# 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 _publ_contact_author_name 'Kitagawa, Susumu' _publ_contact_author_email kitagawa@icems.kyoto-u.ac.jp _publ_section_title ; Control of the charge-transfer interaction between a flexible porous host and aromatic guests by framework isomerism ; loop_ _publ_author_name Y.Takashima S.Furukawa S.Kitagawa # END of CIF # Attachment '- Framework2_782567.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-05-07 at 18:52:46 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : cid #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_cid _database_code_depnum_ccdc_archive 'CCDC 782567' #TrackingRef '- Framework2_782567.cif' _audit_creation_date 2010-05-07T18:52:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Zn_NDI_CID ; _chemical_formula_sum 'C30 H14 N4 O8 S Zn' _chemical_formula_weight 655.93 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.373(6) _cell_length_b 11.875(7) _cell_length_c 15.088(9) _cell_angle_alpha 93.108(7) _cell_angle_beta 104.184(5) _cell_angle_gamma 105.905(6) _cell_volume 1718.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.82 _exptl_absorpt_correction_T_min 0.7184 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 93(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type Saturn724+ _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_radiation_monochromator confocal _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_unetI/netI 0.1156 _diffrn_reflns_number 19158 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.81 _diffrn_reflns_theta_full 27.81 _diffrn_measured_fraction_theta_full 0.95 _diffrn_measured_fraction_theta_max 0.95 _reflns_number_total 7742 _reflns_number_gt 5156 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 diffused electron densities resulting from residual solvent molecules were removed from the data set using the SQUEEZE routine of PLATON and refined further using the data generated. ; _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^)+(0.1177P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7742 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.2074 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.326 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.175 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn01 Zn 0.56708(5) 0.39462(5) 0.43062(3) 0.01951(18) Uani 1 1 d . . . S1 S 0.97271(12) 0.61771(10) 0.57350(8) 0.0219(3) Uani 1 1 d . . . O6 O 0.7257(4) -0.0159(3) 0.7022(2) 0.0313(8) Uani 1 1 d . . . O5 O 0.3562(4) 0.0878(3) 0.7494(3) 0.0358(9) Uani 1 1 d . . . O3 O 0.6645(3) 0.5370(3) 0.5276(2) 0.0296(8) Uani 1 1 d . . . O2 O 0.6413(3) 0.1822(3) 0.3526(2) 0.0299(8) Uani 1 1 d . . . O1 O 0.7399(3) 0.3731(3) 0.4070(2) 0.0274(7) Uani 1 1 d . . . O4 O 0.3596(3) 0.3140(3) 0.3877(2) 0.0239(7) Uani 1 1 d . . . O8 O 0.6884(4) 0.6119(4) 0.0514(3) 0.0430(10) Uani 1 1 d . . . N2 N 0.5503(4) 0.0448(3) 0.7339(3) 0.0243(9) Uani 1 1 d . . . N1 N 0.5641(4) 0.2759(4) 0.5337(3) 0.0239(9) Uani 1 1 d . . . C5 C 0.8651(4) 0.6916(4) 0.6034(3) 0.0202(9) Uani 1 1 d . . . O7 O 0.3301(4) 0.7304(4) 0.1057(3) 0.0434(10) Uani 1 1 d . . . C4 C 0.9372(5) 0.8034(4) 0.6468(3) 0.0275(11) Uani 1 1 d . . . H2 H 0.8949 0.8574 0.6676 0.033 Uiso 1 1 calc R . . N4 N 0.5402(4) 0.4993(4) 0.3177(3) 0.0269(9) Uani 1 1 d . . . C9 C 0.5605(5) 0.1267(4) 0.6659(3) 0.0242(10) Uani 1 1 