data_LFF3-Zn _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 N4 O13 Zn2' _chemical_formula_weight 631.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8594(4) _cell_length_b 14.7599(4) _cell_length_c 11.4301(4) _cell_angle_alpha 90 _cell_angle_beta 91.303(3) _cell_angle_gamma 90 _cell_volume 2168.91(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8164 _cell_measurement_theta_min 3.8683 _cell_measurement_theta_max 69.7256 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.933 _exptl_crystal_F_000 1280 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 3.477 _shelx_estimated_absorpt_T_min 0.624 _shelx_estimated_absorpt_T_max 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95270 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0733 _diffrn_reflns_number 8113 _diffrn_reflns_av_unetI/netI 0.0398 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.561 _diffrn_reflns_theta_max 69.726 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_point_group_measured_fraction_full 0.977 _reflns_number_total 3951 _reflns_number_gt 3369 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.4493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3951 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.25009(3) 0.50510(2) 0.35959(3) 0.01409(10) Uani 1 1 d . . . . . Zn2 Zn 0.73755(3) 0.16188(2) 0.55116(3) 0.01358(10) Uani 1 1 d . . . . . N1 N 0.38823(16) 0.42788(15) 0.38398(19) 0.0131(4) Uani 1 1 d . . . . . N2 N 0.44866(17) 0.38675(15) 0.46632(19) 0.0146(4) Uani 1 1 d . . . . . N3 N 0.13405(16) 0.41708(14) 0.40845(18) 0.0114(4) Uani 1 1 d . . . . . N4 N 0.07435(16) 0.34799(14) 0.37116(18) 0.0117(4) Uani 1 1 d . . . . . O1 O 0.28585(14) 0.48131(13) 0.19131(16) 0.0166(4) Uani 1 1 d . . . . . O2 O 0.40643(14) 0.42291(13) 0.07608(16) 0.0176(4) Uani 1 1 d . . . . . O3 O 0.65896(16) 0.22950(14) 0.41151(19) 0.0244(5) Uani 1 1 d . . . . . O4 O 0.60802(17) 0.27540(16) 0.58473(18) 0.0281(5) Uani 1 1 d . . . . . O5 O 0.23812(14) 0.54601(12) 0.52859(16) 0.0164(4) Uani 1 1 d . . . . . O6 O 0.13458(16) 0.53136(13) 0.68083(16) 0.0189(4) Uani 1 1 d . . . . . O7 O 0.86457(14) 0.24696(12) 0.52827(16) 0.0167(4) Uani 1 1 d . . . . . O8 O 0.93500(15) 0.19245(13) 0.36426(16) 0.0199(4) Uani 1 1 d . . . . . O9 O 0.19148(16) 0.62393(13) 0.30934(17) 0.0217(4) Uani 1 1 d . . . . . H9A H 0.180698 0.663228 0.358295 0.033 Uiso 1 1 d R U . . . H9B H 0.167956 0.642343 0.246442 0.033 Uiso 1 1 d R U . . . O10 O 0.76752(15) 0.17295(12) 0.72515(15) 0.0171(4) Uani 1 1 d . . . . . H10A H 0.792566 0.130154 0.761815 0.026 Uiso 1 1 d R U . . . H10B H 0.729180 0.200849 0.768755 0.026 Uiso 1 1 d R U . . . O11 O 0.81561(15) 0.04909(13) 0.50254(18) 0.0251(5) Uani 1 1 d . . . . . H11C H 0.868312 0.024375 0.528653 0.038 Uiso 1 1 d R U . . . H11D H 0.796786 0.021406 0.443577 0.038 Uiso 1 1 d R U . . . O12 O 0.61723(15) 0.06854(13) 0.57164(18) 0.0233(4) Uani 1 1 d . . . . . H12A H 0.554860 0.079880 0.573412 0.035 Uiso 1 1 d R U . . . H12B H 0.623758 0.021211 0.534962 0.035 Uiso 1 1 d R U . . . C1 C 0.4224(2) 0.39950(17) 0.2808(2) 0.0134(5) Uani 1 1 d . . . . . C2 C 0.5045(2) 0.33895(18) 0.2948(2) 0.0161(5) Uani 1 1 d . . . . . H2 H 0.541879 0.308985 0.235445 0.019 Uiso 1 1 calc R U . . . C3 C 0.5196(2) 0.33217(18) 0.4144(2) 0.0156(5) Uani 1 1 d . . . . . C4 C 0.4249(2) 0.39900(19) 0.5909(2) 0.0173(5) Uani 1 1 d . . . . . H4A H 0.406934 0.463290 0.604667 0.021 Uiso 1 1 calc R U . . . H4B H 0.487894 0.384884 0.638950 0.021 Uiso 1 1 calc R U . . . C5 C 0.3358(2) 0.33958(18) 0.6308(2) 0.0145(5) Uani 1 1 d . . . . . C6 C 0.2970(2) 0.26766(18) 0.5650(2) 0.0165(5) Uani 1 1 d . . . . . H6 H 0.326265 0.254218 0.491402 0.020 Uiso 1 1 calc R U . . . C7 C 0.2157(2) 0.21514(18) 0.6056(2) 0.0152(5) Uani 1 1 d . . . . . H7 H 0.190557 0.165994 0.559337 0.018 Uiso 1 1 calc R U . . . C8 C 0.1703(2) 0.23310(18) 0.7131(2) 0.0142(5) Uani 1 1 d . . . . . C9 C 0.2096(2) 0.30553(19) 0.7789(2) 0.0172(5) Uani 1 1 d . . . . . H9 H 0.179971 0.319376 0.852126 0.021 Uiso 1 1 calc R U . . . C10 C 0.2911(2) 0.35744(19) 0.7393(2) 0.0174(5) Uani 1 1 d . . . . . H10 H 0.317109 0.405903 