# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mattes, Benjamin' _publ_contact_author_email mattes@sfst.net _publ_author_name B.Mattes data_ZnTBC_C2c _database_code_depnum_ccdc_archive 'CCDC 865525' #TrackingRef '- ZnTBC_C2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnTBC _chemical_melting_point ? _chemical_formula_moiety 'C8 H4 N4 O2 Zn' _chemical_formula_sum 'C8 H4 N4 O2 Zn' _chemical_formula_weight 253.52 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 _symmetry_space_group_name_Hall '-C 2yc' 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 10.073(5) _cell_length_b 34.113(17) _cell_length_c 6.791(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.866(7) _cell_angle_gamma 90.00 _cell_volume 2134.0(19) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2176 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.04 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3944 _exptl_absorpt_correction_T_max 0.6578 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11014 _diffrn_reflns_av_R_equivalents 0.1776 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1874 _reflns_number_gt 1499 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT+ ' _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^)+(0.0486P)^2^+73.9532P] 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 1874 _refine_ls_number_parameters 134 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.1119 _refine_ls_wR_factor_ref 0.2429 _refine_ls_wR_factor_gt 0.2343 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_restrained_S_all 1.238 _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 1.32625(15) -0.62502(3) 1.03558(17) 0.0232(5) Uani 1 1 d . . . O1 O 1.3772(10) -0.5750(2) 1.1825(12) 0.0278(13) Uani 1 1 d . . . N1 N 1.5686(11) -0.3678(2) 1.1624(13) 0.0219(16) Uani 1 1 d U . . C1 C 1.5000 -0.5585(4) 1.2500 0.0212(19) Uani 1 2 d SU . . O2 O 1.3809(10) -0.6732(2) 1.1989(12) 0.0278(13) Uani 1 1 d . . . N2 N 1.5422(12) -0.3302(2) 1.1984(14) 0.0216(16) Uani 1 1 d U . . C2 C 1.5000 -0.5141(4) 1.2500 0.0211(17) Uani 1 2 d SU . . C3 C 1.3718(14) -0.4943(3) 1.1891(15) 0.0210(15) Uani 1 1 d U . . H3 H 1.2832 -0.5085 1.1447 0.025 Uiso 1 1 calc R . . N3 N 1.1157(13) -0.6193(3) 0.854(2) 0.054(3) Uani 1 1 d U . . C4 C 1.3696(14) -0.4537(3) 1.1913(15) 0.0211(14) Uani 1 1 d U . . H4 H 1.2807 -0.4399 1.1535 0.025 Uiso 1 1 calc R . . N4 N 1.0652(14) -0.5825(3) 0.819(2) 0.055(3) Uani 1 1 d U . . C5 C 1.5000 -0.4334(4) 1.2500 0.0206(16) Uani 1 2 d SU . . C6 C 1.5000 -0.3910(4) 1.2500 0.0211(19) Uani 1 2 d SU . . C7 C 1.5000 -0.6898(4) 1.2500 0.027(2) Uani 1 2 d SU . . C8 C 1.5000 -0.7338(4) 1.2500 0.028(2) Uani 1 2 d SU . . C9 C 1.6205(15) -0.7538(3) 1.2430(17) 0.0284(18) Uani 1 1 d U . . H9 H 1.7014 -0.7405 1.2437 0.034 Uiso 1 1 d . . . C10 C 1.6196(15) -0.7954(3) 1.2431(17) 0.0296(19) Uani 1 1 d U . . H10 H 1.6945 -0.8095 1.2360 0.036 Uiso 1 1 d . . . C12 C 1.0000 -0.6413(5) 0.7500 0.040(5) Uani 1 2 d S . . C11 C 1.5000 -0.8148(4) 1.2500 0.031(2) Uani 1 2 d SU . . 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 0.0435(9) 0.0074(6) 0.0156(6) -0.0013(4) 0.0088(6) -0.0064(6) O1 0.045(4) 0.012(2) 0.025(3) -0.004(2) 0.013(3) -0.004(3) N1 0.035(4) 0.010(3) 0.020(3) -0.002(2) 0.011(3) -0.004(3) C1 0.031(4) 0.022(4) 0.012(3) 0.000 0.010(3) 0.000 O2 0.045(4) 0.012(2) 0.025(3) -0.004(2) 0.013(3) -0.004(3) N2 0.035(4) 0.011(3) 0.020(3) -0.001(2) 0.012(3) -0.004(3) C2 0.031(4) 0.021(3) 0.012(3) 0.000 0.010(3) 0.000 C3 0.031(4) 0.021(3) 0.013(3) 0.0006(15) 0.011(3) -0.0001(15) N3 0.039(5) 0.011(3) 0.088(7) 0.006(4) 0.002(5) -0.002(4) C4 0.030(4) 0.022(3) 0.014(3) 0.0004(15) 0.011(3) 0.0007(15) N4 0.040(5) 0.011(3) 0.089(7) 0.006(4) 0.001(5) -0.002(4) C5 0.030(4) 0.022(3) 0.014(3) 0.000 0.013(3) 0.000 C6 0.030(4) 0.022(4) 0.015(3) 0.000 0.012(3) 0.000 C7 0.046(5) 0.010(4) 0.018(4) 0.000 0.006(4) 0.000 C8 0.046(5) 0.010(3) 0.018(3) 0.000 0.005(3) 0.000 C9 0.046(5) 0.011(3) 0.020(3) 0.0005(15) 0.004(3) -0.0006(16) C10 0.046(5) 0.012(3) 0.021(3) 0.0003(15) 0.003(3) -0.0005(16) C12 0.051(14) 0.008(7) 0.049(11) 0.000 0.008(10) 0.000 C11 0.047(5) 0.012(4) 0.022(3) 0.000 0.002(4) 0.000 _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 1.935(7) . ? Zn1 O1 1.939(7) . ? Zn1 N3 1.985(12) . ? Zn1 N1 2.035(9) 5_847 ? O1 C1 1.265(11) . ? N1 C6 1.338(12) . ? N1 N2 1.351(11) . ? N1 Zn1 2.035(9) 5_847 ? C1 O1 1.265(11) 2_857 ? C1 C2 1.51(2) . ? O2 C7 1.242(10) . ? N2 N2 1.302(19) 2_857 ? C2 C3 1.366(14) 2_857 ? C2 C3 1.366(14) . ? C3 C4 1.384(14) . ? C3 H3 0.9500 . ? N3 C12 1.325(14) . ? N3 N4 1.340(14) . ? C4 C5 1.393(14) . ? C4 H4 0.9500 . ? N4 N4 1.27(2) 2_756 ? C5 C4 1.393(14) 2_857 ? C5 C6 1.45(2) . ? C6 N1 1.338(12) 2_857 ? C7 O2 1.242(10) 2_857 ? C7 C8 1.502(19) . ? C8 C9 1.410(15) . ? C8 C9 1.410(15) 2_857 ? C9 C10 1.419(14) . ? C9 H9 0.9294 . ? C10 C11 1.392(15) . ? C10 H10 0.9134 . ? C12 N3 1.325(14) 2_756 ? C12 C11 1.50(2) 7_737 ? C11 C10 1.392(15) 2_857 ? C11 C12 1.50(2) 7_737 ? 