data_wj1001 _audit_creation_date 2014-10-01 _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 ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H17 N O2' _chemical_formula_sum 'C22 H17 N O2' _chemical_formula_weight 327.36 _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 11.71490(16) _cell_length_b 11.30687(12) _cell_length_c 13.08437(17) _cell_angle_alpha 90 _cell_angle_beta 95.1593(12) _cell_angle_gamma 90 _cell_volume 1726.12(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6556 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 72.5220 _cell_measurement_theta_min 4.8500 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92252 _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 ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description '' _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 17042 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.040 _diffrn_reflns_theta_min 4.855 _diffrn_ambient_temperature 293.15 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9595 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 20.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 57.0000 0.0000 84 #__ type_ start__ end____ width___ exp.time_ 2 omega -31.00 63.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -77.0000 60.0000 94 #__ type_ start__ end____ width___ exp.time_ 3 omega -33.00 55.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -38.0000 120.0000 88 #__ type_ start__ end____ width___ exp.time_ 4 omega 23.00 90.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -125.0000 -180.0000 67 #__ type_ start__ end____ width___ exp.time_ 5 omega 20.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 57.0000 150.0000 84 #__ type_ start__ end____ width___ exp.time_ 6 omega 20.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 57.0000 -150.0000 84 #__ type_ start__ end____ width___ exp.time_ 7 omega -31.00 53.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -57.0000 120.0000 84 #__ type_ start__ end____ width___ exp.time_ 8 omega 40.00 98.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 120.0000 58 #__ type_ start__ end____ width___ exp.time_ 9 omega 91.00 176.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 45.0000 -180.0000 85 #__ type_ start__ end____ width___ exp.time_ 10 omega 100.00 178.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 111.0000 90.0000 78 #__ type_ start__ end____ width___ exp.time_ 11 omega 39.00 109.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 60.0000 70 #__ type_ start__ end____ width___ exp.time_ 12 omega 38.00 91.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -150.0000 53 #__ type_ start__ end____ width___ exp.time_ 13 omega 39.00 109.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 150.0000 70 #__ type_ start__ end____ width___ exp.time_ 14 omega 40.00 98.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 -90.0000 58 #__ type_ start__ end____ width___ exp.time_ 15 omega 91.00 176.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 45.0000 60.0000 85 #__ type_ start__ end____ width___ exp.time_ 16 omega 40.00 98.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 60.0000 58 #__ type_ start__ end____ width___ exp.time_ 17 omega 38.00 91.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -60.0000 53 #__ type_ start__ end____ width___ exp.time_ 18 omega 1.00 27.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 93.0000 -67.7414 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 20.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 57.0000 -90.0000 84 #__ type_ start__ end____ width___ exp.time_ 20 omega -33.00 55.