0.786146 0.021 Uiso 1 1 calc R U . . . C11 C 0.0762(2) 0.17834(18) 0.7470(2) 0.0139(5) Uani 1 1 d . . . . . H11A H 0.012857 0.214071 0.728180 0.017 Uiso 1 1 calc R U . . . H11B H 0.073455 0.122727 0.698592 0.017 Uiso 1 1 calc R U . . . C12 C 0.10889(19) 0.43349(17) 0.5199(2) 0.0117(5) Uani 1 1 d . . . . . C13 C 0.03074(19) 0.37506(16) 0.5538(2) 0.0119(5) Uani 1 1 d . . . . . H13 H -0.001303 0.372557 0.627800 0.014 Uiso 1 1 calc R U . . . C14 C 0.00935(19) 0.32148(17) 0.4578(2) 0.0121(5) Uani 1 1 d . . . . . C15 C 0.3692(2) 0.43657(17) 0.1732(2) 0.0136(5) Uani 1 1 d . . . . . C16 C 0.6012(2) 0.2756(2) 0.4761(3) 0.0207(6) Uani 1 1 d . . . . . C17 C 0.1645(2) 0.50890(17) 0.5822(2) 0.0142(5) Uani 1 1 d . . . . . C18 C 0.9298(2) 0.24707(17) 0.4471(2) 0.0137(5) Uani 1 1 d . . . . . O13 O 0.02283(18) 0.48466(15) 0.86912(18) 0.0302(5) Uani 1 1 d . . . . . H13A H 0.050928 0.489016 0.805671 0.045 Uiso 1 1 d R U . . . H13B H 0.004951 0.431615 0.876235 0.045 Uiso 1 1 d R U . . . 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 0.01306(18) 0.01519(18) 0.01419(19) 0.00139(13) 0.00419(13) 0.00203(14) Zn2 0.01233(18) 0.01293(17) 0.01545(18) 0.00085(13) -0.00046(13) 0.00050(13) N1 0.0098(10) 0.0149(10) 0.0146(11) 0.0040(9) -0.0004(8) 0.0003(8) N2 0.0128(10) 0.0171(11) 0.0140(11) 0.0061(9) 0.0002(8) -0.0013(9) N3 0.0105(10) 0.0117(10) 0.0122(10) -0.0013(8) 0.0028(8) -0.0004(8) N4 0.0118(10) 0.0120(10) 0.0115(10) -0.0029(8) 0.0025(8) 0.0015(8) O1 0.0150(9) 0.0203(9) 0.0146(9) 0.0046(8) 0.0031(7) 0.0078(8) O2 0.0170(9) 0.0225(10) 0.0136(9) 0.0040(8) 0.0054(7) 0.0034(8) O3 0.0170(10) 0.0242(10) 0.0320(12) 0.0075(9) 0.0008(8) 0.0079(8) O4 0.0250(11) 0.0379(12) 0.0213(11) 0.0136(9) -0.0033(8) 0.0014(10) O5 0.0179(9) 0.0153(9) 0.0162(9) -0.0014(7) 0.0023(7) -0.0041(8) O6 0.0249(10) 0.0186(9) 0.0134(9) -0.0048(8) 0.0045(8) -0.0057(8) O7 0.0159(9) 0.0155(9) 0.0188(10) -0.0024(8) 0.0055(7) -0.0044(7) O8 0.0240(10) 0.0183(9) 0.0174(10) -0.0072(8) 0.0026(8) -0.0049(8) O9 0.0334(11) 0.0148(9) 0.0170(10) 0.0005(8) 0.0007(8) 0.0086(8) O10 0.0209(10) 0.0171(9) 0.0132(9) 0.0016(8) 0.0009(7) 0.0057(8) O11 0.0204(10) 0.0218(10) 0.0327(12) -0.0108(9) -0.0060(9) 0.0056(9) O12 0.0170(10) 0.0210(10) 0.0323(11) -0.0106(9) 0.0060(8) -0.0046(8) C1 0.0130(12) 0.0144(11) 0.0128(12) 0.0038(10) 0.0012(9) -0.0003(10) C2 0.0118(12) 0.0191(13) 0.0177(13) 0.0015(11) 0.0040(10) 0.0022(10) C3 0.0118(12) 0.0172(12) 0.0179(13) 0.0046(11) 0.0022(10) -0.0009(10) C4 0.0156(13) 0.0242(13) 0.0120(12) 0.0003(11) 0.0009(10) -0.0027(11) C5 0.0153(13) 0.0163(13) 0.0120(12) 0.0058(10) 0.0008(10) 0.0002(10) C6 0.0192(13) 0.0182(13) 0.0121(12) 0.0016(10) 0.0049(10) 0.0008(11) C7 0.0196(13) 0.0139(12) 0.0123(12) -0.0008(10) 0.0025(10) -0.0010(10) C8 0.0153(13) 0.0153(12) 0.0120(12) 0.0062(10) 0.0012(9) 0.0030(10) C9 0.0220(14) 0.0207(13) 0.0091(12) 0.0008(10) 0.0036(10) 0.0007(11) C10 0.0213(14) 0.0191(13) 0.0118(12) -0.0020(10) -0.0011(10) -0.0015(11) C11 0.0163(13) 0.0172(12) 0.0084(12) 0.0024(10) 0.0002(9) -0.0007(10) C12 0.0147(12) 0.0101(11) 0.0104(11) -0.0014(10) 0.0010(9) 0.0019(10) C13 0.0121(12) 0.0124(11) 0.0111(12) -0.0013(10) 0.0021(9) 0.0029(10) C14 0.0107(12) 0.0140(12) 0.0117(12) 0.0004(10) 0.0015(9) 0.0024(10) C15 0.0133(12) 0.0138(12) 0.0137(12) 0.0018(10) 0.0003(10) -0.0018(10) C16 0.0124(13) 0.0240(14) 0.0256(15) 0.0109(12) -0.0013(11) -0.0027(11) C17 0.0169(13) 0.0113(11) 0.0144(13) -0.0013(10) 0.0002(10) 0.0037(10) C18 0.0138(12) 0.0120(12) 0.0153(13) 0.0020(10) -0.0009(10) 0.0010(10) O13 0.0377(13) 0.0314(12) 0.0217(11) -0.0022(9) 0.0091(9) -0.0133(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 O9 1.9886(19) . yes Zn1 O1 2.0185(19) . yes Zn1 O5 2.0330(18) . yes Zn1 N3 2.065(2) . yes Zn1 N1 2.124(2) . yes Zn2 O10 2.0237(18) . yes Zn2 O11 2.028(2) . yes Zn2 O7 2.0815(18) . yes Zn2 O12 2.0888(19) . yes Zn2 O3 2.119(2) . yes Zn2 O4 2.400(2) . yes Zn2 C16 2.562(3) . ? N1 C1 1.335(3) . ? N1 N2 1.351(3) . ? N2 C3 1.362(4) . ? N2 C4 1.475(3) . ? N3 N4 1.340(3) . ? N3 C12 1.343(3) . ? N4 C14 1.368(3) . ? N4 C11 1.472(3) 4_565 ? O1 C15 1.280(3) . ? O2 C15 1.235(3) . ? O3 C16 1.259(4) . ? O4 C16 1.243(4) . ? O5 C17 1.264(3) . ? O6 C17 1.245(3) . ? O7 C18 1.265(3) . ? O8 C18 1.246(3) . ? O9 H9A 0.8200 . ? O9 H9B 0.8200 . ? O10 H10A 0.8199 . ? O10 H10B 0.8199 . ? O11 H11C 0.8200 . ? O11 H11D 0.8199 . ? O12 H12A 0.8201 . ? O12 H12B 0.8200 . ? C1 C2 1.390(4) . ? C1 C15 1.497(3) . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C16 1.504(4) . ? C4 C5 1.521(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.388(4) . ? C5 C10 1.403(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9500 . ? C7 C8 1.398(4) . ? C7 H7 0.9500 . ? C8 C9 1.396(4) . ? C8 C11 1.512(4) . ? C9 C10 1.382(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.386(4) . ? C12 C17 1.495(3) . ? C13 C14 1.375(3) . ? C13 H13 0.9500 . ? C14 C18 1.504(3) 1_455 ? O13 H13A 0.8201 . ? O13 H13B 0.8205 . ? 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 O9 Zn1 O1 88.35(8) . . ? O9 Zn1 O5 88.63(8) . . ? O1 Zn1 O5 168.77(8) . . ? O9 Zn1 N3 111.19(9) . . ? O1 Zn1 N3 109.27(8) . . ? O5 Zn1 N3 81.90(8) . . ? O9 Zn1 N1 145.25(9) . . ? O1 Zn1 N1 79.85(8) . . ? O5 Zn1 N1 96.65(8) . . ? N3 Zn1 N1 103.55(8) . . ? O10 Zn2 O11 104.55(8) . . ? O10 Zn2 O7 86.70(8) . . ? O11 Zn2 O7 93.79(8) . . ? O10 Zn2 O12 93.91(8) . . ? O11 Zn2 O12 82.05(8) . . ? O7 Zn2 O12 175.82(8) . . ? O10 Zn2 O3 141.17(8) . . ? O11 Zn2 O3 114.24(8) . . ? O7 Zn2 O3 89.04(8) . . ? O12 Zn2 O3 93.05(8) . . ? O10 Zn2 O4 84.48(7) . . ? O11 Zn2 O4 165.16(8) . . ? O7 Zn2 O4 98.53(7) . . ? O12 Zn2 O4 85.64(8) . . ? O3 Zn2 O4 58.05(8) . . ? O10 Zn2 C16 112.96(9) . . ? O11 Zn2 C16 141.76(9) . . ? O7 Zn2 C16 95.50(8) . . ? O12 Zn2 C16 88.08(8) . . ? O3 Zn2 C16 29.30(9) . . ? O4 Zn2 C16 28.79(8) . . ? C1 N1 N2 106.2(2) . . ? C1 N1 Zn1 110.07(16) . . ? N2 N1 Zn1 143.03(17) . . ? N1 N2 C3 110.0(2) . . ? N1 N2 C4 119.3(2) . . ? C3 N2 C4 130.4(2) . . ? N4 N3 C12 106.9(2) . . ? N4 N3 Zn1 143.61(17) . . ? C12 N3 Zn1 109.52(17) . . ? N3 N4 C14 110.0(2) . . ? N3 N4 C11 119.1(2) . 4_565 ? C14 N4 C11 130.3(2) . 4_565 ? C15 O1 Zn1 116.99(16) . . ? C16 O3 Zn2 95.21(17) . . ? C16 O4 Zn2 82.85(18) . . ? C17 O5 Zn1 113.92(16) . . ? C18 O7 Zn2 128.94(17) . . ? Zn1 O9 H9A 119.7 . . ? Zn1 O9 H9B 132.5 . . ? H9A O9 H9B 107.4 . . ? Zn2 O10 H10A 120.3 . . ? Zn2 O10 H10B 122.3 . . ? H10A O10 H10B 108.1 . . ? Zn2 O11 H11C 132.5 . . ? Zn2 O11 H11D 119.7 . . ? H11C O11 H11D 107.7 . . ? Zn2 O12 H12A 126.5 . . ? Zn2 O12 H12B 114.8 . . ? H12A O12 H12B 107.3 . . ? N1 C1 C2 111.3(2) . . ? N1 C1 C15 117.3(2) . . ? C2 C1 C15 131.4(2) . . ? C3 C2 C1 104.5(2) . . ? C3 C2 H2 127.8 . . ? C1 C2 H2 127.8 . . ? N2 C3 C2 107.9(2) . . ? N2 C3 C16 126.2(2) . . ? C2 C3 C16 125.8(3) . . ? N2 C4 C5 113.1(2) . . ? N2 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N2 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C10 118.3(2) . . ? C6 C5 C4 122.8(2) . . ? C10 C5 C4 118.9(2) . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 121.4(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 117.7(2) . . ? C9 C8 C11 123.6(2) . . ? C7 C8 C11 118.5(2) . . ? C10 C9 C8 121.1(2) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C5 120.9(3) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? N4 C11 C8 114.8(2) 4_566 . ? N4 C11 H11A 108.6 4_566 . ? C8 C11 H11A 108.6 . . ? N4 C11 H11B 108.6 4_566 . ? C8 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N3 C12 C13 110.2(2) . . ? N3 C12 C17 117.6(2) . . ? C13 C12 C17 132.2(2) . . ? C14 C13 C12 105.5(2) . . ? C14 C13 H13 127.2 . . ? C12 C13 H13 127.2 . . ? N4 C14 C13 107.4(2) . . ? N4 C14 C18 125.1(2) . 1_455 ? C13 C14 C18 127.5(2) . 1_455 ? O2 C15 O1 124.9(2) . . ? O2 C15 C1 120.0(2) . . ? O1 C15 C1 115.1(2) . . ? O4 C16 O3 123.7(3) . . ? O4 C16 C3 120.1(3) . . ? O3 C16 C3 116.1(3) . . ? O4 C16 Zn2 68.36(16) . . ? O3 C16 Zn2 55.48(14) . . ? C3 C16 Zn2 170.4(2) . . ? O6 C17 O5 125.0(2) . . ? O6 C17 C12 118.4(2) . . ? O5 C17 C12 116.6(2) . . ? O8 C18 O7 127.1(2) . . ? O8 C18 C14 119.1(2) . 1_655 ? O7 C18 C14 113.7(2) . 1_655 ? H13A O13 H13B 107.0 . . ? 