# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'En-Qing Gao' _publ_contact_author_name 'Dr En-Qing Gao' _publ_contact_author_email eqgao@chem.ecnu.edu.cn data_2 _database_code_depnum_ccdc_archive 'CCDC 798135' #TrackingRef '- 1-last.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H40 N2 O12 Zn3' _chemical_formula_weight 1153.03 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 trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 16.147(3) _cell_length_b 16.147(3) _cell_length_c 16.624(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3753.7(13) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 648 _cell_measurement_theta_min 2.522 _cell_measurement_theta_max 17.775 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8898 _exptl_absorpt_correction_T_max 0.9290 _exptl_absorpt_process_details SADABS _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 5812 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1431 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1643 _reflns_number_gt 736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0054P)^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 1643 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _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 1.0000 1.0000 1.0000 0.0429(4) Uani 1 6 d S . . Zn2 Zn 1.0000 1.0000 0.78749(5) 0.0683(3) Uani 1 3 d S . . C1 C 0.8738(3) 1.0251(3) 0.8794(3) 0.0601(13) Uani 1 1 d . . . C2 C 0.7796(3) 1.0167(3) 0.9013(3) 0.0666(13) Uani 1 1 d . A . C3 C 0.7739(3) 1.0703(3) 0.9623(3) 0.0923(16) Uani 1 1 d . . . H3A H 0.8288 1.1125 0.9904 0.111 Uiso 1 1 calc R A . C4 C 0.6981(3) 0.9545(3) 0.8616(3) 0.0825(16) Uani 1 1 d . . . H4A H 0.7011 0.9181 0.8195 0.099 Uiso 1 1 calc R A . C5 C 0.6879(3) 1.0623(3) 0.9826(3) 0.110(2) Uani 1 1 d . A . H5A H 0.6859 1.1015 1.0227 0.131 Uiso 1 1 calc R . . C6 C 0.6108(3) 0.9447(3) 0.8832(3) 0.0972(18) Uani 1 1 d . A . H6A H 0.5558 0.9019 0.8555 0.117 Uiso 1 1 calc R . . C7 C 0.6045(3) 0.9976(3) 0.9450(3) 0.0929(17) Uani 1 1 d . . . C8 C 0.5097(3) 0.9822(3) 0.9676(3) 0.113(2) Uani 1 1 d . . . H8A H 0.4589 0.9443 0.9337 0.135 Uiso 1 1 calc R . . N1 N 0.9631(10) 1.0089(15) 0.6671(6) 0.068(4) Uani 0.33 1 d P A -1 C9 C 0.905(4) 0.933(3) 0.627(3) 0.093(14) Uani 0.33 1 d P A -1 H9A H 0.8898 0.8741 0.6493 0.112 Uiso 0.33 1 calc PR A -1 C10 C 0.8662(16) 0.931(5) 0.5563(19) 0.171(16) Uani 0.33 1 d P A -1 H10A H 0.8205 0.8733 0.5341 0.205 Uiso 0.33 1 calc PR A -1 C11 C 0.894(5) 1.016(8) 0.515(3) 0.180(15) Uani 0.33 1 d P A -1 H11A H 0.8690 1.0180 0.4652 0.216 Uiso 0.33 1 calc PR A -1 C12 C 0.956(4) 1.093(3) 0.552(2) 0.140(10) Uani 0.33 1 d P A -1 H12A H 0.9775 1.1508 0.5250 0.167 Uiso 0.33 1 calc PR A -1 C13 C 1.000(4) 1.101(4) 0.637(4) 0.127(19) Uani 0.33 1 d P A -1 H13A H 1.0438 1.1567 0.6630 0.153 Uiso 0.33 1 calc PR A -1 O1 O 0.87916(19) 0.9937(2) 0.81092(18) 0.0732(9) Uani 1 1 d . A . O2 O 0.94088(16) 1.06315(15) 0.92892(16) 0.0594(8) Uani 1 1 d . A . 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 0.0325(4) 0.0325(4) 0.0638(9) 0.000 0.000 0.0162(2) Zn2 0.0701(4) 0.0701(4) 0.0647(8) 0.000 0.000 0.0350(2) C1 0.047(3) 0.040(3) 0.098(5) 0.013(3) -0.004(3) 0.025(2) C2 0.046(3) 0.051(3) 0.109(4) -0.018(3) -0.027(3) 0.029(3) C3 0.050(3) 0.096(4) 0.131(5) -0.050(3) -0.038(3) 0.037(3) C4 0.059(3) 0.072(3) 0.125(5) -0.042(3) -0.027(3) 0.040(3) C5 0.049(3) 0.117(4) 0.166(6) -0.083(4) -0.043(3) 0.043(3) C6 0.046(3) 0.089(4) 0.162(6) -0.057(4) -0.043(3) 0.038(3) C7 0.045(3) 0.090(4) 0.152(5) -0.060(3) -0.036(3) 0.040(3) C8 0.052(3) 0.112(4) 0.186(7) -0.080(4) -0.048(4) 0.050(3) N1 0.044(13) 0.061(10) 0.088(9) -0.006(11) -0.001(8) 0.018(10) C9 0.09(2) 0.09(4) 0.056(19) 0.02(2) 0.017(17) 0.01(2) C10 0.103(17) 0.33(5) 0.07(2) -0.02(3) -0.029(16) 0.10(3) C11 0.18(4) 0.33(6) 0.09(3) -0.04(4) -0.07(2) 0.18(4) C12 0.17(3) 0.13(2) 0.11(3) 0.04(2) 0.00(3) 0.07(2) C13 0.18(3) 0.11(2) 0.15(4) 0.05(3) 0.03(2) 0.11(2) O1 0.066(2) 0.085(2) 0.082(3) -0.0055(19) -0.0163(19) 0.0480(18) O2 0.0412(16) 0.0459(17) 0.096(2) 0.0038(16) -0.0166(16) 0.0252(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 2.079(2) 2_765 ? Zn1 O2 2.079(2) 11_567 ? Zn1 O2 2.079(2) 10_777 ? Zn1 O2 2.079(2) . ? Zn1 O2 2.079(2) 12_657 ? Zn1 O2 2.079(2) 3_675 ? Zn2 O1 1.942(3) 3_675 ? Zn2 O1 1.942(3) 2_765 ? Zn2 O1 1.942(3) . ? Zn2 N1 2.113(10) 2_765 ? Zn2 N1 2.113(10) . ? Zn2 N1 2.113(10) 3_675 ? C1 O2 1.250(4) . ? C1 O1 1.267(4) . ? C1 C2 1.504(5) . ? C2 C4 1.362(4) . ? C2 