d . . . C26 C 0.5308(5) 0.6217(4) 0.1674(3) 0.0272(11) Uani 1 1 d . . . N3 N 0.5204(5) 0.6823(4) 0.0851(3) 0.0303(10) Uani 1 1 d . . . C20 C 0.5238(5) 0.8176(4) -0.0619(3) 0.0267(11) Uani 1 1 d . . . C14 C 0.5292(5) 0.8899(5) -0.1324(3) 0.0263(10) Uani 1 1 d . . . C3 C 1.0817(5) 0.8293(5) 0.6572(3) 0.0278(11) Uani 1 1 d . . . H1 H 1.1475 0.9028 0.686 0.033 Uiso 1 1 calc R . . C28 C 0.4265(6) 0.4731(5) 0.2486(3) 0.0326(12) Uani 1 1 d . . . H12 H 0.3476 0.4123 0.2528 0.039 Uiso 1 1 calc R . . C19 C 0.4182(5) 0.8087(5) -0.0165(3) 0.0296(11) Uani 1 1 d . . . C21 C 0.6192(5) 0.7534(5) -0.0405(3) 0.0293(11) Uani 1 1 d . . . C29 C 0.6492(5) 0.5926(5) 0.3142(3) 0.0299(11) Uani 1 1 d . . . H13 H 0.7308 0.6164 0.3645 0.036 Uiso 1 1 calc R . . C11 C 0.6557(5) 0.3065(5) 0.6177(4) 0.0339(12) Uani 1 1 d . . . H6 H 0.7226 0.3824 0.6312 0.041 Uiso 1 1 calc R . . C12 C 0.4380(5) 0.0325(4) 0.7728(3) 0.0285(11) Uani 1 1 d . . . C15 C 0.6318(5) 0.8967(4) -0.1803(3) 0.0260(10) Uani 1 1 d . . . C18 C 0.3244(6) 0.8705(5) -0.0387(3) 0.0309(11) Uani 1 1 d . . . H8 H 0.2558 0.8653 -0.0061 0.037 Uiso 1 1 calc R . . C10 C 0.6567(6) 0.2327(5) 0.6850(4) 0.0370(13) Uani 1 1 d . . . H5 H 0.7237 0.2563 0.7433 0.044 Uiso 1 1 calc R . . C24 C 0.4169(6) 0.7379(5) 0.0623(3) 0.0312(11) Uani 1 1 d . . . C23 C 0.7263(6) 0.8343(5) -0.1569(3) 0.0312(11) Uani 1 1 d . . . H10 H 0.7965 0.8402 -0.1882 0.037 Uiso 1 1 calc R . . C17 C 0.3291(5) 0.9417(5) -0.1095(3) 0.0304(11) Uani 1 1 d . . . H7 H 0.2626 0.9837 -0.1255 0.037 Uiso 1 1 calc R . . C27 C 0.4155(6) 0.5288(5) 0.1707(3) 0.0344(12) Uani 1 1 d . . . H11 H 0.3331 0.5051 0.1211 0.041 Uiso 1 1 calc R . . C25 C 0.6154(6) 0.6760(5) 0.0344(4) 0.0323(12) Uani 1 1 d . . . C22 C 0.7188(5) 0.7619(5) -0.0867(3) 0.0317(11) Uani 1 1 d . . . H9 H 0.7837 0.7184 -0.071 0.038 Uiso 1 1 calc R . . C16 C 0.6417(5) -0.0245(4) 0.7471(3) 0.0278(11) Uani 1 1 d . . . C2 C 0.8833(5) 0.2629(4) 0.3786(3) 0.0221(10) Uani 1 1 d . . . C13 C 0.4290(5) 0.9511(4) -0.1558(3) 0.0272(11) Uani 1 1 d . . . C6 C 0.7122(5) 0.6328(4) 0.5783(3) 0.0205(9) Uani 1 1 d . . . C30 C 0.6425(6) 0.6529(5) 0.2385(4) 0.0357(13) Uani 1 1 d . . . H14 H 0.7194 0.7179 0.2375 0.043 Uiso 1 1 calc R . . C8 C 0.4662(6) 0.0897(5) 0.5798(3) 0.0353(13) Uani 1 1 d . . . H4 H 0.3995 0.0137 0.5653 0.042 Uiso 1 1 calc R . . C1 C 0.7412(5) 0.2711(4) 0.3786(3) 0.0214(9) Uani 1 1 d . . . C7 C 0.4744(6) 0.1697(4) 0.5155(3) 0.0335(12) Uani 1 1 d . . . H3 H 0.4119 0.1462 0.4556 0.04 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 Zn01 0.0160(3) 0.0215(3) 0.0228(3) 0.0051(2) 0.0069(2) 0.0067(2) S1 0.0174(5) 0.0204(6) 0.0285(6) -0.0007(5) 0.0078(4) 0.0058(5) O6 0.035(2) 0.033(2) 0.0290(18) 0.0114(16) 0.0117(16) 0.0107(17) O5 0.039(2) 0.028(2) 0.040(2) 0.0108(17) 0.0078(17) 0.0100(17) O3 0.0253(18) 0.0232(19) 0.0338(18) -0.0007(15) 0.0040(15) 0.0013(15) O2 0.0189(17) 0.034(2) 0.0346(19) 0.0002(16) 0.0059(14) 0.0064(15) O1 0.0206(17) 0.0248(19) 0.0412(19) 0.0066(15) 0.0148(15) 0.0078(14) O4 0.0180(16) 0.0278(19) 0.0307(17) 0.0089(14) 0.0098(13) 0.0105(14) O8 0.058(3) 0.050(3) 0.039(2) 0.026(2) 0.022(2) 0.033(2) N2 0.023(2) 0.018(2) 0.0253(19) 0.0057(16) 0.0021(16) -0.0004(17) N1 0.022(2) 0.026(2) 0.025(2) 0.0077(17) 0.0074(16) 0.0080(17) C5 0.014(2) 0.024(3) 0.025(2) 0.0020(19) 0.0075(17) 0.0084(19) O7 0.047(2) 0.057(3) 0.035(2) 0.0200(19) 0.0198(18) 