A 0.9300 . ? C3 C59 1.385(8) 2_676 ? C3 H3A 0.9300 . ? C4 C24 1.367(7) 2_775 ? C4 H4A 0.9300 . ? C14 C43 1.496(6) . ? C15 C19 1.383(6) . ? C15 C43 1.394(7) . ? C15 H15A 0.9300 . ? C19 C29 1.391(7) . ? C19 H19A 0.9300 . ? C20 C31 1.510(7) . ? C21 C44 1.502(6) . ? C23 C29 1.508(6) . ? C24 C4 1.367(7) 2_775 ? C24 C32 1.509(7) . ? C26 C31 1.378(6) . ? C26 C57 1.390(7) 2_765 ? C26 H26A 0.9300 . ? C28 C43 1.377(6) . ? C28 C40 1.399(6) . ? C28 H28A 0.9300 . ? C29 C40 1.368(7) . ? C31 C57 1.374(7) . ? C34 C37 1.373(7) . ? C34 C36 1.389(6) . ? C34 H34A 0.9300 . ? C35 C37 1.507(6) . ? C36 C44 1.370(7) . ? C36 H36A 0.9300 . ? C37 C79 1.367(7) . ? C39 C53 1.367(7) . ? C39 C52 1.374(7) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C42 C61 1.388(8) . ? C42 H42A 0.9300 . ? C44 C83 1.368(7) . ? C45 C55 1.395(8) . ? C45 H45A 0.9300 . ? C47 C56 1.370(8) . ? C47 C64 1.377(8) . ? C47 C50 1.500(7) . ? C51 C59 1.499(7) . ? C52 C61 1.390(7) . ? C52 C86 1.503(8) . ? C53 H53A 0.9300 . ? C55 C62 1.354(8) . ? C55 H55A 0.9300 . ? C56 C64 1.394(8) 2_666 ? C56 H56A 0.9300 . ? C57 C26 1.390(7) 2_765 ? C57 H57A 0.9300 . ? C58 C74 1.364(8) . ? C58 H58A 0.9300 . ? C59 C3 1.385(8) 2_676 ? C60 C78 1.375(8) . ? C60 C62 1.389(7) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? C62 C63 1.503(8) . ? C63 C81 1.537(9) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C56 1.394(8) 2_666 ? C64 H64A 0.9300 . ? C70 C73 1.385(8) . ? C70 H70A 0.9300 . ? C71 C72 1.366(9) . ? C71 H71A 0.9300 . ? C72 C85 1.371(8) . ? C72 H72A 0.9300 . ? C73 C84 1.365(8) . ? C73 H73A 0.9300 . ? C74 C84 1.374(9) . ? C74 H74A 0.9300 . ? C75 C84 1.510(8) . ? C75 C77 1.538(9) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C77 C80 1.486(8) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9300 . ? C79 C83 1.399(6) . ? C79 H79A 0.9300 . ? C80 C85 1.515(8) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C86 1.519(8) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C85 1.381(7) . ? C82 C87 1.381(8) . ? C82 H82A 0.9300 . ? C83 H83A 0.9300 . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9300 . ? 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 O10 Zn1 O2 112.39(15) . . ? O10 Zn1 O9 100.44(14) . . ? O2 Zn1 O9 114.27(14) . . ? O10 Zn1 N1 121.62(17) . 1_545 ? O2 Zn1 N1 106.00(15) . 