data_ch-1031-4-2 _audit_creation_date 2014-10-31 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _shelxl_version_number 2014-1 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2013). in preparation. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H12 N2 O3' _chemical_formula_sum 'C11 H12 N2 O3' _chemical_formula_weight 220.23 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.16319(19) _cell_length_b 12.2880(4) _cell_length_c 9.50685(18) _cell_angle_alpha 90 _cell_angle_beta 91.843(2) _cell_angle_gamma 90 _cell_volume 1069.89(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2550 _cell_measurement_temperature 293 _cell_measurement_theta_max 71.1810 _cell_measurement_theta_min 4.6370 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description '' _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_unetI/netI 0.0183 _diffrn_reflns_Laue_measured_fraction_full 0.879 _diffrn_reflns_Laue_measured_fraction_max 0.893 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4742 _diffrn_reflns_point_group_measured_fraction_full 0.879 _diffrn_reflns_point_group_measured_fraction_max 0.893 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.065 _diffrn_reflns_theta_min 5.887 _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9595 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.879 _diffrn_measured_fraction_theta_max 0.893 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -52.00 35.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - -33.5000 57.0000 -90.0000 87 #__ type_ start__ end____ width___ exp.time_ 2 omega -37.00 73.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 -19.0000 -30.0000 110 #__ type_ start__ end____ width___ exp.time_ 3 omega 23.00 90.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 -125.0000 120.0000 67 #__ type_ start__ end____ width___ exp.time_ 4 omega 13.00 106.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 38.0000 -150.0000 93 #__ type_ start__ end____ width___ exp.time_ 5 omega 1.00 76.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 -99.0000 120.0000 75 #__ type_ start__ end____ width___ exp.time_ 6 omega 23.00 90.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 -125.0000 30.0000 67 #__ type_ start__ end____ width___ exp.time_ 7 omega 1.00 76.00 1.0000 1.2300 omega____ theta____ kappa____ phi______ frames - 35.5486 -99.0000 -90.0000 75 #__ type_ start__ end____ width___ exp.time_ 8 omega 37.00 91.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -90.0000 54 #__ type_ start__ end____ width___ exp.time_ 9 omega 37.00 91.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 30.0000 54 #__ type_ start__ end____ width___ exp.time_ 10 omega 37.00 91.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 60.0000 54 #__ type_ start__ end____ width___ exp.time_ 11 omega 100.00 178.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 111.0000 -120.0000 78 #__ type_ start__ end____ width___ exp.time_ 12 omega 40.00 128.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -61.0000 -150.0000 88 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 109.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 30.0000 71 #__ type_ start__ end____ width___ exp.time_ 14 omega 38.00 98.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 -60.0000 60 #__ type_ start__ end____ width___ exp.time_ 15 omega 40.00 115.00 1.0000 4.9200 omega____ theta____ kappa____ phi______ frames - 108.0000 -61.0000 0.0000 75 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'New Gemini, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0670934000 _diffrn_orient_matrix_UB_12 0.0445448000 _diffrn_orient_matrix_UB_13 -0.1390547000 _diffrn_orient_matrix_UB_21 0.0683692000 _diffrn_orient_matrix_UB_22 0.1122211000 _diffrn_orient_matrix_UB_23 0.0319510000 _diffrn_orient_matrix_UB_31 0.1382108000 _diffrn_orient_matrix_UB_32 -0.0338291000 _diffrn_orient_matrix_UB_33 -0.0770564000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1534 _reflns_number_total 1704 _reflns_odcompleteness_completeness 89.