C3 1.366(5) . ? C3 C5 1.371(4) . ? C3 H3A 0.9300 . ? C4 C6 1.386(4) . ? C4 H4A 0.9300 . ? C5 C7 1.375(5) . ? C5 H5A 0.9300 . ? C6 C7 1.371(5) . ? C6 H6A 0.9300 . ? C7 C8 1.472(5) . ? C8 C8 1.329(7) 10_677 ? C8 H8A 0.9300 . ? N1 C9 1.30(6) . ? N1 C13 1.38(6) . ? C9 C10 1.32(6) . ? C9 H9A 0.9300 . ? C10 C11 1.39(7) . ? C10 H10A 0.9300 . ? C11 C12 1.30(7) . ? C11 H11A 0.9300 . ? C12 C13 1.55(7) . ? C12 H12A 0.9300 . ? C13 H13A 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 O2 Zn1 O2 180.000(1) 2_765 11_567 ? O2 Zn1 O2 89.12(10) 2_765 10_777 ? O2 Zn1 O2 90.88(10) 11_567 10_777 ? O2 Zn1 O2 90.88(10) 2_765 . ? O2 Zn1 O2 89.12(10) 11_567 . ? O2 Zn1 O2 180.000(1) 10_777 . ? O2 Zn1 O2 89.12(10) 2_765 12_657 ? O2 Zn1 O2 90.88(10) 11_567 12_657 ? O2 Zn1 O2 90.88(10) 10_777 12_657 ? O2 Zn1 O2 89.12(10) . 12_657 ? O2 Zn1 O2 90.88(10) 2_765 3_675 ? O2 Zn1 O2 89.12(10) 11_567 3_675 ? O2 Zn1 O2 89.12(10) 10_777 3_675 ? O2 Zn1 O2 90.88(10) . 3_675 ? O2 Zn1 O2 180.000(1) 12_657 3_675 ? O1 Zn2 O1 116.08(6) 3_675 2_765 ? O1 Zn2 O1 116.08(6) 3_675 . ? O1 Zn2 O1 116.08(6) 2_765 . ? O1 Zn2 N1 113.9(5) 3_675 2_765 ? O1 Zn2 N1 83.3(3) 2_765 2_765 ? O1 Zn2 N1 106.3(6) . 2_765 ? O1 Zn2 N1 106.3(6) 3_675 . ? O1 Zn2 N1 113.9(5) 2_765 . ? O1 Zn2 N1 83.3(3) . . ? N1 Zn2 N1 32.3(4) 2_765 . ? O1 Zn2 N1 83.3(3) 3_675 3_675 ? O1 Zn2 N1 106.3(6) 2_765 3_675 ? O1 Zn2 N1 113.9(5) . 3_675 ? N1 Zn2 N1 32.3(4) 2_765 3_675 ? N1 Zn2 N1 32.3(4) . 3_675 ? O2 C1 O1 125.0(4) . . ? O2 C1 C2 118.3(4) . . ? O1 C1 C2 116.7(4) . . ? C4 C2 C3 118.8(4) . . ? C4 C2 C1 120.7(4) . . ? C3 C2 C1 120.6(4) . . ? C2 C3 C5 120.6(4) . . ? C2 C3 H3A 119.7 . . ? C5 C3 H3A 119.7 . . ? C2 C4 C6 120.7(4) . . ? C2 C4 H4A 119.6 . . ? C6 C4 H4A 119.6 . . ? C3 C5 C7 121.3(4) . . ? C3 C5 H5A 119.3 . . ? C7 C5 H5A 119.3 . . ? C7 C6 C4 120.7(4) . . ? C7 C6 H6A 119.6 . . ? C4 C6 H6A 119.6 . . ? C6 C7 C5 117.8(4) . . ? C6 C7 C8 118.7(4) . . ? C5 C7 C8 123.5(4) . . ? C8 C8 C7 125.8(6) 10_677 . ? C8 C8 H8A 117.1 10_677 . ? C7 C8 H8A 117.1 . . ? C9 N1 C13 123(3) . . ? C9 N1 Zn2 121(2) . . ? C13 N1 Zn2 115(3) . . ? N1 C9 C10 126(4) . . ? N1 C9 H9A 117.1 . . ? C10 C9 H9A 117.1 . . ? C9 C10 C11 120(4) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 115(4) . . ? C12 C11 H11A 122.4 . . ? C10 C11 H11A 122.4 . . ? C11 C12 C13 127(4) . . ? C11 C12 H12A 116.3 . . ? C13 C12 H12A 116.3 . . ? N1 C13 C12 108(4) . . ? N1 C13 H13A 126.0 . . ? C12 C13 H13A 126.0 . . ? C1 O1 Zn2 115.3(3) . . ? C1 O2 Zn1 129.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C4 -161.9(4) . . . . ? O1 C1 C2 C4 18.9(6) . . . . ? O2 C1 C2 C3 17.0(6) . . . . ? O1 C1 C2 C3 -162.2(4) . . . . ? C4 C2 C3 C5 -0.7(7) . . . . ? C1 C2 C3 C5 -179.6(4) . . . . ? C3 C2 C4 C6 -0.8(7) . . . . ? C1 C2 C4 C6 178.2(4) . . . . ? C2 C3 C5 C7 3.0(8) . . . . ? C2 C4 C6 C7 0.1(7) . . . . ? C4 C6 C7 C5 2.1(7) . . . . ? C4 C6 C7 C8 -177.8(4) . . . . ? C3 C5 C7 C6 -3.6(8) . . . . ? C3 C5 C7 C8 176.3(5) . . . . ? C6 C7 C8 C8 170.3(7) . . . 10_677 ? C5 C7 C8 C8 -9.5(10) . . . 10_677 ? O1 Zn2 N1 C9 162(2) 3_675 . . . ? O1 Zn2 N1 C9 33(2) 2_765 . . . ? O1 Zn2 N1 C9 -82(2) . . . . ? N1 Zn2 N1 C9 53(3) 2_765 . . . ? N1 Zn2 N1 C9 116(3) 3_675 . . . ? O1 Zn2 N1 C13 -21(2) 3_675 . . . ? O1 Zn2 N1 C13 -150(2) 2_765 . . . ? O1 Zn2 N1 C13 94(2) . . . . ? N1 Zn2 N1 C13 -130(3) 2_765 . . . ? N1 Zn2 N1 C13 -67(3) 3_675 . . . ? C13 N1 C9 C10 -7(6) . . . . ? Zn2 N1 C9 C10 169(3) . . . . ? N1 C9 C10 C11 6(7) . . . . ? C9 C10 C11 C12 -2(7) . . . . ? C10 C11 C12 C13 -2(7) . . . . ? C9 N1 C13 C12 3(5) . . . . ? Zn2 N1 C13 C12 -174(2) . . . . ? C11 C12 C13 N1 2(6) . . . . ? O2 C1 O1 Zn2 3.9(5) . . . . ? C2 C1 O1 Zn2 -177.0(2) . . . . ? O1 Zn2 O1 C1 -47.4(3) 3_675 . . . ? O1 Zn2 O1 C1 94.2(3) 2_765 . . . ? N1 Zn2 O1 C1 -175.3(4) 2_765 . . . ? N1 Zn2 O1 C1 -152.4(7) . . . . ? N1 Zn2 O1 C1 -141.7(5) 3_675 . . . ? O1 C1 O2 Zn1 -72.9(5) . . . . ? C2 C1 O2 Zn1 108.0(4) . . . . ? O2 Zn1 O2 C1 16.5(4) 2_765 . . . ? O2 Zn1 O2 C1 -163.5(4) 11_567 . . . ? O2 Zn1 O2 C1 -71(100) 10_777 . . . ? O2 Zn1 O2 C1 -72.6(3) 12_657 . . . ? O2 Zn1 O2 C1 107.4(3) 3_675 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.660 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.048 # Attachment '- 2-last.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 798136' #TrackingRef '- 2-last.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H38 N2 O12 Zn3' _chemical_formula_weight 1151.