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -38.0000 -150.0000 88 #__ type_ start__ end____ width___ exp.time_ 21 omega 20.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 57.0000 90.0000 84 #__ type_ start__ end____ width___ exp.time_ 22 omega -33.00 55.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -38.0000 -60.0000 88 #__ type_ start__ end____ width___ exp.time_ 23 omega 10.00 104.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 77.0000 0.0000 94 #__ type_ start__ end____ width___ exp.time_ 24 omega 1.00 75.00 1.0000 1.0100 omega____ theta____ kappa____ phi______ frames - 36.5421 -99.0000 -30.0000 74 #__ type_ start__ end____ width___ exp.time_ 25 omega 81.00 176.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -150.0000 95 #__ type_ start__ end____ width___ exp.time_ 26 omega 91.00 176.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 45.0000 0.0000 85 #__ type_ start__ end____ width___ exp.time_ 27 omega 87.00 145.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 30.0000 120.0000 58 #__ type_ start__ end____ width___ exp.time_ 28 omega 70.00 178.00 1.0000 4.0400 omega____ theta____ kappa____ phi______ frames - 108.0000 15.0000 -60.0000 108 ; _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 -0.0543571000 _diffrn_orient_matrix_UB_12 -0.0574378000 _diffrn_orient_matrix_UB_13 0.0907752000 _diffrn_orient_matrix_UB_21 -0.0363584000 _diffrn_orient_matrix_UB_22 0.1229731000 _diffrn_orient_matrix_UB_23 0.0360122000 _diffrn_orient_matrix_UB_31 -0.1146855000 _diffrn_orient_matrix_UB_32 -0.0117991000 _diffrn_orient_matrix_UB_33 -0.0666730000 _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 2705 _reflns_number_total 3071 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. 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 ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _refine_diff_density_max 0.190 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.032 _refine_ls_extinction_coef 0.0027(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 3071 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0469 _refine_ls_restrained_S_all 1.054 _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^)+(0.0899P)^2^+0.1568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1381 _refine_ls_wR_factor_ref 0.1433 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Rigid bond restraints C20, C19 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22) ; _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 -0.04469(10) 0.27767(11) 0.37113(10) 0.0760(4) Uani 1 1 d . . . . . O2 O 0.03931(10) 0.44230(10) 0.31613(11) 0.0811(4) Uani 1 1 d . . . . . N1 N 0.34209(11) 0.26332(12) 0.33933(9) 0.0600(3) Uani 1 1 d . . . . . C1 C 0.30729(13) 0.15518(13) 0.37594(10) 0.0570(4) Uani 1 1 d . . . . . C2 C 0.24970(13) 0.33484(13) 0.32477(11) 0.0595(4) Uani 1 1 d . . . . . H2 H 0.2514 0.4122 0.3009 0.071 Uiso 1 1 calc R . . . . C3 C 0.15336(12) 0.27773(13) 0.34998(11) 0.0560(4) Uani 1 1 d . . . . . C4 C 0.18828(13) 0.16046(12) 0.38228(10) 0.0554(4) Uani 1 1 d . . . . . C5 C 0.13148(15) 0.06035(14) 0.41467(12) 0.0665(4) Uani 1 1 d . . . . . H5 H 0.0527 0.0612 0.4191 0.080 Uiso 1 1 calc R . . . . C6 C 0.19517(18) -0.03968(15) 0.43992(14) 0.0773(5) Uani 1 1 d . . . . . H6 H 0.1584 -0.1071 0.4611 0.093 Uiso 1 1 calc R . . . . C7 C 0.31306(18) -0.04206(15) 0.43444(14) 0.0771(5) Uani 1 1 d . . . . . H7 H 0.3534 -0.1109 0.4527 0.093 Uiso 1 1 calc R . . . . C8 C 0.37141(15) 0.05420(15) 0.40289(12) 0.0689(4) Uani 1 1 d . . . . . H8 H 0.4504 0.0524 0.3996 0.083 Uiso 1 1 calc R . . . . C9 C 0.03975(14) 0.32691(13) 0.34753(11) 0.0593(4) Uani 1 1 d . . . . . C10 C 0.45945(14) 0.29723(16) 0.32514(12) 0.0674(4) Uani 1 1 d . . . . . H10A H 0.4578 