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2013)' _refine_diff_density_max 0.174 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 1704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0609 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+0.1820P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1591 _refine_ls_wR_factor_ref 0.1646 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C7(H7), C9(H9), C15(H15) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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 0.12971(15) 0.29508(14) 0.89801(12) 0.0602(5) Uani 1 1 d . . . . . N2 N 0.08424(14) 0.34159(13) 0.67121(13) 0.0381(4) Uani 1 1 d . . . . . C3 C -0.05617(19) 0.47252(16) 0.80501(18) 0.0437(5) Uani 1 1 d . . . . . H3 H 0.0295 0.4953 0.8512 0.052 Uiso 1 1 calc R . . . . N4 N -0.4527(2) 0.53618(17) 0.7984(2) 0.0695(6) Uani 1 1 d . . . . . C5 C -0.05178(17) 0.39044(15) 0.70425(16) 0.0385(4) Uani 1 1 d . . . . . O6 O -0.4540(2) 0.60074(18) 0.8958(3) 0.1030(8) Uani 1 1 d . . . . . C7 C -0.17908(19) 0.35851(17) 0.63366(19) 0.0468(5) Uani 1 1 d . . . . . H7 H -0.1760 0.3042 0.5658 0.056 Uiso 1 1 calc R . . . . C8 C 0.16565(18) 0.29276(16) 0.77607(17) 0.0411(5) Uani 1 1 d . . . . . C9 C -0.3104(2) 0.40664(18) 0.6632(2) 0.0538(5) Uani 1 1 d . . . . . H9 H -0.3959 0.3859 0.6152 0.065 Uiso 1 1 calc R . . . . O10 O -0.5606(2) 0.5113(2) 0.7299(3) 0.1131(9) Uani 1 1 d . . . . . C11 C 0.2736(2) 0.30739(19) 0.4961(2) 0.0561(6) Uani 1 1 d . . . . . H11A H 0.2870 0.2920 0.3973 0.067 Uiso 1 1 calc R . . . . H11B H 0.3320 0.3706 0.5216 0.067 Uiso 1 1 calc R . . . . C12 C 0.1145(2) 0.33084(18) 0.52011(17) 0.0489(5) Uani 1 1 d . . . . . H12A H 0.0869 0.3977 0.4720 0.059 Uiso 1 1 calc R . . . . H12B H 0.0554 0.2724 0.4800 0.059 Uiso 1 1 calc R . . . . C13 C 0.30586(19) 0.23722(19) 0.73745(19) 0.0507(5) Uani 1 1 d . . . . . H13A H 0.3869 0.2832 0.7681 0.061 Uiso 1 1 calc R . . . . H13B H 0.3139 0.1697 0.7900 0.061 Uiso 1 1 calc R . . . . C14 C 0.3226(2) 0.21158(19) 0.5834(2) 0.0556(6) Uani 1 1 d . . . . . H14A H 0.4239 0.1952 0.5658 0.067 Uiso 1 1 calc R . . . . H14B H 0.2643 0.1483 0.5579 0.067 Uiso 1 1 calc R . . . . C15 C -0.1878(2) 0.52009(16) 0.8363(2) 0.0488(5) Uani 1 1 d . . . . . H15 H -0.1920 0.5742 0.9044 0.059 Uiso 1 1 calc R . . . . C16 C -0.31234(19) 0.48607(17) 0.7652(2) 0.0497(5) 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 O1 0.0651(9) 0.0830(12) 0.0326(7) 0.0068(6) 0.0032(6) 0.0241(7) N2 0.0411(7) 0.0420(9) 0.0312(7) 0.0011(6) -0.0005(5) 0.0011(6) C3 0.0483(9) 0.0422(11) 0.0402(9) -0.0038(7) -0.0050(7) -0.0002(7) N4 0.0562(11) 0.0485(12) 0.1044(16) -0.0008(11) 0.0141(10) 0.0097(8) C5 0.0433(9) 0.0381(10) 0.0339(8) 0.0043(7) 0.0000(6) 0.0001(7) O6 0.0780(12) 0.0775(14) 0.155(2) -0.0434(14) 0.0272(12) 0.0154(10) C7 0.0473(9) 0.0469(12) 0.0461(9) -0.0065(8) -0.0031(7) 0.0008(8) C8 0.0422(9) 0.0469(11) 0.0340(8) 0.0011(7) -0.0002(7) 0.0006(7) C9 0.0437(9) 0.0527(13) 0.0645(12) -0.0016(10) -0.0071(8) -0.0002(8) O10 0.0502(10) 0.1146(19) 0.174(2) -0.0378(17) -0.0108(12) 0.0233(10) C11 0.0611(11) 0.0658(15) 0.0423(10) 0.0061(9) 0.0150(8) 0.0034(9) C12 0.0560(10) 0.0595(13) 0.0315(8) 0.0051(8) 0.0024(7) 0.0057(9) C13 0.0445(9) 0.0601(13) 0.0473(10) 0.0071(9) 0.0006(7) 0.0083(8) C14 0.0525(10) 0.0624(15) 0.0526(11) 0.0030(9) 0.0133(8) 0.0102(9) C15 0.0625(11) 0.0366(11) 0.0474(10) -0.0029(8) 0.0033(8) 0.0057(8) C16 0.0477(10) 0.0405(11) 0.0612(11) 0.0063(9) 0.0060(8) 0.0078(7) _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 1.216(2) . ? N2 C5 1.427(2) . ? N2 C8 1.365(2) . ? N2 C12 1.478(2) . ? C3 H3 0.9300 . ? C3 C5 1.392(2) . ? C3 C15 1.381(3) . ? N4 O6 1.219(3) . ? N4 O10 1.206(3) . ? N4 C16 1.470(2) . ? C5 C7 1.384(2) . ? C7 H7 0.9300 . ? C7 C9 1.378(3) . ? C8 C13 1.511(2) . ? C9 H9 0.9300 . ? C9 C16 1.376(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.510(3) . ? C11 C14 1.501(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.510(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15 0.9300 . ? C15 C16 1.373(3) . ? 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 C5 N2 C12 116.35(13) . . ? C8 N2 C5 118.99(12) . . ? C8 N2 C12 123.76(14) . . ? C5 C3 H3 120.0 . . ? C15 C3 H3 120.0 . . ? C15 C3 C5 119.96(16) . . ? O6 N4 C16 117.7(2) . . ? O10 N4 O6 123.2(2) . . ? O10 N4 C16 119.1(2) . . ? C3 C5 N2 120.05(15) . . ? C7 C5 N2 120.16(16) . . ? C7 C5 C3 119.77(16) . . ? C5 C7 H7 119.8 . . ? C9 C7 C5 120.50(18) . . ? C9 C7 H7 119.8 . . ? O1 C8 N2 121.87(15) . . ? O1 C8 C13 120.06(16) . . ? N2 C8 C13 118.05(14) . . ? C7 C9 H9 120.7 . . ? C16 C9 C7 118.64(17) . . ? C16 C9 H9 120.7 . . ? H11A C11 H11B 108.2 . . ? C12 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C14 C11 H11A 109.7 . . ? C14 C11 H11B 109.7 . . ? C14 C11 C12 109.81(16) . . ? N2 C12 C11 112.09(15) . . ? N2 C12 H12A 109.2 . . ? N2 C12 H12B 109.2 . . ? C11 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C8 C13 H13A 108.2 . . ? C8 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C14 C13 C8 116.32(15) . . ? C14 C13 H13A 108.2 . . ? C14 C13 H13B 108.2 . . ? C11 C14 C13 109.56(17) . . ? C11 C14 H14A 109.8 . . ? C11 C14 H14B 109.8 . . ? C13 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C3 C15 H15 120.6 . . ? C16 C15 C3 118.88(18) . . ? C16 C15 H15 120.6 . . ? C9 C16 N4 118.67(18) . . ? C15 C16 N4 119.09(19) . . ? C15 C16 C9 122.24(17) . . ? 