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 16.117(3) _cell_length_b 16.117(3) _cell_length_c 18.073(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4065.7(17) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 839 _cell_measurement_theta_min 2.527 _cell_measurement_theta_max 19.500 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1758 _exptl_absorpt_coefficient_mu 1.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8743 _exptl_absorpt_correction_T_max 0.9469 _exptl_absorpt_process_details SADABS _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 6281 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1778 _reflns_number_gt 1122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker 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^)+(0.0488P)^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 1778 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.873 _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 1.0000 1.0000 1.0000 0.0484(3) Uani 1 6 d S . . Zn2 Zn 1.0000 1.0000 0.80710(3) 0.0575(2) Uani 1 3 d S . . O1 O 0.93818(15) 0.87784(15) 0.93357(11) 0.0641(6) Uani 1 1 d . . . O2 O 1.00365(17) 0.88256(16) 0.82454(12) 0.0713(6) Uani 1 1 d . . . C1 C 0.9741(2) 0.8469(2) 0.88773(18) 0.0602(8) Uani 1 1 d . . . C2 C 0.9824(3) 0.7628(2) 0.90805(17) 0.0695(10) Uani 1 1 d . . . C3 C 0.9377(4) 0.7098(3) 0.9698(2) 0.1073(15) Uani 1 1 d . . . H3A H 0.9012 0.7272 0.9989 0.129 Uiso 1 1 calc R . . C4 C 1.0366(3) 0.7351(3) 0.8670(2) 0.0896(12) Uani 1 1 d . . . H4A H 1.0674 0.7699 0.8248 0.108 Uiso 1 1 calc R . . C5 C 0.9454(4) 0.6326(3) 0.9895(2) 0.1251(18) Uani 1 1 d . . . H5A H 0.9130 0.5974 1.0312 0.150 Uiso 1 1 calc R . . C6 C 1.0467(4) 0.6590(3) 0.8858(2) 0.1069(15) Uani 1 1 d . . . H6A H 1.0843 0.6430 0.8568 0.128 Uiso 1 1 calc R . . C7 C 1.0012(4) 0.6052(3) 0.9482(2) 0.1025(15) Uani 1 1 d . . . C8 C 1.0141(4) 0.5251(3) 0.9692(2) 0.1170(16) Uani 1 1 d . . . H8A H 1.0460 0.5076 0.9353 0.140 Uiso 1 1 calc R . . N1 N 1.0000 1.0000 0.69414(18) 0.0767(15) Uani 1 3 d SG . . C9 C 0.9216(8) 0.9313(11) 0.6548(5) 0.085(4) Uani 0.33 1 d PG . . H9A H 0.8700 0.8822 0.6798 0.102 Uiso 0.33 1 calc PR . . C10 C 0.9202(10) 0.9361(12) 0.5780(4) 0.101(6) Uani 0.33 1 d PG . . H10A H 0.8677 0.8901 0.5517 0.122 Uiso 0.33 1 calc PR . . C11 C 0.9973(12) 1.0095(16) 0.54063(19) 0.107(5) Uani 0.33 1 d PG . . C12 C 1.0758(16) 1.078(2) 0.5800(5) 0.29(3) Uani 0.33 1 d PG . . H12A H 1.1274 1.1275 0.5550 0.349 Uiso 0.33 1 calc PR . . C13 C 1.0772(11) 1.0736(15) 0.6567(5) 0.155(9) Uani 0.33 1 d PG . . H13B H 1.1297 1.1196 0.6831 0.186 Uiso 0.33 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 0.0538(4) 0.0538(4) 0.0375(5) 0.000 0.000 0.02690(18) Zn2 0.0664(3) 0.0664(3) 0.0396(4) 0.000 0.000 0.03321(16) O1 0.0689(15) 0.0570(13) 0.0679(15) -0.0109(11) -0.0024(11) 0.0326(12) O2 0.0987(17) 0.0690(15) 0.0527(14) -0.0033(12) -0.0026(13) 0.0468(14) C1 0.066(2) 0.057(2) 0.057(2) -0.0097(17) -0.0114(17) 0.0297(17) C2 0.096(3) 0.069(2) 0.054(2) -0.0017(18) 0.0027(19) 0.049(2) C3 0.177(5) 0.107(3) 0.087(3) 0.027(3) 0.048(3) 0.108(3) C4 0.133(4) 0.095(3) 0.067(2) 0.014(2) 0.022(2) 0.077(3) C5 0.207(5) 0.123(4) 0.098(3) 0.043(3) 0.064(3) 0.122(4) C6 0.168(5) 0.119(3) 0.080(3) 0.023(3) 0.039(3) 0.106(4) C7 0.160(4) 0.101(3) 0.088(3) 0.012(2) 0.025(3) 0.097(3) C8 0.184(5) 0.112(4) 0.099(4) 0.019(3) 0.041(3) 0.108(4) N1 0.095(2) 0.095(2) 0.040(3) 0.000 0.000 0.0475(12) C9 0.089(10) 0.102(12) 0.034(7) -0.001(8) 0.003(7) 0.026(8) C10 0.075(9) 0.134(14) 0.033(7) -0.003(9) -0.019(7) 0.007(9) C11 0.134(19) 0.113(19) 0.061(6) -0.033(14) -0.051(18) 0.052(16) C12 0.105(16) 0.50(6) 0.088(15) -0.13(3) -0.017(12) 0.02(2) C13 0.135(19) 0.21(3) 0.063(10) 0.014(16) -0.025(12) 0.041(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.085(2) . ? Zn1 O1 2.085(2) 10_777 ? Zn1 O1 2.085(2) 3_675 ? Zn1 O1 2.085(2) 2_765 ? Zn1 O1 2.085(2) 12_657 ? Zn1 O1 2.085(2) 11_567 ? Zn2 O2 1.948(2) 2_765 ? Zn2 O2 1.948(2) . ? Zn2 O2 1.948(2) 3_675 ? Zn2 N1 2.042(3) 2_765 ? Zn2 N1 2.042(3) 3_675 ? Zn2 N1 2.042(3) . ? O1 C1 1.249(3) . ? O2 C1 1.260(4) . ? C1 C2 1.473(4) . ? C2 C3 1.370(5) . ? C2 C4 1.377(5) . ? C3 C5 1.358(5) . ? C3 H3A 0.9300 . ? C4 C6 1.359(5) . ? C4 H4A 0.9300 . ? C5 C7 1.399(5) . ? C5 H5A 0.9300 . ? C6 C7 1.388(5) . ? C6 H6A 0.9300 . ? C7 C8 1.456(5) . ? C8 C8 1.316(8) 10_767 ? C8 H8A 0.9300 . ? N1 C9 1.389(19) 3_675 ? N1 C9 1.39(2) 2_765 ? N1 C9 1.3888 . ? N1 C13 1.3912 . ? N1 C13 1.39(3) 2_765 ? N1 C13 1.39(3) 3_675 ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 H13B 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 O1 Zn1 O1 180.000(1) . 