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 C1 N1 N2 C3 -0.6(3) . . . . ? Zn1 N1 N2 C3 167.9(2) . . . . ? C1 N1 N2 C4 -175.3(2) . . . . ? Zn1 N1 N2 C4 -6.8(4) . . . . ? C12 N3 N4 C14 1.3(3) . . . . ? Zn1 N3 N4 C14 -179.9(2) . . . . ? C12 N3 N4 C11 173.0(2) . . . 4_565 ? Zn1 N3 N4 C11 -8.3(4) . . . 4_565 ? N2 N1 C1 C2 0.6(3) . . . . ? Zn1 N1 C1 C2 -172.04(17) . . . . ? N2 N1 C1 C15 -179.0(2) . . . . ? Zn1 N1 C1 C15 8.4(3) . . . . ? N1 C1 C2 C3 -0.4(3) . . . . ? C15 C1 C2 C3 179.1(3) . . . . ? N1 N2 C3 C2 0.4(3) . . . . ? C4 N2 C3 C2 174.3(2) . . . . ? N1 N2 C3 C16 179.4(2) . . . . ? C4 N2 C3 C16 -6.7(4) . . . . ? C1 C2 C3 N2 0.0(3) . . . . ? C1 C2 C3 C16 -179.0(2) . . . . ? N1 N2 C4 C5 79.2(3) . . . . ? C3 N2 C4 C5 -94.2(3) . . . . ? N2 C4 C5 C6 13.5(4) . . . . ? N2 C4 C5 C10 -167.0(2) . . . . ? C10 C5 C6 C7 0.2(4) . . . . ? C4 C5 C6 C7 179.7(2) . . . . ? C5 C6 C7 C8 0.4(4) . . . . ? C6 C7 C8 C9 -0.3(4) . . . . ? C6 C7 C8 C11 174.8(2) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C11 C8 C9 C10 -175.1(2) . . . . ? C8 C9 C10 C5 0.8(4) . . . . ? C6 C5 C10 C9 -0.8(4) . . . . ? C4 C5 C10 C9 179.7(2) . . . . ? C9 C8 C11 N4 -44.9(3) . . . 4_566 ? C7 C8 C11 N4 140.3(2) . . . 4_566 ? N4 N3 C12 C13 -1.0(3) . . . . ? Zn1 N3 C12 C13 179.79(16) . . . . ? N4 N3 C12 C17 -179.5(2) . . . . ? Zn1 N3 C12 C17 1.3(3) . . . . ? N3 C12 C13 C14 0.3(3) . . . . ? C17 C12 C13 C14 178.5(3) . . . . ? N3 N4 C14 C13 -1.2(3) . . . . ? C11 N4 C14 C13 -171.6(2) 4_565 . . . ? N3 N4 C14 C18 178.8(2) . . . 1_455 ? C11 N4 C14 C18 8.3(4) 4_565 . . 1_455 ? C12 C13 C14 N4 0.5(3) . . . . ? C12 C13 C14 C18 -179.4(2) . . . 1_455 ? Zn1 O1 C15 O2 -173.7(2) . . . . ? Zn1 O1 C15 C1 6.4(3) . . . . ? N1 C1 C15 O2 169.8(2) . . . . ? C2 C1 C15 O2 -9.7(4) . . . . ? N1 C1 C15 O1 -10.2(3) . . . . ? C2 C1 C15 O1 170.3(3) . . . . ? Zn2 O4 C16 O3 -4.1(3) . . . . ? Zn2 O4 C16 C3 175.1(2) . . . . ? Zn2 O3 C16 O4 4.6(3) . . . . ? Zn2 O3 C16 C3 -174.6(2) . . . . ? N2 C3 C16 O4 0.5(4) . . . . ? C2 C3 C16 O4 179.4(3) . . . . ? N2 C3 C16 O3 179.7(3) . . . . ? C2 C3 C16 O3 -1.4(4) . . . . ? Zn1 O5 C17 O6 -170.8(2) . . . . ? Zn1 O5 C17 C12 8.1(3) . . . . ? N3 C12 C17 O6 172.4(2) . . . . ? C13 C12 C17 O6 -5.6(4) . . . . ? N3 C12 C17 O5 -6.5(3) . . . . ? C13 C12 C17 O5 175.4(3) . . . . ? Zn2 O7 C18 O8 -3.6(4) . . . . ? Zn2 O7 C18 C14 177.90(15) . . . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13B O8 0.82 2.04 2.848(3) 166.5 4_466 O13 H13A O6 0.82 1.91 2.704(3) 162.3 . C13 H13 O9 0.95 2.57 3.289(3) 133.2 3_566 C11 H11B O13 0.99 2.50 3.388(3) 149.4 2_546 C11 H11A O8 0.99 2.32 2.974(3) 122.4 4_466 C4 H4B O4 0.99 2.33 2.981(4) 122.5 . C2 H2 O4 0.95 2.30 3.246(3) 170.9 4_565 O12 H12B O2 0.82 1.96 2.746(3) 160.1 2_645 O12 H12A O2 0.82 1.91 2.715(3) 167.0 4_566 O11 H11D O1 0.82 1.94 2.735(3) 161.6 2_645 O11 H11C O13 0.82 1.90 2.690(3) 162.7 2_646 O10 H10B O3 0.82 2.15 2.949(3) 166.5 4_566 O10 H10A O6 0.82 1.85 2.654(3) 168.7 2_646 O9 H9B O8 0.82 1.96 2.731(3) 157.4 2_655 O9 H9A O7 0.82 1.95 2.767(3) 172.4 3_666 Cg1 . Cg1 . . 4.117(1) . 3_566 Cg1 . Cg2 . . 3.582(1) . . C6 H6 Cg3 0.95 2.95 3.665(3) 130 . C4 H4A Cg3 0.99 2.86 3.479(3) 124 3_666 _refine_diff_density_max 0.350 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.078 _shelx_res_file ; TITL LFF3-Zn in P21/c #14 LFF3-Zn.res created by SHELXL-2016/6 at 08:09:44 on 24-Jan-2019 CELL 1.54184 12.8594 14.7599 11.4301 90.000 91.303 90.000 ZERR 4 0.0004 0.0004 0.0004 0.000 0.003 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O Zn UNIT 72 80 16 52 8 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 HTAB O13 O8_$9 HTAB O13 O6 HTAB C13 O9_$11 EQIV $11 -x, -y+1, -z+1 HTAB C11 O13_$10 EQIV $10 -x, y-1/2, -z+3/2 HTAB C11 O8_$9 EQIV $9 x-1, -y+1/2, z+1/2 HTAB C4 O4 HTAB C2 O4_$2 EQIV $2 x, -y+1/2, z-1/2 HTAB O12 O2_$8 HTAB O12 O2_$1 HTAB O11 O1_$8 EQIV $8 -x+1, y-1/2, -z+1/2 HTAB O11 O13_$7 HTAB O10 O3_$1 EQIV $1 x, -y+1/2, z+1/2 HTAB O10 O6_$7 EQIV $7 -x+1, y-1/2, -z+3/2 HTAB O9 O8_$6 EQIV $6 -x+1, y+1/2, -z+1/2 HTAB O9 O7_$5 EQIV $5 -x+1, -y+1, -z+1 CONF SIZE 0.15 0.10 0.10 TEMP -100 WGHT 0.040500 0.449300 FVAR 2.84810 ZN1 5 0.250093 0.505096 0.359587 11.00000 0.01306 0.01519 = 0.01419 0.00139 0.00419 0.00203 ZN2 5 0.737547 