############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_global _audit_creation_method SHELXL-97 _journal_date_recd_electronic 2013-12-11 _journal_date_accepted 2013-12-13 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2014 _journal_volume 70 _journal_issue 1 _journal_page_first o75 _journal_page_last o75 _journal_paper_category QO _journal_paper_doi 10.1107/S1600536813033795 _journal_coeditor_code IS5327 _publ_contact_author_name 'Dr. Akira Uchida' _publ_contact_author_address ; Department of Biomolecular Science Faculty of Science Toho University 2-2-1 Miyama Funabashi Chiba 274-8510 Japan ; _publ_contact_author_email auchida@biomol.sci.toho-u.ac.jp _publ_contact_author_fax '81 47 472 1188' _publ_contact_author_phone '81 47 472 7609' _publ_section_title ;\ (1S*,2S*,4R*,5R*)-Cyclohexane-1,2,4,5-\ tetracarboxylic acid ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Uchida, Akira' . ; Department of Biomolecular Science Faculty of Science Toho University 2-2-1 Miyama Funabashi Chiba 274-8510 Japan ; 'Hasegawa, Masatoshi' . ; Department of Chemistry Faculty of Science Toho University 2-2-1 Miyama Funabashi Chiba 274-8510 Japan ; 'Yamaguchi, Shinya' . ; Department of Research and Development, Gas Chemical Division, Iwatani Industrial Gases Corporation Ltd. 10 Otakasu-cho Amagasaki Hyogo 660-0842 Japan ; 'Takezawa, Eiichiro' . ; Department of Research and Development, Gas Chemical Division, Iwatani Industrial Gases Corporation Ltd. 10 Otakasu-cho Amagasaki Hyogo 660-0842 Japan ; 'Ishikawa, Atsushi' . ; Department of Research and Development, Gas Chemical Division, Iwatani Industrial Gases Corporation Ltd. 10 Otakasu-cho Amagasaki Hyogo 660-0842 Japan ; 'Kagayama, Takashi' . ; Department of Research and Development, Gas Chemical Division, Iwatani Industrial Gases Corporation Ltd. 10 Otakasu-cho Amagasaki Hyogo 660-0842 Japan ; data_I _database_code_depnum_ccdc_archive 'CCDC 976953' _audit_creation_method SHELXL-2013 _chemical_name_systematic ;\ (1S*,2S*,4R*,5R*)-Cyclohexane-1,2,4,5-\ tetracarboxylic acid ; _chemical_name_common ? _chemical_formula_moiety 'C10 H12 O8' _chemical_formula_sum 'C10 H12 O8' _chemical_formula_iupac 'C10 H12 O8' _chemical_formula_weight 260.20 _chemical_melting_point ? _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 trigonal _space_group_name_H-M_alt 'R -3' _space_group_name_Hall '-R 3' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.6970(6) _cell_length_b 17.6970(6) _cell_length_c 9.5455(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2589.0(2) _cell_formula_units_Z 9 _cell_measurement_reflns_used 2340 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.02 _cell_measurement_temperature 298(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.260 _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _shelx_estimated_absorpt_T_min 0.957 _shelx_estimated_absorpt_T_max 0.966 _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.966 _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type ; Bruker APEXII CCD area-detector ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6439 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_theta_min 2.302 _diffrn_reflns_theta_max 