10_777 ? O1 Zn1 O1 90.16(8) . 3_675 ? O1 Zn1 O1 89.84(8) 10_777 3_675 ? O1 Zn1 O1 90.16(8) . 2_765 ? O1 Zn1 O1 89.84(8) 10_777 2_765 ? O1 Zn1 O1 90.16(8) 3_675 2_765 ? O1 Zn1 O1 89.84(8) . 12_657 ? O1 Zn1 O1 90.16(8) 10_777 12_657 ? O1 Zn1 O1 180.00(9) 3_675 12_657 ? O1 Zn1 O1 89.84(8) 2_765 12_657 ? O1 Zn1 O1 89.84(8) . 11_567 ? O1 Zn1 O1 90.16(8) 10_777 11_567 ? O1 Zn1 O1 89.84(8) 3_675 11_567 ? O1 Zn1 O1 180.0 2_765 11_567 ? O1 Zn1 O1 90.16(8) 12_657 11_567 ? O2 Zn2 O2 117.44(4) 2_765 . ? O2 Zn2 O2 117.44(4) 2_765 3_675 ? O2 Zn2 O2 117.44(4) . 3_675 ? O2 Zn2 N1 99.31(7) 2_765 2_765 ? O2 Zn2 N1 99.31(7) . 2_765 ? O2 Zn2 N1 99.31(7) 3_675 2_765 ? O2 Zn2 N1 99.31(7) 2_765 3_675 ? O2 Zn2 N1 99.31(7) . 3_675 ? O2 Zn2 N1 99.31(7) 3_675 3_675 ? N1 Zn2 N1 0.0 2_765 3_675 ? O2 Zn2 N1 99.31(7) 2_765 . ? O2 Zn2 N1 99.31(7) . . ? O2 Zn2 N1 99.31(7) 3_675 . ? N1 Zn2 N1 0.0 2_765 . ? N1 Zn2 N1 0.0 3_675 . ? C1 O1 Zn1 131.4(2) . . ? C1 O2 Zn2 113.7(2) . . ? O1 C1 O2 124.3(3) . . ? O1 C1 C2 118.4(3) . . ? O2 C1 C2 117.3(3) . . ? C3 C2 C4 117.2(3) . . ? C3 C2 C1 121.0(3) . . ? C4 C2 C1 121.8(3) . . ? C5 C3 C2 121.6(4) . . ? C5 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C6 C4 C2 122.6(4) . . ? C6 C4 H4A 118.7 . . ? C2 C4 H4A 118.7 . . ? C3 C5 C7 121.1(4) . . ? C3 C5 H5A 119.4 . . ? C7 C5 H5A 119.4 . . ? C4 C6 C7 120.2(4) . . ? C4 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C5 117.2(4) . . ? C6 C7 C8 120.1(4) . . ? C5 C7 C8 122.7(4) . . ? C8 C8 C7 127.4(5) 10_767 . ? C8 C8 H8A 116.3 10_767 . ? C7 C8 H8A 116.3 . . ? C9 N1 C9 96.13(5) 3_675 2_765 ? C9 N1 C9 96.1(19) 3_675 . ? C9 N1 C9 96(2) 2_765 . ? C9 N1 C13 48(2) 3_675 . ? C9 N1 C13 55(2) 2_765 . ? C9 N1 C13 120.0 . . ? C9 N1 C13 54.8(6) 3_675 2_765 ? C9 N1 C13 120.0(11) 2_765 2_765 ? C9 N1 C13 47.9(14) . 2_765 ? C13 N1 C13 98.4(16) . 2_765 ? C9 N1 C13 120.0(10) 3_675 3_675 ? C9 N1 C13 47.9(6) 2_765 3_675 ? C9 N1 C13 54.8(14) . 3_675 ? C13 N1 C13 98.4(17) . 3_675 ? C13 N1 C13 98.38(7) 2_765 3_675 ? C9 N1 Zn2 120.8(8) 3_675 . ? C9 N1 Zn2 120.8(8) 2_765 . ? C9 N1 Zn2 120.8(4) . . ? C13 N1 Zn2 119.1(4) . . ? C13 N1 Zn2 119.1(4) 2_765 . ? C13 N1 Zn2 119.1(3) 3_675 . ? C10 C9 N1 120.0 . . ? C10 C9 H9A 120.0 . . ? N1 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 N1 120.0 . . ? C12 C13 H13B 120.0 . . ? N1 C13 H13B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 O1 C1 63(100) 10_777 . . . ? O1 Zn1 O1 C1 107.7(2) 3_675 . . . ? O1 Zn1 O1 C1 17.5(3) 2_765 . . . ? O1 Zn1 O1 C1 -72.3(2) 12_657 . . . ? O1 Zn1 O1 C1 -162.5(3) 11_567 . . . ? O2 Zn2 O2 C1 95.7(2) 2_765 . . . ? O2 Zn2 O2 C1 -53.0(3) 3_675 . . . ? N1 Zn2 O2 C1 -158.6(2) 2_765 . . . ? N1 Zn2 O2 C1 -158.6(2) 3_675 . . . ? N1 Zn2 O2 C1 -158.6(2) . . . . ? Zn1 O1 C1 O2 -73.7(4) . . . . ? Zn1 O1 C1 C2 106.8(3) . . . . ? Zn2 O2 C1 O1 5.7(4) . . . . ? Zn2 O2 C1 C2 -174.7(2) . . . . ? O1 C1 C2 C3 10.9(5) . . . . ? O2 C1 C2 C3 -168.7(4) . . . . ? O1 C1 C2 C4 -167.8(3) . . . . ? O2 C1 C2 C4 12.6(5) . . . . ? C4 C2 C3 C5 -0.7(7) . . . . ? C1 C2 C3 C5 -179.4(4) . . . . ? C3 C2 C4 C6 -0.2(6) . . . . ? C1 C2 C4 C6 178.5(4) . . . . ? C2 C3 C5 C7 1.4(8) . . . . ? C2 C4 C6 C7 0.4(7) . . . . ? C4 C6 C7 C5 0.2(8) . . . . ? C4 C6 C7 C8 -178.5(5) . . . . ? C3 C5 C7 C6 -1.1(8) . . . . ? C3 C5 C7 C8 177.6(5) . . . . ? C6 C7 C8 C8 171.1(7) . . . 10_767 ? C5 C7 C8 C8 -7.5(11) . . . 10_767 ? O2 Zn2 N1 C9 -51.9(10) 2_765 . . 3_675 ? O2 Zn2 N1 C9 -171.9(10) . . . 3_675 ? O2 Zn2 N1 C9 68.1(10) 3_675 . . 3_675 ? N1 Zn2 N1 C9 0(100) 2_765 . . 3_675 ? N1 Zn2 N1 C9 0(100) 3_675 . . 3_675 ? O2 Zn2 N1 C9 68.1(10) 2_765 . . 2_765 ? O2 Zn2 N1 C9 -51.9(10) . . . 2_765 ? O2 Zn2 N1 C9 -171.9(10) 3_675 . . 2_765 ? N1 Zn2 N1 C9 0(96) 2_765 . . 2_765 ? N1 Zn2 N1 C9 0(96) 3_675 . . 2_765 ? O2 Zn2 N1 C9 -171.9(12) 2_765 . . . ? O2 Zn2 N1 C9 68.1(12) . . . . ? O2 Zn2 N1 C9 -51.9(12) 3_675 . . . ? N1 Zn2 N1 C9 0(96) 2_765 . . . ? N1 Zn2 N1 C9 0(96) 3_675 . . . ? O2 Zn2 N1 C13 3.9(17) 2_765 . . . ? O2 Zn2 N1 C13 -116.1(17) . . . . ? O2 Zn2 N1 C13 123.9(17) 3_675 . . . ? N1 Zn2 N1 C13 0(100) 2_765 . . . ? N1 Zn2 N1 C13 0(100) 3_675 . . . ? O2 Zn2 N1 C13 -116.1(6) 2_765 . . 2_765 ? O2 Zn2 N1 C13 123.9(6) . . . 2_765 ? O2 Zn2 N1 C13 3.9(6) 3_675 . . 2_765 ? N1 Zn2 N1 C13 0(100) 2_765 . . 2_765 ? N1 Zn2 N1 C13 0(100) 3_675 . . 2_765 ? O2 Zn2 N1 C13 123.9(5) 2_765 . . 3_675 ? O2 Zn2 N1 C13 3.9(5) . . . 