############################################################################## # # # 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 'by CrystalStructure 4.1' _journal_date_recd_electronic 2015-08-25 _journal_date_accepted 2015-09-04 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2015 _journal_volume 71 _journal_issue 10 _journal_page_first o719 _journal_page_last o720 _journal_paper_category HO _journal_paper_doi 10.1107/S2056989015016503 _journal_coeditor_code IS5416 _publ_contact_author_name 'Tomohiko Ishii' _publ_contact_author_address ; Department of Advanced Materials Science Faculty of Engineering Kagawa University 2217-20, Hayashicho, Takamatsu Kagawa 761-0396 Japan ; _publ_contact_author_email tishii@eng.kagawa-u.ac.jp _publ_contact_author_fax '+81-87-864-2414' _publ_contact_author_phone '+81-87-864-2414' _publ_section_title ; Crystal structure of \b-D,L-fructose ; loop_ _publ_author_name _publ_author_address 'Ishii, Tomohiko' ; Department of Advanced Materials Science Faculty of Engineering Kagawa University 2217-20 Hayashi-cho, Takamatsu Kagawa 761-0396 Japan ; 'Senoo, Tatsuya' ; Department of Advanced Materials Science Faculty of Engineering Kagawa University 2217-20 Hayashi-cho, Takamatsu Kagawa 761-0396 Japan ; 'Yoshihara, Akihide' ; Rare Sugar Research Center Kagawa University 2393 Ikenobe Kagawa 761-0795 Japan ; 'Fukada, Kazuhiro' ; Department of Applied Biological Science Faculty of Agriculture Kagawa University 2393 Ikenobe Kagawa 761-0795 Japan ; 'Sakane, Genta' ; Department of Chemistry Faculty of Science Okayama University of Science 1-1 Ridaicho, Kita-ku Okayama 700-0005 Japan ; _publ_section_synopsis . data_I _database_code_depnum_ccdc_archive 'CCDC 1422317' _chemical_name_systematic ; 1,3,4,5,6-Pentahydroxyhexan-2-one ; _chemical_name_common ; \b-D,L-fructose ; _chemical_formula_moiety 'C6 H12 O6' _chemical_formula_sum 'C6 H12 O6' _chemical_formula_iupac 'C6 H12 O6' _chemical_formula_weight 180.16 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' _cell_length_a 5.43124(19) _cell_length_b 7.2727(3) _cell_length_c 10.1342(4) _cell_angle_alpha 69.120(2) _cell_angle_beta 83.907(2) _cell_angle_gamma 78.381(2) _cell_volume 366.09(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4534 _cell_measurement_theta_min 4.67 _cell_measurement_theta_max 68.35 _cell_measurement_temperature 296 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 192.00 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Rigaku, 1995) ; _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.878 _diffrn_ambient_temperature 296 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 