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 O1 119.9(3) . . ? O2 Zn1 N3 115.1(4) . . ? O1 Zn1 N3 103.1(4) . . ? O2 Zn1 N1 100.0(3) . 5_847 ? O1 Zn1 N1 110.3(3) . 5_847 ? N3 Zn1 N1 108.3(5) . 5_847 ? C1 O1 Zn1 126.5(8) . . ? C6 N1 N2 107.8(9) . . ? C6 N1 Zn1 136.3(7) . 5_847 ? N2 N1 Zn1 115.3(6) . 5_847 ? O1 C1 O1 127.0(14) . 2_857 ? O1 C1 C2 116.5(7) . . ? O1 C1 C2 116.5(7) 2_857 . ? C7 O2 Zn1 124.4(8) . . ? N2 N2 N1 108.5(5) 2_857 . ? C3 C2 C3 120.6(14) 2_857 . ? C3 C2 C1 119.7(7) 2_857 . ? C3 C2 C1 119.7(7) . . ? C2 C3 C4 120.6(12) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C12 N3 N4 104.3(11) . . ? C12 N3 Zn1 139.8(9) . . ? N4 N3 Zn1 115.9(9) . . ? C3 C4 C5 118.8(12) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N4 N4 N3 109.7(7) 2_756 . ? C4 C5 C4 120.4(14) . 2_857 ? C4 C5 C6 119.8(7) . . ? C4 C5 C6 119.8(7) 2_857 . ? N1 C6 N1 107.5(13) 2_857 . ? N1 C6 C5 126.3(6) 2_857 . ? N1 C6 C5 126.3(6) . . ? O2 C7 O2 125.9(14) . 2_857 ? O2 C7 C8 117.0(7) . . ? O2 C7 C8 117.0(7) 2_857 . ? C9 C8 C9 122.2(14) . 2_857 ? C9 C8 C7 118.9(7) . . ? C9 C8 C7 118.9(7) 2_857 . ? C8 C9 C10 118.5(12) . . ? C8 C9 H9 122.0 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 118.8(13) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 121.6 . . ? N3 C12 N3 111.0(14) . 2_756 ? N3 C12 C11 124.5(7) . 7_737 ? N3 C12 C11 124.5(7) 2_756 7_737 ? C10 C11 C10 123.2(14) 2_857 . ? C10 C11 C12 118.4(7) 2_857 7_737 ? C10 C11 C12 118.4(7) . 7_737 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O1 C1 78.8(8) . . . . ? N3 Zn1 O1 C1 -151.7(8) . . . . ? N1 Zn1 O1 C1 -36.3(8) 5_847 . . . ? Zn1 O1 C1 O1 -31.2(5) . . . 2_857 ? Zn1 O1 C1 C2 148.8(5) . . . . ? O1 Zn1 O2 C7 -86.0(8) . . . . ? N3 Zn1 O2 C7 150.1(8) . . . . ? N1 Zn1 O2 C7 34.4(8) 5_847 . . . ? C6 N1 N2 N2 -1.0(13) . . . 2_857 ? Zn1 N1 N2 N2 171.3(9) 5_847 . . 2_857 ? O1 C1 C2 C3 -176.9(6) . . . 2_857 ? O1 C1 C2 C3 3.1(6) 2_857 . . 2_857 ? O1 C1 C2 C3 3.1(6) . . . . ? O1 C1 C2 C3 -176.9(6) 2_857 . . . ? C3 C2 C3 C4 -1.1(7) 2_857 . . . ? C1 C2 C3 C4 178.9(7) . . . . ? O2 Zn1 N3 C12 -28.5(17) . . . . ? O1 Zn1 N3 C12 -160.8(14) . . . . ? N1 Zn1 N3 C12 82.4(15) 5_847 . . . ? O2 Zn1 N3 N4 151.2(11) . . . . ? O1 Zn1 N3 N4 18.9(13) . . . . ? N1 Zn1 N3 N4 -97.9(12) 5_847 . . . ? C2 C3 C4 C5 2.1(13) . . . . ? C12 N3 N4 N4 -8(2) . . . 2_756 ? Zn1 N3 N4 N4 172.1(16) . . . 