#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 1 _journal_year 2022 _journal_page_first 63 _journal_page_last 68 #============================================================================= _audit_creation_date 2020-07-30 _audit_creation_method 'by CrystalStructure 4.3' _audit_update_record ? _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2019). CrystalStructure. Version 4.3. Rigaku Corporation, Tokyo, Japan. Burla, M. C., Caliandro, R., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G. (2014). In preparation. SIR2014 Sheldrick, G.M. (2008) SHELXL Version 2018/3, Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; #============================================================================== data_CA3 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H12 N4 O' _chemical_formula_moiety 'C13 H12 N4 O' _chemical_formula_weight 240.26 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' _space_group_IT_number 60 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '1/2-X,1/2-Y,1/2+Z' 3 '1/2+X,1/2-Y,-Z' 4 '-X,+Y,1/2-Z' 5 '-X,-Y,-Z' 6 '-1/2+X,-1/2+Y,-1/2-Z' 7 '-1/2-X,-1/2+Y,+Z' 8 '+X,-Y,-1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 18.0824(3) _cell_length_b 7.86555(14) _cell_length_c 16.1614(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2298.60(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 32237 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 103 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008.00 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.991 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 103 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 36729 _diffrn_reflns_av_unetI/netI 0.0124 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 2.521 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 2633 _reflns_number_gt 2504 _reflns_threshold_expression F^2^>2.0\s(F^2^) _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0974 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2633 _refine_ls_number_parameters 164 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0546P)^2^+1.1177P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.44 _refine_diff_density_min -0.27 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 O1 O 0.15973(4) 0.41076(10) 0.09546(5) 0.01710(19) Uani 1 1 d . . . . . N1 N 0.44370(5) 0.30633(12) -0.08948(6) 0.0154(2) Uani 1 1 d . . . . . N2 N 0.28399(5) 0.44843(11) 0.00681(5) 0.01219(19) Uani 1 1 d . . . . . N3 N 0.25690(5) 0.57796(11) 0.05560(5) 0.01244(19) Uani 1 1 d . . . . . H3 H 0.280115 0.675886 0.059959 0.015 Uiso 1 1 calc R U . . . N4 N 0.18287(5) 0.92209(12) 0.24241(6) 0.0164(2) Uani 1 1 d . . . . . C1 C 0.46907(6) 0.16913(14) -0.12996(7) 0.0179(2) Uani 1 1 d . . . . . H1 H 0.521052 0.154665 -0.134727 0.021 Uiso 1 1 calc R U . . . C2 C 0.42332(6) 0.04734(14) -0.16519(7) 0.0184(2) Uani 1 1 d . . . . . H2 H 0.443604 -0.047878 -0.193344 0.022 Uiso 1 1 calc R U . . . C3 C 0.34712(6) 0.06765(14) -0.15840(7) 0.0168(2) Uani 1 1 d . . . . . H3A H 0.314319 -0.012693 -0.182478 0.020 Uiso 1 1 calc R U . . . C4 C 0.32000(6) 0.20718(13) -0.11588(6) 0.0138(2) Uani 1 1 d . . . . . H4 H 0.268230 0.223858 -0.110037 0.017 Uiso 1 1 calc R U . . . C5 C 0.36986(6) 0.32286(13) -0.08176(6) 0.0121(2) Uani 1 1 d . . . . . C6 C 0.34411(5) 0.47381(13) -0.03400(6) 0.0126(2) Uani 1 1 d . . . . . C7 C 0.39090(6) 0.63125(14) -0.03586(7) 0.0190(2) Uani 1 1 d . . . . . H7A H 0.362427 0.727381 -0.014110 0.023 Uiso 1 1 calc R U . . . H7B H 0.405797 0.655313 -0.092979 0.023 Uiso 1 1 calc R U . . . H7C H 0.435050 0.613918 -0.001720 0.023 Uiso 1 1 calc R U . . . C8 C 0.19259(6) 0.54740(13) 0.09672(6) 0.0122(2) Uani 1 1 d . . . . . C9 C 0.16351(6) 0.69712(13) 0.14371(6) 0.0124(2) Uani 1 1 d . . . . . C10 C 0.20637(6) 0.78411(13) 0.20140(6) 0.0138(2) Uani 1 1 d . . . . . H10 H 0.254888 0.743526 0.212302 0.017 Uiso 1 1 calc R U . . . C11 C 0.11510(6) 0.97909(14) 0.22387(7) 0.0177(2) Uani 1 1 d . . . . . H11 H 0.098428 1.080023 0.250222 0.021 Uiso 1 1 calc R U . . . C12 C 0.06763(6) 0.89938(15) 0.16835(7) 0.0181(2) Uani 1 1 d . . . . . H12 H 0.019697 0.943962 0.157954 0.022 Uiso 1 1 calc R U . . . C13 C 0.09181(6) 0.75333(14) 0.12846(6) 0.0155(2) Uani 1 1 d . . . . . H13 H 0.060225 0.693265 0.091694 0.019 Uiso 1 1 calc 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 O1 0.0153(4) 0.0134(4) 0.0226(4) -0.0025(3) 0.0019(3) -0.0027(3) N1 0.0128(4) 0.0163(4) 0.0172(4) -0.0008(3) 0.0003(3) 0.0006(3) N2 0.0141(4) 0.0103(4) 0.0122(4) -0.0006(3) -0.0007(3) 0.0024(3) N3 0.0140(4) 0.0094(4) 0.0139(4) -0.0013(3) 0.0015(3) -0.0002(3) N4 0.0167(4) 0.0162(4) 0.0163(4) -0.0021(3) 0.0005(3) 0.0004(3) C1 0.0138(5) 0.0191(5) 0.0207(5) -0.0008(4) 0.0019(4) 0.0030(4) C2 0.0209(5) 0.0153(5) 0.0189(5) -0.0030(4) 0.0032(4) 0.0036(4) C3 0.0193(5) 0.0148(5) 0.0163(5) -0.0021(4) -0.0002(4) -0.0022(4) C4 0.0128(5) 0.0149(5) 0.0137(5) 0.0005(4) 0.0005(4) -0.0004(4) C5 0.0137(5) 0.0113(5) 0.0114(4) 0.0014(4) 0.0007(4) 0.0004(4) C6 0.0136(4) 0.0114(5) 0.0127(5) 0.0000(4) -0.0015(4) 0.0004(4) C7 0.0187(5) 0.0147(5) 0.0235(5) -0.0046(4) 0.0060(4) -0.0036(4) C8 0.0125(4) 0.0119(5) 0.0123(4) 0.0004(4) -0.0019(4) 0.0015(4) C9 0.0144(5) 0.0110(4) 0.0120(4) 0.0015(4) 0.0025(4) -0.0002(4) C10 0.0134(5) 0.0136(5) 0.0146(5) 0.0008(4) 0.0010(4) 0.0005(4) C11 0.0187(5) 0.0166(5) 0.0178(5) -0.0034(4) 0.0028(4) 0.0035(4) C12 0.0142(5) 0.0218(5) 0.0184(5) -0.0011(4) 0.0004(4) 0.0052(4) C13 0.0142(5) 0.0181(5) 0.0142(5) -0.0009(4) -0.0001(4) -0.0007(4) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2014 (Burla, et al., 2014)' _computing_structure_refinement 'SHELXL Version 2018/3 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.3 (Rigaku, 2019)' _computing_molecular_graphics 'CrystalStructure 