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 O1 C8 C13 C14 164.2(2) . . . . ? N2 C5 C7 C9 -178.85(17) . . . . ? N2 C8 C13 C14 -17.4(3) . . . . ? C3 C5 C7 C9 -0.6(3) . . . . ? C3 C15 C16 N4 179.81(18) . . . . ? C3 C15 C16 C9 -0.4(3) . . . . ? C5 N2 C8 O1 -4.3(3) . . . . ? C5 N2 C8 C13 177.30(16) . . . . ? C5 N2 C12 C11 164.54(17) . . . . ? C5 C3 C15 C16 -0.9(3) . . . . ? C5 C7 C9 C16 -0.7(3) . . . . ? O6 N4 C16 C9 174.9(2) . . . . ? O6 N4 C16 C15 -5.3(3) . . . . ? C7 C9 C16 N4 -179.02(19) . . . . ? C7 C9 C16 C15 1.2(3) . . . . ? C8 N2 C5 C3 58.1(2) . . . . ? C8 N2 C5 C7 -123.61(19) . . . . ? C8 N2 C12 C11 -26.4(3) . . . . ? C8 C13 C14 C11 43.8(3) . . . . ? O10 N4 C16 C9 -4.4(4) . . . . ? O10 N4 C16 C15 175.4(2) . . . . ? C12 N2 C5 C3 -132.27(18) . . . . ? C12 N2 C5 C7 46.0(2) . . . . ? C12 N2 C8 O1 -173.02(19) . . . . ? C12 N2 C8 C13 8.5(3) . . . . ? C12 C11 C14 C13 -61.1(2) . . . . ? C14 C11 C12 N2 52.3(2) . . . . ? C15 C3 C5 N2 179.66(16) . . . . ? C15 C3 C5 C7 1.4(3) . . . . ? _shelx_res_file ; TITL CELL 1.54184 9.163189 12.287981 9.506846 90 91.8431 90 ZERR 4 0.000185 0.000367 0.000176 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 44 48 8 12 L.S. 40 PLAN 20 TEMP 19.85 fmap 2 MORE -1 BOND $H CONF ACTA SHEL 999 0.837 REM G:/oym/ch-1031-4-2/struct/olex2_ch-1031-4-2/ch-1031-4-2.hkl WGHT 0.112000 0.182000 FVAR 11.65641 O1 4 0.129715 0.295075 0.898008 11.00000 0.06507 0.08301 = 0.03263 0.00682 0.00318 0.02412 N2 3 0.084244 0.341587 0.671208 11.00000 0.04109 0.04198 = 0.03120 0.00113 -0.00051 0.00111 C3 1 -0.056172 0.472516 0.805014 11.00000 0.04831 0.04218 = 0.04021 -0.00380 -0.00497 -0.00019 AFIX 43 H3 2 0.029465 0.495292 0.851222 11.00000 -1.20000 AFIX 0 N4 3 -0.452726 0.536179 0.798390 11.00000 0.05618 0.04853 = 0.10444 -0.00075 0.01410 0.00970 C5 1 -0.051777 0.390442 0.704252 11.00000 0.04334 0.03810 = 0.03391 0.00432 0.00001 0.00013 O6 4 -0.454002 0.600738 0.895758 11.00000 0.07796 0.07754 = 0.15510 -0.04340 0.02716 0.01535 C7 1 -0.179076 0.358513 0.633659 11.00000 0.04725 0.04689 = 0.04605 -0.00651 -0.00308 0.00080 AFIX 43 H7 2 -0.175975 0.304154 0.565754 11.00000 -1.20000 AFIX 0 C8 1 0.165646 0.292763 0.776071 11.00000 0.04219 0.04692 = 0.03399 0.00106 -0.00023 0.00059 C9 1 -0.310375 0.406637 0.663206 11.00000 0.04367 0.05266 = 0.06447 -0.00164 -0.00715 -0.00019 AFIX 43 H9 2 -0.395937 0.385877 0.615216 11.00000 -1.20000 AFIX 0 O10 4 -0.560624 0.511267 0.729913 11.00000 0.05022 0.11459 = 0.17365 -0.03782 -0.01083 0.02331 C11 1 0.273572 0.307388 0.496099 11.00000 0.06112 0.06577 = 0.04231 0.00608 0.01497 0.00339 AFIX 23 H11A 2 0.287049 0.291953 0.397301 11.00000 -1.20000 H11B 2 0.332014 0.370618 0.521601 11.00000 -1.20000 AFIX 0 C12 1 0.114483 0.330839 0.520105 11.00000 0.05596 0.05949 = 0.03146 0.00505 0.00242 0.00567 AFIX 23 H12A 2 0.086861 0.397693 0.471967 11.00000 -1.20000 H12B 2 0.055378 0.272420 0.479973 11.00000 -1.20000 AFIX 0 C13 1 0.305863 0.237221 0.737453 11.00000 0.04454 0.06013 = 0.04732 0.00706 0.00057 0.00832 AFIX 23 H13A 2 0.386862 0.283180 0.768121 11.00000 -1.20000 H13B 2 0.313920 0.169708 0.790003 11.00000 -1.20000 AFIX 0 C14 1 0.322557 0.211579 0.583434 11.00000 0.05249 0.06242 = 0.05257 0.00296 0.01333 0.01021 AFIX 23 H14A 2 0.423902 0.195208 0.565814 11.00000 -1.20000 H14B 2 0.264290 0.148272 0.557875 11.00000 -1.20000 AFIX 0 C15 1 -0.187803 0.520088 0.836301 11.00000 0.06249 0.03657 = 0.04739 -0.00287 0.00327 0.00567 AFIX 43 H15 2 -0.191982 0.574247 0.904385 11.00000 -1.20000 AFIX 0 C16 1 -0.312338 0.486068 0.765198 11.00000 0.04766 0.04045 = 0.06117 0.00627 0.00602 0.00780 HKLF 4 REM REM R1 = 0.0609 for 1534 Fo > 4sig(Fo) and 0.0640 for all 1704 data REM 145 parameters refined using 0 restraints END WGHT 0.1116 0.1825 REM Highest difference peak 0.174, deepest hole -0.344, 1-sigma level 0.071 Q1 1 0.1241 0.2966 0.9952 11.00000 0.05 0.17 Q2 1 0.0327 0.3600 0.4660 11.00000 0.05 0.17 Q3 1 0.0898 0.3150 0.9890 11.00000 0.05 0.17 Q4 1 -0.3794 0.6111 0.9627 11.00000 0.05 0.16 Q5 1 0.2253 0.4835 0.8624 11.00000 0.05 0.16 Q6 1 -0.2283 0.2387 0.5876 11.00000 0.05 0.15 Q7 1 0.1317 0.4533 0.5121 11.00000 0.05 0.15 Q8 1 0.1391 0.5387 0.8201 11.00000 0.05 0.14 Q9 1 -0.3460 0.2305 0.6229 11.00000 0.05 0.14 Q10 1 0.2281 0.2395 0.3615 11.00000 0.05 0.14 Q11 1 0.2132 0.2633 0.3051 11.00000 0.05 0.13 Q12 1 -0.1633 0.2134 0.4801 11.00000 0.05 0.13 Q13 1 -0.5022 0.5497 0.9016 11.00000 0.05 0.13 Q14 1 -0.3919 0.4097 0.5551 11.00000 0.05 0.13 Q15 1 -0.4223 0.6252 0.8252 11.00000 0.05 0.13 Q16 1 0.5464 0.3597 0.8597 11.00000 0.05 0.13 Q17 1 0.4376 0.2811 0.3166 11.00000 0.05 0.13 Q18 1 0.2338 0.5103 0.5577 11.00000 0.05 0.13 Q19 1 -0.3549 0.2400 0.7114 11.00000 0.05 0.13 Q20 1 0.2020 0.5045 0.7678 11.00000 0.05 0.13 ; _shelx_res_checksum 98556 _shelx_hkl_file ; 0 0 -1 458.065 46.3543 3 0 0 -2 710793. 