2_756 ? C3 C4 C5 C4 -1.0(6) . . . 2_857 ? C3 C4 C5 C6 179.0(6) . . . . ? N2 N1 C6 N1 0.4(5) . . . 2_857 ? Zn1 N1 C6 N1 -169.6(11) 5_847 . . 2_857 ? N2 N1 C6 C5 -179.6(5) . . . . ? Zn1 N1 C6 C5 10.4(11) 5_847 . . . ? C4 C5 C6 N1 47.8(7) . . . 2_857 ? C4 C5 C6 N1 -132.2(7) 2_857 . . 2_857 ? C4 C5 C6 N1 -132.2(7) . . . . ? C4 C5 C6 N1 47.8(7) 2_857 . . . ? Zn1 O2 C7 O2 36.2(4) . . . 2_857 ? Zn1 O2 C7 C8 -143.8(4) . . . . ? O2 C7 C8 C9 161.3(6) . . . . ? O2 C7 C8 C9 -18.7(6) 2_857 . . . ? O2 C7 C8 C9 -18.7(6) . . . 2_857 ? O2 C7 C8 C9 161.3(6) 2_857 . . 2_857 ? C9 C8 C9 C10 0.0(7) 2_857 . . . ? C7 C8 C9 C10 180.0(7) . . . . ? C8 C9 C10 C11 0.0(14) . . . . ? N4 N3 C12 N3 2.9(8) . . . 2_756 ? Zn1 N3 C12 N3 -177.3(19) . . . 2_756 ? N4 N3 C12 C11 -177.1(8) . . . 7_737 ? Zn1 N3 C12 C11 2.7(19) . . . 7_737 ? C9 C10 C11 C10 0.0(7) . . . 2_857 ? C9 C10 C11 C12 180.0(7) . . . 7_737 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.020 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.193 # 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 0.500 0.000 -0.003 277 111 ' ' 2 1.000 0.500 0.001 277 111 ' ' _platon_squeeze_details ; ; # Attachment '- ZnTBC_P-1.cif' data_ZnTBC _database_code_depnum_ccdc_archive 'CCDC 865526' #TrackingRef '- ZnTBC_P-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ZnTBC _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 N8 O6.3 Zn2' _chemical_formula_weight 543.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.791(3) _cell_length_b 9.604(4) _cell_length_c 17.722(10) _cell_angle_alpha 101.826(10) _cell_angle_beta 96.500(10) _cell_angle_gamma 106.425(7) _cell_volume 1066.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2176 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.04 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540.8 _exptl_absorpt_coefficient_mu 2.3 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11188 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3759 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1577P)^2^+14.8742P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3759 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.1051 _refine_ls_wR_factor_ref 0.2864 _refine_ls_wR_factor_gt 0.2687 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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 0.92349(19) 0.46284(14) 0.75074(7) 0.0179(5) Uani 1 1 d . . . Zn2 Zn 0.84143(19) 0.80966(14) 0.74932(7) 0.0178(5) Uani 1 1 d . . . C2 C 