0.161881 0.551161 11.00000 0.01233 0.01293 = 0.01545 0.00085 -0.00046 0.00050 N1 3 0.388226 0.427883 0.383980 11.00000 0.00980 0.01493 = 0.01458 0.00395 -0.00037 0.00025 N2 3 0.448665 0.386750 0.466318 11.00000 0.01280 0.01711 = 0.01403 0.00613 0.00025 -0.00129 N3 3 0.134051 0.417084 0.408447 11.00000 0.01045 0.01171 = 0.01221 -0.00134 0.00278 -0.00042 N4 3 0.074348 0.347989 0.371161 11.00000 0.01176 0.01201 = 0.01145 -0.00293 0.00249 0.00147 O1 4 0.285852 0.481314 0.191313 11.00000 0.01505 0.02034 = 0.01458 0.00462 0.00307 0.00781 O2 4 0.406430 0.422912 0.076077 11.00000 0.01701 0.02245 = 0.01357 0.00404 0.00544 0.00340 O3 4 0.658961 0.229495 0.411510 11.00000 0.01701 0.02422 = 0.03199 0.00754 0.00080 0.00790 O4 4 0.608020 0.275397 0.584735 11.00000 0.02504 0.03787 = 0.02127 0.01357 -0.00334 0.00142 O5 4 0.238118 0.546006 0.528585 11.00000 0.01789 0.01528 = 0.01619 -0.00144 0.00226 -0.00411 O6 4 0.134576 0.531360 0.680832 11.00000 0.02494 0.01857 = 0.01337 -0.00484 0.00447 -0.00566 O7 4 0.864566 0.246959 0.528266 11.00000 0.01595 0.01550 = 0.01884 -0.00241 0.00552 -0.00437 O8 4 0.934997 0.192448 0.364258 11.00000 0.02399 0.01829 = 0.01742 -0.00725 0.00264 -0.00490 O9 4 0.191484 0.623925 0.309344 11.00000 0.03344 0.01480 = 0.01699 0.00047 0.00073 0.00862 AFIX 3 H9A 2 0.180698 0.663228 0.358295 11.00000 -1.50000 H9B 2 0.167956 0.642343 0.246442 11.00000 -1.50000 AFIX 0 O10 4 0.767522 0.172949 0.725154 11.00000 0.02092 0.01714 = 0.01320 0.00164 0.00087 0.00565 AFIX 3 H10A 2 0.792566 0.130154 0.761815 11.00000 -1.50000 H10B 2 0.729180 0.200849 0.768755 11.00000 -1.50000 AFIX 0 O11 4 0.815607 0.049089 0.502537 11.00000 0.02040 0.02182 = 0.03273 -0.01080 -0.00599 0.00564 AFIX 3 H11C 2 0.868312 0.024375 0.528653 11.00000 -1.50000 H11D 2 0.796786 0.021406 0.443577 11.00000 -1.50000 AFIX 0 O12 4 0.617232 0.068536 0.571640 11.00000 0.01703 0.02099 = 0.03226 -0.01063 0.00596 -0.00464 AFIX 3 H12A 2 0.554860 0.079880 0.573412 11.00000 -1.50000 H12B 2 0.623758 0.021211 0.534962 11.00000 -1.50000 AFIX 0 C1 1 0.422357 0.399499 0.280803 11.00000 0.01301 0.01438 = 0.01279 0.00380 0.00120 -0.00032 C2 1 0.504502 0.338955 0.294844 11.00000 0.01182 0.01906 = 0.01770 0.00145 0.00404 0.00219 AFIX 43 H2 2 0.541879 0.308985 0.235445 11.00000 -1.20000 AFIX 0 C3 1 0.519557 0.332166 0.414442 11.00000 0.01179 0.01719 = 0.01790 0.00460 0.00223 -0.00090 C4 1 0.424919 0.399002 0.590945 11.00000 0.01563 0.02415 = 0.01201 0.00033 0.00088 -0.00270 AFIX 23 H4A 2 0.406934 0.463290 0.604667 11.00000 -1.20000 H4B 2 0.487894 0.384884 0.638950 11.00000 -1.20000 AFIX 0 C5 1 0.335797 0.339578 0.630842 11.00000 0.01528 0.01628 = 0.01195 0.00577 0.00076 0.00019 C6 1 0.296994 0.267664 0.564967 11.00000 0.01925 0.01820 = 0.01213 0.00156 0.00488 0.00084 AFIX 43 H6 2 0.326265 0.254218 0.491402 11.00000 -1.20000 AFIX 0 C7 1 0.215737 0.215136 0.605575 11.00000 0.01960 0.01387 = 0.01235 -0.00078 0.00248 -0.00098 AFIX 43 H7 2 0.190557 0.165994 0.559337 11.00000 -1.20000 AFIX 0 C8 1 0.170258 0.233099 0.713072 11.00000 0.01527 0.01530 = 0.01199 0.00621 0.00117 0.00297 C9 1 0.209634 0.305531 0.778891 11.00000 0.02198 0.02071 = 0.00909 0.00084 0.00362 0.00069 AFIX 43 H9 2 0.179971 0.319376 0.852126 11.00000 -1.20000 AFIX 0 C10 1 0.291056 0.357442 0.739294 11.00000 0.02132 0.01911 = 0.01175 -0.00203 -0.00110 -0.00150 AFIX 43 H10 2 0.317109 0.405903 0.786146 11.00000 -1.20000 AFIX 0 C11 1 0.076211 0.178340 0.746984 11.00000 0.01626 0.01719 = 0.00838 0.00241 0.00018 -0.00073 AFIX 23 H11A 2 0.012857 0.214071 0.728180 11.00000 -1.20000 H11B 2 0.073455 0.122727 0.698592 11.00000 -1.20000 AFIX 0 C12 1 0.108888 0.433488 0.519893 11.00000 0.01475 0.01009 = 0.01040 -0.00135 0.00098 0.00194 C13 1 0.030743 0.375059 0.553798 11.00000 0.01214 0.01240 = 0.01112 -0.00127 0.00205 0.00291 AFIX 43 H13 2 -0.001303 0.372557 0.627800 11.00000 -1.20000 AFIX 0 C14 1 0.009351 0.321478 0.457816 11.00000 0.01070 0.01397 = 0.01173 0.00036 0.00153 0.00242 C15 1 0.369200 0.436573 0.173183 11.00000 0.01327 0.01383 = 0.01374 0.00183 0.00032 -0.00182 C16 1 0.601164 0.275598 0.476060 11.00000 0.01240 0.02398 = 