_publ_contact_author_name 'Franc Perdih' _publ_contact_author_address ; Faculty of Chemistry and Chemical Technology University of Ljubljana Vecna pot 113, P. O. Box 537 SI-1000 Ljubljana Slovenia ; _publ_contact_author_email franc.perdih@fkkt.uni-lj.si loop_ _publ_author_name _publ_author_address 'Lovel Kukuljan' ; Faculty of Chemistry and Chemical Technology University of Ljubljana Vecna pot 113, P. O. Box 537 SI-1000 Ljubljana Slovenia ; 'Kristof Kranjc' ; Faculty of Chemistry and Chemical Technology University of Ljubljana Vecna pot 113, P. O. Box 537 SI-1000 Ljubljana Slovenia ; 'Franc Perdih' ; Faculty of Chemistry and Chemical Technology University of Ljubljana Vecna pot 113, P. O. Box 537 SI-1000 Ljubljana Slovenia ; _publ_requested_journal 'Acta Chim. Slov.' _publ_section_title ; Synthesis and Structural Evaluation of 5-Methyl-6-acetyl Substituted Indole and Gramine ; data_7 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H11 N O' _chemical_formula_sum 'C11 H11 N O' _chemical_formula_weight 173.21 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' _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' _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, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.2632(7) _cell_length_b 5.2027(2) _cell_length_c 9.4496(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 897.88(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1025 _cell_measurement_theta_min 4.8020 _cell_measurement_theta_max 73.3060 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_F_000 368 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.656 _shelx_estimated_absorpt_T_min 0.827 _shelx_estimated_absorpt_T_max 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56380 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4933 _diffrn_reflns_number 1994 _diffrn_reflns_av_unetI/netI 0.0261 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.843 _diffrn_reflns_theta_max 70.044 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.749 _diffrn_reflns_point_group_measured_fraction_full 0.761 _reflns_number_total 1280 _reflns_number_gt 1172 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.416 _reflns_Friedel_fraction_max 0.472 _reflns_Friedel_fraction_full 0.491 _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 'CrysAlis PRO (Agilent, 2013)' _computing_cell_refinement 'CrysAlis PRO (Agilent, 2013)' _computing_data_reduction 'CrysAlis PRO (Agilent, 2013)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0413P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_ls_extinction_coef 0.0110(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Flack x determined using 327 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.1(2) _chemical_absolute_configuration . _refine_ls_number_reflns 1280 _refine_ls_number_parameters 121 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.17960(12) -0.1721(5) 0.0749(2) 0.0756(6) Uani 1 1 d . . . . . N1 N 0.39789(12) 0.5175(4) 0.3697(2) 0.0578(6) Uani 1 1 d . . . . . H1 H 0.3744 0.6177 0.4261 0.069 Uiso 1 1 calc R U . . . C1 C 0.47210(15) 0.5114(6) 0.3517(3) 0.0652(7) Uani 1 1 d . . . . . H1A H 0.5052 0.6169 0.3988 0.078 Uiso 1 1 calc R U . . . C2 C 0.49055(13) 0.3305(6) 0.2557(3) 0.0637(7) Uani 1 1 d . . . . . H2 H 0.5377 0.2892 0.2261 0.076 Uiso 1 1 calc R U . . . C3 C 0.42438(12) 