29.993 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _refine_special_details ? _reflns_number_total 1653 _reflns_number_gt 1388 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_gt 0.1131 _refine_ls_wR_factor_ref 0.1189 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_number_reflns 1653 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+1.9122P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.377 _refine_diff_density_min -0.208 _refine_ls_extinction_method none _refine_ls_extinction_coef . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2007)' _computing_data_reduction 'SAINT-Plus (Bruker, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009) ; _computing_publication_material 'SHELXL2013 (Sheldrick, 2008)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.51496(8) 0.07671(7) -0.08154(11) 0.0279(3) Uani d 1 . . H H1A 0.4929 0.1116 -0.1242 0.034 Uiso calc 1 . . H H1B 0.5770 0.1045 -0.1011 0.034 Uiso calc 1 . . C C2 0.50063(7) 0.07293(7) 0.07787(11) 0.0233(2) Uani d 1 . . H H2 0.4383 0.0484 0.0969 0.028 Uiso calc 1 . . C C3 0.53165(7) 0.01523(7) 0.14585(11) 0.0242(2) Uani d 1 . . H H3 0.5944 0.0414 0.1285 0.029 Uiso calc 1 . . C C4 0.55013(8) 0.16503(7) 0.13456(12) 0.0283(3) Uani d 1 . . C C5 0.51702(8) 0.00882(8) 0.30236(12) 0.0267(3) Uani d 1 . . O O1 0.62253(6) 0.19739(7) 0.18327(13) 0.0471(3) Uani d 1 . . H H4 0.5352(17) 0.2558(18) 0.151(3) 0.083(8) Uiso d 1 . . O O2 0.50596(8) 0.20615(8) 0.12244(15) 0.0543(3) Uani d 1 . . O O3 0.46919(7) 0.03210(7) 0.35746(9) 0.0380(3) Uani d 1 . . O O4 0.55716(7) -0.02417(7) 0.37025(10) 0.0400(3) Uani d 1 . . H H5 0.5485(19) -0.0245(19) 0.467(3) 0.110(10) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0389(6) 0.0247(5) 0.0218(5) 0.0171(5) 0.0021(4) 0.0033(4) C2 0.0259(5) 0.0227(5) 0.0214(5) 0.0123(4) 0.0009(4) 0.0002(4) C3 0.0274(5) 0.0268(5) 0.0198(5) 0.0147(4) 0.0014(4) 0.0015(4) C4 0.0309(6) 0.0246(5) 0.0267(5) 0.0119(5) 0.0041(4) 0.0008(4) C5 0.0310(6) 0.0282(5) 0.0214(5) 0.0153(5) -0.0010(4) 0.0009(4) O1 0.0302(5) 0.0342(5) 0.0672(8) 0.0088(4) -0.0056(5) -0.0095(5) O2 0.0559(7) 0.0333(5) 0.0820(9) 0.0285(5) -0.0212(6) -0.0187(5) O3 0.0517(6) 0.0540(6) 0.0237(4) 0.0380(5) 0.0042(4) 0.0031(4) O4 0.0531(6) 0.0611(7) 0.0238(4) 0.0420(6) 0.0015(4) 0.0059(4) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C3 10_655 1.5370(16) ? C1 C2 . 1.5386(15) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C4 . 1.5130(15) ? C2 C3 . 1.5251(15) ? C2 H2 . 0.9800 ? C3 C5 . 1.5108(15) ? C3 H3 . 0.9800 ? C4 O1 . 1.2049(16) ? C4 O2 . 1.3126(16) ? C5 O3 . 1.2295(15) ? C5 O4 . 1.2961(14) ? O2 H4 . 0.81(3) ? O4 H5 . 0.94(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 C1 C2 10_655 . 111.06(9) ? C3 C1 H1A 10_655 . 109.4 ? C2 C1 H1A . . 109.4 ? C3 C1 H1B 10_655 . 109.4 ? C2 C1 H1B . . 109.4 ? H1A C1 H1B . . 108.0 ? C4 C2 C3 . . 111.15(9) ? C4 C2 C1 . . 108.23(9) ? C3 C2 C1 . . 110.07(9) ? C4 C2 H2 . . 109.1 ? C3 C2 H2 . . 109.1 ? C1 C2 H2 . . 109.1 ? C5 C3 C2 . . 111.43(9) ? C5 C3 C1 . 10_655 109.53(9) ? C2 C3 C1 . 10_655 110.89(9) ? C5 C3 H3 . . 108.3 ? C2 C3 H3 . . 108.3 ? C1 C3 H3 10_655 . 108.3 ? O1 C4 O2 . . 123.84(12) ? O1 C4 C2 . . 123.74(11) ? O2 C4 C2 . . 