3_675 ? O2 Zn2 N1 C13 -116.1(5) 3_675 . . 3_675 ? N1 Zn2 N1 C13 0(96) 2_765 . . 3_675 ? N1 Zn2 N1 C13 0(96) 3_675 . . 3_675 ? C9 N1 C9 C10 44.3(11) 3_675 . . . ? C9 N1 C9 C10 -52.6(11) 2_765 . . . ? C13 N1 C9 C10 0.0 . . . . ? C13 N1 C9 C10 72.9(14) 2_765 . . . ? C13 N1 C9 C10 -78.4(14) 3_675 . . . ? Zn2 N1 C9 C10 175.8(6) . . . . ? N1 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 N1 0.0 . . . . ? C9 N1 C13 C12 -69.2(12) 3_675 . . . ? C9 N1 C13 C12 75.1(13) 2_765 . . . ? C9 N1 C13 C12 0.0 . . . . ? C13 N1 C13 C12 -45.8(6) 2_765 . . . ? C13 N1 C13 C12 54.0(6) 3_675 . . . ? Zn2 N1 C13 C12 -175.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.601 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.063 # Attachment '- 3-last.cif' data_sq _database_code_depnum_ccdc_archive 'CCDC 798137' #TrackingRef '- 3-last.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 N2 O15 Zn3' _chemical_formula_weight 1233.11 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 trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 16.1001(6) _cell_length_b 16.1001(6) _cell_length_c 40.628(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9120.3(8) _cell_formula_units_Z 6 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4749 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7076 _exptl_absorpt_correction_T_max 0.7898 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42174 _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5962 _reflns_number_gt 2311 _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 bpea components of the structure exhibit symmetry imposed 3-fold disorder around the 32 symmetry site or a 3-fold axis, and the dataset collected is of limited quality and the bpea components could not be refined to have reasonable geometries without restraints. Thus, 10 distance restraints for the py-CH~2~CH~2~-py moieties were applied (5 DFIX instructions for bonds C27-C30, C30-C30_$17, C33-C36, C36-C37, C37-C40; 5 DANG instructions for 1,3-atom pairs: C30-C26, C30-C28, C36-C32, C36-C34, C37-C39). To prevent individual atoms from becoming 'non-positive-definite' , the ISOR instruction was applied to seven C atoms (42 restraints) of the disordered bpea molecules (C28, C30, C32, C34, C39, C40 and C42). ; _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^)+(0.0753P)^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 5962 _refine_ls_number_parameters 426 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.871 _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 0.0000 0.0000 0.5000 0.0336(3) Uani 1 6 d S . . Zn2 Zn 0.0000 0.0000 0.41315(2) 0.0438(3) Uani 1 3 d S . . Zn3 Zn 0.3333 0.6667 0.35584(2) 0.0364(2) Uani 1 3 d S . . Zn4 Zn 0.3333 0.6667 0.44259(2) 0.0439(3) Uani 1 3 d S . . Zn5 Zn 0.3333 0.6667 0.76927(2) 0.0439(3) Uani 1 3 d S . . O1 O 0.1224(2) 0.0626(2) 0.47063(7) 0.0481(8) Uani 1 1 d . . . O2 O 0.1161(2) -0.0054(2) 0.42258(7) 0.0526(9) Uani 1 1 d . . . O3 O 0.2167(2) 0.6711(2) 0.43367(7) 0.0526(9) Uani 1 1 d . . . O4 O 0.2115(2) 0.6040(2) 0.38531(7) 0.0507(8) Uani 1 1 d . . . O5 O -0.5446(2) 0.7289(2) 0.32690(8) 0.0537(9) Uani 1 1 d . . . O6 O -0.5475(2) 0.6666(3) 0.27778(8) 0.0641(11) Uani 1 1 d . . . C1 C 0.1523(3) 0.0253(3) 0.45081(11) 0.0401(12) Uani 1 1 d . . . C2 C 0.2362(4) 0.0172(3) 0.45952(11) 0.0432(12) Uani 1 1 d . . . C3 C 0.2565(4) -0.0452(4) 0.44314(12) 0.0588(15) Uani 1 1 d . . . H3A H 0.2170 -0.0815 0.4259 0.071 Uiso 1 1 calc R . . C4 C 0.2940(4) 0.0671(4) 0.48536(13) 0.0740(19) Uani 1 1 d . . . H4A H 0.2795 0.1072 0.4975 0.089 Uiso 1 1 calc R . . C5 C 0.3339(4) -0.0556(4) 0.45147(13) 0.0718(17) Uani 1 1 d . . . H5A H 0.3461 -0.0979 0.4397 0.086 Uiso 1 1 calc R . . C6 C 0.3717(4) 0.0601(5) 0.49388(14) 0.088(2) Uani 1 1 d . . . H6A H 0.4110 0.0982 0.5109 0.106 Uiso 1 1 calc R . . C7 C 0.3944(4) -0.0030(4) 0.47769(14) 0.0693(17) Uani 1 1 d . . . C8 C 0.4736(4) -0.0162(5) 0.48713(13) 0.0783(19) Uani 1 1 d . . . H8A H 0.4880 -0.0523 0.4728 0.094 Uiso 1 1 calc R . . C9 C 0.1809(4) 0.6407(3) 0.40539(12) 0.0467(13) Uani 1 1 d . . . C10 C 0.0973(3) 0.6499(4) 0.39612(12) 0.0463(13) Uani 1 1 d . . . C11 C 0.0700(4) 0.7036(4) 0.41497(13) 0.0702(17) Uani 1 1 d . . . H11A H 0.1040 0.7332 0.4340 0.084 Uiso 1 1 calc R . . C12 C 0.0463(4) 0.6068(5) 0.36827(15) 0.090(2) Uani 1 1 d . . . H12A H 0.0636 0.5698 0.3555 0.108 Uiso 1 1 calc R . . C13 C -0.0090(5) 0.7143(5) 0.40579(16) 0.093(2) Uani 1 1 d . . . H13A H -0.0267 0.7506 0.4187 0.112 Uiso 