0.939(2) 0.1907(13) 0.8705(6) 0.026(3) Uani 1 1 d . . . C8 C 0.9391(17) 0.6922(13) 0.8807(7) 0.022(3) Uani 1 1 d . . . C5 C 0.9780(18) 0.7321(13) 0.9668(6) 0.020(2) Uani 1 1 d . . . C4 C 1.124(2) 0.8714(14) 1.0086(7) 0.028(3) Uani 1 1 d . . . H4 H 1.1913 0.9383 0.9815 0.033 Uiso 1 1 calc R . . C6 C 0.878(2) 0.6341(14) 1.0090(7) 0.027(3) Uani 1 1 d . . . H6 H 0.7818 0.5420 0.9821 0.032 Uiso 1 1 calc R . . C7 C 1.0807(19) 0.3276(13) 0.9095(7) 0.025(3) Uani 1 1 d . . . H7 H 1.1477 0.3935 0.8817 0.030 Uiso 1 1 calc R . . C3 C 0.834(2) 0.0914(13) 0.9101(7) 0.026(3) Uani 1 1 d . . . H3 H 0.7355 0.0008 0.8826 0.031 Uiso 1 1 calc R . . O1 O 0.9910(12) 0.7974(9) 0.8473(4) 0.0233(18) Uani 1 1 d . . . O2 O 0.8522(12) 0.5554(9) 0.8465(4) 0.0199(17) Uani 1 1 d . . . N1 N 0.884(2) 0.2450(11) 0.7385(6) 0.038(3) Uani 1 1 d . . . C1 C 0.892(2) 0.1502(14) 0.7830(7) 0.031(3) Uani 1 1 d . . . C16 C 0.8092(17) 0.5674(13) 0.6172(6) 0.020(2) Uani 1 1 d . . . C9 C 1.3634(16) 0.6178(12) 0.7180(6) 0.018(2) Uani 1 1 d . . . C12 C 0.6767(18) 0.3689(15) 0.4917(7) 0.026(3) Uani 1 1 d . . . H12 H 0.6464 0.2984 0.5212 0.032 Uiso 1 1 calc R . . C14 C 0.8129(17) 0.6244(14) 0.4867(6) 0.022(3) Uani 1 1 d . . . H14 H 0.8702 0.7255 0.5124 0.026 Uiso 1 1 calc R . . C11 C 0.6317(18) 0.3221(14) 0.4096(7) 0.026(3) Uani 1 1 d . . . H11 H 0.5700 0.2213 0.3841 0.031 Uiso 1 1 calc R . . C13 C 0.7650(16) 0.5179(13) 0.5288(6) 0.019(2) Uani 1 1 d . . . N5 N 1.2292(15) 0.5717(11) 0.7634(5) 0.024(2) Uani 1 1 d . . . O3 O 0.7715(12) 0.4651(9) 0.6517(5) 0.0244(18) Uani 1 1 d . . . O4 O 0.8781(13) 0.7061(9) 0.6488(5) 0.0269(19) Uani 1 1 d . . . N7 N 1.5175(15) 0.7224(12) 0.8394(5) 0.027(2) Uani 1 1 d . . . N6 N 1.3296(15) 0.6399(12) 0.8402(5) 0.025(2) Uani 1 1 d . . . O10 O 1.215(6) 0.936(4) 0.745(2) 0.243(15) Uiso 1 1 d . . . C21 C 0.7753(19) 0.5798(13) 0.4064(7) 0.026(3) Uiso 1 1 d . . . H21 H 0.8130 0.6509 0.3777 0.031 Uiso 1 1 calc R . . C20 C 0.6814(17) 0.4296(12) 0.3674(6) 0.018(2) Uiso 1 1 d . . . N2 N 0.835(2) 0.1644(16) 0.6654(9) 0.059(4) Uiso 1 1 d . . . N3 N 0.815(3) 0.0283(18) 0.6666(10) 0.068(4) Uiso 1 1 d . . . N8 N 1.5462(15) 0.7115(12) 0.7632(5) 0.025(2) Uani 1 1 d . . . N4 N 0.847(2) 0.0127(12) 0.7383(6) 0.041(3) Uani 1 1 d . . . O11 O 0.698(6) 0.958(4) 0.441(2) 0.15(2) Uiso 0.62(6) 1 d P . . O12 O 0.943(5) 0.986(3) 0.4779(17) 0.030(11) Uiso 0.28(3) 1 d P . . O13 O 0.819(5) 0.948(3) 0.3797(19) 0.066(14) Uiso 