0.02560 0.01090 -0.00133 -0.00268 C17 1 0.164483 0.508896 0.582189 11.00000 0.01688 0.01132 = 0.01437 -0.00132 0.00019 0.00368 C18 1 0.929839 0.247070 0.447084 11.00000 0.01382 0.01201 = 0.01533 0.00204 -0.00085 0.00101 O13 4 0.022826 0.484656 0.869116 11.00000 0.03768 0.03145 = 0.02172 -0.00219 0.00906 -0.01326 AFIX 3 H13A 2 0.050928 0.489016 0.805671 11.00000 -1.50000 H13B 2 0.004951 0.431615 0.876235 11.00000 -1.50000 AFIX 0 HKLF 4 REM LFF3-Zn in P21/c #14 REM R1 = 0.0306 for 3369 Fo > 4sig(Fo) and 0.0389 for all 3951 data REM 334 parameters refined using 0 restraints END WGHT 0.0406 0.4432 REM Highest difference peak 0.350, deepest hole -0.435, 1-sigma level 0.078 Q1 1 0.2944 0.5443 0.3719 11.00000 0.05 0.35 Q2 1 0.6161 0.3389 0.6179 11.00000 0.05 0.35 Q3 1 0.1764 0.4345 0.3740 11.00000 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1014.42 5 4 -4 4 231687. 3575.67 5 5 -4 4 46942.8 1714.60 5 6 -4 4 53911.2 1949.40 5 7 -4 4 9331.95 872.535 5 8 -4 4 10431.6 989.369 5 -8 4 -4 11575.4 895.059 19 -9 4 -4 18067.1 1165.98 19 9 -4 4 19046.6 1361.39 5 9 -4 4 18893.6 1153.71 15 9 -4 4 21938.8 1312.34 11 10 -4 4 38255.0 1679.76 15 10 -4 4 41307.8 1801.98 11 11 -4 4 10489.7 873.639 15 11 -4 4 10484.1 900.375 11 12 4 4 11939.2 951.640 15 12 -4 4 11205.0 842.913 15 12 -4 4 12155.4 902.510 11 13 -4 4 1378.85 300.032 11 -13 -4 -4 919.282 276.420 14 -13 4 -4 999.770 241.861 14 13 -4 4 719.268 222.866 15 13 4 4 1065.53 305.751 15 -14 -4 -4 7851.29 552.196 14 14 4 4 8560.19 599.002 15 -14 5 4 2966.76 346.505 19 -13 5 4 1939.36 350.840 19 13 -5 -4 1749.48 332.629 8 -12 5 4 29410.2 1393.76 19 12 -5 -4 29811.9 1387.27 8 -11 5 4-11.0166 208.005 19 11 -5 -4-111.007 222.303 8 10 -5 -4 30321.9 1545.76 8 -10 5 4 28709.8 1456.26 19 9 -5 -4 6935.67 760.234 8 -9 5 4 7140.78 719.464 19 9 5 -4 6459.59 893.508 7 8 -5 -4 456.127 218.346 8 -8 5 4 705.585 251.039 19 -8 -5 4 390.156 171.571 12 8 5 -4 1071.92 430.693 7 7 5 -4 4998.76 756.511 7 -4 -5 4 133775. 2826.44 5 -3 -5 4 10.0815 196.454 5 -2 -5 4 65530.1 1822.21 5 -1 -5 4 669.858 247.230 5 1 5 -4 320.997 167.543 3 -1 5 4 561.813 198.342 4 0 -5 4 17429.9 941.661 5 0 5 4 14959.1 861.929 4 0 5 -4 15998.1 854.963 3 0 -5 4 16530.2 833.867 4 1 5 4-275.386 257.658 4 1 -5 4 128.112 212.819 5 2 -5 4 30347.3 1284.67 5 3 -5 4 42681.0 1570.06 5 4 -5 4 22190.7 1202.92 5 5 -5 4 18588.1 1155.93 5 6 -5 4 8473.02 846.557 5 7 -5 4 2676.61 533.164 5 8 -5 4 19099.9 1336.94 5 8 -5 4 21792.0 1290.53 11 9 -5 4 22965.5 1501.68 5 9 -5 4 21778.0 1346.66 11 10 -5 4 18319.2 1255.52 11 11 5 4 40052.6 1721.49 15 11 -5 4 41051.6 1793.44 11 12 5 4 4347.13 549.625 15 12 -5 4 4458.78 573.149 11 -12 -5 -4 4173.18 511.350 14 13 5 4 20551.3 1024.13 15 -13 -5 -4 21501.5 999.034 14 13 -5 4 19973.9 999.286 11 -13 6 4 489.629 205.662 19 13 -6 -4 751.031 243.384 8 -12 6 4 51345.5 1728.36 19 12 -6 -4 47790.9 1739.82 8 -11 6 4 3305.11 501.142 19 11 -6 -4 2571.93 473.628 8 -10 6 4 36363.8 1576.41 19 10 -6 -4 34399.4 1666.36 8 9 -6 -4 2160.38 464.446 8 -9 6 4 2242.62 406.726 19 9 6 -4 1001.13 419.676 7 -8 6 4 22699.1 1171.82 19 8 -6 -4 25097.1 1385.14 8 -8 -6 4 25466.9 1322.13 12 8 6 -4 22376.3 1596.12 7 7 6 -4 4545.12 712.559 7 -4 -6 4 86232.6 2359.16 5 -3 -6 4 27537.3 1298.77 5 -2 -6 4 28603.1 1290.76 5 -1 -6 4 66834.6 1931.74 5 0 6 4 26735.4 1160.58 4 0 -6 4 25681.1 1213.32 5 1 6 4 430.301 227.095 4 1 -6 4 479.069 311.377 5 2 -6 4 4101.16 541.850 5 3 -6 4 2932.84 510.808 5 4 -6 4 9682.26 865.682 5 5 -6 4 51485.2 2004.10 5 6 -6 4 4492.78 643.994 5 7 -6 4 2414.57 441.053 11 7 -6 4 2310.28 409.452 8 7 -6 4 3704.59 604.558 5 8 -6 4 6472.38 761.707 11 8 -6 4 5419.57 768.102 5 9 -6 4 7589.30 840.193 11 10 -6 4 7138.39 795.025 11 -10 -6 -4 7453.24 698.970 14 10 6 4 7136.43 715.320 15 11 6 4 2484.53 438.824 15 -11 -6 -4 1976.49 365.400 14 12 6 4 463.797 221.560 15 12 -6 4-247.704 274.605 11 -12 -6 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360.034 246.306 11 13 -7 4 10903.0 691.133 11 13 -8 -4 3886.02 399.945 8 12 -8 -4 9596.56 736.306 8 11 -8 -4 7525.28 743.970 8 10 -8 -4 594.700 375.856 8 -9 -8 4 212.329 171.319 17 9 -8 -4-23.8978 254.240 8 8 -8 -4 7732.53 812.808 8 -8 -8 4 7919.97 741.644 12 -7 -8 4 217.098 185.527 13 7 -8 -4-185.344 253.715 8 -7 -8 4-101.227 191.487 12 7 8 -4 237.369 321.338 7 -6 -8 4 50802.8 1785.00 13 -6 -8 4 47947.6 1726.52 12 6 -8 -4 49060.7 1851.98 8 -4 -8 4 35054.6 1637.89 5 -3 -8 4 316.226 287.560 5 -2 -8 4 42130.9 1722.77 5 -1 -8 4 2438.28 472.155 5 0 -8 4 26238.9 1366.06 5 1 -8 4 46567.3 1848.23 5 2 -8 4 56878.6 2092.90 5 3 -8 4 2750.37 518.377 5 4 -8 4 121283. 