2553.65 3 0 0 -2 710767. 3286.35 4 0 0 -3 4.22464 29.5612 4 0 0 -3 28.5874 26.3169 3 0 0 -4 24191.8 871.494 4 0 0 -4 24536.8 985.928 2 0 0 -5 97.4654 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54.5418 9 7 7 0 3226.15 283.703 11 7 7 0 3033.36 283.082 15 7 7 0 3348.28 302.674 9 7 7 1 3301.76 283.290 11 7 7 1 3137.98 291.820 15 7 7 1 3237.51 298.854 9 7 7 2 40.2119 50.4426 11 7 7 2 0.61989 35.1349 15 7 7 2 13.0382 46.5909 9 7 7 3 203.025 78.8666 11 7 7 3 144.375 72.9244 9 7 7 4 8367.72 430.040 11 7 7 4 7574.49 433.223 10 7 7 4 7377.65 434.632 9 7 7 5-1.69159 28.5293 11 7 7 5-13.8824 42.0738 10 7 7 5 34.2738 45.8279 9 7 7 6 7959.56 372.807 10 7 8 -7 130.370 40.0730 15 7 8 -6 1574.61 148.144 15 7 8 -5 59.9945 32.9826 15 7 8 -4 921.567 136.340 15 7 8 -4 854.469 132.163 9 7 8 -3 1196.57 161.489 15 7 8 -3 1296.79 173.174 9 7 8 -2 162.966 64.6669 15 7 8 -2 196.007 71.0297 9 7 8 -1 5518.02 355.546 11 7 8 -1 5596.80 368.305 15 7 8 -1 5923.82 389.187 9 7 8 0-5.59554 45.0347 11 7 8 0 5.05290 42.5554 15 7 8 0-5.07881 51.6940 9 7 8 1 3002.03 263.152 11 7 8 1 2379.57 248.883 15 7 8 1 2662.59 268.440 9 7 8 2-11.9576 50.3329 11 7 8 2 68.1149 68.5147 15 7 8 2 21.0268 38.1025 9 7 8 3 1983.56 207.675 11 7 8 3 2165.77 232.862 9 7 8 4 1420.64 170.033 11 7 8 4 1482.19 183.560 10 7 8 4 1301.73 175.266 9 7 8 5 1743.76 172.464 11 7 8 5 1655.63 176.094 10 7 8 5 1348.11 162.256 9 7 8 6 1170.66 126.503 10 7 9 -6 1884.13 136.361 15 7 9 -5 362.241 74.1802 15 7 9 -4 102.766 25.2673 15 7 9 -4-8.23861 31.1638 9 7 9 -3 1708.06 177.888 15 7 9 -3 1573.55 179.549 9 7 9 -2 39.6968 43.4180 15 7 9 -2 78.9538 34.5363 9 7 9 -1 2032.14 202.488 11 7 9 -1 2133.09 213.119 15 7 9 -1 2244.04 237.942 9 7 9 0 1240.18 162.012 11 7 9 0 1023.29 154.589 15 7 9 0 1276.71 180.594 9 7 9 1 4874.56 340.503 9 7 9 1 5131.47 329.530 11 7 9 1 4301.53 309.882 15 7 9 2 680.885 120.418 11 7 9 2 679.006 126.679 9 7 9 3 738.043 122.523 11 7 9 3 458.686 102.432 9 7 9 4 3032.05 227.652 11 7 9 4 2894.51 235.152 10 7 9 4 3014.42 241.637 9 7 9 5 4726.31 249.011 11 7 9 5 4520.79 258.003 10 7 9 5 4189.13 245.897 9 7 10 -4 19.1520 17.7004 15 7 10 -4 27.1612 21.2596 9 7 10 -3 133.277 41.4203 15 7 10 -3 184.547 60.4099 9 7 10 -2 177.649 59.9694 15 7 10 -2 109.391 43.3359 9 7 10 -1-1.77489 30.0754 9 7 -10 0 192.376 55.3759 12 7 10 0 213.770 55.7279 11 7 10 0 276.415 82.7871 9 7 -10 1 170.404 56.3569 12 7 10 1 183.280 59.3529 11 7 10 1 318.406 82.6199 9 7 10 2 1698.24 170.864 11 7 10 2 1404.76 166.083 9 7 10 3 1140.45 134.048 11 7 10 3 906.396 125.240 10 7 10 3 917.805 127.136 9 7 10 4 32.1273 20.4747 11 7 10 4 60.7036 32.3963 10 7 10 4 69.6806 39.5642 9 7 11 -3 307.090 62.3050 9 7 11 -2 18.6760 27.3804 9 7 11 -1 110.653 56.6934 9 7 -11 0 801.189 98.1468 12 7 11 0 1017.72 128.061 9 7 11 0 788.770 99.2713 11 7 -11 1 363.656 67.4354 12 7 11 1 219.504 49.1042 11 7 11 1 386.842 82.4990 9 7 -11 2 51.0871 27.6364 12 7 11 2 8.73507 28.4382 11 7 11 2-1.07434 30.9412 9 7 11 3 1430.57 126.779 11 7 11 3 1610.36 138.862 10 8 0 -8 3360.79 189.787 13 8 0 -7 8.58675 32.2985 13 8 0 -6 637.688 114.653 13 8 0 -5 50.0586 55.9390 13 8 0 -4 906.032 149.922 11 8 0 -4 974.683 148.931 13 8 0 -3 4.18546 44.1831 11 8 0 -3-72.6619 75.0113 13 8 0 -2 19341.2 707.313 11 8 0 -2 20598.7 687.477 13 8 0 -1 81.8872 57.7765 11 8 0 -1-46.9421 68.8962 13 8 0 0 138578. 1922.30 11 8 0 0 135258. 1830.41 15 8 0 0 138753. 1821.28 13 8 0 1 14.3149 56.9248 11 8 0 1 257.529 93.9400 15 8 0 2 182439. 2242.38 11 8 0 2 187620. 2320.46 10 8 0 2 182558. 