6710 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_theta_min 4.673 _diffrn_reflns_theta_max 68.236 _diffrn_reflns_theta_full 67.687 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 \s(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1329 _reflns_number_gt 1211 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.0950 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_number_reflns 1329 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.1404P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.32 _refine_diff_density_min -0.23 _refine_ls_extinction_method ; SHELXL2013 (Sheldrick, 2015) ; _refine_ls_extinction_coef 0.125(6) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.0492 0.0322 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; _computing_data_collection ; RAPID-AUTO (Rigaku, 2009) ; _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2009) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2009) ; _computing_structure_solution ; SIR2011 (Burla et al., 2012) ; _computing_structure_refinement ; SHELXL2013 (Sheldrick, 2015) ; _computing_molecular_graphics ; CrystalStructure (Rigaku, 2014) ; _computing_publication_material ; CrystalStructure (Rigaku, 2014) ; 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 1.19555(19) 0.09152(15) 0.87814(12) 0.0325(3) Uani d . 1 . . O O2 0.66671(18) 0.27440(15) 0.92243(11) 0.0287(3) Uani d . 1 . . O O3 0.50386(19) 0.33842(16) 0.65941(12) 0.0294(3) Uani d . 1 . . O O4 0.34223(18) 0.76120(15) 0.58108(11) 0.0264(3) Uani d . 1 . . O O5 0.81908(18) 0.84537(14) 0.60893(12) 0.0290(3) Uani d . 1 . . O O6 0.96847(17) 0.47716(14) 0.82413(11) 0.0223(3) Uani d . 1 . . C C1 1.0136(3) 0.1818(2) 0.77318(17) 0.0265(4) Uani d . 1 . . C C2 0.8236(2) 0.34747(19) 0.80373(15) 0.0195(3) Uani d . 1 . . C C3 0.6557(2) 0.46432(19) 0.67791(15) 0.0190(3) Uani d . 1 . . C C4 0.4906(3) 0.6455(2) 0.70256(15) 0.0200(3) Uani d . 1 . . C C5 0.6558(3) 0.77295(19) 0.72899(16) 0.0223(3) Uani d . 1 . . C C6 0.8182(3) 0.6457(2) 0.85210(16) 0.0254(4) Uani d . 1 . . H H1A 1.30779 0.15812 0.86062 0.0390 Uiso calc R 1 . . H H1C 0.92594 0.08085 0.76811 0.0318 Uiso calc R 1 . . H H1B 1.0976 0.23653 0.68208 0.0318 Uiso calc R 1 . . H H2A 0.74136 0.16995 0.97716 0.0345 Uiso calc R 1 . . H H3A 0.55367 0.31042 0.58847 0.0353 Uiso calc R 1 . . H H3B 0.76216 0.5097 0.59244 0.0227 Uiso calc R 1 . . H H4A 0.19353 0.75392 0.60178 0.0317 Uiso calc R 1 . . H H4B 0.37832 0.60041 0.78545 0.0240 Uiso calc R 1 . . H H5A 0.74552 0.94902 0.55285 0.0348 Uiso calc R 1 . . H H5B 0.55062 0.8858 0.75058 0.0268 Uiso calc R 1 . . H H6A 0.92669 0.72507 0.86923 0.0305 