3234.67 5 5 -8 4 6479.99 789.468 5 -6 -8 -4 1920.92 396.041 17 6 -8 4 1427.55 384.045 11 6 -8 4 1435.02 446.706 5 7 -8 4 4835.06 668.610 11 -7 -8 -4 5127.22 613.134 17 7 -8 4 4826.05 720.546 5 8 -8 4 32633.9 1685.07 11 9 -8 4 21116.4 1368.78 11 10 -8 4 19691.1 1287.03 11 11 -8 4 106.482 239.438 11 12 -8 4 31836.1 1337.90 11 13 -8 4 517.224 164.877 11 12 -9 -4 1244.89 291.053 8 11 -9 -4 674.762 279.109 8 10 -9 -4 2809.58 489.816 8 -9 -9 4 331.056 224.953 17 9 -9 -4 126.304 245.522 8 8 -9 -4 5244.99 679.217 8 -7 -9 4 14206.8 1031.08 13 7 -9 -4 14763.1 1077.59 8 7 9 -4 14774.5 1283.68 7 -6 -9 4 11053.7 824.979 9 6 -9 -4 11780.3 935.072 8 -6 -9 4 11842.0 917.433 13 -5 -9 4 1347.44 297.250 9 -5 -9 4 576.668 226.848 13 5 -9 -4 1295.53 333.168 8 -4 -9 4 3717.96 597.848 5 -3 -9 4 6745.65 754.229 5 -2 -9 4 24190.2 1360.03 5 -1 -9 4 4861.87 654.615 5 0 -9 4 2031.39 425.029 5 1 -9 4 8530.35 849.635 5 2 -9 4 6196.80 752.180 5 3 -9 4 11787.8 1040.44 5 -4 -9 -4 3984.94 519.618 17 4 -9 4 3433.56 617.450 5 -5 -9 -4 10215.5 871.742 17 5 -9 4 10606.7 1049.63 5 5 -9 4 11062.0 912.691 11 -6 -9 -4 763.791 313.680 17 6 -9 4 213.108 242.934 11 6 -9 4 402.495 347.853 5 7 -9 4 584.030 302.474 11 8 -9 4 27744.1 1544.12 11 9 -9 4 2865.41 550.106 11 10 -9 4 1620.90 421.539 11 11 -9 4-44.2965 231.127 11 12 -9 4 1773.99 335.393 11 12 -10 -4 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1 5 36144.8 1481.66 4 -3 1 -5 147311. 2444.58 2 3 -1 5 156541. 3042.65 4 3 -1 5 154736. 2398.94 5 3 1 5 149346. 3134.88 4 4 -1 5 9268.84 792.644 4 4 -1 5 9570.29 643.511 5 5 -1 5 79258.6 1957.46 5 5 -1 5 77922.8 2365.50 4 8 -1 5 1629.91 378.036 15 8 1 5 1116.00 320.030 15 9 -1 5 14869.0 1101.31 15 9 1 5 13641.7 1057.59 15 10 1 5 26660.5 1521.38 15 10 -1 5 24726.2 1453.43 15 11 -1 5 6501.81 778.228 15 11 1 5 5703.27 729.286 15 12 -1 5 1932.83 451.522 15 12 1 5 1094.64 370.676 15 -12 -1 -5 1455.64 404.837 14 13 -1 5 14282.6 935.751 15 -13 -1 -5 15857.5 977.733 14 -13 1 -5 14936.2 927.280 14 13 1 5 13989.3 942.535 15 14 -1 5 490.506 192.920 15 14 1 5 285.166 199.929 15 -14 -1 -5 275.068 160.773 14 -14 1 -5 131.342 146.392 14 -14 2 5 1325.82 287.814 19 -14 -2 5 1110.68 209.610 19 -13 -2 5 409.289 223.060 19 -13 2 5 138.264 273.961 19 -12 2 5 20842.9 1237.80 19 -12 -2 5 21785.8 1192.13 19 -11 -2 5 6541.65 693.219 19 -11 2 5 5873.22 705.141 19 -10 -2 5 6721.81 720.181 19 10 -2 -5 6795.25 688.364 8 -9 2 5 3325.14 519.253 19 -9 -2 5 2764.30 457.100 19 9 -2 -5 2404.22 415.201 8 9 -2 -5 2847.25 618.008 7 9 2 -5 3677.31 726.724 7 8 -2 -5 15105.8 1181.91 7 8 2 -5 14967.3 1271.88 7 7 -2 -5 4504.50 625.059 7 7 2 -5 4947.77 743.881 7 6 -2 -5 57906.1 1941.25 7 6 2 -5 57146.6 2171.61 7 5 -2 -5 12406.7 820.305 7 -4 2 5 27881.3 1308.37 4 -3 -2 5 2818.26 463.763 4 -3 -2 5 3446.84 442.301 5 -3 2 5 2479.97 430.170 4 3 2 -5 2532.95 316.392 3 -2 -2 5 33035.2 1404.22 4 2 2 -5 31655.8 1050.45 3 -2 2 5 34756.9 1397.62 4 -2 -2 5 33729.9 1216.38 5 -1 -2 5 44843.8 1583.70 4 -1 2 5 44830.2 1557.78 4 -1 -2 5 41943.1 1296.87 5 1 2 -5 42892.0 1188.45 3 0 2 5 158484. 2951.27 4 0 -2 5 159352. 2455.41 5 0 2 -5 153124. 