112.41(11) ? O3 C5 O4 . . 124.14(11) ? O3 C5 C3 . . 121.25(10) ? O4 C5 C3 . . 114.60(10) ? C4 O2 H4 . . 109.5(18) ? C5 O4 H5 . . 111.8(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C3 C1 C2 C4 10_655 . . . 178.45(9) ? C3 C1 C2 C3 10_655 . . . 56.81(13) ? C4 C2 C3 C5 . . . . 61.11(12) ? C1 C2 C3 C5 . . . . -179.00(9) ? C4 C2 C3 C1 . . . 10_655 -176.60(9) ? C1 C2 C3 C1 . . . 10_655 -56.70(13) ? C3 C2 C4 O1 . . . . 25.59(16) ? C1 C2 C4 O1 . . . . -95.39(14) ? C3 C2 C4 O2 . . . . -155.53(11) ? C1 C2 C4 O2 . . . . 83.49(13) ? C2 C3 C5 O3 . . . . 14.47(16) ? C1 C3 C5 O3 10_655 . . . -108.61(13) ? C2 C3 C5 O4 . . . . -166.81(10) ? C1 C3 C5 O4 10_655 . . . 70.12(13) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O2 H4 O1 3_665 0.81(3) 1.93(3) 2.705(2) 160(3) O4 H5 O3 10_656 0.94(3) 1.70(3) 2.6320(10) 176(3) _shelx_hkl_checksum 71526 _shelx_hkl_file ; -2 1 0 715.11 9.61 -1 -1 0 729.53 9.68 -1 -1 0 713.89 9.78 -1 2 0 713.88 9.67 1 1 0 725.62 9.63 -2 1 0 716.87 9.60 -3 0 0 6763.58 89.97 -3 3 0 6643.64 85.02 0 -3 0 6570.99 87.30 0 3 0 6779.08 86.42 -3 3 0 6657.72 86.61 -3 0 0 6643.63 83.40 -2 -2 0 7319.96 91.30 2 2 0 7163.24 88.49 -4 2 0 7236.23 92.15 -2 4 0 7156.14 92.50 -4 2 0 6947.52 89.45 -2 -2 0 7096.77 92.43 -1 -4 0 9443.14 125.30 1 4 0 9999.66 125.79 -5 1 0 9656.50 122.00 -4 5 0 9650.72 119.25 -1 -4 0 9458.50 118.75 -4 5 0 9684.07 123.97 -5 1 0 9615.53 121.99 -5 4 0 71.22 2.26 -1 5 0 72.53 2.62 -4 -1 0 76.32 2.67 -4 -1 0 75.77 1.82 -5 4 0 71.89 2.53 -6 3 0 1486.20 19.91 -3 -3 0 1510.31 20.27 -3 -3 0 1522.19 19.65 -6 3 0 1499.77 19.96 3 3 0 1480.47 19.95 -6 0 0 297.81 4.53 -6 6 0 286.87 6.10 -6 6 0 292.13 5.35 0 6 0 285.42 6.17 -6 0 0 293.92 5.79 -5 7 0 5137.81 64.69 -5 7 0 5078.84 62.91 -2 -5 0 5157.24 66.33 -7 2 0 5067.42 62.78 2 5 0 5187.47 62.77 -7 2 0 5192.98 62.40 -2 -5 0 5209.84 62.61 -7 5 0 322.72 6.13 -2 7 0 324.05 6.77 5 2 0 318.68 6.34 -5 -2 0 321.69 6.74 -7 5 0 315.82 6.43 -5 -2 0 330.50 5.44 -7 8 0 2216.49 28.13 -8 1 0 2198.10 27.49 -8 1 0 2213.34 29.92 -7 8 0 2185.72 29.84 -8 1 0 2214.71 29.19 1 7 0 2216.80 29.74 4 4 0 107.97 3.50 -4 -4 0 97.98 3.03 -8 4 0 104.84 3.44 -4 8 0 96.93 3.61 -8 4 0 99.16 3.38 -4 -4 0 107.44 3.66 -8 7 0 981.12 14.46 -1 8 0 1005.84 15.75 -7 -1 0 1016.10 13.36 -8 7 0 993.89 15.48 -6 9 0 216.62 4.48 -9 3 0 205.96 5.24 3 6 0 211.96 5.54 -9 3 0 210.63 5.63 -6 9 0 204.76 5.72 -3 -6 0 221.32 5.57 6 3 0 693.07 11.62 -3 9 0 682.22 12.23 -6 -3 0 707.49 10.42 -9 6 0 688.94 11.74 -9 6 0 685.79 11.32 -6 -3 0 678.43 12.13 0 9 0 3.59 1.30 -9 9 0 4.41 1.27 -9 0 0 4.39 1.33 -9 0 0 4.60 1.15 -9 0 0 3.38 0.59 -9 9 0 5.16 1.08 2 8 0 217.45 6.06 -8 10 0 217.71 6.24 -10 2 0 216.31 6.18 -10 2 0 215.56 5.70 -8 10 0 227.80 4.99 -5 10 0 43.57 2.92 -5 -5 0 41.84 2.30 -10 5 0 43.21 2.56 -5 10 0 43.37 1.97 -10 5 0 44.58 2.65 5 5 0 42.72 2.56 -5 -5 0 37.24 2.57 -10 8 0 888.11 13.87 -8 -2 0 893.38 12.38 -10 8 0 864.57 14.73 -2 10 0 889.65 15.21 -8 -2 0 878.52 15.22 8 2 0 865.43 14.35 1 10 0 91.80 4.37 -10 11 0 89.66 3.27 -10 11 0 90.54 4.20 -11 1 0 88.39 3.82 -11 1 0 83.45 4.17 -11 4 0 281.89 6.82 -7 11 0 295.56 5.80 -11 4 0 271.46 7.11 -7 11 0 269.07 7.31 -4 -7 0 291.15 7.26 4 7 0 287.24 7.20 -7 -4 0 2.78 