0.020(2) C4 0.019(2) 0.028(3) 0.037(3) 0.001(2) 0.008(2) 0.010(2) N4 0.022(2) 0.035(2) 0.0246(19) 0.0084(18) 0.0080(16) 0.0081(18) C9 0.017(2) 0.033(3) 0.021(2) 0.000(2) 0.0050(18) 0.007(2) C26 0.039(3) 0.020(3) 0.026(2) 0.007(2) 0.014(2) 0.009(2) N3 0.037(2) 0.030(2) 0.026(2) 0.0095(18) 0.0118(18) 0.009(2) C20 0.029(3) 0.026(3) 0.027(2) 0.009(2) 0.007(2) 0.011(2) C14 0.025(2) 0.029(3) 0.025(2) 0.005(2) 0.0080(19) 0.008(2) C3 0.020(2) 0.026(3) 0.036(3) 0.002(2) 0.008(2) 0.004(2) C28 0.031(3) 0.035(3) 0.031(3) 0.013(2) 0.005(2) 0.011(2) C19 0.033(3) 0.030(3) 0.025(2) 0.009(2) 0.008(2) 0.007(2) C21 0.034(3) 0.026(3) 0.025(2) 0.004(2) 0.005(2) 0.006(2) C29 0.024(3) 0.030(3) 0.030(3) 0.007(2) 0.005(2) 0.001(2) C11 0.030(3) 0.026(3) 0.035(3) 0.008(2) 0.003(2) -0.005(2) C12 0.033(3) 0.020(3) 0.028(2) 0.004(2) 0.005(2) 0.004(2) C15 0.028(3) 0.026(3) 0.019(2) 0.0022(19) 0.0033(19) 0.004(2) C18 0.034(3) 0.037(3) 0.024(2) 0.007(2) 0.008(2) 0.013(2) C10 0.041(3) 0.030(3) 0.028(3) 0.007(2) 0.001(2) -0.002(2) C24 0.035(3) 0.032(3) 0.023(2) 0.006(2) 0.004(2) 0.007(2) C23 0.034(3) 0.032(3) 0.030(3) 0.005(2) 0.009(2) 0.014(2) C17 0.031(3) 0.026(3) 0.034(3) 0.006(2) 0.009(2) 0.006(2) C27 0.039(3) 0.032(3) 0.024(2) 0.004(2) 0.000(2) 0.004(2) C25 0.036(3) 0.030(3) 0.031(3) 0.008(2) 0.010(2) 0.010(2) C22 0.031(3) 0.034(3) 0.031(3) 0.010(2) 0.009(2) 0.010(2) C16 0.031(3) 0.024(3) 0.024(2) 0.003(2) 0.006(2) 0.004(2) C2 0.017(2) 0.023(3) 0.023(2) 0.0029(19) 0.0025(17) 0.0041(19) C13 0.026(2) 0.025(3) 0.023(2) 0.002(2) 0.0008(19) 0.001(2) C6 0.021(2) 0.021(3) 0.022(2) 0.0079(19) 0.0076(18) 0.008(2) C30 0.045(3) 0.038(3) 0.035(3) 0.018(2) 0.018(2) 0.020(3) C8 0.043(3) 0.020(3) 0.031(3) 0.005(2) -0.003(2) -0.001(2) C1 0.019(2) 0.028(3) 0.019(2) 0.0036(19) 0.0054(17) 0.008(2) C7 0.044(3) 0.020(3) 0.026(2) 0.004(2) -0.001(2) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn01 O1 1.989(3) . ? Zn01 O4 2.022(3) . ? Zn01 O3 2.022(4) . ? Zn01 N1 2.155(4) . ? Zn01 N4 2.170(4) . ? S1 C5 1.720(4) . ? S1 C2 1.721(5) 2_766 ? O6 C16 1.215(6) . ? O5 C12 1.208(6) . ? O3 C6 1.239(6) . ? O2 C1 1.224(6) . ? O1 C1 1.268(6) . ? O4 C6 1.275(5) 2_666 ? O8 C25 1.209(6) . ? N2 C16 1.404(6) . ? N2 C12 1.405(6) . ? N2 C9 1.454(6) . ? N1 C7 1.314(6) . ? N1 C11 1.346(6) . ? C5 C4 1.369(7) . ? C5 C6 1.488(6) . ? O7 C24 1.225(6) . ? C4 C3 1.411(6) . ? C4 H2 0.95 . ? N4 C28 1.318(6) . ? N4 C29 1.363(6) . ? C9 C10 1.340(7) . ? C9 C8 1.385(7) . ? C26 C30 1.320(8) . ? C26 C27 1.400(7) . ? C26 N3 1.465(6) . ? N3 C24 1.393(7) . ? N3 C25 1.402(7) . ? C20 C21 1.396(7) . ? C20 C14 1.404(6) . ? C20 C19 1.411(7) . ? C14 C13 1.412(7) . ? C14 C15 1.414(7) . ? C3 C2 1.369(7) 2_766 ? C3 H1 0.95 . ? C28 C27 1.375(7) . ? C28 H12 0.95 . ? C19 C18 1.363(7) . ? C19 C24 1.493(6) . ? C21 C22 1.365(7) . ? C21 C25 1.496(7) . ? C29 C30 1.378(7) . ? C29 H13 0.95 . ? C11 C10 1.376(7) . ? C11 H6 0.95 . ? C12 C13 1.489(7) 1_546 ? C15 C23 1.376(7) . ? C15 C16 1.482(6) 1_564 ? C18 C17 1.399(7) . ? C18 H8 0.95 . ? C10 H5 0.95 . ? C23 C22 1.404(7) . ? C23 H10 0.95 . ? C17 C13 1.369(7) . ? C17 H7 0.95 . ? C27 H11 0.95 . ? C22 H9 0.95 . ? C16 C15 1.482(6) 1_546 ? C2 C3 1.369(7) 2_766 ? C2 C1 1.504(6) . ? C2 S1 1.721(5) 2_766 ? C13 C12 1.489(7) 1_564 ? C6 O4 1.275(5) 2_666 ? C30 H14 0.95 . ? C8 C7 1.396(7) . ? C8 H4 0.95 . ? C7 H3 0.95 . ? 