2272.86 3 1 2 5 1509.93 335.690 4 1 -2 5 935.313 214.106 5 -1 2 -5 1026.84 231.231 2 1 -2 5 1284.34 333.412 4 -2 2 -5 14116.4 764.713 2 2 -2 5 12724.1 844.683 4 2 -2 5 13412.3 748.208 5 2 2 5 13413.3 945.793 4 3 -2 5 1317.62 344.600 4 -3 2 -5 916.660 235.995 2 3 -2 5 1029.27 257.299 5 4 -2 5 88450.7 2330.23 4 4 -2 5 85167.4 2048.35 5 5 -2 5 4827.53 560.911 4 5 -2 5 4070.27 504.864 5 6 -2 5 16502.0 1029.13 5 7 -2 5 2570.03 439.176 5 8 -2 5 17593.2 1144.28 15 8 2 5 17721.1 1144.38 15 8 -2 5 15556.1 1084.68 5 9 -2 5 1809.93 373.271 11 9 -2 5 1488.60 391.741 15 9 2 5 1264.54 358.323 15 10 -2 5 19393.9 1282.89 15 10 2 5 19931.7 1303.01 15 11 -2 5 3643.23 588.518 15 11 2 5 3424.04 583.562 15 -12 -2 -5 12778.1 973.680 14 -12 2 -5 11624.3 885.798 14 12 2 5 11839.9 941.503 15 12 -2 5 13190.7 987.316 15 13 -2 5 7034.96 647.547 15 13 2 5 6957.97 675.803 15 -13 -2 -5 7174.17 661.742 14 -13 2 -5 8982.95 696.067 14 14 2 5 3167.17 376.430 15 -14 2 -5 4112.42 391.176 14 -14 -2 -5 2938.39 361.362 14 -14 3 5 9831.29 633.787 19 -13 3 5 13998.1 908.486 19 -13 -3 5 14327.0 804.684 19 -12 3 5 6515.05 703.202 19 -12 -3 5 6723.81 651.359 19 -11 -3 5 21881.2 1215.44 19 -11 3 5 22538.5 1318.68 19 11 -3 -5 21970.3 1224.72 8 -10 -3 5 5252.27 609.930 19 -10 3 5 4199.46 599.858 19 10 -3 -5 4899.03 626.789 8 9 -3 -5 14783.2 1051.03 8 -9 -3 5 14596.2 1000.32 19 -9 3 5 14401.9 1042.91 19 9 3 -5 14985.1 1322.25 7 -8 3 5 7671.71 727.596 19 -8 -3 5 7493.70 696.549 19 -8 -3 5 8809.90 789.404 12 8 3 -5 9070.42 1019.15 7 7 3 -5 5178.06 771.637 7 6 3 -5 2597.22 514.528 7 -4 3 5 36982.1 1496.84 4 3 3 -5 497.345 184.933 3 -3 3 5 123.501 209.875 4 -3 -3 5 12.9516 219.628 5 2 3 -5 4443.82 432.931 3 -2 -3 5 3349.73 487.510 4 -2 -3 5 4259.71 477.544 5 -2 3 5 4056.21 504.206 4 -1 -3 5 106.435 243.791 4 -1 -3 5 637.286 263.247 5 1 3 -5 76.6790 169.395 3 -1 3 5-25.4237 209.214 4 0 -3 5 5583.15 523.945 5 0 3 -5 5221.13 457.562 3 0 -3 5 4889.23 532.496 4 0 3 5 5101.43 567.134 4 1 -3 5 10229.0 757.852 4 1 -3 5 10517.2 704.477 5 1 3 5 9625.33 799.371 4 2 -3 5 38898.7 1441.01 4 2 -3 5 38998.1 1355.92 5 2 3 5 40628.7 1645.19 4 -2 3 -5 38399.3 1329.18 2 3 -3 5-70.0125 180.755 5 3 -3 5 226.345 231.966 4 4 -3 5 724.567 246.440 4 4 -3 5 1028.80 301.832 5 5 -3 5 11264.6 842.645 5 6 -3 5 4121.74 559.186 5 7 -3 5-56.6834 220.033 5 8 -3 5 18466.8 1154.77 15 8 3 5 16860.2 1107.39 15 8 -3 5 17838.1 1229.03 5 8 -3 5 18629.7 1152.61 11 9 -3 5 3012.51 494.001 11 9 -3 5 2518.94 479.078 15 9 3 5 2254.32 441.685 15 9 -3 5 2764.45 534.734 5 10 -3 5 4060.11 593.091 15 10 3 5 6294.97 745.030 15 10 -3 5 5579.17 670.705 11 11 -3 5 580.556 269.686 11 11 -3 5 388.949 216.459 15 11 3 5 451.362 280.924 15 -11 -3 -5 93.7150 225.712 14 12 -3 5 103.344 207.626 15 12 3 5 776.822 316.032 15 -12 -3 -5 1019.85 348.657 14 -12 3 -5 490.252 237.221 14 13 3 5 191.304 193.477 15 13 -3 5 434.484 224.107 15 -13 -3 -5 363.158 206.214 14 -13 3 -5 590.181 217.609 14 14 3 5 8314.64 559.640 15 -14 -3 -5 7385.34 525.134 14 -14 4 5 1498.56 259.937 19 -13 4 5 13016.5 838.346 19 -12 4 5 85.3162 209.739 19 12 -4 -5-121.627 220.935 8 -11 4 5 27364.0 1412.56 19 11 -4 -5 25691.3 1355.65 8 -10 4 5 4403.11 598.362 19 10 -4 -5 4177.83 601.399 8 -9 4 5 2463.05 458.365 19 9 -4 -5 1859.13 428.861 8 9 4 -5 3436.51 690.393 7 -8 4 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-3 13-163.809 167.835 18 3 -3 13 29407.5 1124.91 19 3 -3 13 30758.5 1133.50 18 4 -3 13 329.616 151.458 18 -4 -4 13 7008.77 505.875 19 -3 -4 13 372.404 188.589 19 -2 -4 13 3189.55 397.466 19 -1 -4 13 1346.06 276.799 19 0 -4 13 4409.71 472.586 19 1 -4 13 1858.12 335.836 19 2 -4 13 11853.7 730.601 19 3 -4 13 1149.44 247.458 19 3 -4 13 810.571 215.785 18 4 -4 13 2882.00 332.555 18 -3 -5 13 1141.45 215.513 19 -2 -5 13 594.852 197.850 19 -1 -5 13-18.7700 165.599 19 0 -5 13 7299.77 555.200 19 1 -5 13 4180.97 434.259 19 2 -5 13 8272.31 572.933 19 3 -5 13 626.448 171.075 19 0 -6 13 7613.98 512.237 19 0 0 0 0.00 0.00 0 TITL LFF_3 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 12.859388 14.759847 11.430098 90.0000 91.3025 90.0000 ZERR 9.00 0.000390 0.000414 0.000356 0.0000 0.0027 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 TREF HKLF 4 END ; _shelx_hkl_checksum 62821 _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{5135942d-dfe2-4351-9398-9740c65aa103}" "_publcif_info_datablock.publ_exptl" loop_ _publcif_info_cif.paper_type CE loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{5135942d-dfe2-4351-9398-9740c65aa103}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? _publcif_funding_html ;Natural Science Foundation of China (grant No. 21571118 and 21671124). ;