Uiso calc R 1 . . H H6B 0.71231 0.59981 0.93633 0.0305 Uiso calc R 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 O1 0.0202(6) 0.0153(5) 0.0465(8) -0.0003(4) -0.0014(5) 0.0066(5) O2 0.0251(6) 0.0190(5) 0.0265(6) 0.0006(4) 0.0037(5) 0.0074(4) O3 0.0292(6) 0.0280(6) 0.0361(7) -0.0153(5) -0.0002(5) -0.0118(5) O4 0.0160(5) 0.0236(6) 0.0298(6) -0.0001(4) -0.0051(4) 0.0019(5) O5 0.0208(5) 0.0154(5) 0.0385(7) -0.0035(4) -0.0014(5) 0.0060(5) O6 0.0186(5) 0.0164(5) 0.0309(6) -0.0004(4) -0.0061(4) -0.0071(4) C1 0.0223(7) 0.0144(7) 0.0389(9) -0.0022(6) -0.0001(6) -0.0054(6) C2 0.0176(7) 0.0123(6) 0.0242(8) -0.0039(5) 0.0003(6) -0.0007(5) C3 0.0177(7) 0.0140(7) 0.0233(8) -0.0070(5) -0.0006(6) -0.0020(6) C4 0.0158(7) 0.0163(7) 0.0213(8) -0.0018(5) -0.0019(6) 0.0013(6) C5 0.0198(7) 0.0131(7) 0.0315(9) -0.0005(5) -0.0002(6) -0.0060(6) C6 0.0272(8) 0.0199(7) 0.0304(8) -0.0015(6) -0.0044(6) -0.0107(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 . . 1.4153(19) no O2 C2 . . 1.4017(16) no O3 C3 . . 1.419(2) no O4 C4 . . 1.4395(16) no O5 C5 . . 1.4305(17) no O6 C2 . . 1.423(2) no O6 C6 . . 1.4298(19) no C1 C2 . . 1.520(2) no C2 C3 . . 1.5304(19) no C3 C4 . . 1.521(2) no C4 C5 . . 1.517(2) no C5 C6 . . 1.5075(19) no O1 H1A . . 0.820 no O2 H2A . . 0.820 no O3 H3A . . 0.820 no O4 H4A . . 0.820 no O5 H5A . . 0.820 no C1 H1C . . 0.970 no C1 H1B . . 0.970 no C3 H3B . . 0.980 no C4 H4B . . 0.980 no C5 H5B . . 0.980 no C6 H6A . . 0.970 no C6 H6B . . 0.970 no 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O6 C6 . . . 113.25(10) no O1 C1 C2 . . . 111.97(14) no O2 C2 O6 . . . 111.23(13) no O2 C2 C1 . . . 112.44(10) no O2 C2 C3 . . . 107.69(10) no O6 C2 C1 . . . 105.55(11) no O6 C2 C3 . . . 109.06(10) no C1 C2 C3 . . . 110.86(13) no O3 C3 C2 . . . 109.62(10) no O3 C3 C4 . . . 110.08(11) no C2 C3 C4 . . . 110.04(13) no O4 C4 C3 . . . 110.05(13) no O4 C4 C5 . . . 109.74(10) no C3 C4 C5 . . . 109.27(11) no O5 C5 C4 . . . 110.97(14) no O5 C5 C6 . . . 107.71(11) no C4 C5 C6 . . . 108.69(11) no O6 C6 C5 . . . 110.67(14) no C1 O1 H1A . . . 109.469 no C2 O2 H2A . . . 109.478 no C3 O3 H3A . . . 109.476 no C4 O4 H4A . . . 109.467 no C5 O5 H5A . . . 109.473 no O1 C1 H1C . . . 109.215 no O1 C1 H1B . . . 109.220 no C2 C1 H1C . . . 109.218 no C2 C1 H1B . . . 109.221 no H1C C1 H1B . . . 107.907 no O3 C3 H3B . . . 109.026 no C2 C3 H3B . . . 109.028 no C4 C3 H3B . . . 109.024 no O4 C4 H4B . . . 109.255 no C3 C4 H4B . . . 109.253 no C5 C4 H4B . . . 109.254 no O5 C5 H5B . . . 109.808 no C4 C5 H5B . . . 109.810 no C6 C5 H5B . . . 109.807 no O6 C6 H6A . . . 109.512 no O6 C6 H6B . . . 109.511 no C5 C6 H6A . . . 