0.3670 0.2818 0.081 Uiso 1 1 calc R . . . . H10B H 0.4949 0.2340 0.2891 0.081 Uiso 1 1 calc R . . . . C11 C 0.53320(12) 0.32315(12) 0.42333(11) 0.0554(4) Uani 1 1 d . . . . . C12 C 0.48868(14) 0.33712(15) 0.51669(12) 0.0645(4) Uani 1 1 d . . . . . H12 H 0.4100 0.3315 0.5208 0.077 Uiso 1 1 calc R . . . . C13 C 0.56077(17) 0.35948(16) 0.60416(13) 0.0740(5) Uani 1 1 d . . . . . H13 H 0.5301 0.3681 0.6669 0.089 Uiso 1 1 calc R . . . . C14 C 0.67625(17) 0.36901(15) 0.59958(15) 0.0767(5) Uani 1 1 d . . . . . H14 H 0.7243 0.3830 0.6589 0.092 Uiso 1 1 calc R . . . . C15 C 0.72083(15) 0.35783(16) 0.50698(17) 0.0794(5) Uani 1 1 d . . . . . H15 H 0.7994 0.3658 0.5032 0.095 Uiso 1 1 calc R . . . . C16 C 0.65049(14) 0.33495(15) 0.41950(14) 0.0689(4) Uani 1 1 d . . . . . H16 H 0.6819 0.3273 0.3570 0.083 Uiso 1 1 calc R . . . . C17 C -0.06427(14) 0.50396(15) 0.30965(12) 0.0651(4) Uani 1 1 d . . . . . C18 C -0.14616(16) 0.48533(17) 0.22993(14) 0.0771(5) Uani 1 1 d . . . . . H18 H -0.1372 0.4263 0.1818 0.093 Uiso 1 1 calc R . . . . C19 C -0.24288(17) 0.5567(2) 0.22282(16) 0.0876(5) Uani 1 1 d . U . . . H19 H -0.2996 0.5455 0.1693 0.105 Uiso 1 1 calc R . . . . C20 C -0.25567(18) 0.6431(2) 0.29339(17) 0.0917(6) Uani 1 1 d . U . . . H20 H -0.3210 0.6902 0.2880 0.110 Uiso 1 1 calc R . . . . C21 C -0.1733(2) 0.6604(2) 0.37150(16) 0.0926(7) Uani 1 1 d . . . . . H21 H -0.1824 0.7196 0.4195 0.111 Uiso 1 1 calc R . . . . C22 C -0.07661(17) 0.59132(18) 0.38035(13) 0.0777(5) Uani 1 1 d . . . . . H22 H -0.0200 0.6037 0.4338 0.093 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0592(7) 0.0681(7) 0.1002(9) 0.0110(6) 0.0040(6) -0.0019(5) O2 0.0604(7) 0.0683(7) 0.1165(10) 0.0253(6) 0.0195(6) 0.0133(5) N1 0.0565(7) 0.0650(7) 0.0578(7) -0.0006(5) 0.0006(5) 0.0039(5) C1 0.0638(9) 0.0583(8) 0.0477(7) -0.0056(6) -0.0022(6) 0.0068(6) C2 0.0652(9) 0.0556(8) 0.0565(8) 0.0005(6) -0.0016(6) 0.0040(6) C3 0.0574(8) 0.0555(7) 0.0538(7) -0.0030(6) -0.0024(6) 0.0039(6) C4 0.0608(8) 0.0559(7) 0.0480(7) -0.0049(5) -0.0025(6) 0.0038(6) C5 0.0712(10) 0.0614(9) 0.0656(9) -0.0010(7) 0.0001(7) -0.0028(7) C6 0.0966(14) 0.0574(9) 0.0766(10) 0.0042(8) 0.0006(9) -0.0007(8) C7 0.0946(13) 0.0591(9) 0.0758(10) 0.0023(8) -0.0029(9) 0.0169(9) C8 0.0713(10) 0.0706(10) 0.0634(9) -0.0056(7) -0.0015(7) 0.0176(8) C9 0.0609(9) 0.0579(8) 0.0577(8) 0.0005(6) -0.0018(6) 0.0038(6) C10 0.0623(9) 0.0819(10) 0.0592(8) 0.0000(7) 0.0119(7) 0.0023(8) C11 0.0537(8) 0.0503(7) 0.0628(8) 0.0031(6) 0.0077(6) 0.0042(6) C12 0.0556(8) 0.0732(9) 0.0655(9) -0.0020(7) 0.0091(7) 0.0047(7) C13 0.0838(12) 0.0737(10) 0.0635(9) -0.0023(8) 0.0019(8) 0.0037(9) C14 0.0790(12) 0.0603(9) 0.0862(12) 0.0030(8) -0.0182(9) -0.0045(8) C15 0.0542(9) 0.0729(10) 0.1091(14) 0.0094(10) -0.0033(9) -0.0091(8) C16 0.0601(9) 0.0663(9) 0.0823(11) 0.0059(7) 0.0180(8) -0.0010(7) C17 0.0587(9) 0.0666(9) 0.0710(9) 0.0193(7) 0.0116(7) 0.0099(7) C18 0.0763(11) 0.0786(11) 0.0768(10) 0.0049(8) 0.0088(8) 0.0017(9) C19 0.0699(11) 0.1133(15) 0.0777(11) 0.0234(9) -0.0042(8) 0.0070(10) C20 0.0796(13) 0.1093(14) 0.0887(12) 0.0311(9) 0.0206(10) 0.0366(11) C21 0.1071(16) 0.0977(14) 0.0758(12) 0.0034(10) 0.0238(11) 0.0330(12) C22 0.0804(12) 0.0912(12) 0.0613(9) 0.0104(8) 0.0047(8) 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 O1 C9 1.1995(19) . ? O2 C9 1.3677(19) . ? O2 C17 1.3953(19) . ? N1 C1 1.388(2) . ? N1 C2 1.351(2) . ? N1 C10 1.455(2) . ? C1 C4 1.405(2) . ? C1 C8 1.394(2) . ? C2 H2 0.9300 . ? C2 C3 1.366(2) . ? C3 C4 1.440(2) . ? C3 C9 1.440(2) . ? C4 C5 1.398(2) . ? C5 H5 0.9300 . ? C5 C6 1.379(2) . ? C6 H6 0.9300 . ? C6 C7 1.390(3) . ? C7 H7 0.9300 . ? C7 C8 1.369(3) . ? C8 H8 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.511(2) . ? C11 C12 1.380(2) . ? C11 C16 1.386(2) . ? C12 H12 0.9300 . ? C12 C13 1.383(2) . ? C13 H13 0.9300 . ? C13 C14 1.364(3) . ? C14 H14 0.9300 . ? C14 C15 1.368(3) . ? C15 H15 0.9300 . ? C15 C16 1.373(3) . ? C16 H16 0.9300 . ? C17 C18 1.369(3) . ? C17 C22 1.370(3) . ? C18 H18 0.9300 . ? C18 C19 1.388(3) . ? C19 H19 0.9300 . ? C19 C20 1.361(3) . ? C20 H20 0.9300 . ? C20 C21 1.355(3) . ? C21 H21 0.9300 . ? C21 C22 1.373(3) . ? C22 H22 0.9300 . ? 