0.2151(5) 0.2086(3) 0.0505(6) Uani 1 1 d . . . . . C4 C 0.40678(14) 0.0214(5) 0.1116(3) 0.0534(6) Uani 1 1 d . . . . . H4 H 0.4442 -0.0613 0.0626 0.064 Uiso 1 1 calc R U . . . C5 C 0.33502(13) -0.0494(5) 0.0871(2) 0.0485(5) Uani 1 1 d . . . . . C6 C 0.27762(12) 0.0808(4) 0.1616(2) 0.0462(5) Uani 1 1 d . . . . . C7 C 0.29462(12) 0.2722(5) 0.2596(2) 0.0481(5) Uani 1 1 d . . . . . H7 H 0.2576 0.3560 0.3090 0.058 Uiso 1 1 calc R U . . . C8 C 0.36733(12) 0.3359(5) 0.2823(2) 0.0477(5) Uani 1 1 d . . . . . C9 C 0.32080(18) -0.2590(5) -0.0189(3) 0.0598(6) Uani 1 1 d . . . . . H9A H 0.3012 -0.4068 0.0287 0.090 Uiso 1 1 calc R U . . . H9B H 0.3658 -0.3046 -0.0649 0.090 Uiso 1 1 calc R U . . . H9C H 0.2863 -0.1995 -0.0881 0.090 Uiso 1 1 calc R U . . . C10 C 0.19925(15) 0.0221(5) 0.1379(3) 0.0541(6) Uani 1 1 d . . . . . C11 C 0.14216(13) 0.2022(6) 0.1944(4) 0.0683(8) Uani 1 1 d . . . . . H11A H 0.1390 0.1839 0.2953 0.102 Uiso 1 1 calc R U . . . H11B H 0.0956 0.1622 0.1526 0.102 Uiso 1 1 calc R U . . . H11C H 0.1553 0.3759 0.1714 0.102 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 0.0742(13) 0.0725(13) 0.0801(14) -0.0130(12) -0.0054(11) -0.0204(11) N1 0.0608(12) 0.0618(13) 0.0508(11) -0.0102(10) 0.0009(9) -0.0046(10) C1 0.0544(12) 0.0755(17) 0.0657(18) -0.0074(14) -0.0096(13) -0.0087(13) C2 0.0493(11) 0.0723(17) 0.0695(17) -0.0101(15) -0.0055(12) 0.0014(12) C3 0.0510(11) 0.0539(13) 0.0466(12) 0.0014(10) 0.0008(10) 0.0019(10) C4 0.0548(12) 0.0558(14) 0.0497(14) -0.0028(11) 0.0046(11) 0.0050(11) C5 0.0621(13) 0.0442(11) 0.0394(11) 0.0036(10) 0.0024(10) 0.0007(11) C6 0.0530(11) 0.0442(11) 0.0413(10) 0.0070(9) 0.0020(9) -0.0052(10) C7 0.0514(10) 0.0488(12) 0.0440(11) -0.0001(10) 0.0060(9) -0.0021(10) C8 0.0544(11) 0.0489(12) 0.0397(11) 0.0000(9) 0.0005(9) -0.0030(10) C9 0.0789(17) 0.0507(13) 0.0499(13) -0.0040(11) 0.0030(12) -0.0067(13) C10 0.0587(14) 0.0541(14) 0.0494(13) 0.0123(12) -0.0025(10) -0.0102(11) C11 0.0501(11) 0.0627(16) 0.092(2) 0.0109(16) -0.0048(13) -0.0004(12) _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 C10 1.226(4) . ? N1 C1 1.366(3) . ? N1 C8 1.374(3) . ? N1 H1 0.8600 . ? C1 C2 1.349(4) . ? C1 H1A 0.9300 . ? C2 C3 1.421(3) . ? C2 H2 0.9300 . ? C3 C4 1.400(4) . ? C3 C8 1.402(3) . ? C4 C5 1.381(3) . ? C4 H4 0.9300 . ? C5 C6 1.433(3) . ? C5 C9 1.503(4) . ? C6 C7 1.394(3) . ? C6 C10 1.481(3) . ? C7 C8 1.385(3) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.500(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? 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 C8 108.2(2) . . ? C1 N1 H1 125.9 . . ? C8 N1 H1 125.9 . . ? C2 C1 N1 110.3(2) . . ? C2 C1 H1A 124.8 . . ? N1 C1 H1A 124.8 . . ? C1 C2 C3 107.0(2) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? C4 C3 C8 118.5(2) . . ? C4 C3 C2 134.8(2) . . ? C8 C3 C2 106.7(2) . . ? C5 C4 C3 121.3(2) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 119.1(2) . . ? C4 C5 C9 118.0(2) . . ? C6 C5 C9 123.0(2) . . ? C7 C6 C5 120.1(2) . . ? C7 C6 C10 117.6(2) . . ? C5 C6 C10 122.3(2) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N1 C8 C7 130.3(2) . . ? N1 C8 C3 107.8(2) . . ? C7 C8 C3 121.9(2) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C6 121.8(3) . . ? O1 C10 C11 119.0(2) . . ? C6 C10 C11 119.3(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 C8 N1 C1 C2 -0.3(3) . . . . ? N1 