1 1 calc R . . C14 C -0.0294(5) 0.6168(6) 0.35884(16) 0.112(3) Uani 1 1 d . . . H14A H -0.0623 0.5874 0.3396 0.134 Uiso 1 1 calc R . . C15 C -0.0590(4) 0.6712(5) 0.37786(16) 0.083(2) Uani 1 1 d . . . C16 C -0.1403(5) 0.6839(5) 0.36908(16) 0.103(3) Uani 1 1 d . . . H16A H -0.1613 0.7112 0.3848 0.124 Uiso 1 1 calc R . . C17 C -0.1846(5) 0.6605(6) 0.34150(18) 0.133(3) Uani 1 1 d . . . H17A H -0.1638 0.6332 0.3257 0.159 Uiso 1 1 calc R . . C18 C -0.2665(5) 0.6735(6) 0.33292(15) 0.102(3) Uani 1 1 d . . . C19 C -0.3076(6) 0.6469(7) 0.30193(17) 0.158(4) Uani 1 1 d . . . H19A H -0.2802 0.6250 0.2865 0.190 Uiso 1 1 calc R . . C20 C -0.3041(5) 0.7134(6) 0.35346(16) 0.124(3) Uani 1 1 d . . . H20A H -0.2752 0.7367 0.3738 0.149 Uiso 1 1 calc R . . C21 C -0.3887(5) 0.6518(7) 0.29319(15) 0.129(3) Uani 1 1 d . . . H21A H -0.4177 0.6293 0.2728 0.154 Uiso 1 1 calc R . . C22 C -0.3841(5) 0.7202(5) 0.34506(14) 0.103(3) Uani 1 1 d . . . H22A H -0.4096 0.7452 0.3600 0.124 Uiso 1 1 calc R . . C23 C -0.4250(4) 0.6901(4) 0.31491(12) 0.0630(16) Uani 1 1 d . . . C24 C -0.5117(4) 0.6969(4) 0.30610(12) 0.0476(13) Uani 1 1 d . . . N1 N 0.0070(13) 0.0113(13) 0.36314(16) 0.089(6) Uani 0.33 1 d PG . . C25 C -0.0051(16) -0.0695(12) 0.3465(3) 0.080(8) Uani 0.33 1 d PG . . H25A H -0.0250 -0.1265 0.3579 0.096 Uiso 0.33 1 calc PR . . C26 C 0.012(2) -0.0651(13) 0.3129(3) 0.19(3) Uani 0.33 1 d PGD . . H26A H 0.0043 -0.1192 0.3018 0.226 Uiso 0.33 1 calc PR . . C27 C 0.042(2) 0.0200(15) 0.2959(2) 0.13(2) Uani 0.33 1 d PGD . . C28 C 0.0542(16) 0.1008(12) 0.3125(3) 0.169(18) Uani 0.33 1 d PGDU . . H28A H 0.0741 0.1578 0.3011 0.203 Uiso 0.33 1 calc PR . . C29 C 0.0367(13) 0.0965(11) 0.3461(3) 0.054(5) Uani 0.33 1 d PG . . H29A H 0.0448 0.1505 0.3572 0.065 Uiso 0.33 1 calc PR . . C30 C 0.0670(16) 0.0233(18) 0.2596(2) 0.164(13) Uani 0.33 1 d PDU . . H30A H 0.1361 0.0598 0.2569 0.197 Uiso 0.33 1 calc PR . . H30B H 0.0447 -0.0413 0.2517 0.197 Uiso 0.33 1 calc PR . . C36 C 0.284(2) 0.663(3) 0.5968(3) 0.34(4) Uani 0.33 1 d PD A -1 H36A H 0.2763 0.7167 0.6039 0.405 Uiso 0.33 1 calc PR A -1 H36B H 0.2274 0.6045 0.6036 0.405 Uiso 0.33 1 calc PR A -1 C37 C 0.3714(16) 0.670(3) 0.6135(3) 0.104(13) Uani 0.33 1 d PD A -1 H37A H 0.4281 0.7303 0.6079 0.125 Uiso 0.33 1 calc PR A -1 H37B H 0.3808 0.6180 0.6063 0.125 Uiso 0.33 1 calc PR A -1 N2 N 0.3333 0.6667 0.49285(13) 0.081(3) Uani 1 3 d SG A . C31 C 0.2828(13) 0.5800(3) 0.5095(2) 0.065(8) Uani 0.33 1 d PG . . H31A H 0.2628 0.5225 0.4984 0.078 Uiso 0.33 1 calc PR . . C32 C 0.2620(13) 0.5791(10) 0.5427(2) 0.086(8) Uani 0.33 1 d PGDU A . H32A H 0.2281 0.5211 0.5539 0.104 Uiso 0.33 1 calc PR . . C33 C 0.2918(15) 0.6649(14) 0.55935(16) 0.119(15) Uani 0.33 1 d PGD . . C34 C 0.342(2) 0.7516(11) 0.5427(3) 0.36(5) Uani 0.33 1 d PGDU A . H34A H 0.3623 0.8090 0.5538 0.432 Uiso 0.33 1 calc PR . . C35 C 0.3632(18) 0.7525(4) 0.5095(3) 0.128(13) Uani 0.33 1 d PG . . H35A H 0.3970 0.8105 0.4983 0.154 Uiso 0.33 1 calc PR A . N3 N 0.3333 0.6667 0.71890(13) 0.071(2) Uani 1 3 d SG A . C38 C 0.353(2) 0.7469(8) 0.7002(3) 0.157(16) Uani 0.33 1 d PG . . H38A H 0.3594 0.8014 0.7104 0.189 Uiso 0.33 1 calc PR . . C39 C 0.364(3) 0.7457(13) 0.6663(3) 0.135(13) Uani 0.33 1 d PGDU A . H39A H 0.3774 0.7994 0.6538 0.162 Uiso 0.33 1 calc PR . . C40 C 0.3549(19) 0.6642(14) 0.65107(15) 0.121(14) Uani 0.33 1 d PGDU . . C41 C 0.3349(18) 0.5840(11) 0.6697(2) 0.129(15) Uani 0.33 1 d PG A . H41A H 0.3288 0.5295 0.6595 0.154 Uiso 0.33 1 calc PR . . C42 C 0.3242(16) 0.5852(6) 0.7036(2) 0.056(5) Uani 0.33 1 d PGU . . H42B H 0.3108 0.5315 0.7161 0.067 Uiso 0.33 1 calc PR A . 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 0.0378(5) 0.0378(5) 0.0251(7) 0.000 0.000 0.0189(2) Zn2 0.0520(4) 0.0520(4) 0.0275(5) 0.000 0.000 0.0260(2) Zn3 0.0408(4) 0.0408(4) 0.0277(5) 0.000 0.000 0.02038(18) Zn4 0.0514(4) 0.0514(4) 0.0291(5) 0.000 0.000 0.0257(2) Zn5 0.0509(4) 0.0509(4) 0.0298(5) 0.000 0.000 0.0255(2) O1 0.0410(19) 0.052(2) 0.052(2) 0.0043(18) 0.0122(15) 0.0238(19) O2 0.055(2) 0.071(3) 0.040(2) 0.0019(18) 0.0055(17) 0.038(2) O3 0.048(2) 0.075(3) 0.040(2) 0.0010(18) 0.0039(17) 0.035(2) O4 0.044(2) 0.057(2) 0.052(2) 0.0020(18) 0.0104(16) 0.026(2) O5 0.043(2) 0.057(2) 0.056(2) 0.0064(18) 0.0131(16) 0.021(2) O6 0.061(3) 0.101(3) 0.043(2) -0.005(2) -0.0029(19) 0.051(2) C1 0.037(3) 0.049(3) 0.033(3) 0.007(2) 0.007(2) 0.020(3) C2 0.050(3) 0.044(3) 0.039(3) -0.004(2) 0.004(2) 0.026(3) C3 0.053(4) 0.078(4) 0.060(4) -0.019(3) -0.022(3) 