1_545 ? O9 Zn1 N1 101.84(15) . 1_545 ? O4 Zn2 O1 129.66(16) . . ? O4 Zn2 O5 114.62(16) . . ? O1 Zn2 O5 107.58(15) . . ? O4 Zn2 N2 97.87(16) . . ? O1 Zn2 N2 103.62(15) . . ? O5 Zn2 N2 96.35(17) . . ? O4 Zn2 O11 89.08(15) . . ? O1 Zn2 O11 92.81(15) . . ? O5 Zn2 O11 55.87(15) . . ? N2 Zn2 O11 151.33(15) . . ? O4 Zn2 C32 103.61(16) . . ? O1 Zn2 C32 100.49(15) . . ? O5 Zn2 C32 28.46(16) . . ? N2 Zn2 C32 124.64(18) . . ? O11 Zn2 C32 27.43(15) . . ? O12 Zn3 O7 109.11(17) . 1_456 ? O12 Zn3 O3 109.68(16) . . ? O7 Zn3 O3 128.88(16) 1_456 . ? O12 Zn3 N3 105.21(18) . . ? O7 Zn3 N3 98.23(16) 1_456 . ? O3 Zn3 N3 102.36(16) . . ? O13 Zn4 O6 122.20(18) . . ? O13 Zn4 O8 106.55(17) . 1_456 ? O6 Zn4 O8 127.59(17) . 1_456 ? O13 Zn4 N4 110.51(19) . 1_565 ? O6 Zn4 N4 90.48(16) . 1_565 ? O8 Zn4 N4 89.53(16) 1_456 1_565 ? O13 Zn4 O14 87.55(18) . . ? O6 Zn4 O14 82.88(16) . . ? O8 Zn4 O14 81.04(16) 1_456 . ? N4 Zn4 O14 161.47(18) 1_565 . ? C14 O1 Zn2 128.1(3) . . ? C14 O2 Zn1 122.2(3) . . ? C23 O3 Zn3 121.2(3) . . ? C21 O4 Zn2 138.4(3) . . ? C32 O5 Zn2 104.1(4) . . ? C23 O6 Zn4 143.4(4) . . ? C35 O7 Zn3 131.3(4) . 1_654 ? C35 O8 Zn4 134.1(4) . 1_654 ? C21 O9 Zn1 124.6(3) . . ? C20 O10 Zn1 108.0(3) . . ? C32 O11 Zn2 77.8(3) . . ? C50 O12 Zn3 115.3(4) . . ? C51 O13 Zn4 116.8(4) . . ? C50 O14 Zn4 148.6(4) . . ? C42 N1 C53 116.4(5) . . ? C42 N1 Zn1 123.8(3) . 1_565 ? C53 N1 Zn1 119.8(3) . 1_565 ? C45 N2 C78 115.9(5) . . ? C45 N2 Zn2 121.5(4) . . ? C78 N2 Zn2 121.7(3) . . ? C87 N3 C71 115.6(5) . . ? C87 N3 Zn3 124.0(4) . . ? C71 N3 Zn3 120.1(4) . . ? C70 N4 C58 114.8(5) . . ? C70 N4 Zn4 125.3(4) . 1_545 ? C58 N4 Zn4 119.8(4) . 1_545 ? C59 C1 C3 120.3(6) . . ? C59 C1 H1A 119.8 . . ? C3 C1 H1A 119.8 . . ? C4 C2 C24 119.6(5) . . ? C4 C2 H2A 120.2 . . ? C24 C2 H2A 120.2 . . ? C1 C3 C59 120.9(5) . 2_676 ? C1 C3 H3A 119.5 . . ? C59 C3 H3A 119.5 2_676 . ? C24 C4 C2 121.0(5) 2_775 . ? C24 C4 H4A 119.5 2_775 . ? C2 C4 H4A 119.5 . . ? O1 C14 O2 124.6(4) . . ? O1 C14 C43 117.3(4) . . ? O2 C14 C43 118.1(4) . . ? C19 C15 C43 119.6(5) . . ? C19 C15 H15A 120.2 . . ? C43 C15 H15A 120.2 . . ? C15 C19 C29 120.1(4) . . ? C15 C19 H19A 120.0 . . ? C29 C19 H19A 120.0 . . ? O16 C20 O10 123.6(5) . . ? O16 C20 C31 121.1(4) . . ? O10 C20 C31 115.3(4) . . ? O4 C21 O9 125.9(4) . . ? O4 C21 C44 116.4(4) . . ? O9 C21 C44 117.6(5) . . ? O6 C23 O3 124.7(4) . . ? O6 C23 C29 116.8(5) . . ? O3 C23 C29 118.6(5) . . ? C4 C24 C2 119.4(5) 2_775 . ? C4 C24 C32 120.8(4) 2_775 . ? C2 C24 C32 119.8(5) . . ? C31 C26 C57 120.5(5) . 