C1 C2 C3 0.5(4) . . . . ? C1 C2 C3 C4 179.6(3) . . . . ? C1 C2 C3 C8 -0.5(3) . . . . ? C8 C3 C4 C5 0.6(4) . . . . ? C2 C3 C4 C5 -179.5(3) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C3 C4 C5 C9 180.0(2) . . . . ? C4 C5 C6 C7 -1.4(3) . . . . ? C9 C5 C6 C7 179.4(2) . . . . ? C4 C5 C6 C10 178.0(2) . . . . ? C9 C5 C6 C10 -1.2(3) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? C10 C6 C7 C8 -178.7(2) . . . . ? C1 N1 C8 C7 -178.3(3) . . . . ? C1 N1 C8 C3 0.0(3) . . . . ? C6 C7 C8 N1 178.7(2) . . . . ? C6 C7 C8 C3 0.6(3) . . . . ? C4 C3 C8 N1 -179.8(2) . . . . ? C2 C3 C8 N1 0.3(3) . . . . ? C4 C3 C8 C7 -1.3(4) . . . . ? C2 C3 C8 C7 178.8(2) . . . . ? C7 C6 C10 O1 -166.2(2) . . . . ? C5 C6 C10 O1 14.4(4) . . . . ? C7 C6 C10 C11 12.7(3) . . . . ? C5 C6 C10 C11 -166.6(2) . . . . ? 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 N1 H1 O1 0.86 2.04 2.893(3) 174.2 3_565 C11 H11C O1 0.96 2.56 3.513(4) 171.2 1_565 _refine_diff_density_max 0.124 _refine_diff_density_min -0.096 _refine_diff_density_rms 0.027 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL cu453 in Pca21 #29 CELL 1.54184 18.2632 5.2027 9.4496 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0002 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, Y, 1/2 + Z SYMM 1/2 + X, - Y, Z SFAC C H N O UNIT 44 44 4 4 MERG 2 SHEL 22.1 0.82 FMAP 2 PLAN 20 ACTA BOND $H CONF SIZE 0.30 0.20 0.03 L.S. 10 EQIV $1 -x+1/2, y+1, z+1/2 HTAB N1 O1_$1 EQIV $2 x, y+1, z HTAB C11 O1_$2 WGHT 0.041300 0.035300 EXTI 0.010959 FVAR 9.77430 O1 4 0.179600 -0.172082 0.074878 11.00000 0.07422 0.07247 = 0.08007 -0.01301 -0.00539 -0.02040 N1 3 0.397892 0.517482 0.369730 11.00000 0.06083 0.06183 = 0.05079 -0.01020 0.00087 -0.00457 AFIX 43 H1 2 0.374387 0.617703 0.426070 11.00000 -1.20000 AFIX 0 C1 1 0.472098 0.511381 0.351676 11.00000 0.05440 0.07547 = 0.06566 -0.00742 -0.00956 -0.00871 AFIX 43 H1A 2 0.505189 0.616898 0.398801 11.00000 -1.20000 AFIX 0 C2 1 0.490548 0.330482 0.255745 11.00000 0.04930 0.07229 = 0.06952 -0.01012 -0.00547 0.00140 AFIX 43 H2 2 0.537658 0.289163 0.226106 11.00000 -1.20000 AFIX 0 C3 1 0.424383 0.215055 0.208573 11.00000 0.05103 0.05394 = 0.04658 0.00143 0.00084 0.00193 C4 1 0.406778 0.021358 0.111561 11.00000 0.05484 0.05581 = 0.04969 -0.00281 0.00462 0.00501 AFIX 43 H4 2 0.444158 -0.061312 0.062624 11.00000 -1.20000 AFIX 0 C5 1 0.335020 -0.049431 0.087067 11.00000 0.06207 0.04420 = 0.03935 0.00359 0.00242 0.00066 C6 1 0.277622 0.080842 0.161624 11.00000 0.05300 0.04418 = 0.04134 0.00703 0.00203 -0.00515 C7 1 0.294620 0.272174 0.259581 11.00000 0.05137 0.04881 = 0.04402 -0.00006 0.00604 -0.00207 AFIX 43 H7 2 0.257621 0.355972 0.309016 11.00000 -1.20000 AFIX 0 C8 1 0.367328 0.335856 0.282329 11.00000 0.05444 0.04894 = 0.03969 0.00005 0.00046 -0.00298 C9 1 0.320801 -0.259028 -0.018878 11.00000 0.07886 0.05068 = 0.04985 -0.00396 0.00304 -0.00667 AFIX 137 H9A 2 0.301228 -0.406836 0.028738 11.00000 -1.50000 H9B 2 0.365818 -0.304641 -0.064929 11.00000 -1.50000 H9C 2 0.286276 -0.199487 -0.088115 11.00000 -1.50000 AFIX 0 C10 1 0.199252 0.022075 0.137853 11.00000 0.05874 0.05406 = 0.04945 0.01235 -0.00250 -0.01023 C11 1 0.142162 0.202229 0.194395 11.00000 0.05015 0.06269 = 0.09194 0.01090 -0.00484 -0.00036 AFIX 137 H11A 2 0.138998 0.183858 0.295297 11.00000 -1.50000 H11B 2 0.095621 0.162181 0.152638 