109.511 no C5 C6 H6B . . . 109.513 no H6A C6 H6B . . . 108.082 no 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 C2 O6 C6 C5 . . . . -61.73(13) no C6 O6 C2 O2 . . . . -58.74(12) no C6 O6 C2 C1 . . . . 179.03(9) no C6 O6 C2 C3 . . . . 59.88(13) no O1 C1 C2 O2 . . . . -68.49(15) no O1 C1 C2 O6 . . . . 52.95(13) no O1 C1 C2 C3 . . . . 170.90(9) no O2 C2 C3 O3 . . . . -57.21(15) no O2 C2 C3 C4 . . . . 63.99(14) no O6 C2 C3 O3 . . . . -178.02(10) no O6 C2 C3 C4 . . . . -56.82(13) no C1 C2 C3 O3 . . . . 66.18(13) no C1 C2 C3 C4 . . . . -172.62(10) no O3 C3 C4 O4 . . . . -62.10(13) no O3 C3 C4 C5 . . . . 177.33(9) no C2 C3 C4 O4 . . . . 176.97(10) no C2 C3 C4 C5 . . . . 56.41(12) no O4 C4 C5 O5 . . . . -58.98(13) no O4 C4 C5 C6 . . . . -177.25(10) no C3 C4 C5 O5 . . . . 61.77(12) no C3 C4 C5 C6 . . . . -56.50(14) no O5 C5 C6 O6 . . . . -61.97(15) no C4 C5 C6 O6 . . . . 58.34(14) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1A O3 . . 1_655 0.82 2.28 2.9202(14) 135 yes O2 H2A O1 . . . 0.82 2.60 2.9721(14) 110 yes O2 H2A O1 . . 2_757 0.82 1.93 2.7224(13) 161 yes O3 H3A O4 . . 2_666 0.82 1.96 2.7831(18) 177 yes O4 H4A O5 . . 1_455 0.82 2.01 2.7893(13) 158 yes O5 H5A O4 . . 2_676 0.82 2.05 2.8431(12) 163 yes _shelx_hkl_file ; 0 0 1 22.52 1.85 0 0 1 24.78 1.94 0 0 1 25.81 1.66 0 0 1 25.86 1.49 0 0 1 22.46 1.81 0 0 1 23.91 2.10 0 0 1 20.29 1.42 0 0 -1 21.43 1.35 0 0 -1 19.45 1.60 0 0 -1 19.79 1.41 0 0 -1 16.00 1.52 0 0 -1 17.54 1.36 0 0 -1 19.94 1.18 0 0 -1 29.72 1.32 0 0 -1 28.21 1.49 0 0 221893.30 1778.70 0 0 216514.24 1348.25 0 0 213570.89 1115.38 0 0 213973.43 1155.85 0 0 213310.74 1099.52 0 0 -210874.99 897.33 0 0 -212553.31 1032.59 0 0 -215622.21 1275.33 0 0 -218268.30 1490.50 0 0 -220099.62 1632.78 0 0 -219608.79 1590.78 0 0 -212665.98 1049.61 0 0 -214341.03 1184.20 0 0 3 77.04 5.64 0 0 3 82.18 6.12 0 0 3 83.58 7.54 0 0 3 127.35 7.86 0 0 3 75.29 5.10 0 0 -3 80.14 6.03 0 0 -3 78.04 5.09 0 0 -3 81.11 6.84 0 0 -3 81.27 5.24 0 0 -3 66.51 5.33 0 0 -3 76.52 4.02 0 0 -3 87.27 7.23 0 0 -3 72.76 4.49 0 0 412732.77 1005.09 0 0 410727.06 868.71 0 0 412781.07 999.25 0 0 410715.89 853.86 0 0 411508.90 917.92 0 0 4 8402.70 682.73 0 0 4 9679.61 760.95 0 0 411223.71 904.92 0 0 410327.21 825.83 0 0 -4 9554.98 766.93 0 0 -410288.63 825.33 0 0 -411147.16 897.52 0 0 -411864.96 938.88 0 0 -410619.65 856.20 0 0 -411738.43 930.95 0 0 -412424.32 983.54 0 0 5 180.58 12.11 0 0 5 223.57 16.98 0 0 5 309.72 20.42 0 0 5 204.77 14.80 0 0 5 204.32 12.56 0 0 5 210.29 14.58 0 0 5 214.85 17.24 0 0 -5 204.61 15.99 0 0 -5 194.47 14.22 0 0 -5 178.33 10.47 0 0 -5 216.95 13.08 0 0 -5 234.19 15.71 0 0 -5 211.68 12.72 0 0 -5 218.62 16.71 0 0 6 84.76 17.13 0 0 6 83.17 11.26 0 0 -6 85.11 15.82 0 0 -6 78.56 8.43 0 0 -6 86.58 8.43 0 0 -6 86.08 10.55 0 0 -6 93.60 8.80 0 0 -7 137.98 17.31 0 0 -7 156.04 13.49 0 0 -7 138.36 12.94 0 0 -7 143.77 16.69 0 0 -8 1015.09 77.48 0 0 -8 932.06 76.22 0 0 -9 65.95 12.53 0 0 -9 49.97 11.82 0 0 -10 248.36 21.34 0 0 -10 215.37 19.77 0 0 -11 34.49 4.41 0 1 -10 3.99 5.57 0 1 -9 60.42 9.77 0 1 -9 62.36 13.36 0 1 -813027.51 1130.67 0 1 -813367.82 1170.94 0 1 -812410.23 1080.33 0 1 -7 502.24 57.50 0 1 -7 488.61 39.56 0 1 -7 566.62 52.72 0 1 -6 9788.14 805.08 0 1 -6 9560.42 782.77 0 1 -6 9094.18 735.75 0 1 -6 9338.59 766.01 0 1 -5 628.68 41.65 0 1 -5 624.10 41.79 0 1 -5 492.90 29.95 0 1 -5 565.24 37.22 0 1 -5 595.48 37.14 0 -1 5 574.04 40.42 0 -1 5 587.29 38.67 0 -1 5 478.21 34.79 0 -1 5 453.63 31.15 0 -1 5 607.11 36.23 0 1 -4 3201.35 214.23 0 1 -4 3630.80 242.25 0 1 -4 3621.96 252.48 0 1 -4 3465.57 237.07 0 1 -4 3720.82 252.60 0 1 -4 3484.68 242.10 0 1 -4 3473.36 244.79 0 1 -4 3321.25 225.23 0 -1 4 3216.62 219.72 0 -1 4 2884.55 202.58 0 -1 4 3101.51 221.03 0 -1 4 3346.51 236.80 0 -1 4 3495.65 242.96 0 -1 4 3201.74 214.67 0 -1 4 3156.18 212.38 0 -1 4 2908.50 198.17 0 1 -3 52.92 3.67 0 1 -3 41.89 3.99 0 1 -3 41.19 4.71 0 1 -3 79.28 6.91 0 1 -3 44.21 4.97 0 1 -3 44.99 3.68 0 1 -3 46.90 3.31 0 1 -3 42.98 6.24 0 -1 3 37.89 3.84 0 -1 3 45.30 6.74 0 -1 3 46.88 6.94 0 -1 3 42.71 3.35 0 -1 3 48.14 3.50 0 -1 3 47.81 5.42 0 -1 3 40.03 3.29 0 1 -2 2846.21 182.59 0 1 -2 2813.21 184.81 0 1 -2 2751.69 182.82 0 1 -2 2728.79 179.41 0 1 -2 3005.81 196.37 0 1 -2 2952.89 191.81 0 1 -2 2905.06 193.25 0 1 -2 3218.71 207.91 0 -1 2 2787.89 183.18 0 -1 2 2917.53 195.75 0 -1 2 2862.49 192.05 0 -1 2 2892.78 190.68 0 -1 2 3197.68 206.89 0 -1 2 2802.30 179.34 0 1 -1 609.06 36.86 0 1 -1 534.79 27.08 0 1 -1 553.00 29.78 0 1 -1 539.95 29.62 0 1 -1 542.56 28.79 0 1 -1 595.39 34.82 0 1 -1 660.01 36.97 0 1 -1 533.74 29.59 0 -1 1 598.15 37.43 0 -1 1 504.93 28.60 0 -1 1 604.39 32.84 0 -1 1 588.53 33.05 0 -1 1 602.08 36.93 0 -1 1 574.21 34.12 0 -1 1 655.02 33.10 0 1 0 6404.65 453.35 0 1 0 5439.05 386.27 0 1 0 7113.12 503.03 0 1 0 5948.25 423.45 0 1 0 7690.65 542.36 0 1 0 5009.11 355.18 0 1 0 5924.12 420.97 0 1 0 5331.69 371.32 0 -1 0 7322.60 518.90 0 -1 0 5489.94 390.58 0 -1 0 5702.81 405.05 0 -1 0 5224.37 371.17 0 -1 0 5170.75 369.81 0 -1 0 5780.95 411.13 0 -1 0 7933.51 559.07 0 1 1 132.76 5.90 0 1 1 122.43 6.97 0 1 1 131.31 7.42 0 1 1 118.70 7.46 0 1 1 114.13 6.04 0 1 1 170.66 8.89 0 1 1 122.09 8.59 0 1 1 118.53 6.67 0 -1 -1 121.86 7.49 0 -1 -1 173.38 8.97 0 -1 -1 109.47 5.15 0 -1 -1 118.30 6.67 0 -1 -1 111.67 6.27 