0.044(3) C4 0.072(4) 0.122(6) 0.061(4) -0.033(4) -0.018(3) 0.074(4) C5 0.076(4) 0.094(5) 0.070(4) -0.024(4) -0.013(3) 0.061(4) C6 0.089(5) 0.128(6) 0.087(5) -0.061(4) -0.052(4) 0.084(5) C7 0.066(4) 0.099(5) 0.067(4) -0.030(3) -0.014(3) 0.060(4) C8 0.071(4) 0.125(5) 0.075(5) -0.039(4) -0.028(3) 0.076(4) C9 0.045(3) 0.044(3) 0.044(3) 0.010(3) 0.012(3) 0.017(3) C10 0.045(3) 0.054(4) 0.048(3) -0.004(3) 0.002(3) 0.032(3) C11 0.075(4) 0.081(5) 0.064(4) -0.017(3) -0.012(3) 0.047(4) C12 0.088(5) 0.135(6) 0.086(5) -0.047(4) -0.020(4) 0.086(5) C13 0.098(6) 0.132(7) 0.099(5) -0.027(5) -0.021(4) 0.094(5) C14 0.103(6) 0.187(8) 0.095(5) -0.071(5) -0.050(4) 0.110(6) C15 0.069(5) 0.126(6) 0.079(5) -0.025(4) -0.016(4) 0.068(5) C16 0.110(6) 0.165(7) 0.081(5) -0.034(5) -0.027(4) 0.104(6) C17 0.128(7) 0.258(11) 0.090(5) -0.057(6) -0.030(5) 0.154(8) C18 0.110(6) 0.187(8) 0.063(4) -0.020(5) -0.011(4) 0.115(6) C19 0.169(8) 0.351(13) 0.072(5) -0.083(6) -0.039(5) 0.218(10) C20 0.102(6) 0.251(10) 0.071(5) -0.059(5) -0.029(4) 0.127(7) C21 0.134(7) 0.274(11) 0.062(4) -0.071(5) -0.039(4) 0.166(8) C22 0.091(5) 0.199(8) 0.070(4) -0.054(5) -0.036(4) 0.112(6) C23 0.062(4) 0.097(5) 0.043(3) -0.004(3) -0.003(3) 0.050(4) C24 0.039(3) 0.061(4) 0.042(3) 0.010(3) 0.011(3) 0.025(3) N1 0.14(2) 0.035(11) 0.041(7) -0.012(10) -0.048(19) 0.001(17) C25 0.099(19) 0.12(2) 0.065(14) 0.023(14) 0.044(15) 0.08(2) C26 0.40(7) 0.15(3) 0.11(3) 0.01(3) 0.09(4) 0.20(5) C27 0.15(4) 0.18(5) 0.070(14) 0.01(4) 0.019(15) 0.09(4) C28 0.39(5) 0.26(4) 0.016(13) -0.011(17) -0.02(2) 0.29(4) C29 0.078(15) 0.059(14) 0.027(9) 0.017(8) 0.004(8) 0.035(12) C30 0.24(2) 0.20(2) 0.030(13) -0.016(15) 0.012(12) 0.09(2) C36 0.44(11) 0.55(10) 0.10(2) 0.19(5) 0.05(4) 0.30(9) C37 0.08(2) 0.15(2) 0.062(14) 0.04(2) 0.029(12) 0.04(2) N2 0.103(5) 0.103(5) 0.036(5) 0.000 0.000 0.051(2) C31 0.14(3) 0.068(13) 0.010(8) 0.014(8) 0.024(15) 0.073(19) C32 0.076(13) 0.091(15) 0.024(11) 0.011(10) 0.006(10) -0.010(10) C33 0.19(4) 0.16(3) 0.047(11) -0.03(2) 0.011(16) 0.11(3) C34 0.56(9) 0.36(8) 0.14(4) -0.06(4) 0.06(6) 0.21(6) C35 0.23(3) 0.078(16) 0.031(12) -0.004(11) -0.04(2) 0.04(3) N3 0.093(4) 0.093(4) 0.027(4) 0.000 0.000 0.046(2) C38 0.28(4) 0.26(4) 0.070(16) 0.08(2) 0.09(2) 0.24(4) C39 0.22(4) 0.08(2) 0.09(2) 0.021(17) -0.02(3) 0.07(2) C40 0.22(4) 0.15(3) 0.054(10) 0.02(4) 0.01(3) 0.14(3) C41 0.22(3) 0.11(2) 0.015(11) 0.016(11) 0.014(17) 0.05(2) C42 0.080(11) 0.069(12) 0.009(7) 0.004(7) -0.007(8) 0.030(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.083(3) 3 ? Zn1 O1 2.083(3) 9_556 ? Zn1 O1 2.083(3) 8_556 ? Zn1 O1 2.083(3) . ? Zn1 O1 2.083(3) 7_556 ? Zn1 O1 2.083(3) 2 ? Zn2 O2 1.951(3) 3 ? Zn2 O2 1.951(3) . ? Zn2 O2 1.951(3) 2 ? Zn2 N1 2.038(7) 2 ? Zn2 N1 2.038(7) 3 ? Zn2 N1 2.038(7) . ? Zn3 O5 2.068(3) 2_675 ? Zn3 O5 2.068(3) 3_455 ? Zn3 O5 2.068(3) 1_655 ? Zn3 O4 2.079(3) 3_565 ? Zn3 O4 2.079(3) . ? Zn3 O4 2.079(3) 2_665 ? Zn4 O3 1.948(3) . ? Zn4 O3 1.948(3) 3_565 ? Zn4 O3 1.948(3) 2_665 ? Zn4 N2 2.042(5) . ? Zn4 N2 2.042(5) 3_565 ? Zn4 N2 2.042(5) 2_665 ? Zn5 O6 1.951(3) 11_456 ? Zn5 O6 1.951(3) 12_676 ? Zn5 O6 1.951(3) 10_656 ? Zn5 N3 2.046(6) . ? O1 C1 1.236(5) . ? O2 C1 1.269(5) . ? O3 C9 1.269(5) . ? O4 C9 1.244(5) . ? O5 C24 1.238(5) . ? O5 Zn3 2.068(3) 1_455 ? O6 C24 1.270(5) . ? O6 Zn5 1.951(3) 10_565 ? C1 C2 1.465(6) . ? C2 C4 1.366(6) . ? C2 C3 1.374(6) . ? C3 C5 1.380(7) . ? C4 C6 1.355(6) . ? C5 C7 1.406(7) . ? C6 C7 1.404(7) . ? C7 C8 1.446(6) . ? C8 C8 1.282(9) 7_656 ? C9 C10 1.475(6) . ? C10 C12 1.367(6) . ? C10 C11 1.381(6) . ? C11 C13 1.416(7) . ? C12 C14 1.362(7) . ? C13 C15 1.363(7) . ? C14 C15 1.418(7) . ? C15 C16 1.466(7) . ? C16 C17 1.280(8) . ? C17 C18 1.477(8) . ? C18 C20 1.364(7) . ? C18 C19 1.387(8) . ? C19 C21 1.392(8) . ? C20 C22 1.389(7) . ? C21 C23 1.365(7) . ? C22 C23 1.360(6) . ? C23 C24 1.497(7) . ? N1 C25 1.3900 . ? N1 C29 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C27 C30 1.520(11) . ? C28 C29 1.3900 . ? C30 C30 1.449(19) 4 ? C36 C37 1.516(19) . ? C36 C33 1.525(11) . ? C37 C40 1.543(13) . ? N2 C31 1.3900 . ? N2 C35 1.3901 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? N3 C38 1.3900 . ? N3 C42 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 180.00(18) 3 9_556 ? O1 Zn1 O1 89.55(12) 3 8_556 ? O1 Zn1 O1 90.45(12) 9_556 8_556 ? O1 Zn1 O1 90.45(12) 3 . ? O1 Zn1 O1 89.55(12) 9_556 . ? O1 Zn1 O1 89.55(12) 8_556 . ? O1 Zn1 O1 89.55(12) 3 7_556 ? O1 Zn1 O1 90.45(12) 9_556 7_556 ? O1 Zn1 O1 90.45(12) 8_556 7_556 ? O1 Zn1 O1 180.00(13) . 