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 Zn01 O4 138.12(15) . . ? O1 Zn01 O3 95.74(15) . . ? O4 Zn01 O3 126.10(13) . . ? O1 Zn01 N1 93.33(14) . . ? O4 Zn01 N1 84.53(14) . . ? O3 Zn01 N1 91.85(15) . . ? O1 Zn01 N4 91.53(14) . . ? O4 Zn01 N4 87.59(14) . . ? O3 Zn01 N4 94.01(16) . . ? N1 Zn01 N4 171.97(16) . . ? C5 S1 C2 91.2(2) . 2_766 ? C6 O3 Zn01 170.4(3) . . ? C1 O1 Zn01 119.5(3) . . ? C6 O4 Zn01 113.9(3) 2_666 . ? C16 N2 C12 125.4(4) . . ? C16 N2 C9 118.0(4) . . ? C12 N2 C9 116.2(4) . . ? C7 N1 C11 117.8(4) . . ? C7 N1 Zn01 120.8(3) . . ? C11 N1 Zn01 121.4(3) . . ? C4 C5 C6 128.4(4) . . ? C4 C5 S1 112.1(3) . . ? C6 C5 S1 119.5(3) . . ? C5 C4 C3 112.3(4) . . ? C5 C4 H2 123.8 . . ? C3 C4 H2 123.8 . . ? C28 N4 C29 117.6(4) . . ? C28 N4 Zn01 123.4(3) . . ? C29 N4 Zn01 118.8(3) . . ? C10 C9 C8 121.3(5) . . ? C10 C9 N2 121.9(4) . . ? C8 C9 N2 116.8(4) . . ? C30 C26 C27 119.4(5) . . ? C30 C26 N3 122.7(5) . . ? C27 C26 N3 118.0(4) . . ? C24 N3 C25 125.5(4) . . ? C24 N3 C26 118.5(4) . . ? C25 N3 C26 116.0(4) . . ? C21 C20 C14 119.6(4) . . ? C21 C20 C19 121.6(4) . . ? C14 C20 C19 118.8(4) . . ? C20 C14 C13 119.2(4) . . ? C20 C14 C15 119.3(4) . . ? C13 C14 C15 121.5(4) . . ? C2 C3 C4 112.6(5) 2_766 . ? C2 C3 H1 123.7 2_766 . ? C4 C3 H1 123.7 . . ? N4 C28 C27 123.8(5) . . ? N4 C28 H12 118.1 . . ? C27 C28 H12 118.1 . . ? C18 C19 C20 121.1(4) . . ? C18 C19 C24 119.6(5) . . ? C20 C19 C24 119.1(5) . . ? C22 C21 C20 120.4(4) . . ? C22 C21 C25 119.1(5) . . ? C20 C21 C25 120.5(5) . . ? N4 C29 C30 120.7(5) . . ? N4 C29 H13 119.6 . . ? C30 C29 H13 119.6 . . ? N1 C11 C10 122.9(5) . . ? N1 C11 H6 118.5 . . ? C10 C11 H6 118.5 . . ? O5 C12 N2 120.3(4) . . ? O5 C12 C13 123.2(5) . 1_546 ? N2 C12 C13 116.4(4) . 1_546 ? C23 C15 C14 120.0(4) . . ? C23 C15 C16 119.9(4) . 1_564 ? C14 C15 C16 120.0(4) . 1_564 ? C19 C18 C17 120.0(5) . . ? C19 C18 H8 120 . . ? C17 C18 H8 120 . . ? C9 C10 C11 118.1(5) . . ? C9 C10 H5 121 . . ? C11 C10 H5 121 . . ? O7 C24 N3 121.5(4) . . ? O7 C24 C19 121.6(5) . . ? N3 C24 C19 116.9(4) . . ? C15 C23 C22 119.8(5) . . ? C15 C23 H10 120.1 . . ? C22 C23 H10 120.1 . . ? C13 C17 C18 120.3(5) . . ? C13 C17 H7 119.8 . . ? C18 C17 H7 119.8 . . ? C28 C27 C26 117.3(5) . . ? C28 C27 H11 121.3 . . ? C26 C27 H11 121.3 . . ? O8 C25 N3 121.1(5) . . ? O8 C25 C21 123.4(5) . . ? N3 C25 C21 115.5(4) . . ? C21 C22 C23 120.7(5) . . ? C21 C22 H9 119.6 . . ? C23 C22 H9 119.6 . . ? O6 C16 N2 120.3(4) . . ? O6 C16 C15 123.4(5) . 1_546 ? N2 C16 C15 116.3(4) . 1_546 ? C3 C2 C1 128.7(4) 2_766 . ? C3 C2 S1 111.8(4) 2_766 2_766 ? C1 C2 S1 119.5(4) . 2_766 ? C17 C13 C14 120.6(4) . . ? C17 C13 C12 119.8(5) . 1_564 ? C14 C13 C12 119.6(4) . 1_564 ? O3 C6 O4 125.0(4) . 2_666 ? O3 C6 C5 118.7(4) . . ? O4 C6 C5 116.3(4) 2_666 . ? C26 C30 C29 121.0(5) . . ? C26 C30 H14 119.5 . . ? C29 C30 H14 119.5 . . ? C9 C8 C7 116.5(5) . . ? C9 C8 H4 121.7 . . ? C7 C8 H4 121.7 . . ? O2 C1 O1 127.1(4) . . ? O2 C1 C2 118.8(4) . . ? O1 C1 C2 114.2(4) . . ? N1 C7 C8 123.3(5) . . ? N1 C7 H3 118.3 . . ? C8 C7 H3 118.3 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # 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 0.017 0.003 567 126 ' ' _platon_squeeze_details ; ; # END of CIF _chemical_name_common Zn_NDI_CID # Attachment '- Framework1_782568.