0 -1 -1 145.54 6.50 0 -1 -1 139.04 7.08 0 1 225631.67 2282.65 0 1 220808.52 1833.23 0 1 220896.76 1869.04 0 1 225847.07 2309.89 0 1 219337.40 1709.64 0 1 225917.20 2287.96 0 -1 -223590.26 2103.37 0 -1 -220937.38 1847.03 0 -1 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461.48 41.50 5 5 0 449.28 32.53 5 5 0 405.53 31.51 -5 -5 0 436.57 39.61 5 5 1 602.68 56.85 5 5 1 668.95 69.98 -5 -5 -1 696.59 55.06 5 5 2 593.19 49.69 5 5 2 633.13 54.44 -5 -5 -2 638.47 50.28 5 5 3 0.14 7.36 5 5 3 1.11 6.88 -5 -5 -3 0.29 5.60 5 5 4 141.34 21.78 5 5 4 152.71 19.93 -5 -5 -4 167.93 15.68 -5 -5 -4 158.59 15.44 5 5 5 201.61 23.85 5 5 5 228.59 22.65 -5 -5 -5 235.20 20.72 -5 -5 -5 182.63 17.65 5 5 6 26.45 10.96 5 5 6 30.74 8.75 -5 -5 -6 32.09 9.93 -5 -5 -6 31.53 9.65 5 5 7 466.48 31.99 5 5 7 564.73 41.65 -5 -5 -7 668.82 48.32 -5 -5 -7 549.24 43.43 -5 -5 -8 377.36 31.89 -5 -5 -8 295.33 38.00 5 6 0 161.80 14.33 5 6 0 202.23 31.88 -5 -6 0 205.81 23.23 5 6 1 508.47 42.31 5 6 1 403.54 32.44 -5 -6 -1 489.96 41.59 5 6 2 1066.14 78.20 5 6 2 910.11 68.82 -5 -6 -2 1033.25 88.11 5 6 3 0.02 5.77 5 6 3 0.93 6.60 -5 -6 -3 0.95 5.54 5 6 4 26.80 8.86 5 6 4 35.48 12.21 -5 -6 -4 29.21 8.97 5 6 5 216.54 17.41 5 6 5 205.18 22.28 -5 -6 -5 224.08 22.49 5 6 6 23.78 9.01 -5 -6 -6 19.26 5.82 5 6 7 33.10 7.65 -5 -6 -7 30.04 7.85 6 -1 -3 32.19 9.11 -6 1 3 32.81 18.81 6 -1 -2 221.38 22.47 -6 1 2 259.12 27.11 6 -1 -1 410.50 49.83 -6 1 1 417.21 36.32 6 -1 0 7.54 10.95 6 -1 0 26.22 5.91 -6 1 0 5.48 9.21 6 -1 1 595.83 45.31 6 -1 1 534.27 45.26 -6 1 -1 612.96 42.33 -6 1 -1 431.09 29.08 6 -1 2 11.42 6.04 6 -1 2 0.50 10.04 -6 1 -2 0.07 4.60 -6 1 -2 0.20 4.30 6 0 -3 -0.14 5.01 -6 0 3 1.77 9.75 6 0 -2 808.14 61.60 -6 0 2 845.73 76.41 6 0 -1 60.54 15.27 -6 0 1 52.06 20.99 6 0 0 8563.29 720.36 6 0 0 7013.17 563.67 6 0 0 7381.59 588.35 -6 0 0 8177.06 679.14 6 0 1 504.40 42.62 6 0 1 512.25 38.27 6 0 1 449.43 37.53 -6 0 -1 506.16 46.16 6 0 2 594.07 44.38 6 0 2 590.85 45.86 6 0 2 513.13 51.77 -6 0 -2 592.11 46.33 -6 0 -2 495.64 41.50 6 0 3 305.30 27.75 6 0 3 275.57 35.56 -6 0 -3 312.07 25.98 -6 0 -3 262.62 28.96 6 0 4 130.59 16.75 6 0 4 122.42 24.92 -6 0 -4 130.19 13.71 -6 0 -4 112.59 13.98 6 1 -3 0.08 14.95 -6 -1 3 9.23 6.27 -6 -1 3 9.31 6.65 6 1 -2 498.90 42.25 -6 -1 2 497.24 34.98 -6 -1 2 484.90 39.51 6 1 -1 539.15 46.67 6 1 -1 633.64 52.18 -6 -1 1 566.14 46.93 6 1 0 989.89 75.64 6 1 0 919.59 68.74 6 1 0 1011.94 74.15 -6 -1 0 1043.26 80.77 6 1 1 270.40 29.35 6 1 1 316.43 45.22 -6 -1 -1 300.22 35.55 6 1 2 4282.87 332.50 6 1 2 4473.11 349.78 6 1 2 4398.76 341.46 -6 -1 -2 4680.22 380.22 6 1 3 221.18 17.76 6 1 3 267.00 28.98 -6 -1 -3 271.70 