2319.63 9 8 0 3 29.5226 52.8983 10 8 0 3 39.1560 61.7009 9 8 0 4 8171.06 486.294 10 8 0 5 10.3537 47.7483 10 8 0 6 271.300 88.6220 10 8 0 7 17.8369 38.0224 10 8 -1 -8 58.3717 27.2960 13 8 1 -8 73.9858 34.3437 13 8 -1 -7 3789.01 235.447 13 8 1 -7 3992.47 246.771 13 8 -1 -6 4213.03 273.859 13 8 1 -6 4576.61 289.644 13 8 -1 -5 3219.40 256.570 13 8 1 -5 3997.25 287.853 13 8 -1 -4 6414.05 407.281 11 8 1 -4 6428.97 405.482 11 8 -1 -4 6578.96 378.365 13 8 1 -4 6672.51 383.848 13 8 -1 -3 605.055 124.753 11 8 1 -3 851.384 151.413 11 8 1 -3 598.328 118.012 15 8 -1 -3 1038.14 150.795 13 8 1 -3 453.547 97.7021 13 8 -1 -2 25342.3 817.257 11 8 1 -2 24407.4 789.326 11 8 -1 -2 24472.6 753.864 13 8 1 -2 23744.3 744.651 13 8 -1 -1 119.189 69.0649 11 8 1 -1 118.002 63.6492 11 8 1 -1 41.0653 37.6795 15 8 -1 -1 71.2876 55.3960 13 8 1 -1 25.6129 44.7713 13 8 -1 0 1195.92 181.951 11 8 1 0 1194.77 175.773 11 8 1 0 1092.85 159.412 15 8 -1 0 1249.35 176.820 13 8 1 0 1082.03 159.615 13 8 -1 1 1311.91 197.575 11 8 1 1 1303.67 188.584 11 8 1 1 1352.52 183.524 15 8 -1 2 23993.8 817.510 11 8 1 2 24516.3 814.019 11 8 -1 2 24223.7 834.302 10 8 1 2 25077.6 849.656 10 8 1 2 25618.0 867.505 9 8 1 2 24439.1 802.204 15 8 1 3 104.740 62.2574 11 8 -1 3 152.278 69.7495 10 8 1 3 122.381 59.4037 10 8 1 3 179.036 87.7775 9 8 -1 4 10749.9 555.803 10 8 1 4 10899.8 555.682 10 8 1 4 11070.5 563.033 9 8 -1 5 217.142 79.1970 10 8 1 5 185.358 75.9053 10 8 -1 6 51.6337 54.9412 10 8 1 6-24.5400 41.3146 10 8 -1 7 198.725 66.8195 10 8 1 7 161.160 60.2337 10 8 2 -8 45.4893 28.8232 13 8 -2 -7 2004.02 162.219 13 8 2 -7 2321.85 187.198 13 8 2 -6 1204.65 143.836 15 8 -2 -6 1484.31 159.632 13 8 2 -6 1268.33 152.581 13 8 2 -5 9231.09 427.913 15 8 -2 -5 10138.3 446.747 13 8 2 -5 9365.62 436.249 13 8 2 -4 142.680 69.7191 11 8 2 -4 100.411 52.9038 15 8 -2 -4 130.148 59.2979 13 8 2 -4 100.412 57.9924 13 8 -2 -3 290.508 96.9243 11 8 2 -3 141.108 69.3731 11 8 2 -3 101.129 54.7239 15 8 -2 -3 176.127 73.3689 13 8 2 -3 109.531 54.4632 13 8 -2 -2 10721.0 531.894 11 8 2 -2 12131.7 557.076 11 8 2 -2 10834.5 504.177 15 8 -2 -2 11171.7 512.248 13 8 2 -2 12398.3 541.095 13 8 -2 -1 1738.91 216.952 11 8 2 -1 1706.69 207.284 11 8 2 -1 1822.14 206.751 15 8 -2 -1 2019.32 220.914 13 8 2 -1 1619.41 203.067 13 8 -2 0 29456.2 908.567 11 8 2 0 28312.9 845.844 11 8 2 0 29390.0 843.890 15 8 -2 0 29160.3 840.872 13 8 2 0 28851.3 845.903 13 8 -2 1 8570.05 495.235 11 8 2 1 8346.41 461.139 11 8 2 1 8337.70 477.408 10 8 2 1 7638.94 459.467 9 8 2 1 8587.02 466.739 15 8 -2 2 2312.42 255.221 11 8 2 2 2104.20 237.079 11 8 2 2 2214.26 239.685 15 8 2 2 2378.33 262.023 10 8 2 2 2846.00 284.223 9 8 2 3 15488.7 627.036 11 8 -2 3 16277.3 692.357 10 8 2 3 17075.6 697.424 10 8 2 3 16817.2 697.732 9 8 -2 4 92.5769 62.7657 10 8 2 4 229.623 99.8871 10 8 2 4 130.620 68.3739 9 8 -2 5 1193.89 182.854 10 8 2 5 1028.61 167.204 10 8 -2 6 4115.90 308.313 10 8 2 6 3856.51 291.966 10 8 2 7 555.539 100.361 10 8 3 -8 535.632 75.0324 13 8 3 -7 2071.35 165.666 15 8 3 -7 2402.10 186.350 13 8 3 -6 24.4826 26.7559 15 8 3 -6 8.53172 38.0827 13 8 3 -5 157.852 74.2526 15 8 -3 -5 65.1830 37.3923 13 8 3 -5 144.149 59.7527 13 8 3 -4 10534.5 504.365 11 8 3 -4 11093.9 490.838 15 8 -3 -4 10173.4 462.848 13 8 3 -4 10801.6 488.948 13 8 3 -3 23624.8 764.209 11 8 3 -3 23599.3 738.934 15 8 -3 -3 22876.3 716.301 13 8 3 -3 24088.7 749.335 13 8 -3 -2 8495.49 480.204 11 8 3 -2 9038.18 465.101 15 8 3 -2 7363.37 428.461 11 8 -3 -2 8015.94 437.211 13 8 3 -2 8772.32 458.705 13 8 -3 -1 4706.16 359.906 11 8 3 -1 5231.35 361.024 11 8 3 -1 4903.53 348.392 15 8 -3 -1 5280.87 358.097 13 8 3 -1 5017.42 350.251 13 8 -3 0 12254.7 589.589 11 8 3 0 13273.6 570.440 11 8 3 0 11340.9 548.425 9 8 3 0 12193.5 547.433 15 8 3 0 12049.2 549.198 13 8 -3 1 2.64500 49.0995 11 8 3 1 19.1974 33.4164 11 8 3 1-23.9410 74.2501 10 8 3 1-43.7669 66.1644 9 8 3 2 171.279 60.2774 11 8 3 2 47.3035 36.4320 10 8 3 2 156.532 66.3045 15 8 3 2 136.947 77.1487 9 8 3 3 23041.5 749.990 11 8 -3 3 23193.6 803.800 10 8 3 3 23997.4 819.703 10 8 3 3 24729.5 831.496 9 8 3 4 1963.78 207.550 11 8 -3 4 2081.73 239.850 10 8 3 4 2366.05 255.273 10 8 3 4 1829.59 225.204 9 8 -3 5 2616.54 259.869 10 8 3 5 2159.53 232.581 10 8 3 5 2140.54 229.815 9 8 3 6 111.296 49.6301 10 8 3 7 1690.44 162.795 10 8 4 -7 2995.81 196.134 15 8 4 -7 3367.08 210.806 13 8 4 -6 1219.02 142.613 15 8 4 -6 1359.40 150.450 13 8 4 -5 3832.67 272.093 15 8 4 -5 3942.30 275.857 13 8 4 -4 26644.4 759.294 15 8 4 -4 26451.5 749.760 13 8 4 -3 2575.76 253.962 11 8 4 -3 2902.38 260.902 15 8 -4 -3 2851.52 253.740 13 8 4 -3 3056.51 264.819 13 8 4 -2 20647.9 715.759 11 8 4 -2 20528.9 704.221 15 8 -4 -2 19251.0 673.350 13 8 4 -2 20021.5 684.727 13 8 -4 -1 3588.32 314.810 11 8 4 -1 3621.36 298.383 11 8 4 -1 4009.13 315.591 15 8 4 -1 3356.51 286.770 13 8 -4 0 4837.38 369.953 11 8 4 0 5089.84 353.228 11 8 4 0 4545.50 348.996 9 8 4 0 4973.10 355.564 15 8 4 0 4842.46 347.658 13 8 -4 1 60.2322 47.2515 11 8 4 1 77.9680 49.6858 11 8 4 1-21.0855 36.5069 10 8 4 1 30.6956 48.2629 15 8 4 1-32.8840 52.9208 9 8 4 2 1270.49 179.017 11 8 4 2 1670.81 214.133 10 8 4 2 1493.80 199.708 9 8 4 2 1457.36 194.894 15 8 4 3 