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-05-10 at 20:39:54 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : zn_s_ndi_nocid absorb #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_zn_s_ndi_nocid _database_code_depnum_ccdc_archive 'CCDC 782568' #TrackingRef '- Framework1_782568.cif' _audit_creation_date 2010-05-10T20:39:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C30 H14 N4 O8 S Zn' _chemical_formula_weight 655.88 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.615(5) _cell_length_b 16.644(5) _cell_length_c 19.660(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 91.890(5) _cell_angle_gamma 90.000(5) _cell_volume 5761(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 0.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_T_min 0.7975 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type Saturn724+ _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_radiation_monochromator confocal _diffrn_reflns_av_R_equivalents 0.1213 _diffrn_reflns_av_unetI/netI 0.102 _diffrn_reflns_number 60561 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.83 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 13398 _reflns_number_gt 7775 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 diffused electron densities resulting from residual solvent molecules were removed from the data set using the SQUEEZE routine of PLATON and refined further using the data generated. ; _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^)+(0.0935P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13398 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 0.88 _refine_ls_restrained_S_all 0.88 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.91 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.060721(19) 0.10596(2) 0.489980(15) 0.03820(12) Uani 1 1 d . . . S1 S 0.30547(5) 0.28426(5) 0.48659(4) 0.0490(2) Uani 1 1 d . . . O3 O 0.10250(13) -0.00675(14) 0.48907(11) 0.0509(5) Uani 1 1 d . . . O4 O -0.05201(11) 0.12495(13) 0.48626(10) 0.0443(5) Uani 1 1 d . . . O1 O 0.19344(18) 0.15273(19) 0.48820(13) 0.0734(8) Uani 1 1 d . . . C5 C 0.18325(17) -0.11567(18) 0.50340(14) 0.0385(6) Uani 1 1 d . . . O5 O 0.08395(18) -0.03403(17) 0.16839(12) 0.0747(8) Uani 1 1 d . . . O7 O 0.11211(18) -0.03178(18) 0.81332(12) 0.0771(8) Uani 1 1 d . . . O2 O 0.09132(16) 0.22616(17) 0.49181(12) 0.0682(8) Uani 1 1 d . . . N4 N 0.06878(16) 0.09881(16) 0.59876(13) 0.0480(6) Uani 1 1 d . . . N2 N 0.07558(19) 0.10078(18) 0.16828(13) 0.0574(8) Uani 1 1 d . . . N1 N 0.06355(15) 0.10083(16) 0.38133(12) 0.0436(6) Uani 1 1 d . . . N3 N 0.08769(19) 0.10062(19) 0.81231(13) 0.0596(8) Uani 1 1 d . . . O6 O 0.0711(2) 0.23510(19) 0.16847(13) 0.0983(11) Uani 1 1 d . . . C13 C 0.0923(2) 0.0291(2) 0.06121(15) 0.0550(9) Uani 1 1 d . . . C1 C 0.1612(2) 0.2186(3) 0.49092(15) 0.0592(10) Uani 1 1 d . . . C8 C 0.1324(2) 0.0764(3) 0.28106(16) 0.0618(10) Uani 1 1 d . . . H4 H 0.1775 0.0595 0.2612 0.074 Uiso 1 1 calc R . . C12 C 0.0854(2) 0.0276(2) 0.13607(16) 0.0575(9) Uani 1 1 d . . . C27 C 0.1443(2) 0.0860(3) 0.70090(18) 0.0737(12) Uani 1 1 d . . . H11 H 0.1923 0.078 0.7221 0.088 Uiso 1 1 calc R . . C26 C 0.0822(2) 0.0984(2) 0.73809(15) 0.0578(10) Uani 1 1 d . . . C3 C 0.1880(2) 0.3686(2) 0.50246(18) 0.0590(9) Uani 1 1 d . . . H1 H 0.1373 0.3845 0.5071 0.071 Uiso 1 1 calc R . . C9 C 0.0713(2) 0.1008(2) 0.24154(15) 0.0547(9) Uani 1 1 d . . . O8 O 0.0734(2) 0.23326(18) 0.81112(13) 0.0948(11) Uani 1 1 d . . . C19 C 0.0996(2) 