1.24 7 4 0 2.88 1.11 -7 -4 0 3.62 0.96 -4 11 0 2.04 1.28 -11 7 0 1.03 1.07 -11 7 0 0.53 0.89 -11 10 0 722.64 12.10 -10 -1 0 714.76 13.80 -11 10 0 723.46 13.46 -1 11 0 693.47 13.57 10 1 0 721.46 12.93 -9 12 0 73.73 2.94 3 9 0 70.43 3.84 -12 3 0 77.23 3.97 -9 12 0 66.25 3.79 -12 3 0 65.47 3.41 -12 6 0 69.78 3.44 6 6 0 68.87 3.59 -12 6 0 66.81 3.49 -6 12 0 78.86 4.03 -6 -6 0 85.84 4.02 -6 12 0 79.04 2.83 -12 9 0 1.95 1.10 9 3 0 1.56 1.18 -12 9 0 2.14 1.17 -3 12 0 1.95 1.46 -9 -3 0 0.56 1.22 -9 -3 0 1.72 0.85 -12 12 0 10.05 1.60 -12 0 0 13.66 2.06 0 12 0 14.19 2.39 -12 12 0 11.14 2.06 -12 0 0 14.39 2.42 -13 2 0 14.32 2.09 -11 13 0 8.56 2.01 -13 2 0 10.27 2.08 2 11 0 9.30 2.05 -11 13 0 13.86 1.65 5 8 0 11.01 2.00 -8 13 0 11.43 1.42 -13 5 0 13.39 1.99 -13 5 0 8.83 1.86 -8 13 0 8.76 1.96 -5 -8 0 10.64 1.95 8 5 0 4.00 1.38 -13 8 0 0.93 1.23 -8 -5 0 -0.11 1.16 -13 8 0 1.55 1.28 -5 13 0 5.04 1.71 -11 -2 0 5.08 1.65 11 2 0 5.15 1.54 -13 11 0 5.92 1.46 -2 13 0 6.69 1.84 -13 11 0 2.52 1.55 -13 14 0 486.54 11.85 -14 1 0 467.58 11.79 1 13 0 488.79 11.79 -14 1 0 476.60 10.86 -14 4 0 806.94 14.78 -14 4 0 801.37 15.64 4 10 0 812.85 15.48 -10 14 0 826.08 16.10 -14 7 0 585.27 12.02 -7 14 0 570.93 9.83 7 7 0 554.91 11.76 -14 7 0 575.67 11.83 -7 -7 0 538.91 12.14 -7 14 0 550.25 12.48 -14 10 0 472.04 10.19 -4 14 0 489.42 11.70 -14 10 0 487.07 11.07 -10 -4 0 488.66 11.59 10 4 0 482.54 10.66 -13 -1 0 18.46 2.82 -1 14 0 18.29 2.81 13 1 0 13.34 2.19 -14 13 0 19.44 2.22 -14 13 0 17.02 2.63 -15 3 0 200.10 7.32 -12 15 0 197.25 7.33 3 12 0 214.84 7.43 -15 3 0 202.84 6.73 -15 6 0 417.39 10.42 6 9 0 400.06 10.03 -15 6 0 396.77 9.69 -9 15 0 426.65 11.00 9 6 0 562.90 12.16 -6 15 0 547.10 12.94 -15 9 0 579.15 12.10 -15 9 0 568.39 12.39 -9 -6 0 563.99 12.86 12 3 0 40.62 3.17 -12 -3 0 38.79 3.64 -3 15 0 33.91 3.57 -15 12 0 38.28 3.40 -15 12 0 35.89 2.87 0 15 0 137.68 6.39 -15 0 0 138.43 6.55 15 0 0 154.70 6.08 -15 15 0 145.44 6.41 -16 2 0 177.81 7.35 -14 16 0 178.82 7.28 2 14 0 178.97 7.21 -16 2 0 166.93 6.41 -16 5 0 368.93 10.36 -16 5 0 376.76 9.64 -11 16 0 375.63 10.65 5 11 0 366.22 9.99 -8 16 0 13.86 2.59 -16 8 0 15.31 2.56 8 8 0 19.20 2.64 -16 8 0 16.31 2.49 -8 -8 0 15.90 2.60 -16 11 0 268.03 7.78 -16 11 0 274.52 8.51 -11 -5 0 252.40 8.61 11 5 0 267.54 8.01 -5 16 0 263.39 8.81 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5.30 2.31 -1 19 4 1.33 1.78 21 -2 -4 18.51 3.74 -18 20 4 29.99 4.61 2 18 -4 29.31 4.64 -20 2 -4 30.47 4.62 -20 5 -4 11.01 2.98 -15 20 4 14.08 3.13 5 15 -4 12.76 3.08 -12 20 4 20.02 3.60 8 12 -4 21.22 3.76 -20 8 -4 20.85 3.67 -20 11 -4 63.03 5.38 -9 20 4 54.94 5.05 11 9 -4 47.58 4.89 -20 14 -4 27.58 4.00 -6 20 4 35.70 4.30 14 6 -4 27.45 3.98 17 3 -4 0.70 2.16 -3 20 4 1.40 1.72 20 0 -4 4.98 2.75 -21 4 -4 -1.30 2.20 4 17 -4 -0.75 2.13 -17 21 4 -0.77 2.07 -21 7 -4 -3.06 1.61 7 14 -4 -2.10 1.67 -14 21 4 -0.14 1.72 10 11 -4 36.25 4.68 -11 21 4 29.06 4.26 -21 10 -4 23.32 3.93 -8 21 4 3.78 2.13 -21 13 -4 4.25 2.46 13 8 -4 5.36 2.45 -21 16 -4 1.41 2.01 16 5 -4 1.76 2.46 -5 21 4 5.62 2.33 19 2 -4 8.45 2.99 6 16 -4 11.38 3.47 -16 22 4 9.08 3.27 -22 6 -4 8.80 3.26 -13 22 4 10.22 3.14 -22 9 -4 11.28 3.40 9 13 -4 9.85 3.07 -22 12 -4 3.02 2.19 -10 