2_765 ? C31 C26 H26A 119.8 . . ? C57 C26 H26A 119.8 2_765 . ? C43 C28 C40 120.2(4) . . ? C43 C28 H28A 119.9 . . ? C40 C28 H28A 119.9 . . ? C40 C29 C19 120.5(4) . . ? C40 C29 C23 120.4(5) . . ? C19 C29 C23 119.1(5) . . ? C57 C31 C26 120.1(5) . . ? C57 C31 C20 120.1(4) . . ? C26 C31 C20 119.7(5) . . ? O11 C32 O5 122.1(5) . . ? O11 C32 C24 121.8(5) . . ? O5 C32 C24 116.1(5) . . ? O11 C32 Zn2 74.8(3) . . ? O5 C32 Zn2 47.4(3) . . ? C24 C32 Zn2 163.0(4) . . ? C37 C34 C36 120.1(5) . . ? C37 C34 H34A 120.0 . . ? C36 C34 H34A 120.0 . . ? O8 C35 O7 125.5(4) . . ? O8 C35 C37 117.8(5) . . ? O7 C35 C37 116.7(5) . . ? C44 C36 C34 120.1(5) . . ? C44 C36 H36A 119.9 . . ? C34 C36 H36A 119.9 . . ? C79 C37 C34 119.8(4) . . ? C79 C37 C35 121.2(5) . . ? C34 C37 C35 118.9(5) . . ? C53 C39 C52 121.1(5) . . ? C53 C39 H39A 119.4 . . ? C52 C39 H39A 119.4 . . ? C29 C40 C28 119.7(5) . . ? C29 C40 H40A 120.2 . . ? C28 C40 H40A 120.2 . . ? N1 C42 C61 123.2(5) . . ? N1 C42 H42A 118.4 . . ? C61 C42 H42A 118.4 . . ? C28 C43 C15 120.0(4) . . ? C28 C43 C14 120.4(4) . . ? C15 C43 C14 119.6(4) . . ? C83 C44 C36 120.0(4) . . ? C83 C44 C21 119.2(5) . . ? C36 C44 C21 120.8(5) . . ? N2 C45 C55 123.2(5) . . ? N2 C45 H45A 118.4 . . ? C55 C45 H45A 118.4 . . ? C56 C47 C64 119.0(5) . . ? C56 C47 C50 121.6(5) . . ? C64 C47 C50 119.3(5) . . ? O14 C50 O12 125.0(5) . . ? O14 C50 C47 118.7(6) . . ? O12 C50 C47 116.3(5) . . ? O15 C51 O13 123.1(5) . . ? O15 C51 C59 120.9(5) . . ? O13 C51 C59 115.9(5) . . ? C39 C52 C61 116.2(5) . . ? C39 C52 C86 124.1(5) . . ? C61 C52 C86 119.4(5) . . ? N1 C53 C39 122.9(5) . . ? N1 C53 H53A 118.5 . . ? C39 C53 H53A 118.5 . . ? C62 C55 C45 120.5(5) . . ? C62 C55 H55A 119.8 . . ? C45 C55 H55A 119.8 . . ? C47 C56 C64 121.6(6) . 2_666 ? C47 C56 H56A 119.2 . . ? C64 C56 H56A 119.2 2_666 . ? C31 C57 C26 119.4(5) . 2_765 ? C31 C57 H57A 120.3 . . ? C26 C57 H57A 120.3 2_765 . ? N4 C58 C74 123.4(6) . . ? N4 C58 H58A 118.3 . . ? C74 C58 H58A 118.3 . . ? C1 C59 C3 118.7(5) . 