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 C9 O2 C17 118.34(12) . . ? C1 N1 C10 125.90(13) . . ? C2 N1 C1 108.64(13) . . ? C2 N1 C10 125.35(14) . . ? N1 C1 C4 107.86(12) . . ? N1 C1 C8 129.82(15) . . ? C8 C1 C4 122.31(15) . . ? N1 C2 H2 124.7 . . ? N1 C2 C3 110.60(14) . . ? C3 C2 H2 124.7 . . ? C2 C3 C4 106.68(13) . . ? C2 C3 C9 126.44(14) . . ? C4 C3 C9 126.85(14) . . ? C1 C4 C3 106.20(13) . . ? C5 C4 C1 119.03(14) . . ? C5 C4 C3 134.77(15) . . ? C4 C5 H5 120.8 . . ? C6 C5 C4 118.34(17) . . ? C6 C5 H5 120.8 . . ? C5 C6 H6 119.3 . . ? C5 C6 C7 121.50(17) . . ? C7 C6 H6 119.3 . . ? C6 C7 H7 119.1 . . ? C8 C7 C6 121.73(16) . . ? C8 C7 H7 119.1 . . ? C1 C8 H8 121.5 . . ? C7 C8 C1 117.07(16) . . ? C7 C8 H8 121.5 . . ? O1 C9 O2 122.62(14) . . ? O1 C9 C3 126.66(15) . . ? O2 C9 C3 110.70(13) . . ? N1 C10 H10A 108.6 . . ? N1 C10 H10B 108.6 . . ? N1 C10 C11 114.66(12) . . ? H10A C10 H10B 107.6 . . ? C11 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C12 C11 C10 122.83(14) . . ? C12 C11 C16 118.42(15) . . ? C16 C11 C10 118.74(14) . . ? C11 C12 H12 119.9 . . ? C11 C12 C13 120.15(16) . . ? C13 C12 H12 119.9 . . ? C12 C13 H13 119.6 . . ? C14 C13 C12 120.81(17) . . ? C14 C13 H13 119.6 . . ? C13 C14 H14 120.3 . . ? C13 C14 C15 119.40(16) . . ? C15 C14 H14 120.3 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.49(16) . . ? C16 C15 H15 119.8 . . ? C11 C16 H16 119.7 . . ? C15 C16 C11 120.70(16) . . ? C15 C16 H16 119.7 . . ? C18 C17 O2 121.04(16) . . ? C18 C17 C22 121.09(16) . . ? C22 C17 O2 117.60(16) . . ? C17 C18 H18 120.9 . . ? C17 C18 C19 118.28(18) . . ? C19 C18 H18 120.9 . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.73(19) . . ? C20 C19 H19 119.6 . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.06(18) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 119.8 . . ? C20 C21 C22 120.5(2) . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 119.35(19) . . ? C17 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? 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 O2 C17 C18 C19 -174.34(15) . . . . ? O2 C17 C22 C21 174.69(16) . . . . ? N1 C1 C4 C3 -1.26(15) . . . . ? N1 C1 C4 C5 178.20(13) . . . . ? N1 C1 C8 C7 -178.24(15) . . . . ? N1 C2 C3 C4 -0.45(16) . . . . ? N1 C2 C3 C9 177.86(13) . . . . ? N1 C10 C11 C12 -12.5(2) . . . . ? N1 C10 C11 C16 168.39(14) . . . . ? C1 N1 C2 C3 -0.35(17) . . . . ? C1 N1 C10 C11 -73.91(19) . . . . ? C1 C4 C5 C6 0.5(2) . . . . ? C2 N1 C1 C4 1.02(15) . . . . ? C2 N1 C1 C8 -179.44(15) . . . . ? C2 N1 C10 C11 101.84(17) . . . . ? C2 C3 C4 C1 1.05(15) . . . . ? C2 C3 C4 C5 -178.29(16) . . . . ? C2 C3 C9 O1 -178.74(16) . . . . ? C2 C3 C9 O2 -0.2(2) . . . . ? C3 C4 C5 C6 179.76(15) . . . . ? C4 C1 C8 C7 1.2(2) . . . . ? C4 C3 C9 O1 -0.8(3) . . . . ? C4 C3 C9 O2 177.74(14) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C5 C6 C7 C8 -0.6(3) . . . . ? C6 C7 C8 C1 -0.2(3) . . . . ? C8 C1 C4 C3 179.16(13) . . . . ? C8 C1 C4 C5 -1.4(2) . . . . ? C9 O2 C17 C18 -76.3(2) . . . . ? C9 O2 C17 C22 109.70(18) . . . . ? C9 C3 C4 C1 -177.25(13) . . . . ? C9 C3 C4 C5 3.4(3) . . . . ? C10 N1 C1 C4 177.37(13) . . . . ? C10 N1 C1 C8 -3.1(2) . . . . ? C10 N1 C2 C3 -176.72(13) . . . . ? C10 C11 C12 C13 179.29(15) . . . . ? C10 C11 C16 C15 -179.62(16) . . . . ? C11 C12 C13 C14 0.5(3) . . . . ? C12 C11 C16 C15 1.2(2) . . . . ? C12 C13 C14 C15 0.9(3) . . . . ? C13 C14 C15 C16 -1.2(3) . . . . ? C14 C15 C16 C11 0.2(3) . . . . ? C16 C11 C12 C13 -1.6(2) . . . . ? C17 O2 C9 O1 -1.2(2) . . . . ? C17 O2 C9 C3 -179.81(14) . . . . ? C17 C18 C19 C20 0.1(3) . . . . ? C18 C17 C22 C21 0.6(3) . . . . ? C18 C19 C20 C21 0.2(3) . . . . ? C19 C20 C21 C22 -0.1(3) . . . . ? C20 C21 C22 C17 -0.3(3) . . . . ? C22 C17 C18 C19 -0.5(3) . . . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.058 0.108 0.625 8.5 0.4 ? 2 -0.058 0.892 0.375 8.5 0.3 ? 3 0.442 0.608 0.875 8.5 0.3 ? 4 0.558 0.392 0.125 8.5 0.4 ? _shelx_res_file ; TITL wj1001 in P2(1)/n CELL 1.54184 11.714896 11.306873 13.084371 90 95.1593 90 ZERR 4 0.000155 0.000121 0.00017 0 0.0012 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 88 68 4 8 DELU 0.001 0.001 C20 C19 L.S. 40 PLAN 20 TEMP 20 MORE -1 BOND $H CONF fmap 2 53 acta SHEL 999 0.837 REM C:/Users/Lenovo/Desktop/wj1001/olex2_wj1001/wj1001-mask.hkl WGHT 0.089900 0.156800 EXTI 0.002670 FVAR 6.60776 O1 4 -0.044693 0.277672 0.371133 11.00000 0.05921 0.06806 = 0.10019 0.01104 0.00401 -0.00193 O2 4 0.039305 0.442298 0.316135 11.00000 0.06045 0.06829 = 0.11654 0.02529 0.01947 0.01331 N1 3 0.342092 0.263324 0.339329 11.00000 0.05648 0.06497 = 0.05779 -0.00060 0.00065 0.00394 C1 1 0.307291 0.155180 0.375936 11.00000 0.06379 0.05827 = 0.04774 -0.00565 -0.00223 0.00680 C2 1 0.249698 0.334838 0.324771 11.00000 0.06516 0.05558 = 0.05646 0.00048 -0.00158 0.00403 AFIX 43 H2 2 0.251426 0.412230 0.300892 11.00000 -1.20000 AFIX 0 C3 1 0.153364 0.277733 0.349984 11.00000 0.05738 0.05547 = 0.05384 -0.00302 -0.00244 0.00393 C4 1 0.188284 0.160460 0.382281 11.00000 0.06083 0.05589 = 0.04804 -0.00492 -0.00253 0.00384 C5 1 0.131476 0.060346 0.414666 11.00000 0.07124 0.06140 = 0.06563 -0.00102 0.00010 -0.00277 AFIX 43 H5 2 0.052687 0.061201 0.419066 11.00000 -1.20000 AFIX 0 C6 1 0.195174 -0.039683 0.439917 11.00000 0.09665 0.05736 = 0.07658 0.00425 0.00058 -0.00066 AFIX 43 H6 2 0.158408 -0.107101 0.461100 11.00000 -1.20000 AFIX 0 C7 1 0.313064 -0.042055 0.434436 11.00000 0.09461 0.05908 = 0.07583 0.00228 -0.00287 0.01694 AFIX 43 H7 2 0.353368 -0.110861 0.452682 11.00000 -1.20000 AFIX 0 C8 1 0.371415 0.054205 0.402893 11.00000 0.07131 0.07059 = 0.06335 -0.00561 -0.00145 0.01761 AFIX 43 H8 2 0.450362 0.052357 0.399582 11.00000 -1.20000 AFIX 0 C9 1 0.039750 0.326908 0.347535 11.00000 0.06089 0.05789 = 0.05774 0.00052 -0.00179 0.00384 C10 1 0.459449 0.297229 0.325143 11.00000 0.06230 0.08187 = 0.05923 -0.00004 0.01191 0.00235 AFIX 23 H10A 2 0.457779 0.366953 0.281843 11.00000 -1.20000 H10B 2 0.494925 0.234033 0.289104 11.00000 -1.20000 AFIX 0 C11 1 0.533204 0.323145 0.423331 11.00000 0.05372 0.05029 = 0.06278 0.00312 0.00774 0.00422 C12 1 0.488683 0.337123 0.516688 11.00000 0.05559 0.07320 = 0.06550 -0.00203 0.00915 0.00470 AFIX 43 H12 2 0.410029 0.331502 0.520808 11.00000 -1.20000 AFIX 0 C13 1 0.560767 0.359478 0.604164 11.00000 0.08383 0.07365 = 0.06354 -0.00232 0.00187 0.00374 AFIX 43 H13 2 0.530108 0.368113 0.666879 11.00000 -1.20000 AFIX 0 C14 1 0.676250 0.369012 0.599581 11.00000 0.07896 0.06032 = 0.08623 0.00300 -0.01821 -0.00453 AFIX 43 H14 2 0.724251 0.382988 0.658889 11.00000 -1.20000 AFIX 0 C15 1 0.720833 0.357834 0.506977 11.00000 0.05423 0.07287 = 0.10911 0.00936 -0.00333 -0.00907 AFIX 43 H15 2 0.799359 0.365787 0.503215 11.00000 -1.20000 AFIX 0 C16 1 0.650491 0.334949 0.419499 11.00000 0.06013 0.06629 = 0.08226 0.00585 0.01795 -0.00103 AFIX 43 H16 2 0.681900 0.327295 0.357037 11.00000 -1.20000 AFIX 0 C17 1 -0.064269 0.503958 0.309651 11.00000 0.05867 0.06660 = 0.07102 0.01929 0.01157 0.00994 C18 1 -0.146162 0.485327 0.229928 11.00000 0.07632 0.07860 = 0.07682 0.00494 0.00880 0.00165 AFIX 43 H18 2 -0.137223 0.426335 0.181764 11.00000 -1.20000 AFIX 0 C19 1 -0.242877 0.556734 0.222822 11.00000 0.06992 0.11331 = 0.07775 0.02342 -0.00417 0.00702 AFIX 43 H19 2 -0.299584 0.545473 0.169263 11.00000 -1.20000 AFIX 0 C20 1 -0.255674 0.643103 0.293392 11.00000 0.07961 0.10926 = 0.08870 0.03111 0.02055 0.03656 AFIX 43 H20 2 -0.320993 0.690242 0.287987 11.00000 -1.20000 AFIX 0 C21 1 -0.173318 0.660443 0.371501 11.00000 0.10707 0.09772 = 0.07575 0.00338 0.02382 0.03304 AFIX 43 H21 2 -0.182387 0.719619 0.419469 11.00000 -1.20000 AFIX 0 C22 1 -0.076613 0.591315 0.380346 11.00000 0.08043 0.09115 = 0.06135 0.01042 0.00469 0.01333 AFIX 43 H22 2 -0.020031 0.603670 0.433813 11.00000 -1.20000 AFIX 0 HKLF 4 REM wj1001 in P2(1)/n REM R1 = 0.0469 for 2705 Fo > 4sig(Fo) and 0.0515 for all 3071 data REM 227 parameters refined using 1 restraints END WGHT 0.0903 0.1537 REM Highest difference peak 0.190, deepest hole -0.191, 1-sigma level 0.032 Q1 1 0.0123 0.3811 0.2741 11.00000 0.05 0.19 Q2 1 -0.2373 0.4849 0.1955 11.00000 0.05 0.14 Q3 1 0.2018 0.3345 0.3797 11.00000 0.05 0.14 Q4 1 0.1596 0.2234 0.3905 11.00000 0.05 0.14 Q5 1 0.1865 0.3034 0.2969 11.00000 0.05 0.14 Q6 1 -0.1243 0.4618 0.2904 11.00000 0.05 0.13 Q7 1 0.6821 0.4018 0.5421 11.00000 0.05 0.12 Q8 1 0.3401 0.2362 0.3968 11.00000 0.05 0.12 Q9 1 0.4990 0.3014 0.3829 11.00000 0.05 0.12 Q10 1 0.5043 0.3733 0.4629 11.00000 0.05 0.12 Q11 1 -0.0025 0.3040 0.4126 11.00000 0.05 0.11 Q12 1 0.0396 0.4257 0.3673 11.00000 0.05 0.11 Q13 1 0.2424 0.1399 0.3476 11.00000 0.05 0.11 Q14 1 0.5996 0.2827 0.4237 11.00000 0.05 0.11 Q15 1 -0.0930 0.5230 0.3675 11.00000 0.05 0.10 Q16 1 0.1445 0.1034 0.3615 11.00000 0.05 0.10 Q17 1 0.3189 0.3190 0.3808 11.00000 0.05 0.10 Q18 1 0.6245 0.4135 0.6127 11.00000 0.05 0.10 Q19 1 0.6816 0.4007 0.4513 11.00000 0.05 0.10 Q20 1 0.3371 0.0928 0.3604 11.00000 0.05 0.10 ; _shelx_res_checksum 77866 _shelx_hkl_file ; -13 0 -3 43.85 17.90 -13 0 -1 309.04 49.42 -13 0 1 964.66 93.15 -13 0 3 288.31 50.73 -13 0 5 0.02 15.57 -13 0 7 215.21 25.13 -13 1 -4 0.01 15.33 -13 1 -3 0.06 18.71 -13 1 -2 16.48 17.73 -13 1 -1 1235.50 99.45 -13 1 0 65.72 22.13 -13 1 1 81.34 19.76 -13 1 2 533.98 96.35 -13 1 3 364.17 51.12 -13 1 4 93.55 19.34 -13 1 5 910.42 47.94 -13 1 6 305.74 22.58 -13 2 -3 139.80 33.08 -13 2 -2 375.96 56.64 -13 2 -1 7.28 20.53 -13 2 0 1638.47 118.26 -13 2 1 176.79 42.41 -13 2 2 192.82 44.54 -13 2 3 316.14 51.67 -13 2 4 219.13 41.40 -13 2 5 592.48 46.24 -13 2 6 606.14 35.65 -13 3 -3 130.10 30.40 -13 3 -2 291.77 48.74 -13 3 -1 38.59 19.10 -13 3 0 648.13 72.43 -13 3 1 366.48 58.94 -13 3 2 92.70 33.53 -13 3 3 346.26 53.35 -13 3 4 28.38 20.13 -13 3 5 96.92 24.86 -13 4 -2 91.54 28.47 -13 4 -1 234.68 42.90 -13 4 0 15.39 26.33 -13 4 1 0.13 18.38 -13 4 2 90.21 32.27 -13 4 3 170.39 36.46 -13 4 4 4.93 18.71 -12 0 -6 81.61 25.80 -12 0 -4 581.03 71.82 -12 0 -2 131.03 34.76 -12 0 0 530.30 77.55 -12 0 2 800.88 91.34 -12 0 4 989.78 70.59 -12 0 6 4.98 19.94 -12 0 8 0.02 14.99 -12 1 -6 487.21 57.79 -12 1 -5 512.49 63.74 -12 1 -4 22.37 26.27 -12 1 -3 20.40 16.12 -12 1 -2 343.50 40.67 -12 1 -1 1778.71 108.50 -12 1 0 271.15 39.80 -12 1 1 275.46 64.70 -12 1 2 4316.26 148.74 -12 1 3 443.97 47.83 -12 1 4 326.94 28.35 -12 1 5 1149.65 52.43 -12 1 6 4.83 11.85 -12 1 7 98.49 19.35 -12 1 8 26.09 14.07 -12 1 9 223.95 19.50 -12 2 -6 147.58 33.08 -12 2 -5 10.71 22.82 -12 2 -4 65.78 30.93 -12 2 -3 506.04 70.71 -12 2 -2 27.03 25.80 -12 2 -1 50.81 27.43 -12 2 0 124.52 40.53 -12 2 1 2918.00 172.91 -12 