0.0294(2) 0.92047(15) 0.0561(9) Uani 1 1 d . . . C7 C 0.1261(2) 0.0770(2) 0.35054(15) 0.0541(9) Uani 1 1 d . . . H3 H 0.1679 0.0598 0.3777 0.065 Uiso 1 1 calc R . . C16 C 0.0749(3) 0.1745(3) 0.13589(18) 0.0717(11) Uani 1 1 d . . . C10 C 0.0070(2) 0.1265(3) 0.27122(16) 0.0611(10) Uani 1 1 d . . . H5 H -0.0347 0.145 0.2446 0.073 Uiso 1 1 calc R . . C4 C 0.25086(19) -0.0781(2) 0.49552(17) 0.0543(8) Uani 1 1 d . . . H2 H 0.2559 -0.0224 0.4894 0.065 Uiso 1 1 calc R . . C21 C 0.0828(3) 0.1737(3) 0.91921(17) 0.0674(11) Uani 1 1 d . . . C14 C 0.0872(2) 0.1009(2) 0.02647(15) 0.0542(9) Uani 1 1 d . . . C24 C 0.1012(2) 0.0279(3) 0.84528(15) 0.0568(9) Uani 1 1 d . . . C30 C 0.0136(2) 0.1083(3) 0.70748(17) 0.0720(12) Uani 1 1 d . . . H14 H -0.03 0.1145 0.7333 0.086 Uiso 1 1 calc R . . C18 C 0.1062(2) -0.0403(3) 0.95564(16) 0.0648(10) Uani 1 1 d . . . H8 H 0.1149 -0.0886 0.9323 0.078 Uiso 1 1 calc R . . C25 C 0.0811(3) 0.1739(3) 0.84414(17) 0.0701(11) Uani 1 1 d . . . C11 C 0.0045(2) 0.1247(2) 0.34159(15) 0.0549(9) Uani 1 1 d . . . H6 H -0.0404 0.1409 0.3623 0.066 Uiso 1 1 calc R . . C2 C 0.2095(2) 0.2914(2) 0.49317(16) 0.0518(8) Uani 1 1 d . . . C20 C 0.0898(2) 0.1012(2) 0.95457(15) 0.0545(9) Uani 1 1 d . . . C28 C 0.1351(2) 0.0853(3) 0.63138(17) 0.0722(12) Uani 1 1 d . . . H12 H 0.1778 0.0748 0.6054 0.087 Uiso 1 1 calc R . . C15 C 0.0790(3) 0.1732(3) 0.06032(16) 0.0678(11) Uani 1 1 d . . . C17 C 0.1002(2) -0.0412(3) 0.02664(16) 0.0645(10) Uani 1 1 d . . . H7 H 0.1016 -0.0903 0.0503 0.077 Uiso 1 1 calc R . . C22 C 0.0756(3) 0.2429(3) -0.04596(18) 0.0863(15) Uani 1 1 d . . . H9 H 0.0717 0.2917 -0.0699 0.104 Uiso 1 1 calc R . . C23 C 0.0737(3) 0.2435(3) 0.02573(19) 0.0821(14) Uani 1 1 d . . . H10 H 0.0689 0.2922 0.0493 0.099 Uiso 1 1 calc R . . C29 C 0.0085(2) 0.1090(3) 0.63736(16) 0.0675(11) Uani 1 1 d . . . H13 H -0.0394 0.117 0.6158 0.081 Uiso 1 1 calc R . . C6 C 0.10688(17) -0.0789(2) 0.50291(13) 0.0400(7) 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 0.0410(2) 0.0419(2) 0.03169(18) 0.00093(14) 0.00228(13) 0.00200(15) S1 0.0513(5) 0.0425(5) 0.0532(5) -0.0027(3) 0.0017(3) -0.0072(4) O3 0.0522(14) 0.0467(15) 0.0537(13) 0.0005(10) 0.0016(10) 0.0115(11) O4 0.0373(11) 0.0515(14) 0.0444(11) 0.0039(9) 0.0037(8) -0.0012(10) O1 0.100(2) 0.0567(18) 0.0626(16) 0.0009(13) -0.0076(14) -0.0296(17) C5 0.0381(15) 0.0387(17) 0.0386(14) 0.0039(12) 0.0013(11) 0.0019(12) O5 0.121(2) 0.0663(18) 0.0382(13) 0.0079(12) 0.0162(13) 0.0100(16) O7 0.119(2) 0.0746(19) 0.0371(13) -0.0089(12) -0.0005(13) 0.0067(17) O2 0.0629(17) 0.086(2) 0.0557(14) 0.0025(13) 0.0032(11) -0.0388(15) N4 0.0512(16) 0.0530(18) 0.0398(14) 0.0017(11) 0.0007(11) -0.0011(13) N2 0.082(2) 0.062(2) 0.0284(13) 0.0032(12) 0.0067(12) 0.0001(16) N1 0.0482(15) 0.0497(17) 0.0329(12) 0.0005(10) 0.0016(10) 0.0038(12) N3 0.079(2) 0.072(2) 0.0274(13) 0.0004(13) 0.0006(12) -0.0037(16) O6 0.187(4) 0.072(2) 0.0368(14) -0.0048(13) 0.0147(16) 0.000(2) C13 0.070(2) 0.067(2) 0.0289(15) 0.0031(14) 0.0080(14) 0.0041(18) C1 0.075(3) 0.069(3) 0.0332(16) 0.0025(16) -0.0025(15) -0.031(2) C8 0.065(2) 0.081(3) 0.0398(17) 0.0002(17) 0.0098(15) 0.007(2) C12 0.069(2) 0.066(3) 0.0376(17) 0.0029(16) 0.0013(15) 0.0038(19) C27 0.065(2) 0.116(4) 0.0397(18) 0.008(2) -0.0041(16) 0.016(2) C26 0.071(2) 0.074(3) 0.0278(15) 0.0051(14) -0.0015(14) -0.0123(19) C3 0.0373(18) 0.072(3) 