26.84 -6 -1 -3 231.26 19.95 6 1 4 50.27 14.17 6 1 4 42.06 12.83 -6 -1 -4 47.27 12.43 -6 -1 -4 45.12 9.83 6 1 5 6.27 8.94 6 1 5 5.66 7.55 -6 -1 -5 4.03 11.99 -6 -1 -5 4.34 6.93 6 2 -3 182.68 19.15 -6 -2 3 181.35 19.20 6 2 -2 247.69 23.96 6 2 -2 233.40 17.99 -6 -2 2 256.67 23.14 6 2 -1 261.84 29.83 6 2 -1 282.94 34.68 -6 -2 1 284.83 24.57 -6 -2 1 280.19 23.13 6 2 0 2335.93 171.20 6 2 0 2043.65 145.20 6 2 0 2287.44 169.93 -6 -2 0 2423.16 176.44 6 2 1 187.45 22.84 6 2 1 191.85 24.12 -6 -2 -1 197.94 24.40 6 2 2 485.39 35.53 6 2 2 510.44 60.64 -6 -2 -2 495.12 44.48 6 2 3 18.42 12.41 6 2 3 29.91 11.79 -6 -2 -3 24.79 11.58 -6 -2 -3 6.24 8.62 6 2 4 321.87 32.24 6 2 4 297.85 28.28 -6 -2 -4 321.44 31.14 -6 -2 -4 269.59 22.65 6 2 5 8.90 10.92 -6 -2 -5 18.30 9.86 -6 -2 -5 11.80 7.11 6 3 -2 63.32 11.63 6 3 -2 64.63 9.47 -6 -3 2 73.54 22.04 6 3 -1 40.51 10.09 6 3 -1 44.79 10.50 -6 -3 1 79.18 18.78 6 3 0 1.79 6.08 6 3 0 1.45 4.41 6 3 0 0.65 9.11 -6 -3 0 15.47 5.85 6 3 1 644.07 44.43 6 3 1 581.71 43.73 6 3 1 678.62 56.65 -6 -3 -1 717.99 60.33 6 3 2 1086.50 79.98 6 3 2 1174.28 91.23 -6 -3 -2 1234.90 88.66 6 3 3 60.69 28.12 -6 -3 -3 84.03 15.96 6 3 4 8.21 12.96 6 3 4 222.95 25.64 -6 -3 -4 14.30 11.63 -6 -3 -4 29.37 5.98 6 3 5 282.48 28.64 -6 -3 -5 277.16 26.30 -6 -3 -5 226.96 19.31 6 3 6 508.74 40.63 6 3 6 454.87 36.61 -6 -3 -6 531.18 40.82 -6 -3 -6 401.63 30.33 6 4 0 176.41 19.86 6 4 0 168.56 20.28 -6 -4 0 172.26 17.11 6 4 1 40.29 4.85 6 4 1 45.12 14.54 6 4 1 50.36 23.72 -6 -4 -1 48.98 8.52 6 4 2 33.51 9.86 6 4 2 37.73 13.37 -6 -4 -2 24.16 6.32 6 4 3 755.57 57.26 6 4 3 817.00 64.46 6 4 4 302.67 28.89 6 4 4 334.36 32.15 -6 -4 -4 305.50 33.02 6 4 5 106.21 16.67 6 4 5 113.00 17.27 -6 -4 -5 113.54 15.55 6 5 3 7.94 12.90 6 5 3 5.75 8.31 ; _shelx_hkl_checksum 90860 _shelx_res_file ; TITL 20150618 CELL 1.54187 5.43124 7.27268 10.13419 69.12000 83.90730 78.38060 ZERR 2 0.00019 0.00025 0.00038 0.00210 0.00220 0.00210 LATT 1 SFAC C H O UNIT 12 24 12 L.S. 30 FMAP 2 PLAN -15 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 23.0 ACTA SIZE 0.100 0.100 0.100 WGHT 0.037400 0.140400 EXTI 0.124538 FVAR 4.23251 O1 3 1.195549 0.091523 0.878141 11.00000 0.02019 0.01532 = 0.04654 0.00658 -0.00140 -0.00032 AFIX 147 H1A 2 1.307789 0.158122 0.860620 11.00000 -1.20000 AFIX 0 O2 3 0.666705 0.274399 0.922435 11.00000 0.02506 0.01899 = 0.02652 0.00736 0.00365 0.00057 AFIX 147 H2A 2 0.741364 0.169948 0.977159 11.00000 -1.20000 AFIX 0 O3 3 0.503862 0.338420 0.659415 11.00000 0.02919 0.02797 = 0.03610 -0.01185 -0.00020 -0.01527 AFIX 147 H3A 2 0.553674 0.310425 0.588472 11.00000 -1.20000 AFIX 0 O4 3 0.342233 0.761200 0.581085 