2 2 10.67 24.62 -12 2 3 408.87 47.70 -12 2 4 81.25 14.26 -12 2 5 12.14 9.69 -12 2 6 28.05 12.75 -12 2 7 491.10 36.10 -12 2 8 43.31 12.50 -12 3 -6 93.07 25.12 -12 3 -5 293.13 47.30 -12 3 -4 20.12 26.53 -12 3 -3 22.13 26.60 -12 3 -2 245.64 47.52 -12 3 -1 720.57 79.77 -12 3 0 106.90 28.57 -12 3 1 294.67 41.98 -12 3 2 1155.98 60.12 -12 3 3 571.05 53.25 -12 3 4 48.47 13.59 -12 3 5 549.03 35.17 -12 3 6 38.51 12.03 -12 3 7 0.00 14.14 -12 3 8 0.06 10.82 -12 4 -5 27.01 17.92 -12 4 -4 22.24 23.85 -12 4 -3 380.15 58.76 -12 4 -2 169.48 29.58 -12 4 -1 110.13 28.67 -12 4 0 136.85 30.41 -12 4 1 464.57 38.55 -12 4 2 48.75 16.74 -12 4 3 1819.25 90.69 -12 4 4 195.07 31.35 -12 4 5 170.93 20.46 -12 4 6 0.12 10.00 -12 4 7 59.90 13.81 -12 5 -4 301.65 46.61 -12 5 -3 0.09 20.43 -12 5 -2 375.10 39.32 -12 5 -1 24.73 15.32 -12 5 0 298.37 38.48 -12 5 1 561.83 34.71 -12 5 2 248.26 23.65 -12 5 3 582.04 34.33 -12 5 4 88.72 17.51 -12 5 5 138.73 15.07 -12 5 6 127.81 15.63 -12 6 -2 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991.75 55.39 4 1 12 39.23 14.38 4 1 13 312.89 27.55 4 1 14 572.50 36.61 4 2 4 108.80 17.14 4 2 5 7054.91 171.01 4 2 6 95.08 36.28 4 2 7 465.13 81.47 4 2 8 28.08 57.98 4 2 9 1589.33 69.69 4 2 10 2530.39 102.98 4 2 11 882.43 51.89 4 2 12 18.26 13.40 4 2 13 419.72 30.88 4 2 14 111.01 21.33 4 3 4 3839.39 107.46 4 3 532723.79 476.55 4 3 6 307.18 37.90 4 3 7 2837.83 130.81 4 3 8 671.16 40.40 4 3 9 711.78 47.55 4 3 10 321.59 33.41 4 3 11 263.93 25.84 4 3 12 0.11 13.07 4 3 13 0.01 13.28 4 3 14 79.37 13.97 4 4 4 279.08 32.11 4 4 5 12.92 16.91 4 4 6 6946.65 197.55 4 4 7 3409.40 148.66 4 4 8 604.69 43.31 4 4 9 1212.40 61.73 4 4 10 32.16 15.60 4 4 11 224.44 31.21 4 4 12 236.32 29.75 4 4 13 770.85 55.47 4 5 4 8298.45 183.82 4 5 5 1941.67 98.24 4 5 6 2240.58 118.13 4 5 7 1336.98 69.27 4 5 8 57.32 17.39 4 5 9 969.82 55.56 4 5 10 1762.37 84.16 4 5 11 0.03 15.47 4 5 12 17.08 18.22 4 5 13 79.48 19.55 4 6 4 24.47 19.04 4 6 5 26.40 30.03 4 6 6 103.35 23.95 4 6 7 78.07 22.00 4 6 8 157.06 33.03 4 6 9 403.46 51.02 4 6 10 1507.44 92.26 4 6 11 80.93 19.47 4 6 12 30.35 10.84 4 7 4 7058.07 135.35 4 7 5 4324.75 139.18 4 7 6 15.44 21.44 4 7 7 0.00 23.74 4 7 8 2804.52 178.30 4 7 9 1640.68 97.16 4 7 10 33.44 20.70 4 7 11 791.63 48.56 4 7 12 806.73 41.10 4 8 4 267.80 27.33 4 8 5 1244.33 72.24 4 8 6 3966.16 125.82 4 8 7 44.27 31.64 4 8 8 561.49 56.55 4 8 9 774.21 70.05 4 8 10 989.85 66.35 4 8 11 1744.49 63.28 4 9 4 431.81 38.08 4 9 5 1261.40 61.98 4 9 6 771.10 54.41 4 9 7 1300.97 81.98 4 9 8 0.00 14.17 4 9 9 425.45 44.53 4 9 10 110.79 18.35 4 10 4 38.00 14.95 4 10 5 8.88 13.95 4 10 6 1319.16 65.65 4 10 7 16.91 24.06 4 10 8 542.25 37.54 4 10 9 153.98 24.03 4 11 4 154.05 24.43 4 11 5 58.72 14.42 4 11 6 400.47 40.49 4 11 7 97.72 19.83 4 12 4 108.12 17.14 4 12 5 9.09 10.46 5 0 5 6260.94 216.06 5 0 7 8539.06 613.91 5 0 9 1024.74 78.54 5 0 11 1914.54 153.93 5 0 13 334.71 61.17 5 1 521477.67 331.94 5 1 6 246.50 41.71 5 1 7 5202.75 212.26 5 1 8 417.54 31.90 5 1 9 3305.89 99.58 5 1 10 3810.08 147.14 5 1 11 104.48 28.54 5 1 12 61.14 21.00 5 1 13 957.49 66.96 5 2 5 2534.36 118.56 5 2 6 35.33 27.65 5 2 7 23.45 30.31 5 2 8 3223.27 197.28 5 2 9 4196.03 128.98 5 2 10 9.58 22.16 5 2 11 26.89 23.91 5 2 12 27.08 20.60 5 2 13 106.20 26.19 5 3 5 1081.96 92.21 5 3 6 105.46 58.73 5 3 7 6116.87 131.97 5 3 8 1043.34 64.41 5 3 9 1294.41 62.87 5 3 10 1103.91 57.80 5 3 11 1145.12 65.73 5 3 12 26.27 13.18 5 3 13 55.78 30.25 5 4 514193.98 341.91 5 4 6 3616.01 204.18 5 4 7 1245.72 59.84 5 4 8 3836.62 107.62 5 4 9 277.37 31.63 5 4 10 870.51 50.64 5 4 11 787.25 45.74 5 4 12 23.32 15.99 5 4 13 2.46 16.71 5 5 5 431.77 56.81 5 5 6 521.76 44.54 5 5 7 654.08 53.41 5 5 