7_556 ? O1 Zn1 O1 90.45(12) 3 2 ? O1 Zn1 O1 89.55(12) 9_556 2 ? O1 Zn1 O1 180.00(13) 8_556 2 ? O1 Zn1 O1 90.45(12) . 2 ? O1 Zn1 O1 89.55(12) 7_556 2 ? O2 Zn2 O2 116.24(6) 3 . ? O2 Zn2 O2 116.24(6) 3 2 ? O2 Zn2 O2 116.24(6) . 2 ? O2 Zn2 N1 97.7(5) 3 2 ? O2 Zn2 N1 105.4(5) . 2 ? O2 Zn2 N1 100.8(5) 2 2 ? O2 Zn2 N1 100.8(5) 3 3 ? O2 Zn2 N1 97.7(5) . 3 ? O2 Zn2 N1 105.4(5) 2 3 ? N1 Zn2 N1 7.7(9) 2 3 ? O2 Zn2 N1 105.4(6) 3 . ? O2 Zn2 N1 100.8(5) . . ? O2 Zn2 N1 97.7(5) 2 . ? N1 Zn2 N1 7.7(9) 2 . ? N1 Zn2 N1 7.7(9) 3 . ? O5 Zn3 O5 90.87(13) 2_675 3_455 ? O5 Zn3 O5 90.87(13) 2_675 1_655 ? O5 Zn3 O5 90.87(13) 3_455 1_655 ? O5 Zn3 O4 89.32(13) 2_675 3_565 ? O5 Zn3 O4 179.41(14) 3_455 3_565 ? O5 Zn3 O4 89.67(13) 1_655 3_565 ? O5 Zn3 O4 89.67(13) 2_675 . ? O5 Zn3 O4 89.32(13) 3_455 . ? O5 Zn3 O4 179.41(14) 1_655 . ? O4 Zn3 O4 90.13(12) 3_565 . ? O5 Zn3 O4 179.41(13) 2_675 2_665 ? O5 Zn3 O4 89.67(13) 3_455 2_665 ? O5 Zn3 O4 89.32(13) 1_655 2_665 ? O4 Zn3 O4 90.13(12) 3_565 2_665 ? O4 Zn3 O4 90.13(12) . 2_665 ? O3 Zn4 O3 116.62(6) . 3_565 ? O3 Zn4 O3 116.62(6) . 2_665 ? O3 Zn4 O3 116.62(6) 3_565 2_665 ? O3 Zn4 N2 100.72(9) . . ? O3 Zn4 N2 100.72(9) 3_565 . ? O3 Zn4 N2 100.72(9) 2_665 . ? O3 Zn4 N2 100.72(9) . 3_565 ? O3 Zn4 N2 100.72(9) 3_565 3_565 ? O3 Zn4 N2 100.72(9) 2_665 3_565 ? N2 Zn4 N2 0.0 . 3_565 ? O3 Zn4 N2 100.72(9) . 2_665 ? O3 Zn4 N2 100.72(9) 3_565 2_665 ? O3 Zn4 N2 100.72(9) 2_665 2_665 ? N2 Zn4 N2 0.0 . 2_665 ? N2 Zn4 N2 0.0 3_565 2_665 ? O6 Zn5 O6 116.92(6) 11_456 12_676 ? O6 Zn5 O6 116.92(6) 11_456 10_656 ? O6 Zn5 O6 116.92(6) 12_676 10_656 ? O6 Zn5 N3 100.22(10) 11_456 . ? O6 Zn5 N3 100.22(10) 12_676 . ? O6 Zn5 N3 100.22(10) 10_656 . ? C1 O1 Zn1 130.0(3) . . ? C1 O2 Zn2 115.1(3) . . ? C9 O3 Zn4 114.5(3) . . ? C9 O4 Zn3 130.5(3) . . ? C24 O5 Zn3 133.4(3) . 1_455 ? C24 O6 Zn5 114.7(3) . 10_565 ? O1 C1 O2 124.3(5) . . ? O1 C1 C2 119.1(4) . . ? O2 C1 C2 116.6(4) . . ? C4 C2 C3 117.5(5) . . ? C4 C2 C1 121.4(4) . . ? C3 C2 C1 121.1(4) . . ? C2 C3 C5 122.0(5) . . ? C6 C4 C2 122.2(5) . . ? C3 C5 C7 120.5(5) . . ? C4 C6 C7 121.7(5) . . ? C6 C7 C5 116.0(5) . . ? C6 C7 C8 123.4(5) . . ? C5 C7 C8 120.6(5) . . ? C8 C8 C7 127.7(7) 7_656 . ? O4 C9 O3 124.5(5) . . ? O4 C9 C10 118.6(5) . . ? O3 C9 C10 117.0(5) . . ? C12 C10 C11 118.6(5) . . ? C12 C10 C9 120.5(5) . . ? C11 C10 C9 120.9(5) . . ? C10 C11 C13 121.1(5) . . ? C14 C12 C10 121.3(5) . . ? C15 C13 C11 119.7(6) . . ? C12 C14 C15 121.1(6) . . ? C13 C15 C14 118.2(6) . . ? C13 C15 C16 118.2(6) . . ? C14 C15 C16 123.5(6) . . ? C17 C16 C15 125.3(7) . . ? C16 C17 C18 124.8(7) . . ? C20 C18 C19 116.5(6) . . ? C20 C18 C17 124.0(6) . . ? C19 C18 C17 119.4(6) . . ? C18 C19 C21 121.9(6) . . ? C18 C20 C22 122.2(6) . . ? C23 C21 C19 119.1(6) . . ? C23 C22 C20 119.7(6) . . ? C22 C23 C21 120.2(6) . . ? C22 C23 C24 119.5(5) . . ? C21 C23 C24 120.3(5) . . ? O5 C24 O6 124.9(5) . . ? O5 C24 C23 118.4(5) . . ? O6 C24 C23 116.7(5) . . ? C25 N1 C29 120.0 . . ? C25 N1 Zn2 115.2(8) . . ? C29 N1 Zn2 124.1(8) . . ? N1 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 C30 118.1(10) . . ? C28 C27 C30 121.8(10) . . ? C27 C28 C29 120.0 . . ? C28 C29 N1 120.0 . . ? C30 C30 C27 110.8(15) 4 . ? C37 C36 C33 112.4(19) . . ? C36 C37 C40 108.3(14) . . ? C31 N2 C35 120.0 . . ? C31 N2 Zn4 119.1(4) . . ? C35 N2 Zn4 119.0(5) . . ? C32 C31 N2 120.0 . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 C36 118.9(11) . . ? C34 C33 C36 120.2(11) . . ? C35 C34 C33 120.0 . . ? C34 C35 N2 120.0 . . ? C38 N3 C42 120.0 . . ? C38 N3 Zn5 123.0(4) . . ? C42 N3 Zn5 116.5(4) . . ? N3 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 C37 123.3(16) . . ? C39 C40 C37 116.7(16) . . ? C42 C41 C40 120.0 . . ? C41 C42 N3 120.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.378 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.062 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.673 0.250 184 46 ' ' 2 0.000 0.327 0.750 184 47 ' ' 3 0.099 0.461 0.091 24 2 ' ' 4 0.099 0.638 0.591 24 2 ' ' 5 0.327 0.327 0.250 184 47 ' ' 6 0.327 1.000 0.750 184 46 ' ' 7 0.362 0.901 0.091 24 2 ' ' 8 0.362 0.461 0.591 24 2 ' ' 9 0.461 0.099 0.409 24 3 ' ' 10 0.461 0.362 0.909 24 3 ' ' 11 0.539 0.638 0.091 24 2 ' ' 12 0.673 1.000 0.250 184 46 ' ' 13 0.539 0.901 0.591 24 2 ' ' 14 0.673 0.673 0.750 184 47 ' ' 15 0.638 0.539 0.409 24 3 ' ' 16 0.638 0.099 0.909 24 3 ' ' 17 0.901 0.362 0.409 24 3 ' ' 18 0.901 0.539 0.909 24 3 ' ' _platon_squeeze_details ; ;