0.068(2) -0.0122(19) 0.0042(15) -0.0050(17) C9 0.073(2) 0.063(2) 0.0284(15) 0.0002(14) 0.0054(14) 0.0020(18) O8 0.178(4) 0.067(2) 0.0401(14) 0.0060(13) 0.0050(16) 0.008(2) C19 0.064(2) 0.072(3) 0.0329(16) -0.0025(16) 0.0023(14) -0.0034(19) C7 0.053(2) 0.072(2) 0.0369(16) -0.0017(15) 0.0034(13) 0.0114(17) C16 0.101(3) 0.075(3) 0.0401(19) -0.0026(19) 0.0065(18) 0.004(2) C10 0.063(2) 0.086(3) 0.0339(16) -0.0013(16) -0.0077(14) 0.011(2) C4 0.049(2) 0.051(2) 0.064(2) 0.0018(16) 0.0014(15) -0.0040(16) C21 0.098(3) 0.068(3) 0.0359(18) -0.0017(17) 0.0081(17) -0.006(2) C14 0.070(2) 0.061(2) 0.0320(15) -0.0007(14) 0.0051(14) -0.0031(18) C24 0.064(2) 0.075(3) 0.0306(16) -0.0055(16) -0.0026(14) -0.0020(19) C30 0.068(3) 0.116(4) 0.0324(17) -0.0005(18) 0.0091(16) 0.000(2) C18 0.094(3) 0.065(3) 0.0355(17) -0.0009(16) 0.0033(17) 0.013(2) C25 0.101(3) 0.074(3) 0.0349(17) 0.0076(18) -0.0005(18) -0.004(2) C11 0.056(2) 0.075(3) 0.0342(16) -0.0033(15) 0.0026(13) 0.0098(18) C2 0.051(2) 0.060(2) 0.0445(17) -0.0010(15) 0.0036(13) -0.0188(17) C20 0.069(2) 0.063(2) 0.0315(15) 0.0042(14) 0.0001(14) -0.0046(18) C28 0.059(2) 0.119(4) 0.0385(18) 0.0035(19) 0.0003(15) 0.018(2) C15 0.095(3) 0.074(3) 0.0343(17) 0.0052(17) 0.0048(17) -0.006(2) C17 0.092(3) 0.066(3) 0.0355(17) 0.0037(16) 0.0093(17) 0.012(2) C22 0.150(5) 0.067(3) 0.042(2) 0.0073(19) 0.012(2) 0.007(3) C23 0.134(4) 0.069(3) 0.044(2) 0.0016(19) 0.007(2) 0.002(3) C29 0.054(2) 0.114(4) 0.0341(17) 0.0027(18) 0.0002(14) 0.005(2) C6 0.0447(17) 0.050(2) 0.0258(13) -0.0031(12) 0.0030(11) 0.0044(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.010(2) . ? Zn1 O3 2.015(2) . ? Zn1 O2 2.072(3) . ? Zn1 N1 2.140(2) . ? Zn1 N4 2.142(3) . ? Zn1 O1 2.465(3) . ? Zn1 C1 2.578(4) . ? S1 C5 1.688(3) 2_556 ? S1 C2 1.703(4) . ? O3 C6 1.233(4) . ? O4 C6 1.258(4) 3_556 ? O1 C1 1.236(5) . ? C5 C4 1.358(4) . ? C5 C6 1.478(4) . ? C5 S1 1.688(3) 2_546 ? O5 C12 1.207(4) . ? O7 C24 1.194(4) . ? O2 C1 1.239(5) . ? N4 C28 1.333(4) . ? N4 C29 1.337(4) . ? N2 C16 1.382(5) . ? N2 C12 1.387(5) . ? N2 C9 1.445(4) . ? N1 C7 1.335(4) . ? N1 C11 1.341(4) . ? N3 C25 1.378(5) . ? N3 C24 1.390(5) . ? N3 C26 1.460(4) . ? O6 C16 1.198(5) . ? C13 C17 1.363(5) . ? C13 C14 1.378(5) . ? C13 C12 1.481(4) . ? C1 C2 1.480(5) . ? C8 C9 1.367(5) . ? C8 C7 1.374(4) . ? C8 H4 0.94 . ? C27 C26 1.351(5) . ? C27 C28 1.371(5) . ? C27 H11 0.94 . ? C26 C30 1.342(5) . ? C3 C2 1.353(5) . ? C3 C4 1.395(5) 2_556 ? C3 H1 0.94 . ? C9 C10 1.360(5) . ? O8 C25 1.187(5) . ? C19 C18 1.354(5) . ? C19 C20 1.383(5) . ? C19 C24 1.480(4) . ? C7 H3 0.94 . ? C16 C15 1.490(5) . ? C10 C11 1.386(4) . ? C10 H5 0.94 . ? C4 C3 1.395(5) 2_546 ? C4 H2 0.94 . ? C21 C22 1.349(6) 1_556 ? C21 C20 1.396(5) . ? C21 C25 1.475(5) . ? C14 C15 1.386(5) . ? C14 C20 1.416(4) 1_554 ? C30 C29 1.379(5) . ? C30 H14 0.94 . ? C18 C17 1.403(4) 1_556 ? C18 H8 0.94 . ? C11 H6 0.94 . ? C20 C14 1.416(4) 1_556 ? C28 H12 0.94 . ? C15 C23 1.354(6) . ? C17 C18 1.403(4) 1_554 ? C17 H7 0.94 . ? C22 C21 1.349(5) 1_554 ? C22 C23 1.411(5) . ? C22 H9 0.94 . ? C23 H10 0.94 . ? C29 H13 0.94 . ? C6 O4 1.258(4) 3_556 ? 