22 4 3.82 2.23 12 10 -4 3.30 2.27 15 7 -4 16.66 3.71 -7 22 4 11.88 3.20 -22 15 -4 5.92 2.61 -4 22 4 109.13 7.03 18 4 -4 116.05 7.33 -23 8 -4 3.76 2.47 8 15 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-10 -0.09 1.25 -3 -2 -10 0.47 1.36 -2 5 -10 0.37 1.55 2 -3 -10 2.71 1.79 -3 1 -10 3.65 1.92 1 2 -10 4.38 1.82 2 -3 -10 3.41 1.58 -3 4 -10 2.05 1.53 -1 -3 -10 -0.33 1.36 4 -1 -10 -0.25 1.24 -1 -3 -10 -0.22 1.38 4 -1 -10 1.20 1.40 7 -4 -10 7.52 2.27 -4 -3 -10 8.00 2.54 -7 4 10 7.86 2.18 -3 7 -10 8.46 2.50 -4 -3 -10 9.04 2.38 -4 0 -10 8.86 2.35 4 -4 -10 10.76 2.62 0 4 -10 4.73 1.84 3 1 -10 16.71 2.83 -4 3 -10 17.81 3.04 1 -4 -10 16.99 3.15 3 1 -10 16.48 2.49 -6 2 10 9.22 2.37 -4 6 -10 12.91 2.87 -2 -4 -10 11.81 2.74 6 -2 -10 12.40 2.57 6 -2 -10 13.84 2.44 -5 -4 -10 12.06 2.65 -4 9 -10 10.86 2.81 -9 5 10 14.86 2.97 -5 -4 -10 17.55 3.21 6 -5 -10 55.29 4.27 -5 -1 -10 50.70 4.24 -1 6 -10 57.84 4.56 2 3 -10 20.35 2.73 2 3 -10 21.58 3.19 -5 2 -10 23.83 3.41 3 -5 -10 19.27 3.22 -5 5 -10 29.37 3.81 0 -5 -10 34.85 4.04 5 0 -10 36.86 3.51 -3 -5 -10 30.23 4.00 -5 8 -10 22.22 3.60 -8 3 10 27.46 3.53 -6 -5 -10 80.65 5.79 -5 11 -10 76.53 5.84 -11 6 10 83.85 5.57 8 -6 -10 132.55 6.36 -6 -2 -10 130.22 6.36 -8 6 10 125.82 6.14 -6 -2 -10 129.66 7.02 -2 8 -10 136.97 7.12 5 -6 -10 9.23 2.33 1 5 -10 8.84 2.27 -6 1 -10 4.45 1.86 4 2 -10 -1.74 1.26 2 -6 -10 0.82 1.54 -6 4 -10 0.42 1.56 -1 -6 -10 0.54 1.60 -6 7 -10 0.82 1.81 -6 10 -10 11.31 2.92 -10 4 10 9.71 2.63 -4 -6 -10 11.49 2.96 -13 7 10 8.09 2.73 -6 13 -10 8.02 2.77 -7 -6 -10 3.27 2.31 -10 7 10 -1.32 1.40 -7 -3 -10 -0.57 1.59 -3 10 -10 -0.98 1.61 -7 -3 -10 1.66 1.90 7 -7 -10 15.27 2.76 -7 0 -10 18.19 3.28 0 7 -10 19.77 3.29 3 4 -10 11.12 2.47 -7 3 -10 13.58 2.88 4 -7 -10 8.63 2.47 1 -7 -10 58.64 5.10 6 1 -10 53.51 4.39 -7 6 -10 59.36 5.08 -9 2 10 226.73 8.75 -7 9 -10 219.16 9.35 -2 -7 -10 202.93 9.12 -5 -7 -10 5.27 2.42 -7 12 -10 13.70 3.33 -12 5 10 8.21 2.59 -15 8 10 5.79 2.74 -8 -7 -10 6.62 2.92 -7 15 -10 4.35 2.60 -12 8 10 35.43 4.40 -4 12 -10 39.85 4.81 -8 -4 -10 39.76 4.69 -8 -4 -10 36.53 4.23 -8 -1 -10 22.93 3.59 -1 9 -10 27.31 3.94 -8 -1 -10 22.83 3.75 9 -8 -10 31.53 3.69 -9 8 10 26.72 3.49 2 6 -10 15.36 2.88 -8 2 -10 23.11 3.61 6 -8 -10 15.62 2.96 5 3 -10 84.51 5.07 3 -8 -10 85.05 5.67 -8 5 -10 87.64 5.84 8 0 -10 13.05 2.79 0 -8 -10 13.30 3.05 -8 8 -10 11.98 2.91 -8 11 -10 66.21 5.81 -3 -8 -10 76.40 5.79 -11 3 10 75.48 5.38 -8 14 -10 6.66 2.91 -14 6 10 3.66 2.34 -6 -8 -10 10.14 2.89 -9 -5 -10 3.70 2.20 -5 14 -10 2.90 2.32 -14 9 10 4.47 2.37 -9 -2 -10 2.62 1.89 -9 -2 -10 2.96 2.23 -11 9 10 4.35 2.08 -2 11 -10 3.47 2.35 -9 1 -10 1.53 1.84 1 8 -10 -0.83 1.48 8 -9 -10 0.40 1.65 5 -9 -10 70.83 5.21 -9 4 -10 80.19 5.52 4 5 -10 85.35 5.17 7 2 -10 -0.68 1.45 2 -9 -10 3.73 2.12 -9 7 -10 0.69 1.96 10 -1 -10 55.74 4.94 -9 10 -10 53.48 5.24 -1 -9 -10 54.04 5.28 -9 13 -10 3.03 2.36 -13 4 10 1.34 2.04 -4 -9 -10 -0.13 1.67 -7 -9 -10 8.45 3.26 -16 7 10 8.45 3.11 -10 -6 -10 0.27 2.17 -16 10 10 3.42 2.42 -10 -3 -10 -0.58 1.97 -3 13 -10 2.54 2.08 -13 10 10 1.08 1.90 -10 -3 -10 -0.06 1.71 -10 0 -10 18.43 3.46 0 10 -10 17.14 3.22 10 -10 -10 14.95 3.02 0 10 -10 17.50 3.39 -10 10 10 19.98 3.48 7 -10 -10 