8 1492.95 67.54 5 5 9 206.13 30.27 5 5 10 162.43 24.05 5 5 11 65.14 24.80 5 5 12 43.19 16.73 5 6 512419.43 996.41 5 6 6 0.02 22.11 5 6 7 421.82 51.95 5 6 8 1555.82 79.92 5 6 9 2012.09 150.94 5 6 10 1155.10 63.16 5 6 11 2754.11 123.23 5 6 12 591.17 101.30 5 7 5 6259.13 268.76 5 7 611261.02 363.20 5 7 7 1730.44 142.59 5 7 8 5001.28 199.13 5 7 9 8449.05 208.89 5 7 10 12.09 14.30 5 7 11 187.02 22.93 5 8 5 5006.92 140.42 5 8 6 724.65 65.22 5 8 7 6128.98 257.66 5 8 8 671.22 68.71 5 8 9 132.51 29.96 5 8 10 174.31 23.19 5 9 5 958.48 73.93 5 9 6 828.18 65.71 5 9 7 989.48 101.58 5 9 8 43.16 17.90 5 9 9 24.45 16.62 5 10 5 858.24 65.38 5 10 6 1079.35 69.27 5 10 7 17.06 10.90 5 10 8 37.26 19.39 5 11 5 388.50 40.29 5 11 6 336.94 33.73 6 0 6 233.24 96.01 6 0 8 3000.00 134.42 6 0 10 4691.93 235.94 6 0 12 59.51 35.95 6 1 6 2064.46 169.32 6 1 7 1775.39 68.56 6 1 8 210.10 24.60 6 1 9 56.76 21.15 6 1 10 49.54 19.24 6 1 11 1008.02 74.76 6 1 12 1148.58 74.04 6 1 13 101.05 28.75 6 2 610851.70 361.28 6 2 7 211.29 29.85 6 2 8 292.59 35.58 6 2 9 44.57 19.46 6 2 10 288.38 34.70 6 2 11 779.07 66.66 6 2 12 205.14 35.02 6 2 13 713.00 52.02 6 3 6 4874.98 122.48 6 3 7 0.01 23.27 6 3 8 2938.83 107.83 6 3 9 527.88 46.69 6 3 10 66.95 21.79 6 3 11 161.98 30.84 6 3 12 1184.81 74.04 6 3 13 212.98 40.81 6 4 6 315.58 31.06 6 4 7 447.63 37.43 6 4 8 673.49 46.35 6 4 9 1760.16 71.74 6 4 10 1398.89 87.02 6 4 11 220.12 35.34 6 4 12 1339.68 105.29 6 5 6 2302.46 122.63 6 5 7 357.64 33.97 6 5 810946.23 189.37 6 5 9 145.71 28.52 6 5 10 1320.84 81.65 6 5 11 219.02 32.75 6 5 12 401.66 56.64 6 6 612865.99 281.64 6 6 7 2106.09 92.70 6 6 8 9159.10 186.68 6 6 9 2219.20 108.32 6 6 10 9.00 17.64 6 6 11 633.95 97.66 6 7 6 1183.03 83.98 6 7 7 247.44 32.15 6 7 8 642.51 48.65 6 7 9 1397.40 107.77 6 7 10 42.61 18.99 6 8 6 270.52 56.79 6 8 7 922.81 70.42 6 8 8 257.23 36.12 6 8 9 317.75 42.44 6 8 10 427.74 37.61 6 9 6 213.44 48.92 6 9 7 35.81 17.52 6 9 8 8.99 14.12 6 10 6 36.70 17.57 6 10 7 614.91 47.65 7 0 7 980.48 77.78 7 0 9 543.01 57.29 7 0 11 9.85 24.47 7 1 7 6779.93 142.98 7 1 8 182.77 26.97 7 1 9 854.44 50.32 7 1 10 517.39 44.77 7 1 11 1177.34 77.99 7 1 12 473.05 46.15 7 2 7 14.40 30.37 7 2 8 3152.39 111.88 7 2 9 590.71 49.48 7 2 10 2539.21 95.16 7 2 11 80.23 23.46 7 2 12 270.95 35.63 7 3 7 590.50 42.22 7 3 8 79.20 21.26 7 3 9 604.93 48.90 7 3 10 32.45 18.98 7 3 11 385.96 44.16 7 3 12 494.01 44.49 7 4 7 8909.27 189.80 7 4 8 673.58 52.51 7 4 9 376.30 39.09 7 4 10 1062.29 73.60 7 4 11 2324.21 141.66 7 5 7 1166.16 59.51 7 5 8 5223.39 121.15 7 5 9 176.29 35.38 7 5 10 662.62 80.14 7 5 11 1280.29 99.23 7 6 7 22.12 16.67 7 6 8 1880.68 81.24 7 6 9 602.13 102.10 7 6 10 10.85 21.37 7 7 7 649.28 47.44 7 7 8 49.53 28.71 7 7 9 756.12 55.34 7 7 10 366.89 33.44 7 8 7 403.11 46.15 7 8 8 1.35 17.29 7 8 9 29.00 11.30 7 9 7 206.49 29.82 8 0 8 1121.96 82.15 8 0 10 78.33 33.73 8 1 8 137.74 21.63 8 1 9 1704.68 67.77 8 1 10 822.77 68.22 8 1 11 778.11 59.68 8 2 8 4585.99 132.69 8 2 9 989.48 59.88 8 2 10 206.84 29.41 8 2 11 1302.21 72.03 8 3 8 52.26 17.41 8 3 9 1505.97 73.28 8 3 10 113.38 28.05 8 3 11 149.52 26.24 8 4 8 1417.38 72.07 8 4 9 186.55 27.20 8 4 10 622.31 75.50 8 4 11 86.21 28.20 8 5 8 225.11 37.50 8 5 9 24.29 28.41 8 5 10 130.04 35.36 8 6 8 168.09 30.23 8 6 9 166.51 40.49 8 7 8 70.31 15.94 8 7 9 185.18 37.20 8 8 8 0.01 11.63 9 0 9 921.51 67.76 9 0 11 289.80 43.33 9 1 9 1767.40 76.02 9 1 10 725.63 55.09 9 2 9 29.33 14.57 9 2 10 67.48 41.70 9 3 9 344.23 34.49 9 3 10 478.12 61.31 9 4 9 114.65 25.22 9 4 10 60.56 23.86 9 5 9 0.01 29.26 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 89199 _olex2_submission_special_instructions 'No special instructions were received'