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 O3 120.45(9) . . ? O4 Zn1 O2 96.02(11) . . ? O3 Zn1 O2 143.52(11) . . ? O4 Zn1 N1 91.46(9) . . ? O3 Zn1 N1 86.19(9) . . ? O2 Zn1 N1 92.36(10) . . ? O4 Zn1 N4 94.47(9) . . ? O3 Zn1 N4 86.84(10) . . ? O2 Zn1 N4 91.59(10) . . ? N1 Zn1 N4 172.50(10) . . ? O4 Zn1 O1 152.39(10) . . ? O3 Zn1 O1 86.96(10) . . ? O2 Zn1 O1 56.57(11) . . ? N1 Zn1 O1 86.85(9) . . ? N4 Zn1 O1 90.00(10) . . ? O4 Zn1 C1 124.29(13) . . ? O3 Zn1 C1 115.21(13) . . ? O2 Zn1 C1 28.31(13) . . ? N1 Zn1 C1 89.86(10) . . ? N4 Zn1 C1 90.59(10) . . ? O1 Zn1 C1 28.27(11) . . ? C5 S1 C2 92.04(17) 2_556 . ? C6 O3 Zn1 157.6(2) . . ? C6 O4 Zn1 131.5(2) 3_556 . ? C1 O1 Zn1 80.9(2) . . ? C4 C5 C6 127.6(3) . . ? C4 C5 S1 111.5(3) . 2_546 ? C6 C5 S1 120.9(2) . 2_546 ? C1 O2 Zn1 99.2(3) . . ? C28 N4 C29 116.7(3) . . ? C28 N4 Zn1 121.2(2) . . ? C29 N4 Zn1 122.2(2) . . ? C16 N2 C12 124.7(3) . . ? C16 N2 C9 117.3(3) . . ? C12 N2 C9 117.8(3) . . ? C7 N1 C11 117.4(3) . . ? C7 N1 Zn1 120.7(2) . . ? C11 N1 Zn1 121.8(2) . . ? C25 N3 C24 125.1(3) . . ? C25 N3 C26 118.2(3) . . ? C24 N3 C26 116.7(3) . . ? C17 C13 C14 120.2(3) . . ? C17 C13 C12 119.6(3) . . ? C14 C13 C12 120.1(3) . . ? O1 C1 O2 123.3(4) . . ? O1 C1 C2 117.6(4) . . ? O2 C1 C2 119.2(4) . . ? O1 C1 Zn1 70.8(2) . . ? O2 C1 Zn1 52.49(19) . . ? C2 C1 Zn1 171.6(3) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 H4 120.8 . . ? C7 C8 H4 120.8 . . ? O5 C12 N2 120.1(3) . . ? O5 C12 C13 122.8(3) . . ? N2 C12 C13 117.0(3) . . ? C26 C27 C28 118.0(4) . . ? C26 C27 H11 121 . . ? C28 C27 H11 121 . . ? C30 C26 C27 120.6(3) . . ? C30 C26 N3 118.3(3) . . ? C27 C26 N3 121.1(3) . . ? C2 C3 C4 112.8(3) . 2_556 ? C2 C3 H1 123.6 . . ? C4 C3 H1 123.6 2_556 . ? C10 C9 C8 120.0(3) . . ? C10 C9 N2 119.9(3) . . ? C8 C9 N2 120.1(3) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 C24 119.4(3) . . ? C20 C19 C24 120.4(3) . . ? N1 C7 C8 123.2(3) . . ? N1 C7 H3 118.4 . . ? C8 C7 H3 118.4 . . ? O6 C16 N2 120.1(3) . . ? O6 C16 C15 123.4(4) . . ? N2 C16 C15 116.5(3) . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H5 120.8 . . ? C11 C10 H5 120.8 . . ? C5 C4 C3 112.5(3) . 2_546 ? C5 C4 H2 123.7 . . ? C3 C4 H2 123.7 2_546 . ? C22 C21 C20 119.6(3) 1_556 . ? C22 C21 C25 120.4(4) 1_556 . ? C20 C21 C25 119.9(3) . . ? C13 C14 C15 121.4(3) . . ? C13 C14 C20 119.6(3) . 1_554 ? C15 C14 C20 118.9(3) . 1_554 ? O7 C24 N3 120.5(3) . . ? O7 C24 C19 123.3(4) . . ? N3 C24 C19 116.2(3) . . ? C26 C30 C29 118.6(3) . . ? C26 C30 H14 120.7 . . ? C29 C30 H14 120.7 . . ? C19 C18 C17 120.6(4) . 1_556 ? C19 C18 H8 119.7 . . ? C17 C18 H8 119.7 1_556 . ? O8 C25 N3 119.9(3) . . ? O8 C25 C21 123.2(4) . . ? N3 C25 C21 116.9(3) . . ? N1 C11 C10 122.5(3) . . ? N1 C11 H6 118.7 . . ? C10 C11 H6 118.7 . . ? C3 C2 C1 128.1(4) . . ? C3 C2 S1 111.1(3) . . ? C1 C2 S1 120.8(3) . . ? C19 C20 C21 121.0(3) . . ? C19 C20 C14 119.3(3) . 1_556 ? C21 C20 C14 119.7(3) . 1_556 ? N4 C28 C27 123.4(3) . . ? N4 C28 H12 118.3 . . ? C27 C28 H12 118.3 . . ? C23 C15 C14 121.0(3) . . ? C23 C15 C16 118.9(4) . . ? C14 C15 C16 120.0(3) . . ? C13 C17 C18 120.0(4) . 1_554 ? C13 C17 H7 120 . . ? C18 C17 H7 120 1_554 . ? C21 C22 C23 121.2(4) 1_554 . ? C21 C22 H9 119.4 1_554 . ? C23 C22 H9 119.4 . . ? C15 C23 C22 119.5(4) . . ? C15 C23 H10 120.2 . . ? C22 C23 H10 120.2 . . ? N4 C29 C30 122.6(3) . . ? N4 C29 H13 118.7 . . ? C30 C29 H13 118.7 . . ? O3 C6 O4 126.0(3) . 3_556 ? O3 C6 C5 117.1(3) . . ? O4 C6 C5 116.8(3) 3_556 . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # 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 0.341 -0.060 0.049 3606 562 ' ' _platon_squeeze_details ; ;