0.40(4) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0206(8) 0.0259(8) 0.0089(7) 0.0027(5) -0.0007(5) 0.0124(6) Zn2 0.0201(8) 0.0255(8) 0.0082(7) -0.0002(5) -0.0019(5) 0.0128(6) C2 0.048(8) 0.020(6) 0.010(6) -0.001(5) 0.003(5) 0.014(6) C8 0.011(5) 0.031(7) 0.026(6) 0.008(5) 0.001(5) 0.013(5) C5 0.025(6) 0.032(6) 0.005(5) -0.001(4) -0.004(4) 0.020(5) C4 0.036(7) 0.037(7) 0.014(6) 0.008(5) 0.003(5) 0.018(6) C6 0.038(7) 0.035(7) 0.014(6) 0.008(5) -0.001(5) 0.023(6) C7 0.028(7) 0.027(6) 0.017(6) 0.005(5) -0.003(5) 0.010(5) C3 0.040(7) 0.019(6) 0.015(6) 0.000(5) -0.005(5) 0.011(5) O1 0.022(4) 0.032(5) 0.013(4) 0.001(3) -0.002(3) 0.011(4) O2 0.020(4) 0.032(5) 0.009(4) 0.000(3) 0.001(3) 0.015(4) N1 0.082(9) 0.014(5) 0.011(5) -0.002(4) -0.003(5) 0.014(5) C1 0.055(9) 0.032(7) 0.003(5) -0.002(5) -0.001(5) 0.014(6) C16 0.013(5) 0.036(7) 0.017(6) 0.006(5) 0.004(4) 0.018(5) C9 0.009(5) 0.027(6) 0.014(5) 0.002(4) -0.005(4) 0.005(5) C12 0.019(6) 0.046(8) 0.016(6) 0.007(5) 0.001(5) 0.014(6) C14 0.020(6) 0.034(7) 0.012(5) -0.002(5) 0.001(4) 0.017(5) C11 0.019(6) 0.037(7) 0.017(6) -0.004(5) -0.001(5) 0.011(5) C13 0.012(5) 0.036(7) 0.013(6) -0.001(5) -0.001(4) 0.016(5) N5 0.022(5) 0.042(6) 0.011(5) 0.003(4) -0.002(4) 0.020(5) O3 0.022(4) 0.032(5) 0.017(4) 0.007(4) -0.003(3) 0.008(4) O4 0.037(5) 0.029(5) 0.017(4) 0.000(4) 0.007(4) 0.017(4) N7 0.019(5) 0.052(7) 0.012(5) 0.001(4) 0.004(4) 0.017(5) N6 0.025(6) 0.044(6) 0.005(4) 0.003(4) 0.000(4) 0.016(5) N8 0.025(5) 0.043(6) 0.013(5) 0.006(4) 0.006(4) 0.017(5) N4 0.080(9) 0.034(6) 0.012(5) 0.007(5) -0.007(5) 0.025(6) _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 1.928(7) . ? Zn1 O3 1.939(8) . ? Zn1 N1 1.995(10) . ? Zn1 N5 2.006(10) . ? Zn2 O4 1.934(8) . ? Zn2 O1 1.952(8) . ? Zn2 N4 1.990(11) 1_565 ? Zn2 N8 2.026(10) 1_455 ? C2 C7 1.377(17) . ? C2 C3 1.385(17) . ? C2 C1 1.491(15) . ? C8 O1 1.260(14) . ? C8 O2 1.264(14) . ? C8 C5 1.469(15) . ? C5 C6 1.395(18) . ? C5 C4 1.413(18) . ? C4 C3 1.386(16) 2_767 ? C6 C7 1.391(16) 2_767 ? C7 C6 1.391(16) 2_767 ? C3 C4 1.386(16) 2_767 ? N1 N2 1.318(18) . ? N1 C1 1.328(16) . ? C16 O3 1.243(14) . ? C16 O4 1.260(14) . ? C16 C13 1.511(15) . ? C9 N5 1.326(15) . ? C9 C20 1.457(15) 2_766 ? C12 C13 1.371(17) . ? C12 C11 1.402(16) . ? C14 C13 1.373(16) . ? C14 C21 1.371(16) . ? C11 C20 1.384(17) . ? N5 N6 1.386(13) . ? N7 N6 1.301(14) . ? C21 C20 1.392(16) . ? C20 C9 1.457(15) 2_766 ? N2 N3 1.28(2) . ? N8 C9 1.357(14) . ? N8 N7 1.374(13) . ? N8 Zn2 2.026(10) 1_655 ? N4 N3 1.310(19) . ? N4 C1 1.324(16) . ? N4 Zn2 1.990(11) 1_545 ? O11 O13 1.44(5) . ? O11 O12 1.64(5) . ? O12 O12 0.97(6) 2_776 ? O12 O13 1.76(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 N8 N7 105.8(9) . . ? C9 N8 Zn2 138.0(8) . 