4.3' #============================================================================== # 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 O1 C8 1.2282(13) . ? N1 C1 1.3427(14) . ? N1 C5 1.3472(13) . ? N2 C6 1.2871(13) . ? N2 N3 1.3783(12) . ? N3 C8 1.3608(13) . ? N3 H3 0.8800 . ? N4 C11 1.3388(14) . ? N4 C10 1.3408(13) . ? C1 C2 1.3878(16) . ? C1 H1 0.9500 . ? C2 C3 1.3915(15) . ? C2 H2 0.9500 . ? C3 C4 1.3846(15) . ? C3 H3A 0.9500 . ? C4 C5 1.3946(14) . ? C4 H4 0.9500 . ? C5 C6 1.4908(14) . ? C6 C7 1.5002(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.4966(14) . ? C9 C13 1.3919(14) . ? C9 C10 1.3922(14) . ? C10 H10 0.9500 . ? C11 C12 1.3910(15) . ? C11 H11 0.9500 . ? C12 C13 1.3879(15) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? 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 C1 N1 C5 117.47(9) . . ? C6 N2 N3 118.60(9) . . ? C8 N3 N2 116.90(8) . . ? C8 N3 H3 121.5 . . ? N2 N3 H3 121.5 . . ? C11 N4 C10 116.78(9) . . ? N1 C1 C2 123.43(10) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.60(10) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 118.74(10) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 118.98(9) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.76(9) . . ? N1 C5 C6 115.75(9) . . ? C4 C5 C6 121.49(9) . . ? N2 C6 C5 113.93(9) . . ? N2 C6 C7 127.93(10) . . ? C5 C6 C7 118.09(9) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 N3 124.04(9) . . ? O1 C8 C9 121.81(9) . . ? N3 C8 C9 114.14(9) . . ? C13 C9 C10 118.75(9) . . ? C13 C9 C8 119.17(9) . . ? C10 C9 C8 122.07(9) . . ? N4 C10 C9 123.53(9) . . ? N4 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N4 C11 C12 123.93(10) . . ? N4 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C13 C12 C11 118.57(10) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C9 118.30(10) . . ? C12 C13 H13 120.8 . . ? C9 C13 H13 120.8 . . ? 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 C6 N2 N3 C8 178.93(9) . . . . ? C5 N1 C1 C2 1.41(16) . . . . ? N1 C1 C2 C3 -0.04(17) . . . . ? C1 C2 C3 C4 -0.84(16) . . . . ? C2 C3 C4 C5 0.34(15) . . . . ? C1 N1 C5 C4 -1.94(15) . . . . ? C1 N1 C5 C6 178.04(9) . . . . ? C3 C4 C5 N1 1.10(15) . . . . ? C3 C4 C5 C6 -178.88(9) . . . . ? N3 N2 C6 C5 177.57(8) . . . . ? N3 N2 C6 C7 0.13(16) . . . . ? N1 C5 C6 N2 -147.36(9) . . . . ? C4 C5 C6 N2 32.62(13) . . . . ? N1 C5 C6 C7 30.35(13) . . . . ? C4 C5 C6 C7 -149.68(10) . . . . ? N2 N3 C8 O1 3.17(15) . . . . ? N2 N3 C8 C9 -175.91(8) . . . . ? O1 C8 C9 C13 -54.36(14) . . . . ? N3 C8 C9 C13 124.75(10) . . . . ? O1 C8 C9 C10 126.73(11) . . . . ? N3 C8 C9 C10 -54.17(13) . . . . ? C11 N4 C10 C9 -1.93(15) . . . . ? C13 C9 C10 N4 -1.29(16) . . . . ? C8 C9 C10 N4 177.63(9) . . . . ? C10 N4 C11 C12 3.12(16) . . . . ? N4 C11 C12 C13 -1.02(17) . . . . ? C11 C12 C13 C9 -2.32(16) . . . . ? C10 C9 C13 C12 3.39(15) . . . . ? C8 C9 C13 C12 -175.56(9) . . . . ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; TITL CA3 shelxl.res created by SHELXL-2018/3 at 10:39:25 on 30-Jul-2020 CELL 0.71075 18.08240 7.86555 16.16140 90.00000 90.00000 90.00000 ZERR 8 0.00033 0.00014 0.00029 0.00000 0.00000 0.00000 LATT 1 SYMM .50-X, .50-Y, .50+Z SYMM .50+X, .50-Y, -Z SYMM -X, +Y, .50-Z SFAC C H N O UNIT 104 96 32 8 SHEL 8.147145 0.769625 L.S. 5 FMAP 2 PLAN 10 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -170.0 ACTA SIZE 0.120 0.110 0.100 WGHT 0.054600 1.117700 FVAR 1.08082 O1 4 0.159734 0.410760 0.095457 11.00000 0.01532 0.01341 = 0.02256 -0.00246 0.00193 -0.00269 N1 3 0.443698 0.306327 -0.089480 11.00000 0.01279 0.01633 = 0.01723 -0.00077 0.00026 0.00064 N2 3 0.283989 0.448435 0.006814 11.00000 0.01409 0.01029 = 0.01218 -0.00064 -0.00070 0.00235 N3 3 0.256899 0.577965 0.055602 11.00000 0.01402 0.00938 = 0.01392 -0.00129 0.00155 -0.00021 AFIX 43 H3 2 0.280115 0.675886 0.059959 11.00000 -1.20000 AFIX 0 N4 3 0.182868 0.922089 0.242410 11.00000 0.01668 0.01622 = 0.01625 -0.00215 0.00047 0.00043 C1 1 0.469067 0.169127 -0.129957 11.00000 0.01381 0.01909 = 0.02066 -0.00079 0.00192 0.00304 AFIX 43 H1 2 0.521052 0.154665 -0.134727 11.00000 -1.20000 AFIX 0 C2 1 0.423321 0.047341 -0.165187 11.00000 0.02093 0.01534 = 0.01891 -0.00297 0.00316 0.00363 AFIX 43 H2 2 0.443604 -0.047878 -0.193344 11.00000 -1.20000 AFIX 0 C3 1 0.347116 0.067649 -0.158398 11.00000 0.01934 0.01477 = 0.01630 -0.00214 -0.00025 -0.00223 AFIX 43 H3A 2 0.314319 -0.012693 -0.182478 11.00000 -1.20000 AFIX 0 C4 1 0.320002 0.207181 -0.115878 11.00000 0.01284 0.01485 = 0.01369 0.00051 0.00051 -0.00038 AFIX 43 H4 2 0.268230 0.223858 -0.110037 11.00000 -1.20000 AFIX 0 C5 1 0.369863 0.322859 -0.081758 11.00000 0.01366 0.01133 = 0.01141 0.00140 0.00067 0.00043 C6 1 0.344105 0.473811 -0.034002 11.00000 0.01360 0.01143 = 0.01267 0.00005 -0.00147 0.00041 C7 1 0.390901 0.631254 -0.035864 11.00000 0.01872 0.01473 = 0.02354 -0.00463 0.00598 -0.00364 AFIX 137 H7A 2 0.362427 0.727381 -0.014110 11.00000 -1.20000 H7B 2 0.405797 0.655313 -0.092979 11.00000 -1.20000 H7C 2 0.435050 0.613918 -0.001720 11.00000 -1.20000 AFIX 0 C8 1 0.192588 0.547403 0.096720 11.00000 0.01248 0.01188 = 0.01228 0.00035 -0.00187 0.00149 C9 1 0.163514 0.697118 0.143711 11.00000 0.01442 0.01095 = 0.01196 0.00148 0.00249 -0.00019 C10 1 0.206374 0.784112 0.201403 11.00000 0.01337 0.01358 = 0.01459 0.00083 0.00101 0.00053 AFIX 43 H10 2 0.254888 0.743526 0.212302 11.00000 -1.20000 AFIX 0 C11 1 0.115099 0.979087 0.223874 11.00000 0.01873 0.01659 = 0.01785 -0.00339 0.00282 0.00350 AFIX 43 H11 2 0.098428 1.080023 0.250222 11.00000 -1.20000 AFIX 0 C12 1 0.067633 0.899384 0.168350 11.00000 0.01425 0.02182 = 0.01838 -0.00107 0.00040 0.00516 AFIX 43 H12 2 0.019697 0.943962 0.157954 11.00000 -1.20000 AFIX 0 C13 1 0.091809 0.753331 0.128463 11.00000 0.01418 0.01806 = 0.01425 -0.00091 -0.00008 -0.00066 AFIX 43 H13 2 0.060225 0.693265 0.091694 11.00000 -1.20000 AFIX 0 HKLF 