11812.7 530.756 11 8 -4 3 10763.0 533.114 10 8 4 3 11723.7 562.889 10 8 4 3 10593.5 543.420 9 8 4 4 8524.32 430.851 11 8 -4 4 9192.67 488.296 10 8 4 4 8919.57 483.524 10 8 4 4 9361.07 492.738 9 8 4 5 127.276 63.8148 10 8 4 5 77.4254 66.1348 9 8 4 6 2656.17 227.555 10 8 4 7 84.2426 32.0237 10 8 5 -7 1448.86 129.551 15 8 5 -7 1547.65 130.036 13 8 5 -6 2505.92 199.430 15 8 5 -6 2342.30 187.474 13 8 5 -5 16886.1 560.087 15 8 5 -5 15249.3 518.460 13 8 5 -4 1669.43 190.367 15 8 5 -4 1454.88 171.185 13 8 5 -3 9430.86 465.184 11 8 5 -3 10261.0 479.794 15 8 5 -3 9853.64 453.947 13 8 5 -2 2397.35 239.227 11 8 5 -2 2384.13 236.113 15 8 5 -2 2475.91 233.184 13 8 5 -1 7738.70 431.597 15 8 5 -1 7025.99 419.203 9 8 5 0 2118.22 226.072 11 8 5 0 2116.51 227.653 15 8 5 0 2173.23 238.613 9 8 5 1 239.031 73.2696 11 8 5 1 152.915 76.5233 15 8 5 1 170.620 72.8555 9 8 5 2 210.234 78.7013 11 8 5 2 157.140 81.5690 10 8 5 2 265.006 90.1069 15 8 5 2 98.8780 55.3739 9 8 5 3 1380.91 180.626 11 8 5 3 1651.81 212.257 10 8 5 3 1781.85 212.305 9 8 5 4 1521.50 179.341 11 8 5 4 1500.06 190.679 10 8 5 4 1273.36 178.288 9 8 5 5 6387.71 327.764 11 8 5 5 7114.13 390.161 10 8 5 5 6976.92 393.487 9 8 5 6 326.678 80.3080 10 8 6 -7 292.435 54.1891 15 8 6 -6-16.9469 36.4532 15 8 6 -6-9.96913 25.3979 13 8 6 -5 3310.91 239.856 15 8 6 -5 3118.69 215.105 13 8 6 -4 2098.91 202.770 15 8 6 -4 1856.81 180.385 13 8 6 -3 3075.66 260.358 15 8 6 -2 1619.47 192.403 11 8 6 -2 1547.67 190.517 15 8 6 -2 1628.41 190.745 9 8 6 -1 2156.06 224.513 11 8 6 -1 1937.11 216.751 15 8 6 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148.204 68.8890 10 8 7 3 73.7474 49.5901 9 8 7 4 1980.01 183.770 11 8 7 4 2122.22 205.120 10 8 7 4 2246.47 216.797 9 8 7 5 70.1678 33.9263 11 8 7 5 57.5312 41.1678 10 8 7 5 109.133 48.9027 9 8 8 -5 4351.78 231.228 15 8 8 -4 381.769 80.1211 15 8 8 -3 632.686 109.844 15 8 8 -3 585.847 96.9585 9 8 8 -2 2843.58 228.842 15 8 8 -2 2761.62 228.487 9 8 8 -1 504.267 99.2898 11 8 8 -1 383.125 86.1039 15 8 8 -1 567.376 110.415 9 8 8 0 13950.6 523.291 11 8 8 0 12950.0 515.546 15 8 8 0 12790.5 524.063 9 8 8 1 2159.70 207.373 11 8 8 1 2238.32 214.130 15 8 8 1 2305.16 225.070 9 8 8 2 1528.88 169.499 11 8 8 2 1689.93 189.263 10 8 8 2 1744.31 192.092 9 8 8 3 1602.84 165.684 11 8 8 3 1412.37 165.275 10 8 8 3 1461.45 171.007 9 8 8 4 1345.67 139.328 11 8 8 4 1409.22 155.212 10 8 8 4 1216.13 145.687 9 8 8 5 511.848 77.7900 10 8 9 -4 1162.35 115.355 15 8 9 -3 83.9528 31.4247 15 8 9 -3 53.3943 31.7791 9 8 9 -2 64.8224 39.8806 15 8 9 -2-21.6728 31.5149 9 8 9 -1 401.243 77.7047 11 8 9 -1 338.077 77.0203 15 8 9 -1 429.046 88.3662 9 8 9 0 3499.10 238.778 11 8 9 0 2916.22 219.822 15 8 9 0 3282.49 246.811 9 8 9 1 1312.84 147.958 11 8 9 1 1131.94 146.545 9 8 9 2 901.297 119.477 11 8 9 2 680.725 106.457 10 8 9 2 750.667 116.716 9 8 9 3 386.545 77.0381 11 8 9 3 380.348 82.5995 10 8 9 3 381.591 81.0695 9 8 9 4 83.4576 37.3040 11 8 9 4 59.3872 30.1856 10 8 10 -2 65.2204 37.2025 9 8 10 -1 140.875 47.9712 9 8 10 0 527.686 79.1651 11 8 10 0 863.139 113.918 9 8 10 1 714.970 94.0954 11 8 10 1 726.094 100.415 10 8 10 1 705.379 99.8534 9 8 10 2 431.952 71.7955 11 8 10 2 443.438 77.1179 10 8 10 2 454.144 74.7402 9 9 0 -7 1384.48 118.351 13 9 0 -6 12.9232 27.8503 13 9 0 -5 178.596 62.8344 13 9 0 -4 18.1449 46.1631 11 9 0 -4 54.6823 44.0987 13 9 0 -3 2229.46 231.030 11 9 0 -3 2460.86 225.644 13 9 0 -2-34.2100 65.3349 11 9 0 -2 80.5345 59.1313 13 9 0 -1 534.689 118.335 11 9 0 -1 379.625 91.3063 13 9 0 0-61.4463 67.1720 11 9 0 1 171.502 68.7118 11 9 0 2-38.8861 59.2784 11 9 0 2 153.521 61.0275 10 9 0 3 2712.54 260.900 10 9 0 4-8.56537 37.8677 10 9 0 5 7235.15 382.034 10 9 0 6-36.2722 31.3951 10 9 -1 -7 995.335 95.0532 13 9 1 -7 1451.63 123.958 13 9 -1 -6 1858.72 160.379 13 9 1 -6 1929.97 163.973 13 9 -1 -5-6.91698 40.1590 13 9 1 -5 44.3665 38.1157 13 9 1 -4 1925.07 203.300 11 9 -1 -4 2021.61 195.534 13 9 1 -4 1986.19 194.197 13 9 -1 -3 1721.90 201.440 11 9 1 -3 1557.09 189.334 11 9 -1 -3 1493.61 175.682 13 9 1 -3 1616.25 183.001 13 9 -1 -2 61.3314 43.1323 11 9 1 -2 12.3493 35.2487 11 9 1 -2 41.5159 46.5618 15 9 -1 -2 27.9663 38.1745 13 9 1 -2 23.1996 43.1944 13 9 -1 -1 450.617 106.033 11 9 1 -1 533.671 114.029 11 9 1 -1 566.553 112.218 15 9 -1 -1 579.668 111.739 13 9 1 -1 447.745 97.9769 13 9 -1 0 237.863 84.7677 11 9 1 0 239.154 77.1473 11 9 1 0 221.978 73.6073 15 9 -1 1 7906.76 450.032 11 9 1 1 8205.31 450.037 11 9 1 1 7521.71 424.423 15 9 -1 2-46.6528 48.6533 11 9 1 2 5.47650 48.1293 11 9 1 2 41.6055 48.3965 10 9 1 2-11.5917 40.6838 9 9 1 3 10122.8 467.049 11 9 -1 3 9792.78 483.126 10 9 1 3 10386.1 500.670 10 9 -1 4-27.1500 53.0512 10 9 1 4 27.7852 34.8777 10 9 -1 5 67.8727 42.1064 10 9 1 5 72.9702 46.1309 10 9 -1 6 53.4458 32.7978 10 9 1 6 36.0872 32.6939 10 9 2 -7 3289.21 178.947 13 9 -2 -6 2896.77 188.649 13 9 2 -6 3532.98 218.021 13 9 -2 -5 104.562 45.9461 13 9 2 -5 126.349 62.0154 13 9 2 -4 939.152 136.784 11 9 2 -4 853.377 122.606 15 9 -2 -4 1225.28 153.747 13 9 2 -4 1155.85 151.135 13 9 2 -3 2527.77 241.176 11 9 2 -3 2544.20 226.028 15 9 -2 -3 2765.85 238.219 13 9 2 -3 2311.22 219.124 13 9 -2 -2 483.629 115.373 11 9 2 -2 380.394 94.4231 11 9 2 -2 481.464 100.745 15 9 -2 -2 402.605 95.8502 13 9 2 -2 474.043 101.267 13 9 -2 -1 5743.19 381.294 11 9 2 -1 5985.73 378.182 11 9 2 -1 5590.97 353.194 15 9 -2 -1 6144.35 372.861 13 9 2 -1 5649.06 360.374 13 9 -2 0 3359.57 296.576 11 9 2 0 3419.52 284.845 11 9 2 0 3343.86 277.226 15 9 -2 1 3759.29 308.902 11 9 2 1 3760.28 299.395 11 9 2 1 3587.48 288.709 15 9 2 2 113.363 51.8361 11 9 2 2-4.74169 37.9754 10 9 2 2 80.8828 53.6233 9 9 2 3 1032.56 150.535 11 9 2 3 1068.27 162.946 10 9 -2 3 976.335 148.827 10 9 2 3 960.899 157.128 9 9 -2 4 390.358 96.2724 10 9 2 4 421.373 100.659 10 9 -2 5 27.5697 31.8754 10 9 2 5 23.6978 31.6059 10 9 2 6 9.23478 30.1074 10 9 3 -6 533.645 78.6435 15 9 3 -6 566.090 85.8443 13 9 3 -5 117.380 42.4144 15 9 -3 -5 144.308 48.5540 13 9 3 -5 193.588 58.5054 13 9 3 -4 921.046 133.716 11 9 3 -4 926.518 129.203 15 9 -3 -4 900.829 124.901 13 9 3 -4 937.751 134.561 13 9 3 -3 18.5211 33.0061 11 9 3 -3 60.1141 52.6428 15 9 -3 -3 37.1798 38.0724 13 9 3 -3 42.1836 31.0152 13 9 3 -2 5078.93 339.657 11 9 3 -2 4307.56 300.054 15 9 -3 -2 4577.52 311.117 13 9 3 -2 4474.31 309.006 13 9 -3 -1 10501.6 513.163 11 9 3 -1 10782.4 500.825 11 9 3 -1 10183.6 476.686 15 9 3 -1 9776.31 467.369 13 9 -3 0 6455.49 403.408 11 9 3 0 6630.03 392.968 11 9 3 0 6424.30 387.447 15 9 -3 1 893.229 149.409 11 9 3 1 1075.25 154.062 11 9 3 1 737.388 131.611 10 9 3 1 790.223 136.469 15 9 3 1 784.292 137.654 9 9 3 2 3745.12 289.018 11 9 3 2 3771.65 298.312 10 9 3 2 4085.06 316.712 9 9 3 3 3587.46 269.691 11 9 3 3 3810.31 295.407 10 9 3 3 3725.07 297.437 9 9 3 4 1096.96 137.696 11 9 3 4 1354.25 171.078 10 9 3 4 1245.98 161.483 9 9 3 5 17.8904 34.5098 10 9 3 6 1364.91 136.721 10 9 4 -6 5575.60 244.728 15 9 4 -6 6527.70 271.699 13 9 4 -5 208.249 54.7783 15 9 4 -5 229.968 59.7864 13 9 4 -4 233.595 64.9129 15 9 4 -4 336.685 80.8309 13 9 4 -3 3985.44 284.527 11 9 4 -3 4346.46 288.589 15 9 4 -3 4588.75 291.701 13 9 4 -2 4875.77 326.572 11 9 4 -2 4956.51 321.374 15 9 4 -2 5010.79 317.343 13 9 4 -1 1095.71 159.569 11 9 4 -1 963.809 142.783 15 9 4 -1 888.922 129.457 13 9 4 0 139.507 58.3327 11 9 4 0 136.808 73.7795 15 9 4 0 172.359 57.1882 9 9 4 1 1105.61 157.176 11 9 4 1 1048.23 153.255 10 9 4 1 1007.19 156.466 15 9 4 1 902.864 141.315 9 9 4 2 19.8587 31.0834 11 9 4 2 19.5097 40.1119 10 9 4 2-27.8550 34.8467 9 9 4 3 5091.51 312.625 11 9 4 3 5292.30 339.922 10 9 4 3 5531.75 348.286 9 9 4 4 10.7886 20.6941 11 9 4 4 54.3315 43.2266 10 9 4 4 101.272 52.8788 9 9 4 5 1997.96 183.474 10 9 4 6 63.9645 33.0037 10 9 5 -6 298.881 56.3619 15 9 5 -5 1147.86 125.436 15 9 5 -5 1050.07 112.760 13 9 5 -4 1962.74 179.229 15 9 5 -4 1850.58 167.093 13 9 5 -3 4366.88 281.191 11 9 5 -3 4945.37 301.390 15 9 5 -3 4642.39 277.045 13 9 5 -2 10716.3 465.941 11 9 5 -2 10730.5 460.109 15 9 5 -2 9699.81 413.794 13 9 5 -1 40.0866 36.0890 11 9 5 -1 66.9137 52.1698 15 9 5 0 155.883 61.5980 11 9 5 0 254.990 77.7311 15 9 5 0 185.555 66.0971 9 9 5 1 70.6544 43.9855 11 9 5 1 135.033 60.5936 10 9 5 1 92.6609 50.0968 15 9 5 1-0.48719 31.5033 9 9 5 2 1275.35 158.883 11 9 5 2 1350.19 169.631 10 9 5 2 1433.86 178.671 9 9 5 3 372.693 84.7218 11 9 5 3 239.301 63.9190 10 9 5 3 178.141 53.8510 9 9 5 4 321.223 70.0354 11 9 5 4 232.522 64.1276 10 9 5 4 305.515 79.9516 9 9 5 5 125.788 48.0317 10 9 6 -5 3571.60 204.353 15 9 6 -4 9991.27 382.078 15 9 6 -3 318.926 76.5304 15 9 6 -2 308.817 79.3249 11 9 6 -2 315.956 79.6248 15 9 6 -1 871.269 126.756 11 9 6 -1 935.833 139.357 15 9 6 -1 758.965 120.570 9 9 6 0 1391.00 165.530 11 9 6 0 1549.00 171.981 10 9 6 0 1572.21 178.754 9 9 6 0 1445.06 169.598 15 9 6 1 154.973 59.4157 11 9 6 1 115.842 47.0458 10 9 6 1 181.647 65.7135 15 9 6 1 157.695 56.0360 9 9 6 2 18.5448 38.5131 11 9 6 2-14.9991 38.1610 10 9 6 2 2.56932 33.2368 9 9 6 3 54.3741 31.9994 11 9 6 3 58.6296 57.3718 10 9 6 3-19.2486 36.4192 9 9 6 4 1391.66 133.469 11 9 6 4 1565.86 157.573 10 9 6 4 1674.10 164.809 9 9 6 5 104.294 41.3391 10 9 7 -4 7525.21 300.406 15 9 7 -3 91.0589 