2_676 ? C1 C59 C51 120.7(5) . . ? C3 C59 C51 120.6(5) 2_676 . ? C78 C60 C62 120.1(5) . . ? C78 C60 H60A 119.9 . . ? C62 C60 H60A 119.9 . . ? C42 C61 C52 120.1(5) . . ? C42 C61 H61A 120.0 . . ? C52 C61 H61A 120.0 . . ? C55 C62 C60 116.9(5) . . ? C55 C62 C63 122.3(5) . . ? C60 C62 C63 120.8(6) . . ? C62 C63 C81 111.1(5) . . ? C62 C63 H63A 109.4 . . ? C81 C63 H63A 109.4 . . ? C62 C63 H63B 109.4 . . ? C81 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C47 C64 C56 119.4(6) . 2_666 ? C47 C64 H64A 120.3 . . ? C56 C64 H64A 120.3 2_666 . ? N4 C70 C73 124.9(6) . . ? N4 C70 H70A 117.6 . . ? C73 C70 H70A 117.6 . . ? C72 C71 N3 122.6(6) . . ? C72 C71 H71A 118.7 . . ? N3 C71 H71A 118.7 . . ? C71 C72 C85 121.2(6) . . ? C71 C72 H72A 119.4 . . ? C85 C72 H72A 119.4 . . ? C84 C73 C70 119.6(6) . . ? C84 C73 H73A 120.2 . . ? C70 C73 H73A 120.2 . . ? C58 C74 C84 121.4(6) . . ? C58 C74 H74A 119.3 . . ? C84 C74 H74A 119.3 . . ? C84 C75 C77 111.1(5) . . ? C84 C75 H75A 109.4 . . ? C77 C75 H75A 109.4 . . ? C84 C75 H75B 109.4 . . ? C77 C75 H75B 109.4 . . ? H75A C75 H75B 108.0 . . ? C80 C77 C75 110.1(6) . . ? C80 C77 H77A 109.6 . . ? C75 C77 H77A 109.6 . . ? C80 C77 H77B 109.6 . . ? C75 C77 H77B 109.6 . . ? H77A C77 H77B 108.1 . . ? N2 C78 C60 123.4(5) . . ? N2 C78 H78A 118.3 . . ? C60 C78 H78A 118.3 . . ? C37 C79 C83 120.1(5) . . ? C37 C79 H79A 120.0 . . ? C83 C79 H79A 120.0 . . ? C77 C80 C85 117.1(5) . . ? C77 C80 H80A 108.0 . . ? C85 C80 H80A 108.0 . . ? C77 C80 H80B 108.0 . . ? C85 C80 H80B 108.0 . . ? H80A C80 H80B 107.3 . . ? C86 C81 C63 112.1(6) . . ? C86 C81 H81A 109.2 . . ? C63 C81 H81A 109.2 . . ? C86 C81 H81B 109.2 . . ? C63 C81 H81B 109.2 . . ? H81A C81 H81B 107.9 . . ? C85 C82 C87 119.9(5) . . ? C85 C82 H82A 120.0 . . ? C87 C82 H82A 120.0 . . ? C44 C83 C79 119.8(5) . . ? C44 C83 H83A 120.1 . . ? C79 C83 H83A 120.1 . . ? C73 C84 C74 115.9(5) . . ? C73 C84 C75 121.4(6) . . ? C74 C84 C75 122.5(6) . . ? C72 C85 C82 116.4(6) . . ? C72 C85 C80 118.7(5) . . ? C82 C85 C80 124.8(6) . . ? C52 C86 C81 117.4(5) . . ? C52 C86 H86A 108.0 . . ? C81 C86 H86A 108.0 . . ? C52 C86 H86B 108.0 . . ? C81 C86 H86B 108.0 . . ? H86A C86 H86B 107.2 . . ? N3 C87 C82 124.2(5) . . ? N3 C87 H87A 117.9 . . ? C82 C87 H87A 117.9 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.555 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.187