11.00000 -1.50000 H11C 2 0.155339 0.375918 0.171429 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu453 in Pca21 #29 REM R1 = 0.0320 for 1172 Fo > 4sig(Fo) and 0.0361 for all 1280 data REM 121 parameters refined using 1 restraints END WGHT 0.0403 0.0378 REM Highest difference peak 0.124, deepest hole -0.096, 1-sigma level 0.027 Q1 1 0.3272 0.3119 0.2262 11.00000 0.05 0.12 Q2 1 0.3906 0.2573 0.2315 11.00000 0.05 0.12 Q3 1 0.3008 0.0210 0.1213 11.00000 0.05 0.11 Q4 1 0.4457 0.2347 0.2390 11.00000 0.05 0.11 Q5 1 0.4481 -0.2195 0.1769 11.00000 0.05 0.10 Q6 1 0.2826 0.2238 0.1879 11.00000 0.05 0.10 Q7 1 0.2435 0.0457 0.1702 11.00000 0.05 0.10 Q8 1 0.1476 0.4048 0.2269 11.00000 0.05 0.09 Q9 1 0.1503 -0.1467 -0.0417 11.00000 0.05 0.08 Q10 1 0.3668 -0.0474 0.1217 11.00000 0.05 0.08 Q11 1 0.3614 -0.0015 0.0818 11.00000 0.05 0.08 Q12 1 0.2232 0.3877 0.2390 11.00000 0.05 0.08 Q13 1 0.4914 0.7356 0.2404 11.00000 0.05 0.08 Q14 1 0.2430 -0.3499 0.0400 11.00000 0.05 0.08 Q15 1 0.5500 0.3055 0.1685 11.00000 0.05 0.07 Q16 1 0.0864 0.1021 0.2131 11.00000 0.05 0.07 Q17 1 0.2663 -0.2595 -0.0891 11.00000 0.05 0.07 Q18 1 0.2488 -0.2333 -0.0524 11.00000 0.05 0.07 Q19 1 0.1310 -0.1142 0.0766 11.00000 0.05 0.07 Q20 1 0.2091 -0.1670 -0.0087 11.00000 0.05 0.07 ; 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-20 0 1 2216.66 152.711 8 -20 0 2 89.4836 47.0781 8 -20 0 4 133.308 39.3153 5 -20 0 5 668.613 58.8502 5 -20 1 -4 197.041 37.6476 8 -20 1 -3 45.5396 30.5478 8 -20 -1 -2 9.91014 23.9725 8 -20 1 -2 28.9326 31.1988 8 -20 -1 -1 94.2739 41.2576 8 -20 1 -1 70.4115 44.7932 8 -20 -1 0-21.9968 41.9847 8 -20 1 0 64.3545 44.0491 8 20 1 1-17.3320 42.1586 9 -20 -1 1 123.406 48.6267 8 -20 1 1 76.0007 41.1842 8 20 1 2 62.9206 53.9618 9 -20 1 2 13.7645 25.3563 8 20 1 3 43.8268 67.3064 9 -20 -1 3-6.36495 17.3118 5 20 1 4 157.246 57.0493 9 -20 -1 4 235.618 34.6941 5 20 1 5-35.7129 35.7869 9 -20 1 5-12.8395 16.2448 5 -20 2 -4 391.457 42.1275 8 -20 2 -3 153.140 36.2151 8 -20 2 -2 498.680 59.6273 8 -20 2 -1 588.300 67.0610 8 -20 2 0 438.565 58.2704 8 -20 2 1 485.781 56.7850 8 20 2 1 450.123 83.4267 9 -20 2 2 382.300 41.3918 8 20 2 2 363.636 76.2182 9 20 2 3 146.712 60.9824 9 20 2 4 341.569 65.3917 9 -21 0 -3-0.10044 18.3216 8 -21 0 -2 2.06797 26.0583 8 -21 0 -1-21.6375 33.9627 8 -21 0 0-17.7080 36.6417 8 -21 0 1-29.0564 35.7962 8 21 0 2 31.1374 35.1918 9 21 0 3 35.6092 36.5665 9 21 0 4-87.4880 37.3721 9 -21 0 4-4.05631 16.1108 5 -21 1 -3 1210.55 79.4924 8 -21 1 -2 47.0428 29.2694 8 -21 1 -1 776.657 79.1919 8 -21 1 0 233.023 51.1726 8 -21 1 1 688.578 72.1115 8 -21 1 2 19.4996 19.1132 8 21 1 2 50.4250 35.7551 9 21 1 3 931.461 99.3618 9 -21 1 4 392.047 41.8672 5 21 1 4 312.156 56.9098 9 -21 2 -2 299.361 38.8212 8 -21 2 -1 429.239 46.6855 8 -21 2 0 101.331 25.0030 8 -22 0 -2 302.534 38.0611 8 -22 0 -1 1552.11 91.0624 8 -22 0 0 287.176 45.9999 8 -22 1 -2-23.0344 18.4806 8 -22 1 -1 836.416 65.0099 8 -22 1 0 103.560 26.9503 8 -22 1 1 699.826 56.2856 8 0 0 0 0.00 0.00 0 TITL cu453 in Pca2(1) REM Pca2(1) (#29, found as Pc2(1)b in cab setting) CELL 1.54184 18.263198 5.202652 9.449561 90.0000 90.0000 90.0000 ZERR 4.00 0.000695 0.000199 0.000344 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y, z SYMM -x+1/2, y, z+1/2 SFAC C H N O UNIT 44.00 44.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 22570