1_655 ? N7 N8 Zn2 115.5(7) . 1_655 ? N3 N4 C1 104.2(11) . . ? N3 N4 Zn2 116.6(10) . 1_545 ? C1 N4 Zn2 139.0(8) . 1_545 ? O2 Zn1 O3 118.5(3) . . ? O2 Zn1 N1 113.1(4) . . ? O3 Zn1 N1 102.4(4) . . ? O2 Zn1 N5 102.9(4) . . ? O3 Zn1 N5 111.2(4) . . ? N1 Zn1 N5 108.7(5) . . ? O4 Zn2 O1 121.3(3) . . ? O4 Zn2 N4 105.4(4) . 1_565 ? O1 Zn2 N4 117.2(4) . 1_565 ? O4 Zn2 N8 107.9(4) . 1_455 ? O1 Zn2 N8 98.6(4) . 1_455 ? N4 Zn2 N8 104.8(5) 1_565 1_455 ? C7 C2 C3 121.8(11) . . ? C7 C2 C1 119.1(11) . . ? C3 C2 C1 119.0(11) . . ? O1 C8 O2 125.6(11) . . ? O1 C8 C5 117.4(11) . . ? O2 C8 C5 117.0(10) . . ? C6 C5 C4 118.7(10) . . ? C6 C5 C8 121.6(11) . . ? C4 C5 C8 119.7(11) . . ? C3 C4 C5 120.2(11) 2_767 . ? C7 C6 C5 120.9(12) 2_767 . ? C2 C7 C6 119.0(12) . 2_767 ? C4 C3 C2 119.3(11) 2_767 . ? C8 O1 Zn2 125.9(7) . . ? C8 O2 Zn1 122.1(7) . . ? N2 N1 C1 106.2(10) . . ? N2 N1 Zn1 114.6(9) . . ? C1 N1 Zn1 139.2(8) . . ? N4 C1 N1 109.9(10) . . ? N4 C1 C2 124.7(11) . . ? N1 C1 C2 125.5(11) . . ? O3 C16 O4 126.4(11) . . ? O3 C16 C13 115.7(10) . . ? O4 C16 C13 117.9(10) . . ? N5 C9 N8 109.6(9) . . ? N5 C9 C20 124.1(10) . 2_766 ? N8 C9 C20 126.2(10) . 2_766 ? C13 C12 C11 120.4(12) . . ? C13 C14 C21 119.1(11) . . ? C20 C11 C12 118.4(11) . . ? C12 C13 C14 121.1(10) . . ? C12 C13 C16 120.0(11) . . ? C14 C13 C16 118.9(10) . . ? C9 N5 N6 106.8(9) . . ? C9 N5 Zn1 137.6(7) . . ? N6 N5 Zn1 114.7(7) . . ? C16 O3 Zn1 127.0(8) . . ? C16 O4 Zn2 127.6(7) . . ? N6 N7 N8 109.4(9) . . ? N7 N6 N5 108.3(9) . . ? C14 C21 C20 120.9(11) . . ? C11 C20 C21 120.1(11) . . ? C11 C20 C9 118.9(10) . 2_766 ? C21 C20 C9 121.0(10) . 2_766 ? N3 N2 N1 107.7(14) . . ? N2 N3 N4 112.0(15) . . ? O13 O11 O12 69(2) . . ? O12 O12 O11 152(5) 2_776 . ? O12 O12 O13 158(5) 2_776 . ? O11 O12 O13 49.8(18) . . ? O11 O13 O12 61(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 5.278 _refine_diff_density_min -1.770 _refine_diff_density_rms 0.247 _vrf_PLAT057_ALERT_3_A ; PROBLEM: Correction for Absorption Required RT(exp) ... 1.43 RESPONSE: no adsorption correction did ; _vrf_PLAT057_ALERT_2_A ; PROBLEM: Short Inter D...A Contact O11 .. O12 .. 1.64 Ang. RESPOMSE: O11 and O12 are disordered H2O guest inside the channels. ;