20.91 3.45 3 7 -10 13.16 2.81 -10 3 -10 19.45 3.62 6 4 -10 -0.84 1.47 -10 6 -10 0.46 1.94 4 -10 -10 1.98 1.98 1 -10 -10 55.97 5.36 -10 9 -10 58.70 5.48 9 1 -10 46.81 4.65 -10 12 -10 131.33 7.61 -2 -10 -10 140.94 8.07 -5 -10 -10 6.61 2.87 -10 15 -10 10.96 3.36 -15 5 10 9.71 3.10 -11 -4 -10 25.62 4.19 -15 11 10 22.12 3.94 -11 -4 -10 15.73 3.68 -4 15 -10 27.94 4.46 -1 12 -10 23.14 3.59 -1 12 -10 23.10 3.83 -12 11 10 24.49 3.89 -11 -1 -10 30.15 4.32 -11 -1 -10 24.95 3.98 2 9 -10 0.27 1.66 9 -11 -10 2.73 2.06 -11 2 -10 0.17 1.99 -11 5 -10 9.44 2.62 5 6 -10 9.27 2.62 6 -11 -10 7.33 2.69 -11 8 -10 9.64 3.03 3 -11 -10 4.49 2.52 8 3 -10 1.65 2.10 11 0 -10 63.65 5.47 -11 11 -10 77.65 6.38 0 -11 -10 64.79 6.00 -14 3 10 146.33 8.31 -3 -11 -10 149.89 8.49 -11 14 -10 143.05 8.25 -14 12 10 7.18 2.72 -2 14 -10 3.76 2.23 -12 -2 -10 6.03 2.59 -12 -2 -10 6.00 2.71 11 -12 -10 2.76 2.10 1 11 -10 6.61 2.67 -12 1 -10 2.50 2.22 -11 12 10 3.61 1.92 -12 4 -10 -0.42 1.88 4 8 -10 1.59 1.82 8 -12 -10 4.95 2.51 5 -12 -10 -2.62 1.65 7 5 -10 -3.18 1.29 -12 7 -10 4.38 2.44 10 2 -10 12.59 3.16 2 -12 -10 17.18 3.61 -12 10 -10 18.04 3.79 -1 -12 -10 26.25 4.49 -12 13 -10 37.35 5.02 13 -1 -10 38.83 4.87 -13 13 10 8.60 2.75 0 13 -10 11.84 3.24 -13 0 -10 10.65 3.01 -13 0 -10 12.72 3.44 10 -13 -10 34.10 4.44 3 10 -10 29.75 4.18 -13 3 -10 24.29 4.06 -13 6 -10 75.10 6.19 6 7 -10 79.62 5.50 7 -13 -10 72.09 6.20 -13 9 -10 19.51 3.99 4 -13 -10 14.12 3.35 9 4 -10 13.49 3.11 1 -13 -10 2.74 2.56 -13 12 -10 9.97 3.12 12 1 -10 3.46 2.20 2 12 -10 53.15 5.24 -14 2 -10 55.97 5.67 -12 14 10 50.65 5.14 -14 5 -10 -1.86 2.04 9 -14 -10 0.21 1.92 5 9 -10 -1.47 1.83 6 -14 -10 23.60 4.12 8 6 -10 29.42 4.18 -14 8 -10 20.30 3.90 11 3 -10 3.62 2.44 -14 11 -10 -0.55 2.37 3 -14 -10 1.01 2.04 -15 4 -10 3.73 2.70 4 11 -10 2.73 2.37 11 -15 -10 6.99 2.84 7 8 -10 -1.03 1.91 8 -15 -10 -0.47 2.02 -15 7 -10 2.10 2.25 10 5 -10 1.15 2.13 5 -15 -10 2.91 2.40 -15 10 -10 1.68 2.57 6 10 -10 1.73 2.35 10 -16 -10 1.95 2.24 9 7 -10 14.08 3.31 7 -16 -10 12.36 3.42 0 -1 -11 18.43 3.01 1 0 -11 15.03 2.85 -1 1 -11 15.16 2.87 2 -2 -11 72.05 4.64 0 2 -11 76.49 5.19 2 -2 -11 70.93 5.14 -2 0 -11 83.58 5.25 3 -1 -11 73.21 4.79 -1 -2 -11 80.56 5.57 -2 3 -11 79.20 5.37 -1 -2 -11 66.24 4.59 -3 -1 -11 13.77 2.83 -1 4 -11 13.88 2.90 4 -3 -11 17.84 3.09 2 1 -11 0.13 1.48 -3 2 -11 5.14 2.14 1 -3 -11 -1.80 1.44 -2 -3 -11 152.64 7.78 -3 5 -11 141.15 7.30 5 -2 -11 159.63 7.25 6 -4 -11 38.29 4.09 -4 -2 -11 40.30 4.67 -2 6 -11 43.98 4.70 -4 -2 -11 40.96 4.13 1 3 -11 25.61 3.67 -4 1 -11 33.73 3.99 3 -4 -11 28.61 3.94 -4 4 -11 1.56 2.00 4 0 -11 6.78 2.10 0 -4 -11 5.53 2.14 -4 7 -11 94.93 6.29 7 -3 -11 85.09 5.36 -3 -4 -11 86.21 6.11 -5 -3 -11 21.71 3.88 -3 8 -11 29.27 4.30 5 -5 -11 1.88 1.85 0 5 -11 0.33 1.72 -5 0 -11 1.80 1.79 3 2 -11 10.64 2.54 -5 3 -11 15.43 3.06 2 -5 -11 5.35 2.39 6 -1 -11 124.98 6.16 -5 6 -11 132.82 7.26 -1 -5 -11 117.43 6.93 6 -1 -11 125.06 6.39 -5 9 -11 72.62 6.07 -9 4 11 68.00 5.07 -4 -5 -11 62.37 5.75 -6 -4 -11 160.23 8.38 -4 10 -11 144.60 8.02 -1 7 -11 266.18 10.38 -6 -1 -11 269.43 9.66 7 -6 -11 260.54 9.73 -6 2 -11 138.02 7.15 2 4 -11 136.45 7.01 4 -6 -11 139.20 7.29 5 1 -11 67.30 4.82 1 -6 -11 59.53 