46.5126 15 9 7 -2 1171.98 131.599 11 9 7 -2 1262.98 143.401 15 9 7 -1 60.5125 38.0791 11 9 7 -1-24.3287 34.0825 15 9 7 -1-0.81153 33.7663 9 9 7 0 875.727 124.626 11 9 7 0 675.553 104.758 10 9 7 0 995.201 135.071 15 9 7 0 778.305 117.681 9 9 7 1 1417.30 154.528 11 9 7 1 1201.64 144.170 10 9 7 1 1379.69 158.473 9 9 7 2 449.665 85.3736 11 9 7 2 461.186 91.9538 10 9 7 2 497.269 96.5896 9 9 7 3 2316.96 177.133 11 9 7 3 2581.71 200.825 10 9 7 3 2322.09 190.711 9 9 7 4 151.214 45.2776 10 9 7 4 146.417 44.9103 9 9 8 -3 1191.49 116.133 15 9 8 -2 1.56872 20.0558 15 9 8 -1 240.690 60.3457 11 9 8 -1 188.176 57.4188 15 9 8 -1 107.166 39.0329 9 9 8 0 4003.69 236.686 11 9 8 0 3523.95 219.750 10 9 8 0 3875.79 240.130 9 9 8 0 3747.80 230.651 15 9 8 1 130.016 51.5431 11 9 8 1 99.4756 40.0027 10 9 8 1 58.5549 34.5440 9 9 8 2 933.346 110.700 11 9 8 2 789.058 106.974 10 9 8 2 796.719 105.608 9 9 8 3 78.3453 33.7905 11 9 8 3 61.4249 29.5146 10 9 8 3 76.0535 30.8460 9 9 9 0 664.377 87.1077 9 10 0 -5-13.9172 28.9409 13 10 0 -4 880.571 112.042 13 10 0 -3-55.2728 55.0843 11 10 0 -3-11.7889 31.8399 13 10 0 -2 512.152 100.924 11 10 0 -2 413.771 90.4194 13 10 0 -1-2.40938 34.4157 11 10 0 0 218.035 74.9924 11 10 0 1-27.3758 40.4793 11 10 0 2 2554.83 212.327 11 10 0 3-16.8703 24.0816 10 10 0 4 3252.96 211.821 10 10 -1 -5 44.0318 28.5126 13 10 1 -5 49.4552 28.2944 13 10 1 -4 786.311 107.759 13 10 -1 -4 602.220 91.1451 13 10 1 -3-21.4802 45.8905 11 10 -1 -3 37.1537 31.5196 13 10 1 -3 68.8481 40.5268 13 10 -1 -2 108.961 54.4440 11 10 1 -2 98.1186 54.0693 11 10 1 -2 121.608 48.5928 13 10 -1 -1 1970.13 200.215 11 10 1 -1 2222.94 209.873 11 10 -1 0 162.705 66.9805 11 10 1 0 129.567 51.9843 11 10 -1 1 464.666 99.8464 11 10 1 1 416.653 93.3384 11 10 -1 2 4482.93 276.530 11 10 1 2 5194.13 302.271 11 10 1 3 1598.06 162.675 10 10 -1 4 2226.01 169.892 10 10 1 4 2189.80 176.606 10 10 2 -5 501.687 75.0721 13 10 2 -4 530.044 85.6183 13 10 2 -3 476.678 93.6645 11 10 2 -3 521.550 92.7718 13 10 2 -2 57.1619 40.2941 11 10 2 -2 64.7837 47.8363 15 10 2 -2 42.1725 39.3987 13 10 -2 -1 581.252 111.079 11 10 2 -1 506.382 98.4785 11 10 2 -1 412.750 85.6289 15 10 -2 0 3789.32 274.788 11 10 2 0 3868.56 275.067 11 10 -2 1 16.8063 41.3394 11 10 2 1-8.66811 39.4736 11 10 2 2 3904.10 258.828 11 10 2 3 1545.93 148.457 11 10 2 3 1664.27 163.691 10 10 2 4 1738.17 155.011 10 10 3 -5 24.1210 17.6657 13 10 3 -4 610.710 82.6245 15 10 3 -4 809.401 101.394 13 10 3 -3 745.989 111.065 11 10 3 -3 703.149 100.671 15 10 3 -3 792.086 109.455 13 10 3 -2 164.563 51.9960 11 10 3 -2 81.0051 26.0060 15 10 3 -1 114.707 52.2906 11 10 3 -1 115.049 46.5388 15 10 3 0 1225.09 152.765 11 10 3 0 1162.76 146.456 15 10 3 1 5523.97 312.360 11 10 3 2 22.9108 33.0854 11 10 3 2 9.25385 33.7364 10 10 3 3 1971.49 164.634 11 10 3 3 1905.79 169.092 10 10 3 4 954.045 112.076 10 10 4 -4 18.5810 20.3839 15 10 4 -4 6.15642 20.7894 13 10 4 -3 260.339 64.1834 11 10 4 -3 129.305 47.0970 15 10 4 -3 170.916 48.8582 13 10 4 -2 176.149 57.6750 11 10 4 -2 133.115 49.3966 15 10 4 -1 74.9550 43.8886 11 10 4 -1 54.2415 35.7354 15 10 4 0 56.7298 39.7150 11 10 4 0 19.4859 29.5647 15 10 4 1 3609.59 242.420 11 10 4 2 35.1290 37.5429 11 10 4 2-11.1112 31.4132 10 10 4 2 4.87296 20.3541 9 10 4 3 85.2617 32.7719 11 10 4 3 117.498 39.6568 10 10 4 4 1199.82 116.086 10 10 5 -3 211.737 55.4350 15 10 5 -2 30.1819 25.7974 11 10 5 -2 9.58164 27.1763 15 10 5 -1 26.1699 36.8288 11 10 5 -1 63.5531 36.9079 15 10 5 0 83.9050 35.0014 11 10 5 0 100.270 46.6840 15 10 5 1 35.4789 30.5371 11 10 5 1 13.8426 18.3201 9 10 5 2 221.334 54.7544 11 10 5 2 185.427 52.9041 10 10 5 2 146.730 50.0982 9 10 5 3 118.516 32.0182 11 10 5 3 111.246 41.9714 10 10 6 -3-23.0140 24.0064 15 10 6 -2 469.018 73.7844 15 10 6 -1 548.180 85.1625 11 10 6 -1 584.057 88.3532 15 10 6 0 222.268 57.2370 11 10 6 1 2626.40 182.938 11 10 6 1 1829.91 145.635 9 10 6 2 65.5340 29.2228 11 11 0 0 7.93354 21.2071 11 11 0 1 737.657 89.9448 11 11 1 -1 1428.51 134.234 11 11 1 0 266.665 57.6700 11 11 1 1 437.250 70.9629 11 11 2 -2 118.072 37.3374 11 11 2 -1 1897.32 151.420 11 11 2 0 82.2513 38.4091 11 11 2 1 118.195 44.7052 11 11 3 -1 1932.05 144.926 11 11 3 0 1830.60 141.976 11 0 0 0 0.00 0.00 0 TITL ch-1031-4-2 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 9.163189 12.287981 9.506846 90.0000 91.8431 90.0000 ZERR 5.00 0.000185 0.000367 0.000176 0.0000 0.0020 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 55.00 50.00 5.00 5.00 TREF HKLF 4 END ; _shelx_hkl_checksum 68909 _olex2_submission_special_instructions 'No special instructions were received'