4 REM CA3 REM wR2 = 0.0988, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0383 for 2504 Fo > 4sig(Fo) and 0.0402 for all 2633 data REM 164 parameters refined using 0 restraints END WGHT 0.0524 1.1275 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y+1/2, z HTAB N3 O1_$1 HTAB N3 N2_$1 EQIV $2 x+1/2, -y+1/2, -z HTAB C1 O1_$2 HTAB C7 O1_$1 EQIV $3 x-1/2, -y+3/2, -z HTAB C12 N1_$3 REM Highest difference peak 0.442, deepest hole -0.273, 1-sigma level 0.065 Q1 1 0.3572 0.3980 -0.0560 11.00000 0.05 0.44 Q2 1 0.1776 0.6286 0.1188 11.00000 0.05 0.44 Q3 1 0.3636 0.5510 -0.0332 11.00000 0.05 0.40 Q4 1 0.3450 0.2664 -0.1033 11.00000 0.05 0.39 Q5 1 0.0907 0.9218 0.2052 11.00000 0.05 0.39 Q6 1 0.0773 0.8110 0.1595 11.00000 0.05 0.38 Q7 1 0.1279 0.7267 0.1350 11.00000 0.05 0.38 Q8 1 0.3378 0.1426 -0.1376 11.00000 0.05 0.38 Q9 1 0.1799 0.7279 0.1772 11.00000 0.05 0.37 Q10 1 0.1873 0.7578 0.1648 11.00000 0.05 0.36 ; _shelx_res_checksum 67239 _shelx_hkl_file ; -2 0 025794.84 1622.59 2 0 020692.20 1345.92 2 0 021394.76 1360.39 0 0 2 3592.96 58.08 0 0 -2 3498.81 61.93 0 0 -2 3686.02 59.98 2 0 1 0.56 0.89 -2 0 1 1.38 0.40 2 0 -1 1.62 0.43 -2 0 -1 2.94 0.84 2 0 -1 1.64 1.14 -2 0 1 3.41 1.10 0 -1 0 4.78 0.31 0 -1 0 2.30 0.77 1 0 2 5061.84 100.99 -1 0 -2 4970.09 105.70 1 0 2 5137.24 109.07 1 0 -2 5182.97 113.72 -1 0 -2 5211.87 103.69 1 0 -2 5067.59 110.58 -1 0 2 4804.19 106.26 -1 0 2 5173.23 99.33 -1 0 2 4955.42 106.36 1 -1 0 2645.58 38.66 -1 1 0 2634.06 38.28 -1 1 0 2537.69 37.77 -1 -1 0 2634.11 37.91 1 1 0 2603.40 37.66 1 -1 0 2452.44 36.68 -1 -1 0 2498.03 37.90 1 1 0 2476.22 37.86 0 -1 1 -0.88 1.80 0 -1 -1 -1.20 1.12 0 -1 -1 -0.55 0.61 0 1 1 -1.04 0.89 0 -1 -1 -2.72 1.52 0 1 -1 -4.05 1.77 1 -1 -1 57.79 1.48 -1 1 -1 55.09 1.31 -1 -1 1 60.64 1.71 1 1 1 54.53 1.71 -1 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33.01 4 -4 -3 1988.70 36.37 4 4 3 2056.23 43.21 4 -4 3 2043.64 33.50 -4 -4 -3 1972.40 38.01 -4 4 -3 2016.46 32.24 -4 -4 -3 1962.59 37.22 4 4 -3 1998.50 35.67 -4 -4 3 2105.04 37.41 -4 -4 3 1967.88 29.38 -4 4 3 2061.54 36.15 4 4 3 2007.58 38.56 -4 -4 3 2003.44 33.95 4 -4 3 1952.58 35.56 9 0 -5 -0.23 3.46 -9 0 -5 -3.71 2.45 -9 0 -5 5.83 4.09 -9 0 5 0.52 1.34 9 0 5 1.93 4.54 -9 0 5 -0.83 3.34 9 0 -5 -1.12 1.68 -9 0 -5 -2.02 2.15 -8 3 1 290.10 7.39 -8 3 1 277.48 5.21 8 -3 1 282.65 5.06 -8 -3 -1 298.40 6.27 8 3 -1 303.14 6.20 -8 -3 -1 295.16 7.54 8 3 1 267.89 8.23 8 -3 -1 290.37 8.37 -8 3 -1 279.12 5.13 -8 -3 1 286.79 5.93 8 3 1 290.28 8.52 -8 -3 1 289.36 7.78 8 -3 -1 278.63 4.64 -8 3 -1 287.91 7.20 8 -3 1 298.92 5.85 2 3 -7 540.11 7.98 2 3 7 519.11 7.80 2 3 -7 515.01 7.17 -2 3 -7 499.99 8.38 -2 -3 7 508.68 8.94 2 -3 -7 515.12 7.30 2 3 7 530.49 8.76 -2 3 7 501.85 8.10 2 -3 7 518.93 7.91 -2 -3 7 540.54 8.44 -2 3 7 502.93 9.54 -2 -3 -7 526.59 9.35 2 -3 7 513.48 4.98 -2 -3 7 539.42 7.09 -2 3 -7 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