5.28 -6 5 -11 51.00 4.99 -6 8 -11 209.34 9.44 8 -2 -11 219.86 8.60 -2 -6 -11 208.70 9.46 -5 -6 -11 2.57 2.12 -6 11 -11 3.37 2.36 -11 5 11 0.78 1.98 -7 -5 -11 2.08 2.17 -12 7 11 3.74 2.23 -5 12 -11 2.93 2.58 -7 -2 -11 3.33 2.12 -7 -2 -11 0.53 2.01 -2 9 -11 2.09 2.06 6 -7 -11 2.60 2.11 1 6 -11 1.51 1.90 -7 1 -11 3.03 2.25 3 -7 -11 207.59 9.20 -7 4 -11 217.45 9.22 4 3 -11 215.19 8.73 7 0 -11 3.39 2.04 -7 7 -11 3.84 2.29 0 -7 -11 4.04 2.26 -7 10 -11 4.65 2.42 -3 -7 -11 -0.98 1.84 -10 3 11 3.37 2.19 -7 13 -11 19.29 4.16 -13 6 11 18.45 3.71 -6 -7 -11 21.94 3.88 -14 8 11 6.03 2.76 -8 -3 -11 64.45 5.90 -3 11 -11 68.41 6.08 8 -8 -11 249.13 9.66 0 8 -11 238.67 9.89 -8 0 -11 264.14 9.90 3 5 -11 34.10 4.17 -8 3 -11 36.94 4.47 5 -8 -11 36.20 4.47 -8 6 -11 37.49 4.76 6 2 -11 36.19 4.03 2 -8 -11 37.32 4.60 -8 9 -11 80.83 6.09 -1 -8 -11 76.30 5.99 9 -1 -11 73.13 5.43 -8 12 -11 4.23 2.93 -12 4 11 2.47 2.17 -4 -8 -11 2.25 2.19 -4 13 -11 5.16 2.76 -13 9 11 3.22 2.30 -9 -4 -11 5.91 2.79 -9 -1 -11 13.44 3.16 -9 -1 -11 11.00 3.12 -1 10 -11 15.63 3.40 7 -9 -11 77.82 5.80 -9 2 -11 72.54 5.66 2 7 -11 79.90 5.83 5 4 -11 5.15 2.07 -9 5 -11 9.45 2.91 4 -9 -11 4.24 2.19 1 -9 -11 119.44 7.41 8 1 -11 119.02 6.67 -9 8 -11 106.72 6.96 11 -2 -11 1.27 1.98 -2 -9 -11 -1.94 1.91 -9 11 -11 1.22 2.16 -14 5 11 2.51 2.44 -10 -2 -11 93.76 6.79 -10 -2 -11 98.43 6.68 -2 12 -11 106.95 7.19 -10 1 -11 75.74 5.82 1 9 -11 63.98 5.71 9 -10 -11 67.05 5.62 6 -10 -11 171.87 8.50 -10 4 -11 166.92 8.41 4 6 -11 165.59 7.62 3 -10 -11 14.67 3.53 -10 7 -11 14.57 3.48 7 3 -11 13.23 3.03 10 0 -11 3.76 2.26 0 -10 -11 -0.52 2.18 -10 10 -11 -1.86 1.89 -11 0 -11 3.38 2.45 0 11 -11 2.55 2.03 -11 0 -11 0.40 2.13 3 8 -11 9.65 2.77 8 -11 -11 12.51 3.24 -11 3 -11 4.27 2.85 -11 6 -11 8.69 3.01 6 5 -11 10.86 2.77 5 -11 -11 9.76 3.23 2 -11 -11 0.68 2.25 9 2 -11 0.78 2.03 -11 9 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5.01 -4 8 -12 41.14 5.07 -4 -4 -12 35.37 4.83 -5 -2 -12 24.00 4.18 7 -5 -12 22.88 3.76 -2 7 -12 27.70 4.37 4 -5 -12 13.89 3.03 -5 1 -12 16.05 3.30 1 4 -12 11.13 3.11 -5 4 -12 -1.51 1.75 1 -5 -12 1.75 2.06 4 1 -12 2.06 1.98 -2 -5 -12 16.75 3.55 -5 7 -12 11.25 3.24 -5 10 -12 2.85 2.28 -5 -5 -12 1.26 2.08 -6 -3 -12 37.43 4.98 -3 9 -12 31.92 4.87 6 -6 -12 19.53 3.69 0 6 -12 16.45 3.58 -6 0 -12 26.92 4.04 3 -6 -12 183.32 8.84 -6 3 -12 147.78 7.81 3 3 -12 160.00 7.92 -6 6 -12 36.43 4.85 0 -6 -12 48.89 5.25 -6 9 -12 16.27 3.82 -3 -6 -12 18.44 4.05 -7 -1 -12 50.68 5.12 -1 8 -12 70.59 6.10 -7 -1 -12 58.21 5.85 -7 2 -12 66.63 5.71 5 -7 -12 60.96 5.51 2 5 -12 65.80 5.62 -7 5 -12 52.79 5.44 2 -7 -12 43.18 5.09 5 2 -12 48.25 4.75 -7 8 -12 6.09 2.48 -1 -7 -12 6.94 2.79 1 7 -12 395.88 13.29 7 -8 -12 390.20 12.98 -8 1 -12 393.22 12.88 4 -8 -12 42.59 5.15 -8 4 -12 50.09 5.31 4 4 -12 44.14 4.84 -8 7 -12 28.80 4.53 1 -8 -12 23.51 4.12 7 1 -12 29.25 4.02 -9 0 -12 17.08 3.68 3 6 -12 1.23 2.14 6 -9 -12 4.20 2.72 -9 3 -12 2.50 2.32 -9 6 -12 29.76 4.61 6 3 -12 21.38 3.77 3 -9 -12 29.73 4.52 8 -10 -12 3.88 2.55 -10 2 -12 -2.56 2.03 5 -10 -12 104.35 7.18 5 5 -12 102.72 6.68 -10 5 -12 115.25 7.51 7 -11 -12 90.21 6.61 -11 4 -12 80.59 6.35 1 -1 -13 60.15 5.69 -2 -1 -13 0.87 2.00 -1 3 -13 6.20 2.73 3 -2 -13 0.72 2.13 -2 2 -13 180.44 8.67 0 -2 -13 182.31 9.06 2 0 -13 179.73 8.85 5 -3 -13 55.86 5.39 -2 5 -13 50.85 5.50 2 -3 -13 13.36 3.23 1 2 -13 11.25 3.13 -3 1 -13 15.84 3.43 4 -1 -13 11.04 3.01 -3 4 -13 14.09 3.49 -1 -3 -13 5.66 2.64 0 4 -13 120.74 7.33 4 -4 -13 122.85 7.39 -4 3 -13 -2.37 1.92 1 -4 -13 -1.85 1.66 -4 6 -13 31.86 4.86 3 -5 -13 9.14 2.77 2 3 -13 12.26 3.25 -5 2 -13 11.87 3.42 -5 5 -13 7.98 2.92 4 2 -13 2.19 2.25 -6 4 -13 0.87 2.13 0 0 0 0.00 0.00 0 0 0 0.00 0.00 ; _shelx_res_checksum 10381 _shelx_res_file ; TITL hasegawa2 in R-3 CELL 0.71073 17.6970 17.6970 9.5455 90.000 90.000 120.000 ZERR 9.00 0.0006 0.0006 0.0006 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H O UNIT 90 108 72 L.S. 4 BOND $H ACTA CONF SIZE 0.33 0.26 0.26 FMAP 2 PLAN 20 TEMP 0 WGHT 0.060700 1.912200 FVAR 0.40364 MOLE 1 C1 1 0.514964 0.076711 -0.081540 11.00000 0.03890 0.02472 = 0.02183 0.00327 0.00208 0.01713 AFIX 23 H1A 2 0.492890 0.111607 -0.124180 11.00000 -1.20000 H1B 2 0.576963 0.104532 -0.101104 11.00000 -1.20000 AFIX 0 C2 1 0.500627 0.072927 0.077874 11.00000 0.02595 0.02272 = 0.02141 0.00022 0.00087 0.01226 AFIX 13 H2 2 0.438271 0.048432 0.096934 11.00000 -1.20000 AFIX 0 C3 1 0.531650 0.015225 0.145850 11.00000 0.02742 0.02676 = 0.01983 0.00147 0.00142 0.01467 AFIX 13 H3 2 0.594382 0.041373 0.128477 11.00000 -1.20000 AFIX 0 C4 1 0.550134 0.165028 0.134564 11.00000 0.03087 0.02463 = 0.02666 0.00077 0.00414 0.01189 C5 1 0.517022 0.008820 0.302361 11.00000 0.03102 0.02822 = 0.02138 0.00092 -0.00103 0.01529 O1 3 0.622526 0.197387 0.183267 11.00000 0.03024 0.03420 = 0.06720 -0.00954 -0.00556 0.00882 H4 2 0.535239 0.255785 0.151410 11.00000 0.08276 O2 3 0.505964 0.206154 0.122441 11.00000 0.05586 0.03326 = 0.08203 -0.01874 -0.02123 0.02849 O3 3 0.469189 0.032100 0.357461 11.00000 0.05167 0.05401 = 0.02366 0.00314 0.00424 0.03797 O4 3 0.557156 -0.024170 0.370247 11.00000 0.05306 0.06110 = 0.02380 0.00587 0.00150 0.04199 H5 2 0.548467 -0.024466 0.467192 11.00000 0.10961 HKLF 4 REM hasegawa2 in R-3 REM R1 = 0.0414 for 1388 Fo > 4sig(Fo) and 0.0491 for all 1653 data REM 90 parameters refined using 0 restraints END WGHT 0.0582 2.0431 REM Highest difference peak 0.377, deepest hole -0.208, 1-sigma level 0.045 Q1 1 0.6667 0.3333 -0.1667 10.16667 0.05 0.38 Q2 1 0.5249 0.1176 0.1065 11.00000 0.05 0.36 Q3 1 0.5168 0.0051 0.2192 11.00000 0.05 0.34 Q4 1 0.6201 0.2069 0.1051 11.00000 0.05 0.30 Q5 1 0.5111 0.0764 0.0030 11.00000 0.05 0.30 Q6 1 0.5199 0.0483 0.1102 11.00000 0.05 0.28 Q7 1 0.4942 0.0322 -0.1122 11.00000 0.05 0.28 Q8 1 0.5419 0.2209 0.0656 11.00000 0.05 0.24 Q9 1 0.4666 0.0325 0.4281 11.00000 0.05 0.16 Q10 1 0.5147 0.0528 0.3445 11.00000 0.05 0.14 Q11 1 0.4642 -0.0052 0.3232 11.00000 0.05 0.14 Q12 1 0.6398 0.2461 0.2013 11.00000 0.05 0.13 Q13 1 0.5932 -0.0224 0.3382 11.00000 0.05 0.11 Q14 1 0.6527 0.1753 0.1372 11.00000 0.05 0.11 Q15 1 0.6667 0.3333 0.3333 10.16667 0.05 0.11 Q16 1 0.4582 0.0638 0.3238 11.00000 0.05 0.11 Q17 1 0.6655 0.2989 0.2603 11.00000 0.05 0.10 Q18 1 0.4049 -0.0291 0.2219 11.00000 0.05 0.10 Q19 1 0.5497 0.0091 0.3436 11.00000 0.05 0.10 Q20 1 0.4510 0.1016 -0.1041 11.00000 0.05 0.10 ; _shelxl_version_number .2013