11.00000 0.01604 0.02360 = 0.02983 0.00189 -0.00509 -0.00011 AFIX 147 H4A 2 0.193533 0.753916 0.601777 11.00000 -1.20000 AFIX 0 O5 3 0.819084 0.845368 0.608929 11.00000 0.02078 0.01542 = 0.03847 0.00602 -0.00136 -0.00354 AFIX 147 H5A 2 0.745520 0.949022 0.552846 11.00000 -1.20000 AFIX 0 O6 3 0.968475 0.477159 0.824128 11.00000 0.01864 0.01639 = 0.03092 -0.00711 -0.00614 -0.00038 C1 1 1.013587 0.181776 0.773182 11.00000 0.02230 0.01440 = 0.03891 -0.00538 -0.00007 -0.00219 AFIX 23 H1C 2 0.925935 0.080848 0.768110 11.00000 -1.20000 H1B 2 1.097602 0.236535 0.682078 11.00000 -1.20000 AFIX 0 C2 1 0.823604 0.347467 0.803733 11.00000 0.01765 0.01232 = 0.02422 -0.00071 0.00027 -0.00392 C3 1 0.655671 0.464324 0.677906 11.00000 0.01774 0.01396 = 0.02334 -0.00201 -0.00055 -0.00698 AFIX 13 H3B 2 0.762162 0.509695 0.592440 11.00000 -1.20000 AFIX 0 C4 1 0.490592 0.645464 0.702559 11.00000 0.01575 0.01628 = 0.02134 0.00129 -0.00190 -0.00182 AFIX 13 H4B 2 0.378320 0.600413 0.785451 11.00000 -1.20000 AFIX 0 C5 1 0.655816 0.772952 0.728988 11.00000 0.01978 0.01311 = 0.03146 -0.00605 -0.00019 -0.00051 AFIX 13 H5B 2 0.550617 0.885796 0.750575 11.00000 -1.20000 AFIX 0 C6 1 0.818194 0.645690 0.852095 11.00000 0.02716 0.01994 = 0.03037 -0.01070 -0.00442 -0.00148 AFIX 23 H6A 2 0.926694 0.725070 0.869228 11.00000 -1.20000 H6B 2 0.712306 0.599809 0.936334 11.00000 -1.20000 AFIX 0 HKLF 4 REM 20150618 REM R1 = 0.0368 for 1211 Fo > 4sig(Fo) and 0.0404 for all 1329 data REM 115 parameters refined using 0 restraints END WGHT 0.0374 0.1404 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB O1 O2_$1 HTAB O1 O3_$1 EQIV $2 -x+2, -y, -z+2 HTAB O2 O1_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB O3 O4_$3 EQIV $4 x-1, y, z HTAB O4 O5_$4 EQIV $5 -x+1, -y+2, -z+1 HTAB O5 O4_$5 HTAB C1 O3_$1 HTAB C4 O6_$4 EQIV $6 -x+1, -y+1, -z+2 HTAB C6 O2_$6 REM Highest difference peak 0.322, deepest hole -0.233, 1-sigma level 0.052 Q1 1 0.7355 0.4097 0.7429 11.00000 0.05 0.32 Q2 1 0.7397 0.7111 0.7798 11.00000 0.05 0.26 Q3 1 0.5727 0.5586 0.6868 11.00000 0.05 0.22 Q4 1 0.9206 0.2634 0.7938 11.00000 0.05 0.18 Q5 1 0.5270 0.1512 0.5218 11.00000 0.05 0.17 Q6 1 1.0000 0.0000 1.0000 10.50000 0.05 0.17 Q7 1 0.9109 0.0692 0.8212 11.00000 0.05 0.16 Q8 1 1.1075 0.1216 0.8377 11.00000 0.05 0.15 Q9 1 0.5679 0.7116 0.7016 11.00000 0.05 0.15 Q10 1 0.4448 0.6760 0.6639 11.00000 0.05 0.15 Q11 1 0.3411 0.9485 0.5008 11.00000 0.05 0.14 Q12 1 0.7335 -0.0039 0.8939 11.00000 0.05 0.14 Q13 1 0.8433 0.4070 0.9397 11.00000 0.05 0.13 Q14 1 0.5818 0.9954 0.6949 11.00000 0.05 0.13 Q15 1 0.6260 0.1429 0.7143 11.00000 0.05 0.13 ; _shelx_res_checksum 88357